JP2011005369A - Microtreatment apparatus - Google Patents

Abstract

PROBLEM TO BE SOLVED: To provide a microtreatment apparatus in which a component flowing into the direction orthogonal to the flow direction of a liquid to be treated is induced so that an inter-electrode voltage is made lower than before.SOLUTION: The microtreatment apparatus includes a flow path L2 for circulating the liquid Ma to be treated, and a cathode K and an anode P which are exposed in the flow path L2 and used for applying an electric field to the liquid Ma to be treated. An electric field application part includes an agitation part 7 comprising a plurality of grooves 7a or/and a plurality of projections.

Description

  The present invention relates to a micro processing apparatus.

The microchemical process realizes a chemical process in a small space by connecting micron-order process equipment (micro-processing apparatus) via a micron-order channel (micro-channel). One of the micro-processing apparatuses includes electrolysis in which a compound is electrochemically decomposed by applying a voltage to the compound, and electrolytic synthesis in which a substance is synthesized by applying a voltage.
In this specification, the apparatus for performing the electrolysis and the apparatus for performing the electrolytic synthesis are collectively referred to as a micro-processing apparatus.

  For example, the following Non-Patent Document 1 discloses a micro-process for synthesizing benzaldehyde by passing a toluene solution containing methanol and ethanol as a solvent between an anode (electrode) and a cathode (electrode) arranged opposite to each other. An apparatus is disclosed. Unlike the batch type micro-processing apparatus, this micro-processing apparatus is a continuous micro-processing apparatus that continuously synthesizes benzoylaldehyde by continuously flowing a toluene solution between electrodes.

H. Wendt et al., “Anodic Synthesis of Benzaldehydes-II. Optimization of the Direct Anodic Oxidation of Toluenes in Methanol and Ethanol”, Electrochimica Acta, Vol. 37, No. 11, pp1959-1969, 1992.

  By the way, as described above, the main feature of the micro processing apparatus is that the system is miniaturized. Therefore, the continuous processing apparatus is also required to be miniaturized. However, in a continuous micro-processing apparatus, when the distance between the anode and the cathode (distance between the electrodes) is reduced with the miniaturization of the apparatus, the flow of the liquid to be processed is laminarized, and the flow field is increased. It becomes a state occupied by the velocity component in the flow direction of the liquid to be treated. In such a flow field, mixing of the solute and the solvent in the liquid to be treated is difficult to occur, and as a result, there is a problem that the voltage between the electrodes increases. Since the micro processing apparatus generally pursues not only miniaturization of the apparatus but also labor saving of power consumption, an increase in power consumption due to an increase in inter-electrode voltage is an important technical problem to be solved.

The present invention has been made in view of the above-described circumstances, and has the following objects.
(1) Inducing a flow component in a direction orthogonal to the flow direction of the liquid to be treated.
(2) The voltage between the electrodes is lowered as compared with the conventional case.

  In order to achieve the above object, in the present invention, as a first solving means, a flow path through which the liquid to be processed flows, and an action part that is exposed in the flow path and performs a predetermined action on the liquid to be processed In the micro-processing apparatus comprising the above, a means is adopted in which the action section includes a stirring section comprising a plurality of grooves or / and a plurality of protrusions.

  As a second solving means, in the first solving means, a flow path is formed by laminating a plurality of functional layers subjected to predetermined processing, and an action part is provided in any functional layer. Adopt the means.

  As a third solving means, in the first or second solving means, the agitating section is composed of a plurality of grooves whose extending direction is inclined at a predetermined angle with respect to the extending direction of the flow path. adopt.

  As a fourth solving means, in any one of the first to third solving means, the action part is an anode and a cathode disposed in opposition to each other in the flow path, and stirring is performed on one or both of the anode and the cathode. Adopting the means that the part is provided.

  As the fifth solving means, a means is adopted in which the diaphragm for separating the anode and the cathode is provided in the fourth solving means.

  As a sixth solving means, in the first to third solving means, a means is adopted in which the action part is a catalyst supporting part.

  As a seventh solving means, in the first to third solving means, a means that the action part is a light emitting part is adopted.

  According to the present invention, since the stirrer is provided, it is possible to induce a flow component in a direction orthogonal to the flow direction of the liquid to be treated, and as a result, the voltage between the electrodes can be reduced as compared with the related art.

It is a disassembled perspective view which shows the whole structure of the micro processing apparatus A which concerns on one Embodiment of this invention. It is a XX arrow directional view in the lamination | stacking state of 1st-5th functional layer S1-S5 in the said FIG. In the micro-processing apparatus A which concerns on one Embodiment of this invention, it is an enlarged view which shows the detailed structure of the stirring part 7, and a modification. It is a figure which shows the performance of the micro processing apparatus A which concerns on one Embodiment of this invention, (a) is a yield characteristic (experimental result), (b) has shown the voltage characteristic (experimental result) between electrodes. It is the front view which shows the structural example of the micro processing apparatus B which concerns on the modification of this invention, and a YY arrow directional view.

Hereinafter, an embodiment of the present invention will be described with reference to the drawings.
As shown in FIG. 1, the micro-processing apparatus A according to this embodiment is configured by stacking first to fifth functional layers S1 to S5. In FIG. 1, the developed state before lamination is shown so that the state of mechanical processing applied to the first to fifth functional layers S1 to S5 can be easily understood. The first to fifth functional layers S1 to S5 are secretly bonded and integrated in the order shown in the figure to form two flow paths L1 and L2 as shown in FIG.

  That is, the first functional layer S1 is a thin plate in which a pair of through holes 1 and 2 are formed. The through holes 1 and 2 are round holes provided at a predetermined interval, and one through hole 1 corresponds to the inlet IN1 (first inlet) of the liquid to be treated in the first flow path L1, and the other through hole. 2 corresponds to the outlet OUT1 (first outlet) of the liquid to be processed in the first flow path L1. The first functional layer S1 is made of a conductive material (for example, metal) so as to function as the cathode K (electrode). The interval between the through holes 1 and 2 is 30 mm, for example.

  The second functional layer S2 is a thin plate in which a long through hole 3 having a length (for example, 30 mm) matching the interval between the through holes 1 and 2 is formed. The second functional layer S2 is made of a non-conductive material and has a thickness of 100 μm, for example. The width of the elongated through hole 3 is, for example, 1 mm. The third functional layer S3 is a diaphragm for electrochemically isolating the cathode K described above from an anode P (electrode) to be described later, more specifically, a cation permeable membrane that allows only cations to pass therethrough. is there.

  Here, as is apparent from FIG. 2, the first flow path L1 is formed by the first to third functional layers S1 to S3. That is, the first flow path L1 includes a circumferential surface of the elongated through hole 3 formed in the second functional layer S2 and a lower surface of the first functional layer S1 positioned above the elongated through hole 3. And an area where the cathode K is exposed, and is surrounded by three surfaces including the upper surface of the third functional layer S3 located below the elongated through hole 3.

  The through hole 1 formed at one end of the first functional layer S1 is for allowing the first processing target liquid Ha to flow into the first flow path L1. Further, the through hole 2 formed at the other end of the first functional layer S1 passes through the first flow path L1, and is obtained as a result of the predetermined processing being performed on the first processing target liquid Ha. The processed liquid Hb is discharged to the outside.

  The fourth functional layer S4 is a thin plate that is identical in shape to the second functional layer S2 described above, and is formed of a non-conductive material in the same manner as the second functional layer S2. That is, the fourth functional layer S4 has a thickness of, for example, 100 μm, and the long through hole 4 formed in the fourth functional layer S4 has a length of, for example, 30 mm and a width of, for example, 1 mm.

  The fifth functional layer S5 is a thin plate in which a pair of through-holes 5 and 6 (round holes) that are separated at a predetermined interval are formed, and a stirring portion 7 is formed between the through-holes 5 and 6. One through hole 5 corresponds to the inlet IN2 (second inlet) of the liquid to be processed in the second flow path L2, and the other through hole 6 has an outlet OUT2 (second outlet) of the liquid to be processed in the second flow path L2. It corresponds to. The interval between the through holes 5 and 6 is, for example, 30 mm, similar to the through holes 1 and 2 of the first functional layer S1 described above. The fifth functional layer S5 is formed of a conductive material (for example, metal) so as to function as the anode P (electrode).

  As is apparent from FIG. 2, the second flow path L2 is formed by the third to fifth functional layers S3 to S5. That is, the second flow path L2 includes the peripheral surface of the elongated through hole 4 formed in the fourth functional layer S4 and the lower surface of the third functional layer S3 located above the elongated through hole 4. And a region surrounded by three surfaces including the upper surface of the fifth functional layer S5 located on the lower side of the elongated through-hole 4 and the anode P is exposed. Such a second flow path L2 has exactly the same shape as the first flow path L1, and has a positional relationship facing the first flow path L1 across the third functional layer S3 (cation permeable membrane). It is in.

  The through hole 5 formed at one end of the fifth functional layer S5 is for allowing the second processing target liquid Ma to flow into the second flow path L2. Further, the through hole 6 formed at the other end of the fifth functional layer S5 passes through the second flow path L2, and is obtained as a result of the predetermined processing being performed on the second processing target liquid Ma. The second processed liquid Mb is discharged to the outside.

  The stirrer 7 is the most characteristic component in the present micro-processing apparatus A, and the direction from the through hole 5 (inlet IN2) to the through hole 6 (outlet OUT2) in the second flow path L2 (from the left in FIG. 2) This is for inducing a flow in the facing direction (vertical direction in FIG. 2) of the anode P and the cathode K with respect to the processing target liquid flowing in the right direction).

  As shown in the enlarged view of FIG. 3A, the stirring unit 7 includes a plurality of long grooves 7a formed at predetermined intervals. Each long groove 7a is a long recess having a predetermined length and a predetermined depth, and is inclined by a predetermined angle θ with respect to an axis (indicated by a one-dot chain line) connecting the centers of the through holes 5 and 6. The direction made is defined as the extending direction. Since the axis connecting the centers of the through holes 5 and 6 is the same as the extending direction of the second flow path L2, the extending direction of each long groove 7a is relative to the extending direction of the second flow path L2. Is inclined by an angle θ. In the present embodiment, the angle θ = 45 °.

  FIG. 3B to FIG. 3D show a modification of the stirring unit 7 as described above. The stirring unit 7A according to the first modification is composed of a plurality of long grooves 7b having an angle θ different from that of the long grooves 7a. The angle θ of each long groove 7b is, for example, −45 °. The stirring unit 7B according to the second modified example includes a plurality of long protrusions 7c instead of the long grooves 7a. Each long protrusion 7c has the same shape as each of the long grooves 7a described above, but is provided as a protrusion instead of a recess. The stirring unit 7C according to the third modification is a combination of the long groove 7a and the long protrusion 7c. That is, the stirring unit 7C is formed by alternately arranging the long grooves 7a and the long protrusions 7c.

  Here, the first functional layer S1 functioning as the cathode K (electrode) and the fifth functional layer S5 functioning as the anode P (electrode) are action units that act on the liquid to be treated as a pair. In other words, the present micro-processing apparatus A performs electrolytic synthesis by applying an electric field to the first and second processing target liquids Ha and Ma by the action part including the cathode K and the anode P.

  Next, the function and effect of the microprocessing apparatus A configured as described above will be described in detail with reference to FIG. 4 and Table 1 as well.

The first processing target liquid Ha in the present embodiment is obtained by dissolving tetraethylammonium tetrafluoroborate (Et ₄ NBF ₄ ) as an electrolytic solution in methanol (MeOH) as a solvent. The second treatment target liquid Ma is methanol (MeOH) as a solvent, tetraethylammonium tetrafluoroborate (Et ₄ NBF ₄ ) as an electrolyte, and 4-methoxytoluene (MeOC ₇ H ₈ ) as a medium. It has been dissolved. Note that the first processing target liquid Ha functions exclusively as an electrolytic solution, and is not directly involved in the production of the target product of the microprocessing apparatus A.

  Of the first processing target liquid Ha and the second processing target liquid Ma, the first processing target liquid Ha is adjacent to the cathode K through the third functional layer S3 (cation permeable membrane). Of the first flow path L1 and the second flow path L2 in which a predetermined DC electric field is applied by the anode P, the first flow path L1 flows into the first flow path L1 through the first inlet IN1. On the other hand, the second processing target liquid Ma is also adjacent to each other via the third functional layer S3 (cation permeable membrane), and the first flow path L1 in which a predetermined DC electric field is applied by the cathode K and the anode P. Of the second flow path L2, the second flow path L2 flows into the second flow path L2.

Of the first flow path L 1 and the second flow path L 2, the second flow path L 2 in which the second processing target liquid Ma containing 4-methoxytoluene (MeOC ₇ H ₈ ) circulates has the chemical formula (1). The reaction shown in FIG.

That is, 4-methoxytoluene (MeOC ₇ H ₈ ) reacts with methanol (MeOH) by the action of a direct current electric field to react with p-anisaldehyde dimethyl acetal (Me ₃ O ₃ C ₇ H ₅ ), hydrogen ions (H ⁺ ), Is generated. One product, p-anisaldehyde dimethyl acetal (Me ₃ O ₃ C ₇ H ₅ ), is a product of the present micro-processing apparatus A, and the second processed liquid is passed through the second outlet OUT2. It is discharged to the outside as a component of Mb. The other product, hydrogen ions (H ⁺ ), is a cation, passes through the third functional layer S3 (cation permeable membrane), moves to the first flow path L1, and further from the cathode K. The electrons are received to become hydrogen gas (H ₂ ), and are discharged to the outside as a component of the first treated liquid Hb through the first outlet OUT1.

In the reaction in the second flow path L2, in order to improve the yield of p-anisaldehyde dimethyl acetal (Me ₃ O ₃ C ₇ H ₅ ), a good dispersion state of the solute in the solvent, that is, 4-methoxytoluene ( The stirring state of MeOC ₇ H ₈ ) against methanol (MeOH) is important. In order to save power in the present micro processing apparatus A, it is necessary to reduce the voltage difference between the cathode K and the anode P, that is, the interelectrode voltage E. In order to reduce the interelectrode voltage E, the mobility of ions in the opposing direction (vertical direction in FIG. 2) of the cathode K and the anode P in the second flow path L2 is improved to improve the cathode K and the anode P. It is necessary to reduce the electrical resistance between them.

The stirring unit 7 in the present micro-processing apparatus A has an advantageous effect in reducing the reaction voltage E as shown by the following experimental results. That is, when a plurality of currents flowing between the cathode K and the anode P and the flow rate of the second treated liquid Mb are set as shown in Table 1, p-anisaldehyde dimethyl acetal (Me ₃ O ₃ C ₇ The yield of H ₅ ) was as shown in the graph of FIG. 4A, and the interelectrode voltage E (voltage) was the value shown in the graph of FIG. 4B. The relationship between the current and the flow velocity in Table 1 is set as a relationship in which the energization amount (electric amount) is chemically equivalent in the reaction of the chemical formula (1).

  In FIG. 4, the present micro-processing apparatus A (that is, the case where the stirring unit 7 is provided in the second flow path L2) is shown as a “mixer pattern”. In addition, FIG. 4 shows a case where the stirring unit 7 is not provided (no pattern) and a case where a plurality of grooves parallel to the flow path direction are provided (linear groove pattern) as comparative examples for the “mixer pattern”.

  As can be seen from FIG. 4A, the yields of the “mixer pattern” and the “linear groove pattern” are improved when the current (flow velocity) is increased as compared to “no pattern”. On the other hand, as can be seen from FIG. 4B, the voltage of the “mixer pattern” is lower than that of the “linear groove pattern” and “no pattern”. From such experimental results shown in FIG. 4, it is confirmed that the stirring unit 7 in the present micro-processing apparatus A has an advantageous effect on the voltage drop in comparison with the “linear groove pattern” and “no pattern”. It was.

  That is, according to the present micro-processing apparatus A, it is possible to induce a flow component in a direction orthogonal to the flow direction of the second processing target liquid Ma, that is, the facing direction of the cathode K and the anode P. As a result, As a result, the inter-electrode voltage E can be reduced as compared with the prior art.

In addition, this invention is not limited to the said embodiment, For example, the following modifications can be considered.
(1) In the above-described embodiment, the micro processing apparatus A that has a pair of electrodes composed of the cathode K and the anode P as the working portion has been described. However, the working portion is not limited to the pair of electrodes. As the action part other than the pair of electrodes, for example, a catalyst supporting part that catalyzes the treatment target liquid, a light emitting part that irradiates light of various wavelengths, and the like are conceivable.

  FIG. 5 shows a configuration example of a micro-processing apparatus B including an action unit that applies the catalytic action and the light irradiation to the liquid to be treated. As shown in this figure, the micro-processing apparatus B is configured by laminating three functional layers Sa to Sc, and is internally formed by an inlet IN, a flow path L, an outlet OUT, and three functional layers Sa to Sc. The space formed in (1) is provided with a flow path L, a stirring part 7 and an action part R (catalyst carrying part or light emitting part). The flow path L is an internal space formed by the three functional layers Sa to Sc. Of the three functional layers Sa to Sc, the surface functional layers Sa and Sc are action portions R (catalyst carrying portions or light emitting portions) for the liquid to be processed that passes through the flow path L. The liquid to be treated that has flowed into the flow path L from the inlet IN is subjected to catalyst treatment or light irradiation by the action part R when passing through the flow path L, and is discharged to the outside as a treated liquid from the outlet OUT.

  A stirrer 7 similar to that of the micro-processing apparatus A is provided in each of the functional layers Sa and Sc that form one surface of the flow path L. That is, in this micro-processing apparatus B, as shown in FIG. 5B, the agitation units 7 are respectively provided on the two surfaces (upper surface and lower surface) of the flow path L so as to face each other. The liquid to be treated that passes through the flow path L by the agitating unit 7 in such an opposed state can be effectively subjected to catalytic treatment by promoting vertical agitation, or effective over a wider range. Can be irradiated with light.

(2) In the above-described embodiment and modification, the agitation units 7 and 7A to 7C including the long grooves 7a and 7b or the long protrusions 7c shown in FIG. 3 are employed, but the present invention is not limited to this. Any shape may be used as long as it can induce a flow component in the opposite direction of the acting portion with respect to the treatment target liquid.

  A ... micro processing device, S1 ... first functional layer (action part), S2 ... second functional layer, S3 ... third functional layer, S4 ... fourth functional layer, S5 ... fifth functional layer ( Action part), L1 ... first flow path, L2 ... second flow path, IN1 ... first inlet, OUT1 ... first outlet, IN2 ... second inlet, OUT2 ... second outlet, 1 ... through hole, 2 ... through Holes, 3 ... elongate through holes, 4 ... elongate through holes, 5 ... through holes, 6 ... through holes, 7, 7A-7C ... agitation sections, 7a, 7b ... elongate grooves, 7c ... elongate protrusions

Claims (7)

In a micro processing apparatus comprising a flow path through which a liquid to be treated flows and an action part that is exposed in the flow path and performs a predetermined action on the liquid to be treated.
The working section includes a stirring section including a plurality of grooves and / or a plurality of protrusions.   The micro processing apparatus according to claim 1, wherein a flow path is formed by laminating a plurality of functional layers subjected to predetermined processing, and an action portion is provided in any one of the functional layers.   The micro-processing apparatus according to claim 1 or 2, wherein the agitation unit includes a plurality of grooves whose extending direction is inclined at a predetermined angle with respect to the extending direction of the flow path.   The action part is an anode and a cathode that are arranged to face each other in the flow path, and a stirring part is provided for either one or both of the anode and the cathode. Micro processing equipment.   5. The micro-processing apparatus according to claim 4, further comprising a diaphragm that separates the anode and the cathode.   The micro-processing apparatus according to claim 1, wherein the action part is a catalyst support part.   The micro-processing apparatus according to claim 1, wherein the action unit is a light-emitting unit.

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