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Solid polycarboxylate superplasticizer prepared by using supercritical CO2 as solvent as well as preparation method and application of solid polycarboxylate superplasticizer

A technology of polycarboxylate and water reducer, which is applied in the field of solid polycarboxylate water reducer and its preparation, can solve the problems of complex production process, use of organic solvents, high viscosity of materials, etc., achieve high reactivity, improve dispersion performance, The effect of uniform heat transfer performance

Pending Publication Date: 2022-01-28
CHINA BUILDING MATERIALS ACAD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] In view of this, the main purpose of the present invention is to provide a 2 Solid polycarboxylate water-reducer prepared as a solvent and its preparation method and application, which pass CO 2 The gas transforms into liquid CO under the condition that the temperature is higher than the critical temperature of 31.26°C and the pressure is higher than the critical pressure of 72.9 atm 2 , using supercritical CO 2 As a solvent, it solves the problems of high material viscosity, difficult heat dissipation, gelation, use of organic solvents, complex production process, high cost and other problems in the preparation process of traditional solid polycarboxylate water reducer, and CO 2 Can be changed between gas and liquid as needed, easy to recycle and reuse

Method used

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  • Solid polycarboxylate superplasticizer prepared by using supercritical CO2 as solvent as well as preparation method and application of solid polycarboxylate superplasticizer
  • Solid polycarboxylate superplasticizer prepared by using supercritical CO2 as solvent as well as preparation method and application of solid polycarboxylate superplasticizer
  • Solid polycarboxylate superplasticizer prepared by using supercritical CO2 as solvent as well as preparation method and application of solid polycarboxylate superplasticizer

Examples

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Effect test

Embodiment 1

[0053] This embodiment provides a method using supercritical CO 2 The method for preparing solid polycarboxylate water reducer for solvent comprises the following steps:

[0054] 1) Introduce CO into the reactor of supercritical fluid 2 Gas, control the pressure in the reactor to 10MPa to make it into supercritical CO 2 ;

[0055] 2) Add 100g of isopentenol polyoxyethylene ether macromonomer into the premelt kettle, heat and melt it into a liquid state, transfer the liquid polyether macromonomer to the reactor of supercritical fluid through a pressure pump, and then transfer it to the reactor of supercritical fluid Add 0.2g of ammonium persulfate, 13g of acrylic acid, and 0.5g of mercaptoethanol; heat up to 35°C while mechanically stirring, and keep CO 2 The fluid volume is 100mL, the control speed is 100rpm, and then keep warm for 2h;

[0056] 3) After the reaction is completed, open the pressure relief valve, drop 1g of neutralizing agent sodium hydroxide (solid) into th...

Embodiment 2

[0058] This embodiment provides a method using supercritical CO 2 The method for preparing solid polycarboxylate water reducer for solvent comprises the following steps:

[0059] 1) Introduce CO into the reactor of supercritical fluid 2 Gas, control the pressure in the reactor to 12MPa to make it into supercritical CO 2 ;

[0060] 2) Add 120g of methallyl polyoxyethylene ether macromonomer into the pre-melting kettle, after heating and melting into a liquid state, the liquid polyether macromonomer is transferred to the reaction kettle of supercritical fluid by a pressure pump, and then Add 0.36g dicyclohexyl peroxydicarbonate, 18g methacrylic acid, 0.72g mercaptoacetic acid; heat up to 40°C while stirring mechanically, keep CO 2 The fluid volume is 140mL, the speed is controlled at 150rpm, and then the reaction is kept for 3h;

[0061] 3) After the reaction is completed, open the pressure relief valve, drop into 1.2g neutralizing agent potassium hydroxide (solid) in the re...

Embodiment 3

[0063] This embodiment provides a method using supercritical CO 2 The method for preparing solid polycarboxylate water reducer for solvent comprises the following steps:

[0064] 1) Introduce CO into the reactor of supercritical fluid 2 Gas, control the pressure in the reactor to 15MPa, make it into supercritical CO 2 ;

[0065] 2) Add 150g of vinyl glycol ether-based polyoxyethylene ether macromonomer into the pre-melting kettle, heat and melt it into a liquid state, and transfer the liquid polyether macromonomer to the supercritical fluid reaction kettle through a pressure pump , and then add 0.6g of azobisisobutyronitrile, 27g of acrylamide, 1.0g of mercaptopropionic acid; while stirring mechanically, the temperature is raised to 45°C, and the CO 2 The fluid volume is 300mL, the speed is controlled at 200rpm, and then the reaction is kept for 4h;

[0066] 3) After the reaction is completed, open the pressure relief valve, drop into 2.25g neutralizing agent sodium hydrox...

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Abstract

The invention relates to a solid polycarboxylate superplasticizer prepared by using supercritical CO2 as a solvent as well as a preparation method and application of the solid polycarboxylate superplasticizer. The method comprises the following steps: converting CO2 gas into supercritical CO2 under 10-30 Mpa; heating and melting an unsaturated polyether macromonomer into a liquid state, transferring the liquid state macromonomer into supercritical CO2, adding an initiator, an unsaturated acid or anhydride small monomer and a molecular weight regulator into the liquid state, heating to 35-80 DEG C while stirring, controlling the rotating speed to be 100-400rpm, and carrying out heat preservation reaction for 2-6 hours; after the reaction is finished, releasing the pressure, adding a neutralizer into the mixture, introducing CO2 gas, uniformly stirring, and adjusting the pH value of the mixed solution to 5.0-7.0; and releasing the pressure again, cooling to room temperature, and slicing or grinding to obtain the solid polycarboxylate superplasticizer. According to the invention, the supercritical CO2 fluid is used as a reaction medium, toxic and harmful organic solvents are not used, the synthesis process is simple and convenient, the cost is reduced, and the problems of high material viscosity, difficult heat dissipation and gelation in the preparation process of the traditional solid polycarboxylate superplasticizer are effectively solved.

Description

technical field [0001] The invention relates to the technical field of mortar or concrete admixture, in particular to a 2 A solid polycarboxylate water reducer prepared as a solvent, a preparation method and application thereof. Background technique [0002] Polycarboxylate superplasticizer is an indispensable fifth component in the preparation of mortar or cement concrete. It has small dosage, high water reducing rate, good slump retention performance and moderate air-entraining performance. It is very suitable for preparing high-strength, large-scale Fluid, self-compacting concrete has been widely used in the field of concrete engineering technology. At present, most of the widely used polycarboxylate superplasticizers are liquid products with a concentration of 10% to 40%. Due to the remote distance of some construction sites, the cost of transportation of low-concentration polycarboxylate superplasticizers is high, so the development of solid polycarboxylate superplasti...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F283/06C08F220/06C08F220/56C08F220/58C04B24/26C04B24/16C04B103/30
CPCC08F283/065C04B24/165C04B24/2647C04B24/2694C04B2103/302C08F220/06C08F220/56C08F220/585Y02P20/54
Inventor 高瑞军黄韵蓓郭君华王宏霞高春勇
Owner CHINA BUILDING MATERIALS ACAD
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