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Method for synthesizing polycarboxylate superplasticizer through binary copolymerization of 6C polyether macromonomer under heterogeneous catalysis by cobalt oxide

A heterogeneous catalysis, polyether macromonomer technology, applied in the field of water reducing agent preparation, can solve problems such as increasing energy consumption, dispersing performance, insufficient slump retention performance, and reducing product market competitiveness.

Pending Publication Date: 2021-08-27
SICHUAN TONGZHOU CHEM TECH +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

In the process of free radical polymerization to prepare polycarboxylate superplasticizers, the activity of polyether macromonomers is much lower than that of small molecular unsaturated carboxylic acid monomers; Copolymerization can only prolong the dropping time of small molecular monomers, so the preparation time of polycarboxylate water reducer is generally more than 3 hours; use heating method to synthesize polycarboxylate water reducer, the polymerization reaction temperature is usually 40~60℃ , Higher temperature increases energy consumption and production cost, thereby reducing the market competitiveness of the product, and the dispersion performance and slump retention performance of the product are also insufficient

Method used

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  • Method for synthesizing polycarboxylate superplasticizer through binary copolymerization of 6C polyether macromonomer under heterogeneous catalysis by cobalt oxide
  • Method for synthesizing polycarboxylate superplasticizer through binary copolymerization of 6C polyether macromonomer under heterogeneous catalysis by cobalt oxide
  • Method for synthesizing polycarboxylate superplasticizer through binary copolymerization of 6C polyether macromonomer under heterogeneous catalysis by cobalt oxide

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Embodiment 1

[0049] A method for the cobalt oxide heterogeneously catalyzed binary copolymerization of a 6C polyether macromonomer into a polycarboxylate water reducer, the steps are: prepare A liquid (weigh 3.55 g of small monomer and 15.83 g of distilled water) and B liquid respectively solution (0.03g of ascorbic acid, 0.3g of thioglycolic acid and 18g of distilled water) for use, add 36g of macromonomer (i.e. diethylene glycol monovinyl ether, referred to as EPEG, the same hereinafter) and 15g of distilled water in a three-necked flask equipped with a thermometer , at room temperature, gradually lower the temperature and stir to dissolve. When the temperature is controlled to 2°C and the macromonomer is completely dissolved, add 0.01g of cobalt oxide and 5g of water, mix and stir for 10min, then add 0.15g of hydrogen peroxide and 0.5g of water, and mix well Finally, use a constant pressure dropping funnel to drop A solution (48min) and B solution (78min) at a constant speed at the same ...

Embodiment 2

[0051] A method for cobalt oxide heterogeneously catalyzed binary copolymerization of a 6C polyether macromonomer into a polycarboxylate water reducer, the steps are: prepare A liquid (weighing 3.4 g of small monomer and 16 g of distilled water) and B liquid respectively (ascorbic acid 0.02g, thioglycolic acid 0.1g and distilled water 19g) stand-by, in the there-necked flask that is equipped with thermometer, add macromonomer (EPEG) 35g and distilled water 16g, at room temperature, cool down gradually and stir to dissolve, treat that temperature controls to When the macromonomer is completely dissolved at 2°C, add 0.08g of cobalt oxide and 3g of water, mix and stir for 20 minutes, then add 0.25g of hydrogen peroxide and 0.5g of water, mix well, and add liquid A at a constant speed at the same time using a constant pressure dropping funnel ( 48min drop) and B solution (75min drop), the holding time is 0.5h, the material after the reaction is left to room temperature, and the cob...

Embodiment 3

[0053] A method for heterogeneously catalyzed two-component copolymerization of cobalt oxide of 6C polyether macromonomer into polycarboxylate water reducer, the steps are: prepare A liquid (weigh 3.3g of small monomer and 14g of distilled water) and B liquid respectively (ascorbic acid 0.03g, thioglycolic acid 0.2g and distilled water 18g) stand-by, in the there-necked flask that is equipped with thermometer, add macromonomer (EPEG) 34g and distilled water 15g, at room temperature, cool down gradually and stir to dissolve, treat that temperature controls to When the macromonomer is completely dissolved at 5°C, add 0.15g of cobalt oxide and 5g of water, mix and stir for 5 minutes, then add 0.35g of hydrogen peroxide and 0.5g of water, after mixing evenly, use a constant pressure dropping funnel to add liquid A at a constant speed at the same time ( 45min drop) and B solution (75min drop), the holding time is 0.5h, and the reacted material is allowed to stand to room temperature...

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Abstract

The invention discloses a method for synthesizing a polycarboxylate superplasticizer through binary copolymerization of 6C polyether macromonomer under heterogeneous catalysis by cobalt oxide. The method is characterized by comprising the following steps: weighing raw materials including a macromonomer, a small monomer, a chain transfer agent, a reducing agent, an oxidizing agent, a catalyst and water, mixing the small monomers and the water to prepare a solution A, and mixing the reducing agent, the chain transfer agent and the water to prepare a solution B, adding the solution C into the solution B, wherein the macromonomer is diethylene glycol monovinyl ether; and adding the macromonomer and the water into a reactor with a thermometer, controlling a temperature to be 0-20 DEG C, adding the catalyst and the water, conducting stirring and mixing, adding the oxidizing agent and the water, performing mixing and stirring, dropwise adding the solution A and the solution B at a constant speed at the same time, and carrying out a heat-preserved reaction, wherein the total time of dropwise addition and reaction is 1-2 hours. The polycarboxylate superplasticizer prepared through binary copolymerization of 6C polyether macromonomer under heterogeneous catalysis by cobalt oxide is especially suitable for concrete preparation, and has the advantages of excellent cement dispersion performance and aging slump retaining performance, good compressive strength and durability, and strong practicability.

Description

technical field [0001] The invention belongs to the preparation of water reducers, and relates to a method for heterogeneously catalyzed binary copolymerization of cobalt oxide of 6C polyether macromonomers into polycarboxylate water reducers. The cobalt oxide heterogeneously catalyzed binary copolymerization of the 6C polyether macromonomer (namely: diethylene glycol monovinyl ether) prepared by the invention is suitable for concrete preparation. Background technique [0002] The development of modern concrete admixture technology is the key to the development of modern concrete technology and plays a decisive role. Concrete admixture is an essential component in modern concrete except cement, sand, stone, water, and admixtures, especially the third-generation polycarboxylate high-performance admixture, which accounts for 10% of the amount of concrete admixture used. About 80%, it is one of the important technical ways to reduce the amount of cement, improve the utilizatio...

Claims

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Application Information

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IPC IPC(8): C08F283/06C08F220/06C08F4/40C04B24/26C04B103/30
CPCC08F283/065C08F4/40C04B24/2647C04B2103/302C08F220/06
Inventor 舒豆豆舒学军刘才林张恒通任先艳杨海君何年罗率
Owner SICHUAN TONGZHOU CHEM TECH
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