CN115045125A - Lyocell staple fiber loose fiber dyeing crosslinking agent and dyeing method - Google Patents
Lyocell staple fiber loose fiber dyeing crosslinking agent and dyeing method Download PDFInfo
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- CN115045125A CN115045125A CN202210665987.3A CN202210665987A CN115045125A CN 115045125 A CN115045125 A CN 115045125A CN 202210665987 A CN202210665987 A CN 202210665987A CN 115045125 A CN115045125 A CN 115045125A
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- 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
- D06P1/44—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 insoluble pigments or auxiliary substances, e.g. binders
- D06P1/64—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 insoluble pigments or auxiliary substances, e.g. binders using compositions containing low-molecular-weight organic compounds without sulfate or sulfonate groups
- D06P1/642—Compounds containing nitrogen
- D06P1/6426—Heterocyclic compounds
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D251/00—Heterocyclic compounds containing 1,3,5-triazine rings
- C07D251/02—Heterocyclic compounds containing 1,3,5-triazine rings not condensed with other rings
- C07D251/04—Heterocyclic compounds containing 1,3,5-triazine rings not condensed with other rings having no double bonds between ring members or between ring members and non-ring members
-
- 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
- D06P3/00—Special processes of dyeing or printing textiles, or dyeing leather, furs, or solid macromolecular substances in any form, classified according to the material treated
- D06P3/58—Material containing hydroxyl groups
- D06P3/60—Natural or regenerated cellulose
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Abstract
本发明提供一种莱赛尔短丝纤维散纤染色交联剂及染色方法。本发明的交联剂首先制备二乙烯三胺与双氰胺的缩聚体；然后取1，3，5‑三丙烯酰基六氢‑1，3，5‑三嗪交联剂100重量份加注到反应容器中，同时在反应容器中加注10—15重量份步骤1.1制备的二乙烯三胺与双氰胺的缩聚体混合搅拌，以每分钟0.5℃速率升温到50℃时保温反应20分钟；再以每分钟0.5℃速率升温到80℃保温搅拌反应120分钟得到本发明所述1，3，5‑三丙烯酰基六氢‑1，3，5‑三嗪改性交联剂产物。用于做为莱赛尔短丝纤维散纤染色交联剂。本发明成功的解决了现有纤维交联制备工艺中存在的交联不匀、交联不充分的工艺弊端。The invention provides a lyocell staple fiber loose fiber dyeing cross-linking agent and a dyeing method. The cross-linking agent of the present invention firstly prepares a polycondensate of diethylenetriamine and dicyandiamide; In the reaction vessel, add 10-15 parts by weight of diethylenetriamine prepared in step 1.1 and the polycondensate of dicyandiamide to mix and stir simultaneously in the reaction vessel, and heat the reaction vessel for 20 minutes at a rate of 0.5°C per minute to 50°C. Then, the temperature is raised to 80°C at a rate of 0.5°C per minute for 120 minutes to obtain the 1,3,5-triacryloylhexahydro-1,3,5-triazine modified crosslinking agent product of the present invention. Used as a cross-linking agent for lyocell staple fiber loose fiber dyeing. The invention successfully solves the technical drawbacks of uneven cross-linking and insufficient cross-linking existing in the existing fiber cross-linking preparation process.
Description
Technical Field
The invention relates to a lyocell short fiber loose fiber dyeing cross-linking agent and a dyeing method, belonging to the technical field of dyeing and finishing and cross-linking of fiber materials.
Background
Lyocell fibres have numerous advantages in the context of new textile materials and are not described in detail here. The emphasis is on its disadvantages and its impact on subsequent dyeing applications. The fibrillation characteristics are the biggest defects of the lyocell fiber material, and the practical defects that the fiber fabric is not resistant to washing, is easy to hook, is easy to fall wool to cause fabric damage and the like greatly reduce the durability and the economical efficiency of the fiber material fabric. In order to eliminate one of the defects of the lyocell fiber material, the fibrillation characteristics of the lyocell fiber material are controlled, and various fiber crosslinking preparation treatment processes are adopted.
At present, the lyocell fiber crosslinking preparation process mainly utilizes the action of a resin crosslinking agent and fibers to carry out fiber crosslinking preparation production, and the process method mainly comprises the processes of spraying and crosslinking preparation on the surface layer of a fiber bundle before fiber cutting, spraying and permeating crosslinking preparation after the fiber bundle is cut and the like.
For example, there are some processes of spraying a crosslinking agent on the surface of a tow before fiber cutting or a preparation process of dipping and binding fibers by a long vehicle, and some processes of spraying a crosslinking agent solution after fiber cutting and a preparation process of permeating and crosslinking. As downstream application merchants of the lyocell fiber material, in the practical process of product development and dyeing production of the lyocell fiber material, the A100 lyocell short silk fibers produced by the fiber crosslinking preparation processes have certain influence on subsequent spinning preparation and dyeing production to different degrees. A brief analysis is made below from the technical aspects of several of the above-described fiber crosslinking preparation processes.
Firstly, the lyocell crosslinked fiber produced by the spray and long-vehicle dip-prick fiber crosslinking preparation process before fiber cutting is mostly acted on the surface layer of the fiber by a crosslinking agent, the wet abrasion resistance detection data after fiber crosslinking is only the detection data before the lyocell crosslinked tow is cut, the fiber crosslinking effect after fiber cutting and spinning is reduced to a certain extent, and the phenomenon that fiber hairiness drops off when color fastness detection is found after dyeing of lyocell short-filament fiber yarn, the fiber coloring condition is observed after fabric forming, and the fabric is in a starry-spotted colored pattern condition.
Secondly, the spraying infiltration fiber crosslinking preparation process after the fiber tows are cut off seems to solve the technical defect of incomplete fiber crosslinking in the fiber crosslinking preparation process, but the fiber crosslinking preparation process has the defects that the glue sticking amount (crosslinking agent) of the fiber body is uneven, even the quality defect of fiber glue blocks can occur, and the subsequent spinning and dyeing production can be seriously influenced. The main marks are quality defects such as incomplete blooming in spinning operation, incomplete cotton carding and the like, and the spinning quality is seriously influenced. Even if the duration and the process strength of the processes of enhancing blooming and cotton carding are increased to meet the requirements of spinning quality process standards, the serious uneven phenomenon of the gluing amount of the fiber body is not solved, and the phenomenon is proved from the plaque spot type color-flower quality defects displayed after the fiber is dyed.
At present, the domestic lyocell fiber crosslinking preparation technology is not mature and is still in a groping stage.
Disclosure of Invention
The invention aims to provide a lyocell short fiber loose fiber dyeing cross-linking agent and a dyeing method aiming at the existing problems, and the invention provides a preparation process for finishing the cross-linking and finishing of lyocell short fiber by applying a loose fiber dyeing process principle.
The above purpose is realized by the following technical scheme:
a method for preparing a lyocell staple fiber loose fiber dyeing crosslinking agent comprises the following steps:
step 1.1, preparing a condensation polymer of diethylenetriamine and dicyandiamide;
step 1.2, taking 100 parts by weight of 1, 3, 5-triacryloylhexahydro-1, 3, 5-triazine cross-linking agent, adding 10-15 parts by weight of the condensation polymer of the diethylenetriamine and the dicyandiamide, prepared in the step 1.1, into a reaction vessel, mixing and stirring, heating to 50 ℃ at the rate of 0.5 ℃ per minute, and keeping the temperature for reaction for 20 minutes; then the temperature is increased to 80 ℃ at the rate of 0.5 ℃ per minute, the reaction is carried out for 120 minutes under the condition of heat preservation and stirring, and the product of the 1, 3, 5-triacryloylhexahydro-1, 3, 5-triazine modified cross-linking agent is obtained.
Further, the preparation of the condensation polymer of diethylenetriamine and dicyandiamide in step 1.1 is that 30.9 parts by weight of diethylenetriamine is added into a reactor, 24.8 parts by weight of dicyandiamide is added under stirring, ammonia is released when the temperature is raised to 100 ℃, then the temperature is raised to 145-160 ℃ at the rate of 0.5 ℃, the material gradually becomes viscous from the liquid state, and after 5-8 hours of reaction, the reactant is discharged, cooled and crushed.
The invention also provides a1, 3, 5-triacryloylhexahydro-1, 3, 5-triazine modified cross-linking agent prepared by the method, which is used as a lyocell short fiber loose fiber dyeing cross-linking agent.
The invention also provides a method for dyeing the loose lyocell short fiber by using the cross-linking agent, which comprises the following steps:
step 2.1, 1, 3, 5-triacryloylhexahydro-1, 3, 5-triazine modified cross-linking agent with the weight ratio of 1.5 percent of the lyocell staple fiber loose fiber to be dyed is filled in a cylinder, and the mixture is diluted into 1: 4000 times of cross-linking agent diluted solution, heating to 40 ℃ at the temperature rising rate of 0.5 ℃, and carrying out heat preservation and leveling for 20 minutes;
2.2, adding soda ash into the cylinder to adjust the pH value of the cross-linking agent solution to 11-12 to be alkaline, and carrying out heat preservation and uniform dyeing for 30-40 minutes when the temperature rise rate is 0.5 ℃ to 60 ℃;
step 2.3, squeezing and removing fiber moisture in the cylinder until the water content of the fiber is 1.8 times of the weight ratio of the fiber; drying by radio frequency hot air at 90 ℃ until the moisture content of the fiber is 20% -25%;
and 2.4.160 ℃ baking and fixing for 3-5 minutes, and then balancing for 6 hours in a balancing chamber with constant temperature of 35 ℃ and relative humidity of 65%.
Compared with the prior art, the invention has the following beneficial effects:
1. after the 1, 3, 5-triacryloylhexahydro-1, 3, 5-triazine cross-linking agent is modified, the hydrophilicity of the molecular structure of the cross-linking agent is improved, the cross-linking agent can be fully dissolved in water, a binding group similar to the molecular structure of a reactive dye is generated through the action of alkaline catalysis, the cross-linking agent is slowly and uniformly attached to a fiber body under the corresponding suitable temperature condition, and the cross-linking agent has the greatest advantage that the cross-linking agent molecules are more uniformly and firmly combined with the fiber.
2. The dyeing uniformity of the lyocell crosslinked fiber prepared by the process is guaranteed, and experiments show that the lyocell fiber is relatively obvious in anionic property after being treated by the fiber crosslinking preparation process, the affinity of the reactive dye and the fiber body is influenced to a certain extent during dyeing, but the problem is not solved, and the problem can be easily solved by slightly improving the anhydrous sodium sulphate concentration ratio in the dye solution.
3. The fiber crosslinking preparation process has low fiber crosslinking process temperature and short process reaction time; the fiber crosslinking preparation equipment is low in investment, the existing fiber loose fiber dyeing equipment in the market can be used for fiber crosslinking preparation mass production, and special fiber crosslinking equipment does not need to be developed.
Detailed Description
A method for preparing a lyocell staple fiber loose fiber dyeing crosslinking agent comprises the following steps:
step 1.1, preparing a condensation polymer of diethylenetriamine and dicyandiamide;
step 1.2, taking 100 parts by weight of 1, 3, 5-triacryloylhexahydro-1, 3, 5-triazine cross-linking agent, adding 10-15 parts by weight of the condensation polymer of the diethylenetriamine and the dicyandiamide, prepared in the step 1.1, into a reaction vessel, mixing and stirring, heating to 50 ℃ at the rate of 0.5 ℃ per minute, and keeping the temperature for reaction for 20 minutes; then the temperature is increased to 80 ℃ at the rate of 0.5 ℃ per minute, the reaction is carried out for 120 minutes under the condition of heat preservation and stirring, and the product of the 1, 3, 5-triacryloylhexahydro-1, 3, 5-triazine modified cross-linking agent is obtained.
Further, the preparation of the condensation polymer of diethylenetriamine and dicyandiamide in step 1.1 is that 30.9 parts by weight of diethylenetriamine is added into a reactor, 24.8 parts by weight of dicyandiamide is added under stirring, ammonia is released when the temperature is raised to 100 ℃, then the temperature is raised to 145-160 ℃ at the rate of 0.5 ℃, the material gradually becomes viscous from the liquid state, and after 5-8 hours of reaction, the reactant is discharged, cooled and crushed.
The invention also provides a1, 3, 5-triacryloylhexahydro-1, 3, 5-triazine modified cross-linking agent prepared by the method, which is used as a lyocell short fiber loose fiber dyeing cross-linking agent.
The invention also provides a method for dyeing the loose lyocell short fiber by using the cross-linking agent, which comprises the following steps:
step 2.1, 1, 3, 5-triacryloylhexahydro-1, 3, 5-triazine modified cross-linking agent with the weight ratio of 1.5 percent of the lyocell staple fiber loose fiber to be dyed is filled in a cylinder, and the mixture is diluted into 1: 4000 times of cross-linking agent dilution solution, heating to 40 ℃ at the temperature rising rate of 0.5 ℃, and carrying out heat preservation and leveling for 20 minutes;
step 2.2, adding soda ash into the cylinder to adjust the pH value of the cross-linking agent solution to be 11-12 to be alkaline, raising the temperature at 0.5 ℃ to 60 ℃, and carrying out thermal insulation and uniform dyeing for 30-40 minutes;
step 2.3, squeezing and removing fiber moisture in the cylinder until the water content of the fiber is 1.8 times of the weight ratio of the fiber; drying by radio frequency hot air at 90 ℃ until the moisture content of the fiber is 20% -25%;
and (3) baking and fixing at the high temperature of 2.4.160 ℃ for 3-5 minutes, and then balancing in a balance chamber with the constant temperature of 35 ℃ and the relative humidity of 65% for 6 hours.
The parameter table of the fiber crosslinking preparation processing technique of the lyocell short fiber loose fiber dyeing method
| Fiber cross-linking finishing bath ratio | 1：6 |
| Crosslinking agent mother liquor filling amount fiber weight ratio | 1.5％ |
| Flow direction of dyeing main pump | Full time forward outflow |
| Flow frequency of dyeing main pump | 45Hz—50Hz |
| Temperature rise rate of exchange reaction between crosslinking agent diluted solution and fiber | 0.5℃/min |
| First reaction temperature and reaction duration | 40℃/20min |
| Adding soda ash to adjust the pH value of the solution to 11-12 | The liquid quantity ratio is 15-20 g/l |
| Second reaction temperature and reaction duration | 60℃/30min—40min |
| Maximum adsorption dye uptake of cross-linking agent fiber | 95％ |
| The temperature process of the drying and dewatering process is timely and long | 90℃/40min |
| Baking set temperature and process duration | 160℃/3min—5min |
| Equilibrium temperature and moisture regain | 35 ℃/6 hours/13% |
The performance and effect detection data after fiber crosslinking and dyeing are shown in the attached table: the detection data of the Lyocell staple fiber bulk fiber crosslinking finishing experiment are reported as follows:
it can be seen from the above table that after the fiber cross-linking is finished, the color washing resistance effect is improved to some extent, the fabric washing pilling effect is improved to some extent, the fiber fibrillation control effect is obviously improved, and the experimental effect is successful.
The technical means disclosed by the scheme of the invention are not limited to the technical means disclosed by the technical means, and also comprise the technical scheme formed by equivalent replacement of the technical features. The present invention is not limited to the above embodiments, but is within the common general knowledge of those skilled in the art.
Claims (4)
1. A method for preparing a lyocell staple fiber loose fiber dyeing crosslinking agent is characterized by comprising the following steps:
step 1.1, preparing a condensation polymer of diethylenetriamine and dicyandiamide;
step 1.2, taking 100 parts by weight of 1, 3, 5-triacryloylhexahydro-1, 3, 5-triazine cross-linking agent, adding 10-15 parts by weight of the condensation polymer of the diethylenetriamine and the dicyandiamide, prepared in the step 1.1, into a reaction vessel, mixing and stirring, heating to 50 ℃ at the rate of 0.5 ℃ per minute, and keeping the temperature for reaction for 20 minutes; then the temperature is increased to 80 ℃ at the rate of 0.5 ℃ per minute, the reaction is carried out for 120 minutes under the condition of heat preservation and stirring, and the product of the 1, 3, 5-triacryloylhexahydro-1, 3, 5-triazine modified cross-linking agent is obtained.
2. The method for preparing the lyocell staple fiber loose fiber dyeing crosslinking agent according to claim 1, wherein the step 1.1 is to add 30.9 parts by weight of diethylenetriamine into the reactor, add 24.8 parts by weight of dicyandiamide under stirring, when the temperature is increased to 100 ℃, ammonia is released, then the temperature is increased to 145-160 ℃ at a rate of 0.5 ℃, the material gradually becomes viscous from a liquid state, and after 5-8 hours of reaction, the reactant is released, cooled and crushed.
3. A1, 3, 5-triacryloylhexahydro-1, 3, 5-triazine modified crosslinking agent prepared by the method of claim 1 or 2 for use as a lyocell staple fiber fluff dyeing crosslinking agent.
4. A method for dyeing lyocell staple fiber loose fibers with the crosslinking agent of claim 3, comprising the steps of:
step 2.1, 1, 3, 5-triacryloylhexahydro-1, 3, 5-triazine modified cross-linking agent with the weight ratio of 1.5 percent of the lyocell staple fiber loose fiber to be dyed is filled in a cylinder, and the mixture is diluted into 1: 4000 times of cross-linking agent diluted solution, heating to 40 ℃ at the temperature rising rate of 0.5 ℃, and carrying out heat preservation and leveling for 20 minutes;
step 2.2, adding soda ash into the cylinder to adjust the pH value of the cross-linking agent solution to be 11-12 to be alkaline, raising the temperature at 0.5 ℃ to 60 ℃, and carrying out thermal insulation and uniform dyeing for 30-40 minutes;
step 2.3, squeezing and removing fiber moisture in the cylinder until the water content of the fiber is 1.8 times of the weight ratio of the fiber; drying by radio frequency hot air at 90 ℃ until the moisture content of the fiber is 20% -25%;
and (3) baking and fixing at the high temperature of 2.4.160 ℃ for 3-5 minutes, and then balancing in a balance chamber with the constant temperature of 35 ℃ and the relative humidity of 65% for 6 hours.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202210665987.3A CN115045125A (en) | 2022-06-14 | 2022-06-14 | Lyocell staple fiber loose fiber dyeing crosslinking agent and dyeing method |
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| CN202210665987.3A CN115045125A (en) | 2022-06-14 | 2022-06-14 | Lyocell staple fiber loose fiber dyeing crosslinking agent and dyeing method |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115627632A (en) * | 2022-10-12 | 2023-01-20 | 中国纺织科学研究院有限公司 | Lyocell staple fiber and preparation method thereof |
| CN117552199A (en) * | 2023-09-30 | 2024-02-13 | 恒天宝丽丝生物基纤维股份有限公司 | Lyocell fiber cross-linking preparation production line device and its use method |
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2022
- 2022-06-14 CN CN202210665987.3A patent/CN115045125A/en not_active Withdrawn
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115627632A (en) * | 2022-10-12 | 2023-01-20 | 中国纺织科学研究院有限公司 | Lyocell staple fiber and preparation method thereof |
| CN117552199A (en) * | 2023-09-30 | 2024-02-13 | 恒天宝丽丝生物基纤维股份有限公司 | Lyocell fiber cross-linking preparation production line device and its use method |
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Application publication date: 20220913 |