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A kind of preparation method of slump-retaining polycarboxylate superplasticizer mother liquor

A technology of water reducer and polycarboxylate, which is applied in the field of preparation of slump-preserving polycarboxylate water reducer mother liquor, which can solve the problems of dangerous use and low explosion limit, and achieve the effects of convenient transportation, good activity and stable performance

Active Publication Date: 2021-07-20
安徽海螺材料科技股份有限公司 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Because the explosion limit of ethylene oxide or propylene oxide is extremely low, it is particularly dangerous to use. It is not possible to use epoxy monomers such as ethylene oxide or propylene oxide to react directly with polycarboxylate water reducers. suitable

Method used

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  • A kind of preparation method of slump-retaining polycarboxylate superplasticizer mother liquor
  • A kind of preparation method of slump-retaining polycarboxylate superplasticizer mother liquor
  • A kind of preparation method of slump-retaining polycarboxylate superplasticizer mother liquor

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[0036]The present invention proposes a method for preparing a slump-preserving polycarboxylate superplasticizer mother liquor, which uses the by-product epoxy compound and polycarboxylate superplasticizer prepolymer in the production process of organosilane coupling agent to directly carry out Ring-opening esterification reaction (ring-opening esterification of carboxylic acid groups and epoxy groups) to generate polycarboxylate superplasticizers, thereby adjusting the length and density of the side chains of polycarboxylate superplasticizers, giving polycarboxylate water-reducing agents The effect of anti-slump agent, in which organosilane coupling agent includes but not limited to γ-(2,3-epoxypropoxy)hydrocarbyl silane coupling agent including KH560, also includes γ-(2,3-epoxy Propoxy)-Propyltriethoxysilane, γ-(2,3-Glycidoxy)-Propylmethyldimethoxysilane, γ-(2,3-Glycidoxy)-Propyl Methyldiethoxysilane. When producing these organosilane coupling agents, the by-products used fo...

Embodiment 1

[0054] (1) Preparation of polycarboxylate superplasticizer prepolymer: 0.082mol 3-methyl-3-butyl-1-polyethylene glycol (2500g / mol) and 0.115mol acrylic acid in unsaturated polyether monomer Under the action of 0.00082mol ammonium persulfate, 0.00246mol ferrous sulfate and 0.00082mol mercaptoacetic acid, keep 80°C for water phase free radical polymerization for 3 hours to obtain polycarboxylate superplasticizer prepolymer;

[0055] (2) Preparation method of slump-preserving polycarboxylate water reducer: add 23.65g (a total of 0.19mol epoxy compound) of the by-product epoxy compound in the industrial production process of organosilane coupling agent KH560 to the polycarboxylate pre- Polymer (based on carboxyl content of 0.29mol) carries out epoxy ring-opening esterification reaction with carboxyl group, wherein the molar ratio of carboxyl group contained in polycarboxylic acid prepolymer to by-product epoxy compound is 1.54, and the reaction temperature is kept at 80 ℃ for two ...

Embodiment 2

[0057] (1) Preparation of polycarboxylate superplasticizer prepolymer: 0.082mol 3-methyl-3-butyl-1-polyethylene glycol (2500g / mol) and 0.31mol acrylic acid in unsaturated polyether monomer Under the action of 0.0028mol ammonium persulfate, 0.0012mol ferrous sulfate and 0.0074mol mercaptoacetic acid, keep 60°C for water phase free radical polymerization for 4.5 hours to obtain polycarboxylate superplasticizer prepolymer;

[0058] (2) Preparation method of slump-preserving polycarboxylate water reducer: add 23.65g (a total of 0.19mol epoxy compound) of the by-product epoxy compound in the industrial production process of organosilane coupling agent KH560 to the polycarboxylate pre- Polymer (based on carboxyl content of 0.31mol) carries out epoxy ring-opening esterification reaction with carboxyl group, wherein the molar ratio of carboxyl group contained in polycarboxylic acid prepolymer to by-product epoxy compound is 100:62, keep the reaction temperature At 85°C for two hours, ...

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Abstract

The invention relates to a method for preparing a mother liquor of a slump-retaining polycarboxylate superplasticizer, comprising the steps of: 1) keeping an unsaturated macromonomer and an unsaturated acid under the action of an initiator, a reducing agent and a chain transfer agent for 25 ~80°C for 3 to 5 hours in water-phase free radical polymerization to obtain a polycarboxylate water reducer prepolymer; 2) Add the by-product epoxy compound in the industrial production process of organosilane coupling agent In the aqueous prepolymer, the carboxyl group is subjected to epoxy ring-opening esterification reaction at 80-90°C for two hours. After the reaction is completed, add a strong base to adjust the pH of the polymer to 5-6, and add water to obtain a mass concentration of 10-6. 60% slump-retaining polycarboxylate superplasticizer. In this method, the by-product epoxy compound and the polycarboxylate superplasticizer prepolymer are directly subjected to ring-opening esterification reaction during the generation of the organosilane coupling agent to adjust the length and density of the side chain of the polycarboxylate superplasticizer. The polycarboxylate water reducer has the effect of slump retention, and has the advantages of simple raw material and preparation process and low cost.

Description

technical field [0001] The invention relates to the technical field of polycarboxylate concrete water-reducer, in particular to a method for preparing a slump-retaining polycarboxylate water-reducer mother liquor. Background technique [0002] The new polycarboxylate superplasticizer is more and more widely used in my country. Its main mechanism of action mainly includes two aspects: one is to adsorb the surface of cement particles through the negatively charged carboxylic acid groups on the main chain of the polymer, so that the cement particles are The second is that the uncharged polymeric side chains are not adsorbed to form a steric repulsion effect. This steric repulsion effect is affected by the number of side chains on the main chain and the length of the side chains. Various polycarboxylate water reducers are prepared based on this mechanism by adjusting the side chain length and side chain density of the copolymer. [0003] But many problems follow, one of the most...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F283/06C08F220/06C08F222/02C08F8/00C04B24/26C04B103/30
CPCC04B24/2605C04B2103/302C08F8/00C08F283/065C08F220/06C08F222/02
Inventor 张瑞涛明金龙江元华陈文韬
Owner 安徽海螺材料科技股份有限公司
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