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Method for preparing cellulose spinning fluid

A technology of spinning solution and cellulose, applied in the preparation of cellulose spinning solution, dissolving cellulose pulp in N-methylmorpholine-N oxide to form spinning solution, which can solve the problem of cost increase, Difficult mixing, difficult operation, etc., to achieve the effect of reducing the content, improving the quality of dissolution, and dissolving evenly

Active Publication Date: 2008-08-13
CHINESE TEXTILE ACAD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The invention uses methanol, ethanol or acetone instead of water to combine with NMMO. Due to the strong water absorption of NMMO, it is difficult to realize the mixing of anhydrous NMMO and the appealing organic solvent, and using an organic solution as the coagulation bath will use a large amount of appealing volatile organic solvents. Solvent, the cost has increased, and the operation has also brought new difficulties

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034]Get 9 grams of NMMO with a water content of 13%, put it in a 100ml beaker, place it in a water bath at 65-70°C, and until the solvent is completely melted, add 0.7 grams of ethanol, mix well, and mix 1 gram of wood pulp (first in 80- Dry in an oven at 90°C for 30-40 minutes) Add the mixed solvent and stir continuously and place the beaker in a water bath at 65-70°C for half an hour to immerse the pulp in the mixed solvent and mix evenly, then move the beaker into a vacuum oven for 50 Vacuum at -70°C for 30 minutes to remove ethanol. Finally, stir the material with a glass rod, and move the beaker into an oven at 90-100°C. After 100 minutes, the material dissolves and becomes a transparent orange-yellow liquid.

Embodiment 2

[0036] Take 8.8 grams of NMMO with a water content of 11%, put it in a 100ml beaker, place it in a water bath at 65-70°C, and until the solvent is completely melted, add 1.2 grams of a mixture of methanol and ethanol (0.6 grams each), mix well, and mix 1.2 Add one gram of bamboo pulp (dried in an oven at 80-90°C for 30-40 minutes first) into the mixed solvent and stir continuously, and place the beaker in a water bath at 65-70°C for half an hour to immerse the pulp in the mixed solvent and mix evenly. Then move the beaker into a vacuum oven and vacuumize at 50-70°C for 30 minutes to remove methanol and ethanol. Finally, stir the material with a glass rod, and move the beaker into a 90-100°C oven. After 150 minutes, the material dissolves, and the solution is transparent, but the color is slightly darker than that of Example 1 and Example 2.

Embodiment 3

[0038] Get 8.7 grams of NMMO with a moisture content of 13%, put it in a 100ml beaker, place it in a water bath at 65-70°C, and until the solvent is completely melted, add 1.3 grams of ethanol and mix well. Dry in an oven at 90°C for 30-40 minutes) Add the mixed solvent and stir continuously and place the beaker in a water bath at 65-70°C for half an hour to immerse the pulp in the mixed solvent and mix evenly, then move the beaker into a vacuum oven for 50 Vacuum at -70°C for 30 minutes to remove ethanol. Finally, stir the material with a glass rod, and move the beaker into an oven at 90-100°C. After 210 minutes, the material dissolves, but the solution is dark brown.

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PUM

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Abstract

The invention relates to a preparation method of cellulose spinning solution, including a mixed solvent with low boiling point, volatile, polar organic solvent as a promoter and the N-methylmorpholine-N oxides (NMMO) of 8-18% moisture content; the cellulose pulp is mixed with the mixed solvent forming a uniform mixed materials; the low boiling point volatile organic solvent is removed from the mixed materials and the low content is lower than 5%, the cellulose of mixed materials is dissolved in the NMMO forming the cellulose spinning solution under heating. The invention is used the promoter delaying swelling and preventing premature dissolution of cellulose to reduce the solvent viscosity, the cellulose is dissolved uniformly, completely, the advantage which the pulp is impregnated directly in the high concentration solvent, and overcomes the abuse of uneven mixed, the used promoter is easy to extract and to recycle.

Description

technical field [0001] The invention relates to a preparation method of a cellulose spinning solution, in particular to a method for dissolving cellulose pulp in N-methylmorpholine-N oxide (NMMO) to form a spinning solution, which belongs to the technical field of textiles. Background technique [0002] The use of N-methylmorpholine-N oxide (NMMO) as a solvent for non-toxic spinning to produce cellulose fibers has published hundreds of patents. But in terms of dissolution process, nothing more than the following two methods. [0003] One method is to mix medium-concentration NMMO (moisture content 20-60%) with cellulose pulp to make pulp porridge, and then pass through a thin-film evaporator-type dissolution kettle to remove excess water under vacuum and heating , so that the system enters the solution state. Such as patent US 509469, CN 1181788, CN 1072284, WO 94 / 653 etc., this method has been used in industrial production. There are also patents that do not use a thin-f...

Claims

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Application Information

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IPC IPC(8): D01F2/02
Inventor 江锡夏江渊
Owner CHINESE TEXTILE ACAD
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