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Preparation method of esters retarding polycarboxylic acid slump retaining agent

A technology of retarding polycarboxylic acid and slump-retaining agent, which is applied in the field of building materials, can solve problems such as not very satisfactory compatibility, long concrete setting time, abnormal concrete performance, etc. Easy to delay bleeding, good effect

Active Publication Date: 2016-01-20
KZJ NEW MATERIALS GROUP CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The compatibility of these additives in the admixture is not very ideal, and often there will be abnormal concrete properties caused by poor compatibility, such as: due to the poor compatibility of the retarder in the admixture, the retarder will be in the admixture The content of the bottom layer of the primer is too high. If you don’t notice it when you use it, the use of admixtures that exceed the standard of the bottom layer retarder will make the concrete set for a long time or even not set, which will bring hidden dangers to engineering applications.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] (1) Mix 52.00g of methacrylic acid, 360.00g of methoxypolyethylene glycol with a molecular weight of 1200, 20.00g of 2-hydroxyphosphonoacetic acid and 8.00g of phenothiazine, heat up to 60°C under nitrogen protection, and add 6.70g of p-toluenesulfonic acid, heat up to 115°C, keep warm for 2 hours, remove water by vacuuming or blowing nitrogen with water during the period, cool down to room temperature after the reaction, and obtain methoxypolyethylene glycol methacrylate , a first mixture of 2-hydroxyphosphonoacetate methacrylate and unreacted methacrylic acid;

[0029] (2) Mix 200.00 g of the first mixture prepared in step (1) with 40.00 g of hydroxyethyl methacrylate to obtain a comonomer mixture solution;

[0030] (3) The above-mentioned comonomer mixture solution, ammonium persulfate aqueous solution (wherein, ammonium persulfate 4.50g, water 30.00g), thioglycolic acid aqueous solution (wherein, thioglycolic acid 1.50g, water 30.00g) are dripped into 100.00g water ...

Embodiment 2

[0033] (1) 60.00g of acrylic acid, 180.00g of methoxypolyethylene glycol with a molecular weight of 600, 240.00g of methoxypolyethylene glycol polypropylene glycol copolymer with a molecular weight of 1200, 20.00g of 2-hydroxyphosphonoacetic acid and 3.00g of Mix hydroquinone and 2.00g of phenothiazine, under the protection of nitrogen, heat up to 50°C, add 10.20g of concentrated sulfuric acid with a mass fraction of 98%, heat up to 110°C, keep warm for 3 hours, during which time vacuum or nitrogen The water-carrying method is used to remove water, and after the reaction is completed, it is cooled to room temperature to obtain the first mixture containing methoxypolyethylene glycol acrylate, 2-hydroxyphosphonoacetate and unreacted acrylic acid;

[0034] (2) 150.00 g of the first mixture prepared in step (1) was mixed with 27.00 g of hydroxyethyl acrylate to obtain a comonomer mixture solution;

[0035] (3) The above-mentioned comonomer mixture solution and potassium persulfate...

Embodiment 3

[0038] (1) 55.00g of maleic anhydride, 154.00g of methoxypolyethylene glycol with a molecular weight of 2400, 120g of ethoxypolyethylene glycol with a molecular weight of 1200, 20.00g of hydroxyethylidene diphosphonic acid and 3.50g of p-phenylene Mix diphenols, under the protection of nitrogen, heat up to 60°C, add 5.50g ethylsulfonic acid, heat up to 110°C, keep warm for 3 hours, remove water by vacuuming or blowing nitrogen with water during the reaction, and drop to At room temperature, the first mixture containing maleic anhydride methoxypolyethylene glycol ester, maleic anhydride and hydroxyethylidene diphosphonate and unreacted maleic anhydride is obtained;

[0039] (2) 150.00 g of the first mixture prepared in step (1) was mixed with 19.00 g of hydroxyethyl acrylate to obtain a comonomer mixture solution;

[0040] (3) Mix the above comonomer mixture solution with hydrogen peroxide aqueous solution (wherein, hydrogen peroxide 1.20g, water 20.00g), ascorbic acid aqueous ...

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PUM

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Abstract

The invention discloses a preparation method of an esters retarding polycarbocylic acid slump retaining agent. The method comprises the following steps that 1, unsaturated carboxylic acid and / or anhydride, alkoxy poly alkylene glycol, hydroxy ethidene diphosphonic acid and / or 2-hydroxyphosphonoacetic acid and polymerization inhibitor are mixed, under the protection of nitrogen, the temperature is increased to range from 40 DEG C to 60 DEG C, a catalyst is added, the temperature is increased to 100-140 DEG C, thermal reaction is conducted for 0.5-3 h, water is removed during the reaction, after reaction is finished, the temperature is cooled to room temperature, and a first mixture is obtained; 2, the first mixture and unsaturated carboxylic acid hydroxyl esters are mixed, 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 in water to conduct reaction, and a copolymer product is obtained; 4, pH of the copolymer product is adjusted to 5-7 through alkali, and the esters retarding polycarbocylic acid slump retaining agent is obtained. According to the preparation method of the esters retarding polycarbocylic acid slump retaining agent, a structure of the hydroxy ethidene diphosphonic acid and / or the 2-hydroxyphosphonoacetic acid is introduced into the esters polycarbocylic acid slump retaining agent, and a finally obtained product has the effects of retardation and slump retaining.

Description

technical field [0001] The invention belongs to the technical field of building materials, and in particular relates to a preparation method of an ester retarding polycarboxylate slump retaining agent. Background technique [0002] In recent years, due to changes in concrete raw materials, problems such as rapid loss of concrete slump, poor workability, and delayed bleeding have become more and more prominent. However, most of these slump-preventing agents are ether-based polycarboxylic acid-based slump-preserving agents, which often have problems such as poor workability and delayed bleeding in practical applications. In summer, in order to make the concrete meet the construction requirements, it is often necessary to compound slump retaining agent and retarder in the water reducer to obtain suitable slump retention and setting time, and in order to solve the problem of poor workability and delayed bleeding For water problems, it is often necessary to compound a certain am...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F290/04C08F220/28C08F230/02C04B24/26
Inventor 蒋卓君方云辉官梦芹钟丽娜陈小路代柱端
Owner KZJ NEW MATERIALS GROUP CO LTD
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