JP4540491B2 - Manufacturing method of microreactor - Google Patents

Description

  The present invention relates to a method for producing a microreactor in which a fine channel and / or a liquid chromatograph column is formed between a plurality of thermoplastic resin substrates.

  In recent years, by using semiconductor processing technology such as photolithography on a substrate such as silicon, a fine channel and a column for liquid chromatography are formed, and various chemical reactions are carried out in the channel, so that an existing analyzer can be used. Research on microreactors for miniaturization and chemical plant miniaturization and high functionality is being actively conducted.

  The material constituting the microreactor has been replaced with a synthetic resin, particularly a thermoplastic resin having good moldability, which is easy to mass-produce from inorganic materials such as glass and silicon wafer.

In order to form a microchannel and a liquid chromatograph in the microreactor, a microchannel and a liquid chromatograph are formed by laminating two substrates formed with a microchannel recess and a liquid chromatograph recess. In general, lamination is performed by bonding with an adhesive, a pressure-sensitive adhesive tape, or the like (see, for example, Patent Document 1 and Patent Document 2).
JP 2001-70784 A JP 2003-522944 A

  However, if an adhesive is applied to the surface of the substrate, and then laminated and bonded with the adhesive, the adhesive flows and flows into the concave portion for the fine channel or the concave portion for the liquid chromatograph. However, depending on the components of the adhesive, there is also a problem of contamination of the object to be detected.

  Although the method of bonding with an adhesive tape is simple, the pressure-sensitive adhesive constituting the pressure-sensitive adhesive tape has low chemical resistance, which limits the reagents that can be used in the microreactor. When this occurs, the liquid leaks, so that there are disadvantages such as the restriction of the microreactor process.

  In view of the above-mentioned drawbacks, the object of the present invention is that a plurality of thermoplastic resin substrates are firmly bonded without clogging an adhesive or the like in a fine flow path or a liquid chromatograph column, and the fine flow path and / or liquid are interposed therebetween. An object of the present invention is to provide a method for easily and inexpensively producing a microreactor in which a chromatographic column is formed.

The method for producing a microreactor according to claim 1, wherein a plurality of thermoplastic resin substrates are laminated, and a fine flow path and / or a liquid chromatograph column section having a width and depth of 0.1 to 10,000 μm are formed between them. A method of manufacturing a microreactor, wherein the microreactor and / or a liquid chromatograph column part is provided with a recess for a liquid crystal column or a thermoplastic resin substrate laminated thereon. , Ultrasonic fusion of ridges having a bottom width of 0.01 to 0.5 mm and a height of 0.01 to 0.5 mm so as to surround the periphery of the fine flow path and / or the liquid chromatograph column when stacked. The thermoplastic resin substrate is laminated, the accumulated oscillation energy is 200 ws or less, the oscillation time is 5 seconds or less, and the pressing pressure of the thermoplastic resin substrate is 0.1 to 10 kg / c. Characterized by ultrasonic welding at a ^second condition.

The substrate material used in the present invention is a thermoplastic resin because it is laminated by ultrasonic fusion.
The type of the thermoplastic resin is not particularly limited, but is preferably a resin that is easily ultrasonically fused and can be easily surface-treated by heating. For example, a polyolefin resin such as polyethylene resin or polypropylene resin, polystyrene Examples thereof include polyacrylic resins such as polyresin, polylactic acid resin, and polymethyl methacrylate, polycarbonate resins, and silicon resins such as polydimethylsiloxane.

  When using various fluids as the microreactor, polyolefin resin with excellent acid resistance, alkali resistance, chemical resistance, etc. is preferable. When measuring the internal state of the microreactor with an optical measurement method, light transmittance Are preferred.

  Various reagents and additives may be added to improve weather resistance, mechanical strength, chemical resistance, and the like.

Further, the size of the substrate is not particularly limited, but if it becomes larger, the handling property as a microreactor is lowered, so that it is preferably 400 cm ² or less, and the thickness is preferably 0.01 to 100 mm. As the thickness decreases, the substrate becomes a film or sheet.

  In the present invention, a plurality of thermoplastic resin substrates are laminated, and a fine channel and / or a liquid chromatograph column are formed between them. When the width and depth of the microchannel liquid and the chromatographic column are reduced, it becomes difficult to send the liquid due to pressure loss when transporting the liquid, and when the width and depth are increased, the flow of the liquid flowing in the microchannel becomes uneven. Or a large amount of a sample for measurement is required, which makes measurement difficult. Therefore, the thickness is 0.1 to 10,000 μm, preferably 10 to 3000 μm, and more preferably 50 to 1000 μm.

  The liquid chromatograph column section is formed by being sandwiched between fine flow paths. The column section is filled with a liquid chromatograph packing material, and a liquid sample containing a measurement substance is allowed to pass through to adsorb the measurement substance. After that, it is a region having functions such as concentration and separation of the measurement substance by allowing the eluent to pass and releasing the measurement substance.

  The shape of the liquid chromatograph column section is not particularly limited, but the inlet direction or the outlet direction of the liquid chromatograph column section is viewed from the fine channel side so that the liquid sample and the eluent flow in or out uniformly. In this case, it is preferable to be symmetrical.

  The volume of the liquid chromatograph column is not particularly limited, but it is assumed that the required amount of separation and adsorption in the column is greater than the maximum amount of the target measurement substance and matrix expected when used. Can be determined.

  The liquid chromatograph column is filled with a liquid chromatograph filler. The method for filling the liquid chromatograph column with the liquid chromatograph filler is, for example, by forming a filler inlet communicating with the liquid chromatograph column on one of the thermoplastic resin substrates and using the liquid chromatograph filler. A dispenser filled with the suspension of the filler is connected to the filler inlet and pressurized to inject the suspension of the filler for liquid chromatography into the column for the liquid chromatograph. After injection, the filler is filled with a sealant. The method of sealing an injection port is mentioned.

The packing material for liquid chromatography is not particularly limited as long as it is a filler for fine particles generally used in liquid chromatography. For example, styrene-divinylbenzene copolymer, polymethacrylate resin, polyhydroxymethacrylate resin, polyvinyl alcohol , Fine particles such as silica and alumina.

  Typical examples include styrene-divinylbenzene copolymer, polymethacrylate resin, polyhydroxymethacrylate resin, polyvinyl alcohol, silica, carrier materials used in liquid chromatography such as alumina, polyethylene, polypropylene, and ethylene-propylene copolymers. Polyolefins; olefin-halogenated olefin copolymers typified by ethylene-tetrafluoroethylene copolymer, ethylene-chlorotrifluoroethylene copolymer; polytetrafluoroethylene, polyvinylidene fluoride, polychlorotrifluoroethylene, etc. Representative halogenated polyolefins and polysulfones, etc .; porous membrane materials such as cellulosic porous membranes; plant fibers such as cotton and hemp; various natural fibers typified by animal fibers such as silk and wool Recycled fibers; fibrous materials such as various synthetic fibers such as polyester fibers and polyamide fibers; monolithic porous inorganic materials such as porous ceramics and porous glass; or polyacrylamide gel, styrene divinylbenzene copolymer, etc. To a carrier such as a porous monolithic porous organic material, the target measurement substance in a liquid sample, for example, physical adsorption, ionic bond, coordination bond, chelate bond, hydrophobic interaction, intramolecular It may be a filler in which an interacting functional group or atomic group such as an interaction due to polarity is fixed.

  In order to prevent the liquid chromatograph packing material packed in the liquid chromatograph column from flowing out of the liquid chromatograph column near the upstream inlet and the downstream outlet of the liquid chromatograph column A filter may be installed, and the filter preferably has a pore size equal to or smaller than the average particle size of the fine particles of the liquid chromatographic filler.

  The material of the filter is a material that has a pore diameter equal to or smaller than the average particle diameter of the liquid chromatographic packing material packed in the column portion and does not dissolve in the solvent used in the liquid chromatograph. There are no particular limitations, and examples include stainless steel, glass, silica, polyether ether ketone, polyvinylidene difluoride, polytetrafluoroethylene, polycarbonate, polyethylene, polypropylene, cellulose mixed ester, and polyethylene terephthalate.

  A filter can be easily produced by cutting a membrane filter, glass fiber filter paper, monolithic glass, or monolithic polymer containing the above material as a main material into an appropriate filter shape, for example, a strip shape, or forming the same shape.

  The above-mentioned material can be used as a filter by forming it into a strip shape, for example, in a state having the aforementioned pore diameter.

When supplying a liquid sample or eluent to a liquid chromatograph, it is preferable to supply the liquid sample or eluent in a laminar flow state. However, as the filter becomes thicker, the flow of the liquid sample or eluent is disturbed. The cross-sectional area of the filter in contact with the inflow / outlet is preferably 10 mm ² or less, more preferably 1 mm ² or less.

  In order to form a microchannel and / or a liquid chromatograph column, a thermoplastic resin substrate having a recess for the microchannel and / or liquid chromatograph column and another thermoplastic resin substrate are formed. What is necessary is just to laminate | stack, and the recessed part for the column part for liquid chromatographs and / or other thermoplastic resin substrates may be formed, and it does not need to be formed.

However, it is cumbersome and costly to form the recesses for the fine flow path and / or the liquid chromatograph column on both thermoplastic resin substrates, so the fine flow path and / or the liquid chromatograph column Laminate a thermoplastic resin substrate in which a concave portion is formed and another thermoplastic resin substrate in which a concave portion for a microchannel and / or a column portion for liquid chromatography is not formed, to form another thermoplastic resin substrate It is preferable to form the fine channel and / or the liquid chromatograph column by covering the concave portion for the fine channel and / or the liquid chromatograph column with, in this case, in this case, the fine channel and / or the liquid chromatograph The width and depth of the concave portion for the graph column is 0.1 to 10,000 μm, preferably 10 to 3000 μm, more preferably 50 to 1000 μm. That.

  In the present invention, when the fine flow path and / or the thermoplastic resin substrate on which the concave portion for the column portion for liquid chromatography is formed or the thermoplastic resin substrate laminated thereon, the fine flow when laminated. A convex ultrasonic fusion part having a bottom face width of 0.01 to 0.5 mm and a height of 0.01 to 0.5 mm is formed so as to surround the periphery of the path and / or the column part for liquid chromatography. .

  The cross-sectional shape of the ultrasonic welded portion of the ridge is preferable because the tip is melted and bonded to another thermoplastic resin substrate by ultrasonic waves, and the tip is sharp, for example, an approximately isosceles triangle A substantially equilateral triangle, a substantially right triangle, a circle, an ellipse and the like, and a substantially isosceles triangle, a substantially regular triangle or a substantially right triangle is preferable.

  The width and height of the ultrasonic welded portion of the ridge are reduced in width or reduced in height, the amount of molten resin decreases, adhesion becomes insufficient, and conversely the width increases or increases in height. As the flow rate increases, the amount of molten resin increases and flows into the microchannel and / or liquid chromatograph column, causing blockage of the microchannel and / or liquid chromatograph column and a decrease in volume. As a result, it becomes impossible to exhibit the desired performance as a non-melted part, the depth of the fine flow path and / or the liquid chromatograph column becomes deep, and it becomes difficult to control the flow rate. 0.01 to 0.5 mm, and the height is 0.01 to 0.5 mm.

  Further, when the ultrasonic fusion part of the ridges is too close to the fine flow path and / or the liquid chromatograph column part, the molten resin becomes a fine flow path and / or the liquid chromatograph column part when the ultrasonic fusion is performed. Into the flow path of the liquid chromatograph and / or the liquid chromatograph column and block the volume of the liquid chromatograph, and the desired performance as a microreactor cannot be achieved. Alternatively, since the flow is difficult to control because the displacement is much larger than the volume of the liquid chromatograph column, the bottom end of the fine channel and / or liquid chromatograph column and the ultrasonic fusion part of the ridge The distance from the part is preferably 0.05 to 2 mm.

  Since the ultrasonic fusion part of the ridge is formed so as to surround the fine channel and / or the liquid chromatograph column part, it has at least four bent parts. Is difficult to design at 90 degrees, and it is difficult to melt the thermoplastic resin of the bent portion with ultrasonic energy as compared with other portions, which may cause poor adhesion. A gentle curved surface is preferable, and a radius of curvature is preferably 0.01 to 1.0 mm.

  Either one of the thermoplastic resin substrates is positioned on the thermoplastic resin substrate so that positioning is easy when the two thermoplastic resin substrates are laminated, and the thermoplastic resin substrate is not displaced when ultrasonically fusing. In addition, a convex fixed portion having a bottom width of 0.01 to 5 mm and a height of 0.001 to 5 mm is formed, and a concave portion into which the fixed portion can be fitted is formed on the other thermoplastic resin substrate. preferable.

The planar shape of the convex fixing part is not particularly limited, and examples thereof include a square, a rectangle, a triangle, a hexagon, a star, a circle, and an oval, and any position of the thermoplastic resin substrate. What is necessary is just to form. Further, it may be a long ridge, or may be formed so as to surround the periphery of the fine channel and / or the column portion for liquid chromatography. The bottom surface and the top surface of the fixed portion may have the same area, or the area may gradually decrease from the bottom surface to the top surface.

  The shape of the concave portion may be any shape that allows the convex fixing portion to be fitted. However, when the convex fixing portion and the concave portion are in contact, when the ultrasonic fusion is performed, the contact portion is formed by ultrasonic waves. Is melted and ultrasonic energy is wasted, so the depth of the recess is deeper than the height of the convex fixing part, and the width of the concave part is wider than the width of the convex fixing part. It is preferable that a gap is substantially formed between the fixed portion and the recess when the thermoplastic resin substrate is laminated.

  The space between the gaps may be small, and if it is large, the thermoplastic resin substrates will be displaced and positioning will not be performed accurately when both of the thermoplastic resin substrates are laminated, so 0.01 to 0.1 mm is preferable.

In the present invention, both the above thermoplastic resin substrates are laminated, and ultrasonic fusion is performed under the conditions of an integrated oscillation energy of 200 ws or less, an oscillation time of 5 seconds or less, and a pressing pressure of the thermoplastic resin substrate of 0.1 to 10 kg / cm ^2. To do.

  The accumulated oscillation energy at the time of ultrasonic welding is 200 ws or less, preferably 50 ws or less, because a portion other than the ultrasonic fusing part melts or the thermoplastic resin substrate is deformed when it becomes large. .

  The oscillation time during ultrasonic welding is also 5 seconds or less, preferably 1 second or less, because the part other than the ultrasonic fusion part is melted or the thermoplastic resin substrate is deformed when it becomes long. is there.

Furthermore, it is necessary to press and hold the thermoplastic resin substrates to be bonded together during ultrasonic fusion, but the adhesive strength decreases when the pressure is lowered, and the thermoplastic resin substrate is cracked or deformed when the pressure is increased. Therefore, the pressing pressure of the thermoplastic resin substrate is 0.1 to 10 kg / cm ² .

  Next, a description will be given with reference to the drawings. FIG. 1 is a plan view showing an example of a thermoplastic resin substrate on which a microchannel and a recess for a liquid chromatograph column are formed, and FIG. 2 is a cross-sectional view taken along line AA in FIG.

  The thermoplastic resin substrate 1 has a length of 30 mm, a width of 50 mm, and a thickness of 1 mm, and a recess 2 for a liquid chromatograph column having a width of 2 mm, a depth of 0.2 mm, and a length of 30 mm is formed in the approximate center. At both ends of the recess 2 for the liquid chromatograph column, through the recesses 3 and 3 for the filter paper installation part having a width of 1 mm, a depth of 0.3 mm, and a length of 20 mm, the width is 1 mm and the depth is 0.2 mm. The recesses 4 and 4 for the fine flow path having a length of about 7 mm are formed.

  A sample and eluent inlet 5 is drilled at one end of the microchannel recesses 4, 4, and a liquid outlet 6 is drilled at the other end. A liquid chromatograph filler inlet 7 is formed at the end of the recess 2 for the liquid chromatograph column. Further, in the vicinity of the periphery of the thermoplastic resin substrate 1, prismatic fixing portions 8, 8,... Having a length of 2.1 mm, a width of 2.1 mm, and a height of 0.2 mm are formed.

  FIG. 3 is a plan view showing an example of a thermoplastic resin substrate in which a microchannel and a recess for a liquid chromatograph column are not formed, and FIG. 4 is a cross-sectional view taken along line BB in FIG.

The thermoplastic resin substrate 9 has a length of 30 mm, a width of 50 mm, and a thickness of 1 mm.
The ultrasonic fusion bonding part 10 which is a protrusion with an isosceles triangle having a sectional shape of m and a height of 0.5 mm is formed. When the thermoplastic resin substrate 1 and the thermoplastic resin substrate 9 are laminated, the ultrasonic fusion part 10 is provided with a concave part 2 for a liquid chromatograph column part, a concave part 3 for a filter paper installation part, and a fine channel part. It is formed so as to surround the periphery of the recess 4 at intervals of 0.5 mm.

  Further, in the vicinity of the periphery of the thermoplastic resin substrate 9, there are prismatic concave portions 11, 11,... Having a length of 2.2 mm, a width of 2.2 mm, and a depth of 0.21 mm, and the thermoplastic resin substrate 1 and the thermoplastic resin substrate. When the 9 is laminated, the fixing portions 8, 8... Of the thermoplastic resin substrate 1 are formed so as to be fitted.

  In order to form a microreactor, after a filter is installed in the recess 3, the upper surfaces of the thermoplastic resin substrate 1 and the thermoplastic resin substrate 9 are opposed to each other, and the fixing portions 8, 8,. It only has to be fitted and bonded under the above-mentioned ultrasonic fusing conditions and filled with a chromatographic filler from the inlet 7, and as a result, a fine flow path between the thermoplastic resin substrate 1 and the thermoplastic resin substrate 9, A microreactor having a liquid chromatograph column section and a filter paper installation section is obtained.

  In the case where the microreactor is formed of three or more thermoplastic resin substrates, a microchannel and a recess for a liquid chromatograph column are formed in one of the adjacent thermoplastic resin substrates. What is necessary is just to form a microreactor by understanding and laminating | stacking as a thermoplastic resin substrate in which the recessed part for the micro resin flow path and the column part for liquid chromatographs is not formed.

The method for producing a microreactor according to claim 6, wherein a plurality of thermoplastic resin substrates are laminated, and a fine channel and / or a liquid chromatograph column having a width and a depth of 0.1 to 10,000 μm are formed between them. A microreactor manufacturing method, wherein at least one of a thermoplastic resin substrate on which a microchannel and / or a recess for a liquid chromatograph column is formed or a thermoplastic resin substrate laminated thereon, A ridged fixed portion having a bottom width of 0.01 to 5 mm and a height of 0.001 to 5 mm is formed so as to surround the fine flow path and / or the liquid chromatograph column when stacked. Is formed with a convex ultrasonic fusion part having a bottom width of 0.01 to 0.5 mm and a height of 0.01 to 0.5 mm, and the fixing part and ultrasonic fusion are provided on the other thermoplastic resin substrate. Part Are engaged that may be concave stripes formed, both of the thermoplastic resin substrate is laminated, integrated oscillation energy 200ws hereinafter oscillation time 5 seconds or less, the thermoplastic resin substrate pressing pressure 0.1 to 10 / cm ² conditions It is characterized by ultrasonic welding.

Hereinafter, only differences from the microreactor manufacturing method according to claims 1 to 5 will be described.
In the present invention, a convex fixing portion is formed on any one of the thermoplastic resin substrates, and a convex ultrasonic fusion portion is formed thereon, and the fixing is performed on the other thermoplastic resin substrate. A recess is formed in which the portion and the ultrasonic fusion portion can be fitted.

  The fixing part is for easy positioning when laminating both thermoplastic resin substrates, and for preventing the thermoplastic resin substrate from shifting when ultrasonically fusing. When either one of the protrusions having a bottom surface width of 0.01 to 5 mm and a height of 0.001 to 5 mm is laminated, it is formed so as to surround the periphery of the fine channel and / or the liquid chromatograph column. .

  The cross-sectional shape of the fixed portion of the ridge is not particularly limited, but the ultrasonic fusion of the ridge having a bottom surface width of 0.01 to 0.5 mm and a height of 0.01 to 0.5 mm is provided thereon. Since a part is formed, a rectangle or a trapezoid is preferable.

When the width of the fixed portion of the ridge is reduced, it is difficult to form an ultrasonic fusion portion thereon, and when the width is widened, it is difficult to form so as to surround the microchannel and / or the liquid chromatograph column portion. Therefore, the bottom face width is 0.01 to 0.5 mm.

  In addition, if the height of the fixed portion of the ridge is lowered, positioning becomes difficult when laminating both thermoplastic resin substrates, and if it is higher, the ridge must be deepened and the thickness of the microreactor must be increased. Since it is inconvenient and uneconomical, it is 0.01 to 0.5 mm.

  On the fixed portion of the ridge, there is formed an ultrasonic fusion portion of a ridge having a bottom width of 0.01 to 0.5 mm and a height of 0.01 to 0.5 mm. The cross-sectional shape is that the tip is melted and bonded to another thermoplastic resin substrate with ultrasonic waves, and therefore the tip is preferably sharp, for example, an approximately isosceles triangle, an approximately equilateral triangle, an approximately right triangle, A circle, an ellipse, etc. are mentioned, A substantially isosceles triangle, a substantially equilateral triangle, or a substantially right triangle is preferable.

  The width and height of the ultrasonic welded portion of the ridge are reduced in width or reduced in height, the amount of molten resin decreases, adhesion becomes insufficient, and conversely the width increases or increases in height. As the flow rate increases, the amount of molten resin increases and flows into the microchannel and / or liquid chromatograph column, causing blockage of the microchannel and / or liquid chromatograph column and a decrease in volume. As a result, it becomes impossible to exhibit the desired performance as a non-melted part, the depth of the fine flow path and / or the liquid chromatograph column becomes deep, and it becomes difficult to control the flow rate. 0.01 to 0.5 mm, and the height is 0.01 to 0.5 mm.

  Further, the cross-sectional shapes of the fixed portion of the ridge and the ultrasonic fused portion of the ridge may be integrated to form a substantially isosceles triangle, a regular regular triangle, or a substantially right triangle. In this case, the bottom surface width is 0.01. It is preferable that the height is set to 0.011 to 5.5 mm.

  When the fixed portion of the ridge is too close to the fine channel and / or the liquid chromatograph column, the molten resin flows into the fine channel and / or the liquid chromatograph column when the ultrasonic fusion is performed. Clogging of the flow path and / or liquid chromatograph column and reduction of the volume cause the desired performance as a microreactor cannot be exhibited. Conversely, if it is too far, the desired fine flow path and / or liquid chromatograph Since the flow is difficult to control because of the large displacement due to the volume of the column for the column, the distance between the fine channel and / or the liquid chromatograph column and the bottom end of the fixed portion of the ridge is 0. 05-2 mm is preferable.

  The shape of the concave portion may be any shape as long as the convex fixing portion can be fitted to the concave portion. When the convex fixing portion and the concave portion are in contact, when the ultrasonic fusion is performed, the contact portion is formed by ultrasonic waves. Is melted and ultrasonic energy is consumed wastefully, the width of the concave portion is made wider than the width of the convex fixing portion, and when both thermoplastic resin substrates are laminated, the fixing portion and the concave portion are It is preferable that a space is substantially formed between them.

  The space between the gaps may be small, and if it is large, the thermoplastic resin substrates will be displaced and positioning will not be performed accurately when both of the thermoplastic resin substrates are laminated, so 0.01 to 0.1 mm is preferable.

  Further, the depth of the concave stripe is shallower than the total height of the fixed portion of the convex stripe and the height of the ultrasonic fused portion of the convex stripe, and when both thermoplastic resin substrates are laminated, the ultrasonic fusion of the convex stripe is performed. It is preferable that the tip of the part is in contact with the bottom of the groove, and further, the bottom surface of the fixed part of the protrusion and the surface of the groove are flush when the ultrasonic fusion part is fused by ultrasonic fusion. It is preferable to be formed as follows.

Next, a description will be given with reference to the drawings. FIG. 5 is a cross-sectional view of the main part showing a different example of the thermoplastic resin substrate on which the recess for the liquid chromatograph column is formed, and FIG. 6 shows the micro channel and the recess for the liquid chromatograph column. It is principal part sectional drawing which shows the example from which the thermoplastic resin board | substrate which is not formed differs.

  The thermoplastic resin substrate 1 ′ has a length of 30 mm, a width of 50 mm, and a thickness of 1 mm, and a recess 2 ′ for a liquid chromatograph column portion having a width of 2 mm and a depth of 0.2 mm is formed in the approximate center. On both sides of the recess 2 ′ for the liquid chromatograph column section, a width of 2.1 mm and a depth of 0.22 mm are spaced 0.5 mm along the end of the recess section 2 ′ for the liquid chromatograph column section. Are formed.

  The thermoplastic resin substrate 9 ′ has a length of 30 mm, a width of 50 mm, and a thickness of 1 mm, and is formed with fixed portions 8 ′ and 8 ′ having a substantially rectangular shape with a cross-sectional shape of a bottom width of 2.0 mm and a height of 0.15 mm. Then, ultrasonic fused portions 10 ′ and 10 ′, which are ridges having an isosceles triangle in cross section with a bottom width of 2.0 mm and a height of 0.09 mm, are formed on the fixing portions 8 ′ and 8 ′. Yes. The fixing portions 8 ′ and 8 ′ are formed so as to be fitted into the recesses 12 and 12 when the thermoplastic resin substrate 1 ′ and the thermoplastic resin substrate 9 ′ are laminated.

  In order to ultrasonically weld the thermoplastic resin substrate 1 ′ and the thermoplastic resin substrate 9 ′, the upper surfaces of the thermoplastic resin substrate 1 ′ and the thermoplastic resin substrate 9 ′ are opposed to each other, and the ultrasonic welded portion 10 ′. 10 ′ and the fixing portions 8 ′ and 8 ′ may be fitted into the recesses 12 and 12 and bonded under the above ultrasonic fusion conditions. As a result, the thermoplastic resin substrate 1 ′ and the thermoplastic resin substrate 9 ′ A microreactor having a liquid chromatograph column or the like formed therebetween is obtained.

  The structure of the manufacturing method of the microreactor according to claim 1 is as described above, and a plurality of thermoplastic resin substrates are firmly bonded without clogging an adhesive or the like in the fine flow path or the liquid chromatograph column, It is possible to easily and inexpensively manufacture a microreactor in which a fine channel and / or a liquid chromatograph column is formed.

  The configuration of the manufacturing method of the microreactor according to claim 2 is as described above, and since the cross-sectional shape of the ultrasonic welded portion of the ridge is an approximately isosceles triangle, an approximately equilateral triangle, or an approximately right triangle, The thermoplastic resin substrate is more firmly bonded by fusing.

  The structure of the manufacturing method of the microreactor according to claim 3 is as described above, and the interval between the fine channel and / or the liquid chromatograph column part and the bottom end part of the ultrasonic fusion part of the ridge is 0. 0.05 mm to 2 mm, the melted thermoplastic resin flows into the fine channel and / or liquid chromatograph column portion even after ultrasonic fusion, and the fine channel and / or liquid chromatograph column portion becomes There is no blockage or volume reduction.

  The structure of the manufacturing method of the microreactor according to claim 4 is as described above, and further, any one of the thermoplastic resin substrates has a convex shape having a bottom surface width of 0.01 to 5 mm and a height of 0.001 to 5 mm. Since the fixing portion is formed and the concave portion into which the fixing portion can be fitted is formed on the other thermoplastic resin substrate, positioning is easy when laminating the thermoplastic resin substrate, and when heat-sealing A microreactor can be easily produced without deviation.

  The structure of the manufacturing method of the microreactor according to claim 5 is as described above, and when the both thermoplastic resin substrates are laminated, a gap is substantially formed between the fixed portion and the concave portion. Since the fixing portion is not melted during the fusion, and the ultrasonic fusion portion and the other thermoplastic resin substrate are ultrasonically fused, the fusion can be efficiently performed.

The structure of the manufacturing method of the microreactor according to claim 6 is as described above, and surrounds the micro flow path and / or the liquid chromatograph column section when laminated on any one of the thermoplastic resin substrates. In any one of the thermoplastic resin substrates, a fixed portion of a ridge having a bottom surface width of 0.01 to 5 mm and a height of 0.001 to 5 mm is formed, and a bottom surface width of 0.01 to 0.5 mm is formed thereon. Since an ultrasonic fusion part having a convex line with a height of 0.01 to 0.5 mm is formed, a plurality of thermoplastic resin substrates can be formed without clogging an adhesive or the like in a fine channel or a column for liquid chromatography. A microreactor that is firmly bonded and in which a fine channel and / or a liquid chromatograph column is formed can be manufactured more easily and inexpensively.

  The structure of the manufacturing method of the microreactor according to claim 7 is as described above, the cross-sectional shape of the fixed portion of the ridge is rectangular or trapezoidal, and the cross-sectional shape of the ultrasonic weld portion of the ridge is substantially isosceles It is a triangle, a substantially equilateral triangle, or a substantially right triangle, or the cross-sectional shape of the fixed portion of the ridge and the ultrasonic fusion portion of the ridge is an integral isosceles triangle, a regular equilateral triangle, or a substantially right triangle. The thermoplastic resin substrate can be more firmly bonded by sonic fusion.

  The structure of the manufacturing method of the microreactor of Claim 8 is as above-mentioned, and the space | interval of the fine flow path and / or the liquid chromatograph column part, and the bottom face edge part of the fixing part of a protruding item | line is 0.05-. Since the thickness is 2 mm, the molten thermoplastic resin flows into the fine channel and / or the liquid chromatograph column even after ultrasonic fusion, and the fine channel and / or the liquid chromatograph column is blocked. , The volume will not decrease.

  The structure of the manufacturing method of the microreactor according to claim 9 is as described above, and the depth of the concave stripe is shallower than the sum of the heights of the fixing portion of the convex stripe and the ultrasonic fusion portion of the convex stripe, When the thermoplastic resin substrate is laminated, the tip of the ultrasonic welded portion of the ridge is brought into contact with the bottom of the concave strip, so that the ultrasonic fusion is performed while pressing the ultrasonic fused portion against the bottom of the concave strip. As a result, it is possible to bond more firmly.

  The structure of the manufacturing method of the microreactor according to claim 10 is as described above, and the width of the concave line is wider than the width of the convex fixing part, and when both the thermoplastic resin substrates are laminated, the fixing part and the concave part are formed. Since a gap is substantially formed between the strips, the fixing portion is not melted when heat-sealing, and the ultrasonic fusion-bonded portion and another thermoplastic resin substrate are ultrasonically fused. Therefore, it can fuse | melt efficiently.

  The structure of the manufacturing method of the microreactor according to claim 11 is as described above, and the curvature radius of the bent portion of the ultrasonic welded portion of the ridge is 0.01 to 0.5 mm. The bent portion and the other thermoplastic resin substrate can be efficiently fused.

  Next, examples of the present invention will be described, but the present invention is not limited to the following examples.

Example 1
A microreactor was manufactured using the thermoplastic resin substrates 1 and 9 made of methyl methacrylate resin shown in FIGS. First, the filter paper was set in the concave portion 3 for the filter paper setting portion of the thermoplastic resin substrate 1 and temporarily fixed with an adhesive.

  Next, the thermoplastic resin substrate 1 is set on the sample stage of the ultrasonic fusion machine, and the thermoplastic resin substrate 9 is fitted on the concave portion 11 on the thermoplastic resin substrate 9, and the ultrasonic fusion part 10 is thermoplastic. Lamination was performed so as to contact the resin substrate 1, and a horn (ultrasonic oscillation jig) was brought into contact with the thermoplastic resin substrate 1 horizontally. Thereby, the ultrasonic wave is uniformly irradiated on the entire surface of the substrate.

Next, ultrasonic fusion was performed under the conditions of an irradiation time of 0.1 second, an integrated oscillation energy of 10 ws, a pressing pressure of 6 kg / cm ² to the thermoplastic resin substrate 9 and a pressing speed of 5 cm / sec, and further filling for liquid chromatography. A liquid chromatograph filler (trade name PS-130, manufactured by Showa Denko KK) was injected from the material inlet 7, and the liquid chromatograph filler 7 was closed with an adhesive to obtain a microreactor. The average particle size of the packing material for liquid chromatograph was 20 μm, which was regenerated in advance with 10 ⁻³ N nitric acid and washed with water before use.

  The sample of the microreactor and the eluent injection port 5 were connected to an HPLC pump (manufactured by Showa Denko KK, trade name: DS-4 type), and water was supplied at a rate of 50 μl / min and passed through. After confirming that water came out from the liquid discharge port 6, the liquid discharge port 6 was closed, water was further supplied from the HPLC pump, and the pump pressure at which water leakage started from the microreactor was measured. cm.

(Comparative Example 1)
The thermoplastic resin substrate 1 and the thermoplastic resin substrate shown in FIG. 1 were bonded with a double-sided adhesive tape to obtain a microreactor. When the pump pressure at which water leakage started from the microreactor was measured in the same manner as in Example 1 using the obtained microreactor, it was 4 kgf / cm.

It is a top view which shows an example of the thermoplastic resin board | substrate in which the recessed part of the microchannel and the column part for liquid chromatographs is formed. It is AA sectional drawing in FIG. It is a top view which shows an example of the thermoplastic resin substrate in which the recessed part of the microchannel and the column part for liquid chromatographs is not formed. It is BB sectional drawing in FIG. It is principal part sectional drawing which shows the different example of the thermoplastic resin substrate in which the recessed part for column parts for liquid chromatographs is formed. It is principal part sectional drawing which shows a different example of the thermoplastic resin board | substrate in which the recessed part for microchannels and the column part for liquid chromatographs is not formed.

Explanation of symbols

DESCRIPTION OF SYMBOLS 1 Thermoplastic resin substrate in which recess for microchannel and liquid chromatograph column is formed 2 Recess for liquid chromatograph column 3 Recess for filter paper installation 4 Recess for microchannel 5 Sample and Eluent inlet 6 Liquid outlet 7 Filler inlet for liquid chromatograph 8 Fixed portion 9 Thermoplastic resin substrate in which the concave portion of the fine channel and the column portion for liquid chromatograph is not formed 10 Ultrasonic fusion portion 11 Recessed portion 12 concave

Claims (4)

A method of manufacturing a microreactor in which a plurality of thermoplastic resin substrates are laminated, and a microchannel and / or a liquid chromatograph column section having a width and depth of 0.1 to 10,000 μm are formed between the substrates. When laminated on at least one of the thermoplastic resin substrate on which the concave portion for the fine channel and / or the column portion for the liquid chromatograph is formed or the thermoplastic resin substrate laminated thereon, the fine channel and / or the liquid chromatograph are laminated. A convex fixed portion having a bottom width of 0.01 to 5 mm and a height of 0.001 to 5 mm is formed so as to surround the periphery of the graph column portion, and a bottom surface width of 0.01 to 0.5 mm and a high height is formed thereon. A convex ultrasonic fusion part having a thickness of 0.01 to 0.5 mm is formed, and a concave line in which the fixing part and the ultrasonic fusion part can be fitted is formed on the other thermoplastic resin substrate. And the depth of the recess Is shallower than the sum of the height of the fixed portion of the ridge and the ultrasonic fusion portion of the ridge, and when both thermoplastic resin substrates are laminated and fused, the bottom of the fixed portion of the ridge and the concave portion The surface is formed so as to be flush with each other, and when both thermoplastic resin substrates are laminated, a gap of 0.01 to 0.1 mm is formed between the fixing portion and the recess, The width of the concave line is wider than the width of the convex fixing part. Both the thermoplastic resin substrates are laminated, the accumulated oscillation energy is 200 ws or less, the oscillation time is 5 seconds or less, and the pressing pressure of the thermoplastic resin substrate is 0.1. A method for producing a microreactor, wherein ultrasonic fusion is performed under a condition of 10 kg / cm ² . The cross-sectional shape of the fixed portion of the ridge is a rectangle or a trapezoid, and the cross-sectional shape of the ultrasonic fused portion of the ridge is a substantially isosceles triangle, a substantially equilateral triangle, or a substantially right triangle, or a fixed portion of the ridge 2. The method of manufacturing a microreactor according to claim 1, wherein the ultrasonic welded portions of the ridges are integrally formed into a substantially isosceles triangle, a regular regular triangle, or a substantially right triangle. 3. The micro of claim 1, wherein a distance between the fine channel and / or the liquid chromatograph column and the bottom end of the fixed portion of the ridge is 0.05 to 2 mm at the time of stacking. Reactor manufacturing method. 4. The method of manufacturing a microreactor according to claim 1 , wherein the radius of curvature of the bent portion of the ultrasonic welded portion of the ridge is 0.01 to 1.0 mm .

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