Liquid crystal aligning agent and liquid crystal display element
A technology of liquid crystal alignment agent and group, applied in liquid crystal materials, chemical instruments and methods, instruments, etc., can solve problems such as inability to meet heat resistance
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Synthetic example 1
[0150] Synthesis example 1 (synthesis of 2,6-diaminobenzothiazole)
[0151] The synthetic raw material 2-amino-6-nitrobenzothiazole directly used the product of Tokyo Chemical Industry Co., Ltd. 97.6 g (0.50 mol) of 2-amino-6-nitrobenzothiazole was dissolved in 3000 ml of ethanol, 90 g of 5% by weight palladium / carbon was added, and the mixture was stirred at 70° C. for 1 hour under a nitrogen atmosphere. Then, 153 ml of hydrazine monohydrate was added, and the mixture was stirred under reflux for 6 hours under nitrogen flow to carry out the reaction. After the reaction was completed, the palladium / carbon was removed by filtration with diatomaceous earth (Celite), and the solvent was removed from the filtrate. The obtained solid was sufficiently washed with distilled water, and then dried to obtain 44.8 g (54.0%) of the target 2,6-diaminobenzothiazole.
[0152] This synthesis operation was repeated according to the above synthesis scheme to ensure the necessary amount of 2,6...
Synthetic example 2
[0154] Synthesis example 2 (synthesis 1 of polyimide)
[0155] 110 g (0.50 moles) of 2,3,5-tricarboxycyclopentylacetic dianhydride as tetracarboxylic dianhydride and 1,3,3a,4,5,9b-hexahydro-8-methyl-5- (Tetrahydro-2,5-dioxo-3-furyl)-naphthalene[1,2-c]-furan-1,3-dione 160g (0.50mol), 84g of p-phenylenediamine as diamine (0.78 mol), 2,6-diaminobenzothiazole 16.5g (0.1 mol), 2,2-bis(trifluoromethyl)-4,4-diaminobiphenyl 32g (0.10 mol) and 3,6 - 6.4 g (0.010 mol) of bis(4-aminobenzoyloxy)cholestane, and 2.8 g (0.03 mol) of aniline as monoamine dissolved in 1200 g of N-methyl-2-pyrrolidone (NMP), The reaction was carried out at 60° C. for 9 hours to obtain a solution containing polyamic acid. A small amount of the obtained polyamic acid solution was taken, and NMP was added to form a solution with a polyamic acid concentration of 10% by weight. The measured solution viscosity was 58 mPa·s.
[0156] Then, 2400 g of NMP was added to the polyamic acid solution prepared above, and th...
Synthetic example 3
[0157] Synthesis example 3 (synthesis 2 of polyimide)
[0158] 110 g (0.50 moles) of 2,3,5-tricarboxycyclopentylacetic dianhydride as tetracarboxylic dianhydride and 1,3,3a,4,5,9b-hexahydro-8-methyl-5- (Tetrahydro-2,5-dioxo-3-furyl)-naphthalene[1,2-c]-furan-1,3-dione 160g (0.50mol), 94g of p-phenylenediamine as diamine (0.87 mol), 2,6-diaminobenzothiazole 16.5g (0.1 mol), 1,3-bis(3-aminopropyl)tetramethyldisiloxane 25g (0.10 mol) and 3,6- 9.6 g (0.015 moles) of bis(4-aminobenzoyloxy) cholestane, and 2.8 g (0.030 moles) of aniline as a monoamine were dissolved in 960 g of NMP, and reacted at 60° C. for 6 hours to obtain A solution of polyamic acid. A small amount of the obtained polyamic acid solution was taken, and NMP was added to form a solution with a polyamic acid concentration of 10% by weight. The measured solution viscosity was 60 mPa·s.
[0159] Then, 2700 g of NMP was added to the obtained polyamic acid solution, and 400 g of pyridine and 410 g of acetic anhydride ...
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