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CN112721258A - Preparation method of polyvinyl alcohol polarizing film for TFT - Google Patents

Preparation method of polyvinyl alcohol polarizing film for TFT Download PDF

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Publication number
CN112721258A
CN112721258A CN202011589127.3A CN202011589127A CN112721258A CN 112721258 A CN112721258 A CN 112721258A CN 202011589127 A CN202011589127 A CN 202011589127A CN 112721258 A CN112721258 A CN 112721258A
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polyvinyl alcohol
polarizing film
film
producing
mixed solution
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Chinese (zh)
Inventor
潘晓明
徐学斌
李家鸣
高申保
吴福胜
陈喜成
杨阳
司家清
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Hefei Derege Photoelectric Technology Co ltd
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Hefei Derege Photoelectric Technology Co ltd
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B29WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29DPRODUCING PARTICULAR ARTICLES FROM PLASTICS OR FROM SUBSTANCES IN A PLASTIC STATE
    • B29D11/00Producing optical elements, e.g. lenses or prisms
    • B29D11/0074Production of other optical elements not provided for in B29D11/00009- B29D11/0073
    • B29D11/00788Producing optical films
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B29WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29DPRODUCING PARTICULAR ARTICLES FROM PLASTICS OR FROM SUBSTANCES IN A PLASTIC STATE
    • B29D11/00Producing optical elements, e.g. lenses or prisms
    • B29D11/0073Optical laminates
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J5/00Manufacture of articles or shaped materials containing macromolecular substances
    • C08J5/18Manufacture of films or sheets
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2329/00Characterised by the use 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; Hydrolysed polymers of esters of unsaturated alcohols with saturated carboxylic acids; Derivatives of such polymer
    • C08J2329/02Homopolymers or copolymers of unsaturated alcohols
    • C08J2329/04Polyvinyl alcohol; Partially hydrolysed homopolymers or copolymers of esters of unsaturated alcohols with saturated carboxylic acids
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2429/00Characterised by the use 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; Hydrolysed polymers of esters of unsaturated alcohols with saturated carboxylic acids; Derivatives of such polymer
    • C08J2429/02Homopolymers or copolymers of unsaturated alcohols
    • C08J2429/04Polyvinyl alcohol; Partially hydrolysed homopolymers or copolymers of esters of unsaturated alcohols with saturated carboxylic acids
    • 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
    • C08K13/00Use of mixtures of ingredients not covered by one single of the preceding main groups, each of these compounds being essential
    • C08K13/02Organic and inorganic ingredients
    • 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
    • C08K3/38Boron-containing compounds
    • 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
    • C08K5/00Use of organic ingredients
    • C08K5/04Oxygen-containing compounds
    • C08K5/05Alcohols; Metal alcoholates
    • C08K5/053Polyhydroxylic alcohols
    • 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
    • C08K5/00Use of organic ingredients
    • C08K5/16Nitrogen-containing compounds
    • C08K5/22Compounds containing nitrogen bound to another nitrogen atom
    • C08K5/23Azo-compounds

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  • Engineering & Computer Science (AREA)
  • Manufacturing & Machinery (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Ophthalmology & Optometry (AREA)
  • Mechanical Engineering (AREA)
  • Materials Engineering (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • Shaping By String And By Release Of Stress In Plastics And The Like (AREA)

Abstract

The invention discloses a preparation method of a polyvinyl alcohol polarizing film for a TFT (thin film transistor), which is prepared by adding a non-iodine dye into a polyvinyl alcohol solution, extruding and defoaming, casting to form a film, dry stretching, hot air sizing and drying, trimming and rolling. By adopting the non-iodine dye and matching with proper process conditions, the prepared polarizing film has better optical performance, humidity resistance and temperature resistance compared with an iodine polarizing film, and can meet the application requirements of outdoor high-temperature and high-humidity environments and TFT (thin film transistor) display screens.

Description

Preparation method of polyvinyl alcohol polarizing film for TFT
Technical Field
The invention relates to the technical field of polarizer preparation, in particular to a preparation method of a polyvinyl alcohol polarizing film for a TFT (thin film transistor).
Background
The LCD/OLED display is widely applied to indoor display of televisions, notebook computers and the like, and is also applied to outdoor fields of mobile phones, vehicle-mounted display, outdoor electronic signs, outdoor cameras and the like. Therefore, in order to maintain good performance of the display even under outdoor conditions, the polarizer used as a key material for LCD/OLED display needs to have excellent temperature and humidity resistance.
The prior method for producing the polaroid comprises the steps of uniformly mixing water, polyvinyl alcohol, a plasticizer and an auxiliary agent according to a certain proportion, carrying out tape casting film forming and drying to prepare a polyvinyl alcohol original film, swelling the original film, dyeing, washing, stretching, color complementing and drying, and attaching functional films to the upper surface and the lower surface of the original film to prepare the polaroid. The method has the advantages of complex production process, long flow, more guide rollers contacted with the film, and more quality control points during production, thus leading to low yield and high comprehensive cost of the polaroid. Patents CN103724642A and CN107619566A both disclose a method for preparing a polyvinyl alcohol polarizer, in which iodine is used as a dye and a polyvinyl alcohol aqueous solution is uniformly mixed and then cast into a film, which is simple, but has two common defects: when the iodine-containing polyvinyl alcohol solution is extruded and defoamed, iodine can volatilize from an extrusion exhaust port, so that the transmittance of a film formed by tape casting is greatly reduced, and the polarization degree and the optical performance of the prepared polaroid are poor; iodine as a dichroic substance is easy to sublimate and unstable at high temperature, so that the temperature resistance and the humidity resistance of the polarizer are poor. The above defects result in that the performance of the obtained polarizer can not meet the application requirements of the TFT display screen.
Disclosure of Invention
In order to avoid the defects of the prior art, the invention provides a preparation method of a polyvinyl alcohol polarizing film for a TFT (thin film transistor), aiming at improving the optical property and the temperature and humidity resistance of the polarizing film and enabling the polarizing film to meet the application requirements of a TFT display screen.
In order to achieve the purpose, the invention adopts the following technical scheme:
a preparation method of a polyvinyl alcohol polarizing film for a TFT (thin film transistor) is carried out according to the following steps:
step 1, fully stirring water, polyvinyl alcohol, a plasticizer and a surfactant in a dissolving kettle until the water, the polyvinyl alcohol, the plasticizer and the surfactant are uniformly mixed, and introducing inert gas into the dissolving kettle while stirring to remove oxygen so as to prevent the prepared polaroid from yellowing;
step 2, pressurizing and heating the dissolving kettle to dissolve the polyvinyl alcohol to obtain a mixed solution A;
step 3, preparing a mixed solution of dye and boric acid in an auxiliary kettle, and then adding the mixed solution into the dissolving kettle to be fully mixed with the mixed solution A obtained in the step 2 to obtain a mixed solution B;
and 4, extruding and defoaming the mixed solution B, performing tape casting film forming and drying to obtain a film with the moisture content of 10-30%, then performing dry stretching, feeding the stretched film into a drying oven for hot air shaping and drying, and finally trimming and rolling to obtain the polyvinyl alcohol polarizing film for the TFT. And (3) attaching the TAC film or the PMMA film to the upper part and the lower part of the prepared polarizing film, and drying to obtain the original polarizer plate.
Further, in the step 1, the polyvinyl alcohol is formed by mixing a first polyvinyl alcohol with a polymerization degree of 2000-5000-. The proportion not only can ensure the tensile strength of the film, but also can reduce the dissolution temperature of the polyvinyl alcohol, so that the polyvinyl alcohol is easier to dissolve in a water solvent.
Further, in step 1, the water is pure water having a resistivity of 1 to 20 M.OMEGA.cm (preferably 12 to 18 M.OMEGA.cm).
Further, in the step 1, the addition amount of the plasticizer is 10 to 20% (preferably 12 to 15%) of the mass of the polyvinyl alcohol, and the addition amount of the surfactant is 0.01 to 0.1% (preferably 0.04 to 0.06%) of the mass of the polyvinyl alcohol.
Further, in step 1, the inert gas may be helium, argon or nitrogen, preferably nitrogen.
Further, in step 2, the temperature of the pressurization and temperature rise is 100-. Under the same drying condition, the speed of the production line under the mass fraction can be improved by 15-20%.
Furthermore, in step 3, the dye used needs to have strong affinity to the polyvinyl alcohol film, the color phase does not change and the dye does not sublime when being heated, and the moisture-proof, heat-proof and sun-proof performances are better than those of the iodine polarizing film dye. The dyes may be, depending on the dyeing color, sodium β -naphthol azo-p-benzenesulfonate, 1-phenylazo-2-naphthol, triarylmethane, 1,3, 3-trimethyl-2- [2- (1-methyl-2-phenyl-1H-indol-3-yl) ethyl ] -3H-indoxyl, 3,3 ' -dioxo-2, 2 ' -biindolyl-5, 5 ' -disulfonic acid disodium salt, one or more of 1, 2-dihydroxy anthraquinone, tetraazabenzene, naftifine S, sulphur blue BN, 4-methyl-1-ethyl-3-cyano-5-amino-6-hydroxy-2-pyridone.
Further, in step 3, the amount of the dye is 0.01 to 1.0% (preferably 0.06 to 0.5%, more preferably 0.06 to 0.5%) by mass of the polyvinyl alcohol, and the amount of the boric acid is 0.01 to 2.0% by mass of the polyvinyl alcohol.
Further, in step 4, the moisture content of the film is preferably 15 to 25%, at which the toughness and strength of the film are in the optimum state, most easily stretched.
Furthermore, in step 4, the dry stretching is preferably performed by using three or more guide rollers for segmented multistage stretching, and the stretching magnification by using the method is higher, can reach 7 times and is 5-5.5 times better than that of single-stage stretching.
Further, in the step 4, the drying mode of the hot air shaping and drying is air floating type. The film is prevented from contacting with the guide roller in the mode, pollution is reduced, and the film is easier to shape in the oven and eliminate the internal stress of the film due to the air floating type.
The invention has the beneficial effects that:
1. by adopting the non-iodine dye and matching with proper process conditions, the prepared polarizing film has better optical performance, humidity resistance and temperature resistance compared with an iodine polarizing film, and can meet the application requirements of outdoor high-temperature and high-humidity environments and TFT (thin film transistor) display screens.
2. The process method of the invention can reduce the dissolution temperature of the polyvinyl alcohol, improve the production efficiency and simultaneously improve the stretching multiplying power of the PVA optical film.
Detailed Description
The present invention will be described in detail with reference to the following embodiments in order to make the aforementioned objects, features and advantages of the invention more comprehensible. The following disclosure is merely exemplary and illustrative of the inventive concept, and those skilled in the art will appreciate that various modifications, additions and substitutions are possible, without departing from the scope and spirit of the invention as disclosed in the accompanying claims.
Example 1
This example prepares a polyvinyl alcohol polarizing film for TFT by the following steps:
step 1, weighing 800kg of PVA (with the polymerization degree of 2600 and the alcoholysis degree of 99.97%), 200kg of PVA (with the polymerization degree of 550 and the alcoholysis degree of 99.1%), 120kg of glycerol as a plasticizer, 0.5kg of sodium dodecyl benzene sulfonate as a surfactant and a certain amount of pure water (with the resistivity of 15M omega cm), fully stirring in a dissolving kettle until the mixture is uniformly mixed, and introducing inert gas nitrogen into the dissolving kettle while stirring to remove oxygen so as to prevent the prepared polaroid from yellowing.
And 2, pressurizing and heating the dissolving kettle to 140 ℃ and 0.5MPa to dissolve the polyvinyl alcohol to obtain a mixed solution A, wherein the mass concentration of the polyvinyl alcohol is 36%.
And 3, preparing a mixed solution of the 1-phenylazo-2-naphthol dye and boric acid (0.4 kg of dye and 0.6kg of boric acid) in the auxiliary kettle, and then adding the mixed solution into the dissolving kettle to be fully mixed with the mixed solution A obtained in the step 2 to obtain a mixed solution B.
And 4, extruding and defoaming the mixed solution B, carrying out tape casting to form a film (the film forming speed is 12m/min), forming the film and drying to obtain a film with the moisture content of 20%, and then stretching the film for four times by five guide rollers, wherein the stretching ratio of the film to the film is 2:3.5:5.5:7, and finally, the film is stretched for 7 times. And after stretching, feeding the film into an air floating type drying oven for hot air shaping and drying, and finally cutting edges and rolling to obtain the polyvinyl alcohol polarizing film for the TFT. And attaching TAC films to the upper and lower parts of the polarizer and drying to obtain the polarizer original plate.
Comparative example 1
This comparative example prepared a polyvinyl alcohol polarizing film by the following steps:
step 1, weighing 1000kg of PVA (with the polymerization degree of 2600 and the alcoholysis degree of 99.97%), 120kg of glycerol plasticizer, 0.5kg of sodium dodecyl benzene sulfonate surfactant and a certain amount of pure water (with the resistivity of 15M omega cm), fully stirring in a dissolving kettle until the mixture is uniformly mixed, and introducing inert gas nitrogen into the dissolving kettle while stirring to remove oxygen, so that the prepared polarizer is not yellowed.
And 2, pressurizing and heating the dissolving kettle to 155 ℃ and 0.6MPa to dissolve the polyvinyl alcohol to obtain a mixed solution A, wherein the mass concentration of the polyvinyl alcohol is 36%.
And 3, preparing a mixed solution of the 1-phenylazo-2-naphthol dye and boric acid (0.4 kg of dye and 0.6kg of boric acid) in the auxiliary kettle, and then adding the mixed solution into the dissolving kettle to be fully mixed with the mixed solution A obtained in the step 2 to obtain a mixed solution B.
And 4, extruding and defoaming the mixed solution B, carrying out tape casting to form a film (the film forming speed is 12m/min), forming the film and drying to obtain a film with the moisture content of 20%, and then stretching the film for four times by five guide rollers, wherein the stretching ratio of the film to the film is 2:3.5:5.5:7, and finally, the film is stretched for 7 times. And after stretching, feeding the film into an air floating type drying oven for hot air shaping and drying, and finally cutting edges and rolling to obtain the polyvinyl alcohol polarizing film. And attaching TAC films to the upper and lower parts of the polarizer and drying to obtain the polarizer original plate.
Compared with example 1, the present comparative example uses only polyvinyl alcohol having a high degree of polymerization, and has poor solubility in water and a high dissolution temperature.
Comparative example 2
This comparative example prepared a polyvinyl alcohol polarizing film in the same manner as in example 1 except that: in the step 4, the three guide rollers are used for stretching for two times, the stretching ratio for two times is 3:5.5, and finally the stretching time reaches 5.5 times.
Compared with example 1, the comparative example has two times of stretching and lower stretching ratio.
Comparative example 3
To verify the humidity and temperature resistance of the polarizing film obtained in example 1, a comparative example was conducted to an iodine-based polarizing film in the same manner as in example 1 except that the dye used was iodine/potassium iodide dye.
The optical property ratios of the polarizing films obtained in the respective examples and comparative examples are shown in table 1.
TABLE 1
Figure RE-GDA0002989706530000041
As can be seen from the table, compared with the iodine polarizing film, the moisture-proof and temperature-resistant polarizing film prepared by the invention is superior to the iodine polarizing film, can meet the requirements of outdoor high-temperature and high-humidity environment and TFT, and has higher stretching multiple and lower raw material dissolution temperature.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents and improvements made within the spirit and principle of the present invention are intended to be included within the scope of the present invention.

Claims (10)

1. A preparation method of a polyvinyl alcohol polarizing film for a TFT is characterized by comprising the following steps:
step 1, fully stirring water, polyvinyl alcohol, a plasticizer and a surfactant in a dissolving kettle until the water, the polyvinyl alcohol, the plasticizer and the surfactant are uniformly mixed, and introducing inert gas into the dissolving kettle while stirring to remove oxygen;
step 2, pressurizing and heating the dissolving kettle to dissolve the polyvinyl alcohol to obtain a mixed solution A;
step 3, preparing a mixed solution of dye and boric acid in an auxiliary kettle, and then adding the mixed solution into the dissolving kettle to be fully mixed with the mixed solution A obtained in the step 2 to obtain a mixed solution B;
and 4, extruding and defoaming the mixed solution B, performing tape casting film forming and drying to obtain a film with the moisture content of 10-30%, then performing dry stretching, feeding the stretched film into a drying oven for hot air shaping and drying, and finally trimming and rolling to obtain the polyvinyl alcohol polarizing film for the TFT.
2. The method of producing a polyvinyl alcohol polarizing film for TFTs according to claim 1, characterized in that: in the step 1, the polyvinyl alcohol is formed by mixing a first polyvinyl alcohol with the polymerization degree of 2000-S-5000 and the alcoholysis degree of 99.0-99.99% and a second polyvinyl alcohol with the polymerization degree of 300-S-2000 and the alcoholysis degree of 98.0-99.99% according to the mass ratio of 1-6: 1.
3. The method of producing a polyvinyl alcohol polarizing film for TFTs according to claim 1, characterized in that: in step 1, the water is pure water with resistivity of 1-20M omega cm.
4. The method of producing a polyvinyl alcohol polarizing film for TFTs according to claim 1, characterized in that: in the step 1, the addition amount of the plasticizer accounts for 10-20% of the mass of the polyvinyl alcohol, and the addition amount of the surfactant accounts for 0.01-0.1% of the mass of the polyvinyl alcohol.
5. The method of producing a polyvinyl alcohol polarizing film for TFTs according to claim 1, characterized in that: in step 2, the temperature of the pressurization and temperature rise is 100-165 ℃, and the pressure is 0.3-1.0 MPa.
6. The method of producing a polyvinyl alcohol polarizing film for TFTs according to claim 1, characterized in that: in the step 2, the mass concentration of the polyvinyl alcohol in the obtained mixed solution A is 25-45%.
7. The method of producing a polyvinyl alcohol polarizing film for TFTs according to claim 1, characterized in that: in the step 3, the dye accounts for 0.01-1.0% of the mass of the polyvinyl alcohol, and the boric acid accounts for 0.01-2.0% of the mass of the polyvinyl alcohol.
8. The method of producing a polyvinyl alcohol polarizing film for TFTs according to claim 1, characterized in that: the dye is one or a mixture of more of beta-naphthol azo sodium p-benzenesulfonate, 1-phenylazo-2-naphthol, triarylmethane, 1,3, 3-trimethyl-2- [2- (1-methyl-2-phenyl-1H-indol-3-yl) ethyl ] -3H-indoxyl, 3,3 ' -dioxo-2, 2 ' -bisindolyl-5, 5 ' -disulfonic acid disodium salt, 1, 2-dihydroxyanthraquinone, tetraazabenzene, naftifine S, sulphur blue BN, and 4-methyl-1-ethyl-3-cyano-5-amino-6-hydroxy-2-pyridone.
9. The method of producing a polyvinyl alcohol polarizing film for TFTs according to claim 1, characterized in that: in step 4, the dry stretching is segmented multi-stage stretching by three or more guide rollers.
10. The method of producing a polyvinyl alcohol polarizing film for TFTs according to claim 1, characterized in that: in the step 4, the drying mode of the hot air shaping and drying is air floating.
CN202011589127.3A 2020-12-29 2020-12-29 Preparation method of polyvinyl alcohol polarizing film for TFT Pending CN112721258A (en)

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Cited By (1)

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Publication number Priority date Publication date Assignee Title
CN116100839A (en) * 2023-03-09 2023-05-12 合肥德瑞格光电科技有限公司 Preparation method of light and thin polarizer original sheet

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US20170106609A1 (en) * 2015-02-15 2017-04-20 Roger Wen Yi Hsu Methods And Systems For Making An Optical Functional Film
CN107533181A (en) * 2015-04-29 2018-01-02 特里亚佩克斯有限公司 Light polarizing film, prepare its method and include its polarized lenses
CN107619566A (en) * 2017-10-18 2018-01-23 中国石油化工集团公司 A kind of preparation method of polyvinyl alcohol polaroid
CN110441853A (en) * 2019-08-14 2019-11-12 佛山纬达光电材料股份有限公司 A kind of resistance to xenon lamp test polaroid and preparation method thereof

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侯少武,滕朝晖,杨俊生著: "《聚乙烯醇市场 生产技术 应用》", 31 March 2017, 北京燕山出版社 *
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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN116100839A (en) * 2023-03-09 2023-05-12 合肥德瑞格光电科技有限公司 Preparation method of light and thin polarizer original sheet

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Application publication date: 20210430