Liquid crystal alignment agent, liquid crystal display element, and manufacturing method of liquid crystal display element
A technology of liquid crystal display element and liquid crystal alignment agent, applied in liquid crystal materials, chemical instruments and methods, optics, etc., can solve the problems of uneven ODF, uneven display, etc., and achieve favorable product qualification rate, excellent vertical alignment, excellent Effect of Vertical Orientation Constraint
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[0496] The present invention will be further specifically described below through examples, wherein the present invention is not limited by these examples. In the following, the weight average molecular weight of the polyorganosiloxane polymer was evaluated by the following method.
[0497] [Weight average molecular weight]
[0498] The weight-average molecular weight of the polyorganosiloxane polymer was obtained from the results of gel permeation chromatography measurement under the following conditions using the following apparatus, and is a polystyrene-equivalent value using monodisperse polystyrene as a standard substance.
[0499] Measuring device: manufactured by Tosoh Corporation, model "8120-GPC"
[0500] Column: manufactured by Tosoh Corporation, "TSKgelGRCXLII"
[0501] Solvent: THF
[0502] Sample concentration: 5% by weight
[0503] Sample injection volume: 100μL
[0504] Column temperature: 40°C
[0505] Column pressure: 68kgf / cm 2
[0506]
Synthetic example A-1
[0508] In a reaction vessel equipped with a stirrer, a thermometer, a dropping funnel, and a reflux condenser, 13.9 g of oxalic acid and 19.5 g of ethanol were added and stirred to prepare an ethanol solution of oxalic acid. Then, the solution was heated to 70° C. under a nitrogen atmosphere, and a mixture of 15.1 g of tetraethoxysilane and 1.6 g of vinyltriethoxysilane as raw material silane compounds was added dropwise thereto. After the dropwise addition was completed, it was kept at a temperature of 70° C. for 6 hours, then cooled to 25° C., and then 40.0 g of butyl cellosolve was added to obtain a polyorganosiloxane (A) containing polyorganosiloxane ( A-1) solution.
[0509] The polyorganosiloxane (A-1) contained in this solution had a weight average molecular weight Mw of 12,000.
Synthetic example A-2~A-10
[0511] In the above-mentioned Synthesis Example A-1, the type and amount of the silane compound used as a raw material, and the amounts of oxalic acid and ethanol used are respectively set as described in 1 of Table 1, and the above-mentioned synthesis method is followed in addition. Solutions containing polyorganosiloxanes (A-2) to (A-10) as polyorganosiloxanes (A) were prepared in the same manner as in Example A-1.
[0512] In synthesis examples A-7 and A-8, two kinds of silane compounds (a2-3) were used.
[0513] The weight-average molecular weight Mw of each polyorganosiloxane contained in each solution is shown together in Table 1-1, and synthesis examples A-9 and A-10 are reference synthesis examples.
[0514]
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