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Method for preparing regenerated cellulose fibers with cellulose carbamate

A carbamate and regenerated cellulose technology, applied in the field of natural polymers and textiles, can solve the problems of high cost, harsh dissolution conditions, and difficult industrialization implementation, and achieve the effects of low cost, short production cycle, and simple and convenient operation.

Inactive Publication Date: 2012-09-26
WUHAN UNIV +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The method disclosed in the patent US 2008 / 0023874A1 is to use N-methyl-N-oxide morpholine (NMMO) as a solvent to obtain a spinning stock solution, and extrude it through a spinneret at 85-95 ° C in 10% NMMO It is solidified and formed in an aqueous solution, and regenerated in a sodium hydroxide solution with a mass fraction of 0.3-1.0% and a temperature of 60-95°C, washed with water, and dried to obtain a certain strength of cellulose urethane fiber, and the strength of the fiber is 3.5- 6.9cN / dtex, the elongation at break is 4.5-9.0%; NMMO solvents and ionic liquids have strong solubility, but they are difficult to implement industrially due to the limitations of harsh dissolution conditions and high cost.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] a. Take 700 grams of cellulose carbamate samples with a nitrogen content of 1.232% (viscosity-average molecular weight 10.2×10 4 ) uniformly dispersed at 10.00×10 4 gram is obtained by dissolving 7.5wt% sodium hydroxide and 1.6wt% zinc oxide in water, put it in the refrigerator and freeze to -10°C, take it out of the refrigerator after freezing, thaw at 50°C, and stir to obtain 6.54wt % Cellulose Carbamate Solution.

[0026] B, the cellulose carbamate solution obtained by dissolving is filtered, left standing in vacuum for defoaming treatment, the gas pressure is 0.2MPa during filtration, the filter cloth is a cotton cloth with a fineness of 350 mesh, the defoaming vacuum degree is 0.01MPa, and the time is After 5 hours, the cellulose urethane spinning dope used for spinning was obtained.

[0027] c. Extrude the spinning stock solution through the spinneret under the action of compressed air and metering pump, and solidify it in an acid bath. The bath composition is ...

Embodiment 2

[0029] The preparation steps of the cellulose urethane spinning dope are the same as in Example 1.

[0030] Under the action of compressed air or nitrogen and metering pump, the spinning stock solution is extruded through the spinneret hole and solidified in an acid bath. The gas pressure of the liquid storage tank during spinning is 0.2MPa, and the spinneret is 0.08mm×75 hole, the acid bath composition is 11wt% sulfuric acid, 1.5wt% zinc sulfate, 20wt% sodium sulfate, the temperature of the coagulation bath is 25°C, and the immersion time of the filaments in the acid bath is 0.04s; the formed tow is pulled out by the coagulation roller After that, it is washed and regenerated in the water shower area, the rotation speed of the coagulation roller is 27m / min, the rotation ratio of the washing roller and the coagulation roller is 1.02, and the washing temperature is 28°C; finally, the cellulose amino group with high strength can be obtained after oiling and drying. Formate fiber...

Embodiment 3

[0032] a. Take 700 grams of cellulose carbamate with a nitrogen content of 1.785% (viscosity-average molecular weight 10.0×10 4 ) uniformly dispersed at 10.0×10 4 gram is obtained by dissolving 7.5wt% sodium hydroxide and 1.6wt% zinc oxide in water, put it in the refrigerator and freeze to -12°C, take it out from the refrigerator after freezing, thaw at 25°C, and stir to get 6.54 wt% cellulose carbamate solution.

[0033] B, the cellulose carbamate solution obtained by dissolving is filtered, left standing in vacuum for defoaming treatment, the gas pressure is 0.3MPa during filtration, the filter cloth is a cotton cloth with a fineness of 300 mesh, the defoaming vacuum degree is 0.02MPa, and the time is After 8 hours, the cellulose urethane spinning dope used for spinning was obtained.

[0034] c. Under the pressure of compressed air or nitrogen and the suction of metering pump, the spinning stock solution is extruded through the spinneret hole and solidified in the acid bat...

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Abstract

The invention relates to a method for preparing regenerated cellulose fibers with cellulose carbamate. The method is characterized by using a solvent composition for dissolving the cellulose carbamate, uniformly dispersing a certain amount of cellulose carbamate in the solvent composition, freezing to the temperature below minus 10 DEG C at a low temperature condition, taking out the frozen mixture and thawing the frozen mixture at a temperature not higher than 50 DEG C, carrying out wet spinning and obtaining the regenerated cellulose fibers after solidifying, washing and drying silk, wherein the solvent composition is a water solution containing 6-10wt% of sodium hydroxide and 0.1-3wt% of zinc oxide. The method has the effect of solving the two problems of difficult dissolution of the cellulose carbamate and instable solution in the previous processes and has high industrial application value.

Description

field of invention [0001] The invention relates to a method for preparing regenerated cellulose fibers from cellulose carbamate, which belongs to the fields of natural polymers and textiles. technical background [0002] For a long time, the relative backwardness of viscose production technology has become a bottleneck for the further development of regenerated cellulose fibers. With the improvement of environmental protection awareness around the world, this contradiction has become increasingly prominent. Seeking new solvents for green processing of regenerated cellulose fibers is a new way to solve this contradiction. The most notable of these are N-methylmorpholine-N-oxide (NMMO), NaOH / urea water systems, ionic liquids, and cellulose carbamate processes. [0003] The cellulose carbamate process is a new process for preparing regenerated cellulose fibers from cellulose carbamate. The basic principle is to react urea and pretreated cellulose under high temperature condit...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): D01F2/24D01D1/02D01D5/06
Inventor 周金平付飞亚汤炼李道喜
Owner WUHAN UNIV
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