Liquid crystal alignment agent containing polyamic acid ester and polyamic acid, and liquid crystal alignment film
A technology of liquid crystal alignment agent and polyamic acid ester, which is applied in the direction of instruments, optics, nonlinear optics, etc., can solve the problems of high volume resistivity, unknown improvement of liquid crystal alignment agent characteristics, and large residual charge, etc., to achieve improved electrical characteristics , fine unevenness reduction, whitening reduction effect
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[0185] Examples are given below to further specifically illustrate the present invention. However, the present invention is not construed as being limited to these Examples.
[0186] The abbreviations used in Examples and Comparative Examples and the measurement methods of each characteristic are as follows.
[0187] 1,3DMCBDE-Cl: dimethyl 1,3-bis(chlorocarbonyl)-1,3-dimethylcyclobutane-2,4-dicarboxylate
[0188] ODA: 4,4'-diaminodiphenyl ether
[0189] BDA: 1,2,3,4-butanetetracarboxylic dianhydride
[0190] CBDA: 1,2,3,4-cyclobutanetetracarboxylic dianhydride
[0191] NMP: N-methyl-2-pyrrolidone
[0192] γ-BL: γ-butyrolactone
[0193] BCS: Butyl Cellosolve
[0194] PAE: polyamic acid ester
[0195] PAA: polyamic acid
[0196] 【Chemical 32】
[0197]
[0198] [viscosity]
[0199] In the synthesis example, the viscosity of the polyamic acid ester and the polyamic acid solution was measured using an E-type viscometer TVE-22H (manufactured by Toki Sangyo Co., Ltd. (To...
Synthetic example 1
[0239] A 300-ml four-neck flask equipped with a stirring device was set in a nitrogen atmosphere, 8.0129 g (40.02 mmol) of ODA, 157.25 g of NMP, and 7.13 g (90.13 mmol) of pyridine as a base were added and stirred to dissolve. Next, stirring this diamine solution, 12.2295 g (37.61 mmol) of 1,3DM-CBDE-Cl was added, and it was made to react under water cooling for 4 hours. The obtained polyamic acid ester solution was added to 1747g of water while stirring, and the precipitated white precipitate was removed by filtration, followed by washing once with 1747g of water, once with 1747g of ethanol, and three times with 437g of ethanol , obtained by drying 16.65g of white polyamic acid ester resin powder. The yield is 95.3%. In addition, the molecular weight of this polyamic acid ester is Mn=13104, Mw=29112.
[0240] The obtained polyamic acid ester resin powder of 1.8731g was taken in the Erlenmeyer flask of 50 ml, NMP of 16.89g was added, it stirred and melt|dissolved at room tem...
Synthetic example 2
[0242] A 300-ml four-necked flask equipped with a stirring device was set in a nitrogen atmosphere, 7.0154 g (35.03 mmol) of ODA, 140.77 g of NMP, and 6.50 g (82.22 mmol) of pyridine as a base were added and dissolved by stirring. Next, stirring this diamine solution, 11.1392 g (34.26 mmol) of 1,3DM-CBDE-Cl was added, and it was made to react under water cooling for 4 hours. The obtained polyamic acid ester solution was added to 1564g of water while stirring, and the precipitated white precipitate was removed by filtration, followed by washing once with 1564g of water, once with 1564g of ethanol, and three times with 391g of ethanol , obtained 14.33g of white polyamic acid ester resin powder through drying. The yield was 91.6%. Moreover, the molecular weight of this polyamic acid ester is Mn=24228, Mw=61076.
[0243] The obtained polyamic acid ester resin powder of 1.7324g was taken in the Erlenmeyer flask of 50 ml, NMP of 15.65g was added, it stirred and dissolved at room t...
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