Method of increasing alkaline lignin sulfonation yield

A technology of alkali lignin and sulfonation, applied in the field of improving the reaction activity of alkali lignin, can solve the problems of not being green and environmental protection, water pollution treatment pressure increases, etc., to achieve improved sulfonation efficiency, increased reaction activity, and easy recycling Effect

Inactive Publication Date: 2017-09-15
SOUTH CHINA UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The use of strong alkali oxidants has caused an increase in the pressure of water pollution treatment, which is not a green and environmentally friendly method

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Get the alkali lignin (purity is 85%, particle diameter is 80 meshes, water content is 3%) extracted from wheat straw caustic soda anthraquinone pulping black liquor, add 1-ethyl-3-methylimidazole acetate and mix pre- After the treatment, deionized water is added to stop the reaction, followed by centrifugation (3000r / min) and freeze-drying to obtain the pretreated alkali lignin. Perform vacuum distillation to recover 1-ethyl-3-methylimidazolium acetate. The treatment conditions are as follows: the amount of 1-ethyl-3-methylimidazole acetate is 400% of the mass of dry alkali lignin, the treatment temperature is 80° C., and the treatment time is 60 minutes. The sulfonation modification process of lignin is as follows: the alkali lignin sample after pretreatment is added into deionized water, the consumption of water is 300% of lignin quality, magnetic stirring (300r / min, 20min), heating to 95 ℃, Add hydrogen peroxide, control the temperature at 95°C, react for 1 hour, t...

Embodiment 2

[0028] Get the alkali lignin (purity is 80%, particle diameter is 85 orders, water content is 1%) that eucalyptus wood alkaline sulfurous acid pulping black liquor extracts, add 1-ethyl-3-methylimidazole acetate Mixing pretreatment, adding deionized water after the treatment is completed to terminate the reaction, followed by centrifugation (rotating speed 3200r / min), freeze-drying to obtain the pretreated alkali lignin. Perform vacuum distillation to recover 1-ethyl-3-methylimidazolium acetate. The treatment conditions are as follows: the amount of 1-ethyl-3-methylimidazole acetate is 450% of the mass of dry alkali lignin, the treatment temperature is 85° C., and the treatment time is 90 minutes. The sulfonation modification process of lignin is as follows: the alkali lignin sample after pretreatment is added into deionized water, the consumption of water is 300% of lignin quality, magnetic stirring (300r / min, 20min), heating to 95 ℃, Add hydrogen peroxide, control the tempe...

Embodiment 3

[0034] Take commercial alkali lignin (purity is 95%, particle size is 90 mesh, water content is 2%), add 1-ethyl-3-methylimidazole acetate to mix pretreatment, add deionized water after the treatment is completed The reaction was terminated, followed by centrifugation (3500 r / min) and freeze-drying to obtain pretreated alkali lignin. Perform vacuum distillation to recover 1-ethyl-3-methylimidazolium acetate. The treatment conditions are as follows: the amount of 1-ethyl-3-methylimidazole acetate is 500% of the mass of dry alkali lignin, the treatment temperature is 90° C., and the treatment time is 120 minutes. The sulfonation modification process of lignin is as follows: the alkali lignin sample after pretreatment is added into deionized water, the consumption of water is 300% of lignin quality, magnetic stirring (300r / min, 20min), heating to 95 ℃, Add hydrogen peroxide, control the temperature at 95°C, react for 1 hour, then add formaldehyde and sodium sulfite, keep the rea...

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Abstract

The invention belongs to the field of increasing alkaline lignin reaction activity and discloses a method of increasing alkaline lignin sulfonation yield. In the method, alkaline lignin is subjected to pretreatment to increase the alkaline lignin sulfonation yield. The pretreatment includes the steps of: 1) adding the alkaline lignin to 1-ethyl-3-methylimidazole acetate or 1-ethyl-3-methylimidazole chloride salt, and uniformly mixing the components for treatment; 2) after the treatment is completed, adding water to terminate the reaction; 3) centrifuging and freeze-drying the reaction product to prepare pretreated alkaline lignin; and 4) performing pressure-reduced distillation to recycle the 1-ethyl-3-methylimidazole acetate or the 1-ethyl-3-methylimidazole chloride salt. The solvents in the pretreatment method are green and environment-friendly and can be recycled without pollution, so that the method has simple process and operations, is suitable for industrial production and has excellent application prospect.

Description

technical field [0001] The invention belongs to the field of improving the reaction activity of alkali lignin, and in particular relates to a method for increasing the sulfonation yield of alkali lignin. Background technique [0002] Lignin, as one of the most abundant reserves of natural polymers on the earth, ranks second only to cellulose. Worldwide, approximately 30 million tons of lignin waste are obtained annually by various chemical pulping methods. As a by-product of the biomass refining process, most of the lignin is burned as a fuel in the alkali recovery process, but the calorific value of lignin is low, and the combustion of a large amount of lignin causes a waste of biomass energy. Therefore, it is urgent to explore a method that can utilize lignin with high value in order to rationally utilize this biomass resource. [0003] Lignin molecules contain a large number of active groups, such as methoxyl groups, phenolic hydroxyl groups, alcoholic hydroxyl groups, ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08H7/00
CPCC08H6/00
Inventor 张志礼杨仁党
Owner SOUTH CHINA UNIV OF TECH
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