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Microwave synthesis method of fiber carbamate

A carbamate and cellulose technology, applied in the field of rapid synthesis of cellulose carbamate, can solve the problems of high cost, high energy consumption, and restrictions on the industrialization of CarbaCell, and achieve shortened production cycle, reduced production cost, high industrial The effect of applying value

Inactive Publication Date: 2009-12-09
WUHAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

These production processes consume a lot of energy and cost, which restricts the industrialization of CarbaCell

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] 100 grams of cotton linter pulp (the degree of polymerization is 590) is soaked in 100 grams of urea aqueous solution with a concentration of 40% by weight. The mixture was stirred at room temperature for 1 hour to fully mix the cellulose and aqueous urea solution, then the stirring was stopped, filtered (the filtrate was recovered and reused), extruded, and then the wet mixture was vacuum-dried. Get 10 grams of dried cellulose / urea solid mixture and put it in a microwave heater, react for 2 minutes under 255W power, then wash off unreacted urea with water (water washing solution is recovered and reused), and obtain cellulose carbamate after drying The ester product has a nitrogen content of 0.651% (weight percent concentration). Infrared spectrum shows that the product is at 1713cm -1 Place shows the characteristic absorption peak of carbamate carbonyl (C=O), the solid of product 13 C NMR at 158.1 ppm showed the characteristic chemical shift of the carbamate carbonyl...

Embodiment 2

[0022] 100 grams of cotton linter pulp (the degree of polymerization is 590) is soaked in 100 grams of urea aqueous solution with a concentration of 40% by weight. The mixture was stirred at room temperature for 1 hour to fully mix the cellulose and aqueous urea solution, then the stirring was stopped, filtered (the filtrate was recovered and reused), extruded, and then the wet mixture was vacuum-dried. Get 10 grams of dried cellulose / urea solid mixture and put it in a microwave heater, react for 3 minutes at a power of 255W, then wash off unreacted urea with water (the washing solution is recovered and reused), and dry to obtain cellulose carbamate The ester product has a nitrogen content of 1.923% (weight percent concentration). Infrared spectrum shows that the product is at 1713cm -1 Place shows the characteristic absorption peak of carbamate carbonyl (C=O), the solid of product 13 C NMR at 158.1 ppm showed the characteristic chemical shift of the carbamate carbonyl group...

Embodiment 3

[0024] 100 grams of cotton linter pulp (the degree of polymerization is 590) is soaked in 100 grams of urea aqueous solution with a concentration of 40% by weight. The mixture was stirred at room temperature for 1 hour to fully mix the cellulose and aqueous urea solution, then the stirring was stopped, filtered (the filtrate was recovered and reused), extruded, and then the wet mixture was vacuum-dried. Get 10 grams of dry cellulose / urea solid mixture and put it in a microwave heater, react for 5 minutes under 255W power, then wash off unreacted urea with water (water washing solution is recovered and reused), and obtain cellulose carbamate after drying The ester product has a nitrogen content of 2.427% (weight percent concentration). Infrared spectrum shows that the product is at 1713cm -1 Place shows the characteristic absorption peak of carbamate carbonyl (C=O), the solid of product 13 C NMR at 158.1 ppm showed the characteristic chemical shift of the carbamate carbonyl g...

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Abstract

The invention discloses a technology of a microwave heating synthesis method of fiber carbamate; the method is that: firstly, the fiber is soaked in carbamide aqueous solution for completely adsorbing the carbamide, the fiber / carbamide even mixture is obtained by filtering and drying, and then the fiber / carbamide mixture is placed in a microwave oven for being heated, thereby obtaining the fiber carbamate. The synthesis technology of the fiber carbamate provided by the invention has no solvent pollution, organic solvents and any catalyzers do not need, the reacting time is speed, and the energy consumption is low. The synthesized fiber carbamate products has good dissolubility in 6 to 10 wt% of NaOH aqueous solution within the temperature range of -10 to 5 DEG C, and the concentrated solution which is stable, transparent and is suitable for industrial spinning and membrane manufacturing can be prepared.

Description

technical field [0001] The invention relates to a method for rapidly synthesizing cellulose carbamate, in particular to a method for rapidly synthesizing cellulose carbamate through microwave heating of cellulose / urea solid mixture. The synthesized cellulose carbamate has good solubility in NaOH aqueous solution and can be used for industrial spinning, film making and other cellulose products. Background technique [0002] Cellulose is the most abundant renewable plant resource on earth, with an annual output of about 200 billion tons. It can produce regenerated cellulose silk, film and non-woven fabrics, etc. So far, the production of cellophane and rayon still adopts the traditional and backward viscose method. Since the production process uses a large amount of CS 2 It causes serious pollution of air, soil and lakes, and damages human health. Developed countries such as the United States, Western Europe, Japan and other countries have banned the production of this metho...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08B15/06
Inventor 周金平郭义张俐娜
Owner WUHAN UNIV
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