CA1082402A - Process for the rapid, continuous and waterless dye- ing and texturizing and heat-setting textiles and plastic materials - Google Patents
Process for the rapid, continuous and waterless dye- ing and texturizing and heat-setting textiles and plastic materialsInfo
- Publication number
- CA1082402A CA1082402A CA276,337A CA276337A CA1082402A CA 1082402 A CA1082402 A CA 1082402A CA 276337 A CA276337 A CA 276337A CA 1082402 A CA1082402 A CA 1082402A
- Authority
- CA
- Canada
- Prior art keywords
- liquid
- low boiling
- textile
- boiling organic
- dyeing
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired
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Classifications
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06B—TREATING TEXTILE MATERIALS USING LIQUIDS, GASES OR VAPOURS
- D06B9/00—Solvent-treatment of textile materials
- D06B9/02—Solvent-treatment of textile materials solvent-dyeing
-
- D—TEXTILES; PAPER
- D02—YARNS; MECHANICAL FINISHING OF YARNS OR ROPES; WARPING OR BEAMING
- D02G—CRIMPING OR CURLING FIBRES, FILAMENTS, THREADS, OR YARNS; YARNS OR THREADS
- D02G1/00—Producing crimped or curled fibres, filaments, yarns, or threads, giving them latent characteristics
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06C—FINISHING, DRESSING, TENTERING OR STRETCHING TEXTILE FABRICS
- D06C7/00—Heating or cooling textile fabrics
- D06C7/02—Setting
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06P—DYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
- D06P1/00—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed
- D06P1/90—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed using dyes dissolved in organic solvents or aqueous emulsions thereof
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06B—TREATING TEXTILE MATERIALS USING LIQUIDS, GASES OR VAPOURS
- D06B3/00—Passing of textile materials through liquids, gases or vapours to effect treatment, e.g. washing, dyeing, bleaching, sizing, impregnating
- D06B3/10—Passing of textile materials through liquids, gases or vapours to effect treatment, e.g. washing, dyeing, bleaching, sizing, impregnating of fabrics
- D06B3/18—Passing of textile materials through liquids, gases or vapours to effect treatment, e.g. washing, dyeing, bleaching, sizing, impregnating of fabrics combined with squeezing, e.g. in padding machines
Landscapes
- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Mechanical Engineering (AREA)
- Coloring (AREA)
- Treatment Of Fiber Materials (AREA)
- Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
Abstract
Abstract of the Disclosure A process is disclosed for the rapid, continuous and waterless dyeing of textile and plastic materials in which the dyestuff is dissolved, suspended or dispersed in a high boiling solvent, such as glycol or glycol ether, for carrying out the dyeing step per se, after which the dyed textile or plastic ma-terial (after cooling if desired) is subjected to a washing with a low boiling organic liquid such as methanol or ethanol (prefer-ably the former) or a chlorinated hydrocarbon solvent, and sub-sequently dried. The entire series of operations is carried out under nonaqueous or substantially nonaqueous conditions with the complete or substantially complete recovery and recycling of the used dyestuff, the used high boiling solvent, and the used low boiling organic wash liquid. In this way the entire operation is conducted in a relatively inexpensive fashion and in a completely or substantially completely closed cyclic system with essentially complete recovery and reuse of the treating liquids so that not only is the cost of the overall operation greatly minimized but also without any need for pollution of natural water resources such as rivers and wells such as has in the past taken place to a more or less serious extent where effluents of a substantially aqueous nature, but containing serious amounts of polluting sub-stances, were discharged into rivers and the like thereby creating environmental problems.
In the case of textile materials such as woven or knitted fabrics, texturizing and heat-setting thereof may be effected simultaneously with the dyeing operation either to a relatively smaller extent due to the natural moisture pickup of the starting textile material, or to a relatively greater [and predetermined) extent by first incorporating in the textile material a still greater amount of a liquid texturizing agent (e.g., water or methanol) in an amount on the order of 10 to 60% by weight.
Finally, one may omit the dyestuff during the last-mentioned procedure and in that way bring about an excellent texturizing and heat-setting, only, of the textile material.
In the case of textile materials such as woven or knitted fabrics, texturizing and heat-setting thereof may be effected simultaneously with the dyeing operation either to a relatively smaller extent due to the natural moisture pickup of the starting textile material, or to a relatively greater [and predetermined) extent by first incorporating in the textile material a still greater amount of a liquid texturizing agent (e.g., water or methanol) in an amount on the order of 10 to 60% by weight.
Finally, one may omit the dyestuff during the last-mentioned procedure and in that way bring about an excellent texturizing and heat-setting, only, of the textile material.
Description
lOBZ402 This application includes improvements over the invention described and claimed in my prior copending Canadian application Serial No. 267,471, filed January 9, 1976.
.
Said Canadian Application 267,471 describes a process for the rapid, continuous and waterless dyeing of textile and plastic materials in an essentially closed system, with treatment of the textile or plastic material with a dyestuff dissolved, suspended or dispersed in a high boiling solvent for carrying out the dyeing step, followed by cooling and then washing with a 7OW
boilir.g organic liq~!id such as methanol or ethanol, ~oll~wed ~inally by drying. The high boiling organic solvent, the low boiling organic liquid, and the dyestuff are recoveréd and re-cycled in an essentially closed system with resulting advantages in minimizing or eliminating water and air pollution which hereto-fore have created serious environmental problems.
; In addition, the process of the prior application offers distinct advantages in these energy-conscious days by providing substantial economies with respect to the energy requirements for the process.
According to further improvements~ the dyeing procedure of the above-mentioned copending Canad~an application may, if desired, be effectively combined, when treating a textile material such as a woven or knitted fabric, with a texturizing and heat-setting operation thereby resulting in a still further improved textile finishing operation that combines both text-urizing and heat-setting :
~ .
I . . -1-L 1 i 108Z402 ~ .
, on the one hand with dyeing on the other hand, all in one com-~ bined operation and therefore with very substantial savings in ¦~, processing costs.
! j Additionally, by omitting the dyestuff during the pro-¦ cedure mentioned in the preceding paragraph, one may very ~ effectively achieve a texturizing and heat-setting, only, of the ¦ textile material.
In what follows, the rapid, continuous and waterless or essentially waterless dyeing of textile and plastic materials will be described substantially as described in my prior copend-ing app'ication wit~ only minor changes, after which the still further i~provements will be described.
With the current emphasis upon pollution control, it is evident that more effective measures for pollution control are becoming increasingly necessary in view of the stringency of such controls, to say nothing of the cost. In the case of dye plants, it is extremely expensive to treat the effluents from such plants and in some cases a treatment sufficient to bring about approval by environmental protection authorities for the discharge of effluents from the dye plants into ground water -(whether in the form of rivers or wells or the like) is in fact prohi~itively expensive. Indeed, there are communities through-out various parts of the world that do not allow dyeing and finishing plants to be located within their borders.
The present invention has for one of its objects a ~ process for dyeing textile and plastic materials that will I'
.
Said Canadian Application 267,471 describes a process for the rapid, continuous and waterless dyeing of textile and plastic materials in an essentially closed system, with treatment of the textile or plastic material with a dyestuff dissolved, suspended or dispersed in a high boiling solvent for carrying out the dyeing step, followed by cooling and then washing with a 7OW
boilir.g organic liq~!id such as methanol or ethanol, ~oll~wed ~inally by drying. The high boiling organic solvent, the low boiling organic liquid, and the dyestuff are recoveréd and re-cycled in an essentially closed system with resulting advantages in minimizing or eliminating water and air pollution which hereto-fore have created serious environmental problems.
; In addition, the process of the prior application offers distinct advantages in these energy-conscious days by providing substantial economies with respect to the energy requirements for the process.
According to further improvements~ the dyeing procedure of the above-mentioned copending Canad~an application may, if desired, be effectively combined, when treating a textile material such as a woven or knitted fabric, with a texturizing and heat-setting operation thereby resulting in a still further improved textile finishing operation that combines both text-urizing and heat-setting :
~ .
I . . -1-L 1 i 108Z402 ~ .
, on the one hand with dyeing on the other hand, all in one com-~ bined operation and therefore with very substantial savings in ¦~, processing costs.
! j Additionally, by omitting the dyestuff during the pro-¦ cedure mentioned in the preceding paragraph, one may very ~ effectively achieve a texturizing and heat-setting, only, of the ¦ textile material.
In what follows, the rapid, continuous and waterless or essentially waterless dyeing of textile and plastic materials will be described substantially as described in my prior copend-ing app'ication wit~ only minor changes, after which the still further i~provements will be described.
With the current emphasis upon pollution control, it is evident that more effective measures for pollution control are becoming increasingly necessary in view of the stringency of such controls, to say nothing of the cost. In the case of dye plants, it is extremely expensive to treat the effluents from such plants and in some cases a treatment sufficient to bring about approval by environmental protection authorities for the discharge of effluents from the dye plants into ground water -(whether in the form of rivers or wells or the like) is in fact prohi~itively expensive. Indeed, there are communities through-out various parts of the world that do not allow dyeing and finishing plants to be located within their borders.
The present invention has for one of its objects a ~ process for dyeing textile and plastic materials that will I'
-2-f `~` 108Z40Z
eliminate all polluting effluents as well as air pollution that might otherwise result from the dyeing operation.
After the initial capital expenditure for the necessary machinery, the process described hereinafter is relatively inex-pensive and moreo~er requires considerably less energy t~ keep it in operation. The latter feature is in and of itself a further extremely attractive feature of the process in these critical days of energy shortages.
The process of the present invention in one of its em-bodiments involves dyeing the textile or plastic material with the dyestuff dissolved, suspended or dispersed in a relatively high boiling liquid such as a glycol or.~glycol ether, and after the dyeing operation washing the dyed material in a relatively low boiling organic liquid such as methanol or ethanol or a relatively low boiling chlorinated hydrocarbon solvent such as CH2C12, CC14 or C~C13. The wash liquor is then subjected to suitable treatment for recovery and/or separation of the compon-ents thereof, such as by distillation at a relatively low temper-ature, which enables the low boiling organic liquid to be taken over as vapor and thereafter readily conaensed, while the high boiling liquid and residual color or dyestuff remain. The dis-tilled low boiling organic liquid is recovered and continuously recycled through the washing apparatus while the high boiling liquid containing the-residual color is recyclea through the dye-ing appara u after suitably replenishing the color o- dyestuf~
~o~z402 which has been absorbed by the textile material passing through the process.
In one aspect, the present invention resides in a process for texturizing and heat-setting textile material containing a low boiling texturizing agent in liquid phase in an amount sufficient to cause flashing of the low boiling text-urizing agent upon contact of the thus-treated textile material with a high boiling organic liquid at a relatively high temperature, comprising contacting textile material impregnated with the low boiling liquid texturizing agent with the high boiling organic liquid at a high temperature thus texturizing and heat-setting the textile material, cooling the texturized textile material and washing same with a low boiling organic liquid which is free or substantially free of water, followed by drying the texturized textile material, the washing and drying steps being carried out in an essentially closed system, with the separation and recovery of the low boiling organic wash liquid, the low boiling organic wash liquid thus recovered being recycled to the washing step and with the low boiling organic wash liquid vaporized from the textile material during the drying step being recovered, and with the low boiling texturizing agent that is evaporated during the texturizing and heat-setting being removed from the high temper-ature textile material contacting zone as a mixture thereof with vapor of the high boiling organic liquid.
In another aspect, the invention resides in the improvement in a process for dyeing textile or plastic material with a dyestuff dissolved or suspended or dispersed in a high boiling organic liquid which is free or substantially
eliminate all polluting effluents as well as air pollution that might otherwise result from the dyeing operation.
After the initial capital expenditure for the necessary machinery, the process described hereinafter is relatively inex-pensive and moreo~er requires considerably less energy t~ keep it in operation. The latter feature is in and of itself a further extremely attractive feature of the process in these critical days of energy shortages.
The process of the present invention in one of its em-bodiments involves dyeing the textile or plastic material with the dyestuff dissolved, suspended or dispersed in a relatively high boiling liquid such as a glycol or.~glycol ether, and after the dyeing operation washing the dyed material in a relatively low boiling organic liquid such as methanol or ethanol or a relatively low boiling chlorinated hydrocarbon solvent such as CH2C12, CC14 or C~C13. The wash liquor is then subjected to suitable treatment for recovery and/or separation of the compon-ents thereof, such as by distillation at a relatively low temper-ature, which enables the low boiling organic liquid to be taken over as vapor and thereafter readily conaensed, while the high boiling liquid and residual color or dyestuff remain. The dis-tilled low boiling organic liquid is recovered and continuously recycled through the washing apparatus while the high boiling liquid containing the-residual color is recyclea through the dye-ing appara u after suitably replenishing the color o- dyestuf~
~o~z402 which has been absorbed by the textile material passing through the process.
In one aspect, the present invention resides in a process for texturizing and heat-setting textile material containing a low boiling texturizing agent in liquid phase in an amount sufficient to cause flashing of the low boiling text-urizing agent upon contact of the thus-treated textile material with a high boiling organic liquid at a relatively high temperature, comprising contacting textile material impregnated with the low boiling liquid texturizing agent with the high boiling organic liquid at a high temperature thus texturizing and heat-setting the textile material, cooling the texturized textile material and washing same with a low boiling organic liquid which is free or substantially free of water, followed by drying the texturized textile material, the washing and drying steps being carried out in an essentially closed system, with the separation and recovery of the low boiling organic wash liquid, the low boiling organic wash liquid thus recovered being recycled to the washing step and with the low boiling organic wash liquid vaporized from the textile material during the drying step being recovered, and with the low boiling texturizing agent that is evaporated during the texturizing and heat-setting being removed from the high temper-ature textile material contacting zone as a mixture thereof with vapor of the high boiling organic liquid.
In another aspect, the invention resides in the improvement in a process for dyeing textile or plastic material with a dyestuff dissolved or suspended or dispersed in a high boiling organic liquid which is free or substantially
3~ free of water and at a relatively high temperature, followed by cooling the dyed textile or plastic material and washing same ~ 4 -`12' L~
108~402 with a low boiling organic liquid which is free or substantiallyfree of water, followed by drying the washed and dyed textile or plastic material, which improvement comprises carrying out the dyeing, the washing and the drying steps in cyclic manner and in an essentially closed system with the partially exhausted dyestuff liquor from the dy~i~g step being recycled for the treatment of further textile or plastic material to be dyed, with the separation and recovery of the low boiling wash liquor with low boiling wash liquid recovered therefrom being recycled to the washing step and the residual high boiling liquid con-taining residual dyestuff being recycled to the dyeing step, and with the low boiling liquid vaporized from the textile material in the drying step being recovered and returned to the low boiling liquid washing step, and wherein one or more additives for imparting resistance to ultraviolet degradation, improved fastness to light, flame retardance or antistatic properties axe added to the high boiling liquid.
The invention, in a further aspect, resides in the improvement in a process for dyeing a textile or plastic material with a dyestuff dissolved or suspended or dispersed in a high boiling organic liquid which is free or substantially free of water and at a relatively high temperature, followed by cooling the dyed textile or plastic material and washing same with a low boiling organic liquid which is free or substantially free of water, followed by drying the washed and dyed textile or plastic material, which improvement comprises carrying out the dyeing, the washing and the drying steps in cyclic manner and in an essentially closed system with the partially exhausted dyestuff liquor from the dyeing step being recycled for the treatment of further textile or plastic material to be dyed, with the separation and recovery of the low boiling wash liquor with low boiling wash liquid recovered therefrom being recycled ~ - 4a -i~
~08240Z
to the washing step and the residual high boiling liquid con-taining residual dyestuff being recycled to the dyeing step, and with the low boiling liquid vaporized from the textile material in the drying step being recovered and returned to the low boiling liquid washing step, and wherein one or more additives for imparting resistance to ultraviolet degradation, improved fastness to light, flame retardance or antistatic properties are added to the high boiling liquid, and wherein one or more additives for imparting antistatic properties, oil and/or water repellancy, softening properties, or crease-resist-ance are applied to the textile material after washing and before drying.
The invention, in a yet further aspect, resides in the improvement in a process for dyeing a textile or plastic material with a dyestuff dissolved or suspended or dispersed in a high boiling organic liquid which is free or substantially free of water and at a relatively high temperature, followed by cooling the dyed textile or plastic material and washing same with a low boiling organic liquid which is free or substantially free of water, followed by drying the washed and dyed textile or plastic material, which improvement comprises carrying out the dyeing, the washing and the drying steps in cyclic manner and in an essentially closed system with the partially exhausted dyestuff liquor from the dyeing step being recycled for the treatment of further textile or plastic material to be dyed, with the separation and recovery of the low bo_ling wash liquor with low boiling wash liquid recovered therefrom being recycled to the washing step and the residual high boiling liquid con-taining residual dyestuff being recycled to the dyeing step, and with the low boiling liquid vaporized from the textilematerial in the drying step being recovered and returned to the low boiling liquid washing step, and wherein one or more ~ - 4b -additives for imparting resistance to ultraviolet degradation, improved fastness to light, flame retardance or antistatic properties are added to the high boiling liquid, and wherein the textile or plastic material is treated while in a sub-stantially relaxed or untensioned condition.
The dyeing process described herein is particularly desirable in connection with the dyeing of polyester textile materials, by which is meant a textile material based upon polyethylene tereph~halate or the like, but is not limited to the dyeing of such materials. It may be applied to the dyeing of nylon, acrylic, or other well known commercial textile mater-ials, including materials of natural origin such as wool or cotton.
The textile material undergoing any of the treatments described hereinafter may be in any of the conventional forms well known in the art, such as continuous filament yarn, staple yarn, tow, woven or knitted fabric or the like. The yarn may be in the form of a warp of yarn comprising dozens or even hundreds of individual yarn ends.
Although the dyeing of polyester material has advanced considerably in recent years, in most cases it is still necessary to use dyeing assistants such as phenol derivatives. These phenol derivatives are extremely difficult to remove from the effluents of the dyeing operation, and accordingly, the present process represents an especially attractive way of avoiding dif-ficulties from this particular source. Moreover, the instant dyeing process allows a !textile plant, and especially the dye-house, to be located in a water-poor area.
After the textile material has been washed in the low boiling organic liquid, such as methanol, for example, the il~
.~ ~08240;~
textile material is passed into a low temperature dryer in order to remove and recover all traces of methanol.
Although the dyeing step per se may be carried out in any desired manner, one particularly effective way of doing so without departing from the spirit and scope of the present inven-tion is to proceed as described in connection with the apparatus disclosed in my U.S. Patent No. 3,558,260, granted January 26, 1971.
Alternatively, the apparatus dlsclosed in my U.S. Patent No.
108~402 with a low boiling organic liquid which is free or substantiallyfree of water, followed by drying the washed and dyed textile or plastic material, which improvement comprises carrying out the dyeing, the washing and the drying steps in cyclic manner and in an essentially closed system with the partially exhausted dyestuff liquor from the dy~i~g step being recycled for the treatment of further textile or plastic material to be dyed, with the separation and recovery of the low boiling wash liquor with low boiling wash liquid recovered therefrom being recycled to the washing step and the residual high boiling liquid con-taining residual dyestuff being recycled to the dyeing step, and with the low boiling liquid vaporized from the textile material in the drying step being recovered and returned to the low boiling liquid washing step, and wherein one or more additives for imparting resistance to ultraviolet degradation, improved fastness to light, flame retardance or antistatic properties axe added to the high boiling liquid.
The invention, in a further aspect, resides in the improvement in a process for dyeing a textile or plastic material with a dyestuff dissolved or suspended or dispersed in a high boiling organic liquid which is free or substantially free of water and at a relatively high temperature, followed by cooling the dyed textile or plastic material and washing same with a low boiling organic liquid which is free or substantially free of water, followed by drying the washed and dyed textile or plastic material, which improvement comprises carrying out the dyeing, the washing and the drying steps in cyclic manner and in an essentially closed system with the partially exhausted dyestuff liquor from the dyeing step being recycled for the treatment of further textile or plastic material to be dyed, with the separation and recovery of the low boiling wash liquor with low boiling wash liquid recovered therefrom being recycled ~ - 4a -i~
~08240Z
to the washing step and the residual high boiling liquid con-taining residual dyestuff being recycled to the dyeing step, and with the low boiling liquid vaporized from the textile material in the drying step being recovered and returned to the low boiling liquid washing step, and wherein one or more additives for imparting resistance to ultraviolet degradation, improved fastness to light, flame retardance or antistatic properties are added to the high boiling liquid, and wherein one or more additives for imparting antistatic properties, oil and/or water repellancy, softening properties, or crease-resist-ance are applied to the textile material after washing and before drying.
The invention, in a yet further aspect, resides in the improvement in a process for dyeing a textile or plastic material with a dyestuff dissolved or suspended or dispersed in a high boiling organic liquid which is free or substantially free of water and at a relatively high temperature, followed by cooling the dyed textile or plastic material and washing same with a low boiling organic liquid which is free or substantially free of water, followed by drying the washed and dyed textile or plastic material, which improvement comprises carrying out the dyeing, the washing and the drying steps in cyclic manner and in an essentially closed system with the partially exhausted dyestuff liquor from the dyeing step being recycled for the treatment of further textile or plastic material to be dyed, with the separation and recovery of the low bo_ling wash liquor with low boiling wash liquid recovered therefrom being recycled to the washing step and the residual high boiling liquid con-taining residual dyestuff being recycled to the dyeing step, and with the low boiling liquid vaporized from the textilematerial in the drying step being recovered and returned to the low boiling liquid washing step, and wherein one or more ~ - 4b -additives for imparting resistance to ultraviolet degradation, improved fastness to light, flame retardance or antistatic properties are added to the high boiling liquid, and wherein the textile or plastic material is treated while in a sub-stantially relaxed or untensioned condition.
The dyeing process described herein is particularly desirable in connection with the dyeing of polyester textile materials, by which is meant a textile material based upon polyethylene tereph~halate or the like, but is not limited to the dyeing of such materials. It may be applied to the dyeing of nylon, acrylic, or other well known commercial textile mater-ials, including materials of natural origin such as wool or cotton.
The textile material undergoing any of the treatments described hereinafter may be in any of the conventional forms well known in the art, such as continuous filament yarn, staple yarn, tow, woven or knitted fabric or the like. The yarn may be in the form of a warp of yarn comprising dozens or even hundreds of individual yarn ends.
Although the dyeing of polyester material has advanced considerably in recent years, in most cases it is still necessary to use dyeing assistants such as phenol derivatives. These phenol derivatives are extremely difficult to remove from the effluents of the dyeing operation, and accordingly, the present process represents an especially attractive way of avoiding dif-ficulties from this particular source. Moreover, the instant dyeing process allows a !textile plant, and especially the dye-house, to be located in a water-poor area.
After the textile material has been washed in the low boiling organic liquid, such as methanol, for example, the il~
.~ ~08240;~
textile material is passed into a low temperature dryer in order to remove and recover all traces of methanol.
Although the dyeing step per se may be carried out in any desired manner, one particularly effective way of doing so without departing from the spirit and scope of the present inven-tion is to proceed as described in connection with the apparatus disclosed in my U.S. Patent No. 3,558,260, granted January 26, 1971.
Alternatively, the apparatus dlsclosed in my U.S. Patent No.
4,055,971 granted November 1, 1977 may also be employed.
After the textiie material leaves the dyeing a~paratus, it is preferably passed through a cooling zone where its tempera-ture is reduced from an elevated temperature just below the boiling point of the low boiling organic solvent to (for example) about 140~F, after which it is then passed through a washer where it is washed with the low boiling organic liquid such as (and preferably) methanol.
The washing step may ~e carried out in any conventional manner, although preferably I employ a cascade washing system involving a series of washing steps according to which the methan-ol is introduced just ahead of the point where the textile or plastic material leaves the washer and then is passed concurrentl~
with respect to the direction of movement of the textile material and through a series of "cascade" zones back to a point just afte~
the textile material enters the washing apparatus where the ..
.
~` 108240Z
concentration of high boiling liquid and residual unfixed color or dyestuff carried therein is the greatest.
The methanol or other low boiling organic wash li~uor is then passed to a suitable separatory device such as aistilla-tion apparatus where the methanol is distilled off at a relatively low temperature, condensed, and then returned to the methanol washing device.
The textile material after passing through the low boiling organic liquid washing device is then passed into a low temperature dryer to evaporate residual low boiling organic liquid (e.g., methanol) still clinging to tLe textile material.
The methanol thus evaporated is passea overhead to a condenser where it is condensed and, if desired, returned to the methanol washing step.
The textile material then leaves the dryer in finished form ready for such further treatment as any dyed textile mater-ial may be conventionally subjected to thereafter.
As indicated above, the partially exhausted dyestuff liquor leaving the dyeing step is recycled to the dyeing step, after addition of make-up dyestuff as desired and/or make-up glycol or glycol ether as desired, as well as with the addition of the glycol or glycol ether recovered from the distillation apparatus.
After a given dyelot of textile material has been com-pleted, the glycol or glycol ether containing the dyestuff may be separately stored and used again when a similar shade of dyeing . ..
is to be repeated. In the meantime, the dyeing apparatus can be cleaned very readily with the low boiling organic liquid, such as methanol, and the methanol thus employed may be returned to the ~ distillation unit for purification and separation and recycling to the methanol washing step for the next dyelot.
The process of this embodiment of the present invention may be further illustrated by reference to the accompanying draw-ings where (in ~igure 1) the various steps are shown in schematic fashion.
Reference numeral 1 represents the incoming textile ma-terial to be dyed which passes into the dyeing apparatus 2.
There i.t is subjected to the action of an appropriate dyestuf~
dissolved, suspended or dispersed in a suitable high boiling or- ¦
ganic liquid such as ethylene glycol, diethylene glycol, triethyl-ene glycol, tetraethylene glycol, propylene glycol, or the methyl-or ethyl- mono- or di-ether of such glycols.
The partially exhausted dyestuff liquor is removed from the dyeing apparatus 2 via line 3 from which it passes to a . storage chamber or sump 4 for the residual dyestuff-high boiling liquid mixture. From sump 4 the dyestuff-high boiling liquid mixture is recycled via line 5 to the dyeing apparatus 2, passing through a conventional heat exchanger Sa.to adjust it to the desired temperature of dyeing.
. Make-up dyestuff is added when and as needed via line 6 and make-up high boiling liquid is added when and as needed via line 7.
The textile material passes from the dyeing chamber via line 8 to a cooling chamber 9. There the d~ed textile material .
Il 1082402 . i I
¦ is cooled from a temperature of just below the normal boiling point of the high boiling organic solvent down to a temperature of (for example) about 140~F by passing cooling air into the cool-~ ing chamber 9 via line 10 and out via line 11. Excess non-fixed i dyestuff and excess high boiling liquid is removed from the ¦ textile material by conventional means (not shown) such as by passing the textile material between squeeze rolls near the exit end of the cooling chamber 9. This excess non-fixed dyestuff ln admixture with the excess high boiling liquid is returnëd to the dyestuff liquor sump 4 via line 3a.
The dyed material, now cooled and at least partially freed of excess non-fixed dyestuff and excess high boiling liquid, is shown at 12 as passing into a low boiling organic liquid washing device 13 where it is subjected to washing to remove re-sidual high boiling liquid and residual (non-fixed) dyestuff.
The organic wash liquid may conveniently be methanol or other low boiling aliphatic alcohol or a chlorinated hydrocarbon of the kind mentioned above. Methanol is preferred Wash liquor leaves the methanol washer 13 via line 14 and is passed to recovery apparatus 15 which may suitably take the form of distillation apparatus. There the relatively volatile low boiling organic liquid, such as methanol, is distilled away ~rom the high boiling liquid, condensed and returned via line 16 to the methanol washing apparatus 13. Make-up methanol may be introduced when and as needed via line 17.
. i. ~08240Z
I
Returning to the separator~ or distillation apparatus . 1 15, the recovered high boiling organic liquid with the residual dyestuff which remains after the vaporization of the methanol . ¦ therefrom is recycled via line 18 to the partially exhausted ¦ dyestuff liquor sump 4, whereby it is returned to the dyeing operation carried out in dyeing apparatus 2.
The textile material aftex the washing step is passed as shown by reference numeral 22 into the dryer 23 where it i5 contacted with air introduced via line 24. This air may be warm or hot, as obtained from ~ heating device (not shown). The air passes through and/or in contact with the washed textile material . picking up residual low boiling organic liquid still clinging to the textile material, an~ leaves the drying device 23 via line 25. The air leaving via line 25, and carrying vapors of the low boiling organic liquid, is then passed into a condenser 20 where the low boiling organic liquid is recovered and recycled to the methanol washing step via line 21. The air is removed from the condenser 20 via conventional vent means not shown. Alter-natively, the methanol vapor (with residual air) leaving via line 25 may be separately disposed of, such as by burning in a waste heat boiler (not shown~ to effect still further economies in o~eration.
losZ402 1 !
In this manner the dyed, (optionally) cooled, washed and dried textile or plastic material leaves the dryer 23 as shown at 26 as a finished dyed textile or plastic material ready for such other textile treating operations as may be desired.
It will be noted from the description o~ the schematic drawing of Figure 1 thus described that the material flow is com-pletely cyclic in nature with no or essentially no liquid efflu-ents from the system. Consequently, the system is completely free from problems normally associated with dye plants where aqueous or largely aqueous systems are involved and wherein the aqueous systems at some point or another must be discharged from the plant into rivers or wells or other surface water thereby creating effluent problems of an environmentally undesirable nature.
Moreover, the use of the low boiling organic li~uid for washing purposes requires a significantly lesser energy input to the system, which is an additional highly desirable feature of the process.
By way of still further illustration, the following examples of dyeing are set forth:
Example 1 A nyion fabric, type 66, is dyed in ethylene glycol con-taining 1/2~ of Acid Blue ~25. ~he sample is dyed at 300~F for 12 seconds. After cooling, the sample is washed in methanol and then dried at a low temperature. This dyeing gives a heavy blue shade with much better fastness properties than dyeing by conven-tional methods. Moreover, the partially exhausted dyestuff liquor ..
~j after addition of makeup ethylene glycol is returned to the dyeing operation. The wash methanol is distilled for recovery and recycling of recovered methanol.
I Example 2 ~ ~ polyester fabric is dyed in a dye-liquor containing ethylene glycol and 1/2% of Disperse Blue ~56. The polyester material is dyed at 320F for 30 seconds. After dyeing, the sample is then washed in methanol and dried at a low temperature.
The dyeing results in a full blue with excellent fastness proper-ties. Separation and recovery of both the ethylene glycol and methanol may be as described above.
Example 3 A wool fabric is dyed in ethylene glycol containing 1/2~ of Acid Blue ~25. The sample is dyed at 300F for 12 seconds After cooling, the sample is washed in methanol and then dried at a low temperature. This dyeing gives a heavy blue shade with much better fastness properties than dyeing by conventional me-thods. Moreover, the partially exhausted dyestuff liquor after addition of ma~eup ethylene glycol is returned to the dyeing operation. The wash methanol is distilled for recovery and re-cycling of recovered material in the manner ~escribed above.
Example 4 An acrylic fabric is dyed in a dye-liquor containing ethylene glycol and 1/2~ of Disperse Blue ~56. The acrylic ~ mater 1 is dyed at 320~P for 30 seconds. After dyeing, the . 108Z40Z
sample is then ~Jashed in methanol and dried at a low temperature.
The dyeing results in a full blue with excellent fastness prop- !
I erties. Separation and recovery of both the ethylene glycol and ¦
¦ methanol may be as described above.
It should be noted in passing that I do not claim to be the first to have suggested the step of dyeing a textile material in a nonaqueous dye bath such as a glycol or a glycol ether.
Societa Rhodiaceta's French Patent No. ~55,260 (and the generally corresponding Swiss Patent No. 230,891) suggested such a step for the dyeing of nylon many years ago. Moreover, more recently Laucius et al, in J. S. Patent Mo. 2,.~82,119, suggested the dyeing of polyester in a nonaqueous dyebath comprising various glycols. See also Olpin et al U. S. Patent No. 2,461,612.
Moreover, I do not claim to be the first to suggest the step per se of washing dyed textile products with a low boiling or-ganic liquid, such as an alcohol, because that too was suggested in the Societa Rhodiaceta patents mentioned above, although there it is a matter of indifference whether water or a low boiling alcohol is employed as the washing liquid. See the French patent at page 2, lines 58 et ~ However, neither the prior art just cited nor any other prior art, so far as I am aware, has sugges-ted, much less recognized, the desirability of operating the dyeing and washing steps in the manner indica-ted herein with complete or substantially complete recycling of the various ma-terials involved and with a completely or substantially co~pletel~
nonaqueous system, for the sake of lesser costs, and more ~ I
!i 1 1, 1 importantly, with a view to present-day environemntal and energy conservation considera~ions.
' It is to be particularly noted in connection with this 1 embodiment of the present invention that it conveniently provides ~ what is in e~fect a nonaqueous or substantially nonaqueous closed j or essentially closed treating system, and therefore with no need to discharge potentially polluting aqueous wastes to ground water. If as a result of long-continued operationt a build-up of significant (though still relatively small) amounts of water should occur, such as from the use of aqueous dye concentrates to make up the dilute dyestuff-high boiling organic liquid treating s()lution and/or from moisture unavoidahly present in the air used for the cooling and drying steps, such water can be easily re-moved from any of the treating liquids by conventional means (not shown) such as by passing same through a bed of a commercial dehydrating agent such as Drierite.
The description up to this point has dealt primarily with dyeing alone. Hereinafter descripti~e matter relating to dyeing combined with texturizin~, as well as descriptive matter relating to texturizing alone, is presented.
Texturizing, etc. In the case of a textile material such as woven or knitted fabric, as distinguished from a plastic material in the form of a film, the surface-to-volume ratio is substantially highex due to the yarn structure of the woven or knitted textile material. Consequently, there will normally be a certain amount of moisture pickup from the atmosphere so that at least some texturizing and heat-setting will take place when the textile material is brought into contact with the hot hi~h oiling organic liq~id.
Generally, however, where it is desired to secure a really significant degree of texturizing and heat-setting simul-I taneously with the dyeing~ a pre-treatment Gf the textile materia~
¦ to incorporate therein a low boiling liquid texturizing agent j will be preferred. This objective is achieved very conveniently by simply passing the woven or knitted textile material through a bath of low boiling liquid texturizing agent (such as water or methanol) so as to incorporate therein a predetermined amount of low boiling liquid texturizing agent, such as of the order of 10 to 60~, on a weight basis. Where water is selected as the low ~oiling liquid texturizinq agent, a convenient way of incorporat-ing the desired amount of water in the woven or knitted textile material is to contact same with steam from a series of steam jets, or else with very fine jets of water, with the jets placed above and/or below the path of travel of the textile material just prior to its contact with the hot high boiling organic liquid; for example, as the woven or knitted textile material is introduced into the process viaan otherwise conventional tenter-frame arrangement.
Thus, in order to effect the texturizing and heat-settin mentioned above, the textile material undergoing processing is first treated with a low boiling texturizing agent, such as water or methanol in the liquid phase, or in the case of water, in the form of steam or very fine sprays. The amount of low boiling texturizing agent employed for this purpose will vary, depending on the degree of texturizing desired It is preferably in the I
¦ range of from 10 to 60% by weight, based on the weight of the textile material. It is of course necessary to employ sufficient ~ of the low boiling texturizing agent to impart the desired de-¦ gree of texturizing and heat-setting, while at the other extreme it is necessary to avoid employing so much as to defeat the purpose of the texturizing operation. The amount, in any case, will be such that when the textile material containing the low boiling texturizing agent in liquid phase is subjected to the hot dyestuff-containing high boiling organic solvent, this brings about an "explosion", as it were, or a flashing of the low boiling liquid to vapor, thus producing a volumization or bulking of the textile material.. The net result of this procedure is to bring about the desired texturizing and heat-setting of the textile material while it is being dyed.
As shown in Figure 2, the textile material is first passed through a trough 200 containing the low boiling liquid texturizing agent by means of a series of guide rolls 202, and thence between squeeze rolls 204 by means of which the liquid texturizing agent in excess of the desired predetermined amoun~
to be left in the textile material is removed and (in the case of methanol) returned to the trough 200 via line 206. When methanol is used, suitable hoods or enclosures (not shown) are pro~ided for the protection of the workmen and to minimize any fire hazard. The thus-treated textile material is then passed to the dyeing step 2 and the succeeding steps of Figure 1 as a consequence of which texturizing and heat-setting are combined with dyeing.
..
`
Il 1082402 The low boiling texturizing agen~ present in the tex-tile material in liquid phase, and which thereafter is subjected ¦
to the relatively high temperature of the hot dyestuff-containing ~ high boiling organic solvent in 2, flashes off during the dyeing operation and is removed via line 210. This low boiling liquid which is flashed off in the form of vapor will then be associated !
with some vapor of the high boiling organic solvent such as glycol, some of which indeed may be present in the form of par-ticles of "mist". This mixture is passed through a recovery system which may take the form of a condenser and/or filter 212, thereby assuring the separation and removal of substantially all of the high boiling organic solvent including the mist particles.
The condensate and/or filtrate may then be passed to a fraction-ator 214 for the removal of substantially all of~the low boiling liquid, with the remaining high boiling organic solvent being recycled to the dyestuff sump 4 via line 216. The low boiling liquid (if methanol) is thus separated and reused, or int~e case of water, it will be evaporated from the high boiling liquid in the dyestuff sump 4. In the event the low boiling texturizing agent is methanol, the reclaimed methanol may be conveniently condensed and recycled for use at a later stage of the process such as in the washing step. On the other hand, the reclaimea methanol without condensation may be sent directly-.
. .
.
- ~ ~ _t ~ to a waste heat boiler where it can be burned, thereby reducing j the energy requirements for the system derived from the burning ~ of valuable fossil fuels.
j Alternatively, the low boiling texturizing agent may be introduced into the textile material in the desired predetermined amounts, via sprays of fine jets of liquid water or methanol, or 3ets of steam, located above and/or below the path of travel of . the textile material just prior to its introduction to the dyeing step 2 of Figure 1.
The texturizing and heat-setting is performed under con-trolled conditions of a predetermined relatively high temperature and a predetermined content of low boiling liquid.texturizing agent. The textile material when in the form of woven or knittea ......... ... ... .... ... goods may be conveniently introduced into-the process by means of a conventional tenter-frame that can be adjusted to overfeed the textile material lengthwise, and including also provision for narrowing the tenter-frame to texturize wiathwise as well. In this way the degree of texturizing and heat-setting in either.the . length direction or the width direction (or both) may readily be - 20 controlled.
. As a still further embodiment of the invention, if one wishes only to texturize and heat-set the textile material with-. out at the same time dyeing same, one need only refrain from : adding a dyestùff to the high boiling organic liquid and instead otherwise proceed as already described.above, with the pre-treat-l ment such in Figure 2 followed by treatment as in Figure 1.
I
. .
. -17-~o~240z ¦1 Most texturizing yarns for weaving or knitting are in ¦¦ the 100 denier range. The actual cost of separately texturizing 100 denier yarn is about $0.22 per pound. To texturize a 30 ¦ denier yarn costs about $1.10 per pound, since the machine time I for 30 denier yarn is about four times the machine time for 100 ¦ denier yarn for equivalent number of pounds produced. At the present time, due to high cost there are no fabrics available made from texturized 30 denier yarns. By weaving or ~nitting an untexturized 30 denier yarn and then texturizing the resulting woven or knitted article as described herein, the texturizing can be done at substantially no additional cost during the dyeing operation. The remarkable savings thus made possible by the present improved operation combining both texturizing and dyeing offer vast possibilities for increased markets for texturized and heat-set woven and knitted textile materials o~ the finest denier. Consequently, the industry will have available a wider selection of textile materials readily adaptable for fabrication into natural-silk-like articles of manufacture.
It should be mentioned that when the procedures des-cribed herein include a texturizing and heat-setting operation, either alone or in combination with dyeing, it is important that the textile material shall be in a relaxed or relatively unten-sioned condition during the texturizing. This can be assured ~y supporting the textile material on an endless traveling tenter-~5 irame.
~' , It will be understood that no claim is made broadly to texturizing per se, since such texturizing has long been known;
e.g., see my U.S. Reissue Patent No. Re. 27,773. The treatment des-cribed herein may also have the additional beneficial effect of minimizing pilling when treating, e.g., polyester--see my U.S. Patent No. 2,938,811.
Still further details on texturizing are as follows:
Texturizing and voluminizing are performed on a Hermesol machine (see my U.S. Patent 4,055,971, granted November 1, 1977).
The greige goods coming off the loom or knitting machine are fed into a tenter-frame, with overfeeding of the material.
On the way to the dyeing chamber, the textile material is wetted between 20 and 60% with a low boiling solvent. As the tenter-frame enters the Hermesol dyeing chamber, the tenter-frame, with the textile material in place, is contracted to a predetermined width.
Immediately upon entry of the wetted textile material into the dyeing chamber, an "explosion" occurs; thus causing the yarn, in both the widthwise and lengthwise directions, to become entangled; thus texturizing the yarn in a woven or knitted fabric. It is thus possible to by-pass a separate expensive tex-turizing process of synthetic materials in yarn form.
Example 5 A woven polyamide fabric, constructed with a 60 denier warp and a 70 denier filling weighing 50 grams per square meter, after texturizing as previously described, weighed 86 grams per square meter showing a texturizing and shrinkage of 22% in the ~B
Il ~08240Z i . !
¦ warp and 22% in the filling. Another woven polyamide fabric j constructed of a 70 denier warp and 70 denier filling weighed 51 grams per square meter before texturizing. After texturizing, it weighed 82 grams per square meter showing a texturizing and ~ shrinkage of 22% in the warp and 17% in the filling.
¦ Example 6 A woven polyester fabric, constructed with 3 ply, 100 denier polyester yarn in both warp and filling before texturizing, weighed 115 grams per square meter, and after texturizing, 177 grams per square meter, showing a warp shrinkage of 19% and a fil _ ling shrinkage of 18%.
Example 7 A woven polyester and ~ol fabric constructed of 3 ply, 100 denier in the warp and 100~ wool in the filling, weighed 139 grams pér square meter. After texturizing, it weighed 169 grams per square meter, showing a shrinkage of 18~ in the warp and ~%
volumimizing of the wool.
Example 8 A polyamide, tubular, knitted fabric, constructed of 110 denier yarn, weighed 121 grams per square meter, and after texturizing, the weight was 169 grams per square meter.
Example 9 A polyester, tubular, knitted fabric, constructed of 100 denier polyester, weighed 118 grams per square meter, and after texturizing, 198 grams per square meter.
A11 of the aforementioned fabrics were wetted with a very fine water spray before entering the dyeing chamber.
In all cases the high boiling liquid in the dye chamber was ethylene glycol. The high temperature high boiling liquia was at a temperature of 175C, while for the polyamide, the temperature of the dyeing liquid was 155C.
While the textile material was being texturized and voluminized in the dyeing chamber, it was simultaneously heat-set; thus saving another expensive operation in conventional fabric finishing.
After this fabric passed through the dyeing chamber, it was then cooled in another chamber and here the excess ethylene glycol was removed from the fabric.
From the cooling chamber, the textile material was washed in methanol. After the methanol wash, the excess methanol was removed and the textile material was then dried at 93C.
Reference is made to my U.S. Patent No. 3,530,214 entitled "Method for Treating Textile Materials to Uniformly Set Their Shape"; to my U.S. Patent No. Re.27,773 entitled "Method for the Continuous Texturizing or Voluminizing of Textile Materials"; and to my U.S. Patent No. 2,938,811 entitled "Method of Conditioning Polyester Textile Material and the Resulting Products".
Woven polyester fabric constructed with 70 denier polyester yarn in both warp and filling weighed 40 grams per square meter and after texturizing, 61 grams per square meter.
The warp showed a texturizing and shrinkage of 20%, while the filling showed 17~. In the previous sample, only clear ethylene glycol was used in the dyeing chamber. In the present sample, 2 grams of Dispersed Blue 56 per liter was added to the ethylene glycol resulting in a deep blue dyeing on the polyester material.
Otherwise, the fabric was handled as described before. In one operation, the textile material was texturized, voluminized, ~, Il 1082402 .` ....... I
¦ heat-set and dyed. The washing of dyed materials in methanol is superior to the use of ~ny other washing or cleaning method. In ~ the case of dyed polyester, it is unnecessary to give a chemial ¦ wash to remove excess and unfixed dyestuff to prevent crocking.
A polyamide flat-knitted fabric, constructed of 30 denier polyamide weighing 55 grams before texturizing and 78 grams after texturizing, was exposed in the dyeing chamber at a temperature of 155C, to ethylene glycol containing 3 grams per liter of Acid Red No. 151. The fabric was dyed a deep red.
Here, again, the fabric was texturized, heat-set and dyed in one operation. As mentioned before, the }igh boiling liquid in all the aforementioned samples was ethylene glycol and in the case of fabrics containing polyester, the temperature was 175C and in the case of polyamides, the temperature was 155C. In all the aforementioned examples, the exposure time in the dyeing chamber was 20 second The glycol and methanol were recycled.
In all the aforementioned examples, the fabrics were constructed of untexturized, drawn yarns.
;~ Still further detailed examples are as follows:
Example 10 A polyester double knit fabric, 285 grams per linear meter, is dyed continuously in a dye liquor containing ethylene glycol and 1.0 gram per liter (g/l~ of Disperse Blue ~56 (crude, unstandardized) and 0.5 g/l of phosphoric acid at 175C for 45 seconds, the dye liquor being applied to the moving web of fabric by spraying from a circulating reservoir of dye liquid at the 108Z~O~
¦ rate of 375 liters per minute (lpm). The fabric after exposure to the dye liquor is then conducted through a cooling chamber I where cool air impinges on the surface of the fabric to lower the ¦ temperature of said fabric to 70C, after which the fabric is washed by spraying with methanol at 10C to remove residual glycol and surface dye. The fabric is then passed into a drying chamber where hot air at 110C impinges on both fabric surfaces simultaneously to remove the last traces of methanol; The par-tially exhausted dye liquor, after addition of make-~p ethylene glycol and dye, is returned to the dyeing operation. -Spectrophometric measurement of sam~les of circulating dye liquor ana reflectance measurements of thP dyed cloth during the course of dyeing 365 meters of cloth showed a depletion of 15% of the original dyebath concentration due to exhaustion which is made up for by adaing to the aforementioned ma~eup ethylene glycol.
Methanol used in the washing step is collected, along with ethylene glycol and a small amount of dye, ana fractionally distilled from the high-boiling glycol and then returned to the washing stage. The residue of the distillation is returned to the dye makeup tank. Methanol was distilled off at the rate of 3,785 liters per hour.
The abric was overfed into the dyebath by 10~ and allowed to shrink 10% in the width-wise direction.
The dyed fabric i5 a bright blue, uniformly coverin~
the entire fabric surfaces and having excellent fastness proper-ties. Penetration of the fabric and the individual fibers is ¦~ excellent.
.:.
l -23- l ~082402 Example 11 ¦ A nylon type 66 tufted carpet fabric, weighing 625 ¦! grams per square meter of surface fiber, is dyed continuously l in a dye liquor containing Disperse Blue ~56 (crude, unstandard-~ ized) and 0.5 g/l phosphoric acid at 155C for 45 secon~s, the dye being applied to the carpet fabric by spraying, followed by cooling, washing and drying in the manner described in Example 5, including recycling of glycol and methanol.
The resultant dyeing is uniformly level.
In practicing this invention, it may also be advantag-eous to include dyebath additives to impart resistance to ultra-violet degradation of polyester and nylon, improved fastness to light, flame retardance, antistatic properties, and the like.
For example, the following chemical reagents can be ad~ed to the 15 ~ dyebath In of Figure 1 for the following ob; ecti~es:
.
,~; , ' ~`; .
.
~ -24-Table I
Reagent Ch~nical O~nposition Fil~er Advantages "Uvinul D-49" 2,4-dimet~xy-b~zopher~one Polyester (&~c Greatly improved (trad~nark) (made ~y General Aniline & U.S. Patent No. light fastness &
Film (G~F)) 3,943,105) fabric stability "Uvinul D-49" Do Polyamide (See ~proved light U.S. Patent N~. fastness an~l sun-3,771,949) light stability "Tinuvin 327" Benzc)triazole derivative Polyamide (See nnpr~ light (trademark) (made by Ciba/Geigy) U.S. Patent N~. fastness 3,771,949) ~:
"Uvinul 490" Benzophen~ne derivative Polyester (See ~proved light (trad~nark) (made by G~F) U.S. Patent N~. fastness and 3,943,105) fabric stability "Anti-Blaze Chlorinated phosphonate Polyester Flan~ retardance 19" (made by ~bil Ch~mical Polyamide (trad~ark) Co.) "Fir~naster ~ris-dibraTopropyl- Polyes~r Flame retardance 200" p}sphate (made by Acrylic ~-(trademark) Michigan Chemical Co.) :-(See also my U.S. Patent No. 3,943,105 for additional disclosure relative to ultraviolet absorbers.) 1:2 . ~ ", ~
10t~Z402 ¦ At a later stage of the process, antistatic agents, oil ¦ and water repellents, softening ana other hand-modifying agents, i crease-resisting resins, and the like may be applied to the ¦ fabric(s) such as at reference numeral 22 in Figure 1 of the accompanying drawings (i.e., between methanol washing and drying). .
These agents may be applied to the washed textile material in the form of a solution or dispersion of the selected agent in a solvent or other suitable carrier.
The following Table II illustrates these treatments:
1o8240Z
Table II
Chemical Ckmposition or Other Identifi-Reagent cation Fibex (s) A~vantages "Avitex E" Antistatic Agent Cell~losic, animal and Excellent anti-(trademark) (made by DuPont) synthetic fibers, e.g., static properties Polyamide, Polyester, even at low humid-Acrylic, Olefin, etc. ities "Siligan PA"Antistatic Agent Do Do (trademark) (made by EASF Wyan-dotte) "Statexan Antistatic Agent Do Do PKN" (made by Bayer Far-(trademark) ben Industries) "Zepel" Fluorinated Compound Polyamide, Polyester, Excellent oil, (trademark) (made by DuPDnt) Acrylic and other oe l- water and soil lulosic synthetics, resistance and animal fibers "SOotchr FluDroc æbon Com~ Do Do gard" pound (made by (trademark) Minnesota Mining &
Manufacturing Co.) "Avibone A"Nbux~n~difier (made Cellulosic Softening of (trademark) by DuPont) cellulosic fibers "Ceramine Hand-mDdifier (made Acrylic, Polyamide Softening Agent HS" by Sandoz Chemical (trademark) Co.) "Methan~l Hand-mDdifier (made Acrylic, Polyamide Do 20 Lubricant by DuPont) (trademark) "AerDtex Melaminerformalde- Cellulosic and blends Anti-crease prop-Cream" hyde resin (made by of celluclosic with erties and stabil-(trademark) American Cyanamid synthetic fibers ization Co. ) .. .:
"Ahcovel" Synthetic amine for- Do Do (trademark) maldehyde resin (made by Imperial Chemical Ind.) "Rbanite Synthetic amine ~or- Do DD
Rrl" maldehyfle resin (trademark) (made by Rchm & Haas Co.) -.~ .
~ - 27 -. . ~ .
It can be seen from the above that the process of this ¦ application provides a complete system for dyeing, texturizing ¦ and heat-setting, and finishing (and various combinations thereof) of a wide variety of fabrics and blends in a closed continuous environment.
After the textiie material leaves the dyeing a~paratus, it is preferably passed through a cooling zone where its tempera-ture is reduced from an elevated temperature just below the boiling point of the low boiling organic solvent to (for example) about 140~F, after which it is then passed through a washer where it is washed with the low boiling organic liquid such as (and preferably) methanol.
The washing step may ~e carried out in any conventional manner, although preferably I employ a cascade washing system involving a series of washing steps according to which the methan-ol is introduced just ahead of the point where the textile or plastic material leaves the washer and then is passed concurrentl~
with respect to the direction of movement of the textile material and through a series of "cascade" zones back to a point just afte~
the textile material enters the washing apparatus where the ..
.
~` 108240Z
concentration of high boiling liquid and residual unfixed color or dyestuff carried therein is the greatest.
The methanol or other low boiling organic wash li~uor is then passed to a suitable separatory device such as aistilla-tion apparatus where the methanol is distilled off at a relatively low temperature, condensed, and then returned to the methanol washing device.
The textile material after passing through the low boiling organic liquid washing device is then passed into a low temperature dryer to evaporate residual low boiling organic liquid (e.g., methanol) still clinging to tLe textile material.
The methanol thus evaporated is passea overhead to a condenser where it is condensed and, if desired, returned to the methanol washing step.
The textile material then leaves the dryer in finished form ready for such further treatment as any dyed textile mater-ial may be conventionally subjected to thereafter.
As indicated above, the partially exhausted dyestuff liquor leaving the dyeing step is recycled to the dyeing step, after addition of make-up dyestuff as desired and/or make-up glycol or glycol ether as desired, as well as with the addition of the glycol or glycol ether recovered from the distillation apparatus.
After a given dyelot of textile material has been com-pleted, the glycol or glycol ether containing the dyestuff may be separately stored and used again when a similar shade of dyeing . ..
is to be repeated. In the meantime, the dyeing apparatus can be cleaned very readily with the low boiling organic liquid, such as methanol, and the methanol thus employed may be returned to the ~ distillation unit for purification and separation and recycling to the methanol washing step for the next dyelot.
The process of this embodiment of the present invention may be further illustrated by reference to the accompanying draw-ings where (in ~igure 1) the various steps are shown in schematic fashion.
Reference numeral 1 represents the incoming textile ma-terial to be dyed which passes into the dyeing apparatus 2.
There i.t is subjected to the action of an appropriate dyestuf~
dissolved, suspended or dispersed in a suitable high boiling or- ¦
ganic liquid such as ethylene glycol, diethylene glycol, triethyl-ene glycol, tetraethylene glycol, propylene glycol, or the methyl-or ethyl- mono- or di-ether of such glycols.
The partially exhausted dyestuff liquor is removed from the dyeing apparatus 2 via line 3 from which it passes to a . storage chamber or sump 4 for the residual dyestuff-high boiling liquid mixture. From sump 4 the dyestuff-high boiling liquid mixture is recycled via line 5 to the dyeing apparatus 2, passing through a conventional heat exchanger Sa.to adjust it to the desired temperature of dyeing.
. Make-up dyestuff is added when and as needed via line 6 and make-up high boiling liquid is added when and as needed via line 7.
The textile material passes from the dyeing chamber via line 8 to a cooling chamber 9. There the d~ed textile material .
Il 1082402 . i I
¦ is cooled from a temperature of just below the normal boiling point of the high boiling organic solvent down to a temperature of (for example) about 140~F by passing cooling air into the cool-~ ing chamber 9 via line 10 and out via line 11. Excess non-fixed i dyestuff and excess high boiling liquid is removed from the ¦ textile material by conventional means (not shown) such as by passing the textile material between squeeze rolls near the exit end of the cooling chamber 9. This excess non-fixed dyestuff ln admixture with the excess high boiling liquid is returnëd to the dyestuff liquor sump 4 via line 3a.
The dyed material, now cooled and at least partially freed of excess non-fixed dyestuff and excess high boiling liquid, is shown at 12 as passing into a low boiling organic liquid washing device 13 where it is subjected to washing to remove re-sidual high boiling liquid and residual (non-fixed) dyestuff.
The organic wash liquid may conveniently be methanol or other low boiling aliphatic alcohol or a chlorinated hydrocarbon of the kind mentioned above. Methanol is preferred Wash liquor leaves the methanol washer 13 via line 14 and is passed to recovery apparatus 15 which may suitably take the form of distillation apparatus. There the relatively volatile low boiling organic liquid, such as methanol, is distilled away ~rom the high boiling liquid, condensed and returned via line 16 to the methanol washing apparatus 13. Make-up methanol may be introduced when and as needed via line 17.
. i. ~08240Z
I
Returning to the separator~ or distillation apparatus . 1 15, the recovered high boiling organic liquid with the residual dyestuff which remains after the vaporization of the methanol . ¦ therefrom is recycled via line 18 to the partially exhausted ¦ dyestuff liquor sump 4, whereby it is returned to the dyeing operation carried out in dyeing apparatus 2.
The textile material aftex the washing step is passed as shown by reference numeral 22 into the dryer 23 where it i5 contacted with air introduced via line 24. This air may be warm or hot, as obtained from ~ heating device (not shown). The air passes through and/or in contact with the washed textile material . picking up residual low boiling organic liquid still clinging to the textile material, an~ leaves the drying device 23 via line 25. The air leaving via line 25, and carrying vapors of the low boiling organic liquid, is then passed into a condenser 20 where the low boiling organic liquid is recovered and recycled to the methanol washing step via line 21. The air is removed from the condenser 20 via conventional vent means not shown. Alter-natively, the methanol vapor (with residual air) leaving via line 25 may be separately disposed of, such as by burning in a waste heat boiler (not shown~ to effect still further economies in o~eration.
losZ402 1 !
In this manner the dyed, (optionally) cooled, washed and dried textile or plastic material leaves the dryer 23 as shown at 26 as a finished dyed textile or plastic material ready for such other textile treating operations as may be desired.
It will be noted from the description o~ the schematic drawing of Figure 1 thus described that the material flow is com-pletely cyclic in nature with no or essentially no liquid efflu-ents from the system. Consequently, the system is completely free from problems normally associated with dye plants where aqueous or largely aqueous systems are involved and wherein the aqueous systems at some point or another must be discharged from the plant into rivers or wells or other surface water thereby creating effluent problems of an environmentally undesirable nature.
Moreover, the use of the low boiling organic li~uid for washing purposes requires a significantly lesser energy input to the system, which is an additional highly desirable feature of the process.
By way of still further illustration, the following examples of dyeing are set forth:
Example 1 A nyion fabric, type 66, is dyed in ethylene glycol con-taining 1/2~ of Acid Blue ~25. ~he sample is dyed at 300~F for 12 seconds. After cooling, the sample is washed in methanol and then dried at a low temperature. This dyeing gives a heavy blue shade with much better fastness properties than dyeing by conven-tional methods. Moreover, the partially exhausted dyestuff liquor ..
~j after addition of makeup ethylene glycol is returned to the dyeing operation. The wash methanol is distilled for recovery and recycling of recovered methanol.
I Example 2 ~ ~ polyester fabric is dyed in a dye-liquor containing ethylene glycol and 1/2% of Disperse Blue ~56. The polyester material is dyed at 320F for 30 seconds. After dyeing, the sample is then washed in methanol and dried at a low temperature.
The dyeing results in a full blue with excellent fastness proper-ties. Separation and recovery of both the ethylene glycol and methanol may be as described above.
Example 3 A wool fabric is dyed in ethylene glycol containing 1/2~ of Acid Blue ~25. The sample is dyed at 300F for 12 seconds After cooling, the sample is washed in methanol and then dried at a low temperature. This dyeing gives a heavy blue shade with much better fastness properties than dyeing by conventional me-thods. Moreover, the partially exhausted dyestuff liquor after addition of ma~eup ethylene glycol is returned to the dyeing operation. The wash methanol is distilled for recovery and re-cycling of recovered material in the manner ~escribed above.
Example 4 An acrylic fabric is dyed in a dye-liquor containing ethylene glycol and 1/2~ of Disperse Blue ~56. The acrylic ~ mater 1 is dyed at 320~P for 30 seconds. After dyeing, the . 108Z40Z
sample is then ~Jashed in methanol and dried at a low temperature.
The dyeing results in a full blue with excellent fastness prop- !
I erties. Separation and recovery of both the ethylene glycol and ¦
¦ methanol may be as described above.
It should be noted in passing that I do not claim to be the first to have suggested the step of dyeing a textile material in a nonaqueous dye bath such as a glycol or a glycol ether.
Societa Rhodiaceta's French Patent No. ~55,260 (and the generally corresponding Swiss Patent No. 230,891) suggested such a step for the dyeing of nylon many years ago. Moreover, more recently Laucius et al, in J. S. Patent Mo. 2,.~82,119, suggested the dyeing of polyester in a nonaqueous dyebath comprising various glycols. See also Olpin et al U. S. Patent No. 2,461,612.
Moreover, I do not claim to be the first to suggest the step per se of washing dyed textile products with a low boiling or-ganic liquid, such as an alcohol, because that too was suggested in the Societa Rhodiaceta patents mentioned above, although there it is a matter of indifference whether water or a low boiling alcohol is employed as the washing liquid. See the French patent at page 2, lines 58 et ~ However, neither the prior art just cited nor any other prior art, so far as I am aware, has sugges-ted, much less recognized, the desirability of operating the dyeing and washing steps in the manner indica-ted herein with complete or substantially complete recycling of the various ma-terials involved and with a completely or substantially co~pletel~
nonaqueous system, for the sake of lesser costs, and more ~ I
!i 1 1, 1 importantly, with a view to present-day environemntal and energy conservation considera~ions.
' It is to be particularly noted in connection with this 1 embodiment of the present invention that it conveniently provides ~ what is in e~fect a nonaqueous or substantially nonaqueous closed j or essentially closed treating system, and therefore with no need to discharge potentially polluting aqueous wastes to ground water. If as a result of long-continued operationt a build-up of significant (though still relatively small) amounts of water should occur, such as from the use of aqueous dye concentrates to make up the dilute dyestuff-high boiling organic liquid treating s()lution and/or from moisture unavoidahly present in the air used for the cooling and drying steps, such water can be easily re-moved from any of the treating liquids by conventional means (not shown) such as by passing same through a bed of a commercial dehydrating agent such as Drierite.
The description up to this point has dealt primarily with dyeing alone. Hereinafter descripti~e matter relating to dyeing combined with texturizin~, as well as descriptive matter relating to texturizing alone, is presented.
Texturizing, etc. In the case of a textile material such as woven or knitted fabric, as distinguished from a plastic material in the form of a film, the surface-to-volume ratio is substantially highex due to the yarn structure of the woven or knitted textile material. Consequently, there will normally be a certain amount of moisture pickup from the atmosphere so that at least some texturizing and heat-setting will take place when the textile material is brought into contact with the hot hi~h oiling organic liq~id.
Generally, however, where it is desired to secure a really significant degree of texturizing and heat-setting simul-I taneously with the dyeing~ a pre-treatment Gf the textile materia~
¦ to incorporate therein a low boiling liquid texturizing agent j will be preferred. This objective is achieved very conveniently by simply passing the woven or knitted textile material through a bath of low boiling liquid texturizing agent (such as water or methanol) so as to incorporate therein a predetermined amount of low boiling liquid texturizing agent, such as of the order of 10 to 60~, on a weight basis. Where water is selected as the low ~oiling liquid texturizinq agent, a convenient way of incorporat-ing the desired amount of water in the woven or knitted textile material is to contact same with steam from a series of steam jets, or else with very fine jets of water, with the jets placed above and/or below the path of travel of the textile material just prior to its contact with the hot high boiling organic liquid; for example, as the woven or knitted textile material is introduced into the process viaan otherwise conventional tenter-frame arrangement.
Thus, in order to effect the texturizing and heat-settin mentioned above, the textile material undergoing processing is first treated with a low boiling texturizing agent, such as water or methanol in the liquid phase, or in the case of water, in the form of steam or very fine sprays. The amount of low boiling texturizing agent employed for this purpose will vary, depending on the degree of texturizing desired It is preferably in the I
¦ range of from 10 to 60% by weight, based on the weight of the textile material. It is of course necessary to employ sufficient ~ of the low boiling texturizing agent to impart the desired de-¦ gree of texturizing and heat-setting, while at the other extreme it is necessary to avoid employing so much as to defeat the purpose of the texturizing operation. The amount, in any case, will be such that when the textile material containing the low boiling texturizing agent in liquid phase is subjected to the hot dyestuff-containing high boiling organic solvent, this brings about an "explosion", as it were, or a flashing of the low boiling liquid to vapor, thus producing a volumization or bulking of the textile material.. The net result of this procedure is to bring about the desired texturizing and heat-setting of the textile material while it is being dyed.
As shown in Figure 2, the textile material is first passed through a trough 200 containing the low boiling liquid texturizing agent by means of a series of guide rolls 202, and thence between squeeze rolls 204 by means of which the liquid texturizing agent in excess of the desired predetermined amoun~
to be left in the textile material is removed and (in the case of methanol) returned to the trough 200 via line 206. When methanol is used, suitable hoods or enclosures (not shown) are pro~ided for the protection of the workmen and to minimize any fire hazard. The thus-treated textile material is then passed to the dyeing step 2 and the succeeding steps of Figure 1 as a consequence of which texturizing and heat-setting are combined with dyeing.
..
`
Il 1082402 The low boiling texturizing agen~ present in the tex-tile material in liquid phase, and which thereafter is subjected ¦
to the relatively high temperature of the hot dyestuff-containing ~ high boiling organic solvent in 2, flashes off during the dyeing operation and is removed via line 210. This low boiling liquid which is flashed off in the form of vapor will then be associated !
with some vapor of the high boiling organic solvent such as glycol, some of which indeed may be present in the form of par-ticles of "mist". This mixture is passed through a recovery system which may take the form of a condenser and/or filter 212, thereby assuring the separation and removal of substantially all of the high boiling organic solvent including the mist particles.
The condensate and/or filtrate may then be passed to a fraction-ator 214 for the removal of substantially all of~the low boiling liquid, with the remaining high boiling organic solvent being recycled to the dyestuff sump 4 via line 216. The low boiling liquid (if methanol) is thus separated and reused, or int~e case of water, it will be evaporated from the high boiling liquid in the dyestuff sump 4. In the event the low boiling texturizing agent is methanol, the reclaimed methanol may be conveniently condensed and recycled for use at a later stage of the process such as in the washing step. On the other hand, the reclaimea methanol without condensation may be sent directly-.
. .
.
- ~ ~ _t ~ to a waste heat boiler where it can be burned, thereby reducing j the energy requirements for the system derived from the burning ~ of valuable fossil fuels.
j Alternatively, the low boiling texturizing agent may be introduced into the textile material in the desired predetermined amounts, via sprays of fine jets of liquid water or methanol, or 3ets of steam, located above and/or below the path of travel of . the textile material just prior to its introduction to the dyeing step 2 of Figure 1.
The texturizing and heat-setting is performed under con-trolled conditions of a predetermined relatively high temperature and a predetermined content of low boiling liquid.texturizing agent. The textile material when in the form of woven or knittea ......... ... ... .... ... goods may be conveniently introduced into-the process by means of a conventional tenter-frame that can be adjusted to overfeed the textile material lengthwise, and including also provision for narrowing the tenter-frame to texturize wiathwise as well. In this way the degree of texturizing and heat-setting in either.the . length direction or the width direction (or both) may readily be - 20 controlled.
. As a still further embodiment of the invention, if one wishes only to texturize and heat-set the textile material with-. out at the same time dyeing same, one need only refrain from : adding a dyestùff to the high boiling organic liquid and instead otherwise proceed as already described.above, with the pre-treat-l ment such in Figure 2 followed by treatment as in Figure 1.
I
. .
. -17-~o~240z ¦1 Most texturizing yarns for weaving or knitting are in ¦¦ the 100 denier range. The actual cost of separately texturizing 100 denier yarn is about $0.22 per pound. To texturize a 30 ¦ denier yarn costs about $1.10 per pound, since the machine time I for 30 denier yarn is about four times the machine time for 100 ¦ denier yarn for equivalent number of pounds produced. At the present time, due to high cost there are no fabrics available made from texturized 30 denier yarns. By weaving or ~nitting an untexturized 30 denier yarn and then texturizing the resulting woven or knitted article as described herein, the texturizing can be done at substantially no additional cost during the dyeing operation. The remarkable savings thus made possible by the present improved operation combining both texturizing and dyeing offer vast possibilities for increased markets for texturized and heat-set woven and knitted textile materials o~ the finest denier. Consequently, the industry will have available a wider selection of textile materials readily adaptable for fabrication into natural-silk-like articles of manufacture.
It should be mentioned that when the procedures des-cribed herein include a texturizing and heat-setting operation, either alone or in combination with dyeing, it is important that the textile material shall be in a relaxed or relatively unten-sioned condition during the texturizing. This can be assured ~y supporting the textile material on an endless traveling tenter-~5 irame.
~' , It will be understood that no claim is made broadly to texturizing per se, since such texturizing has long been known;
e.g., see my U.S. Reissue Patent No. Re. 27,773. The treatment des-cribed herein may also have the additional beneficial effect of minimizing pilling when treating, e.g., polyester--see my U.S. Patent No. 2,938,811.
Still further details on texturizing are as follows:
Texturizing and voluminizing are performed on a Hermesol machine (see my U.S. Patent 4,055,971, granted November 1, 1977).
The greige goods coming off the loom or knitting machine are fed into a tenter-frame, with overfeeding of the material.
On the way to the dyeing chamber, the textile material is wetted between 20 and 60% with a low boiling solvent. As the tenter-frame enters the Hermesol dyeing chamber, the tenter-frame, with the textile material in place, is contracted to a predetermined width.
Immediately upon entry of the wetted textile material into the dyeing chamber, an "explosion" occurs; thus causing the yarn, in both the widthwise and lengthwise directions, to become entangled; thus texturizing the yarn in a woven or knitted fabric. It is thus possible to by-pass a separate expensive tex-turizing process of synthetic materials in yarn form.
Example 5 A woven polyamide fabric, constructed with a 60 denier warp and a 70 denier filling weighing 50 grams per square meter, after texturizing as previously described, weighed 86 grams per square meter showing a texturizing and shrinkage of 22% in the ~B
Il ~08240Z i . !
¦ warp and 22% in the filling. Another woven polyamide fabric j constructed of a 70 denier warp and 70 denier filling weighed 51 grams per square meter before texturizing. After texturizing, it weighed 82 grams per square meter showing a texturizing and ~ shrinkage of 22% in the warp and 17% in the filling.
¦ Example 6 A woven polyester fabric, constructed with 3 ply, 100 denier polyester yarn in both warp and filling before texturizing, weighed 115 grams per square meter, and after texturizing, 177 grams per square meter, showing a warp shrinkage of 19% and a fil _ ling shrinkage of 18%.
Example 7 A woven polyester and ~ol fabric constructed of 3 ply, 100 denier in the warp and 100~ wool in the filling, weighed 139 grams pér square meter. After texturizing, it weighed 169 grams per square meter, showing a shrinkage of 18~ in the warp and ~%
volumimizing of the wool.
Example 8 A polyamide, tubular, knitted fabric, constructed of 110 denier yarn, weighed 121 grams per square meter, and after texturizing, the weight was 169 grams per square meter.
Example 9 A polyester, tubular, knitted fabric, constructed of 100 denier polyester, weighed 118 grams per square meter, and after texturizing, 198 grams per square meter.
A11 of the aforementioned fabrics were wetted with a very fine water spray before entering the dyeing chamber.
In all cases the high boiling liquid in the dye chamber was ethylene glycol. The high temperature high boiling liquia was at a temperature of 175C, while for the polyamide, the temperature of the dyeing liquid was 155C.
While the textile material was being texturized and voluminized in the dyeing chamber, it was simultaneously heat-set; thus saving another expensive operation in conventional fabric finishing.
After this fabric passed through the dyeing chamber, it was then cooled in another chamber and here the excess ethylene glycol was removed from the fabric.
From the cooling chamber, the textile material was washed in methanol. After the methanol wash, the excess methanol was removed and the textile material was then dried at 93C.
Reference is made to my U.S. Patent No. 3,530,214 entitled "Method for Treating Textile Materials to Uniformly Set Their Shape"; to my U.S. Patent No. Re.27,773 entitled "Method for the Continuous Texturizing or Voluminizing of Textile Materials"; and to my U.S. Patent No. 2,938,811 entitled "Method of Conditioning Polyester Textile Material and the Resulting Products".
Woven polyester fabric constructed with 70 denier polyester yarn in both warp and filling weighed 40 grams per square meter and after texturizing, 61 grams per square meter.
The warp showed a texturizing and shrinkage of 20%, while the filling showed 17~. In the previous sample, only clear ethylene glycol was used in the dyeing chamber. In the present sample, 2 grams of Dispersed Blue 56 per liter was added to the ethylene glycol resulting in a deep blue dyeing on the polyester material.
Otherwise, the fabric was handled as described before. In one operation, the textile material was texturized, voluminized, ~, Il 1082402 .` ....... I
¦ heat-set and dyed. The washing of dyed materials in methanol is superior to the use of ~ny other washing or cleaning method. In ~ the case of dyed polyester, it is unnecessary to give a chemial ¦ wash to remove excess and unfixed dyestuff to prevent crocking.
A polyamide flat-knitted fabric, constructed of 30 denier polyamide weighing 55 grams before texturizing and 78 grams after texturizing, was exposed in the dyeing chamber at a temperature of 155C, to ethylene glycol containing 3 grams per liter of Acid Red No. 151. The fabric was dyed a deep red.
Here, again, the fabric was texturized, heat-set and dyed in one operation. As mentioned before, the }igh boiling liquid in all the aforementioned samples was ethylene glycol and in the case of fabrics containing polyester, the temperature was 175C and in the case of polyamides, the temperature was 155C. In all the aforementioned examples, the exposure time in the dyeing chamber was 20 second The glycol and methanol were recycled.
In all the aforementioned examples, the fabrics were constructed of untexturized, drawn yarns.
;~ Still further detailed examples are as follows:
Example 10 A polyester double knit fabric, 285 grams per linear meter, is dyed continuously in a dye liquor containing ethylene glycol and 1.0 gram per liter (g/l~ of Disperse Blue ~56 (crude, unstandardized) and 0.5 g/l of phosphoric acid at 175C for 45 seconds, the dye liquor being applied to the moving web of fabric by spraying from a circulating reservoir of dye liquid at the 108Z~O~
¦ rate of 375 liters per minute (lpm). The fabric after exposure to the dye liquor is then conducted through a cooling chamber I where cool air impinges on the surface of the fabric to lower the ¦ temperature of said fabric to 70C, after which the fabric is washed by spraying with methanol at 10C to remove residual glycol and surface dye. The fabric is then passed into a drying chamber where hot air at 110C impinges on both fabric surfaces simultaneously to remove the last traces of methanol; The par-tially exhausted dye liquor, after addition of make-~p ethylene glycol and dye, is returned to the dyeing operation. -Spectrophometric measurement of sam~les of circulating dye liquor ana reflectance measurements of thP dyed cloth during the course of dyeing 365 meters of cloth showed a depletion of 15% of the original dyebath concentration due to exhaustion which is made up for by adaing to the aforementioned ma~eup ethylene glycol.
Methanol used in the washing step is collected, along with ethylene glycol and a small amount of dye, ana fractionally distilled from the high-boiling glycol and then returned to the washing stage. The residue of the distillation is returned to the dye makeup tank. Methanol was distilled off at the rate of 3,785 liters per hour.
The abric was overfed into the dyebath by 10~ and allowed to shrink 10% in the width-wise direction.
The dyed fabric i5 a bright blue, uniformly coverin~
the entire fabric surfaces and having excellent fastness proper-ties. Penetration of the fabric and the individual fibers is ¦~ excellent.
.:.
l -23- l ~082402 Example 11 ¦ A nylon type 66 tufted carpet fabric, weighing 625 ¦! grams per square meter of surface fiber, is dyed continuously l in a dye liquor containing Disperse Blue ~56 (crude, unstandard-~ ized) and 0.5 g/l phosphoric acid at 155C for 45 secon~s, the dye being applied to the carpet fabric by spraying, followed by cooling, washing and drying in the manner described in Example 5, including recycling of glycol and methanol.
The resultant dyeing is uniformly level.
In practicing this invention, it may also be advantag-eous to include dyebath additives to impart resistance to ultra-violet degradation of polyester and nylon, improved fastness to light, flame retardance, antistatic properties, and the like.
For example, the following chemical reagents can be ad~ed to the 15 ~ dyebath In of Figure 1 for the following ob; ecti~es:
.
,~; , ' ~`; .
.
~ -24-Table I
Reagent Ch~nical O~nposition Fil~er Advantages "Uvinul D-49" 2,4-dimet~xy-b~zopher~one Polyester (&~c Greatly improved (trad~nark) (made ~y General Aniline & U.S. Patent No. light fastness &
Film (G~F)) 3,943,105) fabric stability "Uvinul D-49" Do Polyamide (See ~proved light U.S. Patent N~. fastness an~l sun-3,771,949) light stability "Tinuvin 327" Benzc)triazole derivative Polyamide (See nnpr~ light (trademark) (made by Ciba/Geigy) U.S. Patent N~. fastness 3,771,949) ~:
"Uvinul 490" Benzophen~ne derivative Polyester (See ~proved light (trad~nark) (made by G~F) U.S. Patent N~. fastness and 3,943,105) fabric stability "Anti-Blaze Chlorinated phosphonate Polyester Flan~ retardance 19" (made by ~bil Ch~mical Polyamide (trad~ark) Co.) "Fir~naster ~ris-dibraTopropyl- Polyes~r Flame retardance 200" p}sphate (made by Acrylic ~-(trademark) Michigan Chemical Co.) :-(See also my U.S. Patent No. 3,943,105 for additional disclosure relative to ultraviolet absorbers.) 1:2 . ~ ", ~
10t~Z402 ¦ At a later stage of the process, antistatic agents, oil ¦ and water repellents, softening ana other hand-modifying agents, i crease-resisting resins, and the like may be applied to the ¦ fabric(s) such as at reference numeral 22 in Figure 1 of the accompanying drawings (i.e., between methanol washing and drying). .
These agents may be applied to the washed textile material in the form of a solution or dispersion of the selected agent in a solvent or other suitable carrier.
The following Table II illustrates these treatments:
1o8240Z
Table II
Chemical Ckmposition or Other Identifi-Reagent cation Fibex (s) A~vantages "Avitex E" Antistatic Agent Cell~losic, animal and Excellent anti-(trademark) (made by DuPont) synthetic fibers, e.g., static properties Polyamide, Polyester, even at low humid-Acrylic, Olefin, etc. ities "Siligan PA"Antistatic Agent Do Do (trademark) (made by EASF Wyan-dotte) "Statexan Antistatic Agent Do Do PKN" (made by Bayer Far-(trademark) ben Industries) "Zepel" Fluorinated Compound Polyamide, Polyester, Excellent oil, (trademark) (made by DuPDnt) Acrylic and other oe l- water and soil lulosic synthetics, resistance and animal fibers "SOotchr FluDroc æbon Com~ Do Do gard" pound (made by (trademark) Minnesota Mining &
Manufacturing Co.) "Avibone A"Nbux~n~difier (made Cellulosic Softening of (trademark) by DuPont) cellulosic fibers "Ceramine Hand-mDdifier (made Acrylic, Polyamide Softening Agent HS" by Sandoz Chemical (trademark) Co.) "Methan~l Hand-mDdifier (made Acrylic, Polyamide Do 20 Lubricant by DuPont) (trademark) "AerDtex Melaminerformalde- Cellulosic and blends Anti-crease prop-Cream" hyde resin (made by of celluclosic with erties and stabil-(trademark) American Cyanamid synthetic fibers ization Co. ) .. .:
"Ahcovel" Synthetic amine for- Do Do (trademark) maldehyde resin (made by Imperial Chemical Ind.) "Rbanite Synthetic amine ~or- Do DD
Rrl" maldehyfle resin (trademark) (made by Rchm & Haas Co.) -.~ .
~ - 27 -. . ~ .
It can be seen from the above that the process of this ¦ application provides a complete system for dyeing, texturizing ¦ and heat-setting, and finishing (and various combinations thereof) of a wide variety of fabrics and blends in a closed continuous environment.
Claims (25)
1. A process for texturizing and heat-setting textile material containing a low boiling texturizing agent in liquid phase in an amount sufficient to cause flashing of the low boiling texturizing agent upon contact of the thus-treated textile material with a high boiling organic liquid at a relatively high temperature, comprising contacting textile material impregnated with the low boiling liquid texturizing agent with the high boiling organic liquid at a high temperature thus texturizing and heat-setting the textile material, cooling the texturized textile material and washing same with a low boiling organic liquid which is free or substantially free of water, followed by drying the texturized textile material, the washing and drying steps being carried out in an essentially closed system, with the separation and recovery of the low boiling organic wash liquid, the low boiling organic wash liquid thus recovered being recycled to the washing step and with the low boiling organic wash liquid vaporized from the textile material during the drying step being recovered, and with the low boiling texturizing agent that is evaporated during the texturizing and heat-setting being removed from the high temper-ature textile material contacting zone as a mixture thereof with vapor of the high boiling organic liquid.
2. A process as defined in claim 1, wherein the high boiling organic liquid is selected from the class consisting of ethylene glycol, diethylene glycol, triethylene glycol, tetra-ethylene glycol, propylene glycol, and the methyl- and ethyl-mono- and di-ethers of such glycols.
3. A process as defined in claim 1, wherein the high boiling organic liquid is a lower alkylene glycol.
4. A process as defined in claim 1, wherein the high boiling organic liquid is a lower alkyl ether of a lower alkylene glycol.
5. A process as defined in claim 1, wherein the low boiling organic liquid is a lower alkanol.
6. A process as defined in claim 1, wherein the low boiling organic liquid is methanol.
7. A process as defined in claim 1, wherein the low boiling organic liquid is selected from the class consisting of CH2C12,CC14 and CHC13.
8. A process as defined in claim 1, wherein the low boiling organic liquid is a chlorinated paraffinic hydro-carbon.
9. A process as defined in claim 1, wherein the high boiling organic liquid contains a suitable dyestuff dissolved, suspended or dispersed therein, whereby the textile material is texturized, heat-set and dyed simultaneously.
10. A process as defined in claim 9, wherein the high boiling organic liquid is selected from the class con-sisting of ethylene glycol, diethylene glycol, triethylene glycol, tetraethylene glycol, propylene glycol, and the methyl- and ethyl- mono- and di-ethers of such glycols.
11. A process as defined in claim 10, wherein the high boiling organic liquid is a lower alkylene glycol.
12. A process as defined in claim 10, wherein the high boiling organic liquid is a lower alkyl ether of a lower alkylene glycol.
13. A process as defined in claim 10, wherein the low boiling organic liquid is a lower alkanol.
14. A process as defined in claim 10, wherein the low boiling organic liquid is methanol.
15. A process as defined in claim 10, wherein the low boiling organic liquid is selected from the class consisting of CH2C12, CC14 and CHC13
16. A process as defined in claim 10, wherein the low boiling organic liquid is a chlorinated paraffinic hydrocarbon.
17. A process as defined in claim 1, wherein the textile material is treated while in a substantially relaxed or untensioned condition.
18. A process as defined in claim 9, wherein the textile material is treated while in a substantially relaxed or untensioned condition.
19. A process as defined in claim 1, wherein one or more additives for imparting resistance to ultraviolet degradation, improved fastness to light, flame retardance or-antistatic properties are added to the high boiling liquid.
20. A process as defined in claim 9, wherein one or more additives for imparting resistance to ultraviolet degradation, improved fastness to light, flame retardance or antistatic properties are added to the high boiling liquid.
21. A process as defined in claim 1, wherein one or more additives for imparting antistatic properties, oil and/or water repellancy, softening properties, or crease-resistance are applied to the textile material after washing and before drying.
22. A process as defined in claim 9, wherein one or more additives for imparting antistatic properties, oil and/or water repellancy, softening properties, or crease-resistance are applied to the textile material after washing and before drying.
23. In a process for dyeing a textile or plastic material with a dyestuff dissolved or suspended or dispersed in a high boiling organic liquid which is free or substantially free of water and at a relatively high temperature, followed by cooling the dyed textile or plastic material and washing same with a low boiling organic liquid which is free or substantially free of water, followed by drying the washed and dyed textile or plastic material, the improvement comprising carrying out the dyeing, the washing and the drying steps in cyclic manner and in an essentially closed system with the partially exhausted dyestuff liquor from the dyeing step being recycled for the treatment of further textile or plastic material to be dyed, with the separation and recovery of the low boiling wash liquor with low boiling wash liquid recovered therefrom being recycled to the washing step and the residual high boiling liquid con-taining residual dyestuff being recycled to the dyeing step, and with the low boiling liquid vaporized from the textile material in the drying step being recovered and returned to the low boiling liquid washing step, and wherein one or more additives for imparting resistance to ultraviolet degradation, improved fastness to light, flame retardance or antistatic properties are added to the high boiling liquid.
24. In a process for dyeing a textile or plastic material with a dyestuff dissolved or suspended or dispersed in a high boiling organic liquid which is free or substantially free of water and at a relatively high temperature, followed by cooling the dyed textile or plastic material and washing same with a low boiling organic liquid which is free or substantially free of water, followed by drying the washed and dyed textile or plastic material, the improvement comprising carrying out the dyeing, the washing and the drying steps in cyclic manner and in an essentially closed system with the partially exhausted dyestuff liquor from the dyeing step being recycled for the treatment of further textile or plastic material to be dyed, with the separation and recovery of the low boiling wash liquor with low boiling wash liquid recovered therefrom being recycled to the washing step and the residual high boiling liquid con-taining residual dyestuff being recycled to the dyeing step, and with the low boiling liquid vaporized from the textile material in the drying step being recovered and returned to the low boiling liquid washing step, and wherein one or more additives for imparting resistance to ultraviolet degradation, improved fastness to light, flame retardance or antistatic properties are added to the high boiling liquid, and wherein one or more additives for imparting antistatic properties, oil and/or water repellency, softening properties, or crease-resist-ance are applied to the textile material after washing and before drying.
25. In a process for dyeing a textile or plastic material with a dyestuff dissolved or suspended or dispersed in a high boiling organic-liquid which is free or substantially free of water and at a relatively high temperature, followed by cooling the dyed textile or plastic material and washing same with a low boiling organic liquid which-is free or substantially free of water, followed by drying the washed and dyed textile or plastic material, the improvement comprising carrying out the dyeing, the washing and the drying steps in cyclic manner and in an essentially closed system with the partially exhausted dyestuff liquor from the dyeing step being recycled for the treatment of further textile or plastic material to be dyed, with the separation and recovery of the low boiling wash liquor with low boiling wash liquid recovered therefrom being recycled to the washing step and the residual high boiling liquid con-taining residual dyestuff being recycled to the dyeing step, and with the low boiling liquid vaporized from the textile material in the drying step being recovered and returned to the low boiling liquid washing step, and wherein one or more additives for imparting resistance to ultraviolet degradation, improved fastness to light, flame retardance or antistatic properties are added to the high boiling liquid, and wherein the textile or plastic material is treated while in a sub-stantially relaxed or untensioned condition.
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| US750,910 | 1976-12-15 | ||
| US05/750,910 US4115054A (en) | 1976-01-09 | 1976-12-15 | Process for the rapid, continuous and waterless dyeing and texturizing and heat-setting of textile and plastic materials |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CA1082402A true CA1082402A (en) | 1980-07-29 |
Family
ID=25019636
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CA276,337A Expired CA1082402A (en) | 1976-12-15 | 1977-04-18 | Process for the rapid, continuous and waterless dye- ing and texturizing and heat-setting textiles and plastic materials |
Country Status (15)
| Country | Link |
|---|---|
| JP (1) | JPS5845520B2 (en) |
| AU (1) | AU504783B2 (en) |
| BE (1) | BE853506A (en) |
| BR (1) | BR7702430A (en) |
| CA (1) | CA1082402A (en) |
| CH (1) | CH617560GA3 (en) |
| DD (1) | DD132984A5 (en) |
| DE (1) | DE2716600C2 (en) |
| ES (1) | ES457863A2 (en) |
| FR (1) | FR2374461A1 (en) |
| GB (1) | GB1576885A (en) |
| HU (1) | HU184164B (en) |
| IT (1) | IT1125742B (en) |
| NL (1) | NL175650C (en) |
| PL (1) | PL104374B1 (en) |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| FR2599392B1 (en) * | 1986-06-02 | 1989-02-24 | Texinox Sarl | PROCESS FOR TREATING TEXTILE MATERIALS AND TREATMENT PLANT FOR CARRYING OUT SAID METHOD |
| CN106393203A (en) * | 2016-12-08 | 2017-02-15 | 无锡同心塑料制品有限公司 | Length fixing equipment of foam plastic cold press |
| WO2025007343A1 (en) * | 2023-07-06 | 2025-01-09 | 亚临界(上海)技术有限公司 | Continuous waterless dyeing apparatus for polyester fabric and dyeing method |
Family Cites Families (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2882119A (en) * | 1959-04-14 | Process for dyeing polyester materials | ||
| US27773A (en) * | 1860-04-10 | Knife and fork cleaner | ||
| CH187092A (en) * | 1934-11-22 | 1936-10-31 | Wacker Chemie Gmbh | Device for the continuous soaking of wide webs with volatile solvents and for drying the soaked webs. |
| FR955260A (en) * | 1941-08-28 | 1950-01-11 | ||
| US2461612A (en) * | 1944-04-18 | 1949-02-15 | Celanese Corp | Dyeing of resins with polyhydroxy alcohol assistants |
| US2938811A (en) * | 1959-11-09 | 1960-05-31 | Martin Proc Company Inc | Method of conditioning polyester textile material and the resulting products |
| JPS503431B1 (en) * | 1965-10-05 | 1975-02-04 | ||
| US3530214A (en) * | 1967-02-24 | 1970-09-22 | Julius Hermes | Method for treating textile materials to uniformly set their shape |
| GB1162964A (en) * | 1967-09-06 | 1969-09-04 | Ici Ltd | Treatment of Textile Materials |
| GB1265493A (en) * | 1968-03-19 | 1972-03-01 | Artos Meier-Windhorst Kg | Process and apparatus for texturising endless yarn |
| US3558260A (en) * | 1968-05-08 | 1971-01-26 | Julius Hermes | Method for the rapid and continuous dyeing of mixtures of textile materials |
| FR2065645A1 (en) * | 1969-10-15 | 1971-08-06 | Hermes Julius | Texturising or bulking of textile products |
| USRE27773E (en) * | 1971-01-27 | 1973-10-02 | Method for the continuous texturizing or voluminizing op textile materials | |
| CH566417A (en) * | 1972-05-09 | 1975-09-15 | Recovery of dyes and solvents - by contacting the dyed fibres with a low b.pt. solvent evaporating and then extracting with water |
-
1977
- 1977-04-12 BE BE176635A patent/BE853506A/en not_active IP Right Cessation
- 1977-04-14 NL NLAANVRAGE7704066,A patent/NL175650C/en not_active IP Right Cessation
- 1977-04-14 DE DE2716600A patent/DE2716600C2/en not_active Expired
- 1977-04-14 JP JP52042127A patent/JPS5845520B2/en not_active Expired
- 1977-04-14 GB GB15580/77A patent/GB1576885A/en not_active Expired
- 1977-04-15 BR BR7702430A patent/BR7702430A/en unknown
- 1977-04-15 HU HU77MA287A patent/HU184164B/en not_active IP Right Cessation
- 1977-04-15 CH CH470877A patent/CH617560GA3/en unknown
- 1977-04-15 ES ES457863A patent/ES457863A2/en not_active Expired
- 1977-04-18 CA CA276,337A patent/CA1082402A/en not_active Expired
- 1977-04-18 FR FR7711593A patent/FR2374461A1/en active Granted
- 1977-04-18 AU AU24343/77A patent/AU504783B2/en not_active Expired
- 1977-04-29 DD DD7700198674A patent/DD132984A5/en unknown
- 1977-04-29 PL PL1977197745A patent/PL104374B1/en unknown
- 1977-04-29 IT IT22986/77A patent/IT1125742B/en active
Also Published As
| Publication number | Publication date |
|---|---|
| PL104374B1 (en) | 1979-08-31 |
| CH617560GA3 (en) | 1980-06-13 |
| PL197745A1 (en) | 1978-06-19 |
| HU184164B (en) | 1984-07-30 |
| NL175650B (en) | 1984-07-02 |
| JPS5845520B2 (en) | 1983-10-11 |
| DE2716600C2 (en) | 1983-12-15 |
| NL175650C (en) | 1984-12-03 |
| DE2716600A1 (en) | 1978-06-22 |
| BE853506A (en) | 1977-10-12 |
| FR2374461B1 (en) | 1980-06-13 |
| AU504783B2 (en) | 1979-10-25 |
| FR2374461A1 (en) | 1978-07-13 |
| ES457863A2 (en) | 1978-07-16 |
| DD132984A5 (en) | 1978-11-22 |
| BR7702430A (en) | 1978-08-01 |
| IT1125742B (en) | 1986-05-14 |
| CH617560B (en) | |
| AU2434377A (en) | 1978-10-26 |
| GB1576885A (en) | 1980-10-15 |
| NL7704066A (en) | 1978-06-19 |
| JPS5374198A (en) | 1978-07-01 |
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