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Free radical and cation hybridized trigger for optical solidification and its preparing process and application

A technology of photocuring initiators and cations, applied in organic chemistry and other fields, can solve the problems of less types of initiators, severe volume shrinkage, and long process routes

Inactive Publication Date: 2002-10-30
XIANGTAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Its disadvantages are: 1. After curing, the volume shrinks severely, which reduces the adhesion; 2. Oxygen in the air has a polymerization inhibition effect, which affects the degree of polymerization and molecular weight; 3. There is no post-curing effect, and those dead angles that cannot be irradiated by ultraviolet lamps Can not be cured
But cations also have disadvantages: 1. The curing speed is slow; 2. The water in the system hinders the curing; 3. There are few types of initiators, and there are few applicable monomers.
[0008] This makes the synthesis of this compound quite difficult, and the operational route is long, and productive rate is low (total yield rate is 9.8%), and will consume a large amount of silver salts, and its cost is quite high
Especially due to the strong electron-withdrawing effect of iodide cations, the oxidation step is quite difficult, and it takes a long time to reflow to complete

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] Add 2.58g 4-C to the two-neck round bottom flask 6 h 5 COC 6 h 4 C 6 h 5 , 3.60g C 6 h 5 I(OCOCH 3 ) 2 , 10ml of acetic anhydride, add dropwise a solution of 10.0ml of concentrated sulfuric acid and 6ml of acetic anhydride under cooling and stirring in an ice bath, stir for 0.5 hours, then heat and stir in a water bath at 45-55°C for 4 hours, cool the reaction mixture, add into 20ml of water, suction filtered to obtain the filtrate, the filtrate was washed twice with n-hexane and diethyl ether, and 2.6g of KPF was added to the filtrate under vigorous stirring 6 In 30ml of aqueous solution, a large amount of white solid was formed, which was filtered, washed with a small amount of distilled water, and dried in vacuum at 50°C to obtain the product 4-PhCOC 6 h 4 C 6 h 4 I + Ph PF 6 - 4.15 g, 68.5% yield. Product melting point: 154-158°C, 1 HNMR (CDCl 3 , TMS) δ / ppm: 8.05-8.15 (4H, m, 11, 13, 14, 18Ar-H), 7.78-7.88 (4H, m, 1, 5, 6, 8Ar-H), 7.49-7.72 (10H ...

Embodiment 2

[0039] Add 2.74g 4-C to a two-neck round bottom flask 6 h 5 COC 6 h 4 OC 6 h 5 , 3.22g C 6 h 5 I(OCOCH 3 ) 2 , 12ml of acetic anhydride, add dropwise a mixed solution of 3ml of acetic anhydride and 12ml of concentrated sulfuric acid under ice-bath cooling and stirring, after stirring for 0.5 hours, then heat in a 40-50°C water bath, stir for 4 hours, cool, and the reaction mixture Pour it into water, filter with suction to get the filtrate, wash the filtrate twice with n-hexane and ether, add 2.6g of KPF dissolved in the filtrate under vigorous stirring 6 In 30ml of aqueous solution, a large amount of white solid was formed, which was filtered, washed with a small amount of distilled water, and dried under vacuum at 50°C to obtain the product 4-C 6 h 5 COC 6 h 4 OC 6 h 4 I + C 6 h 5 PF 6 - 2.31 g, 38% yield.

Embodiment 3

[0041] Add 2.58g of 4-PhCOPhOCH in a two-neck round bottom flask 2 CH 2 Oph, 3.22g PhI (OCOCH 3 ) 2 16ml of acetic anhydride, add dropwise a mixed solution of 2ml of acetic anhydride and 16ml of concentrated sulfuric acid under cooling and stirring in an ice bath, stir for 1.5 hours, then heat in a water bath at 70-75°C, stir for 3 hours, and then let it cool Then add water, filter with suction to get the filtrate, wash the filtrate twice with n-hexane and ether, add 2.6g of KPF dissolved in the filtrate under vigorous stirring 6 In 30ml of aqueous solution, a large amount of white solid was formed, which was filtered, washed with a small amount of distilled water, and dried under vacuum at 50°C to obtain the product 4-PhCOPhOCH 2 CH 2 OPhI + Ph PF 6 - 4.30 g, 71% yield.

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PUM

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Abstract

A hybridized free radical-cation trigger for optical solidification features that it contains both free radical trigger and cation trigger, so it can be used for the cation-type or free radical-type optical solidifying systems. Its advantages are high triggering performance, and simple preparing process.

Description

Technical field [0001] The invention relates to a novel hybrid photoinitiator and its preparation method and application. The compound has a dual structure of a free radical photoinitiator and a cationic photoinitiator. Background technique [0002] At present, radiation curing technology is widely used in coatings, inks, printing plate making, dental restoration and optical disc manufacturing and other fields. Compared with traditional curing technology, light curing technology has incomparable advantages such as environmental friendliness, energy saving, short time, fast curing, easy operation, etc., so it has been developed rapidly. Especially in recent years, the voice of eliminating pollution and protecting the environment has become higher and higher, and the light curing technology has shown its strong vitality. [0003] Photocuring of polymer monomers or prepolymers must use photoinitiators. According to its initiation mechanism, it can be divided into cationic pho...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C49/807C08F4/32
Inventor 阳年发曹靖杨利文
Owner XIANGTAN UNIV
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