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Method for preparing powdered polycarboxylic acid water reducer by adopting ultrasonics in bulk polymerization

A bulk polymerization and ultrasonic technology, applied in the field of preparation of polycarboxylate water reducer, can solve the problems of affecting the initiation efficiency of the initiator, long synthesis time, difficulty in heat dissipation, etc., achieve good water reducing rate and retention, and improve the efficiency of large orders. Volume conversion rate, safe and reliable effect of the preparation process

Inactive Publication Date: 2019-07-09
刘翠芬
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method avoids post-treatment processes such as high-temperature spray drying or solvent separation, but there are some problems in the whole reaction itself due to the absence of solvent in bulk polymerization. As a result, the mass transfer efficiency is affected, so its synthesis time is generally longer. On the other hand, in bulk polymerization, as the reaction time is prolonged, the viscosity of the entire product system will rise sharply, thereby affecting the initiation efficiency of the initiator in the product system. Therefore, the conversion rate of the product in bulk polymerization is usually not too high, and due to the high viscosity of the product, it will also cause difficulty in heat dissipation during the reaction process, and the temperature of the reaction system will increase, which will reduce the controllability of the entire reaction process.
[0005] The above technologies have not given specific instructions on how to make the method of preparing powder polycarboxylate water reducer in bulk polymerization short, the production cost is low, the conversion rate of macromonomer is high, the preparation process is safe and reliable, and it is environmentally friendly. mentoring program

Method used

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  • Method for preparing powdered polycarboxylic acid water reducer by adopting ultrasonics in bulk polymerization
  • Method for preparing powdered polycarboxylic acid water reducer by adopting ultrasonics in bulk polymerization
  • Method for preparing powdered polycarboxylic acid water reducer by adopting ultrasonics in bulk polymerization

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] Example 1: For the method of preparing powder polycarboxylate water reducer by ultrasonic wave in the bulk polymerization, the polycarboxylate water reducer is made of the following components and raw materials in parts by mass: 85 parts of allyl polyoxyethylene ether (TPEG, molecular weight 2400) macromonomer, 20.1 parts of acrylic acid, 0.2 part of azobisisobutyronitrile as an initiator, and 0.1 part of thioglycolic acid as a chain transfer agent; It is ultrasonic wave of 600W. The method for preparing powder polycarboxylate water reducer by ultrasonic wave in the bulk polymerization includes the following process steps: 1. put 85 parts of methallyl polyoxyethylene ether (TPEG) macromonomer into the reactor in parts by mass , use ultrasonic heating with a power of 600W (heating in an ultrasonic wave with a power of 600W) to raise the temperature to 65°C and start stirring to melt it; ② (simultaneously) mix 20.1 parts of acrylic acid and 0.1 parts of chain transfer age...

Embodiment 2

[0016]Example 2: For the method of preparing powder polycarboxylate water reducer by ultrasonic waves in the bulk polymerization, the polycarboxylate water reducer is made of the following components and raw materials in parts by mass: 120 parts of allyl polyoxyethylene ether (TPEG, molecular weight 2400) macromonomer, 25.3 parts of acrylic acid, 1.5 parts of initiator i.e. azodiisopropylimidazoline hydrochloride, 1.6 parts of chain transfer agent i.e. thioglycolic acid ; The ultrasonic wave used is an ultrasonic wave with a power of 800W. The method for preparing powder polycarboxylate water reducer by ultrasonic wave in the bulk polymerization includes the following process steps: 1. put 120 parts of methallyl polyoxyethylene ether (TPEG) macromonomer into the reactor in parts by mass In the process, heat up to 70°C with an ultrasonic power of 800W and start stirring to melt it; ②Mix 25.3 parts of acrylic acid and 1.6 parts of chain transfer agent, and stir well to obtain li...

Embodiment 3

[0017] Example 3: For the method of preparing powder polycarboxylate water reducer by ultrasonic waves in the bulk polymerization, the polycarboxylate water reducer is made of the following components and raw materials in parts by mass: 150 parts of allyl polyoxyethylene ether (TPEG, molecular weight 2400) macromer, 28.9 parts of acrylic acid, 2.7 parts of azoisobutylcyanoformamide as initiator, and 2.7 parts of mercaptopropionic acid as chain transfer agent; Ultrasonic waves are ultrasonic waves with a power of 1000W. The method for preparing powder polycarboxylate water reducer by ultrasonic wave in the bulk polymerization includes the following process steps: 1. put 150 parts of methallyl polyoxyethylene ether (TPEG) macromonomer into the reactor in parts by mass In the process, heat up to 75°C with an ultrasonic power of 1000W and start stirring to melt it; ②Mix 28.9 parts of acrylic acid and 2.7 parts of chain transfer agent, and stir well to obtain liquid A; ③After the m...

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Abstract

The invention relates to a method for preparing a powdered polycarboxylic acid water reducer by adopting ultrasonics in bulk polymerization. The polycarboxylic acid water reducer is prepared from thefollowing raw materials: a methylallyl polyoxyethylene ether macromonomer, acrylic acid, an initiator and a chain transfer agent. The method for preparing the powdered polycarboxylic acid water reducer comprises the steps: putting 85-150 parts (by mass) of the methylallyl polyoxyethylene ether macromonomer into a reaction vessel, heating the temperature of the methylallyl polyoxyethylene ether macromonomer to 65 DEG C to 75 DEG C with ultrasonic waves, and starting to carry out stirring to melt the methylallyl polyoxyethylene ether macromonomer; mixing 20.1-32.2 parts of acrylic acid with thechain transfer agent, and carrying out uniform stirring thoroughly, so as to prepare a solution A; adding the initiator into the reaction vessel after the monomer at the bottom of the reaction vesselis melted completely, carrying out stirring dissolving, then, starting to dropwise add the prepared solution A by adopting a constant-flow pump, and carrying out a heat-preserving aging reaction afterdropwise adding is completed; and carrying out discharging after the reaction ends up, and carrying out cooling, thereby obtaining the solid polycarboxylic acid water reducer. According to the method, the cycle of synthetic reaction is short, the production cost is low, the conversion ratio of the macromonomer is relatively high, and the preparation process is safe, reliable and environmentally friendly.

Description

technical field [0001] The invention relates to a preparation method of a polycarboxylate water reducer, in particular to a method for preparing a powder polycarboxylate water reducer by ultrasonic waves in bulk polymerization, which belongs to the preparation method of a concrete admixture. Background technique [0002] Water reducer is the most commonly used admixture in the concrete industry. Its main function is to reduce the water-cement ratio, which can greatly improve the performance of concrete while saving water. The development of water reducers has mainly gone through three stages: lignin sulfonate, naphthalene-based high-efficiency water reducer and polycarboxylate high-performance water reducer. Among them, polycarboxylate water reducer is the third generation product. Its advantages such as high water reducing rate, good slump retention performance, diversity of molecular design and harmless production process quickly occupied a large number of markets. Howeve...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F283/06C08F220/06C08F2/38C04B24/26C04B103/30
CPCC04B24/2605C04B2103/302C08F2/38C08F283/065C08F220/06
Inventor 王龙飞倪涛宋欣刘昭洋吴伟董树强李茜茜刘翠芬康静
Owner 刘翠芬