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Method for continuously preparing cellulose/ionic liquid solution

A technology of ionic liquid and cellulose, which is applied in the field of continuous preparation of cellulose/ionic liquid solution, which 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. Transportation and other issues, to maintain product quality, uniform preparation, and avoid severe degradation

Active Publication Date: 2007-12-12
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-methylimidazole chloride salt and 3.33 g of wood pulp powder into a 200 ml beaker, stir with a glass rod to form a slimy mixture, and then use a small spoon to feed CS -194 single-screw extruder, the extruder screw diameter is 10 mm, and the ratio of length to diameter is 8. The temperature of the fuselage and machine head is set at 100~120℃, the feeding funnel is cooled with tap water, and the rotation speed of the extruder is 30~100 rpm. A uniform and transparent amber cellulose solution is obtained on the machine head, and small bubbles can be seen by careful observation.

Embodiment 2

[0033] Add 300 grams of ionic liquid 1-butyl-3-methylimidazole chloride salt and 40 grams of wood pulp powder into a reaction kettle with a volume of 1 liter equipped with a vacuum system. After vacuuming to -0.1MPa, start stirring and stirring. Speed ​​300 rpm, stop stirring after half an hour, let the atmosphere open, open the kettle to take out the uniform slime-like mixture, and then use the feeder to feed the Haake single-screw extruder, the extruder screw diameter is 30 mm, length The diameter ratio is 30. The temperature of the feeding section is set at 60°C, the other sections are at 90-120°C, and the speed of the extruder is 50-250 rpm. A uniform and transparent amber cellulose solution is obtained at the handpiece, and an obvious bubble appears every 30 to 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 into a 1 liter reactor equipped with a vacuum system, and vacuumize Start stirring after reaching -0.1MPa, stirring speed 300 rpm, after 1 hour, stop stirring, let the atmosphere open, open the kettle to take out the uniform sludge mixture, and then feed it into the twin-screw extruder and extruder with a screw conveyor The screw diameter is 30 mm and the length to diameter ratio is 45. The temperature of the feeding section is set to 40°C, and the remaining sections are gradually increased from 60°C to 90-120°C, the head temperature is 100°C, and the extruder speed is 60-600 rpm. When strips begin to appear at the nose, turn on the vacuum exhaust system. The resulting cellulose solution was uniform and transparent, and no bubbles were observed with naked eyes.

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

Claims

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Application Information

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IPC IPC(8): C08J3/02C08L1/02B29C47/38B29C47/92B29C48/395B29C48/92
CPCB29C2947/92704B29C2947/9259B29C48/92B29C2948/9259B29C2948/92704
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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