JP5084614B2 - Micro chemical plant and manufacturing method thereof - Google Patents

Description

  The present invention relates to a microchemical plant constituted by microchannels which are minute passages and a method for producing the same.

  The target microchemical plant uses a millimeter-sized to micron-sized passage formed on a substrate or a space portion that forms the passage. For example, a passage such as a reactor has a large surface area per volume of a reaction solution. It is excellent in diffusibility of reaction heat generated in the inside and temperature control when cooling from the outside, and in a minute passage, molecular dispersion is large, and uniform mixing can be easily realized in a short time. These characteristics are useful, for example, as a microreaction apparatus such as chemistry and biochemistry, a microanalysis apparatus, a microelectrophoresis apparatus, etc.

  By the way, as the substrate, resin is used together with glass, metal and ceramic. As a manufacturing method, for example, there is a configuration in which a passage space is formed in one base material and the space is closed by joining the other substrate to the one substrate. In addition, as a resin configuration example, Patent Document 1 discloses, as a microchemical plant particularly excellent in chemical resistance, a first fluororesin layer made of an amorphous fluororesin and an amorphous fluororesin bonded thereto. The structure provided with the channel | path which consists of the space part (concave part) formed in the joint surface side of the 2nd fluororesin layer which becomes and the 2nd fluororesin layer of the 1st fluororesin layer is disclosed. As the manufacturing method, a step of forming the first fluororesin layer on a first substrate such as glass, a step of forming a passage made of a space (concave portion) in the first fluororesin layer, At least a step of forming the second fluororesin layer on the substrate and a step of joining the surface of the first fluororesin layer and the surface of the second fluororesin layer are performed.

On the other hand, in Patent Document 2, when both base materials are joined with a liquid adhesive, the coating thickness may be uneven or it is difficult to remove the solvent. The manufacturing method which closes the space part (groove part) provided in the surface facing the other base material of one base material by using and bonding is formed is disclosed. Here, the material of the base material is arbitrary.
JP 2005-279493 A JP 2007-136292 A

  In the manufacturing method of Patent Document 1, it is described that the passage space (concave portion) can be formed by selective etching, dry etching, and a method in which a convex mold is engraved in a heated state. However, in the etching or engraving method, it is difficult to form the passage space (concave portion) in a micron size with a uniform width and depth with high accuracy, and lack in mass productivity. In the manufacturing method of Patent Document 2, it is described that the passage space (groove) can be formed by micromachining or etching, but there is a problem similar to that of Patent Document 1.

  From the background described above, the present inventors have repeatedly studied the material selection of the base material and the passage formation method. As a result, the resin is used as the base material and the passage formation method is devised so that it can be easily formed with high accuracy. It was discovered that it was possible to arrive at the present invention. That is, the object of the present invention is, as a microchemical plant and a manufacturing method thereof, particularly excellent in chemical resistance, and a functional passage having a catalyst attached to a part of the passage is highly accurate, easy to manufacture, and excellent in mass productivity. There is to provide a configuration.

  In order to achieve the above object, the present invention of claim 1 uses a resin powder as the substrate in the method of manufacturing a microchemical plant having a flow path provided in a substrate excellent in chemical resistance. A preforming step of compressing the resin powder in a state where the core for forming the flow path is disposed in the resin powder, and a sintered body obtained by the preforming step is fired, and the core is fired from the obtained sintered body. It is characterized by being subjected to a sintering / core removal step in which the passage is formed by being decomposed and removed by the heat of time. In the above invention, “the core is decomposed and removed by heat during firing” includes a configuration in which the core is decomposed / vaporized / incinerated by heat and a core is melted and removed by heat. .

  Further, the present invention of claim 2 is a method of manufacturing a microchemical plant having a flow path provided in a base material having excellent chemical resistance, wherein resin powder is used as the base material. From a preforming step of compressing the flow path forming core in a state of being disposed, a sintering step of firing the compressed body obtained in the preforming step, and a sintered body obtained in the sintering step A core removing step of chemically melting the core to form the passage is characterized.

  In the first aspect of the invention, as a base material resin, for example, as a microchemical plant such as various reactors and analyzers having excellent chemical resistance, heat resistance, and weather resistance by simply selecting a fluororesin powder such as PTFE. In addition, the core can be molded at a low temperature in the sintering process, and the core inserted into the compressed body can be decomposed and removed by heat during firing, so that the passage can be efficiently formed simultaneously with the formation of the sintered body. For this reason, the production method of the present invention is excellent in mass productivity and is not easily restricted by the shape of the passage, thereby contributing to the expansion of the application field of the microchemical plant.

  In the invention of claim 2, as in the case of claim 1, various reaction devices and analyzers excellent in chemical resistance, heat resistance and weather resistance can be obtained simply by selecting a fluororesin powder such as PTFE as the base resin. In addition, the compact can be sintered into a sintered body at a low temperature in the sintering process, and the core inserted into the sintered body can be chemically melted to efficiently form a passage. . For this reason, the manufacturing method of the present invention is excellent in mass productivity and is not easily restricted by the shape of the passage, thereby contributing to the expansion of the application field of the microchemical plant.

  In invention of Claim 3, it is a microchemical plant made by the manufacturing method of Claim 1 or 2 as a microchemical plant which has the flow path provided in the base material excellent in chemical resistance. Therefore, what has the advantage of Claim 1 or 2 mentioned above can be provided.

  Hereinafter, a first embodiment corresponding to claim 1, a second embodiment corresponding to claim 2, and a third embodiment corresponding to claim 3 will be described as a microchemical plant and a manufacturing method thereof according to the present invention. In this description, after describing the base material common to each form, the main part of the 1st form, the 2nd form, and the 3rd form is explained in full detail.

(Substrate) The substrate used in the manufacturing method of each embodiment may be a chemical-resistant resin powder satisfying characteristics or performance according to the purpose of use. For example, it is a fluororesin, and commercially available products include PTFE (tetrafluoroethylene) resin, PFA (tetrafluoroethylene / perfluoroalkoxyethylene copolymer) resin, FEP (tetrafluoroethylene / hexafluoropropylene copolymer). ) Resin, ETFE (tetrafluoroethylene / ethylene copolymer) resin, PVDF (vinylidene fluoride) resin, PVF (vinyl fluoride) resin, CTFE (chlorotrifluoroethylene) resin, ECTFE (ethylene / chlorotrifluoroethylene) ) Resin and AF (amorphous fluoropolymer) resin. These are thermoplastic resins that are excellent in chemical resistance, heat resistance, weather resistance, wear resistance, and the like, and thus are suitable as base materials for microchemical plants. Further, such a resin powder may be mixed with a filler such as carbon fiber powder, preferably in the range of about 1 to 15% by weight.

(First Embodiment) The manufacturing method of FIG. 1 corresponds to claim 1 and requires a preforming step and a sintering step. First, in the pre-molding step, a compression molding die is used, and after the passage forming core 11 is disposed in the cavity of the die, the resin powder for base material is filled and then compression molding is performed. . Here, the mold is the same as that normally used for compression molding, and the mold body forms a powder charging part, and has an upper and lower punch that moves up and down with respect to the powder charging part. doing. The core 11 is a thin line or rod for forming a passage, but may be tubular. The outer diameter of such a wire or tube is set according to the intended passage, but is usually from millimeter to micron size. The material may be any material that can be decomposed and removed at the firing temperature in the next sintering step, such as wax, paper, and organic fiber.

  That is, in the case of the compressed body 1 of (a), for example, the lower punch is raised with respect to the powder charging portion of the die body, and the cavity corresponding to the compressed body 1 is defined by the powder charging portion and the upper end surface of the lower punch. Form. Next, after about half of the total amount of resin powder is charged into the cavity, the core 11 is placed on the charged resin powder, and the resin powder remains on the placed core 11. Input the amount.

  Then, from the above resin powder charged state, the upper punch is lowered and simultaneously the lower punch is raised to compress and compress the fluororesin powder. Thus, in the pre-forming, the double pressing method of the upper and lower punches is preferable. However, in principle, a one-push method in which the lower punch is fixed and pressed by the upper punch is also possible. Further, the pressure applied in the preforming is 15 to 50 MPa when the resin powder is a fluororesin (PTFE resin) powder alone, and the above filler is mixed into the fluororesin (PTFE resin) powder from various tests. In some cases, about 40 to 150 MPa is preferable.

(Sintering step) In this step, the compact 1 obtained in the pre-forming step is put in a heating furnace and heated to a temperature slightly higher than the melting point, and the powders are fused together in a core insertion state. The heating furnace is preferably a hot air circulation type from the viewpoint of uniform firing. Although the firing temperature varies depending on the resin used, for example, in the case of a fluororesin, it is 400 ° C. or lower, preferably 360 to 380 ° C.

  In the sintering process, when the compressed body 1 is heated to the firing temperature, it is molded into a sintered body 1A that is baked by mutual diffusion of molecules, and the inserted core 11 is decomposed by heat during firing. Removed. That is, in this configuration, a material that is decomposed at the firing temperature is used as the core 11, and the passage 11a is formed by being decomposed and removed from the sintered body 1A from which the core itself can be obtained. This deforms the passage 11a by the core transfer method, and a complicated shape or a three-dimensional flow passage can be easily formed as the flow passage. Of course, the sintered body 1A is treated by air cooling at room temperature as a cooling after firing.

  The microchemical plant 10 in FIG. 1C is an example in which connecting pipes 6 are connected to both ends of each passage 11a formed in the sintered body 1A in FIG. Therefore, in the case of the microchemical plant 10, for example, a fluid such as a test solution can be introduced into the passage 11 a from the one side connecting pipe 6 and discharged from the other side connecting pipe 6. As a modification, for example, the shape of the core 11 is set three-dimensionally to form a more complicated passage, or each passage is connected via one side connection pipe 6 or a similar communication pipe. It is to lengthen the full length of the passage. In addition, in the microchemical plant 10 composed of the unit sintered body 1A, for example, a fluid reservoir, a merging portion, a branching portion, and the like can be provided at an appropriate location of the sintered body 1A together with the passage.

(Second Embodiment) The manufacturing method of FIG. 2 corresponds to claim 2 and includes a preforming step, a sintering step, and a core removing step. Among these, the preforming process is almost the same as the first embodiment except for the core. That is, in this step, a compression molding die is used, the core 12 is placed in the cavity of the die, the resin powder for base material is filled, and then compression molding is performed. Here, the mold is the same as that normally used for compression molding, and the mold body forms a powder charging part, and has an upper and lower punch that moves up and down with respect to the powder charging part. doing. The shape of the core 12 is a thin line or rod for forming a passage, but it may be tubular, and a Y-shape is shown, but it is designed according to the desired shape of the passage. The material does not change its shape at the firing temperature in the next sintering step and is chemically dissolved, and is preferably glass or resin.

  In the case of the compressed body corresponding to the sintered body 2A of (a), for example, the lower punch is raised with respect to the powder charging portion of the die body, and the compressed body 1 is formed by the powder charging portion and the upper end surface of the lower punch. A cavity corresponding to is defined. Next, after about half of the total amount of resin powder is charged into the cavity, the core 12 is positioned and arranged on the charged resin powder, and the resin powder is placed on the arranged core 12. Fill the remaining amount.

  From the charged state of the resin powder, the upper punch is lowered and simultaneously the lower punch is raised to compress and compress the fluororesin powder. Thus, in the pre-forming, the double pressing method of the upper and lower punches is preferable. In addition, the pressure applied in the preforming is the same as in the first embodiment. For example, when the resin powder is a fluororesin (PTFE resin) powder alone, 15-50 MPa, and the filler described above is used for the fluororesin (PTFE resin) powder. When mixed, about 40 to 150 MPa is preferable.

(Sintering process) In this process, a hot-air circulating heating furnace is used, and the compact obtained in the preforming process is put into the heating furnace and heated to a temperature slightly higher than the melting point, and the powder is inserted into the core. We fuse together. In this case as well, although the firing temperature varies depending on the resin used, for example, in the case of a fluororesin, it is 400 ° C. or lower, preferably 360 to 380 ° C. In addition, the sintered body 2A obtained is treated by air cooling at room temperature as cooling after firing.

(Core Removal Step) In this step, for example, the inserted core 12 is removed by being chemically dissolved by immersing the sintered body 2A of FIG. The That is, in this configuration, the core 12 is made of an acid or alkali-soluble glass, and the core itself is removed by being dissolved in a solution while being inserted in the sintered body 2A. In particular, it is preferable to use a fluororesin having excellent chemical resistance. This advantage is that a passage formed in the trace of the core 12 is not deformed, and a complicated shape of the flow path and a three-dimensional flow path can be easily formed.

  The microchemical plant 20 in FIG. 2 (c) has a connecting pipe 6 attached to each passage end of the sintered body 2A in FIG. 2 (b). That is, in this configuration feature, the connecting pipe 6 is connected to both ends of each passage 12a formed in the sintered body 2A of FIG. Therefore, in the case of the microchemical plant 20, for example, a fluid such as a test solution can be introduced into each passage 12 a from the one side connection pipe 6 and the connection pipe 6 and discharged from the other side connection pipe 6. As this modification, for example, the shape of the core for forming the passage is set three-dimensionally to form a more complicated passage, or a plurality of passages are formed, or each passage is connected to the connecting pipe 6 or similar. It is connected through a communication pipe to form the full length of the passage. Furthermore, the above-described passage is to make a functional passage by inserting a catalyst or the like into an appropriate portion of the passage using a core that is removed during heat or chemically during sintering. In addition, in the microchemical plant 20 composed of the unit sintered body 2A, for example, a fluid reservoir, a merging portion, a branching portion, and the like can be provided at an appropriate location of the sintered body 2A together with the passage.

(Third Embodiment) The microchemical plant 30 in FIG. 3B shows an example in which a plurality of sintered bodies having a passage formed by the above manufacturing method are stacked. The microchemical plant 30 in the figure includes a sintered body 5A having a passage 15a similar to the first embodiment, a sintered body 4A having a passage 14a similar to the second embodiment, and the same passage 13a as the sintered body 5A. In a state where the sintered bodies 3A are stacked in this order, the passage ends on the same side of the sintered bodies 3A and 5A are connected by the connecting pipe 9, and the connecting pipe 6 is attached to the other passage ends. A first passage which is on both sides and connects each passage 13a of the sintered bodies 3A and 5A with the connecting pipe 9, and a second passage which connects each other passage 13a of the sintered bodies 3A and 5A with the connecting pipe 9; And a third passage formed of a Y-shaped passage 14a provided between the first passage and the second passage.

  That is, the above structural features are the microchannels by laminating a large number of sintered bodies 3A to 5A having passages created in the first form and the second form as shown in FIG. The first passages are formed as third passages, and the sintered bodies 3A to 5A are integrated with a simple fastening member such as a plurality of bolts 7C and nuts 6 or an adhesive (not shown). The connection pipe 9 communicates the passages of the same or different sintered bodies. Of course, the configuration of FIG. 3 is an example of a plurality of stacked layers. As for the passage design, not only the passage is formed between the opposing side surfaces of the sintered body, but, for example, in the case of a rectangular sintered body, the entrance of the passage is one side on the left and right, one side on the front and back, both sides on the left and right It can be arranged according to the purpose, such as the front and back side surfaces. For this reason, in the above configuration, the sintered body having the passage obtained in the sintering / core removal step of the first form and / or the sintering having the passage obtained in the core removal step of the second form. By stacking a plurality of unit sintered bodies using the body as a unit, for example, a three-dimensional flow path can be easily formed and expansion of the application field can be expected.

  As described above, the present invention only has to substantially include the configuration specified in the claims, and details can be further changed with reference to each embodiment.

(A) shows the compressed body obtained in the pre-compression process of the manufacturing method of the first embodiment, (b) shows a sintered body that has been fired, and (c) shows a microchemical plant using the sintered body. Is shown. (A) shows the sintered body obtained in the sintering step of the manufacturing method of the second embodiment, (b) shows the sintered body after the core has been chemically removed, and (c) shows the sintered body. A microchemical plant using a ligation is shown. (A) shows the some sintered compact produced by the manufacturing method of the 1st form and the 2nd form, (b) has shown the microchemical plant which laminated | stacked the some sintered compact.

Explanation of symbols

DESCRIPTION OF SYMBOLS 1 ... Compressed body 1A-5A ... Sintered body 6, 9 ... Connection pipe 7 ... Bolt (fastening member)
8 ... Nut (fastening member)
DESCRIPTION OF SYMBOLS 11, 12 ... Core 11a, 12a, 13a, 14a, 15b ... Passage 10, 20, 30 ... Micro chemical plant

Claims (3)

In a manufacturing method of a microchemical plant having a channel provided in a base material excellent in chemical resistance,
Using a resin powder as the base material, a preforming step of compressing the resin powder in a state where the flow path forming core is disposed;
The sintered compact obtained by the preforming step is fired, and the core is decomposed and removed from the obtained sintered body by heat during firing to form the passage and the core removing step. A manufacturing method of a microchemical plant characterized by the above. In a manufacturing method of a microchemical plant having a channel provided in a base material excellent in chemical resistance,
Using a resin powder as the base material, a preforming step of compressing the resin powder in a state where the flow path forming core is disposed;
A sintering step of firing the compact obtained in the preforming step;
A microchemical plant manufacturing method comprising: a core removing step of chemically melting the core from the sintered body obtained in the sintering step to form the passage.   A microchemical plant having a flow path provided in a base material excellent in chemical resistance, wherein the microchemical plant is produced by the manufacturing method according to claim 1.

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