JP2508394Y2 - Chemical reaction vessel reaction temperature control device - Google Patents

Description

[Detailed Description of the Invention] [Industrial field of application] The present invention relates to a reaction temperature control device for a chemical reaction vessel,
More specifically, the present invention relates to a reaction temperature control device that can automatically and sensitively control the temperature inside a reaction container.

[Conventional technology and technical problems to be solved]

Most of the chemical reactions accompanied by heat generation cannot obtain an effective reaction unless the temperature condition is raised more than necessary, but once the reaction occurs, self-heating occurs and the temperature rises randomly. If the temperature rises too much, side reactions may occur at the same time and adverse reaction conditions may result, and in some cases there is even the risk of causing an explosion.

In order to solve such a problem, the heat of reaction may be artificially released to the outside of the reaction system. Then, as a simple means for releasing such reaction heat to the outside, a temperature control jacket is provided around the reaction vessel, and the temperature control solution is circulated in the jacket. There is a method of releasing the heat to the outside by releasing the heat by the same temperature control solution when the temperature rises due to the reaction caused by the reaction. It has already been registered as a utility model as an "apparatus" (Jikkou 3-34274).

However, in the case of this technique, particularly when the heat generation rate associated with the reaction is high, it is necessary to increase the amount of the temperature control liquid or lower the temperature. Moreover, when the reactions do not occur on average over time and the reactions occur randomly and suddenly, the changes in the liquid temperature and the flow rate to be applied are not regular, and therefore the current reactions are being detected accurately. The temperature and contact area of the heat transfer liquid had to be changed, but in the previously proposed device, the contact area with the heat transfer liquid (the surface area of the reaction vessel immersed in the heat transfer liquid)
However, in the case of overreaction, the cooling capacity was insufficient and it was not possible to completely prevent danger. For this reason, in the past, when conducting a reaction experiment on a laboratory scale, unmanning was ideal, and in practice, the experimenter had to rely on his / her actual work, and a long-time chemical reaction could not endure. Moreover, it is common to conduct several reaction experiments on a laboratory scale at the same time, and these experiments are often monitored by one person alone, and there was a risk that an accident could occur due to fatigue or lack of care.

In order to solve such a problem, a forced cooling / heating type automatic temperature control device has been proposed in the past. The forced cooling / heating type automatic temperature control device means that the temperature control solution in the heat exchange tank is circulated in the temperature control jacket around the reaction vessel, and when the temperature of the reaction vessel is lower than a certain temperature, this temperature control solution is used. When the temperature of the reaction vessel is higher than a certain temperature, the cooling water is introduced into the cooling coil tube provided in the heat exchange tank to cool the entire temperature control liquid to cool the reaction vessel. Is. However, this automatic temperature controller cools all the temperature control liquid in the heat exchange tank and lowers the temperature of the reaction vessel, so the response is poor, and when the temperature in the reaction vessel rises sharply, it is not possible to respond and side reactions There was a risk of explosions and explosions, which was dangerous. In the case where the exothermic reaction and the endothermic reaction are sequentially performed in the reaction vessel, if the temperature rises due to the exothermic reaction and cooling is performed by the control device, the endothermic reaction suddenly and violently occurs and the temperature is If it goes down too much, all the temperature-adjusted liquid in the heat exchange tank of the control unit must be warmed to raise the temperature in the reaction vessel, resulting in poor response and the inability to carry out chemical reactions under constant reaction conditions. there were.

The present invention was made in view of the above-mentioned problems in the conventional reaction temperature control method, and the temperature control can be automatically performed even if a person does not constantly monitor it, and the method can be used rapidly. It is a technical subject to provide a practical reaction temperature control device capable of performing a chemical experiment in a safe state even in response to a temperature change.

[Means adopted for solving the problem]

Means adopted by the inventor for solving the problems will be described below with reference to the accompanying drawings.

That is, according to the present invention, the reaction temperature of the chemical reaction container is controlled so that the reaction temperature in the reaction container R can be controlled to a required value by exchanging the temperature adjustment liquid in the temperature adjustment jacket J arranged around the container R. In the management device, a heating tank 1 for heating the temperature adjusting liquid; a cooling tank 2 for cooling the cooling liquid; a temperature in a heat exchange passage 42 communicating with the heating tank 1 in proportion to the amount of the cooling liquid supplied. Heat exchange tank 3 that draws heat from the liquid preparation
And a heat exchange passage 42 for connecting the temperature control jacket J and the heating tank 1 to allow the temperature control liquid in the heating tank 1 to be placed in the heat exchange tank 3 by driving the circulation pump 41. Supply path 4 for supplying to the temperature control jacket J of the reaction vessel R via
And; a reflux path 5 for refluxing the temperature control liquid from the temperature control jacket J to the heating tank 1, and a cooling liquid injection pump 61 is driven to inject the cooling liquid in the cooling tank 2 into the heat exchange tank 3 and the heat exchange tank. An injection path 6 for increasing the liquid level in 3; a conduit member for connecting the cooling tank 2 and the heat exchange 3 to each other, and a flow rate control valve
The flow control valve 73 is controlled to open and close, and when the control valve 73 is opened, the cooling liquid in the heat exchange tank 3 is discharged and recirculated to the cooling tank 2 so that the cooling liquid level can be lowered. A discharge path 7; a temperature sensor 81 having a thermosensitive element 81a in the reaction container R, which sequentially detects the current temperature in the reaction container and outputs a current temperature signal; and a current temperature signal output by the temperature sensor 81. And a temperature controller 8 for controlling opening / closing of the flow rate control valve 73 arranged in the discharge passage 7 when the current temperature signal value deviates from the shiki value.
Temperature control liquid supply temperature sensor 91 disposed in the supply path 4
And the time-dependent chemical reaction data that is progressing in the reaction vessel R based on the measured value signals sent from the temperature control liquid reflux temperature sensor 92 and the flow meter 93 arranged in the reflux path 5. Computer with a function to store and output
The technical feature is that the above-mentioned technical problem is overcome in that a "reaction temperature control device for a chemical reaction container" is configured by integrating the above technical means.

〔Example〕

Hereinafter, the present invention will be described in more detail with reference to the embodiments shown in the accompanying drawings.

The heating tank 1 is provided with a heating heater 11 and a temperature control device 12, the heating tank 1 collects a temperature control liquid (water) in the tank, and the heating heater 11 has a heating part in the heating tank 1 and The temperature control liquid can be heated, and the heating temperature controller 12 can turn on / off the power switch of the heater 11 to keep the temperature control liquid at a constant temperature higher than the below-mentioned condition temperature.

The cooling tank 2 includes a cooling cooler 21 and a cooling temperature controller 22,
The cooling tank 2 stores a cooling liquid (water) in the tank, and a cooling cooler.
21 can take heat from the cooling liquid in the cooling tank 2 to cool it, and the cooling temperature controller 22 can keep the cooling liquid in a required low temperature state.

The heat exchange tank 3 has an injection hole (not shown) at a lower portion of the tank to which an injection pipe of an injection passage 6 described later is jointed, and an overflow prevention pipe 71 of an exhaust passage 7 is jointed at an upper portion of the tank. There is a flow prevention hole (not shown), and a discharge hole (not shown) to which a discharge pipe 72 of a discharge passage 7 described later is jointed at the bottom of the tank.
There is.

The supply passage 4 has a circulation pump 41 and a heat exchange coil pipe 42 interposed in the middle of the supply passage 4. By driving the circulation pump 41, the temperature control liquid in the heating tank 1 is supplied to the temperature control jacket J around the reaction vessel R. The heat exchange coil tube 42 which can be sent out and is a heat exchange path is arranged in the heat exchange tank 3 in the middle of the supply path 4.

The reflux path 5 connects the temperature adjusting jacket J and the heating tank 1 in a watertight state, and causes the temperature adjusting solution in the jacket J to return to the heating tank 1 by the liquid pressure of the temperature adjusting solution sent through the supply path 4. .

The injection path 6 is provided with a cooling liquid injection pump 61, and
The cooling liquid in the cooling tank 2 is poured into the heat exchange tank 3.

The discharge passage 7 includes an overflow prevention pipe 71, a discharge pipe 72, and a flow rate control valve 73. The overflow prevention pipe 71 is located above the heat exchange tank 3 so that the cooling liquid has a constant liquid level in the heat exchange tank 3. When the temperature reaches, the cooling liquid is discharged to prevent the overflow and is returned to the cooling tank 2, and a flow rate control valve 73 whose opening and closing is controlled by the temperature controller 8 is provided in the middle of the pipe. Further, the discharge pipe 72 is connected to the bottom of the heat exchange tank 3, and the cooling liquid in the heat exchange tank 3 can be returned to the cooling tank 2 while the flow rate is adjusted by opening / closing the flow rate adjusting valve 73.

As the temperature controller 8, a controller including a microcomputer is used in the present embodiment, and a safe reaction temperature condition can be input and set as a shiki value in accordance with a chemical substance adopted in the experiment. The temperature controller 8 has a thermosensitive element 81 inserted in the reaction vessel R.
An electric current temperature signal output from the temperature sensor 81 is input based on the current temperature in the reaction container R detected by a. Thus, in the temperature controller 8, the signal value of the current temperature signal input from the temperature sensor 81 is compared with the above-mentioned shiki value, and when the signal value of the present temperature signal is higher than the shiki value, the flow control valve 73 is closed. If the signal value of the current temperature signal is lower than the threshold value, the flow control valve 73 is opened, and the liquid level of the cooling liquid in the heat exchange tank is adjusted up and down accordingly.

Further, the supply passage 4 is provided with a detection portion inside the supply passage 4, and a temperature adjustment liquid supply temperature sensor 91 capable of measuring the temperature adjustment liquid temperature inside the supply passage 4 is provided. A temperature control liquid recirculation temperature sensor 92 that is arranged in the passage 5 and can measure the temperature control liquid recirculation temperature in the recirculation passage 5 is further provided.
A flow meter 93 is provided downstream of 92 so that the flow rate of the temperature control liquid flowing in the reflux passage 5 can be measured as an electric signal. Then, the three types of measurement data values that are continuously output from the temperature sensors 91 and 92 and the flow meter 93 during the reaction are loaded into a computer 94 (in this embodiment, NEC: PC9801), and are stored in advance. Process according to the fixed calculation program. Thus, by this, the reaction heat generation amount for each time can be calculated, and by simultaneously processing the data such as the viscosity in the reaction vessel to be measured at the same time, the time change of the reaction can be confirmed, and the computer 94
Is displayed on a display (not shown), printed out from a printer (not shown), and when an abnormality is detected, an alarm is issued from an alarm device (not shown).

[How to use the apparatus of this embodiment]

The method of using the reaction temperature control device of this example is as follows.

When performing a chemical reaction test in the reaction vessel R incorporated in the apparatus of the present embodiment, the signal value of the current temperature signal output by the temperature sensor 81 based on the generated heat sensed by the thermosensitive element 81a in the reaction vessel R When the temperature in the temperature controller (controller) 8 is lower than the threshold value and the temperature in the reaction vessel R is lower than the condition temperature necessary for the progress of the reaction, the liquid height of the cooling liquid in the heat exchange tank 3 is lowered to lower the cooling liquid. Heat exchange coil tube 42
In order not to submerge, the temperature control liquid having a high temperature in the heating tank 3 is introduced into the temperature control jacket J enclosing the reaction vessel R, and the temperature inside the vessel is raised. On the contrary, when the signal value of the current temperature signal output by the temperature sensor 81 is higher than the shiki value set in the temperature controller 8 and the temperature in the reaction vessel R is higher than the condition temperature suitable for the reaction, The liquid height of the cooling liquid in the heat exchange tank 3 is raised to submerge the heat exchange coil pipe 42 to cool the temperature control liquid in the coil pipe 42, and the cooled temperature control liquid is introduced into the temperature control jacket J for reaction. The temperature inside the container R shall be lowered.

With respect to the progress of the chemical reaction in the reaction vessel R, the computer 94 calculates the amount of heat of reaction generated for each time, and simultaneously processes the data such as the viscosity in the reaction vessel to be measured simultaneously. While the progress of the reaction is automatically calculated over time, confirmed and accumulated,
It is displayed on a display (not shown), is printed out from a printer (not shown), and when an abnormality is detected, an alarm is issued from an alarm device (not shown), so that automatic management can be safely performed.

Although the present embodiment is constructed generally as described above, the present invention is not limited to this embodiment, and various modifications can be made within the "claim for utility model registration". In particular,
The computer 94 controls the operation and stoppage of the injection pump 61 that injects the cooling liquid into the heat exchange tank 3, sets the temperature of the temperature adjusting liquid and the cooling liquid to change with the progress of the reaction, and controls the temperature. You can use silicone oil as the liquid,
Alternatively, it goes without saying that design changes such as integrating the function of the temperature controller 8 into the computer 94 (and vice versa) are within the technical scope of the present invention.

[Effect of the present invention]

As described above with reference to the examples, the present invention is advantageous for reaction experiments using relatively small chemical reaction vessels,
The reaction temperature control device manufactured by applying the present invention is
Even if the chemical reaction is carried out unattended, the reaction temperature can be kept stable.

In addition, unlike the conventional automatic temperature control device, the temperature control liquid is not cooled and heated to control the temperature, but only the amount supplied to the jacket of the temperature control liquid that has been heated in advance is cooled. Since the amount of heat energy of the temperature control liquid to be cooled is small, the temperature in the reaction vessel can be quickly lowered. In addition, since the temperature control liquid in the heating tank is always kept warm to the required heating state, the conversion from cooling to warming is quick and a very excellent response is exhibited.

Therefore, according to the device of the present invention, the ability to respond to changes in reaction temperature is high, and it is advantageous when performing a chemical reaction test involving a side reaction that may lead to overheating or explosion or a sequential reaction having an exothermic or endothermic process. In addition, it can be said that it is excellent in safety because it can prevent an explosion accident.

As described above, according to the present invention, even for a chemical reaction that requires a long time, the reaction temperature can be automatically controlled in an almost unattended state, and a great reduction of monitoring labor can be achieved. In addition, it can be expected to improve safety, and its industrial utility value is extremely high.

[Brief description of drawings]

FIG. 1 is a block diagram schematically showing a reaction temperature control device according to an embodiment of the present invention. 1 ... Heating tank, 2 ... Cooling tank, 3 ... Heat exchange tank, 4 ...
Supply path, 5 ... reflux path, 6 ... injection path, 7 ... discharge path,
8 ... Control device, 11 ... Heater, 12 ... Temperature control device, 21 ... Cooling cooler, 22 ... Temperature control device, 41 ...
Circulation pump, 42 Heat exchange path (heat exchange coil tube), 61
…… Injection pump, 71 …… Overflow prevention pipe, 72 …… Discharge pipe, 73 …… Flow control valve, 81 …… Temperature sensor, 81a ……
Heat sensitive element, 91 ... Temperature control liquid supply temperature sensor, 92 ... Temperature control liquid recirculation temperature sensor, 93 ... Flowmeter, 94 ... Computer, R ... Reaction container, J ... Temperature control jacket.

Claims (1)

(57) [Scope of utility model registration request] 1. The reaction temperature in a reaction vessel R
In a reaction temperature control device for a chemical reaction container in which the temperature control liquid in a temperature control jacket J disposed around the is controlled to a required value, a heating tank 1 for heating the temperature control liquid; A cooling bath 2 for cooling; a heat exchange bath 3 for removing heat from the temperature control liquid in a heat exchange passage 42 communicating with the heating bath 1 in proportion to the amount of the cooling liquid supplied.
And a pipe member that connects the temperature control jacket J and the heating tank 1 to the heat exchange path 42 for arranging the temperature control liquid in the heating tank 1 in the heat exchange tank 3 by driving the circulation pump 41. Supply path 4 for supplying to the temperature control jacket J of the reaction vessel R via
And; a reflux path 5 for refluxing the temperature control liquid from the temperature control jacket J to the heating tank 1, and a cooling liquid injection pump 61 is driven to inject the cooling liquid in the cooling tank 2 into the heat exchange tank 3 and the heat exchange tank. An injection path 6 for increasing the liquid level in 3; a conduit member for connecting the cooling tank 2 and the heat exchange 3 to each other, and a flow rate control valve
The flow control valve 73 is controlled to open and close, and when the control valve 73 is opened, the cooling liquid in the heat exchange tank 3 is discharged and recirculated to the cooling tank 2 so that the cooling liquid level can be lowered. A discharge path 7; a temperature sensor 81 having a thermosensitive element 81a in the reaction container R, which sequentially detects the current temperature in the reaction container and outputs a current temperature signal; and a current temperature signal output by the temperature sensor 81. And a temperature controller 8 for controlling opening / closing of the flow rate control valve 73 arranged in the discharge passage 7 when the current temperature signal value deviates from the shiki value.
Temperature control liquid supply temperature sensor 91 disposed in the supply path 4
And the time-dependent chemical reaction data that is progressing in the reaction vessel R based on the measured value signals sent from the temperature control liquid reflux temperature sensor 92 and the flow meter 93 arranged in the reflux path 5. Computer with a function to store and output
A reaction temperature control device for a chemical reaction container, comprising: