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Synthesis method of polycarboxylate superplasticizer by taking polyether macromonomer as raw material

A technology of polyether macromonomer and synthesis method, which is applied in the synthesis of polycarboxylate water reducer and the synthesis field of polycarboxylate water reducer. Problems such as high heat release rate can achieve the effect of improving frost resistance and early strength performance

Pending Publication Date: 2022-01-07
江苏金木土科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the polymerization reaction reported in the literature and patents generally starts at a low temperature of about 5-15°C. Further, the dropwise addition time of the unsaturated acid is short, resulting in a large heat release rate during the polymerization reaction, requiring special cooling means Controlling the temperature of the polymerization process
In the stage of industrial mass production, the polymerization equipment should not be too large, and technical thresholds such as special refrigeration units need to be equipped, which limits the promotion and application of this type of polyether macromonomer in small and medium-sized water reducer manufacturers.

Method used

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  • Synthesis method of polycarboxylate superplasticizer by taking polyether macromonomer as raw material

Examples

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preparation example Construction

[0031] A kind of synthetic method of the polycarboxylate water-reducer taking polyether macromonomer as raw material, comprises the following steps,

[0032] S1. Preparation of dripping liquid: prepare unsaturated carboxylic acid, freezing point lowering additive, water, and cooling agent into dripping liquid A according to a certain mass ratio; chain transfer agent, reducing agent, freezing point lowering additive, water, and cooling agent The mass ratio is prepared into dripping solution B;

[0033] The consumption of freezing point depressing additive and cooling agent is the same in the above-mentioned dripping solution A and dripping solution B preparation process, and the mass ratio of described unsaturated carboxylic acid and the polyether macromonomer containing terminal ethyleneoxy structure is 1:(5 ~10), the prepared water reducer has better performance characteristics.

[0034]The consumption ratio of each substance in the preparation process of the dripping soluti...

Embodiment 1

[0049] Dropping solution A: Weigh 20.0 parts of acrylic acid, add 33.1 parts of water, stir well, add 1.14 parts of sodium nitrate as a freezing point lowering additive, and 2.86 parts of cooling agent ice cubes, fully stir and dissolve, and the preparation of dropping solution A is completed;

[0050] Dropping solution B: Weigh 0.24 parts of mercaptopropionic acid and 0.12 parts of L-ascorbic acid, add water and dilute to an aqueous solution with a mass concentration of 2%. Add 1.14 parts of sodium nitrate additive for lowering the freezing point, 2.86 parts of ice cubes for cooling agent, fully stir and dissolve, and the preparation of dripping liquid B is completed;

[0051] Weigh 100 parts of EPEG-5000 polyether macromonomer in a reaction device, add 150 parts of water, and prepare an aqueous solution with a mass concentration of 40%. Weigh 0.60 parts of 30% solid-containing hydrogen peroxide and add it to the reaction device, and the preparation of the primer solution is ...

Embodiment 2

[0053] Dropping solution A: Weigh 9.3 parts of methacrylic acid, 5.0 parts of itaconic anhydride, add 16.1 parts of water, stir well, add 1.79 parts of calcium nitrite for lowering the freezing point, and 3.56 parts of ammonium nitrate as a cooling agent, fully stir to dissolve, drop The preparation of liquid A is completed;

[0054] Dropping solution B: Weigh 0.91 part of thioglycolic acid and 0.34 part of white block, add water and dilute to an aqueous solution with a mass concentration of 5%. Add 1.79 parts of calcium nitrite to lower the freezing point additive, 3.56 parts of ammonium nitrate as a cooling agent, fully stir and dissolve, and the preparation of dripping liquid B is completed;

[0055] Weigh 100 parts of VPEG-3000 polyether macromonomer in a reaction device, add 66.7 parts of water, and prepare an aqueous solution with a mass concentration of 60%. Weigh 0.91 parts of sodium persulfate and add it to the reaction device, and the preparation of the primer solut...

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Abstract

The invention discloses a synthesis method of a polycarboxylate superplasticizer by taking a polyether macromonomer as a raw material. The synthesis method comprises the following steps: using unsaturated carboxylic acid, a freezing point reducing additive, water and a cooling agent into a dropwise adding solution A according to a certain mass ratio; preparing a dropwise adding solution B from a chain transfer agent, a reducing agent, a freezing point reducing additive, water and a cooling agent according to a certain mass ratio; adding a polyether macromonomer containing a vinyloxy-terminated structure, an oxidant and water into a reaction device according to a certain mass, and conducting stirring for a certain time to prepare a bottoming solution; and dropwise adding the dropwise adding solution A and the dropwise adding solution B into the bottoming solution of the reaction device within a certain time, and continuously conducting reacting for 30-60 minutes after the dropwise adding is finished, so as to obtain a polycarboxylate superplasticizer finished product. According to the preparation method of the polycarboxylate superplasticizer, existing synthesis equipment does not need to be modified, a refrigerating unit does not need to be added, a freezing point reducing additive and a cooling agent are added, the polymerization reaction is continuously cooled through dropwise adding liquid, and the effect of polymerizing the polycarboxylate superplasticizer at the reduced temperature is achieved.

Description

technical field [0001] The invention relates to a method for synthesizing a polycarboxylate water-reducer, in particular to a method for synthesizing a polycarboxylate water-reducer with polyether macromonomer as a raw material, and belongs to the field of concrete admixture applications. Background technique [0002] Polycarboxylate superplasticizer belongs to the third generation of high-performance superplasticizer, which is synthesized by free radical polymerization of acrylic monomer and polyether macromonomer in water phase. The molecular structure of polycarboxylate superplasticizer is comb-shaped, the main chain is grafted with carboxylic acid adsorption groups, and the side chain is a polyether segment with a certain molecular weight. Low, high water reducing rate, good fluidity retention ability and other performance advantages. [0003] Polyether macromonomers commonly used in the synthesis of polycarboxylate superplasticizers are allyl polyethylene glycol ether ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F283/06C08F220/06C08F222/04C08F222/02C08F220/20C04B24/26C04B103/30
CPCC08F283/065C04B24/2605C04B24/2694C04B2103/302C08F220/06C08F222/04C08F222/02C08F220/20
Inventor 范士敏刘江张磊牟忠江王国锋王碧涛
Owner 江苏金木土科技有限公司
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