Benzophenone photoinitiator containing cyclic acetal and method for preparing same

A technology of benzophenone and photoinitiator, which is applied in the field of photoinitiator and its preparation, can solve problems such as restricted application, toxicity and carcinogenicity, and easy yellowing of cured film, so as to reduce yellowing and toxicity, and reduce production cost Low, easy-to-operate effect

Inactive Publication Date: 2012-02-22
HANGZHOU INST OF ADVANCED MATERIAL BEIJING UNIV OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, amine compounds are toxic and carcinogenic, and the cured film caused b

Method used

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  • Benzophenone photoinitiator containing cyclic acetal and method for preparing same
  • Benzophenone photoinitiator containing cyclic acetal and method for preparing same
  • Benzophenone photoinitiator containing cyclic acetal and method for preparing same

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Add 0.02mol (3.96g) of 4-hydroxybenzophenone to 28mL of 37% formaldehyde solution at room temperature, slowly add 150mL of hydrochloric acid and 30mL of phosphoric acid mixed acid solution dropwise for more than 2 hours, and slowly heat up after the dropwise addition , stirred at 48°C for 6 hours, cooled to room temperature, filtered, washed the filter cake with water until neutral, dried, recrystallized with a mixed solvent of ethanol and water (10:3v / v), dried in vacuo to obtain 1,3- Dioxybenzohexane benzophenone 4.15g, yield 86.5%.

Embodiment 2

[0022] Add 0.02mol (3.96g) of 4-hydroxybenzophenone to 28mL of 37% formaldehyde solution at room temperature, slowly add 150mL of hydrochloric acid, 10mL of mixed acid solution of perchloric acid for more than 2 hours, after the dropwise addition Slowly heat up, stir at 50°C for 8 hours, cool to room temperature, filter, wash the filter cake with water until neutral, dry, recrystallize with a mixed solvent of ethanol and water (10:2v / v), and dry in vacuo to obtain 1, 3.24 g of 3-dioxobenzohexane benzophenone, yield 67.5%.

Embodiment 3

[0024] Add 0.02mol (4.24g) of 4-hydroxy-4'methylbenzophenone to 28mL of 37% formaldehyde solution at room temperature, slowly add 100mL of hydrochloric acid and 20g of p-toluenesulfonic acid mixed acid solution for more than 2 hours After the dropwise addition, the temperature was raised slowly, stirred at 10°C for 6 hours, filtered, the filter cake was washed with water until neutral, dried, recrystallized with a mixed solvent of ethanol and water (10:1 v / v), dried in vacuo to obtain 1 , 3.68 g of 3-dioxobenzohexane-4'methylbenzophenone, yield 72.4%.

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Abstract

The invention discloses benzophenonen photoinitiator containing cyclic acetal represented by a below formula and a method for preparing the same. 4-hydroxy benzophenonen or derivative of the 4-hydroxy benzophenonen and methanal as raw materials react for 1 to 10 hours at the temperature of 10 to 70 DEG C with acid water solution as a solvent to obtain the benzophenonen containing cyclic acetal. By introducing cyclic acetal into the benzophenone and due to the fact that the cyclic acetal can be used as assistant igniting agent of the benzophenone, the compound can be used as photoinitiator independently to replace a benzophenonen/amine igniting system so as to reduce xanthochromia and toxicity caused by an assistant amine igniting agent, thereby having wide application prospects in the field of light curing industry.

Description

technical field [0001] The invention belongs to a photoinitiator and a preparation method thereof, in particular to a benzophenone photoinitiator containing cyclic acetal and a preparation method thereof. Background technique [0002] The photopolymerization reaction of multifunctional monomers such as bis(meth)acrylate can quickly form a highly crosslinked polymer network structure. Especially important in areas with high sexual demands. [0003] The photoinitiator is a key component of the photocuring system, which is related to whether the oligomer and diluent of the formulation system can quickly change from liquid to solid when light is irradiated. Its basic function characteristics are: the initiator molecule has a certain light absorption ability in the ultraviolet region (250-400nm) or visible region (400-800nm), after directly or indirectly absorbing light energy, the initiator molecule transitions from the ground state to the excited singlet state , through inter...

Claims

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Application Information

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IPC IPC(8): C08F2/48C07D319/08C07D407/06
Inventor 聂俊马贵平孟准梁鹏总
Owner HANGZHOU INST OF ADVANCED MATERIAL BEIJING UNIV OF CHEM TECH
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