CA2251728A1 - Method for producing a reinforced fiber composite - Google Patents
Method for producing a reinforced fiber composite Download PDFInfo
- Publication number
- CA2251728A1 CA2251728A1 CA002251728A CA2251728A CA2251728A1 CA 2251728 A1 CA2251728 A1 CA 2251728A1 CA 002251728 A CA002251728 A CA 002251728A CA 2251728 A CA2251728 A CA 2251728A CA 2251728 A1 CA2251728 A1 CA 2251728A1
- Authority
- CA
- Canada
- Prior art keywords
- nmmo
- fiber assembly
- cellulose
- aqueous
- solution
- 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.)
- Abandoned
Links
- 239000000835 fiber Substances 0.000 title claims abstract description 41
- 238000004519 manufacturing process Methods 0.000 title abstract description 5
- 239000002131 composite material Substances 0.000 title abstract 6
- LFTLOKWAGJYHHR-UHFFFAOYSA-N N-methylmorpholine N-oxide Chemical compound CN1(=O)CCOCC1 LFTLOKWAGJYHHR-UHFFFAOYSA-N 0.000 claims abstract description 36
- 238000000034 method Methods 0.000 claims abstract description 30
- 229920002678 cellulose Polymers 0.000 claims abstract description 23
- 239000001913 cellulose Substances 0.000 claims abstract description 23
- 239000000243 solution Substances 0.000 claims abstract description 22
- 238000005406 washing Methods 0.000 claims abstract description 6
- 239000007864 aqueous solution Substances 0.000 claims abstract description 5
- 150000001412 amines Chemical class 0.000 claims description 8
- 238000005728 strengthening Methods 0.000 claims description 8
- 229920000297 Rayon Polymers 0.000 claims description 6
- HEMHJVSKTPXQMS-UHFFFAOYSA-M sodium hydroxide Inorganic materials [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 7
- 229920003043 Cellulose fiber Polymers 0.000 description 6
- 239000004745 nonwoven fabric Substances 0.000 description 6
- 239000002904 solvent Substances 0.000 description 5
- 150000003512 tertiary amines Chemical class 0.000 description 5
- 238000005470 impregnation Methods 0.000 description 4
- 239000003960 organic solvent Substances 0.000 description 4
- 229920000433 Lyocell Polymers 0.000 description 3
- 238000004090 dissolution Methods 0.000 description 3
- 239000002657 fibrous material Substances 0.000 description 3
- 238000009987 spinning Methods 0.000 description 3
- 239000000725 suspension Substances 0.000 description 3
- 229920001131 Pulp (paper) Polymers 0.000 description 2
- 230000000712 assembly Effects 0.000 description 2
- 238000000429 assembly Methods 0.000 description 2
- -1 cyclic amine Chemical class 0.000 description 2
- 238000001704 evaporation Methods 0.000 description 2
- 230000008020 evaporation Effects 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 238000001556 precipitation Methods 0.000 description 2
- 238000003825 pressing Methods 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 229920000742 Cotton Polymers 0.000 description 1
- 239000007900 aqueous suspension Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000007664 blowing Methods 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 229910017053 inorganic salt Inorganic materials 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 150000004682 monohydrates Chemical class 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 239000002964 rayon Substances 0.000 description 1
- 239000012266 salt solution Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000002352 surface water Substances 0.000 description 1
- 230000008961 swelling Effects 0.000 description 1
- 229920002994 synthetic fiber Polymers 0.000 description 1
- 239000012209 synthetic fiber Substances 0.000 description 1
- 239000008399 tap water Substances 0.000 description 1
- 235000020679 tap water Nutrition 0.000 description 1
Classifications
-
- D—TEXTILES; PAPER
- D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
- D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
- D04H1/00—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
- D04H1/40—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties
- D04H1/58—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties by applying, incorporating or activating chemical or thermoplastic bonding agents, e.g. adhesives
- D04H1/587—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties by applying, incorporating or activating chemical or thermoplastic bonding agents, e.g. adhesives characterised by the bonding agents used
-
- D—TEXTILES; PAPER
- D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
- D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
- D04H1/00—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
- D04H1/40—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties
- D04H1/42—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties characterised by the use of certain kinds of fibres insofar as this use has no preponderant influence on the consolidation of the fleece
- D04H1/425—Cellulose series
-
- D—TEXTILES; PAPER
- D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
- D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
- D04H1/00—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
- D04H1/40—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties
- D04H1/58—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties by applying, incorporating or activating chemical or thermoplastic bonding agents, e.g. adhesives
- D04H1/64—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties by applying, incorporating or activating chemical or thermoplastic bonding agents, e.g. adhesives the bonding agent being applied in wet state, e.g. chemical agents in dispersions or solutions
- D04H1/645—Impregnation followed by a solidification process
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
- D06M13/322—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing nitrogen
- D06M13/388—Amine oxides
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M23/00—Treatment of fibres, threads, yarns, fabrics or fibrous goods made from such materials, characterised by the process
- D06M23/10—Processes in which the treating agent is dissolved or dispersed in organic solvents; Processes for the recovery of organic solvents thereof
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
- D06M2101/02—Natural fibres, other than mineral fibres
- D06M2101/04—Vegetal fibres
- D06M2101/06—Vegetal fibres cellulosic
Landscapes
- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Dispersion Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Chemical Or Physical Treatment Of Fibers (AREA)
- Artificial Filaments (AREA)
- Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
- Nonwoven Fabrics (AREA)
- Reinforced Plastic Materials (AREA)
- Manufacture Of Alloys Or Alloy Compounds (AREA)
- Yarns And Mechanical Finishing Of Yarns Or Ropes (AREA)
- Paper (AREA)
Abstract
The invention relates to a method for producing a reinforced fiber composite which contains cellulosic fibers, the cellulose being present in the crystalline structure cellulose II, by bringing said fiber composite into contact with an aqueous solution of N-methylmorpholin-N-oxide (NMMO) at an elevated temperature and subsequently washing said fiber composite. Said method is characterized in that the fiber composite is brought into contact with the aqueous solution in such a way that the reationship -947 + 0.30xlog(10)t + 0.046xT - 3.53xC + 645xlog(10)C where t is the time in minutes during which the fiber composite is kept in contact with the aqueous NMMO solution, T is the temperature of the aqueous NMMO solution in ~C and C is the concentration of the NMMO in % mass in relation to the aqueous NMMO solution, gives a figure in the region of 0.30 and 1.70 on the condition that the temperature T is less than 130 ~C and the concentration C lies in the region of 70 to 84 % mass.
Description
CA 022~1728 1998-10-14 l Z ?~
Process for Producin~g a Strer~thened Fiber A~c~rnhly The present invention relates to a process for producing a strengthened fiber assembly cont~ining cellulosic fibers with the cellulose being present in the crystalline structure of cellulose II, by contacting the fiber assembly with an aqueous solution of N-methylmorpholine-N-oxide (NMMO) at elevated temperature and subsequently washing the fiber assembly.
For the purposes of this description and the annexed claims, the expression "fiber assembly"
is to denote any kind of wovens, nonwovens or random webs.
During the past years, a number of processes in which cellulose is dissolved in an organic solvent, a combination of an organic solvent with an inorganic salt, or in aqueous salt solutions, without forming a derivative have been described as alternatives to the viscose process. Cellulose fibers made of such solutions were given the generic name lyocell by BISFA (The Tntern~tional Bureau for the Standardisation of Man-Made Fibres). According to the BISFA definition, lyocell is a cellulose fiber obtained from an organic solvent by means of a spinning process. By "organic solvent", a ~ e of an organic chemical and water is understood by BISFA.
To date but a single process for the production of a cellulose fiber of the lyocell type has, however, become accepted to the point of large-scale realization, namely the amine oxide process. In that process, N-methylmorpholine-N-oxide (NMMO) is preferably used as the solvent. For the purposes of the instant specification, the term "tertiary amine oxides"
substitutionally is referred to by the abbreviation " NMMO", NMMO additionally representing the presently plef~lled N-methylmorpholine-N-oxide.
Tertiary amine oxides have been known for long as alternative solvents for cellulose. Thus, it is known, for instance, from U.S. Patent No. 2,179,181 that tertiary amine oxides are capable of dissolving high-quality chemical pulp without the formation of derivatives and that cellulose moulded bodies such as fibers may be obtained from such solutions by precipitation.
U.S. Patents Nos. 3,447,939, 3,447,956 and 3,508,941 describe further processes for the production of cellulose solutions with cyclic amine oxides being used as the preferred solvents. In all of those processes, cellulose is physically dissolved at elevated temperature.
In EP-A - 0 356 419 to applicant a process is decribed, which preferably is carried out in a thin-layer treating apparatus in which a suspension of the comminlltecl pulp in an aqueous tertiary amine oxide is spread in the form of a thin layer, transported over a heating surface, while the surface of the thin layer is exposed to a vacuum. During transportation of the CA 022~1728 1998-10-14 suspension over the heating surface water is evaporated and the cellulose can be dissolved such that a spinnable cellulose solution is discharged from the thin-layer treating apparatus.
A process and an arrangement for spinning cellulose solutions are known, for instance, from WO 93/19230 to applicant. There, the spinning solution is spun in the hot state and the filaments obtained are introduced into a plecipilation bath in order to precipitate the cellulose contained therein, the filaments being cooled prior to their introduction into the precipitation bath. Cooling is effected immediately after moulding and, preferably, consists in horizontally blowing air at the cellulose moulded body.
German Patent No. 902 427 describes the strengthening of a fleece of cellulose fibers by means of a lye bath co~ g S to 15 % NaOH. The celluose fibers are swollen by the lye bath and thereby strengthened.
From WO 95/07386 to applicant, a process for producing paper is known, in which an aqueous suspension of commin~-te-l cellulose material is mechanically treated and subsequently subjected to a sheet forming procedure, the suspension cont~ining tertiary amine oxide. That process allows for the production of high-strength paper.
A process for strengthening a fibrous material is known from US-A - 3,447,956.
Strengthening is effected in that the fibrous m~t~n~l iS soaked with an amine oxide and heated to a temperature at which the amine oxide is able to strengthen the fibrous material. Proposed fibrous materials are wovens and nonwovens cOI~t~ natural cellulosic fibers such as, e.g., wood pulp, cotton, linen, but also synthetic fibers such as rayon (viscose fibers). Particularly plefe..ed is the treatment of paper with amine oxide. In doing so, NMMO apparently is used as a monohydrate in the molten or liquid state or dissolved in a volatile solvent capable of being evaporated.
From WO 96/37653 fiber assemblies provided with a cellulosic coat, impregnation or sheath are known. Those fiber assemblies are produced by coating the fiber assembly on one side with a solution of cellulose in aqueous NMMO, whereupon the layer is coagulated in a water bath.
US-A - 4,196,282 describes the three-component system NMMO/H2O/cellulose and the so-called "dissolution frame", i.e., those conditions under which the cellulose dissolves in aqueous NMMO.
CA 022~1728 1998-10-14 Furthermore, it is known that cellulose fibers may be swollen with NMMO (Chancy et al., "Swelling and Dissolution of Cellulose in Amine OxidelWater Systems"; J. App. Pol. Sci:
Appl. Pol. Symp. 37, 239-259 (1983)).
The invention has as its object to provide a process of the initially defined kind, in which a fiber assembly can be strengthened without cumbersome evaporation of a volatile solvent and without requiring the use, or preparation by evaporation, of an NMMO monohydrate.
The process according to the invention for producing a strengthened fiber assembly cont~ining cellulosic fibers with the cellulose being present in the crystalline structure of cellulose II, by contacting the fiber assembly with an aqueous solution of N-methylmorpholine-N-oxide (N~O) at elevated temperature and subsequently washing the fiber assembly is characterized in that contacting is effected in a manner that from the relation -947 + 0.30xlog(,0)t + 0.046xT - 3.53xC + 645xlog(10)C
wherein t indicates the time in min~tes during which the fiber assembly is contacted with the aqueous NMMO solution, T indicates the temperature of the aqueous NMMO solution in ~C
and C is the concentration of NMMO in % by mass, based on the aqueous NMMO solution, a number in the range of 0.30 to 1.70 and, preferably, in the range of 0.5 to 1.5 and, in a particularly pl~f~ d manner, in the range of 0.8 to 1.2 results with the proviso that the temperature T is smaller than 130~C and the concentration C ranges between 70 and 84 % by mass.
The invention is based on the finding that, for strengthening an assembly of cellulose fibers such as, e.g., a nonwoven, the three parameters mentioned, i.e., the concentration of the NMMO solution, its temperature and the time of impregnation, app~ently are essential and sufficient and that, in addition, they must be chosen such that the above relation is met. If, in contrast, these parameters are chosen such that a value smaller than 0.30 results from the relation, no strengthening of the assembly will be obtained. If, on the other hand, the parameters are chosen such that a value of more than 1.70 results from the relation, the dissolution of the fiber assembly in the NMMO solution is observed.
In the process according to the invention, the temperature T preferably is smaller than 100~C.
A particular embodiment of the process according to the invention is characterized in that the fiber assembly is pressed before washing. Pressing may be effected in a simple manner, e.g., by conducting the nonwoven between two rolls exerting a p-es~u-e on the fiber assembly.
CA 022~1728 1998-10-14 The use of a fiber assembly cont~ining fibers produced at least partially according to the amine oxide process or the viscose process has proved particularly successful in the process according to the invention.
The invention will be explained in more detail by way of the following examples.
Ge~eral workin~ in~truction Slightly needle punched viscose nonwovens each having a size of 12 x 16 cm and a weight per unit area of about 70 g/cm2 were immersed into an aqueous NMMO solution between two sieves and allowed to impregnate, whereupon the impregnated nonwovens were pressed by means of a laboratory press (pressing plessul~: 3 bars; corresponding to a line pressure of 12.6 N/mm at a nonwoven width of 12 cm). After this, the pressed nonwovens were washed with tap water for 15 minuteS
Fx~les According to the above working instruction, several tests were carried out, the parameters to be set according to the invention, i.e., the concentration of the respective NMMO solution (in % by mass, based on the total mass of the solution), its temperature (in ~C) and the time of impregnation (in minlltes) having been chosen as indicated in Table 1 below. A11 of the examples comply with the above-defined relation. The values resulting with the respective parameters are also apparent from the Table.
Table 1 Ex. NMMO Concentration Temperature Time Value 84.0 80 0.08 0.95
Process for Producin~g a Strer~thened Fiber A~c~rnhly The present invention relates to a process for producing a strengthened fiber assembly cont~ining cellulosic fibers with the cellulose being present in the crystalline structure of cellulose II, by contacting the fiber assembly with an aqueous solution of N-methylmorpholine-N-oxide (NMMO) at elevated temperature and subsequently washing the fiber assembly.
For the purposes of this description and the annexed claims, the expression "fiber assembly"
is to denote any kind of wovens, nonwovens or random webs.
During the past years, a number of processes in which cellulose is dissolved in an organic solvent, a combination of an organic solvent with an inorganic salt, or in aqueous salt solutions, without forming a derivative have been described as alternatives to the viscose process. Cellulose fibers made of such solutions were given the generic name lyocell by BISFA (The Tntern~tional Bureau for the Standardisation of Man-Made Fibres). According to the BISFA definition, lyocell is a cellulose fiber obtained from an organic solvent by means of a spinning process. By "organic solvent", a ~ e of an organic chemical and water is understood by BISFA.
To date but a single process for the production of a cellulose fiber of the lyocell type has, however, become accepted to the point of large-scale realization, namely the amine oxide process. In that process, N-methylmorpholine-N-oxide (NMMO) is preferably used as the solvent. For the purposes of the instant specification, the term "tertiary amine oxides"
substitutionally is referred to by the abbreviation " NMMO", NMMO additionally representing the presently plef~lled N-methylmorpholine-N-oxide.
Tertiary amine oxides have been known for long as alternative solvents for cellulose. Thus, it is known, for instance, from U.S. Patent No. 2,179,181 that tertiary amine oxides are capable of dissolving high-quality chemical pulp without the formation of derivatives and that cellulose moulded bodies such as fibers may be obtained from such solutions by precipitation.
U.S. Patents Nos. 3,447,939, 3,447,956 and 3,508,941 describe further processes for the production of cellulose solutions with cyclic amine oxides being used as the preferred solvents. In all of those processes, cellulose is physically dissolved at elevated temperature.
In EP-A - 0 356 419 to applicant a process is decribed, which preferably is carried out in a thin-layer treating apparatus in which a suspension of the comminlltecl pulp in an aqueous tertiary amine oxide is spread in the form of a thin layer, transported over a heating surface, while the surface of the thin layer is exposed to a vacuum. During transportation of the CA 022~1728 1998-10-14 suspension over the heating surface water is evaporated and the cellulose can be dissolved such that a spinnable cellulose solution is discharged from the thin-layer treating apparatus.
A process and an arrangement for spinning cellulose solutions are known, for instance, from WO 93/19230 to applicant. There, the spinning solution is spun in the hot state and the filaments obtained are introduced into a plecipilation bath in order to precipitate the cellulose contained therein, the filaments being cooled prior to their introduction into the precipitation bath. Cooling is effected immediately after moulding and, preferably, consists in horizontally blowing air at the cellulose moulded body.
German Patent No. 902 427 describes the strengthening of a fleece of cellulose fibers by means of a lye bath co~ g S to 15 % NaOH. The celluose fibers are swollen by the lye bath and thereby strengthened.
From WO 95/07386 to applicant, a process for producing paper is known, in which an aqueous suspension of commin~-te-l cellulose material is mechanically treated and subsequently subjected to a sheet forming procedure, the suspension cont~ining tertiary amine oxide. That process allows for the production of high-strength paper.
A process for strengthening a fibrous material is known from US-A - 3,447,956.
Strengthening is effected in that the fibrous m~t~n~l iS soaked with an amine oxide and heated to a temperature at which the amine oxide is able to strengthen the fibrous material. Proposed fibrous materials are wovens and nonwovens cOI~t~ natural cellulosic fibers such as, e.g., wood pulp, cotton, linen, but also synthetic fibers such as rayon (viscose fibers). Particularly plefe..ed is the treatment of paper with amine oxide. In doing so, NMMO apparently is used as a monohydrate in the molten or liquid state or dissolved in a volatile solvent capable of being evaporated.
From WO 96/37653 fiber assemblies provided with a cellulosic coat, impregnation or sheath are known. Those fiber assemblies are produced by coating the fiber assembly on one side with a solution of cellulose in aqueous NMMO, whereupon the layer is coagulated in a water bath.
US-A - 4,196,282 describes the three-component system NMMO/H2O/cellulose and the so-called "dissolution frame", i.e., those conditions under which the cellulose dissolves in aqueous NMMO.
CA 022~1728 1998-10-14 Furthermore, it is known that cellulose fibers may be swollen with NMMO (Chancy et al., "Swelling and Dissolution of Cellulose in Amine OxidelWater Systems"; J. App. Pol. Sci:
Appl. Pol. Symp. 37, 239-259 (1983)).
The invention has as its object to provide a process of the initially defined kind, in which a fiber assembly can be strengthened without cumbersome evaporation of a volatile solvent and without requiring the use, or preparation by evaporation, of an NMMO monohydrate.
The process according to the invention for producing a strengthened fiber assembly cont~ining cellulosic fibers with the cellulose being present in the crystalline structure of cellulose II, by contacting the fiber assembly with an aqueous solution of N-methylmorpholine-N-oxide (N~O) at elevated temperature and subsequently washing the fiber assembly is characterized in that contacting is effected in a manner that from the relation -947 + 0.30xlog(,0)t + 0.046xT - 3.53xC + 645xlog(10)C
wherein t indicates the time in min~tes during which the fiber assembly is contacted with the aqueous NMMO solution, T indicates the temperature of the aqueous NMMO solution in ~C
and C is the concentration of NMMO in % by mass, based on the aqueous NMMO solution, a number in the range of 0.30 to 1.70 and, preferably, in the range of 0.5 to 1.5 and, in a particularly pl~f~ d manner, in the range of 0.8 to 1.2 results with the proviso that the temperature T is smaller than 130~C and the concentration C ranges between 70 and 84 % by mass.
The invention is based on the finding that, for strengthening an assembly of cellulose fibers such as, e.g., a nonwoven, the three parameters mentioned, i.e., the concentration of the NMMO solution, its temperature and the time of impregnation, app~ently are essential and sufficient and that, in addition, they must be chosen such that the above relation is met. If, in contrast, these parameters are chosen such that a value smaller than 0.30 results from the relation, no strengthening of the assembly will be obtained. If, on the other hand, the parameters are chosen such that a value of more than 1.70 results from the relation, the dissolution of the fiber assembly in the NMMO solution is observed.
In the process according to the invention, the temperature T preferably is smaller than 100~C.
A particular embodiment of the process according to the invention is characterized in that the fiber assembly is pressed before washing. Pressing may be effected in a simple manner, e.g., by conducting the nonwoven between two rolls exerting a p-es~u-e on the fiber assembly.
CA 022~1728 1998-10-14 The use of a fiber assembly cont~ining fibers produced at least partially according to the amine oxide process or the viscose process has proved particularly successful in the process according to the invention.
The invention will be explained in more detail by way of the following examples.
Ge~eral workin~ in~truction Slightly needle punched viscose nonwovens each having a size of 12 x 16 cm and a weight per unit area of about 70 g/cm2 were immersed into an aqueous NMMO solution between two sieves and allowed to impregnate, whereupon the impregnated nonwovens were pressed by means of a laboratory press (pressing plessul~: 3 bars; corresponding to a line pressure of 12.6 N/mm at a nonwoven width of 12 cm). After this, the pressed nonwovens were washed with tap water for 15 minuteS
Fx~les According to the above working instruction, several tests were carried out, the parameters to be set according to the invention, i.e., the concentration of the respective NMMO solution (in % by mass, based on the total mass of the solution), its temperature (in ~C) and the time of impregnation (in minlltes) having been chosen as indicated in Table 1 below. A11 of the examples comply with the above-defined relation. The values resulting with the respective parameters are also apparent from the Table.
Table 1 Ex. NMMO Concentration Temperature Time Value 84.0 80 0.08 0.95
2 82.0 80 0.08 1.30
3 82.0 70 0.17 0.94
4 80.6 70 0.50 1.20 80.6 80 0.08 1.42 6 80.6 80 0.50 1.66 7 78.2 70 1.00 1.29 8 76.2 70 0.50 1.00 9 76.2 80 0.17 1.32 73.9 70 4.00 0.81 11 74.2 80 0.50 1.07 12 74.2 90 0.17 1.39 13 71.9 90 2.00 1.02 CA 022~1728 1998-10-14 14 71.9 100 0.17 1.16 70.0 100 0.50 0.49 Examples 1 to 15 fall within the scope of invention, since the values resulting from the above-mentioned relation with the NMMO concentrations, tempeldlu~es and times of impregnation are within the range defined by the invention. All of the nonwovens were found to be strengthened after having been treated according to the invention.
Similarly good results could be obtained with a nonwoven comprised of fibers produced according to the amine oxide process.
Compar~tive Fxan~ples For reasons of comparison, additional tests were carried out according to the general working instruction, yet the parameters had been chosen such that the relation was not met. These examples are summarized in Table 2.
Table 2 Ex. NMMOConcentrationTemperature Time Value 16 82.0 90 0.17 1.86 17 80.6 80 1.00 1.75 18 80.6 90 0.08 1.88 19 78.2 80 2.00 1.84 78.2 90 0.08 1.88 21 76.2 90 0.50 1.92 22 76.2 100 0.08 2.14 23 74.2 100 0.08 1.75 24 72.2 70 4.00 0.29 72.2 120 4.00 2.59 26 70.0 80 12.0 -0.10 27 70.0 90 2.00 0.21 28 70.0 100 0.08 0.25 In case of Examples 16 to 23 and 25, whose parameters yielded values larger than 1.70, the nonwoven dissolved in the NMMO solution.
In case of Examples 24 and 26 to 28, whose parameters yielded values smaller than 0.30, no strengthening of the nonwoven was obtained.
Similarly good results could be obtained with a nonwoven comprised of fibers produced according to the amine oxide process.
Compar~tive Fxan~ples For reasons of comparison, additional tests were carried out according to the general working instruction, yet the parameters had been chosen such that the relation was not met. These examples are summarized in Table 2.
Table 2 Ex. NMMOConcentrationTemperature Time Value 16 82.0 90 0.17 1.86 17 80.6 80 1.00 1.75 18 80.6 90 0.08 1.88 19 78.2 80 2.00 1.84 78.2 90 0.08 1.88 21 76.2 90 0.50 1.92 22 76.2 100 0.08 2.14 23 74.2 100 0.08 1.75 24 72.2 70 4.00 0.29 72.2 120 4.00 2.59 26 70.0 80 12.0 -0.10 27 70.0 90 2.00 0.21 28 70.0 100 0.08 0.25 In case of Examples 16 to 23 and 25, whose parameters yielded values larger than 1.70, the nonwoven dissolved in the NMMO solution.
In case of Examples 24 and 26 to 28, whose parameters yielded values smaller than 0.30, no strengthening of the nonwoven was obtained.
Claims (7)
1. A process for producing a strengthened fiber assembly containing cellulosic fibers with the cellulose being present in the crystalline structure of cellulose II, by contacting the fiber assembly with an aqueous solution of N-methylmorpholine-N-oxide (NMMO) at elevated temperature and subsequently washing the fiber assembly, characterized in that contacting is effected in a manner that from the relation -947 + 0.30xlog(10)t + 0.046xT - 3.53xC + 645xlog(10)C
wherein t indicates the time in minutes during which the fiber assembly is contacted with the aqueous NMMO solution, T indicates the temperature of the aqueous NMMO solution in °C
and C is the concentration of NMMO in % by mass, based on the aqueous NMMO solution, a number in the range of 0.30 to 1.70 results with the proviso that the temperature T is smaller than 130°C and the concentration C ranges between 70 and 84 % by mass.
wherein t indicates the time in minutes during which the fiber assembly is contacted with the aqueous NMMO solution, T indicates the temperature of the aqueous NMMO solution in °C
and C is the concentration of NMMO in % by mass, based on the aqueous NMMO solution, a number in the range of 0.30 to 1.70 results with the proviso that the temperature T is smaller than 130°C and the concentration C ranges between 70 and 84 % by mass.
2. A process according to claim 1, characterized in that the parameters t, T and C are chosen such that a number in the range of 0.5 to 1.5 results from the relation.
3. A process according to claim 2, characterized in that the parameters t, T and C are chosen such that a number in the range of 0.8 to 1.2 results from the relation.
4. A process according to any one of claims 1 to 3, characterized in that the temperature T is smaller than 100°C.
5. A process according to any one of claims 1 to 4, characterized in that the fiber assembly is pressed prior to washing.
6. A process according to any one of claims 1 to 5, characterized in that a fiber assembly whose fibers have at least partially been produced according to the amine oxide process is used for strengthening.
7. A process according to any one of claims 1 to 5, characterized in that a fiber assembly whose fibers have at least partially been produced according to the viscose process is used for strengthening.
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| ATA319/97 | 1997-02-25 | ||
| AT0031997A AT404368B (en) | 1997-02-25 | 1997-02-25 | METHOD FOR PRODUCING A FASTENED FIBER COMPOSITE |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CA2251728A1 true CA2251728A1 (en) | 1998-09-03 |
Family
ID=3487424
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CA002251728A Abandoned CA2251728A1 (en) | 1997-02-25 | 1998-02-25 | Method for producing a reinforced fiber composite |
Country Status (12)
| Country | Link |
|---|---|
| EP (1) | EP0901533B1 (en) |
| JP (1) | JP2000509771A (en) |
| CN (1) | CN1105798C (en) |
| AT (2) | AT404368B (en) |
| AU (1) | AU727252B2 (en) |
| BR (1) | BR9805914A (en) |
| CA (1) | CA2251728A1 (en) |
| DE (1) | DE59800265D1 (en) |
| ES (1) | ES2152745T3 (en) |
| ID (1) | ID20258A (en) |
| NO (1) | NO310205B1 (en) |
| WO (1) | WO1998038373A1 (en) |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE102009028306B4 (en) * | 2009-08-06 | 2011-04-21 | Tpr Fiberdur Gmbh & Co. Kg | double tube |
| EP2363108B1 (en) | 2010-03-02 | 2017-08-30 | Neubourg Skin Care GmbH & Co. KG | Foam formulation containing at least one triterpenoid |
| DE202015102564U1 (en) | 2015-05-19 | 2015-08-13 | W. Pelz Gmbh & Co. Kg | Oral tobacco pack |
| CN105728565A (en) * | 2016-04-22 | 2016-07-06 | 安徽联盟模具工业股份有限公司 | Rotating flip type no-indention mold |
Family Cites Families (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE902427C (en) * | 1948-10-12 | 1955-04-04 | Dr Otto Eisenhut | Process for the production of strong, washable, fabric-like, felted fabrics from cellulose fibers without spinning and weaving |
| US3447956A (en) * | 1966-09-02 | 1969-06-03 | Eastman Kodak Co | Process for strengthening swellable fibrous material with an amine oxide and the resulting material |
| AT401072B (en) * | 1993-09-06 | 1996-06-25 | Chemiefaser Lenzing Ag | METHOD FOR PRODUCING PAPER |
| JP3488302B2 (en) * | 1995-01-31 | 2004-01-19 | ユニチカ株式会社 | Hand processing method of cellulose fiber cloth |
| JP3445865B2 (en) * | 1995-04-06 | 2003-09-08 | 花王株式会社 | Cellulosic fiber modification method |
| EP0827557A1 (en) * | 1995-05-22 | 1998-03-11 | Akzo Nobel N.V. | Shaped bodies coated, impregnated or covered with a cellulosic composition |
-
1997
- 1997-02-25 AT AT0031997A patent/AT404368B/en not_active IP Right Cessation
-
1998
- 1998-02-25 CN CN98800507A patent/CN1105798C/en not_active Expired - Lifetime
- 1998-02-25 CA CA002251728A patent/CA2251728A1/en not_active Abandoned
- 1998-02-25 DE DE59800265T patent/DE59800265D1/en not_active Expired - Lifetime
- 1998-02-25 ES ES98903942T patent/ES2152745T3/en not_active Expired - Lifetime
- 1998-02-25 JP JP10537058A patent/JP2000509771A/en active Pending
- 1998-02-25 EP EP98903942A patent/EP0901533B1/en not_active Expired - Lifetime
- 1998-02-25 AU AU62001/98A patent/AU727252B2/en not_active Ceased
- 1998-02-25 WO PCT/AT1998/000040 patent/WO1998038373A1/en not_active Ceased
- 1998-02-25 AT AT98903942T patent/ATE196329T1/en not_active IP Right Cessation
- 1998-02-25 ID IDW980103A patent/ID20258A/en unknown
- 1998-02-25 BR BR9805914A patent/BR9805914A/en active Search and Examination
- 1998-10-20 NO NO19984883A patent/NO310205B1/en not_active IP Right Cessation
Also Published As
| Publication number | Publication date |
|---|---|
| EP0901533B1 (en) | 2000-09-13 |
| AU6200198A (en) | 1998-09-18 |
| ID20258A (en) | 1998-11-12 |
| JP2000509771A (en) | 2000-08-02 |
| DE59800265D1 (en) | 2000-10-19 |
| BR9805914A (en) | 1999-08-24 |
| ES2152745T3 (en) | 2001-02-01 |
| ATE196329T1 (en) | 2000-09-15 |
| NO984883D0 (en) | 1998-10-20 |
| EP0901533A1 (en) | 1999-03-17 |
| ATA31997A (en) | 1998-03-15 |
| AU727252B2 (en) | 2000-12-07 |
| CN1224474A (en) | 1999-07-28 |
| NO984883L (en) | 1998-10-20 |
| AT404368B (en) | 1998-11-25 |
| CN1105798C (en) | 2003-04-16 |
| WO1998038373A1 (en) | 1998-09-03 |
| NO310205B1 (en) | 2001-06-05 |
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