JP2016120461A - Precision distillation refining apparatus and method - Google Patents

Abstract

PROBLEM TO BE SOLVED: To provide a precision distillation refining apparatus and method which heats a distillation object substance to be precisely distilled and refined properly in a short time in the whole process of distillation, can accurately control the heating temperature, thereby, can refine a high-purity distilled product with a preferable yield and is excellent also in energy efficiency.SOLUTION: In a precision distillation refining apparatus having a distillation tower including a boiler part into which raw material to be distilled and refined is charged, a gas-liquid contact part and a condenser part, a plurality of receivers into which respective products as fractions after distillation refining flow through a process line from the distillation tower and a vacuum pump for turning the receivers and the condenser part of the distillation tower into a decompressed state or a vacuum state through a vacuum line as main constituent elements, electromagnetic inductive heating means for performing temperature control respectively independently for the distillation tower, the process line, the receivers and the vacuum line which constitute the distillation refining apparatus is provided such that respective zones can be controlled in optimum temperature conditions in accordance with a kind of the raw material or the product in the whole processes of distillation refining to perform the distillation refining.SELECTED DRAWING: Figure 1

Description

  The present invention relates to distillation purification, and more particularly to a precision distillation purification apparatus suitable for precision distillation purification such as high-purity separation and purification, separation of specific impurities, and separation of isomers, and a precision distillation purification method using the same.

  A mixture that can be evaporated (vaporized) without being decomposed under normal pressure or reduced pressure does not form an azeotrope, and in principle, by distillation at an appropriate temperature and pressure, as long as there is a difference in boiling points, It is known to completely isolate and purify.

  However, when the substance to be distilled is not a liquid but a high melting point solid, heating must be maintained so that it does not solidify not only in the distillation column but also in the process line, vacuum line, receiver, etc. Boiler heating using steam or hot water, which is a heat source, can only deal with solid substances having a melting point of up to about 100 ° C., and if the temperature is higher than that, it is necessary to cope with high-pressure gas regulations. In particular, blockages in process line piping and the like become a problem, and in order to prevent this, a strong heat insulating material and heat insulation measures are required, which also increases apparatus maintenance. Moreover, in the case of a high melting point raw material, it is difficult to heat and evaporate it in a short time in the conventional heating method for a pot such as a reboiler of a distillation tower.

  When steam that is widely used in chemical plants is used as a heat source for distillation, it is necessary to install a steam trap for drainage, which is the main cause of reduced thermal efficiency, and steam must be used in a dry state. If the pressure drops due to pressure loss such as piping resistance, the steam temperature will drop, or the water hammer (water hammer action) will occur if drainage is not performed properly. There is a risk of damage to the equipment.

  For example, Patent Document 1 discloses that an outer tube is provided on the outer wall of the distillation tower and hot air is sent to the outer tube in order to prevent clogging due to polymerization of the distilled substance. Further, Patent Document 2 provides a jacket that surrounds the outer periphery of the distillation tower from an empty portion of the distillation tower to a steam delivery line, and passes a reduced-pressure steam through the jacket, thereby allowing a distilled substance (gas phase) to pass through the cylinder. It is disclosed that the temperature is maintained at a temperature higher than this temperature. However, although Patent Documents 1 and 2 disclose constant heat retention, they do not teach strict temperature control over the entire process line including a distillation column.

  On the other hand, for example, Patent Document 3 discloses that a distillation apparatus is provided with a cooling device in order to prevent a reduction in the recovery rate of the active ingredient due to thermal polymerization during the distillation operation.

  Some heating devices other than boilers use resistance heating means such as nichrome wires in laboratory-level distillation devices, but there are problems such as fires and they cannot be widely used. Patent Document 4 discloses a heating method using a heat medium that can be heated to about 300 ° C. However, there are problems such as high price of silicon oil used as a heat medium and high price of heavy oil and kerosene used as fuel for heating the heat medium.

  Furthermore, attempts have been made to use electromagnetic induction heating as a heating means. For example, Patent Document 5 discloses using electromagnetic induction heating as a heat source instead of a boiler or reboiler of a distillation column. However, Patent Document 5 does not teach the point of heating efficiency over the entire process line. Patent Document 6 discloses electromagnetic induction heating of the evaporation section and the collection section in order to purify a high melting point material (amorphous solid material). However, this is a special horizontal type apparatus mainly for purifying solid materials, and is completely different from a general distillation tower in which reflux is performed. Patent Document 7 discloses using superheated steam generated by electromagnetic induction heating in a rotary heat treatment apparatus (rotary retort furnace) used in the research and development stage. However, Patent Document 7 does not teach application to a general distillation apparatus.

Japanese Patent Publication No. 48-32513 Japanese Patent No. 4095471 Japanese Patent Publication No.62-49916 JP 2008-231053 A Japanese Unexamined Patent Publication No. 7-39745 Japanese Patent No. 5248721 Japanese Patent No. 5401152

  Accordingly, an object of the present invention is to heat a distillation target substance to be precision distilled and purified appropriately and in a short time in the entire distillation process, and to control the heating temperature with high accuracy, thereby yielding a high-purity distilled product. An object of the present invention is to provide a precision distillation purification apparatus and method that can be purified well and that is excellent in energy efficiency.

As a result of intensive studies to solve the above-mentioned problems, the present inventors have found that not only the distillation tower but also the entire distillation apparatus such as a process line is independent by electromagnetic induction heating depending on the raw materials and products to be refined by distillation. The inventors have found that the object can be achieved by precisely controlling the temperature and completed the present invention.
That is, the precision distillation refining apparatus of the present invention is a distillation column having a kettle part, a gas-liquid contact part and a condenser part charged with a raw material to be distilled and purified as a fraction after distillation purification from the distillation tower through a process line. Distillation that constitutes a distillation purification apparatus in a precision distillation purification apparatus mainly comprising a plurality of receivers into which each product flows and a vacuum pump for bringing the condenser section of the distillation tower into a vacuum or vacuum state through a vacuum line The tower, process line, receiver, and vacuum line are equipped with electromagnetic induction heating means that independently control the temperature, and each zone is controlled to the optimum temperature condition according to the type of raw materials and products in the entire distillation purification process. It is possible to refine by distillation.

  Further, in the precision distillation purification method of the present invention, the raw material to be distilled and purified is charged into the distillation tower of the precision distillation purification apparatus, the kettle portion of the distillation tower is heated to a predetermined temperature by an electromagnetic induction heating means, and evaporated. Gas-liquid contact, temperature-controlled by electromagnetic induction heating means, gas-liquid contact, rectification, condensing in condenser, condensed fraction taken out from distillation tower via process line and received by receiver That the distillation column and the process line are depressurized by a vacuum pump connected to the vacuum line, and the process line, the vacuum line and the receiver are each independently provided by at least one electromagnetic induction heating means. And the valve is controlled so that the receiver receives fractions with different boiling ranges.

According to the present invention, each of the distillation pot, process line, vacuum line and receiver constituting the distillation purification apparatus is equipped with precision heating means for independently controlling the temperature by electromagnetic induction heating means, and in all the steps of distillation purification, Since each zone (location) is controlled to the optimum temperature conditions according to the type of raw materials and products, it is possible to refine the distillation, so that the substance to be distilled can be heated appropriately and in a short time at all locations in the distillation process. The heating temperature can be strictly controlled. Therefore, a high-purity fraction (distilled product) can be purified with a high yield, and the energy efficiency can be greatly improved as compared with the conventional boiler method, and the contribution to energy saving is also remarkable.
It can be widely applied to fields that require precision distillation purification, such as high-purity separation and purification, separation of specific impurities, and separation of isomers. This is particularly effective in precision distillation purification on an experimental scale at universities and research institutions.

Overall structure diagram showing an example of the precision distillation purification apparatus of the present invention Overall structure diagram showing an example of a conventional distillation purification device

  The precision distillation purification apparatus of the present invention has a distillation tower, process line, receiver, vacuum line and vacuum pump as main components, and the distillation tower, process line, vacuum line and receiver can each be controlled independently. Equipped with a simple electromagnetic induction heating means. The distillation column has a raw material charging section, a kettle section, a gas-liquid contact section, and a condenser section, and the kettle section and the gas-liquid contact section are each provided with electromagnetic induction heating means capable of independently controlling the temperature. ing. The distillation column may be a continuous distillation column or a batch distillation column. The pot portion may be of a reboiler type or a type of heating the tower bottom from the outside. The distillation column may be made of metal, glass, or a material lined with glass, resin, or the like, but the part to be electromagnetically heated is preferably made of metal.

  Such electromagnetic induction heating means generates heat by flowing a high-frequency current through an induction coil disposed around the heat generating material. The frequency of the high-frequency current is generally 50 to 500 Hz, but may be a commercial frequency. The exothermic temperature is preferably one that can be applied from room temperature up to about 700 ° C. and can be controlled with an accuracy of 0.1 ° C. The dielectric coil may be detachable at each attachment site.

  In order to perform distillation purification by controlling the optimum temperature conditions in the entire distillation purification process by such electromagnetic induction heating means, the distillation tower, process line, vacuum line and receiver are each made of materials that can generate heat by the electromagnetic induction heating means. It has a configured heat generating part.

  The electromagnetic induction heating means as the heat generating part is necessary for the distillation tower, process line, vacuum line, and zone (location) that requires temperature control or heating of the receiver, and the entire main components generate heat by the electromagnetic induction heating means. It is preferable to be composed of materials that can be used, but as long as distillation purification can be performed by controlling each part to the optimum temperature conditions according to the type of raw materials and products in the entire distillation purification process, temperature control is performed on each component. The portion requiring the heat treatment may be partially made of a heat generating material. In the case of a distillation tower, it has a kettle part, a gas-liquid contact part and a condenser part, but the whole including the kettle part, the gas-liquid contact part and the condenser part may be composed of a heat generating material, or the kettle part and the gas-liquid contact. Only the portion may be made of a heat generating material. The heat generating part may be arranged in a plurality of zones from the bottom to the top in the gas-liquid contact part, and the temperature may be controlled independently in each zone of the gas-liquid contact part. In the gas-liquid contact portion, the tower main body can be used as a heat generating material. However, when a filler (regular arrangement or irregular arrangement) is present, the filler may be used as a heat generating material. The condenser part normally does not need to be heated because it performs a condensation function in reflux distillation, but from the viewpoint of precise temperature control of the entire distillation process, the condenser part may also serve as a heating part. The kettle and the gas-liquid contact section of the distillation column each have at least one electromagnetic induction heating means, but it is not necessary to use all of the heating as electromagnetic induction heating, and it may be partially heated by steam heating or the like. . However, it is preferable to use electromagnetic induction heating for the entire heat source of the pot portion.

The process line is a line through which a fraction flows, and heating is necessary when the fraction has a high melting point. Also in the case of the process line, the heat generating part may be arranged in a plurality of zones in the reflux line or the receiver line. Each receiver into which a fraction (distilled product) flows also has a heat generating part that can be temperature controlled independently for each receiver depending on the fraction, but it is not necessary for all receivers to have it. , At least one is sufficient. For example, a part of the receiver may be heated by steam heating or the like. The same applies to piping in the process line, and a part of the piping may be heated by steam heating or the like.
The distillation column is reduced in pressure or vacuum through a vacuum line from a vacuum pump, but this vacuum line is also likely to be heated because there is a risk of clogging when the fraction has a high melting point, At least a part is electromagnetic induction heating.
In this way, the temperature of each zone (location) can be precisely controlled (in increments of 0.1 ° C) by electromagnetic induction heating means in all distillation purification processes. It becomes possible to purify.

  The raw materials to be distilled and purified are charged into the distillation tower, and after reflux distillation by gas-liquid contact, flow into each receiver via the process line for each fraction, but the temperature of the distillation tower, process line and receiver The temperature is precisely controlled by the electromagnetic induction heating means provided at each location so that the temperature decreases sequentially toward the downstream side of the distillation process. When distilling a target substance having a high melting point or freezing point, a fraction (distilled product) can be obtained without solidification by heating the process line to a predetermined temperature above the freezing point by electromagnetic induction heating means. it can.

  As described above, the material used for the electromagnetic induction heating means of the heating section of the distillation column and process line which is the main component of the distillation purification apparatus of the present invention is the material of the distillation column itself and the material of the piping of the process line itself. It is preferable that heat is generated by electromagnetic induction heating means. In this case, it is preferable to use an inert material for the raw material and fraction to be distilled and purified. Moreover, it is good also considering only the inner side which contacts a distillate as an inert material. The shape of the heat generating portion formed of such a heat generating material is not limited, and can be applied to various distillation towers and receivers, for example, cylindrical or flask-shaped distillation pots, cylindrical or rectangular parallelepiped receivers. The material that is inert to the distillation target substance means that it does not react with the distillation target substance under the distillation purification conditions, and that the distillation target substance does not react with the compound that is decomposed during distillation purification. It does not have a catalytic action for decomposition reactions such as these and other components, and does not contaminate purified substances subject to distillation, and does not react with atmospheric gases such as oxygen gas that is touched during use or rest including. For example, even if a metal is oxidized and rusted and this is physically peeled off and contaminates the purified distillation target substance, it cannot be said that it is an inert material for the distillation target substance. The degree of slight contamination of the substance to be distilled is not allowed.

  Examples of materials that can generate heat by such electromagnetic induction heating means include metals and ceramics having electromagnetic properties. Iron is generally used as the metal magnetic material, but stainless steel or the like is preferable from the viewpoint of long-term stability. Examples of materials that are inert to the material to be distilled include metals, glass, ceramics, and high heat resistant resins. Some substances to be distilled may react with materials constituting the distillation purification apparatus, be denatured by metal catalytic action, or may be contaminated by impurities derived from metals. For this reason, it is preferable to prevent contamination by coating the inner surface using an inert material, or to use an inert material such as magnetic ceramics as a heating element.

  The precision distillation purification apparatus and precision distillation purification method of the present invention can be applied to various precision distillation purifications. Separation and purification of high purity, such as separation and purification of compounds with a boiling point difference of around 1 ° C to 99.9%, separation of specific impurities, such as separation of impurities in the order of ppm and ppb, separation of isomers, such as ortho It can be applied to separation into para, iso and normal, and cis and trans. In addition, it is applicable not only to liquid distillation target substances, but also to high-melting-point solid distillation target substances, and is excellent in yield and energy efficiency.

  Hereinafter, embodiments of the present invention will be described with reference to the drawings. FIG. 1 is an overall structural diagram showing an example of a precision distillation purification apparatus of the present invention. For comparison, FIG. 2 shows an overall structural diagram showing an example of a conventional distillation purification apparatus. 1 and 2, the same reference numerals indicate the same components. In the conventional apparatus, the process line 2 has a double piping structure in order to heat with steam from a boiler (not shown).

The precision distillation purification apparatus shown in FIG. 1 includes a distillation tower 1, a process line 2, a vacuum line 3, a receiver 4 and a vacuum pump 5 as main components. The distillation column 1 has a pot portion 11 located at the bottom, a gas-liquid contact portion 12 located at the center, where a filler is present, and a condenser portion 13 at the top. The distillation raw material is charged from the raw material charging section 14, but in the case of a batch-type distillation tower, the raw material charging section 14 may be shared with the residual tank outlet 15 at the bottom of the tower that becomes the kettle section. . At the lower part of the condenser section 13, there is a fraction outlet 16, which is connected to each receiver 41, 42 or 43 via the process line 2. A valve is provided in front of each receiver and is controlled so that a fraction in a predetermined temperature range flows in. For example, the first fraction or a fraction close thereto is flowed into the receiver 41, the middle fraction having a higher boiling range is flowed into the receiver 42, and the high boiling fraction having a higher boiling range is flowed into the receiver 43. An outlet is provided in the lower part of each of the receivers 41, 42, 43, and the outlet is taken out by opening the valve.
It should be noted that one of the valves before and after the receiver is preferably closed during operation so that the entire distillation purification apparatus including the distillation tower 1 is maintained at a reduced pressure.
The process line 2 and the receivers 41, 42, 43 are connected to the vacuum line 3 and connected to the vacuum pump 5. Similarly, the condenser section 13 of the distillation tower 1 is connected to the vacuum pump 5 through the vacuum line 3. These vacuum lines 3 are provided with a header 31 and a trap 32 in front of the vacuum pump 5. In the trap 32, a normal temperature solid component is removed by passing a gas through the cleaning liquid.

The pot portion 11 and the gas-liquid contact portion 12 of the distillation tower 1 each have heating means, and at least a part of the pot portion 11 and the gas-liquid contact portion 12 is the electromagnetic induction heating means 6. The amount of heat to be supplied may be supplied by steam or the like, and the electromagnetic induction heating means 6 may be used to finely adjust the temperature, or the total amount of heat may be supplied by the electromagnetic induction heating means 6.
The process line 2, the vacuum line 3 and the receivers 41, 42 and 43 need to be kept warm or heated when distilling high melting point raw materials, etc., but at least a part of this heat is supplied by electromagnetic induction heating means 6. To do. Then, at least a part of the process line 2 may be heated by the electromagnetic induction heating means 6, for example, the heat of the process line 2 may be supplied by the electromagnetic induction heating means 6, and the other may be supplied by steam or the like. The same applies to the vacuum line 3, and the same applies to the receivers 41, 42 and 43. The electromagnetic induction heating means 6 (61, 62, 63, 64) provided in these places is preferably detachable.
The material for the electromagnetic induction heating is preferably a heat-generating material such as iron, and an induction coil is disposed on the outer periphery thereof. A thermocouple and a power supply control device for adjusting voltage and the like are provided for precise control of temperature. The power supply control device is connected to an AC power supply, converts this into high-frequency power, outputs it to the induction coil, and can control supply power by a signal from a thermocouple. The induction coil and temperature controller used for electromagnetically heating the heat-generating material may be those used in conventionally known electromagnetic induction devices. In order to heat the distillation column 1, the process line 2, the vacuum line 3 and the receiver 4 to a predetermined temperature, the induction coil is installed so as to surround the outer periphery thereof with a predetermined length. In this way, it is possible to quickly and precisely heat a part that needs to be heated by a distillation purification apparatus by electromagnetic induction heating.For example, a temperature rising rate is high from about several minutes to about 60 minutes for raising the temperature from room temperature to 400 ° C., and The accuracy of temperature control can also be increased.

  A method for purifying a substance to be distilled containing impurities using the precision distillation purification apparatus of FIG. 1 will be described. Distillation raw material is charged into the distillation tower 1, and induction coils as electromagnetic induction heating means 61 are arranged around each heating part of the pot 11, gas-liquid contact 12 and condenser 13, and are independently induced from an AC power source. When an alternating current is passed through the coil, heat is generated by the heat generating material, and distillation is started in a state in which the pot portion 11, the gas-liquid contact portion 12 and the condenser portion 13 are temperature-controlled at respective predetermined temperatures. For example, when several fractions are obtained by batch distillation, the temperature of the pot 11, the temperature of the gas-liquid contact unit 12, and the temperature of the condenser 13 are gradually increased, and the target fraction is extracted from the outlet 16. . Temperature control is performed by a power supply control device connected to a thermocouple. The temperature control by the power supply control device can be performed by turning on / off the AC power supply or controlling the inverter.

The first fraction from the outlet 17 enters the first fraction receiver 41 via the process line 2. When the fraction becomes the second fraction having a higher boiling point, the valve connected to the receiver 41 is closed, and the valve connected to the receiver 42 is opened via the process line 2 and placed in the receiver 42. Similarly, when the third fraction is reached, it is placed in the receiver 43. Repeat this if there are many types of fractions, but if the receiver 41 is replaced with another receiver or cleaned during distillation, the number of receivers and the number of process lines should be minimized. Is possible.
The receivers 41, 42, 43 and at least a part of the process line 2 connected to the receiver are temperature-controlled by electromagnetic induction heating means 62. These are preferably controlled independently.

  The vacuum line 3 is also heated and kept warm. At least a part of the vacuum line 3 is temperature-controlled by electromagnetic induction heating means 63. These are preferably controlled independently.

  Therefore, in the entire distillation process, the electromagnetic induction heating means 61, 62, 63, 64 are used for each zone (location) of the distillation tower 1, the process line 2, the vacuum line 3, and the receiver 4 (41, 42, 43). It is possible to control the temperature appropriately for distilling and extracting the distillation raw material. That is, optimum temperature management is possible for each point of the distillation process. Therefore, the loss of thermal energy is extremely reduced, and the thermal efficiency is remarkably improved. This is in contrast to steam heating by a boiler.

  Even when the substance to be distilled is a high melting point substance, electromagnetic induction is performed in the same manner as the electromagnetic induction heating means 61 of the distillation pot 1 for each part of the process line 2, the vacuum line 3 and the receiver 4 (41, 42, 43). The temperature is controlled by the heating means 62, 63, and 64 so that it is controlled to be lower than the boiling point and higher than the melting point in the distilling component outflow process so as not to solidify.

  After completion of distillation purification or during distillation purification, the objective purified fraction collected in the receiver 4 is recovered as a product.

1 Distillation tower
11 Kettle
12 Gas-liquid contact area
13 Condenser section
2 Process line
3 Vacuum line
31 header
32 traps
4, 41, 42, 43 Receiver
5 Vacuum pump
6, 61, 62, 63, 64 Electromagnetic induction heating means

Claims (2)

  A distillation tower having a kettle part, a gas-liquid contact part and a condenser part charged with raw materials to be distilled, a plurality of receivers into which each product as a fraction after distillation purification flows from the distillation tower through a process line; and In a precision distillation refining apparatus mainly comprising a vacuum pump for reducing the pressure or vacuum state through a vacuum line for the condenser part of the distillation tower, the distillation tower, process line, receiver, and vacuum line constituting the distillation refining apparatus In addition, it is equipped with electromagnetic induction heating means that independently control the temperature, and it is possible to perform distillation purification by controlling each zone to the optimum temperature condition according to the type of raw materials and products in all distillation purification processes. A precision distillation refining device.   The raw material to be distilled is charged into the distillation tower of the precision distillation purification apparatus according to claim 1, the kettle of the distillation tower is heated to a predetermined temperature by the electromagnetic induction heating means and evaporated, and the temperature is heated by the electromagnetic induction heating means. Gas-liquid contact in the controlled gas-liquid contact section, rectification, condensation in the condenser section, extraction of the condensed fraction from the distillation tower via the process line and reception at the receiver, distillation tower and process The pressure of the line is reduced by a vacuum pump connected to the vacuum line, and the process line, the vacuum line and the receiver are each independently temperature controlled by electromagnetic induction heating means provided in at least one place, And a valve is controlled so that the receiver receives fractions having different boiling ranges.

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