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Fluorine-containing nano-sio with photoinitiating activity 2 The preparation method of microsphere and nanometer sio 2

A technology of photoinitiation and photoinitiator, which is applied in the direction of dyeing low molecular organic compound treatment, coating, fibrous filler, etc. It can solve the problems of oxygen inhibition and coating surface properties to be improved, so as to improve stability and gloss Good degree, good weather resistance

Active Publication Date: 2020-11-06
安庆北化大科技园有限公司
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  • 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

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  • Fluorine-containing nano-sio with photoinitiating activity <sub>2</sub> The preparation method of microsphere and nanometer sio <sub>2</sub>
  • Fluorine-containing nano-sio with photoinitiating activity <sub>2</sub> The preparation method of microsphere and nanometer sio <sub>2</sub>
  • Fluorine-containing nano-sio with photoinitiating activity <sub>2</sub> The preparation method of microsphere and nanometer sio <sub>2</sub>

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

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

[0033] (1) Add 100mL of ethanol, 2.5g of ammonia water, and 16.2g of deionized water into a 250mL three-necked flask and stir them evenly. The alcohols are used as the reaction medium. Take 44.274g of trimethoxypropylaminosilane In a constant pressure funnel, add it dropwise to the above mixed solution at room temperature within 1 hour. After the dropwise addition, raise the temperature to 45°C, stir and react for 6 hours to obtain nano-silica microspheres with polymerizable groups on the surface Solution; wherein the concentrations of ammonia, water, and trimethoxypropylaminosilane in the entire solution are 0.9mol / L, 5.52mol / L, and 1.2mol / L, respectively.

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

Embodiment 2

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

[0046] (1) Add 100mL of methanol, 1g of ammonia water, and 10g of deionized water into a 250mL three-necked flask, stir mechanically, and mix evenly. Take 22.137g of trimethoxypropylaminosilane in a constant pressure funnel and add it dropwise Add it to the above mixed solution within 1 hour at room temperature. After the dropwise addition, raise the temperature to 40°C, stir and react for 6 hours to obtain a solution of nano-silica microspheres with polymerizable groups on the surface; ammonia, water, trimethoxy The concentration of propylaminosilane in the whole solution is 0.44mol / L, 4.17mol / L and 0.75mol / L respectively;

[0047] (2) Nitrogen is passed to the nano-silica microsphere solution prepared in step (1), and a constant pressure dropping funnel is used to drop 56.8 g of heptadecylfluorodecyltriethoxysilane to the above soluti...

Embodiment 3

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

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

[0060] (2) Nitrogen is passed to the nano-silica microsphere solution prepared in step (1), and a constant pressure dropping funnel is used to drop 56.8 g of heptadecylfluorode...

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Abstract

The invention discloses fluorine-containing nano-SiO with photoinitiating activity 2 Preparation method of microspheres and nano-SiO 2 , involving the field of polymer material synthesis, based on the existing nano-SiO 2 When it 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. The present invention includes the following steps: preparing fluorocarbon modified nano-SiO with active sites 2 ; The acrylate containing the initiator structure is added to the prepared fluorocarbon modified nano-SiO 2 In the solution, the photoinitiator structure is grafted on the surface of silicon dioxide through Michael addition reaction. The beneficial effect of the present invention is that the preparation method is simple, and the obtained nano-SiO can be improved. 2 The stability of microspheres, adding them into the formula of light-curing coatings, can obtain coatings with high surface hardness, scratch resistance, good gloss, good weather resistance and anti-oxidation and polymerization inhibition. At the same time, the surface of the coating can also Has hydrophobic properties.

Description

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

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F292/00C09C1/28C09C3/08C09D163/10C09D7/62
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
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