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Method for realizing efficient graft polymerization of acrylonitrile on surface of silica gel microparticles by utilizing mercapto-Ce(IV) salt redox initiation system

A technology of silica gel particles and graft polymerization, which is applied in the field of efficient graft polymerization of acrylonitrile on the surface of silica gel particles, can solve problems such as difficulty in introducing initiating groups, and achieve the effect of high grafting degree

Inactive Publication Date: 2012-05-09
ZHONGBEI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

In the "grafting" method, if the initiator group is introduced on the surface of the solid particle (called surface-initiated grafting method, "Surface-initiated grafting"), since the initiator species is located on the surface of the particle, the efficiency of graft polymerization is higher ( This method also includes various active polymerization methods initiated by the surface). However, it is often difficult to introduce initiating groups on the surface of solid particles

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  • Method for realizing efficient graft polymerization of acrylonitrile on surface of silica gel microparticles by utilizing mercapto-Ce(IV) salt redox initiation system
  • Method for realizing efficient graft polymerization of acrylonitrile on surface of silica gel microparticles by utilizing mercapto-Ce(IV) salt redox initiation system
  • Method for realizing efficient graft polymerization of acrylonitrile on surface of silica gel microparticles by utilizing mercapto-Ce(IV) salt redox initiation system

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Effect test

Embodiment 1

[0021] A method for realizing efficient graft polymerization of acrylonitrile on the surface of silica gel particles by using a mercapto-Ce(IV) salt redox initiation system, including the following steps:

[0022] (1) Surface modification of silica gel with a coupling agent containing sulfhydryl groups: Take 30g of silica gel particles and place them in 150 mL of a 5% methanesulfonic acid aqueous solution, stir and activate them at reflux temperature for 8 hours, and the activated silica particles Wash with distilled water repeatedly until it is neutral, filter by suction, and dry in vacuum. Then add 2.5g of activated silica gel particles to 120ml of toluene solvent, and add 2.5ml of coupling agent γ-mercaptopropyltrimethoxysilane at 110°C After reacting for 12 hours, after the reaction is finished, suction filtration, the product particles are washed with toluene first, then washed with ethanol repeatedly, and dried in vacuum to obtain the modified silica particles MPMS-SiO with ...

Embodiment 2

[0026] A method for realizing efficient graft polymerization of acrylonitrile on the surface of silica gel particles by using a mercapto-Ce(IV) salt redox initiation system, including the following steps:

[0027] (1) Surface modification of silica gel with sulfhydryl-containing coupling agent: Take 30g of silica gel particles and place them in 150 mL of methanesulfonic acid aqueous solution with a concentration of 7%, stir and activate them at reflux temperature for 10 hours. The activated silica gel particles Wash with distilled water repeatedly until it is neutral, filter with suction, and dry in vacuum. Then add 2.5g of activated silica gel particles to 130ml of toluene solvent, and add 3.5ml of coupling agent γ-mercaptopropyltrimethoxysilane, at 110℃ After reacting for 12 hours, after the reaction is finished, suction filtration, the product particles are washed with toluene first, then washed with ethanol repeatedly, and dried in vacuum to obtain the modified silica particle...

Embodiment 3

[0031] A method for realizing efficient graft polymerization of acrylonitrile on the surface of silica gel particles by using a mercapto-Ce(IV) salt redox initiation system, including the following steps:

[0032] (1) Surface modification of silica gel with a coupling agent containing sulfhydryl groups: Take 30g of silica gel particles and place them in 150 mL of a 6% methanesulfonic acid aqueous solution, stir and activate them at reflux temperature for 9 hours. The activated silica gel particles Wash with distilled water repeatedly until it is neutral, filter by suction, and dry in vacuum. Then add 2.5g of activated silica gel particles to 125ml of toluene solvent, and add 3.0ml of coupling agent γ-mercaptopropyltrimethoxysilane at 110°C After reacting for 12 hours, after the reaction is finished, suction filtration, the product particles are first washed with toluene, then repeatedly washed with ethanol, and dried under vacuum to obtain modified silica particles MPMS-SiO with s...

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Abstract

The invention discloses a method for realizing efficient graft polymerization of acrylonitrile on the surface of silica gel microparticles by utilizing a mercapto-Ce(IV) salt redox initiation system. The method comprises the following steps of: (1) surface modification of silica gel by using a mercapto-containing coupling agent: reacting silica gel microparticles in a methane sulfonic acid aqueous solution, then adding activated silica gel microparticles to a toluene solvent, and adding gamma-mercaptopropyl trimethoxy silane (MPMS) as a coupling agent to prepare modified silica gel microparticles MPMS-SiO2 containing mercapto on the surface; and (2) graft polymerization of acrylonitrile: adding the modified microparticles MPMS-SiO2, DMF (dimethyl formamide) and AN (acrylonitrile) monomer to a four-neck flask, introducing nitrogen for 30 min, then adding a water solution dissolved with ammonium cerous sulfate and concentrated sulfuric acid, and reacting to obtain grafted microparticlesPAN / SiO2. In the method disclosed by the invention, the mercapto-Ce(IV) salt redox initiation system is utilized to initiate graft polymerization, and the active spots are located on the surface of acarrier, thus the method has high grafting degree and is a high-efficiency surface-initiated grafting method.

Description

Technical field [0001] The invention relates to a synthetic method for efficiently grafting PAN on the surface of silica gel particles, in particular to a method for realizing efficient graft polymerization of acrylonitrile on the surface of silica gel particles by using a mercapto-Ce(IV) salt redox initiation system. Background technique [0002] Grafting functional macromolecules on the surface of inorganic particles, combining the functionality of functional macromolecules with the excellent mechanical properties, thermal and chemical stability of inorganic particles, is currently an important way to prepare functional composite particles. Grafting functional macromolecules on the surface of inorganic particles can give the particles many new characteristics, such as adsorption performance, chemical activity, biological activity, optical activity, chelating performance of metal ions and dispersibility, etc., which can be widely used in chromatographic fixation Phase, heterogen...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F292/00C08F220/44C08F4/40
Inventor 高保娇杜瑞奎安富强
Owner ZHONGBEI UNIV
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