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Preparation method and application of high water reduction type polycarboxylic acid super plasticizer

A technology of superplasticizer and polycarboxylic acid, applied in sustainable waste treatment, solid waste management, climate sustainability, etc., can solve the problem of self-polymerization of unsaturated ester monomers, insufficient carboxyl ratio and other problems

Active Publication Date: 2021-07-06
JIANGSU SOBUTE NEW MATERIALS
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In order to solve this problem, the patent CN104387536B specially reported a method of increasing the proportion of carboxyl groups in polycarboxylic acid products by hydrolysis of unsaturated ester monomers, but this method also has the problem of self-polymerization of unsaturated ester monomers and the increase in the proportion of carboxyl groups still not enough problem

Method used

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  • Preparation method and application of high water reduction type polycarboxylic acid super plasticizer
  • Preparation method and application of high water reduction type polycarboxylic acid super plasticizer
  • Preparation method and application of high water reduction type polycarboxylic acid super plasticizer

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Experimental program
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Effect test

Embodiment 1

[0051] The preparation steps of described high water-reducing polycarboxylate superplasticizer are as follows:

[0052] Synthesis of side chain macromonomer C-1: Add 30wt% hydrogen peroxide (0.028mol, 3.18g) and 50g of solvent water into a four-necked flask equipped with a stirrer and a thermometer, stir evenly, and control the temperature to 10°C. At this temperature, a solution consisting of acrylic acid (1mol, 72g), hydroxyethyl acrylate (1mol, 116g), E-1 (0.2mol, 32.4g), L-ascorbic acid (0.007mol, 1.23g) and water 138g was added dropwise. The mixed solution of C-1 was added dropwise for 2 hours, and after the dropwise addition was completed, it was incubated for 1 hour to obtain an aqueous solution of C-1, and GPC measured M w is 1020;

[0053] The synthesis of high water-reducing polycarboxylate superplasticizer: add isopentenyl polyoxyethylene ether (M w 1000, 0.4mol, 400g) and 400g of water, stir evenly, control the temperature to 50°C, at this temperature, dropwise a...

Embodiment 2

[0055] The preparation steps of described high water-reducing polycarboxylate superplasticizer are as follows:

[0056] Synthesis of side chain macromonomer C-2: Add 30wt% hydrogen peroxide (0.0645mol, 7.31g) and 50g of solvent water into a four-necked flask equipped with a stirrer and a thermometer, stir evenly, and control the temperature to 20°C. At this temperature, a solution consisting of hydroxyethyl acrylate (1mol, 116g), acrylic acid (1mol, 72g), E-2 (0.15mol, 24g), L-ascorbic acid (0.0215mol, 3.78g) and water 160g was added dropwise. Mix the solution, add it dropwise for 1h, and keep it warm for 1h after the dropwise addition is completed to obtain the aqueous solution of C-1, which is measured by GPC. w is 1250;

[0057] The synthesis of high water-reducing polycarboxylate superplasticizer: add vinyl polyoxyethylene ether (M w 2000, 0.5mol, 1000g) and 500g of water, stir evenly, control the temperature to be 40°C, at this temperature, dropwise add methacrylic acid...

Embodiment 3

[0059] The preparation steps of described high water-reducing polycarboxylate superplasticizer are as follows:

[0060]Synthesis of side chain macromonomer C-3: Add 30wt% hydrogen peroxide (0.135mol, 15.3g) and 50g of solvent water to a four-necked flask equipped with a stirrer and a thermometer, stir evenly, and control the temperature to 30°C. At this temperature, a mixture of hydroxyethyl acrylate (1mol, 116g), methacrylic acid (1mol, 86g), E-3 (0.135mol, 25.7g), L-ascorbic acid (0.00846mol, 1.49g) and water was added dropwise. The mixed solution of 160g composition, dropwise time 1h, insulation 1h after dropwise addition, obtain the aqueous solution of C-3, GPC records M w for 1510;

[0061] The synthesis of high water-reducing polycarboxylate superplasticizer: add methallyl polyoxyethylene ether (M w 3000, 0.65mol, 1950g) and 1000g of water, stir evenly, control the temperature at 20°C, at this temperature, add dropwise fumaric acid (2.6mol, 301.6g), mercaptopropionic a...

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Abstract

The invention discloses a preparation method and application of a high water reduction type polycarboxylic acid super plasticizer. According to the invention, a main chain monomer A, a side chain macromonomer B and a side chain macromonomer C are subjected to a free radical copolymerization reaction in water to prepare the polycarboxylic acid superplasticizer, wherein the structural formula of the monomer A is defined in the specification, R1 is -H or-COOH, R2 is -H, -CH3 or -CH2COOH, R3 is -OH, -NH2 or C1-C4 alkyl, the structure of the monomer B is defined in the specification, R5 is -O-, -CH2O-, -CH2CH2O- or -OCH2CH2CH2CH2O-, and the monomer C structure is defined in the specification; the high water reduction type polycarboxylic acid super plasticizer is prepared by adopting a two-step one-pot method, the process is simple, the production process is green and environment-friendly, the cost is low, and large-scale production is facilitated; and the ultimate water reduction of the high water reduction type polycarboxylic acid super plasticizer is far better than that of the existing product, and the harsh requirements of high fluidity, long slump retaining time, viscosity reduction and the like of ultrahigh-strength concrete can be met.

Description

technical field [0001] The invention relates to a preparation method of a high water-reducing polycarboxylic acid superplasticizer and its application as a cement dispersant, belonging to the technical field of concrete admixtures. Background technique [0002] Polycarboxylate superplasticizer (commonly known as water reducing agent in China), has become the current concrete admixture market due to its low dosage, high water reducing rate, good slump retention, strong molecular structure adjustability, and environmental protection. most important product. Polycarboxylate superplasticizer is a comb-shaped water-soluble polymer, which is composed of a main chain rich in carboxylic acid groups and a side chain of polyoxyethylene ether. The carboxylic acid groups on the polycarboxylic acid main chain can be directional adsorbed on the surface of positively charged cement or cement hydrate, while the polyoxyethylene ether side chains stretch in the solution to form a hydration l...

Claims

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Application Information

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IPC IPC(8): C08F283/06C08F220/06C08F220/20C08F222/02C08F220/18C08F220/56C08F220/14C08F220/54C04B24/26C04B103/30
CPCC08F283/065C04B24/2694C04B2103/302C08F220/06C08F220/20C08F222/02C08F220/56C08F220/14C08F220/54Y02W30/91
Inventor 李申桐杨勇舒鑫周栋梁王涛黄振张建纲张倩倩
Owner JIANGSU SOBUTE NEW MATERIALS
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