Novel thermal radical generator, method for producing the same, liquid crystal sealing agent, and liquid crystal display cell
A technology of groups and methyl groups, applied in the field of new silyl benzopinacol, can solve the problems of liquid crystal infiltration, leakage and sealing, and contamination of liquid crystals.
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[0172] The present invention will be described in more detail below by way of examples.
[0173] In addition, this invention is not limited to a following example.
[0174] In addition, unless otherwise specified in the Examples, a part means a mass part, and % means a mass %.
Embodiment A
[0176] Synthesis of 1-Hydroxy-2-trimethylsilyloxy-1,1,2,2-tetraphenylethane (Silylated Benzopinacol)
[0177]100 parts (0.28 mol) of commercially available benzopinacol (manufactured by Tokyo Chemical Industry Co., Ltd.) were dissolved in 350 parts of dimethylformaldehyde. 32 parts (0.4 mol) of pyridine as a basic catalyst and 150 parts (0.58 mol) of BSTFA (manufactured by Shin-Etsu Chemical Co., Ltd.) as a silylation agent were added thereto, and the temperature was raised to 70° C., followed by stirring for 2 hours. The obtained reaction liquid was cooled, and 200 parts of water were added, stirring, and the product was precipitated and the unreacted silylating agent was deactivated. The precipitated product was separated by filtration and washed with water sufficiently. Then, the obtained product was dissolved in acetone, and water was added to recrystallize and purify. 105.6 parts of target 1-hydroxy-2-trimethylsilyloxy-1,1,2,2-tetraphenylethane were obtained (yield 88.3...
experiment example 1
[0182] In order to see the effect of the thermal radical generating agent of the present invention, gelation time (time for curing on a hot plate at 120° C.) and foaming test of the sample at 120° C. were implemented.
[0183] (experiment method)
[0184] With respect to 10 parts of acrylic acid adducts of bisphenol A type epoxy resin (manufactured by Nippon Kayaku Co., Ltd.: R93100), in Test Example 1 (this invention), 0.1 part of 1 of the present invention was mixed as a thermal radical generating agent. -Hydroxy-2-trimethylsilyloxy-1,1,2,2-tetraphenylethane; 0.1 part of benzopinacol as a thermal radical generator was mixed in Test Example 2 (comparative use) ; Mix 0.1 part of (2-ethylhexanoic acid) tert-butyl peroxide (manufactured by Kayaku Akuzo Co., Ltd.: カヤエステル O) as a thermal free radical generating agent in Test Example 3 (comparative use), and use a three-roll mill Machine kneading to prepare respective samples.
[0185] The time until the obtained sample was place...
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