JP4602140B2 - Temperature control device - Google Patents

Description

  The present invention relates to a temperature control device capable of controlling the internal temperature of a reaction vessel or the like used for chemical synthesis of chemicals, pharmaceuticals, etc. in a wide temperature range.

  Conventionally, in a temperature control device used for such an application, steam, hot water, etc. are used on the high temperature side, and cold water, brine, etc. are used on the cold side, and a plurality of these heat media are used. A method of switching and using these heat media in accordance with a combination and a necessary temperature range has been taken.

In this case, since a plurality of types of heat media are used, there are disadvantages that the facilities are complicated and the operation is complicated.
In order to solve this inconvenience, one using silicone oil as a heat medium has been proposed.

  By using this silicone oil as a heat medium, the temperature can be controlled by a single heat medium in a wide temperature range of, for example, −40 ° C. to 150 ° C. or more. Silicone oil also has an advantage that high heat transfer performance can be obtained because of its low kinematic viscosity and excellent fluidity.

However, many commercially available silicone oils have a flash point of less than 250 ° C. Silicone oils with a flash point of less than 250 ° C are designated as dangerous goods under the Fire Service Law. It is subject to various restrictions due to laws and regulations such as having to take explosion-proof measures. For this reason, equipment costs increase, safety management becomes troublesome, and equipment introduction is often avoided.
JP-A-6-79166

  As a result of various studies on the flash point of this silicone oil, the present inventors have found that even if the silicone oil has a flash point of less than 250 ° C., the flash point can be raised to 250 ° C. or higher by a refining operation. It has been found that silicone oil having a flash point of 250 ° C. or higher can be sufficiently used as a thermal refrigerant, and has found optimum conditions for use as a thermal refrigerant.

  Therefore, the subject in the present invention is a temperature control device that uses a heat medium that is not regarded as a dangerous material in the Fire Service Act, enables temperature control in a wide temperature range with a single heat medium, and obtains sufficient heat transfer performance. There is in getting.

To solve this problem,
The invention according to claim 1 is a plurality of heat medium tanks for storing heat mediums having different temperatures;
A plurality of heating / cooling sources for heating or cooling individual heating media in these heating medium tanks and maintaining a constant temperature;
A plurality of circulation pipes for individually extracting the heat medium in these heat medium tanks and returning them to the respective heat medium tanks;
A jacket circulation pipe having a circulation pump that surrounds the object to be controlled and circulates the heat medium in a jacket for heating and cooling the object;
A supply pipe for supplying the heat medium from the plurality of heat medium tanks to the jacket circulation pipe;
Provided with return piping that distributes the heat medium from the jacket circulation piping back to the individual circulation piping,
The temperature control device is characterized in that the heat medium is silicone oil having a flash point of 250 ° C. or higher.

The invention according to claim 2 is the spiral baffle jacket having a baffle which the jacket is formed in a spiral shape,
The temperature control device according to claim 1, wherein the circulation pump has a flow rate of the heat medium in the jacket of 1 m / second or more.

  In the invention according to claim 3, the supply amount of the heat medium from the supply pipe to the jacket circulation pipe is equal to or less than 1/3 of the heat medium quantity circulating in each circulation pipe or the heat medium quantity circulating in the jacket circulation pipe. The temperature control device according to claim 1, wherein a plurality of flow rate adjusting valves are provided in the supply pipe.

  The invention according to claim 4 is that among the heat medium tanks, a heat medium tank that stores a heat medium having a temperature of 0 ° C. or less is connected to a dry air supply pipe that feeds dry air having a dew point of −40 ° C. or less. The temperature control device according to claim 1 or 2, characterized in that

The invention according to claim 5, the control unit is provided, et al is to model predictive control the temperature control of the temperature control object, the control unit includes a master controller and a slave controller,
The master controller is a model predictive controller that includes the process model, and creates a control signal based on the deviation between the temperature data of the contents in the temperature controlled object and a preset temperature, and this control signal is The process model is transmitted to the slave controller, and the process model includes a gain K [−] indicating a relationship between the jacket inlet temperature and the temperature of the contents in the controlled object, a first-order lag time T [sec], and a dead time L A first-order lag time process with [sec] as a configuration parameter,
The slave controller is a model predictive controller including a process model, and the control signal from the master controller, the temperature of the contents inside the controlled object, the temperature of the heat medium flowing into the jacket, and the heat medium flowing out of the jacket A control signal is generated based on the temperature data of the temperature, and the control signal is sent to a flow rate adjustment valve provided in the supply pipe to adjust the opening of the flow rate adjustment valve. gain K indicating the relationship between the opening and the jacket inlet temperature regulating valve [-], wherein the primary delay time T [sec], a first-order lag dead time processes and configuration parameters dead time L [sec] A temperature control device according to claim 1 or 2.

According to a sixth aspect of the present invention, the temperature control unit further includes an internal temperature setting profile generator, and the internal temperature setting profile generator is only for a time in consideration of a response delay due to a dead time of the temperature controlled object. 6. The temperature control apparatus according to claim 5 , wherein an internal temperature profile having a phase advanced is generated and sent to the master controller in time series .

According to claim 7 invention, the jacket is not a structure in which the flow path in the jacket is divided into a plurality of stages are divided in a flow path of a plurality of different lengths in the horizontal direction, different thermal medium of these The temperature control unit switches the control parameter for model predictive control according to the length of the flow path when switching to a flow path having a length . It is a temperature control device.

In the invention according to claim 8, the overall heat transfer coefficient for heat transfer from the jacket to the temperature controlled object when the temperature controlled object is controlled through the jacket is 150 to 300 kcal / m ² · hr · ° C. The temperature control device according to claim 1, wherein the temperature control device is a temperature control device.

  According to the first, second, and third aspects of the invention, by adopting a silicone oil having a flash point of 250 ° C. or higher as a heat medium, it is possible to avoid designation of dangerous goods under the Fire Service Law, and to simplify the equipment. And safety management becomes easy. Moreover, by using this silicone oil, temperature control in a wide temperature range from −40 ° C. to 150 ° C. can be performed with a single heat medium with simple equipment.

  Further, by setting the flow rate of the heat medium in the jacket surrounding the temperature controlled object to 1 m / second or more, good heat transfer performance can be obtained, and the temperature controlled object can be rapidly raised and lowered.

  In addition, the maximum supply amount of the heat medium from the supply pipe to the jacket circulation pipe is a plurality of flow rates that make the amount of the heat medium circulating in each circulation pipe or 1/3 or less of the heat medium quantity circulating in the jacket circulation pipe By providing the adjustment valve in the supply pipe, the rapid temperature change of the heat medium in the jacket circulation pipe is alleviated, and thereby the rapid change of the jacket temperature is suppressed. At the same time, a rapid temperature change of the heat medium in the heat medium tank is suppressed, damage to the apparatus used for heating and cooling is avoided, and a heat medium having a stable temperature is supplied.

  Furthermore, by providing a plurality of heat medium tanks that store heat mediums having different temperatures, a load due to temperature changes that may damage the thermal refrigerant side device even with respect to rapid control temperature changes required for the controlled object. It is possible to respond to the temperature change more quickly without being subjected to this.

Moreover, according to the invention concerning Claim 4, it can prevent that a water | moisture content mixes in a low-temperature heat medium, and a heat medium freezes with the water | moisture content contained in a heat medium, and piping is not obstruct | occluded.
Furthermore, according to the invention concerning Claim 5, 6, and 7, the internal temperature of a to-be-temperature-controlled object can be controlled more accurately.

A major feature of the present invention is that a silicone oil having a flash point of 250 ° C. or higher (hereinafter sometimes referred to as a high flash point silicone oil) is used as a heat medium.
The high flash point silicone oil in the present invention is not particularly limited in other physical properties as long as the flash point is 250 ° C. or higher, but it is preferable that the kinematic viscosity is small. Specifically, the kinematic viscosity at 25 ° C. is preferably 50 centistokes or less, more preferably 35 centistokes or less.

  In order to obtain this high flash point silicone oil, for example, a commercially available silicone oil having a flash point of less than 250 ° C. may be obtained by separating and removing low boiling components by distillation under reduced pressure or normal pressure to recover the high boiling components. it can. Moreover, it can collect | recover and obtain as an extraction residue which extracted and removed the low molecular component with solvents, such as acetone, methanol, and ethanol.

The high flash point silicone oil in the present invention can be prepared by mixing a plurality of silicone oils having different manufacturing processes and methods using the flash point as an index.
In the temperature control device using the high flash point silicone oil obtained by the above method, it is not necessary to deal with dangerous substances in the Fire Service Act, the entire facility can be configured easily, and the facility cost can be reduced. Moreover, since temperature control becomes possible by a single heat medium in a wide temperature range from −40 ° C. to 150 ° C., the operation performance and maintenance performance of the facility are remarkably improved.

Since the high flash point silicone oil in the present invention is generally more viscous than the silicone oil having a low flash point, the heat transfer performance is low and the temperature controllability may be inferior.
The temperature control apparatus of the present invention is provided with various means for solving such problems.

FIG. 1 shows an example of a temperature control device of the present invention.
In FIG. 1, reference numeral 1 denotes a first heat medium tank. The first heat medium tank (hereinafter referred to as the first tank) stores high flash point silicone oil heated to room temperature or higher, for example, 150 ° C., as the heat medium.

A pipe 2 is connected to the lower part of the first tank 1, and the heat medium extracted from the pipe 2 is sent to the heat exchanger 4 through the pump 3, where it exchanges heat with steam, hot water, and the like. And is returned to the top of the first tank 1 through the pipe 5.
Further, a temperature controller 6 is attached to the pipe 5, and the temperature of the heat medium flowing through the pipe 5 is monitored, and the supply amount of steam or the like to the heat exchanger 4 is adjusted so as to keep the temperature at a predetermined value. It has come to be.
The tube 2, the pump 3, the heat exchanger 4, the tube 5 and the temperature controller 6 constitute a heating source.

  A pipe 7 is connected to the bottom of the first tank 1, and the heat medium extracted from the first tank 1 is sent from the pipe 7 to the pump 8, and further passes through the pipe 9 to the top of the first tank 1. Returned, a first circulation pipe A is formed in which the heat medium circulates from the first tank 1 through the pipe 7, the pump 8, and the pipe 9.

Further, a pipe 10 is connected in the middle of the pipe 9, and a part of the heat medium flowing through the pipe 9 branches to the pipe 10 and flows to the first flow rate adjusting valve 11 through the pipe 10, where the flow rate is adjusted. In addition, it passes through the pipe 12 and is sent to the circulation pump 13.
This pipe 10 constitutes a supply pipe.

  Moreover, the code | symbol 21 shows a 2nd heat-medium tank in FIG. The second heat medium tank (hereinafter referred to as the second tank) stores high flash point silicone oil that has been cooled to room temperature or lower, for example, −40 ° C., as the heat medium.

A pipe 22 is connected to the lower part of the second tank 21, and the heat medium extracted from the pipe 22 is sent to the heat exchanger 24 through the pump 23, where heat exchange with liquefied chlorofluorocarbon, liquefied ammonia, etc. Then, it is cooled and returned to the top of the second tank 21 through the pipe 25.
Further, a temperature controller 26 is attached to the pipe 25, the temperature of the heat medium flowing through the pipe 25 is monitored, and the supply amount to the heat exchanger 24 such as liquefied chlorofluorocarbon is maintained so as to keep the temperature at a predetermined value. It has come to be adjusted.
The tube 22, the pump 23, the heat exchanger 24, the tube 25 and the temperature controller 26 constitute a cooling source.

  A pipe 27 is connected to the bottom of the second tank 21, and the heat medium extracted from the second tank 21 is sent from the pipe 27 to the pump 28, and further passes through the pipe 29 to the top of the second tank 21. Returned, a second circulation pipe B is formed in which the heat medium circulates from the second tank 21 through the pipe 27, the pump 28, and the pipe 29.

Further, a pipe 30 is connected in the middle of the pipe 29, and a part of the heat medium flowing through the pipe 29 branches to the pipe 30 and flows to the second flow rate adjusting valve 31 through the pipe 30, where the flow rate is adjusted. In addition, it joins the pipe 12 and is sent to the circulation pump 13.
The pipe 30 constitutes a supply pipe.

  In addition, a pipe 32 is connected to the top of the second tank 21, and dry air having a dew point of −40 ° C. or less from a dry air supply source (not shown) is always supplied to the upper space in the second tank 21. Moisture absorption is not generated in the heat medium that has been sent to a low temperature.

  The heat medium pumped from the circulation pump 13 is sent to the jacket 43 surrounding the reactor (temperature controlled object) 42 through the pipe 41, where the reactor 42 is heated and cooled to a predetermined temperature. , Flows out into the pipe 44, and further returns to the circulation pump 13 through the pipe 45, thereby constituting a jacket circulation pipe.

The pipe 41 is provided with a flow meter 46 for measuring the flow rate of the heat medium flowing therethrough and a thermometer 47 for measuring the temperature of the heat medium. Temperature measurement data from the thermometer 47 is sent to the slave controller 48. It is designed to be entered.
A thermometer 49 for measuring the temperature of the heat medium flowing therethrough is also attached to the pipe 44, and temperature measurement data from the thermometer 49 is also input to the slave controller 48.

The reactor 42 is provided with a thermometer 50 for measuring the temperature of the reactant in the reactor 42. Temperature measurement data from the thermometer 50 is input to the master controller 51 and the slave controller 48. Yes. These controllers constitute cascade control.
Further, a pipe 61 is connected to the pipe 44, and a part of the heat medium circulating and flowing in the jacket circulation pipe is extracted to the pipe 61, and the extracted heat medium is supplied to the first feedback valve 62 or the second It flows through either one of the feedback valves 63.

The first feedback valve 62 and the second feedback valve 63 are both on-off valves, and the heat medium that has passed through the first feedback valve 62 is sent to the pipe 9 through the pipe 64 and is supplied to the first circulation pipe A. It is supposed to be returned.
The heat medium that has passed through the second feedback valve 63 is sent to the pipe 29 through the pipe 65 and returned to the second circulation pipe B.

  The master controller 51 is a model predictive controller that includes a process model, and is based on a deviation between temperature data from a thermometer 50 that measures the temperature of a reactant in the reactor 42 and a preset temperature. A control signal is generated, and this control signal (set value of the slave controller 48) is sent to the slave controller 48.

The slave controller 48 is a model predictive controller including a process model, and generates a control signal based on the set value control signal from the master controller 51, the temperature data from the thermometer 50, the thermometer 47, and the thermometer 49, After the split range processing, this is sent to the first flow rate adjustment valve 11 and the second flow rate adjustment valve 31, respectively, and the opening degree of these flow rate adjustment valves 11, 31 is adjusted.
Here, the data from the thermometer 50 and the thermometer 49 is a feedforward signal. The slave controller 48 performs control such that the set value of the slave controller 48 becomes the measured value of the thermometer 47 by controlling the flow rate of the heat medium supplied from the supply pipe to the jacket circulation pipe.

  The internal temperature setting profile generator 52 is connected to the master controller 51, and sends the internal temperature profile to the master controller 51 in time series as an internal temperature profile whose phase has been advanced by a time considering the response delay due to the dead time of the reactor.

  There are four types of temperature control modes according to the present invention: control stop, outer bath control, inner temperature control, and program control. Outer bath control is controlled by the slave controller 48, and inner temperature control is cascaded between the slave controller 48 and the master controller 51. The control and program control are cascade control of the slave controller 48 and the master controller 51 whose control target is the set temperature of the master controller 51 by the internal temperature setting profile generator 52.

  Further, the jacket 43 surrounding the reactor 42 is a spiral baffle plate jacket having a baffle plate 43a formed in a spiral shape as shown in FIG. By flowing through the gap between the adjacent baffle plates 43a and 43a, the flow rate of the heat medium in the jacket 43 is 1 m / second or more, preferably 1.2 to 2 m / second, more preferably 1.5 to 2 m. Per second.

  As the jacket 43, the illustrated spiral baffle jacket is an example of a preferable embodiment, but the shape and the mounting structure are not particularly limited, and are appropriately designed in consideration of heat transfer to the reactor 42. The

Next, an operation method of this temperature control device will be described.
First, the flow of the heat medium when starting up the apparatus will be described.
First, the pump 8 and the pump 28 are operated to circulate the heat medium in the first tank 1 and the second tank 21 in the first circulation pipe A and the second circulation pipe B, respectively.

At the same time, the pump 3 and the pump 23 are operated to cause the heat medium in the first tank 1 and the second tank 21 to flow to the heat exchangers 4 and 24, where the temperature of the heat medium in the first tank 1 is 150 The temperature of the heat medium in the second tank 21 is cooled to -40 ° C.
This set temperature is kept constant by controlling the supply amounts of steam and liquefied fluorocarbons sent to the heat exchangers 4 and 24 by the temperature controllers 6 and 26.

  Next, one of the first flow rate adjustment valve 11 and the second flow rate adjustment valve 31 is opened, and either one of the heat medium at 150 ° C. and the heat medium at −40 ° C. is sent to the circulation pump 13. This heat medium is sent to the jacket 43 of the reactor 42. The heat medium flowing out from the jacket 43 circulates in the jacket circulation pipe.

  When the heat medium is circulated in the jacket circulation pipe, one of the first feedback valve 62 and the second feedback valve 63 is opened, and a part of the heat medium in the jacket circulation pipe is placed in the first circulation pipe A. And return to one of the second circulation pipes B.

  After the above initial operation, for example, when a heating medium having a set temperature of 80 ° C. is flown into the jacket 43, the temperature control mode is set to the outer bath control, and the set value of the slave controller 48 is set to 80 ° C. According to an instruction from the controller 48, the opening degree of either the first flow rate adjustment valve 11 or the second flow rate adjustment valve 31 is adjusted, the supply amount of the heat medium at 150 ° C. or the heat medium at −40 ° C. is controlled, and the jacket circulation Send it to the pipe.

  Then, the temperature of the heat medium flowing in the jacket circulation pipe is monitored by the thermometer 47. When the temperature deviates from the set temperature of 80 ° C., the slave controller 48 selects the first flow rate adjustment valve 11 or the second flow rate adjustment valve. 31 is adjusted so that the set temperature is maintained at 80 ° C.

  At this time, when the first flow rate adjustment valve 11 is opened, the first feedback valve 62 is opened. When the second flow rate adjustment valve 31 is opened, the second feedback valve 63 is opened. When the heat medium is sent from the circulation pipe A to the jacket circulation pipe, the heat medium is returned from the jacket circulation pipe to the first circulation pipe A, and the heat medium is sent from the second circulation pipe B to the jacket circulation pipe. When this is done, control is performed so that the heat medium is returned from the jacket circulation pipe to the second circulation pipe B. By controlling in this way, it becomes possible to make uniform the liquid quantity of the several heat medium tank which stores the heat medium from which temperature differs.

  In addition, when the heat medium is sent from the first circulation pipe A or the second circulation pipe B to the jacket circulation pipe, the supply amount of the heat medium from the first or second circulation pipe A or B is the first amount. The discharge pressures of the pump 8 and the pump 28 that supply the heat medium are adjusted so that the flow rate of the heat medium circulating in the circulation pipe A, the second circulation pipe B, or the jacket circulation pipe is always 1/3 or less. Is done.

  When such control is not performed, when switching from heating to cooling and from cooling to heating, the temperature of the heat medium in the first circulation pipe A or the second circulation pipe B rapidly changes. Unless the capacity of the first tank 1 or the second tank 21 is made very large, the temperature of the heat medium in the first tank 1 or the second tank 21 changes rapidly, and stable supply of the heat medium cannot be performed. Further, when the cooling medium of the second tank 21 is cooled directly by using a high flash point silicone oil as the refrigerant of the refrigerator, an abnormality occurs in the refrigerator.

  Further, when the jacket 43 is the spiral baffle jacket shown in FIG. 2, the interval between the adjacent baffle plates 43 a, 43 a is narrowed, and the pumping amount of the circulation pump 13 is made larger than usual. By setting the flow rate of the heat medium to 1 m / sec, the flow rate of the heat medium in the jacket 43 can be increased and the amount of heat transfer can be increased.

For example, as a reactor 42, using a stainless with steel stirrer vessel having an inner volume of 1 m ^3, the temperature of the heat medium as a -10 ° C., so that the overall heat transfer coefficient 200kcal ^{/ m} 2 · hr · ℃ about In this case, the gap between adjacent baffle plates may be about 50 mm and the flow rate may be about 1.2 m / second.
In the temperature control apparatus of the present invention preferably has the overall heat transfer coefficient to the temperature-controlled, such as the reactor 42 is 150kcal ^{/ m} 2 · hr · ℃ or higher, more preferably, 180~300kcal / ^{m 2} · Hr · ° C.

  Further, since the second tank 21 stores a low-temperature heat medium at −40 ° C., it is necessary to prevent the heat medium from absorbing moisture. For this purpose, an evacuation line (not shown) is connected to the second tank 21 to perform evacuation by vacuum. This is a measure for filling the second tank 21 with the heat medium, because air is often involved due to its high viscosity, and is a means for facilitating moisture absorption. In addition, when filling the second tank 21 with the heat medium, it is possible to fill the second tank 21 while heating, and to remove the moisture absorbed by the filling.

In the present invention, it is preferable to employ model predictive control in order to more accurately control the internal temperature of the reactor 42.
In the reactor 42, in the course of progress of the batch process, property changes such as generation of reaction heat due to addition of reactants and catalyst, change in viscosity of contents, etc. occur. Therefore, maintaining the internal temperature at a set temperature, This is difficult with conventional PID control.
In particular, the program control of PID control cannot avoid the control delay due to the process dead time and time constant with respect to the set profile, which causes the phenomenon that the heating heat medium and the cooling heat medium are alternately supplied. As a result, controllability deteriorates.

For this reason, model predictive control is performed in order to perform highly accurate temperature control of the internal temperature of the reactor 42.
The model predictive control includes the operation amount and controlled amount in the reactor 42, for example, dynamic characteristics between the opening degree of the control valves 11 and 31 and the jacket inlet temperature 47, the jacket inlet temperature 47 and the internal temperature 50 of the reactor 42. An internal model that appropriately expresses the dynamic characteristics, the dynamic characteristics between the jacket inlet temperature 47 and the jacket outlet temperature 49, and the dynamic characteristics between the internal temperature 50 of the reactor 42 and the jacket outlet temperature 49 is constructed. Thus, temperature control of the internal temperature 50 of the reactor 42 and the jacket inlet temperature 47 is performed.

The internal model needs to be able to express the heat transfer of the reactor 42, and in order to construct the internal model, a material balance equation, a heat balance equation, a dynamic characteristic of the control valve, and the like are required. However, since these include many uncertain parameters, exact modeling is difficult. The internal model of this model predictive control assumes a simple first-order lag dead time process and performs a step response test to estimate each parameter (gain, first-order lag time, dead time) constituting them.
The internal model is expressed by the following equation.

  Here, G (S): transfer function, K: gain [−], T: primary delay time [sec], and L: dead time [sec].

  The step response test is a test for obtaining the relationship between the step input and the step response, and an example thereof is shown in FIG. For example, the step input is the valve opening, and the step response is the jacket inlet temperature. In this model predictive control, since the internal model is assumed as a first-order lag dead time process, gain K [−], first-order lag time T [sec], and dead time L [sec] are obtained from the step response results.

The gain K [−] indicating the relationship between the jacket inlet temperature and the internal temperature obtained by the step response test, the primary delay time T [sec], and the dead time L [sec] are used as an internal model of the master controller 51, and the valve opening and the jacket The relationship with the inlet temperature is gain K [−], primary delay time T [sec], and dead time L [sec] are internal models of the slave controller 48.
The model predictive cascade control program configured in this way can predict how the temperature will change in the future, for example, after changing the opening of the control valve, and thereby perform control in advance. Therefore, controllability more than PID control can be realized.

  Next, the example which compared the result of having implemented program control by PID cascade control and program control by model prediction control using the same temperature control apparatus is shown. FIG. 4 shows an example of the temperature control result of the crystallization process by PID cascade control, and FIG. 5 shows the valve opening result. In the PID cascade control, the jacket inlet temperature vibrates and the followability of the internal temperature with respect to the internal temperature set value is not good. Further, as apparent from FIG. 5, the supply of useless high-temperature heat medium and the alternate supply of low-temperature heat medium can be seen.

FIG. 6 shows the temperature control result of the crystallization process by model predictive control, and FIG. 7 shows an example of the valve opening result. Thus, in the model predictive control, the jacket inlet temperature does not oscillate and shows a smooth movement, and the followability of the internal temperature with respect to the internal temperature set value is improved.
Further, in all the batch processes, the maximum internal temperature deviation with respect to the internal temperature set value was 4.9 ° C. in the PID control, but the maximum internal temperature deviation with respect to the internal temperature set value is 2. It became 1 degreeC and controllability improved.
As is clear from FIG. 7, the supply of the hot medium and the supply of the low-temperature medium decreased as compared with the PID cascade control. In this example, in the entire batch process, the supply amount of the high-temperature heat medium was 1/6 of the PID control, and the supply amount of the low-temperature heat medium was 1/8.

Furthermore, in the present invention, in a reactor having a jacket having a structure divided into a plurality of stages in the horizontal direction, the effective jacket height (effective heat transfer area) is used in accordance with the water level of the solution in the reaction vessel. It is possible to switch the number of division stages and switch the length of the flow path in the jacket.
FIG. 8 is an example in which the height of the effective jacket can be switched between two ways. When the water level is high, the valve 82 is opened and the valve 81 is closed, thereby increasing the height of the effective jacket and lengthening the flow path in the jacket.

  When the water level is low, the valve 82 is closed and the valve 81 is opened, so that the effective jacket is lowered and the flow path in the jacket is shortened. Thus, when the flow path length in the jacket changes, the heat transfer to the process changes. Therefore, if the control parameter for model prediction is constant, the controllability is slightly deteriorated.

  In such a case, it is desirable to change the control parameter of the model predictive control according to the circulation pipe length. That is, the above-described gain K [−], first-order lag time T [sec], and dead time L [sec] are switched between three parameter sets for each circulation pipe length, and model predictive control is performed, thereby enabling more accurate temperature. Control can be realized.

It is a schematic block diagram which shows an example of the temperature control apparatus of this invention. It is a section explanatory view showing an example of the spiral baffle jacket in the present invention. It is step response explanatory drawing represented by the opening degree of the valve | bulb in the temperature control in this invention, and the jacket inlet temperature as the response result. It is program control explanatory drawing by the conventional PID control. It is a figure which shows the opening degree state of the 1st and 2nd flow regulating valve at the time of PID control implementation of FIG. It is program control explanatory drawing by the model prediction control in this invention. It is a figure which shows the opening degree state of the 1st and 2nd flow regulating valve at the time of model predictive control implementation of FIG. It is explanatory drawing which shows piping switching of the heating circulation system around a jacket.

Explanation of symbols

1, 2... Heat medium tank, 2, 22, ... Pipe, 3, 23 ... Pump 4, 24
..Heat exchanger, 7, 27 ... Tube, 8, 28 ... Pump, 9, 29 ... Tube, 10
, 30 ... Supply pipe, 11, 31 ... Flow rate adjusting valve, 64, 65 ... Return pipe,
13 .. Circulation pump, 41 .. Pipe, 42 .. Reactor (temperature controlled object), 43
・ Jacket, 44, 45, 61 ・ ・ Pipe, 62, 63 ・
・ Return valve, 48 ・ ・ Slave controller, 51 ・ ・ Master controller,
52 .. Internal temperature setting profile setting device

Claims (8)

A plurality of heat medium tanks for storing heat mediums having different temperatures;
A plurality of heating / cooling sources for heating or cooling individual heating media in these heating medium tanks and maintaining a constant temperature;
A plurality of circulation pipes for individually extracting the heat medium in these heat medium tanks and returning them to the respective heat medium tanks;
A jacket circulation pipe having a circulation pump that surrounds the object to be controlled and circulates the heat medium in a jacket for heating and cooling the object;
A supply pipe for supplying the heat medium from the plurality of heat medium tanks to the jacket circulation pipe;
Provided with return piping that distributes the heat medium from the jacket circulation piping back to the individual circulation piping,
A temperature control device, wherein the heat medium is a silicone oil having a flash point of 250 ° C or higher. The jacket is a spiral baffle jacket provided with a baffle formed in a spiral;
The temperature control device according to claim 1, wherein the circulation pump sets the flow rate of the heat medium in the jacket to 1 m / second or more.   There are a plurality of flow rate adjustment valves that reduce the amount of heat medium supplied from the supply piping to the jacket circulation piping to 1/3 or less of the amount of heat medium circulating in each circulation piping or the amount of heat medium circulating in the jacket circulation piping. The temperature control device according to claim 1, wherein the temperature control device is provided in a supply pipe.   3. A dry air supply pipe for feeding dry air having a dew point of −40 ° C. or less is connected to a heat medium tank that stores a heat medium having a temperature of 0 ° C. or less among the heat medium tanks. The temperature control device described. Controller for model predictive control of the temperature control of the temperature control object is provided, et al is, the control unit includes a master controller and a slave controller,
The master controller is a model predictive controller that includes the process model, and creates a control signal based on the deviation between the temperature data of the contents in the temperature controlled object and a preset temperature, and this control signal is The process model is transmitted to the slave controller, and the process model includes a gain K [−] indicating a relationship between the jacket inlet temperature and the temperature of the contents in the controlled object, a first-order lag time T [sec], and a dead time L A first-order lag time process with [sec] as a configuration parameter,
The slave controller is a model predictive controller including a process model, and the control signal from the master controller, the temperature of the contents inside the controlled object, the temperature of the heat medium flowing into the jacket, and the heat medium flowing out of the jacket A control signal is generated based on the temperature data of the temperature, and the control signal is sent to a flow rate adjustment valve provided in the supply pipe to adjust the opening of the flow rate adjustment valve. It is a first-order lag dead time process having gain K [-], a first-order lag time T [sec], and a dead time L [sec] representing the relationship between the opening of the regulating valve and the jacket inlet temperature. The temperature control device according to claim 1 or 2. The temperature control unit further includes an internal temperature setting profile generator. The internal temperature setting profile generator generates an internal temperature profile whose phase has been advanced by a time period that takes into account a delay in response due to the dead time of the temperature controlled object. 6. The temperature control device according to claim 5, wherein the temperature control device is generated and sent to the master controller in time series . The jacket is divided into a plurality of stages in the horizontal direction, and the flow path in the jacket is divided into a plurality of different length flow paths, and the heat medium is switched to the different length flow paths. 6. The temperature control apparatus according to claim 5 , wherein, when supplying, the temperature control unit switches a control parameter for model predictive control in accordance with a length of the flow path . The overall heat transfer coefficient for heat transfer from the jacket to the temperature controlled object when controlling the temperature controlled object through the jacket is 150 to 300 kcal / m ² · hr · ° C. Item 3. The temperature control device according to Item 1 or 2.

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