A kind of α-hydroxyalkyl phenyl ketone photoinitiator and its preparation method and application
A technology of hydroxyalkyl phenyl ketone and photoinitiator, which is applied in the field of a-hydroxyalkyl phenyl ketone photoinitiator and its preparation, can solve the problem of poor interface adhesion and polymerization transformation of methionate monomer Incomplete and other problems, to achieve the effect of guaranteeing adhesion, reducing the content of free photoinitiators, and improving the cross-linked network
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Embodiment 1
[0024] Dissolve 19.0g (0.1mol) of purified p-toluenesulfonyl chloride in 50ml of dry toluene, add 8.2g of pyridine, cool the reaction flask to below 2°C in an ice-water bath, add 10.1g (0.11mol) of methylthioethanol, and stir magnetically Reacted for 4 hours, and filtered by cold to remove the solid pyridine hydrochloride. Add 22.2g of 4-(2-hydroxyl-2-methylpropionyl)phenol sodium salt, 50ml of deionized water, and 2.3g of trimethylhexadecylammonium chloride to the above toluene solution, stir mechanically rapidly, and heat to 80 ℃, reacted for 6 hours, cooled, separated, collected the toluene layer, washed 3 times with deionized water, dried the toluene solution, concentrated it to about one-third of the original volume by distillation under reduced pressure, and refrigerated overnight at -10°C to precipitate a crystalline product. It was quickly filtered by cooling and dried to obtain 20.8 g of the product. H NMR detection (CDCl 3 , δppm) 1.59 (6H, s), 2.21 (3H, s), 2.88 (...
Embodiment 2
[0026] Same as Example 1, change 10.1g (0.11mol) methylthioethanol to 11.7g (0.11mol) 3-methylthiopropanol. 23.7 g of product were obtained. H NMR detection (CDCl 3 , δppm) 1.56 (6H, s), 2.23 (3H, s), 2.30 (2H, m), 2.86 (2H, t), 4.21 (2H, t), 6.99 (2H, d), 7.75 (2H, d ); Raw material 3-methylthiopropanol signal appears in the proton nuclear magnetic spectrum, compares through area integration, calculates the mol ratio of target compound and remaining raw material methylthioethanol in the product to be 1:0.04. GC-MS: M + 268. The uncorrected product was 96% pure by chromatography.
Embodiment 3～4
[0027] Embodiment 3~4 and comparative example 1
[0028] Take light-curable resin, reactive diluent, and photoinitiator, mix them evenly, and prepare a test formula for light-curable coatings, coat them on a stainless steel sheet, control the wet film thickness to 25 μm, and irradiate with a 1000W medium-pressure mercury lamp for 10 sec, with a light intensity of 12.6 mW / cm 2(320~400nm). After 24 hours, the adhesion of the cured coating was measured by the 100-gram method, and the smell was tested after the coating was baked at 70°C for 8 hours. The test results are shown in Table 1 below.
[0029] Table 1
[0030]
[0031] Note: B-100 is a conventional epoxy acrylic resin photocuring resin (produced by Guangzhou Boxing Chemical); the Chinese name of TMPTA is trimethylolpropane triacrylate; the Chinese name of TPGDA is tripropylene glycol diacrylate; the Chinese name of HEMA is formazan 2-hydroxyethyl acrylate. The Chinese name of Darocur1173 is 2-hydroxy-2-methyl-1-ph...
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