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Lignin grafted polycarboxylate with high carboxyl content and its preparation method and application

A branch polycarboxylate and lignin technology, which is applied in the field of lignin grafted polycarboxylate with high carboxyl content and its preparation, can solve the problem of difficult preparation of lignin carboxylate with high carboxyl content and the influence of lignin carboxylic acid Solve problems such as salt use performance and low solubility, achieve good steric hindrance, good dispersion performance, and improve dispersion stability

Active Publication Date: 2020-02-18
SOUTH CHINA UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Due to the low content of hydroxyl groups in lignin molecules, especially the relatively low content of phenolic hydroxyl groups with strong activity, and each hydroxyl group can only introduce one carboxyl group at most, the amount of carboxyl groups that can be introduced is limited by the hydroxyl content of lignin, so it is difficult to prepare Lignin carboxylate with high carboxyl content
The carboxyl content of the lignin carboxylate prepared by the method reported in the literature is basically lower than 2mmol / g, so the solubility in neutral and weakly acidic aqueous solutions is low. The performance of additives

Method used

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  • Lignin grafted polycarboxylate with high carboxyl content and its preparation method and application
  • Lignin grafted polycarboxylate with high carboxyl content and its preparation method and application
  • Lignin grafted polycarboxylate with high carboxyl content and its preparation method and application

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038] Mix 10g of glycidyl acrylate, 30g of acrylic acid, 20g of methyl methacrylate and 100g of deionized water evenly, and heat up to 50°C; dissolve 0.5g of ammonium persulfate in 20g of deionized water, and then drop them in 0.5 hours. Then, it was reacted at 50°C for 0.5 hours. Dissolve 100g of sulfonated alkali lignin in 200g of deionized water, then add it to the above reaction solution, raise the temperature to 60°C, keep the temperature for 3 hours, and finish the reaction, adjust the pH of the product to neutral with 30% sodium hydroxide solution, that is To obtain lignin grafted polycarboxylate.

[0039] Purify the product of Example 1, add hydrochloric acid to the lignin-grafted polycarboxylate reaction solution obtained after the reaction to adjust pH=2, stir for 15 minutes and then centrifuge to remove the supernatant, take the precipitate and add a certain amount of deionized water, Adjust the pH to 7, filter to remove insoluble matter, and dialyze the remaining...

Embodiment 2

[0045] Mix 16g of glycidyl methacrylate and 5g of allyl glycidyl ether, 32g of crotonic acid, 25g of butyl acrylate and 120g of deionized water, and heat up to 60°C; dissolve 1g of potassium persulfate in 26g of deionized water , and then the dropwise addition was completed in 0.5 hours, and then reacted at 60° C. for 1 hour. Dissolve 100g of sulfonated alkali lignin in 230g of deionized water, then add it to the above reaction solution, raise the temperature to 80°C, keep it warm for 1 hour, and finish the reaction. Use 30% sodium hydroxide solution to adjust the pH of the product to neutral, that is To obtain lignin grafted polycarboxylate.

[0046] Can be tested according to the same test method of embodiment 1, the polycarboxylic acid monomer of the product obtained in this embodiment 2 is connected with lignin by an ether bond, wherein m=2~3, n=30~40, R=-H or -C 4 h 9 . The carboxylic acid group content of the product obtained in Example 2 is 2.8-3.2 mmol / g, and the w...

Embodiment 3

[0048] Mix 20g of methallyl glycidyl ether, 36g of maleic acid, 40g of ethyl acrylate and 150g of deionized water, and heat up to 70°C; dissolve 1.5g of benzoyl peroxide in 40g of deionized water, and then The dropwise addition was completed in 1 hour, and then reacted at 70° C. for 1 hour. Dissolve 100g of sodium lignosulfonate in 300g of deionized water, then add it to the above reaction solution, raise the temperature to 90°C, and keep the temperature for 1.5 hours to complete the reaction. Use 30% sodium hydroxide solution to adjust the pH of the product to neutral, that is To obtain lignin grafted polycarboxylate.

[0049] Can be tested according to the same testing method of embodiment 1, the polycarboxylic acid monomer of the product obtained in this embodiment 3 is connected with lignin by an ether bond, wherein m=2~3, n=20~30, R=-H or -C 2 h 5 . The carboxylic acid group content of the product obtained in Example 3 is 2.5-2.9 mmol / g, and the weight-average molecul...

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Abstract

The invention discloses a high carboxyl content lignin grafted polycarboxylate, a preparation method and application thereof. The preparation method includes: by weight, mixing 10-30 parts of alkenylglycidyl ester, 30-50 parts of alkenyl carboxylic acid, 20-40 parts of alkenyl carboxylate and 100-200 parts of deionized water evenly, and performing heating to 50-80DEG C to obtain a mixed solution;dissolving 0.5-1.5 parts of an initiator in 20-40 parts of deionized water, then adding the mixture into the mixed solution, and carrying out reaction at 50-80DEG C to obtain a reaction solution; dissolving 100 parts of lignin in 200-300 parts of deionized water, then adding the mixture into the reaction solution, performing heating to 60-90DEG C, carrying out heat preservation reaction, and adjusting he pH of the product to neutral so as to obtain the lignin grafted polycarboxylate. The lignin grafted polycarboxylate has a carboxyl content up to 2.0-3.3mmol / g, which is close to the carboxylcontent of a high-efficiency polycarboxylate dispersant, and can be used as a high-efficiency dispersant in the field of pesticide preparations.

Description

technical field [0001] The invention relates to a lignin carboxylate, in particular to a lignin grafted polycarboxylate with high carboxyl content, a preparation method and application thereof. Background technique [0002] Lignin is the second largest natural renewable resource in nature and belongs to a natural polyphenolic polymer compound. At present, industrial lignin mainly comes from the by-products of forestry industry and paper industry. Due to insufficient utilization, industrial lignin has been discharged into the environment as waste for a long time, causing environmental pollution and waste of resources. With the country's increasing emphasis on environmental protection and natural resources, the application of lignin natural resources in industry has also received more and more attention. The main skeleton of lignin is a natural aromatic ring polymer compound composed of a hydrophobic skeleton composed of phenylpropane structural units and a small amount of hy...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F289/00C08F220/06C08F220/32C08F220/14C08F220/04C08F220/18C08F216/16C08F222/02
CPCC08F289/00C08F220/18
Inventor 周明松汪冬平邱学青杨东杰庞煜霞
Owner SOUTH CHINA UNIV OF TECH
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