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Novel siliceous macro-molecule photoinitiator and its preparation method

A photoinitiator and macromolecular technology, which is applied in the synthesis of new silicon-containing macromolecular photoinitiators, can solve the problems of easy migration, poor compatibility, and toxicity of small molecule photoinitiators, and achieve low mobility and heat resistance. High performance and good photoinitiating activity

Inactive Publication Date: 2012-04-11
BEIJING UNIV OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] In order to improve the toxicity, easy migration and poor compatibility of small molecule photoinitiators, the object of the invention provides a kind of novel silicon-containing macromolecular photoinitiator whose general formula is (I) and its synthesis method

Method used

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  • Novel siliceous macro-molecule photoinitiator and its preparation method
  • Novel siliceous macro-molecule photoinitiator and its preparation method
  • Novel siliceous macro-molecule photoinitiator and its preparation method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Synthesis of 1173-PMHS macromolecular photoinitiator

[0024] Add 16.40g (0.1mol) of 1173 (2-methyl-2-hydroxy-1-phenyl-1-propanone), 6.25g of hydrogen-containing silicone oil (hydrogen content 1.6mol / 100g), and 50ml of tetrahydrofuran into a three-necked flask , blow nitrogen, drop 0.04g catalyst tetramethylammonium hydroxide after 5min, stir at room temperature for 20min, gradually raise the temperature to 50°C, after constant temperature reaction for 8h, reduce the pressure to 1.33kPa and rotary steam to 130°C to remove solvent and unreacted 1173, a transparent product was obtained.

[0025] Depend on figure 1 It can be seen that at 3453cm -1 The place is the largest absorption peak of C-OH in raw material 1173, at 3066-2868cm -1 The stretching vibration absorption peak of the characteristic C-H of phenyl, 1674cm -1 It is the characteristic absorption peak of carbonyl; from the comparison of the infrared spectrum of the product, it can be seen that the absorption ...

Embodiment 2

[0029] Synthesis of 185-PMHS macromolecular photoinitiator

[0030] 22.10g (0.1mol) 185 (2-methyl-2-hydroxyl-1-(4-tert-butyl)phenyl-1-propanone), 35.0g hydrogen-containing silicone oil (hydrogen content 0.18mol / 100g), Add 50ml of tetrahydrofuran into the three-necked flask, pass nitrogen gas, drop in 0.05g of catalyst tetramethylammonium hydroxide after 5min, stir at room temperature for 20min, gradually raise the temperature to 60°C, and react at constant temperature for 8h, reduce the pressure to 1.33kPa and rotate to 130 The solvent and unreacted 185 were removed at ℃ to obtain a transparent product.

[0031] Its structural formula is as follows:

[0032]

Embodiment 3

[0034] Synthesis of 184-PMHS macromolecular photoinitiator

[0035] Add 20.40g (0.1mol) of 184 (1-hydroxy-cyclohexyl-phenyl ketone), 40.0g of hydrogen-containing silicone oil (hydrogen content 0.18mol / 100g), and 60ml of tetrahydrofuran into a three-necked flask, blow nitrogen, and after 5min Add 0.07g of catalyst tetramethylammonium hydroxide dropwise, stir at room temperature for 20min, gradually raise the temperature to 70°C, and react at constant temperature for 8h, reduce the pressure to 1.33kPa and rotary evaporate to 130°C to remove the solvent and unreacted 184 to obtain a transparent product .

[0036] Its structural formula is as follows:

[0037]

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Abstract

The invention discloses a novel siliceous macro-molecule photoinitiator and its preparation method, which belongs to the free radical photoinitiator field. A structural formula R1 of the photoinitiator is benzoin group with hydroxyl, benzoin ethers group, benzophenone and camphorquinone group; R2 is C1-C8 alkyl; N=3-500, x=1-50, y=1-50. The preparation method comprises the following steps: adding a mixture of hydrogen-containing silicone oil and a solvent in a reactor, adding a micromolecule photoinitiator, introducing nitrogen for 5 minutes, adding 0.3-1 mass part of catalyst, stirring at room temperature for 20 minutes; gradually heating to the temperature of 50-70 DEG C, reacting at constant temperature for 5-8 hours; pressure reducing and carrying out rotary evaporation to remove the solvent and unreacted micromolecule photoinitiator after the reaction is completed to obtain the siliceous macro-molecule photoinitiator. The siliceous macro-molecule photoinitiator has excellent fluidity, dissolvability and excellent reactivity.

Description

technical field [0001] The invention relates to the synthesis of a novel silicon-containing macromolecule photoinitiator, which belongs to the field of polymer material synthesis; meanwhile, the material is a photosensitive macromolecule material, and belongs to the field of free radical photoinitiators. Background technique [0002] Due to the advantages of high efficiency, energy saving and environmental protection, photopolymerization and photocuring technology can be used especially in some heat-sensitive places. Photopolymerization is the use of light as the reaction power, through the light acting on the photosensitive compound, so that a series of photophysical and photochemical reactions occur, and active substances are synthesized, thereby initiating the polymerization of active monomers, and finally converting the liquid resin into a solid state polymer materials. Photoinitiator is an important part of photopolymerization or photocuring system, which not only affe...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F2/48C08G77/38C08G77/12
Inventor 张军营甘禄铜
Owner BEIJING UNIV OF CHEM TECH