Method for rapidly synthesizing polycarboxylic acid water reducers through microwaves and supersonic waves

A technology of ultrasonic wave and branched polycarboxylic acid, applied in the field of organic synthesis, can solve problems such as instability of the copolymer, and achieve the effects of inhibiting the hydration speed, shortening the reaction speed and reducing the production cost.

Inactive Publication Date: 2012-12-19
谢艾民
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the copolymerization reaction, there are problems such as the instability of the copolymer caused by the difficult control of the copolymerization process conditions

Method used

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  • Method for rapidly synthesizing polycarboxylic acid water reducers through microwaves and supersonic waves
  • Method for rapidly synthesizing polycarboxylic acid water reducers through microwaves and supersonic waves

Examples

Experimental program
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Effect test

Embodiment 1

[0021] Example 1: Microwave Ultrasonic Rapid Synthesis of Polycarboxylate Water Reducer

[0022] Be the polyethylene glycol 100.0g of molecular weight 1000, glucose 10.4g and maltose 9.8g, catalyzer p-toluenesulfonic acid 2.1g (1.5% of raw material gross mass), polymerization inhibitor Resorcinol 0.14g (raw raw material gross mass 0.1%) into a four-necked flask, place the reactor in a microwave and ultrasonic reactor, and irradiate the above mixture with 1000-2000W microwave ultrasonic waves. When the temperature rises to 80°C, add 21.6g of acrylic acid dropwise from a drop funnel, and take a sample after 20 minutes of reaction The measured esterification rate was 60.4%, and the reaction was stopped to obtain an esterified product.

[0023] Add 56.88g of sodium methpropylene sulfonate, 10.0g of chain transfer agent isopropanol and 225.84g of distilled water into the reactor, heat to 70°C, add dropwise the esterification product, 47.56g of acrylic acid, 7.37g of ammonium persul...

Embodiment 2

[0024] Example 2: Microwave Ultrasonic Rapid Synthesis of Polycarboxylate Water Reducer

[0025] Be the Polyethylene Glycol 100.0g of molecular weight 1000, glucose 5.0g and maltose 4.9g, catalyzer p-toluenesulfonic acid 2.0g (1.5% of raw material gross mass), polymerization inhibitor Resorcinol 0.13g (raw raw material gross mass 0.1%) into a four-necked flask, place the reactor in a microwave and ultrasonic reactor and irradiate the above-mentioned mixture with 1000-2000W microwave and ultrasonic waves to rapidly heat up to 80°C and add 16.21g of acrylic acid dropwise from a drop funnel. After 20 minutes of reaction, the esterification rate was measured to be 72.5% by sampling, and the reaction was stopped to obtain an esterified product.

[0026] Add 51.55g of sodium methacrylate sulfonate, 6.0g of chain transfer agent isopropanol and 204.14g of distilled water into the reactor, place the reactor in a microwave and ultrasonic reactor, and irradiate the above with 1000W-2000W...

Embodiment 3

[0027] Example 3: Microwave Ultrasonic Rapid Synthesis of Polycarboxylate Water Reducer

[0028] Be the polyethylene glycol 100.0g of molecular weight 1000, glucose 2.0g, maltose 2.98g, catalyzer p-toluenesulfonic acid 2.0g (1.5% of raw material gross mass), polymerization inhibitor Resorcinol 0.13g (raw raw material gross mass 0.1%) into a four-necked flask, place the reactor in a microwave and ultrasonic reactor, and irradiate the above mixture with 1000-2000W microwave and ultrasonic waves to rapidly heat up to 80°C. Add 13.53 g of acrylic acid dropwise from a drop funnel After 20 minutes of reaction, the esterification rate was measured by sampling to 80%, and the reaction was stopped to obtain an esterified product.

[0029] Add 47.48g of sodium methpropylene sulfonate, 6.0g of chain transfer agent isopropanol and 400.68g of distilled water into the reactor, place the reactor in a microwave and ultrasonic reactor, and use 1000W to 2000W microwave and ultrasonic radiation ...

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Abstract

A method for promoting the synthesis of polycarboxylic acid system cement water reducers through using microwaves and supersonic waves utilizes the microwaves to improve the temperature of reactants to make the interface temperature rapidly reach above 80DEG C. The reactants rapidly complete a reaction through stirring and vibrating reaction mediums by supersonic waves. The time for completing the reaction of the reactants is reduced to 10-30min under the radiation of the microwaves and the supersonic waves from original 5-10h. The method belongs to the organic synthesis field. In the invention, the relation between performance requirements of the cement water reducer and the monomer molecule structure activity is analyzed, and the monomer molecule structure selection and the monomer ration are optimized, so monosaccharide oligosaccharides comprising glucose and maltose, polyethylene glycol, hydroquinone, sodium methylbenzenesulfonate, methylpropylbenzene, sodium sulfonate, ammonium persulfate and sodium hypophosphite are selected. A microwave and supersonic wave technology is introduced on the basis of the adoption of the ammonium persulfate and the sodium hypophosphite as the initiators to rapidly synthesize polycarboxylic acid system water reducer products through utilizing the microwaves and the supersonic waves. The method provided by the invention has the advantages of substantial time shortening, energy consumption reduction, pollution reduction, and improvement of the paste fluidities of the products, is a new method having the characteristics of safety, high efficiency and energy saving, environmental protection and simple operation, and accords with the trend of times.

Description

Technical field: [0001] The invention discloses a method for synthesizing and promoting a polycarboxylate cement water reducer by using microwave ultrasonic waves, which belongs to the technical field of organic synthesis. Specifically, it uses ammonium persulfate and sodium hypophosphite as an initiator to combine the following three raw materials: ① monosaccharides and oligosaccharides; ② methoxypolyethylene glycol or polyethylene glycol; ③ unsaturated Carboxylic acid or unsaturated acid anhydride is added to the reactor, hydroquinone is used as a polymerization inhibitor, stirred and heated to 70-120°C for esterification reaction, polycarboxylic acid is synthesized under microwave and ultrasonic radiation, and after 20 minutes of reaction, samples are taken to measure grafting After reaching 40-90%, stop the reaction to obtain the esterification product. Background technique: [0002] Polycarboxylate cement superplasticizer is currently the most promising new generation ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C04B24/28C04B24/26C08F290/06C08F2/46C08F2/56C08G65/48
Inventor 谢艾民
Owner 谢艾民
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