A regenerated cellulose fiber material and a method for producing and using the same
By using a composite spinning solution of aprotic polar solvent and polyarylamide solution, the problems of strength and fibrillation of regenerated cellulose fibers have been solved, and high-strength, low-fibrillation regenerated cellulose fiber materials have been prepared for application in textiles, clothing and hygiene materials.
Patent Information
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2025-01-09
- Publication Date
- 2026-03-31
AI Technical Summary
The dry/wet strength and fibrillation degree of existing regenerated cellulose fibers are not ideal, which affects the dimensional stability and abrasion resistance of fabrics, and traditional spinning processes cause environmental pollution problems.
A composite spinning solution is formed using an aprotic polar solvent and a polyarylamide solution. Polyarylamide/cellulose composite fibers are prepared by a dry-jet wet spinning process, followed by stretching, oiling, and drying to form high-strength regenerated cellulose fiber materials.
It significantly improves the dry/wet strength of regenerated cellulose fibers and reduces fibrillation, thereby enhancing the mechanical properties and processing ease of the fibers, making them suitable for textiles, apparel, and hygiene materials.
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Figure CN119800537B_ABST
Abstract
Description
Technical Field
[0001] This invention relates to the field of regenerated cellulose technology, and more specifically to a regenerated cellulose fiber material, its preparation method, and its application. Background Technology
[0002] Regenerated cellulose fibers are produced by dissolving natural cellulose (such as wood pulp and cotton linters) in a specific solvent to form a polymer solution, which is then regenerated into the desired solid fiber form through various fiber spinning techniques. Regenerated cellulose fibers are characterized by good moisture absorption, comfortable wear, and excellent spinnability, and are often blended with cotton, wool, or various synthetic fibers for use in various clothing and decorative textiles. Traditional wet spinning processes for producing viscose fibers are being replaced by new environmentally friendly cellulose dissolving systems, such as ionic liquids, sodium hydroxide (NaOH) / urea / thiourea systems, or N-methylmorpholine-N-oxide (NMMO) solvents, due to significant environmental pollution issues. Research and development of technologies and processes to achieve green, environmentally friendly, and high-strength regenerated cellulose fibers have significant social and economic benefits, and are conducive to promoting the sustainable development and product upgrading of my country's chemical fiber industry.
[0003] Currently, the production of sustainable, high-performance fabrics requires high dry / wet strength in individual (short fiber) fibers. While the inexpensive NaOH / urea / thiourea system can rapidly dissolve cellulose and produce novel cellulose composite fibers through wet spinning, the strength issues exhibited by these fibers (especially since wet strength is typically only about half of dry strength) often lead to poor dimensional stability and abrasion resistance in fabrics made from such cellulose fibers. Ionic liquids and NMMO, as solvents for cellulose, require crucial viscosity control during the spinning process: excessively high viscosity affects the fluidity of the spinning solution, leading to spinning difficulties and consequently impacting fiber formation and properties; excessively low temperatures result in excessively high spinning solution viscosity; excessively high temperatures lead to cellulose degradation. Furthermore, lyocell fibers typically exhibit a high tendency to fibrillate under wet, swollen, or high-mechanical-abrasion conditions, limiting their application in the textile and apparel industry.
[0004] Therefore, while ensuring the toughness of regenerated cellulose fibers, efficiently improving the dry / wet strength of the fibers and reducing the degree of fibrillation is a common technical challenge in both scientific research and production practice. Summary of the Invention
[0005] This invention provides a regenerated cellulose fiber material, its preparation method, and its application, in order to solve the problems of insufficient dry / wet strength and fibrillation degree of regenerated cellulose in the prior art.
[0006] In a first aspect, the present invention provides a method for preparing regenerated cellulose fiber material, comprising the following steps: adding a co-solvent to swell cellulose pulp, then adding it to a dissolving system and stirring to dissolve it, thereby obtaining a cellulose solution; wherein the co-solvent is an aprotic, polar solvent; adding a polyarylamide solution to the cellulose solution under high-speed stirring to form a polyarylamide / cellulose composite spinning solution; spinning the polyarylamide / cellulose composite spinning solution through a spinning device and then introducing it into a deionized water coagulation bath to obtain polyarylamide / cellulose composite fiber; and performing post-treatment operations on the polyarylamide / cellulose composite fiber to obtain the regenerated cellulose fiber material.
[0007] As one possible implementation, the mass ratio of the cellulose pulp, the co-solvent, and the dissolving system is 1:8~12:8~12; and / or, the solid content of the cellulose solution is 4 wt%~10 wt%.
[0008] And / or, the mass ratio of the polyarylamide solution to the cellulose solution is 1:19~99; and / or, the swelling time is 50~70 min; and / or, the stirring and dissolving conditions are: temperature 70~90℃, duration 200~300 min.
[0009] As one possible implementation, the post-processing operation includes the following steps: sequentially stretching, oiling, and drying the polyaramid / cellulose composite fiber to obtain the regenerated cellulose fiber material.
[0010] As one possible implementation, the polyarylamide is any one of heterocyclic aromatic polyamide, poly(p-phenylene terephthalamide), poly(p-phenylene terephthalamide), and poly(m-phenylene isophthalamide); and / or, the co-solvent is any one of 1,3-dimethyl-2-imidazolinone, N,N-dimethylformamide, dimethyl sulfoxide, N,N-dimethylacetamide, acetonitrile, and hexamethylphosphoric triamine; and / or, the dissolution system is any one of 1-butyl-3-methylimidazolium chloride, N-methylmorpholine-N-oxide, imidazolium-type ionic liquid, quaternary ammonium-type ionic liquid, pyrrolidine-type ionic liquid, piperidine-type ionic liquid, and N-methylmorpholine-N-oxide.
[0011] As one possible implementation, the preparation process of the heterocyclic aromatic polyamide includes the following steps: adding p-phenylenediamine, 2-(4-aminophenyl)-5-aminobenzimidazole and terephthaloyl chloride to a dimethylacetamide / lithium chloride solution in a molar ratio of 1:1:2 to obtain a solution of the heterocyclic aromatic polyamide.
[0012] In a second aspect, the present invention provides a regenerated cellulose fiber material prepared by the preparation method described in any possible implementation of the first aspect.
[0013] As one possible implementation, its wet strength is 60.27~79.38 MPa and its dry strength is 192.32~218.06 MPa, and its strength will be further improved in industrial production.
[0014] Thirdly, the present invention provides the application of regenerated cellulose fiber materials prepared by the preparation method described in any possible implementation of the first aspect or the regenerated cellulose fiber materials described in any possible implementation of the second aspect in the fields of textiles and / or sanitary materials.
[0015] As one possible implementation, the regenerated cellulose fiber material is blended with natural and synthetic fibers for use in textiles.
[0016] As one possible implementation, the natural fibers include, but are not limited to, cotton, wool, linen, and bamboo fibers; and / or, the synthetic fibers include, but are not limited to, polyester, spandex, and nylon.
[0017] As one possible implementation, the textiles are used in clothing or decoration.
[0018] The decisive factors for the mechanical properties of regenerated cellulose fibers are the purity of the pulp, the solid content of the spinning solution, or the added reinforcing components. Excessive solid content in the spinning solution leads to increased viscosity, which is detrimental to the spinning process. In regenerated cellulose fiber solutions with added reinforcing components, due to the extremely strong hydrogen bonding between cellulose molecular chains, it is difficult for the reinforcing components to form a homogeneous system with cellulose. Therefore, most processes simultaneously introduce a cross-linking system to avoid phase separation between components. The technical solution provided by this invention introduces an aramid system to reinforce the regenerated cellulose fibers. Both have extremely strong hydrogen bonding between their molecular chains, easily forming a homogeneous system. Furthermore, due to the recombination of hydrogen bonds, the mechanical properties of the regenerated cellulose fibers are significantly improved, and the degree of fibrillation is greatly reduced. In ionic liquid or NMMO systems, the viscosity of the spinning solution is very high. Although high temperatures can reduce the viscosity of the spinning solution, they can cause cellulose degradation. The addition of non-proton polar solvents can effectively reduce the viscosity of the spinning solution, which is beneficial to the spinning process.
[0019] This invention provides a regenerated cellulose fiber material (taking heterocyclic aromatic polyamide as an example). In an ionic liquid system (taking 1-butyl-3-methylimidazolium chloride as an example), a polyarylamide solution is uniformly mixed with a cellulose solution in different proportions to form a polyarylamide / cellulose composite spinning solution. The solution is then spun through a dry-jet wet spinning process and enters a deionized water coagulation bath after being spun by a spinning device to prepare polyarylamide / cellulose composite fibers. The polyarylamide / cellulose composite fibers are then stretched, oiled, and dried to obtain the regenerated cellulose fiber material. The added reinforcing component, polyarylamide, possesses high strength and high modulus. Adding it to regenerated cellulose fibers improves mechanical properties and reduces fibrillation. Furthermore, polyarylamide acts as a reinforcing skeleton in regenerated cellulose fibers, enabling them to withstand greater tensile and compressive forces, thereby increasing fiber strength and modulus. Further, the amide groups on the polyarylamide molecular chain and the hydroxyl groups on the regenerated cellulose fiber molecular chain can form more intermolecular hydrogen bonds and exhibit mass transfer differences, achieving a cross-linked interpenetrating network structure within the fiber molecular chains. This increases the bonding force between fibers, significantly improving the mechanical strength and toughness of the fiber while significantly reducing fibrillation. Simultaneously, the regenerated cellulose fiber material provided by this invention, due to the introduction of a non-protic polar solvent (using 1,3-dimethyl-2-imidazolinone as an example of a co-solvent), reduces the apparent viscosity of the cellulose spinning solution, ensuring smooth processing of the spinning solution. It is simple, cost-effective, highly repeatable, and has significant reinforcing effects, showing potential for large-scale industrial production. Attached Figure Description
[0020] To more clearly illustrate the technical solutions in the embodiments of the present invention or the prior art, the drawings used in the description of the embodiments or the prior art will be briefly introduced below. Obviously, the drawings described below are only some embodiments of the present invention. For those skilled in the art, other drawings can be obtained based on these drawings without creative effort.
[0021] Figure 1 The images show the morphology of heterocyclic aromatic polyamide / cellulose composite spinning solutions A1, A2, and A3 provided in the embodiments of the present invention, wherein a is cellulose solution-D, b is heterocyclic aromatic polyamide / cellulose composite spinning solution-A1, c is heterocyclic aromatic polyamide / cellulose composite spinning solution-A2, and d is heterocyclic aromatic polyamide / cellulose composite spinning solution-A3.
[0022] Figure 2Figure A shows the characterization results provided in the embodiments of the present invention. A represents the quantitative and comparative results of the tensile breaking strength (wet strength) and tensile breaking strength (dry strength) of regenerated cellulose fiber material-D and various regenerated cellulose composite fibers. B represents the elongation at break of regenerated cellulose fiber material-D.
[0023] Figure 3 The image shows the appearance morphology of the heterocyclic aromatic polyamide / cellulose composite fiber-A2 provided in the embodiments of the present invention, wherein a is the macroscopic morphology of the fiber, b is the single fiber strength-elongation relationship curve, c is the fiber surface morphology under scanning electron microscopy, and d is the fiber cross-sectional morphology under scanning electron microscopy.
[0024] Figure 4 The images are optical microscope images of heterocyclic aromatic polyamide-reinforced regenerated cellulose fiber material-A2 and regenerated cellulose fiber material-D provided in the embodiments of the present invention, wherein a, b, and c are regenerated cellulose fiber material-D, and d, e, and f are heterocyclic aromatic polyamide-reinforced regenerated cellulose fiber material-A2. Detailed Implementation
[0025] The technical solutions of the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of the present invention.
[0026] To address the issues of insufficient dry / wet strength and fibrillation degree of regenerated cellulose in existing technologies, this invention provides an experimental method for preparing regenerated cellulose fiber materials.
[0027] A solubilizing agent (aprotic, polar solvent) is added to cellulose pulp to induce swelling, and then added to a dissolving system and stirred to dissolve, yielding a cellulose solution. A polyarylamide solution is added to the cellulose solution under high-speed stirring to form a polyarylamide / cellulose composite spinning solution. The polyarylamide / cellulose composite spinning solution is spun through a spinning device and then placed in a deionized water coagulation bath to obtain polyarylamide / cellulose composite fibers. The polyarylamide / cellulose composite fibers are then subjected to post-treatment to obtain regenerated cellulose fiber materials.
[0028] In this invention, the mass ratio of cellulose pulp, cosolvent, and dissolving system is 1:8~12:8~12; and / or, the solid content of the cellulose solution is 4 wt%~10 wt%; the mass ratio of polyarylamide solution to cellulose solution is 1:19~99; the swelling time is 50~70 min; and the stirring and dissolving conditions are: temperature 70~90℃ and time 200~300 min. The polyarylamide is any one of heterocyclic aromatic polyamide, poly(p-phenyleneamide), poly(p-phenylene terephthalamide), and poly(m-phenylene isophthalamide); the cosolvent is any one of 1,3-dimethyl-2-imidazolinone, N,N-dimethylformamide, dimethyl sulfoxide, N,N-dimethylacetamide, acetonitrile, and hexamethylphosphoric triamine; the dissolution system is any one of 1-butyl-3-methylimidazolium chloride, N-methylmorpholine-N-oxide, imidazolium-type ionic liquid, quaternary ammonium-type ionic liquid, pyrrolidine-type ionic liquid, piperidine-type ionic liquid, and N-methylmorpholine-N-oxide.
[0029] The technical solutions of this invention under the above conditions can all obtain the target product, and the fiber toughness, dry / wet strength and fibrillation degree of the target product can achieve the ideal effect.
[0030] In the embodiments provided by this invention, the preparation conditions of products A1, A2, and A3 were used as examples for characterization and testing. This demonstrated that the regenerated cellulose fiber material provided by this invention has good orientation and a uniform, defect-free cross-section; the regenerated cellulose fiber material provided by this invention has excellent tensile breaking strength and satisfactory fracture toughness; and the regenerated cellulose fiber material provided by this invention has excellent mechanical properties and a significantly lower degree of fibrillation.
[0031] The technical solution of the present invention will be further described below with reference to specific embodiments.
[0032] Example 1
[0033] This embodiment provides an experiment for preparing regenerated cellulose fiber materials.
[0034] Preparation of products A1, A2, and A3: p-phenylenediamine, 2-(4-aminophenyl)-5-aminobenzimidazole, and terephthaloyl chloride were added to a dimethylacetamide / lithium chloride (DMAc / LiCl) solution in a molar ratio of 1:1:2. The reaction was carried out at 30°C for 4 h to obtain a heterocyclic aromatic polyamide solution-A with a solid content of 5%. 10 g of cellulose pulp was added to 95 g of 1,3-dimethyl-2-imidazolinone and swollen for 1 h. Then, 95 g of 1-butyl-3-methylimidazolium chloride was added, and the mixture was stirred and dissolved at 80°C for 4 h to obtain a cellulose solution-A with a solid content of 5 wt%. A heterocyclic aromatic polyamide solution-A was added to a cellulose solution-A at mass ratios of 1:99, 2:98, and 3:97 under stirring at 1000 rpm to obtain heterocyclic aromatic polyamide / cellulose composite spinning solutions-A1, A2, and A3. These solutions were then spun into fibers using a spinning device and subsequently placed in a deionized water coagulation bath to obtain heterocyclic aromatic polyamide / cellulose composite fibers-A1, A2, and A3. Heterocyclic aromatic polyamide / cellulose composite fiber-A1, heterocyclic aromatic polyamide / cellulose composite fiber-A2, and heterocyclic aromatic polyamide / cellulose composite fiber-A3 were sequentially stretched, oiled, and dried to obtain heterocyclic aromatic polyamide-regenerated cellulose fiber material-A1, heterocyclic aromatic polyamide-regenerated cellulose fiber material-A2, and heterocyclic aromatic polyamide-regenerated cellulose fiber material-A3.
[0035] Preparation of Product B: m-Phenylenediamine and isophthaloyl chloride were added to a DMAc / LiCl solution in a 1:1 molar ratio. The reaction was carried out at 30℃ for 4 h to obtain a poly(m-phenylenediamine) solution-B with a solid content of 5%. 5 g of cellulose pulp, 86 g of NMMO, and 9 g of water were mixed and stirred at 90℃ for 4 h to obtain a cellulose solution-B with a solid content of 5 wt%. The poly(m-phenylenediamine) solution-B was added to the cellulose solution-B at a mass ratio of 2:98 under stirring at 1000 rpm to obtain a poly(m-phenylenediamine) / cellulose composite spinning solution-B. The poly(m-phenylenediamine) / cellulose composite spinning solution-B was spun through a spinning device and sequentially fed into a coagulation bath containing 30 wt% and 10 wt% NMMO aqueous solutions to obtain poly(m-phenylenediamine) / cellulose composite fiber-B. Poly(m-phenylene isophthalamide) / cellulose composite fiber-B was sequentially stretched, oiled, and dried to obtain poly(m-phenylene isophthalamide) reinforced regenerated cellulose fiber material-B.
[0036] Preparation of Product C: m-Phenylenediamine and isophthaloyl chloride were added to a DMAc / LiCl solution in a 1:1 molar ratio. The reaction was carried out at 30℃ for 4 h to obtain a solution-C of heterocyclic aromatic polyamide with a solid content of 5%. 10 g of cellulose pulp was added to 95 g of 1,3-dimethyl-2-imidazolinone for swelling for 1 h, followed by the addition of 95 g of 1-butyl-3-methylimidazolium chloride. The mixture was stirred and dissolved at 80℃ for 4 h to obtain a cellulose solution-C with a solid content of 5 wt%. Cellulose solution-C was spun through a spinning device and then placed in a deionized water coagulation bath to obtain cellulose composite fiber-C. Cellulose composite fiber-C was then subjected to stretching, oiling, and drying to obtain regenerated cellulose fiber material-C. The surface of the regenerated cellulose fiber material-C was coated with the heterocyclic aromatic polyamide solution-C, rinsed with water for 10 min for solvent exchange, and then dried to obtain heterocyclic aromatic polyamide-reinforced regenerated cellulose fiber material-C.
[0037] Preparation of Product D: 5 g of cellulose pulp was added to 95 g of 1-butyl-3-methylimidazolium chloride and stirred at 80 °C for 4 h to obtain a cellulose solution-D with a solid content of 5 wt%. Cellulose solution-D was spun into fibers using a spinning device and then placed in a deionized water coagulation bath to obtain cellulose composite fiber-D. Cellulose composite fiber-D was then subjected to stretching, oiling, and drying to obtain regenerated cellulose fiber material-D.
[0038] Example 2
[0039] This embodiment provides a performance characterization experiment for regenerated cellulose fiber materials.
[0040] Rheological characterization of spinning solution: The composite spinning solution to be tested was tested using a digital viscometer (SNB-2, China). 50 mL of the spinning solution to be tested was taken into a beaker and measured at 80℃ using an L4 rotor. The measurement unit is mPa·s.
[0041] Characterization of single-fiber mechanical properties: The mechanical properties of the regenerated cellulose composite fiber under test were tested using an electronic single-yarn tensile tester (YM061, China). The clamping distance was set to 30 mm, the tensile speed was fixed at 10 mm / min, and each sample was measured 5 times and the average value was taken. The wet and dry strength (MPa), elongation at break (%) and breaking energy (cN·mm) were calculated and recorded.
[0042] Fiber morphology characterization: The surface and cross-sectional micromorphology of the regenerated cellulose composite fiber under test were tested using a scanning electron microscope (FEI Quanta 200, USA). For the fiber cross-section, the intact sample was subjected to liquid nitrogen brittle fracture treatment.
[0043] Characterization of antigen-induced fibrillation properties: The regenerated cellulose fiber material under test was evaluated using optical microscopy, and the fibrillation index was calculated (the calculation formula is as follows: I). f = In the formula: I f , where f is the fibrillation index and f is the ratio of the length of the fibrillated fiber to the total fiber length L). The regenerated cellulose fiber material to be tested was cut into small segments of about 2 cm in length, mixed with deionized water, and a fiber slurry with a concentration of 0.1% was prepared. Then, it was treated in an ultrasonic cell disruptor at 500 W for 30 min and 60 min, and the fibrillation performance was evaluated by optical microscopy.
[0044] In this embodiment, the heterocyclic aromatic polyamide / cellulose composite spinning solution-A1, heterocyclic aromatic polyamide / cellulose composite spinning solution-A2, heterocyclic aromatic polyamide / cellulose composite spinning solution-A3, poly(m-phenylene isophthalamide) / cellulose composite spinning solution-B, heterocyclic aromatic polyamide solution-C, and cellulose solution-D from Example 1 were used as the composite spinning solutions to be tested; the heterocyclic aromatic polyamide / cellulose composite fibers-A1, heterocyclic aromatic polyamide / cellulose composite fibers-A2, heterocyclic aromatic polyamide / cellulose composite fibers-A3, and poly(m-phenylene isophthalamide) from Example 1 were used as the composite spinning solutions to be tested. Cellulose composite fiber-B, cellulose composite fiber-C, and cellulose composite fiber-D were used as the regenerated cellulose composite fibers to be tested. Heterocyclic aromatic polyamide-reinforced regenerated cellulose fiber materials-A1, A2, A3, B, C, and D (from Example 1) were used as the regenerated cellulose fiber materials to be tested, and the results are shown in Table 1. Figures 1-4 The results are shown.
[0045] Table 1 Performance characterization results of regenerated cellulose fiber materials
[0046]
[0047] The forms of cellulose solution-D, heterocyclic aromatic polyamide / cellulose composite spinning solution-A1, heterocyclic aromatic polyamide / cellulose composite spinning solution-A2, and heterocyclic aromatic polyamide / cellulose composite spinning solution-A3 are as follows: Figure 1 As shown, the regenerated cellulose spinning solutions with different proportions of heterocyclic aromatic polyamides all exhibit good spinnability. With the increase of the proportion of heterocyclic aromatic polyamides, the apparent viscosity of the spinning solution decreases, which is beneficial for spinning.
[0048] The morphology of the heterocyclic aromatic polyamide / cellulose composite fiber-A1 in Example 1 was observed by scanning electron microscopy, and the results were as follows: Figure 3 The results are shown. (By...) Figure 3 It can be clearly seen that the fibers have good orientation and the cross-section is uniform and free of defects, which is conducive to improving the mechanical properties of the fibers.
[0049] From Table 1 and Figure 2It is known that the heterocyclic aromatic polyamide-reinforced regenerated cellulose fiber materials-A1, A2, and A3 (nascent fibers) prepared in Example 1 of this invention have tensile breaking strength (wet strength) of 60.27~79.38 MPa, and the tensile breaking strength (wet strength) of regenerated cellulose fiber material-D (nascent fibers) is 54.39 MPa; the tensile breaking strength (dry strength) of heterocyclic aromatic polyamide-reinforced regenerated cellulose fiber materials-A1, A2, and A3 (nascent fibers) is 192.32~218.06 MPa, and the tensile breaking strength (dry strength) of regenerated cellulose fiber material-D (nascent fibers) is 154.16 MPa. MPa; the corresponding elongation at break is 200.07%~222.21%, the latter being 219.88%; compared with regenerated cellulose fiber material-D, the breaking work is improved, and the prepared fiber has qualified toughness.
[0050] Optical microscopic images of heterocyclic aromatic polyamide-reinforced regenerated cellulose fiber material-A2 and regenerated cellulose fiber material-D are shown below. Figure 4 As shown, by Figure 4 It can be seen that after fibrillation treatment, the heterocyclic aromatic polyamide / cellulose composite fiber-A2 has a smooth surface with no fine fibrils appearing; while the fibrillation index of regenerated cellulose fiber material-D increases with treatment time, successively reaching 0, 0.1, and 0.2, indicating that fibrillation gradually becomes more severe. This shows that the reinforcing component, heterocyclic aromatic polyamide, added in this scheme forms more intermolecular hydrogen bonds with the regenerated cellulose, realizing a cross-linked interpenetrating network structure of molecular chains within the fiber, improving the mechanical properties of the fiber, and reducing the degree of fibrillation.
[0051] Although preferred embodiments of the invention have been described, those skilled in the art, upon learning the basic inventive concept, can make other changes and modifications to these embodiments. Therefore, the appended claims are intended to be interpreted as including the preferred embodiments as well as all changes and modifications falling within the scope of the invention.
[0052] Obviously, those skilled in the art can make various modifications and variations to this invention without departing from its spirit and scope. Therefore, if these modifications and variations fall within the scope of the claims of this invention and their equivalents, this invention also intends to include these modifications and variations.
Claims
1. A method for the production of regenerated cellulose fibre material, characterised in that, The method comprises the following steps: adding a swelling agent to the cellulose pulp to swell, and then adding a dissolving system to obtain a cellulose solution; wherein the swelling agent is a non-protic polar solvent; adding a polyaramid solution to the cellulose solution under high-speed stirring to form a polyaramid / cellulose composite spinning solution; wherein the polyaramid is a heterocyclic aromatic polyamide, and the preparation process of the polyaramid comprises the following steps: adding p-phenylenediamine, 2-(4-aminophenyl)-5-aminobenzimidazole and terephthaloyl chloride into a dimethylacetamide / lithium chloride solution at a molar ratio of 1:1:2 to obtain a solution of the heterocyclic aromatic polyamide; spinning the polyaramid / cellulose composite spinning solution through a dry-jet wet spinning process to obtain a polyaramid / cellulose composite fiber; performing a post-treatment operation on the polyaramid / cellulose composite fiber to obtain the regenerated cellulose fiber material; wherein the fibrillation index of the regenerated cellulose fiber material is less than 0.1; wherein the swelling agent is any one of 1,3-dimethyl-2-imidazolidinone, N,N-dimethylformamide, dimethyl sulfoxide, N,N-dimethylacetamide, acetonitrile and hexamethylphosphoric triamide; and / or the dissolving system is any one of 1-butyl-3-methylimidazolium chloride, N-methylmorpholine-N-oxide, an imidazole-based ionic liquid, a quaternary ammonium-based ionic liquid, a pyrrolidine-based ionic liquid, a piperidine-based ionic liquid and N-methylmorpholine-N-oxide.
2. The production method according to claim 1, characterized by, The mass ratio of the cellulose pulp, the swelling agent and the dissolving system is 1:8~12:8~12; and / or the solid content of the cellulose solution is 4 wt% ~ 10 wt%; and / or the mass ratio of the polyaramid solution and the cellulose solution is 1:19~99; and / or the swelling time is 50~70 min; and / or the stirring and dissolving condition is a temperature of 70~90℃ and a time of 200~300 min.
3. The preparation method according to claim 1, characterized in that, The post-treatment operation comprises the following steps: performing drawing, oiling and drying operations on the polyaramid / cellulose composite fiber in sequence to obtain the regenerated cellulose fiber material.
4. The regenerated cellulose fiber material prepared by the preparation method of any one of claims 1~3.
5. The regenerated cellulosic fibrous material according to claim 4, characterized in that, The wet strength of the regenerated cellulose fiber material is 60.27~79.38 MPa, and the dry strength is 192.32~218.06 MPa.
6. The application of the regenerated cellulose fiber material prepared by the preparation method of any one of claims 1~3 in the field of textile and / or sanitary materials.
7. Use according to claim 6, characterized in that, The regenerated cellulose fiber material is blended with natural fibers and synthetic fibers to be used in textiles.
8. Use according to claim 7, characterized in that, The natural fibers include but are not limited to cotton, wool, hemp and bamboo fiber; and / or the synthetic fibers include but are not limited to polyester, spandex and nylon; and / or the textiles are used for clothing or decoration.
Citation Information
Patent Citations
Semi-continuous preparation method for solution of heterocycle-containing aromatic polyamide copolymer
CN101985497A
Nanometer aramid fiber reinforced regenerated cellulose fiber material, preparation method and application
CN114507910A