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 uneven printing, easy decrease in polymer solubility, easy increase in polymer cohesion, etc., to achieve increased yield and reduced The effect of bad printing
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[0139] Hereinafter, the present invention will be described more specifically by way of examples, but the present invention is not limited by these examples.
[0140] The solution viscosity of each polymer solution in a synthesis example, and the imidization rate of a polyimide can be measured by the following method.
[0141] [Solution Viscosity of Polymer Solution]
[0142] The solution viscosity (mPa·s) of the polymer solution can be measured at 25° C. using an E-type rotational viscometer on a solution adjusted to a polymer concentration of 10% by weight using a predetermined solvent.
[0143] [Imidation rate of polyimide]
[0144] Put the polyimide solution into pure water, dry the resulting precipitate under reduced pressure at room temperature, dissolve it in deuterated dimethyl sulfoxide, and measure it at room temperature with tetramethylsilane as the standard substance 1 H-NMR. according to income 1 From the H-NMR spectrum, the imidization rate [%] was obtained b...
Synthetic example 1
[0148] [Synthesis Example 1: Synthesis of Polyimide (PI-1)]
[0149] 22.4 g (0.1 mol) of 2,3,5-tricarboxycyclopentylacetic dianhydride (TCA) as tetracarboxylic dianhydride, 2.2 g (0.02 mol) of p-phenylenediamine (PDA) as diamine, 10.5g (0.02 mole) of cholestanyl 3,5-diaminobenzoate (HCDA), 4.9g (0.01 mole) of cholestanyloxy-2,4-diaminobenzene (HCODA) and 3,5 - 7.6g (0.05mol) of diaminobenzoic acid (DAB) was dissolved in 190g 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 . About the obtained polyamic-acid solution, NMP was added and the solution whose polyamic-acid density|concentration was 10 weight% was measured and the solution viscosity was 88 mPa*s.
[0150] Next, 442 g of NMP was added to the obtained polyamic-acid solution, and 11.9 g of pyridine and 15.3 g of acetic anhydride were added, and the dehydration ring-closure reaction was performed at 110 degreeC for 4 hours. After the dehy...
Synthetic example 2
[0151] [Synthesis Example 2: Synthesis of Polyimide (PI-2)]
[0152] 22.4 g (0.1 mol) of TCA as tetracarboxylic dianhydride, 5.4 g (0.05 mol) of PDA as diamine, 10.5 g (0.02 mol) of HCDA, 4.9 g (0.01 mol) of HCODA and 4,4'-bis 5.4 g (0.02 mol) of amino-1,1'-biphenyl-2,2'-dicarboxylic acid (DBCA) was dissolved in 195 g of NMP, and the reaction was carried out at 60°C for 6 hours to obtain a polyamic acid containing 20% by weight The solution. About the obtained polyamic-acid solution, the solution viscosity measured by adding NMP and making it into the solution whose polyamic-acid density|concentration is 10 weight% was 33 mPa*s.
[0153]Next, 452 g of NMP was added to the obtained polyamic-acid solution, and 11.9 g of pyridine and 15.3 g of acetic anhydride were added, and the dehydration ring-closure reaction was performed at 110 degreeC for 4 hours. After the dehydration ring-closing reaction, the solvent in the system was replaced with new NMP to obtain a solution conta...
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