Liquid crystal aligning agent, liquid crystal aligning film and liquid crystal display element
A liquid crystal aligning agent and solvent technology, used in liquid crystal materials, instruments, optics, etc., can solve problems such as uneven coating, and achieve the effect of narrowing the frame and reducing the non-display area.
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[0117] Hereinafter, the present invention will be further specifically described through examples, but the present invention is not limited to these examples.
[0118] In the following examples and comparative examples, the imidation ratio of the polyimide in the polymer solution, the solution viscosity of the polymer solution, the weight average molecular weight of the polymer, and the epoxy equivalent were measured by the following methods.
[0119] [Imidation rate of polyimide]
[0120] The polyimide solution was put into pure water, and the obtained precipitate was fully dried under reduced pressure at room temperature, and then dissolved in deuterated dimethyl sulfoxide, using tetramethylsilane as a reference substance, at room temperature down test 1 H-NMR (Nuclear Magnetic Resonance, NMR). according to income 1 From the H-NMR spectrum, the imidization rate [%] was determined by the following formula (x).
[0121] Imidization rate [%] = (1-A 1 / A 2 ×α)×100...(x)
...
Synthetic example 1
[0134] [Synthesis Example 1: Synthesis of Polyimide (PI-1)]
[0135] 22.4 g (0.1 mol) of 2,3,5-tricarboxycyclopentylacetic dianhydride (2,3,5-tricarboxy cyclopentyl acetic dianhydride, TCA) as tetracarboxylic dianhydride, terephthalic diamine as diamine Amine (p-phenylene diamine, PDA) 8.6g (0.08 mol) and 3,5-diaminobenzoic acid cholestanyl ester (cholestanyl 3,5-diaminobenzoate, HCDA) 10.5g (0.02 mol), dissolved in N- In 166 g of methyl-2-pyrrolidone (N-methyl-2-pyrrolidone, NMP), reaction was performed at 60 degreeC for 6 hours, and the solution containing the polyamic acid of 20 weight% was obtained. A small amount of the obtained polyamic acid solution was fractionated, and NMP was added to obtain a solution having a polyamic acid concentration of 10% by weight. The measured solution viscosity was 90 mPa·s.
[0136] Next, NMP was added to the obtained polyamic acid solution to obtain a solution having a polyamic acid concentration of 7% by weight, 11.9 g of pyridine and 1...
Synthetic example 2
[0137] [Synthesis Example 2: Synthesis of Polyimide (PI-2)]
[0138]22.5 g (0.1 mol) of TCA as tetracarboxylic dianhydride, 6.1 g (0.04 mol) of 3,5-diaminobenzoic acid (3,5-diamino benzoic acid, 35DAB) as diamine, cholestalkoxy 5.0 g (0.010 moles) of cholestanyloxy-2,4-diaminobenzene (cholestanyloxy-2,4-diaminobenzene, HCODA) and 9.3 g (0.020 moles) of the compound (LDA) represented by the formula (D-1-5) , 4-(4-aminophenoxycarbonyl)-1-(4-aminophenyl) piperidine (4-(4-aminophenoxycarbonyl)-1-(4-aminophenyl)piperidine, APPC) 9.4g (0.030 mole) , was dissolved in 210 g of NMP, and reacted at 60° C. for 6 hours to obtain a solution containing 20% by weight of polyamic acid. A small amount of the obtained polyamic acid solution was fractionated, and NMP was added to obtain a solution having a polyamic acid concentration of 10% by weight. The solution viscosity measured was 76 mPa·s.
[0139] Next, NMP was added to the obtained polyamic acid solution to obtain a solution having ...
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