Preparation method and application of comb-shaped block polycarboxylate superplasticizer

A technology of superplasticizer and polycarboxylic acid, which is applied in the field of preparation of comb-shaped block polycarboxylic acid superplasticizer, can solve the problems of reduced catalytic efficiency and achieve strong regional adaptability, low dosage and convenient transportation Effect

Inactive Publication Date: 2019-08-23
中科广化(重庆)新材料研究院有限公司 +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, because the polymerization of unsaturated acid is still used in the preparation process, it may lead to the complexation of the polymer and the metal catalyst, and the catalytic efficiency is reduced.

Method used

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  • Preparation method and application of comb-shaped block polycarboxylate superplasticizer
  • Preparation method and application of comb-shaped block polycarboxylate superplasticizer
  • Preparation method and application of comb-shaped block polycarboxylate superplasticizer

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0045] (1) Mix p-toluenesulfonyl chloride, benzyl methacrylate, cuprous bromide, pentamethyldiethylenetriamine and tetrahydrofuran in a molar ratio of 1:100:1:0.8:1:100, and pass Into N 2 O in the solution 2 discharge, the N 2 Carry out atom transfer controlled radical polymerization under protection, react at room temperature for 3 hours, and precipitate with a mixed solvent of methanol:water=1:1 after the reaction to obtain a macromolecular initiator.

[0046] (2) the macroinitiator prepared in the step (1), polyethylene glycol methacrylate (molecular weight 950g / mol), cuprous bromide, pentamethyldiethylenetriamine and tetrahydrofuran are molar ratio 1:100:1:1:100 mix evenly, pass into N 2 O in the solution 2 Exhaust, exhaust air, blow nitrogen after continuous operation, in N 2 Atom transfer controllable radical polymerization was carried out under protection, and the reaction was carried out at 35° C. for 12 hours. After the reaction was completed, it was precipitated...

Embodiment 2

[0049] (1) Mix benzyl chloride, benzyl methacrylate, cuprous bromide, copper bromide, tetramethylethylenediamine and toluene in a molar ratio of 1:50:0.5:0.5:1:50, and pass it into N 2 O in the solution 2 discharge, the N 2 Atom transfer controllable radical polymerization was carried out under protection, and the reaction was carried out at room temperature for 4.5 hours. After the reaction was completed, it was precipitated in ethanol to obtain a macromolecular initiator.

[0050] (2) The macromolecular initiator obtained in step (1), polyethylene glycol acrylate (molecular weight 2000g / mol), cuprous bromide, pentamethyldiethylenetriamine and acetone are molar ratio 1:50 :1:1:50 mix, pass into N 2 O in the solution 2 Exhaust, exhaust air, blow nitrogen after continuous operation, in N 2 Carry out atom transfer controlled radical polymerization under protection, react at 25° C. for 24 hours, and precipitate in methanol after the reaction to obtain a comb-shaped block cop...

Embodiment 3

[0053] (1) Ethyl 2-bromoisobutyrate, benzyl methacrylate, cuprous bromide, copper bromide, pentamethyldiethylenetriamine and toluene in a molar ratio of 1:200:0.1:0.1: 0.25:100 mix, pass into N 2 O in the solution 2 discharge, the N 2 Carry out atom transfer controlled free radical polymerization under protection, react at room temperature for 3 hours, and precipitate in a mixed solvent of methanol:acetone=3:1 after the reaction to obtain a macromolecular initiator.

[0054] (2) with step (1) gained macromolecular initiator, polyethylene glycol methacrylate (molecular weight 450g / mol), cuprous bromide, 2,2'-bipyridyl and anisole in molar ratio 1: 150:0.5:0.5:150 mixed, pass into N 2 O in the solution 2 Exhaust, exhaust air, blow nitrogen after continuous operation, in N 2 Atom transfer controllable radical polymerization was carried out under protection, and the reaction was carried out at 25° C. for 24 hours. After the reaction, it was precipitated in a mixed solvent of ...

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Abstract

The invention belongs to the technical field of super plasticizers and discloses a preparation method and application of a comb-shaped block polycarboxylate superplasticizer. According to the invention, a halide is used as an initiator, metal copper ions and ligands are used as a catalytic system, unsaturated acid ester is taken as a monomer, and a free radical polymerization reaction is carried out to generate a macromolecular initiator; then the macromolecular initiator is taken as an initiator and unsaturated polyether is used as a monomer to generate a comb-shaped block copolymer; and thecomb-shaped block copolymer is subjected to acidolysis to obtain the comb-shaped block superplasticizer, wherein carboxylic acid chain segments obtained by acidolysis serve as anchoring groups to be adsorbed on the surface of cement particles, and hydrophilic polyether is used as steric hindrance groups, so that dispersibility reduction of cement particles due to influence of calcium ions in cement pores on the carboxylic acid chain segments can be prevented, and finally, the cement particles are uniformly dispersed. Meanwhile, a large amount of free water generated by agglomeration is released, so that the purpose of improving fluidity of cement slurry is achieved. The super plasticizer has the characteristics of low mixing amount, high cement slurry fluidity and the like.

Description

technical field [0001] The invention belongs to the technical field of superplasticizers, in particular to a preparation method and application of a comb-shaped block polycarboxylic acid superplasticizer. Background technique [0002] Compared with ordinary concrete, high-performance concrete has the advantages of multi-functionality, high strength and environmental friendliness, and these advantages mainly rely on the development of concrete admixtures. Among them, the concrete superplasticizer is the one with the largest amount and the widest application range among all admixtures. The water reducer is actually a surfactant that can highly disperse the cement particles and stabilize the dispersion system. The high-efficiency water reducer has a good dispersion effect on cement, and is recognized as the third leap in concrete technology after reinforced concrete and prestressed reinforced concrete technology. Polycarboxylate superplasticizer is a high-efficiency superplas...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F293/00C08F299/02C04B24/24C04B103/32
CPCC04B24/24C04B2103/32C08F293/005C08F299/02
Inventor 庞浩李佳霖廖兵黄健恒喻培韬刘琦
Owner 中科广化(重庆)新材料研究院有限公司
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