JP4720679B2 - Separation and recovery method of thermosetting resin - Google Patents

Description

  The present invention relates to a thermosetting resin separation and recovery method for decomposing a thermosetting resin, particularly plastic waste containing a thermosetting resin, and separating and recovering the decomposition product.

Conventionally, most plastic waste has been landfilled or incinerated, and has not been effectively used. However, in recent years, it has become mandatory to collect and reuse plastic waste. Therefore, as one of the attempts to recycle plastic waste, a method has been proposed in which plastic waste is decomposed into oil by a reaction using supercritical water as a reaction medium to recover useful materials. For fiber reinforced plastics, a method has been proposed in which plastic components are decomposed using supercritical water or subcritical water, and fibers such as glass fibers and carbon fibers are recovered and reused (see Patent Document 1). . In this method, since plastic becomes an oily component having a low molecular weight due to decomposition, this is mainly reused as a liquid fuel. In addition, a method for decomposing plastics utilizing a hydrolysis reaction with high-temperature steam has been proposed. According to this method, plastics can be decomposed once.
Japanese Patent Laid-Open No. 10-87872

  However, according to the conventional plastic decomposition method, the decomposition temperature of the plastic is high, and fibers such as glass fiber and carbon fiber can be recovered and reused. Becomes an oily substance composed of various components, and it is difficult to obtain a degradation product of constant quality.

  The present invention has been made to solve the above-mentioned problems, and its purpose is to recover glass fiber in a form that can be reused as glass and to recover a resin decomposition product that has become a monomer or oligomer in a high yield. Another object of the present invention is to provide a method for separating and recovering a thermosetting resin.

The feature of the method for separating and recovering a thermosetting resin according to the present invention is that a glass fiber and a resin obtained by decomposing a thermosetting resin containing glass fibers in a reaction tank using a supercritical fluid or a subcritical fluid. A method for separating and recovering a thermosetting resin for separating and recovering a decomposed product, wherein each of the reaction tanks is formed by a mesh part formed so as to allow fluid to pass but not glass fiber to pass through the reaction tank. to include a lower surface, bisected into an inner region and an outer region, a thermosetting resin accommodated in the inner region, and the step of decomposing a thermosetting resin by using a supercritical fluid or subcritical fluid, the outer region extraction fluid from the discharge valve provided on the lower surface of the anti応漕, by taking out the glass fibers from a discharge valve provided in a counter応漕lower surface of the inner region, and a step of taking out the glass fibers contained in the container from the fluid It is to.

  According to the method for separating and recovering a thermosetting resin according to the present invention, glass fibers can be recovered in a form that can be reused as glass. Moreover, according to the method for separating and recovering a thermosetting resin according to the present invention, a resin decomposition product that has become a monomer or an oligomer is recovered in a high yield, and used as a raw material for a thermosetting resin, a low shrinkage agent, a dispersion material, Can be reused.

  Hereinafter, a method for separating and recovering a thermosetting resin according to an embodiment of the present invention will be described with reference to the drawings.

  In the method for separating and recovering a thermosetting resin according to an embodiment of the present invention, first, as shown in FIG. 1, a net portion 3 formed so as to allow fluid to pass but not glass fiber to pass is provided on the lower surface and side surface. A storage container 4 is attached to the reaction tank 2, and a thermosetting resin 5 containing glass fiber is stored in the storage container 4. At this time, the thermosetting resin 5 may be pulverized to such a size that the decomposed glass fiber can be accommodated in the storage container 4, but there is a risk of damaging the properties of the glass fiber. It is desirable to store in the storage container 4 as it is or cut into a size that fits in the storage container 4.

  Next, after the water 6 is allowed to flow into the reaction tank 2, the lid 7 is attached to the upper part of the reaction tank 2 so that the reaction tank 2 is sealed. At this time, the mixing ratio of the thermosetting resin 5 and the water 6 is not particularly limited, but the amount of water added is in the range of 200 to 500 parts by mass with respect to 100 parts by mass of the thermosetting resin. It is desirable. Further, the amount of alkali added to the water 6 in order to promote the hydrolysis treatment of the thermosetting resin 5 is not particularly limited, but 50 to 50 parts by mass with respect to 100 parts by mass of the resin component of the thermosetting resin 5. It is desirable to be in the range of 100 parts by mass.

  Next, the thermosetting resin 5 is hydrolyzed by heating the reaction tank 2 to a temperature not higher than the thermal decomposition temperature of the thermosetting resin 5. At this time, it is desirable to set the heating temperature within a range of 180 to 270 [° C.]. When the heating temperature is less than 180 [° C.], it takes a lot of time for the thermosetting resin 5 to hydrolyze due to the temperature-dependent influence being larger than the effect of hydrolysis by alkali. The decomposition product cannot be recovered with high yield. On the other hand, when the heating temperature is 270 [° C.] or higher, the thermosetting resin 5 is randomly decomposed due to the effect of thermal decomposition, and the thermosetting resin 5 is again subjected to similar thermosetting. It may be difficult to reuse as a raw material for a conductive resin, a low shrinkage agent, and a dispersant. The heating time varies depending on conditions such as the reaction temperature, and is preferably about 1 to 4 hours below the temperature at which the influence of thermal decomposition does not occur. However, the shorter heating time is more preferable because the processing cost can be reduced. . Specifically, when the heating temperature is 230 [° C.], the heating time is 2 hours, and the blending ratio of the thermosetting resin 5 and water 6 is 1: 4, the decomposition product is recovered with the highest yield, and the thermosetting property is obtained. The resin 5 can be reused again as the same thermosetting resin raw material, low shrinkage agent, and dispersant.

  Next, after completion of the hydrolysis treatment, the reaction tank 2 is cooled to room temperature, and the storage container 4 is taken out from the reaction tank 2. At this time, since the net 3 is formed on the lower and side surfaces of the storage container 4 so as to allow fluid to pass but not glass fiber, heat in the reaction tank 2 is dissolved in subcritical water. The decomposition liquid 9 containing a curable resin remains, and only the glass fiber 8 can be recovered in the storage container 4. The decomposition solution 9 can be recovered by opening the drain valve 1 provided at the lower part of the reaction tank 2.

  In addition, when the thermosetting resin 5 contains an inorganic filler, when the net part 3 is formed to a size that allows the inorganic filler to pass through, the decomposition liquid 9 contains the inorganic filler, but the decomposition liquid 9 Since glass fiber 8 is not contained, the inorganic filler can be easily recovered by solid-liquid separation of the decomposition solution 9. Further, the decomposition solution 9 can be reused as a high-quality dispersant without performing solid-liquid separation. Moreover, the glass fiber 8 which remained in the storage container 4 can be collect | recovered with the shape before decomposition | disassembly, and can be reused as glass fiber or a glass molded product.

  Further, in the present embodiment, the mesh part 3 is formed so as to allow fluid to pass but not glass fiber, but as shown in FIG. 2, only the fluid is allowed to pass, and the glass fiber 8 and the inorganic filler 10 are allowed to pass. By forming the net portion 3 so as not to pass solid content such as the like, the decomposition solution 9 and the solid content may be recovered without performing solid-liquid separation. According to such a method, the glass fiber 8 and the inorganic filler 10 remaining in the storage container 4 can be easily separated and collected by a sieve after drying.

  Moreover, in this embodiment, although the glass fiber 8 was collect | recovered by removing the storage container 4 from the reaction tank 2 after completion | finish of a hydrolysis process, as shown in FIG. The glass bulb 8 is decomposed by disposing the discharge valve 11 and the discharge valve 1 at the lower part of each of the inner region and the outer region of the mesh part 3 and opening the discharge valve 11 and the discharge valve 1 after hydrolysis. The liquid 9 may be separated and recovered. Also in this case, as shown in FIG. 4, by forming the net portion 3 so that only the fluid is allowed to pass and not the solid content such as the glass fiber 8 and the inorganic filler 10 is allowed to pass, the discharge valve after the hydrolysis treatment. 11 and the discharge valve 1 may be opened to recover the solid content and the decomposition solution 9.

  As mentioned above, although the embodiment to which the invention made by the present inventors was applied has been described, the present invention is not limited by the description and the drawings that form part of the disclosure of the present invention according to this embodiment. That is, it should be added that other embodiments, examples, operation techniques, and the like made by those skilled in the art based on the above embodiments are all included in the scope of the present invention.

It is a schematic diagram for demonstrating the separation-and-recovery method of the thermosetting resin used as embodiment of this invention. It is a schematic diagram for demonstrating the application example of the separation-and-recovery method of the thermosetting resin shown in FIG. It is a schematic diagram for demonstrating the isolation | separation collection method of the thermosetting resin which becomes other embodiment of this invention. It is a schematic diagram for demonstrating the application example of the separation-and-recovery method of the thermosetting resin shown in FIG.

Explanation of symbols

1: drain valve 2: reaction tank 3: mesh part 4: storage container 5: thermosetting resin 6: water 7: lid 8: glass fiber 9: decomposition solution 10: inorganic filler

Claims (2)

Separation and recovery of thermosetting resin to separate and recover glass fiber and resin decomposition products obtained by decomposing thermosetting resin containing glass fiber in a reaction tank using supercritical fluid or subcritical fluid A method,
The inside of the reaction vessel is divided into an inner region and an outer region so as to include the lower surface of the reaction vessel, respectively, by a mesh portion formed so as to allow fluid to pass but not glass fiber. Containing the thermosetting resin;
Decomposing the thermosetting resin using a supercritical fluid or subcritical fluid;
The step of taking out the glass fiber from the fluid by taking out the fluid from the discharge valve provided on the lower surface of the reaction vessel in the outer region and taking out the glass fiber from the discharge valve provided on the lower surface of the reaction vessel in the inner region. A method for separating and recovering a thermosetting resin, comprising:   2. The method for separating and recovering a thermosetting resin according to claim 1, wherein the thermosetting resin contains an inorganic filler, and the mesh portion is formed so as not to pass the inorganic filler and the glass fiber. A method for separating and recovering a thermosetting resin.

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