Liquid crystal alignment agent, liquid crystal alignment film and liquid crystal display element
A technology of liquid crystal aligning agent and solvent, which is applied in the direction of liquid crystal materials, chemical instruments and methods, instruments, etc., can solve the problems of needing to add structures, etc., and achieve the effect of excellent voltage retention characteristics and excellent linearity
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[0125] Examples are given below to further describe the present invention in detail. However, the present invention is not limited to these Examples.
[0126] In addition, the abbreviations used in the Example and the comparative example, and the measuring method of each characteristic are as follows.
[0127] 1,3DMCBDA: 1,3-Dimethyl 1,2,3,4 cyclobutane tetracarboxylic dianhydride
[0128] CBDA: 1,2,3,4-cyclobutanetetracarboxylic dianhydride
[0129] DA-1: the diamine of the following formula DA-1
[0130] DA-2: the diamine of the following formula DA-2
[0131] DA-3: the diamine of the following formula DA-3
[0132]
[0133] Boc in the above formula DA-2 and the above formula DA-3 represents a tert-butoxycarbonyl group.
[0134]
[0135] NMP: N-methyl-2-pyrrolidone
[0136] BCS: Butyl Cellosolve
[0137] GBL: gamma-butyrolactone
[0138] BCA: Butyl Cellosolve Acetate
[0139] PB: Propylene glycol monobutyl ether
[0140] DME: Dipropylene glycol dimethyl ether ...
Synthetic example 1
[0158] Take 1.88g (7.70mmol) DA-1 and 1.17g (2.11mmol) DA-3, 1.67g (4.20mmol) DA-2 in a 50mL four-neck flask with a stirring device and a nitrogen inlet tube, add 40.00gNMP , and stirred while feeding nitrogen gas to make it dissolve. While stirring the diamine solution, add 2.04g (9.10mmol) 1,3DMCBDA and continue to stir. After the viscosity is stabilized, add 0.62g (3.16mmol) CBDA, and further add NMP so that the solid content concentration becomes 15% by mass. Under stirring for 24 hours, a solution of polyamic acid (PAA-1) was obtained. The viscosity at 25° C. of this polyamic acid solution was 212 mPa·S.
Synthetic example 2
[0160] 30 g of PAA-1 obtained in Synthesis Example 1 was weighed into a 100 mL four-necked flask equipped with a stirring device and a nitrogen gas introduction tube, and diluted with NMP to a solid content concentration of 8% by mass.
[0161] Next, 2.61 g (25.5 mmol) of acetic anhydride and 0.67 g (8.47 mmol) of pyridine were added and dissolved. Next, stirring this solution, it heated at 55 degreeC, and it was made to react for 3 hours. The obtained polyamic acid-soluble polyimide acid solution was added to methanol in an amount equivalent to 3.5 times the total solution, stirring, and reprecipitated. The reprecipitated powder is filtered by natural filtration or suction filtration, and then washed twice with 0.188l (5.86mmol) of methanol respectively, and dried to obtain white polyamic acid-soluble polyimide resin Powder (PWD-1). The molecular weight of this resin powder was Mn=13493, Mw=27207.
[0162] The PWD-1 obtained above was dissolved in NMP to obtain a polyamic ...
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