JPH04277033A - Apparatus for automatically controlling chemical reaction - Google Patents

Abstract

PURPOSE:To automatically control a chemical reaction experiment by connecting a plurality of chemical reactors to a computer to monitor the reaction states of the respective reactors by said computer and controlling the cooling, heating and chemical liquid dropping mechanisms of the respective chemical reactors on the basis of the monitoring by the computer. CONSTITUTION:A plurality of chemical reactors A'-having cooling, heating and chemical liquid dropping mechanisms are connected to a computer CPU 1. The computer monitors the reaction states of the respective chemical reactors and, on the basis of this monitoring, the cooling, heating and chemical solution dripping mechanisms of the respective reactors are controlled by the computer. As a result, a chemical reaction experiment can automatically be controlled. Especially, when many experiments are simultaneously performed, the marked conservation of labor is achieved. Reaction control is really practical over various reaction conditions, the recording and storage of various data, safe control or the like.

Description

[Detailed description of the invention]

0001

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to an automatic chemical reaction management system that can manage the reaction conditions of a plurality of chemical reaction tanks at once, and is particularly useful when conducting reaction tests.

0002

BACKGROUND OF THE INVENTION The chemical properties of many atoms or aggregates thereof change significantly due to slight changes in the orbits of electrons flying around the outside. For this reason, even if the same chemical substances are mixed and reacted, changes in conditions such as temperature, pressure, molar concentration ratio, presence or absence of catalyst, etc. will cause the reaction rate, reaction process, and products after the reaction to differ. be.

[0003] Therefore, the productivity when producing substances by chemical reactions must be greatly influenced by the reaction conditions of the reactions. Therefore, it is strongly desired to carry out the reaction under more preferable reaction conditions, but to do so, it is necessary to conduct numerous experiments and collect data.

[0004] The development of new chemical substances also begins by conducting reaction experiments under conditions different from those used up until now.

[0005] However, these chemical reaction experiments often last several hours or more, and in today's shortage of engineers, there tends to be a shortage of human resources to actually conduct the experiments.

[0006]

[Problems to be Solved by the Invention] The present invention was made in view of the problem of lack of manpower in conventional experiment execution. The technical challenge is to provide the following.

[0007]

[Means for Solving the Problems] In the present invention, the temperature inside a plurality of chemical reaction tanks each equipped with a cooling mechanism, a heating mechanism, a stirring mechanism, a chemical liquid dropping mechanism, a vacuum pressure control mechanism, etc. is controlled. , vacuum pressure, calculated rotational torque of the stirring mechanism,
Collect information such as elapsed time, and based on this information,
Chemistry that automatically performs multiple reaction experiments by operating heating mechanisms, cooling mechanisms, chemical liquid dropping mechanisms, vacuum pressure control mechanisms, etc. to match pre-given reaction conditions. The company provided an automatic reaction management system, and at this time, if necessary, the temperature, vacuum pressure,
Memorizes information such as the rotational torque of the stirring mechanism and elapsed time,
It can also be configured to output.

[0008]

[Embodiments] The present invention will be explained below based on first to fourth embodiments.

The first embodiment shown in FIGS. 1 and 2 is aimed at controlling the reaction temperature and chemical solution dropping conditions when conducting the same type of experiment in a plurality of reaction vessels.

First, 8 jacket-type reaction tanks A and B
... is installed, and each of the eight reaction tanks is equipped with a cooling mechanism, a heating mechanism, and three systems of chemical liquid dripping mechanisms. The combination of each reaction tank and each mechanism is shown in experimental equipment A.
'・B'・... Then, these eight experimental devices A
', B', . . . are simultaneously centrally controlled by one controller CPU1.

[0011] Below, the system configuration will be explained using one of these experimental apparatuses (experimental apparatus A') as a representative example, which mainly uses jacket type reaction vessels.

Naturally, this reaction tank A is also provided with a cooling mechanism, a heating mechanism, and three systems of chemical liquid dropping mechanisms, and the controller CPU
1 and is connected via a communication cable.

Among these, the cooling mechanism includes a temperature sensor A0 that measures the temperature inside the tank in real time, and a cooler A11.
A cooling path A12 that guides the cooling water supplied by the cooler A11 into the jacket surrounding the reaction tank A, a circulation pump A13, and a cooling fan A14 that blows cold air around the reaction tank A. The operation of the cooler A11 and the cooling fan A14 is controlled by the controller CPU1.

The heating mechanism includes the temperature sensor A0, an electric heater A21 controlled by the controller CPU1, and a heating tank A22 that stores the heat medium heated by the heater A21 and warms the reaction tank A. The entire system is an oil bath system.

Furthermore, the three systems of chemical liquid dropping mechanisms each include a storage container A31 storing added chemical liquids α, β, and γ, a chemical liquid path A32 for feeding the chemical liquid in the containers into the reaction tank A, and a storage container A31 that stores the added chemical liquids α, β, and γ. Electronic balance A33 and chemical pump A to be measured
34. Of these, chemical liquid pump A
34 is a metering drip pump manufactured by Todoroki Sangyo Co., Ltd. (model number: C
P1-1) is used. This metered drip pump is
The dropping speed can be changed according to commands from the controller CPU1, and the electronic balance notifies the weight change of the container, integrates the amount of drug solution dropped per predetermined time, and reports this integrated value to the controller CPU1. You can also do it.

The controller CPU1 is: ■ 32-bit small computer model number, manufactured by NEC Corporation; PC-9801DX2; ■ Monitor device model number, manufactured by NEC Corporation; PC-KD882; ■ Printer device model number, manufactured by NEC Corporation; PC-PR101G2; ■ Memory device model number manufactured by I/O Data Co., Ltd.: PI
O-9234G-4ML■ Manufactured by CONTEC I
Analog-digital converter model number with F circuit; AD12-16TA (98) CONT
Digital-to-analog converter with IF circuit manufactured by EC Model number: DA12-16 (98) ■ Communication cable with IF circuit manufactured by NEC Corporation RS2
32C model number: PC-9861K.

[0017] Among these, small computers are equipped with
The experiment is prepared by inputting and setting the experiment start temperature, the allowable temperature difference between the experiment temperature and the allowable temperature difference, the abnormality determination temperature, and the amount and type of chemical solution to be dropped. The experiment start temperature is the temperature at which the experiment starts, and the inside of the tank is maintained at this temperature before the experiment. In addition, the amount of chemical solution dropped can be entered into a graph displayed on the monitor for each type of drop, with the vertical axis showing the drop amount and the horizontal axis showing the elapsed time. It can also be set so that the amount changes.

When the controller CPU1 is actually instructed to start the experiment, the controller CPU1 starts the experiment from one reaction tank among the eight reaction tanks. First, controller CPU1
opens the communication line to the cooling mechanism, heating mechanism, chemical liquid dripping mechanism, etc. installed in reaction tank A, which will perform the starting operation first.
Communicate control commands to each mechanism. That is, an experiment start operation is performed on the experimental apparatus A'. In accordance with this control command from the controller CPU1, in the reaction tank A, the preset chemical solution dropping at time 0 is started, and the heating mechanism or cooling mechanism is activated to bring the temperature inside the tank closer to the experimental temperature. The experiment begins. The experiment start operation on experimental device A' is performed during the first 0.15 seconds, and after 0.15 seconds, the other 7
The experiment start operation is performed for each of the reaction vessels B, C, . . . while switching the communication line to each experimental apparatus B', C', . . . in turn every 0.15 seconds.

[0019] When the experiment is started in all the reaction vessels, the controller CPU1 again opens the communication circuit to each mechanism of the first reaction vessel A, and receives information from each mechanism such as the temperature inside the measurement vessel and the amount of chemical solution dropped. This data is stored in combination with the elapsed time from the start of the experiment in reaction tank A. This data collection is also performed in 0.15 seconds, and 0.1 seconds from the start of data collection.
After 5 seconds have elapsed, data collection (hereinafter referred to as monitoring) begins for each of the other seven reaction tanks, switching the communication line to each mechanism corresponding to each reaction tank in turn every 0.15 seconds. ). thus,
When the monitoring for all seven reaction vessels is completed, the system returns to reaction vessel A and repeats monitoring for the eight reaction vessels in order every 0.15 seconds until the end of the experiment. In addition, if it is set in advance to change the amount of chemical solution dropped after a predetermined period of time has elapsed, the first communication to the reaction tank will be resumed after a certain period of time has elapsed from the experiment start operation in each reaction tank. At this time, a new control command is sent to the chemical liquid dropping mechanism corresponding to the reaction tank to change the dropping amount.

Now, when the temperature inside a certain reaction tank changes as the experiment progresses, the controller CPU1 receives the measured value of the temperature inside the tank when monitoring that reaction tank, and sets the measured temperature. If the temperature is higher than the experimental temperature by more than an allowable temperature difference, a command to operate the cooling mechanism is issued during this monitoring time. Conversely, if the measured temperature is lower than the set experimental temperature by more than the allowable temperature difference, a command to operate the heating mechanism is issued. After this, when the 0.15 seconds of monitoring time is over, the other 7 tanks are monitored and 1.0
The reactor is monitored again after 5 seconds. This one
．． During the 05 second gap, the heating and cooling mechanisms are operating according to the previous commands. Then, when the reaction tank is again monitored, the controller CPU1 is also informed of the measured value of the temperature inside the tank, and issues a new appropriate control command based on this measured value. However, this cooling mechanism
The temperature inside the tank is adjusted by repeatedly controlling the operation of the heating mechanism.

However, when a large amount of the additive chemical solution is dropped in a short period of time, the measurable temperature inside the tank is temporarily unstable, so the cooling mechanism, The operation control of the heating mechanism is temporarily suspended.

Furthermore, if the temperature inside the reaction tank becomes higher than the abnormality judgment value during the experiment, this will be discovered during monitoring of the reaction tank, and the dropping of the chemical solution will be immediately stopped. It activates the cooling mechanism and issues a command to stop the reaction. However, as the temperature rises,
This is only true if you are conducting an experiment where the reaction is progressing.

[0023] In addition, the temperature inside the tank communicated from the temperature sensor in each reaction tank and the amount of chemical solution dripping sent from the chemical pump are combined with the elapsed time from the start of the experiment in each reaction tank, which is measured by a small computer. , are stored for each reaction tank (however, in this example, up to 48 hours). This data can be output and displayed on a monitor device even during monitoring execution, and can also be output from a printer device. Furthermore, even after the experiment is finished, the data is saved and can be output when desired.

Note that in the first embodiment, the controller C
Since the PU 1 can communicate with and control only one experimental device at a time, a method is adopted in which each experimental device is controlled in turn.

[0025] When the reactions have finished in the eight reaction vessels, the products in each reaction vessel are collected and inspected, the data stored in the controller CPU1 is organized, and the equipment is cleaned up afterward. If you do this, the experiment will end. The set values of the reaction conditions used when conducting this experiment can be stored in the controller CPU 1 (up to 99 patterns), and can be recalled at any time to perform the experiment under the same conditions. .

In addition, the second embodiment shown in FIGS. 3 and 4 makes it possible to control the reaction temperature, chemical drop conditions, and viscosity of the liquid in the reaction tanks when conducting the same type of experiment in a plurality of reaction tanks. purpose.

Similar to the first embodiment, eight jacket-type reaction tanks I, J,... are installed at the same time, and each of the eight reaction tanks is equipped with a cooling mechanism, a heating mechanism, three systems of chemical liquid dripping mechanisms, and , a stirring mechanism is provided. Therefore, the combinations of each reaction tank and each mechanism are referred to as experimental apparatuses I', H', . . . . Furthermore, one controller CPU2 is also installed, which simultaneously controls each mechanism of these eight reaction tanks.

The system configuration of one of these experimental apparatuses (experimental apparatus I') will be explained below as a representative example.

Naturally, this reaction tank I is also provided with a cooling mechanism, a heating mechanism, and three systems of chemical solution dropping mechanisms, and is further provided with a stirring mechanism. Each of these mechanisms is linked to the controller CPU2 via a communication cable.

Of these, the cooling mechanism is similar to the first embodiment.
Temperature sensor I0 that measures the temperature inside the tank in real time,
A cooler I11 and a cooling path I1 that guides the cooling water supplied by the cooler I11 into the jacket around the reaction tank I.
2, a circulation pump I13, and a cooling fan I14 that blows cold air around the reaction tank I. Further, as in the first embodiment, the operation of the cooler I11 and the cooling fan I14 is controlled by the controller CPU2.

The heating mechanism includes the temperature sensor I0, an electric heater I21 controlled by the controller CPU2, and a heating tank I22 that stores the heat medium heated by the heater I21 and warms the reaction tank I. This point can be said to be the same as the first embodiment.

[0032] On the other hand, the three systems of chemical liquid dripping mechanisms are still
Storage containers I31 storing additive chemical solutions δ, ε, and ζ, respectively
and a chemical liquid path I32 that sends the chemical liquid in the container into the reaction tank I,
It also includes an electronic balance I33 for measuring the weight of the storage container and a chemical liquid pump I34. Among these, a fixed-quantity dripping pump (model number: CP2-1) manufactured by Todoroki Sangyo Co., Ltd. is used as the chemical liquid pump I34. This fixed-quantity dripping pump can change the dripping speed according to commands from the controller CPU2, and also integrates the amount of drug solution dripped per predetermined time based on changes in the weight of the container sent from the electronic balance, and controls this cumulative value. device CPU2.

On the other hand, the stirring mechanism includes a stirring shaft I41 housed in the reaction tank I and a stirring shaft I4.
1 is configured by an electric circuit I42 that drives the motor. The electric circuit I42 is connected and controlled by the controller CPU2, and estimates the rotational torque of the electric circuit I42 from the current value and effective rotation speed in the circuit, and transmits the estimated value to the controller CPU2.
It is set to be sent to 2.

To explain this rotational torque estimation method in more detail, the motor that rotates the stirring shaft I41 has a certain relational expression between the voltage, current value, rotational torque, and rotational speed within a predetermined rotational speed range. To establish. Now, since the voltage is constant, circuit I42 measures the current and rotation speed, and then
Rotational torque can be calculated from a predetermined relational expression.

In addition, the controller CPU2 is a 32-bit small computer model number manufactured by NEC Corporation; PC-
9801DX2 ■ Monitor device model number manufactured by NEC Corporation; PC-KD882 ■ Printer device model number manufactured by NEC Corporation; PC-PR101GS ■ Communication cable with IF circuit manufactured by NEC Corporation RS2
32C model number; composed of PC-9861K, etc.

Among these, the experiment start temperature, the allowable temperature difference between the experiment temperature and the allowable temperature, the abnormality determination temperature, the amount of the chemical solution to be dropped, the type of the droplet, and the abnormal rotational torque value are input and set in the small computer in advance. Note that the experiment start temperature is the temperature at which the experiment starts, and the inside of the tank is maintained at this temperature before the experiment. In addition, the amount of chemical solution dropped can be entered into a graph displayed on the monitor for each type of drop, with the vertical axis showing the drop amount and the horizontal axis showing the elapsed time. It can also be set so that the amount changes.

When the controller CPU2 is actually instructed to start the experiment, the controller CPU2 performs the same experiment management as in the first embodiment. That is, the controller CPU2 starts the experiment starting operation from one reaction tank among the eight reaction tanks, and controls the cooling mechanism, heating mechanism, and chemical liquid disposed in the reaction tank I that performs the starting operation first. Open communication lines to dripping mechanism, stirring mechanism, etc.
After communicating the control command to each mechanism within 0.15 seconds, the other 7
While switching the communication lines to each mechanism corresponding to each reaction tank in turn every 0.15 seconds, the experiment start operation is performed for each reaction tank. In addition, according to a control command from the controller CPU2, in each reaction tank, dropping of the set chemical solution at time 0 is started, and at the same time the heating mechanism or cooling mechanism is activated and the temperature inside the tank approaches the experimental temperature. It is the same as the example.

[0038] When the experiment is started in all the reaction vessels, the controller CPU2 again opens the communication circuit to each mechanism of the first reaction vessel I, and receives information from each mechanism such as the temperature inside the measuring vessel and the amount of chemical solution dropped. , the estimated viscosity of the liquid in the tank is communicated, and this data is
It is stored in combination with the elapsed time from the start of the experiment in reaction tank I. In other words, monitoring is performed in the same way as in the first embodiment. This monitoring is also performed for 0.15 seconds, and when 0.15 seconds have passed from the start of monitoring,
Monitoring is performed for each of the other seven reaction tanks while switching the communication line to each mechanism corresponding to each reaction tank in turn every 0.15 seconds. When the monitoring of all seven reaction vessels is completed in this way, the system returns to reaction vessel I and repeats the monitoring of the eight reaction vessels in order every 0.15 seconds until the end of the experiment. In addition, if it is set in advance to change the amount of chemical solution dropped after a predetermined period of time has elapsed, the first communication to the reaction tank will be resumed after a certain period of time has elapsed from the experiment start operation in each reaction tank. At this time, a new control command is sent to the chemical liquid dripping mechanism to change the dripping amount.

Now, as the experiment progresses, when the temperature inside a certain reaction tank changes, the controller CPU 2 is notified of the measured value of the temperature inside the tank when monitoring that reaction tank.
If the measured temperature is higher than the set experimental temperature by more than an allowable temperature difference, a command to operate the cooling mechanism is issued during this monitoring time. Conversely, if the measured temperature is lower than the set experimental temperature by more than the allowable temperature difference, a command to operate the heating mechanism is issued. After this, when the 0.15 second monitoring period is over, the remaining 7 tanks will be monitored and 1
．． After 0.5 seconds, the reaction vessel is monitored again. At this time, the measured value of the temperature inside the tank is also communicated, and an appropriate control command is issued based on this measured value. By repeating this control of the cooling mechanism and heating mechanism, the temperature inside the tank is adjusted.

Further, when the controller CPU 2 discovers that the internal temperature of a certain reaction tank exceeds the abnormality determination temperature, the same countermeasures as in the first embodiment are taken. In other words, the dropping of the chemical solution is stopped and the temperature inside the tank is lowered.

Furthermore, during monitoring, the rotational torque for stirring is notified from the stirring mechanism of each reaction tank, but as the experiment progresses, the viscosity changes significantly in a certain reaction tank, and this rotational torque becomes an abnormal rotational torque value. If it exceeds the controller CP
U2 stops dropping the chemical into this reaction tank.

[0042] The temperature inside each reaction tank, the amount of chemical solution dropped,
The rotational torque value is stored for each reaction tank in combination with the elapsed time from the start of the experiment in each reaction tank, which is measured by a small computer (however, in this example, up to 48 hours). This data can be output and displayed on a monitor device even during monitoring execution, and can also be output from a printer device. Furthermore, even after the experiment is finished, the data is saved and can be output when desired.

[0043] When the reactions have finished in the eight reaction vessels, the products in each reaction vessel are collected and inspected, and the data stored in the controller CPU 2 is organized, and the equipment is cleaned up afterward. If you do this, the experiment will end. The reaction condition settings used when conducting this experiment can be stored in the controller CPU 2 (up to 99 patterns), and can be recalled at any time to perform the experiment under the same conditions. .

In the third embodiment shown in FIGS. 5 and 6, when conducting the same type of experiment in a plurality of reaction vessels, the reaction temperature, chemical solution dropping conditions, pressure in the reaction vessels, and nitrogen partial pressure in the reaction vessels are adjusted. The purpose is to manage.

Five polymerization test apparatuses Q', R', . . . are installed in connection with one controller CPU3. This polymerization test device is a polymerization test system manufactured by Todoroki Sangyo Co., Ltd. (model number;
DS-1) with the addition of three systems of chemical liquid dripping mechanisms and a nitrogen flow rate control mechanism. Note that this polymerization test system is composed of a reaction tank, a cooling mechanism, a heating mechanism, and a vacuum pressure control mechanism.

The polymerization test apparatus will be explained below by taking the polymerization test apparatus Q' as an example.

The cooling mechanism built into the polymerization test system includes a temperature sensor Q that measures the temperature inside the tank in real time.
0 and a cooling fan Q14. Further, the heating mechanism is an oil bath type that is composed of the temperature sensor Q0 and a heating tank Q22 that can be raised and lowered to store a heat medium and warm the reaction tank. The reaction tank Q incorporated in the polymerization test system is located just before the cooling fan Q14 and can be blown with cold air when necessary, but on the other hand, the reaction tank Q is also located above the heating tank. The lower heating tank Q
22 rises and is immersed in the heat medium inside the heating tank Q22, thereby raising the temperature inside the tank.

The vacuum pressure control mechanism incorporated in the polymerization test system includes a vacuum pressure sensor Q51, a vacuum device Q52,
It is composed of a vacuum solenoid valve Q53 and an airtight conduit Q54. The vacuum pressure sensor Q51 sends the measured vacuum pressure to the controller CPU.
3, and the controller CPU3 operates the vacuum solenoid valve Q53 based on this measured vacuum pressure.

[0049] A nitrogen flow rate control mechanism which is additionally provided with this vacuum pressure control mechanism operates in cooperation with the vacuum pressure control mechanism. The nitrogen flow control mechanism includes a mass flow meter Q71, a flow control valve Q72, a vacuum solenoid valve Q73, and a pneumatic pipe Q74.
, a constant pressure valve Q75. Thus, the airtight pipe Q54 of the vacuum pressure control mechanism and the pneumatic pipe Q74 of the nitrogen flow rate control mechanism merge and are connected into the reaction tank Q. The vacuum sensor Q51 is located within an area including the reaction tank Q that is divided into the same vacuum pressure state by a vacuum solenoid valve Q53 provided in the airtight pipe Q54 and a vacuum solenoid valve Q73 provided in the pneumatic pipe Q74. The vacuum pressure is measured here and communicated to the controller CPU3. The controller CPU3 operates the vacuum solenoid valve Q53 according to this measured vacuum pressure to keep the vacuum pressure constant, and is also informed of the current value of the nitrogen flow rate per unit time in the pneumatic pipe Q74 from the mass flowmeter Q71, The flow rate control valve Q72 and the vacuum solenoid valve Q73 are operated to control the nitrogen flow rate so that the oxygen generated by the reaction does not remain in the reaction tank Q to a dangerous extent. Further, the constant pressure valve Q75 keeps the supply pressure of nitrogen to the pneumatic pipe Q74 constant.

Furthermore, as in the first embodiment, the chemical liquid dripping mechanism that is additionally installed includes three storage containers Q31 storing three types of additive chemical liquids, a chemical liquid path Q32 for feeding the chemical liquid in each container into the reaction tank, It is composed of an electronic balance Q33 that measures the weight of the storage container and a chemical liquid pump Q34. Among these, as the chemical liquid pump, a metered drip pump (model number: CP1-1) manufactured by Todoroki Sangyo Co., Ltd. is used, as in the first embodiment.
It is possible to change the dropping speed according to a command from the controller CPU3, or to integrate the amount of drug solution dropped per predetermined time based on a change in the weight of the container sent from the electronic balance Q33, and to notify this integrated value to the controller CPU3. can.

On the other hand, the controller CPU 3 is a 32-bit small computer manufactured by NEC Corporation, model number: PC-
9801DX2 ■ Monitor device model number made by NEC Corporation; PC-KD882 ■ Printer device model number made by NEC Corporation; PC-PR101GS ■ Memory device model number PIO-9234G-4ML made by I・O Data Corporation ■ IF circuit made by CONTEC Corporation Analog-to-digital converter model number: AD12-16TA (98) ■ Consists of a communication cable with IF circuit RS232C manufactured by NEC Corporation, model number PC-9861K.

Among these, the experiment start temperature, the allowable temperature difference between the experiment temperature and the allowable temperature difference, the abnormality judgment temperature, the amount of the chemical solution to be dropped, the type of the drop, and the experimental vacuum pressure can be input and set in advance into the small computer. The experiment start temperature is the temperature at which the experiment starts, and the inside of the tank is kept at this temperature in advance. Further, the experimental vacuum pressure is a value that should be maintained in the reaction tank from the time of starting the experiment throughout the experiment, and in reality, the vacuum pressure in the tank is controlled by the controller CPU3 operating the vacuum device. is maintained within a predetermined vacuum pressure range centered around the experimental vacuum pressure value. Furthermore, the amount of chemical solution dropped can be entered into a graph displayed on the monitor for each type of drop, with the vertical axis showing the drop amount and the horizontal axis showing the elapsed time. It can also be set so that the amount changes.

When the controller CPU3 is actually instructed to start the experiment, the controller CPU3 selects one of the five polymerization test apparatuses.
Perform the experiment start operation from the machine. First, the controller CPU3 opens a communication line to the polymerization test device that performs the starting operation first, and communicates a control command to the device. This controller CPU
In response to the control command from 3, in the polymerization test apparatus, the set chemical solution drop at time 0 is started, and the heating mechanism or cooling mechanism is activated so that the temperature inside the tank approaches the experimental temperature.
Experiments begin in the reaction tank. In this third embodiment as well, the experiment start operation for the polymerization test apparatus is performed during the first 0.15 seconds, and after 0.15 seconds, the experiment start operation for the other four polymerization test apparatuses is performed for 0.15 seconds. While switching the communication line to each polymerization test device in turn, perform the experiment start operation for each.

[0054] When the experiment is started in the total polymerization test device, the controller CPU3 again opens the communication circuit to the polymerization test device where the experiment was first started, and the temperature inside the measuring tank and the dropping of the chemical solution are transmitted from the device. This data is stored in combination with the elapsed time from the start of the experiment in the polymerization test apparatus. This monitoring is also carried out for 0.15 seconds, and after 0.15 seconds have passed from the start of monitoring, the other four polymerization test devices are monitored while switching the communication line to each device in turn every 0.15 seconds. This is what we do. Also, in the third embodiment,
When the monitoring of all four polymerization test devices is completed, return to the beginning and set 0 to 5 polymerization test devices.
．． Monitoring is repeated every 15 seconds until the end of the experiment. In addition, if the drop amount of the chemical solution is set in advance to change after a predetermined period of time has elapsed, the initial communication to each polymerization test device will be restarted after a certain period of time has elapsed from the experiment start operation in each polymerization test device. At this time, a new control command is sent to the polymerization test device to change the dripping amount.

Now, as the experiment progresses, when the temperature inside the reaction tank changes in a certain polymerization test device, the controller CPU 3 receives the measured value of the temperature inside the tank when monitoring the polymerization test device. If the measured temperature is higher than the set experimental temperature by more than an allowable temperature difference, a command is issued to operate the cooling mechanism during this monitoring time. Also, conversely,
If the measured temperature is lower than the set experimental temperature by more than an allowable temperature difference, a command is issued to activate the heating mechanism. After this, 0.15
When the monitoring time of seconds is over, the other four devices are monitored, and after 0.60 seconds, this polymerization test device is monitored again. During this monitoring, the measured value of the temperature inside the tank is also communicated, and appropriate control commands are issued based on this measured value. By repeating this control of the cooling mechanism and heating mechanism, the temperature inside the tank is adjusted.

[0056] Additionally, if during an experiment, the temperature inside the reaction tank of a certain polymerization test device becomes higher than the abnormality judgment value, this will be discovered during monitoring of the polymerization test device, and the chemical solution will be immediately removed. A command is issued to stop the dripping, activate the cooling mechanism, and stop the reaction.

Furthermore, if during an experiment, the internal vacuum pressure of the reaction tank of a certain polymerization test device deviates from the predetermined vacuum pressure range centered on the set experiment vacuum pressure, when monitoring the polymerization test device, , the controller CPU3 discovers this and operates the vacuum solenoid valve Q53 during the same monitoring period. Of course, the vacuum solenoid valve Q53 is operated to reduce the pressure when the vacuum pressure inside the tank is higher than the set vacuum pressure, and to increase the pressure when the vacuum pressure inside the tank is lower than the set vacuum pressure. This operation remains valid until the next time of monitoring of the polymerization test apparatus, and at the time of new monitoring, the controller CPU3 is once again notified of the vacuum pressure in the tank and performs a new operation if necessary.

The controller CPU3 simultaneously controls the nitrogen partial pressure within the reaction tank. The amount of gas generated is estimated from the temperature and vacuum pressure changes in the chamber, and the amount of nitrogen flowing in, and the amount of gas and nitrogen flow rate to be extracted from the reaction chamber by the vacuum pressure control mechanism is determined to prevent the generated gas from accumulating in an amount that will support the experiment. The control mechanism determines the flow rate of nitrogen flowing into the reaction tank, and the flow rate control valve,
It operates vacuum solenoid valves, etc.

[0059] In addition, data such as the temperature inside the reaction tank, the amount of chemical solution dropped, and the vacuum pressure inside the tank from each polymerization test device are processed by a small computer and combined with the elapsed time from the start of the experiment in each polymerization test device. and stored for each polymerization test apparatus (however, in this example, up to 48 hours' worth of data). This data can be output and displayed on a monitor device even during monitoring execution, and can also be output from a printer device. Furthermore, even after the experiment is finished, the data is saved and can be output when desired.

[0060] When the reactions in the five polymerization test apparatuses are completed in this way, the products in the reaction vessels of each polymerization test apparatus are collected and inspected, and the data stored in the controller CPU3 is organized, and then the instruments are removed. If you clean up afterward, such as washing,
The experiment ends. The reaction condition settings used when conducting this experiment can be stored in the controller CPU 3 (up to 99 patterns), and can be recalled at any time to perform the experiment under the same conditions. .

The fourth embodiment shown in FIG. 7 and FIG. 8 shows the reaction temperature, chemical drop conditions, viscosity of the liquid in the reaction tank, vacuum pressure in the tank, The purpose is to control the nitrogen partial pressure inside the tank.

Five automatic reaction devices V', W', . . . are connected to one controller CPU4. This automatic reaction device is manufactured by Todoroki Sangyo Co., Ltd. (model number TDML-1).
It consists of a jacket-type reaction tank, a cooling mechanism, a heating mechanism, three systems of chemical liquid dropping mechanisms, a stirring mechanism, a vacuum pressure control mechanism, a PH management mechanism, and a nitrogen flow rate control mechanism.

[0063] These automatic reaction apparatuses will be explained below, taking automatic reaction apparatus V' as an example.

The cooling mechanism installed in the automatic reaction device includes a temperature sensor V0 that measures the temperature inside the tank in real time, an electronic cooling device V1, and water supplied by the electronic cooling device V1 into a jacket around the reaction tank. Guiding waterway V2,
Furthermore, it is composed of a circulation pump V3 provided in the waterway V2, and a cooling fan V14 that blows cold air around the reaction tank.

The heating mechanism includes the temperature sensor V0, the electronic cooling device V1, the water channel V2, the circulation pump V3, and a heating tank that stores the heat medium produced by the electric heater V21 and the heater V21 to warm the reaction tank. Constructed by V22.

[0066] However, in the automatic reaction device, the third
As in the embodiment, the heating tank V22 is raised and lowered to receive heat,
The temperature inside the tank is controlled by blowing air from the cooling fan V14. In addition to this, electronic cooling device V1
In some cases, cold or hot water produced by a jacket is guided into the jacket and its temperature is regulated.

On the other hand, the three-system chemical liquid dropping mechanism includes three storage containers V31, a chemical liquid path V32 for feeding the chemical liquid in the containers into the reaction tank V, an electronic balance V33 for measuring the weight of the storage container V31, and a chemical liquid pump V34. It is made up of. This chemical pump V34 can change the dropping speed according to the commands of the controller CPU4, and
The change in the weight of the container is sent from the electronic balance V33, and the amount of drug solution dropped per predetermined time is integrated, and this integrated value is sent to the controller C.
It is also possible to notify the PU4.

The stirring mechanism is composed of a stirring shaft V41 housed in the reaction tank and an electric circuit V42 that drives the stirring shaft V41. As in the second embodiment, the electric circuit V42 is connected to and controlled by the controller CPU4, and controls the stirring resistance that the stirring shaft V42 receives.
The estimated value is estimated from the current value in the circuit and the effective rotational speed, and is sent to the controller CPU4.

As in the third embodiment, the vacuum pressure control mechanism is composed of a vacuum pressure sensor V51, a vacuum device V52, a vacuum solenoid valve V53, and an airtight conduit V54. Vacuum pressure sensor V51
communicates the measured vacuum pressure to the controller CPU4, and
Based on this measured vacuum pressure, PU4 activates the vacuum solenoid valve V53.
to operate.

Further, as in the third embodiment, a nitrogen flow rate control mechanism operates in cooperation with this vacuum pressure control mechanism to adjust the vacuum pressure. The nitrogen flow control mechanism is a mass flowmeter V
71, a flow rate control valve V72, a vacuum solenoid valve V73, a pneumatic pipe V74, and a constant pressure valve V75. Thus, the airtight pipe V54 of the vacuum pressure control mechanism and the pneumatic pipe V74 of the nitrogen flow rate control mechanism merge and are connected into the reaction tank V. The vacuum sensor V51 is located within an area including the reaction tank V that is divided into the same vacuum pressure state by a vacuum solenoid valve V53 provided in the airtight pipe V54 and a vacuum solenoid valve V73 provided in the pneumatic pipe V74. The vacuum pressure is measured here and communicated to the controller CPU4. The controller CPU4 controls the vacuum solenoid valve V5 according to this measured vacuum pressure.
3 to keep the vacuum pressure constant, and mass flowmeter V
The current value of the nitrogen flow rate per unit time is communicated from 71, and the flow rate control valve V72 and the vacuum solenoid valve V73 are operated to prevent oxygen generated by the reaction from remaining in the reaction tank V to a dangerous extent. Further, the constant pressure valve V75 keeps the supply pressure of nitrogen to the pneumatic pipe V74 constant.

The pH control mechanism is composed of a device for dropping an acidic additive into the reaction tank, a device for dropping a basic additive into the reaction tank, and a pH sensor V61. Both the acidic additive dropping device and the basic additive dropping device have storage containers V61a and V61b, chemical channels V62a and V62b, and electronic balances V63a and V63b, similar to the chemical dropping mechanism.
, chemical liquid pumps V64a and V64b. Therefore, the pH sensor V61 notifies the controller CPU4 of the current pH value in the reaction tank, and the acidic additive liquid dropping device and the basic additive liquid dropping device are controlled by the controller CPU4 to appropriately supply the additive liquid to the tank. drip inside.

[0072] As the controller CPU 4, ■ 32-bit small computer model number manufactured by NEC Corporation;
PC-9801DX2 ■ Manufactured by NEC Corporation Monitor device model number; PC-KD882 ■ Manufactured by NEC Corporation Printer device model number; PC-PR101GS ■ I・O Data Corporation Memory device model number; PIO-9234G-4ML ■ Manufactured by NEC Corporation Communication cable with IF circuit RS232C model number: PC-9861K etc. are adopted.

Naturally, this small computer has information in advance such as the experiment start temperature, the allowable temperature difference between the experiment temperature and the abnormality judgment temperature, the amount and type of chemical solution to be dropped, the abnormal rotational torque value, the method to be used when abnormal rotational torque occurs, and the optimum The pH value and ideal nitrogen flow rate must be input and set. The conditions for this experiment are:
This is done for each automatic reactor. In other words, different conditions can be set for each automatic reaction device.

When the controller CPU 4 is actually instructed to start the experiment, the experiment start operation is first performed in one reaction tank, as in the first to third embodiments. In other words, to one automatic reaction device,
It issues commands such as dropping chemical liquids and controlling temperature. This experiment start operation is performed within 0.15 seconds as in the first to third examples, but regarding the start of the experiment in the next reaction tank,
This is slightly different from the first to third embodiments. That is, in Examples 1 to 3, experiments were conducted under the same reaction conditions, so
Whereas the same experiment starting operation could be performed, in the fourth example, the experiment was conducted with different reaction conditions for each reaction tank, so the starting operation was performed under different condition commands than the first automatic reaction device. It must be done. Therefore, in order to start the experiment in the second automatic reaction device after starting the experiment in the first automatic reaction device, the controller CPU 4 sets the second reaction condition setting value in place of the first reaction condition setting value. After recalling the values, the second automatic reaction device is operated to start the experiment in 0.15 seconds based on the reaction condition set values. After this, the experiment start operation is performed in the same manner for the remaining three automatic reaction devices.

[0075] When the experiment is started in the fully automatic reaction apparatus, the controller CPU 4 again calls up the reaction condition setting values for the first automatic reaction apparatus, and also reads the temperature inside the measurement tank from the automatic reaction apparatus. The amount of chemical solution dropped, the estimated viscosity of the liquid in the tank, the vacuum pressure in the tank, the pH value of the liquid in the tank, the current flow rate of nitrogen, etc. are communicated, and this data is combined with the elapsed time from the start of the experiment in the automatic reaction device. memorize it. This monitoring is also performed for 0.15 seconds, and after 0.15 seconds have elapsed from the start of monitoring, the other four automatic reaction devices are called up to their respective reaction condition settings, and then monitoring is performed for 0.15 seconds. This is what we do. In this way, monitoring of all five automatic reaction devices has been completed, and needless to say, we will go back and monitor them in order.

However, when the temperature inside the reaction tank of an automatic reaction device changes as the experiment progresses, the controller CPU 4
is communicated the measured value of the temperature inside the tank when monitoring the automatic reaction tank, and if the measured temperature is higher than the experimental temperature set for the automatic reaction tank by more than the allowable temperature difference, , a command is issued to activate the cooling mechanism. Conversely, if the measured temperature is lower than the set experimental temperature by more than the allowable temperature difference, a command to operate the heating mechanism is issued. Further, the next monitoring of the automatic reaction tank is also controlled appropriately, and as a result, temperature control is executed in the same manner as in the first to third embodiments.

[0077] In addition, if a specific automatic reaction device is set so that the amount of the chemical solution dropped changes with time, the amount of the chemical solution dropped during monitoring of the automatic reaction device will change as time elapses from the start of the experiment in the automatic reaction device. The drug solution dropping mechanism can be controlled to change the amount of drops.

Furthermore, as the experiment progresses, in a particular automatic reaction device, if the viscosity of the liquid in the reaction tank changes significantly and the stirring torque for stirring exceeds the abnormal rotational torque value, this abnormal viscosity will be detected during monitoring. is notified, and the controller CPU 4 performs control to reduce the amount of medicine dripped into the automatic reaction device based on the setting conditions.

Further, the vacuum pressure control inside the reaction tank is almost the same as in the third embodiment. In other words, if the internal vacuum pressure of the reaction tank of an automatic reaction device during an experiment deviates from a predetermined vacuum pressure range centered on the experimental vacuum pressure set for the automatic reaction device, the automatic reaction device will be monitored. Sometimes,
The controller CPU4 discovers this and operates the vacuum device during the same monitoring time. Of course, the vacuum device is operated to reduce the pressure when the vacuum pressure inside the tank is higher than the set vacuum pressure, and to increase the pressure when the vacuum pressure inside the tank is lower than the set vacuum pressure.

Furthermore, the controller CPU4 also controls the nitrogen partial pressure within the reaction tank, as in the third embodiment. The amount of gas generated is estimated from the temperature and vacuum pressure changes in the chamber, and the amount of nitrogen flowing in, and the amount of gas and nitrogen flow rate to be extracted from the reaction chamber by the vacuum pressure control mechanism is determined to prevent the generated gas from accumulating in an amount that will support the experiment. The control mechanism determines the flow rate of nitrogen flowing into the reaction tank and operates the flow control valve, vacuum solenoid valve, etc.

Further, the controller CPU 4 is notified of the pH value of the liquid in each reaction tank when monitoring each automatic reaction device. If this pH value is greater than a certain value than the pH value set for the automatic reaction device, the acidic additive liquid dripping device of the PH control mechanism is activated during the same monitoring, and the acidic additive liquid is is dropped into the tank to lower the pH value in the tank. Conversely, if the measured pH value is the set pH
If the value is smaller than the specified value, the basic additive liquid dripping device is activated to drop the basic additive liquid into the tank, and the pH in the tank is reduced.
Increase H value. With this operation, the pH value in the reaction tank is
It is controlled to stay within a certain range around the set pH value.

In addition, the temperature inside the measurement tank, the amount of chemical solution dropped, the estimated viscosity of the liquid inside the tank, the vacuum pressure inside the tank, the pH value of the liquid inside the tank, the current value of the nitrogen flow rate, etc. that are notified to the controller CPU 4 are determined by each automatic reaction. For each apparatus, the time from the start of the experiment and the set reaction conditions for each reaction tank are stored in the controller CPU 4, and can be output from a monitor or printer when necessary.

[0083]

[Effects of the Invention] As explained above with reference to the embodiments, the automatic chemical reaction management system of the present invention allows chemical reactions in multiple reaction vessels to be managed at once unattended, making it especially possible to conduct many experiments simultaneously. In some cases, significant labor savings can be achieved. In addition, the reaction management is truly practical, covering a wide range of areas including various reaction conditions, various data recording storage, and safety management.

As described above, the chemical reaction automatic management system of the present invention has great industrial utility value.

[Brief explanation of the drawing]

FIG. 1 is an overall schematic block diagram in a first embodiment.

FIG. 2 is a partial block diagram illustrating a peripheral system of a reaction tank in the first embodiment.

FIG. 3 is an overall schematic block diagram in a second embodiment.

FIG. 4 is a partial block diagram illustrating a peripheral system of a reaction tank in a second embodiment.

FIG. 5 is an overall schematic block diagram in a third embodiment.

FIG. 6 illustrates the polymerization test apparatus in the third example.
FIG. 2 is a partial block diagram.

FIG. 7 is an overall schematic block diagram in a fourth embodiment.

FIG. 8 illustrates an automatic reaction device in the fourth embodiment,
FIG. 2 is a partial block diagram.

[Explanation of symbols]

CPU1 Controller A'・B'... Experimental equipment CPU2 Controller I’・J’・… Experimental equipment CPU3 Controller Q’・R’・…Polymerization test device CPU4 Controller V’・W’・… Automatic reaction device

Claims (1)

[Scope of Claims] [Claim 1] A system for simultaneously managing reaction conditions in a plurality of chemical reaction vessels, which can set a basic temperature for carrying out chemical reactions in the vessels, and also Receives the temperature inside the tank from a temperature sensor provided, and when the temperature inside the receiving tank deviates upward from the basic temperature, activates the cooling mechanism installed in the reaction tank that transmitted the temperature inside the tank. An automatic chemical reaction management system characterized by controlling the temperature inside the reaction tank to maintain it below a certain temperature. [Claim 2] A system that simultaneously manages reaction conditions in a plurality of chemical reaction tanks, which can set a basic temperature for carrying out chemical reactions in the tanks, and can also control the reaction conditions from a temperature sensor installed in each tank. When the temperature inside the tank is received and the temperature inside the receiving tank deviates downward from the basic temperature, the reaction is started by controlling the operation of the heating mechanism installed in the reaction tank that sent the temperature inside the tank. An automatic chemical reaction management system that maintains the internal temperature of the tank above a certain temperature. [Claim 3] A system for simultaneously managing reaction conditions in multiple chemical reaction tanks, which can set a basic temperature for carrying out chemical reactions in the tanks, and can also control the temperature from a temperature sensor installed in each tank. When the temperature inside the tank is received and the temperature inside the receiving tank deviates downward from the basic temperature, the operation of the heating mechanism installed in the reaction tank that sent the temperature inside the tank is controlled to control the temperature of the reaction tank. When the temperature inside the tank is increased and the temperature inside the receiving tank deviates upward from the basic temperature, the operation of the cooling mechanism installed in the reaction tank that sent the temperature inside the tank is controlled, and the temperature inside the receiving tank is increased. A chemical reaction automatic management system that lowers the internal temperature. 4. The automatic chemical reaction management system according to claim 3, wherein a condition for the difference between the basic temperature and the temperature in the tank for starting cooling or starting heating can be set. 5. Storing the internal temperature of each reaction tank sent from a temperature sensor installed in a plurality of chemical reaction tanks at fixed time intervals, and storing the stored temperature of each tank at predetermined time intervals. The chemical reaction automatic management system according to any one of claims 1 to 4, wherein the average value is stored and outputted. [Claim 6] An abnormal temperature can be set, and when the temperature inside the tank sent from the reaction tank exceeds the set abnormal temperature, the heating mechanism of the reaction tank is stopped and the cooling mechanism is activated. The chemical reaction automatic management system according to claim 3, characterized in that: 7. A system that simultaneously manages reaction conditions in a plurality of chemical reaction tanks, which allows setting of multiple sets of reaction elapsed time and chemical solution input amount, and also allows a predetermined period of time from the reaction start time recognized by the system to be set. When the time period has elapsed, by operating the chemical solution dripping mechanism provided in each reaction tank,
An automatic chemical reaction management system characterized by dripping a predetermined amount of chemical solution into each tank. 8. A system for simultaneously managing reaction conditions in a plurality of chemical reaction vessels, the system comprising:
Multiple chemical solution input amounts can be set, and when a predetermined time has elapsed from the reaction start time recognized by the system, by operating a predetermined chemical solution dripping mechanism provided in each reaction tank,
An automatic chemical reaction management system characterized by dropping a predetermined amount of chemical solution of a predetermined type into each tank. 9. The current weight of the chemical solution storage tank is sent from an electronic balance under the chemical solution storage tank provided corresponding to each reaction tank,
9. The automatic chemical reaction management system according to claim 7, wherein the amount of the chemical solution dropped into each reaction tank is determined based on the change in the current weight, and the dripping flow rate of the chemical solution dropping mechanism is adjusted. 10. It has a function of receiving the calculated value of the rotational torque of the stirring mechanism in each reaction tank from the stirring mechanism that stirs the liquid in the tank of each chemical reaction tank, and according to a predetermined setting pattern. 10. The automatic chemical reaction management system according to claim 7, wherein the type and amount of the chemical solution to be dropped are adjusted based on the rotational torque calculation value. 11. The calculated value of the rotational torque of the stirring mechanism in each reaction tank is electrically transmitted from the stirring mechanism that stirs the liquid in the tank of each chemical reaction tank, and this transmitted information is stored and output. A chemical reaction automatic management system according to any one of claims 1 to 10. 12. A system for simultaneously managing reaction conditions in a plurality of chemical reaction vessels, which can set the basic vacuum pressure for carrying out chemical reactions in the vessels, and also control the vacuum pressure provided in each chemical reaction vessel. Current pressure information in the reaction tank is sent from the control mechanism, and if this pressure information value is higher than the set basic vacuum pressure by a certain value or more, operate the vacuum pressure control mechanism to reduce the pressure and the pressure information value becomes the set basic vacuum. An automatic chemical reaction management system characterized in that when the pressure is lower than a certain value, the vacuum pressure control mechanism is operated to increase the pressure. Claim 14: When information is sent from the reaction condition changing mechanism and instruments installed in each chemical reaction tank, the system itself always receives information from one chemical reaction tank, and 15. The automatic chemical reaction management system according to claim 1, wherein the reaction vessels that send information in increments are alternated in a predetermined order. [Claim 15] When managing the reaction conditions of each chemical reaction tank based on preset information, information serving as a management standard can be set separately for each chemical reaction tank. The chemical reaction automatic management system according to any one of claims 1 to 14, characterized in that: