Method for preparing cement water reducer from lignin

A technology of lignin and water reducing agent, applied in the directions of lignin derivatives, chemical instruments and methods, organic chemistry, etc., can solve the problem of low charge density and carboxyl group content of lignin, and low sulfonation degree of sulfomethylated lignin products , the water reduction effect is not very obvious, etc., to achieve the effect of increasing hydrophilic properties, abundant raw materials, and reducing pollutant emissions

Inactive Publication Date: 2016-10-26
ANYANG HUASEN PAPER
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  • Summary
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Problems solved by technology

However, the oxidizing agent used in the prior art is hydrogen peroxide, and the oxidizing ability of the oxidizing agent is not very high, and the charge density and carboxyl content of the oxidized lignin are low, which eventually leads to a low degree of sulfonation of the sulfomethylated lignin product, thereby The effect of water reduction is not very obvious; and a large number of air bubbles are easily generated during the reaction process, which brings unnecessary troubles to the oxidation reaction

Method used

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Embodiment 1

[0017] In specific implementation 1, the present invention can be realized by the following steps:

[0018] (1) Oxidation reaction of lignin: the reaction formula is Lignin + HNO 3 → Lignin-CHO + Lignin-COOH, according to the reaction formula, weigh 5g of absolute dry lignin and 120ml of nitric acid solution with a concentration of 8%, add it to a 500ml round bottom flask and stir evenly, the stirring speed is 200~500rpm (200~ 500r / min), oxidation reaction at 100°C for 1 hour, the reaction solution was cooled to room temperature, the pH value of the reaction solution was adjusted to neutral with 4M sodium hydroxide solution, and the reaction solution was purified by dialysis for 24~ 48h, change the water every 6h, cut off the oxidized lignin whose molecular weight is greater than 500g / mol, and obtain the oxidized lignin solution after dialysis purification;

[0019] (2) Sulfomethylation reaction of oxidized lignin: the reaction formula is Lignin-CHO + CH 2 O + SO 3 Na - ...

Embodiment 2

[0024] In specific implementation 2, the present invention can be realized by the following steps:

[0025] (1) Oxidation reaction of lignin: Weigh 5g of absolute dry lignin and 108ml of nitric acid solution with a concentration of 9% into a round bottom flask and stir evenly at a stirring speed of 200~500rpm. Oxidation reaction at 95°C After 1.5 hours, the solution after the reaction was cooled to room temperature, and the pH value of the solution after the reaction was adjusted to neutrality with 4M sodium hydroxide solution, and the reaction solution was purified by dialysis with a dialysis bag for 24 to 48 hours, and the water was changed every 6 hours. 500g / mol of oxidized lignin, obtained the oxidized lignin solution after dialysis purification.

[0026] In this embodiment, the content of carboxyl groups in the oxidized lignin is 1.97 millioquivalents per gram, and the charge density of lignin is 3.9 millioquivalents per gram.

[0027](2) Sulfomethylation reaction of ox...

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Abstract

The invention relates to a method for preparing a cement water reducer from lignin. The method can effectively improve hydrophilicity of lignin, so that solubility of lignin is improved, surface reaction performance of lignin can be better improved, and the cement water reducer is prepared. The method includes the steps that lignin and a nitric acid solution are mixed, so that lignin is subjected to oxidation reaction for 0.5-2.5 h at 60-100 DEG C; after oxidation reaction, the reaction mixture is cooled to room temperature with cold water, and then the pH value of the cooled reaction solution is adjusted to be neutral with a 4M sodium hydroxide solution; dialysis and purification are conducted by means of a dialysis bag, the product is dried, and the cement water reducer is obtained. The method is simple, raw materials are rich, cost is low, lignin in slurrying waste liquid can be fully and effectively used, pollution is reduced, and discharge of pollutants is reduced.

Description

technical field [0001] The invention relates to chemical industry, in particular to a method for preparing cement water reducing agent from lignin. Background technique [0002] Pulping waste liquid contains a large amount of lignin, accounting for about 1% to 2% of the total waste liquid, which is difficult to degrade under natural conditions. If the waste liquid is discharged directly without treatment, it will cause serious environmental pollution. And lignin is an important industrial raw material, which can be widely used as cement water reducer, adhesive and dispersant after treatment. Therefore, the treatment and utilization of papermaking black liquor has received extensive attention and research. [0003] In order to improve the stability of lignin, sulfonic acid groups can be introduced to generate lignosulfonate. The molecular structure of sodium lignosulfonate is complex, and the relative molecular weight is about 2000-100000. To improve its dispersion perfor...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08H7/00C07G1/00C04B24/18C04B103/30
CPCC08H6/00C04B24/18C04B2103/302C07G1/00
Inventor 刘洁贺文明
Owner ANYANG HUASEN PAPER
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