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Method for synthesizing ultrahigh-viscosity lithium carboxymethyl cellulose of ultralow solvent system

A technology of carboxymethyl cellulose and synthesis method, which is applied in the direction of electrical components, circuits, battery electrodes, etc., can solve the problems of low conversion efficiency of carboxymethyl cellulose lithium, many residual ions, and large amount of solvent, etc., and achieve product conversion Efficiency improvement, low residual sodium salt content, and small amount of solvent

Pending Publication Date: 2020-07-03
瑞红锂电池材料(苏州)有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The purpose of the present invention is how to solve the problems of low conversion efficiency of carboxymethyl cellulose lithium in the prior art, large amount of solvent, many residual ions, and low viscosity

Method used

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  • Method for synthesizing ultrahigh-viscosity lithium carboxymethyl cellulose of ultralow solvent system
  • Method for synthesizing ultrahigh-viscosity lithium carboxymethyl cellulose of ultralow solvent system
  • Method for synthesizing ultrahigh-viscosity lithium carboxymethyl cellulose of ultralow solvent system

Examples

Experimental program
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Effect test

Embodiment 1

[0028] In a 5-liter vertical enamel reactor, take 1000g of CMC-Na and 4050g of 10% sulfuric acid solution into the glass-lined reactor. Stir continuously at 20°C. After 120min, stop the reaction and centrifuge to remove the mother liquor. Later, the solid was retained to obtain CMC-H. Spray and wash the materials in the centrifuge with demineralized water at 40°C for 20 minutes, and discharge the materials. Add all the CMC-H obtained by centrifugation to 5 times the mass of an 80% alcohol system, stir continuously, add 0.36kg of solid lithium hydroxide, react at 35°C for 120min, and then centrifuge. After the mother liquor is removed by centrifugation, the material in the centrifuge is sprayed and washed with 70% ethanol for 20 minutes, and the material is discharged to obtain CMC-Li, which can be dried, crushed and sieved.

Embodiment 2

[0030] In a 5-liter vertical reactor, take 1 kg of CMC-Na and 2 kg of sulfuric acid solution with a concentration of 30% and add it to the glass-lined reactor. Stir continuously at 35 ° C. After 100 minutes, stop the reaction and perform centrifugation. After the mother liquor is removed by centrifugation , The solid was retained to give CMC-H. Spray and wash the materials in the centrifuge with demineralized water at 50°C for 18 minutes, and discharge the materials. Add all the CMC-H obtained by centrifugation to 8 times the mass of an 85% alcohol system, stir continuously, add 0.36kg of solid lithium hydroxide, react at 40°C for 120min, and then centrifuge. After the mother liquor is removed by centrifugation, the material in the centrifuge is sprayed and washed with 75% ethanol for 20 minutes, and the material is discharged to obtain CMC-Li, which can be dried, crushed and sieved.

Embodiment 3

[0032] In a 5-liter vertical reactor, take 200g of CMC-Na and 972g of 25% sulfuric acid solution into the glass-lined reactor. Stir continuously at 40°C. After 150min, stop the reaction and centrifuge. After the mother liquor is removed by centrifugation , The solid was retained to give CMC-H. Spray and wash the materials in the centrifuge with demineralized water at 35°C for 16 minutes, and discharge the materials. Add all the CMC-H obtained by centrifugation to 10 times the mass of an 85% alcohol system, stir continuously, add 35g of solid lithium hydroxide, react at 40°C for 120min, and then centrifuge. After the mother liquor is removed by centrifugation, the materials in the centrifuge are sprayed and washed with 80% ethanol for 15 minutes, and the materials are discharged to obtain CMC-Li, which can be dried, pulverized and sieved.

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Abstract

The invention discloses a method for synthesizing ultrahigh-viscosity lithium carboxymethyl cellulose of an ultralow solvent system. The method is a two-step synthesis method and specifically comprises the following steps: mixing CMC-Na and sulfuric acid or nitric acid with the concentration of 10-50%, adding the obtained mixture into a glass lining reactor, stirring, centrifuging, and removing acid mother liquor to obtain CMC-H without adding any organic solvent; washing with softened water; and mixing the washed CMC-H, a lithium hydroxide solid and an organic solvent, reacting at 20-50 DEG C, centrifuging, removing mother liquor, and washing the obtained product. The viscosity of the lithium carboxymethyl cellulose prepared by the method is far higher than that of lithium carboxymethylcellulose prepared by other methods, the cost is lower, the conversion is more direct, the efficiency is higher, the solvent amount is smaller, and industrial production is easier to realize.

Description

technical field [0001] The invention relates to the field of chemical modification of natural macromolecules, in particular to a method for synthesizing ultrahigh viscosity carboxymethyl cellulose lithium in an ultralow solvent system. Background technique [0002] Carboxymethylcellulose lithium (CMC-Li) can be used as an aqueous binder material in lithium-ion batteries. [0003] The preparation method of carboxymethyl cellulose lithium in the prior art is divided into one-step method and two-step method: one-step method is to react cellulose, lithium hydroxide solution and chloroacetic acid in an organic solvent at a certain temperature and for a reaction time to obtain CMC-Li, this method is because the dissolubility of lithium hydroxide is relatively low, less than 13%, causes alkalinity on the low side, can't react with cellulose preferably to form alkali cellulose. In the actual reaction process, in most cases, cellulose cannot react, and the synthesis rate of CMC-Li i...

Claims

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Application Information

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IPC IPC(8): C08B11/12H01M4/62
CPCC08B11/12H01M4/622Y02E60/10
Inventor 于倩邱磊
Owner 瑞红锂电池材料(苏州)有限公司
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