A kind of preparation method of ether high water retention type polycarboxylate water reducer

A water-retaining, polycarboxylic acid technology, applied in the field of building admixtures, can solve the problems of poor product water-retention performance, increased concrete viscosity, and increased pumping costs, and achieves increased steric hindrance effect, stable fluidity, and reduced cost. The effect of high water rate

Active Publication Date: 2021-05-25
KZJ NEW MATERIALS GROUP CO LTD +1
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Problems solved by technology

CN107759744A discloses the preparation method of polycarboxylate slump-retaining agent of slump-retaining and water-reducing type. The product prepared by the method has good slump-retaining performance, but the phenomenon of hysteresis amplification will occur, and the phenomenon of bleeding after the concrete is prone to occur. The product The water retention performance is not good
CN105669919A discloses a high water retention polycarboxylate water reducer and its preparation method. The water reducer prepared by this method has a certain water retention effect, but at the same time it can increase the viscosity of concrete, which is not conducive to pumping. and will increase pumping costs

Method used

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  • A kind of preparation method of ether high water retention type polycarboxylate water reducer

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Experimental program
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Effect test

Embodiment 1

[0023] (1) Esterification reaction: 180.00g of glucose, 663.60g of ethyl 2-amino-4-methyl-5-phospho-3-pentenoate, 6.80g of phenothiazine and 8.50g of p-toluenesulfonic acid were added to the reaction kettle Mix in the middle, under the protection of nitrogen, react at a constant temperature of 100°C for 4.0h, during which the water is removed by vacuuming or nitrogen with water, and after the reaction is completed, it is lowered to room temperature, and the esterification product and unreacted 2-amino - mixtures of ethyl 4-methyl-5-phospho-3-pentenoate;

[0024] (2) Monomer blending: 8.00g of the mixture prepared in step (1), 1.50g of methyl 3-fluorocinnamate, 200.00g of methallyl alcohol polyoxyethylene ether with a molecular weight of 2400 and 14.00g of acrylic acid Mix, and add 100.00g water to make it dissolve, obtain comonomer mixture solution;

[0025] (3) Copolymerization reaction: the above-mentioned comonomer mixture solution, hydrogen peroxide aqueous solution (wher...

Embodiment 2

[0028] (1) Esterification reaction: Add 180.00g glucose, 627.00g 2-amino-4-methyl-5-phospho-3-pentenoic acid, 8.20g phenothiazine and 12.00g ethylsulfonic acid into the reaction kettle and mix , under the protection of nitrogen, react at a constant temperature of 110°C for 3.0h, during which time the water is removed by vacuuming or nitrogen with water. - mixtures of methyl-5-phospho-3-pentenoic acid;

[0029] (2) Monomer blending: 4.00g of the mixture prepared in step (1), 2.0g of methyl 4-fluorocinnamate, 200.00g of methallyl polyoxyethylene polyoxypropylene ether with a molecular weight of 3000 and 18.00g of methacrylic acid was mixed, and 100.00g of water was added to dissolve it to obtain a comonomer mixture solution;

[0030] (3) Copolymerization reaction: the above-mentioned comonomer mixture solution, azobisisobutylamidine hydrochloride aqueous solution (wherein azobisisobutylamidine hydrochloride 4.00g, water 40.00g) and sodium acetate aqueous solution (wherein Sodi...

Embodiment 3

[0033](1) Esterification reaction: 180.00g of glucose, 543.40g of 2-amino-4-methyl-5-phosphonopent-3-enoic acid, 6.00g of hydroquinone and 8.80g of benzenesulfonic acid were added to the reaction kettle Mix, under the protection of nitrogen, react at a constant temperature of 110°C for 2.0h, during which time, remove water by vacuuming or nitrogen with water, and cool down to room temperature after the reaction, to obtain esterification products and unreacted 2-amino- Mixtures of 4-methyl-5-phosphonopent-3-enoic acid;

[0034] (2) Monomer blending: 6.00g of the mixture prepared in step (1), 1.80g of 3-(3-fluorophenyl) ethyl acrylate, 200.00g of isopentenol polyoxyethylene ether with a molecular weight of 1200 Mix with 22.00g fumaric acid, and add 100.00g water to make it dissolve, obtain comonomer mixture solution;

[0035] (3) Copolymerization reaction: the above-mentioned comonomer mixture solution, azobiscyanovaleric acid aqueous solution (wherein azobiscyanovaleric acid 3...

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Abstract

The invention discloses a preparation method of an ether-based high water-retaining polycarboxylate water-reducer, which comprises the following steps: (1) esterification reaction; (2) monomer blending; (3) copolymerization reaction; (4) and react. The preparation method of the present invention grafts glucose, the esterification product of the first compound, and the unsaturated fluorine-containing monomer into the polycarboxylic acid molecular chain by copolymerization, and introduces glucose into the molecular structure of the prepared polycarboxylate water reducer. Ester structure, fluorophenyl structure, phosphoric acid group structure, amino structure, etc., under the mutual synergy of these structures, the polycarboxylate superplasticizer of the present invention has high water retention and can effectively lock the water in concrete , control the hydrolysis rate of the ester group, will not lag behind bleeding, and the concrete fluidity is stable.

Description

technical field [0001] The invention belongs to the technical field of building admixtures, and in particular relates to a preparation method of an ether-based high water-retaining polycarboxylate water-reducer. Background technique [0002] Polycarboxylate superplasticizer has outstanding advantages such as high water reducing rate, good adaptability to cement, and excellent slump retention performance. It has become the most important product in the concrete admixture market. With the construction of large-scale infrastructure such as nuclear power, water conservancy, bridges, and tunnels in my country, especially the planning and implementation of railway passenger dedicated line network projects, the market demand for polycarboxylate water reducers continues to grow. Polycarboxylate water reducer is a kind of surfactant containing carboxyl graft copolymer in its molecule. Its unique molecular structure makes it have many unique advantages, such as low dosage, high water ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F283/06C08F220/06C08F222/02C08F222/06C04B24/26C04B103/30
CPCC04B24/2605C04B2103/302C08F283/065C08F220/06C08F222/02C08F222/06
Inventor 官梦芹郭鑫祺蒋卓君李祥河陈晓彬林添兴郭元强
Owner KZJ NEW MATERIALS GROUP CO LTD
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