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A kind of terminal ethylenically unsaturated phosphonic acid monomer and its preparation method

An unsaturated, alkenyl-terminated technology, which is applied in the field of alkenyl-terminated groups, can solve problems such as inability to undergo copolymerization reactions and limited application ranges

Active Publication Date: 2018-08-21
河北凯瑞化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

But also because of its inability to undergo copolymerization, its application range is limited

Method used

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  • A kind of terminal ethylenically unsaturated phosphonic acid monomer and its preparation method
  • A kind of terminal ethylenically unsaturated phosphonic acid monomer and its preparation method
  • A kind of terminal ethylenically unsaturated phosphonic acid monomer and its preparation method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] In the reaction flask equipped with stirrer, reflux condenser, thermometer, dropping funnel, and heat exchange, according to the calculation of phosphorus trichloride, acrylic acid and water molar ratio is 1:3.15:1, first add 200g of acrylic acid, and then slowly Slowly add 121.1g of phosphorus trichloride and keep stirring. The time of dropping is about 1h. The temperature of the cold water bath is controlled below 40°C. ℃, after reflux reaction for 30 minutes, continue to slowly raise the temperature to 110~120 ℃, and keep at this temperature for 2 hours, until no hydrogen chloride is produced, and the hydrogen chloride gas generated during the reaction is absorbed with water. Release the supernatant, the by-product unsaturated acyl chloride can be used as an acylating reagent, the lower layer product is moved to a distillation bottle, add 15.78g of water and distill under reduced pressure for 1~2h, remove the by-product acrylic acid and residual HCl, and the reaction ...

Embodiment 2

[0028] According to phosphorus trichloride, acrylic acid and water molar ratio is 1:3.2:1 calculation, at first add 200g acrylic acid, then slowly add dropwise 119.2g phosphorus trichloride and keep stirring, other conditions are the same as embodiment 1, lower floor product shifts Add 15.63g of water to the distillation bottle for distillation under reduced pressure. After the reaction was completed, the hydroxypropenylidene diphosphonic acid of the product was obtained, and the content of the product was analyzed by the thorium nitrate rapid titration method. The calculated yield was 85.68%, and 230.19 g of water was added to form a 40% aqueous solution.

Embodiment 3

[0030] According to the calculation that the molar ratio of phosphorus trichloride, methacrylic acid and water is 1:3.15:1, first add 200g of methacrylic acid, then slowly add 101.3g of phosphorus trichloride dropwise and keep stirring, other conditions are the same as in Example 1 , the lower floor product was moved to a distillation bottle and added 13.28g of water for distillation under reduced pressure. After the reaction was over, the hydroxymethylacrylic acid diphosphonic acid was obtained. The content of the product was analyzed by the thorium nitrate rapid titration method. The calculated yield was 83.88%, and 194.15% of water was added. g into a 40% aqueous solution.

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Abstract

The invention relates to an alkenyl-terminated unsaturated phosphonic acid monomer and a preparation method thereof. The monomer has the structure shown in the following formula, wherein R represents -H or -CH3. The method comprises the steps as follows: unsaturated carboxylic acid and a polymerization inhibitor are added to a reaction flask, then phosphorus trichloride is dropwisely added, the mixture is stirred continuously to react at the controlled temperature, the obtained system is heated slowly for a reflux reaction, the obtained system is slowly heated and reacts at the constant temperature, a lower layer product is subjected to reduced pressure distillation after the reaction ends, unsaturated carboxylic acid and residual HCl are removed, the content of the product is analyzed with a rapid thorium nitrate titration method, the yield is calculated, and an aqueous solution is prepared. A phosphate group is introduced while the high polymerization activity of double bonds of unsaturated acid is reserved, and a polycarboxylate superplasticizer with high dispersibility, high slump retention and high adaptability is acquired through polymerization with acrylic acid and alkenyl polyoxyethylene ether macromonomers.

Description

technical field [0001] The present invention relates to a terminal ethylenically unsaturated phosphonic acid monomer and its preparation method, especially a terminal alkenyl group introduced into conventional phosphonic acid with high polymerization activity and applied to the synthesis of polycarboxylic acid water reducer middle. Background technique [0002] Under the condition of low water-cement ratio and low dosage, the polycarboxylate superplasticizer has the outstanding advantages of high pulp fluidity, small slump loss, and environmental protection. Judging from the structure and composition of the polymerized monomers of the existing commercialized polycarboxylic acid-based high-performance water reducers, it is mainly composed of polyoxyethylene ethers and ester macromonomers with unsaturated double bonds and unsaturated acids. , in order to improve the adaptability of the concrete and the dispersibility of the superplasticizer, different reactive monomers are ad...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F9/38C08F283/06C08F220/06C08F230/02C04B24/26C04B103/30
CPCC04B24/2694C04B2103/302C07F9/3817C08F283/065C08F220/06C08F230/02
Inventor 吕志平范向前王卫星关建奇宋录武
Owner 河北凯瑞化工有限公司
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