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Preparation method of polycarboxylic copolymer with high solid content

A technology of high solid content, polycarboxylic acid, applied in the field of preparation of high solid content polycarboxylate water reducing agent, can solve the problems of long production cycle and low production efficiency, and achieve lower product price, no formaldehyde content and low price Effect

Inactive Publication Date: 2012-08-08
SHANGHAI RES INST OF BUILDING SCI CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the traditional production process has a long production cycle, the solid content of the product is only about 20%, and the production efficiency is low

Method used

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  • Preparation method of polycarboxylic copolymer with high solid content

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] 1) Add 100 grams of methoxypolyethylene glycol with a molecular weight of 2000 in a reactor equipped with a stirring device, 0.04 grams of inhibitor hydroquinone, 7.2 grams of monomeric acrylic acid, 2 grams of catalyst concentrated sulfuric acid, and heat to 115° C., stirred and reacted for 5 hours to obtain an esterified liquid.

[0028] 2) Control the temperature to 80°C, add dropwise a mixed solution of 10.08 g of acrylic acid and 0.9 g of chain transfer agent mercaptoacetic acid in the esterification solution, and the dropwise addition time is 2 hours, while adding the initiator benzyl peroxide in batches Acyl 2.4 g. After keeping the temperature for 1 hour, add the aqueous solution of the initiator ammonium persulfate dropwise for 1 hour, the reaction temperature is 60°C, and keep the temperature for 1 hour.

Embodiment 2

[0030] 1) Add 100 grams of methoxypolyethylene glycol with a molecular weight of 2000 in a reactor equipped with a stirring device, 0.04 grams of inhibitor hydroquinone, 6.48 grams of monomeric acrylic acid, 2 grams of catalyst concentrated sulfuric acid, and heat to 115° C., stirred and reacted for 5 hours to obtain an esterified liquid.

[0031] 2) Control the temperature at 80°C, add dropwise a mixed solution of 10.08 grams of acrylic acid, 1.7 grams of hydroxyethyl acrylate and 0.9 grams of chain transfer agent mercaptoacetic acid in the esterification solution, and the dropping time is 2 hours. Add 2.4 grams of initiator benzoyl peroxide. After keeping warm for 1 hour, add the initiator ammonium persulfate aqueous solution dropwise for 1 hour, the reaction temperature is 60°C, and keep warm for 1 hour.

Embodiment 3

[0033] 1) in the reactor that stirring device is housed, adding molecular weight is 100 grams of methoxypolyethylene glycol of 2000, 0.04 grams of inhibitor hydroquinone, 9 grams of monomer acrylic acid, 1.5 grams of catalyzer p-toluenesulfonic acid, Heating to 115° C., stirring for 5 hours to obtain an esterification solution.

[0034] 2) Control the temperature at 80°C, add 14.7 grams of maleic anhydride, dropwise add a mixed solution of 2 grams of styrene and 0.7 grams of chain transfer agent mercaptoacetic acid, dropwise for 2 hours, and add esterification solution in batches while dropping And initiator benzoyl peroxide 1.8 grams, insulation 1 hour gets final product, and product is solid after cooling.

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Abstract

The invention discloses a preparation method of a polycarboxylic copolymer with high solid content. The preparation method comprises the following specific synthetic steps: sequentially adding methoxy polyethylene glycol, a polymerization inhibitor A, unsaturated carboxylic acid B and an esterification catalyst C into a reaction kettle; esterfying the mixture under the condition that the temperature is 110-120DEG C to synthesize a methoxy polyethylene glycol (methyl) acrylic ester macromonomer; removing the generated water in the reaction process; adding the prepared esterifying liquid into the reaction kettle; controlling the temperature at 70-80DEG C; dropping a mixed solution of an unsaturated monomer D and a chain transfer agent E by stirring for 1.5 to 2 hours; meanwhile, adding an initiator F in several times; after dropping, preserving the temperature for 1-2 hours; and finally, obtaining a product with the solid content of 100 percent. The polycarboxylic copolymer has the advantages that: firstly, the product is environment-friendly, dispenses with formaldehyde and three-waste discharge and belongs to low-alkali products; and secondly, compared with domestic like products, the polycarboxylic copolymer with the high solid content, which is disclosed by the invention, has high solid content and reduced cost in the production, transportation and storage process and reduced price of products.

Description

technical field [0001] The invention relates to a method for preparing a water reducer, in particular to a method for preparing a high solid content polycarboxylate water reducer. Background technique [0002] The use of concrete water reducing agent in concrete can significantly reduce the water consumption of concrete. According to the water-cement ratio law of concrete strength, the lower the water consumption, the higher the concrete strength. Another purpose is to keep the water consumption of single concrete constant, which can significantly improve the fluidity of fresh concrete to meet the pumping process requirements of modern concrete construction. Concrete water reducers have been used since the 1940s. The first generation product is lignosulfonate prepared from papermaking waste liquid. The second generation water reducer is naphthalene sulfonate formaldehyde condensate invented by Germany and Japan. Melamine sulfonated formaldehyde condensate, aliphatic sulfona...

Claims

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Application Information

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IPC IPC(8): C08F290/06C08F2/02C08F2/38C04B24/26C04B103/30
Inventor 朱玲丁志明周南南汪梁周普玉杨晓晨
Owner SHANGHAI RES INST OF BUILDING SCI CO LTD
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