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A kind of preparation method of ether polycarboxylic acid slump retaining agent

The technology of ether polycarboxylic acid and slump retention agent is applied in the field of building admixtures, which can solve the problems of insufficient slump retention performance, excessive loss, delayed bleeding, etc., and achieves improved slump retention performance, low production cost, and spatial location. The effect of increasing the resistance effect

Active Publication Date: 2018-11-30
KZJ NEW MATERIALS GROUP CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002] At present, polycarboxylate slump-retaining agents are more and more widely used in the market, and the products can solve some slump problems to a certain extent, but in the face of factors such as high mud content, high stone powder content, and cement changes, polycarboxylate In actual application, the slump retaining agent has defects such as insufficient slump retaining performance, too fast loss, poor sensitivity, hysteresis bleeding, etc., especially in the medium and low grade concrete mix, the rapid loss and poor sensitivity are particularly obvious

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] (1) Esterification reaction: 100.00g of itaconic anhydride, 200.00g of dimethyl maleic anhydride, 40.00g of methyl hydroxyacetate, 20.00g of methyl hydroxypropionate, 1.20g of concentrated sulfuric acid, 2.50g of benzenesulfonic acid, p- Add 2.3g of hydroquinone and 2.4g of phenothiazine into the reaction kettle and mix them. Under the protection of nitrogen, react at a constant temperature of 60°C for 8 hours. During this period, use vacuum or nitrogen with water to remove water. After the reaction, the temperature drops to At room temperature, the first mixture of esterification product and unreacted unsaturated anhydride is obtained.

[0025] (2) Copolymerization reaction: Add 30.50g of the first mixture prepared in step (1), 200.00g of 4-hydroxybutyl vinyl polyoxyethylene ether and 360.00g of water into the reactor, stir until it dissolves evenly, and wait until the temperature When the temperature is stable at 15°C, start to drop a mixture of 1.50g of ammonium pers...

Embodiment 2

[0028] (1) Esterification reaction: 65.00g of itaconic anhydride, 280.00g of dimethyl maleic anhydride, 20.00g of citraconic anhydride, 35.00g of ethyl glycolate, 43.00g of ethyl hydroxypropionate, 2.00g of benzenesulfonic acid, Add 3.00g of p-toluenesulfonic acid, 1.90g of phenothiazine and 3.50g of diphenylamine into the reaction kettle and mix them. Under the protection of nitrogen, react at a constant temperature of 70°C for 7h. Water was removed, and the temperature was lowered to room temperature after the reaction, and the first mixture of esterified product and unreacted unsaturated anhydride was obtained.

[0029] (2) Copolymerization reaction: Add 28.20g of the first mixture prepared in step (1), 200.00g of 4-hydroxybutyl vinyl polyoxyethylene ether and 280.00g of water into the reactor, stir until it dissolves evenly, and wait until the temperature When the temperature is stable at 25°C, put 1.80g of hydrogen peroxide into the reaction kettle, stir evenly, start to ...

Embodiment 3

[0032] (1) Esterification reaction: 70.00g citraconic anhydride, 200.00g dimethyl maleic anhydride, 30.00g methyl glycolate, 40.00g dimethyl tartrate, 3.80g concentrated sulfuric acid, 6.20g p-toluenesulfonic acid , 5.30g of hydroquinone and 2.80g of diphenylamine were added to the reaction kettle and mixed. Under the protection of nitrogen, they were reacted at a constant temperature of 80°C for 6h. to room temperature, the first mixture of esterified product and unreacted unsaturated anhydride is obtained.

[0033] (2) Copolymerization reaction: Add 23.40g of the first mixture prepared in step (1), 200.00g of 4-hydroxybutyl vinyl polyoxyethylene ether and 180.00g of water into the reaction kettle, stir until it dissolves evenly, wait until the temperature When the temperature is stable at 40°C, put 1.20g of hydrogen peroxide into the reactor, stir evenly, start to drop the mixture of 0.40g of ascorbic acid, 1.50g of trisodium phosphate and 30.00g of water, and start to add d...

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PUM

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Abstract

The invention discloses a preparation method of an ether polycarboxylic acid slump retaining agent, which comprises the following steps: (1) esterification reaction; (2) copolymerization reaction; (3) neutralization reaction. The preparation method of the present invention uses the esterification product of the esterification of aliphatic hydroxy ester and unsaturated acid anhydride in the copolymerization of polycarboxylic acid slump-retaining agent, and introduces a carboxyl group and double ester compound into the polycarboxylic acid molecular chain structure. The molecular structure of the base, the negatively charged carboxylate will not affect the electrostatic repulsion effect of the superplasticizer, and at the same time can improve the workability and sensitivity of the concrete. The double ester group is hydrolyzed under the alkaline condition of cement paste, and more carboxyl groups are slowly released, which can improve the slump performance of concrete. lower.

Description

technical field [0001] The invention belongs to the technical field of building admixtures, and in particular relates to a preparation method of an ether polycarboxylic acid slump-retaining agent. Background technique [0002] At present, polycarboxylate slump-retaining agents are more and more widely used in the market, and the products can solve some slump problems to a certain extent, but in the face of factors such as high mud content, high stone powder content, and cement changes, polycarboxylate In actual application, the slump retaining agent has defects such as insufficient slump retaining performance, too fast loss, poor sensitivity, hysteresis bleeding, etc., especially in the medium and low grade concrete mix, the rapid loss and poor sensitivity are particularly obvious. Therefore, it is of great significance to develop a slump-retaining agent that can satisfy the use of various materials and has good slump-retaining effect, workability and sensitivity. Contents...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F283/06C08F220/18C08F220/14C08F230/02C04B24/26
CPCC04B24/246C08F283/065C08F220/1808C08F220/281
Inventor 官梦芹方云辉林艳梅蒋卓君赖华珍钟丽娜林倩李格丽林添兴
Owner KZJ NEW MATERIALS GROUP CO LTD
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