JP2020131057A - Rotary evaporator - Google Patents

Abstract

To accurately detect a liquid level in a distillation flask or a distillate recover flask and to enable continuous operation of a rotary evaporator.SOLUTION: A first optical fiber sensor 28, of which a tip 28a is located at a lower limit management position of a liquid level, is provided in a distillation flask 14, the first optical fiber sensor 28 emits a signal to a control part 25 after a mixed liquid in the distillation flask 14 reduces, the tip 28a thereof leaves the liquid level from the liquid immersion state, and a set time has lapsed, and the control part 25 operates an electromagnetic valve 15 on the basis of the signal, and supplies the mixed liquid into the distillation flask 14. A second optical fiber sensor 29, of which a tip 29a is located at an upper limit management position of the liquid level, is provided in a distillate recover flask 19, the second optical fiber sensor 29 emits a signal to the control part 25 after a distillate in the distillate recover flask 19 increases, the tip 29a thereof immerses into the distillate, and a set time has lapsed, and the control part 25 operates a distillate discharge pump 22 on the basis of the signal, and discharges the distillate from the distillate recover flask 19.SELECTED DRAWING: Figure 1

Description

The present invention relates to a rotary evaporator. Specifically, the evaporation flask containing the mixed solution is heated while rotating, and the vapor evaporated from the mixed solution is introduced into a cooler to cool the various components in the mixed solution. It relates to a rotary evaporator used for separation and concentration.

Conventionally, as a rotary evaporator, a mixed liquid container for accommodating a mixed liquid, a mixed liquid supply line for supplying the mixed liquid from the mixed liquid container to a distillation flask, a vacuum pump for vacuuming the inside of the rotary evaporator system, and a vacuum state. A driving means for rotating the distillation flask, a heating bath for heating the distillation flask, a cooler for cooling the vapor evaporated from the mixed solution, and a distillate recovery for storing the distillate condensed by the cooler. Some were provided with a flask and a distillate discharge pump for discharging the distillate from the distillate recovery flask into the distillate recovery container (see, for example, Patent Document 1).

JP-A-2009-106819

Rotary evaporators such as the above-mentioned Patent Document 1 are required to enable continuous operation in order to increase the amount of processing. For that purpose, the liquid level of the mixed solution in the distillation flask and the distillation of the mixed solution are required. There was a need for a means to detect the liquid level of the distillate in the liquid recovery flask. However, in various switches such as a float type liquid level switch conventionally used as a liquid level detecting means, for example, bubbles generated when a mixed solution is injected into a distillation flask and liquid level turbulence due to rotation of the distillation flask , It was difficult to accurately detect the liquid level due to changes in the viscosity, temperature, color, capacitance, etc. of the mixed liquid due to distillation.

Therefore, an object of the present invention is to provide a rotary evaporator that can accurately detect the liquid level of the mixed liquid in the distillation flask and the liquid level of the distillate in the distillate recovery flask and enable continuous operation. There is.

In order to achieve the above object, the rotary evaporator of the present invention includes a mixed liquid supply line for supplying the mixed liquid from a mixed liquid container containing the mixed liquid to a distillation flask, an electromagnetic valve provided in the mixed liquid supply line, and the like. A vacuum pump that creates a vacuum inside the rotary evaporator system, a driving means that rotates the distillation flask in the vacuum state, a heating bath that heats the distillation flask, and a cooler that cools the vapor evaporated from the mixed solution. A rotary evaporator equipped with a distillate recovery flask for storing the distillate condensed by the cooler and a distillate discharge pump for discharging the distillate from the distillate recovery flask into the distillate recovery container. A first optical fiber sensor, which is airtightly inserted into the distillation flask and whose tip is arranged at a lower limit control position of the liquid level, is provided, and the first optical fiber sensor reduces the amount of mixed liquid in the distillation flask. A signal is sent to the control unit after the tip portion leaves the liquid surface from the immersion state and a set time elapses. Based on the signal, the control unit operates the electromagnetic valve, and the mixed liquid is placed in the distillation flask. Is provided, and a second optical fiber sensor is provided which is airtightly inserted into the distillate recovery flask and whose tip is arranged at the upper limit control position of the liquid level. The second optical fiber sensor is the distillate recovery flask. The amount of distillate in the flask increases, the tip of the flask infiltrates into the distillate, and after a lapse of a set time, a signal is sent to the control unit, and the control unit operates the distillate discharge pump based on the signal. It is characterized in that it is provided with a second optical fiber sensor that discharges the distillate from the distillate recovery flask to the distillate recovery container.

Further, it is preferable that at least the portion of the first optical fiber sensor and the second optical fiber sensor to be inserted into the rotary evaporator is coated with fluororesin.

Further, it is preferable that the operating times of the solenoid valve and the distillate discharge pump can be set individually.

According to the rotary evaporator of the present invention, when the mixed solution in the distillation flask is reduced to a predetermined amount or less by the first optical fiber sensor, the electromagnetic valve is opened and the inside of the distillation flask is in a vacuum state. The mixture can be automatically introduced into the distillation flask. Further, since the tip of the first optical fiber sensor leaves the liquid surface from the immersion state and sends a signal to the control unit after a set time elapses, the mixed liquid in the distillation flask is mixed when the vacuum rises at the initial stage of distillation or when the mixture is mixed. It is possible to reliably detect the liquid level without being affected by bubbles or liquid level turbulence generated when additional liquid is supplied, or the concentration or change of the mixed liquid, and the liquid volume of the mixed liquid is always maintained at an appropriate level. be able to.

Furthermore, when the amount of distillate in the distillate recovery flask increases to a predetermined amount or more by the second optical fiber sensor, the distillate discharge pump operates to automatically discharge the distillate from the distillate recovery flask. Can be discharged. Further, since the tip of the second optical fiber sensor penetrates into the distillate and operates after the set time has elapsed, it is affected by the turbulence of the liquid level generated by the return of air bubbles from the piping on the distillate discharge pump side. The liquid level can be reliably detected without any trouble, and the amount of the distillate can be maintained at an appropriate level at all times.

This enables continuous operation of the rotary evaporator, which was not possible in the past, and it is now possible to process a relatively large volume of mixed solution with a small-scale rotary evaporator, reducing the equipment installation space and reducing the equipment installation space. , The processing process can be reduced, the cost can be reduced, and the distillation quality can be stabilized by continuous operation.

It is explanatory drawing of the rotary evaporator which shows one embodiment of this invention. Similarly, it is explanatory drawing which shows the distillate recovery flask and the distillate discharge pump. Similarly, it is sectional drawing of the introduction pipe of the mixed liquid supply line and the introduction part which introduces the 1st optical fiber sensor. Similarly, it is a cross-sectional view of a main part of a distillation flask when distilling a mixed solution.

1 to 4 are diagrams showing an example of a form of the rotary evaporator of the present invention. The rotary evaporator 11 of this embodiment is provided in the mixed liquid container 12 for accommodating the mixed liquid, the distillation flask 14 in which the mixed liquid is injected from the mixed liquid container 12 via the mixed liquid supply line 13, and the mixed liquid supply line 13. The electromagnetic valve 15 provided, the driving means 16 for rotating the distillation flask 14, the heating bath 17 for heating the distillation flask 14, and the steam evaporated from the distillation flask 14 and led out from the distillation flask 14 are cooled and condensed. The distillate recovery flask 19 for collecting the distillate condensed by the cooler 18, and the distillate recovery flask 19 for leading the distillate from the distillate recovery flask 19 to the distillate recovery container 20. Inside the line 21, the distillate discharge pump 22 and the check valve 23 provided in the distillate recovery line 21, the distillation flask 14, the cooler 18, and the distillate recovery flask 19 (inside the rotary evaporator system). It is provided with a vacuum pump 24 for reducing the pressure of the flask, a controller 24a for controlling the degree of vacuum, and a control unit 25 for continuously operating the rotary evaporator 11.

The distillation flask 14 is fixed in an oblique state with the connection port facing upward, and the bottom side is arranged in the heating bath 17. The connection port is airtightly connected to the lower end of the drive means 16 provided with the rotary joint 26 internally via a connector 26a, and a branch pipe 27 branched in a substantially cross shape is airtightly connected to the upper end of the drive means 16. It is connected. In the branch pipe 27, the cooler 18 is airtightly connected to the upper part, the distillate recovery flask 19 is connected to the lower part, the driving means 16 is airtightly connected to one side, and the mixed liquid is airtightly connected to the other side via the packing 27a. An introduction portion 27b through which the introduction pipe 13a of the supply line 13 penetrates is formed.

The mixed liquid supply line 13 extends from the mixed liquid container 12 to the introduction portion 27b of the branch pipe 27 via the solenoid valve 15, and the introduction pipe 13a provided at the tip penetrates the packing 27a to the introduction portion 27b. Is airtightly inserted into the branch pipe 27 and the driving means 16, and further airtightly inserted into the distillation flask 14 via the connector 26a. Further, the tip of the introduction pipe 13a is bent toward the inner wall below the distillation flask 14.

Further, the first optical fiber sensor 28 led out from the control unit 25 is airtightly inserted into the distillation flask 14 in a state of being bound to the introduction pipe 13a. The first optical fiber sensor 28 is a photoelectric sensor that emits light such as visible light or infrared light from a light projecting unit and detects light reflected by a detection object or a change in the amount of light to be shielded by a light receiving unit to obtain an output signal. At least, the branch pipe 27, the driving means 16, and the portion introduced into the distillation flask 14 are coated with a pipe-shaped fluororesin, and the tip portion 28a is sealed with the fluororesin in a conical shape.

The tip portion 28a of the first optical fiber sensor 28 includes a light receiving portion, is arranged at a lower limit control position of the liquid level, and is usually in an immersion state. When the amount of the mixed solution in the distillation flask 14 is reduced, the tip 28a leaves the liquid surface and after a lapse of a set time, a signal is sent to the control unit 25, and the control unit 25 presses the solenoid valve 15 based on the signal. Since it opens and the inside of the distillation flask 14 is in a vacuum state, the mixed solution is automatically sucked into the distillation flask 14.

The distillate recovery flask 19 is connected to the pipe 21a of the distillate recovery line 21 at the bottom, and the pipe 21a is connected to the suction port of the distillate discharge pump 22. A pipe 21b connected to the distillate recovery container 20 is connected to the discharge port of the distillate discharge pump 22 via a check valve 23.

Further, the second optical fiber sensor 29 led out from the control unit 25 is airtightly inserted into the distillate recovery flask 19. The second optical fiber sensor 29 is a photoelectric sensor similar to the first optical fiber sensor 28, and at least the portion introduced into the distillate recovery flask 19 is coated with a pipe-shaped fluororesin, and the tip portion 29a is made of fluororesin. It is sealed in a conical shape.

The tip portion 29a of the second optical fiber sensor 29 is provided with a light receiving portion, and the tip portion is arranged at an upper limit control position of the liquid level, and is usually in a state of not contacting the liquid level. When the amount of distillate in the distillate recovery flask 19 increases, the tip 29a comes into contact with the liquid surface, and after a lapse of a set time, a signal is sent to the control unit 25, and the control unit 25 is based on the signal. Operates the distillate discharge pump 22 to automatically discharge the distillate from the distillate recovery flask 19 into the distillate recovery container 20.

In the above-described embodiment, the control unit 25, the first optical fiber sensor 28, the solenoid valve 15, the second optical fiber sensor 29, and the distillate discharge pump 22 form a control circuit for continuous operation. There is.

Next, an operation method for recovering distilled water by distilling tap water using the rotary evaporator 11 described above will be described. First, as the operating conditions of the rotary evaporator 11, the degree of vacuum is 53 hPa, the temperature of the heating bath 17 is 70 ° C., the rotation speed of the distillation flask 14 is 100 rpm, and the temperature of the cooling water introduced into the cooler 18 is 10 ° C. The tap water introduced into the distillation flask 14 begins to evaporate at 35 ° C., and the rotation of the distillation flask 14 promotes evaporation. When evaporation is promoted and the liquid level is lowered, the tip 28a of the first optical fiber sensor 28 is exposed from the liquid immersion state, and when a preset time (2 to 10 seconds) elapses, a signal is sent to the control unit 25. The control unit 25 opens the solenoid valve 15 for a set time based on this signal, and automatically introduces tap water into the distillation flask 14.

The tap water in the distillation flask 14 violently foams due to the degassing phenomenon of the gas contained in the tap water when the vacuum rises at the initial stage of distillation and when tap water is additionally supplied. Further, the rotation of the distillation flask 14 may cause shaking or turbulence on the liquid surface, but the first optical fiber sensor 28 operates after a preset time has elapsed after the tip 28a is exposed from the liquid surface. Therefore, there is no risk of malfunction such as chattering.

Further, when the vapor is condensed and liquefied by the cooler 18, the distillate that has flowed down into the distillate recovery flask 19, reaches the set liquid level, the tip 29a of the second optical fiber sensor 29 reaches the liquid level. When the infiltration has elapsed and a preset time (2 to 10 seconds) has elapsed, a signal is sent to the control unit 25, and the control unit 25 operates the distillate discharge pump 22 based on this signal to discharge the distillate. It is automatically discharged to the distillate collection container 20.

Since the tip 29a of the second optical fiber sensor 29 enters the distillate and operates after a preset time has elapsed, the liquid level is raised by the return of air bubbles from the pipe 21a of the distillate recovery line 21. Even if it is disturbed, it will not be affected by it.

As described above, according to the rotary evaporator of this embodiment, the liquid surface sways, foams, foams, droplets, and changes in liquid concentration, color, and viscosity, as well as changes in capacitance and temperature. The liquid level in the distillation flask 14 and the liquid level in the distillate recovery flask 19 are accurately detected by the first optical fiber sensor 28 and the second optical fiber sensor 29 without being affected, and the liquid amount is always appropriate. Since it can be maintained at the above level, continuous operation of the rotary evaporator, which was not possible in the past, has become possible. As a result, the equipment installation space of the rotary evaporator 11 can be reduced, the processing process can be reduced, the cost can be reduced, and the distillation quality can be stabilized.

11 ... rotary evaporator, 12 ... mixed liquid container, 13 ... mixed liquid supply line, 13a ... introduction pipe, 14 ... distillation flask, 15 ... electromagnetic valve, 16 ... driving means, 17 ... heating bath, 18 ... cooler, 19 ... Distillate recovery flask, 20 ... Distillate recovery container, 21 ... Distillate recovery line, 21a, 21b ... Piping, 22 ... Distillate discharge pump, 23 ... Check valve, 24 ... Vacuum pump, 25 ... Control unit, 26 ... rotary joint, 26a ... connector, 27 ... branch pipe, 27a ... packing, 27b ... introduction unit, 28 ... first optical fiber sensor, 28a ... tip portion, 29 ... second optical fiber sensor, 29a ... tip portion

Claims (3)

A mixed liquid supply line that supplies the mixed liquid from the mixed liquid container that houses the mixed liquid to the distillation flask, an electromagnetic valve provided in the mixed liquid supply line, a vacuum pump that creates a vacuum in the rotary evaporator system, and a vacuum. A driving means for rotating the distillation flask in the state, a heating bath for heating the distillation flask, a cooler for cooling the vapor evaporated from the mixed solution, and a distillate for storing the distillate condensed by the cooler. A rotary evaporator equipped with a distillate recovery flask and a distillate discharge pump for discharging distillate from the distillate recovery flask into a distillate recovery container.
A first optical fiber sensor that is airtightly inserted into the distillation flask and arranges the tip portion at the lower limit control position of the liquid level is provided, and the first optical fiber sensor reduces the mixed liquid in the distillation flask and the tip portion. Leaves the liquid surface from the liquid immersion state and emits a signal to the control unit after a lapse of a set time, and based on the signal, the control unit operates the electromagnetic valve to supply the mixed solution into the distillation flask. ,
A second optical fiber sensor that is airtightly inserted into the distillate recovery flask and whose tip is arranged at the upper limit control position of the liquid level is provided, and the second optical fiber sensor is used for the distillate in the distillate recovery flask. Increases, the tip portion infiltrates into the distillate, and after a lapse of a set time, a signal is emitted to the control unit, and the control unit operates the distillate discharge pump based on the signal to distill off the distillate. A rotary evaporator characterized by comprising a second optical fiber sensor for discharging the distillate from the liquid recovery flask into the distillate recovery container. The rotary evaporator according to claim 1, wherein the first optical fiber sensor and the second optical fiber sensor are characterized in that at least a portion inserted into the rotary evaporator is coated with a fluororesin. The rotary evaporator according to claim 1 or 2, wherein the operating time of the solenoid valve and the distillate discharge pump can be set individually.

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