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A kind of preparation method and application of modified titanium dioxide as photoinitiator

A titanium dioxide and modification technology, which is applied in the field of preparation of modified titanium dioxide, can solve the problems of poor loading modification efficiency, insufficient efficiency of titanium dioxide photoinitiator, and efficiency that cannot meet the requirements of the application, and achieve the goal of improving the initiation efficiency Effect

Active Publication Date: 2022-04-15
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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  • A kind of preparation method and application of modified titanium dioxide as photoinitiator
  • A kind of preparation method and application of modified titanium dioxide as photoinitiator
  • A kind of preparation method and application of modified titanium dioxide as photoinitiator

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0044] Example 1 Fluorinated titanium powder (FTIO 2 Preparation

[0045] Accurate weighing 10.00g TiO 2 (Naked the surface of the particles, there is no surface-containing anatase-containing modified substance, Di-titanium titanium dioxide, D 50 The original particle size is 0.3-1.2 μm), 10.00GNH 4 F, dissolved in 150 ml of deionized water, ultrasound (200W) oscillation of dispersed TiO 2 Particles until the titanium white powder scraper particle diameter is less than 2.5 μm. The medium temperature magnetic force was then stirred (960 rpm) for 6 h, and the white lasu liquor cence (10500 rpm) was taken for 5 min, poured down, washed with deionized water, after washing (200W) oscillated for 10 min, then centrifugation (10500 rpm) for 5 min, fell To the supernatant, washed with deionized water, the above-mentioned ultrasound-centrifugal operation was repeated 3 times to remove unscapable NH 4 F; Finally, the above product was dried in a 65 ° C oven for 6 h to give a fluorinated TiO ...

Embodiment 2

[0048] Example 2 Male uric acid @ftio 2 Preparation

[0049] Exactly weighs 10.00 g of fluorinated TiO 2 , 15.00g of mission, dissolved in 150 ml of deionized water, ultrasound (200W) oscillation dispersion reunion TiO 2 Particles until the titanium white powder scraper particle diameter is less than 2.5 μm. Then 60 ° C magnetic stir (960 rpm) for 6 h, and the white lasu liquor centrifugation (10500 rpm) was taken for 5 min, and the supernatant was poured, washed with deionized water. After washing, the ultrasound (200W) was oscillated for 10 min, and then centrifuged (10500 rpm) was separated for 5 min. Pour the supernatant, washed with deionized water, the above ultrasound-centrifugal operation was repeated 3 times to remove unscaded glycine; 2 .

[0050] Get the acquired murret @ftio 2 Perform XPS detection, the particle surface element binding energy signal analysis shows that 1s Performing a peak fitting, a C-C signal appears at 284.8EV, a C-O signal appears at 286.3EV, and a...

Embodiment 3

[0051] Example 3 Citric acid @ftio 2 Preparation

[0052] Accurate weighing 10.00 g of the fluorinated TiO 2 , 15.00g of citric acid, dissolved in 150 mL deionized water, ultrasound (200W) oscillating dispersion reunion TiO 2 Particles until the titanium white powder scraper particle diameter is less than 2.5 μm. Then 60 ° C magnetic stir (960 rpm) for 6 h, and the white lasu liquor centrifugation (10500 rpm) was taken for 5 min, and the supernatant was poured, washed with deionized water. After washing, the ultrasound (200W) was oscillated for 10 min, and then centrifuged (10500 rpm) was separated for 5 min. The supernatant was pressed, washed with deionized water, and the above ultrasound-centrifugal operation was repeated 3 times to remove unscaptive carboxylic acids. Finally, the above product was vacuum 6 h in a 65 ° C oven to give citric acid @ftio 2 .

[0053] Getting citric acid @ftio 2 Perform XPS detection, the particle surface element binding energy signal analysis show...

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Abstract

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. The invention first converts the Ti-OH bond structure on the surface of the titanium dioxide particle into a Ti-F bond structure , and then transform the Ti-F bond structure on the surface of the titanium dioxide particles into a titanium-carboxylate structure, thereby preparing the modified titanium dioxide. The prepared modified titanium dioxide has significant activity of photoinitiating the polymerization and crosslinking of acrylate monomers or / and resins, and can be used as a photoinitiator in the photocuring fields of white photocurable coatings and inks.

Description

Technical field [0001] The present invention belongs to the technical field of photocurable materials, and more particularly to the preparation method of modified titanium white powder as a photoinitiator. Background technique [0002] Light curing is based on a monomer or resin containing a particular group, under synergistic action of the photoinitiator, a material processing technique for rapidly aggregating cross-linkage is rapidly aggregated by ultraviolet radiation, and the mechanism includes free radical light curing and Censored, so-called specific groups generally refer to (meth) acrylate or epoxy group. Based on photocurable coating, ink, ink, adhesives developed by photocurable techniques, and has a global coating and ink development direction due to dissolving without solvents. White photocurable coatings colored with titanium powder, ink, due to a higher proportion of titanium powder contained in its formulation, and titanium white powder can absorb most ultraviolet ...

Claims

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Application Information

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Patent Type & Authority Patents(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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