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CN-117552123-B - Regenerated bamboo fiber and preparation method and application thereof

CN117552123BCN 117552123 BCN117552123 BCN 117552123BCN-117552123-B

Abstract

The invention relates to the technical field of fiber regeneration, in particular to regenerated bamboo fiber and a preparation method and application thereof. The method comprises the steps of (1) conducting defoaming treatment on spinning solution of a bamboo cellulose carbamate solution to obtain spinning solution, (2) conducting spinning extrusion on the spinning solution into a coagulating bath, conducting water washing and drying molding after molding in the coagulating bath to obtain regenerated bamboo fibers, wherein the bamboo cellulose carbamate solution comprises 6-10wt% of sodium hydroxide, 0.5-6wt% of urea, 84-94wt% of water and 6-9wt% of bamboo cellulose carbamate, and the nitrogen content of the bamboo cellulose carbamate is not higher than 1.0% based on the total weight of the bamboo cellulose carbamate solution.

Inventors

  • XU DINGFENG
  • LIANG PIN
  • LI XINGXING
  • LI YIBAO

Assignees

  • 赣南师范大学

Dates

Publication Date
20260505
Application Date
20230302

Claims (11)

  1. 1. The preparation method of the regenerated bamboo fiber is characterized by comprising the following steps: (1) Carrying out deaeration treatment on the spinning solution of the bamboo cellulose carbamate solution to obtain spinning solution; (2) Spinning the spinning solution, extruding the spinning solution into a coagulating bath, forming in the coagulating bath, and washing, drying and forming to obtain regenerated bamboo fibers; the bamboo cellulose carbamate solution comprises, based on the total weight of the bamboo cellulose carbamate solution: 6-10 wt% of sodium hydroxide, 0.5-6 wt% of urea, 84-94 wt% of water and 6-9 wt% of bamboo cellulose carbamate; The nitrogen content of the bamboo cellulose carbamate is not higher than 1.0%.
  2. 2. The preparation method according to claim 1, wherein, The molecular weight of the bamboo cellulose carbamate is 3.7-5W, and/or The bamboo cellulose carbamate has a nitrogen content of 0.6-1.0%, and/or The bamboo fiber carbamate has characteristic peaks of type I cellulose.
  3. 3. The preparation method according to claim 1, wherein, The solution comprises 7-8 wt% of sodium hydroxide, 4-6 wt% of urea, 86-89 wt% of water and 6-9 wt% of bamboo cellulose carbamate.
  4. 4. A method of preparing a bamboo cellulose carbamate solution according to any one of claims 1 to 3, comprising: Cooling a solution containing 6-10wt% of sodium hydroxide, 0.5-6wt% of urea and 84-94wt% of water to minus 5-10deg.C, and dispersing the bamboo cellulose carbamate into the solution to obtain a bamboo cellulose carbamate solution.
  5. 5. The method of claim 4, wherein the method of preparing a bamboo cellulose carbamate solution further comprises centrifuging the dispersed bamboo cellulose carbamate solution.
  6. 6. The preparation method according to claim 5, wherein the centrifugation conditions comprise a rotation speed of 5000-8000RPM, a time of 5-10min and a temperature of 5-10 ℃.
  7. 7. The method of claim 1, wherein the coagulation bath comprises 5-15 wt% sulfuric acid, 0-20% sodium sulfate by weight.
  8. 8. The production method according to claim 1, wherein in the step (2), the molding temperature is 3 to 25 ℃.
  9. 9. Regenerated bamboo fiber produced by the production method according to any one of claims 1 to 8.
  10. 10. The regenerated bamboo fiber according to claim 9, wherein the regenerated bamboo fiber is type II cellulose, and/or The dry breaking strength of the regenerated bamboo fiber is 0.91-2.0 cN/dtex.
  11. 11. Use of regenerated fibres as claimed in claim 9 or 10 in bacteriostatic materials.

Description

Regenerated bamboo fiber and preparation method and application thereof Technical Field The invention relates to the technical field of fiber regeneration, in particular to regenerated bamboo fiber and a preparation method and application thereof. Background Plant cellulose is used as the most abundant renewable natural polymer material on earth, and is widely distributed in trees, cotton, bamboo, straw, sea squirts and seaweeds on land, and the plant cellulose has the characteristics of large storage capacity, reproducibility, degradability and the like, so that the cellulose resource is fully utilized, the ecological environment can be protected, and the excessive dependence on petroleum resource is relieved. However, each glucosyl ring in the cellulose macromolecules has three hydroxyl groups, which have decisive influence on reactions such as oxidation, esterification, etherification, graft copolymerization and the like of cellulose, and because cellulose has the structural characteristics of polyhydroxy, a large number of hydrogen bonds exist in molecules and among the molecules, and the molecular chains are closely arranged to form a highly ordered crystallization area due to the existence of the large number of hydrogen bonds, the characteristics of the cellulose are difficult to dissolve in common solvents, and the cellulose is difficult to melt and process. Therefore, it is significant to use a green, inexpensive and efficient solvent to dissolve cellulose. For a long time, the viscose method plays a dominant role in the field of producing regenerated cellulose filaments and films, but the viscose fiber production steps are complicated, and reagents such as zinc sulfate, sulfite, sodium sulfide and the like are used in the production process, so that a large amount of carbon disulfide and hydrogen sulfide harmful gases are generated, (J.macromol.Sci-Rev.macromol.Chem1980, C18 (1), 1) are seriously not in line with the current environmental protection policy in China. In addition, the commercial dissolution system N-methylmorpholine-N-oxide (NMMO) is also expensive and energy-intensive (see Chinese patent ZL97107819. X). In recent years, ionic liquids have been used as a green system, which has good solubility and good recycling properties (see CN 1140422, CN 03116642.3, CN 100572432C), but the system also has the disadvantages that the solution is gel-like and industrial spinning is difficult to perform. The cellulose carbamate technology is a new technology for preparing regenerated cellulose fibers by taking Cellulose Carbamate (CC) as a raw material. The whole production flow of the cellulose carbamate technology is green. However, the dissolution ability of cellulose carbamate is affected by factors such as molecular weight, dissolution temperature, alkali concentration, esterification degree, and the like. Therefore, various methods of dissolving cellulose carbamate have been proposed, such as adding a certain cellulose carbamate to 10wt% sodium hydroxide solution at-5 ℃ and continuously stirring for 1-3 hours (see U.S. Pat. No. 4530999). The scholars can also immerse the cellulose carbamate in 1-2wt% sodium hydroxide solution at 0 ℃, then pour the sodium hydroxide solution at about-20 ℃ into the mixed solution, and stir at-6 ℃ (see WO 2007/060296 Al). In addition, it has been proposed by the scholars to put a certain amount of cellulose carbamate into an aqueous solution of 6-10wt% of sodium hydroxide and 0.1-3wt% of zinc oxide, stir the mixture uniformly, freeze the mixture at-10 to-20 ℃ for 3-5 hours, and then defrost the mixture at room temperature (see CN 102432894B). However, the method has the defects of excessively high alkali consumption, long time consumption, high zinc oxide price and the like, and is not beneficial to industrialization. Although sodium hydroxide is the least expensive reagent to dissolve cellulose carbamate, the solvent only dissolves cellulose with low degree of polymerization (DP < 400), and the solution is unstable, easy to gel, and the strength of the cellulose filaments obtained later is poor (see us patent 4634470). Disclosure of Invention The invention aims to solve the problems of low antibacterial capacity and even loss of antibacterial capacity of regenerated bamboo fibers caused by dissolution and regeneration processes of bamboo cellulose carbamate in the prior art, and provides a regenerated bamboo fiber and a preparation method and application thereof. In order to achieve the above object, a first aspect of the present invention provides a method for preparing regenerated bamboo fiber, comprising: (1) Carrying out deaeration treatment on the spinning solution of the bamboo cellulose carbamate solution to obtain spinning solution; (2) Spinning the spinning solution, extruding the spinning solution into a coagulating bath, forming in the coagulating bath, and washing, drying and forming to obtain regenerated bamboo fibers; the bamboo cellulose carbamate