Preparation method of homogeneous spinning solution

A spinning solution and solution technology, applied in the field of regenerated cellulose fibers, can solve the problems of large structure of vacuum dehydration and dissolving equipment, unfavorable for industrial production, complex and other problems, to avoid excessive degradation, avoid easy entrainment of air bubbles, and short dissolution time Effect

Active Publication Date: 2021-03-02
ZHENGZHOU ZHONGYUAN SPANDEX ENG TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method is similar to the method for preparing cellulose solution with NMMO as solvent in CN1211509C and CN1042165A. The vacuum dehydration and dissolving equipment required by this method is relatively large and complex in structure, which is not conducive to industrial production

Method used

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Examples

Experimental program
Comparison scheme
Effect test

preparation example Construction

[0029] Specifically, the invention provides a method for preparing a homogeneous spinning solution of a mixture of low-temperature molten salt and cellulose, keratin or cellulose keratin, comprising:

[0030] a) Premix low-temperature molten salt at a temperature of t1 with cellulose, keratin or cellulose-keratin mixture to obtain a fluffy premix A with a ratio of bulk density to compacted density of 0.29 to 0.32, and t1 is 5~50℃;

[0031] b) Fully mix the premix A with the low-temperature molten salt at a temperature of t2 until a homogeneous and transparent solution is obtained, wherein t1

[0032] The low-temperature molten salt suitable for the present invention is selected from 1-ethyl-3-methylimidazole diethyl phosphate ([EMIM]DEP), 1-methyl-3-methylimidazole phosphate ([MMIM]DMP), 1-Ethyl-3-methylimidazole acetate, 1-propyl-3-methylimidazole acetate, 1-butyl-3-methylimidazole acetate, 1-allyl-3- Methylimidazole acetate, 1-methylallyl-3-methylimidazole acetat...

Embodiment 1

[0048] 1) First shape 20g to about 1cm 2 The cellulose pulp was added to the mixing tank A, and vacuumed to -0.1MPa. Then 80 g of 1-allyl-3-methylimidazolium chloride salt ([AMIM]Cl) with a water content of about 1200 ppm was added to mixing tank A at a temperature of about 40°C. Stir for 20 minutes at a stirring speed of approximately 80 rpm to obtain a bulk density of approximately 0.286 g / cm 3 , The compacted density is about 0.923g / cm 3 The premix has a looseness of about 0.3099.

[0049] 2) Under the condition of keeping the vacuum degree of the system at about -0.1MPa, add 135g of [AMIM]Cl at a temperature of about 121°C into the mixing tank A to fully mix it with the premix to obtain a viscosity of about 968Pa • A homogeneous transparent cellulose solution of s.

Embodiment 2

[0051] 1) First, 18g of cellulose powder (DP=1000) and 2g of keratin protein pulverized into fine powder (the bulk density of the mixed powder of cellulose and keratin protein is about 0.33g / cm 3 ) into the mixing tank A, and vacuum to -0.09MPa. Then add 70g of 1-ethyl-3-methylimidazolium diethyl phosphate ([EMIM]DEP) with a water content of about 6000ppm into mixing tank A at a temperature of about 38°C at a stirring speed of about 60 rpm Stir for 20 minutes to obtain a bulk density of about 0.283g / cm 3 , The compacted density is about 0.962g / cm 3 The premix has a looseness of about 0.2942.

[0052] 2) Under the condition of keeping the vacuum degree of the system at about -0.09MPa, add 120g of [EMIM]DEP at a temperature of about 121°C into the mixing tank A to fully mix it with the premix to obtain a viscosity of about 4180Pa Homogeneous transparent solution of s.

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Abstract

The invention relates to a preparation method of a homogeneous spinning solution of a mixture of a low-temperature molten salt and cellulose, keratin or cellulose keratin. The preparation method comprises the following steps: a, premixing the low-temperature molten salt at the temperature of t1 with the cellulose, the keratin or the cellulose keratin, to obtain a fluffy premix A of which the ratioof bulk density to compaction density is 0.29-0.32, wherein t1 is 5-50 DEG C; and b, fully mixing the premix A with the low-temperature molten salt at the temperature of t2 until a homogeneous transparent solution is obtained, wherein t2 is more than t1 and less than 210 DEG C. According to the preparation method disclosed by the invention, the low-temperature molten salt is added through the twosteps, so that sufficient swelling of the cellulose and the keratin is guaranteed, the phenomenon of a white core is avoided, dissolving time is shortened, and excessive degradation in a dissolving process is prevented.

Description

technical field [0001] The invention relates to the field of regenerated cellulose fibers, in particular to a method for preparing a homogeneous spinning solution of a mixture of low-temperature molten salt and cellulose, keratin or cellulose keratin. Background technique [0002] With the over-exploitation and increasing tension of non-renewable resources, the research and development of renewable resources have attracted more and more attention. Cellulose, keratin, etc., as abundant renewable resources, have received great attention. Cellulose, keratin or a mixture of cellulose / keratin can be dissolved in a certain solvent to prepare a homogeneous transparent solution, which can be made into filaments, short fibers, films, foaming materials, etc. by controlling the coagulation and molding conditions. Natural cellulose has high crystallinity, and there are a large number of hydrogen bonds between molecules and molecules, and it has characteristics such as insoluble, insolu...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): D01D1/02D01F2/02D01F8/02D01F4/00
CPCD01D1/02D01F2/02D01F8/02D01F4/00
Inventor 钱小磊化丹丹袁祖涛张豪李昊洋
Owner ZHENGZHOU ZHONGYUAN SPANDEX ENG TECH
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