A kind of photoinitiator and preparation method thereof
A technology of photoinitiator and alkoxy group, applied in the field of photocuring, can solve the problem of difficult introduction of reactive groups, and achieve the effects of complete reaction, consumption saving and permeability inhibition.
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Embodiment 12
[0046] The preparation of embodiment 12,4,6-trimethylbenzoylphenylphosphonic acid
[0047] Only the commonly used preparation methods for 2,4,6-trimethylbenzoylphenylphosphonic acid are given below.
[0048] Add 80ml butanone-2 into the three-necked flask, take 31.6g (0.1mol) ethyl 2,4,6-trimethylbenzoylphenylphosphonate and mix it, add 15g (0.1mol) of sodium iodide, Stir and heat to 65°C. During the reaction, precipitates are continuously precipitated. React for 24 hours. After cooling, filter and separate. The liquid is a mixture of butanone-2 and ethyl iodide, which can be used for other purposes after fractional distillation. The resulting solid was washed with acetone, dried, dissolved in 150ml of deionized water, and the solution was acidified with 1M sulfuric acid to adjust the pH value to 1. After standing for several hours, the substituted aroylphenylphosphonic acid precipitated and crystallized completely. , filtered, washed with water, and dried in vacuum. The pro...
Embodiment 2
[0050] Add 80ml of toluene and 28.8g (0.1mol) of 2,4,6-trimethylbenzoyl-phenylphosphonic acid into the three-neck flask, stir and heat to 60°C until the substituted phosphonic acid is completely dissolved. Add 18.3g novolak epoxy resin F-51 (epoxy equivalent 182, average epoxy functionality 3.4, product from Wuxi Resin Factory), continue to stir and react at 60°C for 3 hours, and the acid value has dropped to 3.2mgKOH / g by sampling. Indicating that the reaction tended to be complete, the solvent was evaporated under reduced pressure to obtain 45.6 g of viscous macromolecular photoinitiator. Infrared spectrum detection shows that the raw epoxy resin is 913cm -1 The characteristic absorption peak of the epoxy group disappears. The number average molecular weight of the raw material novolak epoxy resin F-51 measured by GPC is 580; the number average molecular weight of the phosphonated product is 1670, and the molecular weight dispersion is 1.23.
Embodiment 3
[0052] Same as Example 1 step, just replace 18.3g polyfunctional epoxy compound novolac epoxy resin F-51 in Example 1 with 20.0g o-cresol novolac epoxy resin NPCN-702 (produced by Taiwan Nanya Resin Company, epoxy The equivalent weight is 197, the average epoxy functionality is 3.7), stirred and reacted at 65°C for 3 hours, the acid value has dropped to 4.1mgKOH / g by sampling, indicating that the reaction is becoming complete, and the solvent is evaporated under reduced pressure to obtain a semi-solid macromolecule Photoinitiator 46.8g. Infrared spectrum detection shows that the raw epoxy resin is 913cm -1 The characteristic absorption peak of the epoxy group disappears. GPC records the number average molecular weight of the raw material o-cresol novolac epoxy resin NPCN-702 is 670; the number average molecular weight of the phosphonated product is 1820, and the molecular weight dispersion is 1.29.
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