JP7258324B2 - Method for bonding resin using carbon dioxide, bonded object therefor, and apparatus for bonding resin - Google Patents

Description

TECHNICAL FIELD The present invention relates to a resin bonding method using carbon dioxide, an adhesive product using the method, and a resin bonding apparatus. A method of fixing and adhering the resin in a state where the shape is fixed by pressing in a plasticized state to deform the resin surface so as to be engaged, and discharging carbon dioxide in the pressed state, and the adherend and its realization It relates to a device for

Porous bodies having continuous pores are used for filter applications by themselves, and for industrial applications when carrying a catalyst. When producing a porous body using resin, it is common to mix a foaming agent with the resin raw material and foam it during the molding process. Further, in the case of carrying a carrier on a porous body, it was common to introduce the carrier afterward into the finished porous body.

On the other hand, there is also a method of overlapping resin sheets to form a porous body. There is a method in which the resin sheet is stacked on another resin sheet before being pressed, but the problem of clogging the pores of the porous body and the method of stacking one layer at a time reduces the productivity of multilayer lamination, and it is composed of several layers. However, the application was limited to non-woven fabric filters. In the case of the method of laminating sheets, it seems easy to carry a drug or catalyst inside, but as long as the above method is used, the drug inserted between the sheets will be taken into the adhesive or the molten resin. hard to avoid. In addition, in the case of medical and food applications, there are problems such as the influence of the solvent component of the adhesive on foods, and heat denaturation of the chemical in the case of a chemical that is sensitive to heat.

As a bonding method that does not use an adhesive, as a prior art, for example, solid resin fine particles are welded using carbon dioxide in a subcritical or supercritical state, and open cells in which voids are formed between the particles and a method of manufacturing a structure such as a support for biological culture (Patent Document 1).

However, in this method, specifically, the resin fine particles are brought into a subcritical or supercritical state to weld the resin surface. In the process of releasing, the carbon dioxide that has entered the resin has the property of acting as a so-called release agent that separates the resins when desorbing (discharging), and there is no clear method for avoiding this. That is, in the method shown in the example of Patent Document 1, a very slow decompression method is shown, but the decompression rate is preventively in a fairly wide range of 0.01 MPa / min to 10 MPa / min. However, it is unknown how to avoid the action of carbon dioxide acting as a release agent, which occurs when the pressure is rapidly reduced.

On the other hand, in the present invention, the step of releasing (discharging) carbon dioxide is preferably performed under conditions of 10 MPa/10 seconds or less, preferably instantaneous release to the atmosphere using a ball valve or the like, and high-speed processing is possible. Therefore, it has an advantage over the prior art. In addition, carbon dioxide is discharged from continuous pores opened in the fibrous adhesive in a pressed state, thereby suppressing carbon dioxide from acting as a releasing agent.

In addition, as other prior art developed by the present inventors, there is a process of plasticizing the resin by impregnating the resin with carbon dioxide by bringing liquid carbon dioxide into contact with the resin surface, and a mold for the plasticized resin. A method and apparatus for transferring the fine structure of the mold surface to the resin (Patent Document 2) have been proposed. However, this method and apparatus are intended to transfer the fine structure of the surface of the mold to the resin. It is not assumed at all that the resin surfaces are deformed so as to mesh with each other, and carbon dioxide is discharged while the resins are pressed to fix the shape and adhere or join them while the resins are meshed with each other.

As shown in the prior art (Patent Document 2), the present inventor first brought liquid carbon dioxide into contact with the surface of the resin to impregnate the resin with carbon dioxide to plasticize the resin. Then, by pressing the mold against the plasticized resin, we developed a shape transfer method and device that can realize the merits of the imprint method that can transfer the fine structure of the mold surface to the resin in a short time. We have applied for a patent, but in the process of further research and development, we use carbon dioxide in a liquid, gas-liquid mixed state, or near-liquid state to plasticize the surface of the fibrous resin and press it. It was found that by deforming the resin surface so as to mesh and discharging carbon dioxide in a pressed state, it is possible to fix the shape and bond and join the resin in the meshed state. was completed.

Patent No. 5205636 JP 2014-188950 A

The present invention is essentially different in bonding principle from the prior art disclosed in Patent Document 1 in that it does not employ a method of fusing resins together over time. Moreover, the present invention differs from the prior art in that it does not assume molding without applying a load, and always targets bonding and molding under press conditions. In addition, in the present invention, carbon dioxide is impregnated into the resin only on the surface layer, so there is no need to wait for the resin to start welding, and the decompression is also rapid, so the processing time from the introduction of carbon dioxide to the completion of discharge can be maximized. It is also characterized by a high-speed process of 5 minutes at .

Although the present invention does not restrict three-dimensional adhesion, basically, two-dimensional porous-like or cotton-like fibrous resin sheets are laminated while carbon dioxide is applied without applying a high temperature. An object of the present invention is to provide a method of bonding with a chisel and an adhesive therefor.
In addition, the present invention provides adhesives in which foodstuffs, drugs, enzymes, catalysts, etc. are included between fibrous resin sheets, and resin sheet adhesives in which fibrous resin sheets having different functions are superimposed and laminated. It is intended to provide
Further, the present invention makes it possible to easily control the sustained release property of a drug encapsulating material carrying a drug or the like, and to control the sustained release property by the number of laminated resin sheets. The object is to provide a medicinal adhesive or the like that enables
A further object of the present invention is to provide the above-described bonding method, an adhered article, and a resin bonding apparatus capable of realizing them.

The present invention for solving the above problems consists of the following technical means.
(1) A method for bonding fibrous resin,
A step of plasticizing the surface of the fibrous resin by impregnating the resin with carbon dioxide in a liquid or a gas-liquid mixed state or a state close to the liquid, and pressing the resin surface in a plasticized state. a step of deforming the resin surface so that it meshes with each other; and a step of fixing the shape and bonding the resin in the meshed state by discharging carbon dioxide in the pressed state. Method.
(2) introducing liquid or gaseous carbon dioxide into a sealed container; in the case of gas introduction, the gaseous carbon dioxide is liquefied or compressed by reducing the volume of the closed container with a piston; The resin is impregnated with carbon dioxide by bringing carbon dioxide in a similar state into contact with the resin to plasticize the surface of the fibrous resin, and the plasticized resin is pressed by lowering the piston as it is to press the resin surface. The method according to (1) above, wherein the step of deforming to mesh.
(3) While the fibrous resin is pressed, carbon dioxide in a liquid state, gas-liquid mixed state, or near-liquid state is circulated through the fibrous resin to plasticize the surface of the fibrous resin and press it. The method according to (1) above, wherein the surface of the resin in a plasticized state is deformed so as to mesh with it.
(4) The method according to any one of (1) to (3) above, wherein the fibrous resin is a thermoplastic resin.
(5) The method according to any one of (1) to (3) above, wherein the fibrous resin is a composite material containing a thermoplastic resin.
(6) The method according to any one of (1) to (5) above, wherein the fibrous resin is a porous resin sheet.
(7) The method according to any one of (1) to (5) above, wherein the fibrous resin is a cottony resin.
(8) As a fibrous resin, one selected from foodstuffs, drugs (medicine, agriculture, industry), pigments, adsorbents, deodorants, fragrances, insect repellents, electronic device materials, enzymes or catalysts. The method according to any one of the above (1) to (7), wherein the resin supporting is used.
(9) The method according to any one of (1) to (8) above, wherein a plurality of resins having different properties are used as the fibrous resin.
(10) A method of carrying out a plurality of adhesion treatments at the same time by performing the adhesion methods described in (1) to (9) with one or more separators interposed therebetween.
(11) An adhesive having a structure in which fibrous resins bonded by the bonding method according to any one of (1) to (10) are bonded or bonded in a single layer or multiple layers. In addition, an adhesive having a structure in which fibrous resins are bonded or joined in a single layer or multiple layers, the surface of the fibrous resin is not melted, and the dioxide is in a liquid or a gas-liquid mixed state or a state close to liquid. An adherent whose shape is fixed and adhered while being plasticized by carbon and being deformed so that the resin surface is engaged.
(12) An apparatus used in the resin bonding method according to any one of (1), (2), (4) to (10) above,
Consists of a base portion and a container portion,
The base portion can hold a fibrous resin that is a material to be treated,
The container portion has an opening into which the resin held by the base portion is inserted, and the opening portion can be brought into close contact with the base portion. having a piston as a means for liquefying carbon dioxide by maintaining or reducing the volume of said enclosed space, the piston being an introduction of liquid or gaseous carbon dioxide into said enclosed space, and It has a carbon discharge part and has the ability to press fibrous resin,
a step of disposing the resin in the space formed by the base portion and the container portion;
immersing the surface of the resin in liquid carbon dioxide to plasticize it;
a step of pressing the plasticized resin;
a step of releasing carbon dioxide;
The apparatus is characterized in that by performing these series of steps, the shape of the fibrous resin is fixed in a meshed state and adhered.
(13) The above-described (12), wherein unevenness is provided on the surface of the base portion or the piston to change the pressing strength of the in-plane fibrous resin, thereby enabling partial adhesion. device .
( 14 ) The adhesive according to (11) above, wherein the fibrous resin is a thermoplastic resin.
( 15 ) The adhesive according to (11), wherein the fibrous resin is a composite material containing a thermoplastic resin.
(1 6 ) The adhesive according to any one of (11), (1 4 ) to (1 5 ), wherein the fibrous resin is a porous resin sheet.
(1 7 ) The adhesive according to any one of (11), (1 4 ) to (1 5 ), wherein the fibrous resin is a cotton-like resin.
(1 8 ) fibrous resins are selected from foodstuffs, drugs (medicine, agriculture, industry), pigments, adsorbents, deodorants, fragrances, insect repellents, electronic device materials, enzymes or catalysts, among others The adhesive according to any one of the above (11), (1 4 ) to (1 7 ), which is a resin supporting one species.
(1 9 ) The adhesive according to any one of (11), (1 4 ) to (1 8 ), wherein the fibrous resin is a plurality of resins having different properties.
(20) An apparatus used in the resin bonding method according to any one of (1), (2), (4) to (10) above,
Consists of a base portion and a container portion,
The base portion can hold a fibrous resin that is a material to be treated,
The container portion has an opening into which the resin held by the base portion is inserted, and the opening portion can be brought into close contact with the base portion. has a liquid or gaseous carbon dioxide introduction part into the sealed space and a carbon dioxide discharge part, and liquefies or compresses the carbon dioxide by maintaining or reducing the volume of the sealed space Having a piston as a means, the piston has the ability to press fibrous resin,
a step of disposing the resin in the space formed by the base portion and the container portion;
immersing the surface of the resin in liquid carbon dioxide to plasticize it;
a step of pressing the plasticized resin;
a step of releasing carbon dioxide;
The apparatus is characterized in that by performing these series of steps, the shape of the fibrous resin is fixed in a meshed state and adhered.
(21) The above-described (20), wherein unevenness is provided on the surface of the base portion or the piston to change the press strength of the in-plane fibrous resin, thereby enabling partial adhesion. device.
(22) An apparatus used in the resin bonding method according to any one of (1) and (3) to (9), comprising a base portion,
The base portion is capable of holding the fibrous resin, which is the material to be treated, with the edge of the fibrous resin open to the atmosphere, and has a carbon dioxide inlet,
The piston has the ability to press fibrous resin,
The process of pressing the resin,
A step of injecting carbon dioxide in a pressed state, and plasticizing and deforming the surface of the resin in the process in which carbon dioxide oozes out from the edges of the pressed fibrous resin;
A step of stopping the injection and discharging carbon dioxide into the atmosphere from the edge of the pressed fibrous resin,
The apparatus is characterized in that by performing these series of steps, the shape of the fibrous resin is fixed in a meshed state and adhered.

Next, the present invention will be described in more detail.
The present invention is a method for adhering fibrous resin, in which carbon dioxide in a liquid, gas-liquid mixed state, or near-liquid state is brought into contact with the resin to impregnate the resin with carbon dioxide, thereby bonding the surface of the fibrous resin. A process of plasticizing the resin, a process of pressing the resin in a plasticized state to deform the resin surface so that it meshes, and a process of releasing carbon dioxide in the pressed state to fix the shape while the resin is meshed. and a step of adhering.

Regarding fibrous resins, the present inventors have found that certain resins such as polyester, acrylic, polycarbonate, polyvinyl chloride, and ABS resins are plasticized on the surface even with liquid carbon dioxide, and are pressed in a plasticized state. Through experiments, it was discovered that by deforming the resin surfaces so as to mesh with each other and releasing carbon dioxide in the pressed state, it is possible to fix the shape and bond the resins together by bonding. In particular, when carbon dioxide in a liquid or gas-liquid mixed state is used, the shape can be fixed at room temperature for bonding, so there is an advantage that the apparatus does not require a heating mechanism.

In the present invention, the carbon dioxide is liquefied by pressurizing the carbon dioxide introduced in the form of gas or liquid into the container portion (pressure container). In that case, it is not necessary to liquefy all the carbon dioxide in the pressure vessel, and it is sufficient to liquefy to the extent that the surface of the fibrous resin that is the material to be treated is soaked. Therefore, the present invention has the advantage of not requiring a large-scale apparatus because the pressing force can be reduced compared to the conventional technique using subcritical or supercritical carbon dioxide.

The method and apparatus for adhering fibrous resins of the present invention involve bringing carbon dioxide in a liquid, gas-liquid mixed state, or near-liquid state into contact with the surface of the resin to impregnate the resin with carbon dioxide, thereby plasticizing the resin. and a step of fixing and bonding the shape in a state where the resin is engaged by discharging carbon dioxide while the plasticized resin is pressed.

In the present invention, substantially liquid carbon dioxide or gas-liquid mixture carbon dioxide is used. The advantages of using liquid carbon dioxide or gas-liquid mixed carbon dioxide compared to using gaseous carbon dioxide or supercritical carbon dioxide are as follows. That is, while carbon dioxide in a supercritical state needs to be heated to 31°C or higher, it is not necessary to heat the gas or liquid significantly, so a heating mechanism may be unnecessary in the device. Therefore, liquid carbon dioxide or carbon dioxide in a gas-liquid mixed state is preferred.

Among these, gaseous carbon dioxide hardly plasticizes or requires a considerable amount of time for plasticization. State carbon dioxide is preferred.

Compared to the supercritical state, the liquid state, especially the gas-liquid mixed state, is relatively easy to control the pressure and temperature, and the time range for contacting carbon dioxide with the resin surface can be selected widely. From a certain point of view, these states are preferred. The gas-liquid mixed state has the advantage that even if the volume of the closed space containing carbon dioxide changes, the pressure changes only by changing the ratio of the gas phase and the liquid phase. In addition, in terms of the gas mixture state, when using a piston to change the volume of a sealed space containing carbon dioxide, the torque becomes constant when the piston moves, and from the carbon dioxide to the piston Since the applied load is constant, there is an advantage that the detection accuracy of the load by the press is increased, and it is excellent in safety and controllability.

In the present invention, the carbon dioxide in the liquid or gas-liquid mixed state is, for example, 3 MPa to 7 MPa and 0 ° C. to 30 ° C., but from the viewpoint of rapid plasticization of the resin and thus improvement of throughput, It is preferably 0° C. or higher and 3 MPa or higher. Further, from the viewpoint of temperature control, 20° C. to 30° C., which can be realized with hot water or the like and is easy to control, is more preferable. In addition, even in a supercritical state where the temperature exceeds 30 ° C, the density of near-liquid carbon dioxide is 0.4 g / mL (approximately half the density of liquid carbon dioxide) or more (near-liquid state) ), the effect of making the torque constant when the piston moves cannot be expected, but adhesion itself is possible.

The pressure of carbon dioxide is preferably 7 MPa or less. Carbon dioxide in a gas-liquid mixed state (on the liquid/gas boundary line) is preferable from the viewpoint of temperature and pressure control. In the phase diagram of carbon dioxide represented by pressure and temperature, carbon dioxide in the region surrounded by the liquid/gas boundary line, the temperature line of 0° C., and the pressure line of 7.38 MPa is preferable. In addition, even in a supercritical state, the pressure is selected so that the density of carbon dioxide close to liquid can be maintained at 0.4 g / mL (about half the density of liquid carbon dioxide) or more. It is possible, and needless to say, the scope of the present invention also includes the use of subcritical or supercritical carbon dioxide in the bonding process.

In the present invention, a process of plasticizing a resin by impregnating the resin with carbon dioxide by bringing the carbon dioxide in a liquid state, a gas-liquid mixed state, or a state close to a liquid into contact with the surface of the resin, that is, a process in which the resin is placed in a closed space. A step of placing, a step of introducing liquid carbon dioxide into the closed space to plasticize the surface of the fibrous resin, and a step of discharging carbon dioxide, and pressing in the plasticized state to engage the resin surface It is characterized by including a step of fixing and bonding the shape in a state where the resin is engaged by deforming and discharging carbon dioxide in a pressed state. The advantage of liquid introduction is that the compression process for liquefaction can be omitted compared to gas introduction, so that the plasticization time can be shortened and rapid plasticization can be achieved.

In the present invention, when the resin is plasticized by impregnating the resin with carbon dioxide in a liquid state, a gas-liquid mixed state, or a state close to the liquid state, the resin is placed in a closed space. and after introducing the gaseous carbon dioxide into the enclosed space, the volume of the enclosed space is reduced to liquefy the carbon dioxide. The advantages of gas introduction and pressurization are that, compared to liquid introduction, gas is introduced, the process is easy, a pressurization pump can be dispensed with, and the apparatus can be simplified.

In the present invention, as another aspect, the piston is pressed against the fibrous resin without using a processing container, so that the piston, the base portion, and the resin hold carbon dioxide in a liquid state, a gas-liquid mixed state, or a state close to a liquid state. It is possible to configure a space that In this case, the edge of the resin in contact with the atmosphere acts as a discharge valve with reduced discharge. In this method, since a liquefaction process using a piston cannot be used, liquid carbon dioxide is directly injected into the fibrous resin, and carbon dioxide in a liquid, gas-liquid mixed state, or a state close to liquid is injected into the fibrous resin. should be generated. Therefore, it is necessary to provide a carbon dioxide inlet in the base and inject liquid carbon dioxide using a pump. Also, the flow rate of the pump is adjusted so that the pressure is maintained above the vapor pressure (ie liquid carbon dioxide is introduced). In this case, although there is a disadvantage of using a pump, there is a great advantage that the object to be treated can be spot treated without the need for a large treatment container that covers the entire resin to be treated. Alternatively, by changing the position a little and repeatedly pressing, or by using a roller instead of a piston to apply pressure to the resin sheet, it is possible to feed the resin as a sheet and make it a continuous process, shortening the takt time and automating it. It has the great advantage of facilitating

The present invention is characterized in that the resin is a thermoplastic resin. The resin is more preferably an amorphous thermoplastic resin or a thermoplastic resin with a reduced degree of crystallinity, since plasticization of the resin by impregnation with carbon dioxide is relatively effective. Amorphous thermoplastic resins or thermoplastic resins with reduced crystallinity include, for example, ABS resin (hereinafter referred to as ABS), acrylic resin (hereinafter referred to as PMMA), polyethylene terephthalate (hereinafter referred to as PET) , polycarbonate (hereinafter referred to as PC), polyvinyl chloride (hereinafter referred to as PVC), polystyrene (hereinafter referred to as PS), cyclic olefin copolymer (hereinafter referred to as COC), cycloolefin polymer (hereinafter referred to as COP ) and polypropylene (hereinafter referred to as PP). More preferably, the resin is an amorphous thermoplastic resin with polar groups (eg, ABS, PMMA, PET, PC, PVC). This is because these resins are more effective at plasticizing the resin by impregnation with liquid carbon dioxide. In addition, it is also possible to bond composite materials containing thermoplastic resins such as cellulose-polyester composite materials.

1. Re-adhesion of adhesives adhered by the method of the present invention In order to confirm that the adhesives adhered by the method of the present invention can be further re-adhered, 128 sheets of PET nonwoven fabric were adhered to resin porous bodies (three pieces). were prepared and tried to be re-adhered by the method of the present invention. As a result, the resin porous bodies (three pieces) were rebonded to form one long porous body. This is because the bonded material obtained by this technique maintains the shape of the fiber. That is, the fibers to be bonded by the method of the present invention include adhesives bonded by the method of the present invention. includes.

2. Adhesion in which a fiber not plasticized by carbon dioxide is sandwiched between resin fibers The present invention includes adhesion of resin fibers, support of catalysts , drugs , etc., and further plasticization by carbon dioxide between adhesives. Bonding can include sandwiching non-woven fibers (eg, metal fibers such as copper mesh). In the present invention, for example, it is possible to bond by sandwiching a copper mesh between the adhesives, thereby making it possible to make a conductive fiber or a product thereof in which an electrode of an electronic device is provided between the adhesives. be. That is, in the present invention, as the fibrous resin, it is possible to provide the conductive layer by sandwiching fibers made of a material such as metal that is not plasticized by carbon dioxide.

3. Simultaneous adhesion A method of producing multiple pieces at once is effective for improving productivity. Pushing with a piston is applying pressure, and the pressure does not change no matter how many sheets are sandwiched in series via a separator. If the area of the piston is increased by arranging them on a plane, the pressure must be increased, increasing the operating load of the device. In the embodiment, an example of five sheets is shown, but theoretically there is no limit to the number of sheets.

The present invention also relates to an apparatus for use in the invention according to the method of the present invention. The device is composed of a base and a container, the container has an opening, and the resin can be introduced into a closed space composed of the base and the container by a simple operation, and It is also easy to take out the resin after the treatment. Also, a means for reducing (compressing) the volume of the sealed space is a piston.

The device according to the present invention has, for example, a piston as means for holding or reducing (compressing) the volume of the closed space, and the piston has the ability to press the resin while the surface of the resin is plasticized. Therefore, it is possible to press the resin in a closed space.

[Overview of technology]
Here, to summarize the outline of the technology according to the present invention, the present invention presses the surface of a fibrous resin in a plasticized state with carbon dioxide in a liquid, gas-liquid mixed state, or near-liquid state to flatten the resin surface. The present invention relates to a technique for fixing and bonding resins in a meshed state by deforming them so as to mesh with each other and discharging carbon dioxide in a pressed state. In the present invention, "the resin surface is deformed so as to mesh with each other, and the shape is fixed and adhered while the resin is meshed" means that, as shown in FIG. It refers to bonding in a state where a well-defined recess of the resin fiber is observed. A schematic of the device of the present invention is shown in FIG. Next, an example of a processing method assumed by this device will be specifically described.

[Processing method 1]
In processing method 1, a fibrous resin is set in a closed space composed of a base, a pressure vessel, and a piston. Carbon dioxide gas, which is close to vapor pressure, is introduced, and the piston is lowered to compress and liquefy to form a resin sheet. After plasticizing with liquid carbon dioxide, press to deform the resin surface so that it meshes, and by discharging carbon dioxide in the pressed state, the shape is fixed and adhered while the resin is meshed. be.

The flow of processing method 1 and the operation of the apparatus are shown in order from (a) to (h) below. The first stage, that is, the step of plasticizing the resin, includes the step (a) of placing the fibrous resin in the space formed by connecting the pressure vessel (container portion) and the base portion, lowering the piston and Part) and the base portion form a closed space (b), the step (c) of introducing gaseous carbon dioxide, the piston is lowered, and the volume of the pressure vessel, that is, the pressure vessel, the piston, and the base portion. The step (d) of reducing the volume of the enclosed space, liquefying the carbon dioxide, and soaking the fibrous resin in the liquid carbon dioxide is carried out in this order. Through these series of steps, the surface of the resin becomes plasticized. The degree of plasticization of the resin can be adjusted by selecting the duration of step (d) soaking the resin in liquid carbon dioxide.

In the latter step, that is, the step of pressing the resin, the piston is further lowered, and the step (e) of pressing the resin fibers whose surfaces are plasticized by the piston and the base portion is performed. The step (f) of pressing, the step (g) of returning the piston, and the step (h) of taking out the bonded resin are performed in this order. Through these series of steps, the resin surfaces are deformed so as to mesh with each other, and carbon dioxide is discharged while the resins are pressed, so that the bonded resin can be obtained with the shape fixed in the meshed state. The degree of adhesion can be adjusted by the plasticizing time selected in step (d) and the press pressure in step (e).

[Processing method 2]
In processing method 2, a fibrous resin is set in a closed space composed of a base portion and a pressure vessel, pressed, and then liquid carbon dioxide is introduced to plasticize the resin sheet with liquid carbon dioxide. 2) A method in which the plasticized state is pressed to deform the surfaces so as to engage with each other, and the shape is fixed in the state in which the resin is engaged to bond. Since liquid carbon dioxide is introduced from the beginning, the process of processing method 1, in which the piston is lowered to liquefy the carbon dioxide, is omitted.

The flow of processing method 2 and the operation of the apparatus are shown in order from (a) to (g) below. The first stage is the step (a) of setting the fibrous resin in the space formed by connecting the pressure vessel (vessel part) and the base part, lowering the piston and sealing the piston, the pressure vessel (vessel part) and the base part. The step (b) of forming the space and the step (c) of introducing liquid carbon dioxide and soaking the surface of the resin sheet with the liquid carbon dioxide are carried out in this order. A series of these steps brings the resin into a plasticized state. The degree of plasticization of the resin can be adjusted by selecting the duration of step (c) soaking the resin in liquid carbon dioxide. When the liquid carbon dioxide is introduced, part of it is vaporized, but it is sufficient if the gas-liquid mixture is formed and the surface of the resin is covered with the liquid carbon dioxide.

Then, in the latter stage, the piston is lowered and the resin fibers whose surfaces are plasticized are pressed between the piston and the base portion (d), the carbon dioxide is discharged and the shape is fixed in a state where the fibers are engaged (e), and the piston is lowered. The returning step (f) and the step (g) of taking out the bonded resin are performed in this order. Through these series of steps, the resin surfaces are deformed so as to mesh with each other, and carbon dioxide is discharged while the resins are pressed, so that the bonded resin can be obtained with the shape fixed in the meshed state.

[Processing method 3]
In processing method 3, a fibrous resin is set between the base and the piston without using a pressure vessel. By plasticizing, the surface of the resin is deformed so that it fits into the pressed state, and the shape is fixed in the state where the resin is meshed.

The flow of processing method 3 and the operation of the apparatus are shown in the order of (a) to (e) below. Step (a) of setting fibrous resin on the base part, step (b) of lowering the piston and pressing the fibrous resin with the piston and the base part, liquid carbon dioxide in the pressed fibrous resin is injected, and the surface of the fibrous resin is plasticized with liquid carbon dioxide, so that the surface of the resin is deformed so that it fits into the pressed state (c), and the step of returning the piston (d) ) and the step (e) of taking out the bonded resin. Through a series of these steps, the resin surface is deformed so as to be engaged, and carbon dioxide is discharged in a pressed state, thereby obtaining a resin that is fixed in shape and adhered while the resin is engaged. The degree of adhesion can be adjusted by selecting the pressing pressure in step (b) and the duration of the step of injecting liquid carbon dioxide into the resin in step (c).

The present invention can be carried out by any of the processing methods 1 to 3. The specific processes and conditions for carrying out the present invention can be appropriately changed within the same or equivalent range as the processes and conditions shown in Examples 1 to 11. Further, the basic configuration of the device of the present invention is, for example, a device equipped with a carbon dioxide introduction valve, a carbon dioxide discharge valve, a pressure vessel, a piston, and a base portion, as shown in FIG. , the specific configuration thereof can be appropriately designed as necessary, and the configuration is not limited.

In the embodiment of the apparatus shown in FIG. 19, the base portion (2) can hold fibrous resin (1), which is the material to be treated. The pressure vessel (3) serves as a container section and has a structure having an opening that can be brought into close contact with the base section (2), so that the base section (2) and the piston (6) can form a sealed space. Liquid or gaseous carbon dioxide can be introduced into the closed space through a carbon dioxide introduction valve (4) connected to the pressure vessel (3). A piston (6) provides a means for maintaining or reducing the volume of the enclosed space. By sandwiching the fibrous resin (1) between the tip of the piston (6) and the base portion (2), pressing in the presence of carbon dioxide is realized. In the figure, (5) indicates a carbon dioxide discharge valve.

FIG. 20 shows an embodiment in which the base portion of FIG. 19 is replaced by a piston. The base portion does not need to be a plate, and any configuration can be applied as long as it has a structure capable of pressing resin.

FIG. 21 shows an embodiment in which the base and container are integrated. However, in the case of such a form, it is difficult to separate the base part and the container to take out the processed material sticking to the bottom of the container, so as shown in FIG. It is necessary to devise a configuration in which the carbon dioxide is sent to the bottom while the piston is lifted to blow away the material to be treated that is stuck to the bottom.

The position and number of carbon dioxide inlets and outlets are appropriately selected depending on the sample to be treated and the shape of the container. It should be noted that it is not necessary to provide both an inlet and an outlet in the container, and there is also an embodiment in which the container is provided with one inlet serving both as an inlet and an outlet, as shown in FIG.

FIG. 28 shows an embodiment in which the carbon dioxide introduction/discharge part is provided on the side of the piston instead of the container. By providing the carbon dioxide inlet and outlet on the piston side, the container can be easily removed. This means that you can set the material in a container at another location, set it under the piston connected to the pipe, press it, and then move the container to another location to take out the sample. . If a plurality of containers are prepared, the sample introduction and discharge time seemingly disappears, and the press part becomes a form of pressing by replacing the container, increasing the number of presses. Combined with the production of multiple pieces with one press, it is possible to dramatically improve the productivity per unit time.

The present invention provides the following special effects.
(1) Bonding is performed by deformation of the resin surface based on the principle of nanoimprinting without using resin welding, so there is no need to wait for welding, and in addition, rapid pressure reduction is possible and the processing time is extremely short.
(2) Carbon dioxide that has entered the resin has the property of acting as a so-called release agent that separates the resins when desorbing (discharging). It suppresses the action as a release agent.
(3) By using liquid carbon dioxide, the resin can be plasticized at a temperature near room temperature, and the plasticized resin can be adhered, so that a heating mechanism is unnecessary or a simple heating mechanism can be used.
(4) Since it is not necessary to liquefy all the carbon dioxide in the pressure vessel, the press force can be reduced and a large-scale device is not required.
(5) In the gas-liquid mixed state, only the ratio of the gas phase and the liquid phase changes due to the change in volume, and the pressure does not change much. Excellent controllability.
(6) In some embodiments, the resin product can be pressed in a continuous process without being cut to fit the pressure vessel.
(7) Since a plurality of layers of fibrous resin to be adhered can be adhered at once, the productivity is extremely high compared to the method of adhering one layer at a time.
(8) It is possible to re-adhere part or all of the adhered objects adhered by the method of the present invention.
(9) Metal fibers can be sandwiched between resin fibers for bonding.
(10) The productivity of the laminate (adhesive) can be dramatically improved by alternately laminating the separators between the objects to be adhered and simultaneously adhering them.

1 shows a conceptual diagram of an apparatus used in the method of Example 1. FIG. The result of bonding the nonwoven fabric for tea bags is shown. A laser microscope photograph of the result of adhering clean room cloths is shown. 1 shows a conceptual diagram of an apparatus used in the method of Example 2. FIG. The result of bonding the nonwoven fabric for tea bags is shown. 1 shows a conceptual diagram of an apparatus used in the method of Example 3. FIG. The results of bonding polyester cotton are shown. 4 shows a conceptual diagram of an apparatus used in the method of Example 4. FIG. The result of putting instant green tea (pseudo- drug ) into the non-woven fabric for tea bag and adhering it is shown. 1 shows a conceptual diagram of an apparatus used in the method of Example 5. FIG. The result of adhering a lens cleaner (polyester) to a tea bag nonwoven fabric is shown. 1 shows a conceptual diagram of an apparatus used in the method of Example 6. FIG. The result of adhering the conductive cloth is shown. 1 shows a conceptual diagram of an apparatus used in the method of Example 7. FIG. Results after carbon dioxide treatment are shown. Results are shown after soaking in water. 1 shows a conceptual diagram of an apparatus used in the method of Example 8. FIG. The result of bonding the nonwoven fabric for tea bags is shown. 1 shows the basic configuration of the device of the present invention; 1 shows an example of embodiment of the device of the invention. 1 shows an example of embodiment of the device of the invention. 1 shows an example of embodiment of the device of the invention. 1 shows an example of embodiment of the device of the invention. 128 sheets of PET non-woven fabric are adhered to each other to form a resin porous body (three pieces). The results of re-adhering the adhered objects (three resin porous bodies to which 128 sheets of PET nonwoven fabric were adhered) that were adhered by the method of the present invention are shown. A photograph of a copper mesh sandwiched between 32 sheets of PET nonwoven fabric is shown. The results are shown in which a copper mesh was sandwiched between 32 sheets of PET nonwoven fabric and adhered. 1 shows an example of embodiment of the device of the invention. A photograph of a stainless steel separator used to separate the object to be adhered from the object to be adhered (32 pieces of PET nonwoven fabric are adhered) is shown.

EXAMPLES Next, the present invention will be specifically described based on examples, but the present invention is not limited to the following examples.

Here, the operating conditions for pressing the resin in a plasticized state and discharging carbon dioxide will be described.
(1) Press pressure The press pressure is 2 MPa or more, preferably 5 MPa or more (6 MPa in all examples).
(2) Introduction pressure of carbon dioxide Regarding the introduction pressure of carbon dioxide, there is no limit on the introduction pressure of carbon dioxide if it liquefies in the gaseous state during the press because it becomes vapor pressure in the process of lowering the piston. critical temperature of carbon), it is necessary to adjust the introduction pressure so that the density of carbon dioxide with the piston lowered is 0.4 g/mL (approximately half the density of liquid carbon dioxide) or more. becomes. In Examples other than Example 2, the gas was introduced at a pressure close to the cylinder pressure at room temperature.

(3) Decompression As for decompression, it is desirable to decompress as quickly as possible in order to desorb (discharge) carbon dioxide and fix the shape. It is 10 MPa/10 sec or less, preferably 10 MPa/1 sec or less. In the examples other than Example 2, all are instantaneously opened to the atmosphere by ball valves. In addition, in the case of the method of injecting carbon dioxide during pressing by sandwiching between the piston and the base portion without using the pressure vessel of Example 2, the edge of the material to be treated is open to the atmosphere, and the carbon dioxide is immediately released when the injection is stopped. Carbon is released.
(4) Material to be treated In the present invention, since carbon dioxide must be desorbed (exhausted) in a pressed state, the material to be treated is a porous or cotton-like fiber with continuous pores. It must be a resin with a shape. If carbon dioxide remains in the resin, the resins will be separated from each other by the release action of carbon dioxide, making adhesion impossible.

Next, experiments conducted to examine the effectiveness of the method of the present invention are shown as examples. In the following examples, the apparatus of Figure 19 or an equivalent apparatus was used. A fibrous resin 1 was placed in a space composed of a base portion 2 and a pressure vessel 3 as a container portion, and fixed with hexagon socket head bolts 8 at the four corners. The pressure vessel 3 is sealed by the base portion 2, the piston 6, and the O-ring 7 to form a closed space. In this state, the fibrous resin 1 was set in a pressing device, and an adhesion test of the fibrous resin 1 was conducted.

In the figure, 4 indicates a carbon dioxide introduction valve, and 5 indicates a carbon dioxide discharge valve. SUS316 was used as the material for the base portion 2, the pressure vessel 3, and the piston 6.

Example 1
[Example of introducing gaseous carbon dioxide, liquefying it with a piston, and then lowering the piston to press a resin sheet (fibrous resin sheet)]
FIG. 1 shows a conceptual diagram of the apparatus used in the method of this embodiment. At room temperature, carbon dioxide corresponding to the vapor pressure of carbon dioxide (cylinder pressure: 6 MPa in this embodiment) is instantly introduced by opening the ball valve for introduction, and the piston is lowered to reduce the volume in the pressure vessel. Thus, carbon dioxide was liquefied, and a state was created in which the surface of the resin sheet was immersed in liquid carbon dioxide.

In this state, the surface of the resin sheet is impregnated with carbon dioxide to plasticize the surface. After that, the piston is further lowered to press the resin sheet. With the piston lowered, the ball valve on the right side is opened to release carbon dioxide. was expelled instantaneously, the piston was returned to its original position, and the adhesive was taken out. The processing time for the entire process is about 4 minutes. In addition, the treatment was performed at room temperature without providing a heating facility.

FIG. 2 shows the result of bonding 50 non-woven fabrics (polyester-polyethylene composite material) for tea bags (in the figure, the left side is before treatment, and the right side is after treatment).

Similarly, 24 non-woven fabrics for range filters (70% polyester, 30% acrylic composite), 50 non-woven fabrics for draining filters (polyester-pulp composite), 36 non-woven fabrics for wiping (90% acrylic, 10% PET composite), wiping Adhesion was also confirmed for 16 non-woven fabrics (composite material of 55% cellulose and 45% polyester) and 4 cloths for clean rooms (composite material of 70% polyester and 30% nylon). This bonding method can be used to bond any number of sheets, indicating its application to filters whose thickness can be freely controlled.
Note) Items without percentages are for materials that do not specify percentages. Clean room cloths are woven fabrics, not non-woven fabrics. Since the weight is adjusted to about 0.6 g, the number of sheets differs depending on the material.

FIG. 3 shows the result of observing with a KEYENCE VK-9500 laser microscope after carefully peeling off the central cloth after adhering 6 pieces of clean room cloth (composite material of 70% polyester and 30% nylon). No weld marks were observed, and dents in the resin fibers with clear contours due to meshing were observed.

Example 2
[Example in which liquid carbon dioxide is introduced from the lower center of the resin sheet and discharged from the end of the resin sheet exposed to the atmosphere]
FIG. 4 shows a conceptual diagram of the apparatus used in the method of this example. In this example, experiments were conducted without using a pressure vessel, but instead using a base portion with an open introduction port that allows carbon dioxide to be introduced from the center instead of a normal base portion. After stacking the fibrous resin sheets and setting them, lower the piston to press the resin sheets. In the pressed state, open the valve for carbon dioxide introduction and operate the pump to make it higher than the vapor pressure of carbon dioxide (cylinder pressure). Liquid carbon dioxide under pressure (8 MPa) was introduced from the bottom center of the resin sheet for 1 minute, and discharged from the end of the resin sheet opened to the atmosphere. In addition, the treatment was performed at room temperature without providing a heating facility.

Then, after stopping the pump and closing the valve, the piston was returned to its original position and the adhesive was removed.

FIG. 5 shows the result of bonding 50 nonwoven fabrics for tea bags (polyester-polyethylene composite material).

Example 3
[Introduce gaseous carbon dioxide, liquefy it with a piston, plasticize the cotton-like resin, lower the piston to press the cotton, open the ball valve for discharge, and instantaneously discharge carbon dioxide. example]
FIG. 6 shows a conceptual diagram of the apparatus used in the method of this example. After setting the cotton-like resin in the container, at room temperature, open the ball valve for introduction of carbon dioxide equivalent to the vapor pressure of carbon dioxide (cylinder pressure) and instantly introduce it, lower the piston, and enter the pressure container. By reducing the volume of the carbon dioxide, while liquefying the carbon dioxide, the piston is further lowered to press the cotton-like resin, and with the piston lowered, the ball valve for ejection on the right side is opened to instantly exhaust carbon dioxide. After that, the piston was returned to its original position and the adhesive was removed. The processing time for the entire process is about 4 minutes. In addition, the treatment was carried out at room temperature without providing a heating facility.

FIG. 7 shows the result of adhering 0.6 g of polyester cotton (in the figure, the left side is before treatment and the right side is after treatment).

Example 4
[Introducing gaseous carbon dioxide, lowering the piston to liquefy it, lowering the piston further to place the powder in the center of the sheet, and pressing using the base part with the center recessed Example in which only the peripheral portion is adhered]
FIG. 8 shows a conceptual diagram of the apparatus used in the method of this example. After stacking the resin sheets with the object to be enclosed in the center and setting, at room temperature, carbon dioxide is instantly introduced by opening the ball valve for introduction on the left side by the vapor pressure of carbon dioxide (cylinder pressure), and the piston While lowering and liquefying, the piston is further lowered to press the resin sheet, and with the piston lowered, the ball valve for discharging on the right side is opened to instantly discharge carbon dioxide, and then the piston is returned to its original position. to remove the adhesive. The processing time for the entire process is about 4 minutes. In addition, the treatment was carried out at room temperature without providing a heating facility.

FIG. 9 shows the results of attaching instant green tea as a pseudo-drug to non-woven fabric for tea bags (polyester-polyethylene composite material).

This result has two meanings: production of a porous body containing powder and production of a porous body in which only the peripheral portion is adhered, excluding the central portion. The success of the powder-encapsulating porous material indicates that it is possible to produce a drug-carrying porous material. It was shown that it is possible to produce a drug-carrying porous material with controlled sustained release. The control of sustained release is suggested to be applied to pharmaceuticals, agricultural chemicals, insect repellents, deodorants, fragrances, and the like.

Example 5
[Example of introducing gaseous carbon dioxide, liquefying it with a piston, and then lowering the piston further to press a different resin sheet]
FIG. 10 shows a conceptual diagram of the apparatus used in the method of this example. After stacking and setting porous-like fibrous resin sheets, gaseous carbon dioxide is instantly introduced by opening the ball valve for introduction on the left side by cylinder pressure, lowering the piston to liquefy, and lowering the piston further. After pressing the resin sheet with the piston lowered, the ball valve for discharge on the right side was opened to instantly discharge carbon dioxide, and then the piston was lifted to take out the adhesive. The processing time for the entire process is about 4 minutes. In addition, the treatment was carried out at room temperature without providing a heating facility.

FIG. 11 shows the result of adhering a lens cleaner (polyester) between 50 tea bag nonwoven fabrics (polyester-polyethylene composite material). The middle layer of adhesive in the figure is the lens cleaner TORAYSEE (fabric).

Since it is possible to bond dissimilar materials in layers, it has been shown to be applicable to, for example, filters with different porous shapes for each layer. By combining layers of sheets on which enzymes and catalysts are supported, the possibility of a catalyst support that advances sequential reactions by passing solutions was demonstrated.

Example 6
[Example of introducing gaseous carbon dioxide, liquefying it with a piston, and then lowering the piston further to press a conductive sheet on the intermediate layer]
FIG. 12 shows a conceptual diagram of the apparatus used in the method of this example. The conductive-coated polyester cloth was sandwiched between non-woven fabrics and pressed in the presence of carbon dioxide in the same manner as in Example 1 for adhesion. FIG. 13 shows the results. In the figure, the upper row is before treatment, and the lower row is after carbon dioxide treatment. By the above bonding operation, a laminated structure in which a conductive coated polyester cloth (conductive coated cloth) was sandwiched between nonwoven fabrics was realized, and it was found that it is possible to insert an electrode (conductive layer) in the laminated structure. rice field. As a result, it was shown that it can be applied to electronic devices such as capacitors, batteries, and sensors.

Example 7
[Example of introducing gaseous carbon dioxide, liquefying with a piston, and then lowering the piston further to press a resin sheet on which different kinds of powders are arranged side by side]
FIG. 14 shows a conceptual diagram of the apparatus used in the method of this example. Instant green tea and black tea were placed side by side in the center of the non-woven fabric and pressed in the same manner as in Example 1 in the presence of carbon dioxide. The resulting adhesive is shown in FIG. As shown in FIG. 15, the treated adhesive appeared pure white, and shadows of the inclusions were visible when held up to light. When this was immersed in water, green tea and black tea oozed out and a pattern of green tea and black tea appeared (Fig. 16). This indicates that it can be used as a food or toy that shows a picture when placed in water, or as a poultice that can be mixed by soaking it in water before use.

Example 8
[Example showing that treatment is possible with carbon dioxide in a state close to liquid at a state higher than the critical temperature]
FIG. 17 shows a conceptual diagram of the apparatus used in the method of this example. After setting the resin sheet in the pressure vessel connected to the base, lower the piston to the carbon dioxide introduction position, insert the cartridge heater from the cartridge heater insertion port provided between the hexagonal socket bolts of the pressure vessel, and open the pressure vessel. was heated to a temperature of 35°C. After the thermometer attached to the treatment container indicated 35° C. and the treatment container was left for 30 minutes, gaseous carbon dioxide was introduced from a cylinder placed in a room temperature environment in a state close to the cylinder pressure in the same manner as in Example 1. and pressed in the presence of carbon dioxide. At this time, since the temperature of the press environment is higher than the critical temperature of carbon dioxide, only compression occurs without liquefaction. In addition, the pressure of carbon dioxide at the time of pressing is estimated to be about 8.5 MPa from the load applied to the piston, and the density of carbon dioxide is calculated to be about 0.6 g/mL from the temperature (35 ° C) and pressure. Carbon dioxide in a similar state.

FIG. 18 shows the result of bonding 50 nonwoven fabrics for tea bags (polyester-polyethylene composite material). Adhesion was performed in the same manner as in Example 1, and it was shown that adhesion is possible even with carbon dioxide in a nearly liquid state.

Example 9
[Example of further re-adhering the adhered objects adhered by the method of the present invention]
By the same method as in Example 1, 128 sheets of the PET nonwoven fabric shown in FIG. Then, by the same method as in Example 1, re-bonding of the resin porous bodies (three pieces) was attempted. FIG. 25 shows the results.
As a result, it was confirmed that the adherend adhered by the method of the present invention can be re-adhered. By further re-adhering the resin porous body, the strength of the adherend is further increased. Therefore, the method of re-adhering the adherend is very useful for applications where the strength of the adherend is required. In the present invention, one or both of the objects to be adhered, or a part or all of them, are made into a resin porous body adhered by the method of the present invention, thereby designing an appropriate product in which any part of the adherend is reinforced. It is possible to build
Further, when producing a resin porous body carrying powder, the mesh of the fiber sheet alone is too coarse to hold the powder on the fiber sheet before bonding. Even if it falls off, the method of re-adhesion is effective. The powder can be retained at the time of adhesion by adhering the fiber sheet in advance, making the mesh finer, and then putting the powder on it.

Example 10
[Example of adhesion in which metal fiber is sandwiched between adhesives]
By the same method as in Example 6, adhesion was attempted by sandwiching metal fibers between the adhesives. FIG. 26 shows a photograph of a copper mesh sandwiched between 32 pieces of PET nonwoven fabric. FIG. 27 shows the results of the adhesion operation by sandwiching the copper mesh between the adherends and pressing in the presence of carbon dioxide by the same method as in Example 6. It was found that by the above bonding operation, a laminated structure in which a copper mesh is sandwiched between non-woven fabrics can be realized, and an electrode (conductive layer) can be introduced into the laminated structure. This indicates that the technique of the present invention can be applied to electronic devices such as capacitors, batteries, and sensors. It was shown that the present invention can provide a laminated structure in which fibers made of a material that is not plasticized by carbon dioxide, such as metal, are sandwiched between fibrous resins.

Example 11
[Method for Bonding Objects for Improving Productivity of Bonded Objects by Simultaneous Bonding, and Example of Manufacturing Apparatus Provided with Carbon Dioxide Introduction/Exhaust Unit on Piston Side]
FIG. 28 shows a conceptual diagram of the apparatus used in the method of this example. Thirty-two sheets of PET nonwoven fabric and 1 mm-thick stainless steel separators were alternately stacked and simultaneously adhered. In addition, by providing a carbon dioxide introduction and discharge part on the piston side, the container can be easily removed.
That is, the material was set in a container at another location, set under a piston to which a pipe was connected, pressed, and then the container was moved to another location to take out the sample. If a plurality of containers are prepared, the introduction and discharge time of the sample is seemingly eliminated, and the press part is replaced with another container and pressed, increasing the number of times of pressing. However, according to this example, it was found that a plurality of adhesives can be produced by one press, and the productivity per unit time can be dramatically improved. FIG. 29 shows a photograph of the object after adhesion (32 pieces of PET nonwoven fabric are adhered) and the stainless steel separator used to separate the objects to be adhered.

As described in detail above, the present invention relates to a resin bonding method, an adhesive object, and a resin bonding apparatus. It is possible to use a device that does not require a temperature adjustment function or that has a simple temperature adjustment function. Moreover, in the present invention, since it is not necessary to liquefy all the carbon dioxide in the pressure vessel, the pressing force can be reduced and a large-scale apparatus is not required. Further, in some embodiments, the present invention allows the resin article to be fitted and bonded to the pressure vessel without being cut. It is a safe and secure bonding method that does not require high temperatures and uses only carbon dioxide, which is a food additive, so it can be applied to adhesive products such as inclusions of foods and pharmaceuticals, and enzymes and catalysts.

1 fibrous resin 2 base portion 3 pressure vessel 4 carbon dioxide introduction valve 5 carbon dioxide discharge valve 6 piston 7 O-ring 8 hexagon socket head bolt

Claims (19)

A method for bonding fibrous resin,
A step of plasticizing the surface of the fibrous resin by impregnating the resin with carbon dioxide in a liquid or a gas-liquid mixed state or a state close to the liquid, and pressing the resin surface in a plasticized state. a step of deforming the resin surface so that it meshes with each other; and a step of fixing the shape and bonding the resin in the meshed state by discharging carbon dioxide in the pressed state. Method. Liquid or gaseous carbon dioxide is introduced into a sealed container, and in gas introduction, the gaseous carbon dioxide is liquefied by reducing the volume of the sealed container with a piston, and carbon dioxide in a liquid, gas-liquid mixed state, or a state close to liquid is brought into contact with the resin to impregnate the resin with carbon dioxide to plasticize the surface of the fibrous resin, and by lowering the piston as it is, the plasticized resin is pressed and deformed so that the resin surface meshes. 2. The method of claim 1, performing the steps of: In a state where fibrous resin is pressed, carbon dioxide in a liquid, gas-liquid mixed state, or near-liquid state is made to flow through the resin to plasticize the surface of the fibrous resin so that it adapts to the pressed state. 2. The method of claim 1, wherein the surfaces of the resin in the folded state are deformed to engage. The method according to any one of claims 1 to 3, wherein the fibrous resin is a thermoplastic resin. The method according to any one of claims 1 to 3, wherein the fibrous resin is a composite material containing a thermoplastic resin. The method according to any one of claims 1 to 5, wherein the fibrous resin is a porous resin sheet. The method according to any one of claims 1 to 5, wherein the fibrous resin is a flocculent resin. As a fibrous resin, one kind selected from foodstuffs, medicines (medicine, agriculture, industry), pigments, adsorbents, deodorants, fragrances, insect repellents, electronic device materials, enzymes or catalysts is carried between them. The method according to any one of claims 1 to 7, wherein a resin is used. The method according to any one of claims 1 to 8, wherein a plurality of resins with different properties are used as fibrous resins. A method of carrying out a plurality of adhesion treatments at the same time by performing the adhesion method according to any one of claims 1 to 9 with one or more separators interposed therebetween. Adhesives having a structure in which fibrous resins are bonded or bonded in a single layer or multiple layers, and the surface of the fibrous resin is not melted, and the carbon dioxide in a liquid, gas-liquid mixed state, or near-liquid state An adherent whose shape is fixed and adhered in a plasticized state and in a state where the resin surface is deformed so as to mesh with each other. An apparatus used in the resin bonding method according to any one of claims 1, 2, and 4 to 10,
Consists of a base portion and a container portion,
The base portion can hold a fibrous resin that is a material to be treated,
The container portion has an opening into which the resin held by the base portion is inserted, and the opening portion can be brought into close contact with the base portion. having a piston as a means for liquefying carbon dioxide by maintaining or reducing the volume of said enclosed space, the piston being an introduction of liquid or gaseous carbon dioxide into said enclosed space, and It has a carbon discharge part and has the ability to press fibrous resin,
a step of disposing the resin in the space formed by the base portion and the container portion;
immersing the surface of the resin in liquid carbon dioxide to plasticize it;
a step of pressing the plasticized resin;
a step of releasing carbon dioxide;
The apparatus is characterized in that by performing these series of steps, the shape of the fibrous resin is fixed in a meshed state and adhered. 13. The apparatus according to claim 12, wherein unevenness is provided on the surface of the base portion or the piston to change the press strength of the in-plane fibrous resin, thereby enabling partial adhesion. The adhesive according to claim 11, wherein the fibrous resin is a thermoplastic resin.. The adhesive according to claim 11, wherein the fibrous resin is a composite material containing a thermoplastic resin. The adhesive according to any one of claims 11 and 14 to 15, wherein the fibrous resin is a porous resin sheet . The adhesive according to any one of claims 11, 14 to 15 , wherein the fibrous resin is a cotton-like resin . The fibrous resin carried between them a kind selected from foodstuffs, drugs (medicine, agriculture, industry), pigments, adsorbents, deodorants, fragrances, insect repellents, electronic device materials, enzymes or catalysts. The adhesive according to any one of claims 11 and 14 to 17 , which is a resin. The adhesive according to any one of claims 11, 14 to 18 , wherein the fibrous resin is a plurality of resins with different properties .

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