CN111620826A - Method and system for controlling temperature in synthesis of 1,2,4-1H triazole - Google Patents
Method and system for controlling temperature in synthesis of 1,2,4-1H triazole Download PDFInfo
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- CN111620826A CN111620826A CN202010394652.3A CN202010394652A CN111620826A CN 111620826 A CN111620826 A CN 111620826A CN 202010394652 A CN202010394652 A CN 202010394652A CN 111620826 A CN111620826 A CN 111620826A
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- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D249/00—Heterocyclic compounds containing five-membered rings having three nitrogen atoms as the only ring hetero atoms
- C07D249/02—Heterocyclic compounds containing five-membered rings having three nitrogen atoms as the only ring hetero atoms not condensed with other rings
- C07D249/08—1,2,4-Triazoles; Hydrogenated 1,2,4-triazoles
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Abstract
The invention provides a method and a system for controlling temperature in the synthesis of 1,2,4-1H triazole, wherein the method comprises the following steps: measuring the synthesis temperature in the synthesis process of the 1,2,4-1H triazole in real time; when the synthesis temperature is lower than the minimum value of the first preset temperature range, controlling the heat-conducting oil jacket to heat the reactor until the synthesis temperature in the reactor rises to the first preset temperature range; and when the synthesis temperature is higher than the maximum value of the first preset temperature range, controlling the heat-conducting oil jacket to cool the reactor until the synthesis temperature in the reactor is reduced to the first preset temperature range. By setting a first preset temperature range and adopting a heating mode of a heat conduction oil jacket, constant temperature control is carried out, the reaction efficiency of reactants is improved, and the generation of impurity products is reduced.
Description
Technical Field
The invention relates to the technical field of temperature control, in particular to a method and a system for controlling the temperature in the synthesis of 1,2,4-1H triazole.
Background
In the prior art, the synthesis temperature adopted in the process of synthesizing 1,2, 4-1H-triazole is 145-160 ℃, the impurity products of the 1,2, 4-1H-triazole synthesized at the temperature are too much, and in the prior art, a heating mode is adopted in the process of synthesizing 1,2, 4-1H-triazole to heat a saturated steam jacket, and the reaction time of a corresponding batch of materials is 32 hours by adopting the heating mode, so that the reaction efficiency is too low, and in order to ensure that the reaction efficiency is ensured in the process of synthesizing 1,2, 4-1H-triazole, the invention provides a method and a system for controlling the temperature in the synthesis of 1,2, 4-1H-triazole.
Disclosure of Invention
The invention provides a method and a system for controlling the temperature in the synthesis of 1,2,4-1H triazole, which are used for carrying out constant temperature control by setting a first preset temperature range and adopting a heating mode of a heat conduction oil jacket to improve the reaction efficiency of reactants and reduce the generation of impurity products.
The invention provides a method for controlling the temperature in the synthesis of 1,2,4-1H triazole, which comprises the following steps:
measuring the synthesis temperature in the synthesis process of the 1,2,4-1H triazole in real time;
when the synthesis temperature is lower than the minimum value of a first preset temperature range, controlling a heat-conducting oil jacket to heat a reactor until the synthesis temperature in the reactor is raised to the first preset temperature range;
and when the synthesis temperature is higher than the maximum value of the first preset temperature range, controlling the heat-conducting oil jacket to cool the reactor until the synthesis temperature in the reactor is reduced to the first preset temperature range.
Preferably, the real-time measurement of the synthesis temperature in the process of synthesizing the 1,2,4-1H triazole comprises the following steps:
heating the heat conduction oil in the heat conduction oil jacket based on an electric heating pipe;
measuring the heat conduction temperature of the heat conduction oil, and controlling the electric heating pipe to stop heating when the heat conduction temperature reaches a second preset temperature range;
and meanwhile, controlling the heat-conducting oil jacket to be in a constant temperature state, and adding an initial reactant into the reactor to generate the 1,2,4-1H triazole when the heat-conducting oil jacket is in the constant temperature state.
Preferably, the step of controlling the heat conducting oil jacket to cool the reactor comprises:
acquiring a temperature difference value between the synthesis temperature and the maximum value of a first preset temperature range;
according to the temperature difference, selecting a first valve from preset temperature valves to close;
monitoring the synthesis temperature in real time after the first valve is closed;
and when the synthesis temperature reaches a first preset temperature range, selecting a second valve from the first valves to open according to a descending curve of the synthesis temperature.
Preferably, the controlling the heat conducting oil jacket to heat the reactor comprises:
determining the carbon value of the heat conduction oil in the heat conduction oil jacket, and calculating the viscosity eta of the heat conduction oil;
wherein rho represents the liquid density value of the heat transfer oil at a preset temperature K; m represents the relative molecular weight of the heat transfer oil; a1 represents a first contribution value of a molecular group of the thermal oil; a2 represents a second contribution value of the molecular group of the thermal oil;
when the viscosity and the carbon value both meet the heat conduction standard, determining a target temperature corresponding to the heat conduction oil jacket, detecting a current temperature corresponding to the heat conduction oil jacket, and simultaneously acquiring a first operating parameter w1 of the heat conduction oil jacket from a temperature database according to the target temperature t0 and the current temperature t 1;
determining the reaction capacity c of the reactor and the material mass z of the initial reactant, and acquiring a second operating parameter w2 of the heat-conducting oil jacket from a reaction database;
measuring the liquid level h of heat conduction oil in the heat conduction oil jacket, and obtaining a third operating parameter w3 of the heat conduction oil jacket from a heat conduction oil database;
judging whether the volume of the solution of the heat-conducting oil needs to be increased or not according to the first operating parameter w1, the second operating parameter w2 and the third operating parameter w 3;
D＝a1w1*et0-t1+a2w2*e0.2c+0.3z+a3w3*eh；
wherein D represents the operation integrated value based on the operation parameter; a1, a2 and a3 are operation factors of the operation parameters, and a1+ a2+ a3 is 1;
when the operation comprehensive value D is greater than the standard comprehensive value Y, the volume of the solution of the heat conduction oil does not need to be increased;
otherwise, correspondingly increasing the volume of the solution of the heat-conducting oil according to the difference value of the Y and the D;
and when one of the viscosity and the carbon value does not meet the heat conduction standard, early warning and warning are carried out, and meanwhile, the heat conduction oil is replaced.
Preferably, the method further comprises the following steps:
determining the contact surface of the reactor and an initial reactant;
carrying out temperature monitoring on the contact surface, and acquiring the contact temperature of n contact points in the contact surface, wherein the heat conduction temperature T is { T ═ T based on m groups1,T2,...,TmDetermining the point temperatures of n contact points in the contact surface to obtain the point temperature T of each contact pointi＝{Ti1,Ti2,...,TimIn which T ismDenotes the heat conduction temperature, T, of the m-th groupimThe point temperature obtained by temperature transfer of the ith contact point based on the m-th group of heat conduction temperatures is represented, i is 1,2, 3.
Calculating the total temperature difference of each contact point;
ΔTim＝T1-Ti1+T2-Ti2+...+Tm-Tim；
wherein, Delta TimRepresenting the total temperature difference of the ith contact point in temperature transfer based on the m groups of heat conduction temperatures;
calculating the heat conduction value of each contact point;
wherein S isiIndicating the heat conduction value of the ith contact point; max (T)1-Ti1,...,Tm-Tim) Representing the maximum temperature difference of the ith contact point based on the m groups of heat conduction temperatures; min (T)1-Ti1,...,Tm-Tim) Representing the minimum temperature difference of the ith contact point based on the m groups of heat conduction temperatures;iindicating the heat resistance value of the ith contact point;
dividing heat conducting areas of the contact points according to the heat conducting values and the point position information of the contact points, which are currently positioned on the contact surface;
judging whether the area contact surfaces corresponding to the divided heat conduction areas are in heat conduction balance or not;
if yes, no operation is executed;
otherwise, a heating device is arranged at the area part with the unbalanced heat conduction, and the heating device is controlled to locally heat the area part with the unbalanced heat conduction, so that the balanced heating is realized.
Preferably, the first preset temperature range is [170 ℃, 175 ℃).
The invention provides a system for controlling the temperature in the synthesis of 1,2,4-1H triazole, which comprises the following components:
the measuring module is used for measuring the synthesis temperature in the synthesis process of the 1,2,4-1H triazole in real time;
the control module is used for controlling the heat-conducting oil jacket to heat the reactor when the synthesis temperature is lower than the minimum value of a first preset temperature range until the synthesis temperature in the reactor rises to the first preset temperature range;
and when the synthesis temperature is higher than the maximum value of the first preset temperature range, controlling the heat-conducting oil jacket to cool the reactor until the synthesis temperature in the reactor is reduced to the first preset temperature range.
Preferably, the method further comprises the following steps: a rectifying tower and a tail gas treatment device;
the reactor is in two-way communication with the rectifying tower, and the rectifying tower is in one-way communication with the tail gas treatment device;
wherein the reactor is used for containing a first initial reactant and a second initial reactant, and when the first initial reactant and the second initial reactant are reacted, a first product, a second product, a third product and a fourth product are generated;
the rectifying tower is used for receiving the second product, the third product and the fourth product transmitted by the reactor, generating a fifth product when the second product and the third product react, and refluxing the fifth product to the reactor;
the reactor is used for receiving the fifth product, generating a first product, a second product, a third product and a fourth product when the fifth product reacts with the second initial reactant, and executing cyclic processing;
and the rectifying tower is also used for transmitting the redundant third product and the redundant fourth product generated by the generator to the tail gas treatment device for tail gas treatment.
Preferably, the first initial reactant is hydrazine hydrate and the second initial reactant is formamide;
the first product is 1,2, 4-1H-triazole, the second product is formic acid, the third product is ammonia gas, the fourth product is water vapor, and the fifth product is ammonia formate.
Additional features and advantages of the invention will be set forth in the description which follows, and in part will be obvious from the description, or may be learned by practice of the invention. The objectives and other advantages of the invention will be realized and attained by the structure particularly pointed out in the written description and claims hereof as well as the appended drawings.
The technical solution of the present invention is further described in detail by the accompanying drawings and embodiments.
Drawings
The accompanying drawings, which are included to provide a further understanding of the invention and are incorporated in and constitute a part of this specification, illustrate embodiments of the invention and together with the description serve to explain the principles of the invention and not to limit the invention. In the drawings:
FIG. 1 is a flow chart of a method for controlling temperature in the synthesis of 1,2,4-1H triazole in the embodiment of the invention;
FIG. 2 is a structural diagram of a temperature control system in the synthesis of 1,2,4-1H triazole in the embodiment of the invention;
FIG. 3 is a block diagram of processing reactants in an embodiment of the present invention.
Detailed Description
The preferred embodiments of the present invention will be described in conjunction with the accompanying drawings, and it will be understood that they are described herein for the purpose of illustration and explanation and not limitation.
The invention provides a method for controlling the temperature in the synthesis of 1,2,4-1H triazole, which comprises the following steps as shown in figure 1:
step 1: measuring the synthesis temperature in the synthesis process of the 1,2,4-1H triazole in real time;
step 2: when the synthesis temperature is lower than the minimum value of a first preset temperature range, controlling a heat-conducting oil jacket to heat a reactor until the synthesis temperature in the reactor is raised to the first preset temperature range;
and step 3: and when the synthesis temperature is higher than the maximum value of the first preset temperature range, controlling the heat-conducting oil jacket to cool the reactor until the synthesis temperature in the reactor is reduced to the first preset temperature range.
Preferably, the first preset temperature range is [170 ℃, 175 ℃).
In the embodiment, the real-time temperature is measured, so that the synthesis temperature can be conveniently and effectively adjusted in time, the synthesis temperature is ensured to be within the first preset temperature range, the generation of impurity products is reduced, and when the synthesis temperature is 170-175 ℃, the purity of the product obtained by the reaction is obviously improved.
And the temperature range is 170-175 ℃, the reaction time of a batch of materials generally needs 18 hours, and the reaction efficiency is greatly improved.
In this embodiment, the heating treatment may be heating the heat conducting oil in the heat conducting oil jacket, so as to raise the synthesis temperature; the cooling treatment can be cooling and heating the heat conducting oil in the heat conducting oil jacket so as to reduce the synthesis temperature.
The beneficial effects of the above technical scheme are: by setting a first preset temperature range and adopting a heating mode of a heat conduction oil jacket, constant temperature control is carried out, the reaction efficiency of reactants is improved, and the generation of impurity products is reduced.
The invention provides a method for controlling the temperature in the synthesis of 1,2,4-1H triazole, which comprises the following steps before the real-time measurement of the synthesis temperature in the synthesis process of the 1,2,4-1H triazole:
heating the heat conduction oil in the heat conduction oil jacket based on an electric heating pipe;
measuring the heat conduction temperature of the heat conduction oil, and controlling the electric heating pipe to stop heating when the heat conduction temperature reaches a second preset temperature range;
and meanwhile, controlling the heat-conducting oil jacket to be in a constant temperature state, and adding an initial reactant into the reactor to generate the 1,2,4-1H triazole when the heat-conducting oil jacket is in the constant temperature state.
In the embodiment, the heat conducting oil is firstly heated, when the heat conducting oil is heated to a certain temperature, the controller is in a constant temperature state, and then the initial reactant is added into the reactor, so that the waste of the initial reactant is avoided.
In this embodiment, the second predetermined temperature range may include 170 ℃ and 175 ℃, such as: [169 ℃, 176 ℃ C. ].
The beneficial effects of the above technical scheme are: before the 1,2,4-1H triazole is synthesized, the heat conducting oil is heated, the synthesis efficiency of the subsequent 1,2,4-1H triazole is improved, and the waste of initial reactants is avoided.
The invention provides a method for controlling the temperature in the synthesis of 1,2,4-1H triazole, wherein the step of controlling a heat-conducting oil jacket to cool a reactor comprises the following steps:
acquiring a temperature difference value between the synthesis temperature and the maximum value of a first preset temperature range;
according to the temperature difference, selecting a first valve from preset temperature valves to close;
monitoring the synthesis temperature in real time after the first valve is closed;
and when the synthesis temperature reaches a first preset temperature range, selecting a second valve from the first valves to open according to a descending curve of the synthesis temperature.
In this embodiment, the cooling is performed because the synthesis temperature is higher than 175 ℃, and the relevant first valve is selected to be closed by determining the temperature difference, for example, there is a power supply to the heat conducting oil jacket based on the valves 1,2,3, 4,5, and thus heat is supplied, and at this time, the valves 1,2,3 are closed to lower the synthesis temperature, and at the same time, the valve 1 is opened according to the lowering curve of the synthesis temperature.
The beneficial effects of the above technical scheme are: through first valve and second valve, effectual control synthesis temperature, and then improve reaction efficiency.
The invention provides a method for controlling the temperature in the synthesis of 1,2,4-1H triazole, wherein the process of controlling a heat-conducting oil jacket to heat a reactor comprises the following steps:
determining the carbon value of the heat conduction oil in the heat conduction oil jacket, and calculating the viscosity eta of the heat conduction oil;
wherein rho represents the liquid density value of the heat transfer oil at a preset temperature K; m represents the relative molecular weight of the heat transfer oil; a1 represents a first contribution value of a molecular group of the thermal oil; a2 represents a second contribution value of the molecular group of the thermal oil;
when the viscosity and the carbon value both meet the heat conduction standard, determining a target temperature corresponding to the heat conduction oil jacket, detecting a current temperature corresponding to the heat conduction oil jacket, and simultaneously acquiring a first operating parameter w1 of the heat conduction oil jacket from a temperature database according to the target temperature t0 and the current temperature t 1;
determining the reaction capacity c of the reactor and the material mass z of the initial reactant, and acquiring a second operating parameter w2 of the heat-conducting oil jacket from a reaction database;
measuring the liquid level h of heat conduction oil in the heat conduction oil jacket, and obtaining a third operating parameter w3 of the heat conduction oil jacket from a heat conduction oil database;
judging whether the volume of the solution of the heat-conducting oil needs to be increased or not according to the first operating parameter w1, the second operating parameter w2 and the third operating parameter w 3;
D＝a1w1*et0-t1+a2w2*e0.2c+0.3z+a3w3*eh；
wherein D represents the operation integrated value based on the operation parameter; a1, a2 and a3 are operation factors of the operation parameters, and a1+ a2+ a3 is 1;
when the operation comprehensive value D is greater than the standard comprehensive value Y, the volume of the solution of the heat conduction oil does not need to be increased;
otherwise, correspondingly increasing the volume of the solution of the heat-conducting oil according to the difference value of the Y and the D;
and when one of the viscosity and the carbon value does not meet the heat conduction standard, early warning and warning are carried out, and meanwhile, the heat conduction oil is replaced.
In the embodiment, the carbon value and the viscosity are important indexes for measuring the qualification of the heat transfer oil, so whether the heat transfer oil is replaced is determined by judging whether the carbon value and the viscosity of the heat transfer oil are qualified.
In this embodiment, the volume of the solution of the heat transfer oil is increased, and the heat transfer oil may be charged into the heat transfer oil jacket.
In this embodiment, the first operating parameter is, for example, heating power; the second operating parameter is, for example, the heating time; the third operating parameter is, for example, the heat transfer rate of the thermal oil; and a1 is power factor, a2 is time factor, a3 is thermal conductivity rate factor; and the operational composite value may be, for example, a thermal conductivity value and the standard composite value may be, for example, a standard thermal conductivity value.
The beneficial effects of the above technical scheme are: firstly, whether the heat conduction oil is replaced is intelligently judged by determining the carbon value and the viscosity of the heat conduction oil, secondly, a first operating parameter is determined by temperature, a second operating parameter is determined by reaction capacity and material quality, a third operating parameter is determined by liquid level, and then whether the volume of the solution of the heat conduction oil needs to be increased is intelligently determined by an operation comprehensive value, so that a verification basis is provided for effective temperature control in the follow-up process.
The invention provides a method for controlling the temperature in the synthesis of 1,2,4-1H triazole, which further comprises the following steps:
determining the contact surface of the reactor and an initial reactant;
carrying out temperature monitoring on the contact surface, and acquiring the contact temperature of n contact points in the contact surface, wherein the heat conduction temperature T is { T ═ T based on m groups1,T2,...,TmDetermining the point temperatures of n contact points in the contact surface to obtain the point temperature T of each contact pointi＝{Ti1,Ti2,...,TimIn which T ismDenotes the heat conduction temperature, T, of the m-th groupimThe point temperature obtained by temperature transfer of the ith contact point based on the m-th group of heat conduction temperatures is represented, i is 1,2, 3.
Calculating the total temperature difference of each contact point;
ΔTim＝T1-Ti1+T2-Ti2+...+Tm-Tim；
wherein, Delta TimRepresenting the total temperature difference of the ith contact point in temperature transfer based on the m groups of heat conduction temperatures;
calculating the heat conduction value of each contact point;
wherein S isiIndicating the heat conduction value of the ith contact point; max (T)1-Ti1,...,Tm-Tim) Representing the maximum temperature difference of the ith contact point based on the m groups of heat conduction temperatures; min (T)1-Ti1,...,Tm-Tim) Representing the minimum temperature difference of the ith contact point based on the m groups of heat conduction temperatures;iindicating the heat resistance value of the ith contact point;
dividing heat conducting areas of the contact points according to the heat conducting values and the point position information of the contact points, which are currently positioned on the contact surface;
judging whether the area contact surfaces corresponding to the divided heat conduction areas are in heat conduction balance or not;
if yes, no operation is executed;
otherwise, a heating device is arranged at the area part with the unbalanced heat conduction, and the heating device is controlled to locally heat the area part with the unbalanced heat conduction, so that the balanced heating is realized.
In this embodiment, because the reactant can not ensure that every part of contact surface all is heated evenly in the reaction process, consequently, through judging the position that is heated unevenly to carry out local heating to this position, ensure to be heated evenly, improve reaction efficiency for the reaction is abundant.
In this embodiment, the point position information refers to the current coordinates of the contact point, and when the heated unbalanced portion is determined, since the portion is generally a certain area, the accuracy of dividing the heat conduction area is improved based on the point position information and the comprehensive determination of the heat conduction value.
The beneficial effects of the above technical scheme are: through the contact surface of confirming reactant and initial reactant to the point temperature of every contact point is monitored, through multiunit monitoring, obtains the total temperature difference of every contact point, through the heat conduction value of confirming the contact point, and then effectually divides the heat conduction region, owing to in reaction process, there is the unbalanced position of being heated, consequently, through carrying out the local heating to corresponding heat conduction region, the realization is heated balancedly, is convenient for carry out effective control to its synthetic temperature, improves reaction efficiency.
The invention provides a system for controlling the temperature in the synthesis of 1,2,4-1H triazole, as shown in figure 2, comprising:
the measuring module is used for measuring the synthesis temperature in the synthesis process of the 1,2,4-1H triazole in real time;
the control module is used for controlling the heat-conducting oil jacket to heat the reactor when the synthesis temperature is lower than the minimum value of a first preset temperature range until the synthesis temperature in the reactor rises to the first preset temperature range;
and when the synthesis temperature is higher than the maximum value of the first preset temperature range, controlling the heat-conducting oil jacket to cool the reactor until the synthesis temperature in the reactor is reduced to the first preset temperature range.
The beneficial effects of the above technical scheme are: by setting a first preset temperature range and adopting a heating mode of a heat conduction oil jacket, constant temperature control is carried out, the reaction efficiency of reactants is improved, and the generation of impurity products is reduced.
The invention provides a system for controlling the temperature in the synthesis of 1,2,4-1H triazole, which is shown in figure 3 and further comprises: a rectifying tower and a tail gas treatment device;
the reactor is in two-way communication with the rectifying tower, and the rectifying tower is in one-way communication with the tail gas treatment device;
wherein the reactor is used for containing a first initial reactant and a second initial reactant, and when the first initial reactant and the second initial reactant are reacted, a first product, a second product, a third product and a fourth product are generated;
the rectifying tower is used for receiving the second product, the third product and the fourth product transmitted by the reactor, generating a fifth product when the second product and the third product react, and refluxing the fifth product to the reactor;
the reactor is used for receiving the fifth product, generating a first product, a second product, a third product and a fourth product when the fifth product reacts with the second initial reactant, and executing cyclic processing;
and the rectifying tower is also used for transmitting the redundant third product and the redundant fourth product generated by the generator to the tail gas treatment device for tail gas treatment.
Preferably, the first initial reactant is hydrazine hydrate and the second initial reactant is formamide;
the first product is 1,2, 4-1H-triazole, the second product is formic acid, the third product is ammonia gas, the fourth product is water vapor, and the fifth product is ammonia formate.
Since the boiling point of formic acid, ammonia and water vapor generated in the reaction process of the first initial reactant and the second initial reactant is low and is lower than 170 ℃, and the reaction temperature of the first initial reactant and the second initial reactant is 175 ℃ at 170 ℃, if the formic acid, the ammonia and the water vapor are directly cooled and discharged to a tail gas absorption device, the method is obviously very wasteful. Therefore, the technical scheme is provided.
The high-concentration ammonia formate can be separated by arranging the rectifying tower, the ammonia formate flows back to the reactor to react with hydrazine hydrate, the ammonia formate flows back to the reactor through a cooling part together with tail gas in the prior art, the generated formic acid and ammonia gas easily enter a tail gas absorption device to form insufficient conversion of raw materials, namely, the raw material formamide is not fully converted into a product.
The beneficial effects of the above technical scheme are: the generated formic acid and ammonia gas are fully synthesized and flow back to the reactor added with hydrazine hydrate, the recycling of substances is improved, the generated moisture is timely removed out of the reactor, the interference to the reaction is avoided, and the heat consumption can be reduced by arranging the rectifying tower, so that the reaction can be carried out in the positive direction.
It will be apparent to those skilled in the art that various changes and modifications may be made in the present invention without departing from the spirit and scope of the invention. Thus, if such modifications and variations of the present invention fall within the scope of the claims of the present invention and their equivalents, the present invention is also intended to include such modifications and variations.
Claims (9)
1. A method for controlling temperature in the synthesis of 1,2,4-1H triazole is characterized by comprising the following steps:
measuring the synthesis temperature in the synthesis process of the 1,2,4-1H triazole in real time;
when the synthesis temperature is lower than the minimum value of a first preset temperature range, controlling a heat-conducting oil jacket to heat a reactor until the synthesis temperature in the reactor is raised to the first preset temperature range;
and when the synthesis temperature is higher than the maximum value of the first preset temperature range, controlling the heat-conducting oil jacket to cool the reactor until the synthesis temperature in the reactor is reduced to the first preset temperature range.
2. The method of claim 1, wherein the real-time measurement of the synthesis temperature during the synthesis of 1,2,4-1H triazole comprises:
heating the heat conduction oil in the heat conduction oil jacket based on an electric heating pipe;
measuring the heat conduction temperature of the heat conduction oil, and controlling the electric heating pipe to stop heating when the heat conduction temperature reaches a second preset temperature range;
and meanwhile, controlling the heat-conducting oil jacket to be in a constant temperature state, and adding an initial reactant into the reactor to generate the 1,2,4-1H triazole when the heat-conducting oil jacket is in the constant temperature state.
3. The method of claim 1, wherein the step of controlling the conduction oil jacket to cool the reactor comprises:
acquiring a temperature difference value between the synthesis temperature and the maximum value of a first preset temperature range;
according to the temperature difference, selecting a first valve from preset temperature valves to close;
monitoring the synthesis temperature in real time after the first valve is closed;
and when the synthesis temperature reaches a first preset temperature range, selecting a second valve from the first valves to open according to a descending curve of the synthesis temperature.
4. The method according to claim 1, wherein controlling the heat conducting oil jacket to heat the reactor comprises:
determining the carbon value of the heat conduction oil in the heat conduction oil jacket, and calculating the viscosity eta of the heat conduction oil;
wherein rho represents the liquid density value of the heat transfer oil at a preset temperature K; m represents the relative molecular weight of the heat transfer oil; a1 represents a first contribution value of a molecular group of the thermal oil; a2 represents a second contribution value of the molecular group of the thermal oil;
when the viscosity and the carbon value both meet the heat conduction standard, determining a target temperature corresponding to the heat conduction oil jacket, detecting a current temperature corresponding to the heat conduction oil jacket, and simultaneously acquiring a first operating parameter w1 of the heat conduction oil jacket from a temperature database according to the target temperature t0 and the current temperature t 1;
determining the reaction capacity c of the reactor and the material mass z of the initial reactant, and acquiring a second operating parameter w2 of the heat-conducting oil jacket from a reaction database;
measuring the liquid level h of heat conduction oil in the heat conduction oil jacket, and obtaining a third operating parameter w3 of the heat conduction oil jacket from a heat conduction oil database;
judging whether the volume of the solution of the heat-conducting oil needs to be increased or not according to the first operating parameter w1, the second operating parameter w2 and the third operating parameter w 3;
D＝a1w1*et0-t1+a2w2*e0.2c+0.3z+a3w3*eh；
wherein D represents the operation integrated value based on the operation parameter; a1, a2 and a3 are operation factors of the operation parameters, and a1+ a2+ a3 is 1;
when the operation comprehensive value D is greater than the standard comprehensive value Y, the volume of the solution of the heat conduction oil does not need to be increased;
otherwise, correspondingly increasing the volume of the solution of the heat-conducting oil according to the difference value of the Y and the D;
and when one of the viscosity and the carbon value does not meet the heat conduction standard, early warning and warning are carried out, and meanwhile, the heat conduction oil is replaced.
5. The method of claim 1, further comprising:
determining the contact surface of the reactor and an initial reactant;
carrying out temperature monitoring on the contact surface, and acquiring the contact temperature of n contact points in the contact surface, wherein the heat conduction temperature T is { T ═ T based on m groups1,T2,...,TmDetermining the point temperatures of n contact points in the contact surface to obtain the point temperature T of each contact pointi＝{Ti1,Ti2,...,TimIn which T ismDenotes the heat conduction temperature, T, of the m-th groupimThe point temperature obtained by temperature transfer of the ith contact point based on the m-th group of heat conduction temperatures is represented, i is 1,2, 3.
Calculating the total temperature difference of each contact point;
ΔTim＝T1-Ti1+T2-Ti2+...+Tm-Tim；
wherein, Delta TimRepresenting the total temperature difference of the ith contact point in temperature transfer based on the m groups of heat conduction temperatures;
calculating the heat conduction value of each contact point;
wherein S isiIndicating the heat conduction value of the ith contact point; max (T)1-Ti1,...,Tm-Tim) Indicating the ith contact point based onmaximum temperature difference of m groups of heat conduction temperatures; min (T)1-Ti1,...,Tm-Tim) Representing the minimum temperature difference of the ith contact point based on the m groups of heat conduction temperatures;iindicating the heat resistance value of the ith contact point;
dividing heat conducting areas of the contact points according to the heat conducting values and the point position information of the contact points, which are currently positioned on the contact surface;
judging whether the area contact surfaces corresponding to the divided heat conduction areas are in heat conduction balance or not;
if yes, no operation is executed;
otherwise, a heating device is arranged at the area part with the unbalanced heat conduction, and the heating device is controlled to locally heat the area part with the unbalanced heat conduction, so that the balanced heating is realized.
6. The method of claim 1,
the first predetermined temperature range is [170 ℃, 175 ℃).
7. A system for controlling the temperature in the synthesis of 1,2,4-1H triazole is characterized by comprising the following components:
the measuring module is used for measuring the synthesis temperature in the synthesis process of the 1,2,4-1H triazole in real time;
the control module is used for controlling the heat-conducting oil jacket to heat the reactor when the synthesis temperature is lower than the minimum value of a first preset temperature range until the synthesis temperature in the reactor rises to the first preset temperature range;
and when the synthesis temperature is higher than the maximum value of the first preset temperature range, controlling the heat-conducting oil jacket to cool the reactor until the synthesis temperature in the reactor is reduced to the first preset temperature range.
8. The system of claim 7, further comprising: a rectifying tower and a tail gas treatment device;
the reactor is in two-way communication with the rectifying tower, and the rectifying tower is in one-way communication with the tail gas treatment device;
wherein the reactor is used for containing a first initial reactant and a second initial reactant, and when the first initial reactant and the second initial reactant are reacted, a first product, a second product, a third product and a fourth product are generated;
the rectifying tower is used for receiving the second product, the third product and the fourth product transmitted by the reactor, generating a fifth product when the second product and the third product react, and refluxing the fifth product to the reactor;
the reactor is used for receiving the fifth product, generating a first product, a second product, a third product and a fourth product when the fifth product reacts with the second initial reactant, and executing cyclic processing;
and the rectifying tower is also used for transmitting the redundant third product and the redundant fourth product generated by the generator to the tail gas treatment device for tail gas treatment.
9. The system of claim 8,
the first initial reactant is hydrazine hydrate, and the second initial reactant is formamide;
the first product is 1,2, 4-1H-triazole, the second product is formic acid, the third product is ammonia gas, the fourth product is water vapor, and the fifth product is ammonia formate.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114610090A (en) * | 2022-03-09 | 2022-06-10 | 新泰市日进化工科技有限公司 | Temperature control system is used in triazole production based on thing networking |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114610090A (en) * | 2022-03-09 | 2022-06-10 | 新泰市日进化工科技有限公司 | Temperature control system is used in triazole production based on thing networking |
| CN114610090B (en) * | 2022-03-09 | 2023-02-24 | 新泰市日进化工科技有限公司 | Temperature control system for triazole production based on Internet of things |
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