Method of preparing phosphate functional monomers in vinyl pyrrolidone medium and application

A technology of vinylpyrrolidone and functional monomer, which is applied in the field of phosphate ester functional monomer and polycarboxylate water reducer and its preparation, can solve the problems of environmental pollution, separation and recovery of toxic organic solvents, etc., and achieve high dispersion performance, The effect of slowing down the hydration rate and good slump retention ability

Active Publication Date: 2018-04-06
GUIZHOU TIEJIANHENGFA NEW MATERIAL TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The first purpose of the present invention: to provide an industrial preparation method for preparing phosphate functional monomers in vinylpyrrolidone medium, to solve the difficulty of separation and recovery of low boiling point and toxic organic solvents used in the preparation process of existing phosphate functional monomers and environmental pollution problems, while simplifying the synthesis route and use of phosphate ester functional monomers

Method used

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  • Method of preparing phosphate functional monomers in vinyl pyrrolidone medium and application
  • Method of preparing phosphate functional monomers in vinyl pyrrolidone medium and application

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] Add 3.4g of hydroquinone inhibitor and 300g of vinylpyrrolidone into a 1000mL four-neck flask equipped with a stirrer, thermometer and peristaltic pump, o In an ice-water bath at C, under low-speed stirring, 426g of glycidyl methacrylate and 172g of concentrated phosphoric acid were simultaneously added dropwise to the flask, and the drop was completed within 2 to 3 hours, and then the temperature was rapidly raised to 70 o C, keep warm for esterification for 4 hours, add 60g deionized water and heat up to 90 o C, keep warm for 30 minutes to obtain a brownish-yellow liquid that is a phosphate functional monomer with vinylpyrrolidone as a medium.

Embodiment 2

[0018] Add 3.4g of hydroquinone inhibitor and 375g of vinylpyrrolidone into a 1000mL four-necked flask equipped with a stirrer, thermometer and peristaltic pump, o In an ice-water bath at C, under low-speed stirring, 426g of glycidyl methacrylate and 346g of concentrated phosphoric acid were simultaneously added dropwise to the flask, and the drops were completed within 2 to 3 hours, and then the temperature was rapidly raised to 70 o C, keep warm for esterification for 4 hours; add 75g deionized water and heat up to 90 o C, keep warm for 30 minutes to obtain a brownish-yellow liquid that is a phosphate functional monomer with vinylpyrrolidone as a medium.

Embodiment 3

[0020] Add 3.4g of hydroquinone inhibitor and 328g of vinylpyrrolidone into a 1000mL four-neck flask equipped with a stirrer, thermometer and peristaltic pump o In an ice-water bath at C, under low-speed stirring, 426g of glycidyl methacrylate and 230g of concentrated phosphoric acid were simultaneously added dropwise to the flask, and the dripping was completed within 2 to 3 hours, and then the temperature was rapidly raised to 70 o C, keep warm for esterification for 4 hours; add 65g deionized water and heat up to 90 o C, keep warm for 30 minutes to obtain a brownish-yellow liquid that is a phosphate functional monomer with vinylpyrrolidone as a medium.

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Abstract

The invention discloses a method of preparing phosphate functional monomers in a vinyl pyrrolidone medium and application. Vinyl pyrrolidone is used as a reaction medium, after phosphorylation reaction, the final product can be obtained without separation, the phosphate functional monomers serve as third monomers for synthesizing a polycarboxylate superplasticizer, the medium vinyl pyrrolidone canparticipate in polymerization reaction, the step of recovering toxic micromolecular organic solvent with low boiling point is omitted, environment pollution is avoided, and the problem that dispersive capacity and slumps retaining capacity of an existing polycarboxylate superplasticizer contradict is solved. The preparing method of the polycarboxylate superplasticizer which is high in dispersivecapacity, slumps retaining capacity and cement adaptability is provided.

Description

technical field [0001] The invention belongs to the technical field of building materials, and in particular relates to a phosphate ester functional monomer, a polycarboxylate water reducer and a preparation method thereof. Background technique [0002] In recent years, with the continuous expansion of the scale of civil engineering and the continuous improvement of the level of science and technology, some important buildings with high-rise, long-span and special functional requirements have emerged, such as skyscrapers, super-long-span bridges, high-speed railways and giant water conservancy projects. It is required that concrete must have higher strength, better durability, and better stability. Water reducing agent is one of the indispensable important components of high performance concrete. Water reducing agent can reduce the mixing water consumption of concrete during use, improve its durability, improve slump retention, and improve concrete performance. Increase str...

Claims

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Application Information

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IPC IPC(8): C08F283/06C08F220/06C08F230/02C08F2/38C04B24/26C07F9/09C04B103/30
CPCC04B24/246C04B2103/302C07F9/091C08F2/38C08F283/065C08F220/06C08F230/02
Inventor 陈娟李本秀罗秀平王毓许志顺郭威陈凯彭守军蒋天福
Owner GUIZHOU TIEJIANHENGFA NEW MATERIAL TECH CO LTD
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