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Amide/imide structure polycarboxylate superplasticizer and preparation method thereof

A polycarboxylic acid and imide technology, which is applied in the field of polycarboxylic acid water reducing agent and its preparation, can solve the problems of difficult synthesis process, difficult to obtain raw materials, harsh conditions and the like, and achieves safety, environmental protection and water reduction in the synthesis process. Significant dispersion effect and low cost effect

Active Publication Date: 2018-02-02
JIANGSU SOBUTE NEW MATERIALS +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] The present invention aims at the problems that the synthesis process of the existing polycarboxylate water reducer with amide / imide structure is difficult, the raw materials are not easy to obtain, there are many side reactions, the conditions are harsh, and the cost is high. The preparation method of the polycarboxylate water reducer has the advantages of simple and easy controllable process operation, safety and environmental protection in the synthesis process, low cost, energy saving and consumption reduction; and the obtained polycarboxylate water reducer with amide / imide structure has high water reducing rate , Good flow retention performance, long storage period, significantly reduced slurry viscosity when the water-binder ratio is low, etc.

Method used

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  • Amide/imide structure polycarboxylate superplasticizer and preparation method thereof
  • Amide/imide structure polycarboxylate superplasticizer and preparation method thereof
  • Amide/imide structure polycarboxylate superplasticizer and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0063] Step 1) Add 60.0g of amino-terminated polyether (x=1, y=9, Mw=600) and 10.3g of maleic anhydride into the reactor, raise the temperature to 60°C under the protection of nitrogen, add 6.0g of concentrated sulfuric acid, Continue to raise the temperature to 80°C, keep the temperature constant for 6h, and then lower the temperature to obtain the acylated product C.

[0064] Step 2) In the glass reactor equipped with thermometer, stirrer, dropping funnel and nitrogen inlet pipe, add 114.2g deionized water, add 139.6g acylate C simultaneously, purging reaction vessel with nitrogen while stirring, And the temperature was raised to 40° C., and then 0.8 g of ammonium persulfate was added and stirred evenly. Then 13.7g of acrylic acid, 2.0g of hydroxyethyl acrylate phosphate, 1.6g of mercaptoacetic acid, and 103.5g of water were mixed and stirred to form a uniform monomer aqueous solution, which was added dropwise to the reactor for 6 hours. After completion, keep the reaction ...

Embodiment 2

[0066] Step 1) Add 60.0g of amino-terminated polyether (x=9, y=3, Mw=600) and 11.8g of itaconic anhydride into the reactor, raise the temperature to 60°C under the protection of nitrogen, and add 7.2g of benzenesulfonic acid , continue to raise the temperature to 130° C., keep the temperature constant for 2 hours, and cool down to obtain the acylated product C.

[0067] Step 2) In the glass reactor equipped with thermometer, stirrer, dropping funnel and nitrogen inlet pipe, add 174.1g deionized water, add 142.4g acylate C simultaneously, purging reaction vessel with nitrogen while stirring, And the temperature was raised to 45°C, and then 1.9 g of hydrogen peroxide was added and stirred evenly. Then 40.9g of methacrylic acid, 4.9g of hydroxyethyl acrylate phosphate, 5.6g of mercaptoethanol, and 188.2g of water were mixed and stirred to form a uniform monomer aqueous solution, which was added dropwise to the reactor for 4 hours. After the dropwise addition, keep the reaction f...

Embodiment 3

[0069] Step 1) Add 50.0g of amino-terminated polyether (x=19, y=3, Mw=1000) and 8.4g of itaconic anhydride into the reactor, raise the temperature to 60°C under the protection of nitrogen, and add 25.0g of p-toluenesulfonate acid, continue to heat up to 105°C, keep the temperature constant for 5h, and cool down to obtain the acylated product C.

[0070] Step 2) In the glass reactor equipped with thermometer, stirrer, dropping funnel and nitrogen inlet pipe, add 250.2g deionized water, add 166.8g acylate product C simultaneously, purging reaction container with nitrogen while stirring, And the temperature was raised to 55°C, and then 4.5g of potassium persulfate was added and stirred evenly. Then 47.3g of methacrylic acid, 11.0g of hydroxyethyl methacrylate phosphate, 9.0g of hypophosphorous acid, and 275.1g of water are mixed, stirred to make a uniform monomer aqueous solution, which is added dropwise to the reactor, and the dropwise addition time is 5h, after the dropwise ad...

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Abstract

The invention discloses an amide / imide structure polycarboxylate superplasticizer and a preparation method thereof. The amide / imide structure polycarboxylate superplasticizer is synthesized by amidation / imidization of amine-terminated polyether to obtain polymerizable polyether amine, and then copolymerization reaction with active monomers. The preparation method of the polycarboxylate superplasticizer provided by the invention has the advantages of simple and easily controllable technological operation, safe and environment-friendly synthetic process, low cost, energy saving and consumption reduction. Also the obtained amide / imide structure polycarboxylate superplasticizer has the advantages of high water-reducing rate, good flowing retention performance, long storage period, significantreduction of slurry viscosity under a low water-binder ratio and the like, thus solving the problems of great difficulty, difficultly available raw materials, many side reactions, harsh conditions, high cost and the like in the amide / imide polycarboxylate synthesis process.

Description

technical field [0001] The invention relates to the technical field of concrete admixtures in building materials, in particular to a polycarboxylic acid water reducer with an amide / imide structure that can be used as a high-performance water reducer for concrete and a preparation method thereof. Background technique [0002] In the existing literature, polycarboxylate water reducers are divided into four categories according to their chemical composition: (1) methacrylic acid obtained by free radical polymerization of methacrylic acid (MAA) and methyl methacrylate (MPEG ester) / methyl acrylate copolymer. (2) Acryl ether copolymer, its main feature is that the main chain and branch chain are bridged by ether bonds, so it has better stability at high pH and in some high temperature applications. (3) Obtain amide / imide type polycarboxylic acid by grafting EO / PO halo nitrogen compound on (meth)acrylic acid and (or) methoxy-containing ester copolymer. (4) Sika invented a new a...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F290/06C08F220/06C08F230/02C08G65/26C04B24/24C04B103/30
CPCC04B24/246C04B2103/302C08F290/062C08G65/3328C08F220/06C08F230/02
Inventor 王秀梅杨勇舒鑫张建纲赵红霞冉千平
Owner JIANGSU SOBUTE NEW MATERIALS
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