JP6949322B2 - Separate recovery method for composite materials and separate recovery equipment used for this method - Google Patents

Description

The present invention relates to a method for separating and recovering a composite material composed of a plurality of types of resin materials and a separate recovery device used for the method, and in particular, efficiently separates a composite material in which a plurality of types of resin films are laminated in a difficult-to-separate manner. The present invention relates to a separate collection method for collection and a separate collection device used for this method.

Conventionally, as a method for separating mixed waste plastic in which a plurality of types of plastics are mixed, various methods for physically separating the mixed waste plastic using specific gravity, optical characteristics, and the like 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 imparting various functionalities such as oxygen barrier property and weldability. Specifically, this composite material is, for example, polyethylene (PE), polypropylene (PP), polyamide resin (PA), ethylene / vinyl acetate copolymer resin (EVA), polyvinyl alcohol (PVA), ethylene-vinyl alcohol co-weight. Resin films such as coalesced (EVOH), polyvinylidene chloride (PVDC) polyethylene terephthalate (PET), polycarbonate (PC), acrylic resin (PMMA), and cellophane are difficult to separate from each other with or without adhesive. It is closely related to.
On the other hand, in the conventional sorting method described above, it is possible to separate mixed waste plastics in which a plurality of types of plastics are simply mixed, but a composite material in which resin films are laminated in close contact with each other is used. , It is difficult to separate and recycle by type. Therefore, although some composite materials are cascade-recycled, there are few examples of material recycling.
Therefore, in recent years, a technique for separating and recovering a composite material has been developed, and some inventions have already been disclosed in this regard.

First, Patent Documents 1 to 3 disclose inventions relating to a treatment method for separating plastic waste using a separating solvent under the name of "method for treating plastic waste", respectively.
The inventions disclosed in Patent Documents 1 to 3 are all (1) a dissolving step of bringing a separating solvent into contact with plastic waste to form a solid substance composed of a separating solvent solution containing plastic and an undissolved plastic. 2) Solid-liquid separation step to separate the separate solvent solution and the solid substance, (3) Decomposition step to concentrate the fractionated solution and then heat-decompose it, (4) Contact the solid substance with the heated non-condensable gas to solidify it. Separation solvent evaporation step, (5) Liquid separation solvent It is characterized by including a condensing step of producing and a non-condensable gas, (6) a heating step of heating the non-condensable gas, and (7) a circulation step of circulating the heated non-condensable gas to a separating solvent evaporation step. do.
According to the method for treating plastic waste having such characteristics, it is possible to efficiently separate the soluble component and the insoluble component with respect to the fractionating solvent. Further, the separating solvent contained in the solid matter can be efficiently separated and recovered, and the solid matter can be recovered as a solid matter having a low fractionation solvent content. Therefore, it is possible to obtain a decomposition product oil useful as a fuel or a reaction raw material from plastic waste in a high yield.

Next, Patent Document 4 discloses an invention relating to a separate recovery method for separating and recovering a composite material such as a laminated film of a metal foil under the name of "separate recovery method for composite materials".
The invention disclosed in Patent Document 2 constitutes, at least, a crushing step of crushing a composite material into small pieces to obtain a crushed material, and contacting the crushed material with a permeable release agent solution to form a composite material. A thin film material peeling step of peeling each thin film material to obtain a crushed mixture of the thin film material, and a separation treatment of the crushed mixture of the thin film material by multiple specific gravity sorting using a plurality of specific gravity sorting solutions having different specific gravities. It is characterized by having a separate recovery step of separating and recovering a plurality of thin film materials.
According to the method for separating and recovering a composite material having such characteristics, the separation treatment by specific gravity sorting is performed an appropriate number of times using different specific gravity sorting liquids according to the type of thin film material to be separated and recovered, thereby forming a laminated film. Thin film materials such as synthetic resin film and aluminum foil separated from the crushed mixture of each thin film material constituting the above can be individually separated and recovered and reused.

Further, Patent Document 5 discloses an invention relating to a recovery method for recovering copper and nickel from a resin-plated waste material under the name of "a method for recovering a metal component of a resin-plated waste material".
The invention disclosed in Patent Document 5 increases the abundance ratio of a plating film component in a method for recovering a metal component of a resin plating waste material having a copper plating film integrally formed on the surface of a resin base material and a nickel plating film. It is characterized by having a metal component enriched mixture forming step, and then a metal component recovering step of heating and melting the mixture to obtain an alloy containing copper and nickel.
According to the method for recovering the metal component of the resin-plated waste material having such characteristics, copper and nickel can be recovered in a large amount and inexpensively without separating and removing the copper component.

Japanese Unexamined Patent Publication No. 11-21373 Japanese Unexamined Patent Publication No. 11-116728 Japanese Unexamined Patent Publication No. 11-228730 Japanese Unexamined Patent Publication No. 2014-19003 Japanese Unexamined Patent Publication No. 2003-293048

However, in the inventions disclosed in Patent Documents 1 to 3, when the fractionated solvent solution containing plastic is heated in the dissolution step of (1), for example, only plastics suitable for oiling such as PE, PP, and PS are used. Dissolves. Therefore, in the concentration step (3), the separated solvent solution in which the plastic is dissolved as described above is concentrated, and further distilled by the distillation step described in FIG. 1 of Patent Document 1, the recovered heavy oil and medium content are obtained. Since oils and light oils contain a high boiling point component of a fractionating solvent in addition to the above-mentioned dissolved components of plastics, it is difficult to recover only the dissolved components of plastics. That is, there is a problem that horizontal recycling of plastic is difficult.
Further, in the dissolution step (1), the hydrocarbon-based plastics are brought into contact with a separating solvent at 50 to 200 ° C. for 5 minutes or more, preferably 10 to 60 minutes, but under the same conditions, they are in close contact with each other. There is a possibility that the resin in the inner layer of the laminated resin film cannot be sufficiently dissolved, and the composite material such as the laminated film cannot be separated and recovered.
Further, the inventions disclosed in Patent Documents 1 to 3 are intended for general waste, and are not intended for PA, EVA, EVOH, PC, PMMA, etc., which are often used for laminated films. Therefore, it is considered difficult to separate and recover 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, in a normal laminated film, the resin films are heat-sealed directly or through a resin thin film having both affiliations, so that the resin films cannot be peeled off by the release agent solution of the alkaline aqueous solution. There is a problem that the laminated film cannot be collected separately.

Further, in the invention disclosed in Patent Document 5, it is an object to recover the metal component from the resin base material with high efficiency, and it is not an object to regenerate both the metal component and the resin base material. Therefore, the invention disclosed in Patent Document 5 cannot be applied as a method for separating and recovering a composite material such as a laminated 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 according to the type of resin film, regardless of the presence or absence of an adhesive. It is an object of the present invention to provide a separate recovery method for a composite material capable of recovery and horizontal recycling, and a separate recovery device used for this method.

In order to achieve the above object, the first invention is a method for separating and recovering a composite material having a plurality of types of resin films to be laminated, wherein the composite material is formed on at least one of the surfaces thereof and is selected as a solution. The soluble layer is provided with a soluble layer that dissolves effectively and an insoluble layer that adheres to the soluble layer and is insoluble in the solvent, and the solvent is maintained at a first temperature inside a dissolution tank in which the solution is stored. The dissolution step of dissolving the solution to generate a solution containing the solute and the insoluble layer in which the soluble layer is dissolved and the separation step of separating the insoluble layer from the solution are repeated m times (m is a desired natural number). A distillation step is provided after the first separation step, in which the solution after the insoluble layer is separated and / or the solute precipitated by cooling this solution is distilled to recover the solute and purify the solvent. The melting tank is characterized in that the same number of melting tanks as m times are installed.

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 separated from each other in close contact with each other with or without an adhesive. It is considered difficult.
Further, the composite material is, for example, one in which two layers of a soluble layer and an insoluble layer are laminated, or one in which an insoluble layer is sandwiched between the soluble layer and the soluble layer.
The first temperature is a temperature range in which the solvent can dissolve the soluble layer.

In the invention having the above configuration, in the first dissolution step (m = 1), the composite material is charged into the dissolution 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 produced.

Then, in the first (m = 1) separation step carried out following the first dissolution step, only the insoluble layer is separated from the solution by, for example, filtering.
It is considered that the solute is adsorbed on the separated insoluble layer. However, for example, if it is determined that the adsorption amount of the solute is less than the permissible amount as a result of sampling the insoluble layer and determining the adsorption amount of the solute, the second and subsequent repeating steps may not be carried out. .. On the other hand, if this is not the case, a dissolution step and a separation step are added.

In the second (m = 2) dissolution step carried out following the first separation step, a new 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. As a result, 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 in the same manner as in the first separation step.
In the insoluble layer separated in the second separation step, if it is determined that the adsorption amount of the solute is less than the allowable amount as described above, the solution is not carried out after the third (m = 3) dissolution step. On the other hand, if this is not the case, a third dissolution step and a separation step are carried out, respectively. After that, when the dissolution step and the separation step are completed an appropriate number of times (maximum m times), the repeating step is completed, and the separated insoluble layer becomes one of the finally separated recovered products.

After the first separation step, a solution containing a high concentration of solute remains. A distillation step is carried out to recover this solute.
In the distillation step, the solution after the insoluble layer is separated and / or the solute precipitated by leaving this solution to stand or cooling it with a cooling device is distilled. The former solution contains a high concentration of solute, as described above. Further, it is considered that the solution is adsorbed on the latter precipitated solute. Therefore, the object to be distilled by distillation in this step is the solution of the former and / or the solution adsorbed on the precipitated solute of the latter. By this distillation, the former solution is separated into a solute and a solvent, and the solution adsorbed on the latter precipitated solute is separated into a solute and a solvent. That is, the solute can be recovered and the solvent can be purified. This recovered solute becomes the other of the finally sorted recovered products. However, the distillation step may be carried out at any timing in the repeating step as long as it is carried out after the first separation step.

Next, the second invention includes, in the first invention, a step of returning the purified solvent to at least one of the m dissolution tanks after the distillation step. It is a feature.
In such a configuration, in addition to the action of the first invention, in the reconstitution step, the purified solvent is returned to at least one of the m dissolution tanks, and thus in the dissolution step. The purity of the solvent used is improved. Therefore, cleaning of the insoluble layer in the dissolution step is promoted.

Further, in the third invention, in the first or second invention, 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. Moreover, it is characterized in that it is below the boiling point of the solvent.
In the invention having such a configuration, the insoluble layer is, for example, a resin that is insoluble in xylene or toluene, such as PA, PET, PVA, EVOH, and PDVC. When the solvent is a mixture of xylene and toluene, the upper limit of the first temperature is set according to the mixing ratio (weight ratio).
In the invention having the above configuration, in addition to the action of the first or second invention, polyethylene or polypropylene and a resin which is insoluble in xylene or toluene such as PA are the final recovered products. Then, when the distillation step is carried out, high-purity xylene or toluene is recovered.

In the fourth invention, in the first or second invention, the soluble layer is made of ethylene-vinyl acetate copolymer resin, the insoluble layer is made of polyethylene or polypropylene, the solvent is cyclohexane, and the solvent is cyclohexane. The temperature of 1 is characterized by being 40 ° C. or higher and lower than the boiling point of the solvent.
In the invention having such a structure, in addition to the action of the first or second invention, polyethylene or polypropylene and an ethylene-vinyl acetate copolymer resin are the final recovered products. Then, when the distillation step is carried out, high-purity cyclohexane is recovered.

Subsequently, in the fifth invention, in the first or second invention, the soluble layer is made of acrylic resin, the insoluble layer is made of polycarbonate, and the solvent is a mixture of methanol and ethyl acetate, or a ketone solvent. It is at least one selected from the group consisting of, and is characterized in that the first temperature is 20 ° C. or higher and lower 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 and the like. When the solvent is a mixture of methanol and ethyl acetate, the upper limit of the first temperature is set according to the mixing ratio (weight ratio).
In the invention having the above configuration, in addition to the action of the first or second invention, the polycarbonate and the acrylic resin are the final recovered products. Then, when the distillation step is carried out, a mixture of high-purity methanol and ethyl acetate or the above-mentioned ketone solvent is recovered.

Subsequently, in the sixth invention, in any one of the first to fifth inventions, when the composite material includes an aluminum layer, the aluminum layer dissolution in which a solvent for an aluminum layer that selectively dissolves the aluminum layer is stored is stored. Inside the tank, an aluminum layer melting step is provided in which the aluminum layer solvent is maintained at a second temperature to dissolve the aluminum layer, and this aluminum layer melting step is performed when the aluminum layer coats the soluble layer. It is provided before the second dissolution step, while it is provided after the repeat step when the aluminum layer is provided between the soluble and insoluble layers, the aluminum layer solvent is an alkali or acid, and a second. The temperature is characterized by being 30 ° C. or higher and 90 ° C. or lower.

In the invention of such a configuration, the aluminum layer is deposited on, for example, a soluble layer or an insoluble layer. Of these, when the aluminum layer coats the soluble layer, the solvent does not reach the soluble layer and cannot dissolve it unless the aluminum layer is removed first. Therefore, before the first dissolution step. An aluminum layer melting step is carried out.
On the other hand, when the aluminum layer is provided between the soluble layer and the insoluble layer, the aluminum layer dissolution step is carried out on the insoluble layer after the repeating step, that is, after the insoluble layer is finally recovered. do.

In the invention having 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 in which the solvent for the aluminum layer is stored. It is thrown in. Since the solvent for the aluminum layer is maintained at the second temperature, the aluminum layer dissolves in the solvent for the aluminum layer and changes to an aluminum solute. On the other hand, the soluble layer and the insoluble layer are insoluble in the solvent for the aluminum layer.
Therefore, when the aluminum layer melting step is carried out before the first melting step, a solution containing the aluminum solute and the composite material from which the aluminum layer has 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 melting tank installed in the first melting step, and the soluble layer and the insoluble layer are subsequently separated and recovered.

When the aluminum layer melting step is carried out 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 melting tank. Therefore, the insoluble layer and the already removed soluble layer are separated and recovered.
Thus, the soluble layer and the insoluble layer are the final recoveries.

Further, the seventh invention is a separate recovery device used in the separate recovery method for composite materials according to any one of the first to sixth inventions, which comprises m of the dissolution tanks and m of the dissolution tanks. M heaters, each of which is installed to maintain the solvent at the first temperature, and at least one filter vessel that houses the composite material or insoluble layer and filters the insoluble layer to separate it from the solution, and m. M stirring members that are provided in each of the melting tanks and stir the composite material or insoluble layer contained in the filtration container, m motors that drive the m stirring members, and the first melting member. A distillation apparatus that distills the solute precipitated by cooling the storage tank in which the solution stored in the tank is transferred and stored, 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 nth melting tank (n = m, m-1 ... 2, n is a natural number of 2 or more) has a height of the upper edge of each ( The flow is arranged so as to be equal to or higher than the height of the upper edge of the n-1) th dissolution tank, and the solution flows out from the nth dissolution tank to the (n-1) th dissolution tank. It is characterized in that each road is provided.
That is, when the melting tanks are arranged next to each other, the height of the upper edge of the melting tank arranged on the upstream side is always the height of the upper edge of the melting 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 melting tank installed in the first melting step among the three melting tanks is a composite housed in a filtration container. The material is put in. The insoluble layer contained in the filtration vessel is put into the second to third melting tanks, which are installed in the second to third melting steps, respectively. When one filtration vessel is provided, the filtration vessel is sequentially moved to the first to third dissolution tanks for use. On the other hand, when three filtration containers are provided, they are used by immersing them in each of the three dissolution tanks without moving them.

Further, when the composite material is put into the first melting 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 agitated and the dissolution of the soluble layer is promoted. Further, when the insoluble layer is put into the second to third dissolution tanks, the solution is similarly agitated by the stirring members, and the washing of the insoluble layer and the dissolution of the soluble layer are promoted.

Further, for example, when m is 3, the height of the upper edge of the third melting tank is equal to or higher than the height of the upper edge of the second melting tank, and the second melting tank is above it. Each is arranged so that the height of the edge is equal to or higher than the height of the upper edge of the first melting tank.
In addition, a flow path for the solution to flow out from the third dissolution tank to the second dissolution tank is provided, and a flow path for the solution to flow out from the second dissolution tank to the first dissolution tank is provided. Therefore, a part of the solution stored in the third dissolution tank was mixed with the solution stored in the second dissolution tank, and further stored in the second dissolution tank in which the third solution was 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 into the first dissolution tank.
When m is 4, in addition to the above, the fourth melting tank is arranged so that the height of the upper edge thereof is equal to or higher than the height of the upper edge of the third melting tank. A flow path for the solution to flow out from the fourth dissolution tank to the third dissolution tank is provided.
Then, for example, when m is 2, the second melting tank is arranged so that the height of the upper edge thereof is equal to or higher than the height of the upper edge of the first melting tank, and the second melting tank is arranged. A flow path for the solution to flow out from the dissolution tank to the first dissolution tank is provided.
For example, when m is 1, the height of the upper edge of the melting tank is not specified as described above, and there is no flow path.
Further, in the storage tank, one of the solution stored in the first dissolution tank, that is, the solution generated in the first dissolution step and each solution flowing down from the upstream dissolution tank to the first dissolution tank. The solution in which the parts are merged is transferred and stored by, for example, a transfer pipe.
Further, in the distillation apparatus, a solution containing a high concentration of the solute stored in the first dissolution tank and / or the solute precipitated by cooling this solution is distilled. As described above, this distillation apparatus separates the solution into a solute and a solvent, recovers the solute, and purifies the solvent.

Then, in the eighth invention, in the seventh invention, the stirring member includes a shaft body coaxially connected to the rotation 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 so as to be spaced apart from each other with the shaft body interposed therebetween.
In the invention having such a configuration, in addition to the action of the seventh invention, the plurality of stirring rods are put into the melting tank because their tips are arranged at intervals from each other with the shaft body interposed therebetween. Separation of the soluble layer from the composite or insoluble layer is promoted.

According to the first invention, since a solvent that selectively dissolves the soluble layer is used in the dissolution step, the solution is dissolved regardless of whether or not the soluble layer is adhered to the insoluble layer via an 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. Further, since the insoluble layer is washed with the solvent each time the repeating step including the dissolution step and the separation step is repeated, the insoluble layer can be recovered with high purity.

Further, since the solute can be separated from the solution or the like 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 invention, the composite material in which the resin films are laminated in close contact with each other can be efficiently separated and recovered according to the type of the resin film.

According to the second invention, in addition to the effect of the first invention, the high-purity solvent purified in the distillation step promotes the washing of the insoluble layer in the dissolution step, so that the insoluble layer finally recovered is insoluble. 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 insoluble in xylene or toluene are the final recovered products, and are therefore often used in laminated films. The resin can be recovered efficiently.

According to the fourth invention, in addition to the effects of the first or second invention, polyethylene or polypropylene and the ethylene-vinyl acetate copolymer resin are the final recovered products, so that the same as in the third invention. , Resins that are often used in laminate films can be efficiently recovered.

According to the fifth invention, in addition to the effects of the first or second invention, polycarbonate and acrylic resin are the final recovered products, so that they are often used for laminated films as in the third invention. It is possible to efficiently recover the resin.

According to the sixth invention, in addition to the effect 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 collect the resin part of the aluminum vapor deposition film waste that has been landfilled and incinerated.

According to the seventh invention, m dissolution tanks are provided, and since a new solvent is initially stored in these dissolution tanks, the dissolution efficiency of the composite material and the cleaning efficiency of the separated insoluble layer are improved. Can be made to. Further, since each of the m melting tanks is provided with a heater and a stirring member, it is possible to further promote the melting of the soluble layer and the cleaning of the insoluble layer.
Further, since 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, the solute in the storage tank and / or the distillation apparatus. Can be efficiently recovered.

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

It is a block diagram of the separate collection apparatus which concerns on Example 1. FIG. FIG. 5 is a plan view of a stirring member constituting the separate collection device according to the first embodiment. It is a process drawing of the separate recovery method of the composite material which concerns on Example 2. FIG. (A) and (b) are examples of the separate recovery method of the composite material according to Example 2, respectively. (A) and (b) are examples of the separate recovery method of the composite material according to Example 2, respectively. (A) and (b) are examples of the separate recovery method of the composite material according to Example 2, respectively. (A) and (b) are process charts of the method for separating and recovering composite materials according to the first and second modifications of Example 2, respectively. (A) to (c) are vertical cross-sectional views showing the structure of the composite material, respectively.

First, the configuration of the composite material 50, which is the target of separate collection in this embodiment, will be described with reference to FIG. 8A. FIG. 8A is a vertical cross-sectional view showing the structure of the composite material.
As shown in FIG. 8A, for example, the composite material 50 is obtained by laminating two types of resin films on each other without using an adhesive, and is formed on both sides of the composite material 50 and selectively selected as a solvent. A soluble layer 50a, 50b that dissolves, and an insoluble layer 50c that is sandwiched between the soluble layer 50a and the soluble layer 50b and adheres to the soluble layers 50a, 50b and is insoluble in a solvent are provided.
Further, 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 formed by laminating a plurality of types of resin films in close contact with each other and difficult to separate.

Next, the separate collection device according to the first embodiment of the present invention will be described with reference to FIGS. 1 and 2. FIG. 1 is a configuration diagram of a separate collection device according to the first embodiment.
As shown in FIG. 1, the separate recovery device 1 according to the first embodiment is a separate recovery device used for carrying out the separate recovery method for the composite material according to the second embodiment described later.
The separate collection device 1 includes three melting tanks 2 to 4, three heaters 5 to 7 installed in the melting tanks 2 to 4, and three filtration containers 8 to containing a composite material or an insoluble layer. 10 is provided.
Of these, the melting tanks 2 to 4 are installed for use in the melting steps (see FIG. 3) of steps S1 (1), S1 (2), and S1 (3), respectively. Heaters 5 to 7 are provided to maintain the solvent at the first temperature T ₁ (° C.), respectively. Further, the filtration containers 8 to 10 are all cylindrical containers in which mesh-shaped 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. do.

Further, the separate collection device 1 includes three stirring members 11 to 13 provided in each of the three melting tanks 2 to 4 and three motors 14 to 16 for driving the three stirring members 11 to 13, respectively. Be prepared. Of these, the stirring members 11 to 13 are provided to stir the composite material or the insoluble layer that has been put into the melting tanks 2 to 4 while being housed in the filtration vessels 8 to 10. Further, the motors 14 to 16 are supported by the lids 2a to 4a of the melting tanks 2 to 4 via the support rods 17, respectively.

Further, the separate collection device 1 is provided with a 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 provided, transferred and stored. A cooling device 19 for cooling the solution is provided. An on-off valve (not shown) is attached to the transfer pipe 18a.
Further, the separate recovery device 1 dissolves the solution stored in the first dissolution tank 2 and the solution stored in the storage tank 18 by cooling the solution in the cooling device 19 to distill the solute precipitated. 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 in the distillation apparatus 20 to 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 to the first dissolution tank 2 from the storage tank 18 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.

Then, the height of the upper edge 4b of the third melting tank 4 becomes equal to or higher than the height of the upper edge 3b of the second melting tank 3, and the second melting tank 3 has its upper edge. The heights of 3b are arranged in a row so as to be equal to or higher than the height of the upper edge 2b of the first melting tank 2.
Further, the flow path 22 through which the solution flows out 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. Be done. Further, 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.
As a result, 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 When the liquid level of the solution stored in the first dissolution tank 2 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 into the melting 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, becomes the solution of the dissolution tank 2, is transferred to the storage tank 18, and is stored. NS.

Next, the configuration of the stirring member constituting the separate collection device according to the first embodiment will be described in detail with reference to FIG. FIG. 2 is a plan view of a stirring member constituting the separate collection device according to the first embodiment. The components shown in FIG. 1 are designated by the same reference numerals in FIG. 2, and the description thereof will be omitted.
As shown in FIG. 2, the stirring member 11 has a shaft body 11a coaxially connected to the rotating shaft of the motor 14 (see FIG. 1) via a joint (not shown), and laterally from the shaft body 11a. A pair of stirring rods 11c and 11c that are bifurcated via the rods 11b are provided. Further, the shaft body 11a and the horizontal bar 11b are connected by a cross clamp 11d so as to be orthogonal to each other. Further, the pair of stirring rods 11c and 11c are arranged so that their tips thereof are 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 in which the thickness does not change. The stirring members 12 and 13 also have the same configuration as the stirring member 11.
Further, the forms of the stirring rods 11c and 11c do not need to be specified as shown in particular, and may be appropriately changed according to the form of the object to be processed.

In the separate recovery device 1 having such a configuration, the first melting tank 2 used in the melting step of step S1 (1) does not pass through the mesh-shaped plate-shaped member of the filtration vessel 8 in advance. The composite material 50 (see FIG. 8) crushed into small pieces is charged in a state of being contained in the filtration container 8. In the second to third dissolution tanks 3 and 4, which are used in the dissolution steps of steps S1 (2) and S1 (3), respectively, the insoluble layers are contained in the filtration vessels 9 and 10, respectively. It is thrown in. These insoluble layers are an insoluble layer that has already undergone the dissolution step of step S1 (1) and an insoluble layer that has already undergone the dissolution step of steps S1 (1) and S1 (2). However, when the separate collection device 1 includes only one filtration container 8, the filtration container 8 is sequentially moved to the first to third dissolution tanks 2 to 4 for use.

In the first melting tank 2, the solvent is _{maintained at the first temperature T 1} (° C.) by the heater 5, and the stirring rods 11c and 11c are rotationally driven around the shaft body 11a by the motor 14. Therefore, the solution is stirred and the dissolution of the soluble layers 50a and 50b (see FIG. 8) is promoted.
Further, in the second to third dissolution tanks 3 and 4, the solution is agitated by the stirring members 12 and 13, respectively, as in the dissolution tank 2, and the insoluble layer 50c (see FIG. 8) is washed and soluble. Dissolution of 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, and when the preset dissolution time t elapses, the filtration vessels 8 to 10 are taken out from the dissolution tanks 2 to 4, respectively. Next, of the filtration vessels 8 to 10, the filtration vessels 8 and 9 are charged into the dissolution tanks 3 and 4. Further, the filtration vessel 10 is set in a centrifugal filter (not shown), the solution adsorbed on the insoluble layer is removed, and the insoluble layer is dried in a dryer (not shown). As a result, the insoluble layer contained in the filtration vessel 10 becomes one of the final recovered products.
After that, when the dissolution time t elapses after the filtration vessel 9 is put into the dissolution tank 4, the filtration vessel 9 is taken out from the dissolution tank 4 and set in the centrifugal filter, and the filtration vessel 9 is set in the same manner as in the case of the filtration vessel 10. The insoluble layer contained in is one of the final recovered products. Similarly, the insoluble layer contained in the filtration vessel 8 is one of the final recovered products.

As described above, according to the separate recovery device 1, three melting tanks 2 to 4 are provided, and these melting tanks 2 to 4 are newly developed before the melting 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. Further, since the melting tanks 2 to 4 are provided with the heaters 5 to 7 and the stirring members 11 to 13, respectively, it is possible to further promote the melting of the soluble layers 50a and 50b and the cleaning of the insoluble layer 50c. Therefore, the insoluble layer, which is one of the final recovered products, can be recovered with high purity.
Further, since the insoluble layer is housed in the filtration vessels 8 to 10 and can be easily taken out from the dissolution tanks 2 to 4 and separated from the solution, the usability is also good.
Further, 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, so that it is the other of the final recovered products. The solute can be recovered efficiently.
In addition, as shown in FIG. 2, since the tips of the stirring rods 11c and 11c are arranged at intervals from each other with the shaft body 11a in between, the rotation of each of the rotation shafts of the motors 14 to 16 causes the inside of the melting tank to rotate. The solvent and solution stored in 4 to 6 tend to form a vortex, and the separation of the soluble layer from the composite material 50 and the insoluble layer charged in the dissolution tanks 4 to 6 is promoted. Therefore, the separation efficiency of the soluble layer can be improved, and the purity of the insoluble layer and the solute collected separately 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, the method for separating and recovering the composite material according to the second embodiment of the present invention will be described with reference to FIGS. 3 and 4. FIG. 3 is a process diagram of the method for separating and recovering the composite material according to the second embodiment. The components shown in FIGS. 1 and 2 are designated by the same reference numerals in FIG. 3, and the description thereof will be omitted. Further, since the reference numerals described in each paragraph match the reference numerals of the components shown in FIGS. 1, 2 and 8, the description thereof will be omitted.
The method for separating and recovering the composite material according to the second embodiment (hereinafter, referred to as the method for separating and collecting the composite material) 30 is for separately collecting the composite material 50 by using the separate and recovering device 1 according to the first embodiment.

As shown in FIG. 3, in the separate recovery method 30 according to Example 2, the soluble layer is formed by maintaining _{the solution at the first temperature T 1 (° C.) inside the dissolution tanks 2 to 4 in which the solution is stored.} Step S3 in which the dissolution step of dissolving 50a and 50b to generate a solution containing the solute in which the soluble layers 50a and 50b are dissolved and the insoluble layer 50c and the separation step of separating the insoluble layer 50c from this solution are repeated three times, respectively. It is provided with a repeating process of. The first to third dissolution steps are referred to as the dissolution steps of steps S1 (1), S1 (2), and S1 (3), respectively, and the similarly repeated separation steps are referred to as steps S2 (1) and S2, respectively. This is called the separation step of (2) and S2 (3). Further, the separation steps of steps S2 (1), S2 (2), and S2 (3) are carried out immediately after the dissolution steps of steps S1 (1), S1 (2), and S1 (3), respectively.
Further, in the separate recovery method 30, after the separation step of step S2 (3), the separated insoluble layer 50c is removed from the solution adsorbed on the insoluble layer 50c using a centrifugal filter (not shown). The drying step of step 4 is provided for drying with a dryer (not shown). However, the drying step of step 4 may be omitted.

Further, in the fractional recovery method 30, after the separation step of step S2 (1), the solution after the insoluble layer 50c is separated and the solute precipitated by cooling this solution in the cooling device 19 are distilled by the distillation device 20. The distillation step of step S5 is provided for distilling, recovering the solute, and purifying the solvent. In some cases, one of the distillation of the solution after the insoluble layer 50c is separated and the distillation of the precipitated solute may not be carried out.
Which is not carried out is mainly determined by the material of the soluble layers 50a and 50b and the insoluble layer 50c and the type of solvent.
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 housed in a filtration container (not shown) and transferred from the storage tank 18 to the distillation apparatus 20.

In addition, the separate recovery method 30 includes a return step of step 6 in which the purified solvent is returned to the dissolution tank 4 after the distillation step of step S5. However, the return step of step S6 may be omitted. Further, 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.
Further, in the separate recovery method 30, after the dissolution step of step S1 (1), the solution remaining in the storage tank 18 after the precipitated solute is transferred to the distillation apparatus 20 is transferred to the dissolution tank 2 via the return pipe 18b. A storage tank solution return step (not shown) is provided. The step of returning the solution to the storage tank can also be omitted. Further, 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, this example does not limit the invention of the present application. The components shown in FIGS. 1 to 3 are designated by the same reference numerals in FIGS. 4 to 6 and the description thereof will be omitted.
First, the method of Example A will be described with reference to Table 1 and FIG. 4 (a) and 4 (b) are examples of the separate collection method according to the second embodiment, respectively.
The sample used in Example A is a laminated film in which PE which is a soluble layer 50a and 50b and PA which is an insoluble layer 50c are laminated in close contact with each other without using an adhesive, and is in step S1 (1). ), It was sorted in advance with a screen of 30 mmφ and then crushed into an indefinite shape by a crusher.
About 40 g of this sample was collected three times, and the dissolution step of step S1 (1) to the drying step of step 4 were carried out for each sample (sample numbers 1 to 3), and the recovered PA residue. The weight (g) of each was measured.
Further, the distillation step of step S5 was carried out for each sample collected, and the total weight (g) of the recovered PE residue was measured. In this embodiment, only one filtration container 8 is used.

More specifically, in the dissolution steps of steps S1 (1) to S1 (3), 1.4 (L) of xylene was added as a PE solvent to each of the dissolution tanks 2 to 4 having a capacity of 2 (L). The xylene was stored and the xylene was heated to _{maintain the first temperature T 1} = 100-120 (° C.).
Of these, in the dissolution steps of steps S1 (1) and S1 (2), the inside of the filtration vessel 8 containing the sample was stirred by the stirring members 11 and 12, respectively, for 10 minutes. However, in the third dissolution step of step S1 (3), the inside of the filtration vessel 8 was stirred by the stirring member 13 for 3 minutes.
Further, in the drying step of step 4, the recovered PA residue was dried by a drier after removing the solution mainly containing xylene with a centrifugal filter.
In the distillation process of step S5, by solution maintained at a first temperature T ₁ of the post-lysis step of Step S1 (1), the residue of PE deposited by cooling to room temperature in the refrigerator 19, The mixture was separated by a centrifugal filter and dried while 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 recovery amount is the total weight of the residue PE _C A (PE) is 72.83 (g), and the recovery amount is the total weight of the residue PA _C A (PA) is 47.89 (g) and became. _Therefore, the weight ratio of C A (PE) and _C A (PA) is 60.2 (%): was 39.6 (%). Further, recovery of _C A (PE) and _C A total amount of (PA) is 120.72 (g), and the the total sampling volume 121.01 (g), 99.8 (% ) in a weight ratio of It became. Therefore, it was found that PE and PA were recovered with good efficiency.
The PE concentrations (% by weight) in the solutions stored in the first to third dissolution tanks 2 to 4 were 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. 4 (a) and 4 (b) 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 that high-purity PE and PA were regenerated, respectively.
As described above, from the results of Table 1 and FIG. 4, it was found that according to the separate collection method 30, the laminated film in which PE and PA are laminated in close contact with each other can be efficiently separated and collected according to the type.

Subsequently, the method of Example B will be described with reference to Table 2 and FIG. 5 (a) and 5 (b) are examples of the separate collection method according to the second embodiment, respectively.
The sample used in Example B is a wrap film in which EVA which is a soluble layer 50a and 50b and PO (a mixture of PP and PE) which is an insoluble layer 50c are laminated in close contact with each other without using an adhesive. Therefore, before the melting step of step S1 (1), the film was previously cut into small pieces having a maximum length of 50 to 70 mm.
About 30 g of this sample was collected 5 times, and the total weight (g) of the recovered EVA residue and PE residue was measured in the same manner as in Example A.
Further, cyclohexane was stored in each of the dissolution tanks 2 to 4 as a solvent for EVA in an amount of 1.4 (L), and the cyclohexane was heated to _{maintain the first temperature T 1} = 50 (° C.). Other than this, the method of Example B 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 amount of EVA residue recovered and the amount of PO residue recovered. As a result, the recovery amount _C B is the total weight of the residue EVA (EVA) is 58.10 (g), and the recovery amount is the total weight of the residue PE _C B (PE) and 91.32 (g) became. _Therefore, the weight ratio of C B (EVA) and _C B (PO) is 38.6 (%): was 60.6 (%). The total amount of the recovery amount _C A (EVA) and _C A (PO) whereas 149.42 (g), the total sampling volume 150.58 (g), in a weight ratio 99.2 (%) and 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, FIGS. 5 (a) and 5 (b) are IR spectra of 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 that high-purity EVA and PO were regenerated, respectively.
As described above, from the results of Table 2 and FIG. 5, it was found that according to the separate collection method 30, the wrap film in which EVA and PO are laminated in close contact with each other can be efficiently separated and collected according to the type.

Finally, the method of Example C will be described with reference to Table 3 and FIG. 5 (a) and 5 (b) are examples of the separate collection method according to the second embodiment, respectively.
The sample used in Example C is a laminated film in which PMMA, which is the soluble layers 50a and 50b, and PC, which is the insoluble layer 50c, are laminated in close contact with each other without using an adhesive, and is in step S1 (1). ), It is cut into small pieces having a maximum length of 5 to 20 mm in advance.
After collecting 3 g of this sample and putting it in a beaker having a volume of 100 (mL), 60 (mL) of acetone at room temperature was poured into the beaker as a solvent for PMMA, and the mixture was stirred with a stirrer for 20 minutes. Then, the residue of PC was taken out from a beaker, dried in a dryer, and recovered. That is, the dissolution step of step S1 (1), the separation step of step S2 (1), and the drying step of step 4 were carried out.
Further, the solution remaining in the beaker was dried while collecting acetone with a vacuum distillation apparatus, and the PMMA residue was recovered. That is, the distillation step of step S5 was carried out. 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, it became collection amount is the weight of the residue PMMA _C C (PMMA) is 2.5 (g), and the recovery amount _C C is the weight of the PC residue (PC) is 0.72 (g) .. _Therefore, the weight ratio of C C (PMMA) and _C C (PC) is 83.3 (%): was 24.0 (%). Further, it recovered amount _C C and (PMMA) the total amount of _C C (PC) is 3.22 (g), and the relative total 3 (g) of the sample collection amount, the weight ratio 107.3 and (%) rice field. From this result, it is considered that the solvent may remain in at least one of PMMA and PC due to insufficient drying. Therefore, IR spectra were measured for these.

6 (a) and 6 (b) 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 PMMA and PC having acceptable purity were regenerated, respectively.
As described above, from the results of Table 3 and FIG. 6, it was found that the laminated film in which PMMA and PC are laminated in close contact with each other can be efficiently separated and collected according to the type.

As described above, according to the separate recovery method 30, based on 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 used as a solvent type and an insoluble layer. By appropriately selecting the number of times the 50c is washed, it can be efficiently sorted and collected according to the type of resin film. Therefore, for example, it is possible to realize horizontal recycling of the composite material 50, which was conventionally unseparable, such as a laminated film.

Next, the separate collection method according to the first and second modifications of the separate collection method of Example 2 will be described with reference to FIG. 7. 7 (a) and 7 (b) are process diagrams of the method for separating and recovering the composite material according to the first and second modifications of Example 2, respectively. The components shown in FIGS. 1 to 6 are designated by the same reference numerals in FIG. 7, and the description thereof will be omitted. Further, since the reference numerals described in each paragraph match the reference numerals of the components shown in FIGS. 1 to 6 and 8, the description thereof will be omitted.

First, the configurations of the composite materials 50A and 50B, which are the objects of separate collection in this embodiment, will be described with reference to FIGS. 8 (b) and 8 (b), respectively. 8 (a) and 8 (b) are vertical cross-sectional views showing the structure of the composite material, 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 coat 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 separated and recovered. The aluminum layer 50d may be coated with only one of the soluble 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. Can't.
Therefore, it was decided to separate and recover the soluble layers 50a and 50b and the insoluble layer 50c of the composite materials 50A and 50B by carrying out the separate recovery method according to the first and second modifications of this example.

As shown in FIGS. 7 (a) and 7 (b), in the separate recovery methods 30a and 30b according to the first and second modifications of the second embodiment, the composite materials 50A and 50B have the aluminum layer 50d, respectively. When the aluminum layer 50d is provided, the solvent for the aluminum layer is heated to a second temperature by a heater (not shown) inside the aluminum layer melting tank (not shown) storing the solvent for the aluminum layer 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 (% by weight) sodium hydroxide, 2 to 10 (% by weight) dilute hydrochloric acid or dilute sulfuric acid is used. The second temperature T ₂ is 30 ° C. or higher and 90 ° C. or lower. Since the distillation step of step S5 and the return step of step S6 are the same as those of the separate recovery method 30, the illustration of these steps will be omitted.

As shown in FIG. 7A, in the separate recovery method 30a according to the first modification of Example 2, the aluminum layer melting step of step S7 is provided before the melting step of step S1 (1).
In the aluminum layer melting step of step S7, since the solvent for the aluminum layer is _{maintained at the second temperature T 2} , the aluminum layer 50d is dissolved in the solvent for the aluminum layer and changed to an aluminum solute. Therefore, a solution containing the aluminum solute and the composite material 50A from which the aluminum layer 50d has been removed is generated inside the aluminum layer melting tank.
Then, since the composite material 50A from which the aluminum solute and the aluminum layer 50d have been removed has been changed to a composite material having the same composition as the composite material 50, when the separate recovery method 30 is carried out on this composite material, The soluble layers 50a and 50b and the insoluble layer 50c are separately collected.
When the aluminum layer 50d is provided between the multi-layered insoluble layers 50c, the aluminum layer 50d is exposed to the surface by combining a plurality of separate separation methods 30 in which different types of solvents are selected. , It is advisable to newly implement the separate collection method 30a. That is, when the aluminum layer 50d is provided between the multilayer insoluble layers 50c, the separate recovery method 30a is applied.

Further, in the separate recovery method 30b according to the second modification of Example 2, the aluminum layer melting step of step S7 is a step 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, inside the third melting 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 melting tank and the aluminum layer melting step of step S7 is carried out, the insoluble layer 50c is separated and recovered.

As described above, according to the separate recovery methods 30a and 30b, the aluminum layer 50d can be removed even when the composite material includes the aluminum layer 50d as in the composite materials 50A and 50B. .. More specifically, among the 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 landfilled and incinerated in the past.

The separate collection methods 30, 30a, 30b according to the present invention and the separate collection device 1 used therein are not limited to those shown in the present embodiment. For example, in the repeating step of step S3, the melting step and the separating step are carried out only once, and these steps may be repeated twice or four times or more, respectively.
Further, the drying step of step 4, the returning step of step 6, and the returning step of the storage tank solution may be omitted respectively. Further, in the storage tank 18, the cooling device 19 may be omitted, and the solution may be cooled by leaving it to stand.
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 in close contact with each other and difficult to separate, the separate recovery method 30 in which different types of solvents are selected for the insoluble layer 50c can be used. , May be carried out again.

INDUSTRIAL APPLICABILITY The present invention can be used as a separate recovery method for efficiently separating and recovering a composite material in which a plurality of types of resin films are laminated in a difficult-to-separate manner, and a separate recovery device used therefor.

1 ... Separation and recovery device 2-4 ... Melting tank 2a-4a ... Lid body 2b-4b ... Upper edge 5-7 ... Heater 8-10 ... Filter container 11-13 ... Stirring member 11a ... Shaft body 11b ... Horizontal bar 11c ... Stir bar 11d ... Cross clamp 14-16 ... Motor 17 ... Support rod 18 ... Storage tank 18a ... Transfer pipe 18b ... Return pipe 19 ... Cooling device 20 ... Distiller 20a ... Transfer pipe 21 ... Return pipe 21a ... Condenser 22, 23 ... Channels 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 (6)

A method for separating and recovering a composite material having a plurality of types of resin films to be laminated.
The composite material comprises a soluble layer formed on at least one of its surfaces and selectively soluble in a solvent, and an insoluble layer that adheres to the soluble layer and is insoluble in the solvent.
Inside the dissolution tank in which the solvent is stored, the solvent is maintained at a first temperature to dissolve the soluble layer, and a solution containing the solute in which the soluble layer is dissolved and the insoluble layer is produced. A repeating step of repeating the step and the separation step of separating the insoluble layer from the solution m times (m is a desired natural number), and
After the first of the separation steps, the solution after the insoluble layer is separated, the solution及Biko distilling the solution adsorbed onto the solute precipitated by cooling, thereby recovering said solute the Distillation process to purify the solvent and
After the distillation step, a step of returning the purified solvent to at least one of the dissolution tanks in which the same number of times as the number of times is installed is provided.
The soluble layer is made of an ethylene-vinyl acetate copolymer resin.
The insoluble layer is made of polyethylene or polypropylene and is made of polyethylene or polypropylene.
The solvent is cyclohexane and
A method for separating and recovering a composite material, wherein the first temperature is 40 ° C. or higher and lower than the boiling point of the solvent. A method for separating and recovering a composite material having a plurality of types of resin films to be laminated.
The composite material comprises a soluble layer formed on at least one of its surfaces and selectively soluble in a solvent, and an insoluble layer that adheres to the soluble layer and is insoluble in the solvent.
Inside the dissolution tank in which the solvent is stored, the solvent is maintained at a first temperature to dissolve the soluble layer, and a solution containing the solute in which the soluble layer is dissolved and the insoluble layer is produced. A repeating step of repeating the step and the separation step of separating the insoluble layer from the solution m times (m is a desired natural number), and
After the first of the separation steps, the solution after the insoluble layer is separated, the solution及Biko distilling the solution adsorbed onto the solute precipitated by cooling, thereby recovering said solute the Distillation process to purify the solvent and
After the distillation step, a step of returning the purified solvent to at least one of the dissolution tanks in which the same number of times as the number of times is installed is provided.
The soluble layer is made of acrylic resin and is made of acrylic resin.
The insoluble layer is made of polycarbonate and 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.
A method for separating and recovering a composite material, wherein the first temperature is 20 ° C. or higher and lower than the boiling point of the solvent. A method for separating and recovering a composite material having a plurality of types of resin films to be laminated.
The composite material coats a soluble layer formed on at least one of the surfaces thereof and selectively soluble in a solvent, an insoluble layer that adheres to the soluble layer and is insoluble in the solvent, and the soluble layer. With an aluminum layer ,
Inside the dissolution tank in which the solvent is stored, the solvent is maintained at a first temperature to dissolve the soluble layer, and a solution containing the solute in which the soluble layer is dissolved and the insoluble layer is produced. A repeating step of repeating the step and the separation step of separating the insoluble layer from the solution m times (m is a desired natural number), and
After the first separation step, the solution after the insoluble layer is separated and / or the solution adsorbed on the solute precipitated by cooling the solution is distilled to recover the solute. A distillation step of purifying the solvent and
An aluminum layer melting step is provided in which the solvent for the aluminum layer is maintained at a second temperature to dissolve the aluminum layer inside the aluminum layer melting tank in which the solvent for the aluminum layer that selectively dissolves the aluminum layer is stored. ,
This aluminum layer melting step is provided before the first melting step.
The solvent for the aluminum layer is an alkali or an acid, and the solvent is
The second temperature is 30 ° C. or higher and 90 ° C. or lower.
A method for separating and recovering a composite material, wherein the melting tank is installed in the same number as the m times. A separate recovery device used in the separate recovery method for a composite material according to claim 1 or 2.
With the m melting tanks
The m first heaters, which are installed in the m melting tanks and maintain the solvent at the first temperature, respectively.
With at least one filtration vessel accommodating the composite material or the insoluble layer and filtering the insoluble layer to separate it from the solution.
The m stirring members provided in the m melting tanks and stirring the composite material or the insoluble layer contained in the filtration vessel, respectively.
The m motors that drive the m stirring members, respectively, and the m motors.
A storage tank in which the solution stored in the first dissolution tank is transferred and stored, and
It said accumulated in the dissolution tank 1 th solution, equipped with a distillation device for distilling the solution adsorbed onto the solute precipitated by cooling the solution stored in及beauty before Symbol reservoir,
When the m is a natural number of 2 or more, the nth melting tank (n = m, m-1, 2, n is a natural number of 2 or more) has a height of the upper edge of (n). -1) The nth melting tank is arranged so as to be equal to or higher than the height of the upper edge of the (n-1) th melting tank, and the n-1th melting tank is transferred to the (n-1) th melting tank. A separate and recovery device characterized in that each flow path through which a solution flows is provided. A separate recovery device used in the separate recovery method for a composite material according to claim 3.
With the m melting tanks
The aluminum layer dissolution tank storing the solvent for the aluminum layer that selectively dissolves the aluminum layer, and the aluminum layer dissolution tank.
The m first heaters, which are installed in the m melting tanks and maintain the solvent at the first temperature, respectively.
Inside the aluminum layer melting tank, a second heater that maintains the solvent for the aluminum layer at the second temperature, and
With at least one filtration vessel accommodating the composite material or the insoluble layer and filtering the insoluble layer to separate it from the solution.
The m stirring members provided in the m melting tanks and stirring the composite material or the insoluble layer contained in the filtration vessel, respectively.
The m motors that drive the m stirring members, respectively, and the m motors.
A storage tank in which the solution stored in the first dissolution tank is transferred and stored, and
A distillation apparatus is provided for distilling the solution adsorbed on the solute precipitated by cooling the solution stored in the first dissolution tank and / or the solution stored in the storage tank.
When the m is a natural number of 2 or more, the nth melting tank (n = m, m-1, 2, n is a natural number of 2 or more) has a height of the upper edge of (n). -1) The nth melting tank is arranged so as to be equal to or higher than the height of the upper edge of the (n-1) th melting tank, and the n-1th melting tank is transferred to the (n-1) th melting tank. A separate and recovery device characterized in that each flow path through which a solution flows is provided. The stirring member includes a shaft body coaxially connected to the rotation shaft of the motor, and a plurality of stirring rods branched from the shaft body.
More the stirring bar is separate collection apparatus according to claim 4 or claim 5, characterized in that the distal ends are spaced from each other across the shaft body.

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