Preparation method of fluorine-containing nano-SiO2 microspheres with photo-initiating activity and nano-SiO2

A technology of photoinitiation and photoinitiator, which is applied in the field of polymer material synthesis, can solve the problems of oxygen inhibition and coating surface properties to be improved, and achieve the effect of improving stability, good gloss and good weather resistance

Active Publication Date: 2019-02-15
安庆北化大科技园有限公司
View PDF4 Cites 8 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The problem to be solved by the present invention is that when the existing nano-silica is directly filled into the photocuring coating, the problem of oxygen inhibition is prone to occur, and the surface properties of the coating after photocuring need to be improved.

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • Preparation method of fluorine-containing nano-SiO2 microspheres with photo-initiating activity and nano-SiO2
  • Preparation method of fluorine-containing nano-SiO2 microspheres with photo-initiating activity and nano-SiO2
  • Preparation method of fluorine-containing nano-SiO2 microspheres with photo-initiating activity and nano-SiO2

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] A fluorine-containing nano-SiO with photoinitiated activity 2 The preparation method of microspheres comprises the following steps:

[0033] (1) Add 100mL of ethanol, 2.5g of ammonia water to a 250mL three-necked flask, stir after 16.2g of deionized water, mix well, wherein alcohols are the reaction medium, take 44.274g of trimethoxypropylamine silane and set it In a constant pressure funnel, it was added dropwise to the above mixed solution within 1 hour at room temperature. After the dropwise addition, the temperature was raised to 45 °C, and the reaction was stirred for 6 hours to obtain nano-silica microspheres with polymerizable groups on the surface. solution; the concentrations of ammonia, water and trimethoxypropylaminosilane in the whole solution are 0.9mol / L, 5.52mol / L and 1.2mol / L respectively.

[0034] (2) Pour nitrogen into the nano-silica microsphere solution prepared in step (1), use a constant pressure dropping funnel, and dropwise add 56.8 g of heptade...

Embodiment 2

[0045] A fluorine-containing nano-SiO with photoinitiated activity 2 The preparation method of microspheres comprises the following steps:

[0046] (1) Add 100 mL of methanol, 1 g of ammonia water, and 10 g of deionized water to a 250 mL three-necked flask with mechanical stirring, mix well, take 22.137 g of trimethoxypropylaminosilane and place it in a constant pressure funnel, dropwise It was added to the above mixed solution within 1 hour at room temperature. After the dropwise addition was completed, the temperature was raised to 40 °C, and the reaction was stirred for 6 hours to obtain a nano-silica microsphere solution with polymerizable groups on the surface. The concentration of propylaminosilane in the whole solution is 0.44mol / L, 4.17mol / L and 0.75mol / L respectively;

[0047] (2) Pour nitrogen into the nano-silica microsphere solution prepared in step (1), use a constant pressure dropping funnel, and add 56.8 g of heptadecafluorodecyltriethoxysilane dropwise to the ...

Embodiment 3

[0058] A fluorine-containing nano-SiO with photoinitiated activity 2 The preparation method of microspheres comprises the following steps:

[0059] (1) Add 100 mL of isopropanol, 0.5 g of ammonia water, and 18 g of deionized water into a 250 mL three-necked flask with mechanical stirring, and mix well. 33.205 g of γ-mercaptopropyltrimethoxysilane was placed in a constant pressure funnel, and added to the above mixed solution in a dropwise manner within 1 h at room temperature. After the dropwise addition, the temperature was raised to 60 °C, and the reaction was stirred for 3 h to obtain a nano-silica microsphere solution with polymerizable groups on the surface; the concentrations of ammonia, water, and γ-mercaptopropyltrimethoxysilane in the entire solution were respectively. are 0.19mol / L, 6.72mol / L and 1mol / L;

[0060] (2) Pour nitrogen into the nano-silica microsphere solution prepared in step (1), use a constant pressure dropping funnel, and add 56.8 g of heptadecafluo...

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to view more

PUM

PropertyMeasurementUnit
Pencil hardnessaaaaaaaaaa
Pencil hardnessaaaaaaaaaa
Login to view more

Abstract

The invention discloses a preparation method of fluorine-containing nano-SiO2 microspheres with photo-initiating activity and nano-SiO2, relates to the field of high polymer material synthesis and aims to solve the problems that existing nano-SiO2 is prone to oxygen inhibition when applied to a photo-cured coating by direct filling and surface performance of the photo-cured coating is required tobe improved. The preparation method comprises following steps: fluorocarbon modified nano-SiO2 with active sites is prepared; acrylic ester with an initiator structure is added to a prepared fluorocarbon modified nano-SiO2 solution, and the silica surface is grafted with a photoinitiator structure by a Michael addition reaction. The preparation method has beneficial effects as follows: the preparation method is simple, stability of the prepared nano-SiO2 microspheres can be improved, and when the nano-SiO2 microspheres are added to a formula of the photo-cured coating, a coating with high surface hardness, scratch resistance, good glossiness, good weather fastness and oxygen inhibition resistance can be obtained and the coating surface can further has hydrophobic performance.

Description

technical field [0001] The invention relates to the field of polymer material synthesis, in particular to a fluorine-containing nano-SiO with photo-initiating activity 2 Preparation method of microspheres and nano-SiO 2 . Background technique [0002] The light-curing system mainly includes various oligomers, functionalized monomers and various photoinitiator systems, etc., and has been widely used in various light-curing coatings, photoresists, light-curing inks, electronic packaging materials, adhesives, etc. Mixtures, CD replication, paper glazing and other fields, showing good prospects for development. [0003] The main function of the photoinitiator in this system is to absorb ultraviolet light or visible light radiation energy, so that oligomers and diluents can be rapidly converted from liquid substances to solid compounds. At present, the photoinitiator systems that have been successfully developed and applied can be mainly divided into: (1) free radical photoini...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to view more

Application Information

Patent Timeline
no application Login to view more
IPC IPC(8): C09C1/28C09C3/08C09D163/10C09D7/62
CPCC01P2004/64C08K2201/011C09C1/28C09C3/08C09D7/62C09D163/10C08J9/06C08J9/04C08K3/36
Inventor 聂俊李三保朱晓群王群璎
Owner 安庆北化大科技园有限公司
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Try Eureka
PatSnap group products