JP2001252501A - Distillation apparatus - Google Patents

Abstract

PROBLEM TO BE SOLVED: To provide a distillation apparatus for enabling the detection of a control element with a sensor to enable the distillation of a solvent without requiring a number of persons or cost. SOLUTION: In the distillation apparatus wherein a round-bottomed flask 11 storing an organic solvent is heated by a mantle heater 12 and the vapor generated from the round-bottomed flask 11 is guided to cooling pipes 43, 45 to be cooled and liquefied, the liquid surface monitor pipe 18 made of transparent glass allowed to communicate with the round-bottomed flask 11 in order to detect the liquid surface level of the organic solvent stored in the flask 11 is vertically provided and a first optical sensor 20 is arranged to the outer periphery of the liquid surface monitor pipe 18 at the position corresponding to the liquid surface level of the flask 11 and, when the first optical sensor 20 detects the presence of the solvent through the glass pipe, a heating means is controlled on the basis of the detection signal of the optical sensor.

Description

DETAILED DESCRIPTION OF THE INVENTION

[0001]

TECHNICAL FIELD The present invention relates to a distillation apparatus for distilling and separating an organic solvent and the like.

[0002]

2. Description of the Related Art For example, an organic solvent used for extracting a sample or the like contains many impurities and cannot be reused as it is. For this reason, in the past, except for refining in some large-scale plants, most of them were disposed of in small-scale research facilities. However, easy disposal may adversely affect the environment. In particular, halogen-based organic solvents should easily generate harmful substances when incinerated. There were various problems such as costs involved in disposal. Therefore, it has been desired to purify these used organic solvents at each small-scale facility or the like using a distillation apparatus. Here, the minimum basic components of the distillation apparatus are a heater, a heating vessel, and a cooling apparatus that collects steam evaporated from the heating vessel and cools the same (generally, cooling water is circulated through a glass cooling pipe). ) Is required.

[0003]

However, small-scale facilities do not have large-scale plants or personnel, and therefore have the following problems. 1) It is troublesome to constantly monitor control elements such as the amount of the solvent in the heating vessel, the internal pressure, and the flow rate of the cooling water during the distillation. Difficulty. 2) Of course, it is not impossible to equip the distillation apparatus with various sensors for detecting control elements, but if these sensors are directly exposed to an organic solvent, the sensors will be corroded or damaged. For this reason, at present, used organic solvents are not sufficiently purified in small-scale research facilities. The present invention has been made to solve the problems involved in the conventional technology. It is an object of the present invention to provide a distillation apparatus which enables detection of a control element by a sensor and thereby enables distillation of a solvent without adding labor or cost.

[0004]

Means for Solving the Problems According to the first aspect of the present invention, there is provided a container made of light-transmitting glass for storing a solvent, heating means for heating the container, and heating of the heating means. The liquid level of the solvent stored in the container in a distillation apparatus including a conduit for guiding the vapor generated from the container by the conduit, and a cooler connected to the conduit for cooling and liquefying the introduced vapor. A first optical sensor is disposed at an outer peripheral surface position corresponding to the liquid level in the container to detect the level, and when the first optical sensor detects the presence or absence of the solvent through the container, a detection signal is output. The gist of the present invention is that the heating means is controlled based on the following. In such a configuration, the first optical sensor is disposed at a position corresponding to the liquid level of the container on the outer periphery of the container made of light-transmitting glass, and the first optical sensor is disposed at a position corresponding to the liquid level of the container, for example, a target to be distilled. The first optical sensor is disposed at a position corresponding to the lowest liquid level at which the solvent does not become empty. Here, the type and system of the optical sensor are not limited as long as it converts light energy into an electric signal. In addition, the optical sensor is a concept including an infrared sensor. The first optical sensor detects the presence or absence of a solvent through the same container, and when the state changes from a state in which the solvent is detected to a state in which the solvent is not detected, that is, when the solvent is reduced by evaporation, the first light sensor is used. The optical sensor outputs a detection signal. Based on the detection signal, the heating unit is controlled in a direction to suppress the heating. Here, suppression is a concept that also includes stopping. Also,
It does not only mean that the first optical sensor is actually disposed on the same horizontal plane as its position. For example, if it is difficult to dispose the first optical sensor at the lowest liquid level position in the above example, the first optical sensor is provided at a slightly upper position, for example, a clock circuit is provided, and the control operation mode is set after a lapse of a fixed time after detection. It is also possible.

According to the second aspect of the present invention, a container for storing the solvent, a heating means for heating the container, a conduit for guiding steam generated from the container by heating the heating means, and a conduit connected to the conduit. In a distillation apparatus having a cooler that cools and liquefies the introduced steam, a bypass pipe communicating with the vessel is set up to detect a liquid level of the solvent stored in the vessel, A first optical sensor is disposed on the outer periphery of the bypass conduit at a position corresponding to a liquid level of the container, and at least the bypass conduit at a position where the first optical sensor is disposed has a light transmitting property. The gist is that the heating means is controlled based on a detection signal when the first optical sensor detects the presence or absence of the solvent through the glass conduit. And In such a configuration, the first optical sensor is disposed at a position corresponding to the liquid level of the same vessel on the outer periphery of the bypass pipe, and the bypass pipe at that position is at least a glass pipe made of light-transmitting glass. . The entire bypass pipeline may be a glass pipeline. Then, the first optical sensor is provided at a position corresponding to the liquid level of the container, for example, at a position corresponding to the lowest liquid level at which the solvent to be distilled does not become empty. The concept of the optical sensor is the same as described above. The first optical sensor detects the presence or absence of a solvent through the glass pipe, and when the state is changed from the state in which the solvent is detected to the state in which the solvent is not detected, that is, when the solvent is reduced by evaporation, the first optical sensor is used. One optical sensor outputs a detection signal. Based on the detection signal, the heating unit is controlled in a direction to suppress the heating. Here, suppression is a concept that also includes stopping. Further, it does not mean that the first optical sensor is actually arranged on the same horizontal plane as the position. For example, if the position of the connection of the bypass line to the container is higher than the bottom of the container, the first optical sensor is provided slightly above the bottom of the container. It is also possible to switch to the control operation mode after a certain time has elapsed.

According to the third aspect of the present invention, the first or second aspect is provided.
In addition to the configuration of the invention, a manometer filled with a liquid for detecting the pressure in the container is connected to the container, and a second optical sensor is provided at a position on the outer periphery of the manometer for detecting a predetermined pressure. The manometer at least at the position where the second optical sensor is provided is constituted by a glass conduit made of light-transmitting glass, and the second optical sensor detects the presence or absence of the liquid through the glass conduit. Then, the gist is that the heating means is controlled based on the detection signal. In such a configuration, in addition to the effect of the invention of claim 1 or 2, a second optical sensor is disposed at a position corresponding to the liquid level of the container on the outer periphery of the manometer, and the manometer at that position is at least light-transmitting. It is a glass pipeline made of glass. The entire manometer may be a glass conduit. Then, the second optical sensor is disposed at a position corresponding to a predetermined pressure in the container. The concept of the optical sensor is the same as described above. The second optical sensor detects the presence / absence of a liquid through the glass conduit, and detects that the liquid inside the container has become too large above a predetermined value. When the state of detecting the liquid is detected, or when the state of detecting the liquid is changed to the state of not detecting the liquid (any of these may be considered depending on the arrangement position of the second optical sensor), the second light The sensor outputs a detection signal. Based on the detection signal, the heating unit is controlled in a direction to suppress the heating. Here, suppression is a concept that also includes stopping. Further, the heating means does not need to be controlled immediately based on the detection signal from the second optical sensor. For example, it is also possible to provide a clock circuit and set the control operation mode after a lapse of a predetermined time after detection.

According to a fourth aspect of the present invention, in addition to the configuration of any one of the first to third aspects of the present invention, the cooler indirectly cools the steam by circulating a refrigerant across a partition wall. Along the way from the inlet to the outlet of the refrigerant pipe for supplying the refrigerant, a glass pipe made of light-transmitting glass is formed, and a third optical sensor is provided on the outer periphery of the glass pipe. The gist is that when the optical sensor of No. 3 detects the presence or absence of the same refrigerant in the same glass conduit, the heating means is controlled based on the detection signal. In such a configuration, in addition to the function of the first or second aspect of the present invention, a third optical sensor is provided in a portion formed by a glass pipe around the refrigerant pipe. The position of the third optical sensor is not limited as long as the third optical sensor is located in the glass channel portion. Here, the concept of the optical sensor is the same as described above. Third, the presence or absence of refrigerant through the same glass pipe
The third optical sensor outputs a detection signal when it is determined that the supply of the refrigerant has stopped because the optical sensor has detected the refrigerant and has stopped detecting the refrigerant from the state where the refrigerant has been detected.
Based on the detection signal, the heating unit is controlled in a direction to suppress the heating. Suppression is a concept that also includes suspension. Also,
The heating means does not need to be controlled immediately based on the detection signal from the third optical sensor. For example, it is also possible to provide a clock circuit and set the control operation mode after a lapse of a predetermined time after detection. According to a fifth aspect of the present invention, in addition to the configuration of the fourth aspect, the third optical sensor is disposed after a curved pipe portion formed immediately before the refrigerant pipe outlet and the same outlet. . In such a configuration, in addition to the operation of the third aspect of the invention, when the supply of the refrigerant is stopped, the refrigerant is retracted in the bent tube portion which is provided upright, so that the refrigerant is not detected from the state in which the refrigerant is reliably detected. You can see that

[0008]

According to the first aspect of the present invention, the first
Is disposed around the outer periphery of the container made of light transmissive glass to detect the presence or absence of the solvent through the glass, so that the first optical sensor is not exposed to the solvent,
Since the optical sensor does not corrode or break, the monitoring of the amount of the solvent can be automated. Claim 2
In the invention described in (1), the first optical sensor is disposed in a glass pipe made of light-transmitting glass, and the presence or absence of a solvent is detected from the outer periphery through the glass. As a result, the first optical sensor is not corroded or damaged, so that the monitoring of the amount of the solvent can be automated. According to the invention described in claim 3, in addition to the effect of the invention described in claim 1, the second aspect
Is disposed in the glass conduit of a manometer made of light-transmitting glass, and the presence or absence of a liquid is detected from the outer periphery of the manometer through the glass, so that the second optical sensor is exposed to solvent vapor. Since the second optical sensor is not immersed in the liquid in the manometer and does not corrode or break, the monitoring of the pressure in the container can be automated. . According to the invention described in claim 4, in addition to the effects of the invention described in claim 1 or 2, the third optical sensor is disposed in a glass pipe made of light-transmitting glass, and the third optical sensor is passed through the glass from the outer periphery thereof. Since the presence or absence of the refrigerant is detected, the third optical sensor is not immersed in the refrigerant,
Since the third optical sensor is not corroded or damaged, monitoring of the cooling state can be automated. According to the invention described in claim 5, in addition to the effect of the invention described in claim 4, it is possible to reliably detect that the supply of the refrigerant has stopped.

[0009]

An embodiment of the present invention will be described below with reference to FIGS. As shown in FIG. 1, an eggplant flask 11 with a branch (hereinafter simply referred to as a flask 11) is provided in a mantle heater 12. The flask 11 includes first to third branch pipes 13 to 15.
A drain pipe 16 is formed to project downward from the lower part of the flask 11, and the drain pipe 16 is provided with a drain cock 17. A liquid level monitoring pipe 18 extends laterally from the drain pipe 16. The liquid level monitoring pipe 18 is an upright pipe section 19 made of an upright transparent cylindrical glass pipe.
It has. The upper part of the standing pipe part 19 is open. A first optical sensor 20 is provided at a position on the outer periphery of the standing pipe portion 19 and substantially corresponding to a bottom position of the flask 11. A first thermocouple 21 as a temperature sensor is inserted into the flask 11 from the opening 13 a of the first branch pipe 13. The first thermocouple 21 is surrounded by a protective tube (not shown) to prevent corrosion. Second
The opening 14a of the branch pipe 14 serves as an inlet for a used organic solvent. In the opening 14a, a stirrer 22 is disposed above the main opening 11a of the flask 11. The stirrer 22 is a motor 23 and an output shaft of the motor 23 (not shown).
, And the rod 24 is inserted into the flask 11 through the main opening 11a. A rotating body 25 is fixed to the tip of the rod 24. The main opening 11a and the openings 13a and 14a of the first and second branch pipes 13 and 14 are closed with a ground glass stopper (not shown).

The third branch pipe 15 is connected to a branching forked pipe 26. The first branch pipe 27 of the forked pipe 26 has the first
A rectification tower 28 is connected via a cock 27a, and a water removal pipe 30 is connected to the second branch pipe 29 via a second cock 29a. The rectification tower 28 is for condensing the vapor introduced from the third branch pipe 15 and condensing the distilled low-boiling component (here, an organic solvent). Water removal tube 3
The first cooling pipe 31 is connected to the upper part of the “0”. The cooling pipe 31 includes an inner pipe IT and an outer pipe OT surrounding the inner pipe IT. The outer pipe OT has a cooling water inlet IP for introducing and discharging cooling water and a cooling water outlet OP. In addition, the inner pipe IT is also used for all the cooling pipes described below.
In addition, the outer pipe OT, the cooling water inlet IP and the cooling water outlet OP are formed, but they are overlapped, and only the illustration is shown, and the description is omitted. In addition, a steam inlet and a steam outlet are also formed in each cooling pipe, but these will be described as necessary. A second cooling pipe 33 is connected to the branch pipe 32 of the forked pipe 26. A manometer 34 is connected to the second cooling pipe 33. The manometer 34 is constituted by a pair of parallel transparent glass pipes connected in parallel and connected at the lower part, and is shaped like a hairpin. A funnel 35 is connected to the end of the manometer 34. Water (which may be tap water) is supplied into the manometer 34, and the water level fluctuates in response to the internal pressure of the flask 11. In FIG. 1, a second optical sensor 36 is provided on the outer periphery of the glass conduit on the right side.

At the upper part of the rectification column 28, a deformed connecting pipe 37 is provided.
Is connected. A second thermocouple 40 as a temperature sensor is inserted into the first branch pipe 38 from the opening 38a of the first branch pipe 38 of the deformed connection pipe 37. The second thermocouple 40 is surrounded by a protective tube (not shown) to prevent corrosion. A head cooling pipe 43 is connected to the second branch pipe 41 of the deformed connection pipe 37. The head cooling pipe 43 is arranged horizontally with a slight inclination. A final-stage cooling pipe 45 is connected to the third branch pipe 44 of the modified connection pipe 37. A cock 46 is provided in the middle of the third branch pipe 44.

Next, a circulation path of cooling water from a cooling water supply means (not shown) (for example, water supply) to each cooling pipe will be described. The cooling water outlet OP and the cooling water outlet OP of each cooling pipe are connected by a rubber tube R. As shown in FIG. 1, the cooling water is supplied from a cooling water inlet to a rubber tube R.
Through the cooling water inlet IP of the second cooling pipe 33 and further into the adjacent first final-stage cooling pipe 45. The cooling water further introduced into the first cooling pipe 31 from the last cooling pipe 45 is led to the head cooling pipe 43 and then the rubber tube R
Is introduced into the curved pipe portion 47 and further led to the cooling water outlet. The curved tube portion 47 is composed of a pair of standing glass conduits connected at the upper portion and bent in a hairpin shape. A branch pipe 48 is connected to the curved pipe section 47, and a check valve 49 is connected to the end of the branched pipe 48 at a position substantially the same as the uppermost position of the bent pipe section 47. A third optical sensor 50 is disposed on the outer periphery of a transparent cylindrical glass pipe connecting the curved pipe part 47 and the branch pipe 48.

Next, an outline of the distillation of the distillation apparatus having the above-described configuration will be described. The used organic solvent stored in the flask 11 is heated by the mantle heater 12. The mantle heater 12 includes first and second thermocouples 21,
Control is performed with a target temperature set at 40 as a temperature sensor. At the beginning of heating, the first cock 27a is closed and the second cock 29a is open. The vapor of the organic solvent containing water that has been heated and rises rises from the third branch pipe 15 and the second branch pipe 29 toward the moisture removal pipe 30, and is cooled by the first cooling pipe 31. The organic solvent containing condensed water is separated from the water in the water removing tube 30 and only the organic solvent is returned to the flask 11. Here, the pre-distillation of the water removal is completed. Next, the process proceeds to main distillation. Contrary to the pre-distillation, the first cock 27a is opened and the second cock 2
Close 9a. Then, the organic solvent in the flask 11 from which water has been removed is heated again. The vapor of the organic solvent containing water that has been heated and rises rises from the third branch pipe 15 and the first branch pipe 27 to the rectification tower 28. Low-boiling substances (organic solvent) obtained by removing high-boiling substances in the rectification column 28 and shrinking them
Is guided to the head cooling pipe 43 above the rectification tower 28 via the modified connecting pipe 37. The organic solvent is introduced into the inside through the vapor inlet 43a of the head cooling pipe 43, and when cooled and liquefied, it drip from the same vapor inlet 43a and travels along the third branch pipe 44 of the deformed connecting pipe 37 to be disposed further below. To the final cooling pipe 45. In addition, the cock 46 is turned to turn the third branch pipe 44.
The reflux ratio can be adjusted by changing the previous pressure. The cooled purified organic solvent is discharged from the solvent outlet 45a of the final-stage cooling pipe 45. At this time, if the internal pressure of the flask 11 increases, the manometer 3
The distilled water in 4 receives the pressure change, and the water level in the right glass pipe (the side where the second optical sensor 36 is disposed) in FIG. Further, when the supply of the cooling water is interrupted, the cooling water is not drained even if the cooling water is not circulated, unless the cooling water inlet is opened, and the cooling water is discharged into each rubber tube R and the cooling pipes 31, 33, 43. , 45. However, since the outside air is introduced into the curved pipe portion 47 by the check valve 49, the cooling water after the curved pipe portion 47 is drained, and the cooling water does not stay in the curved pipe portion 47. Therefore, it is possible to detect the presence or absence of the cooling water of the third optical sensor 50 at this position.

Next, the electrical configuration of the apparatus will be described. As shown in FIG. 2, the control device 51 including various memories and arithmetic devices includes the first to third sensors 20 and 3.
6, 50, the first and second thermocouples 21, 40, the mantle heater 12, and the motor 23 are connected. Furthermore, LEDs 53 to 5 for sensors, mantle heaters and motors
5, a timer 56, a temperature controller 57, and a notification buzzer 58 as notification means are connected. The LED 53 is turned on when the control device 51 determines that a detection signal has been output from each of the sensors 20, 36, and 50. Each sensor 20, 3
The LEDs 53 are divided every 6, 50. The LED 54 is turned on when the mantle heater 12 is operating normally. The LED 55 is turned on when the motor 23 is operating normally. Timer 56 sets the maximum distillation time. The temperature controller 57 sets the temperature of the mantle heater 12. The determination as to whether or not the temperature has been reached is made by the first and second thermocouples 21 and 40. Information buzzer 5
Numeral 8 is sounded when the mantle heater 12 is stopped according to the input of the sensor.

Next, the processing operation of the present distillation apparatus will be described with reference to the flowchart of FIG. The following processes are performed by an interrupt process executed every 2 ms until one of the optical sensors 20, 36, 50 is turned on. In step S1, the control device 51 determines whether the first optical sensor 20 is on. Here, if it is still in the OFF state, it is determined that there is still the organic solvent in the container 11, and the process proceeds to step S2. On the other hand, if it is determined to be on, it is determined that the organic solvent has evaporated and disappeared, and it is determined in step S3 whether the flag F1 is set, that is, whether or not the flag F1 is "1". If the flag F1 is not "1" (that is, "0"), the flag F1 is set to "1" in step S4. Then, in step S5, the process is suspended until one minute is measured by a clock circuit (not shown) in the control device 51. On the other hand, when it is determined in step S3 that the flag F1 is "1", it is determined that the first optical sensor 20 was in the ON state one minute before, and the process proceeds to step S6 for the first time. The device 51 stops the mantle heater 12 and the motor 23. In addition, at step S7, the LE for the first optical sensor 20 is used.
D53 is turned on, conversely, the LEDs 54 and 55 indicating the operating state of the mantle heater 12 and the motor 23 are turned off, and the notification buzzer 58 is sounded, and the process is terminated. As described above, the determination once again after the lapse of one minute is that even when the organic solvent is still in the container 11, the liquid level may be erroneously detected due to the vibration or the stirring of the stirrer 22. It is possible.

On the other hand, if it is determined that the first optical sensor 20 is still in the off state and the process proceeds to step S2, it is determined whether or not the second optical sensor 36 is on. Here, if it is still in the off state, it is determined that the internal pressure of the container 11 is within the predetermined range, and the process proceeds to step S8. On the other hand, if it is determined that the switch is on, it is determined that the internal pressure has exceeded the predetermined range, and step S9
It is determined whether the flag F1 is set, that is, whether it is "1". If the flag F1 is not "1", the flag F1 is set to "1" in step S10.
Stand up. Then, in step S11, the control device 5
It is held until 30 seconds are measured by a clock circuit (not shown) in 1. On the other hand, if it is determined in step S9 that the flag F1 is "1", it is determined that the second optical sensor 36 is in the ON state 30 seconds before, and the process first proceeds to step S12 to perform control. The device 51 stops the mantle heater 12 and the motor 23. Step S1
In step 3, the LED 53 for the second optical sensor 36 is turned on, the LEDs 54 and 55 indicating the operating states of the mantle heater 12 and the motor 23 are turned off, and the notification buzzer 58 is sounded, and the process is terminated. The reason why the determination is made once again after the elapse of 30 seconds is that, for example, when the pressure has not been sufficiently stabilized, it may be detected that the pressure accidentally becomes equal to or higher than a predetermined value.

On the other hand, if it is determined that the second optical sensor 36 is still in the off state and the process proceeds to step S8, it is determined whether the third optical sensor 50 is on. Here, if the cooling water is still in the off state, it is determined that the cooling water is circulating smoothly, and the processing is temporarily terminated, and the apparatus enters a standby state for normal interrupt processing. On the other hand, if it is determined to be on, it is determined that the supply of the cooling water has been interrupted, and it is determined in step S14 whether the flag F1 is set, that is, whether or not the flag F1 is "1". If the flag F1 is not "1", "1" is set to the flag F1 in step S15. And
In step S16, the process is suspended until the clock circuit (not shown) in the control device 51 measures 15 seconds. On the other hand, if it is determined in step S14 that the flag F1 is "1", it is determined that the third optical sensor 50 was in the ON state 15 seconds before, and the process first proceeds to step S17 to perform control. The device 51 includes the mantle heater 12 and the motor 23.
To stop. At the same time, in step S18, the LED 53 for the third optical sensor 50 is turned on, and conversely, the mantle heater 1 is turned on.
Then, the LEDs 54 and 55 indicating the operating state of the motor 2 and the motor 23 are turned off, and the notification buzzer 58 is sounded, and the process is terminated. The determination once again after the elapse of 15 seconds is to avoid a case where it is determined that the supply of the cooling water has been stopped due to a temporary decrease in the water pressure, mixing of bubbles, or the like.

With this configuration, the present embodiment has the following advantages. (1) Even if the used organic solvent in the flask 11 is not visually observed to evaporate during distillation, the solvent is monitored by the first optical sensor 20 attached to the liquid level monitoring tube 18 because the solvent is monitored. Since the mantle heater 12 can be turned off when it runs out, it is not necessary to constantly arrange personnel near the distillation apparatus, which contributes to cost reduction. (2) Since the first optical sensor 20 can detect the presence or absence of the solvent in the flask 11 in the atmosphere without being immersed in the solvent, the first optical sensor 20 can be prevented from being corroded or broken due to the detection. . (3) The first optical sensor 20 is mounted on the liquid level monitoring tube 18 and the flask 11 accommodated in the mantle heater 12
No need to attach to the bottom. Therefore, the first optical sensor 2
0 can be easily attached and the mantle heater 1
No exposure to the heat of 2. Further, fine mounting can be easily performed because the mounting member is attached to the rod-shaped standing pipe portion 19 as described above. (4) Even if it is not visually observed that the internal pressure in the flask 11 increases during the distillation, the second optical sensor 36 attached to the manometer 34 monitors this, so that personnel are always present near the distillation apparatus. This eliminates the need for arrangement, which contributes to cost reduction.

(5) Since the second optical sensor 36 is mounted on the outer periphery of the manometer 34 in the atmosphere, the second optical sensor 36 is passed through the distilled water or the second cooling pipe 33 to the manometer 34. The second optical sensor 36 is not exposed to any solvent vapor, and there is no risk of corrosion or failure of the second optical sensor 36 due to the exposure. (6) Since the third optical sensor 50 is mounted on the outer periphery of the curved tube part 47 in the atmosphere, the third optical sensor 50 is not exposed to the cooling water, and the corrosion caused by the exposure ( There is no risk of rust or failure. Further, the trouble of disposing the third optical sensor 50 in flowing water is eliminated. (7) When the supply of the cooling water is interrupted The cooling water in the curved tube portion 47 at the position of the third optical sensor 50 is reliably retracted by the curved tube portion 47, so that the supply of the cooling water is surely interrupted. Can be detected. (8) The control device 51 controls the first to third sensors 20, 36,
Even if any of the detection signals 50 is received, the mantle heater 12 and the motor 23 are not stopped immediately, but a confirmation operation of waiting a predetermined time just in case is performed. Therefore, the mantle heater 12 and the motor 23 do not stop even if the detection signal is erroneously recognized only once in some time.

The present invention can be embodied with the following modifications. -Although the 1st optical sensor 20 was provided in the erected tube part 19, you may comprise so that this may be attached to the flask 11. FIG. However, since the bending rate and transmittance of the mounting surface may vary depending on the mounting position, a cylindrical body such as a cylindrical shape in which the bending rate and transmittance of the lower part of the container does not change is preferable. -The joining height of the liquid level monitoring tube 18 with the flask 11 can be changed. If the internal pressure of the flask 11 is almost constant, the second optical sensor 36 is not necessarily required. -If the supply of the cooling water is interrupted, the internal pressure of the flask 11 is increased, so that the supply of the cooling water is indirectly interrupted by the second optical sensor 36. Therefore, the third optical sensor 50 is not always necessary. -If it is a simple distillation apparatus, the rectification column 28 as described above is unnecessary. The steam is cooled in a plurality of stages, but the number of stages can be changed. The heating means may be other than the mantle heater 12. -The shape of the manometer 34 is not limited to the above. -All the components constituting the distillation apparatus do not need to be made of transparent glass. At least in the present invention, the optical sensors 20, 36, and 50 only need to be partially transparent, as long as the difference in the internal state can be determined from the outer periphery at that position. In addition, since the term “transparent” means that light can be transmitted, glass having a certain degree of fogging may be used. In the flowchart of the above embodiment, one minute is set in step S5, 30 seconds is set in step S11, and 15 minutes is set in step S16.
After waiting for a second, the detection signal is detected again. However, this waiting time can be freely changed. Further, in the above embodiment, the detection signal is detected again only once, but may be detected twice or more. In addition, the present invention can be freely implemented without departing from the gist of the present invention.

Other technical ideas of the present invention that can be grasped from the above embodiment will be described below as additional notes. (1) A detection signal from the optical sensor is output to a control unit, and the control unit controls the heating unit based on input of the detection signal a predetermined number of times at a predetermined time. The distillation apparatus according to claim 1. (2) The distillation apparatus according to any one of claims 1 to 5, wherein the control means controls the heating means, and notifies the control means by a notification means.

[0022]

[Brief description of the drawings]

FIG. 1 is a conceptual configuration diagram of a distillation apparatus according to an embodiment of the present invention.

FIG. 2 is a block diagram illustrating an electrical configuration of the same distillation apparatus.

FIG. 3 is a flowchart illustrating a processing operation of the same distillation apparatus.

[Explanation of symbols]

11: Eggplant flask with branches as container, 12: Mantle heater as heating means, 15: Third branch pipe, 18 ...
Liquid level monitoring tube as a bypass line, 20: first optical sensor, 26: bifurcated tube, 28: rectification tower, 34: manometer,
36: a second optical sensor, 37: a deformed connecting pipe, 43: a head cooling pipe, 45: a final cooling pipe, 47: a curved pipe section as a refrigerant pipe, 50: a third optical sensor.

 ──────────────────────────────────────────────────続 き Continued on the front page (71) Applicant 500117440 Koichi Suzui 2-4-1, Ryumiminami, Okazaki City, Aichi Prefecture (71) Applicant 500116443 Kazuhiro Kobayashi 222, Yamanecho, Tenpaku-ku, Nagoya City, Aichi Prefecture (71) Applicant 500118160 Seiko Kondo 346 1 Yasyu-cho, Okazaki-shi, Aichi (71) Applicant 500116753 Kiyonori Kato 44-44, Tokoro-Ako, Fujikawa-cho, Okazaki-shi, Aichi Prefecture (72) Inventor Tadakazu Komaru 1803 Sakurasaku, Nagakute-cho, Aichi-gun, Aichi Prefecture (72) Inventor Tomonori Toyoda 3-8-11 Tatsumi-minami, Okazaki-shi, Aichi Prefecture (72) Inventor Koichi Suzui 2-Tatsumi-minami, Okazaki-shi, Aichi Prefecture No. 4 1 (72) Inventor Kazuhiro Kobayashi 222, Yamane-cho, Tempaku-ku, Nagoya City, Aichi Prefecture (72) Inventor Seiko Kondo 346, 1 Yasui-cho, Okazaki City, Aichi Prefecture (72) Inventor Kato Law Okazaki, Aichi Prefecture Fujikawa-cho Pass ARACO 44 address 24 F-term (reference) 4D076 AA12 BA02 BC03 CA19 EA02X EA02Y EA04X EA04Y EA06X EA12X EA13Y EA14X EA15X EA15Y EA16X HA03 HA14

Claims (5)

[Claims] 1. A container made of light-transmitting glass for storing a solvent, a heating unit for heating the container, a conduit for guiding vapor generated from the container by heating the heating unit, and a connection to the conduit. A cooling device for cooling and liquefying the introduced steam, wherein an outer peripheral surface position corresponding to the liquid level in the container for detecting the liquid surface level of the solvent stored in the container. A first optical sensor, and when the first optical sensor detects the presence or absence of the same solvent through the same container, the first optical sensor controls the heating means based on the detection signal. Distillation equipment. 2. A container for storing a solvent, a heating unit for heating the container, a conduit for guiding steam generated from the container by heating the heating unit, and a vapor connected and introduced to the conduit. In a distillation apparatus having a cooler that cools and liquefies, a bypass line communicating with the container is set up to detect a liquid level of the solvent stored in the container,
A first optical sensor is disposed on the outer periphery of the bypass conduit at a position corresponding to the liquid level of the container, and at least the bypass conduit at a position where the first optical sensor is disposed is formed of light-transmitting glass. And wherein the first optical sensor detects the presence or absence of the solvent through the glass conduit and controls the heating means based on the detection signal. Distillation equipment. 3. A manometer filled with a liquid for detecting a pressure in the container is connected to the container, and a second optical sensor is provided at a position on the outer periphery of the manometer for detecting a predetermined pressure. At least the manometer at the position where the second optical sensor is provided is constituted by a glass conduit made of light-transmitting glass, and when the second optical sensor detects the presence or absence of the liquid through the glass conduit, The distillation apparatus according to claim 1, wherein the heating unit is controlled based on a detection signal. 4. The cooling device is of a type in which a vapor is indirectly cooled by circulating a refrigerant through a partition wall, and a light transmitting portion is provided on the way from an inlet to an outlet of a refrigerant pipe for supplying the refrigerant. A third optical sensor is provided on the outer periphery of the glass conduit, and the third optical sensor detects the presence or absence of the refrigerant in the glass conduit. The distillation apparatus according to any one of claims 1 to 3, wherein the heating unit is controlled based on a detection signal. 5. The distillation apparatus according to claim 4, wherein the third optical sensor is disposed after a curved pipe portion formed immediately before the refrigerant pipe outlet and the refrigerant pipe outlet.