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US20140366575A1 - Low-temperature gas supply device, heat transfer medium-cooling device, and low-temperature reaction control device - Google Patents

Low-temperature gas supply device, heat transfer medium-cooling device, and low-temperature reaction control device Download PDF

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Publication number
US20140366575A1
US20140366575A1 US14/345,523 US201214345523A US2014366575A1 US 20140366575 A1 US20140366575 A1 US 20140366575A1 US 201214345523 A US201214345523 A US 201214345523A US 2014366575 A1 US2014366575 A1 US 2014366575A1
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Prior art keywords
temperature
low
gas
transfer medium
heat transfer
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Inventor
Shigemasa Yamazumi
Masahiro Yonekura
Masahiro Takeuchi
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Nippon Sanso Holdings Corp
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Nippon Sanso Holdings Corp
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Assigned to TAIYO NIPPON SANSO CORPORATION reassignment TAIYO NIPPON SANSO CORPORATION ASSIGNMENT OF ASSIGNORS INTEREST (SEE DOCUMENT FOR DETAILS). Assignors: TAKEUCHI, MASAHIRO, YAMAZUMI, SHIGEMASA, YONEKURA, MASAHIRO
Publication of US20140366575A1 publication Critical patent/US20140366575A1/en
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    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25D—REFRIGERATORS; COLD ROOMS; ICE-BOXES; COOLING OR FREEZING APPARATUS NOT OTHERWISE PROVIDED FOR
    • F25D3/00—Devices using other cold materials; Devices using cold-storage bodies
    • F25D3/10—Devices using other cold materials; Devices using cold-storage bodies using liquefied gases, e.g. liquid air
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J5/00—Arrangements of cold exchangers or cold accumulators in separation or liquefaction plants
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J1/00—Processes or apparatus for liquefying or solidifying gases or gaseous mixtures
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J5/00—Arrangements of cold exchangers or cold accumulators in separation or liquefaction plants
    • F25J5/002—Arrangements of cold exchangers or cold accumulators in separation or liquefaction plants for continuously recuperating cold, i.e. in a so-called recuperative heat exchanger

Definitions

  • the present invention relates to a low-temperature gas supply device, heat transfer medium-cooling device, and low-temperature reaction control device.
  • the present application claims priority on the basis of Japanese Patent Application No. 2011-223716, filed in Japan on Oct. 11, 2011, the contents of which are incorporated herein by reference.
  • a low-temperature reaction device In the low-temperature reaction device, a double structure container disposed with an independent vessel (jacket), in which a heat transfer medium is able to flow outside a reaction vessel, is used, and by supplying a heat transfer medium controlled to a low temperature to the jacket part, the reaction liquid in the reaction vessel is cooled and adjusted to be a constant temperature.
  • an independent vessel in which a heat transfer medium is able to flow outside a reaction vessel
  • the heat transfer medium supplied to the reaction vessel is temperature-controlled in the heat exchanger so as to be cooled below the predefined temperature by heat-exchange with a low-temperature-liquefied gas (for example, liquefied nitrogen) of lower temperature than the solidification point of the heat transfer medium, and then is supplied to the jacket of the reaction vessel.
  • a low-temperature-liquefied gas for example, liquefied nitrogen
  • These cooling devices need to be prevented from freezing a heat transfer medium in a heat exchanger. This is because the heat transfer medium freezes and blocks a flow channel, and there is a case where the heat transfer medium cannot be circulated. Also, when the heat transfer medium freezes and blocks a flow channel, the loss of pressure increases; therefore a pump having greater quality than design quality is needed, heat intrusion from the pump increases, and thus the usage of the low-temperature-liquefied gas for cooling increases.
  • the cooling temperature of the heat transfer medium in order to prevent the freezing of the heat transfer medium from advancing, the cooling temperature of the heat transfer medium must be set at a sufficiently higher temperature than the solidification point of the heat transfer medium. Therefore, the low-temperature quality, which the heat transfer medium potentially has, could not be sufficiently used.
  • Patent document 1 it is realized by providing a device for blocking the supply of the low-temperature-liquefied gas using the difference of the pressure of the heat transfer medium between the introducing part and the discharging part in the heat exchanger or using a temperature of an evaporation gas at the discharging part of the low-temperature-liquefied gas in the heat exchanger. Also, in Patent document 2, it is realized by detecting the temperature of the heat-transfer surface in the heat exchanger and controlling a supply quantity of the low-temperature-liquefied gas.
  • a temperature of a liquefied nitrogen is greatly different from that of nitrogen gas of room temperature and because the liquefied nitrogen has large cold energy in a small flow, a control of a very little flow is difficult and after mixing, there is a problem in that a flow of the low-temperature-liquefied nitrogen gas becomes pulsative or a temperature becomes uneven due to poor mixing.
  • efficient or large mixing equipment is needed, which incurs cost increases.
  • the invention provides the following:
  • a low-temperature gas supply device capable of supplying a low-temperature gas refrigerant which is accurately and stably controlled; a heat transfer medium-cooling device in which the low-temperature gas refrigerant is introduced and a heat transfer medium which does not solidify, which is accurately and stably controlled, can be discharged by heat-exchange with the low-temperature gas refrigerant; and a low-temperature reaction control device, in which stable control can be realized over a broad range using the heat transfer medium.
  • the present invention employs the following devices in order to solve the above problems.
  • the low-temperature gas supply device of the present invention because, after reducing the difference of temperature between a low-temperature-liquefied gas and a gas of a temperature higher than the low-temperature-liquefied gas, they are mixed, uniform mixing is realized as well as avoiding the particularity of a mixing unit, thereby enlarging the range of choice.
  • the temperature control of the low-temperature gas refrigerant is stable by adjusting the respective flows of the respective gases before mixing.
  • the control for a pulsatile change of flow is avoided, the pulsatile change of flow resulting from a pulsatile change of temperature due to poor mixing, the control is stable.
  • the changed value can be suitably followed.
  • a cold energy of a low-temperature-liquefied gas can be efficiently used in order to produce low-temperature gas refrigerant.
  • the device can be downsized compared with using a general mixing apparatus.
  • the temperature of a heat transfer medium circulated in a circulation route can be stably controlled with accuracy, and the intended temperature of the heat transfer medium can be set more suitably with the solidification point of the heat transfer medium in mind. That is, in the second heat exchanger, the intended temperature of the heat transfer medium can be set near to the solidification point without freezing the heat transfer medium.
  • the setting can prevent the circulation route from being blocked due to freezing and lower the loss of pressure in the route due to blocking, and thus excess heat is prevented from entering, thus saving power of the entire device.
  • a low-temperature reaction device of the present invention can control a low temperature of a reaction vessel using the heat transfer medium which is stably and accurately controlled to a low temperature near the solidification point, stable control is possible within a broad temperature range.
  • FIG. 1 is a schematic diagram showing a low-temperature gas supply device, heat transfer medium-cooling device, and low-temperature reaction control device according to the first embodiment of the present invention.
  • FIG. 2 is a schematic diagram showing a low-temperature gas supply device, heat transfer medium-cooling device, and low-temperature reaction control device according to the second embodiment of the present invention.
  • FIG. 3 is a schematic diagram showing a low-temperature gas supply device, heat transfer medium-cooling device, and low-temperature reaction control device according to the third embodiment of the present invention.
  • FIG. 4 is a schematic diagram showing a low-temperature gas supply device, heat transfer medium-cooling device, and low-temperature reaction control device according to the fourth embodiment of the present invention.
  • FIG. 1 is a schematic diagram according to the first embodiment, in which a low-temperature gas supply device, a heat transfer medium-cooling device, and low-temperature reaction control of the present invention are used.
  • a low-temperature gas supply device 100 A includes a room temperature route 1 A, from an one end of which a room temperature nitrogen gas (GN 2 )NNG is introduced as a gas of higher temperature than a low-temperature-liquefied gas described below, a low-temperature route 2 A, from an one end of which a liquefied nitrogen (LN 2 )LN (for example, ⁇ 196° C.) is introduced as the low-temperature-liquefied gas, a mixing route 3 A, in which a mixed gas and a low-temperature nitrogen gas refrigerant described below flows, an ejector (mixed device) 4 A, in which the room temperature nitrogen gas NNG introduced from the another end of the room temperature route 1 A and a gas (referred to as “liquefied nitrogen vaporization gas” hereinafter) LNG resulting from a vaporization of the liquefied nitrogen LN are mixed to produce a mixed gas CG, a first
  • the low-temperature route 2 A and the mixing route 3 A run parallel to each other and are constructed so that the liquefied nitrogen LN and the mixed gas CG flowing through the respective routes are heat-exchanged with each other.
  • the low-temperature route 2 A and the mixing route 3 A are disposed so that the liquefied nitrogen LN and the mixed gas CG flow in the opposite direction to each other, i.e., so as to be an opposite flow.
  • a heat transfer medium-cooling device 200 A includes, in addition to the low-temperature gas supply device 100 A described above, a heat transfer medium circulation route 21 , in which a heat transfer medium HM is circulated, a second heat exchanger 22 , through which the mixing route 3 A and the heat transfer medium circulation route 21 running parallel to each other penetrate and which is disposed so that the low-temperature nitrogen gas refrigerant CNG and a heat transfer medium HM flowing through the respective routes are heat-exchanged with each other, a heat transfer medium circulation pump 23 in order to circulate the heat transfer medium HM flowing through the heat transfer medium circulation route 21 , a second temperature detector 24 which detects a temperature of the heat transfer medium HM circulated in the heat transfer medium circulation route 21 , a second temperature adjusting device 25 which output a second control signal CS 2 based on the temperature detected by the second temperature detector 24 , a second flow adjusting valve 26 which adjusts a flow of the low-temperature nitrogen gas refrigerant CNG flowing through
  • a low-temperature reaction control device 300 A includes, in addition to the heat transfer medium-cooling device 200 A described above, a low-temperature reaction vessel 31 .
  • the low-temperature reaction vessel 31 is provided with a jacket 31 a which can circulate the heat transfer medium HM, and a stir motor 31 b in order to stir a reaction liquid.
  • the liquefied nitrogen (LN 2 ) LN is introduced from one end of the low-temperature route 2 A to the first heat exchanger 5 A.
  • the liquefied nitrogen LN becomes the liquefied nitrogen vaporization gas LNG by heat-exchange with the mixed gas CG flowing through the mixing route 3 A in the first heat exchanger 5 A.
  • the liquefied nitrogen vaporization gas LNG discharged from the first heat exchanger 5 A and the room temperature nitrogen gas NNG introduced from one end of the room temperature route 1 A are introduced to the ejector 4 A and mixed due to their pressure differences.
  • the mixed gas CG discharged from the ejector 4 A is introduced to the first heat exchanger 5 A, is heat-exchanged with the liquefied nitrogen LN flowing through the low-temperature route 2 A, the temperature of the mixed gas CG being averaged due to an effect of a disturbed flow at the same time, and is discharged as the low-temperature nitrogen gas refrigerant CNG.
  • the first temperature detector 6 A detects a temperature of the low-temperature nitrogen gas refrigerant CNG flowing at the downstream of the mixing route 3 A below the first heat exchanger 5 A.
  • the first temperature adjusting device 7 A outputs the first control signal CS 1 according to the difference between the temperature detected by the first temperature detector 6 A and the designed temperature (intended temperature) of the low-temperature nitrogen gas refrigerant CNG.
  • the flow adjusting valve 8 A adjusts the flow of the room temperature nitrogen gas NNG flowing through the room temperature route 1 A based on the first control signal CS 1 .
  • the flow adjusting valve 9 A adjusts the flow of the liquefied nitrogen vaporization gas LNG flowing at the downstream of the low-temperature route 2 A below the first heat exchanger 5 A, based on the first control signal CS 1 .
  • the low-temperature nitrogen gas refrigerant CNG is adjusted to be a designed temperature.
  • the flow of the liquefied nitrogen vaporization gas LNG introduced to the ejector 4 A may be adjusted at the first side of the first heat exchanger 5 A, when there is a construction so as to adjust the flow at the second side of the first heat exchanger 5 A in the above manner, i.e., the flow of the liquefied nitrogen vaporization gas LNG, i.e., the flow of the vaporization gas of a single phase, it is possible to adjust the flow more precisely, compared with the manner in which the flow is adjusted at the first side of the first heat exchanger 5 A, i.e., the flow of the heat exchanger LN with a phase-change is adjusted.
  • the low-temperature nitrogen gas refrigerant CNG adjusted to be the designed temperature is supplied to the second heat exchanger 22 and cools the heat transfer medium HM flowing through the heat transfer medium circulation route 21 by heat-exchange.
  • the second temperature detector 24 detects the temperature of the heat transfer medium HM circulated in the heat transfer medium circulation route 21 .
  • the second temperature adjusting device 25 outputs the second control signal CS 2 according to the difference between the temperature detected by the second temperature detector 24 and the designed temperature (the intended temperature) of the heat transfer medium HM.
  • the second flow adjusting valve 26 adjusts the flow of the low-temperature nitrogen gas refrigerant CNG flowing through the mixing route 3 A based on the second control signal CS 2 .
  • the heat transfer medium HM which is adjusted to be the desired temperature as described above is supplied to a jacket 31 a of the low-temperature reaction vessel 31 by action of the heat transfer medium circulation pump 23 .
  • the reaction liquid inside the reaction vessel is cooled and adjusted to be the constant temperature.
  • the uniform mixture can be realized. Because the ejector 4 A is adopted for mixing, even if their pressures are different from each other, mixing can be realized easily and the device can be downsized compared with when the general mixer is used.
  • the liquefied nitrogen LN is translated to the liquefied nitrogen vaporization gas LNG of the similar temperature with the room temperature nitrogen gas NNG by using the first heat exchanger 5 A and they are mixed, a temperature control of the low-temperature nitrogen gas refrigerant CNG due to the flow control of the room temperature nitrogen gas NNG and the liquefied nitrogen vaporization gas LNG is stable.
  • the control of a pulsatile change of the flow is avoided, the pulsatile change of the flow resulting from a pulsatile change of temperature due to poor mixing, the control is stable.
  • the intended temperature of the low-temperature nitrogen gas refrigerant CNG is changed, the changed value can be suitably followed.
  • the cold energy of the liquefied nitrogen LN is efficiently used in order to produce the low-temperature nitrogen gas refrigerant CNG.
  • the intended temperature of the heat transfer medium HM can be set more suitably with the solidification point of the heat transfer medium in mind. That is, in the second heat exchanger 22 , the intended temperature of the heat transfer medium HM can be set near to the solidification point without freezing the heat transfer medium HM.
  • the setting can prevent the heat transfer medium circulation route 21 from being blocked due to freezing and lower the loss of pressure in the route due to blocking, and thus excess heat is prevented from entering, thus saving power of the entire device.
  • the reaction vessel 31 can be more stably controlled at a low temperature and stable control is possible within a broad temperature range.
  • FIG. 2 shows a schematic diagram according to the second embodiment including the low-temperature gas supply device, the heat transfer medium-cooling device, the low-temperature reaction control device of the present invention.
  • a low-temperature gas supply device 100 B includes a room temperature route 1 B, from an one end of which a room temperature nitrogen gas (GN 2 )NNG is introduced, a low-temperature route 2 B, from an one end of which a liquefied nitrogen (LN 2 )LN (for example, ⁇ 196° C.) is introduced, a mixing route 3 B, in which a low-temperature nitrogen gas refrigerant described below flows, a first heat exchanger 5 B, in which the room temperature nitrogen gas NNG introduced from the room temperature route 113 and the liquefied nitrogen LN introduced from the low-temperature route 2 B are heat-exchanged with each other to discharge each gas as an heat-exchanged nitrogen gas CNNG and a gas (referred to as “liquefied nitrogen vaporization gas” hereinafter) LNG resulting from a vaporization of the liquefied nitrogen LN, an ejector 4 B, in which the heat-exchanged
  • the room temperature route 1 B and the low-temperature route 2 B run parallel to each other and are constructed so that the room temperature nitrogen gas NNG and the liquefied nitrogen LN are heat-exchanged with each other.
  • the room temperature route 1 B and the low-temperature route 2 B are disposed so that the room temperature nitrogen gas NNG and the liquefied nitrogen LN flow in the same direction.
  • a heat transfer medium-cooling device 200 B according to the second embodiment is the same as the heat transfer medium-cooling device 200 A according to the first embodiment except that the low-temperature gas supply device 100 B having a construction as above is included.
  • the low-temperature reaction control device 300 B according to the second embodiment is the same as the low-temperature reaction control device 300 A according to the first embodiment except that the heat transfer medium-cooling device 200 B having a construction as above is included.
  • the room temperature nitrogen gas NNG is introduced into one end of the room temperature route 1 B and is introduced into the first heat exchanger 5 B.
  • the liquefied nitrogen (LN 2 ) LN is introduced to one end of the low-temperature route 2 B and is introduced to the first heat exchanger 513 .
  • the first heat exchanger 5 B discharges the gases as a heat-exchanged nitrogen gas CNNG and a gas (referred to as “liquefied nitrogen vaporization gas” hereinafter) LNG resulting from a vaporization of the liquefied nitrogen LN.
  • the ejector 4 B mixes the heat-exchanged nitrogen gas CNNG and the liquefied nitrogen vaporization gas LNG discharged from the first heat exchanger 5 B using the difference of the pressures thereof and produces the low-temperature nitrogen gas refrigerant CNG.
  • the first temperature detector 6 B detects a temperature of the low-temperature nitrogen gas refrigerant CNG flowing through the mixing route 3 B.
  • the first temperature adjusting device 713 outputs the first control signal CS 1 according to the difference between the temperature detected by the first temperature detector 6 B and the designed temperature (intended temperature) of the low-temperature nitrogen gas refrigerant CNG.
  • the flow adjusting valve 8 B adjusts a flow of the room temperature nitrogen gas NNG flowing at an upper stream of the room temperature route 1 B above the first heat exchanger 5 B, based on the first control signal CS 1 .
  • the first flow adjusting valve 9 B adjusts a flow of the liquefied nitrogen vaporization gas LNG flowing at a downstream of the low-temperature route 2 B below the first heat exchanger 5 B, based on the first control signal CS 1 .
  • the low-temperature nitrogen gas refrigerant CNG is adjusted to be the desired temperature.
  • the flow of the vaporization gas introduced to the ejector 413 may be adjusted at the first side of the first heat exchanger 5 B, in the above manner, when there is a construction so as to adjust the flow at the second side of the first heat exchanger 5 B, i.e., the flow of the liquefied nitrogen vaporization gas LNG, i.e., the flow of the vaporization gas of a single phase, it is possible to adjust the flow more precisely, compared with the manner in which the flow is adjusted at the first side of the first heat exchanger 5 B, i.e., the flow of the heat exchanger LN with a phase-change is adjusted.
  • the low-temperature nitrogen gas refrigerant CNG adjusted to be the designed temperature is supplied to the second heat exchanger 22 and cools the heat transfer medium HM flowing through the heat transfer medium circulation route 21 by heat-exchange.
  • the second temperature detector 24 detects a temperature of the heat transfer medium HM circulated in the heat transfer medium circulation route 21 .
  • the second temperature adjusting device 25 outputs the second control signal CS 2 according to the difference between the temperature detected by the second temperature detector 24 and the designed temperature of the heat transfer medium HM.
  • the second flow adjusting valve 26 adjusts a flow of the low-temperature nitrogen gas refrigerant CNG flowing through the mixing route 3 B, based on the second control signal CS 2 . In this manner, by a feed back control constructed of the second temperature detector 24 , the second temperature adjusting device 25 , and the second flow adjusting valve 26 , the heat transfer medium HM is adjusted to be the desired temperature.
  • the heat transfer medium HM which is adjusted to be the desired temperature as described above is supplied to a jacket 31 a of the low-temperature reaction vessel 31 by action of the heat transfer medium circulation pump 23 . By this supply, the reaction liquid inside the reaction vessel is cooled and adjusted to be the constant temperature.
  • the uniform mixture can be realized. Because the ejector 4 B is adopted for mixing, even if their pressures are different from each other, mixing can be realized easily and the device can be downsized compared with when the general mixer is used.
  • the room temperature nitrogen gas NNG and the liquefied nitrogen LN are translated to the heat-exchanged nitrogen gas CNNG and the liquefied nitrogen vaporization gas LNG, in which the difference of the temperatures thereof is reduced by using the first heat exchanger 5 B, and they are mixed, a temperature control of the low-temperature nitrogen gas refrigerant CNG due to the flow controls of the room temperature nitrogen gas NNG and the liquefied nitrogen vaporization gas LNG is stable.
  • the control of a pulsatile change of the flow is avoided, the pulsatile change of the flow resulting from a pulsatile change of temperature due to poor mixing, the control is stable.
  • the changed value can be suitably followed.
  • the cold energy of the liquefied nitrogen LN is used efficiently in order to produce the low-temperature nitrogen gas refrigerant CNG.
  • the intended temperature of the heat transfer medium HM can be set more suitably with the solidification point in mind. That is, in the second heat exchanger 22 , the intended temperature of the heat transfer medium HM can be set near to the solidification point without freezing the heat transfer medium HM.
  • the setting can prevent the heat transfer medium circulation route 21 from being blocked due to freezing and lower the loss of pressure in the route due to blocking, and thus excess heat is prevented from entering, thus saving power of the entire device.
  • the reaction vessel 31 can be more stably controlled at a low temperature and stable control is possible within a broad temperature range.
  • FIG. 3 shows a schematic diagram according to the third embodiment including the low-temperature gas supply device, the heat transfer medium-cooling device, and the low-temperature reaction control device of the present invention.
  • a low-temperature gas supply device 100 C includes a room temperature route 1 C, from an one end of which a room temperature nitrogen gas (GN 2 )NNG is introduced as a gas of higher temperature than a low-temperature-liquefied gas described below, a low-temperature route 2 C, from one end of which a liquefied nitrogen (LN 2 )LN (for example, ⁇ 196° C.) is introduced as the low-temperature-liquefied gas, a mixing route 3 C, in which a mixed gas and a low-temperature nitrogen gas refrigerant described below flows, an ejector (mixed device) 4 C, in which the room temperature nitrogen gas NNG introduced from the another end of the room temperature route 1 C and a gas (referred to as “liquefied nitrogen vaporization gas” hereinafter) LNG resulting from a vaporization of the liquefied nitrogen LN are mixed to produce the mixed gas CG, a first heat exchange
  • the low-temperature route 2 C and the mixing route 3 C run parallel to each other and are constructed so that the liquefied nitrogen LN and the mixed gas CG which flow through the respective routes are heat-exchanged with each other.
  • the low-temperature route 2 C and the mixing route 3 C are disposed so that the liquefied nitrogen LN and the mixed gas CG flow in the opposite direction to each other, i.e., so as to be an opposite flow.
  • a heat transfer medium-cooling device 200 C includes, in addition to the low-temperature gas supply device 100 C described above, a heat transfer medium circulation route 21 , in which a heat transfer medium HM is circulated, a second heat exchanger 22 , through which the mixing route 3 C and the heat transfer medium circulation route 21 running parallel to each other penetrate and which is disposed so that the low-temperature nitrogen gas refrigerant CNG and a heat transfer medium HM flowing through the respective routes are heat-exchanged with each other, a heat transfer medium circulation pump 23 in order to circulate the heat transfer medium HM in the heat transfer medium circulation route 21 , a second temperature detector 24 which detects a temperature of the heat transfer medium HM circulated in the heat transfer medium circulation route 21 , a second temperature adjusting device 25 which output a second control signal CS 2 based on the temperature detected by the second temperature detector 24 , and a reserve tank 27 in order to absorb an expansion or shrinkage associated with the temperature change of the heat transfer medium.
  • a low-temperature reaction control device 300 C according to the third embodiment is the same as the low-temperature reaction control device 300 A and 300 B according to the first and second embodiments, except that the heat transfer medium-cooling device 200 C constructed as above is included.
  • the liquefied nitrogen (LN 2 ) LN is introduced from one end of the low-temperature route 2 C and to the first heat exchanger 5 C.
  • the liquefied nitrogen LN becomes the liquefied nitrogen vaporization gas LNG by heat-exchange with the mixed gas CG flowing through the mixing route 3 C in the first heat exchanger 5 C.
  • the liquefied nitrogen vaporization gas LNG discharged from the first heat exchanger 5 C and the room temperature nitrogen gas NNG introduced form one end of the room temperature route 1 C are introduced to the ejector 4 C and mixed using the difference of pressures thereof.
  • the mixed gas CG discharged from the ejector 4 C is introduced to the first heat exchanger 5 C, is heat-exchanged with the liquefied nitrogen LN flowing through the low-temperature route 2 C, the temperature of CG being averaged due to an effect of a disturbed flow at the same time, and is discharged as the low-temperature nitrogen gas refrigerant CNG.
  • the first temperature detector 6 C detects a temperature of the low-temperature nitrogen gas refrigerant CNG flowing at the downstream of the mixing route 3 C below the first heat exchanger 5 C.
  • the first temperature adjusting device 7 C outputs a first control signal CS 1 according to the difference between the temperature detected by the first temperature detector 6 C and the designed temperature (intended temperature) of the low-temperature nitrogen gas refrigerant CNG.
  • the flow adjusting valve 8 C adjusts a flow of the room temperature nitrogen gas NNG flowing through the room temperature route 1 C based on the second control signal CS 2 output from the second temperature adjusting device 25 .
  • the flow adjusting valve 9 C adjusts a flow of the liquefied nitrogen vaporization gas LNG flowing at the downstream of the low-temperature route 2 C below the first heat exchanger 5 C, based on the first control signal CS 1 .
  • the flow of the liquefied nitrogen vaporization gas LNG introduced to the ejector 4 C may be adjusted at the first side of the first heat exchanger 5 C, when there is a construction so as to adjust the flow at the second side of the first heat exchanger 5 C in the above manner, i.e., the flow of the liquefied nitrogen vaporization gas LNG, i.e., the flow of the vaporization gas of a single phase, it is possible to adjust the flow more precisely, compared with the manner in which the flow is adjusted at the first side of the first heat exchanger 5 C, i.e., the flow of the heat exchanger LN with a phase-change is adjusted.
  • the low-temperature nitrogen gas refrigerant CNG discharged from the heat exchanger 5 C is supplied to the second heat exchanger 22 and cools the heat transfer medium HM flowing through the heat transfer medium circulation route 21 by heat-exchange.
  • the second temperature detector 24 detects the temperature of the heat transfer medium HM circulated in the heat transfer medium circulation route 21 .
  • the second temperature adjusting device 25 outputs the second control signal CS 2 according to the difference between the temperature detected by the second temperature detector 24 and the designed temperature (the intended temperature) of the heat transfer medium HM.
  • the heat transfer medium HM is adjusted to be the desired temperature.
  • the heat transfer medium HM adjusted to be the desired temperature is supplied to a jacket 31 a of the low-temperature reaction vessel 31 by action of the heat transfer medium circulation pump 23 .
  • the reaction liquid inside the reaction vessel is cooled and adjusted to be the constant temperature.
  • the liquefied nitrogen LN is translated to the liquefied nitrogen vaporization gas LNG of the similar temperature with the room temperature nitrogen gas NNG by using the first heat exchanger 5 C and they are mixed, the uniform mixture can be realized. Because the ejector 4 A is adopted for mixing, even if their pressures are different from each other, mixing can be realized easily and the device can be downsized compared with when the general mixer is used.
  • the liquefied nitrogen LN is translated to the liquefied nitrogen vaporization gas LNG of the similar temperature with the room temperature nitrogen gas NNG by using the first heat exchanger 5 C and they are mixed, a temperature control of the low-temperature nitrogen gas refrigerant CNG due to the flow control of the room temperature nitrogen gas NNG and the liquefied nitrogen vaporization gas LNG is stable.
  • the control of a pulsatile change of the flow is avoided, the pulsatile change of the flow resulting from a pulsatile change of temperature due to poor mixing, the control is stable.
  • the intended temperature of the low-temperature nitrogen gas refrigerant CNG is changed, the changed value can be suitably followed.
  • the cold energy of the liquefied nitrogen LN is used efficiently in order to produce the low-temperature nitrogen gas refrigerant CNG.
  • the intended temperature of the heat transfer medium HM can be set more suitably with the solidification point in mind. That is, in the second heat exchanger 22 , the intended temperature of the heat transfer medium HM can be set near to the solidification point without freezing the heat transfer medium HM.
  • the setting can prevent the heat transfer medium circulation route 21 from being blocked due to freezing and lower the loss of pressure in the route due to blocking, and thus excess heat is prevented from entering, thus saving power of the entire device.
  • the reaction vessel 31 can be more stably controlled at a low temperature and stable control is possible within a broad temperature range.
  • the first low-temperature gas supply device 100 A, the heat transfer medium-cooling device 200 A, and the low-temperature reaction control device 300 A according to the first embodiment as above, have a construction in which flows of the room temperature nitrogen gas NNG introduced to the room temperature route 1 A and the liquefied nitrogen vaporization gas LNG introduced to the low-temperature route 2 A are adjusted based on the temperature of the low-temperature nitrogen gas refrigerant CNG detected by the temperature detector 6 A, i.e., the temperature of the low-temperature nitrogen gas refrigerant CNG flowing at the downstream of the mixing route 3 A below the first heat exchanger 5 A.
  • the construction has advantages that, after the temperature of the low-temperature nitrogen gas refrigerant CNG detected by the temperature detector 6 A reaching within the designed range, the flow of the low-temperature nitrogen gas refrigerant CNG discharged from the heat exchanger 5 A is stable, not is variable.
  • the low-temperature reaction control device 300 A when the necessary cold energy for the heat transfer medium HM increases with increasing a load on the low-temperature reaction vessel 31 , there may be case where the flow of the low-temperature nitrogen gas refrigerant CNG needs to be increased in order to heat-exchanging with the heat transfer medium HM.
  • the low-temperature gas supply device 100 A, the heat transfer medium-cooling device 200 A, and the low-temperature reaction control device 300 A according to the first embodiment when the open level of the flow adjusting valve 26 is maximum, the flow of the low-temperature nitrogen gas refrigerant CNG becomes maximum.
  • the low-temperature gas supply device 100 C, the heat transfer medium-cooling device 200 C, and the low-temperature reaction control device 300 C have a construction which adjusts a flow of the room temperature nitrogen gas NNG as a based flow for increasing or decreasing the flow of the low-temperature nitrogen gas refrigerant CNG based on the temperature of the heat transfer medium HM detected by the temperature detector 24 , i.e., the temperature of the heat transfer medium HM flowing at the downstream of heat transfer medium circulation route 21 below the second heat exchanger 22 .
  • the flow of the low-temperature nitrogen gas refrigerant CNG discharged from the first heat exchanger 5 C can increase or decrease so as to be the designed value according to the temperature of the heat transfer medium HM. Therefore, in order to obtain a necessary cold energy for cooling the heat transfer medium HM, both of the temperature and flow in the low-temperature nitrogen gas refrigerant CNG are adjusted to realize more stable temperature control of the heat transfer medium HM.
  • the device can be downsizing and be low in cost.
  • FIG. 4 shows a schematic diagram according to the fourth embodiment including the low-temperature gas supply device, the heat transfer medium-cooling device, and the low-temperature reaction control device of the present invention.
  • a low-temperature gas supply device 100 D includes a room temperature route 1 D, from an one end of which a room temperature nitrogen gas (GN 2 )NNG is introduced, a low-temperature route 2 D, from an one end of which a liquefied nitrogen (LN 2 )LN (for example, ⁇ 196° C.) is introduced, a mixing route 3 D, in which a low-temperature nitrogen gas refrigerant described below flows, a first heat exchanger 5 D, in which the room temperature nitrogen gas NNG introduced from the room temperature route 1 D and the liquefied nitrogen LN introduced from the low-temperature route 2 D are heat-exchanged with each other to discharge each gas as an heat-exchanged nitrogen gas CNNG and a gas (referred to as “liquefied nitrogen vaporization gas” hereinafter) LNG resulting from a vaporization of the liquefied nitrogen LN, an ejector 4 D, in which the heat-exchanged
  • the room temperature route 1 D and the low-temperature route 2 D run parallel to each other and are constructed so that the room temperature nitrogen gas NNG and the liquefied nitrogen LN are heat-exchanged with each other.
  • the room temperature route 1 D and the low-temperature route 2 D are disposed so that the room temperature nitrogen gas NNG and the liquefied nitrogen LN flow in the same direction.
  • a heat transfer medium-cooling device 200 D includes, in addition to the low-temperature gas supply device 100 D as above, a heat transfer medium circulation route 21 , in which a heat transfer medium HM is circulated, a second heat exchanger 22 , through which the mixing route 3 D and the heat transfer medium circulation route 21 running parallel to each other penetrate and which is disposed so that the low-temperature nitrogen gas refrigerant CNG and a heat transfer medium HM flowing through the respective routes are heat-exchanged with each other, a heat transfer medium circulation pump 23 in order to circulate the heat transfer medium HM circulated in the heat transfer medium circulation route 21 , a second temperature detector 24 which detects a temperature of the heat transfer medium HM circulated in the heat transfer medium circulation route 21 , a second temperature adjusting device 25 which output a second control signal CS 2 based on the temperature detected by the second temperature detector 24 , and a reserve tank 27 in order to absorb an expansion or shrinkage associated with the temperature change of the heat transfer medium.
  • a low-temperature reaction control device 300 D according to the fourth embodiment is the same as the low-temperature reaction control devices 300 A, 300 B, and 300 C according to the first, second, and third embodiments, except that the heat transfer medium-cooling device 200 D constructed as above is included.
  • the room temperature nitrogen gas NNG is introduced from one end of the room temperature route 1 D to the first heat exchanger 5 D.
  • the liquefied nitrogen (LN 2 ) LN is introduced from one end of the low-temperature route 2 D to the first heat exchanger 5 D.
  • the first heat exchanger 5 D discharges the gases as a heat-exchanged nitrogen gas CNNG and a gas (referred to as “liquefied nitrogen vaporization gas” hereinafter) LNG resulting from a vaporization of the liquefied nitrogen LN, in which the difference of the temperatures thereof is reduced.
  • the ejector 4 D mixes the heat-exchanged nitrogen gas CNNG and the liquefied nitrogen vaporization gas LNG discharged from the first heat exchanger 5 D using the difference of the pressures thereof and produces the low-temperature nitrogen gas refrigerant CNG.
  • the first temperature detector 6 D detects a temperature of the low-temperature nitrogen gas refrigerant CNG flowing through the mixing route 3 D.
  • the temperature adjusting device 7 D outputs the first control signal CS 1 according to the difference between the temperature detected by the first temperature detector 6 D and the designed temperature (intended temperature) of the low-temperature nitrogen gas refrigerant CNG.
  • the flow adjusting valve 8 D adjusts a flow of the room temperature nitrogen gas NNG flowing at the upper stream of the room temperature route 1 D above the first heat exchanger 5 D based on the second control signal CS 2 output from the second temperature adjusting device 25 .
  • the first flow adjusting valve 9 D adjusts a flow of the liquefied nitrogen vaporization gas LNG flowing at the downstream of the low-temperature route 2 D below the first heat exchanger 5 D based on the first control signal CS 1 .
  • the flow of the vaporization gas LNG introduced to the ejector 4 D may be adjusted at the first side of the first heat exchanger 5 D, when there is a construction so as to adjust the flow at the second side of the first heat exchanger 5 D in the above manner, i.e., the flow of the liquefied nitrogen vaporization gas LNG, i.e., the flow of the vaporization gas of a single phase, it is possible to adjust the flow more precisely, compared with the manner in which the flow at the first side of the first heat exchanger 5 D, i.e., the flow of the heat exchanger LN with a phase-change, is adjusted.
  • the low-temperature nitrogen gas refrigerant CNG discharged from the ejector 4 D is supplied to the second heat exchanger 22 and cools the heat transfer medium HM flowing in the heat transfer medium circulation route 21 by heat-exchange.
  • the second temperature detector 24 detects a temperature of the heat transfer medium HM circulated in the heat transfer medium circulation route 21 .
  • the second temperature adjusting device 25 outputs the second control signal CS 2 according to the difference between the temperature detected by the second temperature detector 24 and the designed temperature of the heat transfer medium HM.
  • the low-temperature nitrogen gas refrigerant CNG and the heat transfer medium HM are adjusted to be a designed temperature.
  • the heat transfer medium HM adjusted to be the desired temperature is supplied to a jacket 31 a of the low-temperature reaction vessel 31 by action of the heat transfer medium circulation pump 23 .
  • the reaction liquid inside the reaction vessel is cooled and adjusted to be the constant temperature.
  • the uniform mixture can be realized. Because the ejector 4 D is adopted for mixing, even if their pressures are different from each other, mixing can be realized easily and the device can be downsized compared with when the general mixer is used.
  • the room temperature nitrogen gas NNG and the liquefied nitrogen LN are translated to the heat-exchanged nitrogen gas CNNG and the liquefied nitrogen vaporization gas LNG, in which the difference of the temperatures thereof is reduced by using the first heat exchanger 5 D, and they are mixed, a temperature control of the low-temperature nitrogen gas refrigerant CNG due to the flow controls of the room temperature nitrogen gas NNG and the liquefied nitrogen vaporization gas LNG is stable.
  • the control of a pulsatile change of the flow is avoided, the pulsatile change of the flow resulting from a pulsatile change of temperature due to poor mixing, the control is stable.
  • the changed value can be suitably followed.
  • the cold energy of the liquefied nitrogen LN is used efficiently in order to produce the low-temperature nitrogen gas refrigerant CNG.
  • the intended temperature of the heat transfer medium HM can be set more suitably with the solidification point in mind. That is, in the second heat exchanger 22 , the intended temperature of the heat transfer medium HM can be set near to the solidification point without freezing the heat transfer medium HM.
  • the setting can prevent the heat transfer medium circulation route 21 from being blocked due to freezing and lower the loss of pressure in the route due to blocking, and thus excess heat is prevented from entering, thus saving power of the entire device.
  • the reaction vessel 31 can be more stably controlled at a low temperature and stable control is possible within a broad temperature range.
  • the low-temperature gas supply device 100 B, the heat transfer medium-cooling device 200 B, and the low-temperature reaction control device 300 B according to the second embodiment as above, have a construction in which flows of the room temperature nitrogen gas NNG introduced to the room temperature route 1 B and the liquefied nitrogen vaporization gas LNG introduced to the low-temperature route 2 B are adjusted based on the temperature of the low-temperature nitrogen gas refrigerant CNG detected by the temperature detector 6 B, i.e., the temperature of low-temperature nitrogen gas refrigerant CNG flowing at the downstream of the mixing route 3 B below the ejector 4 B.
  • the construction has advantages that, after the temperature of the low-temperature nitrogen gas refrigerant CNG detected by the temperature detector 6 B reaching within the designed range, the flow of the low-temperature nitrogen gas refrigerant CNG discharged from the ejector 4 B is stable, not is variable.
  • the low-temperature reaction control device 300 B when the necessary cold energy for the heat transfer medium HM increases with increasing a load on the low-temperature reaction vessel 31 , there may be case where the flow of the low-temperature nitrogen gas refrigerant CNG needs to be increased in order to heat-exchanging with the heat transfer medium HM.
  • the low-temperature gas supply device 100 B, the heat transfer medium-cooling device 200 B, and the low-temperature reaction control device 300 B according to the second embodiment when the open level of the flow adjusting valve 26 is maximum, the flow of the low-temperature nitrogen gas refrigerant CNG becomes maximum.
  • the low-temperature gas supply device 100 D, the heat transfer medium-cooling device 200 D, and the low-temperature reaction control device 300 D have a construction which adjusts a flow of the room temperature nitrogen gas NNG as a based flow for increasing or decreasing the flow of the low-temperature nitrogen gas refrigerant CNG, based on the temperature of the heat transfer medium HM detected by the temperature detector 24 , i.e., the temperature of 1 the heat transfer medium HM flowing at the downstream of the heat transfer medium circulation route 21 below the second heat exchanger 22 .
  • the flow of the low-temperature nitrogen gas refrigerant CNG discharged from the ejector 4 D can increase or decrease so as to be the designed value according to the temperature of the heat transfer medium HM. Therefore, in order to obtain a necessary cold energy for cooling the heat transfer medium HM, both of the temperature and flow in the low-temperature nitrogen gas refrigerant CNG are adjusted to realize more stable temperature control of the heat transfer medium HM.
  • the device can be downsizing and be low in cost.
  • the low-temperature gas supply devices 100 A- 100 D as above according to the first to fourth embodiments can adopt the following device in addition to the heat transfer medium-cooling devices 200 A to 200 D.
  • a reaction vessel saving a reaction liquid includes a jacket around the reaction vessel or a heat exchanger disposed in the reaction vessel, they can adopt a low-temperature reaction control device which supplies the low-temperature gas to the jacket or the heat exchanger, and thus the reaction liquid can be cooled without freezing at a heat-transfer surface by supplying a preliminary adjusted low-temperature gas.
  • ⁇ can adopt a cold trap which cools, condenses, or solidifies vapor using a coiled tube or other heat exchangers, wherein the vapor is condensed or solidified in uniformly temperature with accuracy by passing the preliminary adjusted low-temperature gas through the inside of the heat exchanger.
  • a flow adjusting valve is shown, but it is not limited to those and can adopt other means for adjusting as appropriate, for example, a massflow controller.
  • the second heat exchanger 22 for example, a double-pipe heat exchanger, plate heat exchanger, plate fin type heat exchanger, shell & tube heat exchanger, and tank & coil heat exchanger can be adopted.
  • a plate heat exchanger is desirable. It is because it is high efficient and contributes the device downsizing.
  • a high efficient heat exchanger such as plate-type is desirable. It is because the temperature difference at the ends becomes small to make mixing easier and the device can be downsizing.
  • a room temperature nitrogen gas NNG and a liquefied nitrogen LN are adopted, they are not necessarily same kind and the different kinds of gases may be mixed.
  • the intended gas in addition to nitrogen, fluorine-based refrigerants such as oxygen, argon, carbon dioxide gas, LNG, hydrofluorocarbons, and chlorofluorocarbons can be used.
  • a gas can be mixed with the low-temperature-liquefied gas, the gas applying any temperature, not only room temperature.
  • a low-temperature gas supply device, heat transfer medium-cooling device, and low-temperature reaction control device can be used for temperature control in a chemical reaction such as organic synthesis or a crystallization reaction.

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  • Combustion & Propulsion (AREA)
  • Filling Or Discharging Of Gas Storage Vessels (AREA)
US14/345,523 2011-10-11 2012-10-11 Low-temperature gas supply device, heat transfer medium-cooling device, and low-temperature reaction control device Abandoned US20140366575A1 (en)

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PCT/JP2012/076315 WO2013054844A1 (ja) 2011-10-11 2012-10-11 低温ガス供給装置、熱媒冷却装置、及び低温反応制御装置

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SG11201400732RA (en) 2014-09-26
CN103874898A (zh) 2014-06-18

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