Liquid crystal aligning agent containing polyamic acid ester-polyamic acid copolymer, and liquid crystal aligning film using the same
A technology of liquid crystal aligning agent and liquid crystal aligning film, applied in the directions of liquid crystal materials, instruments, chemical instruments and methods, etc., can solve the problems of slow residual charge relaxation and high volume resistivity, and achieve fast accumulation of DC relaxation speed and liquid crystal alignment. Low degradation, good anti-aging effect
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[0160] Examples are given below to describe the present invention in more detail. In addition, the present invention is not limitedly interpreted by them.
[0161] The structures and abbreviations of main compounds used in Examples and Comparative Examples are shown below.
[0162] X-1: 2,4-bis(methoxycarbonyl)cyclobutane-1,3-dicarboxylic acid
[0163] X-2: 1,2,3,4-Cyclobutanetetracarboxylic dianhydride
[0164] X-3: pyromellitic dianhydride
[0165] X-4: 3,3’,4,4’-Biphenyltetracarboxylic dianhydride
[0166]
[0167] Y-1: bis(4-aminophenoxy)methane
[0168] Y-2: 1,2-bis(4-aminophenoxy)ethane
[0169] Y-3: 1,3-bis(4-aminophenoxy)propane
[0170] Y-4: 4,4'-diaminodiphenylamine
[0171] Y-5: 4-(2-(methylamino)ethyl)aniline
[0172] Y-6: 1,3-bis(4-aminophenethyl)ureido
[0173] Y-7: 3,5-diaminobenzoic acid
[0174]
[0175] DBOP: Diphenyl (2,3-dihydro-2-thia-3-benzoxazolyl)phosphate
[0176]
[0177] Z-1: 3-Glycidoxypropyltriethoxysilane
[0178]
[0179] ...
Synthetic example 1
[0231] (synthesis example 1) polyamic acid ester solution
[0232] After throwing 174.9 g (672.0 mmol) of X-1 into a 5000 mL four-necked flask equipped with a stirring bar, 3351 g of N-methyl-2-pyrrolidone was added, stirred and dissolved. Next, 148.7 g (1470 mmol) of triethylamine and 180.8 g (700.0 mmol) of Y-3 were added, stirred and dissolved.
[0233] Stirring this solution, DBOP 563.5g (1470mmol) was added, and 460.4g of N-methyl- 2-pyrrolidones were further added, and it stirred at room temperature for 12 hours, and obtained the solution of the polyamic acid ester. The viscosity in temperature 25 degreeC of this polyamic acid ester solution was 61.1 mPa*s.
[0234] This polyamic acid ester solution was poured into methanol (29280g), and the obtained deposit was collected by filtration. After washing|cleaning this deposit with methanol, it dried under reduced pressure at the temperature of 100 degreeC, and obtained the powder of the polyamic acid ester. The molecular ...
Synthetic example 2
[0236] (synthesis example 2) polyamic acid solution
[0237] 9.56 g (37.0 mmol) of Y-3 was put into a 100-mL four-necked flask equipped with a stirring bar, 74.6 g of N-methyl-2-pyrrolidone was added, and it stirred and melt|dissolved while injecting nitrogen gas. Stirring this diamine solution, X-26.89g (35.2mmol) was added, N-methyl-2-pyrrolidone 18.6g was further added, and it stirred at 23 degreeC for 5 hours in nitrogen atmosphere, and obtained the polyamic-acid solution. The viscosity of the polyamic acid solution at a temperature of 25° C. was 436 mPa·s. In addition, the molecular weight of this polyamic acid was Mn=15400, Mw=41700.
[0238] 10.3 g of this polyamic acid solution was divided into a 100 mL Erlenmeyer flask with a stirring bar, 18.7 g of N-methyl-2-pyrrolidone, 0.02 g of Z-1 and 9.68 g of butyl cellosolve were added, and a magnetic stirrer was used to It stirred for 2 hours, and obtained the polyamic-acid solution whose solid content concentration was 4....
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