Liquid crystal alignment agent, liquid crystal alignment film and liquid crystal display element
A liquid crystal alignment agent and solvent technology, applied in liquid crystal materials, instruments, optics, etc., can solve problems such as printability decline, printing plate swelling, and APR resin swelling.
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[0160] Hereinafter, the present invention will be further specifically described using examples, but the present invention is not limited by these examples.
[0161] The solution viscosity of each polymer solution in a synthesis example, the imidization rate of a polyimide, a weight average molecular weight, and epoxy equivalent were measured by the following methods.
[0162] [Solution Viscosity of Polymer Solution]
[0163] The solution viscosity (mPa·s) of the polymer solution was measured at 25°C for a solution adjusted to a polymer concentration of 10% by weight using a predetermined solvent using an E-type rotational viscometer.
[0164] [Imidation rate of polyimide]
[0165] Put the polyimide solution into pure water, dry the obtained precipitate under reduced pressure at room temperature, dissolve it in deuterated dimethyl sulfoxide, use tetramethylsilane as a reference substance, and determination 1 H-NMR ( 1 H-Nuclear Magnetic Resonance, 1 H-NMR). according to ...
Synthetic example 1
[0177][Synthesis Example 1: Synthesis of Polyimide (PI-1)]
[0178] 22.4 g (0.1 mol) of 2,3,5-tricarboxycyclopentylacetic dianhydride as tetracarboxylic dianhydride, 8.6 g (0.08 mol) of p-phenylenediamine as diamine, and 3,5-diamino 10.5 g (0.02 mol) of cholestyl benzoate was dissolved in 166 g of N-methyl-2-pyrrolidone (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, NMP was added to obtain a solution having a polyamic acid concentration of 10% by weight, and the solution viscosity measured for this solution was 90 mPa·s.
[0179] 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 15.3 g of acetic anhydride were added, and a dehydration ring-closure reaction was performed at 110° C. for 4 hours. After the dehydration ring-closure reaction, the...
Synthetic example 2
[0180] [Synthesis Example 2: Synthesis of Polyimide (PI-2)]
[0181] 22.5 g (0.1 mol) of 2,3,5-tricarboxycyclopentylacetic dianhydride as tetracarboxylic dianhydride, 7.6 g (0.07 mol) of p-phenylenediamine as diamine, 3,5-diamino Cholesteryl benzoate 5.2g (0.01 mol) and 4,4'-diaminodiphenylmethane 4.0g (0.02 mol) were dissolved in 157g of NMP, and reacted for 6 hours at 60°C to obtain poly Amic acid 20% by weight solution. A small amount of the obtained polyamic acid solution was fractionated, NMP was added to obtain a solution having a polyamic acid concentration of 10% by weight, and the solution viscosity measured for this solution was 110 mPa·s.
[0182] Next, NMP was added to the obtained polyamic acid solution to obtain a solution having a polyamic acid concentration of 7% by weight, 16.6 g of pyridine and 21.4 g of acetic anhydride were added, and a dehydration ring-closure reaction was performed at 110° C. for 4 hours. After the dehydration ring-closure reaction, the...
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