Method for continuously preparing cellulose/ionic liquid solution

A technology of ionic liquid and cellulose, applied in the field of continuous preparation of cellulose/ionic liquid solution, can solve the problem that the materials dissolved at the same time cannot enter the spinning or film-making process at the same time, the degree of cellulose degradation is different, and it cannot move forward normally. Conveying and other problems to achieve the effect of maintaining product quality, uniform preparation, and avoiding serious degradation

Active Publication Date: 2011-03-30
INST OF CHEM CHINESE ACAD OF SCI +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the research, it was further found that in addition to the low dissolution efficiency, the batch dissolution method has another disadvantage: the materials dissolved at the same time cannot enter the spinning or film making process at the same time, so the degree of cellulose degradation is different.
The reason why the liquid is not added directly at the feeding end is that the ability of the screw to push the low-viscosity liquid forward is very poor. Adding liquid at the feeding end will cause the material to slip and cannot be conveyed normally.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] Add 30 g of ionic liquid 1-allyl-3-methylimidazolium chloride salt and 3.33 g of wood pulp powder into a 200 ml beaker, stir evenly with a glass rod to form a slushy mixture, and then feed CS with a small spoon -194 single-screw extruder, extruder screw diameter is 10mm, aspect ratio is 8. The temperature of the fuselage and the head is set at 100-120°C, the feeding funnel is cooled with tap water, and the speed of the extruder is 30-100 rpm. Obtain a uniform and transparent amber cellulose solution at the handpiece, and fine air bubbles can be seen through careful observation.

Embodiment 2

[0033] Add 300 grams of ionic liquid 1-butyl-3-methylimidazolium chloride salt and 40 grams of wood pulp powder into a reaction kettle equipped with a vacuum system with a volume of 1 liter, and start stirring after vacuuming to -0.1MPa. The speed is 300 rpm, stop stirring after half an hour, ventilate the atmosphere, open the kettle to take out the uniform oozy mixture, and then feed it into the Haake single-screw extruder with a feeder. The screw diameter of the extruder is 30 mm, long The diameter ratio is 30. The temperature of the feeding section is set at 60°C, the temperature of the other sections is 90-120°C, and the speed of the extruder is 50-250 rpm. A uniform and transparent amber cellulose solution was obtained at the machine head, and an obvious bubble appeared every about 30-60 seconds.

Embodiment 3

[0035] Add 500 grams of ionic liquid 1-allyl-3-methylimidazole acetate, 40 grams of wood pulp powder and 80 grams of microcrystalline cellulose in a reaction kettle equipped with a vacuum system with a volume of 1 liter, and vacuumize Start stirring after reaching -0.1MPa, the stirring speed is 300 rpm, stop stirring after 1 hour, ventilate the atmosphere, open the kettle to take out the uniform oozy mixture, and then feed it into the twin-screw extruder with the screw conveyor, the extruder The diameter of the screw is 30 mm, and the aspect ratio is 45. The temperature of the feeding section is set at 40°C, and the rest of the sections are gradually increased from 60°C to 90-120°C, the temperature of the head is 100°C, and the speed of the extruder is 60-600 rpm. When strips of material begin to appear at the machine head, turn on the vacuum exhaust system. The obtained cellulose solution is uniform and transparent, and no air bubbles can be observed with the naked eye.

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PUM

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Abstract

The invention discloses a method for continuously preparing fiber / ionic liquid solution. It comprises following steps: mixing fiber with ionic liquid solution into soft muddy shape, feeding said soft muddy mixture into feed port of screw extruder for continous dissolution, getting fiber / ionic liquid solution at outlet port of screw extruder. The metioned mixture contains no free ionic liquid solution, and does not possess property of gravity flow and deposition. The invention is characterized in that it employs screw extruder to process said muddy mixture, the solution efficiency of fiber can be increased and time can be reduced by making use of cutting action of extruder, and the degradation of fiber can be avoided. If extruding dissloution process and spinning / filming process can be matched together, the heating time for material can be identical, which will stabilize product quality.

Description

technical field [0001] The present invention relates to a continuous preparation method of cellulose / ionic liquid solution in the production of regenerated cellulose material. Background technique [0002] Cellulose is a natural polymer material with excellent performance. It has the advantages of huge reserves, renewable and degradable. The processing and utilization of cellulose materials has positive significance for the circular economy and sustainable development of the world. Since unmodified cellulose cannot be melted, solution processing has been the main means to prepare regenerated cellulose materials. At present, the viscose method is the most important method for producing regenerated cellulose, but it has the disadvantages of large pollution and high energy consumption. [0003] In recent years, new processes for the preparation of regenerated cellulose materials using ionic liquids have attracted attention. Ionic liquid has the characteristics of low melting ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08J3/02C08L1/02B29C47/38B29C47/92B29C48/395B29C48/92
CPCB29C2947/9259B29C2947/92704B29C48/92B29C2948/9259B29C2948/92704
Inventor 武进王三元张军魏广信何嘉松
Owner INST OF CHEM CHINESE ACAD OF SCI
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