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Amino acid modified mud-resistant polycarboxylate water reducer and preparation method thereof

A technology of amino acid and water reducer, which is applied to the preparation of carboxylic acid ester, reaction preparation of carboxylic acid/symmetric anhydride and saturated hydrocarbon, chemical instruments and methods, etc. It can solve the problems of limited short-chain steric hindrance effect, harsh reaction conditions, and anti-adsorption Insufficient capacity and other problems, to achieve the effect of improving anti-adsorption capacity, simplifying synthesis steps, and improving poor fluidity

Active Publication Date: 2022-03-08
CHINA WEST CONSTR ACAD OF BUILDING MATERIALS CO LTD +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the diphenylphosphoryl chloride used in its synthesis is easy to hydrolyze, and the reaction conditions are harsh; at the same time, the steric hindrance effect of the short chain is limited, and the anti-adsorption capacity is insufficient.

Method used

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  • Amino acid modified mud-resistant polycarboxylate water reducer and preparation method thereof
  • Amino acid modified mud-resistant polycarboxylate water reducer and preparation method thereof
  • Amino acid modified mud-resistant polycarboxylate water reducer and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0038] A preparation method of amino acid modified mud-resistant polycarboxylate water reducer, the specific steps are as follows:

[0039] S1, Preparation of Amino Acid Modified Unsaturated Ester:

[0040] S11. Place 0.15 mol of polyethylene glycol with a molecular weight of 400 in a reaction vessel, add 0.15 mol of maleic anhydride at one time under stirring conditions, and continuously feed N 2 , after the maleic anhydride is dissolved, add catalyst sulfuric acid, the amount of sulfuric acid is 0.4% of the total mass of polyethylene glycol and maleic anhydride, and stir and react at 40°C for 3h.

[0041] S12, take 0.12mol of the product of step S11 in the reaction vessel, and continuously feed N 2 , heat up to 50°C, add catalyst tetrabutylammonium chloride, add 0.12mol of epichlorohydrin dropwise within 1.5h, keep warm for 4h, the amount of catalyst added is 0.8% of the total mass of the product in step S11 and epichlorohydrin .

[0042] S13, take 0.10mol of the product ...

Embodiment 2

[0047] A preparation method of amino acid modified mud-resistant polycarboxylate water reducer, the specific steps are as follows:

[0048] S1, Preparation of Amino Acid Modified Unsaturated Ester:

[0049] S11. Place 0.13 mol of polyethylene glycol with a molecular weight of 800 in the reaction vessel, add 0.14 mol of maleic anhydride at one time under stirring conditions, and continuously feed N 2 , after the maleic anhydride is dissolved, add catalyst phosphoric acid, the dosage of phosphoric acid is 0.3% of the total mass of polyethylene glycol and maleic anhydride, and stir and react at 60°C for 2h.

[0050] S12, take 0.11mol of the product of step S11 in the reaction vessel, and continuously feed N 2 , the temperature was raised to 50° C., the catalyst tetrabutylammonium bromide was added, 0.12 mol of epichlorohydrin was added dropwise within 3 hours, and the reaction was kept for 5 hours. The amount of catalyst added was 0.6% of the total mass of the product of step S1...

Embodiment 3

[0056] A preparation method of amino acid modified mud-resistant polycarboxylate water reducer, the specific steps are as follows:

[0057] S1, Preparation of Amino Acid Modified Unsaturated Ester:

[0058] S11. Place 0.14 mol of polyethylene glycol with a molecular weight of 1600 in the reaction vessel, add 0.14 mol of maleic anhydride at one time under stirring conditions, and continuously feed N 2 After the maleic anhydride is dissolved, add the catalyst phosphorous acid, the amount of phosphorous acid is 0.7% of the total mass of polyethylene glycol and maleic anhydride, and stir and react at 70°C for 3h.

[0059] S12, take 0.13mol of the product of step S11 in the reaction vessel, and continuously feed N 2 , heat up to 60°C, add catalyst benzyltrimethylammonium bromide, add 0.13mol of epichlorohydrin dropwise within 2h, keep warm for 6h, the amount of catalyst added is 1.0% of the total mass of the product in step S11 and epichlorohydrin %.

[0060] S13, take 0.12mol o...

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Abstract

The invention discloses an amino acid modified mud-resistant polycarboxylate water reducer, which uses amino acid modified unsaturated ester, unsaturated carboxylic acid and isopentenol polyoxyethylene ether as raw materials, in the process of initiator and chain transfer Under the action of an agent, it is formed by free radical polymerization. The amino acid modified unsaturated ester is prepared from maleic anhydride, polyethylene glycol, epichlorohydrin and amino acid through esterification reaction, ring opening reaction and substitution reaction in sequence under solvent-free conditions. The mass percentage of each raw material is: 3-15% amino acid modified unsaturated ester, 5-13% unsaturated carboxylic acid, 70-90% isopentenol polyoxyethylene ether, 0.5-1.5% initiator and 0.5- 1.0% chain transfer agent. The water reducer of the present invention has the functions of adsorbing anchor groups and steric hindrance structure, and at the same time uses its electrostatic repulsion, non-polar structure and terminal steric hindrance to inhibit the surface adsorption and absorption of clay on the polycarboxylate water reducer. Intercalation adsorption improves the anti-adsorption ability of clay.

Description

technical field [0001] The invention relates to the technical field of concrete admixtures, in particular to an amino acid modified mud-resistant polycarboxylate water reducer and a preparation method thereof. Background technique [0002] With the rapid development of my country's construction industry, the consumption of sand and gravel is huge, and high-quality sand and gravel resources are scarce. Especially in some areas with poor ground quality, the high mud content of sand and gravel has gradually become an urgent problem to be solved in the concrete industry. . A large number of engineering examples and studies have shown that compared with naphthalene-based, melamine-based and sulfamic acid-based water-reducers, polycarboxylate water-reducers (PCE), which are commonly used in concrete production, are more effective in reducing the mud content in aggregates. Sensitive, mainly manifested in the increase of the dosage, the poor effect of concrete slump retention, and t...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F283/06C08F220/06C08F222/22C08G65/331C08G65/333C08G65/337C07C67/035C07C69/60C07C67/28C07C227/18C07C229/12C04B24/26C04B103/30
CPCC08F283/065C08G65/3318C08G65/337C08G65/33306C04B24/2694C07C67/035C07C67/28C07C227/18C04B2103/302C08F220/06C07C69/60C07C229/12
Inventor 高育欣杨文曾超毕耀刘明王福涛张磊叶子
Owner CHINA WEST CONSTR ACAD OF BUILDING MATERIALS CO LTD
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