Preparation method and application of modified titanium dioxide serving as photoinitiator

A titanium dioxide, modification technology, applied in applications, home appliances, coatings, etc., can solve the problems of poor load modification efficiency, reduced fire safety and environmental protection, and insufficient efficiency of titanium dioxide photoinitiators to achieve initiation efficiency Enhanced effect

Active Publication Date: 2021-05-14
SUN YAT SEN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

According to existing research reports, when the surface of titanium dioxide is directly modified with long-chain fatty acids such as oleic acid, palmitic acid, stearic acid, and palmitic acid, because these fatty acids are oily low surface energy liquids or oily solids, titanium dioxide powder It is difficult to disperse directly, resulting in poor loading modification efficiency. Generally, it is better to disperse titanium dioxide and achieve surface modification after diluting with a slightly polar solvent, such as ethanol, acetone, etc.
However, the use of a large amount of organic solvents will lead to a decrease in fire safety and environmental protection, and the carboxylic acid @TiO obtained by direct and simple modification of fatty acids 2 Titanium dioxide, its light-induced curing efficiency is far from meeting the requirements of the application, and its independent light-induced acrylate polymerization conversion rate is generally only 5-10%, and the white paint formula still needs to be combined with more than 2% TPO photoinitiator to achieve The requirement of complete curing indicates that the performance of this modified titanium white photoinitiator is not high enough and needs further improvement

Method used

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  • Preparation method and application of modified titanium dioxide serving as photoinitiator
  • Preparation method and application of modified titanium dioxide serving as photoinitiator
  • Preparation method and application of modified titanium dioxide serving as photoinitiator

Examples

Experimental program
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Effect test

Embodiment 1

[0044] Embodiment 1 titanium dioxide fluoride (FTiO 2 ) preparation

[0045] Accurately weigh 10.00g TiO 2 (anatase-type titanium dioxide with bare particle surface and without any surface-coated modification substances, D 50 The primary particle size is 0.3-1.2μm), 10.00gNH 4 F, dissolved in 150mL deionized water, ultrasonic (200W) vibration to disperse the agglomerated TiO 2 Particles until the particle size of the titanium dioxide scraper is less than 2.5 μm. Then magnetically stir (960rpm) at room temperature for 6h, absorb the white milk slurry and centrifuge (10500rpm) for 5min, pour off the supernatant, wash with deionized water, and ultrasonically (200W) shake for 10min after washing, then centrifuge (10500rpm) for 5min, pour Remove the supernatant, wash with deionized water, and repeat the above ultrasonic-centrifugation operation 3 times to remove unadsorbed NH 4 F; Finally, the above product was vacuum-dried in an oven at 65°C for 6 hours to obtain fluorinated ...

Embodiment 2

[0048] Example 2 hippuric acid @FTiO 2 preparation of

[0049] Accurately weigh the fluorinated TiO of 10.00g embodiment 2 , 15.00g hippuric acid, dissolved in 150mL deionized water, ultrasonic (200W) vibration disperse the agglomerated TiO 2 Particles until the particle size of the titanium dioxide scraper is less than 2.5 μm. Then magnetically stir (960rpm) at 60°C for 6h, absorb the white milk slurry and centrifuge (10500rpm) for 5min, pour off the supernatant, wash with deionized water, and ultrasonically (200W) shake for 10min after washing, then centrifuge (10500rpm) for 5min. Pour off the supernatant, wash with deionized water, and repeat the above ultrasonic-centrifugation operation 3 times to remove unadsorbed glycine; finally, vacuum-dry the above product in an oven at 65°C for 6 hours to obtain hippuric acid@FTiO 2 .

[0050] To get hippurate @FTiO 2 Carried out XPS detection, particle surface element binding energy signal analysis showed that for C 1s Perform...

Embodiment 3

[0051] Example 3 Citric acid@FTiO 2 preparation of

[0052] Accurately weigh the fluorinated TiO of 10.00g embodiment 1 2 , 15.00g citric acid, dissolved in 150mL deionized water, ultrasonic (200W) vibration to disperse the agglomerated TiO 2 Particles until the particle size of the titanium dioxide scraper is less than 2.5 μm. Then magnetically stir (960rpm) at 60°C for 6h, absorb the white milk slurry and centrifuge (10500rpm) for 5min, pour off the supernatant, wash with deionized water, and ultrasonically (200W) shake for 10min after washing, then centrifuge (10500rpm) for 5min. Pour off the supernatant, wash with deionized water, and repeat the above-mentioned ultrasonic-centrifugation operation 3 times to remove unadsorbed carboxylic acid. Finally, the above product was vacuum-dried in an oven at 65°C for 6h to obtain citric acid@FTiO 2 .

[0053] to the resulting citric acid @FTiO 2 Carried out XPS detection, particle surface element binding energy signal analysis...

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Abstract

The invention belongs to the technical field of photocuring materials, and particularly relates to a preparation method and application of modified titanium dioxide serving as a photoinitiator, a Ti-OH bond structure on the surface of a titanium dioxide particle is converted into a Ti-F bond structure, then the Ti-F bond structure on the surface of the titanium dioxide particle is converted into a titanium-carboxylic ester structure, and thus, the modified titanium dioxide is prepared. The prepared modified titanium dioxide has remarkable activity of photo-initiation of polymerization and crosslinking of acrylate monomers or/and resin, and can be used as a photoinitiator to be applied to the photo-curing fields of white photo-curing coatings, printing ink and the like.

Description

technical field [0001] The invention belongs to the technical field of photocurable materials, and in particular relates to a preparation method and application of modified titanium dioxide as a photoinitiator. Background technique [0002] Photocuring is a material processing technology based on monomers or resins containing specific groups. Under the synergy of photoinitiators and ultraviolet radiation, a material processing technology that can quickly polymerize, crosslink and cure, the mechanism includes free radical photocuring and For cationic photocuring, the so-called specific groups generally refer to (meth)acrylate or epoxy groups. Light-curing coatings, inks, and adhesives developed based on light-curing technology do not contain solvents and cure very quickly. They have the advantages of environmental protection, high efficiency, and energy saving, and represent the development direction of global coatings and inks. White light-curing coatings and inks colored w...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F2/48C08F122/14C09D4/02C09D11/101
CPCC08F2/48C08F122/1006C09D4/00C09D11/101
Inventor 黄俊威曾兆华杨建文
Owner SUN YAT SEN UNIV
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