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Preparation method of micro-crosslinked powdery polycarboxylate superplasticizer

A micro-crosslinking, polycarboxylic acid technology, applied in the field of building admixtures, can solve the problems of wide molecular weight distribution of products, difficult to control synthesis process, quality decline, etc., achieve excellent water reducing performance and slump retention performance, overcome the wide molecular weight distribution , the effect of reducing product cost

Active Publication Date: 2020-01-03
KZJ NEW MATERIALS GROUP CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the solid polycarboxylate superplasticizer obtained by spray drying technology is affected by high temperature, and the molecules undergo a chain transfer reaction, which is partially converted into a high molecular weight polymer, resulting in a decline in its quality, and even agglomeration during the production process; bulk polymerization Obtain solid polycarboxylate water reducer, the synthesis process is not easy to control, the molecular weight distribution of the product is wide, and the product performance is not good

Method used

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  • Preparation method of micro-crosslinked powdery polycarboxylate superplasticizer

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] (1) Preparation of micro-crosslinked macromonomer: Add 100g of polyetheramine with a molecular weight of 3000, 10g of crotonic acid, 1g of phenothiazine and 2g of concentrated sulfuric acid into the reaction kettle, heat up to 75°C, keep the temperature for 5h, and react The process removes the water formed.

[0027] (2) Preparation of molecular weight regulator: 100g of sodium hypophosphite, 50g of isobutylene alcohol polyoxyethylene ether with a molecular weight of 500, and 100g of water were added to the reaction kettle, the temperature was raised to 75°C, and 1.5g of hydrogen peroxide was added dropwise within 0.5h. After the addition, keep warm for 0.5h, then evaporate the reaction solution to dryness, add 220g of absolute ethanol, and stir the suspension at room temperature for 0.4h, then filter, and vacuum-dry the filter cake to obtain a molecular weight modifier.

[0028] (3) Bulk polymerization: 100g tetrahydrofuran-propylene oxide copolymerized glycol and acry...

Embodiment 2

[0031] (1) Preparation of micro-crosslinked macromonomer: 100 g of polyetheramine with a molecular weight of 3500, 15 g of itaconic acid, 5 g of hydroquinone and 2 g of concentrated phosphoric acid were added to the reactor, the temperature was raised to 80 ° C, and the reaction was kept for 4 hours. The water formed is removed during the reaction.

[0032] (2) Preparation of molecular weight regulator: 100g of sodium hypophosphite, 65g of isobutylene alcohol polyoxyethylene ether with a molecular weight of 700, and 100g of water were added to the reaction kettle, the temperature was raised to 77°C, and 1.5g of hydrogen peroxide was added dropwise within 0.5h. After the addition, keep warm for 1 h, then evaporate the reaction solution to dryness, add 300 g of absolute ethanol, and stir the suspension at room temperature for 0.5 h, then filter, and vacuum-dry the filter cake to obtain a molecular weight modifier.

[0033] (3) Bulk polymerization: the molecular weight prepared b...

Embodiment 3

[0036] (1) Preparation of micro-crosslinked macromonomer: Add 100g of polyetheramine with a molecular weight of 4000, 30g of itaconic acid, 5g of hydroquinone and 3g of concentrated sulfuric acid into the reactor, heat up to 100°C, and keep the temperature for 3h. The water formed is removed during the reaction.

[0037] (2) Preparation of molecular weight regulator: Add 100g of sodium hypophosphite, 70g of isobutylene alcohol polyoxyethylene ether with a molecular weight of 800, and 100g of water into the reaction kettle, raise the temperature to 80°C, drop 2g of hydrogen peroxide in 0.5h, and drop After completion, keep warm for 0.5h, then evaporate the reaction solution to dryness, add 400g of absolute ethanol, and stir the suspension at room temperature for 0.6h, then filter, and vacuum-dry the filter cake to obtain a molecular weight modifier.

[0038] (3) Bulk polymerization reaction: adjust the molecular weight of 100g tetrahydrofuran-propylene oxide copolymerized glyco...

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Abstract

The invention discloses a preparation method of a micro-crosslinked powdery polycarboxylate superplasticizer. The preparation method comprises the following steps: (1) preparing a micro-crosslinked macromonomer; (2) preparing a molecular weight regulator; (3) carrying out a bulk polymerization reaction; and (4) carrying out cooling and slicing. The product disclosed by the invention is powdery, sothat the cost in production, transportation and storage processes is reduced, and the cost of the product is reduced; and a kneading machine is used for bulk polymerization, so that the problems of high reactant viscosity as well as stirring and heat radiation difficulty in a bulk polymerization process of the polycarboxylate superplasticizer are overcome.

Description

technical field [0001] The invention belongs to the technical field of building admixtures, and in particular relates to a preparation method of a micro-crosslinked powder polycarboxylate water reducer. Background technique [0002] my country's research on polycarboxylate superplasticizers began in 2000, significantly later than Japan, Europe and the United States and other countries. However, around 2007, the domestic polycarboxylate superplasticizer technology developed rapidly, and the polycarboxylate superplasticizer industry showed a rapid development trend, and there was a gap with foreign advanced countries in terms of admixture varieties, application technology and theoretical research. is shrinking. Polycarboxylate superplasticizer has the advantages of low dosage, high water reducing rate, good slump retention, strong molecular structure design, and environmental protection. It has become the most important product in the concrete admixture market. [0003] The ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F283/06C08F220/06C08F220/28C08F2/38C08F2/02C04B24/26C04B24/16C04B103/30
CPCC04B24/165C04B24/2694C04B2103/302C08F2/02C08F2/38C08F220/20C08F283/065C08F220/06C04B24/16C04B24/26C04B24/28C08F222/02C08F283/06C08G65/00
Inventor 林艳梅方云辉柯余良李格丽庄博翔赖华珍张小芳钟丽娜赖广兴
Owner KZJ NEW MATERIALS GROUP CO LTD