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Preparation method of shrinkage-reducing macromonomer and shrinkage-reducing polycarboxylate superplasticizer

A macromonomer and water reducing agent technology, applied in the field of water reducing agent production, can solve the problems of weakening shrinkage reduction effect, reducing shrinkage and consumption of cement-based materials, reducing surface tension, reducing pore pressure, and improving durability and service life effects

Inactive Publication Date: 2021-04-02
北京金隅节能科技有限公司 +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002] The shrinkage reducing agent can effectively reduce the shrinkage of cement-based materials because it can reduce the surface tension of the cement pore solution, and has high use value. Polymerized on the main chain of the water reducing agent, the shrinkage reducing monomer will be consumed by cement hydration, and the shrinkage reducing effect will weaken with time. Therefore, it is necessary to study a shrinkage reducing agent with better time effect to meet people's needs. need

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0046] Embodiment 1, the preparation method of the reduction macromonomer in the present embodiment comprises the following steps:

[0047] S1. Under the action of toluenesulfonic acid, cyclohexane, and hydroquinone, acrylic acid and diethylene glycol monobutyl ether were subjected to esterification reaction at a constant temperature of 100°C for 4 hours, and the esterified small monomer A was obtained after vacuum distillation;

[0048] The mol ratio of described acrylic acid and diethylene glycol monobutyl ether is 2:1;

[0049] The quality of described toluenesulfonic acid is 1.5% of the total mass of acrylic acid and diethylene glycol monobutyl ether;

[0050] The cyclohexane quality is 20% of the total mass of acrylic acid and diethylene glycol monobutyl ether;

[0051] The quality of described hydroquinone is 0.05% of acrylic acid quality;

[0052] S2. Add aniline into the reaction kettle, raise the temperature to 50°C, add tert-butyl peroxybenzoate and stir for 10 minut...

Embodiment 2

[0078] Embodiment 2, the preparation method of the reduction macromonomer in the present embodiment may further comprise the steps:

[0079] S1. Under the action of phosphoric acid, benzene, and phenothiazine, the acid anhydride and ethylene glycol monobutyl ether were subjected to an esterification reaction at a constant temperature of 120°C for 5 hours, and the esterified small monomer A was obtained after vacuum distillation;

[0080] The mol ratio of described acid anhydride and small molecule ether monomer is 3:1;

[0081] The quality of described phosphoric acid is 3% of acid anhydride and ethylene glycol monobutyl ether gross mass;

[0082] The quality of described benzene is 30% of acid anhydride and ethylene glycol monobutyl ether gross mass;

[0083] The quality of described phenothiazine is 3% of acid anhydride quality;

[0084] S2. Add sulfolane into the reaction kettle, raise the temperature to 100°C, add azobisisobutyronitrile and stir for 20 minutes. After the...

Embodiment 3

[0110] Embodiment 3, the preparation method of the reduction macromonomer in the present embodiment, comprises the following steps:

[0111] S1. Under the action of sulfamic acid, toluene, and hydroquinone methyl ether, methacrylic acid and diethylene glycol ether were subjected to an esterification reaction at a constant temperature of 130°C for 7 hours, and the esterified small monomer A was obtained after vacuum distillation;

[0112] The mol ratio of described methacrylic acid and diethylene glycol ether is 5:1;

[0113] The quality of described sulfamic acid is 10% of the total mass of methacrylic acid and diethylene glycol ether;

[0114] The quality of described toluene is 50% of total mass after methacrylic acid and diethylene glycol ether mix;

[0115]The quality of described hydroquinone methyl ether is 5% of methacrylic acid quality;

[0116] S2. Add tetrahydrofuran into the reaction kettle, raise the temperature to 120°C, add dibenzoyl peroxide and stir for 30 mi...

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Abstract

The invention discloses a preparation method of a shrinkage-reducing macromonomer and a shrinkage-reducing polycarboxylate superplasticizer. The preparation method of the shrinkage-reducing macromonomer comprises the following steps: S1, reacting an unsaturated acid small monomer or anhydride with a small molecular ether monomer under the action of a first catalyst, a water-carrying agent and a polymerization inhibitor to obtain an esterified small monomer A; S2, adding an organic solvent into a reaction kettle, adding a first initiator, and dropwise adding a mixed solution of the esterified small monomer A and a terminal group functionalizing agent to obtain a self-polymerization product solution B; and S3, adding unsaturated halogenated hydrocarbon, an acid-binding agent and a second catalyst into the self-polymerization product solution B, and removing the organic solvent to obtain the shrinkage-reducing macromonomer. The preparation method of the shrinkage-reducing polycarboxylatesuperplasticizer comprises the following steps: S4, polymerizing a carboxylic acid small monomer aqueous solution, a shrinkage-reducing macromonomer and an unsaturated macromonomer for 4 hours to 7 hours under the action of an initiator aqueous solution and a chain transfer agent aqueous solution; and S5, adding solvent water to obtain the reduced polycarboxylate superplasticizer with different mass concentrations.

Description

technical field [0001] The invention relates to the field of water reducer production, in particular to a method for preparing a shrinkage-reducing macromonomer and a shrinkage-reducing polycarboxylate water reducer. Background technique [0002] The shrinkage reducing agent can effectively reduce the shrinkage of cement-based materials because it can reduce the surface tension of the cement pore solution, and has high use value. Polymerized on the main chain of the water reducing agent, the shrinkage reducing monomer will be consumed by the hydration of the cement, and the shrinkage reducing effect will weaken with time. Therefore, it is necessary to study a shrinkage reducing agent with better time effect to meet people's use need. Contents of the invention [0003] The object of the present invention is to solve the above problems and provide a method for preparing a shrinkage-reducing macromonomer and a shrinkage-reducing polycarboxylate water-reducer with good time e...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F283/06C08F222/02C08F273/00C04B24/16C04B103/30
CPCC08F283/065C08F273/00C04B24/165C04B2103/302C08F222/02
Inventor 王晓英马建峰杨文杰石龙飞罗紫隆张业明苏鹏举周钰沦黄天勇
Owner 北京金隅节能科技有限公司