WO2012043382A1 - Dispositif d'alimentation pour un monomère polymérisable - Google Patents

Dispositif d'alimentation pour un monomère polymérisable Download PDF

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Publication number
WO2012043382A1
WO2012043382A1 PCT/JP2011/071637 JP2011071637W WO2012043382A1 WO 2012043382 A1 WO2012043382 A1 WO 2012043382A1 JP 2011071637 W JP2011071637 W JP 2011071637W WO 2012043382 A1 WO2012043382 A1 WO 2012043382A1
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Prior art keywords
mass flow
polymerizable monomer
flow rate
temperature
unit
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PCT/JP2011/071637
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English (en)
Japanese (ja)
Inventor
川崎　真一
野上　光秀
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積水化学工業株式会社
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Priority to JP2012536395A priority Critical patent/JP5281203B2/ja
Publication of WO2012043382A1 publication Critical patent/WO2012043382A1/fr

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    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F2/00—Processes of polymerisation
    • C08F2/01—Processes of polymerisation characterised by special features of the polymerisation apparatus used
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J4/00—Feed or outlet devices; Feed or outlet control devices
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
    • B01J8/18—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with fluidised particles
    • B01J8/24—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with fluidised particles according to "fluidised-bed" technique
    • B01J8/46—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with fluidised particles according to "fluidised-bed" technique for treatment of endless filamentary, band or sheet material
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/08—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor
    • B01J2219/0894—Processes carried out in the presence of a plasma

Definitions

  • the present invention relates to an apparatus for supplying a polymerizable monomer to a utilization part thereof, and particularly suitable for performing flow management such as measurement and control of the flow rate of a polymerizable monomer by providing a thermal mass flow meter and a mass flow controller in a supply line.
  • the present invention relates to a supply device.
  • Patent Document 1 describes that as a pretreatment for bonding a protective film for a polarizing plate to a polarizing film, a thin film of a polymerizable monomer is formed on the surface of the protective film and then irradiated with atmospheric pressure plasma. Has been. Thin film formation of the polymerizable monomer is performed by spray coating or the like. Examples of the polymerizable monomer include hydroxyethyl methacrylate (HEMA), acrylic acid, methacrylic acid, and the like.
  • HEMA hydroxyethyl methacrylate
  • a thermal mass flow meter and a thermal mass flow controller are well known.
  • This type of mass flow meter and mass flow controller has a thermal mass flow rate detector.
  • the thermal mass flow rate detection unit heats at least a part of the fluid to be inspected, and detects the mass flow rate based on the temperature distribution in the flow direction of the heated fluid to be inspected.
  • the polymerizable monomer tends to cause a polymerization reaction when heat is applied.
  • the thermal mass flow rate detection unit when the flow rate of the polymerizable monomer is controlled by a thermal mass flow meter or mass flow controller, the polymerization of the polymerizable monomer proceeds in the detection path of the thermal mass flow rate detection unit, and the detection path may eventually be blocked. There is.
  • the present invention has been made based on the above circumstances. When the supply flow rate of the polymerizable monomer is managed (measured or controlled) by a thermal mass flow meter or a thermal mass flow controller, the thermal mass flow rate is determined.
  • An object of the present invention is to prevent the detection path of the detection unit from being clogged by polymerization of a polymerizable monomer and to stably control the flow rate.
  • the present invention provides a supply device for supplying a polymerizable monomer to a utilization unit that uses the polymerizable monomer, and is provided on a supply line that allows the polymerizable monomer to flow in a liquid state.
  • a mass flow controller comprising a mass flow controller or a mass flow meter having a thermal mass flow detector, and a cooling means for cooling the mass flow controller, wherein the set temperature of the cooling means is the polymerizable monomer Is lower than the temperature at which the polymerization reaction occurs and higher than the freezing point of the polymerizable monomer.
  • the mass flow rate management unit can be cooled to the set temperature by the cooling means, and thus the temperature of the polymerizable monomer liquid flowing in the mass flow rate management unit can be kept lower than the temperature causing the polymerization reaction. it can.
  • This can prevent the polymerizable monomer liquid from being polymerized in the detection path of the mass flow rate management unit.
  • the detection path of the thermal mass flow rate detection unit from being blocked by polymerization or solidification of the polymerizable monomer liquid.
  • the flow rate of the polymerizable monomer can be stably controlled, and the reliability of the polymerizable monomer supply device can be improved.
  • the cooling means faces at least the thermal mass flow rate detection unit and the peripheral part of the thermal mass flow rate detection unit in the mass flow rate management unit.
  • the thermal mass flow rate detection unit is locally cooled, but also its peripheral parts (components and ambient gas etc. near the thermal mass flow rate detection unit) can be cooled.
  • the periphery thereof can be maintained at a uniform temperature (for example, about room temperature). Therefore, it is possible to reliably prevent the polymerizable monomer liquid from being polymerized in the detection path, and to reliably prevent the detection path from being blocked.
  • the polymerizable monomer liquid can be heated by the thermal mass flow rate detection unit based on the temperature after cooling in the detection path, a temperature distribution corresponding to the mass flow rate of the polymerizable monomer can be reliably formed. Therefore, the cooling action of the cooling means does not become an obstacle to the thermal detection of the mass flow rate.
  • the set temperature of the cooling means is preferably 15 ° C. to 30 ° C., more preferably 20 ° C. to 25 ° C. (near room temperature). As a result, it is possible to reliably prevent the acrylic acid from being polymerized or solidified in the detection path of the thermal mass flow rate detection unit, and to reliably block the detection path.
  • a vaporizer for vaporizing a polymerizable monomer is interposed between the mass flow management unit and the utilization unit, and the mass flow management unit and the vaporizer are accommodated in one casing.
  • the mass flow management unit and the vaporizer can be arranged close to each other, and the path length of the flow path portion connecting the mass flow management unit and the vaporizer in the supply line can be shortened.
  • the responsiveness of the vaporizer when the set flow rate of the polymerizable monomer is changed can be enhanced. Even when there is a vaporizer near the mass flow management unit and heat for vaporization reaches the mass flow management unit, this heat can be quickly removed from the mass flow management unit by the cooling element.
  • the temperature of the polymerizable monomer in the mass flow rate management unit is rising, and to reliably prevent the polymerizable monomer from causing a polymerization reaction in the mass flow rate management unit.
  • the flow rate of the polymerizable monomer can be controlled more stably, and the reliability of the polymerizable monomer supply device can be further enhanced.
  • the cooling means is preferably a Peltier element. Accordingly, there is no need to provide a temperature control medium (refrigerant) pipe or the like, the apparatus can be made compact, and maintenance can be easily performed.
  • the supply device may further include a temperature adjustment means including a medium temperature adjustment unit that adjusts the temperature of the temperature adjustment medium, and a first heat exchange unit.
  • the first heat exchange unit may include a heat exchange path through which the temperature control medium from the medium temperature control unit flows to exchange heat with the mass flow rate management unit. Thereby, the temperature control (cooling) of the mass flow rate management unit can be reliably performed.
  • the first heat exchange part may function as the cooling means.
  • the temperature control unit further includes a second heat exchange unit that exchanges heat between a portion of the supply line upstream of the mass flow rate management unit and the temperature control medium.
  • a second heat exchange unit that exchanges heat between a portion of the supply line upstream of the mass flow rate management unit and the temperature control medium.
  • the temperature of the mass flow management unit can be made substantially the same as the set temperature of the temperature control medium by heat exchange between the temperature control medium and the mass flow management unit. Therefore, the polymerizable monomer liquid and the mass flow rate management unit can be brought to substantially the same temperature. As a result, when the mass flow rate is detected by the mass flow rate management unit, it is possible to prevent a detection error due to a temperature difference between the mass flow rate management unit and the polymerizable monomer liquid, and it is possible to accurately detect the mass flow rate of the polymerizable monomer.
  • Examples of the polymerizable monomer include monomers having an unsaturated bond and a predetermined functional group.
  • the predetermined functional group is selected from, for example, a hydroxyl group, a carboxyl group, an acetyl group, a glycidyl group, an epoxy group, an ester group having 1 to 10 carbon atoms, a sulfone group, and an aldehyde group.
  • Examples of the monomer having an unsaturated bond and a hydroxyl group include ethylene glycol methacrylate, allyl alcohol, and hydroxyethyl methacrylate (HEMA).
  • Examples of the monomer having an unsaturated bond and a carboxyl group include acrylic acid, methacrylic acid, itaconic acid, maleic acid, 2-methacryloylpropionic acid and the like.
  • Examples of the monomer having an unsaturated bond and an acetyl group include vinyl acetate.
  • Examples of the monomer having an unsaturated bond and a glycidyl group include glycidyl methacrylate.
  • Monomers having an unsaturated bond and an ester group include methyl acrylate, ethyl acrylate, butyl acrylate, t-butyl acrylate, 2-ethylhexyl acrylate, octyl acrylate, methyl methacrylate, ethyl methacrylate, methacrylic acid
  • Examples include butyl, t-butyl methacrylate, isopropyl methacrylate and 2-ethyl methacrylate.
  • Examples of the monomer having an unsaturated bond and an aldehyde group include acrylic aldehyde and crotonaldehyde.
  • the polymerizable monomer may be a monomer having an unsaturated bond but not having a functional group.
  • the polymerizable monomer may be an olefin monomer.
  • the olefin monomer is an unsaturated hydrocarbon having a double bond and no polar functional group, and may be linear or cyclic, and the number of double bonds may be one or two or more.
  • Examples of the linear olefinic monomer include 1-pentene, 1-hexene, 1-heptene, 1-octene and the like.
  • cyclic olefin monomer examples include 1-cyclopentene, 1-cyclohexene, 1-cycloheptene, 1-cyclooctene, and cyclic dienes such as cyclopentadiene and dicyclopentadiene (DCPD).
  • DCPD dicyclopentadiene
  • the polymerizable monomer may be a water-soluble monomer.
  • water-soluble monomers include acetaldehyde, vinyl alcohol, acrylic acid (AA), methacrylic acid, styrene sulfonic acid, acrylamide, methacrylamide, N, N-dimethylaminopropylacrylamide, N, N-dimethylamide and the like.
  • the utilization part is a film surface treatment part that performs a surface treatment for improving the adhesion of a hard-to-adhere optical resin film.
  • the main component of the hardly adhesive optical resin film include triacetate cellulose (TAC), polypropylene (PP), polyethylene (PE), cycloolefin polymer (COP), cycloolefin copolymer (COC), and polyethylene terephthalate. (PET), polymethyl methacrylate (PMMA), polyimide (PI) and the like.
  • the film surface treatment unit preferably includes a plasma generation unit that generates plasma under atmospheric pressure.
  • the vicinity of atmospheric pressure refers to a range of 1.013 ⁇ 10 4 to 50.663 ⁇ 10 4 Pa, and considering the ease of pressure adjustment and the simplification of the apparatus configuration, 1.333 ⁇ 10 4 to 10.664 ⁇ 10 4 Pa is preferable, and 9.331 ⁇ 10 4 to 10.9797 ⁇ 10 4 Pa is more preferable.
  • the polymerizable monomer is supplied from the supply device to the film surface treatment device, and the polymerizable monomer is attached to the hardly adhesive optical resin film in the film surface treatment unit, and is further exposed to plasma near atmospheric pressure. Plasma polymerization.
  • the adhesion promoting layer can be formed on the surface of the hardly adhesive optical resin film, and the adhesiveness with the easily adhesive optical resin film can be enhanced.
  • the main component of the easily adhesive optical resin film include polyvinyl alcohol (PVA) and ethylene vinyl acetate copolymer (EVA).
  • the polymerizable monomer is preferably a monomer having an ethylenically unsaturated double bond and a carboxyl group.
  • examples of such monomers include acrylic acid (CH 2 ⁇ CHCOOH), methacrylic acid (CH 2 ⁇ C (CH 3 ) COOH), and the like.
  • the detection path of the thermal type mass flow rate detection part in a thermal type mass flow meter or a mass flow controller is obstruct
  • FIG. 1 shows a first embodiment of the present invention.
  • 1st Embodiment applies this invention to the film surface treatment apparatus which surface-treats the protective film 9 of the polarizing plate for liquid crystal panel displays.
  • the protective film 9 is composed of, for example, a TAC film mainly composed of triacetate cellulose (TAC).
  • TAC triacetate cellulose
  • the film to be treated is not limited to TAC, but polypropylene (PP), polyethylene (PE), cycloolefin polymer (COP), cycloolefin copolymer (COC), polyethylene terephthalate (PET), polymethyl methacrylate (PMMA), polyimide (PI), or other various resin films may be used.
  • the protective film 9 is surface-treated in the plasma surface treatment unit 2 (use unit).
  • the plasma surface treatment unit 2 includes a pair of roll electrodes 3.
  • a continuous sheet-like processed film 9 is wound around the circumferential surface of each roll electrode 3 about a half turn.
  • An electric field is applied between the pair of electrodes 3, and plasma near atmospheric pressure is generated in the interelectrode space 3a.
  • a nozzle 4 faces the interelectrode space 3a.
  • a discharge generating gas such as nitrogen (N2) is supplied from the nozzle 4 to the interelectrode space 3a.
  • the polymerizable monomer is supplied from the supply device 1 to the film 9 to be processed.
  • This polymerizable monomer contacts the surface of the film 9 and undergoes plasma polymerization in the discharge space 3a.
  • an adhesion promoting layer made of a polymerized monomer film can be formed on the surface of the film 9 to be treated.
  • the film 9 after the surface treatment is bonded to a polarizing film made of a PVA film.
  • An aqueous adhesive such as an aqueous PVA solution is used as the adhesive.
  • the polymerizable monomer supply device 1 will be described. As shown in FIG. 1, the polymerizable monomer supply device 1 includes a supply line 10, a housing 20, a thermal mass flow controller 30, and a vaporizer 40.
  • the supply line 10 includes a liquid supply line 12 extending from the polymerizable monomer supply source 11 and a gas supply line 13 following the line 12.
  • a polymerizable monomer is stored in the supply source 11 in a liquid state.
  • the polymerizable monomer is, for example, acrylic acid (AA), but is not limited thereto, and may be methacrylic acid, and itaconic acid, maleic acid, 2-methacryloylpropionic acid, ethylene glycol methacrylate, allyl alcohol.
  • AA acrylic acid
  • itaconic acid maleic acid
  • 2-methacryloylpropionic acid maleic acid
  • 2-methacryloylpropionic acid ethylene glycol methacrylate
  • allyl alcohol allyl alcohol
  • a mass flow controller 30 is provided in the middle of the liquid supply line 12. Further, the downstream end of the liquid supply line 12 is connected to the vaporizer 40.
  • a gas supply line 13 extends from the vaporizer 40 to the plasma surface treatment unit 2. The vaporizer 40 is interposed between the mass flow controller 30 (mass flow rate management unit) and the plasma surface treatment unit 2 (utilization unit) in the supply line 10.
  • Acrylic acid (polymerizable monomer) is sent from the supply source 11 in a liquid state, and sent to the vaporizer 40 through the flow rate control of the mass flow controller 30.
  • Acrylic acid is vaporized in the vaporizer 40.
  • the vaporizer 40 is provided with a heater 41 and the like for vaporization.
  • the vaporized acrylic acid may be mixed with a carrier gas such as nitrogen (N 2 ).
  • a blowing nozzle 14 is provided at the downstream end of the gas supply line 12.
  • the blowing nozzle 14 faces the film 9 to be processed in the plasma surface treatment unit 2.
  • the acrylic acid vapor vaporized by the vaporizer 40 is blown out from the blowing nozzle 14 through the gas supply line 12.
  • the acrylic acid is condensed and adheres to the surface of the film 9 to be processed.
  • acrylic acid is turned into plasma and polymerized to form the adhesion promoting layer.
  • the thermal mass flow controller 30 (mass flow rate management unit) is configured as follows.
  • the mass flow controller 30 includes a thermal mass flow rate detection unit 31, a control unit 32, and a flow rate control valve 33.
  • the liquid supply line 12 passes through the inside of the mass flow controller 30.
  • a detection path 15 is provided inside the mass flow controller 30.
  • the upstream end of the detection path 15 branches from the liquid supply line 12 in the mass flow controller 30.
  • the downstream end of the detection path 15 merges with a portion of the liquid supply line 12 on the downstream side of the branch portion.
  • a thermal mass flow rate detector 31 is provided in the detection path 15.
  • the thermal mass flow rate detection unit 31 includes a heating unit 34 such as a coil.
  • a pair of heating units 34 are provided on the upstream and downstream sides of the detection path 15.
  • a part of the acrylic acid solution passing through the liquid supply line 12 is diverted to the detection path 15.
  • the upstream part and the downstream part of the detection path 15 are heated by the heating part 34.
  • a temperature distribution according to the mass flow rate of the acrylic acid liquid is formed along the flow direction of the detection path 15.
  • a detection signal corresponding to the temperature distribution is input from the thermal mass flow rate detection unit 31 to the control unit 32.
  • the control unit 32 includes an input / output interface, a microcomputer, a drive circuit for the flow control valve 33, and the like.
  • the control unit 32 operates the flow rate control valve 33 based on the detection signal to control the mass flow rate of the acrylic acid solution in the liquid supply line 12 to be the set flow rate. Further, the detected mass flow rate and the like are displayed on the display unit 35.
  • the mass flow controller 30 is accommodated in the housing 20 together with the vaporizer 40.
  • the mass flow controller 30 and the vaporizer 40 are close to each other. Therefore, the path length of the portion connecting the mass flow controller 30 and the vaporizer 40 in the liquid supply line 12 can be shortened. Thereby, the responsiveness of the vaporizer 40 when the set flow rate of acrylic acid is changed by the mass flow controller 30 can be enhanced.
  • the mass flow controller 30 is provided with a Peltier element 50 (cooling element, cooling means).
  • the heat absorption surface 51 of the Peltier element 50 is directed to the inside of the mass flow controller 30, and the heat dissipation surface 52 is directed to the outside of the mass flow controller 30.
  • the endothermic surface 51 is disposed near the thermal mass flow rate detection unit 31 and faces at least the thermal mass flow rate detection unit 31 and the periphery of the detection unit 31 in the mass flow controller 30.
  • the Peltier element 50 is larger than the area of one side part (bottom part in FIG. 1) of the mass flow controller 30, and the heat absorption surface 51 faces the entire area of the mass flow controller 30.
  • the outer peripheral portion of the Peltier element 50 protrudes outward from the one side portion of the mass flow controller 30 over the entire periphery.
  • the Peltier element 50 may be attached to the outer surface of the body or housing of the mass flow controller 30 or may be embedded in the body or housing of the mass flow controller 30.
  • the set temperature of the Peltier element 50 is higher than the freezing point of the polymerizable monomer and lower than the temperature at which the polymerizable monomer causes a polymerization reaction.
  • the set temperature of the Peltier element 50 is preferably about 15 ° C. to 30 ° C., more preferably about 20 ° C. to 25 ° C. (near room temperature).
  • the freezing point of acrylic acid is 14 ° C.
  • the temperature at which acrylic acid causes a polymerization reaction is about 35 ° C. or higher (see Example 1).
  • the mass flow controller 30 is entirely cooled by the Peltier element 50.
  • the peripheral portion of the thermal mass flow rate detector 31 is cooled.
  • the temperature of acrylic acid flowing through the mass flow controller 30 can be maintained preferably at about 15 ° C. to about 30 ° C., more preferably about 20 ° C. to about 25 ° C. (near room temperature).
  • the upper limit temperature preferably about 30 ° C., more preferably about 25 ° C., it is possible to prevent acrylic acid from causing a polymerization reaction in the mass flow controller 30.
  • the lower limit temperature for cooling by the Peltier element 50 is set to preferably about 15 ° C., more preferably about 20 ° C., it is possible to prevent acrylic acid from being overcooled and solidifying in the mass flow controller 30.
  • the acrylic acid can be prevented from solidifying in the detection path 15.
  • the liquid supply line 12 in the mass flow controller 30 can be prevented from being blocked by polymerization or solidification of acrylic acid.
  • the detection path 15 can be reliably prevented from being blocked by polymerization or solidification of acrylic acid.
  • the acrylic acid flow rate can be stably controlled (managed), and the reliability of the polymerizable monomer supply apparatus 1 can be improved.
  • the Peltier element 50 faces at least the thermal mass flow rate detection unit 31 and its peripheral part in the mass flow controller 30, not only the thermal mass flow rate detection unit 31 is locally cooled but thermal mass flow rate detection.
  • the peripheral part of the part 31 (components near the thermal mass flow rate detection part 31, atmosphere gas, etc.) can also be cooled.
  • the Peltier element 50 faces the entire area of the mass flow controller 30, and the outer periphery of the Peltier element 50 protrudes outward from the mass flow controller 30, so that the entire mass flow controller 30 (including the internal space) and the mass flow can be obtained.
  • the ambient gas around the controller 30 can be uniformly cooled.
  • the acrylic acid liquid is heated in the detection path 15 by the heating unit 34 based on the temperature after cooling (about room temperature). Therefore, the temperature distribution according to the mass flow rate of acrylic acid can be reliably formed, and the mass flow rate of acrylic acid can be reliably detected. Therefore, the cooling effect of the Peltier element 50 does not become an obstacle to the thermal detection of the mass flow rate.
  • the mass flow controller 30 and the vaporizer 40 are accommodated in one housing 20, and the vaporizer 40 is near the mass flow controller 30. For this reason, even in an environment where the heat of the heater 41 reaches the mass flow controller 30, this heat can be quickly removed from the mass flow controller 30 by the Peltier element 50. Therefore, it is possible to prevent the temperature of acrylic acid in the mass flow controller 30 from rising, and it is possible to reliably prevent acrylic acid from causing a polymerization reaction in the mass flow controller 30.
  • the liquid supply line 12 in the mass flow controller 30 can be reliably prevented from being blocked, and in particular, the detection path 15 can be reliably prevented from being blocked. Therefore, the acrylic acid flow rate can be controlled (managed) more stably, and the reliability of the polymerizable monomer supply device 1 can be further enhanced.
  • the Peltier element 50 As a cooling element, there is no need to provide piping for the temperature control medium (refrigerant), the apparatus can be made compact, and maintenance is easy.
  • a thermal mass flow meter 30M is provided as a mass flow rate management unit instead of the mass flow controller 30.
  • the mass flow meter 30M includes the detection path 15 and the thermal mass flow rate detection unit 31, but does not include the control unit 32 and the flow rate control valve 33.
  • the mass flow rate of acrylic acid is measured by the thermal mass flow rate detection unit 31, and the measurement result is displayed on the display unit 35. Alternatively, the measurement result is output to a management unit that manages the operation of the entire system.
  • FIG. 3 shows a third embodiment of the present invention.
  • the third embodiment relates to another aspect of the cooling means. More specifically, the polymerizable monomer supply device 1 of the third embodiment includes a temperature control means 6.
  • the temperature adjustment means 6 includes a medium temperature adjustment unit 60 and a first heat exchange unit 61.
  • the medium temperature adjustment unit 60 includes a chiller, a heat pump, a refrigerator, an electric heater, and the like, and adjusts the temperature of the temperature adjustment medium to be a predetermined value.
  • the set temperature of the temperature control medium is preferably about 15 ° C. to about 30 ° C., more preferably about 20 ° C. to about 25 ° C. (around room temperature). Water is used as the temperature control medium.
  • the temperature adjustment medium is not limited to water, and other liquids may be used, or a gas such as air or nitrogen may be used.
  • the 1st heat exchange part 61 is comprised with the board which consists of a material excellent in thermal conductivity. Examples of the material include metals such as aluminum, stainless steel, and iron.
  • the 1st heat exchange part 61 is comprised with the plate of aluminum.
  • the first heat exchange unit 61 may be attached to the outer surface of the body or housing of the mass flow controller 30 or may be provided inside the body or housing of the mass flow controller 30.
  • the first heat exchange unit 61 faces at least the thermal mass flow rate detection unit 31 of the mass flow controller 30 and the periphery of the detection unit 31.
  • the first heat exchanging part 61 is larger than the area of one side part (the bottom part in FIG. 3) of the mass flow controller 30 and faces the entire area of the mass flow controller 30.
  • the outer peripheral portion of the first heat exchanging portion 61 protrudes outward from the one side portion of the mass flow controller 30 over the entire circumference.
  • Each heat exchange path 61a penetrates the inside of the 1st heat exchange part 61 in one direction (longitudinal direction).
  • the three heat exchange paths 61a are arranged in a direction orthogonal to the extending direction of each other. Thereby, the heat exchange path 61 a is distributed over a wide range of the first heat exchange unit 61.
  • the number of heat exchange paths 61a is not limited to three, and may be one, two, or four or more.
  • the first heat exchange unit 61 may include, for example, a serpentine tube, and the inside of the tube may be a heat exchange path 61a.
  • a medium forward path 63 extends from the outlet port of the medium temperature adjustment unit 60.
  • the medium forward path 63 branches into three and is connected to one end of each heat exchange path 61a. Further, the other end portions of the heat exchange paths 61 a merge into one and continue to the medium return path 64.
  • a medium return path 64 is connected to the inlet port of the medium temperature adjustment unit 60.
  • the branch portion of the medium forward path 63 and the junction portion of the medium return path 64 are respectively provided outside the first heat exchange portion 61, but the branch portion and the junction portion of the first heat exchange portion 61 are provided. It may be formed inside.
  • the total cross-sectional area of the three heat exchange paths 61 a is larger than the cross-sectional area of the forward path 63 and larger than the cross-sectional area of the return path 64.
  • the total channel cross-sectional area is about three times the channel cross-sectional area of the forward path 63 and about three times the channel cross-sectional area of the return path 64.
  • temperature-controlled water water whose temperature is adjusted by the medium temperature adjusting unit 60 (hereinafter referred to as “temperature-controlled water”) is caused to flow to each heat exchange path 61 a via the medium forward path 63.
  • the flow rate of the temperature-controlled water in each heat exchange path 61a is smaller than the flow rate of the temperature-controlled water in the reciprocating paths 63 and 64.
  • This temperature-controlled water exchanges heat with the mass flow controller 30 via the main body of the first heat exchange unit 61.
  • the mass flow controller 30 can be cooled, and the temperature of the mass flow controller 30 can be set to a substantially set temperature (preferably about 20 ° C. to 25 ° C.).
  • the 1st heat exchange part 61 comprises the cooling means of the mass flow controller 30 (mass flow rate management part).
  • the first heat exchanging unit 61 faces at least the thermal mass flow rate detection unit 31 and its peripheral part in the mass flow controller 30 so that only the thermal mass flow rate detection unit 31 is locally controlled (cooled or heated). Instead, the temperature of the peripheral portion of the thermal mass flow rate detection unit 31 (such as constituent members and ambient gas near the thermal mass flow rate detection unit 31) can be controlled.
  • the first heat exchange unit 61 faces the entire area of the mass flow controller 30, and further, the outer periphery of the first heat exchange unit 61 protrudes outward from the mass flow controller 30. Temperature) including the space) and the ambient gas around the mass flow controller 30 can be uniformly controlled.
  • the temperature adjustment water is returned to the medium temperature adjustment path 60 through the medium return path 64, and the temperature is adjusted again by the medium temperature adjustment section 60.
  • the temperature adjustment water circulates in the order of the medium temperature adjustment unit 60, the medium forward path 63, the heat exchange path 61 a, and the medium return path 64.
  • FIG. 5 shows a fourth embodiment of the present invention.
  • the temperature control means 6 of the third embodiment (FIG. 3) further includes a second heat exchange unit 62.
  • the 2nd heat exchange part 62 is comprised with the heat exchanger which has two heat exchange paths 62a and 62b.
  • One heat exchange path 62 a is interposed in the supply line 10 upstream from the mass flow controller 30.
  • the heat exchange path 62 a is interposed in the path portion 12 a from the supply source 11 to the mass flow controller 30 in the liquid supply line 12.
  • a solution of acrylic acid (polymerizable monomer) from the supply source 11 is passed through the heat exchange path 62 a in the course of flowing through the liquid supply line 12.
  • the other heat exchange path 62 b is interposed in the medium forward path 63.
  • the temperature-controlled water from the medium temperature adjustment unit 60 is passed through the heat exchange path 62b in the middle of flowing through the medium outward path 63.
  • the heat exchange path 62b may be interposed in the medium return path 64.
  • the temperature-controlled water may be passed through the heat exchange path 62b during the circulation of the medium return path 64.
  • the flow directions of the two heat exchange paths 62a are the same, but the flow directions of the two heat exchange paths 62a may be opposite to each other.
  • the second heat exchange unit 62 exchanges heat between the acrylic acid solution in the heat exchange path 62a and the temperature-controlled water in the heat exchange path 62b.
  • the heat exchange in the second heat exchanging unit 62 is performed.
  • Acrylic acid solution can be cooled.
  • the acrylic acid solution in the supply line 12 is also low because the environmental temperature of the apparatus 1 is lower than the set temperature, the acrylic acid solution can be heated by heat exchange in the second heat exchanging unit 62. . Therefore, regardless of the environmental temperature, the temperature of the acrylic acid solution can be made substantially the above set temperature (preferably about 20 ° C.
  • the acrylic acid solution can be introduced into the mass flow controller 30.
  • temperature control water is sent to the 1st heat exchange part 61, and the temperature of the mass flow controller 30 is temperature-controlled (cooled), and the temperature of the mass flow controller 30 inside and its periphery is substantially made into the said setting temperature. Therefore, the temperature difference between the acrylic acid solution introduced into the mass flow controller 30 and the mass flow controller 30 becomes substantially zero. As a result, it is possible to prevent a detection error due to a temperature difference between the mass flow controller 30 and the acrylic acid liquid when the mass flow controller 30 detects the mass flow rate, and to accurately detect the mass flow rate of the liquid acrylic acid.
  • FIG. 6 shows a fifth embodiment of the present invention.
  • the second heat exchange unit 65 is provided in the supply source 11 at the upstream end of the supply line 10.
  • the 2nd heat exchange part 65 is comprised by the outer tank.
  • An inner tank constituting the supply source 11 is accommodated in the outer tank 65.
  • the outlet port of the medium temperature control unit 60 and the outer tank 65 are connected by a medium forward path 63a.
  • Temperature-controlled water whose temperature has been adjusted by the medium temperature adjustment unit 60 is filled between the outer tank 65 and the inner tank 11 via the medium forward path 63a.
  • This temperature-controlled water exchanges heat with the liquid acrylic acid inside the inner tank 11 through the peripheral wall of the inner tank 11.
  • the acrylic acid solution in the tank 11 is also higher than the set temperature. When the acrylic acid solution can be cooled.
  • the acrylic acid solution in the tank 11 can be heated when the acrylic acid solution in the tank 11 is also lower than the set temperature. As a result, the temperature of the acrylic acid solution in the tank 11 can be made substantially equal to the set temperature.
  • the set temperature By setting the set temperature to preferably 20 ° C. to 25 ° C., it is possible to reliably prevent the acrylic acid solution from causing a polymerization reaction in the tank 11.
  • the medium forward path 63 b is continuous with the heat exchange path 61 a of the first heat exchange unit 61. Temperature-controlled water between the outer tank 65 and the inner tank 11 is sent to the heat exchange path 61a through the medium forward path 63b.
  • the temperature difference between the temperature of the acrylic acid solution and the temperature inside and around the mass flow controller 30 can be made substantially zero, and the detection error due to the temperature difference is detected when the mass flow rate is detected. It can be prevented from occurring.
  • the present invention is not limited to the above-described embodiment, and various modifications can be employed without departing from the spirit of the present invention.
  • the set temperature of the cooling means 50 and 61 is appropriately adjusted according to the component of the polymerizable monomer so that it is lower than the temperature at which the polymerizable monomer causes a polymerization reaction and higher than the freezing point of the polymerizable monomer.
  • the utilization part 2 is not limited to the one in which the surface of the resin film 9 is coated with a plasma polymerization film of a polymerizable monomer, and may be one in which a polymerizable monomer is applied to a substrate, cloth or the like.
  • the utilization part is not limited to a film or coating of a polymerizable monomer, but may be anything that utilizes a polymerizable monomer, and a device, a place for performing various processes or operations such as mixing, blending, molding, filling, and storage. Plant, system, etc.
  • the cooling means may be a cooling element such as a heat pipe other than the Peltier element.
  • the cooling means may have an air cooling part or a heat radiation part such as a fan or a fin.
  • the cooling means may be of a size that cools only a part of the mass flow rate management units 30 and 30M (preferably the mass flow rate detection unit 31).
  • a plurality of embodiments may be combined with each other.
  • the thermal mass flow controller 30 of the third to fifth embodiments (FIGS. 3 to 6) may be replaced with the thermal mass flow meter M of the second embodiment (FIG. 2).
  • the flow path of the 2nd temperature control medium which circulates between 60 and the 2nd heat exchangers 62 and 65 may be isolate
  • the set temperature of the first temperature control medium and the set temperature of the second temperature control medium may be different.
  • the environmental temperature of the apparatus 1 is measured, it is determined whether or not the measured temperature is higher than a certain set value, and the polymerizable monomer is cooled or added in the second heat exchangers 62 and 65 according to the determination result. You may control to warm.
  • the acrylic monomer as a polymerizable monomer was verified as follows after the progress of polymerization with respect to temperature, The acrylic acid solution was sealed in a stainless steel container and allowed to stand for 1 month at a constant temperature of 20 ° C. to 40 ° C. Thereafter, when the presence or absence of polymerization of acrylic acid in the container was examined, no polymer was present when the acrylic acid temperature was 20 ° C, 25 ° C, or 30 ° C. On the other hand, when the acrylic acid temperature was 35 ° C. and 40 ° C., a polymer was formed. From the above results, it was confirmed that the polymerization progress of the polymerizable monomer liquid can be suppressed by controlling the temperature. In the case of acrylic acid, it was confirmed that the polymerization progress could be reliably suppressed or prevented by maintaining the temperature preferably at about 30 ° C. or less, more preferably at about 25 ° C.
  • the present invention is applicable to the manufacture of a polarizing plate for a flat panel display (FPD), for example.
  • FPD flat panel display

Abstract

L'invention divulgue un dispositif d'alimentation d'un monomère polymérisable dans un élément où le monomère doit être utilisé, le débit du monomère polymérisable étant contrôlé de manière stable (mesuré ou régulé). Un élément de contrôle du flux massique comprenant un contrôleur (30) de flux massique thermique ou un compteur (30M) de flux massique est disposé sur une conduite d'alimentation (10) à travers laquelle on fait s'écouler un monomère polymérisable à l'état liquide. L'élément de contrôle du flux massique (30 ou 30M) est refroidi par un moyen de refroidissement (50), par exemple, un dispositif Peltier. Le moyen de refroidissement (50) est conçu pour présenter une température de réglage inférieure aux températures auxquelles le monomère polymérisable subit une réaction de polymérisation et supérieure au point de solidification du monomère polymérisable.
PCT/JP2011/071637 2010-09-28 2011-09-22 Dispositif d'alimentation pour un monomère polymérisable WO2012043382A1 (fr)

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Cited By (1)

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Publication number Priority date Publication date Assignee Title
CN110882867A (zh) * 2018-09-11 2020-03-17 株式会社爱发科 丙烯汽化器

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JPS5853907A (ja) * 1981-09-28 1983-03-30 Nitto Electric Ind Co Ltd アクリル系モノマ−の重合方法
JPH06128303A (ja) * 1992-08-03 1994-05-10 Tokuyama Soda Co Ltd 重合装置
JPH1095805A (ja) * 1997-08-04 1998-04-14 Tokuyama Corp 共重合用混合モノマーの供給方法
JP2000007709A (ja) * 1998-06-25 2000-01-11 Mitsui Chemicals Inc ポリマーの特性を制御する方法
JP2001131209A (ja) * 1999-11-02 2001-05-15 Nippon Shokubai Co Ltd 吸水性重合体の製造方法、及び該重合体の製造装置
JP2006104282A (ja) * 2004-10-04 2006-04-20 Sumitomo Chemical Co Ltd 連続重合装置およびそれを用いた連続重合方法

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS5853907A (ja) * 1981-09-28 1983-03-30 Nitto Electric Ind Co Ltd アクリル系モノマ−の重合方法
JPH06128303A (ja) * 1992-08-03 1994-05-10 Tokuyama Soda Co Ltd 重合装置
JPH1095805A (ja) * 1997-08-04 1998-04-14 Tokuyama Corp 共重合用混合モノマーの供給方法
JP2000007709A (ja) * 1998-06-25 2000-01-11 Mitsui Chemicals Inc ポリマーの特性を制御する方法
JP2001131209A (ja) * 1999-11-02 2001-05-15 Nippon Shokubai Co Ltd 吸水性重合体の製造方法、及び該重合体の製造装置
JP2006104282A (ja) * 2004-10-04 2006-04-20 Sumitomo Chemical Co Ltd 連続重合装置およびそれを用いた連続重合方法

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110882867A (zh) * 2018-09-11 2020-03-17 株式会社爱发科 丙烯汽化器
JP2020040017A (ja) * 2018-09-11 2020-03-19 株式会社アルバック アクリル気化器
CN110882867B (zh) * 2018-09-11 2022-11-08 株式会社爱发科 丙烯汽化器
JP7201372B2 (ja) 2018-09-11 2023-01-10 株式会社アルバック アクリル気化器

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