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Production method and application of micron-sized supported difunctional polymer brush with nitroxide free radicals and sulfonic groups

A technology of nitroxide free radicals and polymer brushes, which is applied in the preparation of polycarboxylate superplasticizer active macromonomers, bifunctional polymer brushes, and synthesis of polyethylene glycol monomethyl ether acrylate, which can solve the problem of nitrogen oxides Free radicals have no effect of polymerization inhibition, there is no recovery of polymerization inhibitors and acid catalysts, and poor dispersibility, etc., to achieve the effects of easy recycling, large particle size, and improved compatibility

Active Publication Date: 2019-07-05
HEBEI UNIVERSITY OF SCIENCE AND TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The copolymer is a linear random copolymer, because it contains both the lipophilic structural unit TMA and the hydrophilic structural unit HSS, so that it is neither soluble in the oil phase nor in the water phase, and due to the presence of a large number of hydrophilic structural units Existence makes it used in the reaction system of synthetic water reducing agent polyethylene glycol monomethyl ether methacrylate macromonomer, the dispersibility is very poor, resulting in the nitrogen oxide free radicals not having the effect of inhibiting polymerization, and the reaction will cause within 1h Self-aggregation
At present, there is no technical solution to realize the recovery of polymerization inhibitor and acid catalyst at the same time

Method used

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  • Production method and application of micron-sized supported difunctional polymer brush with nitroxide free radicals and sulfonic groups
  • Production method and application of micron-sized supported difunctional polymer brush with nitroxide free radicals and sulfonic groups

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] 1. Preparation of micron-sized bifunctional polymer brushes containing nitroxide radicals and sulfonic acid groups

[0028] (1) Add CuBr to a 100mL three-neck flask 2 (0.0250 g, 0.112 mmol), solvent anisole (30 mL) and magnetic rotor, ultrasonic vibration 2After complete dissolution, add a condenser tube and a thermometer to the three-necked flask, and set the temperature to 40°C. Under nitrogen atmosphere, St (11.6648 g, 112 mmol), PMDETA (0.23 mL, 1.12 mmol), PS-Cl (1 g, 1.12 mmol) and stannous octoate ( 0.36 mL, 1.12 mmol). The reaction temperature was set to 110 °C and reacted for 9 h. After the reaction was completed, the reaction solution was poured into a beaker. Let stand for 12 h, remove the supernatant by filtration, and dry in vacuum until constant weight. The resulting product is the homopolymer brush PS-PSt.

[0029] (2) Add CuBr to a 100 mL three-neck flask 2 (0.0098 g, 0.04 mmol), solvent anisole (30 mL) and magnetic rotor, ultrasonic vibration 2...

Embodiment 2

[0037] 1. Preparation of micron-sized double-tapping functional polymer brushes containing nitroxide radicals and sulfonic acid groups

[0038] (1) Add the catalyst CuBr into a 100 mL three-necked flask 2 (0.0250 g, 0.112 mmol), solvent anisole (30mL) and magnetic rotor, ultrasonic vibration 2 After complete dissolution, add a condenser tube and a thermometer to the three-necked flask, and set the temperature to 40°C. Under nitrogen atmosphere, the monomer St (23.3296 g, 224 mmol), the ligand PMDETA (0.23 mL, 1.12 mmol), and the macroinitiator polystyrene chloride ball PS-Cl (1 g, 1.12 mmol) and reducing agent stannous octoate (0.36 mL, 1.12 mmol). The reaction temperature was set to 110 °C and reacted for 9 h. After the reaction was completed, the reaction solution was poured into a beaker, allowed to stand for 12 h, filtered to remove the supernatant, and vacuum-dried to constant weight. The resulting product is the homopolymer brush PS-PSt.

[0039] (2) Add the cataly...

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Abstract

The invention relates to a micron-sized supported difunctional polymer brush with nitroxide free radicals and sulfonic groups. A production method comprises the steps of using 2,2,6,6-tetramethyl-4-piperidyl methacrylate TMPM and styrene St as monomer, using chloromethylated cross-linked polystyrene micro-spheres with particle size of 74-149 [mu]m and a Cl content of 1.12 mmol / g as a macroinitiator, adopting ARGETATRP for synthesizing a TMPM and St block polymer brush, using m-chloroperbenzoic acid mCPBA for oxidizing piperidyl of the TMPM into the nitroxide free radicals, and using sulfur forsulfonating the St to obtain the difunctional polymer brush. Application of the difunctional polymer brush in synthesis of polycarboxylate water reducer reactive macromonomer is further provided. Theproduced difunctional polymer brush can achieve recovery and recycle of a polymerization inhibitor and an acid catalyst at the same time, the production cost is reduced, and the reaction rate is improved.

Description

technical field [0001] The invention belongs to the technical field of nitroxide free radical polymerization inhibitors and sulfonic acid catalysts, in particular to a preparation method of a micron-sized bifunctional polymer brush immobilized with nitroxide radicals and sulfonic acid groups and its application in polycarboxylic acid Water reducer active macromonomer, especially the application in the synthesis of polyethylene glycol monomethyl ether acrylate. Background technique [0002] Polycarboxylate high-efficiency water reducer has a comb-shaped molecular structure. Compared with the second-generation naphthalene-based and melamine-based water-reducers, it has high water-reducing rate, low slump loss, low alkali content and compatibility with cement. It has attracted widespread attention due to its excellent performance such as good capacitance. At present, the main technical route for the synthesis of polycarboxylic acid-based water reducers is the direct copolymeri...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F293/00C08F283/06C08F265/04C08F220/06C04B24/16C04B103/30
CPCC04B24/165C04B2103/30C08F265/04C08F283/06C08F293/00C08F2438/01C08F220/06Y02P20/584
Inventor 刘少杰王利利张锐郝盼盼赵婷冯树波
Owner HEBEI UNIVERSITY OF SCIENCE AND TECHNOLOGY
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