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Chitosan filament and preparation method thereof

A technology of chitosan and filaments, which is applied in the preparation of spinning solution, rayon manufacturing, textiles and papermaking, etc. It can solve the problems of difficulty in popularization, easy fiber adhesion, low concentration of spinning solution, etc., and achieve stable spinning process , high mechanical strength and high spinning yield

Inactive Publication Date: 2013-11-27
JIANGSU SHENGHONG CHEM FIBRE CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, due to poor spinnability and low production efficiency of chitosan fiber, chitosan is expensive and difficult to promote
The low production efficiency of chitosan fiber is mainly due to the difficulty and long cycle of preparation of high-concentration chitosan spinning solution, and the fiber after the drawing bath is difficult to control and time-consuming in the subsequent processing process.
Most researchers at home and abroad use acidic solution to dissolve chitosan, but the concentration of spinning solution is low, and the dissolution process leads to degradation of chitosan, and the spinning process is unstable.
Although the latest ones also have the use of alkaline solvents to dissolve chitosan, such as patent CN200810059136.x, potassium hydroxide and sodium hydroxide aqueous solutions are used to dissolve chitosan, but the lye causes serious water pollution, difficult recovery, equipment corrosion and other problems.
In addition, because the amino groups in chitosan fibers have a strong ability to absorb ions, the fibers in the coagulation bath are not easy to wash, and the fibers are difficult to dry after washing, and the fibers are easy to stick together.
The complexity of the subsequent treatment of chitosan fibers directly affects the production efficiency of chitosan fibers
The invention adopts a green environment-friendly ionic liquid solvent to dissolve chitosan, reasonably controls the dissolution temperature and time to prepare a high-concentration spinning solution, and solves the problem that continuous production is difficult due to the instability of the spinning solution

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] Synthesis and preparation of mixed ionic liquids: firstly, 1 mol of N-methylimidazole was introduced into a 250ml reactor, nitrogen was introduced to exhaust the air, and then 2 mol of ethyl chloride gas was introduced, the reaction temperature was controlled at 85°C, and after 24 hours of reaction Vacuumize to remove excess ethyl chloride to obtain an intermediate product, dissolve the obtained intermediate product in ethanol, add potassium acetate solution, and react at 80°C for 3 hours to obtain acetic acid of 1-ethyl-3-methylimidazole salt [EMIM]Ac;

[0032] The prepared [EMIM]Ac and 1-H-3-methylimidazolium chloride ([HMIM]Cl) ionic liquid were prepared as a mixed solvent in a mass ratio of 1 / 9.

[0033] The preparation of chitosan spinning solution: the chitosan raw material with a deacetylation degree of 85% and a molecular weight of 400,000 is added to a mixed solvent to form a 5% solution, and 1% propyl gallate is added at the same time. Chitosan was dissolved ...

Embodiment 2

[0037] Synthesis and preparation of mixed ionic liquids: firstly, 5 mol of N-methylimidazole was introduced into a 1L reactor, nitrogen was introduced to exhaust the air, and then 5 mol of ethyl chloride gas was introduced, the reaction temperature was controlled at 70°C, and after 60 hours of reaction Vacuumize to remove excess ethyl chloride to obtain an intermediate product, dissolve the obtained intermediate product in ethanol, add potassium acetate solution, and react at 60°C for 12 hours to obtain acetic acid of 1-ethyl-3-methylimidazole salt [EMIM]Ac;

[0038] The prepared [EMIM]Ac and 1-H-3-methylimidazolium chloride ([HMIM]Cl) ionic liquid were prepared as a mixed solvent at a mass ratio of 9.9 / 0.1.

[0039] Preparation of chitosan spinning solution: Add chitosan raw material with a deacetylation degree of 95% and a molecular weight of 200,000 to a mixed solvent to form a 10% solution, and at the same time add 0.5% propyl gallate, using Chitosan was dissolved by grad...

Embodiment 3

[0043] Synthesis and preparation of mixed ionic liquids: firstly, 1 mol of N-methylimidazole was introduced into a 250ml reactor, nitrogen was introduced to exhaust the air, and then 1.2 mol of ethyl chloride gas was introduced, the reaction temperature was controlled at 75°C, and the reaction was carried out for 12 hours Finally, remove excess ethyl chloride by vacuuming to obtain an intermediate product, dissolve the obtained intermediate product in ethanol, add potassium acetate solution, react at 70°C for 6 hours, and obtain the ester of 1-ethyl-3-methylimidazole salt [EMIM]Ac;

[0044] The prepared [EMIM]Ac and 1-H-3-methylimidazolium chloride ([HMIM]Cl) ionic liquid were prepared as a mixed solvent in a mass ratio of 5 / 5.

[0045] Preparation of chitosan spinning solution: add chitosan raw material with a deacetylation degree of 50% and a molecular weight of 1 million to a mixed solvent to form a 2% solution, and at the same time add 1% sodium borate, using gradient temp...

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Abstract

The invention relates to chitosan filaments and a preparation method thereof. According to the invention, chitosan is dissolved by using a green environment-friendly ionic liquid solvent; dissolving time and temperature are reasonably controlled, such that high-concentration spinning solution is prepared. With the method, continuous production can be carried out, such that that problems of difficulty for carrying out continuous productions due to low stability and poor stability of prior art are solved. According to the invention, during the chitosan filament preparation process, the chitosan is dissolved by using the ionic liquid solvent and the gradient temperature method, degradation is prevented during the chitosan heating process, spinning process is stable, the prepared chitosan fiber has high quality, and spinning yield is high. The chitosan filament provided by the invention has high mechanical strength which is higher than 2.5cN / dex and higher than chitosan fiber prepared by using an acidic solution. Therefore, the filament is suitable for the medical field, and has higher application value.

Description

[0001] technical field [0002] The invention relates to a chitosan filament and a preparation method thereof, in particular to a method for directly dissolving chitosan with a green solvent to prepare the chitosan filament, and belongs to the technical field of chemical fiber material manufacturing methods. [0003] Background technique [0004] Chitosan fiber is a fiber produced from marine organisms such as shrimp, crab, and shell waste. It is currently the only pure marine animal regenerated fiber. It neither relies on petroleum resources nor competes with grain and cotton for land, changes the status quo that all renewable biomass fibers rely on plant raw materials, and creates a new way for marine animal shell waste to be used as raw materials for recycled fibers. Chitosan fiber has many natural excellent properties, such as moisture absorption and air permeability, reactivity, biocompatibility, biodegradability, antibacterial and safety, etc., so it is widely used...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): D01F9/00D01F1/02D01D1/02
Inventor 冯淑芹缪汉根唐俊松梅锋张叶兴田会双
Owner JIANGSU SHENGHONG CHEM FIBRE CO LTD
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