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Preparation method of ether type slump retaining polycarboxylate superplasticizer

A polycarboxylic acid and slump-preserving technology, which is applied in the field of building materials, can solve problems such as rapid slump loss and troublesome concrete construction, and achieve an increase in initial water-reducing rate, excellent slump-preserving effect, and increased steric hindrance effect Effect

Active Publication Date: 2017-02-22
KZJ NEW MATERIALS GROUP CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The excellent water-reducing performance of polycarboxylate superplasticizers has been widely recognized by the industry, but due to factors such as changes in cement, mud content in sand, and stone materials, polycarboxylate superplasticizers have also slumped in practical applications. The problem of excessive loss of strength has brought a lot of trouble to the construction of concrete

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] (1) Mix 239.80g of hydroxyethyl acrylate, 100.00g of terephthalic acid, and 2.21g of phenothiazine. Under nitrogen protection, heat up to 60°C, add 4.23g of p-toluenesulfonic acid, heat up to 120°C, and keep warm for reaction 1h, remove water with the method of evacuating or leading nitrogen belt water during 1h, be down to room temperature after reaction finishes, obtain the first mixture that contains esterification product and unreacted hydroxyethyl acrylate;

[0028] (2) Mix 10.00 g of the first mixture prepared in step (1), 14.50 g of acrylic acid, and 200.00 g of methallyl alcohol polyoxyethylene ether with a molecular weight of 2400, and add 130.00 g of water to dissolve it to obtain a copolymerized monomer Body mixture solution;

[0029] (3) The above-mentioned comonomer mixture solution, ammonium persulfate aqueous solution (wherein, ammonium persulfate 1.63g, water 30.00g), thioglycolic acid aqueous solution (wherein, thioglycolic acid 1.10g, water 30.00g) are...

Embodiment 2

[0032] (1) Mix 110.00g hydroxyethyl acrylate, 110.00g hydroxypropyl acrylate, 100.00g terephthalic acid, 1.60g hydroquinone, 2.00g phenothiazine, heat up to 50°C under nitrogen protection, add 4. 20g of concentrated sulfuric acid with a mass fraction of 98% was heated up to 115°C and kept for 3 hours. During this period, the water was removed by vacuuming or nitrogen-carrying water. After the reaction was completed, it was cooled to room temperature to obtain esterification products and unreacted a first mixture of hydroxyethyl acrylate and hydroxypropyl acrylate;

[0033] (2) Mix 5.00 g of the first mixture prepared in step (1), 16.00 g of acrylic acid, 4.00 g of maleic anhydride, and 142.00 g of methallyl polyoxyethylene polyoxypropylene ether with a molecular weight of 2400, and add 90.00 g of water to dissolve it to obtain a comonomer mixture solution;

[0034] (3) Mix the above-mentioned comonomer mixture solution with hydrogen peroxide aqueous solution (wherein, hydroge...

Embodiment 3

[0037] (1) Mix 240g of hydroxyethyl methacrylate, 100.00g of terephthalic acid, and 3.20g of hydroquinone, under the protection of nitrogen, heat up to 60°C, add 7.30g of ethylsulfonic acid, and heat up to 110°C , heat preservation reaction 2h, remove water with the method of vacuumizing or leading nitrogen band water during, after reaction finishes, drop to room temperature, obtain the first mixture that contains esterification product and unreacted hydroxyethyl methacrylate;

[0038](2) Mix 5.00 g of the first mixture prepared in step (1), 12.00 g of maleic anhydride, and 111.00 g of allyl alcohol polyoxyethylene ether with a molecular weight of 2400, and add 90.00 g of water to dissolve it to obtain a copolymerized monomer Body mixture solution;

[0039] (3) The above-mentioned comonomer mixture solution, potassium persulfate aqueous solution (wherein, potassium persulfate 3.00g, water 30.00g), trisodium phosphate aqueous solution (wherein, trisodium phosphate 1.30g, water ...

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Abstract

The invention discloses a preparation method of an ether type slump retaining polycarboxylate superplasticizer. The preparation method comprises following steps: (1), unsaturated carboxylic acid hydroxyl esters are mixed with benzene dialkyl carboxylic acid and a polymerization inhibitor, the temperature is increased to 40-60 DEG C under the protection of nitrogen, a catalyst is added, the temperature is increased to 100-140 DEG C, a mixture is subjected to heat preservation reaction for 0.5-3 h, water is removed during the reaction, the mixture is cooled to the room temperature after the reaction, and a first mixture is obtained; (2), the first mixture, unsaturated carboxylic acid and / or unsaturated carboxylic acid anhydride and ether type monomers are mixed, water is added to dissolve the components, and a comonomer mixture solution is obtained; (3), the comonomer mixture solution, an initiator aqueous solution and a molecular weight regulator aqueous solution are dropped into water for a reaction, and a copolymerization product is obtained; (4), pH of the copolymerization product is regulated to be 5-7 with alkali, and the ether type slump retaining polycarboxylate superplasticizer is obtained. A benzene dialkyl carboxylic acid structure is introduced into a molecular structure of the polycarboxylate superplasticizer, so that the finally synthesized superplasticizer has excellent water reducing and slump retaining effects.

Description

technical field [0001] The invention belongs to the technical field of building materials, and in particular relates to a preparation method of an ether-based slump-retaining polycarboxylate water reducer. Background technique [0002] In today's world, the social economy is booming, urban construction is advancing by leaps and bounds, and the construction of transportation, hydropower, municipal and other related projects is also developing rapidly. These projects also put forward higher requirements for building concrete. To obtain high standards, high quality and Low-carbon, environment-friendly construction concrete, polycarboxylate water-reducing agent with excellent performance and environmental protection is essential. [0003] The excellent water-reducing performance of polycarboxylate superplasticizers has been widely recognized by the industry, but due to factors such as changes in cement, mud content in sand, and stone materials, polycarboxylate superplasticizers ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F283/06C08F220/06C08F220/28C08F222/14C08F222/06C04B24/26C04B103/30
CPCC04B24/2694C08F283/065C04B2103/30C08F220/281C08F222/14
Inventor 蒋卓君方云辉官梦芹陈小路钟丽娜代柱端尹峻
Owner KZJ NEW MATERIALS GROUP CO LTD
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