CN116021694B - Solution casting large film device and method - Google Patents

Solution casting large film device and method Download PDF

Info

Publication number
CN116021694B
CN116021694B CN202310319660.5A CN202310319660A CN116021694B CN 116021694 B CN116021694 B CN 116021694B CN 202310319660 A CN202310319660 A CN 202310319660A CN 116021694 B CN116021694 B CN 116021694B
Authority
CN
China
Prior art keywords
casting
heat
heating
film
sleeve
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Active
Application number
CN202310319660.5A
Other languages
Chinese (zh)
Other versions
CN116021694A (en
Inventor
于洋
秦宇
高洪图
王乐成
郑重德
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Shenyang Hengjiu Antai Environmental Protection And Energy Saving Technology Co ltd
Original Assignee
Shenyang Hengjiu Antai Environmental Protection And Energy Saving Technology Co ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Shenyang Hengjiu Antai Environmental Protection And Energy Saving Technology Co ltd filed Critical Shenyang Hengjiu Antai Environmental Protection And Energy Saving Technology Co ltd
Priority to CN202310319660.5A priority Critical patent/CN116021694B/en
Publication of CN116021694A publication Critical patent/CN116021694A/en
Application granted granted Critical
Publication of CN116021694B publication Critical patent/CN116021694B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Images

Classifications

    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/30—Hydrogen technology
    • Y02E60/50—Fuel cells

Abstract

The invention provides a solution large film casting device and a method, a film casting disc is arranged in the middle of a bearing surface of a heating part, the film casting disc is used for arranging film casting liquid, and the effective film casting area of the film casting disc is 4-25m 2 The area of the bearing surface is 5-30m 2 The area of the bearing surface is larger than the effective casting area of the casting plate, the heat-insulating water-cooled jacket is sleeved on the heating part and the outer peripheral side of the casting plate, the height adjusting part and the middle part of the casting plate are oppositely arranged, the height adjusting part comprises a first thread heightening component, a first pair of top sleeves of the first thread heightening component penetrate through the heating part to jack up the casting plate, so that casting solution in the middle part of the casting plate flows out of a part towards the edge in advance before film formation, the casting solution in the middle part becomes shallow, the casting solution in the edge becomes deep, and the influence on film thickness uniformity caused by that the casting solution on the edge flows into a part towards the middle part due to the fact that the casting solution in the middle part of the casting plate is higher than the casting solution in the edge in temperature, solvent evaporation is fast and solute crystallization film formation is fast in the film formation process is counteracted.

Description

Solution casting large film device and method
Technical Field
The invention belongs to the technical field of flow batteries, fuel cells and ion membrane electrolytic tanks, and particularly relates to a solution large membrane casting device and a solution large membrane casting method.
Background
The existing film-making methods are usually a dynamic open stretching method, an extrusion film method and a casting method, but have the defects of complex process, expensive equipment, high film-making cost, low crystallinity, anisotropy and the like of the finished film.
For this reason, chinese patent 201110201827.5 proposes a static closed solution casting method, which basically overcomes the above-mentioned drawbacks of the stretching, extruding and casting methods and can be used for an area of 1m 2 The following are the followingPreparation of the film.
But the method is specific to an area of 1m 2 The above film is poor in preparation effect, and is characterized in that the middle part of the film is thick and the edge is thin, and the larger the area of the cast film is, the thicker the middle part of the film is and the thinner the edge is. The method is characterized in that the casting film tray is placed on the peripheral support, the middle part of the casting film tray is lack of support, when the casting film tray is large, the middle part of the casting film tray is deformed and recessed under the action of gravity, the larger the casting film tray is, the more serious the middle part of the casting film tray is deformed and recessed, the deeper the casting film liquid in the middle part of the casting film tray is, the shallower the edge casting film liquid is, and the thicker the middle part of the casting film is, and the thinner the edge is.
Disclosure of Invention
Therefore, the technical problem to be solved by the invention is to provide a solution casting large film device and a solution casting large film method, which can make the thickness of the film more uniform.
In order to solve the problems, according to one aspect of the present invention, there is provided a solution casting large film apparatus comprising a casting plate, a heating portion, a heat-preserving water jacket and a height adjusting portion, wherein the casting plate is disposed in the middle of a bearing surface of the heating portion, the casting plate is used for disposing casting solution, and an effective casting area of the casting plate is 4-25m 2 The area of the bearing surface is 5-30m 2 The area of the bearing surface is larger than the effective casting area of the casting plate, the heat-insulating water-cooled jacket is sleeved on the heating part and the outer peripheral side of the casting plate, the height adjusting part is opposite to the middle part of the casting plate, at least one part of the height adjusting part is positioned between the casting plate and the heating part so as to jack the middle part of the casting plate up from the heating part, the height of the middle part of the casting plate is higher than the height of the edge of the casting plate, and the casting solution on the middle part of the casting plate flows out to one part of the edge of the casting plate in advance before film formation;
the height adjusting part comprises a first thread heightening assembly, the first thread heightening assembly comprises a first height adjusting screw, a first jacking sleeve and a second jacking sleeve, the center point of the casting film tray and the center point of the heating part in the horizontal direction are located on the axis line of the first height adjusting screw, the first jacking sleeve and the second jacking sleeve are connected with the first height adjusting screw through threads, the first jacking sleeve is located on one side, close to the casting film tray, of the second jacking sleeve, the first jacking sleeve penetrates through the heating part to jack up the casting film tray, and the second jacking sleeve is in butt joint with the first jacking sleeve to lock the first jacking sleeve.
Optionally, the height adjusting part includes a plurality of first shims, and the plurality of first shims are uniformly arranged along a circumferential direction of a central position of the casting plate and the heating part in a horizontal direction;
the thickness of the first gasket is 0.6-1.2mm, and the outer diameter of the first gasket is 6-12mm;
the top surface of the first gasket is an arc surface and protrudes in a direction away from the heating part;
the first gasket is made of at least one material selected from aluminum, red copper and polytetrafluoroethylene.
Optionally, the first pair of top sleeves is sleeved at the end part of the first height adjusting screw, which is close to one side of the casting film tray, and the first pair of top sleeves comprises a first cylinder top, the first cylinder top is positioned between the first height adjusting screw and the casting film tray, the outer diameter of the first cylinder top is 18-20mm, the outer wall of the first cylinder top, which faces one side of the casting film tray, is an arc surface, and protrudes towards the direction away from the heating part.
Optionally, the height adjusting part includes a plurality of second thread height adjusting components, the plurality of second thread height adjusting components are uniformly arranged along the circumference of the central positions of the casting film tray and the heating part in the horizontal direction, the second thread height adjusting components include a second height adjusting screw, a third pair of top sleeves and a fourth pair of top sleeves, the third pair of top sleeves and the fourth pair of top sleeves are connected to the second height adjusting screw through threads, the third pair of top sleeves are located on one side of the fourth pair of top sleeves close to the casting film tray, the third pair of top sleeves penetrate through the heating part to jack up the casting film tray, and the fourth pair of top sleeves are propped against the third pair of top sleeves to lock the third pair of top sleeves;
The third is to top sleeve cover is established the second is high to the end that the adjustment screw rod is close to casting film dish one side, the third is to top sleeve includes a second section of thick bamboo top, a second section of thick bamboo top is located between the adjustment screw rod of second height and the casting film dish, the external diameter of a second section of thick bamboo top is 18-20mm, a second section of thick bamboo top is the cambered surface towards the outer wall of casting film dish one side, and to keeping away from the direction protrusion of heating portion.
Optionally, the height of the second thread take-up assembly is less than the height of the first thread take-up assembly.
Optionally, the solution large film casting device further comprises a heat preservation bottom plate, a heat preservation top cover, leveling feet and a temperature control part;
the bottom end of the heat-preserving water-cooling jacket is arranged on the top surface of the heat-preserving bottom plate, the heat-preserving top cover is arranged on the top end of the heat-preserving water-cooling jacket, a heating space is defined by the heat-preserving top cover, the heat-preserving water-cooling jacket and the heat-preserving bottom plate, and the heating part and the casting film tray are arranged in the heating space;
the leveling feet are arranged on the bottom surface of the heat-insulating bottom plate so as to adjust the height and levelness of the heat-insulating bottom plate;
the temperature control part comprises a temperature controller and a temperature probe, the temperature probe is arranged on the edge of the casting film tray to detect the heating temperature, and the temperature probe and the heating part are respectively connected with the temperature controller;
The heat-preservation water-cooling jacket comprises a heat-preservation interlayer and a water-cooling interlayer, the water-cooling interlayer is sleeved on the periphery side of the casting film tray and the heating part, the heat-preservation interlayer is sleeved on the periphery side of the water-cooling interlayer, and the water-cooling interlayer faces the casting film tray and the periphery of the wall surface bottom edge on one side of the heating part is provided with an evaporation condensation solvent collecting tank of the casting film liquid.
In another aspect of the present application, there is provided a solution casting method for forming a film by the solution casting apparatus as described above, the solution casting method comprising the steps of:
placing the heating part in a heat-preservation water-cooling sleeve, so that the heat-preservation water-cooling sleeve is positioned at the outer periphery side of the heating part;
the height adjusting part is arranged in the middle of the bearing surface of the heating part, so that the height of the middle part of the casting film tray is higher than the height of the edge of the casting film tray;
placing a casting film tray on the bearing surfaces of the height adjusting part and the heating part, enabling the height adjusting part to be opposite to the middle part of the casting film tray, and enabling at least one part of the height adjusting part to be positioned between the casting film tray and the heating part, wherein the effective casting film area of the casting film tray is 4-25m 2 The area of the bearing surface is 5-30m 2 The area of the bearing surface is larger than the effective casting area of the casting disc;
pouring a casting solution into the casting plate;
and starting the heating part to heat the casting solution in the casting plate, so that the solvent of the casting solution is evaporated and condensed, and the solute is crystallized to form a film.
Optionally, before the step of placing the heating portion in the insulating water-cooled jacket so that the insulating water-cooled jacket is located on the outer peripheral side of the heating portion, the method further includes:
preparing the casting film liquid;
forming the casting film tray using a float glass plate, a float glass strip and a glass adhesive;
filling a heat-insulating rock wool board with a stainless steel plate interlayer to prepare a heat-insulating bottom board;
the height and levelness of the heat-insulating bottom plate are adjusted through leveling feet on the bottom surface of the heat-insulating bottom plate;
manufacturing a heat-insulating water cooling jacket with an inner stainless steel plate interlayer and an outer stainless steel plate interlayer along the edge of the heat-insulating bottom plate, filling heat-insulating rock wool plates in the outer stainless steel plate interlayer, filling cooling water in the inner stainless steel plate interlayer, and arranging an evaporation and condensation solvent collecting tank of the casting solution in the circumferential direction of the bottom edge of the inner wall of the inner stainless steel plate interlayer;
before the step of placing the height adjusting section in the middle of the carrying surface of the heating section, the method further comprises:
The heating part is arranged in the middle of the heat preservation bottom plate, wherein the heating part comprises a heating pipe rack and a toughened glass plate covered on the top of the heating pipe rack, and the heating pipe rack comprises a rectangular stainless steel hole rack and a plurality of far infrared quartz heating pipes which are inserted in the rectangular stainless steel hole rack and are arranged in parallel at equal intervals;
before the step of pouring the casting solution into the casting plate, the method further comprises:
the heating temperature of the heating part is controlled by a temperature controller, and the heating temperature is detected by a temperature measuring probe arranged on the edge of the casting film tray;
placing a leveling foot level instrument in the middle of the casting film tray, adjusting the height and levelness of the heat-preserving bottom plate through leveling feet on the bottom surface of the heat-preserving bottom plate, enabling the leveling bubble of the leveling foot level instrument to be in zero positions in two mutually perpendicular directions in the casting film tray, and locking the height of the leveling feet;
before the step of heating the casting solution in the casting tray by the start-up heating part to evaporate and condense the solvent of the casting solution, the method further comprises the steps of:
a heat-insulating top cover is arranged on the upper end cover of the heat-insulating water-cooling jacket, so that a heating space is surrounded by the heat-insulating top cover, the heat-insulating water-cooling jacket and the heat-insulating bottom plate, wherein a heat-insulating rock wool plate is filled in an interlayer of the heat-insulating top cover;
The step of heating the casting solution in the casting tray by the start-up heating part to evaporate and condense the solvent of the casting solution, and crystallizing the solute to form a film, comprising:
controlling the heating temperature to be 30-33 ℃ lower than the boiling point of the casting film liquid by the temperature controller;
the step of heating the casting solution in the casting tray by the start-up heating unit to evaporate and condense the solvent of the casting solution, and then crystallizing the solute to form a film, further comprises:
stopping heating;
extracting the gas and condensed solvent from the heating space;
lifting and cutting the film;
detecting and warehousing the film;
recovering the film corners and the condensed solvent.
Advantageous effects
The solution casting large film device and the solution casting large film method provided by the embodiment of the invention provide stable placement positions for casting film liquid by arranging the casting film tray. By arranging the height adjusting part and enabling the height adjusting part to comprise the first thread adjusting component, enabling the center point of the casting film tray and the heating part in the horizontal direction to be positioned on the axis line of the first height adjusting screw rod in the first thread adjusting component, enabling the first opposite sleeve in the first thread adjusting component to penetrate through the heating part to jack up the casting film tray, enabling the middle part of the casting film tray to jack up from the heating part, enabling the height of the middle part of the casting film tray to be higher than the height of the edge of the casting film tray, enabling the depth of casting film liquid on the middle part of the casting film tray to be shallow, enabling the depth of casting film liquid on the edge of the casting film tray to be deep, counteracting the influence of part of casting film liquid on the edge of the casting film tray on film thickness uniformity due to the fact that the casting film liquid on the middle part of the casting film tray is higher than the casting liquid on the edge, solvent evaporation is fast, solute crystallization fast, and the casting film crystallization fast flows into the middle part of the casting film tray, has the advantages of high crystallization degree, isotropy, uniform thickness, uniform finished product, simple structure, low cost, high efficiency, and the like, and can realize 10m of casting film, and can realize the production 2 The above ultra-large area film can be cast for example 10m 2 The super-large area perfluorinated ion exchange membrane lays a foundation for the application of the follow-up super-large area perfluorinated ion exchange membrane, for example, the super-large power full-vanadium redox flow battery pile of 1-10MW level is developed. Through setting up the second to the top sleeve, when needs locking first to the top sleeve, can twist the second to the top sleeve so that second to top sleeve and first to top sleeve looks butt, and then can lock first to top sleeve, guarantee to jack up the casting dish steadily.
Drawings
Fig. 1 is a schematic structural view of a first implementation of an embodiment of the present invention;
FIG. 2 is an enlarged view of FIG. 1 at A;
fig. 3 is a schematic perspective view of a casting plate and a height adjusting section according to a first embodiment of the present invention;
fig. 4 is a schematic perspective view of a casting plate and a height adjusting section according to a second embodiment of the present invention;
fig. 5 is a schematic perspective view of a casting plate and a height adjusting section according to a third embodiment of the present invention;
fig. 6 is a schematic perspective view of a casting plate and a height adjusting section according to a fourth embodiment of the present invention.
The reference numerals are expressed as:
1. A heat-preserving top cover; 2. casting film plate; 3. heating the pipe frame; 4. a heat preservation interlayer; 5. water-cooling the interlayer; 6. a far infrared quartz heating tube; 7. a heat-insulating bottom plate; 8. leveling the screw; 9. a sleeve; 10. a first leveling abutment sleeve; 11. a second leveling centering sleeve; 12. supporting feet; 13. tempered glass plate; 14. a first height adjustment screw; 15. a first pair of top sleeves; 16. a second pair of top sleeves; 17. a first gasket; 18. a second height adjustment screw; 19. and a third pair of top sleeves.
Detailed Description
In the description of the present invention, it should be understood that the terms "center", "longitudinal", "lateral", "length", "width", "thickness", "upper", "lower", "front", "rear", "left", "right", "vertical", "horizontal", "top", "bottom", "inner", "outer", "clockwise", "counterclockwise", etc. indicate orientations or positional relationships based on the orientations or positional relationships shown in the drawings are merely for convenience in describing the present invention and simplifying the description, and do not indicate or imply that the devices or elements referred to must have a specific orientation, be configured and operated in a specific orientation, and thus should not be construed as limiting the present invention.
Furthermore, the terms "first," "second," and the like, are used for descriptive purposes only and are not to be construed as indicating or implying a relative importance or implicitly indicating the number of technical features indicated. Thus, a feature defining "a first" or "a second" may explicitly or implicitly include one or more such feature. In the description of the present invention, the meaning of "a plurality" is two or more, unless explicitly defined otherwise.
In the present invention, unless explicitly specified and limited otherwise, the terms "mounted," "connected," "secured," and the like are to be construed broadly and may be, for example, fixedly connected, detachably connected, or integrally connected; can be mechanically or electrically connected; can be directly connected or indirectly connected through an intermediate medium, and can be communication between two elements. The specific meaning of the above terms in the present invention can be understood by those of ordinary skill in the art according to the specific circumstances.
The preferred embodiments of the present invention will be described below with reference to the accompanying drawings, it being understood that the preferred embodiments described herein are for illustration and explanation of the present invention only, and are not intended to limit the present invention.
Referring to fig. 1 to 3 in combination, according to an embodiment of the present invention, as a first embodiment, there is provided a solution casting large film apparatus comprising a casting plate 2, a heating portion, a heat-retaining water jacket, and a height adjusting portion, the casting plate 2 being disposed in the middle of a bearing surface of the heating portion, the casting plate 2 being for setting a casting solution, an effective casting area of the casting plate 2 being 4 to 25m 2 The area of the bearing surface is 5-30m 2 The area of the bearing surface is larger than the effective casting area of the casting film tray 2, the heat-insulating water-cooled jacket is sleeved on the outer peripheral sides of the heating part and the casting film tray 2, the height adjusting part is arranged opposite to the middle part of the casting film tray 2, and at least one part of the height adjusting part is positioned between the casting film tray 2 and the heating part so as to jack up the middle part of the casting film tray 2 from the heating part, so that casting film liquid on the middle part of the casting film tray 2 flows out of one part of the casting film tray 2 to the edge of the casting film tray 2 in advance before film formation.
The height adjustment part comprises a first thread heightening component, the first thread heightening component comprises a first height adjustment screw 14, a first jacking sleeve 15 and a second jacking sleeve 16, the center points of the casting film tray 2 and the heating part in the horizontal direction are located on the axis line of the first height adjustment screw 14, the first jacking sleeve 15 and the second jacking sleeve 16 are connected to the first height adjustment screw 14 through threads, the first jacking sleeve 15 is located on one side, close to the casting film tray 2, of the second jacking sleeve 16, the first jacking sleeve 15 penetrates through the heating part to jack up the casting film tray 2, and the second jacking sleeve 16 is abutted with the first jacking sleeve 15 to lock the first jacking sleeve 15.
By providing the casting plate 2, a stable placement position is provided for the casting solution. By providing the height adjusting part and making the height adjusting part include the first thread adjusting component, and making the center point of the casting film tray and the heating part in the horizontal direction be located on the axis of the first height adjusting screw in the first thread adjusting component, and the first centering sleeve in the first thread adjusting component passes through the heating part to jack up the casting film tray, the middle part of the casting film tray 2 can be jacked up from the heating part, the height of the middle part of the casting film tray 2 is made higher than the height of the edge of the casting film tray 2, the depth of the casting film liquid on the middle part of the casting film tray 2 is made shallow, and at the same time, the depth of the casting film liquid on the edge of the casting film tray 2 is made deeper, so as to offset the influence on the uniformity of film thickness caused by that the casting film liquid on the edge of the casting film tray 2 flows into a part of the casting film tray 2 due to the fast solvent evaporation, and crystallization, and the method has the advantages of high crystallization degree, isotropy, uniform thickness, high structure, low cost, and the like, and the cost of the casting film can be manufactured at 10m, and the like 2 The above ultra-large area film can be cast for example 10m 2 The super-large area perfluorinated ion exchange membrane lays a foundation for the application of the follow-up super-large area perfluorinated ion exchange membrane, for example, the super-large power vanadium redox flow battery pile development of 1-10MW level. By providing the second centering sleeve 16, when the first centering sleeve needs to be locked, the second centering sleeve 16 can be screwed so that the second centering sleeve 16 is abutted against the first centering sleeve 15, and the first centering sleeve 15 can be locked, thereby ensuring stable jacking of the casting plate 2.
The term "middle" does not refer to the center point alone, but refers to a certain range centered on the center point. In the art, taking a square-shaped casting plate 2 as an example, the "middle" area is a square-shaped area coaxial with the casting plate 2 and half the length of the casting plate 2.
In the art, the membrane area is larger than 1m 2 Namely, large film, the effective film casting area of the film casting disc 2 in the invention is 4-25m 2 The area of the bearing surface is 5-30m 2 The film cast by the solution large film casting device is the large film.
The perfluorinated ion exchange membrane prepared by the solution casting large membrane device and the method of the invention is mainly applied to flow batteries, fuel batteries, ion membrane electrolytic tanks and the like, but the solution casting large membrane device and the method of the invention are not limited to only prepare perfluorinated ion exchange membranes, and the prepared perfluorinated ion exchange membranes are not limited to only be applied to flow batteries, fuel batteries and ion membrane electrolytic tanks.
Wherein, the bottom of the casting film plate 2 can slightly deform and be raised under the action of the height adjusting part, so that the height adjusting part can jack up the middle part of the casting film plate 2 to form a convex hull, and the whole casting film plate 2 is not jacked up from the heating part and separated from the heating part.
Wherein the area of the bearing surface is larger than the effective casting area of the casting plate 2, so that the casting plate 2 can be integrally arranged on the bearing surface.
Wherein the bearing surface is horizontally arranged, so that the casting film tray 2 can be horizontally placed on the bearing surface.
Wherein the first height adjustment screw 14 is vertically disposed. The screw thread of the first height adjusting screw 14 is provided at least on the outer wall of the upper portion of the first height adjusting screw 14.
The first centering sleeve 15 and the second centering sleeve 16 are sleeved on the first height adjusting screw 14 and are in threaded connection with the first height adjusting screw 14, and the first centering sleeve 15 and the second centering sleeve 16 can move on the first height adjusting screw 14 along the axial direction of the first height adjusting screw 14 by screwing the first centering sleeve 15 and the second centering sleeve 16.
Specifically, by screwing the first pair of top sleeves 15, the first pair of top sleeves 15 is lifted up, and then passes upward through the heating portion to extend between the heating portion and the casting plate 2, and then the middle portion of the casting plate 2 is lifted up. By screwing the second pair of top sleeves 16, the second pair of top sleeves 16 is raised to abut against the bottom of the first pair of top sleeves 15, thereby locking the first pair of top sleeves 15 on the first height adjusting screw 14. Unlocking the first pair of top sleeves 15 from the first height adjustment screw 14 can be achieved by screwing the second pair of top sleeves 16, lowering the second pair of top sleeves 16. By screwing the first pair of top sleeves 15, the first pair of top sleeves 15 is lowered, and the first pair of top sleeves 15 can be caused to fall back down below the heating portion from between the heating portion and the casting plate 2, and the middle portion of the casting plate 2 can be caused to fall down due to the loss of support.
The first pair of top sleeves 15 are sleeved at the end part of the first height adjusting screw 14, which is close to one side of the casting film tray 2, the first pair of top sleeves 15 comprise first cylinder tops, the first cylinder tops are positioned between the first height adjusting screw 14 and the casting film tray 2, the outer diameter of the first cylinder tops is 18-20mm, the outer wall of the first cylinder tops, which faces one side of the casting film tray 2, is an arc surface, and protrudes towards a direction away from the heating part.
Wherein, set up the first section of thick bamboo top as the cambered surface, can prevent that the first section of thick bamboo from jack-up casting film dish 2 when causing the damage to casting film dish 2.
Wherein, the connection position between first section of thick bamboo top and the outer peripheral face is rounded off and is handled.
Wherein, the first section of thick bamboo top upwards bulge forms the cambered surface of evagination.
The solution casting large film device also comprises a heat-preserving water-cooling jacket, wherein the heat-preserving water-cooling jacket is sleeved on the heating part and the outer peripheral side of the casting film tray 2 so as to condense solvent vapor evaporated from the casting film liquid in the casting film tray 2 in the film forming process, so that the temperature of the casting film liquid at the edge of the casting film tray 2 is generally lower than that of the casting film liquid in the middle part of the casting film tray 2.
As a second embodiment, as shown in fig. 4, the height adjusting section includes a plurality of first shims 17, and the plurality of first shims 17 are uniformly arranged along the circumferential direction of the central position of the casting plate 2 and the heating section in the horizontal direction. That is, the plurality of first shims 17 are disposed together with the first thread adjusting member to form the height adjusting portion, the plurality of first shims 17 are disposed uniformly along the circumferential direction of the first thread adjusting member, and the height of the plurality of first shims 17 is lower than the height of the first thread adjusting member.
The height adjusting part comprises a first thread height adjusting component, the first thread height adjusting component comprises a first height adjusting screw 14, a first jacking sleeve 15 and a second jacking sleeve 16, the center points of the casting film tray 2 and the heating part in the horizontal direction are located on the axis of the first height adjusting screw 14, the first jacking sleeve 15 and the second jacking sleeve 16 are connected to the first height adjusting screw 14 through threads, the first jacking sleeve 15 is located on one side, close to the casting film tray 2, of the second jacking sleeve 16, the first jacking sleeve 15 penetrates through the heating part to jack up the casting film tray 2, and the second jacking sleeve 16 is abutted with the first jacking sleeve 15 to lock the first jacking sleeve 15.
The number of the first shims 17 may be four, and the four first shims 17 are uniformly arranged along the circumferential direction of the central position of the casting plate 2 and the heating portion in the horizontal direction.
The casting film tray 2 may be square, and four first gaskets 17 are correspondingly disposed on the angular lines of the four corners of the square of the casting film tray 2.
The casting film tray 2 may be rectangular, and four first gaskets 17 are correspondingly disposed on diagonal lines of the rectangle formed by the casting film tray 2.
Wherein, the distance between each first spacer 17 and the center of the casting plate 2 and the heating part in the horizontal direction is the same.
The thickness of the first gasket 17 is 0.6-1.2mm, and the outer diameter of the first gasket 17 is 6-12mm;
the top surface of the first gasket 17 is an arc surface and protrudes in a direction away from the heating part;
the first gasket 17 is made of at least one material selected from aluminum, red copper and polytetrafluoroethylene. That is, the first gasket 17 may be made of one of aluminum, red copper, and polytetrafluoroethylene, may be made of aluminum and red copper, may be made of aluminum and polytetrafluoroethylene, may be made of red copper and polytetrafluoroethylene, and may be made of aluminum, red copper, and polytetrafluoroethylene.
As a third embodiment, as shown in fig. 5, the height adjusting section includes a first screw-thread height adjusting member and a plurality of second screw-thread height adjusting members, the plurality of second screw-thread height adjusting members being uniformly arranged along the circumferential direction of the casting plate 2 and the first screw-thread height adjusting member, the height of the second screw-thread height adjusting members being smaller than the height of the first screw-thread height adjusting members;
the first thread height adjusting assembly comprises a first height adjusting screw 14, a first pair of jacking sleeves 15 and a second pair of jacking sleeves 16, wherein the center points of the casting film tray 2 and the heating part in the horizontal direction are positioned on the axis line of the first height adjusting screw 14, the first pair of jacking sleeves 15 and the second pair of jacking sleeves 16 are connected to the first height adjusting screw 14 through threads, the first pair of jacking sleeves 15 are positioned on one side of the second pair of jacking sleeves 16 close to the casting film tray 2, the first pair of jacking sleeves 15 penetrate through the heating part to jack the casting film tray 2, and the second pair of jacking sleeves 16 are abutted with the first pair of jacking sleeves 15 to lock the first pair of jacking sleeves 15;
The second thread height adjusting assembly comprises a second height adjusting screw 18, a third jacking sleeve 19 and a fourth jacking sleeve, the third jacking sleeve 19 and the fourth jacking sleeve are connected to the second height adjusting screw 18 through threads, the third jacking sleeve 19 is positioned on one side of the fourth jacking sleeve, which is close to the casting disc 2, the third jacking sleeve 19 penetrates through the heating part to jack up the casting disc 2, and the fourth jacking sleeve is abutted against the third jacking sleeve 19 to lock the third jacking sleeve 19;
the height of the second thread heightening component is smaller than that of the first thread heightening component, so that the height of the first thread heightening component for jacking up the casting film tray 2 is higher than that of the second thread heightening component for jacking up the casting film tray 2.
Wherein the first height adjustment screw 14 is vertically disposed. The screw thread of the first height adjusting screw 14 is provided at least on the outer wall of the upper portion of the first height adjusting screw 14.
The first centering sleeve 15 and the second centering sleeve 16 are sleeved on the first height adjusting screw 14 and are in threaded connection with the first height adjusting screw 14, and the first centering sleeve 15 and the second centering sleeve 16 can move on the first height adjusting screw 14 along the axial direction of the first height adjusting screw 14 by screwing the first centering sleeve 15 and the second centering sleeve 16.
Specifically, by screwing the first pair of top sleeves 15, the first pair of top sleeves 15 is lifted up, and then passes upward through the heating portion to extend between the heating portion and the casting plate 2, and then the middle portion of the casting plate 2 is lifted up. By screwing the second pair of top sleeves 16, the second pair of top sleeves 16 is raised to abut against the bottom of the first pair of top sleeves 15, thereby locking the first pair of top sleeves 15 on the first height adjusting screw 14. Unlocking the first pair of top sleeves 15 from the first height adjustment screw 14 can be achieved by screwing the second pair of top sleeves 16, lowering the second pair of top sleeves 16. By screwing the first pair of top sleeves 15, the first pair of top sleeves 15 is lowered, and the first pair of top sleeves 15 can be caused to fall back down below the heating portion from between the heating portion and the casting plate 2, and the middle portion of the casting plate 2 can be caused to fall down due to the loss of support.
The number of the second screw thread height adjusting components may be four, and the four second screw thread height adjusting components are uniformly arranged along the circumference of the central position of the casting film tray 2 and the heating part in the horizontal direction.
The casting film tray 2 may be square, and the four second thread height adjusting components are correspondingly arranged on the angular lines of the four corners of the square of the casting film tray 2.
The casting film tray 2 may be rectangular, and the four second thread height adjusting components are correspondingly disposed on diagonal lines of the rectangle formed by the casting film tray 2.
Wherein, each second screw height adjusting assembly is the same as the distance between the casting plate 2 and the center of the heating part in the horizontal direction.
Wherein the second height adjustment screw 18 is vertically disposed. The threads on the second height adjustment screw 18 are provided at least on the outer wall of the upper portion of the second height adjustment screw 18.
The third top sleeve 19 and the fourth top sleeve are sleeved on the second height adjusting screw 18 and are in threaded connection with the second height adjusting screw 18, and the third top sleeve 19 and the fourth top sleeve can move on the second height adjusting screw 18 along the axial direction of the second height adjusting screw 18 by screwing the third top sleeve 19 and the fourth top sleeve.
Specifically, by screwing the third pair of top sleeves 19, the third pair of top sleeves 19 is lifted up, and then passes upward through the heating portion to extend between the heating portion and the casting plate 2, and then the middle portion of the casting plate 2 is lifted up. By screwing the fourth counter sleeve, the fourth counter sleeve is raised to abut against the bottom of the third counter sleeve 19, thereby locking the third counter sleeve 19 on the second height adjusting screw 18. Unlocking the third set of top sleeves 19 from the second height adjustment screw 18 is achieved by screwing the fourth set of top sleeves, lowering the fourth set of top sleeves. By screwing the third counter sleeve 19, the third counter sleeve 19 is lowered, and the third counter sleeve 19 can be moved back from between the heating portion and the casting plate 2 to below the heating portion, and the middle portion of the casting plate 2 can be moved down due to the loss of support.
The first pair of jacking sleeves 15 are sleeved at the end part of the first height adjusting screw 14, which is close to one side of the casting film tray 2, the first pair of jacking sleeves 15 comprise first cylinder tops, the first cylinder tops are positioned between the first height adjusting screw 14 and the casting film tray 2, the third pair of jacking sleeves 19 are sleeved at the end part of the second height adjusting screw 18, which is close to one side of the casting film tray 2, the third pair of jacking sleeves 19 comprise second cylinder tops, the second cylinder tops are positioned between the second height adjusting screw 18 and the casting film tray 2, the outer diameters of the first cylinder tops and the second cylinder tops are 18-20mm, the outer walls of the first cylinder tops and the second cylinder tops, which face one side of the casting film tray 2, are cambered surfaces, and protrude towards a direction away from the heating part.
Wherein, set up first section of thick bamboo top and second section of thick bamboo top as the cambered surface, can prevent that first section of thick bamboo top and second section of thick bamboo top from jack-up casting dish 2 when causing the damage to casting dish 2.
Wherein, the connection position between the first cylinder top and the second cylinder top and the peripheral surface is rounded.
Wherein, first section of thick bamboo top and second section of thick bamboo top upwards bulge forms the cambered surface of evagination.
As a fourth embodiment, as shown in fig. 6, the height adjusting section includes a plurality of first shims 17, a first screw-thread height adjusting assembly, and a plurality of second screw-thread height adjusting assemblies. Wherein, a plurality of first gaskets 17 and a plurality of second screw thread heightening subassembly are evenly set up along the circumference of first screw thread heightening subassembly, and a plurality of first gaskets 17 can set up in a plurality of second screw thread heightening subassembly one side of keeping away from first screw thread heightening subassembly, and the height of first gasket 17 is less than the height of second screw thread heightening subassembly, and the height of second screw thread heightening subassembly is less than the height of first screw thread heightening subassembly.
The height adjusting part comprises a first thread height adjusting component, the first thread height adjusting component comprises a first height adjusting screw 14, a first jacking sleeve 15 and a second jacking sleeve 16, the center points of the casting film tray 2 and the heating part in the horizontal direction are located on the axis of the first height adjusting screw 14, the first jacking sleeve 15 and the second jacking sleeve 16 are connected to the first height adjusting screw 14 through threads, the first jacking sleeve 15 is located on one side, close to the casting film tray 2, of the second jacking sleeve 16, the first jacking sleeve 15 penetrates through the heating part to jack up the casting film tray 2, and the second jacking sleeve 16 is abutted with the first jacking sleeve 15 to lock the first jacking sleeve 15.
The number of the first gaskets 17 is the same as that of the second thread heightening assemblies, the first gaskets 17, the second thread heightening assemblies and the first thread heightening assemblies which are correspondingly arranged are arranged in a one-to-one correspondence mode and are positioned on the same straight line.
The solution large film casting device also comprises a heat preservation bottom plate 7, a heat preservation top cover 1, leveling feet and a temperature control part;
the bottom end of the heat-preserving water-cooling jacket is arranged on the top surface of the heat-preserving bottom plate 7, the heat-preserving top cover 1 is arranged on the top end of the heat-preserving water-cooling jacket in a covering mode, a heating space is defined by the heat-preserving top cover 1, the heat-preserving water-cooling jacket and the heat-preserving bottom plate 7, and the heating part and the casting film plate 2 are arranged in the heating space;
The leveling feet are arranged on the bottom surface of the heat-insulating bottom plate 7 to adjust the height and levelness of the heat-insulating bottom plate 7;
the temperature control part comprises a temperature controller and a temperature measuring probe, the temperature measuring probe is arranged on the edge of the casting film tray 2 to detect the heating temperature, and the temperature measuring probe and the heating part are respectively connected with the temperature controller;
the heat preservation water cooling jacket comprises a heat preservation interlayer 4 and a water cooling interlayer 5, the water cooling interlayer 5 is sleeved on the periphery of the casting film tray 2 and the heating part, the heat preservation interlayer 4 is sleeved on the periphery of the water cooling interlayer 5, and the water cooling interlayer 5 faces the casting film tray 2 and the periphery of the wall surface bottom edge on one side of the heating part is provided with an evaporation condensation solvent collecting tank of casting film liquid. Through setting up heat preservation bottom plate 7, when providing the position of placing for the heating portion, can also enclose into sealed heating space with heat preservation top cap 1, heat preservation water jacket and heat preservation bottom plate 7, realize the heat preservation function, avoid the heat to scatter and disappear, also guaranteed heating temperature's stability simultaneously. Through setting up leveling lower margin, can adjust heat preservation bottom plate 7, heating portion and casting dish 2 to horizontal position to guarantee the thickness homogeneity of the cast film in different orientation. The temperature control part is arranged to detect the actual temperature and accurately control the heating temperature according to the detected actual temperature. Through set up the evaporation condensation solvent collecting vat of casting film liquid at the water-cooling intermediate layer 5 circumference along, can retrieve the solvent of condensation, when avoiding the solvent to influence the casting film, can also realize the reuse of solvent, reduction in production cost, environmental protection.
The heat-insulating water-cooling jacket comprises a heat-insulating interlayer 4 and a water-cooling interlayer 5, the heat-insulating interlayer 4 and the water-cooling interlayer 5 are of cylindrical structures, the water-cooling interlayer 5 is arranged on the periphery side of the casting film plate 2 and the heating part, and the heat-insulating interlayer 4 is sleeved on the periphery side of the water-cooling interlayer 5. I.e. the water-cooled interlayer 5 is located at the inner side and the heat-insulating interlayer 4 is located at the outer side.
Wherein, the evaporation and condensation solvent collecting tank of the casting solution is arranged at the bottom edge of the wall surface of the water-cooling interlayer 5 facing the casting plate 2 and the heating part.
Wherein, heating portion includes heating pipe support 3 and far infrared quartz heating pipe 6, and casting film dish 2 sets up on the top surface of heating pipe support 3, and far infrared quartz heating pipe 6 is connected with the lateral wall of heating pipe support 3, and heating pipe support 3 is when providing fixed position for far infrared quartz heating pipe 6, and the heat that far infrared quartz heating pipe 6 produced also can evenly transmit to casting film dish 2 through heating pipe support 3.
Specifically, the top surface of the heating pipe frame 3 is the bearing surface of the heating part, and the area is 5-30m 2 Between them.
Specifically, the heating pipe rack 3 comprises a rack body and a toughened glass plate 13 covered on the rack body, and a plurality of far infrared quartz heating pipes 6 are inserted on the rack body.
Wherein, the heating portion sets up on the central point of the top of heat preservation bottom plate 7, and casting film dish 2 sets up on the central point of heating pipe support 3 top surface. Namely, the heat-insulating base plate 7, the heating tube stand 3 and the casting plate 2 are coaxially arranged.
The number of the leveling feet is multiple, and the leveling feet are uniformly arranged on the bottom surface of the heat preservation bottom plate 7 along the circumferential direction of the heat preservation bottom plate 7.
The leveling foundation comprises a leveling screw rod 8, a first leveling opposite-top sleeve 10 and a second leveling opposite-top sleeve 11, the first leveling opposite-top sleeve 10 is located above the second leveling opposite-top sleeve 11, the leveling screw rod 8 is vertically arranged, the first leveling opposite-top sleeve 10 and the second leveling opposite-top sleeve 11 are arranged on the leveling screw rod 8 through threads, the length of a single leveling foundation can be adjusted through screwing the first leveling opposite-top sleeve 10, and further the leveling of the solution casting large film device can be achieved through adjusting a plurality of leveling foundation. The first leveling abutment sleeve 10 can be locked by screwing the second leveling abutment sleeve 11 into abutment with the first leveling abutment sleeve 10.
Wherein, the temperature probe is arranged on the edge of the casting film tray 2.
The temperature measuring probe sends the obtained actual temperature to the temperature controller, the temperature controller compares the actual temperature with a preset temperature, and when the actual temperature is lower than the preset temperature, the heating part is controlled to increase the power, so that the heating temperature is increased. When the actual temperature is higher than the preset temperature, the heating part is controlled to reduce the power, so that the heating temperature is reduced.
In another aspect of the present invention, there is provided a solution casting method for producing a film by the solution casting apparatus as described above, the solution casting method comprising the steps of:
step 1: preparing a casting film liquid;
step 2: the casting disc 2 is made using a float glass plate, a float glass strip and a glass adhesive;
step 3: preparing a heat-insulating bottom plate 7 by filling a heat-insulating rock wool board with a stainless steel plate interlayer;
step 4: the height and levelness of the heat-insulating bottom plate 7 are adjusted through leveling feet on the bottom surface of the heat-insulating bottom plate 7;
step 5: manufacturing a heat-insulating water-cooled jacket with an inner stainless steel plate interlayer and an outer stainless steel plate interlayer along the edge of the heat-insulating bottom plate 7, filling heat-insulating rock wool plates in the outer stainless steel plate interlayer, filling cooling water in the inner stainless steel plate interlayer, and arranging an evaporation and condensation solvent collecting tank of casting solution in the circumferential direction of the bottom edge of the inner wall of the inner stainless steel plate interlayer;
step 6: placing the heating part in a heat-preservation water-cooling sleeve, so that the heat-preservation water-cooling sleeve is positioned at the periphery side of the heating part;
step 7: the heating part is arranged in the middle of the heat preservation bottom plate 7, wherein the heating part comprises a heating pipe rack and a toughened glass plate 13 covered on the top of the heating pipe rack, the heating pipe rack comprises a rectangular stainless steel hole rack and a plurality of far infrared quartz heating pipes 6 which are inserted in the rectangular stainless steel hole rack and are arranged in parallel at equal intervals;
Step 8: placing the height adjusting part in the middle of the bearing surface of the heating part; the height adjusting part comprises a first thread height adjusting component, the first thread height adjusting component comprises a first height adjusting screw 14, a first jacking sleeve 15 and a second jacking sleeve 16, the center points of the casting film tray 2 and the heating part in the horizontal direction are located on the axis of the first height adjusting screw 14, the first jacking sleeve 15 and the second jacking sleeve 16 are connected to the first height adjusting screw 14 through threads, the first jacking sleeve 15 is located on one side, close to the casting film tray 2, of the second jacking sleeve 16, the first jacking sleeve 15 penetrates through the heating part to jack up the casting film tray 2, and the second jacking sleeve 16 is abutted with the first jacking sleeve 15 to lock the first jacking sleeve 15.
Step 9: placing the casting film tray 2 on the bearing surfaces of the height adjusting part and the heating part, enabling the height adjusting part to be opposite to the middle part of the casting film tray 2, and enabling at least one part of the height adjusting part to be positioned between the casting film tray 2 and the heating part, wherein the effective casting film area of the casting film tray 2 is 4-25m 2 The area of the bearing surface is 5-30m 2 The area of the bearing surface is larger than the effective casting area of the casting disc 2;
step 10: the heating temperature of the heating part is controlled by a temperature controller, and the heating temperature is detected by a temperature measuring probe arranged on the edge of the casting film tray 2;
Step 11: placing a leveling foot level gauge in the middle of the casting film tray 2, adjusting the height and levelness of the heat-preserving bottom plate 7 through leveling feet on the bottom surface of the heat-preserving bottom plate 7, enabling the level bubble of the leveling foot level gauge to be in zero positions in two mutually perpendicular directions in the casting film tray 2, and locking the height of the leveling feet;
step 12: pouring the casting solution into a casting disc 2;
step 13: the upper end cover of the heat-insulating water-cooled jacket is provided with a heat-insulating top cover 1, so that the heat-insulating top cover 1, the heat-insulating water-cooled jacket and a heat-insulating bottom plate 7 enclose a heating space, wherein a heat-insulating rock wool board is filled in an interlayer of the heat-insulating top cover 1;
step 14: and starting a heating part to heat the casting film liquid in the casting film tray 2, controlling the heating temperature to be lower than the boiling point of the casting film liquid by a temperature controller to be 30-33 ℃, evaporating and condensing the solvent in the casting film liquid, and crystallizing the solute to form a film.
Step 15: stopping heating, extracting gas and condensed solvent in the heating space, lifting and cutting the film, detecting the film and warehousing; wherein, the qualified film enters a good product warehouse, and the unqualified film enters a bad product warehouse.
Step 16: recovering the film corner and the condensed solvent for circularly preparing the film casting solution.
Example 1
As shown in fig. 1-2, this example 1 is a 2m×2m× 0.05mm perfluorinated ion exchange membrane, comprising the steps of:
1) 0.5kg of perfluorosulfonic acid ion exchange resin (equivalent weight EW=1000 g/eq, density 2.0 g/cm) 3 ) And 10L of dimethylformamide (boiling point 153 ℃ C., density 0.95 g/cm) 3 ) Adding 15L of closed reaction kettle, heating, stirring and dissolving, wherein the dissolving temperature is 200 ℃, and the dissolving time is 4 hours, so that the perfluorinated sulfonic acid ion exchange resin is dissolved in dimethylformamide to prepare about 10L of casting solution with the concentration of 5 wt%;
2) A casting tray 2 having an area of 2.2mX2.2m, a height of 2cm, a depth of 1cm, a tray edge width of 5cm, an inner bottom area of 2.1mX2.1m, and an effective casting area of 2 mX2 m was prepared by using a 10mm float glass plate, a float glass ribbon, and a glass adhesive;
3) Filling a heat-insulating rock wool board with a 1mm stainless steel plate interlayer to prepare a heat-insulating bottom board 7 with the thickness of 3m multiplied by 10 cm;
4) Leveling feet with the height of 10cm are respectively arranged at four corners of the bottom surface of the heat preservation bottom plate 7, each leveling foot comprises a leveling screw rod 8, the upper part of each leveling screw rod 8 extends into the corresponding sleeve 9, the middle part of each leveling screw rod 8 is connected with a first leveling opposite-top sleeve 10 and a second leveling opposite-top sleeve 11 in a screwed mode, supporting feet 12 are fixed at the bottom of each leveling screw rod 8, and the top of each sleeve 9 is fixed on the bottom surface of the heat preservation bottom plate 7. The first leveling opposite-top sleeve 10 is rotated to raise and lower the height of the leveling foot margin, and the second leveling opposite-top sleeve 11 is rotated upwards to be in contact with the first leveling opposite-top sleeve 10, so that the height of the leveling foot margin can be locked;
5) And a heat-insulating water-cooling sleeve with the thickness of 3m multiplied by 0.7m is arranged along the edge of the heat-insulating bottom plate 7 in a circle, and is provided with two stainless steel plate interlayers with the thickness of 10cm and 1mm, wherein the heat-insulating rock wool plates are filled in the stainless steel plate heat-insulating interlayers 4 on the outer side to form the heat-insulating interlayer 4. The inner side of the stainless steel plate water-cooling interlayer 5 is filled with 35cm high cooling water to form the water-cooling interlayer 5. The water-cooling interlayer 5 is arranged around the casting film tray 2 and the heating part towards the bottom of the wall surface at one side of the casting film tray 2 and the heating part, and a casting film liquid evaporation condensation solvent collecting tank with the perimeter of 10.2m multiplied by 5cm multiplied by 10cm in depth is arranged;
6) A heating pipe frame 3 with the area of 2.4mX2.4mX30 cm is arranged on the heat preservation bottom plate 7 in the middle, the heating pipe frame 3 is formed by covering a toughened glass plate 13 with the area of 2.4mX2.4mX2 cm on a frame body, the frame body is formed by inserting 48 far infrared quartz heating pipes 6 which are 2.4m long, 220V in voltage and 300W in parallel equidistant arrangement and have the power density of 0.25W/cm into a rectangular stainless steel hole frame with the area of 2.4mX2.4mX2.4mX28 cm, the heating pipes are 5cm away from the heat preservation bottom plate, and the power density of the heating pipe frame 3 is 0.25W/cm 2 Heating power is 14.4kW;
7) A first height adjusting screw 14 is arranged centrally below the casting film plate 2, the first height adjusting screw 14 is an M12 stainless steel first height adjusting screw 14 with the height of 29.5cm, and two M12 internally threaded stainless steel opposite-top sleeves with the height of 2cm and the outer diameter of 19mm, namely a first opposite-top sleeve 15 and a second opposite-top sleeve 16 are connected to the upper part of the first height adjusting screw 14 in a threaded manner. The top edges of the first pair of top sleeves 15 are rounded, the tops of the first pair of top sleeves 15 are supported at the center of the lower bottom surface of the casting film tray 2, the first height adjusting screw 14 vertically passes through a through hole with the diameter of 22mm in the center of the heating pipe rack 3 and then is welded at the center of the heat insulation bottom plate 7, the first pair of top sleeves 15 are rotated to slightly adjust the height to 30.6cm and to be 0.6cm higher than the heating pipe rack, and the second pair of top sleeves 16 are rotated upwards to lock the height of the first height adjusting screw 14;
8) The casting film tray 2 is placed on the first height adjusting screw 14 and the heating pipe rack 3 in the middle;
9) The heating pipe frame 3 is controlled to heat by a temperature controller, and a temperature measuring probe is arranged on the edge of the casting film tray 2 to detect the actual temperature;
10 The leveling instrument with equal-height support legs is arranged in the casting film tray 2 in the middle, the heights of four leveling feet are adjusted, so that the leveling bubble of the leveling instrument is positioned in zero positions in two mutually perpendicular directions in the casting film tray 2, the casting film tray 2 is positioned horizontally, and the heights of the leveling feet are locked;
11 8.82L of 5wt% casting solution was poured into a casting plate 2 having an inner bottom area of 2.1 m.times.2.1 m, an average depth of the casting solution of 2mm, a center depth of about 1.4mm, and an edge depth of >2mm;
12 A 3m multiplied by 10cm heat-preserving top cover 1 is arranged at the upper end of the heat-preserving water-cooling jacket, the heat-preserving top cover 1 is prepared by filling a heat-preserving rock wool board with a 1mm stainless steel board interlayer, and a sealed heating space is enclosed by the heat-preserving top cover 1, the heat-preserving water-cooling jacket and a heat-preserving bottom board 7;
13 Starting the heating pipe frame 3 to heat the casting solution in the casting plate 2, controlling the heating temperature to be 123 ℃ and 30 ℃ below the boiling point of the solvent, and heating for about 1.5 hours to enable the solvent in the casting solution to be completely evaporated. In the solvent evaporation process, the casting film tray 2 and the casting film liquid therein are in a static closed space, the solvent saturated vapor evaporated diffuses and covers the casting film liquid to the periphery under the heating of the heating pipe rack 3, the solvent saturated vapor which diffuses far contacts the water-cooling interlayer 5 of the heat-preservation water-cooling jacket, the solvent is cooled and condensed on the surface of the water-cooling interlayer 5 to form a liquid solvent, and under the action of gravity, the solvent flows down along the surface of the water-cooling interlayer 5 and is converged into the evaporation and condensation solvent collecting tank of the casting film liquid at the bottom, and the concentration of solute gradually increases along with gradual evaporation and reduction of the solvent in the casting film liquid, so that crystallization and film formation are realized;
Under the action of upward pressure of the first pair of top sleeves 15 and downward gravity of the first pair of top sleeves, the middle part of the film casting disc 2 slightly deforms and protrudes, the edge slightly deforms and sags, so that part of film casting liquid in the middle part of the film casting disc 2 flows out to the edge of the film casting disc 2 in advance before film formation, the film casting liquid in the middle part of the film casting disc 2 is shallower, the edge of the film casting disc 2 is deeper, but the periphery of the film casting disc 2 is provided with a heat-insulating water jacket for cooling and condensing solvent vapor in the film casting liquid, so that the temperature of the film casting liquid in the edge of the film casting disc 2 is lower, the film forming speed of solvent evaporation and solute crystallization is slower, the temperature of the film casting liquid in the middle part is higher, and the solvent evaporation and solute crystallization film formation are faster, and part of the film casting liquid in the middle part of the edge of the film casting disc 2 flows into the middle part of the film casting disc 2, so that the defect that the film casting liquid in the middle part of the film casting disc 2 is shallower is offset is overcome, and the thickness of the middle part and the edge of the film is basically consistent;
14 Stopping heating, extracting the condensed solvent in the evaporation and condensation solvent collecting tank of the casting solution, removing the film from the casting film tray 2 after the casting film tray 2 is cooled, and cutting off 5cm film corners to obtain a finished product of the perfluorinated ion exchange membrane with the thickness error of 2m multiplied by 0.05mm, wherein the thickness error of the film is less than or equal to 0.003mm;
15 Recovering the film corners and condensing solvent for recycling preparation of the casting solution.
Example 2
The example is a 3m x 0.05mm perfluorinated ion exchange membrane, comprising the steps of:
1) 1kg of perfluorosulfonic acid ion exchange resin (equivalent weight EW=1000 g/eq, density 2.0 g/cm) 3 ) And 20L of dimethylformamide (boiling point 153 ℃ C., density 0.95 g/cm) 3 ) Adding 30L of closed reaction kettle, heating, stirring and dissolving, wherein the dissolving temperature is 200 ℃, and the dissolving time is 4 hours, so that the perfluorinated sulfonic acid ion exchange resin is dissolved in dimethylformamide to prepare about 20L of casting solution with the concentration of 5 wt%;
2) A casting tray 2 with a float glass plate of 10mm, a float glass ribbon and a glass adhesive preparation area of 3.2mX3.2 m, a height of 2cm, a depth of 1cm, a tray edge width of 5cm, an inner bottom area of 3.1mX3.1m, and an effective casting area of 3 mX3 m;
3) Filling a heat-insulating rock wool board with a 1mm stainless steel plate interlayer to prepare a 4m multiplied by 10cm heat-insulating bottom plate 7;
4) Leveling feet with the height of 10cm are respectively arranged at four corners of the bottom surface of the heat preservation bottom plate 7, each leveling foot comprises a leveling screw rod 8, the upper part of each leveling screw rod 8 extends into the corresponding sleeve 9, the middle part of each leveling screw rod 8 is connected with a first leveling opposite-top sleeve 10 and a second leveling opposite-top sleeve 11 in a screwed mode, supporting feet 12 are fixed at the bottom of each leveling screw rod 8, and the top of each sleeve 9 is fixed on the bottom surface of the heat preservation bottom plate 7. The first leveling opposite-top sleeve 10 is rotated to raise and lower the height of the leveling foot margin, and the second leveling opposite-top sleeve 11 is rotated upwards to be in contact with the first leveling opposite-top sleeve 10, so that the height of the leveling foot margin can be locked;
5) A4 m multiplied by 0.7m heat-preserving water-cooling jacket is arranged along the edge of the heat-preserving bottom plate 7 upwards in a circle, the heat-preserving water-cooling jacket is provided with two stainless steel plate interlayers with the thickness of 10cm and 1mm, wherein the heat-preserving rock wool plates are filled in the stainless steel plate heat-preserving interlayers 4 on the outer side, and the heat-preserving interlayers 4 are formed. The inner side of the stainless steel plate water-cooling interlayer 5 is filled with 35cm high cooling water to form a water-cooling clamp. The water-cooling interlayer 5 is arranged around the casting film tray 2 and the heating part towards the bottom of the wall surface at one side of the casting film tray 2 and the heating part, and a circle of evaporation and condensation solvent collecting tank of casting film liquid with the perimeter of 14.2m multiplied by 5cm multiplied by 10cm in depth is arranged;
6) A heating pipe frame 3 with the area of 3.4m multiplied by 30cm is centrally arranged on the heat preservation bottom plate 7, the heating pipe frame 3 is formed by covering a toughened glass plate 13 with the area of 3.4m multiplied by 2cm on a frame body, the frame body is formed by inserting 70 far infrared quartz heating pipes 6 which are 3.4m long, 220V in voltage and 400W in power parallel and equidistant arrangement into a rectangular stainless steel hole frame with the area of 3.4m multiplied by 28cm, the distance between the heating pipes is 5cm from the heat preservation bottom plate, and the power density of the heating pipe frame 3 is 0.24W/cm 2 Heating power is 28kW;
7) A first height adjusting screw 14 is arranged centrally below the casting film plate 2, the first height adjusting screw 14 is an M12 stainless steel first height adjusting screw 14 with the height of 29.5cm, and two M12 internally threaded stainless steel opposite-top sleeves with the height of 2cm and the outer diameter of 19mm, namely a first opposite-top sleeve 15 and a second opposite-top sleeve 16 are connected to the upper part of the first height adjusting screw 14 in a threaded manner. The top edges of the first pair of top sleeves 15 are rounded, the tops of the first pair of top sleeves 15 are supported at the center of the lower bottom surface of the casting film tray 2, the first height adjusting screw 14 vertically passes through a through hole with the diameter of 22mm in the center of the heating pipe rack 3 and then is welded at the center of the heat insulation bottom plate 7, the first pair of top sleeves 15 are rotated to slightly adjust the height to 30.8cm and 0.8cm higher than the heating pipe rack, and the second pair of top sleeves 16 are rotated upwards to lock the height of the first height adjusting screw 14;
8) The casting film tray 2 is placed on the first height adjusting screw 14 and the heating pipe rack 3 in the middle;
9) The heating pipe frame 3 is controlled to heat by a temperature controller, and a temperature measuring probe is arranged on the edge of the casting film tray 2 to detect the actual temperature;
10 The leveling instrument with equal-height support legs is arranged in the casting film tray 2 in the middle, the heights of four leveling feet are adjusted, so that the leveling bubble of the leveling instrument is positioned in zero positions in two mutually perpendicular directions in the casting film tray 2, the casting film tray 2 is positioned horizontally, and the heights of the leveling feet are locked;
11 19.22L of 5wt% casting solution was poured into a casting plate 2 having an inner bottom area of 3.1mX3.1 m, an average depth of the casting solution of 2mm, a center depth of about 1.2mm, and an edge depth of >2mm;
12 A 4m multiplied by 10cm heat-preserving top cover 1 is arranged at the upper end of the heat-preserving water-cooling jacket, the heat-preserving top cover 1 is prepared by filling a heat-preserving rock wool board with a 1mm stainless steel plate interlayer, and a sealed heating space is enclosed by the heat-preserving top cover 1, the heat-preserving water-cooling jacket and a heat-preserving bottom plate 7;
13 Starting the heating pipe frame 3 to heat the casting solution in the casting plate 2, controlling the heating temperature to 122 ℃ and lower than the boiling point of the solvent to 31 ℃ for about 1.5 hours, and completely evaporating the solvent in the casting solution. In the solvent evaporation process, the casting film tray 2 and the casting film liquid therein are in a static closed space, the solvent saturated vapor evaporated diffuses and covers the casting film liquid to the periphery under the heating of the heating pipe rack 3, the solvent saturated vapor which diffuses far contacts the water-cooling interlayer 5 of the heat-preservation water-cooling jacket, the solvent is cooled and condensed on the surface of the water-cooling interlayer 5 to form a liquid solvent, and under the action of gravity, the solvent flows down along the surface of the water-cooling interlayer 5 and is converged into the evaporation and condensation solvent collecting tank of the casting film liquid at the bottom, and the concentration of solute gradually increases along with gradual evaporation and reduction of the solvent in the casting film liquid, so that crystallization and film formation are realized;
Under the action of upward pressure of the first pair of top sleeves 15 and downward gravity of the first pair of top sleeves, the middle part of the film casting disc 2 slightly deforms and protrudes, the edge slightly deforms and sags, so that part of film casting liquid in the middle part of the film casting disc 2 flows out to the edge of the film casting disc 2 in advance before film formation, the film casting liquid in the middle part of the film casting disc 2 is shallower, the edge of the film casting disc 2 is deeper, but the periphery of the film casting disc 2 is provided with a heat-insulating water jacket for cooling and condensing solvent vapor in the film casting liquid, so that the temperature of the film casting liquid in the edge of the film casting disc 2 is lower, the film forming speed of solvent evaporation and solute crystallization is slower, the temperature of the film casting liquid in the middle part is higher, and the solvent evaporation and solute crystallization film formation are faster, and part of the film casting liquid in the middle part of the edge of the film casting disc 2 flows to the middle part of the film casting disc 2, so that the defect that the film casting liquid in the middle part of the film casting disc 2 is shallower is offset is overcome, and the thickness of the middle part and the edge of the film is basically consistent;
14 Stopping heating, extracting the condensed solvent in the evaporation and condensation solvent collecting tank of the casting solution, removing the film from the casting film tray 2 after the casting film tray 2 is cooled, and cutting off 5cm film corners to obtain a 3m multiplied by 0.05mm perfluorinated ion exchange membrane finished product, wherein the film thickness error is less than or equal to 0.003mm;
15 Recovering the film corners and condensing solvent for recycling preparation of the casting solution.
Example 3
The example is a 4m x 0.075mm perfluorinated ion exchange membrane comprising the steps of:
1) 3kg of perfluorosulfonic acid ion exchange resin (equivalent weight EW=1000 g/eq, density 2.0 g/cm) 3 ) And 60L dimethylformamide (boiling point 153 ℃ C., density 0.95 g/cm) 3 ) Adding 90L of closed reaction kettle, heating, stirring and dissolving, wherein the dissolving temperature is 200 ℃, and the dissolving time is 4 hours, so that the perfluorinated sulfonic acid ion exchange resin is dissolved in dimethylformamide to prepare about 60L of casting solution with the concentration of 5 wt%;
2) A casting tray 2 having an area of 4.2mX4.2 m, a height of 2cm, a depth of 1cm, a tray edge width of 5cm, an inner bottom area of 4.1mX4.1 m, and an effective casting area of 4 mX4 m was prepared by using a 10mm float glass plate, a float glass ribbon, and a glass adhesive;
3) Filling a heat-insulating rock wool board with a 1mm stainless steel plate interlayer to prepare a heat-insulating bottom board 7 with the thickness of 5m multiplied by 10 cm;
4) Leveling feet with the height of 10cm are respectively arranged at four corners of the bottom surface of the heat preservation bottom plate 7, each leveling foot comprises a leveling screw rod 8, the upper part of each leveling screw rod 8 extends into the corresponding sleeve 9, the middle part of each leveling screw rod 8 is connected with a first leveling opposite-top sleeve 10 and a second leveling opposite-top sleeve 11 in a screwed mode, supporting feet 12 are fixed at the bottom of each leveling screw rod 8, and the top of each sleeve 9 is fixed on the bottom surface of the heat preservation bottom plate 7. The first leveling opposite-top sleeve 10 is rotated to raise and lower the height of the leveling foot margin, and the second leveling opposite-top sleeve 11 is rotated upwards to be in contact with the first leveling opposite-top sleeve 10, so that the height of the leveling foot margin can be locked;
5) And a 5m multiplied by 0.7m heat-preserving water-cooling jacket is arranged along the edge of the heat-preserving bottom plate 7 upwards and circularly, the heat-preserving water-cooling jacket is provided with two stainless steel plate interlayers with the thickness of 1mm and the thickness of 10cm, wherein the heat-preserving rock wool plates are filled in the stainless steel plate heat-preserving interlayers 4 on the outer side to form the heat-preserving interlayers 4. The inner side of the stainless steel plate water-cooling interlayer 5 is filled with 35cm high cooling water to form a water-cooling clamp. The water-cooling interlayer 5 is arranged around the casting film tray 2 and the heating part towards the bottom of the wall surface at one side of the casting film tray 2 and the heating part, and a circle of evaporation and condensation solvent collecting tank of casting film liquid with the circumference of 18.2m multiplied by 5cm multiplied by 10cm in width and depth is arranged;
6) A heating pipe frame 3 with the area of 4.4mX4.4mX30 cm is centrally placed on the heat preservation bottom plate 7, the heating pipe frame 3 is formed by covering 4.4mX4.4mX2 cm toughened glass plates 13 on a frame body, the frame body is formed by inserting 90 far infrared quartz heating pipes 6 which are 4.4m long, 220V in voltage and 500W in parallel and equidistant in power in a rectangular stainless steel hole frame with the length of 4.4mX4.4mX28 cm, the heating pipes are 5cm away from the heat preservation bottom plate, and the power density of the heating pipe frame 3 is 0.23W/cm 2 The heating power is 45kW;
7) A first height adjusting screw 14 is arranged centrally below the casting film plate 2, the first height adjusting screw 14 is an M12 stainless steel first height adjusting screw 14 with the height of 29.5cm, and two M12 internally threaded stainless steel opposite-top sleeves with the height of 2cm and the outer diameter of 19mm, namely a first opposite-top sleeve 15 and a second opposite-top sleeve 16 are connected to the upper part of the first height adjusting screw 14 in a threaded manner. The top edges of the first pair of top sleeves 15 are rounded, the tops of the first pair of top sleeves 15 are supported at the center of the lower bottom surface of the casting film tray 2, the first height adjusting screw 14 vertically passes through a through hole with the diameter of 22mm in the center of the heating pipe rack 3 and then is welded at the center of the heat insulation bottom plate 7, the first pair of top sleeves 15 are rotated to slightly adjust the height to 31cm and higher than the heating pipe rack by 1cm, and the second pair of top sleeves 16 are rotated upwards to lock the height of the first height adjusting screw 14;
8) The casting film plate 2 is placed on the first height adjusting screw 14 and the heating pipe rack 3 in the middle, the heating temperature is controlled by a temperature controller, and a temperature measuring probe is placed on the edge of the casting film plate 2 to detect the actual temperature;
9) The heating pipe frame 3 is controlled by a temperature controller to heat, and a temperature detector probe is arranged on the edge of the casting film tray 2 to detect the heating temperature;
10 The leveling instrument with equal-height support legs is arranged in the casting film tray 2 in the middle, the heights of four leveling feet are adjusted, so that the leveling bubble of the leveling instrument is positioned in zero positions in two mutually perpendicular directions in the casting film tray 2, the casting film tray 2 is positioned horizontally, and the heights of the leveling feet are locked;
11 50.43L of 5wt% casting solution having an average depth of 3mm, a central depth of about 2mm and an edge depth of >3mm was poured into the casting plate 2 having an inner bottom area of 4.1mX4.1m;
12 A 5m multiplied by 10cm heat-preserving top cover 1 is arranged at the upper end of the heat-preserving water-cooling jacket, the heat-preserving top cover 1 is prepared by filling a heat-preserving rock wool board with a 1mm stainless steel board interlayer, and a sealed heating space is enclosed by the heat-preserving top cover 1, the heat-preserving water-cooling jacket and a heat-preserving bottom board 7;
13 Starting the heating pipe frame 3 to heat the casting solution in the casting plate 2, controlling the heating temperature to 121 ℃ and the heating time to be about 2 hours, and enabling the solvent in the casting solution to be completely evaporated, wherein the heating temperature is lower than the boiling point of the solvent by 32 ℃. In the solvent evaporation process, the casting film tray 2 and the casting film liquid therein are in a static closed space, the solvent saturated vapor evaporated diffuses and covers the casting film liquid to the periphery under the heating of the heating pipe rack 3, the solvent saturated vapor which diffuses far contacts the water-cooling interlayer 5 of the heat-preservation water-cooling jacket, the solvent is cooled and condensed on the surface of the water-cooling interlayer 5 to form a liquid solvent, and under the action of gravity, the solvent flows down along the surface of the water-cooling interlayer 5 and is converged into the evaporation and condensation solvent collecting tank of the casting film liquid at the bottom, and the concentration of solute gradually increases along with gradual evaporation and reduction of the solvent in the casting film liquid, so that crystallization and film formation are realized;
Under the action of upward pressure of the first pair of top sleeves 15 and downward gravity of the first pair of top sleeves, the middle part of the casting film tray 2 slightly deforms and protrudes, the edge slightly deforms and sags, so that part of casting film liquid in the middle part of the casting film tray 2 flows out to the edge of the casting film tray 2 in advance before film formation, the casting film liquid in the middle part of the casting film tray 2 is shallower, the edge of the casting film tray 2 is deeper, but the periphery of the casting film tray 2 is provided with a heat-insulating water jacket for cooling and condensing solvent vapor in the casting film liquid, so that the casting film liquid in the edge of the casting film tray 2 is lower in temperature, the solvent evaporation and solute crystallization film forming speed are slower, the casting film liquid in the middle part is higher in temperature, and the solvent evaporation and solute crystallization film forming speed are faster, and part of casting film liquid at the edge of the casting film tray 2 flows into the middle part of the casting film tray 2 in the film forming process, so that the defect that the casting film liquid in the middle part of the casting film tray 2 is shallower is offset, and the thickness of the middle part and the edge of the casting film are basically consistent;
14 Stopping heating, extracting the condensed solvent in the evaporation and condensation solvent collecting tank of the casting solution, removing the film from the casting plate 2 after the casting plate 2 is cooled, and cutting off the 5cm film corners to obtain a finished product of the 4m multiplied by 0.075mm perfluorinated ion exchange film, wherein the film thickness error is less than or equal to 0.004mm;
15 Recovering the film corners and condensing solvent for recycling preparation of the casting solution.
Example 4
As shown in FIGS. 3 to 4, this example is a 5 m.times.5 m.times.0.1 mm perfluorinated ion exchange membrane, comprising the steps of:
1) 6kg of perfluorosulfonic acid ion exchange resin (equivalent weight EW=1000 g/eq, density 2.0 g/cm) 3 ) And 120L of dimethylformamide (boiling point 153 ℃ C., density 0.95 g/cm) 3 ) Adding 180L of closed reaction kettle, heating, stirring and dissolving, wherein the dissolving temperature is 200 ℃, and the dissolving time is 4 hours, so that the perfluorinated sulfonic acid ion exchange resin is dissolved in dimethylformamide to prepare about 120L of casting solution with the concentration of 5 wt%;
2) A casting tray 2 having an area of 5.2mX5.2 m, a height of 2cm, a depth of 1cm, a tray edge width of 5cm, an inner bottom area of 5.1mX5.1 m, and an effective casting area of 5 mX5 m was prepared by using a 10mm float glass plate, a float glass ribbon, and a glass adhesive;
3) Filling a heat-insulating rock wool board with a 1mm stainless steel plate interlayer to prepare a 6m multiplied by 10cm heat-insulating bottom plate 7;
4) Leveling feet with the height of 10cm are respectively arranged at four corners of the bottom surface of the heat preservation bottom plate 7, each leveling foot comprises a leveling screw rod 8, the upper part of each leveling screw rod 8 extends into the corresponding sleeve 9, the middle part of each leveling screw rod 8 is connected with a first leveling opposite-top sleeve 10 and a second leveling opposite-top sleeve 11 in a screwed mode, supporting feet 12 are fixed at the bottom of each leveling screw rod 8, and the top of each sleeve 9 is fixed on the bottom surface of the heat preservation bottom plate 7. The first leveling opposite-top sleeve 10 is rotated to raise and lower the height of the leveling foot margin, and the second leveling opposite-top sleeve 11 is rotated upwards to be in contact with the first leveling opposite-top sleeve 10, so that the height of the leveling foot margin can be locked;
5) And a 6m multiplied by 0.7m heat-preserving water-cooling jacket is arranged along the edge of the heat-preserving bottom plate 7 upwards in a circle, the heat-preserving water-cooling jacket is provided with two stainless steel plate interlayers with the thickness of 10cm and 1mm, wherein the heat-preserving rock wool plates are filled in the stainless steel plate heat-preserving interlayers 4 on the outer side to form the heat-preserving interlayer 4. The inner side of the stainless steel plate water-cooling interlayer 5 is filled with 35cm high cooling water to form a water-cooling clamp. The water-cooling interlayer 5 is arranged around the casting film tray 2 and the heating part towards the bottom of the wall surface at one side of the casting film tray 2 and the heating part, and a circle of evaporation and condensation solvent collecting tank of casting film liquid with the perimeter of 22.2m multiplied by 5cm multiplied by 10cm in depth is arranged;
6) A heating pipe frame 3 with the area of 5.4mX5.4mX30 cm is arranged on the heat preservation bottom plate 7 in the middle, the heating pipe frame 3 is formed by covering a toughened glass plate 13 with the area of 5.4mX5.4mX2 cm on a frame body, the frame body is formed by inserting 110 far infrared quartz heating pipes 6 which are 5.4m long, 220V in voltage and 600W in parallel equidistant arrangement and have the power of 5.4 mX5.4mX28 cm in a rectangular stainless steel hole frame, the heating pipe is 5cm away from the heat preservation bottom plate, and the power density of the heating pipe frame 3 is 0.23W/cm 2 Heating power is 66kW;
7) A first height adjusting screw 14 is arranged centrally below the casting film plate 2, the first height adjusting screw 14 is an M12 stainless steel first height adjusting screw 14 with the height of 29.5cm, and two M12 internally threaded stainless steel opposite-top sleeves with the height of 2cm and the outer diameter of 19mm, namely a first opposite-top sleeve 15 and a second opposite-top sleeve 16 are connected to the upper part of the first height adjusting screw 14 in a threaded manner. The top edges of the first pair of top sleeves 15 are rounded, the tops of the first pair of top sleeves 15 are supported at the center of the lower bottom surface of the casting film tray 2, the first height adjusting screw rods 14 vertically penetrate through holes with the diameter of 22mm in the center of the heating pipe rack 3 and then are welded at the center of the heat insulation bottom plate 7, the heights of the first height adjusting screw rods 14 are finely adjusted to 31.2cm by rotating the first pair of top sleeves 15, the height of the first height adjusting screw rods is 1.2cm higher than that of the heating pipe rack, and the heights of the first height adjusting screw rods 14 are locked by rotating the second pair of top sleeves 16 upwards;
8) The casting film tray 2 is placed on the first height adjusting screw 14 and the heating pipe rack 3 in the middle;
9) The heating pipe frame 3 is controlled by a temperature controller to heat, and a temperature detector probe is arranged on the edge of the casting film tray 2 to detect the heating temperature;
10 The leveling instrument with equal-height support legs is arranged in the casting film tray 2 in the middle, the heights of four leveling feet are adjusted, so that the leveling bubble of the leveling instrument is positioned in zero positions in two mutually perpendicular directions in the casting film tray 2, the casting film tray 2 is positioned horizontally, and the heights of the leveling feet are locked;
11 104.04L of 5wt% casting solution having an average depth of 4mm, a central depth of about 2.8mm and an edge depth of >4mm was poured into the casting tray 2 having an inner bottom area of 5.1m×5.1 m;
12 A heat-insulating top cover 1 with the length of 6m multiplied by 10cm is arranged at the upper end of the heat-insulating water-cooling jacket, the heat-insulating top cover 1 is prepared by filling a heat-insulating rock wool board with a 1mm stainless steel plate interlayer, and a sealed heating space is enclosed by the heat-insulating top cover 1, the heat-insulating water-cooling jacket and a heat-insulating bottom plate 7;
13 Starting the heating pipe frame 3 to heat the casting solution in the casting plate 2, controlling the heating temperature to 120 ℃ and 33 ℃ below the boiling point of the solvent, and heating for about 2.5 hours to evaporate the solvent in the casting solution. In the solvent evaporation process, the casting film tray 2 and the casting film liquid therein are in a static closed space, the solvent saturated vapor evaporated diffuses and covers the casting film liquid to the periphery under the heating of the heating pipe rack 3, the solvent saturated vapor which diffuses far contacts the water-cooling interlayer 5 of the heat-preservation water-cooling jacket, the surface of the water-cooling interlayer 5 is cooled and condensed into liquid solvent, and under the action of gravity, the liquid solvent flows down along the surface of the water-cooling interlayer 5 and is converged into the evaporation and condensation solvent collecting tank of the casting film liquid at the bottom edge of the liquid, and the concentration of solute gradually increases along with gradual evaporation and reduction of the solvent in the casting film liquid, so that crystallization and film formation are realized;
The middle part of the film casting disc 2 slightly deforms and protrudes upwards, the edge slightly deforms and sags under the action of the upward pressure of the top of the first pair of top sleeves 15 of the first height adjusting screw 14 and the downward gravity of the top sleeves, so that part of the film casting liquid in the middle part of the film casting disc 2 flows out to the edge of the film casting disc 2 in advance before film formation, the film casting liquid in the middle part of the film casting disc 2 is shallower, the edge film casting liquid is deeper, but a heat-insulating water jacket for cooling and condensing solvent vapor in the film casting liquid is arranged at the periphery of the film casting disc 2, so that the temperature of the edge film casting liquid of the film casting disc 2 is lower, the solvent evaporation and solute crystallization film forming speed is slower, the temperature of the middle film casting liquid is higher, the solvent evaporation and solute crystallization film forming are faster, and part of the edge film casting liquid flows into the middle part of the film casting disc 2 in the film forming process, thus the defect that the film casting liquid in the middle part of the film casting disc 2 is shallower is overcome, and the thickness of the middle part and the edge thickness of the cast film is basically consistent;
14 Stopping heating, extracting the condensed solvent in the evaporation and condensation solvent collecting tank of the casting solution, removing the film from the casting film tray 2 after the casting film tray 2 is cooled, and cutting off the 5cm film corners to obtain a finished product of the perfluorinated ion exchange membrane with the thickness error of 5m multiplied by 0.1mm, wherein the thickness error of the film is less than or equal to 0.005mm;
15 Recovering the film corners and condensing solvent for recycling preparation of the casting solution.
It will be readily appreciated by those skilled in the art that the above advantageous ways can be freely combined and superimposed without conflict.
The foregoing description of the preferred embodiments of the invention is not intended to be limiting, but rather is intended to cover all modifications, equivalents, and alternatives falling within the spirit and principles of the invention. The foregoing is merely a preferred embodiment of the present invention, and it should be noted that it will be apparent to those skilled in the art that modifications and variations can be made without departing from the technical principles of the present invention, and these modifications and variations should also be regarded as the scope of the invention.

Claims (8)

1. The utility model provides a solution casting large membrane device which is characterized in that, includes casting dish (2), heating portion, heat preservation water jacket and altitude mixture control portion, casting dish (2) set up the middle part of the loading surface of heating portion, casting dish (2) are used for setting up casting liquid, the effective casting area of casting dish (2) is 4-25m 2 The area of the bearing surface is 5-30m 2 The area of the bearing surface is larger than the effective casting area of the casting disc (2), the heat-insulating water-cooled jacket is sleeved on the heating part and the outer peripheral side of the casting disc (2), the height adjusting part is opposite to the middle part of the casting disc (2), at least one part of the height adjusting part is positioned between the casting disc (2) and the heating part so as to jack the middle part of the casting disc (2) up from the heating part, and the middle part of the casting disc (2) is higher than the edge of the casting disc (2) so as to enable the middle part of the casting disc (2) The casting solution on the part flows out a part of the edge of the casting disc (2) in advance before film forming;
the height adjustment part comprises a first thread heightening assembly, the first thread heightening assembly comprises a first height adjustment screw (14), a first propping sleeve (15) and a second propping sleeve (16), the center point of the casting film tray (2) and the heating part in the horizontal direction is located on the axis line of the first height adjustment screw (14), the first propping sleeve (15) and the second propping sleeve (16) are connected to the first height adjustment screw (14) through threads, the first propping sleeve (15) is located on one side, close to the casting film tray (2), of the second propping sleeve (16), the first propping sleeve (15) penetrates through the heating part to prop up the casting film tray (2), and the second propping sleeve (16) and the first propping sleeve (15) are propped against each other to lock the first propping sleeve (15).
2. The solution casting large film apparatus according to claim 1, wherein the height adjusting section includes a plurality of first shims (17), the plurality of first shims (17) being uniformly arranged along a circumferential direction of a center position of the casting tray (2) and the heating section in a horizontal direction;
The thickness of the first gasket (17) is 0.6-1.2mm, and the outer diameter of the first gasket (17) is 6-12mm;
the top surface of the first gasket (17) is an arc surface and protrudes in a direction away from the heating part;
the first gasket (17) is made of at least one material selected from aluminum, red copper and polytetrafluoroethylene.
3. The solution casting large film device according to claim 1, wherein the first pair of top sleeves (15) are sleeved at the end part of the first height adjusting screw (14) close to one side of the casting film tray (2), the first pair of top sleeves (15) comprise a first cylinder top, the first cylinder top is positioned between the first height adjusting screw (14) and the casting film tray (2), the outer diameter of the first cylinder top is 18-20mm, and the outer wall of the first cylinder top facing one side of the casting film tray (2) is an arc surface and protrudes in a direction away from the heating part.
4. Solution casting large film apparatus according to claim 1, characterized in that the height adjusting section comprises a plurality of second thread adjusting assemblies uniformly arranged along the circumference of the central positions of the casting film tray (2) and the heating section in the horizontal direction, the second thread adjusting assemblies comprising a second height adjusting screw (18), a third counter-top sleeve (19) and a fourth counter-top sleeve, the third counter-top sleeve (19) and the fourth counter-top sleeve being screwed to the second height adjusting screw (18), the third counter-top sleeve (19) being located on the side of the fourth counter-top sleeve close to the casting film tray (2), the third counter-top sleeve (19) passing through the heating section to jack up the casting film tray (2), the fourth counter-top sleeve abutting against the third counter-top sleeve (19) to lock the third counter-top sleeve (19);
The third is to top sleeve (19) cover is established second high adjustment screw rod (18) is close to the tip of casting membrane dish (2) one side, third is to top sleeve (19) include the second section of thick bamboo top, the second section of thick bamboo top is located between second high adjustment screw rod (18) and casting membrane dish (2), the external diameter of second section of thick bamboo top is 18-20mm, the second section of thick bamboo top is towards the outer wall of casting membrane dish (2) one side is the cambered surface, and to keeping away from the direction protrusion of heating portion.
5. The solution casting apparatus as recited in claim 4 wherein the second thread take-up assembly has a height less than a height of the first thread take-up assembly.
6. The solution casting large film device according to claim 1, further comprising a heat-preserving bottom plate (7), a heat-preserving top cover (1), leveling feet and a temperature control part;
the bottom end of the heat-insulating water cooling jacket is arranged on the top surface of the heat-insulating bottom plate (7), the heat-insulating top cover (1) is arranged on the top end of the heat-insulating water cooling jacket in a covering mode, a heating space is surrounded by the heat-insulating top cover (1), the heat-insulating water cooling jacket and the heat-insulating bottom plate (7), and the heating part and the casting film tray (2) are arranged in the heating space;
The leveling feet are arranged on the bottom surface of the heat-insulating bottom plate (7) so as to adjust the height and levelness of the heat-insulating bottom plate (7);
the temperature control part comprises a temperature controller and a temperature probe, the temperature probe is arranged on the edge of the casting film tray (2) to detect the heating temperature, and the temperature probe and the heating part are respectively connected with the temperature controller;
the heat preservation water cooling jacket comprises a heat preservation interlayer (4) and a water cooling interlayer (5), wherein the water cooling interlayer (5) is sleeved on the periphery side of the casting film tray (2) and the heating part, the heat preservation interlayer (4) is sleeved on the periphery side of the water cooling interlayer (5), and the water cooling interlayer (5) faces the casting film tray (2) and the periphery of the wall surface bottom edge on one side of the heating part is provided with an evaporation and condensation solvent collecting tank of the casting film liquid.
7. A solution casting method for producing a film by the solution casting apparatus according to any one of claims 1 to 6, comprising the steps of:
placing the heating part in a heat-preservation water-cooling sleeve, so that the heat-preservation water-cooling sleeve is positioned at the outer periphery side of the heating part;
the height adjusting part is arranged in the middle of the bearing surface of the heating part, so that the height of the middle part of the casting film tray (2) is higher than the height of the edge of the casting film tray (2);
Placing a casting film tray (2) on the bearing surfaces of the height adjusting part and the heating part, enabling the height adjusting part to be opposite to the middle part of the casting film tray (2), and enabling at least one part of the height adjusting part to be positioned between the casting film tray (2) and the heating part, wherein the effective casting film area of the casting film tray (2) is 4-25m 2 The area of the bearing surface is 5-30m 2 The area of the bearing surface is larger than the effective casting area of the casting disc (2);
pouring a casting solution into the casting plate (2);
and starting the heating part to heat the casting solution in the casting plate (2) so as to evaporate and condense the solvent of the casting solution, and crystallizing the solute to form a film.
8. The solution casting method as claimed in claim 7, wherein,
before the step of placing the heating portion in the heat-insulating water-cooling jacket so that the heat-insulating water-cooling jacket is located on the outer peripheral side of the heating portion, the method further comprises:
preparing the casting film liquid;
-making said casting disc (2) using a float glass plate, a float glass strip and a glass glue;
preparing a heat-insulating bottom plate (7) by filling a heat-insulating rock wool board with a stainless steel plate interlayer;
the height and levelness of the heat-insulating bottom plate (7) are adjusted through leveling feet on the bottom surface of the heat-insulating bottom plate (7);
Manufacturing the heat-insulating water-cooling jacket with an inner stainless steel plate interlayer and an outer stainless steel plate interlayer along the edge of the heat-insulating bottom plate (7), filling heat-insulating rock wool plates in the outer stainless steel plate interlayer, filling cooling water in the inner stainless steel plate interlayer, and arranging an evaporation and condensation solvent collecting tank of the casting solution in the circumferential direction of the bottom edge of the inner wall of the inner stainless steel plate interlayer;
before the step of placing the height adjusting section in the middle of the carrying surface of the heating section, the method further comprises:
the heating part is arranged in the middle of the heat preservation bottom plate (7), wherein the heating part comprises a heating pipe frame and a toughened glass plate (13) covered on the top of the heating pipe frame, and the heating pipe frame comprises a rectangular stainless steel hole frame and a plurality of far infrared quartz heating pipes (6) which are inserted in the rectangular stainless steel hole frame and are arranged in parallel at equal intervals;
before the step of pouring the casting solution into the casting plate (2), the method further comprises:
the heating temperature of the heating part is controlled by a temperature controller, and the heating temperature is detected by a temperature measuring probe arranged on the edge of the casting film tray (2);
placing a leveling foot level meter in the middle of the casting film tray (2), adjusting the height and levelness of the heat insulation bottom plate (7) through leveling feet on the bottom surface of the heat insulation bottom plate (7), enabling the leveling bubble of the leveling foot level meter to be in zero positions in two mutually perpendicular directions in the casting film tray (2), and locking the height of the leveling feet;
Before the step of heating the casting solution in the casting tray (2) by the start-up heating part to evaporate and condense the solvent of the casting solution, the method further comprises the steps of:
a heat-insulating top cover (1) is arranged on the upper end cover of the heat-insulating water-cooling jacket, so that a heating space is surrounded by the heat-insulating top cover (1), the heat-insulating water-cooling jacket and the heat-insulating bottom plate (7), wherein a heat-insulating rock wool board is filled in an interlayer of the heat-insulating top cover (1);
the step of heating the casting solution in the casting tray (2) by the start-up heating part to evaporate and condense the solvent of the casting solution, and crystallizing the solute to form a film, comprises the following steps:
controlling the heating temperature to be 30-33 ℃ lower than the boiling point of the casting film liquid by the temperature controller;
the method further comprises the steps of heating the casting solution in the casting plate (2) by the starting heating part, evaporating and condensing a solvent of the casting solution, crystallizing and forming a film of a solute, and then:
stopping heating;
extracting the gas and condensed solvent from the heating space;
lifting and cutting the film;
detecting and warehousing the film;
recovering the film corners and the condensed solvent.
CN202310319660.5A 2023-03-29 2023-03-29 Solution casting large film device and method Active CN116021694B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202310319660.5A CN116021694B (en) 2023-03-29 2023-03-29 Solution casting large film device and method

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202310319660.5A CN116021694B (en) 2023-03-29 2023-03-29 Solution casting large film device and method

Publications (2)

Publication Number Publication Date
CN116021694A CN116021694A (en) 2023-04-28
CN116021694B true CN116021694B (en) 2023-06-02

Family

ID=86072679

Family Applications (1)

Application Number Title Priority Date Filing Date
CN202310319660.5A Active CN116021694B (en) 2023-03-29 2023-03-29 Solution casting large film device and method

Country Status (1)

Country Link
CN (1) CN116021694B (en)

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3357052A (en) * 1965-07-06 1967-12-12 Gen Dynamics Corp Apparatus for making membranes
CN102888010A (en) * 2011-07-19 2013-01-23 北京金能世纪科技有限公司 Solution casting method
CN105483652A (en) * 2015-12-07 2016-04-13 武汉华星光电技术有限公司 Chemical vapor deposition device and use method thereof
CN107857889A (en) * 2017-12-08 2018-03-30 北京金能世纪科技有限公司 A kind of solution casts big film device and method
CN212240868U (en) * 2020-06-02 2020-12-29 成都路维光电有限公司 Top column device for coating mask

Family Cites Families (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP4528231B2 (en) * 2005-09-20 2010-08-18 富士フイルム株式会社 Solution casting equipment and method

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3357052A (en) * 1965-07-06 1967-12-12 Gen Dynamics Corp Apparatus for making membranes
CN102888010A (en) * 2011-07-19 2013-01-23 北京金能世纪科技有限公司 Solution casting method
CN105483652A (en) * 2015-12-07 2016-04-13 武汉华星光电技术有限公司 Chemical vapor deposition device and use method thereof
CN107857889A (en) * 2017-12-08 2018-03-30 北京金能世纪科技有限公司 A kind of solution casts big film device and method
CN212240868U (en) * 2020-06-02 2020-12-29 成都路维光电有限公司 Top column device for coating mask

Also Published As

Publication number Publication date
CN116021694A (en) 2023-04-28

Similar Documents

Publication Publication Date Title
EP2050779B1 (en) Membrane solution casting process
CN116021694B (en) Solution casting large film device and method
CN105762374A (en) Fuel cell catalyst layer and membrane electrode subassembly and preparation method thereof
CN113224364A (en) Vertical assembling device and method for molten carbonate fuel cell stack
CN207831930U (en) A kind of sintering frame
CN109176359B (en) Clamping and centering device for producing thin-film solar cell
CN111793229B (en) Solution film forming apparatus and method
CN102888010B (en) Solution casting method
CN101906215A (en) Manufacturing method of high-strength composite proton exchange membrane
CN210878494U (en) Device for calibrating zero-position installation angle of fan blade
CN107857889A (en) A kind of solution casts big film device and method
CN209866088U (en) Laboratory constant temperature test tube heater
CN210150944U (en) Cooling device for producing high borosilicate glass tube electrode
CN207529822U (en) A kind of chip-type laminated solid aluminum electrolytic capacitor chemical polymerization slot of polymer
CN218974545U (en) All-solid-state battery test die with self-heating function
CN217845530U (en) Aluminum electrolytic capacitor air tightness testing device
CN214199244U (en) Solar heat collecting device
CN207925313U (en) A kind of chip-type laminated solid aluminum electrolytic capacitor chemical polymerization slot of polymer
CN220476811U (en) Continuous plasma sterilizing equipment for ice cream production
CN220526883U (en) Treatment apparatus
CN211251024U (en) PVD film equipment heating device
CN215783408U (en) Novel bubble cap tower tray
CN210522551U (en) Concrete sample test temporary storage device
CN217517034U (en) Water seal tank for water electrolysis hydrogen production equipment
CN220367258U (en) Chromatographic column heating device

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
GR01 Patent grant
GR01 Patent grant