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Method for synthesizing solid polyacrylic-series water reducing agents by aid of microwaves at one step

A technology of polyacrylic acid and water-reducing agent, applied in the field of polycarboxylate water-reducing agent for concrete, can solve the problems of increasing environmental burden, unfavorable industrial production, poor reaction repeatability, etc., achieving easy control of process parameters, reducing production energy consumption, The effect of short reaction time

Inactive Publication Date: 2015-06-24
WUHAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method can obtain solid polycarboxylate superplasticizers with high solid content, but has the following defects: 1. Organic solvents are used in the reaction process, which increases the burden on the environment; 2. Polycarboxylate superplasticizers must be neutralized by alkali , centrifugation and other steps to obtain solid products, the process is complicated and not conducive to industrial production
Secondly, the polyethers used in this patent are isopentenyl alcohol polyoxyethylene ether, isobutenyl alcohol polyoxyethylene ether and allyl alcohol polyoxyethylene ether. Most of the currently commercially available polyethers are solid at room temperature. In this patent It is difficult to mix it into a uniform paste under the ratio of raw materials. Spreading this unevenly mixed paste raw material on a flat plate without stirring during the reaction will lead to different batches of reactions. Poor repeatability, not conducive to industrial production

Method used

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  • Method for synthesizing solid polyacrylic-series water reducing agents by aid of microwaves at one step
  • Method for synthesizing solid polyacrylic-series water reducing agents by aid of microwaves at one step

Examples

Experimental program
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Effect test

Embodiment 1

[0023] First, 200g of allyl polyoxyethylene ether (molecular weight: 1200) is added to the microwave reactor, and at a temperature of 35°C, a microwave frequency of 915MHz, and a microwave radiation power of 100W, the allyl polyoxyethylene ether is After liquid state, 5g of sodium methacrylate, 23.5g of acrylic acid, and 5.5g of azobisisoheptanonitrile were successively added into the microwave reactor under stirring. After the feeding is completed, under the action of a temperature of 70°C and a microwave radiation power of 100W, copolymerize for 20 minutes, stop the reaction, and obtain 234g of a pure solid reaction product, and finally add 351g of water to dilute to obtain a polyacrylic acid-based water reducer with a concentration of 40%.

Embodiment 2

[0025] First, 200g of methallyl polyoxyethylene ether (molecular weight: 2400) is added to the microwave reactor, and at a temperature of 35°C and a microwave radiation power of 100W, the methallyl polyoxyethylene ether is in a liquid state. Finally, under stirring, 2.25g of mercaptopropionic acid, 25g of acrylic acid, and 3.5g of dibenzoyl peroxide were added to the microwave reactor successively. After the feeding is completed, at a temperature of 70°C, a microwave frequency of 2450MHz, and a microwave radiation power of 500W, copolymerize for 20 minutes, stop the reaction, and obtain 230.75g of a pure solid reaction product, and finally add 346.1g of water to dilute to obtain a concentration of 40%. Polyacrylic acid water reducer.

Embodiment 3

[0027] First, 200g of methallyl polyoxyethylene ether (molecular weight: 2400) is added to the microwave reactor, and at a temperature of 35°C and a microwave radiation power of 100W, the methallyl polyoxyethylene ether is in a liquid state. Finally, under stirring, 2.25g of mercaptopropionic acid, 25g of acrylic acid, and 3.5g of dibenzoyl peroxide were added to the microwave reactor successively. After the feeding is completed, the temperature is 60°C, the microwave frequency is 2450MHz, and the microwave radiation power is 1000W, and the copolymerization is carried out for 20 minutes, and the reaction is stopped to obtain 230.75g of a pure solid reaction product, and finally add 346.1g of water to dilute to obtain a concentration of 40%. Polyacrylic water reducer.

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Abstract

The invention provides a method for synthesizing solid polyacrylic-series water reducing agents by the aid of microwaves at one step. The method includes adding unsaturated polyoxyethylene ether into a reactor with a stirring device; melting the unsaturated polyoxyethylene ether under microwave conditions, then sequentially adding chain transfer agents, unsaturated carboxylic acid and initiators into the reactor; stirring the unsaturated polyoxyethylene ether, the chain transfer agents, the unsaturated carboxylic acid and the initiators at the temperatures of 20-70 DEG C for 10-30min, and then stopping the polyoxyethylene ether, the chain transfer agents, the unsaturated carboxylic acid and the initiators from reacting with one another; cooling reaction products of the polyoxyethylene ether, the chain transfer agents, the unsaturated carboxylic acid and the initiators until the temperatures of the reaction products reach the room temperature so as to obtain the solid polyacrylic-series water reducing agents. The method has the advantages that microwave equipment with a stirring function is utilized in procedures for preparing the solid polyacrylic-series water reducing agents, so that various materials which participate in reaction can be uniformly mixed with one another without water or other organic solvents, and can completely react with one another, and the solid polyacrylic-series water reducing agents with excellent performance and the content nearly equal to 100% can be obtained under the conditions of specific microwave reaction frequencies, reaction power and reaction time.

Description

technical field [0001] The invention belongs to the technical field of polycarboxylate water reducer for concrete, and in particular relates to a method for one-step synthesis of solid polyacrylic acid water reducer by using microwaves. Background technique [0002] Polyacrylic acid-based water reducer has become one of the necessary components of concrete because of its high water-reducing rate and excellent slump retention. However, the current polyacrylic acid-based water-reducer is usually an aqueous solution with a content of 10% to 50%. The content of active ingredients is low. On the one hand, this polyacrylic acid water reducer in the form of aqueous solution will greatly increase the transportation cost. On the other hand, it also limits its application in dry powder mortar and narrows the application range of polyacrylic acid water reducer. [0003] Patent CN1919772A reports a preparation method of powder polycarboxylate water reducer, which obtains polycarboxylate...

Claims

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Application Information

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IPC IPC(8): C08F283/06C08F290/06C08F220/06C08F2/38C04B24/26C04B103/30
Inventor 雷家珩陈刚汪海林杜小弟
Owner WUHAN UNIV OF TECH
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