WO2024058132A1 - Procédé pour retirer la couche de revêtement fixée à la feuille verte, et dispositif pour retirer la couche de revêtement fixée à la feuille verte - Google Patents

Procédé pour retirer la couche de revêtement fixée à la feuille verte, et dispositif pour retirer la couche de revêtement fixée à la feuille verte Download PDF

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Publication number
WO2024058132A1
WO2024058132A1 PCT/JP2023/033075 JP2023033075W WO2024058132A1 WO 2024058132 A1 WO2024058132 A1 WO 2024058132A1 JP 2023033075 W JP2023033075 W JP 2023033075W WO 2024058132 A1 WO2024058132 A1 WO 2024058132A1
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Prior art keywords
green sheet
container
coating layer
base film
laminated film
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PCT/JP2023/033075
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English (en)
Japanese (ja)
Inventor
裕太 井澤
裕一 森
知巳 深谷
太寿 西尾
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リンテック株式会社
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Publication of WO2024058132A1 publication Critical patent/WO2024058132A1/fr

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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29B—PREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
    • B29B17/00—Recovery of plastics or other constituents of waste material containing plastics

Definitions

  • the present invention relates to a method for removing a coating layer with green sheets and an apparatus for removing a coating layer with green sheets.
  • Patent Document 1 a resin base material having a coating on its surface is placed in a cleaning container, and the resin base material is mixed with an alkaline aqueous solution in an amount that makes the liquid level higher than the top of the resin base material deposited in the cleaning container.
  • a method for removing a resin substrate coating is disclosed, which includes a coating removal step of stirring at a temperature of 80 to 180° C. at a rotation speed of 2 to 100 m/sec at the tip of a stirring blade.
  • Patent Document 2 discloses a release film in which a release layer is formed on at least one side of a base film through an easily soluble resin layer, and the release film after use is made of an easily soluble resin.
  • a release film characterized in that the release layer on the surface of the film is separated and removed by immersing it in a solvent that can dissolve the easily soluble resin in the solvent, and only the base film is recovered.
  • a collection method is disclosed.
  • the method described in Patent Document 1 is a technique for removing a film on a resin base material using an alkaline aqueous solution.
  • the alkaline aqueous solution after use contains components in the film (for example, a stripping agent), and there is a problem in that the cleaning ability decreases when reused. Another problem is that it takes time and effort to purify the alkaline aqueous solution.
  • a release layer is laminated on at least one side of a base film with an easily soluble resin layer (water-soluble resin or water-dispersible resin) interposed therebetween.
  • the release layer is peeled from the release film by utilizing the property that the easily soluble resin layer is easily dissolved in a solvent.
  • the layer configuration of laminated films is diverse, for example, when the layer formed on the base film is a water-insoluble resin layer, in the method described in Patent Document 2, from the release film to the release layer. is difficult to remove. Furthermore, in the method described in Patent Document 2, there is a possibility that the easily soluble resin layer dissolved in the solvent will re-adhere to the release film. Furthermore, there is a possibility that the solvent may be contaminated by the easily soluble resin layer. In recent technology for recycling base films, there is a need for a technology that can more easily remove a coating layer from a laminated film having a base film and a multilayer coating layer. Examples of the laminated film include a laminated film with ceramic green sheets that has been used in the production of a multilayer ceramic capacitor (MLCC).
  • MLCC multilayer ceramic capacitor
  • the object of the present invention is to provide a method and device for removing a coating layer with a green sheet that can easily remove a coating layer with a green sheet from a laminated film and easily recover the base film separately.
  • a laminated film with a green sheet comprising a base film and a coating layer with a green sheet attached to the surface, the step of cutting the laminated film with a green sheet into strips, and the step of cutting the green sheet after cutting.
  • a step of holding a laminated film with a sheet in a container having a plurality of holes a step of storing the container holding the laminated film with a green sheet and treated water in a storage tank; , the green sheet-attached laminated film is divided into a base film remaining inside the container, floating matter discharged to the outside of the container and floating on the surface side of the treated water, and floating matter discharged to the outside of the container.
  • a step of separating the sediments from the sediments settling on the bottom side of the storage tank, a step of recovering the separated base film from inside the container, and a step of recovering the separated floating materials from the outside of the container. and a floating matter collection step of collecting the separated sediment from the upper side of the storage tank, and a sediment collection step of collecting the separated sediment from the outside of the container and the bottom side of the storage tank, is the residue of the coating layer that has been separated from the base film and has the green sheet attached thereto, and the sediment is the residue of the green sheet that has been separated from both the base film and the coating layer.
  • the separated base film is allowed to sink in the container, the separated floating material is floated outside the container and on the surface side of the treated water, and the separated sediment is
  • the floating matter collection step is a step of filtering out the floating matter with a filter that is removably provided just below the water surface of the storage tank. Method for removing coating layer with green sheet as described.
  • the floating matter collection step includes causing the treated water in the storage tank to overflow, and draining the floating matter that flows out due to the overflow of the treated water from the upper discharge port of the storage tank to the outside of the storage tank.
  • the sediment recovery step is a step of connecting a discharge pipe to a discharge port disposed on the bottom side of the storage tank to discharge the sediment from the storage tank, [1] to [6] above.
  • a laminated film with a green sheet comprising a base film and a coating layer with a green sheet attached to the surface thereof, a cutting means for cutting the laminated film with a green sheet into strips, and a cutting means for cutting the laminated film with a green sheet into strips, holding means for holding the laminated film with green sheets in a container having a plurality of holes; storage means for storing the holding means holding the laminated film with green sheets and treated water; base film recovery means; , comprising a floating matter collection means disposed outside the container and on the upper side of the accommodation means, and a sediment collection means disposed outside the container and on the bottom side of the accommodation means, and the substrate film
  • the collection means is means for collecting the base film separated from the coating layer by taking it out from the container, and the floating matter collection means collects the base film separated from the base film in the treated water of the storage means.
  • a removing device for a coating layer with a green sheet which is a means for collecting waste of the green sheet.
  • a method for removing a coating layer with a green sheet and a method for removing the coating layer with a green sheet that can easily remove the coating layer with a green sheet from a laminated film and easily recover the base film alone. equipment can be provided.
  • FIG. 3 is a diagram for explaining a removal method according to the first embodiment.
  • FIG. 3 is a diagram for explaining a removal method according to the first embodiment.
  • FIG. 3 is a diagram for explaining a removal method according to the first embodiment.
  • FIG. 3 is a diagram for explaining a removal method according to the first embodiment.
  • FIG. 3 is a diagram for explaining a removal method according to the first embodiment. It is a figure for explaining the separation process concerning a modification.
  • a method for removing a coating layer with a green sheet according to the present embodiment (hereinafter also referred to as a removal method according to the present embodiment) is a laminated layer with a green sheet that has a base film and a coating layer on the surface of which a green sheet is attached.
  • a step of cutting the laminated film with green sheets into small pieces (hereinafter also referred to as a cutting step), and a step of holding the cut laminated film with green sheets in a container having a plurality of holes.
  • a holding step a step of accommodating the container in which the laminated film with green sheets is held and the treated water in a storage tank; and a step of storing the laminated film with green sheets in the treated water in the storage tank.
  • a step of separating the separated substrate film into sediment hereinafter also referred to as separation step
  • separation step a step of recovering the separated base film from inside the container; and a step of recovering the separated floating material from the outside of the container.
  • the method includes a floating matter collection step of collecting from the upper side of the storage tank, and a sediment collection step of collecting the separated sediment from the outside of the container and from the bottom side of the storage tank.
  • the floating matter is the dregs of the coating layer that has been separated from the base film and has the green sheet attached thereto (hereinafter also referred to as the dregs of the coating layer with the green sheet), and the sediment is the dregs of the coating layer with the green sheet attached. This is the waste of the green sheet separated from both the material film and the coating layer.
  • the coating layer includes an intermediate layer and a release agent layer, and the intermediate layer is disposed between the base film and the release agent layer.
  • the "laminated film with green sheet" may be simply referred to as the "laminated film.”
  • the treated water is water used to immerse the laminated film with green sheets in the separation process, and is used to penetrate into the interface between the base film and the coating layer and reduce their mutual adhesion.
  • the treated water is preferably ordinary water, ie, industrial water, and may be purified water or distilled water.
  • the water may be water obtained by reusing wastewater used in various industrial productions, or may be water obtained by reusing wastewater after being used in the implementation of this embodiment. When wastewater is to be reused, wastewater may be recycled as appropriate.
  • the treated water may contain additives that add functionality as appropriate, but it is preferable that they do not. Examples of additives include surfactants and water-soluble organic solvents.
  • the concentration of the active ingredient of the additive in the treated water is preferably 0.2% by mass or less, and preferably 0.1% by mass or less, based on the total amount of the treated water. More preferably, the treated water is not water to which additives have been intentionally added. Furthermore, the treated water is preferably neither an alkaline aqueous solution prepared by intentionally adding a basic substance, nor an acidic aqueous solution prepared by intentionally adding an acidic substance. Treated water may contain basic and acidic substances as additives, as it is possible that wastewater can be easily recycled, but in that case, uniform wastewater standards based on the Water Pollution Control Act (other It is preferable that the pH of the treated water is 5.8 or more and 8.6 or less so as to meet the criteria of item (2). In this specification, treated water is water, hot water or superheated water. The temperature of the hot water is, for example, 40°C or more and 100°C or less. Superheated water is liquid water that has been heated under pressure to a temperature above 100°C.
  • FIG. 1A is a cross-sectional view of a green sheet-attached laminated film 50 used in the removal method according to the present embodiment.
  • the laminated film 50 is a film that has been cut into pieces after being subjected to a cutting process.
  • the laminated film 50 includes a base film 51, a coating layer 52, and a green sheet 53.
  • the coating layer 52 includes an intermediate layer 521 and a release agent layer 522, and the intermediate layer 521 is disposed between the base film 51 and the release agent layer 522.
  • the green sheet 53 is attached to a part of the surface of the release agent layer 522 (the surface of the coating layer 52). The position at which the green sheet 53 is attached to the surface of the coating layer 52 is not limited to that shown in FIG. 1A.
  • the position of attachment of the green sheet 53 to the surface of the coating layer 52 varies depending on the cutting location.
  • a indicates the surface of the intermediate layer 521 on the base film side
  • b indicates the surface of the intermediate layer 521 on the release agent layer side
  • d indicates the surface of the release agent layer
  • c indicates the surface of the release agent layer 522 on the intermediate layer side
  • e indicates the green sheet surface.
  • the base film and the intermediate layer are in direct contact with each other.
  • the base film 51 and the intermediate layer 521 are in direct contact
  • the intermediate layer 521 and the release agent layer 522 are in direct contact
  • the release agent layer 522 and the green sheet 53 are in direct contact. ing.
  • the laminated film 50 in the separation step, is held in a container having a plurality of holes and immersed in treated water, so that the interface between the base film 51 and the intermediate layer 521 is treated. Water becomes more likely to infiltrate, and the laminated film 50 can be separated into the base film 51, the dregs of the coating layer with the green sheet (floating matter 54C), and the dregs of the green sheet (sediment 53C) (Fig. (See 2B).
  • the dregs of the green sheet-attached coating layer (floating matter 54C) have the property of floating in the treated water, so they are discharged from the container through the holes of the container and float on the surface of the treated water.
  • the green sheet residue (sediment 53C) has the property of sinking in the treated water, and therefore is discharged from the container through the holes of the container and sinks in the treated water. That is, in the separation step, only the base film 51 can be kept in the container, and unnecessary parts (floating matter 54C and sediment 53C) can be discharged outside the container. Therefore, according to the removal method according to the present embodiment, the coating layer with green sheets can be easily removed from the laminated film. Moreover, the base film can be easily collected alone from inside the container. Note that if the separation step is performed without holding the laminated film in the container, green sheet residue (sediment 53C) tends to adhere to the surface of the base film 51, and the base film 51 is not held alone. It becomes difficult to separate.
  • the removal method according to the present embodiment uses treated water such as warm water, so it is possible to remove the green sheet from the laminated film regardless of the chemical properties of the coating layer and the green sheet.
  • the attached coating layer can be removed. Therefore, the removal method according to this embodiment is a new removal method for collecting and recycling the base film (preferably PET film). Furthermore, the removal method according to the present embodiment does not leave any foreign matter (mainly blasting material) behind, compared to a method in which the coating layer is removed by blasting.
  • the intermediate layer is preferably hydrophilic and water-insoluble.
  • the effect of this embodiment (the effect that the coating layer with the green sheet can be easily removed from the laminated film) is more expressed.
  • the reason for this is thought to be as follows.
  • the intermediate layer 521 in the laminated film 50 is in close contact with the base film 51 mainly due to hydrogen bonds and anchor effects (FIG. 1A). If the intermediate layer 521 is hydrophilic, when the laminated film 50 is held in a container with holes and immersed in treated water, the treated water will more likely infiltrate into the interface between the base film 51 and the intermediate layer 521. The hydrogen bonding and anchoring effect between the intermediate layer 521 and the base film 51 are weakened.
  • the intermediate layer 521 is more easily peeled off from the base film 51 together with the release agent layer 522 (in this embodiment, the release agent layer 522 to which the green sheet 53 is attached to a part of the surface), so that the intermediate layer 521 is more easily peeled off from the base film 51.
  • the coating layer with green sheets can be removed more easily.
  • the intermediate layer is water-insoluble, components of the intermediate layer 521 are prevented from eluting into the treated water. Therefore, since the intermediate layer 521 is water-insoluble, it is possible to prevent the treated water from being contaminated, and it becomes easier to reuse the treated water after use. Furthermore, since the removal method according to the present embodiment does not use an alkaline aqueous solution with a high concentration of alkaline components (for example, pH exceeding 8.6) as the treated water, unlike Patent Document 1, the treated water after use is not used. It has the advantage that there is no need to purify the water, and the cleaning ability of the treated water after use does not decrease.
  • the coating layer with green sheets can be more easily removed from the laminated film, and the treated water can be more easily reused.
  • the amount of "components to be removed" contained in the treated water is extremely small, so the purification process can be simplified and the environmental load can be reduced.
  • an intermediate layer is “hydrophilic” if the contact angle of water on the surface of the intermediate layer on the base film side is 55 degrees or less. do.
  • the contact angle is preferably 50 degrees or less, more preferably 45 degrees or less.
  • the contact angle is determined when the base film of the intermediate layer is contacted after the base film is separated from the laminated film, that is, after the intermediate layer is brought into contact with water and the interface between the intermediate layer and the base film is peeled off. This value is obtained by measuring the contact angle of water on the surface (peeled surface). Purified water is used as the water brought into contact with the intermediate layer when measuring the contact angle of water.
  • a test piece is prepared by the following method, the intermediate layer is separated from the base film of the test piece, and the contact angle of water on the surface of the intermediate layer on the base film side is measured. The obtained value is taken as the contact angle of water on the surface of the intermediate layer on the base film side.
  • a laminated film for measurement is prepared. As the laminated film for measurement, a laminated film before forming a green sheet is used, or a laminated film after the green sheet is peeled off from a laminated film with a green sheet by a known method is used.
  • An adhesive tape with a width of 50 mm is attached to the surface of the release agent layer of the laminated film for measurement, and then cut into a size of 50 mm x 50 mm to prepare a test piece.
  • a glass beaker with a capacity of 500 mL is filled with 300 mL of purified water at 90° C. as treated water, and the entire test piece is immersed in the purified water and left for 3 hours. After that, it was confirmed that the test piece was separated into a laminate in which the release agent layer and the intermediate layer were integrally supported on the adhesive tape, and a base film, and the release agent layer and the intermediate layer were supported.
  • the adhesive tape is taken out of the purified water and dried at room temperature for 24 hours.
  • the contact angle is measured on the surface of the intermediate layer supported on the adhesive tape (the surface of the intermediate layer that was in contact with the surface of the base film).
  • the contact angle is measured by the sessile drop method using a contact angle meter (manufactured by Kyowa Interface Science Co., Ltd., product name "DM-701") according to JIS R3257:1999.
  • a contact angle meter manufactured by Kyowa Interface Science Co., Ltd., product name "DM-701”
  • an intermediate layer is “water-insoluble” is determined by the contact angle of water on the surface of the release agent layer measured using the following method and the water contact angle of the surface of the intermediate layer on the base film side. If the difference between the contact angle and the contact angle is 30 degrees or more, the intermediate layer is determined to be water-insoluble.
  • the difference in contact angle is preferably 40 degrees or more, more preferably 50 degrees or more. If the value of this difference is small, it means that the components constituting the intermediate layer were eluted into water and the partially exposed release agent layer was measured.
  • the contact angle of water on the surface of the release agent layer is not particularly limited, but is usually 80 degrees or more, preferably 85 degrees or more, and more preferably 90 degrees or more.
  • the upper limit of the contact angle of water on the surface of the release agent layer is usually 150 degrees, preferably 140 degrees, and more preferably 130 degrees.
  • the contact angle of water on the surface of the release agent layer is measured by the sessile drop method using a contact angle meter (manufactured by Kyowa Kaimen Kagaku Co., Ltd., product name "DM-701") according to JIS R3257:1999.
  • a contact angle meter manufactured by Kyowa Kaimen Kagaku Co., Ltd., product name "DM-701"
  • the removal method according to the present embodiment can be carried out using, for example, the green sheet-attached coating layer removal apparatus according to the second embodiment (hereinafter also referred to as the removal apparatus according to the second embodiment).
  • 2A to 2D are cross-sectional views of the removal device 100 according to the second embodiment, and are diagrams for explaining the removal method according to the first embodiment.
  • the second embodiment a case will be described in which the green sheet-attached laminated film 50 shown in FIG. 1A is applied to the removing device 100.
  • the removal device 100 is a laminated film 50 with a green sheet, which has a base film 51 and a coating layer 52 on the surface of which a green sheet 53 is attached, and a cutting means for cutting the laminated film with green sheets into strips.
  • a base film collection means 30 a suspended matter collection means disposed outside the container 121 and on the upper side of the storage means
  • a sediment collection means arranged outside the container 121 and on the bottom side of the storage means 20.
  • the base film collecting means 30 is a means for collecting the base film 51 separated from the coating layer by taking it out from the container 121.
  • the floating matter recovery means is a means for recovering coating layer dregs (floating matter 54C) that are separated from the base film 51 and have green sheets attached thereto in the treated water of the storage means 20.
  • the sediment recovery means is a means for recovering green sheet residue (sediment 53C) separated from both the base film 51 and the coating layer 52 in the treated water of the storage means 20.
  • a heating means 22 is arranged on the bottom side of the housing means 20. In the second embodiment, a case will be described in which hot water HW is used as the treated water.
  • the cutting means (not shown) is a means for cutting the green sheet-attached laminated film into strips.
  • Examples of the cutting means include a cutting machine equipped with a cutter.
  • Examples of the cutter include a cutter blade, water jet cutter, laser cutter, and ultrasonic cutter.
  • the holding means 12 is a means for holding the cut laminated film 50 with green sheets in a container 121 having a plurality of holes 121A.
  • the holding means 12 is a container 121.
  • the container 121 includes a container body 123 and a lid 122 for sealing the container body 123.
  • a handle 122A is attached to the top of the lid 122.
  • the plurality of holes 121A are preferably formed on the entire surface of the container 121 (the side and bottom surfaces of the container body 123 and the lid 122).
  • a pair of support stands 14 are arranged at the lower part of the container 121 so that the bottom surface of the storage tank 21 and the bottom surface of the container 121 are separated from each other.
  • the accommodating means 20 is a means for accommodating the holding means 12 and the hot water HW.
  • the storage means 20 is a storage tank 21.
  • the heating means 22 heats water or hot water via the storage tank 21 to adjust the temperature to the hot water HW at a predetermined temperature.
  • a known heater can be used as the heating means.
  • the arrangement position of the heating means is not particularly limited.
  • the base film collecting means 30 is a means for collecting the base film 51 separated from the coating layer by taking it out from the container 121.
  • the base film collecting means 30 includes a container 121 and a lid 122.
  • the floating matter collecting means is means for collecting the coating layer dregs (floating matter 54C) separated from the base film 51 and attached with the green sheet in the hot water HW of the storage means 20.
  • the floating matter collecting means is arranged outside the container 121 and on the upper side of the containing means 20. It is preferable that the floating matter recovery means has a water injection means for overflowing the hot water HW.
  • the floating matter collecting means is a hose 40 (an example of a water injection means) having a discharge port 41 and an upper discharge pipe 16.
  • the upper discharge pipe 16 is removably connected to the upper discharge port 16A from the storage tank 21.
  • the upper discharge pipe 16 has an upper discharge valve 18 .
  • the upper discharge pipe 16 can be opened and closed by the upper discharge valve 18, and discharge of the floating matter 54C and hot water HW is controlled.
  • the floating matter collection means includes a tray having a mesh structure (for example, a colander, etc.), a filter, a scraping member (for example, a scraping plate and a scraping blade, etc.), and a waste collection member. containers, and any combination thereof.
  • the sediment collecting means is a means for recovering the green sheet residue (sediment 53C) separated from both the base film 51 and the coating layer 52 in the hot water HW of the storage means 20.
  • the sediment recovery means is a lower discharge port (not shown) arranged at the bottom side of the storage tank 21 or a lower discharge pipe (not shown) connected to the bottom side of the storage tank 21.
  • the removal method according to the first embodiment is performed, for example, through the following steps.
  • the cutting process is a process of cutting the green sheet-attached laminated film into small pieces.
  • the cutting step is preferably a step of cutting the green sheet-attached laminated film fed out from the roll into thin pieces.
  • FIG. 1B shows a green sheet-attached laminated film (roll-shaped laminated film 50G) that is unwound from a roll 1G. The residue 920 of the green sheet 53 is attached to the surface of the coating layer 52.
  • a recess 910 is formed, and the coating layer 52 is exposed from the recess 910.
  • the laminated film with green sheets used in the removal method according to the present embodiment is preferably a laminated film with ceramic green sheets that has been used for manufacturing a multilayer ceramic capacitor (MLCC).
  • MLCC multilayer ceramic capacitor
  • the laminated film 50G with green sheets fed out from the roll 1G is cut into strips by passing between a pair of nip rolls and a pair of cutter blades in order, for example, to form the laminated film 50 shown in FIG. 1A, for example. is obtained.
  • the shape of the cut laminated film 50 with green sheets is preferably rectangular.
  • the maximum diameter of the hole 121A of the container 121 is preferably smaller than the minimum diameter of the laminated film 50 with green sheets.
  • the hole 121A of the container 121 includes a hole formed in the container body 123 and a hole formed in the lid 122.
  • the maximum diameter of the hole 121A of the container 121 is defined as the value that maximizes the distance between two parallel straight lines that touch from both sides of the outline of the hole 121A.
  • the minimum diameter of the laminated film 50 with green sheets is defined as the value that minimizes the distance between two parallel straight lines that touch from both sides of the outline of the hole 121A.
  • the maximum diameter of the hole 121A of the container 121 is the length of the diagonal line, and the minimum diameter of the hole 121A is the length of the short side.
  • the maximum diameter of the hole 121A of the container 121 is preferably 15 cm or less, more preferably 10 cm or less, and still more preferably 3 cm or less.
  • the lower limit of the maximum diameter of the hole 121A of the container 121 is preferably 0.2 cm or more.
  • the minimum diameter of the laminated film 50 is preferably 0.3 cm or more, more preferably 0.5 cm or more, and still more preferably 0.7 cm or more.
  • the upper limit of the minimum diameter of the laminated film 50 is preferably 20 cm or less. Note that the laminated film before being cut does not need to be wound around a roll.
  • the cutting step may be a step of cutting the prepared laminated film of any size into strips.
  • the holding process is a process of holding the cut laminated film 50 with green sheets in a container 121 having a plurality of holes 121A.
  • the laminated film 50 is held in the container 121 by storing the laminated film 50 in the container 121 and sealing it with a lid 122.
  • the storage step is a step of storing the container 121 holding the green sheet-attached laminated film 50 (container 121 sealed with a lid 122) and the hot water HW as treated water in the storage tank 21 (FIG. 2A).
  • the accommodation step may be a step of putting the container 121 into the storage tank 21 containing the hot water HW, or a step of putting the hot water HW into the storage tank 21 after the container 121 is stored in the storage tank 21. Good too.
  • the hot water HW may be adjusted to a predetermined temperature.
  • the temperature of the hot water HW is, for example, preferably 40°C or higher, more preferably 60°C or higher. Further, the temperature of the hot water HW is preferably 100°C or lower, more preferably 98°C or lower.
  • the green sheet-attached laminated film 50 is separated from the base film 51 remaining inside the container 121 in the hot water HW of the storage tank 21, and is discharged to the outside of the container 121 and floats on the surface side of the hot water HW.
  • This is a step of separating floating matter 54C and sediment 53C which is discharged to the outside of the container 121 and settles to the bottom side of the storage tank 21 (FIG. 2B).
  • the separated base material film 51 is sunk in the container 121, the separated floating material 54C is floated on the outside of the container 121 and on the surface side of the hot water HW, and the separated sediment 53C is allowed to float on the outside of the container 121.
  • the step is to sink it to the bottom side of the hot water HW.
  • the sediment 53C separated from the laminated film 50 is discharged to the outside of the container 121 because the support stand 14 is disposed at the bottom of the container 121. It sinks further below the bottom (to the bottom of the storage tank 21). Thereby, adhesion of the sediment 53C to the surface of the base film 51 is further suppressed.
  • the separation step is performed, for example, while stirring the hot water HW using a stirring means, while vibrating the container 121 using a vibration means, or in a modification described below. It is preferable to carry out the process while rotating the container 121 as in 2.
  • the immersion time of the laminated film 50 in the hot water HW may be, for example, 3 minutes or more and 120 minutes or less, or 5 minutes or more and 100 minutes or less.
  • the base film recovery process is a process of recovering the separated base film 51 from inside the container 121 (FIG. 2D).
  • the base film recovery process is a process of taking out the container 121 from the storage tank 21 and recovering the base film 51 from the container 121. Since the floating matter 54C and the sediment 53C separated from the laminated film 50 are discharged to the outside of the container 121, only the base film 51 remains inside the container 121. Therefore, by taking out the base film 51 from the container 121, the base film 51 with no deposits on its surface can be recovered. Water droplets are removed from the recovered base film 51 by a known method.
  • the floating matter collection process is a process of collecting the separated floating matter 54C from the outside of the container 121 and from the upper side of the storage tank 21 (FIG. 2C).
  • the floating matter 54C is the residue of the coating layer 52 that has been separated from the base film 51 and has the green sheet 53 attached thereto.
  • the floating matter recovery means causes the hot water HW in the storage tank 21 to overflow, and the floating matter 54C flowing out due to the overflow of the hot water HW is discharged from the storage tank 21 through an upper discharge port 16A disposed on the upper side of the storage tank 21. It is preferable that the step is to induce and recover. In the case of FIG.
  • the floating matter collecting means is a step of filtering out the floating matter 54C using a filter that is removably provided just below the water surface of the storage tank 21.
  • the floating matter collecting step may be a step of directly collecting the floating matter 54C from the opening 21A of the storage tank 21 using a floating matter collecting means.
  • the sediment recovery process is a process of recovering the separated sediment 53C from the outside of the container 121 and from the bottom side of the storage tank 21.
  • the sediment 53C is green sheet residue separated from both the base film 51 and the coating layer 52.
  • the sediment recovery step is a step of recovering the separated sediment 53C from a discharge port arranged at the bottom side of the storage tank 21 or a discharge pipe connected to the discharge port.
  • the storage tank 21 as the storage unit 20 may include a pressure lid that seals the storage tank 21 and a pressurizing unit that pressurizes the inside of the storage tank 21.
  • the storage tank 21 provided with a pressure lid and a pressurizing means may be referred to as a pressurized storage tank.
  • the pressurizing means includes a heating means that heats water or hot water to obtain superheated water (treated water), and a pressure control means that controls the atmospheric pressure in the pressurized storage tank to a pressure higher than 1 atmosphere.
  • a known heater can be used as the heating means.
  • the pressure control means include pressure regulating valves (for example, safety valves), pressure regulating valves (for example, relief valves), and pressure regulating valves used in pressure cookers (for example, weight type and spring type).
  • the pressure control means may include a pressure sensor that measures the pressure inside the pressurized reservoir.
  • the pressure control means may further include a control section connected to a pressure sensor, a pressure regulating valve, and the like. When the pressure control means is a pressure regulating valve, the pressure in the pressurized storage tank is adjusted to a predetermined pressure, for example, by controlling the opening area of a steam outlet formed in the pressure lid.
  • the opening or closing of the steam outlet by the pressure regulating valve may be controlled, for example, by a computer control unit according to the pressure value acquired by the pressure sensor, or by using a relief valve to control the pressure in the pressurized storage tank. It may be controlled by a spring force so that the pressure reaches a set pressure, or it may be controlled passively according to pressure changes in a pressurized storage tank, such as when using a pressure regulating valve used in a pressure cooker. .
  • the removal method according to Modification 1 is performed, for example, through the following steps. Points different from the removal method according to the first embodiment will be explained.
  • the removal method according to Modification 1 is an example in which superheated water is used as the treated water.
  • the housing process is a process of housing the container 121 holding the green sheet-attached laminated film 50 and water or hot water in a pressurized storage tank.
  • the green sheet-attached laminated film 50 is separated from the base film 51 remaining inside the container 121 by heating the water or hot water and increasing the pressure in the pressurized storage tank to a pressure higher than 1 atmosphere.
  • the step of separating the floating matter 54C which is discharged to the outside of the container 121 and floats on the surface side of the treated water, and the sediment 53C which is discharged to the outside of the container 121 and settles to the bottom side of the pressurized storage tank. Water or hot water in the pressurized storage tank is heated by a heating means to generate water vapor, thereby increasing the pressure in the pressurized storage tank to a pressure higher than 1 atmosphere.
  • the water or hot water in the pressurized storage tank becomes superheated water by being heated under pressure.
  • the atmospheric pressure in the pressurized storage tank and the temperature of the superheated water are determined by Boyle-Charles' law, and are preferably in the following ranges.
  • the atmospheric pressure in the pressurized storage tank is preferably 1.2 atmospheres or more, more preferably 1.4 atmospheres or more, from the viewpoint of removing the coating layer with green sheets in a shorter time.
  • the atmospheric pressure in the pressurized storage tank is preferably 9.93 atmospheres or less, more preferably 4.7 atmospheres or less, from the viewpoint of suppressing melting of the resin component contained in the laminated film.
  • the temperature of the superheated water is preferably 105°C or higher, more preferably 110°C or higher, from the viewpoint of removing the coating layer with green sheets in a shorter time.
  • the temperature of the superheated water is preferably 180°C or less, more preferably 150°C or less, from the viewpoint of suppressing melting of the resin component contained in the laminated film.
  • the holding time H1 of the laminated film in superheated water when the pressure inside the pressurized storage tank is more than 1 atmosphere (preferably when the target pressure is present) is, for example, The time is preferably 5 minutes or more, and more preferably 10 minutes or more. Further, the holding time H1 is preferably 60 minutes or less, more preferably 40 minutes or less.
  • the laminated film in the separation step, is held in a container having a plurality of holes and immersed in superheated water in a pressurized storage tank, thereby separating the base film and the intermediate film.
  • Superheated water more easily infiltrates the interface with the layer.
  • the coating layer with green sheets can be removed from the laminated film more easily and in a shorter time.
  • the separation step may be performed while rotating the container 121.
  • FIG. 3 is a diagram for explaining the separation process according to Modification 2.
  • the rotating shaft 42 is removably fixed to the lid 122 of the container 121.
  • the rotation time of the rotating shaft 42 is preferably within the same range as the immersion time of the laminated film 50 in the hot water HW.
  • the rotation time of the rotating shaft 42 may be 3 minutes or more and 120 minutes or less, or 5 minutes or more and 100 minutes or less.
  • the rotation speed of the rotating shaft 42 may be, for example, 10 rpm or more and 1000 rpm or less, 15 rpm or more and 750 rpm or less, or 20 rpm or more and 500 rpm or less.
  • the removal device 100 according to the second embodiment may include a circulation means that returns the hot water HW or water W in the storage tank 21 to the storage tank 21 again after filtering it.
  • the removal device according to Modification 1 may have a circulation means for filtering the treated water in the pressurized storage tank after the pressure has been returned to normal pressure, and then returning it to the pressurized storage tank again.
  • the laminated film with green sheets used in the embodiment includes a base film, a coating layer, and a green sheet.
  • the coating layer includes an intermediate layer and a release agent layer.
  • the intermediate layer is arranged between the base film and the release agent layer.
  • the green sheet is attached to any position on the surface of the release agent layer.
  • the intermediate layer may be a single layer, or may be a multilayer consisting of two or more intermediate layers of the same or different types.
  • the release agent layer may be a single layer, or may be a multilayer consisting of two or more release agent layers of the same or different types.
  • the laminated film preferably has a structure in which the base film and the intermediate layer are directly laminated, from the viewpoint of removing the green sheet-attached coating layer from the laminated film and making it easy to recover the remaining base film.
  • direct lamination refers to a configuration in which, for example, there is no other layer between the base film and the intermediate layer, and the layers are in direct contact with each other.
  • the base film, the intermediate layer, the release agent layer, and the green sheet may be directly laminated in this order. That is, the structure may be such that there is no other layer between the base film, the intermediate layer, the release agent layer, and the green sheet, and the layers are in direct contact with each other.
  • a resin film is used in which a resin component that is scheduled to be collected is formed into a film.
  • resin films include polyester films such as polyethylene terephthalate film, polybutylene terephthalate, and polyethylene naphthalate; polyolefin films such as polyethylene film and polypropylene film; polyimide film; polyamide film; polycarbonate film; polyacetate film; ethylene-vinyl acetate copolymer.
  • Ethylene-(meth)acrylic acid copolymer film ethylene-(meth)acrylic acid ester copolymer film; cycloolefin polymer film; polyurethane film; polyphenylene sulfide film; cellophane; etc.
  • the density of the base film is preferably greater than the density of water at 40° C., and more preferably 1.0 g/cm 3 or more. This makes it easier for the base film separated from the laminated film to remain submerged in the treated water in the container, so the base film can be easily recovered from the container by removing the container from the storage tank. can.
  • polyester films are preferred because they have a density higher than that of water at 40°C and excellent heat resistance and strength.
  • a polyester film containing any one of polyethylene terephthalate, polybutylene terephthalate, and polyethylene naphthalate as a main component is preferable.
  • the term "main component” or “main component” means that the proportion of the material in the entire mass is 50% by mass or more.
  • the resin film may contain known fillers, colorants, antistatic agents, antioxidants, organic lubricants, catalysts, and the like. Further, the resin film may be transparent or may be colored as desired.
  • at least one surface of the base film may be subjected to surface treatment such as sputtering, corona discharge, flame, ultraviolet irradiation, electron beam irradiation, and etching treatment such as oxidation, as necessary.
  • the thickness of the base film is not particularly limited, but from the viewpoint of strength, rigidity, etc., it is preferably 10 ⁇ m or more and 500 ⁇ m or less, more preferably 15 ⁇ m or more and 300 ⁇ m or less, and even more preferably 20 ⁇ m or more and 200 ⁇ m or less.
  • the release agent layer is preferably a layer formed from a release agent composition.
  • the release agent composition used to form the release agent layer is not particularly limited as long as it has release properties, and examples include silicone compounds; fluorine compounds; long-chain alkyl group-containing compounds; olefin resins, diene
  • a release agent composition having a thermoplastic resin material such as a thermoplastic resin as a main component can be used.
  • a release agent composition containing an energy ray-curable or thermosetting resin as a main component.
  • examples of the silicone compound include silicone compounds having organopolysiloxane as a basic skeleton. Further, examples of the silicone compound include thermosetting silicone compounds such as addition reaction type and condensation reaction type; energy ray curing type silicone compounds such as ultraviolet ray curing type and electron beam curing type; and the like.
  • examples of the fluorine compound include fluorine silicone compounds, fluorine boron compounds, and poly(perfluoroalkylene ether) chain-containing compounds.
  • the long-chain alkyl group-containing compound may be, for example, a polyvinyl carbamate obtained by reacting a long-chain alkyl isocyanate with a polyvinyl alcohol-based polymer. , an alkyl urea derivative obtained by reacting polyethyleneimine with a long-chain alkyl isocyanate, or a copolymer of a long-chain alkyl (meth)acrylate.
  • a long-chain alkyl-modified alkyd resin using a long-chain fatty acid as a modifier may be used as an alkyd resin obtained by a condensation reaction of a polyhydric alcohol and a polybasic acid.
  • a release agent composition containing an energy ray curable resin as a main component includes, for example, an energy ray curable compound having a reactive functional group selected from a (meth)acryloyl group, an alkenyl group, and a maleimide group, and a polyorganosiloxane.
  • an energy ray-curable compound and a polyorganosiloxane having mutually different molecular structures, polarities, and molecular weights are used.
  • the components become segregated near the outer surface of the release agent layer, and are then hardened by energy rays to fix the segregation. Thereby, the releasability of the release agent layer can be improved.
  • the release agent composition containing an energy ray curable resin as a main component may further contain a photopolymerization initiator.
  • release agent compositions containing a thermosetting resin as a main component include release agent compositions containing a melamine resin as a main component and release agent compositions containing an epoxy resin as a main component.
  • release agent compositions containing a melamine resin as a main component include compositions containing a melamine resin as a main ingredient, an acid catalyst for thermosetting the melamine resin, and a polyorganosiloxane that imparts release properties to the release agent layer.
  • a release agent composition containing an epoxy resin as a main component includes an epoxy resin as a main ingredient, an acidic or basic thermosetting catalyst for thermally curing the epoxy resin, and a polyorganic resin that imparts releasability to the release agent layer.
  • compositions containing siloxanes may be mentioned. Before curing, components derived from polyorganosiloxane become segregated near the outer surface of the release agent layer, and then harden to fix the segregation. Thereby, the releasability of the release agent layer can be improved.
  • the release agent layer may contain other additives in addition to the above-mentioned resin components.
  • other additives include anti-aging agents, light stabilizers, flame retardants, conductive agents, antistatic agents, and plasticizers.
  • the thickness of the release agent layer can be selected as appropriate and is not particularly limited, but for example, preferably 0.02 ⁇ m or more and 5 ⁇ m or less, more preferably 0.03 ⁇ m or more and 2 ⁇ m or less, and still more preferably 0.03 ⁇ m or more and 5 ⁇ m or less. 05 ⁇ m or more and 1.5 ⁇ m or less.
  • the intermediate layer is a layer made of a silane compound that is hydrophilic and water-insoluble, and exhibits polycondensation properties by hydrolysis, from the viewpoint of easier removal of the coating layer from the surface of the intermediate layer on the base film side. It is preferable that there be.
  • the silane compound preferably contains at least one kind selected from a tetrafunctional silane compound represented by the following general formula (a) and an oligomer thereof as a main component.
  • Si(OR) p (X) 4-p (a) [In general formula (a), R represents an alkyl group, and X represents a halogen atom. When a plurality of R's exist, the plurality of R's may be the same or different from each other. When a plurality of Xs exist, the plurality of Xs may be the same or different from each other. p represents an integer from 0 to 4. ] The number of carbon atoms in the alkyl group is preferably 1 or more and 4 or less.
  • the silane compounds represented by the general formula (a) may be used alone or in combination of two or more.
  • the silane compound represented by the general formula (a) preferably includes a silane compound in which p in the general formula (a) is 4.
  • the silane compound in which p in the general formula (a) is 4 ie, the tetrafunctional silane compound
  • At least one of tetramethoxysilane and tetraethoxysilane, or a mixture of tetramethoxysilane and tetraethoxysilane is preferred.
  • Methodsilicate 51 is an average tetramer oligomer of methoxysilane
  • Methodhylsilicate 53A is an average heptamer oligomer of tetramethoxysilane
  • “Ethylsilicate 40” is an average pentamer oligomer of tetraethoxysilane
  • “Ethylsilicate 48” which is an average 10-mer oligomer of tetraethoxysilane
  • EMS-485" which is a mixture of an average 10-mer oligomer of tetramethoxysilane and an average 10-mer oligomer of tetraethoxysilane (both , manufactured by Colcoat Co., Ltd.).
  • the thickness of the intermediate layer is preferably 0.01 ⁇ m or more and 1 ⁇ m or less, more preferably 0.03 ⁇ m or more and 0.5 ⁇ m or less, and even more preferably 0.01 ⁇ m or more and 1 ⁇ m or less, from the viewpoint of easy water infiltration when the intermediate layer comes into contact with water. is 0.05 ⁇ m or more and 0.3 ⁇ m or less.
  • the green sheet is obtained by applying a ceramic slurry to the surface of the release agent layer opposite to the intermediate layer, and then drying the ceramic slurry. Coating can be performed using, for example, a slot die coating method, a doctor blade method, or the like.
  • the ceramic slurry includes ceramic powder, a binder component, a solvent, and the like.
  • the ceramic powder include dielectric powders such as barium titanate, titanium oxide, alumina, zirconia, zinc oxide, aluminum silicate, and silicon nitride.
  • the binder component include butyral resins and acrylic resins.
  • the solvent include organic solvents and aqueous solvents.
  • the laminated film with a green sheet used in each embodiment of the present invention since the green sheet is not attached to the entire surface of the release agent layer, the residue of the coating layer with the green sheet after the separation process (in FIG. 2B) The green sheet partially remains on the surface of the release agent layer and is attached to the floating object 54C), or is not attached to the floating object 54C. Therefore, the properties of the residue in the coating layer with the green sheet are almost the same as the properties of the residue in the coating layer to which no green sheet is attached. Since the laminated film with green sheets used in each embodiment of the present invention has a hydrophilic and water-insoluble intermediate layer, the removed residue of the coating layer with green sheets (floating matter 54C in FIG.
  • the dregs with this structure is immersed in water, the surface of the release agent layer faces the air due to surface tension, and the surface of the intermediate layer faces the water, resulting in stability. In other words, debris with this configuration is more likely to exist at the boundary between water and air than in water.
  • the dregs of the coating layer with green sheets is an extremely thin film, so even if the density is a little high, the buoyancy due to surface tension will prevail, and since the intermediate layer is water-insoluble, it can continue to float on the surface of the water. Conceivable.
  • the laminated film used in each embodiment is generally used when manufacturing, transporting, storing, etc. other functional sheets and various parts used for specific applications. Used to protect the surfaces of sheets and parts. After actually fulfilling the role of protecting these parts, etc., they are often peeled off from the surface and discarded. Therefore, by using the laminated film, the coating layer with green sheet and the base film can be easily separated from the laminated film, so this application has a high contribution from the viewpoint of resource conservation and environmental protection. .
  • the present invention is not limited to the above embodiments.
  • the present invention may include modifications, improvements, etc. within the scope of achieving the objectives of the present invention.

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  • Environmental & Geological Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Separation, Recovery Or Treatment Of Waste Materials Containing Plastics (AREA)

Abstract

Procédé de retrait d'une couche de revêtement fixée sur une feuille verte, le procédé comprenant les étapes suivantes : découpe d'un film stratifié en feuilles vertes en morceaux ; maintien du film stratifié découpé (50) dans un récipient (121) présentant une pluralité de trous (121A) ; stockage du récipient (121) et de l'eau de traitement (par ex, eau chaude (HW)) dans un réservoir de stockage (21) ; séparation du film stratifié (50) dans l'eau de traitement en un film de base qui reste dans le récipient, des matières flottantes qui sont rejetées à l'extérieur du récipient et flottent dans l'eau de traitement, et des sédiments qui sont rejetés à l'extérieur du récipient et se déposent dans le réservoir de stockage (21) ; collecte du film de base, collecte des matières flottantes et collecte des sédiments, les matières flottantes étant les résidus de la couche de revêtement fixée sur la feuille verte, les sédiments étant les résidus de la feuille verte, et la couche de revêtement comprenant une couche intermédiaire et une couche d'agent de démoulage.
PCT/JP2023/033075 2022-09-15 2023-09-11 Procédé pour retirer la couche de revêtement fixée à la feuille verte, et dispositif pour retirer la couche de revêtement fixée à la feuille verte WO2024058132A1 (fr)

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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH03193417A (ja) * 1989-10-13 1991-08-23 Davidson Textron Inc インターフェース位置で連結する層状プラスチックを分離及び回収するための方法
JP2004050681A (ja) * 2002-07-22 2004-02-19 Toray Ind Inc セラミックグリーンシートの製造方法
JP2009291690A (ja) * 2008-06-03 2009-12-17 Tdk Corp 剥離フィルムの洗浄方法、並びに基材フィルム及び剥離フィルムのリサイクル方法
KR20150109125A (ko) * 2014-03-19 2015-10-01 (주)엔에이치리사이텍컴퍼니 Pet 필름의 추출장치

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH03193417A (ja) * 1989-10-13 1991-08-23 Davidson Textron Inc インターフェース位置で連結する層状プラスチックを分離及び回収するための方法
JP2004050681A (ja) * 2002-07-22 2004-02-19 Toray Ind Inc セラミックグリーンシートの製造方法
JP2009291690A (ja) * 2008-06-03 2009-12-17 Tdk Corp 剥離フィルムの洗浄方法、並びに基材フィルム及び剥離フィルムのリサイクル方法
KR20150109125A (ko) * 2014-03-19 2015-10-01 (주)엔에이치리사이텍컴퍼니 Pet 필름의 추출장치

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