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Ester super sustained release polycarboxylic acid slump retaining agent and preparation method thereof

An ultra-sustained-release, polycarboxylic acid technology, applied in the field of building materials, can solve the problems of inability to fully meet market demand, cost increase, insufficient slump retention performance, etc., and achieve fast speed, slump retention, and slump retention capability Effect

Active Publication Date: 2019-03-19
GUANGDONG KEZHIJIE NEW MATERIALS +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] At present, the existing slump-retaining agents in the market can improve the effect of concrete slump-retaining in concrete applications, but the slump-retaining performance is insufficient. Increasing the amount of slump-retaining agents will greatly increase the cost, which cannot fully meet the market demand.

Method used

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  • Ester super sustained release polycarboxylic acid slump retaining agent and preparation method thereof
  • Ester super sustained release polycarboxylic acid slump retaining agent and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] (1) Preparation of unsaturated esterified small monomers:

[0030] Under normal pressure, 41 parts of methacrylic acid, 71 parts of propionic acid, 130 parts of 3-bis(2-hydroxyethyl)amino-2-hydroxypropanesulfonic acid (DIPSO) were added to the reactor, and 0.25 Parts of titanium trichloride, 0.13 parts of 4-hydroxy-2,2,6,6-tetramethylpiperidine-1-oxyl radical and 13 parts of petroleum ether are used for esterification reaction, and the temperature of the esterification reaction is 100°C , the reaction time is 3 hours, and after the reaction is completed, it is lowered to room temperature, and the unsaturated esterified small monomer is obtained.

[0031] (2) Esterification reaction: in parts by weight, 100.00 parts of polyethylene glycol monomethyl ether with a weight average molecular weight of 400, 129 parts of methacrylic acid, 11.45 parts of concentrated sulfuric acid and 4.58 parts of β-phenylnaphthylamine were placed in In the first reaction device, the temperatu...

Embodiment 2

[0035] (1) Preparation of unsaturated esterified small monomers:

[0036] Under normal pressure, 60 parts of methacrylic acid, 162 parts of butyric acid, 130 parts of 3-bis(2-hydroxyethyl)amino-2-hydroxypropanesulfonic acid (DIPSO) were added to the reactor, and 0.55 1 part of sodium p-toluenesulfonate, 0.45 part of N-nitroso-N-phenylhydroxylamine aluminum and 18 parts of cyclohexane, carry out esterification reaction, the esterification reaction temperature is 110 ℃, the reaction time is 4 hours, and the reaction ends After cooling down to room temperature, the unsaturated esterified small monomer is obtained.

[0037](2) Esterification reaction: in parts by weight, 100.00 parts of polyethylene glycol monomethyl ether with a weight average molecular weight of 1000, 43 parts of methacrylic acid, 2.15 parts of concentrated sulfuric acid and 0.72 parts of β-phenylnaphthylamine were placed in In the first reaction device, the temperature was kept at 120° C. for 4 hours to obtain...

Embodiment 3

[0041] (1) Preparation of unsaturated esterified small monomers:

[0042] Under normal pressure, 90 parts of methacrylic acid, 85 parts of butyric acid, 130 parts of 3-bis(2-hydroxyethyl)amino-2-hydroxypropanesulfonic acid (DIPSO) were added to the reactor, and 0.6 Parts of titanium trichloride, 0.35 parts of 4-hydroxy-2,2,6,6-tetramethylpiperidine-1-oxygen free radicals and 40 parts of petroleum ether are subjected to esterification reaction at a temperature of 120°C , the reaction time is 5 hours, after the reaction is completed, it is lowered to room temperature, and the unsaturated esterified small monomer is obtained.

[0043] (2) Esterification reaction: by weight, 100.00 parts of molecular weight is 3000 polyethylene glycol monomethyl ether, 11.48 parts of methacrylic acid, 2.23 parts of concentrated sulfuric acid and 1.11 parts of β-phenylnaphthylamine are placed in the first In the reaction device, the temperature was kept at 110° C. for 5 hours to obtain the esterif...

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Abstract

The invention discloses an ester super sustained release polycarboxylic acid slump retaining agent and a preparation method thereof. The preparation method of the ester super sustained release polycarboxylic acid slump retaining agent comprises the following steps: (1) preparing methacrylic acid, saturated acid and 3-bis(2-hydroxyethyl)amino-2-hydroxypropanesulphonic acid under the action of a catalyst into unsaturated esterified small monomers; (2) stirring methoxypolyethylene glycol, methacrylic acid, concentrated sulphuric acid and beta-phenyl-naphthylamine in a flask, and reacting to obtain esterified monomers MP; and (3) stirring diethyl vinyl phosphate, a cationic photoinitiator A and water in a flask, mixing unsaturated carboxylic acid hydroxyalkyl ester monomers, the esterified monomers MP, unsaturated monocarboxylic acid, the unsaturated esterified small monomers and water, mixing a free radical polymerization photoinitiator B and water, mixing a chain transfer agent and water, irradiating the flask in ultraviolet light, and respectively adding the aqueous solutions into the flask dropwise, continuing reacting, and adding a sodium hydroxide aqueous solution for neutralizing to obtain the ester super sustained release polycarboxylic acid slump retaining agent. The slump retaining agent prepared by the preparation method has good slump retaining capacity for a long time.

Description

technical field [0001] The invention belongs to the technical field of building materials, and in particular relates to an ester ultra-slow-release polycarboxylic acid slump retaining agent and a preparation method thereof. Background technique [0002] As the third generation of new high-performance water reducer, polycarboxylate water reducer has the advantages of high water reducing rate, designable molecular structure, and small air-entrained volume. It is very suitable for preparing high-strength and high-performance concrete. Recognized, it has been widely used in nuclear power, water conservancy, bridges, tunnels and other large-scale infrastructure and other large-scale projects. However, due to the influence of factors such as temperature changes, cement changes, and high mud content in sand and stone materials, the polycarboxylate superplasticizer has the problem of excessive slump loss in application, which affects engineering construction and quality. [0003] T...

Claims

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Application Information

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IPC IPC(8): C08F290/06C08F230/02C08F220/20C08F220/06C08F222/24C08F2/48C04B24/16C04B103/30
CPCC04B24/165C08F290/062C04B2103/302C08F222/103C08F222/24
Inventor 赖广兴方云辉谢木和赖华珍林艳梅李格丽柯余良黄忠钟丽娜张小芳
Owner GUANGDONG KEZHIJIE NEW MATERIALS
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