Preparation method for coating of nano-silica through miniemulsion polymerization

A nano-silica, mini-emulsion polymerization technology, applied in the direction of dyed organosilicon compound treatment, dyed polymer organic compound treatment, fibrous filler, etc., can solve the decrease of organic/inorganic interface strength, unfavorable application, detrimental silane coupling It can improve the uniformity of treatment, increase the lipophilicity, and achieve the effect of high polymerization efficiency.

Inactive Publication Date: 2014-02-05
CHANGZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the existing silane coupling agents generally need to be hydrolyzed before they can be applied to the surface treatment of inorganic materials, resulting in the Si-OH functional groups generated after hydrolysis attracting each other and causing molecular aggregation, thus reducing the performance of silane coupling agents. effect, and even cause the so-called physical adsorption, which reduces the strength of the organic / inorganic interface, which is not conducive to its application

Method used

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  • Preparation method for coating of nano-silica through miniemulsion polymerization
  • Preparation method for coating of nano-silica through miniemulsion polymerization
  • Preparation method for coating of nano-silica through miniemulsion polymerization

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] Example 1: Synthesize P(St-g-KH550) copolymer by ATRP method and introduce microemulsion polymerization to realize nano-silica coating

[0033] Polymerization steps:

[0034] (1) Preparation of P(St-g-KH550)

[0035] Add 20 g of styrene (St) monomer to a 100 mL flask with a stirring device, add 40 mL of ethyl acetate, 1.3 mL of triethylamine, stir under an ice bath, and use a constant pressure dropping funnel to dropwise add 1 mL of 2- The mixed solution of bromoisobutyryl bromide and 10 mL ethyl acetate was dripped in 0.5 h, then the ice bath was removed and the mixture was raised to room temperature and kept stirring for 1 h in the dark. After the completion of the reaction, the product was diluted with tetrahydrofuran (THF), and the reaction mixture was poured into methanol for precipitation, filtered, and vacuum dried to constant weight. The polymer product was dissolved in THF, and the solution was passed through Al 2 O 3 The column adsorbs and removes the copp...

Embodiment 2

[0040] Example 2: Synthesize P(St-g-KH560) copolymer by ATRP method and introduce microemulsion polymerization to realize nano-silica coating

[0041] Polymerization steps:

[0042] (1) Preparation of P(St-g-KH560)

[0043] Add 20 g of styrene monomer to a 100 mL flask with a stirring device, add 40 mL of ethyl acetate, 1.3 mL of triethylamine, stir under an ice bath, and use a constant pressure dropping funnel to add dropwise containing 1 mL of 2-bromoiso The mixed solution of butyryl bromide and 10 mL of ethyl acetate was dripped in 0.5 h, then the ice bath was removed and the mixture was raised to room temperature to continue stirring for 1 h in the dark. After the reaction, the product was diluted with tetrahydrofuran (THF), and the reaction mixture was poured into methanol to precipitate, filtered, and dried in vacuum to a constant weight. The polymer product was dissolved in THF, and the solution was passed through Al 2 O 3 The column adsorbs and removes the c...

Embodiment 3

[0048] Example 3: Synthesize P(St-g-KH570) copolymer by ATRP method and introduce microemulsion polymerization to realize nano-silica coating

[0049] Polymerization steps:

[0050] (1) Preparation of P(St-g-KH570)

[0051] Add 20 g of styrene monomer to a 100 mL flask with a stirring device, add 40 mL of ethyl acetate, 1.3 mL of triethylamine, stir under an ice bath, and use a constant pressure dropping funnel to add dropwise containing 1 mL of 2-bromoiso The mixed solution of butyryl bromide and 10 mL of ethyl acetate was dripped in 0.5 h, then the ice bath was removed and the mixture was raised to room temperature to continue stirring for 1 h in the dark. After the completion of the reaction, the product was diluted with tetrahydrofuran (THF), and the reaction mixture was poured into methanol for precipitation, filtered, and vacuum dried to constant weight. The polymer product was dissolved in THF, and the solution was passed through Al 2 O 3 The column adsorbs ...

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Abstract

The invention relates to a preparation method for coating of nano-silica through miniemulsion polymerization, which relates to the technical field of atom transfer radical polymerization and miniemulsion polymerization. The preparation method comprises the following steps: preparing a macroinitiator to modify the surface of a monomer, removing a solvent and a catalyst and then preparing a graft copolymer from the brominated monomer and a silane coupling agent through the ATRP method; and individually using the copolymer prepared above as a co-stablizer or a silane coupling agent for miniemulsion polymerization so as to finally prepare a stable emulsion particle with narrow particle size distribution and to meet requirements for coating of nano-silica. The preparation method provided by the invention has the advantages of safe process, simple operation and improvement of the characteristic of great possibility of agglomeration of nano-silica caused by a great specific surface area and high surface energy of nano-silica; and with the preparation method, the nano-silica particle with uniform particle size distribution and uniform dispersion is obtained, and the nano-silica particle is better compatible with a polymer.

Description

technical field [0001] The invention relates to the technical fields of atom transfer radical polymerization (ATRP) and miniemulsion polymerization, in particular, it relates to a preparation method for coating nano silicon dioxide on a polymer prepared by the ATRP method. Background technique [0002] Nano silica has surface interface effect, quantum size effect, macroscopic quantum tunneling effect, etc., as well as its high strength, high toughness, and good stability at high temperatures, making it widely used in rubber, plastics, adhesives, etc. , coatings and other fields. But at the same time, nano-silica has small particle size, large specific surface area, strong hydrophilicity, high surface activity, and poor stability, which makes it easy to agglomerate between particles and poor dispersion in polymers, making it itself The excellent properties it has weaken or disappear, which affects people's use of it, so its surface needs to be modified. [0003] Silane co...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F275/00C08F2/44C08K3/36C09C1/28C09C3/12C09C3/10
Inventor 张震乾王佩
Owner CHANGZHOU UNIV
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