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Method for preparing slump-retaining polycarboxylate water reducer by modifying polyether with silane coupling agent

The technology of a silane coupling agent and a halogenated silane coupling agent is applied in the field of soil slump protection type, which can solve problems such as unreported, limited application improvement effect, etc., to achieve good application prospects and market competitiveness, and to protect dispersion and protection. The effect of collapse

Active Publication Date: 2019-06-21
BEIJING UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the products obtained by the above synthetic methods all have certain deficiencies. In the field of concrete superplasticizers, researchers have failed to achieve adsorption-water reduction-slump retention-dispersion by grafting polyether into the siloxane system. Composite functional chemical admixture with application performance
The method of only introducing the molecular structure of the silane coupling agent with siloxane through the main chain greatly limits its application improvement effect. It has been proved that grafting polyether in the silane system can significantly improve the slump performance of the polymer.
Therefore, the innovative use of Williamson etherification reaction and the preparation of terminal alkenyl silane modified polyether can be used as a modified side chain structure of polycarboxylate water reducer to achieve the composite work performance of adsorption-dispersion-slump retention, and at the same time It is also conducive to industrialized production and popularization and application, and there is no report about the work in this area at home and abroad

Method used

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  • Method for preparing slump-retaining polycarboxylate water reducer by modifying polyether with silane coupling agent
  • Method for preparing slump-retaining polycarboxylate water reducer by modifying polyether with silane coupling agent
  • Method for preparing slump-retaining polycarboxylate water reducer by modifying polyether with silane coupling agent

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] First, 2.41g of 3-chloropropyltriethoxysilane, 9.64g of ethanol, and 0.54g of water were sequentially added to the reactor, then 0.06g of acetic acid was added to adjust the pH of the mixture to 6, and the temperature was raised to 60°C for 1 hour of hydrolysis to obtain The hydrolysis product of 3-chloropropyltriethoxysilane; take 12g of methoxypolyoxyethylene ether (molecular weight = 2400) and dissolve it in 120g of sulfolane, stir and heat up to 50°C, add 2g of sodium hydroxide, and react for 0.5 hours , then add the hydrolyzate of 1.57g 3-chloropropyltriethoxysilane and 0.09g tetrabutylphosphorus bromide in turn, react for 2 hours, then filter the reaction solution, and then mix it with methanol-water with a volume ratio of 1:1 The solvent was purified three times and then dried in vacuum to obtain the etherified product of Williamson; 0.41g of γ-methacryloxypropyltrimethoxysilane, 1.64g of ethanol, and 0.39g of water were added to the reactor in sequence, and then ...

Embodiment 2

[0028] After the polycarboxylate superplasticizer solution with a concentration of 40% obtained in Example 1 was stored at 6°C for 20 days, its implementation effect was measured.

Embodiment 3

[0030] First, 1.99g of 3-chloropropyltrimethoxysilane, 35.82g of methanol, and 0.18g of water were sequentially added to the reactor, and then 0.92g of formic acid was added to adjust the pH of the mixture to 3, and the temperature was raised to 30°C for 18 hours of hydrolysis to obtain 3 -The hydrolysis product of chloropropyltrimethoxysilane; 30g nonylphenol polyoxyethylene ether (molecular weight=1500) was dissolved in 30g dimethyl sulfoxide, stirred and heated to 30°C, and 2.24g potassium hydroxide was added, React for 5 hours, then add the hydrolyzate of 0.52g 3-chloropropyltrimethoxysilane and 0.32g tetrabutylammonium bromide successively, react for 1 hour, then filter the reaction solution, and then use methanol- The water mixed solvent was purified 5 times and then vacuum-dried to obtain the etherification product of Williamson; 0.1g of vinyltrimethoxysilane, 1.8g of methanol, and 0.04g of water were added to the reactor in sequence, and then 0.06g of formic acid was ad...

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Abstract

The invention relates to a method using silane coupling agent modified polyether to prepare slump-loss-resistant polycarboxylate superplasticizer. The polycarboxylate superplasticizer is prepared by using a silane coupling agent, a polyether compound, an unsaturated carboxylic acid monomer and the like as the main reaction raw materials and sequentially performing hydrolysis, Williamson etherification, condensation and polymerization. The method specifically includes: hydrolyzing the halogenated silane coupling agent, allowing the hydrolyzed halogenated silane coupling agent to have Williamson etherification reaction with the polyether compound, allowing the etherification product to have condensation reaction with alkenyl silane coupling agent hydrolysate, and allowing the condensation product to have free radical polymerization reaction with unsaturated polyoxyethylene ether, a molecular weight regulator and the unsaturated carboxylic acid monomer under the effect of an initiator to prepare the polycarboxylate superplasticizer with multiple branched silane coupling agent modified polyether side chains. The method has the advantages that the method is simple and easy to control, high in polymerization degree, low in cost, energy-saving, efficient, environmentally friendly and free of pollution, a high steric-hindrance effect is achieved successfully, and the slump loss resistance of the prepared polycarboxylate superplasticizer is better than that of common polycarboxylate superplasticizer.

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 Williamson etherification reaction followed by hydrolysis of a hydrolyzed halogenated silane coupling agent and a polyether compound Condensation of alkenyl silane coupling agent and copolymerization with unsaturated carboxylic acid small monomer and unsaturated polyoxyethylene ether macromonomer to form silane coupling agent modified polyether to prepare slump-retaining polycarboxylate water reducer Preparation. Background technique [0002] Since the beginning of the new century, my country's national economy and scientific and technological strength have grown rapidly, and correspondingly, the entire construction industry in my country has undergone tremendous changes. The amount of concrete and cement has continued to increase, making cement concrete admixtures have become indispensable in the construction industry...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F290/06C08F283/06C08F220/06C08F222/02C08F222/06C08F228/02C08F230/08C04B24/26C04B24/16C04B103/30
CPCC04B24/165C04B24/2605C04B24/2694C04B2103/0059C04B2103/302C08F283/06C08F283/065C08F290/062C08F220/06C08F222/02C08F222/06C08F230/08
Inventor 刘晓赖光洪管佳男王子明奚文博王君慧李卓航张晓磊
Owner BEIJING UNIV OF TECH
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