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A kind of synthetic method of retarding polycarboxylate superplasticizer

A technology of retarding polycarboxylic acid and its synthesis method, which is applied in the field of construction admixtures and can solve problems such as inability to fully utilize it

Active Publication Date: 2021-05-07
SHANGHAI TAIJIE CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, in existing engineering applications, after the commercially available polycarboxylate water reducer is added to precast concrete, the mineral components of the cement undergo a hydration reaction, and the polycarboxylate adsorbed on the surface of the cement particles through the carboxyl group The superplasticizer is gradually consumed, so its effectiveness cannot be fully exerted

Method used

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  • A kind of synthetic method of retarding polycarboxylate superplasticizer
  • A kind of synthetic method of retarding polycarboxylate superplasticizer

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preparation example Construction

[0023] In a preferred embodiment, the synthetic method of the retarded polycarboxylate water reducer comprises the following steps:

[0024] S1: Under the protection of nitrogen, add acrylamide or / and methacrylamide to the first reaction vessel, and add phosphorus trichloride, at a reaction temperature of 0°C to 10°C, stir mechanically, and react for 2 to 5 hours , for example according to the following reaction:

[0025]

[0026] (R is H or methyl); then, add polyhydric alcohol and further react for 2 to 5 hours to generate intermediate A;

[0027] S2: Add the intermediate A, alkali metal alcoholate (as a catalyst), and ethylene oxide or / and propylene oxide to the second reaction vessel (pressure reaction vessel), and react at 160°C to 195°C Under the temperature and reaction pressure of 1.8Mpa~3.6Mpa, anionic ring-opening polymerization reaction is carried out for 4~7 hours to generate multi-branched polyether containing hydrolyzable functional groups; among them, interm...

Embodiment 1

[0040] S1: Under the protection of nitrogen, add 2000g of acrylamide and 2000g of phosphorus trichloride to the first reaction vessel, and stir mechanically at 5°C for 4 hours; then, add 2200g of glycerol for further reaction for 3.5 hours, to generate intermediate A;

[0041] S2: Add 1000g of the intermediate A, 20g of sodium ethoxide, and 20kg of ethylene oxide into the second reaction vessel (pressure reaction vessel), and perform anionic ring-opening polymerization at a reaction temperature of 180°C and a reaction pressure of 1.8Mpa React for 5.5 hours to generate a multi-branched polyether containing hydrolyzable functional groups;

[0042] S3: Add 2000g of the multi-branched polyether containing hydrolyzable functional groups, 220g of acrylic acid and 25g of sodium persulfate to the third reaction vessel; carry out free radical copolymerization reaction at a reaction temperature of 70°C for 4.5 hours, after the reaction is complete , adding 35 wt% sodium hydroxide aqueo...

Embodiment 2

[0044]S1: Under the protection of nitrogen, add 1800g of acrylamide and 2000g of phosphorus trichloride to the first reaction vessel, and stir it mechanically at 5°C for 4 hours; then, add 3200g of butylene glycol for further reaction for 3 hours, to generate intermediate A;

[0045] S2: Add 1000g of the intermediate A, 25g of sodium ethoxide, and 25kg of propylene oxide to the second reaction vessel (pressure reaction vessel), and carry out anionic ring-opening polymerization at a reaction temperature of 175°C and a reaction pressure of 2.6Mpa After 5 hours, a multi-branched polyether containing hydrolyzable functional groups was generated;

[0046] S3: Add 2000 g of the multi-branched polyether containing hydrolyzable functional groups, 280 g of methacrylic acid and 35 g of potassium persulfate to the third reaction vessel; carry out free radical copolymerization reaction at a reaction temperature of 75° C. for 5 hours, and react After completion, add 35wt% sodium hydroxide...

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Abstract

The invention provides a synthetic method of retarding polycarboxylate superplasticizer, which mainly includes the following steps: S1: under the protection of nitrogen, add acrylamide or / and methacrylamide and phosphorus trichloride, at 0 ℃~10℃, react for 2~5 hours, then add polyol for further reaction to generate intermediate A; S2: add intermediate A, alcoholate of alkali metal, and ethylene oxide or / and propylene oxide , the reaction is complete to generate a multi-branched polyether containing a hydrolyzable functional group; S3: Adding a multi-branched polyether containing a hydrolyzable functional group, an unsaturated carboxylic acid and an initiator, a free radical copolymerization reaction occurs, and post-treatment is obtained Retarded polycarboxylate superplasticizer. The retarded polycarboxylate water-reducer prepared according to the synthesis method of the present invention has significantly better initial performance and time-lapse performance than commercially available common polycarboxylate water-reducers.

Description

technical field [0001] The invention belongs to the technical field of building admixtures, and in particular relates to a synthesis method of a retarding polycarboxylate water reducer. Background technique [0002] Polycarboxylate superplasticizer is currently the most widely used construction admixture and plays an irreplaceable role in various concrete construction projects. Generally, polycarboxylate water reducer is based on unsaturated carboxylic acid compound and unsaturated modified polyether (such as 2-propenyl polyethylene glycol ether, 2-methacryl polyethylene glycol ether, etc.) Glycol ether, 3-methyl-3-butenyl polyethylene glycol ether) carry out free radical copolymerization to synthesize product molecules with a comb structure. Polycarboxylate superplasticizer produces molecular thermodynamics and molecular dynamics properties through electrostatic repulsion and steric effects, so as to increase the dispersion of mixed concrete and prolong the setting time (e...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C04B24/26C08G65/28C08F283/06C08F220/06C04B103/30
CPCC04B24/2658C04B2103/302C08F283/065C08G65/2633C08F220/06
Inventor 朱伟亮王少峰
Owner SHANGHAI TAIJIE CHEM
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