JP2000159658A - Manufacturing method of dry film with uniform thickness - Google Patents

Abstract

(57) [Summary] [PROBLEMS] To make it possible to form a dry film having a uniform thickness using a large bat container, and to apply the dried film to industrial production by a casting method. It manufactures high quality dry film with uniform thickness and uses it for oral medicine (periodontal medicine,
Stomatitis treatment, oral band, etc.), external preparation (hemostatic,
Wound / burn protection agent, skin disease treatment agent, etc., systemic treatment (diabetes treatment agent, angina treatment agent, case prevention / treatment agent, etc.)
Apply to etc. SOLUTION: A film-forming solution comprising a film-forming substance and a solvent is flowed into a bat container having a shape in which a central portion 13a protrudes upward from an edge portion 13b in a surface shape of a bottom surface of the bat container 11. A method for producing a film having a uniform thickness in which a film-forming substance is formed by extending the film and then removing the solvent.

Description

DETAILED DESCRIPTION OF THE INVENTION

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a vat container suitable for producing a film having a uniform thickness when a film-forming solution is cast into a vat container and the solvent is evaporated to form a film. .

[0002]

2. Description of the Related Art It has been conventionally known that a thin film is formed by a casting method, and this thin film is used as an oral preparation, an external preparation, a systemic treatment preparation, and the like.
No. 10561, JP-A-8-183732, and the like. In the case of using a vat container and casting the solution for film formation in the vat container and then drying the film,
Although it was possible to perform uniform thickness film formation by setting appropriate film forming conditions using a small bat container, for example, a square bat container having a diameter of about 5 cm or less, or one side of about 5 cm or less, If the bat container is larger than those, it is difficult to produce a dry film having a uniform thickness with the existing bat container. For example, commercially available bat containers made of metal such as aluminum, iron, and stainless steel, or plastic containers such as polyethylene, polypropylene, polystyrene, melanin resin, and Teflon resin have irregular shapes on the bottom surface of the bat. Even when a dried film was produced by the casting method, a film having a uniform thickness could not be produced. Conventionally, as shown in FIG.
A vat container 11 'having a horizontal bottom surface 13' was used, the smoothness of the bottom surface was set well, and the thickness was equalized. In addition, the vat container 11 'on which the film forming solution has been cast.
Was placed directly on the shelf hot plate 31 of the dryer which was adjusted horizontally, and was subjected to a drying treatment to produce a dried film.

[0003]

SUMMARY OF THE INVENTION The present invention relates to a method for producing an industrial dry film by the casting method, in which a film-forming solution is cast into a vat container and the solvent is evaporated to form a film.
This enables production of a dry film having a uniform thickness.

[0004]

Means for Solving the Problems According to the present invention, when producing a dried film by the casting method, the inventors focused on the surface shape of the bottom surface of the vat container for casting the solution for film formation, and as a result, The better the flatness of the surface is, the more even the dried film can be manufactured, and surprisingly, in the surface shape of the bottom surface of the bat container, the center of the surface of the bottom surface of the bat container rises from the peripheral portion and faces upward. By using a bat container having a convex bottom surface shape, that is, a bat container having an upwardly convex surface, even a large bat container can be placed on a horizontally adjusted shelf to achieve uniform thickness. It has been found that a dry film can be produced. Also, when heating from the shelf of the dryer that is adjusted horizontally for the purpose of promoting the evaporation of the solvent of the film-forming solution, the bottom of the vat container cannot uniformly contact the hot plate of the shelf, so that the uniformity of heat reception Can not be obtained. Therefore, it was also found out that the bottom surface of the bat container can receive the widthwise heat of the shelf plate hot plate evenly by floating the bat container from the shelf plate hot plate, and a dry film having a uniform thickness can be produced.

That is, in the method for producing a dry film having a uniform thickness according to the present invention, a bat container having a shape in which a central portion protrudes upward from an edge in a surface shape of a bottom surface of a bat container is provided with a film-forming substance and The method is characterized in that a film-forming solution comprising a solvent is cast, and then the solvent is removed to form a film-forming substance.

[0006]

DETAILED DESCRIPTION OF THE INVENTION Surface shape of bottom surface of vat container The surface shape of the bottom surface of the vat container has a central portion protruding upward with respect to the peripheral portion so that the central portion is raised from the peripheral portion. In addition, it is preferable that there is a continuous or intermittent downward slope from the center to the edge, and it is particularly preferable that there be a concentric or contoured slope from the center to the edge. FIG. 1 is a sectional view of a vat container 11 of the present invention and an explanatory diagram showing a method for removing a solvent. The vat container 11 includes a vat container bottom surface 13 and a side wall 15 connected to the vat container bottom 13, and a film forming solution is cast into the vat container 11. The height difference between the central portion 13a and the peripheral portion 13b of the surface portion 13c of the bat container bottom surface 13 is as follows:
0.2 to 3.0 mm is preferred. The height difference is complicatedly related to the size of the bottom surface 13 of the vat container, the viscosity and amount of the film forming solution to be cast, and the evaporation rate of the solvent. Therefore, the height difference is appropriately selected within the range. In general, the larger the bottom surface 13 of the vat container, the lower the viscosity of the film forming solution to be cast, the larger the amount of the film forming solution to be cast, the faster the evaporation rate of the solvent, the more the center 13a and the side. The optimum value of the height difference from the edge 13b tends to increase. When the height difference between the central portion 13a of the surface portion 13c and the peripheral portion 13b of the vat container bottom surface 13 is less than 0.2 mm, the thickness of the dry film at the central portion of the vat container bottom surface 13 is thicker than that at the peripheral portion of the vat container bottom surface. Conversely, if the height difference exceeds 3.0 mm, the solution cast during the drying process flows to the peripheral portion of the bottom surface of the vat container, so that the thickness of the dry film at the center of the bottom surface of the vat container becomes thin, and the film is dried. The uniformity of the film thickness of the entire film becomes poor. In order to ensure the uniformity of the thickness of the dried film to be formed, the thickness of the bottom surface of the vat container is preferably as uniform as possible. In addition,
The height difference between the central portion 13a and the peripheral portion 13b is actually not as extreme as shown in FIG. FIG. 1 merely shows a large difference in height with respect to the size of the bat container 11 for convenience of illustration. For example, the size of the bat container 11 is 5 cm.
The height difference is 0.2 to 3 for a diameter or one side of ~ 2 m.
mm.

[0007] 2. Shape and size of the whole bat container The shape and size of the whole bat container are not particularly limited, but the size of the whole bat container is determined from the balance with the drying device and the ease of handling. In general, one side of the vat container is preferably 2 m or less, or 2 m or less in diameter, and a vat container having one side of 60 cm or less, or 60 cm in diameter or less can be suitably used. Considering the industrial production of a dry film, the size of the bat container is preferably a bat having a side of 5 cm or more or a diameter of 5 cm or more. The shape of the whole bat container is triangular, quadrangular (square, rectangular,
A diamond, a pentagon or more, a polygon, a circle, an ellipse, or the like can be used. In particular, a square, rectangular, or circular vat container can be preferably used from the viewpoint of application of a dry film and ease of processing in the next step.

[0008] 3. Material of vat container The material of the vat container is not limited, and is made of metal (iron, aluminum, copper, stainless steel, silver, gold, brass, etc.) or plastic (polyethylene, polypropylene, acrylonitrile / styrene resin, acrylonitrile / butadiene / styrene) Resin, polyamide, polyethylene terephthalate, polycarbonate, melanin resin, phenolic resin, urea resin, polyvinyl chloride, terephthalate, polycarbonate, melanin resin, phenolic resin, urea resin, polyvinyl chloride, Teflon resin, etc.), plastic resin Metal and glass materials can be used.

4. Solution for film formation The solution for film formation is composed of a film-forming substance and a solvent, and may contain other additional components. 5. As a film-forming substance, any material capable of forming a film may be used.
There is no limitation, and the following can be exemplified.・ Water-soluble polymer ・ Methylcellulose, hydroxypropylcellulose,
Cellulose lower alkyl ether compounds such as hydroxypropylmethylcellulose ・ Vinyl compounds such as polyvinylpyrrolidone and polyvinyl alcohol ・ Polysaccharides such as pullulan and starch and derivatives thereof ・ Polyacrylamide ・ Polyethylene oxide ・ Polyoxyalkylenes such as high molecular weight polyethylene glycol ・ Carboxy Vinyl polymers ・ Carboxymethylcellulose and its salts such as sodium salt and calcium salt ・ Salts such as polyacrylic acid and sodium salt ・ Salts such as alginic acid, sodium alginate, ammonium alginate, triethanolamine alginate ・ Tragant gum, locust bean gum ・ methacrylic Copolymerized with acrylic acid such as acid, styrene or vinyl ether monomer Polymers and their salts-Polypeptides such as gelatin, agar-Guar gum, xanthan gum-Gum arabic-Chitin, chitosan-Water-insoluble polymer-Ethyl cellulose, cellulose acetate, methacrylic acid, methacrylated trimethylammonium polymer, methacrylic acid Dimethylaminoethyl methacrylic acid copolymer, polyvinyl acetal, dimethylaminoacetate, cellulose acetate, dibutylhydroxypropyl ether

[0010] 6. Any solvent can be used as long as it can dissolve the film-forming substance, and there is no particular limitation. Specifically, water, ethanol, methanol, propanol, isopropanol, acetone, ethyl acetate or a mixed solvent thereof can be used.

7. Other optional components can be added to the film forming solution depending on the use and the like. For example, substances with physiological activity (bactericides, antibiotics, anti-inflammatory drugs,
Antihistamines, etc.), plasticizers, coloring agents, flavoring agents,
There are stabilizers and the like, examples of which are as follows. (1) Drug having bactericidal action Chlorhexidine or hydrochloride, methylosal, silver protein, chloramine, iodoglycerin, iodoform, boric acid, paraformaldehyde, phenol, hexylresorcin, benzalkonium chloride, benzethonium chloride, chlorhexidine gluconate, bromide Phenododecium, decalinium chloride, cetylpyridinium chloride, ofloxacin, pompidone iodotriclosan,
Ethanol and the like.

(2) Drugs having antibacterial activity: tetracycline, tetracycline hydrochloride, benzylpenicillin, ampicillin, carpenicillin, acetylkitasamycin, amoxicillin, pacitracin, cephalothin sodium, cephaloridin, cephalexin,
Erythromycin, chloramphenicol, oxytetracycline hydrochloride, doxycycline hydrochloride, polymyxin sulfate B, fradiomycin sulfate, gentamicin sulfate, minocycline hydrochloride and the like.

(3) Drugs having plaque dissolving action: lysozyme chloride, amylase, dextranase, protease, seratiothiopeptidase and the like. (4) Drugs acting on local anesthesia Procaine hydrochloride, oxyprocaine hydrochloride, tetracaine hydrochloride, chloroprocaine hydrochloride, ethyl aminobenzoate,
Dibucaine, dibucaine hydrochloride, lidocaine, lidocaine hydrochloride, cocaine hydrochloride, thecaine.

(5) Drugs having an anti-inflammatory action: sulpyrine, antipyrine, aspirin, phenylbutazone, mepyrizole, oxyphenbutazone, fenbufen, mefenamic acid, flurbibrofen, diclofenac sodium, ketoprofen, nabroxen,
Tiaramid hydrochloride, pendidamine hydrochloride, alclofenac, ibufenac, perisosasar citrate, ibuprofen, indomethacin, aluminum flufenamic acid, tinorizine hydrochloride, clofezone protidic acid, dexamethasone, triamcinolone acetonide, prostaglandin, isotipendil hydrochloride, mefenamic acid, bufene Kisamac, hydrocortisone, prednisolone, fluonosinolone acetonide, hydrocortisone acetate, prednisolone acetate, methylprednisolone, dexamethasone acetate, betamethasone, betamethasone valerate, tranexamic acid, bisabolol, glycyrrhizin, dipotassium glycyrrhetinic acid, flumethasone, carbazochrome Allantoin etc.

(6) Antihistamines diphenhydramine hydrochloride, chlorpheniramine maleate, clemastine and the like. (7) Drugs having tissue repairing / activating / vascular strengthening effects: ascorbic acid phosphate, rutin, rumin, collagen flavonic acid, TGF-
β, cytokines, vitamin E nicotinate, pionin and the like.

(8) Plasticizer: polyethylene glycol (200-6000), glycerin, propylene glycol, 1,3-butylene glycol, sorbit, ethylene oxide / propylene oxide copolymer, diethyl phthalate, dibutyl phthalate, butyl phthalyl butyl Glycolate, ethylene glycol, dipropylene glycol, triacetin, spun fatty acid lauric acid and the like.

(9) Colorant: tar dye and the like. (10) Flavoring agents: natural or synthetic flavors, saccharin, citric acid, fumaric acid, menthol, peppermint oil, tartaric acid, aspartame and the like.

(11) Stabilizers: vitamin C, vitamin E, sodium sulfite, sodium pyrosulfite, sodium bisulfite, butylhydroxytoluene, propylpyrrole, butylhydroxyanisole and the like.

5. Drying Method The film-forming solution cast in the vat container is dried to produce a dried film having a thickness of preferably 10 to 2000 μm, more preferably 20 to 500 μm. There is no limitation on the drying method, and any method may be used as long as the film forming solution can be dried. As a drying method, a natural drying method, a blast drying method, a heated blast drying method, a heating drying method, a vacuum drying method, a heating vacuum drying method, and the like are generally used.

6. The method of floating the vat container from the shelf hot plate of the dryer By heating, when promoting the evaporation of the solvent of the film-forming solution cast in the vat container, if there is uneven heating on the bottom surface of the vat container, where heat is applied well As the drying proceeds, the thickness of the dried film increases, whereas where the contact with heat is poor, the thickness of the dried film decreases, and as a result, the uniformity of the film thickness of the entire dried film becomes poor. This is because, when the vat container is placed on the shelf hot plate of the dryer, it is difficult for the back surface of the bottom of the vat container and the shelf plate hot plate to evenly adhere to each other, even when the vat container is large or as in the present invention. In a deformed bat in which the center of the surface of the bat bottom surface is raised from the peripheral portion (the center portion protrudes upward), the contact portion with the hot plate is easily localized.

Therefore, as shown in FIG. 1, the bottom surface 13d of the vat container is floated from the hot plate 31 so that the bottom surface 13d of the vat container can evenly receive heat from the hot plate 31 of the dryer. By making the bottom surface 13d evenly receive the heat radiation, it is possible to produce a dry film having a uniform thickness. As shown in FIG. 1, in order to float the bat container bottom surface 13 d from the shelf plate hot plate 31, as shown in FIG.
d, metal, rubber, plastic, glass, paper, pottery, magnetic or porcelain The selected spacer-like piece 21 is attached. As these spacer-like pieces 21, rubber or plastic pieces having poor thermal conductivity can be suitably used.

The floating height of the spacer-like small pieces 21 is not particularly limited as long as the sub-heat can be uniformly obtained from the hot plate of the shelf, but is usually 0.5 mm or more, preferably 2 mm or more. For example, when a 50 cm square bat container is used, rubber having a plane size of several mm square to about 10 mm square may be attached to the four back corners of the bottom surface of the bat container. In addition to the method of attaching or bonding small pieces to the periphery to float the bat container from the shelf hot plate, when manufacturing the bat container, from the beginning only the whole or part of the back edge of the bottom surface of the bat bottom The bat container may be formed so that the butt container is grounded and the center of the bat container floats from the shelf plate hot plate. In addition, there is no restriction on this method as long as the bottom surface of the vat container can be floated from the hot plate of the shelf of the dryer. For example, lift the vat container so that the vat container does not directly rest on the hot plate of the dryer shelf, or attach a guide to the side of the dryer around the hot plate of the dryer shelf, and attach the vat to the guide. A method of placing a container on the container is conceivable.

[0023]

According to the present invention, it is possible to form a dry film having a uniform thickness by using a large bat container. Therefore, the present invention can be applied to industrial production of a dry film by a casting method. As it can produce high quality dry film with uniform thickness, it can be applied to medicines such as oral agents (periodontal agents, stomatitis treatment agents, oral bands, etc.) and external agents (hemostatic agents, wound / burn protection agents, skin diseases) Therapeutic agents, etc.), systemic therapeutic agents (diabetes therapeutic agents, angina pectoris therapeutic agents, anti-case anti-therapeutic agents, etc.) and the like.

[0024]

EXAMPLES Examples 1 to 3 Hydroxypropyl cellulose (300 g) was dissolved in anhydrous ethanol to make a total amount of 10,000 g to prepare a film forming solution. Next, 0.3 g of a film-forming solution was cast per square centimeter of each bat container shown in Table 1, and ethanol was evaporated by a heating vacuum drying method to produce a dried film. The dried film stuck to the bottom surface of each vat container was peeled off using tweezers, and the thickness of the film was measured with a film thickness meter.
Measurement points were uniformly selected at four points 5 cm inward from the center and the periphery, and the film thickness was measured at a total of five measurement points. After calculating the average value ± standard deviation of the film thickness at five points, the coefficient of variation [= (standard deviation / average value) × 100] was determined. The evaluation results are shown in Table 1. The average value of the film thickness was about 70 μm.

[0025]

[Table 1] Table 1: Shape of vat container ・ Thickness of dry film on the surface of the bottom of vat container Size Inner diameter or uniformity of height difference between center and edge and height x width (cm) [Center position -Edge position] Evaluation Comparative Example 1 20 × 20 0.0 mm × Comparative Example 2 40 × 40 0.0 mm × Comparative Example 3 60 × 60 0.0 mm × Example 1 20 × 20 0.5 mm ◎ Example 2 40 × 40 1.0 mm ◎ Example 3 60 × 60 1.5 mm ◎ The vat container used was made of stainless steel coated with Teflon resin by baking. Rubber pieces (thickness: 4 mm) were attached to the four corners on the back side of the bottom surface of the vat container in a 5 mm square, and the back surface of the bottom surface of the vat container was floated from a shelf hot plate of a horizontally adjusted dryer. Evaluation Evaluation criteria ◎: Coefficient of variation is 10% or less ○: Coefficient of variation exceeds 10% and less than 20% △: Coefficient of variation exceeds 20% and less than 30% ×: Coefficient of variation is 30% or more

As shown in Comparative Examples 1 to 3, regardless of the size of the bat container, there is no difference in height between the center portion and the peripheral portion of the bottom surface of the bat container. When a dry film was manufactured using a good bat, the thickness of the dry film at the center and the periphery of the bottom of the bat varied, and the uniformity of the film thickness of the entire dry film was poor. On the other hand, in Examples 1 to 3, although the center of the bottom surface of the vat container was raised by 0.5 to 1.5 mm as compared with the peripheral portion (although there was a difference in height), a film was formed using these vat containers. As a result, the variation in the thickness of the dried film was reduced, and a film having the entire dried film having a uniform thickness was produced.

Examples 4 to 9 A film forming solution was prepared by dissolving 440 g of polyvinyl alcohol and 60 g of propylene glycol in water to make the total amount 10,000 g. Next, 0.52 g of a film forming solution was cast per square centimeter of each bat container shown in Table 2, and water was evaporated by a heating vacuum drying method to produce a dried film. The dried film stuck to the bottom surface of each vat container was peeled off using tweezers, and the thickness of the film was measured with a film thickness meter. Measurement points were uniformly selected at four points 5 cm inward from the center and the periphery, and the film thickness was measured at a total of five measurement points. After calculating the average value ± standard deviation of the film thickness at 5 points,
A coefficient of variation [= (standard deviation / average value) × 100] is obtained,
Table 2 shows the evaluation results. The average value of the film thickness is about 200
μm.

[0028]

[Table 2] Table 2: Shape of vat container • Thickness of dry film on the bottom surface of vat container Size Inner diameter or height x width (cm) of uniformity of height difference between center and periphery [center position] -Edge position] Evaluation Example 4 60 × 60 0.1 mm △ Example 5 60 × 60 4.0 mm △ Example 6 60 × 60 0.2 mm ○ Example 7 60 × 60 0.5 mm ○ Example 8 60 × 60 1.75 mm ◎ Example 9 60 × 60 3.0 mm ○ The vat container used was made of polypropylene. A 10 mm square polypropylene plate (thickness: 5 mm) was attached to the four corners on the back surface side of the bottom surface of the vat container, and the vat container was floated from the hot plate of the drying tray shelf whose bottom surface was adjusted horizontally. Evaluation Evaluation criteria ◎: Coefficient of variation is 10% or less ○: Coefficient of variation exceeds 10% and less than 20% △: Coefficient of variation exceeds 20% and less than 30% ×: Coefficient of variation is 30% or more

As shown in Examples 4 and 5, the center of the bottom surface of the vat container is 0.1 mm or less or 4.0 mm or less as compared with the peripheral portion.
In the bat container of not less than mm, the thickness of the dry film at the center portion and the peripheral portion of the bat bottom was slightly varied, and the uniformity of the film thickness of the entire dry film was slightly good. On the other hand, in Examples 6 to 9, the center of the bottom surface of the vat container was raised by 0.2 to 3.0 mm as compared with the peripheral portion, but when these vat containers were used to form a film, the thickness of the dry film was reduced. Example 8 in which the variation was small, and especially the center part of the bottom surface of the vat container was 1.75 mm higher than the peripheral part, was uniform in thickness.
A good dry film could be manufactured.

Examples 10 to 12 470 g of hydroxypropylcellulose, 10 g of minocycline hydrochloride (titer), 15 g of concentrated glycerin, and 5 g of xylitol were dissolved in anhydrous ethanol to make a total amount of 5,000 g to prepare a solution for film formation. Next, per square centimeter of each vat container shown in Table 3, 0.1% of the film forming solution was used.
26 g was cast and ethanol was evaporated by a vacuum drying method (without heating) to produce a dried film. The dried film stuck to the bottom surface of each vat container was peeled off using tweezers, and the thickness of the film was measured with a film thickness meter. Measurement points are equally selected at 4 points 5 cm inside from the center and the edge,
The film thickness was measured at a total of five measurement points. After calculating the average value ± standard deviation of the film thickness at five points, the coefficient of variation [= (standard deviation /
(Average value) × 100], and the evaluation results are shown in Table 3. The average value of the film thickness was about 200 μm.

[0031]

[Table 3] Table 3: Shape of vat container • Thickness of dry film on the surface of the bottom of vat container Size Inner diameter or uniformity of height difference between center and edge and height x width (cm) [Center position -Edge position] Evaluation Comparative Example 4 50 × 50 0.0 mm × Example 10 50 × 50 0.5 mm ○ Example 11 50 × 50 1.0 mm ◎ Example 12 50 × 50 1.5 mm ◎ Vat container And those made by Stereless. A rubber piece was not attached to the back surface of the bottom surface of the vat container, and the vat container was directly placed on a shelf plate of a horizontally adjusted dryer. Evaluation Evaluation criteria ◎: Coefficient of variation is 10% or less ○: Coefficient of variation exceeds 10% and less than 20% △: Coefficient of variation exceeds 20% and less than 30% ×: Coefficient of variation is 30% or more

This time, the solvent was evaporated by a vacuum drying method without heating, and a rubber film was not attached to the back surface of the bottom of the vat container, but was placed directly on the shelf plate of the dryer to produce a dry film. . As a result, as shown in Comparative Example 4, when a dry film is manufactured using a bat in which the center portion of the surface portion of the bottom surface of the bat container has no difference in the height of the peripheral portion, the same results as in Comparative Examples 1 to 3 are obtained. The thickness of the dried film at the center and the periphery of the bat bottom varied, and the uniformity of the thickness of the entire dried film was poor. On the other hand, in Examples 10 to 12, the center of the bottom surface of the vat container was raised by 0.5 to 1.5 mm as compared with the peripheral portion. However, when the vat container was formed using these vat containers, the thickness of the dry film was reduced. Variation was reduced, and a film having a uniform thickness of the entire dried film could be manufactured.

Examples 13 to 16 470 g of hydroxypropylcellulose, 10 g (potency) of minocycline hydrochloride, 15 g of concentrated glycerin, and 5 g of xylitol were dissolved in anhydrous ethanol to a total amount of 5,000 g to prepare a solution for film formation. Next, the film forming solution was added to each vat container shown in Table 4 per square centimeter.
26 g was cast and ethanol was evaporated by a heating vacuum drying method to produce a dried film. The dried film stuck to the bottom surface of each vat container was peeled off using tweezers, and the thickness of the film was measured with a film thickness meter. Measurement points were uniformly selected at four points 5 cm inward from the center and the periphery, and the film thickness was measured at a total of five measurement points. Average value of film thickness at 5 points ±
After calculating the standard deviation, the coefficient of variation [= (standard deviation / average value)
× 100], and the evaluation results are shown in Table 4. The average value of the film thickness was about 200 μm.

[0034]

[Table 4] Table 4: Shape of vat container • Pressure of dry film on surface of vat container bottom Size Inner diameter or uniformity of height difference between center and periphery Vertical x horizontal (cm) [Center position -Edge Position] Evaluation Comparative Example 5 50 × 50 0.0 mm × Example 13 50 × 50 1.0 mm △ (A 10 mm square rubber piece (thickness 3 mm) was not attached to the back surface of the bottom surface of the bat container. Example 14 50 × 50 0.5 mm ○ Example 15 50 × 50 1.0 mm ◎ Example 16 50 × 50 1.5 mm ◎ The vat container was made of Stereleless. used. Rubber pieces of 10 mm square (thickness 3
mm) was adhered and used, and the back surface of the bottom surface of the vat container was floated from the shelf hot plate of the dryer adjusted horizontally. Evaluation Evaluation criteria ◎: Coefficient of variation is 10% or less ○: Coefficient of variation exceeds 10% and less than 20% △: Coefficient of variation exceeds 20% and less than 30% ×: Coefficient of variation is 30% or more

In this case, the solvent was evaporated by a heating vacuum drying method, and 10 mm
A square rubber piece (thickness: 3 mm) was affixed and placed on a hot plate of a dryer shelf to produce a dried film. As a result, as shown in Comparative Example 5, when a dry film was manufactured using a bat having no height difference between the center portion and the peripheral portion of the surface portion of the bottom surface of the bat container, similar to the results of the comparative examples thus far, The thickness of the dried film at the center and the periphery of the bat bottom varied, and the uniformity of the thickness of the entire dried film was poor. Example 13
As shown in the figure, even when using a bat container in which the center of the bottom surface of the bat container is raised 1.0 mm from the peripheral portion, a 10 mm square rubber piece (thickness 3 m
When the vat container was directly placed on the shelf hot plate without attaching m), the thickness of the dry film at the center and the peripheral portion of the bottom of the vat varied slightly, and the thickness of the dry film as a whole was The uniformity was somewhat good. On the other hand, in Examples 14 to 16, the center of the bottom surface of the vat container was 0.5 to 1.5 m compared to the peripheral portion.
m, but when these bat containers were used to form a film, the variation in the thickness of the dried film was reduced in the same manner as in the results of Examples 8 to 10, and it was possible to produce a film having a uniform thickness of the entire dried film. Was.

[Brief description of the drawings]

FIG. 1 is an explanatory sectional view showing a bat container shown in an embodiment of the present invention.

FIG. 2 is an explanatory sectional view showing a bat container shown in a comparative example of the present invention.

[Explanation of symbols]

 11, 11 'bat container 13, 13' bat container bottom surface 13a central portion 13b peripheral portion 13c surface portion 13d bat container bottom surface 15 side wall 21 spacer-like small piece 31 shelf plate hot plate

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[Procedure amendment]

[Submission date] January 7, 1999 (1999.1.7)

[Procedure amendment 1]

[Document name to be amended] Statement

[Correction target item name] 0025

[Correction method] Change

[Correction contents]

[0025]

[Table 1] Table 1: Shape of vat container ・ Thickness of dry film on the surface of the bottom of vat container Size Inner diameter or uniformity of height difference between center and edge and height x width (cm) [Center position -Edge position] Evaluation Comparative Example 1 20 × 20 0.0 mm × Comparative Example 2 40 × 40 0.0 mm × Comparative Example 3 60 × 60 0.0 mm × Example 1 20 × 20 0.5 mm ◎ Example 2 40 × 40 1.0 mm ◎ Example 3 60 × 60 1.5 mm ◎ The vat container used was made of stainless steel coated with Teflon resin by baking. Rubber pieces (thickness: 4 mm) were attached to the four corners on the back side of the bottom surface of the vat container in a 5 mm square, and the back surface of the bottom surface of the vat container was floated from a shelf hot plate of a horizontally adjusted dryer. Evaluation Evaluation criteria ◎: Coefficient of variation is 10% or less ○: Coefficient of variation exceeds 10%, 20% or less Δ: Coefficient of variation exceeds 20%, less than 30% ×: Coefficient of variation is 30% or more

[Procedure amendment 2]

[Document name to be amended] Statement

[Correction target item name] 0028

[Correction method] Change

[Correction contents]

[0028]

[Table 2] Table 2: Shape of vat container • Thickness of dry film on the bottom surface of vat container Size Inner diameter or height x width (cm) of uniformity of height difference between center and periphery [center position] -Edge position] Evaluation Example 4 60 × 60 0.1 mm △ Example 5 60 × 60 4.0 mm △ Example 6 60 × 60 0.2 mm ○ Example 7 60 × 60 0.5 mm ○ Example 8 60 × 60 1.75 mm ◎ Example 9 60 × 60 3.0 mm ○ The vat container used was made of polypropylene. A 10 mm square polypropylene plate (thickness: 5 mm) was attached to the four corners on the back surface side of the bottom surface of the vat container, and the vat container was floated from the hot plate of the drying tray shelf whose bottom surface was adjusted horizontally. Evaluation Evaluation criteria ◎: Coefficient of variation is 10% or less ○: Coefficient of variation exceeds 10%, 20% or less Δ: Coefficient of variation exceeds 20%, less than 30% ×: Coefficient of variation is 30% or more

[Procedure amendment 3]

[Document name to be amended] Statement

[Correction target item name] 0031

[Correction method] Change

[Correction contents]

[0031]

[Table 3] Table 3: Shape of vat container • Thickness of dry film on the surface of the bottom of vat container Size Inner diameter or uniformity of height difference between center and edge and height x width (cm) [Center position -Edge position] Evaluation Comparative Example 4 50 × 50 0.0 mm × Example 10 50 × 50 0.5 mm ○ Example 11 50 × 50 1.0 mm ◎ Example 12 50 × 50 1.5 mm ◎ Vat container And those made by Stereless. A rubber piece was not attached to the back surface of the bottom surface of the vat container, and the vat container was directly placed on a shelf plate of a horizontally adjusted dryer. Evaluation Evaluation criteria ◎: Coefficient of variation is 10% or less ○: Coefficient of variation exceeds 10%, 20% or less Δ: Coefficient of variation exceeds 20%, less than 30% ×: Coefficient of variation is 30% or more

[Procedure amendment 4]

[Document name to be amended] Statement

[Correction target item name] 0032

[Correction method] Change

[Correction contents]

In this case, the solvent was evaporated by a vacuum drying method without heating, and a rubber film was not attached to the back of the bottom surface of the vat container. Was manufactured. As a result, as shown in Comparative Example 4, when a dry film is manufactured using a bat in which the center portion of the surface portion of the bottom surface of the bat container has no difference in the height of the peripheral portion, the same results as in Comparative Examples 1 to 3 are obtained. The thickness of the dried film at the center and the periphery of the bat bottom varied, and the uniformity of the thickness of the entire dried film was poor. On the other hand, in Examples 10 to 12, the center of the bottom surface of the vat container was raised by 0.5 to 1.5 mm as compared with the peripheral portion. However, when the vat container was formed using these vat containers, the thickness of the dry film was reduced. Variation was reduced, and a film having a uniform thickness of the entire dried film could be manufactured.

[Procedure amendment 5]

[Document name to be amended] Statement

[Correction target item name] 0034

[Correction method] Change

[Correction contents]

[0034]

Table 4 Table 4: Uniformity length × width (cm) [center position of the height difference of Thickness size inside diameter or central dry film on the surface portion of the shape and butt container bottom butt container and edges -Edge Position] Evaluation Comparative Example 5 50 × 50 0.0 mm × Example 13 50 × 50 1.0 mm △ (A 10 mm square rubber piece (thickness 3 mm) was not attached to the back surface of the bottom surface of the bat container. Example 14 50 × 50 0.5 mm ○ Example 15 50 × 50 1.0 mm ◎ Example 16 50 × 50 1.5 mm ◎ The vat container was made of Stereleless. used. Rubber pieces of 10 mm square (thickness 3
mm) was adhered and used, and the back surface of the bottom surface of the vat container was floated from the shelf hot plate of the dryer adjusted horizontally. Evaluation Evaluation criteria ◎: Coefficient of variation is 10% or less ○: Coefficient of variation exceeds 10%, 20% or less Δ: Coefficient of variation exceeds 20%, less than 30% ×: Coefficient of variation is 30% or more

[Procedure amendment 6]

[Document name to be amended] Statement

[Correction target item name] 0035

[Correction method] Change

[Correction contents]

[0035] This time installed, evaporated by Ri solvent heated vacuum drying, also rubber pieces 10mm square on the back side corners of the vat bottom of the container on the shelf plate heat plate by attaching (thickness 3mm) Dryer Thus, a dried film was produced. As a result, as shown in Comparative Example 5, when a dry film was manufactured using a bat having no height difference between the center portion and the peripheral portion of the surface portion of the bottom surface of the bat container, similar to the results of the comparative examples thus far, The thickness of the dried film at the center and the periphery of the bat bottom varied, and the uniformity of the thickness of the entire dried film was poor. Further, as shown in Example 13, even when using a bat container in which the center of the bottom surface of the bat container was raised 1.0 mm from the peripheral portion, a 10 mm square rubber piece (thickness 3 m) was formed on the back surface of the bottom surface of the bat container.
When the vat container was directly placed on the shelf hot plate without attaching m), the thickness of the dry film at the center and the peripheral portion of the bottom of the vat varied slightly, and the thickness of the dry film as a whole was The uniformity was somewhat good. On the other hand, in Examples 14 to 16, the center of the bottom surface of the vat container was 0.5 to 1.5 m compared to the peripheral portion.
m, but when these bat containers were used to form a film, the variation in the thickness of the dried film was reduced in the same manner as in the results of Examples 8 to 10, and it was possible to produce a film having a uniform thickness of the entire dried film. Was.

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Claims (1)

[Claims] 1. A film-forming solution comprising a film-forming substance and a solvent is cast on a bat container having a shape in which a central portion protrudes upward from an edge in a surface shape of a bottom surface of the bat container. And producing a film-forming substance by removing the solvent.