CN101195711B - Polyamic acid component and alignment film produced by the same - Google Patents

Polyamic acid component and alignment film produced by the same Download PDF

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CN101195711B
CN101195711B CN2006101622089A CN200610162208A CN101195711B CN 101195711 B CN101195711 B CN 101195711B CN 2006101622089 A CN2006101622089 A CN 2006101622089A CN 200610162208 A CN200610162208 A CN 200610162208A CN 101195711 B CN101195711 B CN 101195711B
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phenyl
methyl
amido
hexanaphthene
polyamic acid
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CN101195711A (en
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颜传特
黄志雄
黄昭敬
高进旺
洪亭慧
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DALI POLYMER Co Ltd
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DALI POLYMER Co Ltd
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Abstract

The invention relates to polyamic acid composition and an alignment film produced by the polyamic acid composition. The polyamic acid composition comprises polyamic acid A made by a first reaction mixture through reaction, and polyamic acid B made by a second reaction mixture through reaction, the first reaction mixture includes aromatic tetracarboxylic diamine and aromatic diamine, and the second reaction mixture includes aliphatic tetracarboxylic diamine, aromatic diamine with side chains, and non-aromatic diamine. The invention also provides an alignment film produced through the solidification of the polyamic acid composition, and the alignment film can ensure the display device to have higher voltage maintenance proportion, proper pretilt angle and better alignment property during the practical application process.

Description

Polyamic acid component reaches by its prepared alignment film
Technical field
The present invention relates to a kind of polyamic acid component reaches by its prepared alignment film; Particularly relate to a kind of polyamic acid component with particular combination and when practical application, possess and have high voltage to keep ratio (voltage holding atio, VHR), suitable tilt angle (pre-tilt angle) and preferable orientation character (orienting property) alignment film.
Background technology
Current flourish along with the personal information produce market added liquid crystal indicator and had advantages such as frivolous, low power consumption, makes present industry mostly towards the development miniaturized portable message product that has liquid crystal indicator of all kinds.Yet, because general miniaturized product can't provide big driving voltage (driving voltage), so how to reduce the usefulness and the character of required voltage of liquid crystal indicator and lifting liquid crystal indicator, also become the target of the anxious desire development of industry.The character that need improve to liquid crystal indicator; It mainly comprises: the electrical property of tilt angle, liquid crystal indicator [for example current draw (current consumption), voltage keep ratio and retained voltage (residual voltage)], and the reliability of the above-mentioned character behind the life-time service liquid crystal indicator etc.
Generally speaking; The required tilt angle scope of liquid crystal mainly is different according to the drive system of liquid crystal indicator; TN type liquid crystal indicator for example; Because liquid crystal is reversed 90 °; Therefore need 1~6 ° tilt angle approximately; STN type liquid crystal indicator is then because the windup-degree of liquid crystal is big more than (180 ° or 180 °), so need 3~8 ° tilt angle approximately.The TFT liquid crystal indicator generally needs high voltage to keep ratio (about 99% above); Orientation character to liquid crystal does not have too big requirement; The required voltage of STN type liquid crystal indicator is kept then lower (about 80%) of ratio; But the orientation character for liquid crystal is had relatively high expectations, just can not produce " non-homogeneous regional (domain) ".
The Japan (Chisso Corporation of Chisso Corporation (JP) 6-32, Nakanoshima 3-chome, Kitaku, Osaka, Japan) had a series of patents of researching and developing based on the demand, for example USP announces the 6th, 620, and No. 339 and 6,946,169 B1 numbers.Announcing 6 with USP is for B1 number example; It has disclosed a kind of polyamic acid component; This constituent comprise one provide the retained voltage that possesses below the 200mV and 97% above voltage to keep the polyimide resin of ratio polyamic acid A, and one the polyimide resin of the tilt angle that possesses 3~15 ° is provided polyamic acid B.This polyamic acid A possesses an acid constituents and an amine component, and this acid constituents is mainly alicyclic tetracarboxylic dianhydride (alicyclic tetracarboxylic dianhydride), this amine component mainly is by the aromatic diamine shown in the following formula (1):
Figure G061G2208920061214D000021
Wherein, X is an aliphatic divalent group, and each R is respectively hydrogen or methyl, and a and b are the numerical value between 1 to 2.The acid constituents of this polyamic acid B contains 50mol% or above aromatic tetracarboxylic acid's dianhydride, and the amine component of this polyamic acid B contains a diamines, this diamines on its side chain, have one can let the tilt angle of liquid crystal increase group.The ratio A/B of this polyamic acid A and polyamic acid B is 50/50~95/5.The diamines with side-chain radical in the amine component of this polyamic acid B can be as shown in the formula shown in (2) and/or (3):
Figure G061G2208920061214D000022
, in this formula (2), R is hydrogen or the alkyl with 1 to 12 carbon atom, Y is CH < > 2 <> , m is the integer between 0 to 2, and A is phenyl ring or cyclohexane ring, and p is 0 or 1, and Z is oxygen or CH < > 2 <> , n is 0 or 1.In this formula (3), X1 is CH < > 2 <> Or oxygen, R1 and R2 are respectively hydrogen, have the alkyl or the perfluoroalkyl of 1 to 12 carbon atom, and n1 is 0 or 1.The measured tilt angle of the alignment film that utilizes the polyamic acid component of this patent to make is between 5 °~9 °, and voltage is kept ratio and is about 97%~98.4%.This patent is not mentioned the test result about orientation character especially, whether can improve the orientation character of liquid crystal so can't learn prepared alignment film.Again, according to the present demand of industry, voltage is kept the preferable need of ratio greater than 99%, and in order to reach so high standard, and tendency is formed by improvement process conditions and liquid crystal material and promoted mostly at present.
From the above; Obtain to have better electrical character (lower retained voltage or higher voltage are kept ratio), make liquid crystal have the alignment film of suitable tilt angle and preferable orientation character like desire; Can and form to come change by the polyimide structures that constitutes this alignment film; Therefore make this alignment film for looking for preferable polyamic acid component or polyimide, still have an active demand.
Though the alignment film of case can let liquid crystal have suitable tilt angle before above-mentioned; Ratio is the highest can only to reach 98.4% but voltage is kept; And do not test to the orientation character of liquid crystal; And according to the required requirement of industry at present; Voltage keeps that ratio is preferable to be required to be more than 99%; And must let liquid crystal have preferable orientation character, the polyamic acid component of visible above-mentioned preceding case still needs to improve again.
This shows that above-mentioned existing polyamic acid component and alignment film obviously still have inconvenience and defective, and demand urgently further improving in structure and use.For solving the problem of above-mentioned existence; Relevant manufacturer there's no one who doesn't or isn't seeks solution painstakingly; But do not see always that for a long time suitable design is developed completion, and common product does not have appropriate structure to address the above problem, this obviously is the problem that the anxious desire of relevant dealer solves.Therefore how to found a kind of polyamic acid component of novel texture and by its prepared alignment film, belong to one of current important research and development problem in fact, also becoming the current industry utmost point needs improved target.
Because the defective that above-mentioned existing polyamic acid component and alignment film exist; The inventor is based on being engaged in this type of product design manufacturing abundant for many years practical experience and expertise; And the utilization of cooperation scientific principle; Actively study innovation; Reach by its prepared alignment film in the hope of founding a kind of novel polyamic acid component; Can improve general existing polyamic acid component and alignment film, make it have more practicality.Through constantly research, design, and, found out the present invention of true tool practical value finally through after studying sample and improvement repeatedly.
Summary of the invention
First purpose of the present invention is, overcomes the defective that existing polyamic acid component exists, and a kind of polyamic acid component with novel specific polyamic acid combination is provided.
Second purpose of the present invention is, overcomes the defective that existing alignment film exists, and utilizes above-mentioned polyamic acid component obtained and provide a kind of, and better electrical character can be provided, and can let liquid crystal have the alignment film of suitable tilt angle and preferable orientation character.
The object of the invention and solve its technical problem and adopt following technical scheme to realize.According to a kind of polyamic acid component that the present invention proposes, it comprises: a kind of polyamic acid A is to react obtained by a kind of first reaction mixture, and this first reaction mixture contains a kind of aromatic tetracarboxylic acid's dianhydride and a kind of aromatic diamine; And a kind of polyamic acid B, be to react obtained by a kind of second reaction mixture, this second reaction mixture contains a kind of aliphatics tetracarboxylic dianhydride, a kind of aromatic diamine and a kind of non-aromatic diamines with side chain; Wherein, The content ratio of this polyamic acid A and B is between 75: 25 to 30: 70; And in second reaction mixture of this polyamic acid B, this has the aromatic diamine of side chain and the molar ratio of this non-aromatic diamines is between 70: 30 to 1: 99.
The object of the invention and solve its technical problem and also can adopt following technical measures further to realize.
Aforesaid polyamic acid component, the content ratio of wherein said polyamic acid A and polyamic acid B is between 70: 30 to 50: 50.
Aforesaid polyamic acid component, wherein said have the aromatic diamine of side chain and the molar ratio of this non-aromatic diamines is between 45: 55 to 3: 97.
Aforesaid polyamic acid component, wherein said have the aromatic diamine of side chain and the molar ratio of this non-aromatic diamines is 6: 94.
Aforesaid polyamic acid component, aromatic tetracarboxylic acid's dianhydride of wherein said first reaction mixture is to be selected from :1,2; 4; 5-pyromellitic acid dianhydride; Phenylbenzene tetracarboxylic dianhydride, 4,5; 8-naphthalene tetracarboxylic acid dianhydride, 6,7-naphthalene tetracarboxylic acid dianhydride ', 4 '-dimethyl diphenyl silane tetracarboxylic dianhydride, 3 ' '-tetraphenyl silane tetracarboxylic dianhydride, 2,3; 4-furans tetracarboxylic dianhydride '-two (3, the 4-di carboxyl phenyloxy) diphenyl sulfide dianhydride, 4 '-two (3; The 4-di carboxyl phenyloxy) diphenyl sulfone dianhydride '-two (3, the 4-di carboxyl phenyloxy) the diphenyl propane dianhydride; Two (phthalic acid) oxidation phosphniline dianhydride; To benzene-two (triphenylbenzene diformyl) dianhydride; Between benzene-two (triphenylbenzene diformyl) dianhydride; Two (triphenylbenzene dioctyl phthalate)-4,4 '-diphenyl ether dianhydride; Two (triphenylbenzene dioctyl phthalate)-4 '-ditan dianhydride, or these a combination.
Aforesaid polyamic acid component, wherein said aromatic tetracarboxylic acid's dianhydride is 1,2,4,5-pyromellitic acid dianhydride.
Aforesaid polyamic acid component; The aromatic diamine of wherein said first reaction mixture is to be selected from: 2; The two [4-(4-amido phenoxys of 2-) phenyl] HFC-236fa; 2; Two (4-aminocarbonyl phenyl) HFC-236fa ' of 2--two [4-(4-amidos-2-4-trifluoromethylphenopendant) phenyl] HFC-236fa '-two amido-2 '-two (trifluoromethyl) biphenyl '-two [(4-amidos-2-trifluoromethyl) phenoxy octafluoro biphenyl '-two (4-amido phenoxy) biphenyl; Ursol D; Mphenylenediamine '-two amido-3 '-dicarboxyl ditan; 1; Two (4-aminocarbonyl phenyl) benzene ' of 4--benzidine '-dimethyl--4 '-benzidine '-dimethoxy-4 '-benzidine '-dihydroxyl-4 '-benzidine '-dichloro-4 '-benzidine, 3 '-dicarboxyl-4,4-benzidine; Two amido ditans; Two amido diphenyl ethers; 2; 2-two amido diphenyl propane '-two amido sulfobenzides; Two amido benzophenone, two (4-amido phenoxy) benzene of 3-, two (4-amido phenoxy) benzene '-two (4-amido phenoxy) sulfobenzide of 4-, the two [4-(4-amido phenoxys of 2-) phenyl] propane; Or these a combination.
Aforesaid polyamic acid component, wherein said aromatic diamine is 4,4 '-two (4-amido phenoxy) biphenyl.
Aforesaid polyamic acid component, the aliphatics tetracarboxylic dianhydride of wherein said second reaction mixture is selected from: two ring (2,2,2) suffering-7-alkene-2,5,6-tetracarboxylic dianhydride, 2,4-butane tetracarboxylic acid dianhydride, 4-dicarboxyl-1,3,4-tetrahydrochysene-1-naphthalene Succinic anhydried, 5-tricarboxylic basic ring amyl group second dianhydride, 2,4-tetramethylene tetracarboxylic dianhydride, 3-dimethyl--1,3,4-tetramethylene tetracarboxylic dianhydride, 3,4-pentamethylene tetracarboxylic dianhydride, 6-three carboxyls norbornane-2-second dianhydride, 3,5-THF tetracarboxylic dianhydride, or these a combination.
Aforesaid polyamic acid component, wherein said aliphatics tetracarboxylic dianhydride is 1,2,3,4-butane tetracarboxylic acid dianhydride.
Aforesaid polyamic acid component; The aromatic diamine with side chain of wherein said second reaction mixture is to be selected from: the diamines shown in the following formula (I); 1; The two [4-(4-amido phenoxys of 1-) phenyl] the-4-(cyclohexyl methyl) hexanaphthene; 1; The two [4-(4-amido phenoxys of 1-) methyl phenyl methylcyclohexyl)] hexanaphthene; 1; The two [4-(4-amido phenoxys of 1-) methyl phenyl ethyl cyclohexyl)] hexanaphthene; 1; The two [4-(4-amido phenoxys of 1-) methyl phenyl propyl group cyclohexyl)] hexanaphthene; 1; The two [4-(4-amido phenoxys of 1-) methyl phenyl butyl cyclohexyl)] hexanaphthene; 1; The two [4-(4-amido phenoxys of 1-) methyl phenyl amyl group cyclohexyl)] hexanaphthene; 1; The two [4-(4-amido phenoxys of 1-) methyl phenyl hexyl cyclohexyl)] hexanaphthene; 1; The two [4-(4-amido phenoxys of 1-) methyl phenyl heptyl cyclohexyl)] hexanaphthene; 1; The two [4-(4-amido phenoxys of 1-) methyl phenyl octyl group cyclohexyl)] hexanaphthene; 1; Two (4-aminocarbonyl phenyl) the-4-(cyclohexyl methyls of 1-) hexanaphthene; 1; Two (the 4-aminocarbonyl phenyl)-4-[(4-methylcyclohexyl) methyl of 1-] hexanaphthene; 1; Two (the 4-aminocarbonyl phenyl)-4-[(4-ethyl cyclohexyl) methyl of 1-] hexanaphthene; 1; Two (the 4-aminocarbonyl phenyl)-4-[(4-propyl group cyclohexyl) methyl of 1-] hexanaphthene; 1; Two (the 4-aminocarbonyl phenyl)-4-[(4-butyl cyclohexyl) methyl of 1-] hexanaphthene; 1; Two (the 4-aminocarbonyl phenyl)-4-[(4-amyl group cyclohexyl) methyl of 1-] hexanaphthene; 1; Two (the 4-aminocarbonyl phenyl)-4-[(4-hexyl cyclohexyl) methyl of 1-] hexanaphthene; 1; Two (the 4-aminocarbonyl phenyl)-4-[(4-heptyl cyclohexyl) methyl of 1-] hexanaphthene; 1; Two (the 4-aminocarbonyl phenyl)-4-[(4-octyl group cyclohexyl) methyl of 1-] hexanaphthene; 1; The two [4-(4-amido phenoxys of 1-) phenyl] the-4-(phenyl methyl) hexanaphthene; 1; The two [4-(4-amido phenoxys of 1-) methyl phenyl aminomethyl phenyl)] hexanaphthene; 1; The two [4-(4-amido phenoxys of 1-) methyl phenyl ethylphenyl)] hexanaphthene; 1; The two [4-(4-amido phenoxys of 1-) methyl phenyl propyl group phenyl)] hexanaphthene; 1; The two [4-(4-amido phenoxys of 1-) methyl phenyl butyl phenyl)] hexanaphthene; 1; The two [4-(4-amido phenoxys of 1-) methyl phenyl amyl group phenyl)] hexanaphthene; 1; The two [4-(4-amido phenoxys of 1-) methyl phenyl hexyl phenyl)] hexanaphthene; 1; The two [4-(4-amido phenoxys of 1-) methyl phenyl heptyl phenyl)] hexanaphthene; 1; The two [4-(4-amido phenoxys of 1-) methyl phenyl octyl phenyl)] hexanaphthene; 1; Two (4-aminocarbonyl phenyl) the-4-(phenyl methyls of 1-) hexanaphthene; 1; Two (the 4-aminocarbonyl phenyl)-4-[(4-aminomethyl phenyl) methyl of 1-] hexanaphthene; 1; Two (the 4-aminocarbonyl phenyl)-4-[(4-ethylphenyl) methyl of 1-] hexanaphthene; 1; Two (the 4-aminocarbonyl phenyl)-4-[(4-propyl group phenyl) methyl of 1-] hexanaphthene; 1; Two (the 4-aminocarbonyl phenyl)-4-[(4-butyl phenyl) methyl of 1-] hexanaphthene; 1; Two (the 4-aminocarbonyl phenyl)-4-[(4-amyl group phenyl) methyl of 1-] hexanaphthene; 1; Two (the 4-aminocarbonyl phenyl)-4-[(4-hexyl phenyl) methyl of 1-] hexanaphthene; 1; Two (the 4-aminocarbonyl phenyl)-4-[(4-heptyl phenyl) methyl of 1-] hexanaphthene; 1; Two (the 4-aminocarbonyl phenyl)-4-[(4-octyl phenyl) methyl of 1-] hexanaphthene; 1; The two [4-((4-aminocarbonyl phenyls of 1-) phenyl methyl)] the-4-(phenyl methyl) hexanaphthene; 1; The two [4-((4-aminocarbonyl phenyls of 1-) methyl phenyl aminomethyl phenyl methyl))] hexanaphthene; 1; The two [4-((4-aminocarbonyl phenyls of 1-) methyl phenyl ethylphenyl methyl))] hexanaphthene; 1; The two [4-((4-aminocarbonyl phenyls of 1-) methyl phenyl propyl group phenyl methyl))] hexanaphthene; 1; The two [4-((4-aminocarbonyl phenyls of 1-) methyl phenyl butyl phenyl methyl))] hexanaphthene; 1; The two [4-((4-aminocarbonyl phenyls of 1-) methyl phenyl amyl group phenyl methyl))] hexanaphthene; 1; The two [4-((4-aminocarbonyl phenyls of 1-) methyl phenyl hexyl phenyl methyl))] hexanaphthene; 1; The two [4-((4-aminocarbonyl phenyls of 1-) methyl phenyl heptyl phenyl methyl))] hexanaphthene; 1; The two [4-((4-aminocarbonyl phenyls of 1-) methyl phenyl octyl phenyl methyl))] hexanaphthene; Or these a combination
Figure G061G2208920061214D000061
Aforesaid polyamic acid component, wherein said aromatic diamine with side chain are the diamines shown in this formula (I).
Aforesaid polyamic acid component, the non-aromatic diamines of wherein said second reaction mixture is to be selected from: aliphatie diamine, alicyclic diamine or these a combination.
Aforesaid polyamic acid component, wherein said non-aromatic diamines is an alicyclic diamine.
Aforesaid polyamic acid component; Wherein said alicyclic diamine is to be selected from :4 '-two amido dicyclohexyl methyl hydride; 1; 4-diamines basic ring hexane; 1; Two (the 4-amido cyclohexyl) propane of 1-; 2; Two (the 4-amido cyclohexyl) propane of 2-; 1; Two (the 4-amido cyclohexyl) ethane of 1-; 1; Two (the 4-amido cyclohexyl) butane of 1-; 2; Two (4-amido cyclohexyl) the butane amido cyclohexyl)-2-(4-aminomethyl cyclohexyl of 2-) methane; 4-amido-3; 5-Dimethylcyclohexyl-4-amido-3-methyl cyclohexane methylmethane; 4-amido cyclohexyl-4-amido-3-methyl cyclohexane methylmethane; 2; Two (4-amido-3,5-Dimethylcyclohexyl) butane of 2-, two (the 4-amidos-3 of 2-; The 5-Dimethylcyclohexyl) propane; 1; Two (4-amido-3,5-Dimethylcyclohexyl) ethane of 1-, two (4-amido-3-methylcyclohexyl) propane of 2-; 1; Two (4-amido-3-methylcyclohexyl) ethane of 1-, or these a combination.
18 aforesaid polyamic acid components, wherein said alicyclic diamine is 4,4 '-two amido dicyclohexyl methyl hydrides.
Aforesaid polyamic acid component, it also comprises a solvent.
Aforesaid polyamic acid component, it has one between the solids content concn scope between the 4wt% to 20wt%.
Aforesaid polyamic acid component, it has one between the solids content concn scope between the 4wt% to 10wt%.
Aforesaid polyamic acid component, wherein said solvent is to be selected from: N-methyl-2-pyrrolinone, ethylene glycol monobutyl ether, N,N-DIMETHYLACETAMIDE, N, DMSO 99.8MIN., gamma-butyrolactone, tetramethyl-urea, hexamethylphosphorictriamide ,-cresols, xylenol, phenol, halogenation phenol chlorobenzene, ethylene dichloride, tetrachloroethane, pimelinketone or these a combination.
Aforesaid polyamic acid component, wherein said solvent are to be made up of N-methyl-2-pyrrolinone and ethylene glycol monobutyl ether.
Aforesaid polyamic acid component, the part by weight scope of wherein said N-methyl-2-pyrrolinone and ethylene glycol monobutyl ether is between 90: 10 to 60: 40.
Aforesaid polyamic acid component, the ratio of wherein said N-methyl-2-pyrrolinone and ethylene glycol monobutyl ether is 60: 40.
The object of the invention and solve its technical problem and also adopt following technical scheme to realize.According to a kind of alignment film that the present invention proposes, it is by solidifying a polyamic acid component as claimed in claim 1 obtained.
The object of the invention and solve its technical problem and also can adopt following technical measures further to realize.
Aforesaid alignment film, wherein said curing schedule are by this polyamic acid component is dissolved, and coat on the base material again and heat and accomplish.
The present invention compared with prior art has tangible advantage and beneficial effect.Know by above; In order to achieve the above object; Polyamic acid component of the present invention; Be to comprise one to react prepared polyamic acid A and by a kind of first reaction mixture and react prepared polyamic acid B by a kind of second reaction mixture; This first reaction mixture contains a kind of aromatic tetracarboxylic acid's dianhydride and a kind of aromatic diamine, and this second reaction mixture contains a kind of aliphatics tetracarboxylic dianhydride, a kind of aromatic diamine and a kind of non-aromatic diamines with side chain.
Because employed liquid crystal material has more aromatic group mostly (like phenyl ring) in the liquid-crystal display at present; Therefore; As desire to make liquid crystal material to have preferable orientation character; The compatible polyamic acid of structure that is preferably utilization and liquid crystal material prepares alignment film, just is preferably to use the polyamic acid with more aromatic group to prepare.In addition, as desire to make liquid crystal material to possess suitable tilt angle is arranged, the polyamic acid that then preferable use contains side chain prepares alignment film.So; Polyamic acid component of the present invention; Be preferable orientation character and anti-brush mill character (rubbing resistance to be provided by combining this to be used to) polyamic acid A and be used to provide the polyamic acid B of suitable tilt angle and better electrical character, meet the alignment film that industry requires to make.In polyamic acid component of the present invention; This first reaction mixture mainly is to contain the aromatic series reactant; Be aromatic tetracarboxylic acid's dianhydride and aromatic diamine; So that this polyamic acid A provides preferable LCD alignment character; The structure that adds aromatic group again is comparatively firm, more can let this polyamic acid A that preferable anti-brush mill character is provided.This second reaction mixture then is because contain the aromatic diamine that this has side chain; So that this polyamic acid B can provide suitable tilt angle; More because contain this aliphatics tetracarboxylic dianhydride and non-aromatic diamines; Make this polyamic acid B that preferable electrical property is provided, particularly higher voltage keeps ratio.Therefore,, make and utilize the prepared alignment film of polyamic acid component of the present invention to possess better electrical character, and suitable tilt angle and preferable orientation character can be provided, be very suitable for practicality by the combination of above-mentioned specific polyamic acid.
By technique scheme; Polyamic acid component of the present invention reaches has advantage and beneficial effect at least by its prepared alignment film: polyamic acid component of the present invention is the polyamic acid B that is used to that the polyamic acid A of preferable orientation character and anti-brush mill character is provided and is used to provide suitable tilt angle and better electrical character by combining; And let the prepared alignment film of this polyamic acid component of later use possess preferable electrical property is arranged, and make liquid crystal have suitable tilt angle and preferable orientation character.
In sum, the invention relates to that a kind of polyamic acid component reaches by its prepared alignment film.This polyamic acid component; It comprises: one reacts prepared polyamic acid A and by a kind of first reaction mixture reacts prepared polyamic acid B by a kind of second reaction mixture; This first reaction mixture contains a kind of aromatic tetracarboxylic acid's dianhydride and a kind of aromatic diamine, and this second reaction mixture contains a kind of aliphatics tetracarboxylic dianhydride, a kind of aromatic diamine and a kind of non-aromatic diamines with side chain.Also providing a kind of solidifies prepared alignment film with above-mentioned polyamic acid component in addition in the present invention, and this alignment film can make display unit possess higher voltage when practical application and keep ratio, suitable tilt angle and preferable orientation character.The present invention has above-mentioned plurality of advantages; No matter it all has bigger improvement on product structure or function; Obvious improvement is arranged technically; And produced handy and practical effect; And more existing polyamic acid component and alignment film have the outstanding effect of enhancement; Thereby being suitable for practicality more, and having the extensive utility value of industry, really is the new design of a novelty, progress, practicality.
Above-mentioned explanation only is the general introduction of technical scheme of the present invention; Understand technique means of the present invention in order can more to know; And can implement according to the content of specification sheets; And for let above-mentioned and other purposes of the present invention, feature and advantage can be more obviously understandable; The following special preferred embodiment of lifting; And conjunction with figs., specify as follows.
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Reach technique means and the effect that predetermined goal of the invention is taked for further setting forth the present invention; Below in conjunction with accompanying drawing and preferred embodiment; To the polyamic acid component that proposes according to the present invention and by its its embodiment of prepared alignment film, structure, characteristic and effect thereof, specify as after.
Polyamic acid component of the present invention comprises a kind of polyamic acid A and a kind of polyamic acid B.This polyamic acid A reacts obtained by a kind of first reaction mixture, and this first reaction mixture contains a kind of aromatic tetracarboxylic acid's dianhydride and a kind of aromatic diamine.This polyamic acid B reacts obtained by a kind of second reaction mixture, and this second reaction mixture contains a kind of aliphatics tetracarboxylic dianhydride, a kind of aromatic diamine and a kind of non-aromatic diamines with side chain.
Above-mentioned " non-aromatic diamines " speech is to comprise all non-ly to be the diamines of aromatic diamine, its objective is to be used to provide aliphatic group, to let this polyamic acid B that preferable electrical property is provided.
From the above; Polyamic acid A of the present invention and polyamic acid B can provide different efficacies character respectively; So; The content ratio of polyamic acid A and polyamic acid B can be adjusted according to subsequent use and liquid crystal material composition; Preferably; As desire to have concurrently better electrical character, suitable tilt angle and preferable orientation character, then the content ratio of this polyamic acid A and polyamic acid B is between 75: 25 to 30: 70; More preferably, the content ratio of this polyamic acid A and polyamic acid B is between 70: 30 to 50: 50.
In second reaction mixture of this polyamic acid B; This molar ratio with aromatic diamine and this non-aromatic diamines of side chain can be adjusted according to the required tilt angle of subsequent use and the composition of liquid crystal material; Preferably, this has the aromatic diamine of side chain and the molar ratio of this non-aromatic diamines is between 70: 30 to 1: 99; More preferably, this has the aromatic diamine of side chain and the molar ratio of this non-aromatic diamines is between 45: 55 to 3: 97.And in a specific examples of the present invention, this has the aromatic diamine of side chain and the molar ratio of this non-aromatic diamines is 6: 94.
This first reaction mixture mainly is to contain aromatic tetracarboxylic acid's dianhydride and aromatic diamine, but also can optionally add other reactants again, like the aliphatics tetracarboxylic dianhydride.Preferably, this first reaction mixture is to be made up of aromatic tetracarboxylic acid's dianhydride and aromatic diamine.
Aromatic tetracarboxylic acid's dianhydride of this first reaction mixture can be selected any existing aromatic tetracarboxylic acid's dianhydride for use; Preferably; This aromatic tetracarboxylic acid's dianhydride is to be selected from :1; 4; 5-pyromellitic acid dianhydride (pyromellitic dianhydride; Be designated hereinafter simply as " PMDA "); Phenylbenzene tetracarboxylic dianhydride (biphenyl tetracarboxylic dianhydride; Be designated hereinafter simply as " BPDA "); 5; 8-naphthalene tetracarboxylic acid dianhydride (1 dianhydride); 6; 7-naphthalene tetracarboxylic acid dianhydride (2) ' '-tetraphenyl silane tetracarboxylic dianhydride (3 ' '-tetraphenylsilanetetracarboxylicdianhydride ' '-dimethyl diphenyl silane tetracarboxylic dianhydride (3 ' '-dimethyldiphenylsilanetetracarboxylic dianhydride)); 3; 4-furans tetracarboxylic dianhydride (1) '-two (3; The 4-di carboxyl phenyloxy) '-two (3 diphenyl sulfide dianhydride (4 '-bis(3)diphenylsulfide dianhydride); The 4-di carboxyl phenyloxy) '-two (3 diphenyl sulfone dianhydride (4 '-bis(3)diphenylsulfone dianhydride); The 4-di carboxyl phenyloxy) diphenyl propane dianhydride (4 '-bis(3,4-dicarboxyphenoxy)diphenylpropane dianhydride); Two (phthalic acid) oxidation phosphniline dianhydride (bis(phthalic acid)phenylphosphine oxidedianhydride); To benzene-two (triphenylbenzene diformyl) dianhydride (p-phenylene-bis(triphenylphthalic)dianhydride); Between benzene-two (triphenylbenzene diformyl) dianhydride (m-phenylene-bis(triphenylphthalic)dianhydride); Two (triphenylbenzene dioctyl phthalate)-4,4 '-diphenyl ether dianhydride (bis(triphenylphthalicacid)-4 '-diphenylether dianhydride); Two (triphenylbenzene dioctyl phthalate)-4 '-ditan dianhydride (bis(triphenylphthalic acid)-4,4 '-diphenylmethanedianhydride), or these one the combination.And in a concrete example of the present invention, this aromatic tetracarboxylic acid's dianhydride is PMDA.
The aromatic diamine of this first reaction mixture can be any existing aromatic diamine; Preferably; This aromatic diamine is to be selected from: 2; The two [4-(4-amido phenoxys of 2-) phenyl] HFC-236fa (2)phenyl; Be designated hereinafter simply as " HFBAPP "); 2; Two (4-aminocarbonyl phenyl) the HFC-236fa (2)hexafluoropropane of 2-) phenyl '-two [4-(4-amidos-2-4-trifluoromethylphenopendant)] HFC-236fa (2 '-bis[4-(4-amino-2-trifluoromethylphenoxy)phenyl) '-two amido-2 '-two (trifluoromethyl) biphenyl (4 '-diamino-2 '-bis(trifluoromethyl)biphenyl) '-two [(4-amidos-2-trifluoromethyl) phenoxy octafluoro biphenyl (4 '-bis[(4-amino-2-trifluoromethyl)phenoxy) '-two (4-amido phenoxy) biphenyl (4 '-Bis(4-aminophenoxy)biphenyl; Be designated hereinafter simply as " BAPB "); Ursol D (p-phenylenediamine); Mphenylenediamine (m-phenylenediamine) '-two amido-3 '-dicarboxyl ditan (4 '-diamino-3 '-dicarboxydiphenylmethane); 1; Two (4-aminocarbonyl phenyl) the benzene (1)benzene of 4-) '-dicarboxyl-4 '-dichloro-4 '-benzidine (3 '-dichloro-4 '-diaminobiphenyl '-dihydroxyl-4 '-benzidine (3 '-dihydroxy-4 '-diaminobiphenyl '-dimethoxy-4 '-benzidine (3 '-dimethoxy-4 '-diaminobiphenyl '-dimethyl--4 '-benzidine (3 '-dimethyl-4 '-diaminobiphenyl '-benzidine (4 '-diaminobiphenyl))))); 4-benzidine (3 '-dicarboxy-4 '-diaminobiphenyl); Two amido ditan (diaminodiphenylmethane); Two amido diphenyl ether (diaminodiphenyl ether); 2; 2-two amido diphenyl propane (2) '-two amido sulfobenzide (4 '-diaminodiphenylsulfone); Two amido benzophenone (diaminobenzophenone); 1; Two (4-amido phenoxy) the benzene (1)benzene) of 3-; 1; Two (4-amido phenoxy) the benzene (1)benzene of 4-) '-two (4-amido phenoxy) sulfobenzide (4 '-di(4-aminophenoxy)diphenylsulfone); 2; The two [4-(4-amido phenoxys of 2-) phenyl] propane (2)phenyl), or these a combination.And in a concrete example of the present invention, this aromatic diamine is BAPB.
This second reaction mixture mainly is aromatic diamine and the non-aromatic diamines that contains aliphatics tetracarboxylic dianhydride, tool side chain, but also can optionally add other reactants again, as does not have the aromatic diamine of side chain.Preferably, this second reaction mixture is that aromatic diamine and non-aromatic diamines by aliphatics tetracarboxylic dianhydride, tool side chain constitutes.
The aliphatics tetracarboxylic dianhydride of this second reaction mixture can be any existing aliphatics tetracarboxylic dianhydride, and preferably, this aliphatics the tetracarboxylic dianhydride be selected from: two ring (2,2) suffering-7-alkene-2,3,6-tetracarboxylic dianhydride (bicyclo(2,2)oct-7-ene-2,3,5 dianhydride are designated hereinafter simply as " BCDA "), 2; 3; 4-butane tetracarboxylic acid dianhydride (1,2,3 dianhydride; Be designated hereinafter simply as " BDA "), 4-dicarboxyl-1,2; 3; 4-tetrahydrochysene-1-naphthalene Succinic anhydried (3,4-dicarboxy-1,2 are designated hereinafter simply as " TDA "), 3; 5-tricarboxylic basic ring amyl group second dianhydride (2,5-tricarboxycyclopentylacetic dianhydride), 2; 3; 4-tetramethylene tetracarboxylic dianhydride (1,2,3 dianhydride); 1; 3-dimethyl--1,2,3; 4-tetramethylene tetracarboxylic dianhydride (1,2,3 dianhydride), 3,4-pentamethylene tetracarboxylic dianhydride (1,4-cyclopentanetetracarboxylicdianhydride), 5; 6-three carboxyls norbornane-2-second dianhydride (3,6-tricarboxynorbornane-2-acetic dianhydride), 3; 4; 5-THF tetracarboxylic dianhydride (2,3,4 dianhydride), or these a combination.And in a concrete example of the present invention, this aliphatics tetracarboxylic dianhydride is BDA.
This aromatic diamine with side chain can be selected any existing aromatic diamine with side chain for use, particularly has the aromatic diamine of aliphatic lateral chain.Preferably; This aromatic diamine with side chain is to be selected from: the diamines shown in the following formula (I); 1; The two [4-(4-amido phenoxys of 1-) phenyl] the-4-(cyclohexyl methyl) hexanaphthene (1)phenyl)cyclohexane); 1; The two [4-(4-amido phenoxys of 1-) methyl phenyl methylcyclohexyl)] hexanaphthene (1)phenyl)methyl); 1; The two [4-(4-amido phenoxys of 1-) methyl phenyl ethyl cyclohexyl)] hexanaphthene (1)phenyl)methyl); 1; The two [4-(4-amido phenoxys of 1-) methyl phenyl propyl group cyclohexyl)] hexanaphthene (1,1-bis[4-(4-aminophenoxy)phenyl)methyl), the two [4-(4-amido phenoxys of 1-) phenyl butyl cyclohexyl) methyl] hexanaphthene (1)phenyl)methyl); 1; The two [4-(4-amido phenoxys of 1-) methyl phenyl amyl group cyclohexyl)] hexanaphthene (1,1-bis[4-(4-aminophenoxy)phenyl)methyl), the two [4-(4-amido phenoxys of 1-) phenyl hexyl cyclohexyl) methyl] hexanaphthene (1)phenyl)methyl); 1; The two [4-(4-amido phenoxys of 1-) methyl phenyl heptyl cyclohexyl)] hexanaphthene (1,1-bis[4-(4-aminophenoxy)phenyl)methyl), the two [4-(4-amido phenoxys of 1-) phenyl octyl group cyclohexyl) methyl] hexanaphthene (1)phenyl)methyl); 1; Two (4-aminocarbonyl phenyl) the-4-(cyclohexyl methyls of 1-) hexanaphthene (1,1-bis(4-aminophenyl)-4-(cyclohexylmethyl)cyclohexane), two (the 4-aminocarbonyl phenyl)-4-[(4-methylcyclohexyl) methyl of 1-] hexanaphthene (1)-4-[(4-methylcyclohexyl)methyl); 1; Two (the 4-aminocarbonyl phenyl)-4-[(4-ethyl cyclohexyl) methyl of 1-] hexanaphthene (1,1-bis(4-aminophenyl)-4-[(4-ethylcyclohexyl)methyl), two (the 4-aminocarbonyl phenyl)-4-[(4-propyl group cyclohexyl) methyl of 1-] hexanaphthene (1)-4-[(4-propylcyclohexyl)methyl); 1; Two (the 4-aminocarbonyl phenyl)-4-[(4-butyl cyclohexyl) methyl of 1-] hexanaphthene (1,1-bis(4-aminophenyl)-4-[(4-butylcyclohexyl)methyl), two (the 4-aminocarbonyl phenyl)-4-[(4-amyl group cyclohexyl) methyl of 1-] hexanaphthene (1)-4-[(4-pentylcyclohexyl)methyl); 1; Two (the 4-aminocarbonyl phenyl)-4-[(4-hexyl cyclohexyl) methyl of 1-] hexanaphthene (1,1-bis(4-aminophenyl)-4-[(4-hexylcyclohexyl)methyl), two (the 4-aminocarbonyl phenyl)-4-[(4-heptyl cyclohexyl) methyl of 1-] hexanaphthene (1)-4-[(4-heptylcyclohexyl)methyl); 1; Two (the 4-aminocarbonyl phenyl)-4-[(4-octyl group cyclohexyl) methyl of 1-] hexanaphthene (1,1-bis(4-aminophenyl)-4-[(4-octylcyclohexyl)methyl e), the two [4-(4-amido phenoxys of 1-) phenyl] the-4-(phenyl methyl) hexanaphthene (1)phenyl)cyclohexane); 1; The two [4-(4-amido phenoxys of 1-) methyl phenyl aminomethyl phenyl)] hexanaphthene (1,1-bis[4-(4-aminophenoxy)phenyl)methyl), the two [4-(4-amido phenoxys of 1-) phenyl ethylphenyl) methyl] hexanaphthene (1)phenyl)methyl); 1; The two [4-(4-amido phenoxys of 1-) methyl phenyl propyl group phenyl)] hexanaphthene (1,1-bis[4-(4-aminophenoxy)phenyl)methyl), the two [4-(4-amido phenoxys of 1-) phenyl butyl phenyl) methyl] hexanaphthene (1)phenyl)methyl); 1; The two [4-(4-amido phenoxys of 1-) methyl phenyl amyl group phenyl)] hexanaphthene (1,1-bis[4-(4-aminophenoxy)phenyl)methyl), the two [4-(4-amido phenoxys of 1-) phenyl hexyl phenyl) methyl] hexanaphthene (1)phenyl)methyl); 1; The two [4-(4-amido phenoxys of 1-) methyl phenyl heptyl phenyl)] hexanaphthene (1,1-bis[4-(4-aminophenoxy)phenyl)methyl), the two [4-(4-amido phenoxys of 1-) phenyl octyl phenyl) methyl] hexanaphthene (1)phenyl)methyl); 1; Two (4-aminocarbonyl phenyl) the-4-(phenyl methyls of 1-) hexanaphthene (1,1-bis(4-aminophenyl)-4-(phenyl methyl)cyclohexane), two (the 4-aminocarbonyl phenyl)-4-[(4-aminomethyl phenyl) methyl of 1-] hexanaphthene (1)-4-[(4-methylphenyl)methyl); 1; Two (the 4-aminocarbonyl phenyl)-4-[(4-ethylphenyl) methyl of 1-] hexanaphthene (1,1-bis(4-aminophenyl)-4-[(4-ethylphenyl)methyl), two (the 4-aminocarbonyl phenyl)-4-[(4-propyl group phenyl) methyl of 1-] hexanaphthene (1)-4-[(4-propylphenyl)methyl); 1; Two (the 4-aminocarbonyl phenyl)-4-[(4-butyl phenyl) methyl of 1-] hexanaphthene (1,1-bis(4-aminophenyl)-4-[(4-butylphenyl)methyl), two (the 4-aminocarbonyl phenyl)-4-[(4-amyl group phenyl) methyl of 1-] hexanaphthene (1)-4-[(4-pentyl phenyl)methyl); 1; Two (the 4-aminocarbonyl phenyl)-4-[(4-hexyl phenyl) methyl of 1-] hexanaphthene (1,1-bis(4-aminophenyl)-4-[(4-hexylphenyl)methyl), two (the 4-aminocarbonyl phenyl)-4-[(4-heptyl phenyl) methyl of 1-] hexanaphthene (1)-4-[(4-heptylphenyl)methyl); 1; Two (the 4-aminocarbonyl phenyl)-4-[(4-octyl phenyl) methyl of 1-] hexanaphthene (1,1-bis(4-aminophenyl)-4-[(4-octylphenyl)methyl), the two [4-((4-aminocarbonyl phenyls of 1-) methyl) phenyl] the-4-(phenyl methyl) hexanaphthene (1)methyl)phenyl)cyclohexane); 1; The two [4-((4-aminocarbonyl phenyls of 1-) methyl phenyl aminomethyl phenyl methyl))] hexanaphthene (1,1-bis[4-((4-aminophenyl)methyl)phenyl)methyl), the two [4-((4-aminocarbonyl phenyls of 1-) methyl) phenyl ethylphenyl) methyl] hexanaphthene (1)methyl)phenyl)methyl); 1; The two [4-((4-aminocarbonyl phenyls of 1-) methyl phenyl propyl group phenyl methyl))] hexanaphthene (1,1-bis[4-((4-aminophenyl)methyl)phenyl)methyl), the two [4-((4-aminocarbonyl phenyls of 1-) methyl) phenyl butyl phenyl) methyl] hexanaphthene (1)methyl)phenyl)methyl); 1; The two [4-((4-aminocarbonyl phenyls of 1-) methyl phenyl amyl group phenyl methyl))] hexanaphthene (1,1-bis[4-((4-aminophenyl)methyl)phenyl)methyl), the two [4-((4-aminocarbonyl phenyls of 1-) methyl) phenyl hexyl phenyl) methyl] hexanaphthene (1)methyl)phenyl)methyl); 1; The two [4-((4-aminocarbonyl phenyls of 1-) methyl phenyl heptyl phenyl methyl))] hexanaphthene (1,1-bis[4-((4-aminophenyl)methyl)phenyl)methyl), the two [4-((4-aminocarbonyl phenyls of 1-) methyl) phenyl octyl phenyl) methyl] hexanaphthene (1)methyl)phenyl)methyl), or these a combination.In a concrete example of the present invention, this aromatic diamine with side chain is the diamines shown in this formula (I).
Figure G061G2208920061214D000151
Preferably, this non-aromatic diamines is to be selected from: aliphatie diamine (aliphatic amine), alicyclic diamine (alicyclic amine) or these one the combination.And in a concrete example of the present invention, this non-aromatic diamines is an alicyclic diamine.
This aliphatie diamine can be selected any existing aliphatie diamine for use, and preferably, this aliphatie diamine is to be selected from: 1; 4-two amidos-1,1-dimethylbutane (1,4-diamino-1), 4-two amidos-1-ethyl butane (1,4-diamino-1-ethylbutane); 1; 4-two amidos-1,2-dimethylbutane (1,4-diamino-1); 1; 4-two amidos-1,3-dimethylbutane (1,4-diamino-1); 1; 4-two amidos-1,4-dimethylbutane (1,4-diamino-1); 1; 4-two amidos-2,3-dimethylbutane (1,4-diamino-2); 1; 2-two amidos-1-butyl ethane (1,2-diamino-1-butylethane), 6-two amidos-2; 5-dimethylhexane (1,5-dimethylhexane), 6-two amidos-2; 4-dimethylhexane (1,4-dimethylhexane), 6-two amidos-3; 3-dimethylhexane (1,3-dimethylhexane), 6-two amidos-2; 2-dimethylhexane (1,2-dimethylhexane), 6-two amidos-2; 2; 4-trimethyl cyclohexane (1,6-diamino-2,2); 1; 6-two amidos-2,4,4-trimethyl cyclohexane (1,4-trimethylhexane), or these a combination.
This alicyclic diamine can be selected any existing alicyclic diamine for use; Preferably; This alicyclic diamine is to be selected from :4 '-two amido dicyclohexyl methyl hydride (4 '-diaminodicyclohexylmethane; Be designated hereinafter simply as " HDAM "); 1; 4-diamines basic ring hexane (1); 1; Two (4-amido cyclohexyl) the propane (1)propane) of 1-; 2; Two (4-amido cyclohexyl) the propane (2)propane) of 2-; 1; Two (4-amido cyclohexyl) the ethane (1)ethane) of 1-; 1; Two (4-amido cyclohexyl) the butane (1)butane) of 1-; 2; Two (4-amido cyclohexyl) the butane (2)butane) amido cyclohexyl)-2-(4-aminomethyl cyclohexyl of 2-) methane (2-(4-aminocyclohexyl)-2-(4-amino-3-methylcyclohexyl)methane); 4-amido-3; 5-Dimethylcyclohexyl-4-amido-3-methyl cyclohexane methylmethane (4-amino-3); 4-amido cyclohexyl-4-amido-3-methyl cyclohexane methylmethane (4-aminocyclohexyl-4-amino-3-methylcyclohexylmethane); 2; Two (the 4-amidos-3 of 2-; The 5-Dimethylcyclohexyl) butane (2 )butane); 2; Two (the 4-amidos-3 of 2-; The 5-Dimethylcyclohexyl) propane (2 )propane); 1; Two (the 4-amidos-3 of 1-; The 5-Dimethylcyclohexyl) ethane (1 )ethane); 2; Two (4-amido-3-methylcyclohexyl) the propane (2)propane) of 2-; 1; Or these a combination two (4-amido-3-methylcyclohexyl) the ethane (1)ethane of 1-).And in a concrete example of the present invention, this alicyclic diamine is HDAM.
Preferably, this polyamic acid component also comprises a solvent, and this solvent is the concentration that is used to regulate and control this polyamic acid component, is beneficial to the making of follow-up alignment film; More preferably, this polyamic acid component has one between the solids content concn scope between the 4wt% to 20wt%; Again more preferably, this polyamic acid component has one between the solids content concn scope between the 4wt% to 10wt%, and in a concrete example of the present invention, this polyamic acid component has the solids content concn of 8wt%.
Polyamic acid component of the present invention is by prepared polyamic acid A and polyamic acid B being mixed and obtaining.And in a concrete example of the present invention; Polyamic acid A and polyamic acid B are mixed with an amount of above-mentioned solvent respectively; So that the concentration of this polyamic acid A and this polyamic acid B is identical; Again this polyamic acid A and this polyamic acid B are given blending at last, to obtain this polyamic acid component.
Preferably; This solvent is to be selected from: N-methyl-2-pyrrolinone (N-Methyl-2-pyrrolidinone; Be designated hereinafter simply as " NMP "); Ethylene glycol monobutyl ether (Ethyleneglycol monobutyl ether; Be designated hereinafter simply as " BC "); N,N-DIMETHYLACETAMIDE (dimethylacetamide); N (dimethylformamide); DMSO 99.8MIN. (dimethylsulfoxide); Gamma-butyrolactone (γ-butyrolactone); Tetramethyl-urea (tetramethylurea); Hexamethylphosphorictriamide (hexamethylphosphortriamide); Between-cresols (m-cresol); Xylenol (xylenol); Phenol (phenol); Halogenation phenol chlorobenzene (halogenated phenol chlorobenzene); Ethylene dichloride (dichloroethane); Tetrachloroethane (tetrachloroethane); Pimelinketone (cyclohexanone), or these one the combination.More preferably, this solvent is to be made up of NMP and BC.Again more preferably, the part by weight scope of NMP and BC is between 90: 10 to 60: 40.And in a concrete example of the present invention, the part by weight of NMP and BC is 60: 40.
The present invention provides a kind of alignment film in addition; This alignment film is by solidifying above-mentioned polyamic acid component obtained; In solidification process, this polyamic acid component (dehydration that can dewater) and closed loop (ring-closing) reaction and change polyimide fully into.The making method of this alignment film can be carried out according to general method for making; For example; Utilize solvent that above-mentioned polyamic acid component is dissolved; Again it is coated on the base material; Then under proper temperature, carry out roasting in advance (prebakecuring) and roasting admittedly (curing); So that after this polyamic acid component changes polyimide into fully, and then on this base material, form one by alignment film that this polyimide constituted.
Alignment film of the present invention can carry out pre-treatment (for example bristle (rubbing) step according to the treatment process of general alignment film when being subsequently applied to liquid crystal indicator), then assemble according to the structure of general liquid crystal indicator again.
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The present invention will be described further with regard to following examples, but will be appreciated that, said embodiment is the purposes for illustrating only, and should not be interpreted as the restriction that the present invention implements.
[chemical]
(1) employed in aromatic tetracarboxylic acid's dianhydride: embodiment and the comparative example is 1,2,4,5-pyromellitic acid dianhydride (PMDA is by the manufacturing of Britain LANCASTER company).
(2) aromatic diamine: embodiment and comparative example are employed to be 4,4 '-two (4-amido phenoxy) biphenyl (BAPB is by the manufacturing of Japanese WAKAYAMA SEIKA OGYO company).
(3) aliphatics tetracarboxylic dianhydride: embodiment and comparative example are employed is 1,2,3, and 4-butane tetracarboxylic acid dianhydride (BDA is by the manufacturing of Japanese NEW JAPAN CHEMICAL company).
(4) have the aromatic diamine of side chain: embodiment and comparative example are employed be the diamines shown in the above-mentioned formula (I) [be by with molar ratio be 1: 13; 5-dinitrobenzoyl chlorine (3 chloride) with cholesterol (cholesterol) be dissolved in the toluene; Then add 1 pyridine of ear mole not again; Under 25 ℃, react and last 10 hours then; Purified again and obtain dinitro compound; At last this dinitro compound is carried out reduction reaction, can make the diamines shown in the above-mentioned formula (I)].
(5) employed in alicyclic diamine: embodiment and the comparative example is 4,4 '-two amido dicyclohexyl methyl hydrides (HDAM by the new Japanese physics and chemistry (NEW JAPAN CHEMICAL Co of company of Japan, Ltd) makes).
(6) employed in solvent: embodiment and the comparative example is N-methyl-2-pyrrolinone (NMP) and ethylene glycol monobutyl ether (BC) combination, its part by weight is 60: 40.
< > [the common method for making of embodiment 1 and comparative example 1~8] <>
One, the preparation of polyamic acid A1~A4 and B1:
A1: the HDAM of 21.17 grams and the BDA of 19.01 grams are added among the NMP of 206 grams, under 20 ℃ of temperature, stirred 24 hours again, and then add an amount of above-mentioned solvent and dilute, to obtain the polyamic acid A1 that solids content concn is 8wt%.
A2: the HDAM of 8.75 grams, the BDA of 8.02 grams, the BAPB of 4.90 grams and the PMDA of 8.48 grams are added among the NMP of 161 grams; Under 20 ℃ of temperature, stirred 24 hours again; And then add an amount of above-mentioned solvent and dilute, to obtain the polyamic acid A2 that solids content concn is 8wt%.
A3: the HDAM of 4.05 grams, the BDA of 3.71 grams, the BAPB of 20.70 grams and the PMDA of 11.94 grams are added among the NMP of 162 grams; Under 20 ℃ of temperature, stirred 24 hours again; And then add an amount of above-mentioned solvent and dilute, to obtain the polyamic acid A3 that solids content concn is 8wt%.
A4: the BAPB of 26.13 grams and the PMDA of 13.93 grams are added among the NMP of 160 grams, under 20 ℃ of temperature, stirred 24 hours again, and then add an amount of above-mentioned solvent and dilute, to obtain the polyamic acid A4 that solids content concn is 8wt%.
B1: the HDAM of compound shown in the formula (I) of 2.94 grams, 19.09 grams and the BDA of 18.24 grams are added among the NMP of 195 grams; Under 20 ℃ of temperature, stirred 24 hours again; And then add an amount of above-mentioned solvent and dilute, to obtain the polyamic acid B1 that solids content concn is 8wt%.
The above-mentioned content (mol% that is used to prepare each reactant of polyamic acid A1~A4 and B1) arrangement is like following table l.
Table 1
Two, the preparation of the polyamic acid component of embodiment and comparative example
Embodiment 1: the above-mentioned polyamic acid B1 of 250 grams being mixed with the polyamic acid A4 of 250 grams, and under 20 ℃ of temperature, stirred 6 hours, is the polyamic acid component of 8wt% to obtain solids content concn.
Comparative example 1~5: comparative example 1~5 is respectively above-mentioned polyamic acid B1, polyamic acid A1, polyamic acid A2, polyamic acid A3 and polyamic acid A4 in regular turn
Comparative example 6~8: the above-mentioned polyamic acid B1 of 250 grams is mixed with polyamic acid A1, polyamic acid A2 and the polyamic acid A3 of 250 grams respectively; And under 20 ℃ of temperature, stirred 6 hours, to obtain comparative example 6,7 that solids content concn is 8wt% and 8 polyamic acid component respectively.
Three, the preparation of alignment film:
Utilize a spin coater (spin coater) and with/20 seconds speed of 4000 commentaries on classics; The above-mentioned polyamic acid component or the polyamic acid of 3 grams are coated on a tin indium oxide (ITO) glass (length and width are respectively 50 millimeters); Then under 80 ℃ of temperature, baked 10 minutes in advance again; And under 220 ℃ of temperature, baked 60 minutes admittedly; So that this polyamic acid component reaction changes polyimide into, and then on this ito glass, form an alignment film.According to above-mentioned step, can make the alignment film of embodiment 1 and comparative example 1~8 respectively.
[test of the alignment film of embodiment 1 and comparative example 1~8]
The alignment film of embodiment 1 and comparative example 1~8 carries out sample making and test according to following method respectively:
(1) tilt angle test:
Sample making:
Utilize a carding and brushing machine (rubbing machine; By Taiwan hundred million (E-SUN PrecisionIndustrial Co. still) company's manufacturing; Model is ESR-1; Its amount of being pressed into is 0.5 millimeter; Roller diameter is that 170 millimeters (700 change); Platform speed is that 100 mm/min and employed tPile are YA-25; Two ito glasses that are formed with this alignment film are carried out the bristle step respectively; Then from top to bottom stacked in regular turn: a slice is formed with the ito glass of this alignment film, and (this alignment film is) down; A slice polyethylene terephthalate film (polyethylene terephthalate film; It is the PET film; Its length is 50 millimeters; Width is that 5 millimeters and thickness are 50 microns); A slice polyethylene terephthalate film, and a slice is formed with the ito glass (this alignment film is up) of this alignment film.After the mutual contraposition pressing of each above-mentioned layer; Between two polyethylene terephthalate film, insert liquid crystal again (by Taiwan Daily polymer Corp. (DAILYPOLYMERCORP.) manufacturing; Article are called DN-132131; Phase inversion temperature is 90 ℃; This liquid crystal does not contain chiral dope); Promptly coat a sticker then and (be to use epoxide resin AB glue in the formed side all around of above-mentioned each layer; Make by Taiwan Nanya Plastic Cement Industry Co., Ltd (NAN-YAPLATICSCO.)); And form an adhesion coating that coats above-mentioned each layer side, and make an element.At last whole element was heated 5 minutes under 90 ℃ of temperature, just make a tilt angle specimen.
Tilt angle is measured:
After treating that above-mentioned sample drops to room temperature, utilize a tilt angle measuring machine (Tilt Bias AngleMeasuring system again, by the manufacturing of German AUTRONIC company, model is TBA 107) carry out the measurement of tilt angle, its result is respectively shown in following table 2.The character that the numerical value of tilt angle need cooperate liquid crystal is the quality of this sample of decidable, and to stablize tilt angle be preferable keeping.
(2) voltage is kept the test of ratio (VHR) and orientation character:
Sample making:
Likewise utilize a brushing machine (imposing a condition as mentioned above of machine); Two ito glasses that are formed with this alignment film are carried out the bristle step respectively; Get the ito glass that a slice is formed with this alignment film; Edge on this alignment film is coated with a frame glue (Seal again; By the MITSUICHEMICALS of Japan; The manufacturing of INC company); And stay the hole (its purposes is to provide the follow-up liquid crystal of inserting) that a length is about 20 microns; Then get the ito glass that a slice is formed with this alignment film; And on this alignment film, spray most distance piece (spacer; By the manufacturing of SEKISUICHEMICAL company of Japan; Diameter is 6.75 microns and every square centimeter and sprays 150~200 approximately; The purposes of distance piece is to allow and can forms most gaps between two alignment films; For the follow-up liquid crystal of inserting); And then the alignment film that will be printed on the ito glass of frame glue has the alignment film of said distance piece to give parallel relative bonding with spraying, and makes the element with a hole.In this hole, insert a liquid crystal material (by the manufacturing of Taiwan Daily polymer Corp.; Article are called XLC-2185; The composition of this liquid crystal material will be described hereinafter); On this hole, be coated with a ultraviolet optical cement then; Under UV-light, be cured again, to seal this hole and to make a sample.At last entire sample was heated 5 minutes under 90 ℃ of temperature, just make a specimen.
The composition of liquid crystal material:
The employed liquid crystal material of above-mentioned specimen comprises following compounds:
Voltage is kept the ratio test:
Utilize a VHR measuring system (VHR Measuring System; By Japanese Dongyang (Toyo) company's manufacturing; Model is VHR-1A); Specimen is imposed a positive pulse voltage and a negative pulse voltage; During two voltage spaces, make sample be open (open) state; The positive and negative voltage of record and time formed two areas on X, Y axle that continue, again with two area additions divided by 2, promptly obtain the VHR observed value.
The observation of orientation character:
Utilize a polarizing microscope (Polarizing Microscope; By the manufacturing of Japanese NIKON company; Model is Type 120) directly with the adhesive coating of above-mentioned sample of visual inspection and above-mentioned sample and the interface between the liquid crystal layer; Its result is respectively shown in following table 2; The result of table 2 is with the judgement as the result of the liquid crystal layer surface of entire sample, with " not producing non-homogeneous zone (no domain just) " for having best regiospecific.
Table 2
? Polyamic acid is formed Tilt angle (°) VHR(%) Orientation character (whether producing non-homogeneous zone)
Embodiment 1 B1+A4 7.6 99.4 Not
Comparative example 1 B1 35.1 99.4 Be
Comparative example 2 A1 2.4 99.1 Not
Comparative example 3 A2 2.7 97.7 Not
Comparative example 4 A3 2.7 94.3 Not
Comparative example 5 A4 2.2 66.2 Not
Comparative example 6 B1+A1 11 99.4 Be
Comparative example 7 B1+A2 9.2 99.2 Be
Comparative example 8 B1+A3 10 99.5 Be
(result)
Result by table 2 can know, though comparative example 1,6,7 and 8 has good tilt angle and voltage is kept ratio, all produces non-homogeneous zone; Though and comparative example 2,3,4 and 5 has preferable orientation character, tilt angle and voltage are kept ratio and are still remained to be improved, so comparative example 1~8 all can't meet the requirement of industry.And by the result of embodiment 1; Tilt angle is 7.6 °; Voltage is kept ratio up to 99.4% and do not produce non-homogeneous zone; It is thus clear that the alignment film of embodiment 1 can meet the demand of industry fully, prove that simultaneously alignment film of the present invention has suitable tilt angle really, keeps ratio and preferable orientation character greater than 99% voltage.
[content ratio of polyamic acid A and polyamic acid B is inquired into]
According to the blending ratio of following table 3, respectively above-mentioned polyamic acid B1 and polyamic acid A4 are mixed, and under 20 ℃ of temperature, stirred 6 hours, be the polyamic acid component of the embodiment 1~12 of 8wt% to obtain solids content concn.
Then; According to the above-mentioned method for preparing alignment film, respectively prepared polyamic acid component is processed alignment film again, and according to above-mentioned each item testing method; Carry out the test of tilt angle, voltage maintenance ratio and orientation character, the result who is obtained is as shown in table 3 below.
Table 3
Figure DEST_PATH_GFW00000055528600011
(result)
Result by table 3 can know; When the blending ratio of polyamic acid B1 and polyamic acid A4 is between 25: 75~30: 70; The voltage that can obtain 7.3 °~16.1 ° tilt angle~99.4% is kept ratio and is not produced non-homogeneous zone; Particularly when blending ratio during between 30: 70~50: 50; Voltage is kept ratio all up to 99.4%; It is thus clear that possessing higher voltage really, the alignment film of this case keeps ratio; And make liquid crystal have suitable tilt angle and preferable orientation character, so also the polyamic acid component of simultaneous verification this case helps follow-up application really.
In addition; Keep the poor slightly situation of ratio though occur voltage in the The above results; But these results can or improve process conditions (amount of being pressed into of rubbing like storing temperature, time and the brush of alignment film) and wait and adjust by the composition that changes liquid crystal material, and then more meet the requirement of industry.
In sum; Polyamic acid component of the present invention is the polyamic acid B that is used to that the polyamic acid A of preferable orientation character and anti-brush mill character is provided and is used to provide suitable tilt angle and better electrical character by combining; And let the prepared alignment film of this polyamic acid component of later use possess better electrical character (voltage keep ratio can up to 99.4%), and make liquid crystal have suitable tilt angle (7.3 °~16.1 °) and preferable orientation character.
The above; It only is preferred embodiment of the present invention; Be not that the present invention is done any pro forma restriction; Though the present invention discloses as above with preferred embodiment; Yet be not in order to limit the present invention; Anyly be familiar with the professional and technical personnel; In not breaking away from technical scheme scope of the present invention; When the technology contents that can utilize above-mentioned announcement is made a little change or is modified to the equivalent embodiment of equivalent variations; In every case be not break away from technical scheme content of the present invention;, all still belong in the scope of technical scheme of the present invention any simple modification, equivalent variations and modification that above embodiment did according to technical spirit of the present invention.

Claims (25)

1. polyamic acid component is characterized in that it comprises:
A kind of polyamic acid A is to react obtained by a kind of first reaction mixture, and this first reaction mixture contains a kind of aromatic tetracarboxylic acid's dianhydride and a kind of aromatic diamine; And
A kind of polyamic acid B is to react obtained by a kind of second reaction mixture, and this second reaction mixture contains a kind of aliphatics tetracarboxylic dianhydride, a kind of aromatic diamine and a kind of non-aromatic diamines with side chain,
Wherein, The content ratio of this polyamic acid A and B is between 75: 25 to 30: 70; And in second reaction mixture of this polyamic acid B, this has the aromatic diamine of side chain and the molar ratio of this non-aromatic diamines is between 70: 30 to 1: 99.
2. polyamic acid component as claimed in claim 1 is characterized in that the content ratio of wherein said polyamic acid A and polyamic acid B is between 70: 30 to 50: 50.
3. polyamic acid component as claimed in claim 1 is characterized in that wherein saidly having the aromatic diamine of side chain and the molar ratio of this non-aromatic diamines is between 45: 55 to 3: 97.
4. polyamic acid component as claimed in claim 3 is characterized in that wherein saidly having the aromatic diamine of side chain and the molar ratio of this non-aromatic diamines is 6: 94.
5. polyamic acid component as claimed in claim 1, the aromatic tetracarboxylic acid's dianhydride that it is characterized in that wherein said first reaction mixture is to be selected from :1,2; 4; 5-pyromellitic acid dianhydride; Phenylbenzene tetracarboxylic dianhydride, 4,5; 8-naphthalene tetracarboxylic acid dianhydride, 6,7-naphthalene tetracarboxylic acid dianhydride ', 4 '-dimethyl diphenyl silane tetracarboxylic dianhydride, 3 ' '-tetraphenyl silane tetracarboxylic dianhydride, 2,3; 4-furans tetracarboxylic dianhydride '-two (3, the 4-di carboxyl phenyloxy) diphenyl sulfide dianhydride, 4 '-two (3; The 4-di carboxyl phenyloxy) diphenyl sulfone dianhydride '-two (3, the 4-di carboxyl phenyloxy) the diphenyl propane dianhydride; Two (phthalic acid) oxidation phosphniline dianhydride; To benzene-two (triphenylbenzene diformyl) dianhydride; Between benzene-two (triphenylbenzene diformyl) dianhydride; Two (triphenylbenzene dioctyl phthalate)-4,4 '-diphenyl ether dianhydride; Two (triphenylbenzene dioctyl phthalate)-4 '-ditan dianhydride, or these a combination.
6. polyamic acid component as claimed in claim 5 is characterized in that wherein said aromatic tetracarboxylic acid's dianhydride is 1,2,4,5-pyromellitic acid dianhydride.
7. polyamic acid component as claimed in claim 1; The aromatic diamine that it is characterized in that wherein said first reaction mixture is to be selected from: 2; The two [4-(4-amido phenoxys of 2-) phenyl] HFC-236fa; 2; Two (4-aminocarbonyl phenyl) HFC-236fa ' of 2--two [4-(4-amidos-2-4-trifluoromethylphenopendant) phenyl] HFC-236fa '-two amido-2 '-two (trifluoromethyl) biphenyl '-two [(4-amidos-2-trifluoromethyl) phenoxy octafluoro biphenyl '-two (4-amido phenoxy) biphenyl; Ursol D; Mphenylenediamine '-two amido-3 '-dicarboxyl ditan; 1; The two (4-aminocarbonyl phenyls of 4-) benzene '-benzidine '-dimethyl--4 '-benzidine '-dimethoxy-4 '-benzidine '-dihydroxyl-4 '-benzidine '-dichloro-4 '-benzidine, 3 '-dicarboxyl-4,4-benzidine; Two amido ditans; Two amido diphenyl ethers; 2; 2-two amido diphenyl propane '-two amido sulfobenzides; Two amido benzophenone, two (4-amido phenoxy) benzene of 3-, two (4-amido phenoxy) benzene '-two (4-amido phenoxy) sulfobenzide of 4-, the two [4-(4-amido phenoxys of 2-) phenyl] propane; Or these a combination.
8. polyamic acid component as claimed in claim 7 is characterized in that wherein said aromatic diamine is 4,4 '-two (4-amido phenoxy) biphenyl.
9. polyamic acid component as claimed in claim 1, the aliphatics tetracarboxylic dianhydride who it is characterized in that wherein said second reaction mixture is selected from: two ring (2,2,2) suffering-7-alkene-2,5,6-tetracarboxylic dianhydride, 2,4-butane tetracarboxylic acid dianhydride, 4-dicarboxyl-1,3,4-tetrahydrochysene-1-naphthalene Succinic anhydried, 5-tricarboxylic basic ring amyl group second dianhydride, 2,4-tetramethylene tetracarboxylic dianhydride, 3-dimethyl--1,3,4-tetramethylene tetracarboxylic dianhydride, 3,4-pentamethylene tetracarboxylic dianhydride, 6-three carboxyls norbornane-2-second dianhydride, 3,5-THF tetracarboxylic dianhydride, or these a combination.
10. polyamic acid component as claimed in claim 9 is characterized in that wherein said aliphatics tetracarboxylic dianhydride is 1,2,3,4-butane tetracarboxylic acid dianhydride.
11. polyamic acid component as claimed in claim 1; The aromatic diamine with side chain that it is characterized in that wherein said second reaction mixture is to be selected from: the diamines shown in the following formula (I); 1; The two [4-(4-amido phenoxys of 1-) phenyl] the-4-(cyclohexyl methyl) hexanaphthene; 1; The two [4-(4-amido phenoxys of 1-) methyl phenyl methylcyclohexyl)] hexanaphthene; 1; The two [4-(4-amido phenoxys of 1-) methyl phenyl ethyl cyclohexyl)] hexanaphthene; 1; The two [4-(4-amido phenoxys of 1-) methyl phenyl propyl group cyclohexyl)] hexanaphthene; 1; The two [4-(4-amido phenoxys of 1-) methyl phenyl butyl cyclohexyl)] hexanaphthene; 1; The two [4-(4-amido phenoxys of 1-) methyl phenyl amyl group cyclohexyl)] hexanaphthene; 1; The two [4-(4-amido phenoxys of 1-) methyl phenyl hexyl cyclohexyl)] hexanaphthene; 1; The two [4-(4-amido phenoxys of 1-) methyl phenyl heptyl cyclohexyl)] hexanaphthene; 1; The two [4-(4-amido phenoxys of 1-) methyl phenyl octyl group cyclohexyl)] hexanaphthene; 1; Two (4-aminocarbonyl phenyl) the-4-(cyclohexyl methyls of 1-) hexanaphthene; 1; Two (the 4-aminocarbonyl phenyl)-4-[(4-methylcyclohexyl) methyl of 1-] hexanaphthene; 1; Two (the 4-aminocarbonyl phenyl)-4-[(4-ethyl cyclohexyl) methyl of 1-] hexanaphthene; 1; Two (the 4-aminocarbonyl phenyl)-4-[(4-propyl group cyclohexyl) methyl of 1-] two (the 4-aminocarbonyl phenyl)-4-[(4-butyl cyclohexyl) methyl of hexanaphthene ] hexanaphthene; 1; Two (the 4-aminocarbonyl phenyl)-4-[(4-amyl group cyclohexyl) methyl of 1-] hexanaphthene; 1; Two (the 4-aminocarbonyl phenyl)-4-[(4-hexyl cyclohexyl) methyl of 1-] hexanaphthene; 1; Two (the 4-aminocarbonyl phenyl)-4-[(4-heptyl cyclohexyl) methyl of 1-] hexanaphthene; 1; Two (the 4-aminocarbonyl phenyl)-4-[(4-octyl group cyclohexyl) methyl of 1-] hexanaphthene; 1; The two [4-(4-amido phenoxys of 1-) phenyl] the-4-(phenyl methyl) hexanaphthene; 1; The two [4-(4-amido phenoxys of 1-) methyl phenyl aminomethyl phenyl)] hexanaphthene; 1; The two [4-(4-amido phenoxys of 1-) methyl phenyl ethylphenyl)] hexanaphthene; 1; The two [4-(4-amido phenoxys of 1-) methyl phenyl propyl group phenyl)] hexanaphthene; 1; The two [4-(4-amido phenoxys of 1-) methyl phenyl butyl phenyl)] hexanaphthene; 1; The two [4-(4-amido phenoxys of 1-) methyl phenyl amyl group phenyl)] hexanaphthene; 1; The two [4-(4-amido phenoxys of 1-) methyl phenyl hexyl phenyl)] hexanaphthene; 1; The two [4-(4-amido phenoxys of 1-) methyl phenyl heptyl phenyl)] hexanaphthene; 1; The two [4-(4-amido phenoxys of 1-) methyl phenyl octyl phenyl)] hexanaphthene; 1; Two (4-aminocarbonyl phenyl) the-4-(phenyl methyls of 1-) hexanaphthene; 1; Two (the 4-aminocarbonyl phenyl)-4-[(4-aminomethyl phenyl) methyl of 1-] hexanaphthene; 1; Two (the 4-aminocarbonyl phenyl)-4-[(4-ethylphenyl) methyl of 1-] hexanaphthene; 1; Two (the 4-aminocarbonyl phenyl)-4-[(4-propyl group phenyl) methyl of 1-] hexanaphthene; 1; Two (the 4-aminocarbonyl phenyl)-4-[(4-butyl phenyl) methyl of 1-] hexanaphthene; 1; Two (the 4-aminocarbonyl phenyl)-4-[(4-amyl group phenyl) methyl of 1-] hexanaphthene; 1; Two (the 4-aminocarbonyl phenyl)-4-[(4-hexyl phenyl) methyl of 1-] hexanaphthene; 1; Two (the 4-aminocarbonyl phenyl)-4-[(4-heptyl phenyl) methyl of 1-] hexanaphthene; 1; Two (the 4-aminocarbonyl phenyl)-4-[(4-octyl phenyl) methyl of 1-] hexanaphthene; 1; The two [4-((4-aminocarbonyl phenyls of 1-) phenyl methyl)] the-4-(phenyl methyl) hexanaphthene; 1; The two [4-((4-aminocarbonyl phenyls of 1-) methyl phenyl aminomethyl phenyl methyl))] hexanaphthene; 1; The two [4-((4-aminocarbonyl phenyls of 1-) methyl phenyl ethylphenyl methyl))] hexanaphthene; 1; The two [4-((4-aminocarbonyl phenyls of 1-) methyl phenyl propyl group phenyl methyl))] hexanaphthene; 1; The two [4-((4-aminocarbonyl phenyls of 1-) methyl phenyl butyl phenyl methyl))] hexanaphthene; 1; The two [4-((4-aminocarbonyl phenyls of 1-) methyl phenyl amyl group phenyl methyl))] hexanaphthene; 1; The two [4-((4-aminocarbonyl phenyls of 1-) methyl phenyl hexyl phenyl methyl))] hexanaphthene; 1; The two [4-((4-aminocarbonyl phenyls of 1-) methyl phenyl heptyl phenyl methyl))] hexanaphthene; 1; The two [4-((4-aminocarbonyl phenyls of 1-) methyl phenyl octyl phenyl methyl))] hexanaphthene; Or these a combination
Figure RE-FSB00000325216800031
12. polyamic acid component as claimed in claim 11 is characterized in that wherein said aromatic diamine with side chain is the diamines shown in this formula (I).
13. polyamic acid component as claimed in claim 1 is characterized in that the non-aromatic diamines of wherein said second reaction mixture is to be selected from: aliphatie diamine, alicyclic diamine or these a combination.
14. polyamic acid component as claimed in claim 13 is characterized in that wherein said non-aromatic diamines is an alicyclic diamine.
15. polyamic acid component as claimed in claim 14; It is characterized in that wherein said alicyclic diamine is to be selected from :4 '-two amido dicyclohexyl methyl hydride; 1; 4-diamines basic ring hexane; 1; Two (the 4-amido cyclohexyl) propane of 1-; 2; Two (the 4-amido cyclohexyl) propane of 2-; 1; Two (the 4-amido cyclohexyl) ethane of 1-; 1; Two (the 4-amido cyclohexyl) butane of 1-; 2; Two (4-amido cyclohexyl) the butane amido cyclohexyl)-2-(4-aminomethyl cyclohexyl of 2-) methane; 4-amido-3; 5-Dimethylcyclohexyl-4-amido-3-methyl cyclohexane methylmethane; 4-amido cyclohexyl-4-amido-3-methyl cyclohexane methylmethane; 2; Two (4-amido-3,5-Dimethylcyclohexyl) butane of 2-, two (the 4-amidos-3 of 2-; The 5-Dimethylcyclohexyl) propane; 1; Two (4-amido-3,5-Dimethylcyclohexyl) ethane of 1-, two (4-amido-3-methylcyclohexyl) propane of 2-; 1; Two (4-amido-3-methylcyclohexyl) ethane of 1-, or these a combination.
16. polyamic acid component as claimed in claim 15 is characterized in that wherein said alicyclic diamine is 4,4 '-two amido dicyclohexyl methyl hydrides.
17. polyamic acid component as claimed in claim 1 is characterized in that it also comprises a solvent.
18. polyamic acid component as claimed in claim 17 is characterized in that it has one between the solids content concn scope between the 4wt% to 20wt%.
19. polyamic acid component as claimed in claim 18 is characterized in that it has one between the solids content concn scope between the 4wt% to 10wt%.
20. polyamic acid component as claimed in claim 17 is characterized in that wherein said solvent is to be selected from: N-methyl-2-pyrrolinone, ethylene glycol monobutyl ether, N,N-DIMETHYLACETAMIDE, N, DMSO 99.8MIN., gamma-butyrolactone, tetramethyl-urea, hexamethylphosphorictriamide ,-cresols, xylenol, phenol, halogenation phenol chlorobenzene, ethylene dichloride, tetrachloroethane, pimelinketone or these a combination.
21. polyamic acid component as claimed in claim 20 is characterized in that wherein said solvent is to be made up of N-methyl-2-pyrrolinone and ethylene glycol monobutyl ether.
22. polyamic acid component as claimed in claim 21, the part by weight scope that it is characterized in that wherein said N-methyl-2-pyrrolinone and ethylene glycol monobutyl ether is between 90: 10 to 60: 40.
23. polyamic acid component as claimed in claim 22 is characterized in that the ratio of wherein said N-methyl-2-pyrrolinone and ethylene glycol monobutyl ether is 60: 40.
24. an alignment film is characterized in that it is by solidifying a polyamic acid component as claimed in claim 1 obtained.
25. alignment film as claimed in claim 24 is characterized in that wherein said curing schedule is by this polyamic acid component is dissolved, and coats on the base material again and heats and accomplish.
CN2006101622089A 2006-12-06 2006-12-06 Polyamic acid component and alignment film produced by the same Active CN101195711B (en)

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