CN117032359A - Gas phase ammonolysis control system and control method - Google Patents
Gas phase ammonolysis control system and control method Download PDFInfo
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- CN117032359A CN117032359A CN202311060523.0A CN202311060523A CN117032359A CN 117032359 A CN117032359 A CN 117032359A CN 202311060523 A CN202311060523 A CN 202311060523A CN 117032359 A CN117032359 A CN 117032359A
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- 238000005915 ammonolysis reaction Methods 0.000 title claims abstract description 73
- 238000000034 method Methods 0.000 title claims abstract description 38
- 238000006243 chemical reaction Methods 0.000 claims abstract description 153
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims abstract description 61
- 238000010438 heat treatment Methods 0.000 claims abstract description 16
- 229910021529 ammonia Inorganic materials 0.000 claims description 16
- 230000001276 controlling effect Effects 0.000 claims description 13
- 230000001105 regulatory effect Effects 0.000 claims description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 9
- 229910000831 Steel Inorganic materials 0.000 claims description 6
- 239000007788 liquid Substances 0.000 claims description 6
- 238000013507 mapping Methods 0.000 claims description 6
- 239000010959 steel Substances 0.000 claims description 6
- 238000000354 decomposition reaction Methods 0.000 claims description 3
- 238000007599 discharging Methods 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 abstract description 3
- 239000012071 phase Substances 0.000 description 20
- 108091034117 Oligonucleotide Proteins 0.000 description 6
- 238000005485 electric heating Methods 0.000 description 3
- 238000003786 synthesis reaction Methods 0.000 description 3
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 2
- 235000011114 ammonium hydroxide Nutrition 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000004907 flux Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- -1 phosphoramidite triester Chemical class 0.000 description 1
- 125000006239 protecting group Chemical group 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000007790 solid phase Substances 0.000 description 1
Classifications
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- G—PHYSICS
- G05—CONTROLLING; REGULATING
- G05D—SYSTEMS FOR CONTROLLING OR REGULATING NON-ELECTRIC VARIABLES
- G05D27/00—Simultaneous control of variables covered by two or more of main groups G05D1/00 - G05D25/00
- G05D27/02—Simultaneous control of variables covered by two or more of main groups G05D1/00 - G05D25/00 characterised by the use of electric means
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Abstract
The invention discloses a gas-phase ammonolysis control system and a control method, which relate to the technical field of ammonolysis control and comprise a parameter setting module, a controller, a temperature regulator and a pressure regulator; the controller is used for comparing and analyzing the internal temperature of the reaction kettle with preset parameters, so as to drive the temperature regulator to regulate the internal temperature of the reaction kettle; when a heating signal is received, the temperature regulator is used for carrying out temperature regulation index analysis by combining the external environment temperature and the internal temperature of the reaction kettle, and determining the valve opening of the heat conducting oil valve in an auxiliary manner according to the temperature regulation index; the temperature control precision and the stability are effectively improved, the heat energy loss is reduced, and the production cost is reduced; the pressure regulator is used for carrying out pressure regulation index analysis by combining the internal pressure of the reaction kettle and the ammonolysis related parameters so as to obtain the optimal inlet flow of the reaction kettle through analysis; the ammonia gas can enter the reaction kettle at a proper speed, so that the pressure control precision and stability are effectively improved, and the safety of the ammonolysis reaction is improved.
Description
Technical Field
The invention relates to the technical field of ammonolysis control, in particular to a gas-phase ammonolysis control system and a control method.
Background
Oligonucleotide chemical synthesis starts from the end of the forty-th 20 th century to the sixty-th, and the oligonucleotide chemical synthesis method is continuously perfected, so that a solid-phase phosphoramidite triester method widely used today is gradually formed and automatic synthesis is realized; the synthesized oligonucleotide is cleaved under alkaline conditions of ammonia to remove the protecting group on the base and to cleave the synthesized oligonucleotide from the solid support to yield the synthesized oligonucleotide.
The current ammonolysis method mainly comprises an ammonia ammonolysis method, an electric heating ammonia gas phase ammonolysis method, a microwave heating ammonolysis method and other methods; the ammonia water ammonolysis method has the advantages that the treatment flux is small, the ammonolysis efficiency is influenced by low ammonia concentration, and the ammonolysis efficiency is unstable; the microwave heating method has uncontrollable temperature and unstable ammonolysis quality; the electric heating gas phase ammonolysis method has poor temperature stability, and the temperature fluctuation can reach about 10 ℃. The existing common ammonolysis method, ammonia ammonolysis method, generally needs 8-12 hours of ammonolysis, and the concentration of ammonia water has larger deviation; the electric heating gas phase ammonolysis method has large temperature control fluctuation, and the ammonolysis time needs about 2-2.5 hours; based on the defects, the invention provides a gas-phase ammonolysis control system and a control method.
Disclosure of Invention
The present invention aims to solve at least one of the technical problems existing in the prior art. Therefore, the invention provides a gas-phase ammonolysis control system and a control method.
To achieve the above object, an embodiment according to a first aspect of the present invention provides a gas-phase ammonolysis control system applied to a gas-phase ammonolysis apparatus, including a parameter setting module, a temperature acquisition module, a temperature regulator, a pressure acquisition module, and a pressure regulator;
the gas phase ammonolysis device comprises an ammonia steel cylinder, a reaction kettle and a heat conducting oil valve; the ammonia gas cylinder is connected with the reaction kettle through an air inlet pipe, and an air inlet valve is arranged on the air inlet pipe;
the parameter setting module is used for setting preset parameters by a user; the preset parameters comprise a reaction temperature range (W2-W3), a temperature set value, a pressure set value, a temperature correction coefficient and a pressure correction coefficient;
the temperature acquisition module is used for acquiring the internal temperature of the reaction kettle in real time and transmitting the internal temperature of the reaction kettle to the controller; the controller is used for comparing and analyzing the internal temperature of the reaction kettle with preset parameters, so that the temperature regulator is driven and controlled to regulate the internal temperature of the reaction kettle;
when a heating signal is received, the temperature regulator is used for carrying out temperature regulation index WZ analysis by combining the external environment temperature and the internal temperature TN of the reaction kettle, and determining the valve opening of the heat conducting oil valve in an auxiliary mode according to the temperature regulation index WZ; when the internal temperature of the reaction kettle reaches a temperature set value TS, the temperature regulator drives and controls the conduction oil valve to be closed, and generates a temperature standard signal to the controller;
responding to the temperature standard reaching signal, and opening an ammonia gas cylinder and an air inlet valve by a controller; the pressure acquisition module acquires the internal pressure of the reaction kettle in real time and transmits the internal pressure of the reaction kettle to the controller;
when the internal pressure of the reaction kettle is lower than a pressure set value, generating a pressurizing signal; the pressure regulator is used for controlling the opening of the air inlet valve to regulate the internal pressure of the reaction kettle;
the pressure regulator is used for carrying out pressure regulation index YZ analysis by combining the internal pressure of the reaction kettle and the ammonolysis related parameters so as to obtain the optimal inlet flow Lt of the reaction kettle through analysis;
the pressure regulator is used for adaptively regulating the valve opening of the air inlet valve according to the optimal air inlet flow Lt; when the internal pressure of the reaction kettle reaches a pressure set value MS or is in a pressure correction range, the pressure regulator controls the air inlet valve to be closed, and generates a pressure standard signal to the controller.
Further, the specific analysis process of the temperature regulator is as follows:
acquiring an external environment temperature and marking the external environment temperature as TW; comparing the internal temperature TN of the reaction kettle with a reaction temperature range (W2-W3); if TN is lower than the reaction temperature range (W2-W3), the temperature adjustment index WZ is calculated as follows: WZ=b1× (W2-TN) ×W3/W2+b2× (TS-TN) ×W2/TW; wherein b1 and b2 are preset coefficient factors;
if TN is within the reaction temperature range (W2-W3), a temperature adjustment index WZ is calculated using the formula WZ=b2× (TS-TN) ×W2/TW;
setting valve opening thresholds of a plurality of heat conducting oil valves, wherein each valve opening threshold corresponds to a preset temperature regulation index range; matching the temperature adjustment index WZ with all preset temperature adjustment index ranges to obtain corresponding valve opening thresholds and marking the valve opening thresholds as Fm;
the temperature regulator is used for driving and controlling the opening degree of the heat conducting oil valve to reach Fm so as to heat the inside of the reaction kettle.
Further, the specific analysis process of the controller is as follows:
acquiring the internal temperature of the reaction kettle and marking as TN; marking the temperature set point as TS; marking the temperature correction coefficient as Xs; when the internal temperature TN is lower than the reaction temperature range (W2-W3) or (TS-TN)/TS is more than or equal to Xs, generating a heating signal;
and the controller receives the heating signal and then drives and controls the temperature regulator to heat the inside of the reaction kettle until the internal temperature of the reaction kettle reaches a temperature set value.
Further, the specific analysis process of the pressure regulator is as follows:
the internal pressure of the reaction kettle is obtained and marked as M1; marking the pressure set point as MS; marking the pressure correction coefficient as Mx; acquiring ammonolysis related parameters of a reaction kettle, and marking the inlet ammonia gas concentration, the liquid level height, the water temperature and the humidity as M2, M3, M4 and M5 in sequence; calculating a pressure regulation index YZ by using a formula YZ=fX [ (MS-M1) + (M5×b3) ]/(M2×b4+M3×b5+M4×b6), wherein b3, b4, b5 and b6 are all preset coefficient factors; f is a preset equalization coefficient;
determining the optimal inlet air flow of the reaction kettle as Lt according to the pressure regulation index YZ; the method comprises the following steps: a mapping relation table of a pressure regulation index range and an air inlet flow threshold value is prestored in a database;
and determining an air inlet flow threshold corresponding to the pressure regulation index YZ according to the mapping relation table, and marking the air inlet flow threshold as the optimal air inlet flow Lt.
Further, the system also comprises a parameter acquisition module; the parameter acquisition module is used for acquiring ammonolysis related parameters of the reaction kettle and transmitting the ammonolysis related parameters to the controller; the ammonia decomposition related parameters comprise ammonia gas inlet concentration, liquid level height, water temperature and humidity; wherein, the pressure correction range is MS× (1-Mx) -MS× (1+Mx).
Further, the lower end part of the reaction kettle is connected with a heat conduction oil valve, and the heat conduction oil valve is used for conducting heat to the inside of the reaction kettle; a pressure gauge and a PT100 thermocouple are arranged in the reaction kettle; the pressure gauge is used for detecting the internal pressure of the reaction kettle in real time, the PT100 thermocouple is used for detecting the internal temperature of the reaction kettle in real time, and the detected temperature information is displayed in real time through the temperature display meter.
Further, in the use process of the gas phase ammonolysis device, firstly setting the pressure and the temperature of ammonia gas needed in the reaction kettle; heating the reaction kettle to a set temperature through a heat conducting oil valve, and then adding clear water into the reaction kettle; placing a sample plate to be ammonolyzed on a sample rack, and placing the sample rack into a reaction kettle;
then opening an ammonia gas cylinder and an air inlet valve, introducing ammonia gas into the reaction kettle, and closing the air inlet valve after the pressure in the reaction kettle reaches a set pressure; then preserving heat for 1 hour to finish sample ammonolysis operation; and finally, opening an exhaust valve, discharging excessive ammonia gas, taking out an ammonolysis sample, and ending the ammonolysis of the sample.
Further, a gas phase ammonolysis control method comprises the following steps:
step one: a user sets preset parameters in an HMI interface of the system through a parameter setting module;
step two: the internal temperature of the reaction kettle is regulated by controlling the valve opening of the heat conducting oil valve through a temperature regulator; the concrete steps are as follows: the temperature regulator is used for carrying out temperature regulation index WZ analysis by combining the external environment temperature and the internal temperature TN of the reaction kettle, and determining the valve opening of the heat conduction oil valve in an auxiliary manner according to the temperature regulation index WZ;
step three: when the internal temperature of the reaction kettle reaches a temperature set value TS, the temperature regulator drives and controls the conduction oil valve to be closed, and generates a temperature standard signal to the controller; the controller is used for opening an ammonia steel bottle and an air inlet valve and guiding ammonia into the reaction kettle;
step four: the internal pressure of the reaction kettle is regulated by controlling the valve opening of the air inlet valve through a pressure regulator; when the internal pressure of the reaction kettle reaches a pressure set value MS or is in a pressure correction range, the pressure regulator controls the air inlet valve to be closed.
Compared with the prior art, the invention has the beneficial effects that:
1. the parameter setting module is used for setting preset parameters by a user; the temperature acquisition module is used for acquiring the internal temperature of the reaction kettle in real time and transmitting the internal temperature of the reaction kettle to the controller; the controller is used for comparing and analyzing the internal temperature of the reaction kettle with preset parameters, so that the temperature regulator is driven and controlled to regulate the internal temperature of the reaction kettle; when a heating signal is received, the temperature regulator is used for carrying out temperature regulation index WZ analysis by combining the external environment temperature and the internal temperature TN of the reaction kettle, and determining the valve opening of the heat conducting oil valve in an auxiliary mode according to the temperature regulation index WZ; the temperature control precision and the stability are effectively improved, the heat energy loss is reduced, and the production cost is reduced;
2. the pressure acquisition module acquires the internal pressure of the reaction kettle in real time; when the internal pressure of the reaction kettle is lower than a pressure set value, generating a pressurizing signal; the pressure regulator is used for carrying out pressure regulation index YZ analysis by combining the internal pressure of the reaction kettle and the ammonolysis related parameters so as to obtain the optimal inlet flow Lt of the reaction kettle through analysis; the pressure regulator is used for adaptively regulating the valve opening of the air inlet valve according to the optimal air inlet flow rate Lt, so that ammonia gas can enter the reaction kettle at a proper speed, the pressure control precision and stability are effectively improved, and the safety of the ammonolysis reaction is improved.
Drawings
In order to more clearly illustrate the embodiments of the invention or the technical solutions in the prior art, the drawings that are required in the embodiments or the description of the prior art will be briefly described, it being obvious that the drawings in the following description are only some embodiments of the invention, and that other drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
FIG. 1 is a system block diagram of a gas phase ammonolysis control system according to the invention.
FIG. 2 is a schematic block diagram of a gas phase ammonolysis control method according to the invention.
Detailed Description
The technical solutions of the present invention will be clearly and completely described in connection with the embodiments, and it is obvious that the described embodiments are only some embodiments of the present invention, not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
As shown in fig. 1 to 2, a gas phase ammonolysis control system is applied to a gas phase ammonolysis device and comprises a parameter setting module, a temperature acquisition module, a controller, a temperature regulator, a pressure acquisition module, a parameter acquisition module, a pressure regulator and a database;
the gas phase ammonolysis device comprises an ammonia steel cylinder, a reaction kettle and a heat conducting oil valve; the ammonia gas cylinder is connected with the reaction kettle through an air inlet pipe, and an air inlet valve is arranged on the air inlet pipe;
the lower end part of the reaction kettle is connected with a heat conduction oil valve, and the heat conduction oil valve is used for conducting heat to the inside of the reaction kettle; a pressure gauge and a PT100 thermocouple are arranged in the reaction kettle; the pressure gauge is used for detecting the internal pressure of the reaction kettle in real time, the PT100 thermocouple is used for detecting the internal temperature of the reaction kettle in real time, and the detected temperature information is displayed in real time through the temperature display meter;
the parameter setting module is used for setting preset parameters in an HMI interface of the system by a user; the preset parameters comprise a reaction temperature range (W2-W3), a temperature set value, a pressure set value, a temperature correction coefficient and a pressure correction coefficient; in the embodiment, W2-W3 is 45-100 ℃; the temperature set value is in the range of W2-W3;
the temperature acquisition module is connected with the temperature display table and is used for reading the temperature information displayed on the temperature display table and transmitting the read temperature information to the controller; the controller is used for acquiring preset parameters set by a user in the parameter setting module, and comparing and analyzing the preset parameters with the temperature information read by the temperature acquisition module so as to drive and control the temperature regulator to adjust the internal temperature of the reaction kettle;
the specific analysis process of the controller is as follows:
acquiring the internal temperature of the reaction kettle and marking as TN; marking the temperature set point as TS; marking the temperature correction coefficient as Xs; for example Xs takes a value of 1.5%;
when the internal temperature TN is lower than the reaction temperature range (W2-W3) or (TS-TN)/TS is more than or equal to Xs, generating a heating signal; the controller receives the heating signal and then drives and controls the temperature regulator to heat the inside of the reaction kettle until the temperature of the inside of the reaction kettle reaches a temperature set value;
the temperature regulator is used for controlling the valve opening of the heat conducting oil valve to regulate the internal temperature of the reaction kettle; when a heating signal is received, the temperature regulator is used for carrying out temperature regulation index WZ analysis by combining the external environment temperature and the internal temperature TN of the reaction kettle, and determining the valve opening of the heat conducting oil valve in an auxiliary manner according to the temperature regulation index WZ; the specific analysis process is as follows:
acquiring an external environment temperature and marking the external environment temperature as TW; comparing the internal temperature TN of the reaction kettle with a reaction temperature range (W2-W3); if TN is lower than the reaction temperature range (W2-W3), the temperature adjustment index WZ is calculated as follows: WZ=b1× (W2-TN) ×W3/W2+b2× (TS-TN) ×W2/TW; wherein b1 and b2 are preset coefficient factors;
if TN is within the reaction temperature range (W2-W3), a temperature adjustment index WZ is calculated using the formula WZ=b2× (TS-TN) ×W2/TW;
setting valve opening thresholds of a plurality of heat conducting oil valves, wherein each valve opening threshold corresponds to a preset temperature regulation index range; wherein the larger the temperature adjustment index is, the larger the corresponding valve opening threshold value is; matching the temperature adjustment index WZ with all preset temperature adjustment index ranges to obtain corresponding valve opening thresholds and marking the valve opening thresholds as Fm;
the temperature regulator is used for driving and controlling the opening of the heat conducting oil valve to reach Fm, so that the interior of the reaction kettle is heated, the temperature control precision and stability are effectively improved, the heat energy loss is reduced, and the production cost is reduced;
when the internal temperature of the reaction kettle reaches a temperature set value TS, the temperature regulator drives and controls the conduction oil valve to be closed, and generates a temperature standard signal to the controller;
after receiving the temperature reaching signal, the controller opens an ammonia gas cylinder and an air inlet valve to introduce ammonia gas into the reaction kettle; the pressure acquisition module is used for reading the pressure information displayed on the pressure gauge and transmitting the read pressure information to the controller;
the parameter acquisition module is used for acquiring ammonolysis related parameters of the reaction kettle and transmitting the ammonolysis related parameters to the controller; the ammonia decomposition related parameters comprise ammonia gas inlet concentration, liquid level height, water temperature, humidity and the like;
the controller is used for comparing and analyzing the received pressure information with preset parameters so as to drive and control the pressure regulator to adjust the internal pressure of the reaction kettle; when the internal pressure of the reaction kettle is lower than a pressure set value, generating a pressurizing signal; the pressure regulator is used for controlling the valve opening of the air inlet valve to regulate the internal pressure of the reaction kettle;
when receiving the pressurizing signal, the pressure regulator is used for carrying out pressure regulation index YZ analysis by combining the internal pressure of the reaction kettle and the ammonolysis related parameter so as to obtain the optimal inlet flow of the reaction kettle through analysis; the specific analysis process is as follows:
the internal pressure of the reaction kettle is obtained and marked as M1; marking the pressure set point as MS; marking the pressure correction coefficient as Mx;
acquiring ammonolysis related parameters of a reaction kettle, and marking the inlet ammonia gas concentration, the liquid level height, the water temperature and the humidity as M2, M3, M4 and M5 in sequence; calculating a pressure regulation index YZ by using a formula YZ=fX [ (MS-M1) + (M5×b3) ]/(M2×b4+M3×b5+M4×b6), wherein b3, b4, b5 and b6 are all preset coefficient factors; f is a preset equalization coefficient;
determining the optimal inlet air flow of the reaction kettle as Lt according to the pressure regulation index YZ; the method comprises the following steps:
a mapping relation table of a pressure regulation index range and an air inlet flow threshold value is prestored in a database;
according to the mapping relation table, determining an air inlet flow threshold corresponding to the pressure regulation index YZ, and marking the air inlet flow threshold as the optimal air inlet flow Lt;
the pressure regulator is used for adaptively regulating the valve opening of the air inlet valve according to the optimal air inlet flow rate Lt, so that ammonia gas can enter the reaction kettle at a proper speed, the pressure control precision and stability are effectively improved, and the safety of the ammonolysis reaction is improved;
when the internal pressure of the reaction kettle reaches a pressure set value MS or is in a pressure correction range, the pressure regulator controls the air inlet valve to be closed, and generates a pressure standard signal to the controller; wherein, the pressure correction range is MS× (1-Mx) -MS× (1+Mx); for example, mx takes a value of 2%;
in the use process of the gas phase ammonolysis device, firstly setting the pressure and the temperature of ammonia gas required in a reaction kettle; heating the reaction kettle to a set temperature through a heat conducting oil valve, and then adding clear water into the reaction kettle; placing a sample plate to be ammonolyzed on a sample rack, and placing the sample rack into a reaction kettle;
then opening an ammonia gas cylinder and an air inlet valve, introducing ammonia gas into the reaction kettle, and closing the air inlet valve after the pressure in the reaction kettle reaches a set pressure; then preserving heat for 1 hour to finish sample ammonolysis operation; finally, opening an exhaust valve, discharging excessive ammonia gas, taking out an ammonolysis sample, and ending the ammonolysis of the sample; wherein, the sample rack can be simultaneously provided with a plurality of plates of samples, and the samples can be simultaneously ammonolytically treated, so that the operation is convenient, and the subsequent purification treatment speed and quality of the synthesized oligonucleotide product are greatly improved;
a gas phase ammonolysis control method is applied to the gas phase ammonolysis control system, and comprises the following steps:
step one: a user sets preset parameters in an HMI interface of the system through a parameter setting module;
step two: the internal temperature of the reaction kettle is regulated by controlling the valve opening of the heat conducting oil valve through a temperature regulator; the concrete steps are as follows: the temperature regulator is used for carrying out temperature regulation index WZ analysis by combining the external environment temperature and the internal temperature TN of the reaction kettle, and determining the valve opening of the heat conduction oil valve in an auxiliary manner according to the temperature regulation index WZ;
step three: when the internal temperature of the reaction kettle reaches a temperature set value TS, the temperature regulator drives and controls the conduction oil valve to be closed, and generates a temperature standard signal to the controller; the controller is used for opening the ammonia steel cylinder and the air inlet valve and guiding the ammonia into the reaction kettle;
step four: the internal pressure of the reaction kettle is regulated by controlling the valve opening of the air inlet valve through a pressure regulator; when the internal pressure of the reaction kettle reaches a pressure set value MS or is in a pressure correction range, the pressure regulator controls the air inlet valve to be closed.
The above formulas are all formulas with dimensions removed and numerical values calculated, the formulas are formulas which are obtained by acquiring a large amount of data and performing software simulation to obtain the closest actual situation, and preset parameters and preset thresholds in the formulas are set by a person skilled in the art according to the actual situation or are obtained by simulating a large amount of data.
In the description of the present specification, the descriptions of the terms "one embodiment," "example," "specific example," and the like, mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the present invention. In this specification, schematic representations of the above terms do not necessarily refer to the same embodiments or examples. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.
The preferred embodiments of the invention disclosed above are intended only to assist in the explanation of the invention. The preferred embodiments are not intended to be exhaustive or to limit the invention to the precise form disclosed. Obviously, many modifications and variations are possible in light of the above teaching. The embodiments were chosen and described in order to best explain the principles of the invention and the practical application, to thereby enable others skilled in the art to best understand and utilize the invention. The invention is limited only by the claims and the full scope and equivalents thereof.
Claims (8)
1. The gas phase ammonolysis control system is applied to a gas phase ammonolysis device and is characterized by comprising a parameter setting module, a temperature acquisition module, a temperature regulator, a pressure acquisition module and a pressure regulator;
the gas phase ammonolysis device comprises an ammonia steel cylinder, a reaction kettle and a heat conducting oil valve; the ammonia gas cylinder is connected with the reaction kettle through an air inlet pipe, and an air inlet valve is arranged on the air inlet pipe;
the parameter setting module is used for setting preset parameters by a user; the preset parameters comprise a reaction temperature range (W2-W3), a temperature set value, a pressure set value, a temperature correction coefficient and a pressure correction coefficient;
the temperature acquisition module is used for acquiring the internal temperature of the reaction kettle in real time and transmitting the internal temperature of the reaction kettle to the controller; the controller is used for comparing and analyzing the internal temperature of the reaction kettle with preset parameters, so that the temperature regulator is driven and controlled to regulate the internal temperature of the reaction kettle;
when a heating signal is received, the temperature regulator is used for carrying out temperature regulation index WZ analysis by combining the external environment temperature and the internal temperature TN of the reaction kettle, and determining the valve opening of the heat conducting oil valve in an auxiliary mode according to the temperature regulation index WZ; when the internal temperature of the reaction kettle reaches a temperature set value TS, the temperature regulator drives and controls the conduction oil valve to be closed, and generates a temperature standard signal to the controller;
responding to the temperature standard reaching signal, and opening an ammonia gas cylinder and an air inlet valve by a controller; the pressure acquisition module acquires the internal pressure of the reaction kettle in real time and transmits the internal pressure of the reaction kettle to the controller;
when the internal pressure of the reaction kettle is lower than a pressure set value, generating a pressurizing signal; the pressure regulator is used for controlling the opening of the air inlet valve to regulate the internal pressure of the reaction kettle;
the pressure regulator is used for carrying out pressure regulation index YZ analysis by combining the internal pressure of the reaction kettle and the ammonolysis related parameters so as to obtain the optimal inlet flow Lt of the reaction kettle through analysis;
the pressure regulator is used for adaptively regulating the valve opening of the air inlet valve according to the optimal air inlet flow Lt; when the internal pressure of the reaction kettle reaches a pressure set value MS or is in a pressure correction range, the pressure regulator controls the air inlet valve to be closed, and generates a pressure standard signal to the controller.
2. The gas phase ammonolysis control system according to claim 1, wherein the specific analysis process of the temperature regulator is as follows:
acquiring an external environment temperature and marking the external environment temperature as TW; comparing the internal temperature TN of the reaction kettle with a reaction temperature range (W2-W3); if TN is lower than the reaction temperature range (W2-W3), the temperature adjustment index WZ is calculated as follows: WZ=b1× (W2-TN) ×W3/W2+b2× (TS-TN) ×W2/TW; wherein b1 and b2 are preset coefficient factors;
if TN is within the reaction temperature range (W2-W3), a temperature adjustment index WZ is calculated using the formula WZ=b2× (TS-TN) ×W2/TW;
setting valve opening thresholds of a plurality of heat conducting oil valves, wherein each valve opening threshold corresponds to a preset temperature regulation index range; matching the temperature adjustment index WZ with all preset temperature adjustment index ranges to obtain corresponding valve opening thresholds and marking the valve opening thresholds as Fm; the temperature regulator is used for driving and controlling the opening degree of the heat conducting oil valve to reach Fm so as to heat the inside of the reaction kettle.
3. The gas phase ammonolysis control system according to claim 2, wherein the specific analysis process of the controller is as follows:
acquiring the internal temperature of the reaction kettle and marking as TN; marking the temperature set point as TS; marking the temperature correction coefficient as Xs; when the internal temperature TN is lower than the reaction temperature range (W2-W3) or (TS-TN)/TS is more than or equal to Xs, generating a heating signal;
and the controller receives the heating signal and then drives and controls the temperature regulator to heat the inside of the reaction kettle until the internal temperature of the reaction kettle reaches a temperature set value.
4. The gas phase ammonolysis control system according to claim 1, wherein the specific analysis process of the pressure regulator is as follows:
the internal pressure of the reaction kettle is obtained and marked as M1; marking the pressure set point as MS; marking the pressure correction coefficient as Mx; acquiring ammonolysis related parameters of a reaction kettle, and marking the inlet ammonia gas concentration, the liquid level height, the water temperature and the humidity as M2, M3, M4 and M5 in sequence; calculating a pressure regulation index YZ by using a formula YZ=fX [ (MS-M1) + (M5×b3) ]/(M2×b4+M3×b5+M4×b6), wherein b3, b4, b5 and b6 are all preset coefficient factors; f is a preset equalization coefficient;
determining the optimal inlet air flow of the reaction kettle as Lt according to the pressure regulation index YZ; the method comprises the following steps: a mapping relation table of a pressure regulation index range and an air inlet flow threshold value is prestored in a database;
and determining an air inlet flow threshold corresponding to the pressure regulation index YZ according to the mapping relation table, and marking the air inlet flow threshold as the optimal air inlet flow Lt.
5. The gas phase ammonolysis control system according to claim 4, further comprising a parameter acquisition module; the parameter acquisition module is used for acquiring ammonolysis related parameters of the reaction kettle and transmitting the ammonolysis related parameters to the controller; the ammonia decomposition related parameters comprise ammonia gas inlet concentration, liquid level height, water temperature and humidity; wherein, the pressure correction range is MS× (1-Mx) -MS× (1+Mx).
6. The gas-phase ammonolysis control system according to claim 1, wherein the lower end part of the reaction kettle is connected with a heat conduction oil valve, and the heat conduction oil valve is used for conducting heat to the inside of the reaction kettle; a pressure gauge and a PT100 thermocouple are arranged in the reaction kettle; the pressure gauge is used for detecting the internal pressure of the reaction kettle in real time, the PT100 thermocouple is used for detecting the internal temperature of the reaction kettle in real time, and the detected temperature information is displayed in real time through the temperature display meter.
7. The gas-phase ammonolysis control system according to claim 6, wherein the gas-phase ammonolysis device is characterized in that in the use process, firstly, the pressure and the temperature of ammonia gas needed in the reaction kettle are set; heating the reaction kettle to a set temperature through a heat conducting oil valve, and then adding clear water into the reaction kettle; placing a sample plate to be ammonolyzed on a sample rack, and placing the sample rack into a reaction kettle;
then opening an ammonia gas cylinder and an air inlet valve, introducing ammonia gas into the reaction kettle, and closing the air inlet valve after the pressure in the reaction kettle reaches a set pressure; then preserving heat for 1 hour to finish sample ammonolysis operation; and finally, opening an exhaust valve, discharging excessive ammonia gas, taking out an ammonolysis sample, and ending the ammonolysis of the sample.
8. A gas phase ammonolysis control method applied to the gas phase ammonolysis control system according to any one of claims 1-7, comprising the steps of:
step one: a user sets preset parameters in an HMI interface of the system through a parameter setting module;
step two: the internal temperature of the reaction kettle is regulated by controlling the valve opening of the heat conducting oil valve through a temperature regulator; the concrete steps are as follows: the temperature regulator is used for carrying out temperature regulation index WZ analysis by combining the external environment temperature and the internal temperature TN of the reaction kettle, and determining the valve opening of the heat conduction oil valve in an auxiliary manner according to the temperature regulation index WZ;
step three: when the internal temperature of the reaction kettle reaches a temperature set value TS, the temperature regulator drives and controls the conduction oil valve to be closed, and generates a temperature standard signal to the controller; the controller is used for opening an ammonia steel bottle and an air inlet valve and guiding ammonia into the reaction kettle;
step four: the internal pressure of the reaction kettle is regulated by controlling the valve opening of the air inlet valve through a pressure regulator; when the internal pressure of the reaction kettle reaches a pressure set value MS or is in a pressure correction range, the pressure regulator controls the air inlet valve to be closed.
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| CN202311060523.0A CN117032359A (en) | 2023-08-22 | 2023-08-22 | Gas phase ammonolysis control system and control method |
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| CN202311060523.0A CN117032359A (en) | 2023-08-22 | 2023-08-22 | Gas phase ammonolysis control system and control method |
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