JP2018187808A - Method for sorting and collecting composite material and sorting and collecting apparatus used for the same - Google Patents

Abstract

PROBLEM TO BE SOLVED: To provide a method for sorting and collecting composite material efficiently sorting and recovering composite material in which resin film are laminated to each other and for each kind of resin film and a sorting and collecting apparatus used for the same.SOLUTION: A repetition step of step S3 repeating a dissolution step of dissolving a soluble layer by maintaining a solvent at a first temperature inside a dissolution tank in which the solvent is stored and producing a solution containing a solute in which the soluble layer is dissolved and an insoluble layer, and a separation step of separating the insoluble layer from the solution by m times (m=3), a drying step of step 4 drying the separated insoluble layer, a distillation step of step 5 distilling the solution after separation of the insoluble layer and the solute precipitated by cooling this solution and recovering the solute and purifying the solvent after the separation step of step S2 (1), and returning step of step 6 returning the refined solvent to the dissolution tank, are provided.SELECTED DRAWING: Figure 3

Description

  The present invention relates to a method for separating and collecting a composite material composed of a plurality of types of resin materials and a separation and collection apparatus used therefor, and in particular, efficiently separates a composite material in which a plurality of types of resin films are difficult to separate. The present invention relates to a fraction collection method for collection and a fraction collection device used therefor.

Conventionally, as a method for separating mixed waste plastic in which a plurality of types of plastics are mixed, various methods for physically separating using specific gravity and optical characteristics have been proposed.
On the other hand, various composite materials in which aluminum foil, a plurality of types of resin films, and the like are laminated have been developed for the purpose of providing various functions such as oxygen barrier properties and weldability. Specifically, this composite material includes, for example, polyethylene (PE), polypropylene (PP), polyamide resin (PA), ethylene / vinyl acetate copolymer resin (EVA), polyvinyl alcohol (PVA), and ethylene-vinyl alcohol copolymer. Resin films such as coalescence (EVOH), polyvinylidene chloride (PVDC), polyethylene terephthalate (PET), polycarbonate (PC), acrylic resin (PMMA), and cellophane are difficult to separate from each other with or without an adhesive. It is closely attached to.
On the other hand, the conventional separation method described above can separate mixed waste plastics simply by mixing a plurality of types of plastics, but a composite material in which resin films are closely adhered to each other is laminated. It is difficult to sort and recycle by type. Therefore, although some composite materials are cascade recycled, there are few examples of material recycling.
Thus, in recent years, techniques for separating and collecting composite materials have been developed, and several inventions have already been disclosed.

First, Patent Documents 1 to 3 each disclose an invention relating to a processing method for separating plastic waste using a separation solvent under the name of “processing method of plastic waste”.
The inventions disclosed in Patent Literature 1 to Patent Literature 3 are all (1) a dissolution step in which a separation solvent is brought into contact with plastic waste to produce a solid solution composed of a separation solvent solution containing plastic and undissolved plastic, 2) Solid-liquid separation step for separating the separate solvent solution from the solid matter, (3) Decomposition step for concentrating the fractionated solution followed by thermal decomposition, (4) Contacting the solid with a heated non-condensable gas to form a solid A fractionation solvent evaporation step for evaporating the fractionation solvent contained in the product to produce a solid fraction having a fractionation solvent content reduced and a gaseous mixture of fractionation solvent vapor and non-condensable gas; (5) liquid fractionation solvent; And (6) a heating step for heating the non-condensable gas, and (7) a circulation step for circulating the heated non-condensable gas to the fractional solvent evaporation step. To do.
According to the plastic waste processing method having such characteristics, it is possible to efficiently separate a soluble component and an insoluble component in a separation solvent. Moreover, the fractionation solvent contained in the solid can be efficiently separated and recovered, and the solid can be recovered as a solid with a low fractionation solvent content. Therefore, it is possible to obtain cracked product oil useful as a fuel or reaction raw material from plastic waste with a high yield.

Next, Patent Document 4 discloses an invention relating to a separation and collection method for separating and collecting a composite material such as a laminated film of metal foil under the name of “composite material separation and collection method”.
The invention disclosed in Patent Document 2 constitutes a composite material by at least crushing the composite material into small pieces to obtain a crushed material, and contacting the crushed material with an osmotic release agent solution. Each thin film material is peeled to obtain a crushed mixture of thin film materials, and the crushed mixture of thin film materials is separated by a plurality of specific gravity sorting processes using a plurality of specific gravity sorting liquids having different specific gravities. And a separation and recovery step of separating and recovering into a plurality of thin film materials.
According to the method for separating and recovering composite materials having such characteristics, a laminate film can be obtained by performing the separation process by specific gravity sorting appropriately using different specific gravity sorting liquids according to the type of thin film material to be separately collected. The thin film materials such as the synthetic resin film and the aluminum foil separated from the crushed mixture of the thin film materials constituting each can be separately collected and reused.

Further, Patent Document 5 discloses an invention relating to a recovery method for recovering copper and nickel from resin plating waste material under the name of “metal component recovery method of resin plating waste material”.
The invention disclosed in Patent Document 5 increases the abundance ratio of the plating film component in the metal component recovery method of the resin plating waste material having the copper plating film integrally formed on the surface of the resin base material and the nickel plating film. It has a metal component-enriched mixture forming step and a metal component recovery step after which the mixture is heated and melted to obtain an alloy containing copper and nickel.
According to the metal component recovery method for resin plating waste having such characteristics, copper and nickel can be recovered in large quantities and at low cost without separating and removing the copper component.

Japanese Patent Laid-Open No. 11-21373 Japanese Patent Laid-Open No. 11-116728 JP-A-11-228730 JP 2014-19003 A JP 2003-293048 A

However, in the inventions disclosed in Patent Documents 1 to 3, when the fractionation solvent solution containing plastic is heated in the dissolution step (1), only plastics suitable for oiling such as PE, PP, PS, etc. Dissolves. Therefore, in the concentration step (3), the fractionated solvent solution in which the plastic is dissolved is concentrated and further distilled in the distillation step described in FIG. Since oil and light oil contain the high-boiling point component of the fractionation solvent in addition to the above-described plastic-soluble component, it is difficult to recover only the plastic-soluble component. That is, there is a problem that horizontal recycling of plastic is difficult.
In the dissolution step (1), the hydrocarbon-based plastic is brought into contact with a fractionation solvent at 50 to 200 ° C. for 5 minutes or more, preferably 10 to 60 minutes. There is a possibility that the resin in the inner layer of the laminated resin film cannot be sufficiently dissolved and a composite material such as a laminate film cannot be separated and collected.
Further, the inventions disclosed in Patent Documents 1 to 3 are intended for general waste, and do not target PA, EVA, EVOH, PC, PMMA, and the like that are frequently used for laminate films. For this reason, it is considered difficult to separate and collect such a composite material by the inventions disclosed in Patent Documents 1 to 3.

  Next, in the invention disclosed in Patent Document 4, the release agent solution is specifically an alkaline aqueous solution. On the other hand, since the normal laminate film is heat-sealed between resin films directly or via a resin film having both affinity, the resin film cannot be peeled off with an alkaline aqueous release agent solution, There is a problem that the laminated film cannot be collected separately.

  And in the invention disclosed by patent document 5, it makes it a subject to collect | recover a metal component from a resin base material efficiently, and does not make it a subject to reproduce | regenerate both a metal component and a resin base material. Therefore, the invention disclosed in Patent Document 5 cannot be applied as a method for separately collecting a composite material such as a laminate film.

  The present invention has been made in response to such conventional circumstances, and efficiently separates composite materials in which resin films are laminated in close contact with each other regardless of the presence or absence of an adhesive. It is an object of the present invention to provide a method for separating and recovering a composite material that can be recovered and horizontally recycled, and a separation and recovery apparatus used therefor.

  In order to achieve the above object, a first invention is a method for separating and collecting a composite material having a plurality of types of laminated resin films, wherein the composite material is formed on at least one of its surfaces and selected as a solvent. A soluble layer that dissolves automatically, and an insoluble layer that is in close contact with the soluble layer and insoluble in the solvent, and the solvent is maintained at a first temperature inside the dissolution tank in which the solvent is stored. And repeating a dissolution process for generating a solution containing a solute and an insoluble layer in which the soluble layer is dissolved and a separation process for separating the insoluble layer from the solution m times (m is a natural number determined as desired), and After the first separation step, the solution after the insoluble layer has been separated and / or the distillation of the solute deposited by cooling the solution, the distillation step of collecting the solute and purifying the solvent, There are as many dissolution tanks as m times. Characterized in that it is.

In the invention having such a configuration, the soluble layer and the insoluble layer constituting the composite material are different types of resin films, and are in close contact with each other via an adhesive or without an adhesive. It is difficult.
Furthermore, the composite material is, for example, a laminate in which a soluble layer and an insoluble layer are laminated, or a laminate in which an insoluble layer is sandwiched between the soluble layer and the soluble layer.
Moreover, 1st temperature means the temperature range which a solvent can melt | dissolve a soluble layer.

  In the invention having the above-described configuration, in the first melting step (m = 1), the composite material is charged into the melting tank in which the solvent is stored. Since this solvent is maintained at the first temperature, the soluble layer is dissolved by the solvent to become a solute. Since the insoluble layer is not dissolved by such a solvent, a solution containing the solute and the insoluble layer is generated.

In the first separation step (m = 1) performed following the first dissolution step, only the insoluble layer is separated from the solution, for example, by filtration.
In addition, it is thought that the solute adsorb | sucks to the isolate | separated insoluble layer. However, for example, when the amount of solute adsorbed is determined by sampling the insoluble layer and the amount of solute adsorbed is determined to be less than the allowable amount, the second and subsequent repetition steps may not be performed. . On the other hand, if not, a dissolution step and a separation step are added.

In the second (m = 2) dissolution step carried out following the first separation step, a dissolution tank in which a new solvent maintained at the first temperature is stored is newly installed. Therefore, in the first separation step, the insoluble layer separated from the solution is put into the newly installed dissolution tank. Thereby, the solution adsorbed on the insoluble layer separated in the first separation step is washed, and a new solution is generated.
Subsequently, in the second (m = 2) separation step carried out following the second dissolution step, only the insoluble layer is separated from the newly generated solution, as in the first separation step.
In the insoluble layer separated in the second separation step, when it is determined that the solute adsorption amount is not more than the allowable amount in the same manner as described above, the third and subsequent (m = 3) dissolution steps are not performed. On the other hand, if this is not the case, a third dissolution step and a separation step are performed. Thereafter, when an appropriate number of times (maximum m times) of the dissolution step and the separation step are completed, the repetition step is completed, and the separated insoluble layer becomes one of the finally separated recovered materials.

Note that a solution containing a high concentration of solute remains after the first separation step. A distillation step is performed to recover this solute.
In the distillation step, the solution after the insoluble layer is separated and / or the solute deposited by standing or cooling the solution with a cooling device is distilled. As described above, the former solution contains a high concentration of solute. Moreover, it is considered that the solution is adsorbed on the latter deposited solute. Accordingly, the object to be distilled by distillation in this step is the former solution and / or the solution adsorbed on the deposited solute. By this distillation, the former solution is separated into a solute and a solvent, and the solution adsorbed on the latter deposited solute is separated into a solute and a solvent. That is, the solute can be recovered and the solvent can be purified. This collected solute becomes the other of the collected materials finally separated. However, the distillation step may be performed at any timing in the repeating step as long as it is performed after the first separation step.

Next, 2nd invention is equipped with the return process which returns the refine | purified solvent to at least any 1 dissolution tank of m dissolution tanks after a distillation process in 1st invention. Features.
In such a configuration, in addition to the action of the first invention, in the returning step, the purified solvent is returned to at least one of the m dissolving tanks. The purity of the solvent used is improved. Therefore, cleaning of the insoluble layer in the dissolution process is promoted.

Furthermore, the third invention is the first or second invention, wherein the soluble layer is made of polyethylene or polypropylene, the solvent is xylene, toluene or a mixture thereof, and the first temperature is 90 ° C. or higher. And not more than the boiling point of the solvent.
In the invention having such a configuration, the insoluble layer is a resin that does not dissolve in xylene or toluene, such as PA, PET, PVA, EVOH, and PDVC. When the solvent is a mixture of xylene and toluene, an upper limit value of the first temperature is set corresponding to the mixing ratio (weight ratio).
In the invention of the above configuration, in addition to the action of the first or second invention, polyethylene or polypropylene and a resin that does not dissolve in xylene or toluene such as PA are the final recovered product. And if a distillation process is implemented, high purity xylene or toluene will be collect | recovered.

In a fourth aspect based on the first or second aspect, the soluble layer is made of an ethylene / vinyl acetate copolymer resin, the insoluble layer is made of polyethylene or polypropylene, the solvent is cyclohexane, The temperature of 1 is 40 degreeC or more and below the boiling point of a solvent, It is characterized by the above-mentioned.
In the invention having such a configuration, in addition to the action of the first or second invention, polyethylene or polypropylene and an ethylene / vinyl acetate copolymer resin are finally collected. And if a distillation process is implemented, highly purified cyclohexane will be collect | recovered.

Subsequently, in a fifth invention according to the first or second invention, the soluble layer is made of an acrylic resin, the insoluble layer is made of polycarbonate, and the solvent is a mixture of methanol and ethyl acetate, or a ketone solvent. The first temperature is at least 20 ° C. and not more than the boiling point of the solvent.
In the invention having such a configuration, the ketone solvent is acetone, methyl ethyl ketone, methyl isobutyl ketone, or the like. When the solvent is a mixture of methanol and ethyl acetate, the upper limit value of the first temperature is set corresponding to the mixing ratio (weight ratio).
In the invention of the above configuration, in addition to the action of the first or second invention, the polycarbonate and the acrylic resin are finally collected. And if a distillation process is implemented, the mixture of high purity methanol and ethyl acetate, or the said ketone solvent will be collect | recovered.

  Subsequently, according to a sixth aspect of the invention, in any one of the first to fifth aspects, when the composite material includes an aluminum layer, the aluminum layer is dissolved by storing an aluminum layer solvent that selectively dissolves the aluminum layer. Inside the tank, an aluminum layer dissolving step is provided in which the aluminum layer is dissolved by maintaining the solvent for the aluminum layer at the second temperature. When the aluminum layer covers the soluble layer, On the other hand, when the aluminum layer is provided between the soluble layer and the insoluble layer, the aluminum layer solvent is an alkali or an acid, while the aluminum layer is provided between the soluble layer and the insoluble layer. The temperature is 30 ° C. or higher and 90 ° C. or lower.

In the invention having such a configuration, the aluminum layer is deposited on, for example, a soluble layer or an insoluble layer. Among these, when the aluminum layer covers the soluble layer, if the aluminum layer is not removed first, the solvent will not reach the soluble layer and cannot be dissolved. An aluminum layer melting step is performed.
On the other hand, when the aluminum layer is provided between the soluble layer and the insoluble layer, the aluminum layer dissolving step is performed on the insoluble layer after the repeating step, that is, after the insoluble layer is finally recovered. To do.

In the invention of the above configuration, in addition to the action of any one of the first to fifth inventions, the composite material or the finally recovered insoluble layer is placed inside the aluminum layer dissolution tank storing the aluminum layer solvent. It is thrown. Since the aluminum layer solvent is maintained at the second temperature, the aluminum layer dissolves in the aluminum layer solvent and changes to an aluminum solute. On the other hand, the soluble layer and the insoluble layer are not dissolved in the solvent for the aluminum layer.
Therefore, when the aluminum layer melting step is performed before the first melting step, a solution containing the composite material from which the aluminum solute and the aluminum layer have been removed is generated inside the aluminum layer melting tank. Further, the composite material from which the aluminum layer has been removed is put into a dissolution tank installed in the first dissolution step, and then the soluble layer and the insoluble layer are separated and recovered.

In addition, when the aluminum layer dissolving step is performed after the m-th repeating step, a solution containing an insoluble layer from which the aluminum solute and the soluble layer have been removed is generated inside the aluminum layer dissolving tank. Therefore, the insoluble layer and the soluble layer already removed are separated and collected.
Thus, the soluble layer and the insoluble layer become the final recovered product.

Furthermore, the seventh invention is a separation and recovery device used in the method for separating and recovering a composite material according to any one of the first to sixth inventions, wherein m pieces of the dissolution tanks and m pieces of the dissolution tanks are used. M heaters each installed and respectively maintaining the solvent at a first temperature; at least one filtration vessel containing the composite material or insoluble layer and filtering the insoluble layer from the solution; and m The m dissolution members respectively provided in the dissolution tanks for agitating the composite material or the insoluble layer accommodated in the filtration container, m motors for respectively driving the m agitation members, and the first dissolution A distillation apparatus for distilling a solute deposited by cooling a storage tank in which the solution stored in the tank is transferred and stored, a solution stored in the first dissolution tank, and / or a solution stored in the storage tank Where m is a natural number of 2 or more N-th (n = m, m-1,..., 2, where n is a natural number of 2 or more) the height of the upper edge of each of the dissolution tanks is above the (n-1) -th dissolution tank. Each of the flow paths is arranged so as to be equal to or higher than the edge height, and a channel through which the solution flows from the nth dissolution tank to the (n−1) th dissolution tank is provided.
That is, when the dissolution tanks are arranged next to each other, the height of the upper edge of the dissolution tank arranged on the upstream side is always the height of the upper edge of the dissolution tank arranged on the downstream side. It will be arranged above.

  In the invention having such a configuration, for example, when m is 3, the first dissolution tank installed in the first dissolution process among the three dissolution tanks is a composite housed in a filtration container. Material is charged. The insoluble layer accommodated in the filtration container is put into the second to third dissolution tanks installed in the second to third dissolution steps, respectively. When one filtration container is provided, the filtration container is sequentially moved to the first to third dissolution tanks and used. On the other hand, when three filtration containers are provided, they are used by immersing them in three dissolution tanks without moving them.

  When the composite material is put into the first dissolution tank, the solvent is maintained at the first temperature by the first heater, and the first stirring member is driven by the first motor. Therefore, the solution is stirred and the dissolution of the soluble layer is promoted. In addition, when the insoluble layer is put into the second to third dissolution tanks, respectively, the solution is similarly stirred by the stirring members to promote the cleaning of the insoluble layer and the dissolution of the soluble layer.

Further, for example, when m is 3, the height of the upper edge of the third dissolution tank is equal to or higher than the height of the upper edge of the second dissolution tank, and the second dissolution tank is above it. They are arranged so that the edge height is equal to or higher than the upper edge height of the first dissolution tank.
In addition, a flow path is provided for the solution to flow from the third dissolution tank to the second dissolution tank, and a flow path for the solution to flow from the second dissolution tank to the first dissolution tank is provided. Therefore, a part of the solution stored in the third dissolution tank is mixed into the solution stored in the second dissolution tank, and further stored in the second dissolution tank in which the third solution is mixed. A part of the solution is mixed in the first dissolution tank. That is, a part of each solution stored in all the dissolution tanks installed upstream of the first dissolution tank flows down to the first dissolution tank.
When m is 4, in addition to the above, the fourth dissolution tank is arranged so that the height of its upper edge is equal to or higher than the height of the upper edge of the third dissolution tank. A flow path is provided through which the solution flows from the fourth dissolution tank to the third dissolution tank.
For example, when m is 2, the second dissolution tank is arranged so that the height of its upper edge is equal to or higher than the height of the upper edge of the first dissolution tank, and the second dissolution tank A flow path through which the solution flows from the dissolution tank to the first dissolution tank is provided.
For example, when m is 1, there is no regulation of the height of the upper edge of the dissolution tank as described above, and there is no channel.
Further, the storage tank includes a solution stored in the first dissolution tank, that is, a solution generated in the first dissolution process, and one solution of each solution flowing down from the upstream dissolution tank to the first dissolution tank. The solution with which the parts merged is transferred and stored by, for example, a transfer pipe.
In the distillation apparatus, a solution containing the solute stored in the first dissolution tank at a high concentration and / or a solute deposited by cooling this solution is distilled. As described above, the distillation apparatus separates the solution into a solute and a solvent, collects the solute, and purifies the solvent.

And, in an eighth invention according to the seventh invention, the stirring member comprises a shaft body connected coaxially with the rotating shaft of the motor, and a plurality of stirring rods branched from the shaft body,
The plurality of stirring rods are characterized in that their tips are arranged at intervals from each other across the shaft body.
In the invention having such a configuration, in addition to the action of the seventh invention, the plurality of stirring rods are placed in the dissolution tank because their tips are arranged with a space between each other with the shaft interposed therebetween. Separation of the soluble layer from the composite material or insoluble layer is facilitated.

  According to the first invention, since the solvent that selectively dissolves the soluble layer is used in the dissolving step, the solution is used regardless of whether or not the soluble layer is bonded to the insoluble layer via the adhesive. The soluble layer can be present as a liquid and the insoluble layer can be present as a solid. Therefore, the insoluble layer can be easily separated from the soluble layer by the subsequent separation step. Furthermore, since the insoluble layer is washed with the solvent each time the repeating step consisting of the dissolving step and the separating step is repeated, the insoluble layer can be recovered with high purity.

In addition, since the solute can be separated from the solution after the insoluble layer is separated by the distillation step, the soluble layer can also be recovered with high purity.
Therefore, according to the first aspect, the composite material in which the resin films are laminated in close contact with each other can be efficiently separated and collected for each type of resin film.

  According to the second invention, in addition to the effects of the first invention, the high-purity solvent purified in the distillation process promotes the cleaning of the insoluble layer in the dissolution process. The purity of the layer can be further improved. In addition, the solvent can be reused efficiently.

  According to the third invention, in addition to the effects of the first or second invention, polyethylene or polypropylene and a resin that does not dissolve in xylene or toluene become a final recovered product, and thus are frequently used in laminate films. Resin can be efficiently recovered.

  According to the fourth invention, in addition to the effects of the first or second invention, since polyethylene or polypropylene and the ethylene / vinyl acetate copolymer resin are finally collected, the same as the third invention. The resin frequently used in the laminate film can be efficiently recovered.

  According to the fifth invention, in addition to the effects of the first or second invention, the polycarbonate and the acrylic resin become the final recovered product. The resin that is present can be recovered efficiently.

  According to the sixth invention, in addition to the effects of any one of the first to fifth inventions, even when the composite material includes an aluminum layer, the aluminum layer can be removed. It is possible to separate and recover the resin part of the aluminum vapor deposited film waste that has been disposed of by landfill and incineration.

According to the seventh invention, m dissolution tanks are provided, and initially, a new solvent is stored in these dissolution tanks, so that the dissolution efficiency of the composite material and the cleaning efficiency of the separated insoluble layer are improved. Can be made. Moreover, since each of the m dissolution tanks is provided with a heater and a stirring member, dissolution of the soluble layer and cleaning of the insoluble layer can be further promoted.
Furthermore, since a part of each solution stored in all dissolution tanks installed upstream of the first dissolution tank flows down to the first dissolution tank, in the storage tank and / or distillation apparatus, Can be efficiently recovered.

  According to the eighth invention, in addition to the effects of the seventh invention, the plurality of stirring rods facilitates the separation of the soluble layer from the composite material and the insoluble layer charged into the dissolution tank. The separation efficiency of this soluble layer can be increased.

1 is a configuration diagram of a sorting and collecting apparatus according to Embodiment 1. FIG. It is a top view of the stirring member which comprises the fraction collection apparatus concerning Example 1. FIG. 6 is a process diagram of a composite material separation and recovery method according to Embodiment 2. FIG. (A) And (b) is an Example of the separate collection | recovery method of the composite material which concerns on Example 2, respectively. (A) And (b) is an Example of the separate collection | recovery method of the composite material which concerns on Example 2, respectively. (A) And (b) is an Example of the separate collection | recovery method of the composite material which concerns on Example 2, respectively. (A) And (b) is process drawing of the separate collection | recovery method of the composite material which concerns on the 1st and 2nd modification of Example 2, respectively. (A) thru | or (c) is a longitudinal cross-sectional view which shows the structure of a composite material, respectively.

First, the structure of the composite material 50 which is a target for separation and collection according to the present embodiment will be described with reference to FIG. FIG. 8A is a longitudinal sectional view showing the structure of the composite material.
As shown in FIG. 8A, the composite material 50 includes, for example, two types of resin films that are laminated without using an adhesive, and are formed on both surfaces of the composite material 50 and selectively used as a solvent. A soluble layer 50a, 50b to be dissolved, and an insoluble layer 50c sandwiched between the soluble layer 50a and the soluble layer 50b and in close contact with the soluble layers 50a, 50b and insoluble in a solvent are provided.
The soluble layers 50a and 50b are each formed from one type of resin film of the same type. Further, the insoluble layer 50c may be formed of one type of resin film, or may be a plurality of types of resin films that are in close contact with each other and are laminated with difficulty in separation.

Next, the fraction collection apparatus according to the first embodiment of the present invention will be described with reference to FIG. 1 and FIG. FIG. 1 is a configuration diagram of a sorting and collecting apparatus according to the first embodiment.
As shown in FIG. 1, the fraction collection apparatus 1 which concerns on Example 1 is a separation collection apparatus used for implementation of the composite material separation collection method which concerns on Example 2 mentioned later.
The separation and recovery device 1 includes three dissolution tanks 2 to 4, three heaters 5 to 7 installed in the dissolution tanks 2 to 4, and three filtration containers 8 to each containing a composite material or an insoluble layer. 10 is provided.
Among these, dissolution tanks 2 to 4 are installed for use in the dissolution process (see FIG. 3) in steps S1 (1), S1 (2), and S1 (3), respectively. The heaters 5 to 7 are provided to maintain the solvent at the first temperature T ₁ (° C.), respectively. Moreover, the filtration containers 8 to 10 are all cylindrical containers in which mesh-like plate-like members are used on the bottom surface and the peripheral surface, and the contained insoluble layer can be filtered and easily separated from the solution. To do.

  Further, the separation and recovery device 1 includes three stirring members 11 to 13 provided in the three dissolution tanks 2 to 4 and three motors 14 to 16 for driving the three stirring members 11 to 13, respectively. Prepare. Among these, the stirring members 11-13 are provided in order to stir the composite material or insoluble layer thrown into the dissolution tanks 2-4 in the state accommodated in the filtration containers 8-10, respectively. Moreover, the motors 14 to 16 are supported by the lid bodies 2a to 4a of the dissolution tanks 2 to 4 via the support rods 17, respectively.

Further, the separation / recovery device 1 is provided with the storage tank 18 in which the solution stored in the first dissolution tank 2 is transferred and stored via the transfer pipe 18a, and the storage tank 18 is transferred and stored. A cooling device 19 for cooling the solution is provided. An opening / closing valve (not shown) is attached to the transfer pipe 18a.
Furthermore, the fraction collection apparatus 1 includes a distillation apparatus 20 that distills the solute deposited by cooling the solution stored in the first dissolution tank 2 and the solution stored in the storage tank 18 with the cooling apparatus 19; The transfer pipe 20a for transferring the solution stored in the tank 2 to the distillation apparatus 20, the return pipe 21 for returning the solvent purified by the distillation apparatus 20 into the third dissolution tank 4, and the precipitated solute were recovered. A return pipe 18b for returning the solution remaining in the storage tank 18 later from the storage tank 18 into the first dissolution tank 2 is provided. Further, a condenser 21a for temporarily storing the purified solvent is installed in the middle of the return pipe 21, and the return amount of the solvent can be adjusted.

The third dissolution tank 4 has an upper edge 4b whose height is equal to or higher than the upper edge 3b of the second dissolution tank 3, and the second dissolution tank 3 has an upper edge. They are arranged in one row so that the height of 3b is equal to or higher than the height of the upper edge 2b of the first dissolution tank 2.
Further, a flow path 22 through which the solution flows from the third dissolution tank 4 to the second dissolution tank 3 is provided at a height between the upper edge 4b and the liquid level of the second dissolution tank 3. It is done. Furthermore, the flow path 23 through which the solution flows from the second dissolution tank 3 to the first dissolution tank 2 is at a height between the upper edge 3b and the liquid level of the first dissolution tank 2. Provided.
Thereby, the liquid level of the solution stored in the third dissolution tank 4 is lower than the liquid level of the solution stored in the second dissolution tank 3, and the second dissolution tank 3 is used. When the liquid level of the solution stored in the solution is lower than the liquid level of the solution stored in the first dissolution tank 2, the solution stored in the dissolution tank 4 passes through the flow path 22 and the flow path 23. Then, it flows down to the dissolution tank 2. Therefore, a part of the solution stored in the dissolution tanks 3 and 4 installed on the upstream side of the dissolution tank 2 is collected in the dissolution tank 2 and transferred to the storage tank 18 as a solution in the dissolution tank 2 and stored. The

Next, the structure of the stirring member which comprises the fraction collection apparatus based on Example 1 is demonstrated in detail using FIG. FIG. 2 is a plan view of the agitation member constituting the fraction collection device according to the first embodiment. In addition, about the component shown in FIG. 1, the same code | symbol is attached | subjected also in FIG. 2, and the description is abbreviate | omitted.
As shown in FIG. 2, the agitating member 11 includes a shaft body 11a that is coaxially connected to a rotating shaft of a motor 14 (see FIG. 1) via a joint (not shown), and a horizontal member extending from the shaft body 11a. A pair of stirring rods 11c and 11c are provided that are bifurcated via a rod 11b. Moreover, the shaft body 11a and the horizontal bar 11b are connected so as to be orthogonal to each other by a cross clamp 11d. Further, the pair of stirring rods 11c, 11c are arranged with their tips spaced apart from each other with the shaft body 11a interposed therebetween. The pair of stirring rods 11c and 11c may be formed in a tapered shape that tapers toward the tip, or may be formed in a columnar shape whose thickness does not change. The agitating members 12 and 13 have the same configuration as the agitating member 11.
Moreover, the form of the stirring rods 11c and 11c is not particularly required to be specified as illustrated, and may be appropriately changed according to the form of the processing object.

  In the fraction collection apparatus 1 having such a configuration, the first dissolution tank 2 used in the dissolution step of Step S1 (1) does not pass through the mesh-like plate member of the filtration container 8 in advance. The composite material 50 (see FIG. 8) crushed into small pieces is put in a state of being accommodated in the filtration container 8. In the second to third dissolution tanks 3 and 4 used in the dissolution process of steps S1 (2) and S1 (3), insoluble layers are accommodated in the filtration containers 9 and 10, respectively. It is thrown. These insoluble layers are an insoluble layer that has already undergone the dissolution process of step S1 (1) and an insoluble layer that has undergone the dissolution process of steps S1 (1) and S1 (2), respectively. However, when the fraction collection device 1 includes only one filtration container 8, the filtration container 8 is moved from the first to the third dissolution tanks 2 to 4 in order.

In the first dissolution tank 2, the solvent is maintained at the first temperature T ₁ (° C.) by the heater 5, and the stirring rods 11 c and 11 c are driven to rotate about the shaft body 11 a by the motor 14. Therefore, the solution is stirred and dissolution of the soluble layers 50a and 50b (see FIG. 8) is promoted.
Further, in the second to third dissolution tanks 3 and 4, as in the dissolution tank 2, the solutions are stirred by the stirring members 12 and 13, respectively, to wash and dissolve the insoluble layer 50c (see FIG. 8). Dissolution of the layers 50a and 50b is promoted.

After the composite material 50 and the insoluble layer are put into the dissolution tanks 2 to 4, respectively, when a preset dissolution time t elapses, the filtration containers 8 to 10 are taken out from the dissolution tanks 2 to 4, respectively. Next, among the filtration containers 8 to 10, the filtration containers 8 and 9 are put into the dissolution tanks 3 and 4. Moreover, the filtration container 10 is set to a centrifugal filter (not shown), the solution adsorbed on the insoluble layer is removed, and the insoluble layer is dried with a dryer (not shown). Thereby, the insoluble layer accommodated in the filtration container 10 becomes one of the final recovered materials.
Thereafter, when the dissolution time t elapses after the filtration container 9 is put into the dissolution tank 4, the filtration container 9 is taken out from the dissolution tank 4 and set in a centrifugal filter. The insoluble layer housed in is taken as one of the final recovered materials. The insoluble layer accommodated in the filtration container 8 is also one of the final recovered materials.

As described above, according to the separation and recovery device 1, the three dissolution tanks 2 to 4 are provided, and these dissolution tanks 2 to 4 are newly provided before the dissolution step of Step S1 (1). Since the solvent is stored, the dissolution efficiency of the composite material 50 and the cleaning efficiency of the separated insoluble layer can be improved. Furthermore, since the dissolution tanks 2 to 4 are provided with heaters 5 to 7 and stirring members 11 to 13, respectively, dissolution of the soluble layers 50a and 50b and cleaning of the insoluble layer 50c can be further promoted. Therefore, the insoluble layer which is one of the final recovered materials can be recovered with high purity.
Moreover, since an insoluble layer is accommodated in the filtration containers 8-10, since it can take out from the dissolution tanks 2-4 easily and can isolate | separate from a solution, it is convenient.
Furthermore, since a part of the solution stored in the dissolution tanks 3 and 4 is transferred to the storage tank 18 via the dissolution tank 2 and stored and cooled, it is the other of the final recovered materials. Solute can be efficiently recovered.
In addition, as shown in FIG. 2 in particular, the tips of the stirring rods 11c, 11c are arranged at intervals from each other with the shaft body 11a interposed therebetween. The solvent and the solution stored in 4 to 6 are likely to be vortexed, and the separation of the soluble layer from the composite material 50 and the insoluble layer charged into the dissolution tanks 4 to 6 is promoted. Therefore, the separation efficiency of the soluble layer can be increased, and the purity of the separated insoluble layer and solute can be improved.
In addition, since the solvent purified by the distillation apparatus 20 is returned to the third dissolution tank 4, the solvent can be efficiently reused.

Next, a method for separating and collecting a composite material according to the second embodiment of the present invention will be described with reference to FIGS. FIG. 3 is a process diagram of the composite material separation and recovery method according to the second embodiment. 1 and 2 are denoted by the same reference numerals in FIG. 3 and description thereof is omitted. Further, the reference numerals described in the respective paragraphs are the same as the reference numerals of the components shown in FIGS.
The composite material separation and collection method 30 (hereinafter referred to as a separate collection method) 30 according to the second embodiment uses the separation and recovery apparatus 1 according to the first embodiment to separate and collect the composite material 50.

As shown in FIG. 3, the separation and recovery method 30 according to the second embodiment maintains the solvent at the first temperature T ₁ (° C.) inside the dissolution tanks 2 to 4 in which the solvent is stored, respectively. Step S3 in which 50a and 50b are dissolved, a dissolution step for generating a solution containing the dissolved solute dissolved in the soluble layers 50a and 50b and the insoluble layer 50c and a separation step for separating the insoluble layer 50c from the solution are repeated three times. The repetition process is provided. The first to third dissolution processes are referred to as the dissolution processes in steps S1 (1), S1 (2), and S1 (3), respectively. The separation processes that are repeated in the same manner are the steps S2 (1) and S2 respectively. (2), referred to as the separation step of S2 (3). Further, the separation process of steps S2 (1), S2 (2), and S2 (3) is performed immediately after the dissolution process of steps S1 (1), S1 (2), and S1 (3), respectively.
Furthermore, after the separation process of step S2 (3), the separation and recovery method 30 uses the centrifugal filter (not shown) to remove the solution adsorbed on the insoluble layer 50c by using a centrifugal filter (not shown). And a drying step of Step 4 for drying with a dryer (not shown). However, the drying process of step 4 may be omitted.

Moreover, the fraction collection method 30 uses the distillation apparatus 20 to remove the solution after the insoluble layer 50c is separated after the separation step of Step S2 (1) and the solute precipitated by cooling the solution with the cooling device 19. The distillation process of step S5 which refine | purifies a solvent while distilling and recovering a solute is provided. In addition, either one of distillation of the solution after the insoluble layer 50c is separated and distillation of the precipitated solute may not be performed.
Which is not performed is mainly determined by the materials of the soluble layers 50a and 50b and the insoluble layer 50c and the type of solvent.
In addition, the solution after the insoluble layer 50c stored in the dissolution tank 2 is separated is transferred from the dissolution tank 2 to the distillation apparatus 20 via the transfer pipe 20a. Further, the solute precipitated inside the storage tank 18 is accommodated in a filtration container (not shown) and transferred from the storage tank 18 to the distillation apparatus 20.

In addition, the fraction collection method 30 includes a return step of Step 6 for returning the purified solvent to the dissolution tank 4 after the distillation step of Step S5. However, the returning step of step S6 may be omitted. The purified solvent may be returned to the dissolution tank 2 or the dissolution tank 3 or the dissolution tank 2 and the dissolution tank 3 instead of the dissolution tank 4.
Moreover, the fraction collection method 30 is the dissolution tank 2 in which the solution which remained in the storage tank 18 after the precipitated solute was transferred to the distillation apparatus 20 after the melt | dissolution process of step S1 (1) via the return piping 18b. A storage tank solution returning step (not shown) is provided. This storage tank solution returning step can also be omitted. The solution remaining in the storage tank 18 may be returned to the dissolution tank 3 or the dissolution tank 4, or the dissolution tank 3 and the dissolution tank 4.

Next, specific examples A to C will be described with reference to Tables 1 to 3 and FIGS. 4 to 6. However, the present invention is not limited by this illustration. 1 to 3 are denoted by the same reference numerals in FIGS. 4 to 6 and description thereof is omitted.
First, the method of Example A will be described with reference to Table 1 and FIG. FIG. 4A and FIG. 4B are examples of the separation and recovery method according to the second embodiment.
The sample used in Example A was a laminate film in which PE as the soluble layers 50a and 50b and PA as the insoluble layer 50c were laminated in close contact with each other without using an adhesive, and step S1 (1 ) Before the melting step, the material is sorted in advance with a 30 mmφ screen and further crushed into an indefinite shape by a crusher.
About 40 g of this sample was sampled three times, and the dissolution process of step S1 (1) to the drying process of step 4 were performed for each sample (sample numbers 1 to 3) collected, and the recovered PA residue The weight (g) of each was measured.
Moreover, the distillation process of step S5 was implemented for every extract | collected sample, and the total weight (g) of the collect | recovered PE residue was measured. In the present embodiment, only one filtration container 8 is used.

More specifically, in the dissolution process of steps S1 (1) to S1 (3), 1.4 (L) of xylene is used as a solvent for PE in each of the dissolution tanks 2 to 4 having a capacity of 2 (L). The xylene was heated and maintained at the first temperature T ₁ = 100 to 120 (° C.).
Among these, in the dissolution process of steps S1 (1) and S1 (2), the inside of the filtration container 8 containing the sample was stirred for 10 minutes by the stirring members 11 and 12, respectively. However, in the third dissolution step of Step S1 (3), the inside of the filtration container 8 was stirred with the stirring member 13 for 3 minutes.
Furthermore, in the drying process of Step 4, the recovered PA residue was removed with a centrifugal filter from a solution mainly containing xylene and dried with a dryer.
Moreover, in the distillation process of step S5, the residue of PE which precipitated by cooling the solution maintained at _1st temperature T1 after the melt | dissolution process of step S1 (1) to normal temperature with the cooling device 19 is used. It isolate | separated with the centrifugal filter, and it dried, collect | recovering xylene with a vacuum distillation apparatus.
The results of Example A performed by the above method are shown in Table 1 and FIG.

Table 1 shows the amount of PE residue recovered and the amount of PE residue recovered. As a result, the recovered amount C _A (PE), which is the total weight of the PE residue, is 72.83 (g), and the recovered amount C _A (PA), which is the total weight of the PA residue, is 47.89 (g). became. Therefore, the weight ratio of C _A (PE) to C _A (PA) was 60.2 (%): 39.6 (%). Further, the total amount of the recovered amounts C _A (PE) and C _A (PA) is 120.72 (g), which is 99.8 (%) by weight with respect to the total sampling amount of 121.01 (g). It became. Therefore, it was found that PE and PA were recovered with good efficiency.
In addition, PE density | concentration (weight%) in the solution stored by the 1st thru | or 3rd dissolution tanks 2-4 was 5.7, 0.6, and 0.04, respectively. Therefore, it can be understood that PE is sufficiently washed with xylene in the third dissolution tank 4.

Next, FIGS. 4A and 4B are IR (infrared absorption spectroscopy) spectra of the recovered PE residue and PA residue, respectively. From these IR spectra, it was confirmed that the recovered PE residue and PA residue were completely separated, and high-purity PE and PA were regenerated, respectively.
As described above, from the results shown in Table 1 and FIG. 4, it was found that according to the separation and collection method 30, it is possible to efficiently separate and collect the laminate film in which PE and PA are laminated in close contact with each other.

Subsequently, the method of Example B will be described with reference to Table 2 and FIG. FIG. 5A and FIG. 5B are examples of the separation and recovery method according to the second embodiment.
The sample used in Example B is a wrap film in which EVA that is the soluble layers 50a and 50b and PO (a mixture of PP and PE) that is the insoluble layer 50c are laminated in close contact with each other without using an adhesive. And before the melt | dissolution process of step S1 (1), the largest length is previously cut | disconnected by the small piece of 50-70 mm.
About 30 g of this sample was collected five times, and the total weight (g) of the collected EVA residue and PE residue was measured in the same manner as in Example A.
Further, in the dissolution tanks 2 to 4, 1.4 (L) of cyclohexane was respectively stored as an EVA solvent, and the cyclohexane was heated and maintained at the first temperature T ₁ = 50 (° C.). The method of Example B other than this is the same as the method of Example A. The results of Example B performed by the above method are shown in Table 2 and FIG.

Table 2 shows the recovered amount of EVA residue and the recovered amount of PO residue. As a result, the recovery amount C _B (EVA), which is the total weight of the EVA residue, is 58.10 (g), and the recovery amount C _B (PE), which is the total weight of the PE residue, is 91.32 (g). became. Therefore, the weight ratio of C _B (EVA) to C _B (PO) was 38.6 (%): 60.6 (%). In addition, the total amount of recovered amounts C _A (EVA) and C _A (PO) is 149.42 (g), and the total amount of samples collected is 150.58 (g), which is 99.2 (%) by weight. became. Therefore, it was found that EVA and PO were recovered with good efficiency.
The EVA concentrations (% by weight) of the solutions stored in the first to third dissolution tanks 2 to 4 were 3.4, 1.5, and 0.6, respectively. Therefore, it can be understood that EVA is sufficiently washed with cyclohexane in the third dissolution tank 4.

Next, FIG. 5 (a) and FIG. 5 (b) are IR spectra for the recovered EVA residue and PO residue, respectively. From these IR spectra, it was confirmed that the recovered EVA residue and PO residue were completely separated, and high-purity EVA and PO were regenerated, respectively.
As described above, from the results shown in Table 2 and FIG. 5, it was found that according to the separation and collection method 30, it is possible to efficiently separate and collect the wrap film in which EVA and PO are laminated in close contact with each other by type.

Finally, the method of Example C will be described with reference to Table 3 and FIG. FIG. 5A and FIG. 5B are examples of the separation and recovery method according to the second embodiment.
The sample used in Example C is a laminate film in which the PMMA that is the soluble layers 50a and 50b and the PC that is the insoluble layer 50c are laminated in close contact with each other without using an adhesive. ) Is previously cut into small pieces having a maximum length of 5 to 20 mm.
3 g of this sample was collected and put into a beaker having a capacity of 100 (mL), and then 60 (mL) of normal temperature acetone as a PMMA solvent was poured into the beaker and stirred with a stirrer for 20 minutes. Thereafter, the PC residue was taken out from the beaker, dried by a dryer, and collected. That is, the dissolution process in step S1 (1), the separation process in step S2 (1), and the drying process in step 4 were performed.
The solution remaining in the beaker was dried while recovering acetone with a vacuum distillation apparatus, and the PMMA residue was recovered. That is, the distillation step of Step S5 was performed. The results of Example C performed by the above method are shown in Table 3 and FIG.

Table 3 shows the amount of PMMA residue recovered and the amount of PC residue recovered. As a result, the recovery amount C _C (PMMA), which is the weight of the PMMA residue, is 2.5 (g), and the recovery amount C _C (PC), which is the weight of the PC residue, is 0.72 (g). . Therefore, the weight ratio of C _C (PMMA) to C _C (PC) was 83.3 (%): 24.0 (%). Further, the total amount of the recovered amounts C _C (PMMA) and C _C (PC) is 3.22 (g), which is 107.3 (%) in terms of the weight ratio with respect to the total 3 (g) of the sampled amount. It was. From this result, there is a possibility that the solvent remains in at least one of PMMA and PC due to insufficient drying. Therefore, IR spectra were measured for these.

FIGS. 6A and 6B are IR spectra of the recovered PMMA residue and PC residue, respectively. From these IR spectra, it was confirmed that the recovered PMMA residue and PC residue were completely separated, and that PMMA and PC having an acceptable purity were regenerated.
As described above, from the results shown in Table 3 and FIG. 6, it was found that the laminate film in which PMMA and PC are laminated in close contact with each other can be efficiently separated and collected by type.

  As described above, according to the separation and recovery method 30, from the results of Examples A to C, the composite material 50 in which a plurality of types of resin films are laminated in close contact with each other is classified into the type of solvent and the insoluble layer. By appropriately selecting the number of times of cleaning 50c, the resin film can be efficiently sorted and collected for each type of resin film. Therefore, for example, it is possible to realize horizontal recycling of the composite material 50 such as a laminate film, which could not be separated conventionally.

  Next, the fraction collection method according to the first and second modifications of the fraction collection method of Embodiment 2 will be described with reference to FIG. FIG. 7A and FIG. 7B are process diagrams of a composite material separation and recovery method according to first and second modifications of Example 2, respectively. The components shown in FIGS. 1 to 6 are denoted by the same reference numerals in FIG. 7 and the description thereof is omitted. Further, the reference numerals described in the respective paragraphs are the same as those of the constituent elements shown in FIGS. 1 to 6 and FIG.

First, the structure of the composite materials 50A and 50B that are the objects of separation and collection in the present embodiment will be described with reference to FIGS. 8B and 8B, respectively. FIG. 8A and FIG. 8B are longitudinal sectional views showing the structures of the composite materials, respectively.
As shown in FIG. 8A, the composite material 50A is formed by depositing aluminum on both surfaces of the composite material 50 so that the aluminum layers 50d and 50d cover the soluble layers 50a and 50b, respectively. Therefore, even if the composite material 50A is immersed in a solvent that selectively dissolves the soluble layers 50a and 50b, the aluminum layers 50d and 50d prevent the solvent from reaching the soluble layers 50a and 50b. As a result, the soluble layers 50a and 50b and the insoluble layer 50c cannot be collected separately. The aluminum layer 50d may cover only one of the fusible layers 50a and 50b. In this case, the solvent cannot separate and recover either one of the soluble layers 50a and 50b and the insoluble layer 50c.

Further, as shown in FIG. 8B, in the composite material 50B, aluminum is deposited on one surface of the insoluble layer 50c, so that the aluminum layer 50d is provided between the soluble layer 50a and the insoluble layer 50c. . In this case, the soluble layers 50a and 50b can be recovered because they are dissolved by a solvent that selectively dissolves them, but the aluminum layer 50d remains in close contact with the insoluble layer 50c, and the insoluble layer 50c is separated and recovered. I can't.
Therefore, the soluble layers 50a and 50b and the insoluble layer 50c of the composite materials 50A and 50B are separated and recovered by performing the separation and recovery method according to the first and second modifications of the present embodiment.

As shown in FIGS. 7 (a) and 7 (b), the separation and recovery methods 30a and 30b according to the first and second modified examples of the second embodiment are such that the composite materials 50A and 50B each include the aluminum layer 50d. In the case of providing, the aluminum layer solvent is stored at a second temperature by a heater (not shown) inside an aluminum layer dissolution tank (not shown) storing an aluminum layer solvent that selectively dissolves the aluminum layer 50d. maintained at T ₂ comprises an aluminum layer dissolving step of step S7 dissolving an aluminum layer 50d.
At this time, the solvent for the aluminum layer is an alkali or an acid. Specifically, for example, 1 to 20 (wt%) sodium hydroxide, 2 to 10 (wt%) dilute hydrochloric acid or dilute sulfuric acid is used. Further, the temperature _{T 2} of the second is, 30 ° C. or higher, and is 90 ° C. or less. In addition, since the distillation process of step S5 and the return process of step S6 are the same as the fraction collection method 30, illustration of these processes is abbreviate | omitted.

As shown in FIG. 7A, in the fractionated recovery method 30a according to the first modification of the second embodiment, the aluminum layer melting step in step S7 is provided before the melting step in step S1 (1).
In the aluminum layer dissolving step of step S7, the solvent for the aluminum layer, since it is maintained at a second temperature T _2, the aluminum layer 50d is dissolved in a solvent for the aluminum layer changes into aluminum solute. Therefore, a solution containing the composite material 50A from which the aluminum solute and the aluminum layer 50d have been removed is generated inside the aluminum layer dissolution tank.
Then, since the composite material 50A from which the aluminum solute and the aluminum layer 50d have been removed is changed to a composite material having the same configuration as the composite material 50, when the separation and recovery method 30 is performed on the composite material, The soluble layers 50a and 50b and the insoluble layer 50c are collected separately.
In addition, when the aluminum layer 50d is provided between the multilayer insoluble layers 50c, after the aluminum layer 50d is exposed on the surface by combining a plurality of separation and recovery methods 30 in which different types of solvents are selected. In addition, it is preferable to newly implement the separation and collection method 30a. That is, when the aluminum layer 50d is provided between the multilayer insoluble layers 50c, the separation and recovery method 30a is applied.

Further, in the separation and recovery method 30b according to the second modification of the second embodiment, the aluminum layer melting step of step S7 is performed when the aluminum layer 50d is provided between the soluble layer 50a and the insoluble layer 50c. It is provided after the repeating step of S3 and before the drying step of Step 4.
After the repeating step of step S3, in the third dissolution tank 4, the soluble layers 50a and 50b of the composite material 50B are dissolved, and the composite material in which the aluminum layer 50d is in close contact with one surface of the insoluble layer 50c is formed. Has been generated. Therefore, when this composite material is put into the aluminum layer dissolution tank and the aluminum layer dissolution step of step S7 is performed, the insoluble layer 50c is separated and recovered.

  As described above, according to the separate collection methods 30a and 30b, even when the composite material includes the aluminum layer 50d as in the composite materials 50A and 50B, the aluminum layer 50d can be removed. . More specifically, among a plurality of types of resin films constituting the composite material, the aluminum layer 50d can be removed regardless of the position where the aluminum layer 50d is laminated. Therefore, it is possible to separate and collect the resin portion of the aluminum vapor deposited film waste that has been conventionally disposed of by landfill or incineration.

In addition, the fraction collection method 30,30a, 30b which concerns on this invention, and the fraction collection apparatus 1 used for this are not limited to what is shown to a present Example. For example, in the repeating step of step S3, the dissolution step and the separation step are each performed only once, and these steps may be repeated twice or four times or more.
Moreover, the drying process of step 4, the return process of step 6, and the storage tank solution return process may each be omitted. Further, in the storage tank 18, the cooling device 19 may be omitted, and the solution may be cooled by being left standing.
And two or more stirring rods 11c may be provided. In addition, when the insoluble layer 50c is formed by laminating a plurality of types of resin films so as to be difficult to separate, the fraction collection method 30 in which a different type of solvent is selected for the insoluble layer 50c. It may be performed again.

  INDUSTRIAL APPLICABILITY The present invention can be used as a separation and collection method for efficiently separating and collecting a composite material in which a plurality of types of resin films are laminated so as to be difficult to separate, and a separation and collection apparatus used therefor.

DESCRIPTION OF SYMBOLS 1 ... Separation collection apparatus 2-4 ... Dissolution tank 2a-4a ... Lid 2b-4b ... Upper edge 5-7 ... Heater 8-10 ... Filtration container 11-13 ... Stirring member 11a ... Shaft body 11b ... Horizontal bar 11c ... Stirring bar 11d ... Cross clamp 14-16 ... Motor 17 ... Supporting rod 18 ... Storage tank 18a ... Transfer pipe 18b ... Return pipe 19 ... Cooling apparatus 20 ... Distillation apparatus 20a ... Transfer pipe 21 ... Return pipe 21a ... Condenser 22,23 ... Flow path 30, 30a, 30b ... Separation and recovery method 50 ... Composite material 50A ... Composite material 50B ... Composite material 50a, 50b ... Soluble layer 50c ... Insoluble layer 50d ... Aluminum layer

Claims (8)

A method for separating and recovering a composite material having a plurality of types of laminated resin films,
The composite material includes a soluble layer formed on at least one of its surfaces and selectively dissolved in a solvent, an insoluble layer in close contact with the soluble layer and insoluble in the solvent,
In the dissolution tank in which the solvent is stored, the solvent is maintained at a first temperature to dissolve the soluble layer, and the soluble layer dissolves to generate a solution containing the dissolved solute and the insoluble layer. Repeating the step and the separation step of separating the insoluble layer from the solution m times (m is a natural number determined as desired), and
After the first separation step, the solution after the insoluble layer is separated and / or the solute deposited by cooling the solution is distilled, the solute is recovered and the solvent is purified. A distillation process,
The method for separating and collecting composite materials, wherein the dissolution tanks are installed in the same number as the m times.   2. The composite according to claim 1, further comprising a step of returning the purified solvent to at least one of the m dissolution tanks after the distillation process. Method for separating and collecting materials. The soluble layer is made of polyethylene or polypropylene,
The solvent is xylene, toluene or a mixture thereof,
The method for separating and recovering a composite material according to claim 1, wherein the first temperature is 90 ° C. or more and not more than the boiling point of the solvent. The soluble layer is made of an ethylene / vinyl acetate copolymer resin,
The insoluble layer is made of polyethylene or polypropylene,
The solvent is cyclohexane;
The method for separating and recovering a composite material according to claim 1 or 2, wherein the first temperature is 40 ° C or higher and not higher than the boiling point of the solvent. The soluble layer is made of an acrylic resin,
The insoluble layer is made of polycarbonate,
The solvent is at least one selected from the group consisting of a mixture of methanol and ethyl acetate, or a ketone solvent,
3. The method for separating and recovering a composite material according to claim 1, wherein the first temperature is 20 ° C. or more and not more than a boiling point of the solvent. When the composite material includes an aluminum layer, the aluminum layer solvent is maintained at a second temperature inside the aluminum layer dissolution tank in which the aluminum layer solvent that selectively dissolves the aluminum layer is stored. An aluminum layer dissolving step for dissolving the aluminum layer;
The aluminum layer melting step is provided before the first melting step when the aluminum layer covers the soluble layer, while the aluminum layer is provided between the soluble layer and the insoluble layer. Is provided after the repeating step,
The aluminum layer solvent is an alkali or an acid,
The method for separating and recovering a composite material according to any one of claims 1 to 5, wherein the second temperature is 30 ° C or higher and 90 ° C or lower. A separation and recovery apparatus for use in the method for separating and recovering a composite material according to any one of claims 1 to 6,
The m dissolution tanks;
The m heaters respectively installed in the m dissolution tanks and maintaining the solvent at the first temperature;
Containing the composite material or the insoluble layer, and filtering the insoluble layer to separate it from the solution; and
The m stirring members respectively provided in the m dissolving tanks and stirring the composite material or the insoluble layer housed in the filtration container;
The m motors respectively driving the m stirring members;
A storage tank in which the solution stored in the first dissolution tank is transferred and stored;
A distillation apparatus for distilling the solute deposited by cooling the solution stored in the first dissolution tank and / or the solution stored in the storage tank;
When m is a natural number of 2 or more, the n-th (n = m, m−1,..., 2, where n is a natural number of 2 or more) dissolution tank has a height of each upper edge (n -1) arranged so as to be equal to or higher than the height of the upper edge of the number of the dissolution tanks, and from the nth dissolution tank to the (n-1) th dissolution tank, A separation / recovery device, wherein a flow path through which the solution flows is provided. The stirring member includes a shaft body coaxially connected to the rotating shaft of the motor, and a plurality of stirring bars branched from the shaft body,
The sorting and collecting apparatus according to claim 7, wherein the plurality of stirring rods are arranged with their tips spaced apart from each other across the shaft body.

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