WO2013190842A1 - Cooling method and cooling device - Google Patents
Cooling method and cooling device Download PDFInfo
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- WO2013190842A1 WO2013190842A1 PCT/JP2013/003845 JP2013003845W WO2013190842A1 WO 2013190842 A1 WO2013190842 A1 WO 2013190842A1 JP 2013003845 W JP2013003845 W JP 2013003845W WO 2013190842 A1 WO2013190842 A1 WO 2013190842A1
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- heat medium
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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
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- the present invention relates to a heat medium cooling method and a heat medium cooling apparatus. More specifically, the present invention relates to a cooling method and a cooling apparatus that use a small amount of liquid nitrogen required for cooling a heat medium and reduce the loss of the heat medium due to entrainment.
- a low temperature reaction apparatus is known as an apparatus for performing a chemical reaction at a low temperature.
- Patent Document 1 arranges a coiled pipe in the tank, allows liquid nitrogen to flow through the pipe, and cools the reaction liquid through the pipe.
- An apparatus that can be used is disclosed.
- patent document 2 is disclosing the apparatus which flows a heat medium to the jacket attached to the tank wall surface, and cools a reaction liquid via a wall surface. In the apparatus of Patent Document 2, heat exchange is performed between the liquid nitrogen and the heat medium in the heat exchanger to cool the heat medium.
- the method of cooling the reaction liquid with liquid nitrogen via a pipe tends to increase the amount of liquid nitrogen used. Further, when liquid nitrogen is directly introduced into the reaction solution, impurities are likely to be mixed into the reaction solution. On the other hand, as in the apparatus described in Patent Document 2, the method of cooling the reaction liquid with a heat medium cooled with liquid nitrogen easily prevents impurities from being mixed and shortens the rise time. However, the cooling of the heat medium with liquid nitrogen in the heat exchanger is performed using the latent heat of liquid nitrogen, and since sensible heat is not used, the utilization efficiency of liquid nitrogen is low and the consumption of liquid nitrogen tends to increase. .
- An object of the present invention is to provide a heat medium cooling method and a heat medium cooling apparatus that use less liquid nitrogen required for cooling the heat medium.
- the present inventor tried a method of cooling by directly introducing liquid nitrogen into the heat medium.
- the heat medium was discharged to the outside accompanying the nitrogen exhaust gas, resulting in a significant loss of the heat medium. Therefore, the inventor has further studied and completed the invention of the following aspect.
- [4] Means for exchanging heat between the heat medium and liquid nitrogen through a partition, Means for supplying liquid nitrogen to a region on the heat medium side in the heat exchange means; Means for supplying liquid nitrogen to an area on the liquid nitrogen side in the heat exchange means; Heat medium cooling having means for adjusting the amount of liquid nitrogen supplied to the region on the heat medium side in the heat exchange means, and means for adjusting the amount of liquid nitrogen supplied to the region on the liquid nitrogen side in the heat exchange means apparatus.
- [5] means for measuring the temperature of the heat medium; Means for adjusting the amount of liquid nitrogen supplied to the region on the heat medium side and / or means for adjusting the amount of liquid nitrogen supplied to the region on the liquid nitrogen side based on the measured temperature value; 4].
- the heat medium cooling device according to [4] or [5], which is used for adjusting the temperature of the heat medium for the low temperature reactor.
- the heat medium cooling method and the heat medium cooling apparatus of the present invention require a small amount of liquid nitrogen used for cooling the heat medium. Moreover, since there is little heat medium accompanying nitrogen exhaust gas, there is almost no loss of the heat medium.
- the cooling method and heating medium cooling apparatus of the present invention are suitable for cooling a heating medium for a low-temperature chemical reaction system.
- FIG. 1 It is a conceptual diagram which shows the low-temperature chemical reaction system provided with the thermal-medium cooling device which concerns on one Embodiment of this invention. It is a figure which shows the weight change of the heat carrier in Example 1, the temperature change of a heat carrier, and the cumulative consumption weight of liquid nitrogen. It is a figure which shows the temperature change of the thermal medium in Example 1, the temperature change of a container gaseous phase, and the temperature change of a coil exit. It is a figure which shows the weight change of the heat carrier in Example 2, the temperature change of a heat carrier, and the cumulative consumption weight of liquid nitrogen. It is a figure which shows the temperature change of the thermal medium in Example 2, the temperature change of a container gaseous phase, and the temperature change of a coil exit.
- a heat medium cooling device according to an embodiment of the present invention will be described with reference to FIG.
- this invention is not limited by this embodiment,
- transformation, addition, or abbreviation is included in the range suitable for the meaning and objective of this invention.
- the apparatus shown in FIG. 1 has a heat medium cooling device 1, a liquid nitrogen container 11, and a low-temperature reactor 12.
- a jacket 13 is installed in the low temperature reactor 12.
- the heat medium enters the jacket 13 from the heat medium cooling device 1 through the tube 15 and returns from the jacket 13 through the tube 14 to the heat medium cooling device 1.
- the jacket is installed in the low-temperature reactor, but it is not limited to this as long as it is a means (for example, a coiled tube, a multiple tube, etc.) that can adjust the temperature in the reactor with a heat medium.
- the liquid nitrogen container 11 is a container that can store liquid nitrogen, and can supply liquid nitrogen from the liquid nitrogen container 11 to the heat medium cooling device 1.
- the heat medium used in the present invention is not particularly limited as long as it can be used as a heat medium in a heat exchanger such as a jacket, a coiled tube, or a multiple tube.
- a heat exchanger such as a jacket, a coiled tube, or a multiple tube.
- ethylene glycol, acetone, methylene chloride, methanol, ethanol, or an aqueous solution thereof can be used. It is necessary to select a heat medium that does not freeze in the operating temperature range.
- the heat medium has a freezing point that is preferably 10 ° C. or more lower than the lower limit of the use temperature.
- the heat medium suitably used in the present invention has a freezing point of less than ⁇ 80 ° C.
- the heat medium cooling device 1 includes a heat medium container 2 for storing the heat medium, and a coil tube 3 for introducing liquid nitrogen from the liquid nitrogen container 11 and exchanging heat with the heat medium.
- Liquid nitrogen is present inside the coil tube 3, and a heat medium is present outside the coil tube 3, and heat exchange is performed between the two through the tube wall of the coil tube 3.
- the amount of liquid nitrogen supplied to the coil tube 3 is adjusted by a valve 7.
- the supply amount to the coiled tube 3 is not particularly limited, it is preferable to adjust according to the temperature of the heat medium to be measured.
- the liquid nitrogen introduced into the coil tube 3 is preferably completely vaporized during the heat exchange.
- a jacket can be provided around the heat medium container. Liquid nitrogen may be introduced into the jacket, and heat exchange may be performed between the liquid nitrogen and the heat medium via the container wall.
- the heat medium cooling device 1 is provided with a pipe 4 for directly introducing liquid nitrogen from the liquid nitrogen container 11 into the heat medium.
- the liquid nitrogen introduced by the tube 4 is in direct contact with the heat medium, and heat exchange is performed between them.
- the nitrogen subjected to the heat exchange is discharged from the vent at the top of the heat medium container.
- the amount of liquid nitrogen supplied to the tube 4 is adjusted by a valve 6.
- the supply amount to the pipe 4 is not particularly limited, it is preferably adjusted according to the temperature of the heat medium to be measured.
- the heat medium cooling device 1 has a stirring function so that liquid nitrogen introduced directly from the pipe 4 to the heat medium does not remain in the heat medium container 2 in a liquid state.
- the shape of the opening of the tube 4 in the heat medium is not particularly limited, but it is preferable that the opening has a large diameter so that the heat medium does not freeze and block the opening. For example, it can be a trumpet-shaped opening.
- the heat medium cooling device 1 preferably has means (not shown) for measuring the temperature of the heat medium, the temperature of the gas phase portion of the heat medium container 2, and the temperature of the nitrogen exhaust gas from the tube 3. Furthermore, the heat medium cooling device 1 may have means for controlling the means 6 and 7 for adjusting the amount of liquid nitrogen introduced into the pipe 4 and the pipe 3 according to the measured temperature value. preferable.
- liquid nitrogen may be supplied to both the tube 4 and the tube 3 at the same time, or only one of the tube 4 and the tube 3 may be supplied.
- the temperature of the heat medium when the temperature of the heat medium is equal to or higher than the set temperature, it is preferable to supply liquid nitrogen to the coil tube 3 and exchange heat between the heat medium and liquid nitrogen via a partition. Even when the temperature of the heat medium is equal to or higher than the set temperature, a smaller amount of liquid nitrogen than that supplied to the coiled tube 3 is supplied to the tube 4 within a range that does not impair the effects of the present invention. And may be directly contacted to exchange heat.
- the temperature of the heat medium when the temperature of the heat medium is lower than the set temperature, it is preferable to supply liquid nitrogen to the pipe 4 and exchange heat by directly contacting the heat medium and liquid nitrogen. Even when the temperature of the heat medium is lower than the set temperature, the amount of liquid nitrogen smaller than the amount supplied to the tube 4 is supplied to the coil tube 3 within a range that does not impair the effects of the present invention.
- Heat exchange may be performed with nitrogen through a partition. When heat exchange is performed through the partition when the temperature of the heat medium is equal to or higher than the set temperature, loss of the heat medium due to nitrogen entrainment can be eliminated. On the other hand, when the temperature of the heat medium is lower than the set temperature, it is possible to utilize the sensible heat of liquid nitrogen by directly contacting and performing heat exchange.
- the set temperature is preferably any one of temperatures in the range of ⁇ 60 to + 20 ° C.
- the heating medium is ethanol
- the set temperature is preferably any one temperature in the range of ⁇ 40 to ⁇ 10 ° C., more preferably any one temperature in the range of ⁇ 30 to ⁇ 15 ° C. .
- the heat medium cooling device of the present invention can further include means for separating the heat medium from the released nitrogen and means for recovering the vaporized heat medium.
- the apparatus of the present invention can further be provided with a means for recovering the used nitrogen, and can be provided with a means for using the recovered nitrogen as a replacement gas for the reactor.
- Example 1 As shown in FIG. 1, a coil tube 3 having a diameter of 10 mm and a blowing tube 4 having a diameter of 10 mm were attached to the heat medium container 2. One end of the coil tube 3 was installed outside the heat medium container, and the other end was connected to the liquid nitrogen container 11 via the flow rate control valve 7. One end of the blowing pipe 4 was installed in the heat medium container 2, and the other end was connected to the liquid nitrogen container 11 via the flow rate control valve 6. A temperature measuring device was installed at a position immersed in the heat medium, immediately above the liquid surface of the heat medium and in the vicinity of the coil outlet, and the temperature of the heat medium, the temperature of the gas phase of the heat medium container, and the exhaust gas temperature at the coil tube outlet were measured.
- a heat medium 6.02 kg of ethanol (99.5%) was placed in a heat medium container and stirred with a stirrer.
- the liquid nitrogen container and the heat medium container were placed on a platform scale, and the consumption of liquid nitrogen and the change in the weight of the heat medium were measured.
- the heat medium temperature at the start of cooling was 12 ° C.
- the valve 7 was opened and liquid nitrogen was supplied to the coil tube 3 at a flow rate of 6.48 kg / hr.
- the valve 7 was closed and the valve 6 was opened at the same time, and liquid nitrogen was supplied to the blowing pipe 4 at a flow rate of 7.13 kg / hr.
- FIG. 2 and 3 show changes in the weight and temperature of the heat medium, the cumulative consumption weight of liquid nitrogen, the temperature change in the container gas phase, and the temperature change at the coil outlet.
- an upward arrow indicates switching from the coil tube 3 to the blowout tube 4.
- the cumulative consumption of liquid nitrogen was about 6.85 kg, and it could be cooled to -66 ° C. There was almost no loss of the heat medium within the measurement error.
- the coil outlet temperature is lower than the heat medium temperature during the period of heat exchange through the coil tube, and that latent heat is mainly used for cooling and sensible heat is not used much.
- FIG. 3 shows that during the period in which liquid nitrogen is directly introduced, the gas phase temperature of the container is almost the same as the heat medium temperature, and the sensible heat of liquid nitrogen is effectively used for cooling.
- Example 2 The heat medium was cooled by the same method as in Example 1 except that the operating conditions shown in Table 1 were changed.
- 4 and 5 show changes in the weight and temperature of the heat medium, the accumulated consumption weight of liquid nitrogen, the temperature change in the container gas phase, and the temperature change at the coil outlet.
- an upward arrow indicates switching from the coiled tube 3 to the outlet tube 4.
- the cumulative consumption of liquid nitrogen was about 6.98 kg, and it could be cooled to -56 ° C. There was almost no loss of the heat medium within the measurement error. From FIG. 5, it can be seen that the coil exit temperature is lower than the heat medium temperature during the period of heat exchange through the coil tube, and latent heat is mainly used for cooling and sensible heat is not used much. . Further, it can be seen from FIG. 5 that during the period in which liquid nitrogen is directly introduced, the gas phase temperature of the container is almost the same as the heat medium temperature, and the sensible heat of liquid nitrogen is effectively used for cooling.
- Example 1 The heat medium was cooled by the same method as in Example 1 except that the operating conditions shown in Table 1 were changed. 6 and 7 show the weight and temperature change of the heat medium, the cumulative consumption weight of liquid nitrogen, the temperature change of the container gas phase, and the temperature change of the coil outlet.
- the cumulative consumption of liquid nitrogen was about 5.45 kg, and it could be cooled to -55 ° C.
- the heat medium was greatly lost accompanying the nitrogen exhaust gas. From FIG. 7, it can be seen that during the period in which liquid nitrogen is directly introduced, the gas phase temperature of the container is substantially the same as the heat medium temperature, and the sensible heat of liquid nitrogen is effectively used for cooling.
- Example 2 The heat medium was cooled by the same method as in Example 1 except that the operating conditions shown in Table 1 were changed. 8 and 9 show the weight and temperature change of the heat medium, the cumulative consumption weight of liquid nitrogen, the temperature change of the container gas phase, and the temperature change of the coil outlet.
- the cumulative consumption of liquid nitrogen was about 7.37 kg for cooling to ⁇ 56 ° C.
- the cumulative consumption of liquid nitrogen was about 9.49 kg for cooling to ⁇ 66 ° C.
- the cooling rate decreased as the temperature of the heat medium decreased.
- the coil outlet temperature became a temperature near the boiling point of liquid nitrogen. From FIG. 9, it is understood that the coil outlet temperature is lower than the heat medium temperature during the period of heat exchange through the coil tube, and that latent heat is mainly used for cooling and sensible heat is not used much. .
Abstract
A heat medium cooling device is provided with: a means for exchanging heat between a heat medium and liquid nitrogen through a partition; a means for supplying liquid nitrogen to the heat medium-side region of the heat exchange means; a means for supplying liquid nitrogen to the liquid nitrogen-side region of the heat exchange means; a means for adjusting the amount of the liquid nitrogen supplied to the heat medium-side region of the heat exchange means; and a means for adjusting the amount of the liquid nitrogen supplied to the liquid nitrogen-side region of the heat exchange means.
Description
本発明は、熱媒体の冷却方法および熱媒体冷却装置に関する。より詳細には、本発明は、熱媒体の冷却に要する液体窒素の使用量が少なく、かつ同伴による熱媒体の損失が少ない、冷却方法および冷却装置に関する。
The present invention relates to a heat medium cooling method and a heat medium cooling apparatus. More specifically, the present invention relates to a cooling method and a cooling apparatus that use a small amount of liquid nitrogen required for cooling a heat medium and reduce the loss of the heat medium due to entrainment.
化学反応を低温で行うための装置として低温反応装置が知られている。低温反応装置内の反応液を冷却するために、例えば、特許文献１は、槽内にコイル状の配管を配置して、その管に液体窒素を流し、反応液を配管を介して冷却することができる装置を開示している。また、液体窒素を反応液に直接導入して反応液を冷却するという方法も知られている。
さらに、特許文献２は、槽壁面に取り付けたジャケットに熱媒体を流して壁面を介して反応液を冷却する装置を開示している。特許文献２の装置においては熱交換器において液体窒素と熱媒体との間で熱交換し熱媒体を冷却している。 A low temperature reaction apparatus is known as an apparatus for performing a chemical reaction at a low temperature. In order to cool the reaction liquid in the low-temperature reaction apparatus, for example,Patent Document 1 arranges a coiled pipe in the tank, allows liquid nitrogen to flow through the pipe, and cools the reaction liquid through the pipe. An apparatus that can be used is disclosed. Also known is a method in which liquid nitrogen is directly introduced into the reaction solution to cool the reaction solution.
Furthermore,patent document 2 is disclosing the apparatus which flows a heat medium to the jacket attached to the tank wall surface, and cools a reaction liquid via a wall surface. In the apparatus of Patent Document 2, heat exchange is performed between the liquid nitrogen and the heat medium in the heat exchanger to cool the heat medium.
さらに、特許文献２は、槽壁面に取り付けたジャケットに熱媒体を流して壁面を介して反応液を冷却する装置を開示している。特許文献２の装置においては熱交換器において液体窒素と熱媒体との間で熱交換し熱媒体を冷却している。 A low temperature reaction apparatus is known as an apparatus for performing a chemical reaction at a low temperature. In order to cool the reaction liquid in the low-temperature reaction apparatus, for example,
Furthermore,
特許文献１に記載の装置のように、反応液を液体窒素で配管を介して冷却する方法は、液体窒素の使用量が増える傾向がある。また、液体窒素を反応液に直接導入すると反応液への不純物混入などが生じ易い。
一方、特許文献２に記載の装置のように、液体窒素で冷却された熱媒体によって反応液を冷却する方法は、不純物混入の防止、立上時間の短縮などが実現しやすい。
ところが、熱交換器における液体窒素による熱媒体の冷却は、液体窒素の潜熱を利用して行われ、顕熱が利用されないので、液体窒素の利用効率が低く、液体窒素の消費量が多くなり易い。
本発明の課題は、熱媒体の冷却に要する液体窒素の使用量が少ない、熱媒体の冷却方法および熱媒体冷却装置を提供することである。 As in the apparatus described inPatent Document 1, the method of cooling the reaction liquid with liquid nitrogen via a pipe tends to increase the amount of liquid nitrogen used. Further, when liquid nitrogen is directly introduced into the reaction solution, impurities are likely to be mixed into the reaction solution.
On the other hand, as in the apparatus described inPatent Document 2, the method of cooling the reaction liquid with a heat medium cooled with liquid nitrogen easily prevents impurities from being mixed and shortens the rise time.
However, the cooling of the heat medium with liquid nitrogen in the heat exchanger is performed using the latent heat of liquid nitrogen, and since sensible heat is not used, the utilization efficiency of liquid nitrogen is low and the consumption of liquid nitrogen tends to increase. .
An object of the present invention is to provide a heat medium cooling method and a heat medium cooling apparatus that use less liquid nitrogen required for cooling the heat medium.
一方、特許文献２に記載の装置のように、液体窒素で冷却された熱媒体によって反応液を冷却する方法は、不純物混入の防止、立上時間の短縮などが実現しやすい。
ところが、熱交換器における液体窒素による熱媒体の冷却は、液体窒素の潜熱を利用して行われ、顕熱が利用されないので、液体窒素の利用効率が低く、液体窒素の消費量が多くなり易い。
本発明の課題は、熱媒体の冷却に要する液体窒素の使用量が少ない、熱媒体の冷却方法および熱媒体冷却装置を提供することである。 As in the apparatus described in
On the other hand, as in the apparatus described in
However, the cooling of the heat medium with liquid nitrogen in the heat exchanger is performed using the latent heat of liquid nitrogen, and since sensible heat is not used, the utilization efficiency of liquid nitrogen is low and the consumption of liquid nitrogen tends to increase. .
An object of the present invention is to provide a heat medium cooling method and a heat medium cooling apparatus that use less liquid nitrogen required for cooling the heat medium.
本発明者は、上記目的を達成するために、熱媒体に液体窒素を直接導入して冷却する方法を試みた。ところが、窒素排ガスに同伴して熱媒体が外部に排出され熱媒体を大幅に損失する結果となった。そこで、本発明者はさらに検討を重ねることによって以下の態様の発明を完成するに至った。
In order to achieve the above object, the present inventor tried a method of cooling by directly introducing liquid nitrogen into the heat medium. However, the heat medium was discharged to the outside accompanying the nitrogen exhaust gas, resulting in a significant loss of the heat medium. Therefore, the inventor has further studied and completed the invention of the following aspect.
〔１〕 熱媒体と液体窒素との間で仕切りを介して熱交換する工程と
熱媒体と液体窒素との間で直接に接触させて熱交換する工程とを、同時にまたは順不同に行うことを含む熱媒体の冷却方法。
〔２〕 熱媒体の温度が設定温度以上の場合は熱媒体と液体窒素との間で仕切りを介して熱交換する工程を行い、熱媒体の温度が設定温度未満の場合は熱媒体と液体窒素との間で直接に接触させて熱交換する工程を行う、〔１〕に記載の熱媒体の冷却方法。
〔３〕 設定温度が、－６０～＋２０℃の範囲のいずれか一つの温度である、〔２〕に記載の熱媒体の冷却方法。 [1] The step of performing heat exchange between the heat medium and liquid nitrogen through a partition and the step of directly exchanging heat between the heat medium and liquid nitrogen are performed simultaneously or in random order. Cooling method of heat medium.
[2] When the temperature of the heat medium is equal to or higher than the set temperature, a process of exchanging heat is performed between the heat medium and the liquid nitrogen via a partition. When the temperature of the heat medium is lower than the set temperature, the heat medium and the liquid nitrogen The method for cooling a heat medium according to [1], wherein a step of directly contacting and exchanging heat is performed.
[3] The heat medium cooling method according to [2], wherein the set temperature is any one of a range of −60 to + 20 ° C.
熱媒体と液体窒素との間で直接に接触させて熱交換する工程とを、同時にまたは順不同に行うことを含む熱媒体の冷却方法。
〔２〕 熱媒体の温度が設定温度以上の場合は熱媒体と液体窒素との間で仕切りを介して熱交換する工程を行い、熱媒体の温度が設定温度未満の場合は熱媒体と液体窒素との間で直接に接触させて熱交換する工程を行う、〔１〕に記載の熱媒体の冷却方法。
〔３〕 設定温度が、－６０～＋２０℃の範囲のいずれか一つの温度である、〔２〕に記載の熱媒体の冷却方法。 [1] The step of performing heat exchange between the heat medium and liquid nitrogen through a partition and the step of directly exchanging heat between the heat medium and liquid nitrogen are performed simultaneously or in random order. Cooling method of heat medium.
[2] When the temperature of the heat medium is equal to or higher than the set temperature, a process of exchanging heat is performed between the heat medium and the liquid nitrogen via a partition. When the temperature of the heat medium is lower than the set temperature, the heat medium and the liquid nitrogen The method for cooling a heat medium according to [1], wherein a step of directly contacting and exchanging heat is performed.
[3] The heat medium cooling method according to [2], wherein the set temperature is any one of a range of −60 to + 20 ° C.
〔４〕 熱媒体と液体窒素との間で仕切りを介して熱交換するための手段、
該熱交換手段における熱媒体側の領域に液体窒素を供給するための手段、
前記熱交換手段における液体窒素側の領域に液体窒素を供給するための手段、
前記熱交換手段における熱媒体側の領域に供給する液体窒素の量を調節する手段、および
前記熱交換手段における液体窒素側の領域に供給する液体窒素の量を調節する手段を有する、熱媒体冷却装置。
〔５〕 熱媒体の温度を測定する手段と、
測定温度値に基づいて熱媒体側の領域に供給する液体窒素の量を調節する手段および／または液体窒素側の領域に供給する液体窒素の量を調節する手段を制御する手段をさらに有する、〔４〕に記載の熱媒体冷却装置。
〔６〕 低温反応装置用熱媒体の温度調節に用いる、〔４〕または〔５〕に記載の熱媒体冷却装置。 [4] Means for exchanging heat between the heat medium and liquid nitrogen through a partition,
Means for supplying liquid nitrogen to a region on the heat medium side in the heat exchange means;
Means for supplying liquid nitrogen to an area on the liquid nitrogen side in the heat exchange means;
Heat medium cooling having means for adjusting the amount of liquid nitrogen supplied to the region on the heat medium side in the heat exchange means, and means for adjusting the amount of liquid nitrogen supplied to the region on the liquid nitrogen side in the heat exchange means apparatus.
[5] means for measuring the temperature of the heat medium;
Means for adjusting the amount of liquid nitrogen supplied to the region on the heat medium side and / or means for adjusting the amount of liquid nitrogen supplied to the region on the liquid nitrogen side based on the measured temperature value; 4].
[6] The heat medium cooling device according to [4] or [5], which is used for adjusting the temperature of the heat medium for the low temperature reactor.
該熱交換手段における熱媒体側の領域に液体窒素を供給するための手段、
前記熱交換手段における液体窒素側の領域に液体窒素を供給するための手段、
前記熱交換手段における熱媒体側の領域に供給する液体窒素の量を調節する手段、および
前記熱交換手段における液体窒素側の領域に供給する液体窒素の量を調節する手段を有する、熱媒体冷却装置。
〔５〕 熱媒体の温度を測定する手段と、
測定温度値に基づいて熱媒体側の領域に供給する液体窒素の量を調節する手段および／または液体窒素側の領域に供給する液体窒素の量を調節する手段を制御する手段をさらに有する、〔４〕に記載の熱媒体冷却装置。
〔６〕 低温反応装置用熱媒体の温度調節に用いる、〔４〕または〔５〕に記載の熱媒体冷却装置。 [4] Means for exchanging heat between the heat medium and liquid nitrogen through a partition,
Means for supplying liquid nitrogen to a region on the heat medium side in the heat exchange means;
Means for supplying liquid nitrogen to an area on the liquid nitrogen side in the heat exchange means;
Heat medium cooling having means for adjusting the amount of liquid nitrogen supplied to the region on the heat medium side in the heat exchange means, and means for adjusting the amount of liquid nitrogen supplied to the region on the liquid nitrogen side in the heat exchange means apparatus.
[5] means for measuring the temperature of the heat medium;
Means for adjusting the amount of liquid nitrogen supplied to the region on the heat medium side and / or means for adjusting the amount of liquid nitrogen supplied to the region on the liquid nitrogen side based on the measured temperature value; 4].
[6] The heat medium cooling device according to [4] or [5], which is used for adjusting the temperature of the heat medium for the low temperature reactor.
本発明の熱媒体の冷却方法および熱媒体冷却装置は、熱媒体の冷却に要する液体窒素の使用量が少ない。しかも、窒素排ガスに同伴する熱媒体が少ないので熱媒体の損失がほとんどない。
本発明の熱媒体の冷却方法および熱媒体冷却装置は、低温化学反応システム用の熱媒体の冷却に好適である。 The heat medium cooling method and the heat medium cooling apparatus of the present invention require a small amount of liquid nitrogen used for cooling the heat medium. Moreover, since there is little heat medium accompanying nitrogen exhaust gas, there is almost no loss of the heat medium.
The cooling method and heating medium cooling apparatus of the present invention are suitable for cooling a heating medium for a low-temperature chemical reaction system.
本発明の熱媒体の冷却方法および熱媒体冷却装置は、低温化学反応システム用の熱媒体の冷却に好適である。 The heat medium cooling method and the heat medium cooling apparatus of the present invention require a small amount of liquid nitrogen used for cooling the heat medium. Moreover, since there is little heat medium accompanying nitrogen exhaust gas, there is almost no loss of the heat medium.
The cooling method and heating medium cooling apparatus of the present invention are suitable for cooling a heating medium for a low-temperature chemical reaction system.
本発明の一実施形態に係る熱媒体冷却装置を、図１を参照しながら説明する。なお、本発明は、該実施形態によって限定されるものではなく、本発明の趣旨及び目的に適う範囲で、変形、追加、又は省略したものも包含する。
A heat medium cooling device according to an embodiment of the present invention will be described with reference to FIG. In addition, this invention is not limited by this embodiment, The deformation | transformation, addition, or abbreviation is included in the range suitable for the meaning and objective of this invention.
図１に示す装置は、熱媒体冷却装置１、液体窒素容器１１、および低温反応器１２を有する。低温反応器１２にはジャケット１３が設置されている。熱媒体は熱媒体冷却装置１から管１５を通ってジャケット１３に入り、そしてジャケット１３から管１４を通って熱媒体冷却装置１に戻る。図１に示す装置では低温反応器にジャケットが設置されているが、反応器内の温度を熱媒体によって調節することができる手段（例えば、コイル管、多重管など）であればこれに限定されない。液体窒素容器１１は液体窒素を貯蔵できる容器であり、液体窒素容器１１から液体窒素を熱媒体冷却装置１に供給することができる。
The apparatus shown in FIG. 1 has a heat medium cooling device 1, a liquid nitrogen container 11, and a low-temperature reactor 12. A jacket 13 is installed in the low temperature reactor 12. The heat medium enters the jacket 13 from the heat medium cooling device 1 through the tube 15 and returns from the jacket 13 through the tube 14 to the heat medium cooling device 1. In the apparatus shown in FIG. 1, the jacket is installed in the low-temperature reactor, but it is not limited to this as long as it is a means (for example, a coiled tube, a multiple tube, etc.) that can adjust the temperature in the reactor with a heat medium. . The liquid nitrogen container 11 is a container that can store liquid nitrogen, and can supply liquid nitrogen from the liquid nitrogen container 11 to the heat medium cooling device 1.
本発明に用いられる熱媒体は、ジャケット、コイル管、多重管などの熱交換器における熱媒体として用いることができるものであれば、特に限定されない。例えば、エチレングリコール、アセトン、塩化メチレン、メタノール、エタノールまたはこれらの水溶液などが挙げられる。熱媒体としては、使用温度範囲において凍らないものを選択することが必要である。例えば、熱媒体は、その凝固点が、好ましくは使用温度の下限より１０℃以上低い温度である。本発明に好適に用いられる熱媒体は、凝固点が－８０℃未満である。
The heat medium used in the present invention is not particularly limited as long as it can be used as a heat medium in a heat exchanger such as a jacket, a coiled tube, or a multiple tube. For example, ethylene glycol, acetone, methylene chloride, methanol, ethanol, or an aqueous solution thereof can be used. It is necessary to select a heat medium that does not freeze in the operating temperature range. For example, the heat medium has a freezing point that is preferably 10 ° C. or more lower than the lower limit of the use temperature. The heat medium suitably used in the present invention has a freezing point of less than −80 ° C.
熱媒体冷却装置１は、熱媒体を貯留するための熱媒体容器２、液体窒素容器１１から液体窒素を導入し熱媒体との間で熱交換するためのコイル管３とを有する。コイル管３の内側には液体窒素が在り、コイル管３の外側には熱媒体が在って、コイル管３の管壁を介して両者間で熱交換が成される。コイル管３に供給する液体窒素の量は弁７によって調節される。コイル管３への供給量は、特に限定されないが、測定される熱媒体の温度に応じて、調節することが好ましい。コイル管３に導入された液体窒素は熱交換を行っている途中で完全に気化させることが好ましい。
図１に示すコイル管３は、熱媒体と液体窒素との間で仕切りを介して熱交換することができるものであれば、別のものと交換または併用することができる。例えば、コイル管に代えてまたはそれに加えて、熱媒体容器の周りにジャケットを設けることができる。このジャケットに液体窒素を導入し、液体窒素と熱媒体との間で容器壁を介して熱交換してもよい。 The heatmedium cooling device 1 includes a heat medium container 2 for storing the heat medium, and a coil tube 3 for introducing liquid nitrogen from the liquid nitrogen container 11 and exchanging heat with the heat medium. Liquid nitrogen is present inside the coil tube 3, and a heat medium is present outside the coil tube 3, and heat exchange is performed between the two through the tube wall of the coil tube 3. The amount of liquid nitrogen supplied to the coil tube 3 is adjusted by a valve 7. Although the supply amount to the coiled tube 3 is not particularly limited, it is preferable to adjust according to the temperature of the heat medium to be measured. The liquid nitrogen introduced into the coil tube 3 is preferably completely vaporized during the heat exchange.
Thecoil tube 3 shown in FIG. 1 can be exchanged or used together with another one as long as it can exchange heat between the heat medium and liquid nitrogen via a partition. For example, instead of or in addition to the coiled tube, a jacket can be provided around the heat medium container. Liquid nitrogen may be introduced into the jacket, and heat exchange may be performed between the liquid nitrogen and the heat medium via the container wall.
図１に示すコイル管３は、熱媒体と液体窒素との間で仕切りを介して熱交換することができるものであれば、別のものと交換または併用することができる。例えば、コイル管に代えてまたはそれに加えて、熱媒体容器の周りにジャケットを設けることができる。このジャケットに液体窒素を導入し、液体窒素と熱媒体との間で容器壁を介して熱交換してもよい。 The heat
The
熱媒体冷却装置１には、液体窒素容器１１から液体窒素を熱媒体に直接導入するための管４が取り付けられている。管４によって導入された液体窒素は熱媒体に直接に接触し両者間で熱交換が成される。熱交換がなされた窒素は熱媒体容器上部のベントから排出される。管４に供給する液体窒素の量は弁６によって調節される。管４への供給量は、特に限定されないが、測定される熱媒体の温度に応じて、調節することが好ましい。熱媒体冷却装置１は、管４から熱媒体に直接導入された液体窒素が熱媒体容器２内に液体状態で残らないように攪拌機能を有することが好ましい。熱媒体中での管４の開口部の形状は特に制限されないが、熱媒体が凍結して開口部を塞ぐ事態を生じさせないようにするために開口部は大きめの径にしておくことが好ましい。例えば、ラッパ形状の開口部とすることができる。
The heat medium cooling device 1 is provided with a pipe 4 for directly introducing liquid nitrogen from the liquid nitrogen container 11 into the heat medium. The liquid nitrogen introduced by the tube 4 is in direct contact with the heat medium, and heat exchange is performed between them. The nitrogen subjected to the heat exchange is discharged from the vent at the top of the heat medium container. The amount of liquid nitrogen supplied to the tube 4 is adjusted by a valve 6. Although the supply amount to the pipe 4 is not particularly limited, it is preferably adjusted according to the temperature of the heat medium to be measured. It is preferable that the heat medium cooling device 1 has a stirring function so that liquid nitrogen introduced directly from the pipe 4 to the heat medium does not remain in the heat medium container 2 in a liquid state. The shape of the opening of the tube 4 in the heat medium is not particularly limited, but it is preferable that the opening has a large diameter so that the heat medium does not freeze and block the opening. For example, it can be a trumpet-shaped opening.
熱媒体冷却装置１は、熱媒体の温度、熱媒体容器２の気相部の温度、および管３からの窒素排ガスの温度を測定する手段（図示せず。）を有することが好ましい。さらに、熱媒体冷却装置１は、測定された温度の値に応じて、管４および管３に導入する液体窒素の量を調節するための手段６および７を制御するための手段を有することが好ましい。
The heat medium cooling device 1 preferably has means (not shown) for measuring the temperature of the heat medium, the temperature of the gas phase portion of the heat medium container 2, and the temperature of the nitrogen exhaust gas from the tube 3. Furthermore, the heat medium cooling device 1 may have means for controlling the means 6 and 7 for adjusting the amount of liquid nitrogen introduced into the pipe 4 and the pipe 3 according to the measured temperature value. preferable.
本発明においては、液体窒素を管４および管３の両方に同時に供給してもよいし、管４または管３のいずれか一方にだけ供給してよい。
本発明においては、熱媒体の温度が設定温度以上の場合は、コイル管３に液体窒素を供給して、熱媒体と液体窒素との間で仕切りを介して熱交換することが好ましい。なお、熱媒体の温度が設定温度以上の場合でも、本発明の効果を損なわない範囲で、コイル管３に供給する量よりも少ない量の液体窒素を管４に供給して熱媒体と液体窒素とを直接に接触させて熱交換してもよい。 In the present invention, liquid nitrogen may be supplied to both thetube 4 and the tube 3 at the same time, or only one of the tube 4 and the tube 3 may be supplied.
In the present invention, when the temperature of the heat medium is equal to or higher than the set temperature, it is preferable to supply liquid nitrogen to thecoil tube 3 and exchange heat between the heat medium and liquid nitrogen via a partition. Even when the temperature of the heat medium is equal to or higher than the set temperature, a smaller amount of liquid nitrogen than that supplied to the coiled tube 3 is supplied to the tube 4 within a range that does not impair the effects of the present invention. And may be directly contacted to exchange heat.
本発明においては、熱媒体の温度が設定温度以上の場合は、コイル管３に液体窒素を供給して、熱媒体と液体窒素との間で仕切りを介して熱交換することが好ましい。なお、熱媒体の温度が設定温度以上の場合でも、本発明の効果を損なわない範囲で、コイル管３に供給する量よりも少ない量の液体窒素を管４に供給して熱媒体と液体窒素とを直接に接触させて熱交換してもよい。 In the present invention, liquid nitrogen may be supplied to both the
In the present invention, when the temperature of the heat medium is equal to or higher than the set temperature, it is preferable to supply liquid nitrogen to the
また、熱媒体の温度が設定温度未満の場合は管４に液体窒素を供給して、熱媒体と液体窒素とを直接に接触させて熱交換することが好ましい。なお、熱媒体の温度が設定温度未満の場合でも、本発明の効果を損なわない範囲で、管４に供給する量よりも少ない量の液体窒素をコイル管３に供給して、熱媒体と液体窒素との間で仕切りを介して熱交換してもよい。
熱媒体の温度が設定温度以上の場合に仕切りを介して熱交換を行うと、窒素同伴による熱媒体の損失を無くすることができる。一方、熱媒体の温度が設定温度未満の場合に直接に接触させて熱交換を行うことで液体窒素の顕熱を利用することが可能となる。 In addition, when the temperature of the heat medium is lower than the set temperature, it is preferable to supply liquid nitrogen to thepipe 4 and exchange heat by directly contacting the heat medium and liquid nitrogen. Even when the temperature of the heat medium is lower than the set temperature, the amount of liquid nitrogen smaller than the amount supplied to the tube 4 is supplied to the coil tube 3 within a range that does not impair the effects of the present invention. Heat exchange may be performed with nitrogen through a partition.
When heat exchange is performed through the partition when the temperature of the heat medium is equal to or higher than the set temperature, loss of the heat medium due to nitrogen entrainment can be eliminated. On the other hand, when the temperature of the heat medium is lower than the set temperature, it is possible to utilize the sensible heat of liquid nitrogen by directly contacting and performing heat exchange.
熱媒体の温度が設定温度以上の場合に仕切りを介して熱交換を行うと、窒素同伴による熱媒体の損失を無くすることができる。一方、熱媒体の温度が設定温度未満の場合に直接に接触させて熱交換を行うことで液体窒素の顕熱を利用することが可能となる。 In addition, when the temperature of the heat medium is lower than the set temperature, it is preferable to supply liquid nitrogen to the
When heat exchange is performed through the partition when the temperature of the heat medium is equal to or higher than the set temperature, loss of the heat medium due to nitrogen entrainment can be eliminated. On the other hand, when the temperature of the heat medium is lower than the set temperature, it is possible to utilize the sensible heat of liquid nitrogen by directly contacting and performing heat exchange.
該設定温度は、好ましくは－６０～＋２０℃の範囲のいずれか一つの温度である。例えば、熱媒体がエタノールの場合に、設定温度は、好ましくは－４０～－１０℃の範囲のいずれか一つの温度、より好ましくは－３０～－１５℃の範囲のいずれか一つの温度である。
The set temperature is preferably any one of temperatures in the range of −60 to + 20 ° C. For example, when the heating medium is ethanol, the set temperature is preferably any one temperature in the range of −40 to −10 ° C., more preferably any one temperature in the range of −30 to −15 ° C. .
本発明の熱媒体冷却装置には、更に、熱媒体と放出された窒素との分離手段や、気化した熱媒体を回収する手段を更に設けることができる。また、本発明の装置には、用いた窒素を回収する手段を更に設けることができ、回収した窒素を反応器の置換用ガスなどとして使用する手段を設けることもできる。
The heat medium cooling device of the present invention can further include means for separating the heat medium from the released nitrogen and means for recovering the vaporized heat medium. The apparatus of the present invention can further be provided with a means for recovering the used nitrogen, and can be provided with a means for using the recovered nitrogen as a replacement gas for the reactor.
次に、実施例を示し、本発明をより具体的に説明する。
Next, the present invention will be described more specifically by showing examples.
（実施例１）
図１に示すように熱媒体容器２に、直径１０ｍｍのコイル管３、および直径１０ｍｍの吹出し管４を取り付けた。コイル管３の一端は熱媒体容器の外に設置し、他端は流量調節弁７を介して液体窒素容器１１に接続した。吹出し管４の一端は熱媒体容器２内に設置し、他端は流量調節弁６を介して液体窒素容器１１に接続した。熱媒体に浸かる位置、熱媒体の液面直上およびコイル出口付近に温度測定器をそれぞれ設置し、熱媒体の温度、熱媒体容器気相部の温度およびコイル管出口の排ガス温度を測定した。 Example 1
As shown in FIG. 1, acoil tube 3 having a diameter of 10 mm and a blowing tube 4 having a diameter of 10 mm were attached to the heat medium container 2. One end of the coil tube 3 was installed outside the heat medium container, and the other end was connected to the liquid nitrogen container 11 via the flow rate control valve 7. One end of the blowing pipe 4 was installed in the heat medium container 2, and the other end was connected to the liquid nitrogen container 11 via the flow rate control valve 6. A temperature measuring device was installed at a position immersed in the heat medium, immediately above the liquid surface of the heat medium and in the vicinity of the coil outlet, and the temperature of the heat medium, the temperature of the gas phase of the heat medium container, and the exhaust gas temperature at the coil tube outlet were measured.
図１に示すように熱媒体容器２に、直径１０ｍｍのコイル管３、および直径１０ｍｍの吹出し管４を取り付けた。コイル管３の一端は熱媒体容器の外に設置し、他端は流量調節弁７を介して液体窒素容器１１に接続した。吹出し管４の一端は熱媒体容器２内に設置し、他端は流量調節弁６を介して液体窒素容器１１に接続した。熱媒体に浸かる位置、熱媒体の液面直上およびコイル出口付近に温度測定器をそれぞれ設置し、熱媒体の温度、熱媒体容器気相部の温度およびコイル管出口の排ガス温度を測定した。 Example 1
As shown in FIG. 1, a
熱媒体としてエタノール（９９．５％）６．０２ｋｇを熱媒体容器に入れ、攪拌機で攪拌した。液体窒素容器および熱媒体容器を台秤に載せて、液体窒素の消費量および熱媒体の重量変化を測定した。
冷却開始時の熱媒体温度は１２℃であった。まず、弁７を開き液体窒素をコイル管３に流量６．４８ｋｇ／ｈｒで供給した。熱媒体の温度が－２０℃になった時点で弁７を閉じ同時に弁６を開き液体窒素を吹出し管４に流量７．１３ｋｇ／ｈｒで供給した。
図２および図３に、熱媒体の重量および温度変化、液体窒素の累積消費重量、容器気相の温度変化、およびコイル出口の温度変化を示す。図２中、上向き矢印は、コイル管３から吹出し管４への切り替えを示す。
液体窒素の累積消費量が約６．８５ｋｇで、－６６℃まで冷却できた。熱媒体の損失は測定誤差内でほとんど無かった。図３からコイル管を介しての熱交換を行っている期間ではコイル出口温度が熱媒体温度よりも低くなっており、冷却に潜熱が主に使われ顕熱はあまり使われていないことが判る。また、図３から液体窒素を直接に導入している期間では容器気相温度が熱媒体温度とほぼ同じになっており、液体窒素の顕熱が冷却に有効に利用されていることがわかる。 As a heat medium, 6.02 kg of ethanol (99.5%) was placed in a heat medium container and stirred with a stirrer. The liquid nitrogen container and the heat medium container were placed on a platform scale, and the consumption of liquid nitrogen and the change in the weight of the heat medium were measured.
The heat medium temperature at the start of cooling was 12 ° C. First, the valve 7 was opened and liquid nitrogen was supplied to thecoil tube 3 at a flow rate of 6.48 kg / hr. When the temperature of the heat medium reached −20 ° C., the valve 7 was closed and the valve 6 was opened at the same time, and liquid nitrogen was supplied to the blowing pipe 4 at a flow rate of 7.13 kg / hr.
2 and 3 show changes in the weight and temperature of the heat medium, the cumulative consumption weight of liquid nitrogen, the temperature change in the container gas phase, and the temperature change at the coil outlet. In FIG. 2, an upward arrow indicates switching from thecoil tube 3 to the blowout tube 4.
The cumulative consumption of liquid nitrogen was about 6.85 kg, and it could be cooled to -66 ° C. There was almost no loss of the heat medium within the measurement error. It can be seen from FIG. 3 that the coil outlet temperature is lower than the heat medium temperature during the period of heat exchange through the coil tube, and that latent heat is mainly used for cooling and sensible heat is not used much. . In addition, it can be seen from FIG. 3 that during the period in which liquid nitrogen is directly introduced, the gas phase temperature of the container is almost the same as the heat medium temperature, and the sensible heat of liquid nitrogen is effectively used for cooling.
冷却開始時の熱媒体温度は１２℃であった。まず、弁７を開き液体窒素をコイル管３に流量６．４８ｋｇ／ｈｒで供給した。熱媒体の温度が－２０℃になった時点で弁７を閉じ同時に弁６を開き液体窒素を吹出し管４に流量７．１３ｋｇ／ｈｒで供給した。
図２および図３に、熱媒体の重量および温度変化、液体窒素の累積消費重量、容器気相の温度変化、およびコイル出口の温度変化を示す。図２中、上向き矢印は、コイル管３から吹出し管４への切り替えを示す。
液体窒素の累積消費量が約６．８５ｋｇで、－６６℃まで冷却できた。熱媒体の損失は測定誤差内でほとんど無かった。図３からコイル管を介しての熱交換を行っている期間ではコイル出口温度が熱媒体温度よりも低くなっており、冷却に潜熱が主に使われ顕熱はあまり使われていないことが判る。また、図３から液体窒素を直接に導入している期間では容器気相温度が熱媒体温度とほぼ同じになっており、液体窒素の顕熱が冷却に有効に利用されていることがわかる。 As a heat medium, 6.02 kg of ethanol (99.5%) was placed in a heat medium container and stirred with a stirrer. The liquid nitrogen container and the heat medium container were placed on a platform scale, and the consumption of liquid nitrogen and the change in the weight of the heat medium were measured.
The heat medium temperature at the start of cooling was 12 ° C. First, the valve 7 was opened and liquid nitrogen was supplied to the
2 and 3 show changes in the weight and temperature of the heat medium, the cumulative consumption weight of liquid nitrogen, the temperature change in the container gas phase, and the temperature change at the coil outlet. In FIG. 2, an upward arrow indicates switching from the
The cumulative consumption of liquid nitrogen was about 6.85 kg, and it could be cooled to -66 ° C. There was almost no loss of the heat medium within the measurement error. It can be seen from FIG. 3 that the coil outlet temperature is lower than the heat medium temperature during the period of heat exchange through the coil tube, and that latent heat is mainly used for cooling and sensible heat is not used much. . In addition, it can be seen from FIG. 3 that during the period in which liquid nitrogen is directly introduced, the gas phase temperature of the container is almost the same as the heat medium temperature, and the sensible heat of liquid nitrogen is effectively used for cooling.
（実施例２）
表１に示す操業条件に変えた以外は実施例１と同じ手法で熱媒体の冷却を行った。
図４および図５に、熱媒体の重量および温度変化、液体窒素の累積消費重量、容器気相の温度変化、およびコイル出口の温度変化を示す。図４中、上向き矢印は、コイル管３から吹出し管４への切り替えを示す。
液体窒素の累積消費量が約６．９８ｋｇで、－５６℃まで冷却できた。熱媒体の損失は測定誤差内でほとんど無かった。図５からコイル管を介しての熱交換を行っている期間ではコイル出口温度が熱媒体温度よりも低くなっており、冷却に潜熱が主に使われ顕熱はあまり使われていないことが判る。また、図５から液体窒素を直接に導入している期間では容器気相温度が熱媒体温度とほぼ同じになっており、液体窒素の顕熱が冷却に有効に利用されていることがわかる。 (Example 2)
The heat medium was cooled by the same method as in Example 1 except that the operating conditions shown in Table 1 were changed.
4 and 5 show changes in the weight and temperature of the heat medium, the accumulated consumption weight of liquid nitrogen, the temperature change in the container gas phase, and the temperature change at the coil outlet. In FIG. 4, an upward arrow indicates switching from the coiledtube 3 to the outlet tube 4.
The cumulative consumption of liquid nitrogen was about 6.98 kg, and it could be cooled to -56 ° C. There was almost no loss of the heat medium within the measurement error. From FIG. 5, it can be seen that the coil exit temperature is lower than the heat medium temperature during the period of heat exchange through the coil tube, and latent heat is mainly used for cooling and sensible heat is not used much. . Further, it can be seen from FIG. 5 that during the period in which liquid nitrogen is directly introduced, the gas phase temperature of the container is almost the same as the heat medium temperature, and the sensible heat of liquid nitrogen is effectively used for cooling.
表１に示す操業条件に変えた以外は実施例１と同じ手法で熱媒体の冷却を行った。
図４および図５に、熱媒体の重量および温度変化、液体窒素の累積消費重量、容器気相の温度変化、およびコイル出口の温度変化を示す。図４中、上向き矢印は、コイル管３から吹出し管４への切り替えを示す。
液体窒素の累積消費量が約６．９８ｋｇで、－５６℃まで冷却できた。熱媒体の損失は測定誤差内でほとんど無かった。図５からコイル管を介しての熱交換を行っている期間ではコイル出口温度が熱媒体温度よりも低くなっており、冷却に潜熱が主に使われ顕熱はあまり使われていないことが判る。また、図５から液体窒素を直接に導入している期間では容器気相温度が熱媒体温度とほぼ同じになっており、液体窒素の顕熱が冷却に有効に利用されていることがわかる。 (Example 2)
The heat medium was cooled by the same method as in Example 1 except that the operating conditions shown in Table 1 were changed.
4 and 5 show changes in the weight and temperature of the heat medium, the accumulated consumption weight of liquid nitrogen, the temperature change in the container gas phase, and the temperature change at the coil outlet. In FIG. 4, an upward arrow indicates switching from the coiled
The cumulative consumption of liquid nitrogen was about 6.98 kg, and it could be cooled to -56 ° C. There was almost no loss of the heat medium within the measurement error. From FIG. 5, it can be seen that the coil exit temperature is lower than the heat medium temperature during the period of heat exchange through the coil tube, and latent heat is mainly used for cooling and sensible heat is not used much. . Further, it can be seen from FIG. 5 that during the period in which liquid nitrogen is directly introduced, the gas phase temperature of the container is almost the same as the heat medium temperature, and the sensible heat of liquid nitrogen is effectively used for cooling.
（比較例１）
表１に示す操業条件に変えた以外は実施例１と同じ手法で熱媒体の冷却を行った。
図６および図７に、熱媒体の重量および温度変化、液体窒素の累積消費重量、容器気相の温度変化、およびコイル出口の温度変化を示す。
液体窒素の累積消費量が約５．４５ｋｇで、－５５℃まで冷却できた。しかし、熱媒体が窒素排ガスに同伴して大きく損失した。図７から液体窒素を直接に導入している期間では容器気相温度が熱媒体温度とほぼ同じになっており、液体窒素の顕熱が冷却に有効に利用されていることがわかる。 (Comparative Example 1)
The heat medium was cooled by the same method as in Example 1 except that the operating conditions shown in Table 1 were changed.
6 and 7 show the weight and temperature change of the heat medium, the cumulative consumption weight of liquid nitrogen, the temperature change of the container gas phase, and the temperature change of the coil outlet.
The cumulative consumption of liquid nitrogen was about 5.45 kg, and it could be cooled to -55 ° C. However, the heat medium was greatly lost accompanying the nitrogen exhaust gas. From FIG. 7, it can be seen that during the period in which liquid nitrogen is directly introduced, the gas phase temperature of the container is substantially the same as the heat medium temperature, and the sensible heat of liquid nitrogen is effectively used for cooling.
表１に示す操業条件に変えた以外は実施例１と同じ手法で熱媒体の冷却を行った。
図６および図７に、熱媒体の重量および温度変化、液体窒素の累積消費重量、容器気相の温度変化、およびコイル出口の温度変化を示す。
液体窒素の累積消費量が約５．４５ｋｇで、－５５℃まで冷却できた。しかし、熱媒体が窒素排ガスに同伴して大きく損失した。図７から液体窒素を直接に導入している期間では容器気相温度が熱媒体温度とほぼ同じになっており、液体窒素の顕熱が冷却に有効に利用されていることがわかる。 (Comparative Example 1)
The heat medium was cooled by the same method as in Example 1 except that the operating conditions shown in Table 1 were changed.
6 and 7 show the weight and temperature change of the heat medium, the cumulative consumption weight of liquid nitrogen, the temperature change of the container gas phase, and the temperature change of the coil outlet.
The cumulative consumption of liquid nitrogen was about 5.45 kg, and it could be cooled to -55 ° C. However, the heat medium was greatly lost accompanying the nitrogen exhaust gas. From FIG. 7, it can be seen that during the period in which liquid nitrogen is directly introduced, the gas phase temperature of the container is substantially the same as the heat medium temperature, and the sensible heat of liquid nitrogen is effectively used for cooling.
（比較例２）
表１に示す操業条件に変えた以外は実施例１と同じ手法で熱媒体の冷却を行った。
図８および図９に、熱媒体の重量および温度変化、液体窒素の累積消費重量、容器気相の温度変化、およびコイル出口の温度変化を示す。
－５６℃まで冷却するのに液体窒素の累積消費量が約７．３７ｋｇで、－６６℃まで冷却するのに液体窒素の累積消費量が約９．４９ｋｇであった。熱媒体の温度が低くなるほど冷却速度が低下した。熱媒体の温度が約－２０℃になるとコイル出口温度が液体窒素の沸点付近の温度になった。図９からコイル管を介しての熱交換を行っている期間ではコイル出口温度が熱媒体温度よりも低くなっており、冷却に潜熱が主に使われ顕熱はあまり使われていないことが判る。 (Comparative Example 2)
The heat medium was cooled by the same method as in Example 1 except that the operating conditions shown in Table 1 were changed.
8 and 9 show the weight and temperature change of the heat medium, the cumulative consumption weight of liquid nitrogen, the temperature change of the container gas phase, and the temperature change of the coil outlet.
The cumulative consumption of liquid nitrogen was about 7.37 kg for cooling to −56 ° C., and the cumulative consumption of liquid nitrogen was about 9.49 kg for cooling to −66 ° C. The cooling rate decreased as the temperature of the heat medium decreased. When the temperature of the heat medium reached about −20 ° C., the coil outlet temperature became a temperature near the boiling point of liquid nitrogen. From FIG. 9, it is understood that the coil outlet temperature is lower than the heat medium temperature during the period of heat exchange through the coil tube, and that latent heat is mainly used for cooling and sensible heat is not used much. .
表１に示す操業条件に変えた以外は実施例１と同じ手法で熱媒体の冷却を行った。
図８および図９に、熱媒体の重量および温度変化、液体窒素の累積消費重量、容器気相の温度変化、およびコイル出口の温度変化を示す。
－５６℃まで冷却するのに液体窒素の累積消費量が約７．３７ｋｇで、－６６℃まで冷却するのに液体窒素の累積消費量が約９．４９ｋｇであった。熱媒体の温度が低くなるほど冷却速度が低下した。熱媒体の温度が約－２０℃になるとコイル出口温度が液体窒素の沸点付近の温度になった。図９からコイル管を介しての熱交換を行っている期間ではコイル出口温度が熱媒体温度よりも低くなっており、冷却に潜熱が主に使われ顕熱はあまり使われていないことが判る。 (Comparative Example 2)
The heat medium was cooled by the same method as in Example 1 except that the operating conditions shown in Table 1 were changed.
8 and 9 show the weight and temperature change of the heat medium, the cumulative consumption weight of liquid nitrogen, the temperature change of the container gas phase, and the temperature change of the coil outlet.
The cumulative consumption of liquid nitrogen was about 7.37 kg for cooling to −56 ° C., and the cumulative consumption of liquid nitrogen was about 9.49 kg for cooling to −66 ° C. The cooling rate decreased as the temperature of the heat medium decreased. When the temperature of the heat medium reached about −20 ° C., the coil outlet temperature became a temperature near the boiling point of liquid nitrogen. From FIG. 9, it is understood that the coil outlet temperature is lower than the heat medium temperature during the period of heat exchange through the coil tube, and that latent heat is mainly used for cooling and sensible heat is not used much. .
１・・・熱媒体冷却装置
２・・・熱媒体容器
３・・・コイル管
４、５・・・管
６、７・・・弁
８・・・攪拌機
１１・・・液体窒素容器
１２・・・低温反応器
１３・・・ジャケット
１４、１５・・・管
１６・・・ポンプ DESCRIPTION OFSYMBOLS 1 ... Heat-medium cooling device 2 ... Heat-medium container 3 ... Coiled tube 4, 5 ... Tube 6, 7 ... Valve 8 ... Stirrer 11 ... Liquid nitrogen container 12 ...・ Low temperature reactor 13 ... Jacket 14,15 ... Pipe 16 ... Pump
２・・・熱媒体容器
３・・・コイル管
４、５・・・管
６、７・・・弁
８・・・攪拌機
１１・・・液体窒素容器
１２・・・低温反応器
１３・・・ジャケット
１４、１５・・・管
１６・・・ポンプ DESCRIPTION OF
Claims (6)
- 熱媒体と液体窒素との間で仕切りを介して熱交換する工程と
熱媒体と液体窒素との間で直接に接触させて熱交換する工程とを、同時にまたは順不同に行うことを含む熱媒体の冷却方法。 A heat exchange method comprising: performing heat exchange between the heat medium and liquid nitrogen through a partition; and performing heat exchange by directly contacting the heat medium and liquid nitrogen simultaneously or in random order. Cooling method. - 熱媒体の温度が設定温度以上の場合は熱媒体と液体窒素との間で仕切りを介して熱交換する工程を行い、熱媒体の温度が設定温度未満の場合は熱媒体と液体窒素との間で直接に接触させて熱交換する工程を行う、請求項１に記載の熱媒体の冷却方法。 When the temperature of the heat medium is equal to or higher than the set temperature, a process of exchanging heat is performed between the heat medium and liquid nitrogen via a partition. The method for cooling a heat medium according to claim 1, wherein the step of performing heat exchange by direct contact is performed.
- 設定温度が、－６０～＋２０℃の範囲のいずれか一つの温度である、請求項２に記載の熱媒体の冷却方法。 3. The method for cooling a heat medium according to claim 2, wherein the set temperature is any one of a range of −60 to + 20 ° C.
- 熱媒体と液体窒素との間で仕切りを介して熱交換するための手段、
該熱交換手段における熱媒体側の領域に液体窒素を供給するための手段、
前記熱交換手段における液体窒素側の領域に液体窒素を供給するための手段、
前記熱交換手段における熱媒体側の領域に供給する液体窒素の量を調節する手段、および
前記熱交換手段における液体窒素側の領域に供給する液体窒素の量を調節する手段を有する、熱媒体冷却装置。 Means for exchanging heat between the heating medium and liquid nitrogen via a partition;
Means for supplying liquid nitrogen to a region on the heat medium side in the heat exchange means;
Means for supplying liquid nitrogen to an area on the liquid nitrogen side in the heat exchange means;
Heat medium cooling having means for adjusting the amount of liquid nitrogen supplied to the region on the heat medium side in the heat exchange means, and means for adjusting the amount of liquid nitrogen supplied to the region on the liquid nitrogen side in the heat exchange means apparatus. - 熱媒体の温度を測定する手段と、
測定温度値に基づいて熱媒体側の領域に供給する液体窒素の量を調節する手段および／または液体窒素側の領域に供給する液体窒素の量を調節する手段を制御する手段をさらに有する、請求項４に記載の熱媒体冷却装置。 Means for measuring the temperature of the heating medium;
And a means for controlling the means for adjusting the amount of liquid nitrogen supplied to the region on the heat medium side and / or the means for adjusting the amount of liquid nitrogen supplied to the region on the liquid nitrogen side based on the measured temperature value. Item 5. The heat medium cooling device according to Item 4. - 低温反応装置用熱媒体の温度調節に用いる、請求項４または５に記載の熱媒体冷却装置。 The heat medium cooling apparatus according to claim 4 or 5, which is used for temperature adjustment of a heat medium for a low-temperature reactor.
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| CN108800697A (en) * | 2018-05-29 | 2018-11-13 | 航天新长征电动汽车技术有限公司 | A kind of refrigeration injection device, liquid nitrogen refrigerating system and refrigerated van type vehicle |
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| JP2009287822A (en) * | 2008-05-28 | 2009-12-10 | Taiyo Nippon Sanso Corp | Refrigerant cooling device |
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| JPS5526777Y2 (en) * | 1976-03-31 | 1980-06-26 | ||
| JPS57157879U (en) * | 1981-03-30 | 1982-10-04 |
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| JPS5421643A (en) * | 1977-07-18 | 1979-02-19 | Toray Eng Co Ltd | Method of cooling liquid |
| JP2001050622A (en) * | 1999-07-15 | 2001-02-23 | Air Prod And Chem Inc | Method and device for refrigerating product |
| US20020194853A1 (en) * | 2000-06-28 | 2002-12-26 | Cashin Michael D. | Freezer and plant gas system |
| JP2009287822A (en) * | 2008-05-28 | 2009-12-10 | Taiyo Nippon Sanso Corp | Refrigerant cooling device |
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| CN108800697A (en) * | 2018-05-29 | 2018-11-13 | 航天新长征电动汽车技术有限公司 | A kind of refrigeration injection device, liquid nitrogen refrigerating system and refrigerated van type vehicle |
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