Pyridinium salt photoinitiator as well as preparation method and application thereof
A technology of photoinitiator and pyridinium salt, applied in the field of photoinitiator, can solve the problem of easy yellowing of odor polymers, achieve good initiation efficiency, simplify production process, and reduce the use of chemicals
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Embodiment 1
[0045] Embodiment 1: the synthesis of pyridinium salt photoinitiator P1
[0046] The synthetic route of P1 is as follows figure 1 shown.
[0047] Step 1, 3.04g 4-methoxy salicylaldehyde (20mmol) and 3.8ml ethyl acetoacetate (30mmol) were dissolved in 30ml ethanol, 40ul piperidine (0.39mmol) and four drops of glacial acetic acid were added in the solution, Stir and reflux at 80°C. The reaction was monitored by a TLC plate, and after the salicylaldehyde was completely consumed, the mixture was cooled to room temperature, and then the reaction system was filtered to obtain product A as a yellow solid. Yield 86%.
[0048]
[0049] In step 2, 2.18 g of yellow solid product A (10 mmol) was dissolved in 20 ml of chloroform and added to a round bottom flask. Insert a long needle into the bottom of the liquid bromine bottle to absorb 1.6g of liquid bromine (10mmol) into the dropping funnel, then add 5mL of chloroform to dissolve it, and slowly drop it into the round bottom flask...
Embodiment 2
[0054] Example 2: Performance testing of P1
[0055] 1. UV-visible absorption test: preparation 7.4×10 -5 The mol / L acetonitrile solution of P1 prepared in Example 1 was tested for UV-Vis absorption by a TU1901 UV-Vis spectrophotometer from Lambda Corporation of Japan. UV-Vis absorption spectrum such as image 3 shown by image 3 It can be seen that the photoinitiator has absorption at 365nm and 405nm, indicating that the photoinitiator of the present invention can be used as a photoinitiator in the ultraviolet-visible region.
[0056] 2. Photolysis test: Prepare 7.4×10 -5 The acetonitrile solution of P1 prepared in mol / L embodiment 1, get 3mL in the quartz cuvette, add magneton. Use the RUNLED-UVP60 type 405nm point light source to irradiate, fix the distance between the point light source fiber and the cuvette, and use the blue light irradiation meter to measure the radiation power at the cuvette to be 150mW / cm 2 . The ultraviolet-visible absorption was measured with ...
Embodiment 3
[0057] Embodiment 3: P1 polymerization kinetics test
[0058] 1. Tripropylene glycol diacrylate (TPGDA) free radical polymerization kinetics test.
[0059] Such as Figure 5 Shown is the real-time conversion rate curve of TPGDA double bond polymerization initiated by the P1 photoinitiator prepared in Example 1.
[0060] Specific implementation method: add 1wt% pyridinium salt photoinitiator P1 to the resin tripropylene glycol diacrylate (TPGDA), and obtain a uniform mixed resin by mechanical stirring and ultrasonic mixing. It was coated between two layers of KBr salt flakes and subsequently tested. Using Nicolet 6700 real-time infrared spectrometer (spectrum range: 500 ~ 4000cm -1 , resolution 8cm -1 ) to monitor the change of infrared absorption of the group with time during the process of initiating polymerization, and to study the polymerization kinetics by monitoring the reduction of double bonds in TPGDA. The conversion rate is calculated by the following formula.
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