CN111732749B - Preparation method of polyvinyl alcohol optical film - Google Patents
Preparation method of polyvinyl alcohol optical film Download PDFInfo
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- CN111732749B CN111732749B CN202010795047.7A CN202010795047A CN111732749B CN 111732749 B CN111732749 B CN 111732749B CN 202010795047 A CN202010795047 A CN 202010795047A CN 111732749 B CN111732749 B CN 111732749B
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- 239000004372 Polyvinyl alcohol Substances 0.000 title claims abstract description 27
- 229920002451 polyvinyl alcohol Polymers 0.000 title claims abstract description 27
- 239000012788 optical film Substances 0.000 title claims abstract description 20
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- 238000010438 heat treatment Methods 0.000 claims abstract description 55
- 239000010408 film Substances 0.000 claims abstract description 45
- 238000000034 method Methods 0.000 claims abstract description 24
- 230000008569 process Effects 0.000 claims abstract description 21
- 230000014759 maintenance of location Effects 0.000 claims abstract description 8
- 238000001816 cooling Methods 0.000 claims abstract description 7
- 239000011347 resin Substances 0.000 claims abstract description 5
- 229920005989 resin Polymers 0.000 claims abstract description 5
- 238000005096 rolling process Methods 0.000 claims abstract description 5
- 238000010345 tape casting Methods 0.000 claims abstract description 5
- 239000000463 material Substances 0.000 claims abstract description 4
- 238000001035 drying Methods 0.000 claims description 26
- 238000005266 casting Methods 0.000 claims description 13
- 238000007493 shaping process Methods 0.000 claims description 8
- 239000011550 stock solution Substances 0.000 claims description 7
- 229910021642 ultra pure water Inorganic materials 0.000 claims description 4
- 239000012498 ultrapure water Substances 0.000 claims description 4
- 230000008961 swelling Effects 0.000 abstract description 31
- 238000004043 dyeing Methods 0.000 abstract description 9
- 238000004519 manufacturing process Methods 0.000 abstract description 5
- 230000000052 comparative effect Effects 0.000 description 12
- 239000007788 liquid Substances 0.000 description 5
- 239000000203 mixture Substances 0.000 description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- 230000003287 optical effect Effects 0.000 description 3
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 230000010287 polarization Effects 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 229920002545 silicone oil Polymers 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 238000002834 transmittance Methods 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 1
- 229920002284 Cellulose triacetate Polymers 0.000 description 1
- OKOBUGCCXMIKDM-UHFFFAOYSA-N Irganox 1098 Chemical compound CC(C)(C)C1=C(O)C(C(C)(C)C)=CC(CCC(=O)NCCCCCCNC(=O)CCC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)=C1 OKOBUGCCXMIKDM-UHFFFAOYSA-N 0.000 description 1
- NNLVGZFZQQXQNW-ADJNRHBOSA-N [(2r,3r,4s,5r,6s)-4,5-diacetyloxy-3-[(2s,3r,4s,5r,6r)-3,4,5-triacetyloxy-6-(acetyloxymethyl)oxan-2-yl]oxy-6-[(2r,3r,4s,5r,6s)-4,5,6-triacetyloxy-2-(acetyloxymethyl)oxan-3-yl]oxyoxan-2-yl]methyl acetate Chemical compound O([C@@H]1O[C@@H]([C@H]([C@H](OC(C)=O)[C@H]1OC(C)=O)O[C@H]1[C@@H]([C@@H](OC(C)=O)[C@H](OC(C)=O)[C@@H](COC(C)=O)O1)OC(C)=O)COC(=O)C)[C@@H]1[C@@H](COC(C)=O)O[C@@H](OC(C)=O)[C@H](OC(C)=O)[C@H]1OC(C)=O NNLVGZFZQQXQNW-ADJNRHBOSA-N 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 235000019864 coconut oil Nutrition 0.000 description 1
- 239000003240 coconut oil Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 235000011187 glycerol Nutrition 0.000 description 1
- 239000004973 liquid crystal related substance Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 239000004014 plasticizer Substances 0.000 description 1
- 238000004513 sizing Methods 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- 230000002522 swelling effect Effects 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29D—PRODUCING PARTICULAR ARTICLES FROM PLASTICS OR FROM SUBSTANCES IN A PLASTIC STATE
- B29D7/00—Producing flat articles, e.g. films or sheets
- B29D7/01—Films or sheets
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C35/00—Heating, cooling or curing, e.g. crosslinking or vulcanising; Apparatus therefor
- B29C35/02—Heating or curing, e.g. crosslinking or vulcanizing during moulding, e.g. in a mould
- B29C35/04—Heating or curing, e.g. crosslinking or vulcanizing during moulding, e.g. in a mould using liquids, gas or steam
- B29C35/041—Heating or curing, e.g. crosslinking or vulcanizing during moulding, e.g. in a mould using liquids, gas or steam using liquids
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C35/00—Heating, cooling or curing, e.g. crosslinking or vulcanising; Apparatus therefor
- B29C35/02—Heating or curing, e.g. crosslinking or vulcanizing during moulding, e.g. in a mould
- B29C35/04—Heating or curing, e.g. crosslinking or vulcanizing during moulding, e.g. in a mould using liquids, gas or steam
- B29C35/045—Heating or curing, e.g. crosslinking or vulcanizing during moulding, e.g. in a mould using liquids, gas or steam using gas or flames
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C35/00—Heating, cooling or curing, e.g. crosslinking or vulcanising; Apparatus therefor
- B29C35/02—Heating or curing, e.g. crosslinking or vulcanizing during moulding, e.g. in a mould
- B29C35/04—Heating or curing, e.g. crosslinking or vulcanizing during moulding, e.g. in a mould using liquids, gas or steam
- B29C35/06—Heating or curing, e.g. crosslinking or vulcanizing during moulding, e.g. in a mould using liquids, gas or steam for articles of indefinite length
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J7/00—Chemical treatment or coating of shaped articles made of macromolecular substances
- C08J7/08—Heat treatment
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C35/00—Heating, cooling or curing, e.g. crosslinking or vulcanising; Apparatus therefor
- B29C35/02—Heating or curing, e.g. crosslinking or vulcanizing during moulding, e.g. in a mould
- B29C35/04—Heating or curing, e.g. crosslinking or vulcanizing during moulding, e.g. in a mould using liquids, gas or steam
- B29C35/041—Heating or curing, e.g. crosslinking or vulcanizing during moulding, e.g. in a mould using liquids, gas or steam using liquids
- B29C2035/042—Heating or curing, e.g. crosslinking or vulcanizing during moulding, e.g. in a mould using liquids, gas or steam using liquids other than water
- B29C2035/043—Heating or curing, e.g. crosslinking or vulcanizing during moulding, e.g. in a mould using liquids, gas or steam using liquids other than water oil
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C35/00—Heating, cooling or curing, e.g. crosslinking or vulcanising; Apparatus therefor
- B29C35/02—Heating or curing, e.g. crosslinking or vulcanizing during moulding, e.g. in a mould
- B29C35/04—Heating or curing, e.g. crosslinking or vulcanizing during moulding, e.g. in a mould using liquids, gas or steam
- B29C35/045—Heating or curing, e.g. crosslinking or vulcanizing during moulding, e.g. in a mould using liquids, gas or steam using gas or flames
- B29C2035/046—Heating or curing, e.g. crosslinking or vulcanizing during moulding, e.g. in a mould using liquids, gas or steam using gas or flames dried air
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C35/00—Heating, cooling or curing, e.g. crosslinking or vulcanising; Apparatus therefor
- B29C35/02—Heating or curing, e.g. crosslinking or vulcanizing during moulding, e.g. in a mould
- B29C35/04—Heating or curing, e.g. crosslinking or vulcanizing during moulding, e.g. in a mould using liquids, gas or steam
- B29C35/045—Heating or curing, e.g. crosslinking or vulcanizing during moulding, e.g. in a mould using liquids, gas or steam using gas or flames
- B29C2035/047—Heating or curing, e.g. crosslinking or vulcanizing during moulding, e.g. in a mould using liquids, gas or steam using gas or flames other than air
- B29C2035/048—Heating or curing, e.g. crosslinking or vulcanizing during moulding, e.g. in a mould using liquids, gas or steam using gas or flames other than air inert gas
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2329/00—Characterised 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
- C08J2329/02—Homopolymers or copolymers of unsaturated alcohols
- C08J2329/04—Polyvinyl alcohol; Partially hydrolysed homopolymers or copolymers of esters of unsaturated alcohols with saturated carboxylic acids
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- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Thermal Sciences (AREA)
- Oral & Maxillofacial Surgery (AREA)
- Chemical & Material Sciences (AREA)
- Mechanical Engineering (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Processing And Handling Of Plastics And Other Materials For Molding In General (AREA)
- Moulding By Coating Moulds (AREA)
- Polarising Elements (AREA)
Abstract
The invention discloses a preparation method of a polyvinyl alcohol optical film, which is prepared by dissolving, defoaming, tape casting, predrying, heat treating and rolling PVA resin for a film and auxiliary materials. The invention carries out the heat treatment by three processes of preheating, heat treatment and cooling, strictly controls the temperature, the retention time and the tension of the film in each section of the heat treatment, can ensure that the shrinkage rates of the film in the transverse direction and the longitudinal direction are approximate, the swelling degrees in the transverse direction and the longitudinal direction are consistent, the swelling ratio is between 1 and 1.02 percent, and reduces the problem of uneven dyeing caused by overlarge swelling ratio in downstream production.
Description
Technical Field
The invention belongs to the technical field of polyvinyl alcohol films, and particularly relates to a preparation method of a polyvinyl alcohol optical film for a polarizer.
Background
The production method of the existing polyvinyl alcohol optical film comprises the steps of dissolving PVA resin and auxiliary materials in ultrapure water to prepare a casting stock solution, defoaming the casting stock solution by an extruder, carrying out die head casting molding, predrying by a drying guide roller, drying and sizing by a heat treatment oven, and rolling to obtain a finished polyvinyl alcohol optical film.
The polyvinyl alcohol optical film is mainly used for producing polaroids, and the end products are various liquid crystal displays. The performance of the polyvinyl alcohol optical film determines the optical properties of the polarizer, such as the degree of polarization, the light transmittance, the color tone and the like. The polyvinyl alcohol optical film is made into the polarizer after being swelled, stretched and dyed and attached to a TAC film, wherein the film extends in the transverse direction and the longitudinal direction when being swelled, and the extending degree can be expressed by the ratio of the size change of the film before and after being swelled, namely the transverse swelling degree and the longitudinal swelling degree. In actual production, the swelling property of the film is expressed by the ratio of the transverse direction swelling degree to the longitudinal direction swelling degree, i.e., the swelling ratio. If the swelling ratio of the film is too large, the film is not uniform in the transverse and longitudinal extension degrees in the swelling process, and color spots, stripes and other non-uniform dyeing phenomena are easily formed in the subsequent stretching and dyeing processes, so that the optical performance of the polarizer is seriously influenced.
The longitudinal direction can not freely shrink under the action of traction force, namely, under the same process environment, when the polyvinyl alcohol optical film with different transverse and longitudinal shrinkage degrees is subjected to heat treatment, the transverse direction of the film is free shrinkage, which is a main factor causing the change of the swelling ratio of the film.
In the conventional method, the heat treatment process of the film is often a single heating temperature rise process, and the shrinkage degree of the film in the transverse direction and the longitudinal direction is different in each stage of heating. Therefore, a more precise and controllable method is needed to accurately regulate and control the film in different heated states so as to reduce the swelling ratio and improve the optical performance of the polarizer.
Disclosure of Invention
Based on the defects of the prior art, the invention provides a preparation method of a polyvinyl alcohol optical film, and aims to solve the problem of uneven dyeing caused by poor swelling during the subsequent polarizer production and processing.
In order to realize the purpose of the invention, the following technical scheme is adopted:
a preparation method of polyvinyl alcohol optical film is dissolving PVA resin for film and auxiliary materials in ultrapure water to prepare casting film stock solution with mass concentration of 25-35%; and (3) defoaming the casting film stock solution by an extruder, carrying out tape casting through a die head, pre-drying through a drying guide roller, then entering a heat treatment oven for drying and shaping, and rolling to obtain a finished product of the polyvinyl alcohol optical film.
The heat treatment may be a hot air flow type, vacuum type, hot silicone oil type, or the like drying method, and the medium for drying may be nitrogen, compressed air, silicone oil, or the like. The heat treatment is carried out by three processes of preheating, heat treatment and cooling, wherein: the preheating process can be divided into 1 to multiple sections, preferably 1 to 3 sections, and more preferably 2 sections; the heat treatment process can be divided into 1 to more stages, preferably 1 to 3 stages, more preferably 2 stages; the cooling process may be divided into 1 to several stages, preferably 1 to 3 stages, and more preferably 1 stage.
The invention controls the transverse and longitudinal shrinkage of the film by adjusting the temperature, the retention time and the tension of the film in each section of the heat treatment, and reduces the swelling ratio of the film. Take 5 stages of heat treatment as an example:
when the heat treatment is 5 stages, the temperature ranges of the stages are as follows: the temperature of the first section is 50-90 ℃, the temperature of the second section is 60-110 ℃, the temperature of the third section is 80-150 ℃, the temperature of the fourth section is 60-130 ℃, and the temperature of the V section is 30-70 ℃; wherein, the section I is preferably 60-80 ℃, the section II is preferably 70-100 ℃, the section III is preferably 90-130 ℃, the section IV is preferably 90-110 ℃ and the section V is preferably 40-60 ℃.
When the heat treatment is 5 stages, the residence time of the film in each stage of the heat treatment is as follows: 10-40s for the I section, 10-30s for the II section, 5-20s for the III section, 10-30s for the IV section and 20-50s for the V section; wherein, the section I is preferably 15-35s, the section II is preferably 10-25s, the section III is preferably 5-15s, the section IV is preferably 10-20s, and the section V is preferably 20-40s.
When the heat treatment is 5 sections, the tension of each section of the heat treatment is as follows: the first section is 30-100N/m, the second section is 40-90N/m, the third section is 20-70N/m, the fourth section is 40-90N/m, and the fifth section is 30-120N/m; wherein, the section I is preferably 60-90N/m, the section II is preferably 40-80N/m, the section III is preferably 20-50N/m, the section IV is 40-60N/m, and the section V is preferably 60-100N/m.
The preheating process of the heat treatment has lower temperature and longer retention time, and aims to ensure that the film is uniformly heated to lose water, and the film has smaller shrinkage at the moment, so the tension can be higher; the temperature in the heat treatment process is high, the residence time in the process is not too long in order to control the water content of the film, and the film is greatly shrunk in the heat treatment process, so that the tension is lowest, and the shrinkage of the width is compensated by the shrinkage of the length; the purpose of the cooling process is to cool the film to complete the final drying, at which time the film has a lower shrinkage and a higher tension. Therefore, taking the heat treatment as 5 stages as an example, the following should be ensured at the time of setting: the temperature of the section III is highest, the retention time is shortest and the tension is minimum; the section V has the lowest temperature, the longest retention time and the highest tension.
Compared with the prior art, the invention has the beneficial effects that:
the invention carries out the heat treatment by three processes of preheating, heat treatment and cooling, and strictly controls the temperature, the retention time and the tension of the film in each section of the heat treatment, so that the shrinkage rate of the film in the transverse direction and the longitudinal direction is approximate, the swelling degree in the transverse direction and the longitudinal direction is consistent, the swelling ratio is between 1 and 1.02 percent, the problem of uneven dyeing caused by overlarge swelling ratio in downstream production is reduced, and the method has simple operation, economy and feasibility.
Detailed Description
The following examples are given for the detailed implementation and specific operation of the present invention, but the scope of the present invention is not limited to the following examples.
Example 1
500Kg of PVA 1799 film resin, 50Kg of plasticizer glycerin, 2.7Kg of surfactant coconut oil diethanolamide, and 1.3Kg of antioxidant 1098 were dissolved in ultrapure water to prepare a 30% by mass casting solution. And (3) defoaming the casting film stock solution by an extruder, carrying out tape casting forming by a die head, pre-drying by a plurality of drying guide rollers, then drying and shaping in a heat treatment oven, and rolling to obtain a finished product of the polyvinyl alcohol optical film.
In this example, the heat treatment was not conducted in stages, the temperature was 110 ℃ and the heat treatment time was 90 seconds, and the tension in the heat treatment stage was controlled to 50N/m.
Example 2
Liquid preparation, defoaming, tape casting and pre-drying are carried out in the same way as in example 1, and then the mixture enters a heat treatment oven for drying and shaping. Except that the heat treatment in this example was divided into 5 stages, and the temperatures, residence times and tensions in each stage are shown in table 1.
TABLE 1
| Item | I section | II stage | Stage III | IV stage | Section V |
| Temperature (. Degree. C.) | 65 | 90 | 115 | 100 | 50 |
| Dwell time (S) | 30 | 15 | 10 | 15 | 25 |
| Tension (N/m) | 70 | 60 | 30 | 45 | 85 |
Example 3
Liquid preparation, defoaming, casting and pre-drying are carried out in the same way as in example 1, and then the mixture enters a heat treatment oven for drying and shaping. Except that the heat treatment in this example was divided into 5 stages, and the temperatures, residence times and tensions in each stage are shown in table 2.
TABLE 2
| Item | I section | Stage II | Stage III | Stage IV | Section V |
| Temperature (. Degree.C.) | 65 | 85 | 130 | 95 | 55 |
| Dwell time (S) | 30 | 20 | 5 | 10 | 20 |
| Tension (N/m) | 70 | 55 | 20 | 60 | 80 |
Comparative example 1
Liquid preparation, defoaming, casting and pre-drying are carried out in the same way as in example 1, and then the mixture enters a heat treatment oven for drying and shaping. Except that the heat treatment in this comparative example was divided into 5 stages, and the temperatures, residence times and tensions in the respective stages are shown in Table 3.
TABLE 3
| Item | Stage I | Stage II | Stage III | Stage IV | Section V |
| Temperature (. Degree.C.) | 65 | 115 | 100 | 90 | 50 |
| Dwell time (S) | 30 | 10 | 15 | 15 | 25 |
| Tension (N/m) | 70 | 30 | 45 | 60 | 85 |
Comparative example 2
Liquid preparation, defoaming, casting and pre-drying are carried out in the same way as in example 1, and then the mixture enters a heat treatment oven for drying and shaping. Except that the heat treatment in this comparative example was divided into 5 stages, and the temperature, residence time and tension of each stage are shown in table 4.
TABLE 4
| Item | I section | Stage II | Stage III | Stage IV | Section V |
| Temperature (. Degree.C.) | 65 | 90 | 115 | 100 | 50 |
| Dwell time (S) | 30 | 15 | 30 | 25 | 25 |
| Tension (N/m) | 70 | 60 | 30 | 45 | 85 |
Comparative example 3
Liquid preparation, defoaming, casting and pre-drying are carried out in the same way as in example 1, and then the mixture enters a heat treatment oven for drying and shaping. Except that the heat treatment in this comparative example was divided into 5 stages, and the temperature, residence time and tension of each stage are shown in table 5.
TABLE 5
| Item | I section | Stage II | Stage III | Stage IV | Section V |
| Temperature (. Degree.C.) | 65 | 90 | 115 | 100 | 50 |
| Dwell time (S) | 30 | 15 | 10 | 15 | 25 |
| Tension (N/m) | 70 | 60 | 60 | 70 | 85 |
The method for measuring the swelling degree and swelling ratio of the polyvinyl alcohol optical film comprises the following steps: an optical film with the length and the width of 10cm is taken, and after the optical film is immersed and swelled in pure water at 30 ℃ for 10 minutes, the ratio of the transverse (longitudinal) dimension of the film to the original transverse dimension is the transverse (longitudinal) swelling degree, and the ratio of the transverse swelling degree to the longitudinal swelling degree is called as the swelling ratio. The swelling ratio data of the films obtained in the examples and comparative examples are shown in Table 6.
TABLE 6
| Example 1 | Example 2 | Example 3 | Comparative example 1 | Comparative example 2 | Comparative example 3 | |
| Swelling ratio | 1.077 | 1.004 | 1.009 | 1.052 | 1.022 | 1.027 |
As can be seen from Table 6, the PVA optical film produced by the process conditions provided by the invention can obviously reduce the swelling ratio of the film.
The PVA films prepared in the examples and comparative examples were immersed in pure water at 35 ℃ for 1min in a solution containing 1 2 Dip-dyeing in a 30 deg.C dyeing tank with 0.5g/L and KI 20g/L for 100s, stretching while dyeing to 5 times of original length, and fixing in a fixing tank (HBO) 3 -KI 40 g/L), drying for 3min at 100 ℃, attaching cellulose triacetate films to two sides of the PVA film, and drying to obtain the polarizer. The performance index, the degree of polarization and the transmittance of the obtained polarizer were measured, respectively, and the results are shown in table 7.
TABLE 7
As can be seen from the examples and comparative examples, improper control of the temperature and residence time of each part of the heat treatment, improper tension setting of each part of the heat treatment result in differences in the degree of swelling of the film in the transverse and longitudinal directions, and the degree of swelling is relatively large. The invention carries out multi-stage heat treatment on the PVA film, strictly controls the temperature, the residence time and the tension of each stage, can lead the swelling degrees of the film in the transverse direction and the longitudinal direction to be similar, leads the swelling ratio to be between 1 and 1.02 percent, and solves the problem of uneven dyeing caused by the large swelling ratio.
The above description is only exemplary of the present invention and should not be taken as limiting the invention, and any modifications, equivalents, improvements, etc. made within the spirit and principle of the present invention should be included in the scope of the present invention.
Claims (1)
1. A preparation method of a polyvinyl alcohol optical film is characterized by comprising the following steps: dissolving PVA resin for a film and auxiliary materials in ultrapure water to prepare a casting film stock solution; defoaming the casting film stock solution by an extruder, carrying out tape casting through a die head, pre-drying through a drying guide roller, then entering a heat treatment oven for drying and shaping, and rolling to obtain a finished product of the polyvinyl alcohol optical film;
the heat treatment comprises three processes of preheating, heat treatment and cooling; the preheating process of the heat treatment is divided into 2 sections, the heat treatment process is divided into 2 sections, and the cooling process is divided into 1 section, so that the heat treatment comprises 5 sections in total;
when the heat treatment is carried out in 5 stages, the temperature ranges of the stages are as follows: the first section is 60-80 ℃, the second section is 70-100 ℃, the third section is 90-130 ℃, the fourth section is 90-110 ℃, and the fifth section is 40-60 ℃;
when the heat treatment is 5 stages, the residence time of the film in each stage of the heat treatment is as follows: 15-35s for the I section, 10-25s for the II section, 5-15s for the III section, 10-20s for the IV section and 20-40s for the V section;
when the heat treatment is 5 sections, the tension of each section of the heat treatment is as follows: 60-90N/m of section I, 40-80N/m of section II, 20-50N/m of section III, 40-60N/m of section IV and 60-100N/m of section V;
simultaneously, ensuring that: the temperature of the section III is highest, the retention time is shortest and the tension is minimum; the section V has the lowest temperature, the longest retention time and the highest tension.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010795047.7A CN111732749B (en) | 2020-08-10 | 2020-08-10 | Preparation method of polyvinyl alcohol optical film |
Applications Claiming Priority (1)
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| JP2004020629A (en) * | 2002-06-12 | 2004-01-22 | Kuraray Co Ltd | Manufacturing method of polarizing film |
| CN102834235A (en) * | 2010-07-02 | 2012-12-19 | 日本合成化学工业株式会社 | Polyvinyl alcohol-based film, method for manufacturing polyvinyl alcohol-based film, polarized film, and polarizing plate |
| CN103992606A (en) * | 2008-12-18 | 2014-08-20 | 可乐丽股份有限公司 | Polyvinyl alcohol film |
| CN105917256A (en) * | 2014-01-28 | 2016-08-31 | 株式会社可乐丽 | Master film for producing optical film |
| CN108864627A (en) * | 2018-07-02 | 2018-11-23 | 重庆云天化瀚恩新材料开发有限公司 | A kind of polyvinyl alcohol film and preparation method thereof |
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| JP2004020629A (en) * | 2002-06-12 | 2004-01-22 | Kuraray Co Ltd | Manufacturing method of polarizing film |
| CN103992606A (en) * | 2008-12-18 | 2014-08-20 | 可乐丽股份有限公司 | Polyvinyl alcohol film |
| CN102834235A (en) * | 2010-07-02 | 2012-12-19 | 日本合成化学工业株式会社 | Polyvinyl alcohol-based film, method for manufacturing polyvinyl alcohol-based film, polarized film, and polarizing plate |
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