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A kind of anti-clay type polycarboxylate water reducer and its preparation method and application

A technology of polycarboxylic acid and water reducing agent, applied in the field of water reducing agent, can solve problems such as unfavorable expansion of production, hindering intercalation adsorption, small steric hindrance of polyether terminal hydroxyl group, etc., and achieves good fluidity retention ability and fluidity. The effect of small loss ratio and excellent clay resistance

Active Publication Date: 2021-04-27
NANXIONG MATERIAL PRODION BASE OF CHINESE ACADEMY OF SCI GUANGZHOU CHEM +4
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

For example, Xiong Yan et al. (2017) used hydrogen peroxide-ascorbic acid as the redox initiation system, and used polyprenol polyoxyethylene ether, 2-acrylamido-2-methylpropanesulfonic acid, acrylic acid, and hydroxyethyl acrylate And self-made quaternary ammonium salt active monomer, synthesized polycarboxylate water reducer with quaternary ammonium salt active group; experiments show that the dispersion performance of the anti-clay type water reducer is almost poor when the clay content is greater than 4%. affected; however, the clay type used in this method is soil contained in river sand, which is not representative in practice
CN106496447A discloses a star-shaped amphoteric polycarboxylate water reducer with high-efficiency clay resistance and its preparation method. The polycarboxylate water reducer uses polyethylene glycol (meth)acrylate, (meth)acrylic acid and ( Meth)acryloyloxyethyltrimethylammonium chloride is obtained by RAFT polymerization under the chain transfer agent-star-shaped structure of β-cyclodextrin-based dithioester compound; the polycarboxylate water reducer not only reduces water High and exhibits excellent anti-clay effect; however, the monomer synthesis steps of this method are cumbersome, which is not conducive to expanding production
CN105330834A discloses a side chain end group modified polycarboxylic acid series anti-clay water reducer and its preparation method. The method first synthesizes an azide-terminated polycarboxylate water reducer, and then combines it with an alkynyl-terminated benzene Pyridine-like derivatives are subjected to click chemical reaction to obtain polycarboxylic acid-based anti-clay water-reducers whose side chain end groups are benzene-pyridine derivatives; by increasing the size of polyether terminal hydroxyl groups, it is hindered in clay Intercalation adsorption, so as to achieve the purpose of anti-clay; however, the steric hindrance of polyether terminal hydroxyl group obtained by this method is small, and the anti-adhesive effect is not obvious

Method used

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  • A kind of anti-clay type polycarboxylate water reducer and its preparation method and application

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Experimental program
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Effect test

Embodiment 1

[0025] (1) Add 500ml of dichloromethane and 15.2g (0.1mol) of 1-adamantanol into the reaction flask, stir and dissolve, slowly add 9.50g (0.105mol) of acryloyl chloride dropwise, react at 0°C for 12h, after the reaction The solvent was removed and separated by column chromatography to obtain the unsaturated adamantane monomer 1.

[0026] (2) 50ml of water, 1.8g (0.025mol) of acrylic acid (AA), 15g (0.00625mol) of methallyl polyoxyethylene ether (HPEG, Mn=2400), 0.193g (0.000937mol) of ) Unsaturated adamantane monomer 1, 0.687g sodium lauryl sulfate, stirred and dissolved under heating. Dissolve 0.252g hydrogen peroxide in 10ml deionized water to make solution A, dissolve 0.06g thioglycolic acid (TGA) in 10ml deionized water to make solution B, dissolve 0.064g ascorbic acid in 5ml deionized water to make solution C . After the reaction temperature rises to 70°C, add solution A and solution B to the reaction solution in turn, stir and react for 5 minutes, then add solution C, ...

Embodiment 2

[0028] (1) Add 500ml of dichloromethane and 15.2g (0.1mol) of 1-adamantanol to the reaction flask, stir and dissolve, slowly add 9.50g (0.105mol) of acryloyl chloride dropwise, react at 0°C for 12h, after the reaction The solvent was removed and separated by column chromatography to obtain the unsaturated adamantane monomer 1.

[0029] (2) 50ml of water, 1.8g (0.025mol) of acrylic acid (AA), 15g (0.00625mol) of methallyl polyoxyethylene ether (HPEG, Mn=2400), 0.256g (0.00125mol) of ) unsaturated adamantane monomer, 0.687g sodium lauryl sulfate, stirred and dissolved under heating. Dissolve 0.252g hydrogen peroxide in 10ml deionized water to make solution A, dissolve 0.06g thioglycolic acid (TGA) in 10ml deionized water to make solution B, dissolve 0.064g ascorbic acid in 5ml deionized water to make solution C . After the reaction temperature rises to 70°C, add solution A and solution B to the reaction solution in turn, stir and react for 5 minutes, then add solution C, and k...

Embodiment 3

[0031] (1) Add 500ml of dichloromethane and 15.2g (0.1mol) of 1-adamantanol into the reaction flask, stir and dissolve, slowly add 9.50g (0.105mol) of acryloyl chloride dropwise, react at 0°C for 12h, after the reaction The solvent was removed and separated by column chromatography to obtain the unsaturated adamantane monomer 1.

[0032] (2) Add 50ml of water, 2.15g (0.025mol) methacrylic acid (MAA), 15g (0.00625mol) isopentenyl polyoxyethylene ether (TPEG, Mn=2400), 0.128g (0.000625 mol) unsaturated adamantane monomer, 0.687g sodium lauryl sulfate, stirred and dissolved under heating. Dissolve 0.252g hydrogen peroxide in 10ml deionized water to make solution A, dissolve 0.06g thioglycolic acid (TGA) in 10ml deionized water to make solution B, dissolve 0.064g ascorbic acid in 5ml deionized water to make solution C . After the reaction temperature rises to 70°C, add solution A and solution B to the reaction solution in turn, stir and react for 5 minutes, then add solution C, ...

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Abstract

The invention discloses a polycarboxylate water-reducing agent and a preparation method and application thereof. The material containing adamantane structural unit and an unsaturated monomer with a double bond are reacted in a molar ratio of 1:1 to 1:1.5 , to obtain unsaturated adamantane derivatives containing double bonds; then mix unsaturated carboxylic acid monomers, unsaturated polyoxyethylene ether monomers, and unsaturated adamantane derivatives, add deionized water and emulsifier to stir and dissolve, Add initiator and chain transfer agent, react at 50℃~80℃ for 4~6h, after the reaction is completed, cool to room temperature, and then adjust pH to neutrality with alkaline solution to obtain clay-resistant polycarboxylate water reducer. The clay-resistant polycarboxylate water-reducing agent has excellent clay-resistant properties, good dispersing ability and fluidity retention ability, low dosage, and high water-reducing rate.

Description

technical field [0001] The invention relates to the field of water reducers, in particular to a clay-resistant polycarboxylate water reducer and its preparation method and application. Background technique [0002] As an indispensable admixture in the concrete industry, polycarboxylate superplasticizer has the advantages of high water reducing rate, small dosage, high fluidity and flexible structure design. It is widely used in concrete, ceramics and other fields. [0003] Concrete mainly uses sand and gravel as aggregates. Due to the shortage of sand and gravel resources in recent years, many areas have begun to mine sand and gravel resources in places with high clay content, such as mountains and rivers, resulting in an increase in the clay content of concrete sand and gravel aggregates. The quality of sand and gravel directly affects the performance of concrete. Excessive clay content will make the polycarboxylate superplasticizer ineffective and directly lead to a decrea...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F283/06C08F220/18C08F220/06C04B24/26C04B103/30
CPCC04B24/2694C04B2103/302C08F283/065C08F220/18C08F220/06
Inventor 廖兵李思敏庞浩黄健恒年福伟张静斐蒙业云
Owner NANXIONG MATERIAL PRODION BASE OF CHINESE ACADEMY OF SCI GUANGZHOU CHEM