JP2012232244A - Batch type internally thermal exchanging type distillation device - Google Patents

Abstract

PROBLEM TO BE SOLVED: To purify distillation raw materials with high efficiency while saving energy.SOLUTION: A batch type internally thermal exchanging type distillation device includes: a distillation column 1 for distilling the distillation raw materials; a distillation raw material reservoir 22 for reserving the distillation raw materials; a reboiler 23 for heating the distillation raw materials supplied to the bottom side of the distillation column 1 to be in gaseous state; a compressor 28 for pressurizing and compressing the distillation raw materials in gaseous state taken out from the middle part of the distillation column 1 and refluxing them to a distillation column 3; and a condenser 24 for condensing column top steam flowing out of the column top 6 of the distillation column 1 and taking the steam out. A distillation chamber 4 on the upper side including the distillation chamber 4 to which the distillation raw materials in gaseous state pressurized and compressed by the compressor 28 is supplied is assumed as a high-pressure part 20 while the lower side of the high-pressure part 20 is assumed as a low-pressure part 21. Heat exchange is performed between the high-pressure part 20 and the low-pressure part 21 and evaporation of the distillation raw material is facilitated on the low-pressure part 21.

Description

  The present invention relates to a batch-type internal heat exchange distillation apparatus in which a high-pressure part and a low-pressure part are configured inside a distillation column, and heat exchange is performed between the high-pressure part and the low-pressure part.

  Conventionally, as a distillation column for reducing energy consumption used for distillation, an internal heat exchange type distillation column having a low-pressure column and a high-pressure column, and configured to perform heat exchange between the low-pressure column and the high-pressure column is provided. Are known.

  Examples of this type of distillation column include those described in Japanese Patent No. 2694425 (Patent Document 1) and Japanese Patent No. 3184501 (Patent Document 2). The distillation column shown here has a structure in which a plurality of tubes are separated from the inside and outside of the plurality of tubes inside the main body cylinder by connecting the plurality of pipes to the main body cylinder constituting the tower main body by means of both end tube plates. Gas and liquid inlets and outlets are provided inside and outside the pipe, and the operating temperature is varied by making a difference in the operating pressure between the inside and outside of the pipe. By exchanging heat with the part side, the high-pressure part side is configured as the concentrating part and the low-pressure part side as the recovery part.

  In this internal heat exchange type distillation column, the distillation raw material at the boiling point temperature is supplied to the top of the low-pressure part, and the top vapor on the high-pressure part is taken out as a product. In addition, the vapor at the top of the low-pressure section is supplied to the bottom of the high-pressure section through the compressor, and part of the bottom-liquid at the low-pressure section is discharged to the outside as a bottom liquid. Then, it is returned to the bottom of the low-pressure section through a reboiler and subjected to distillation treatment.

  The internal heat exchange type distillation column configured as described above is a method in which the top vapor on the low pressure part side is pressurized and compressed by a compressor and supplied to the high pressure part side to increase the pressure and temperature on the high pressure part side. Since heat exchange with the low-pressure part side is performed, the reboiler load for heating the distillation raw material can be reduced, and energy saving is achieved in one distillation column.

  A reboiling vapor compression column distillation column (Heat-Integrated Batch Distillation Column; HIBaDiC) has been proposed as an application of such an internal heat exchange type distillation column to a batch distillation column. In the apparatus using this distillation column, the entire distillation column is covered with a jacket (reboiler), and the steam from the jacket is compressed and supplied to the distillation column, so that the temperature of the distillation column is raised and heat exchange is performed. ing. As a result, the reboiler load is reduced, and further, separation is promoted by internal reflux, so that operation at a reflux ratio smaller than the minimum reflux ratio is possible, and energy saving is achieved.

Japanese Patent No. 2694425 Japanese Patent No. 3184501

  The apparatus using the reboiling vapor compression batch distillation tower described above has a problem that the amount of heat transfer varies depending on the amount of raw material charged in the jacket, and the apparatus becomes larger. As described above, the internal heat exchange technique is useful for energy saving in the distillation separation process, but a practical batch distillation apparatus adapted to this technique has not yet been proposed.

  Therefore, the present invention enables an internal heat exchange type distillation apparatus using an internal heat exchange type distillation column to be able to purify a distillation raw material with high efficiency, and further achieve energy saving. It is a technical problem to provide a distillation apparatus.

  In order to solve the technical problem as described above, the present invention stores a distillation column in which a distillation raw material is distilled, a distillation raw material supplied into the distillation column from the bottom side of the distillation column, and the distillation column. From the middle part of the distillation column, a distillation raw material storage tank for storing the liquid phase distillation raw material dropped to the bottom of the distillation raw material, a reboiler for heating and vaporizing the distillation raw material supplied to the bottom side of the distillation raw material storage tank A compressor for compressing and compressing the taken-out distillation raw material in a gas phase and refluxing it to the distillation column; and a condenser for condensing the top vapor flowing out from the top of the distillation column and taking it out to the outside. The upper side to which the gas phase distillation raw material pressurized and compressed by the compressor inside the tower is supplied is a high pressure portion, the lower side of the high pressure portion to which the distillation raw material is supplied is a low pressure portion, and the high pressure portion is To exchange heat with the low pressure part Those were.

  As the distillation column used in the present invention, for example, a plurality of shelves provided with a liquid dropping part for dropping a liquid-phase distillation raw material and a vapor transmission part for allowing a gas-phase distillation raw material to permeate are arranged at predetermined intervals. In addition, a plurality of distillation chambers partitioned by shelves are configured in the height direction and a shelving system is used.

  The present invention may further include a reflux means for refluxing a part of the top vapor condensed in the condenser to the top of the distillation tower.

  In the present invention, it is desirable to provide a reflux mechanism for refluxing the distillation raw material stored on the tower bottom side of the high pressure section to the tower top side of the low pressure section.

  The reflux mechanism is provided with a pressure control valve in the middle of a reflux pipe for refluxing the distillation raw material, and reduces the pressure of the distillation raw material refluxed from the high-pressure part side to supply the pressure to the low-pressure part side. desirable.

  Furthermore, the present invention includes a further distillation raw material storage tank for storing the distillation raw material, and preheats the additional distillation raw material supplied from the distillation raw material storage tank to supply it to the tower top side of the low pressure part. It is desirable to provide a heating supply.

  At this time, the further distillation raw material supplied from the further distillation raw material storage tank is supplied in a liquid phase state or a gas-liquid mixed state.

  The present invention pressurizes and compresses a vapor-phase distillation raw material taken out from the middle part of the distillation column and recirculates it to the distillation column, whereby the upper side of the distillation column is used as a high-pressure unit and the lower side thereof is used as a low-pressure unit. By performing heat exchange between the high-pressure part and the low-pressure part, it is possible to reduce the load on the reboiler that heats the distillation raw material in the distillation column and to realize energy saving of the entire apparatus.

  Further, the present invention can be configured without adopting a configuration in which the entire distillation column is covered with a jacket (reboiler), and the distillation column and the reboiler can be arranged apart from each other, so that the entire apparatus can be reduced in size.

  Furthermore, the present invention provides a further distillation energy saving because the further distillation raw material supplied from the top side of the low-pressure part configured in the distillation tower is subjected to heat exchange with the high-pressure part, thereby reducing the energy load of the reboiler. Can be realized.

It is sectional drawing which shows one Embodiment of the distillation tower used for the internal heat exchange type | mold distillation apparatus which concerns on this invention. It is a block diagram which shows schematic structure of one Embodiment of the internal heat exchange type | mold distillation apparatus which concerns on this invention. It is a block diagram which shows schematic structure of other embodiment of the internal heat exchange type | mold distillation apparatus which concerns on this invention.

  Hereinafter, an embodiment of an internal heat exchange type distillation apparatus according to the present invention will be described with reference to the drawings.

  The present invention is a batch type internal heat exchange distillation in which a high pressure part and a low pressure part are configured inside a distillation column to which a distillation raw material is supplied, and heat exchange is performed between the high pressure part and the low pressure part. The apparatus relates to an apparatus, and the distillation apparatus includes, for example, a distillation column 1 configured as shown in FIG. The distillation column 1 includes a column main body 2 formed in a cylindrical shape. In the tower main body 2, a plurality of shelves 3 are arranged at a predetermined interval in the height direction of the tower main body 2. A region partitioned by these shelf 3 is a distillation chamber 4.

  In the present embodiment, eleven shelves 3 are arranged in the tower body 2 to constitute ten distillation chambers 4 in the height direction. And the tower bottom part 5 of the lower side part of the shelf 3 arrange | positioned in the lowest part in the tower main body 2 is made into the supply part of the distillation raw material. Moreover, the tower bottom part 5 becomes a storage part of the distillation raw material in which the distillation raw material made into the liquid phase state in the tower main body 2 is stored. Furthermore, the tower top part 6 at the upper part of the shelf 3 disposed at the uppermost part in the tower body 2 is a steam storage part in which a distillation raw material in a gas phase is stored.

  On the shelf 3, a liquid reservoir portion 7 is provided for retaining a certain amount of the distillation raw material liquid in a liquid phase, and the vapor of the distillation raw material in a vapor state in each distillation chamber 4. Are sequentially provided to the upper distillation chamber 4 and are provided with a plurality of steam rising pipes 8 constituting a vapor transmission section that leads to the tower top section 6. As shown in FIG. 1, these steam rising pipes 8 constitute a liquid reservoir portion 7 on the upper surface side of the shelf 3 by causing a tip portion to protrude a predetermined amount above the shelf 3. Each shelf 3 is provided with a single liquid drop pipe 9 that constitutes a liquid drop part that lowers the distillation raw material retained in the liquid reservoir part 7 to the lower distillation chamber 4 and leads it to the tower bottom part 5. . These liquid downcomers 9 are provided on the outer peripheral side of the shelf 3 so that the liquid phase distillation raw material stored in the liquid reservoir 7 can be dropped on the outer peripheral side of the lower shelf 3. . This is to prevent the distillation action of each distillation chamber 4 from being hindered by the dropwise addition of the distillation raw material liquid.

  The tower top 6 is provided with a steam outlet 10 for taking out the distillation raw material in the gas phase state in the tower body 2, and the side of the tower top 6 is taken out from the steam outlet 10 in a gas phase. Then, a distillate reflux port 11 is provided for refluxing the distillate that has been cooled and condensed into a liquid phase.

  In addition, a distillation raw material supply port 12 is provided at the side of the tower bottom 5 to supply a distillation raw material in a gas phase state into the tower body 2, and the distillation stored in the tower bottom 5 is provided at the bottom. A raw material liquid discharge port 13 for discharging the raw material liquid to the outside of the tower body 2 is provided.

  Further, the distillation column 1 is provided with a steam discharge port 14 for discharging a distillation raw material in a gas phase state to the outside of the column main body 2 in a distillation chamber 4 located at an intermediate portion in the vertical direction. In the present embodiment, the steam outlet 14 is provided on the side of the distillation chamber 4 located at the fifth stage from the bottom. The steam discharged from the steam discharge port 14 is pressurized and compressed on the side of the sixth-stage distillation chamber 4 located above the distillation chamber 4 positioned at the fifth stage where the steam discharge port 14 is provided. A compressed steam supply port 15 to which the compressed steam is supplied is provided.

  Furthermore, the sixth stage distillation chamber 4 is provided with a staying liquid outlet 16 for taking out the staying liquid retained in the liquid reservoir 7 on the shelf 3 to the outside of the tower body 2. The fifth-stage distillation chamber 4 located on the lower side of the chamber 4 is provided with a staying liquid supply port 17 to which the staying liquid taken out from the staying liquid takeout port 16 is supplied.

  The distillation chamber 4 positioned on the upper side including the distillation chamber 4 to which the compressed steam of the distillation column 1 configured as described above is supplied is the distillation chamber 4 positioned on the lower side of the distillation chamber 4 to which the compressed steam is supplied. Higher pressure. Therefore, as shown in the schematic configuration diagram of the distillation apparatus shown in FIG. 2, the distillation column 1 of the present embodiment includes a plurality of upper distillation chambers 4 including the distillation chambers 4 to which compressed steam is supplied, as high-pressure units 20. A plurality of distillation chambers 4 located on the lower side thereof are used as the low pressure part 21. The distillation column 1 constitutes an internal heat exchange type distillation apparatus in which heat is exchanged between the high pressure section 20 and the low pressure section 21 and does not require the exchange of heat with others.

  An embodiment of a distillation apparatus according to the present invention using the distillation column 1 configured as described above will be described with reference to a schematic configuration diagram shown in FIG.

  In FIG. 2 which shows the distillation apparatus which concerns on this invention, as shown in FIG. 1, the distillation column 1 by which the high pressure part 20 and the low pressure part 21 in which heat exchange is performed is comprised inside is shown typically.

  As shown in FIG. 2, the distillation apparatus according to the present invention includes a distillation raw material storage tank 22 in which a distillation raw material supplied into the tower body 2 is stored. Further, the distillation apparatus includes a reboiler 23 that heats the liquid-phase distillation raw material supplied from the distillation raw material storage tank 22 to the tower main body 2 to bring it into a gas phase state. The reboiler 23 and the distillation raw material storage tank 22 are connected by a connecting pipe. Then, the liquid phase distillation raw material supplied from the distillation raw material supply port 12 to the tower bottom 5 located at the lowermost part of the tower main body 2 is brought into a gas phase state by the reboiler 23. The distillation raw material in a gas phase rises in the tower body 2.

  The distillation raw material liquefied inside the distillation column 1 and stored in the column bottom 5 is discharged to the outside from the raw material liquid discharge port 13 and supplied to the distillation raw material storage tank 22. Although not shown, a flow rate adjusting valve is provided between the raw material outlet 13 and the distilled raw material storage tank 22 to adjust the discharge amount of the distilled raw material stored in the tower bottom 5 to the storage tank 22.

  And the distillation apparatus which concerns on this invention is equipped with the condenser 24 which condenses the vapor | steam of the distillation raw material taken out from the vapor | steam taking-out port 10 provided in the tower top part 6. FIG. The steam cooled and condensed by the condenser 24 is taken as a distillate and stored in the distillate storage container 25. A part of the distillate stored in the distillate storage container 25 is taken out of the apparatus as a product, and the rest is returned to the tower top 6 via the distillate reflux port 11 as a reflux liquid.

  A flow rate control valve 27 for controlling the amount of the distillate extracted to the outside of the apparatus is provided on the distillate discharge outlet side of the distillate storage container 25.

  By the way, the distillation apparatus according to the present invention includes a compressor 28 that pressurizes and compresses the vapor of the distillation raw material discharged from the vapor discharge port 14 provided in the distillation chamber 4 located at the uppermost stage on the low pressure section 21 side. . The steam pressurized and compressed by the compressor 28 is supplied from the compressed steam supply port 15 to the distillation chamber 4 located at the lowermost part on the high pressure section 20 side in the tower body 2. That is, the steam discharged from the low pressure part 21 is compressed and compressed by the compressor 28 and supplied to the high pressure part 20.

  Further, the staying liquid retained in the liquid reservoir 7 on the sixth shelf 3 located at the lowermost stage on the high-pressure part 20 side is taken out from the staying liquid outlet 16 to the outside of the distillation column 1 and stays there. It is supplied to the distillation chamber 4 located at the uppermost stage on the low-pressure part 21 side via the liquid supply port 17. At this time, the staying liquid is pressure-adjusted by a throttle valve 29 provided in the middle of the connecting pipe that connects between the staying liquid outlet 16 and the staying liquid supply port 17 and is supplied to the low-pressure part 21 side.

  In this way, the plurality of distillation chambers 4 located at the upper part from the distillation chamber 4 to which the pressurized and compressed steam is supplied become the high-pressure part 20 whose pressure is larger than that of the distillation chamber 4 located at the lower part thereof, on the lower side thereof The plurality of distillation chambers 4 located in the are low pressure parts 21. Since the pressurized and compressed steam is at a high temperature, the high pressure portion 20 side is at a high temperature, and heat exchange is performed between the high pressure portion 20 and the low pressure portion 21.

  An operation procedure for distilling and separating a distillation raw material in the distillation apparatus configured as described above will be described.

  First, a predetermined amount of distillation raw material is charged into the distillation raw material storage tank 22. Next, the reboiler 23 is operated, and the distillation raw material supplied from the distillation raw material storage tank 22 to the tower bottom 5 in the tower body 2 is heated to generate distillation raw material vapor. In addition, supply of the distillation raw material from the distillation raw material storage tank 22 into the tower main body 2 is continued.

  By the way, the vapor | steam of the distillation raw material supplied in the distillation column 1 goes up to the upper distillation chamber 4 from the lower distillation chamber 4 sequentially via the vapor | steam riser 8. As shown in FIG. In the course of ascending the distillation chamber 4 of each stage in the distillation column 1, the distillation raw material that has become liquefied below the gas phase temperature is stored in the liquid reservoir 7 on the shelf 3. The distillation raw material stored in the liquid reservoir 7 is reheated by the vapor of the distillation raw material supplied from the lower side of the distillation column 1 to be in a gas phase, and rises in the distillation column 1. The distillation raw material that has been kept in a liquid state without being vaporized in the liquid reservoir 7 sequentially descends to the liquid reservoir 7 positioned below via the liquid downcomer 9. Each shelf 3 is vaporized by reheating the distillation raw material and the liquid distillation raw material is lowered downward, and is lowered from the lowest shelf 3 in a liquid state, and is formed at the bottom of the distillation column 1. Is stored in the bottom 5 of the tower.

  Then, the distillation raw material that has been raised to the top 6 of the distillation column 1 in the vapor state is taken out from the vapor outlet 10 provided at the top 6 and supplied to the condenser 24. The steam cooled and condensed by the condenser 24 is distilled out of the apparatus as a distillate.

  In the initial stage of the distillation operation, a total reflux operation is performed in which the entire amount of the distillate flowing out from the condenser 24 is refluxed to the top 6 of the column, and the state of vaporization of the distillation raw material in the column body 2 is constant. To a steady state.

  When the inside of the column main body 2 is in a steady state, the vapor of the distillation raw material is discharged from the vapor discharge port 14 provided in the distillation chamber 4 located at the uppermost part on the low pressure part 21 side and supplied to the compressor 28. The compressor 28 to which the steam is supplied pressurizes and compresses the steam and supplies the steam from the distillation supply port 15 to the distillation chamber 4 located at the lowermost part on the high pressure unit 20 side. The compressor 28 pressurizes and supplies steam until each distillation chamber 4 of the high-pressure unit 20 reaches a specified pressure. And the high pressure part 20 side to which the pressure-compressed vapor | steam is supplied becomes high temperature, a temperature difference arises with the low pressure part 21 side, and heat exchange is performed between the high pressure part 20 and the low pressure part 21. By performing this heat exchange, the low temperature portion 21 side is heated, and the distillation raw material in the distillation chamber 4 on the low temperature portion side is heated to promote evaporation.

  Further, the pressure of the staying liquid staying on the high pressure part 20 side is adjusted and supplied to the uppermost distillation chamber 4 on the low pressure part 21 side. Therefore, heat exchange between the high pressure part 20 and the low pressure part 21 is further promoted. Then, the staying liquid stored in the liquid reservoir 7 on the low-pressure part 21 side is heated to promote vaporization, and the generation of steam on the low-pressure part 21 side is promoted.

  Next, the reboiler 23 is operated so that the steam flow rate at the top 6 of the column becomes a specified flow rate, and a total reflux operation is performed in which the total amount of the distillate taken out to the condenser 24 and cooled and condensed is returned to the top 6. Do. Thereafter, while controlling the operation of the compressor 28 and the reboiler 23 so that the steam flow rate at the top 6 is maintained at a specified flow rate, the distillate taken out from the top 6 is withdrawn at a predetermined reflux ratio, and purified by distillation. Get the product.

  As described above, the distillation apparatus according to the present embodiment is configured such that the temperature difference between the high-pressure part 20 side and the low-pressure part 21 side is obtained by pressurizing and compressing steam generated on the low-pressure part 21 side and supplying it to the high-pressure part 20 side. Is further increased, heat exchange between the high-pressure part 20 side and the low-pressure part 21 side is promoted, and the low-pressure part 21 side can be heated using the heat of the high-pressure part 20 side. By transferring heat from the high-pressure part 20 side to the low-pressure part 21 side, the distillation raw material stored in the liquid storage part 7 on the shelf 3 on the low-pressure part 21 side is heated, and the vaporization is performed. Promoted.

  In this way, by using the heat on the high pressure part 20 side to heat the distillation raw material on the low pressure part 21 side, the reboiler 23 that heats and evaporates the distillation raw material supplied from the distillation raw material storage tank 22 is provided. Energy saving can be realized.

  Next, another embodiment of the distillation apparatus according to the present invention will be described. The distillation apparatus according to the present embodiment is an intermediate storage tank that is a further distillation raw material storage tank in which the distillation raw material supplied to the distillation column 1 is stored as shown in FIG. 3 in the distillation apparatus shown in FIG. 31 and a preheater 32 for heating the distillation raw material stored in the intermediate storage tank 31. The distillation raw material stored in the intermediate storage tank 31 is preheated to a constant temperature by the preheater 32 and is supplied to the distillation chamber 4 located at the uppermost part on the low pressure part 21 side of the distillation column 1.

  An operation procedure for distilling and separating a distillation raw material using a distillation apparatus configured as shown in FIG. 3 will be described.

  First, the distillation raw material is charged into the distillation raw material storage tank 22 and the intermediate part storage tank 31. At this time, the distillation raw material is charged into the distillation raw material storage tank 22 and the intermediate storage tank 31 at a ratio of approximately 3: 2. Next, the reboiler 23 is operated to heat the distillation raw material supplied from the distillation raw material storage tank 22 to the tower bottom 5 of the tower main body 2 to generate steam. The distillation raw material vapor rises in the tower body 2.

  Next, after the total reflux operation is in a steady state, the distillation raw material stored in the intermediate storage tank 31 is supplied into the distillation column 1. The distillation raw material supplied from the intermediate storage tank 31 is heated to a constant temperature by the preheater 32 and supplied to the distillation chamber 4 located in the uppermost part on the low pressure part 21 side configured in the distillation tower 1.

  In this distillation apparatus as well, as in the distillation apparatus shown in FIG. 2, vaporization by reheating the distillation raw material and lowering of the liquid distillation raw material are performed at each shelf 3 in the distillation column 1. The liquid is lowered from the lower shelf 3 in a liquid state and is stored in the bottom 5 of the bottom of the distillation column 1.

  And the supply of the distillation raw material stored in the distillation raw material storage tank 22 and the intermediate part storage tank 31 to the distillation column 1 is continued. The distillation raw material stored in the intermediate storage tank 31 is supplied into the distillation column 1 while being heated by the preheater 32.

  In this distillation apparatus as well, in the initial stage of the distillation operation, the distillate is raised to the top 6 of the distillation column 1 in a vapor state, taken out from the vapor outlet 10 of the top 6 and condensed by the condenser 24. A total reflux operation for refluxing the entire amount to the tower top 6 is performed to obtain a steady state in which the state of vaporization of the distillation raw material in the tower body 2 is constant.

  When the inside of the column main body 2 is in a steady state, the vapor of the distillation raw material is discharged from the vapor discharge port 14 provided in the distillation chamber 4 located at the uppermost part on the low pressure part 21 side and supplied to the compressor 28. The compressor 28 to which the steam is supplied pressurizes and compresses the steam and supplies the steam from the distillation supply port 15 to the distillation chamber 4 located at the lowermost part on the high pressure unit 20 side. The compressor 28 pressurizes and supplies steam until each distillation chamber 4 of the high-pressure unit 20 reaches a specified pressure. And the high pressure part 20 side to which the pressure-compressed vapor | steam is supplied becomes high temperature, a temperature difference arises with the low pressure part 21 side, and heat exchange is performed between the high pressure part 20 and the low pressure part 21. By performing this heat exchange, the low temperature portion 21 side is heated, and the distillation raw material in the distillation chamber 4 on the low temperature portion side is heated to promote evaporation.

  Further, in the distillation apparatus of the present embodiment, the staying liquid retained on the high pressure section 20 side is decompressed and supplied to the uppermost distillation chamber 4 on the low pressure section 21 side, and is preheated by the preheater 32. The distillation raw material is supplied from the intermediate storage tank 31. The distillation raw material supplied from the intermediate part storage tank 31 is heated so as to have a certain temperature difference from the high pressure part 20 side. In this way, the distillation raw material is supplied from the high-pressure portion side staying liquid and the intermediate portion storage tank 31, thereby increasing the temperature difference between the high-pressure portion 20 and the low-pressure portion 21, and heat exchange between the high-pressure portion 20 and the low-pressure portion 21. Is further promoted. Then, the staying liquid stored in the liquid reservoir 7 on the low-pressure part 21 side is heated to promote vaporization, and the generation of steam on the low-pressure part 21 side is promoted.

  Next, the reboiler 23 is operated so that the steam flow rate at the top 6 of the column becomes a specified flow rate, and a total reflux operation is performed in which the total amount of the distillate taken out to the condenser 24 and cooled and condensed is returned to the top 6. Do. Thereafter, while controlling the operation of the compressor 28 and the reboiler 23 so that the steam flow rate at the top 6 is maintained at a specified flow rate, the distillate taken out from the top 6 is withdrawn at a predetermined reflux ratio, and purified by distillation. Get the product.

  As described above, the distillation apparatus of the present embodiment also has a high pressure by compressing and compressing the steam generated on the low-pressure part 21 side and supplying it to the high-pressure part 20 side, similarly to the distillation apparatus of the above-described embodiment. The temperature difference between the part 20 side and the low-pressure part 21 side is further increased, and heat exchange between the high-pressure part 20 side and the low-pressure part 21 side is promoted. Can be heated. By transferring heat from the high-pressure part 20 side to the low-pressure part 21 side, the distillation raw material stored in the liquid storage part 7 on the shelf 3 on the low-pressure part 21 side is heated, and the vaporization is performed. Promoted.

  By the way, in the distillation apparatus of the present embodiment, a part of the distillation raw material is supplied from the intermediate reservoir 31 to the distillation chamber 4 located at the uppermost part on the low pressure part 21 side. This distillation raw material is heated to steam by heat exchanged between the high-pressure part 20 and the low-pressure part 21. Therefore, the heat source of the reboiler 23 that heats and evaporates the distillation raw material supplied to the distillation column 1 can be effectively used, and further energy saving can be realized.

  Furthermore, since a part of the distillation raw material can be supplied into the distillation column 1 from the intermediate storage tank 31, and distillation can be performed using the heat in the distillation column 1, the distillation time can be shortened.

  As described above, by using the distillation apparatus according to the present invention, energy saving as the entire distillation apparatus can be realized, and the distillation raw material can be purified with high efficiency.

  In the above-described embodiment, the example using the shelf-type distillation column 1 has been described. However, the present invention is not limited to the above-described example, and a packed material is packed in the column body. It is also possible to use a packed tower in which gas-liquid contact is performed on the surface. Even when this packed tower is adopted, the upper side to which the gas phase distillation raw material compressed by the compressor inside the distillation column is supplied is the high pressure portion, and the lower side of the high pressure portion to which the distillation raw material is supplied Is a low pressure part, and is configured to perform heat exchange between the high pressure part and the low pressure part.

  DESCRIPTION OF SYMBOLS 1 Distillation tower, 2 tower | column main body, 3 shelf, 4 distillation chamber, 7 liquid reservoir part, 8 steam riser pipe, 9 liquid fall pipe, 22 distillation raw material storage tank, 23 reboiler, 24 condenser, 28 compressor, 31 middle Storage tank, 32 preheater

Claims (7)

A distillation column in which distillation raw materials are distilled;
A distillation raw material storage tank in which a distillation raw material supplied into the distillation tower from the bottom side of the distillation tower is stored and a liquid phase distillation raw material lowered to the bottom of the distillation tower is stored;
A reboiler for heating and vaporizing the distillation raw material supplied to the bottom side of the distillation raw material storage tank;
A compressor that pressurizes and compresses the vapor-phase distillation raw material taken out from the middle of the distillation column and returns to the distillation column;
A condenser for condensing the top vapor flowing out from the top of the distillation tower and taking it out;
The upper side to which the gas phase distillation raw material pressurized and compressed by the compressor inside the distillation column is supplied as a high pressure portion, the lower side of the high pressure portion to which the distillation raw material is supplied as a low pressure portion, and the high pressure portion. A batch-type internal heat exchange distillation apparatus characterized in that heat exchange is performed between a section and the low pressure section. The distillation column is provided with a plurality of shelves provided with a liquid drop portion for lowering a liquid-phase distillation raw material and a vapor permeation portion for allowing a vapor-phase distillation raw material to permeate at a predetermined interval. A plurality of distillation chambers partitioned by shelves are configured in the height direction,
A distillation chamber located on the upper side including a distillation chamber to which a distillation raw material in a gas phase pressure-compressed by the compressor inside the distillation tower is supplied is a high-pressure part, and a distillation chamber to which the distillation raw material is supplied 2. The batch type internal heat exchange distillation apparatus according to claim 1, wherein the distillation chamber located on the lower side is a low pressure part, and heat exchange is performed between the high pressure part and the low pressure part.   The batch type internal heat exchange distillation apparatus according to claim 1, further comprising a reflux means for refluxing a part of the top vapor condensed in the condenser to the top of the distillation tower.   The batch-type internal heat exchange distillation apparatus according to claim 1, further comprising a reflux mechanism for refluxing the distillation raw material stored on the tower bottom side of the high pressure part to the tower top side of the low pressure part.   The reflux mechanism is provided with a pressure control valve in the middle of the reflux pipe for refluxing the distillation raw material, and reduces the pressure of the distillation raw material refluxed from the high-pressure part side and supplies it to the low-pressure part side. The batch-type internal heat exchange distillation apparatus according to claim 4.   Provided with a further distillation raw material storage tank for storing the distilled raw material, and further provided with a heating feeder for preheating the additional distillation raw material supplied from the distillation raw material storage tank and supplying it to the top side of the low pressure part A batch-type internal heat exchange distillation apparatus according to any one of claims 1 to 5.   7. The batch-type internal heat according to claim 6, wherein the distillation raw material supplied from the further distillation raw material storage tank is supplied to the tower top side of the low-pressure part in a liquid phase state or a gas-liquid mixed state. Exchange-type distillation equipment.

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