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Method for preparing slump-retaining polycarboxylate water reducer by silylation of amino polyether end groups

An amino polyether and alkenyl silane coupling agent technology is applied in the field of preparing slump-preserving polycarboxylate water-reducing agents by silanization of amino polyether end groups, achieving the effects of convenient operation, enhanced slump-preserving effect, and improved application performance

Active Publication Date: 2019-03-22
中铁一局集团工业贸易有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Therefore, the method of preparing polycarboxylate water reducer by silylation of amino polyether terminal groups not only retains the characteristics of high strength bond energy of silicon oxide silicon, but also realizes the grafting of multiple amino polyether macromers after silane modification. Due to the structural characteristics of the same side chain, it has remarkable molecular structure characteristics and performance advantages. There is no report on this aspect of work at home and abroad.

Method used

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  • Method for preparing slump-retaining polycarboxylate water reducer by silylation of amino polyether end groups
  • Method for preparing slump-retaining polycarboxylate water reducer by silylation of amino polyether end groups
  • Method for preparing slump-retaining polycarboxylate water reducer by silylation of amino polyether end groups

Examples

Experimental program
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Effect test

Embodiment 1

[0029] First, 7.3g of 3-bromopropyltrimethoxysilane, 131.4g of methanol, and 0.54g of water were sequentially added to the reactor, then 2.76g of formic acid was added to adjust the pH of the mixture to 4, and the temperature was raised to 30°C for 17 hours of hydrolysis to obtain 3 -The hydrolysis product of bromopropyltrimethoxysilane; 45g of amino-terminated lauryl polyoxyethylene ether (molecular weight=500) was added to another reaction vessel, 36g of water was added, stirred and heated to 50°C, and then 2.01 The hydrolyzate of g3-bromopropyltrimethoxysilane and 15.12g sodium bicarbonate were heated up to 100°C for 3 hours, then purified 5 times with a methanol-water mixed solvent with a volume ratio of 2:1, and then vacuum-dried to obtain Terminal group silylation modified polyether product; take 0.41g allyltriethoxysilane, 7.38g methanol, 0.11g water and add them to the reactor successively, then add 0.18g formic acid to adjust the pH of the mixed solution to 4, and heat...

Embodiment 2

[0031] After the polycarboxylate superplasticizer solution with a concentration of 35% obtained in Example 1 was stored at 6° C. for 30 days, its implementation effect was measured.

Embodiment 3

[0033] First, 5.96g of 3-chloropropyltrimethoxysilane, 23.84g of ethanol, and 1.62g of water were sequentially added to the reactor, then 0.18g of acetic acid was added to adjust the pH of the mixture to 5, and the temperature was raised to 60°C for 2 hours for hydrolysis to obtain 3 - Hydrolyzed product of chloropropyl trimethoxy silicon; take 90g of aminomethoxy polyoxyethylene ether (molecular weight = 3000) and add it to another reaction vessel, add 108g of water, stir and heat up to 60°C, and then add 4.7g of the hydrolyzed product of 3-chloropropyltrimethoxysilane and 1.26g of sodium bicarbonate were heated up to 60°C for 7 hours, then purified 3 times with a methanol-water mixed solvent with a volume ratio of 1:1, and then vacuum-dried. Obtain end group silylation modified polyether product; take 1.47g vinyltrimethoxysilane, 5.88g ethanol, 2.32g water and add to the reactor successively, then add 0.06g acetic acid to adjust the pH of the mixed solution to 5, and raise th...

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Abstract

The invention relates to a method for preparing a slump loss-resistant type polycarboxylic acid water reducer by silanizing a terminal group of amino polyether. The method provided by the invention takes an amino polyether type compound, a silane coupling agent, an unsaturated carboxylic acid type monomer and the like as main reaction raw materials and a polycarboxylic acid water reducer is prepared through firstly hydrolyzing, substituting, then carrying out condensation, and finally copolymerizing; the method comprises the following steps: firstly hydrolyzing by a halogenated silane coupling agent; then taking the silane coupling agent and the amino polyether type compound to be subjected to substitution reaction; carrying out the condensation on a substituted product and a vinyl silane coupling agent hydrolyzed product; taking a condensed product and unsaturated polyoxyethylene ether, a molecular weight regulator and the unsaturated carboxylic acid type monomer to be subjected to free-radical copolymerization reaction under the action of an initiator to prepare the polycarboxylic acid water reducer with a plurality of branched silane modified polyether side chains. The method provided by the invention has the advantages of simple and easy-to-control process, low cost, energy saving and high efficiency, environmental protection and no pollution; dual modification of the side chains of a main chain of a polycarboxylic acid molecule is successfully realized and more excellent water reduction and slump loss resistance performance, which is better than that of a common polycarboxylic acid water reducer, is represented.

Description

technical field [0001] The invention relates to the technical field of a slump-retaining polycarboxylate water reducer for cement concrete, in particular to a hydrolyzed halosilane coupling agent and an amino polyether compound to replace and react with a hydrolyzed alkenyl silane The specific preparation method of coupling agent condensation and unsaturated carboxylic acid small monomer and unsaturated polyoxyethylene ether macromonomer to form amino polyether end group silanization to prepare slump-retaining polycarboxylate water reducer. Background technique [0002] The continuous development of high-performance concrete has led to higher and higher requirements for concrete chemical admixtures. Scholars are currently working on the development of chemical admixtures that can significantly improve concrete workability, mechanical strength, and durability. Polycarboxylate high-performance water reducer has the characteristics of high water reducing rate, good slump retent...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F283/06C08F290/06C08F220/06C08F222/02C08F222/06C08G65/00C04B24/26C04B103/30
CPCC04B24/2694C04B2103/302C08F283/065C08F290/062C08G65/00C08F220/06C08F222/02C08F222/06
Inventor 刘晓赖光洪管佳男王子明奚文博李卓航王君慧张晓磊
Owner 中铁一局集团工业贸易有限公司
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