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Amino acid-modified mud-resistant polycarboxylic acid water reducing agent and preparation method thereof

An amino acid and water reducing agent technology, which is applied in the preparation of carboxylic acid esters, the preparation of carboxylic acid/symmetric anhydrides and saturated hydrocarbons, and the preparation of cyanide reactions. It can solve the problems of insufficient anti-adsorption ability, harsh reaction conditions, short-chain steric hindrance It can improve the anti-adsorption capacity, simplify the synthesis steps, and improve the poor fluidity.

Active Publication Date: 2020-02-07
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 polycarboxylic acid water reducing agent and preparation method thereof
  • Amino acid-modified mud-resistant polycarboxylic acid water reducing agent and preparation method thereof
  • Amino acid-modified mud-resistant polycarboxylic acid water reducing agent and preparation method thereof

Examples

Experimental program
Comparison scheme
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 polycarboxylic acid water reducing agent. An amino acid-modified unsaturated acid ester, an unsaturated carboxylic acid, and isopentenol polyoxyethylene ether are used as raw materials, and the polycarboxylic acid water reducing agent is formed by free radical polymerization under the action of an initiator and a chain transfer agent. The amino acid-modified unsaturated acid ester is prepared by using maleic anhydride, polyethylene glycol, epichlorohydrin and an amino acid as raw materials, and sequentially carrying out an esterification reaction, a ring-opening reaction and a substitution reaction under the condition of no solvent. The mass percentage of each raw material is as follows: 3-15% of the amino acid-modified unsaturated acid ester, 5-13% of the unsaturated carboxylic acid, 70-90% of the isopentenol polyoxyethylene ether, 0.5-1.5% of the initiator, and 0.5-1.0% of the chain transfer agent. The water reducing agenthas the effects of an absorption anchoring group and a steric hindrance structure, and at the same time, the electrostatic repulsion effect, a non-polar structure, and the terminal steric hindrance effect of the water reducing agent are utilized to inhibit the surface adsorption and intercalation adsorption of the water reducing agent by clay, so that adsorption resistance to clay is improved.

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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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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