CN114213790A - Photo-alignment polyimide composition and preparation process thereof - Google Patents

Photo-alignment polyimide composition and preparation process thereof Download PDF

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Publication number
CN114213790A
CN114213790A CN202111652666.1A CN202111652666A CN114213790A CN 114213790 A CN114213790 A CN 114213790A CN 202111652666 A CN202111652666 A CN 202111652666A CN 114213790 A CN114213790 A CN 114213790A
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parts
particles
polyimide
container
nano
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CN202111652666.1A
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Inventor
张奇
丁丽娜
游石枝
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Nanjing Qingyan New Material Research Institute Co ltd
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Nanjing Qingyan New Material Research Institute Co ltd
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Priority to CN202111652666.1A priority Critical patent/CN114213790A/en
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    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L29/00Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an alcohol, ether, aldehydo, ketonic, acetal or ketal radical; Compositions of hydrolysed polymers of esters of unsaturated alcohols with saturated carboxylic acids; Compositions of derivatives of such polymers
    • C08L29/02Homopolymers or copolymers of unsaturated alcohols
    • C08L29/04Polyvinyl alcohol; Partially hydrolysed homopolymers or copolymers of esters of unsaturated alcohols with saturated carboxylic acids
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09DCOATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D129/00Coating compositions based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an alcohol, ether, aldehydo, ketonic, acetal, or ketal radical; Coating compositions based on hydrolysed polymers of esters of unsaturated alcohols with saturated carboxylic acids; Coating compositions based on derivatives of such polymers
    • C09D129/02Homopolymers or copolymers of unsaturated alcohols
    • C09D129/04Polyvinyl alcohol; Partially hydrolysed homopolymers or copolymers of esters of unsaturated alcohols with saturated carboxylic acids
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09DCOATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D7/00Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
    • C09D7/40Additives
    • C09D7/60Additives non-macromolecular
    • C09D7/61Additives non-macromolecular inorganic
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09DCOATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D7/00Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
    • C09D7/40Additives
    • C09D7/60Additives non-macromolecular
    • C09D7/63Additives non-macromolecular organic
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09DCOATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D7/00Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
    • C09D7/40Additives
    • C09D7/65Additives macromolecular
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/32Phosphorus-containing compounds
    • C08K2003/321Phosphates
    • C08K2003/324Alkali metal phosphate

Abstract

The invention discloses a photo-alignment polyimide composition, which comprises the following specific components in parts by weight: 2-3 parts of dianhydride, 4-10 parts of diamine, 7-10 parts of dihydric alcohol, 5-8 parts of polystyrene and derivatives thereof, 2-4 parts of epoxy resin, 1-4 parts of polyurethane, 800 parts of polyvinyl alcohol, 0.3-0.5 part of SiC nano particles, 2-9 parts of polysilane, SiO 220.1 to 0.2 portion of nano-particles, 0.01 to 0.3 portion of plasticizer, 0.005 to 0.5 portion of dispersant, 0.003 to 0.005 portion of light stabilizer and 0.03 to 0.07 portion of catalyst, and SiC nano-particles and SiO are added2The nano particles adopt a process of pressurizing and stirring with polyimide, so that the quality is stable, the film forming effect is good, the cost is low, and the realization is easy.

Description

Photo-alignment polyimide composition and preparation process thereof
Technical Field
The invention belongs to the technical field of display devices, and particularly relates to a photo-alignment polyimide composition and a preparation process thereof.
Background
With the improvement of the technological level, the lcd panel is widely used in people's work and life, the polyimide alignment film is coated on the color filter of the lcd panel, the quality of the polyimide alignment film directly affects the quality of the lcd panel, and in order to ensure the picture quality and yield of the lcd panel, many manufacturers try to align the liquid crystal by using the photo-alignment technology. This requires that the polyimide should have good stability, uniformity, mechanical properties, high temperature resistance, good affinity with liquid crystal, and good adhesion to the substrate, but the existing polyimide alignment film has unstable quality and needs to be improved in film-forming composition.
Disclosure of Invention
In order to solve the problems, the invention discloses a photo-alignment polyimide composition and a preparation process thereof, and the photo-alignment polyimide composition has the advantages of simple process, stable quality, good film forming effect, low cost and easy realization.
In order to achieve the purpose, the technical scheme of the invention is as follows:
a photo-aligned polyimide composition comprising the following components:
bisanhydrides, diamines, diols, polystyrene and derivatives thereof, epoxy resins, polyurethanes, polyvinyl alcohol, SiC nanoparticles, polysilanes, SiO2Nanoparticles, a plasticizer, a dispersant, a light stabilizer and a catalyst.
The concrete components are as follows in parts by weight: 2-3 parts of dianhydride, 4-10 parts of diamine, 7-10 parts of dihydric alcohol, 5-8 parts of polystyrene and derivatives thereof, and epoxy resin2-4 parts of grease, 1-4 parts of polyurethane, 1200 parts of polyvinyl alcohol 800-20.1-0.2 part of nano-particles, 0.01-0.3 part of plasticizer, 0.005-0.5 part of dispersant, 0.003-0.005 part of light stabilizer and 0.03-0.07 part of catalyst.
As an improvement of the invention, the dispersant is one or more of sodium tripolyphosphate, sodium pyrophosphate, vinyl alcohol, methyl amyl alcohol, cellulose derivatives, polyacrylamide, sodium dodecyl sulfate and fatty acid polyglycol ester.
As an improvement of the invention, the plasticizer is dioctyl terephthalate, and the product has the characteristics of good heat resistance, cold resistance, stability, flexibility and electrical insulation performance.
As an improvement of the invention, the light stabilizer is hexamethylphosphoric triamide, can absorb ultraviolet part, does not change per se, and has good stability.
As a refinement of the present invention, the catalyst is benzyldimethylamine.
As an improvement of the invention, the SiC nanoparticles and SiO2The particle size of the nano-particles is 2-10 nanometers.
A method for preparing a photoalignment polyimide composition, comprising the steps of:
(1) reacting dianhydride and diamine according to a weight ratio to generate a polyimide precursor;
(2) mixing the polyimide precursor obtained in the step (1) with SiC nano-particles and SiO2Putting the nano particles into a container, and stirring under pressure for 10-15 min;
(3) reacting the mixture obtained in the step (2) with dihydric alcohol to generate a polyimide polymer;
(4) adding the rest materials into container, heating and stirring for 3-5min, and naturally cooling.
As an improvement of the invention, the pressure in the container in the step (2) is 16-20 MPa.
As a modification of the invention, the stirring speed of the vessel in the step (2) is 1600-2000/min.
As a modification of the invention, the temperature in the container in the step (4) is 85-90 ℃.
The invention has the beneficial effects that:
the photo-alignment polyimide composition and the preparation process of the invention increase SiC nano particles and SiO2The nano particles adopt a process of pressurizing and stirring with polyimide, so that the quality is stable, the film forming effect is good, the cost is low, and the realization is easy.
Detailed Description
The present invention will be further illustrated below with reference to specific embodiments, which are to be understood as merely illustrative and not limitative of the scope of the present invention.
Example 1
The photo-alignment polyimide composition described in this embodiment includes the following components by weight:
2 parts of dianhydride, 8 parts of diamine, 9 parts of dihydric alcohol, 6 parts of polystyrene and derivatives thereof, 3 parts of epoxy resin, 2 parts of polyurethane, 1000 parts of polyvinyl alcohol, 0.4 part of SiC nano-particles, 5 parts of polysilane, and SiO20.1 part of nano particles, 0.08 part of dioctyl terephthalate, 0.1 part of sodium tripolyphosphate, 0.004 part of hexamethyl phosphoric triamide and 0.05 part of benzyl dimethylamine.
The particle size of the SiC nanoparticles described in this example was 5 nm; SiO 22The particle size of the nanoparticles was 6 nm.
The preparation method of the photo-alignment polyimide composition described in this embodiment includes the following steps:
(1) reacting dianhydride and diamine according to a weight ratio to generate a polyimide precursor;
(2) mixing the polyimide precursor obtained in the step (1) with SiC nano-particles and SiO2The nano particles are put into a container to be pressurized and stirred for 12min, the pressure in the container is 18MPa, and the stirring speed of the container is 1800/min;
(3) reacting the mixture obtained in the step (2) with dihydric alcohol to generate a polyimide polymer;
(4) adding the rest materials into container, heating and stirring for 4min at 88 deg.C, pouring out, and naturally cooling.
Example 2
The photo-alignment polyimide composition described in this embodiment includes the following components by weight:
2 parts of dianhydride, 10 parts of diamine, 7 parts of dihydric alcohol, 8 parts of polystyrene and derivatives thereof, 2 parts of epoxy resin, 4 parts of polyurethane, 800 parts of polyvinyl alcohol, 0.5 part of SiC nano-particles, 2 parts of polysilane, and SiO20.2 part of nano particles, 0.01 part of dioctyl terephthalate, 0.5 part of sodium pyrophosphate, 0.003 part of hexamethyl phosphoric triamide and 0.07 part of benzyl dimethylamine.
The particle size of the SiC nanoparticles described in this example was 2 nm; SiO 22The particle size of the nanoparticles was 10 nm.
The preparation method of the photo-alignment polyimide composition described in this embodiment includes the following steps:
(1) reacting dianhydride and diamine according to a weight ratio to generate a polyimide precursor;
(2) mixing the polyimide precursor obtained in the step (1) with SiC nano-particles and SiO2Putting the nano particles into a container, pressurizing and stirring for 10min, wherein the pressure in the container is 20MPa, and the stirring speed of the container is 1600/min;
(3) reacting the mixture obtained in the step (2) with dihydric alcohol to generate a polyimide polymer;
(4) adding the rest materials into container, heating and stirring for 5min at 85 deg.C, pouring out, and naturally cooling.
Example 3
The photo-alignment polyimide composition described in this embodiment includes the following components by weight:
3 parts of dianhydride, 4 parts of diamine, 10 parts of dihydric alcohol, 5 parts of polystyrene and derivatives thereof, 4 parts of epoxy resin, 1 part of polyurethane, 1200 parts of polyvinyl alcohol, 0.3 part of SiC nano-particles, 9 parts of polysilane, and SiO20.1 part of nano particles, 0.3 part of dioctyl terephthalate, 0.005 part of vinyl alcohol, 0.005 part of hexamethyl phosphoric triamide and 0.03 part of benzyl dimethylamine.
The particle size of the SiC nanoparticles described in this example was 10 nm; SiO 22The particle size of the nanoparticles was 2 nm.
The preparation method of the photo-alignment polyimide composition described in this embodiment includes the following steps:
(1) reacting dianhydride and diamine according to a weight ratio to generate a polyimide precursor;
(2) mixing the polyimide precursor obtained in the step (1) with SiC nano-particles and SiO2Placing the nano particles into a container, pressurizing and stirring for 15min, wherein the pressure in the container is 16MPa, and the stirring speed of the container is 2000/min;
(3) reacting the mixture obtained in the step (2) with dihydric alcohol to generate a polyimide polymer;
(4) adding the rest materials into a container, heating and stirring for 3min at 90 deg.C, and naturally cooling.
The thickness of the film after coating is 60-80nm, the appearance, the light transmittance, the stability, the uniformity, the optical property, the mechanical property and the weather resistance are all good, the affinity and the adherence are good, the quality is stable, and the standard is met.
It should be noted that the above-mentioned contents only illustrate the technical idea of the present invention, and the protection scope of the present invention is not limited thereby, and it is obvious to those skilled in the art that several modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations fall within the protection scope of the claims of the present invention.

Claims (10)

1. A photoaligned polyimide composition, characterized in that: the concrete components are as follows in parts by weight: 2-3 parts of dianhydride, 4-10 parts of diamine, 7-10 parts of dihydric alcohol, 5-8 parts of polystyrene and derivatives thereof, 2-4 parts of epoxy resin, 1-4 parts of polyurethane, 800 parts of polyvinyl alcohol, 0.3-0.5 part of SiC nano particles, 2-9 parts of polysilane, SiO 220.1-0.2 part of nano-particles, 0.01-0.3 part of plasticizer, 0.005-0.5 part of dispersant, 0.003-0.005 part of light stabilizer and 0.03-0.07 part of catalyst.
2. A photoaligned polyimide composition according to claim 1, wherein: the dispersing agent is one or more of sodium tripolyphosphate, sodium pyrophosphate, vinyl alcohol, methyl amyl alcohol, cellulose derivatives, polyacrylamide, sodium dodecyl sulfate and fatty acid polyglycol ester.
3. A photoaligned polyimide composition according to claim 1, wherein: the plasticizer is dioctyl terephthalate.
4. A photoaligned polyimide composition according to claim 1, wherein: the light stabilizer is hexamethylphosphoric triamide.
5. A photoaligned polyimide composition according to claim 1, wherein: the catalyst is benzyldimethylamine.
6. A photoaligned polyimide composition according to claim 1, wherein: the SiC nanoparticles and SiO2The particle size of the nano-particles is 2-10 nanometers.
7. The method of claim 1, wherein the method comprises: the method comprises the following steps:
(1) reacting dianhydride and diamine according to a weight ratio to generate a polyimide precursor;
(2) mixing the polyimide precursor obtained in the step (1) with SiC nano-particles and SiO2Putting the nano particles into a container, and stirring under pressure for 10-15 min;
(3) reacting the mixture obtained in the step (2) with dihydric alcohol to generate a polyimide polymer;
(4) adding the rest materials into container, heating and stirring for 3-5min, and naturally cooling.
8. The method of claim 7, wherein the method comprises: the pressure in the container in the step (2) is 16-20 MPa.
9. The method of claim 7, wherein the method comprises: the stirring speed of the container in the step (2) is 1600-.
10. The method of claim 7, wherein the method comprises: the temperature in the container in the step (4) is 85-90 ℃.
CN202111652666.1A 2021-12-31 2021-12-31 Photo-alignment polyimide composition and preparation process thereof Pending CN114213790A (en)

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Application Number Priority Date Filing Date Title
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CN110776657A (en) * 2019-11-05 2020-02-11 株洲时代新材料科技股份有限公司 High-thermal-conductivity polyimide film and preparation method thereof
CN111978725A (en) * 2020-07-28 2020-11-24 凯正包装科技(广东)有限公司 Antibacterial high-temperature-aging-resistant polyimide film and preparation method thereof
CN113736257A (en) * 2021-09-01 2021-12-03 大同共聚(西安)科技有限公司 MXenes polyvinyl alcohol polyimide composite film and preparation method thereof

Patent Citations (17)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH09118823A (en) * 1996-10-03 1997-05-06 Mitsui Toatsu Chem Inc Polyimide-based composition material
US20070083017A1 (en) * 2005-10-12 2007-04-12 Dueber Thomas E Compositions comprising polyimide and hydrophobic epoxy, and methods relating thereto
US20070232734A1 (en) * 2006-03-31 2007-10-04 Karthikeyan Kanakarajan Polyimide based compositions useful in high frequency circuitry applications and methods relating thereto
JP2008214413A (en) * 2007-03-01 2008-09-18 Toray Ind Inc Thermosetting resin composition
CN101235201A (en) * 2008-02-02 2008-08-06 上海市合成树脂研究所 Method for preparing polyimide nano composite thin film
CN101402743A (en) * 2008-11-25 2009-04-08 北京市射线应用研究中心 Polyimide foam and method of producing the same
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