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A peroxide-ascorbic acid-triggered nipam in sio 2 A Method for Surface Efficient Graft Polymerization

A technology of ascorbic acid and graft polymerization, which is applied in the field of grafting polymers on the surface of particles, can solve problems such as low grafting efficiency of polymers, and achieve the effects of wide application range, improving grafting efficiency and improving utilization rate.

Active Publication Date: 2022-02-11
CHANGZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] The present invention provides a high-efficiency grafting method in order to solve the problem of low polymer grafting efficiency in the common method of particle surface-induced graft polymerization, and specifically provides a method of using peroxide-ascorbic acid to trigger NIPAM on SiO 2 A Method for Surface Efficient Graft Polymerization

Method used

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  • A peroxide-ascorbic acid-triggered nipam in sio <sub>2</sub> A Method for Surface Efficient Graft Polymerization
  • A peroxide-ascorbic acid-triggered nipam in sio <sub>2</sub> A Method for Surface Efficient Graft Polymerization
  • A peroxide-ascorbic acid-triggered nipam in sio <sub>2</sub> A Method for Surface Efficient Graft Polymerization

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Embodiment 1

[0025] A peroxide-ascorbic acid-triggered NIPAM on SiO 2 The method for surface efficient graft polymerization mainly comprises the following steps:

[0026] (1) Dissolve tetraethyl orthosilicate (TEOS) in a mixed solvent of ethanol / distilled water without an appropriate amount of water, adjust the pH to 9 with ammonia water, stir at 40°C for 0.5h, and then add 3-chloropropyl triethoxy base silane (CTS), wherein the molar ratio of CTS to TEOS is 0.1:1, the molar ratio of silanol in the control system is 1:6, and the molar ratio of silicon to water is 1:4, then stir until the system is gel-like, static Place and age, and finally vacuum-dry at 100°C to constant weight, and obtain chloropropylated modified SiO particles after grinding. 2 -Cl;

[0027] (2) SiO 2 -Cl is ultrasonically dispersed in an appropriate amount of toluene, and the catalyst FeCl is added 3 and excess tert-butyl hydroperoxide (TBHP), wherein the molar ratio of the catalyst to TBHP is 0.08:1, stirred and r...

Embodiment 2

[0037] A peroxide-ascorbic acid-triggered NIPAM on SiO 2 The method for surface efficient graft polymerization mainly comprises the following steps:

[0038] (1) Dissolve ethyl orthosilicate (TEOS) in a mixed solvent of ethanol / distilled water without an appropriate amount of water, adjust the pH to 8 with ammonia water, stir at 50°C for 0.5h, and then add 3-chloropropyl triethoxy base silane (CTS), wherein the molar ratio of CTS to TEOS is 0.05:1, the molar ratio of silanol in the control system is 1:5, and the molar ratio of silicon to water is 1:8, then stir until the system is gel-like, static Place and age, and finally vacuum-dry at 100°C to constant weight, and obtain chloropropylated modified SiO particles after grinding. 2 -Cl;

[0039] (2) SiO 2 -Cl is ultrasonically dispersed in an appropriate amount of organic solvent, and the catalyst FeCl is added 3 and excess tert-butyl hydroperoxide (TBHP), wherein the molar ratio of the catalyst to TBHP is 0.05:1, stirred a...

Embodiment 3

[0044] A peroxide-ascorbic acid-triggered NIPAM on SiO 2 The method for surface efficient graft polymerization mainly comprises the following steps:

[0045] (1) Dissolve tetraethyl orthosilicate (TEOS) in a mixed solvent of ethanol / distilled water without an appropriate amount of water, adjust the pH to 9 with ammonia water, stir at 55°C for 0.5h, and then add 3-chloropropyl triethoxy base silane (CTS), wherein the molar ratio of CTS to TEOS is 0.08:1, the molar ratio of silanol in the control system is 1:5, and the molar ratio of silicon to water is 1:4, then stir until the system is gel-like, static Place and age, and finally vacuum-dry at 100°C to constant weight, and obtain chloropropylated modified SiO particles after grinding. 2 -Cl;

[0046] (2) SiO 2 -Cl ultrasonically dispersed in an appropriate amount of CCl 4 , adding the catalyst TiCl 4 and excess tert-butyl hydroperoxide (TBHP), wherein the molar ratio of the catalyst to TBHP is 0.1:1, stirred and reacted at...

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Abstract

The invention discloses a method of using peroxide-ascorbic acid to trigger NIPAM on SiO 2 The method of high-efficiency grafting polymerization on the surface solves the problem of low polymer grafting efficiency under the double active center initiation system. This method utilizes the sol-gel method to prepare surface chloropropylated modified SiO particles. 2 ‑Cl, then surface peroxidation modification to get SiO 2 ‑I, and finally construct the peroxide‑ascorbic acid redox system to induce NIPAM on SiO 2 Efficient graft polymerization on the surface to obtain SiO 2 @PNIPAM. Among the two free radicals formed by the above oxidation-reduction reaction, the surface-anchored free radicals and free ascorbic acid free radicals, ascorbic acid free radicals have low activity and do not have the ability to initiate, so the polymerization reaction is only carried out on the surface of the particles, reducing the amount of polymerization system. The content of free polymers in the medium is greatly improved, and the utilization rate of monomers is greatly improved. It is a high-efficiency surface graft polymerization method.

Description

technical field [0001] The invention relates to a method for grafting polymers on the surface of particles, in particular to a method for using peroxide-ascorbic acid to trigger NIPAM on SiO 2 A method for efficient graft polymerization of surfaces. Background technique [0002] The "Surface-initiated Polymerization (SIP)" method has the advantages of high grafting rate, diversified grafting methods and small grafting steric hindrance. In the past two decades, SIP technology has been used to graft polymers on the surface of materials. The preparation of modified and functionalized organic / inorganic hybrid particles (such as hydrophilic / lipophilic, environmental responsiveness, biocompatibility, etc.) A powerful tool for surface modification and functional design of materials. [0003] For particle surface initiation of conventional free radical polymerization, immobilized azo (peroxy) groups on the surface or constructing a redox initiation system (persulfate or peroxide-r...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F292/00C08F220/54C08F4/40
CPCC08F292/00C08F220/54C08F4/40
Inventor 杨海存蔡子楠刘昊天马文中龚方红陶国良刘春林
Owner CHANGZHOU UNIV