Improved preparation of cellulose spinning solution with ion liquid as solvent

A spinning dope, ionic liquid technology, applied in spinning solution preparation, rayon filament in cellulose solution, etc., can solve the problems of unstable spinning state, increase of broken ends, lower production efficiency, etc. The effect of reducing the number of broken ends, reducing the waste of raw materials and improving production efficiency

Inactive Publication Date: 2009-07-08
DONGHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, we used a polarizing microscope to track the dissolution process of cellulose and found that: due to the strong dissolving ability of pure ionic liquid to cellulose, during the dissolution process, part of the cellulose in contact with the ionic liquid dissolves quickly, thus forming a dissolved The undissolved cellulose is covered by the cellulose slurry, so that the inner layer of cellulose cannot be completely dissolved, so there is uneven dissolution, gel particles are formed in the spinning solution, and eventually the number of broken ends in the spinning process increases, and the spinning Unstable silk status and serious waste
In addition, the apparent viscosity of the spinning dope prepared by this direct dissolution method is relatively high, which limits the solid content of the spinning dope and reduces production efficiency.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] The cellulose cotton pulp of DP=685 is cut into small pieces of 0.5~4cm×0.5~4cm, and then these cellulose pulps are vacuum-8×10 4 Pa and 30 ° C drying equilibrium 20h, so that the moisture content reached 3%; Weigh 189g of ionic liquid [BMIM]Cl, add 9.95g of deionized water to prepare [BMIM]Cl solution with a moisture content of 5%.

[0017] Put the above-mentioned [BMIM]Cl solution with a water content of 5% and 21 grams of pulverized and dried cellulose cotton pulp in a dissolving device and mix them uniformly, first let it stand for swelling at 80°C for 30 minutes, and then vigorously stir for 15 minutes to make it swell into a slurry Porridge, then slowly raise the temperature of the porridge to 100°C under stirring, and remove the water in the porridge by stirring and vacuum distillation. After 4 hours, the cellulose has completely dissolved, and then reduce the stirring speed. At the same time, the temperature of the slurry was lowered to 95° C., and after maintai...

Embodiment 2

[0021] The cellulose cotton pulp with DP=400 was pulverized, and then vacuum-5×10 4 Pa and 50 ° C drying equilibrium for 12 hours, so that the moisture content reached 4%; Weigh 170g of ionic liquid [BMIM]Cl, add 1.72g of deionized water to prepare [BMIM]Cl solution with a moisture content of 1%.

[0022] Put the above-mentioned [BMIM]Cl solution with a water content of 1% and 30 grams of pulverized and dried cellulose cotton pulp into a dissolving device and mix evenly, first let it stand for swelling at 70°C for 15 minutes and then vigorously stir for 25 minutes to make it swell into a slurry Porridge, then slowly raise the temperature of the porridge to 80°C under stirring, and remove the moisture in the porridge by stirring and vacuum distillation. After 2 hours, the cellulose has completely dissolved, and then reduce the stirring speed. At the same time, the temperature of the slurry was lowered to 90° C., and after maintaining the above conditions for 60 minutes, a unifo...

Embodiment 3

[0025] The cellulose wood pulp of DP=1000 is cut into small pieces of 0.5~4cm×0.5~4cm, then these cellulose pulps are vacuum-9×10 4 Pa and 70°C, dry and balance for 10 hours to make the water content reach 2%. Weigh 186g of ionic liquid [BMIM]Cl and add 46.5g of deionized water to prepare [BMIM]Cl solution with a water content of 20%.

[0026] Put the above-mentioned [BMIM]Cl solution with a water content of 20% and 14 grams of pulverized and dried cellulose cotton pulp into a dissolving device and mix evenly, first let it stand for swelling at 100°C for 60 minutes and then vigorously stir for 40 minutes to make it swell into a slurry Porridge, then slowly raise the temperature of the porridge to 125°C under stirring, and remove the water in the porridge by stirring and vacuum distillation. After 8 hours, the cellulose has completely dissolved, and then reduce the stirring speed. At the same time, the temperature of the slurry was lowered to 100° C., and after maintaining the ...

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Abstract

The invention provides a method for preparing an improved fibrino spinning original solution that ion liquid is used as solvent, which includes: two phases of swelling and dissolution, namely, placing dried fibrino dissolving pulp and 1-butyl-3-methyl imidazole villaumite with 1%-20% water ratio into a dissolution device for uniform mixing, firstly, leaving and swelling in 70-100 DEG. C, then stronger stirring for swelling to plasm shape without dissolution; secondly, raising temperature to 80-125 DEG. C slowly in stirring state, stirring and reducing pressure distillation for removing water component, fibrino can be dissolved completely after 2-8h; finally, reducing stirring speed, and reducing temperature of plasm to 90-100 DEG. C and keeping 30-60 min for obtaining straw yellow spinning original solution. The method provided by the invention has advantages that the spinning original solution is more uniform, dissolution is more fully, gelatin particle in the spinning original solution is reduced, the spinning original solution quality is increased; apparent viscosity of the spinning original solution is reduced, accordingly, solid content in the spinning original solution is increased further.

Description

technical field [0001] The invention belongs to the field of preparation of cellulose spinning stock solution, in particular to an improved preparation method of cellulose spinning stock solution using ionic liquid as a solvent. Background technique [0002] Cellulose is the most abundant natural polymer resource on the earth, and a large amount of cellulose can be produced in nature through green photosynthesis every year. Due to the rich source of cellulose raw materials, and the waste of cellulose products can be degraded naturally, or decomposed into carbon dioxide and water by enzymes. Therefore, in today's increasingly scarce petroleum resources, the production and processing of cellulose as a raw material has attracted much attention. And cellulose fiber and its fiber products are more and more subject to people's favor because of having excellent water absorption, moisture permeability and good wearing comfort. The traditional cellulose fiber is mainly produced by ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): D01D1/02D01F2/02
Inventor 蔡涛胡学超张慧慧邵惠丽杨革生
Owner DONGHUA UNIV
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