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Cellulose carbamate dissolved combined solvent and using method thereof

A carbamate and cellulose-dissolving technology, applied in the chemical, textile and material fields, can solve the problems of insoluble matter, low stability, unfavorable cellulose carbamate, etc., achieve low cost, improve solubility, high The effect of industrial application value

Active Publication Date: 2012-05-02
WUHAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The viscose process has significant disadvantages: large amounts of toxic CS are produced during the preparation of the spinning solution 2 and H 2 S gas and heavy metal salts
The colloidal insolubles and low stability contained in the cellulose carbamate solution are also unfavorable for the implementation of the cellulose carbamate process

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] The cellulose carbamate used in the dissolution experiment was prepared as follows: a certain amount of cellulose was soaked in 45 wt% urea aqueous solution, soaked for 24 hours, squeezed out the excess urea solution, and dried in an oven to obtain A cellulose-urea mixture with a urea content of 57 wt%. Get 160 grams of this mixture and put it into a microwave heater, react for 15 minutes under 425 W power, then wash away unreacted urea with water, and dry to obtain a viscosity-average molecular weight of 6.5×10 4 , A cellulose carbamate with a nitrogen content of 1.042%.

[0025] Get 13 grams of the above-mentioned synthetic cellulose carbamate, be uniformly dispersed in 200 grams of solution obtained by dissolving water by 12 grams of sodium hydroxide and 3.2 grams of zinc oxide, freeze 5 hours under the condition of -15 ° C, Then take it out and thaw it at room temperature, stir it evenly to obtain a light yellow 6.1 wt% cellulose carbamate solution. The solution h...

Embodiment 2

[0027] The cellulose carbamate raw material used in the dissolution experiment was prepared as follows: a certain amount of cellulose was immersed in a 40 wt% aqueous urea solution, and after soaking for 24 hours, the excess urea solution was squeezed out and dried in an oven , to obtain a cellulose-urea mixture with a urea content of 52 wt %. Get 10 grams of cellulose urea mixture to react under 225 W power for 5 minutes, then wash with water, and finally obtain the viscosity-average molecular weight of 7.0×10 4 , Cellulose carbamate with a nitrogen content of 2.218%.

[0028] Get 4.2 grams of the above-mentioned synthetic cellulose carbamate, disperse in 100 grams of solution obtained by dissolving 7.0 grams of sodium hydroxide and 0.1 gram of zinc oxide in water, freeze at -17 ° C for 5 hours, and freeze at room temperature Thaw at 20°C and stir to obtain a pale yellow 4.0 wt% cellulose carbamate solution. The solution has no obvious change when placed at room temperature...

Embodiment 3

[0030] The cellulose carbamate raw material used in the dissolution experiment was prepared as follows: a certain amount of cellulose was immersed in 33 wt% urea aqueous solution, soaked for 24 hours, filtered, extruded, and dried to obtain a urea content of 49 wt%. % of cellulose urea mixture. Get the mixture of 90 grams of cellulose and urea and put it into a microwave heater, react for 18 minutes under 340W power, wash with water to obtain a viscosity-average molecular weight of 5.7×10 4 Cellulose carbamate with a nitrogen content of 1.218%.

[0031]Get 27.5 grams of cellulose carbamate obtained by the above-mentioned synthesis and disperse in 400 grams of solution obtained by dissolving 32 grams of sodium hydroxide and 3.2 grams of zinc oxide in water, freeze at -20 ° C for 12 hours, and then Thaw at room temperature and stir to obtain a brown 6.4 wt% cellulose carbamate solution. The solution has no obvious change after being placed at room temperature for 72 hours, and...

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PUM

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Abstract

The invention relates to a cellulose carbamate dissolved combined solvent. The solvent is an aqueous solution comprising 6 to 10 weight percent of sodium hydroxide and 0.1 to 3 weight percent of zinc oxide. A dissolving method comprises the following steps of: dispersing a certain amount of cellulose carbamate in a solvent composite, freezing at the temperature of between -20 and -10 DEG C for 3 to 5 hours or freezing in liquid nitrogen for 3 to 5 minutes, unfreezing at the temperature of less than or equal to 50 DEG C, and dissolving to obtain the cellulose carbamate solution at high concentration of 4 to 15 weigh percent. The obtained cellulose carbamate solution is low in sodium hydroxide content, high in solution stability, and has high mobility after standing at normal temperature for several days, and a gel phenomenon is avoided. The cellulose carbamate solution can be used for preparing fibers and films.

Description

field of invention [0001] The invention relates to a combination solvent for dissolving cellulose carbamate and a method for using the same, belonging to the fields of chemistry, textiles and materials. technical background [0002] Plant cellulose is the most abundant renewable resource on the earth. Making full use of cellulose can not only protect the environment, but also save limited petroleum resources. However, because cellulose contains a large number of intramolecular and intermolecular hydrogen bonds, it is difficult to dissolve and melt process. For a long time, in the field of textile regenerated cellulose fibers, viscose fibers have always occupied a major position. The viscose process has significant disadvantages: large amounts of toxic CS are produced during the preparation of the spinning solution 2 and H 2 S gas and heavy metal salts. In addition, the viscose solution is unstable so that it cannot be stored as an intermediate product, and all steps of i...

Claims

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Application Information

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IPC IPC(8): C08J3/03C08L1/08D01F2/02
Inventor 周金平付飞亚
Owner WUHAN UNIV
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