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Preparation method of super-high-dispersion polycarboxylate-type efficient water reducing agent

A high-efficiency water reducer, polycarboxylate technology, applied in the field of polycarboxylate water reducer for cement concrete, can solve the problems of complex preparation engineering process, very industrialized production, harsh reaction conditions, etc., and achieve rich sources , quick and efficient response, and mature methods

Active Publication Date: 2016-09-28
JIANGSU CHINA RAILWAY ARIT NEW MATEIRALS CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The entire preparation process of this invention is complicated, cumbersome to operate, a large amount of organic solvents are used, the preparation cost is high, the reaction conditions are harsh and the product yield is low, so it is very difficult for industrial production

Method used

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  • Preparation method of super-high-dispersion polycarboxylate-type efficient water reducing agent
  • Preparation method of super-high-dispersion polycarboxylate-type efficient water reducing agent
  • Preparation method of super-high-dispersion polycarboxylate-type efficient water reducing agent

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037]1) Preparation of amino-terminated copolymers: 10 mol of 2-methacrylamine and 2 mol of methyl acrylate were subjected to oxidation-reduction radical polymerization at 25° C. for 30 minutes under 0.01 mol of mercaptoacetic acid to obtain copolymers containing terminal amines. The weight-average molecular weight of the amino-terminated copolymer product is 3000;

[0038] 2) Preparation of unsaturated halogen-terminated copolymers: 10 mol of amine-terminated copolymers obtained in step 1) and 30 mol of 2-bromoisobutyryl bromide were subjected to an esterification reaction at 0°C for 90 minutes to obtain halogen-terminated copolymers ;

[0039] 3) Preparation of super-dispersive water reducer: the copolymerization product of 10mol terminal halogen group obtained in step 2), 50mol butyl methacrylate, 0.01mol CuBr and 0.02mol pentamethyldiethylenetriamine (PMDETA) 50 After reacting at ℃ for 240 minutes, a super-dispersed polycarboxylate superplasticizer can be obtained. The p...

Embodiment 2

[0042] 1) Preparation of amino-terminated copolymers: 10 mol of allylamine and 2.5 mol of ethyl acrylate were subjected to oxidation-reduction free radical polymerization at 30°C for 35 minutes under the action of 0.1 mol of 2-mercaptopropionic acid to obtain copolymers containing terminal amines. The weight-average molecular weight of the amine-based copolymerization product is 3500;

[0043] 2) Preparation of unsaturated halogen-terminated copolymers: 10 mol of amine-terminated copolymers obtained in step 1) and 40 mol of 2-bromoisobutyryl chloride were subjected to an esterification reaction at 5° C. for 80 minutes to obtain halogen-terminated copolymers;

[0044] 3) Preparation of super-dispersive water reducer: react the 10mol terminal halogen copolymer obtained in step 2), 250mol hydroxyethyl acrylate, 0.03mol CuCl, and 0.02mol HMTETA at 55°C for 200 minutes to obtain a super-dispersive type Polycarboxylate superplasticizer, the polycarboxylate high-efficiency water redu...

Embodiment 3

[0047] 1) Preparation of amino-terminated copolymers: 10mol 3-methyl-2-butene-1-amine and 3mol propyl acrylate were subjected to oxidation-reduction free radical polymerization at 35°C under the action of 0.04mol 3-mercaptopropionic acid 40min obtains the copolymerization product containing terminal amino group, and the weight-average molecular weight of the terminal amino group copolymerization product is 4000;

[0048] 2) Preparation of unsaturated halogen-terminated copolymers: 10 mol of amine-terminated copolymers obtained in step 1) and 50 mol of 2-chloroisobutyryl chloride were subjected to an esterification reaction at 10° C. for 70 minutes to obtain halogen-terminated copolymers;

[0049] 3) Preparation of super-dispersive water reducer: the copolymerization product of 10mol terminal halogen group obtained in step 2), 300mol hydroxypropyl acrylate, 0.05mol CuBr, 0.1mol tetrakis [(2-pyridyl) methyl] ethyl Diamine (TPEN) was reacted at 60°C for 180 minutes to obtain a su...

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Abstract

The invention discloses a preparation method of a super-high-dispersion polycarboxylate-type efficient water reducing agent. The preparation method includes the specific steps that firstly a terminal amino-based copolymerization product is prepared, then a terminal halogen-based unsaturated copolymerization product is prepared, finally the obtained terminal halogen-based unsaturated copolymerization product, an unsaturated ester monomer B, a transition metal compound and a ligand react at the temperature of 50-80 DEG C, and the super-high-dispersion polycarboxylate water reducing agent is obtained. Product performance is adjusted by controlling the molecular structure and the molecular weight on a main chain / side chain of the water reducing agent, the reaction speed is high, efficiency is high, the water reducing agent is free of toxin and pollution, and operation is simple. The prepared polycarboxylate-type water reducing agent is the super-high-dispersion polycarboxylate-type efficient water reducing agent and is stable in product performance and low in cost and particularly has an excellent slump retaining effect on stones containing mud and sand.

Description

technical field [0001] The invention relates to the technical field of a polycarboxylate water reducer for cement concrete, in particular to a super-dispersed polycarboxylate combined with an atom transfer radical polymerization (ATRP) reaction and an oxidation-reduction radical polymerization reaction. A preparation method of an acid-based high-efficiency water reducer. Background technique [0002] With the construction of national large-scale infrastructure nuclear power, water conservancy, bridges, high-speed rail, tunnels and various large-scale projects, the commercial concrete industry has developed by leaps and bounds, and the continuous improvement of the strength and performance requirements of concrete has also prompted high-performance concrete. The rapid development of agents. High-performance water reducer is an important material to meet the requirements of high-performance concrete. Due to its good plasticity and excellent application performance, it has bee...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F271/00C08F220/18C08F226/02C08F220/14C04B24/26C04B103/30
CPCC04B24/2688C04B2103/302C08F226/02C08F271/00C08F220/14C08F220/1804
Inventor 钱珊珊张岭王毅姜海东郑春扬郭兆来
Owner JIANGSU CHINA RAILWAY ARIT NEW MATEIRALS CO LTD
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