CN110274512B - Reactor system and process for precisely controlling thermal reaction temperature - Google Patents
Reactor system and process for precisely controlling thermal reaction temperature Download PDFInfo
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- LYGJENNIWJXYER-UHFFFAOYSA-N nitromethane Chemical compound C[N+]([O-])=O LYGJENNIWJXYER-UHFFFAOYSA-N 0.000 description 4
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- WTDHULULXKLSOZ-UHFFFAOYSA-N Hydroxylamine hydrochloride Chemical compound Cl.ON WTDHULULXKLSOZ-UHFFFAOYSA-N 0.000 description 2
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- LPXPTNMVRIOKMN-UHFFFAOYSA-M sodium nitrite Chemical compound [Na+].[O-]N=O LPXPTNMVRIOKMN-UHFFFAOYSA-M 0.000 description 2
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/0006—Controlling or regulating processes
- B01J19/0013—Controlling the temperature of the process
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F28—HEAT EXCHANGE IN GENERAL
- F28F—DETAILS OF HEAT-EXCHANGE AND HEAT-TRANSFER APPARATUS, OF GENERAL APPLICATION
- F28F27/00—Control arrangements or safety devices specially adapted for heat-exchange or heat-transfer apparatus
- F28F27/02—Control arrangements or safety devices specially adapted for heat-exchange or heat-transfer apparatus for controlling the distribution of heat-exchange media between different channels
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J2219/00049—Controlling or regulating processes
- B01J2219/00051—Controlling the temperature
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J2219/00049—Controlling or regulating processes
- B01J2219/00051—Controlling the temperature
- B01J2219/00054—Controlling or regulating the heat exchange system
- B01J2219/00056—Controlling or regulating the heat exchange system involving measured parameters
- B01J2219/00058—Temperature measurement
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Abstract
The reactor system comprises a reactor (R101), wherein the reactor (R101) is a container for material reaction, a reactor jacket is arranged at the periphery of the reactor, a steam or hot water pipeline and a cold water pipeline are connected with the reactor jacket, a circulating pump is arranged on the two pipelines and the reactor jacket, the circulating pump is used for extracting hot water in the reactor jacket for mixed circulation so as to eliminate reaction hot spots in the reactor, and meanwhile, the hot water is used for mixing cold water with the hot water and then entering the reactor jacket so as to eliminate damage of heat carrier temperature mutation entering the reactor jacket to equipment. The device can rapidly and accurately control the temperature required by the reaction.
Description
Technical Field
The present invention relates generally to the field of reaction heat research, and in particular to a reactor system and process for precisely controlling the temperature of a thermal reaction.
Background
In industry, temperature is one of the most common and important operating parameters, and temperature control has very common application in chemical production, metal smelting and other fields. Particularly in exothermic chemical reaction, proper temperature is needed for reaction, for example, steam heating is generally adopted in industry, but heat is released during reaction, reaction materials are easy to raise temperature to be too large to exceed the range of reaction temperature, cooling water is needed to be introduced for cooling at the moment, sudden temperature quenching drop is harmful to equipment materials, and temperature deviation is too large, so that stable control of the reaction is not facilitated. Therefore, reactor temperature control for industrial exothermic reactions has been a difficult operation.
Disclosure of Invention
The invention aims at solving the difficult problem of accurate and stable control of the temperature of a material reaction process in the prior art, and provides a reactor system for accurately controlling the thermal reaction temperature, which is provided with a plurality of pipelines and circulating components which are communicated with the outside Zhou Gatao of a reactor, and is used for switching and introducing thermal media with different temperatures into a reactor jacket according to the reaction process, timely and accurately absorbing heat released by the reaction by controlling the flow of a cooling medium so as to maintain the reaction temperature not to be too high, and circulating the thermal media entering the reactor jacket through the circulating components so as to make the temperature of each part inside the reactor more uniform.
According to one aspect of the invention, a reactor system for precisely controlling the thermal reaction temperature comprises a reactor, wherein the reactor is a container for material reaction, a reactor jacket is arranged on the periphery of the reactor, the reactor jacket is connected with a plurality of pipelines, and the pipelines are used for changing and introducing different phase states or temperature thermal media into the reactor jacket along with the reaction process so as to precisely control the reaction temperature.
Most reactions require different temperatures at different stages, such as at the beginning of the reaction, a heating of the material to a temperature that initiates the reaction, which can be accomplished by a short-time rapid heat supply from a high temperature heat carrier; then enter the reaction and maintain the stage, in order to keep the reaction to go on under the constant temperature, transport the heat carrier flow the same as temperature that the reaction needs through the pipeline, in order to offer the uniform, steady heat to maintain; for exothermic or endothermic reactions, as the reaction proceeds, there is a sudden rise or fall in the temperature of the reaction mass, and for exothermic reactions, a lower heat carrier than the internal temperature of the reactor is required to absorb the excess heat evolved by the reaction, so that the reaction temperature remains constant; for endothermic reactions, a heat carrier that is higher than the temperature inside the reactor is required to release heat to the reactor contents. Therefore, the invention provides a reactor with a plurality of pipelines connected with the peripheral jacket of the reactor, the pipelines are used for conveying heat carriers with different temperatures into the jacket of the reactor, one heat carrier can be conveyed in the same reaction process, and a plurality of heat carriers with different temperatures can be mixed and conveyed in the reactor so as to be mixed in the reactor to meet the temperature required by the reaction, and the flow rates of the different heat carriers can be adjusted according to the temperature required by the reaction. The different phase heat carrier introduced into the reactor jacket refers to the different phase of the same heat carrier, such as hot steam, hot water and ice water mixture, and the temperature of the material in the reactor is quickly raised and the temperature of the material in the reactor is quickly lowered to the required reaction temperature by mixing the heat carrier flows with the heat carrier flows, so that the different phase and the different temperature heat carrier are selected according to the type of reaction and the temperature change characteristics of the reaction process and then are sent into the reactor jacket through one or two of a plurality of pipelines. The heat carrier mainly comprises water and oil, and because of potential safety hazards of oil steam in pipelines, heat conducting oil (high temperature, about 300 ℃) with obvious temperature, hot oil (temperature lower than heat conducting oil) and cold oil (normal temperature oil or oil lower than normal temperature) are generally adopted as heat carriers in a plurality of pipelines.
Further, the pipelines comprise a first pipeline, a second pipeline and a third pipeline, wherein the first pipeline is used for feeding a heat medium with the highest temperature into the jacket of the reactor so as to enable the temperature of materials in the reactor to reach the temperature required by the materials to start reaction in the shortest time; the second pipeline is used for feeding a heat medium with the temperature lower than that of the heat medium of the first pipeline into the reactor jacket and is used for maintaining the temperature required by the reaction; the third pipeline is used for feeding a heat medium with lower temperature into the reactor jacket so as to absorb heat released by materials in exothermic reaction and prevent the reaction temperature from being too high; the first pipeline and the second pipeline are respectively and independently connected with a reactor jacket, or the first pipeline and the second pipeline are integrated into one pipeline, and the same medium with different phases or temperatures is fed into the pipeline in different time periods of the reaction process.
The design of integrating the first pipeline and the second pipeline into one pipeline is designed for most exothermic reactions, a first high-temperature heat carrier is required to be sent into a reactor jacket through the integrated pipeline in the early stage of the reaction, so that the temperature of materials in the reactor is quickly raised to initiate the reaction, then the high-temperature heat carrier is not required to be sent into the subsequent reaction, the integrated pipeline is changed into a second high-temperature heat carrier to maintain the continuous and stable operation of the reaction, the temperature in the reactor is raised along with the exothermic reaction, and the lower-temperature heat carrier is sent into the third pipeline to be mixed with the previous second high-temperature heat carrier so as to prevent the excessive temperature, so that the materials in the reactor are reduced to a proper temperature.
Furthermore, the first pipeline and the second pipeline are integrated steam or hot water pipelines, the third pipeline is a cold water pipeline, and the reactor system further comprises a second valve, a fourth valve, a reaction temperature meter, a temperature controller, a water return pipeline, a condensate pipeline and an overflow valve; the second valve is arranged between the steam or hot water pipeline and the first inlet of the reactor jacket, and controls steam or hot water from a steam source or a hot water source to enter the reactor jacket from the first inlet of the reactor jacket through the steam or hot water pipeline; the cold water pipeline is connected with the second inlet of the reactor jacket through a fourth valve, and the fourth valve is used for controlling cold water from a cold water source to enter the reactor jacket from the second inlet of the reactor jacket through the cold water pipeline; the reaction temperature meter is used for measuring the temperature in the reactor; the temperature controller is respectively connected with the reaction temperature measuring meter and the fourth valve to control the fourth valve to be opened, the flow and closed according to the temperature in the reactor measured by the reaction temperature measuring meter, so as to realize the regulation of the reaction temperature in the reactor through the cold water feeding amount; the condensate pipeline is connected with a first outlet of the reactor jacket, and a sixth valve is arranged on the condensate pipeline; the water return pipeline is connected with a second outlet of the reactor jacket; the overflow valve is arranged on the water return pipeline and is used for preventing the pressure from being blocked and water from overflowing when water is fed into the jacket of the reactor or steam is fed into the jacket of the reactor.
The above reactor system with precisely controlled reaction temperature is suitable for exothermic reactions with reaction temperatures not greater than 100 ℃. Steam is introduced into the reactor jacket through a steam or hot water pipeline, so that the temperature of the reaction materials is quickly raised; after the lowest reaction temperature is reached, the reactants start to react, the reaction releases heat, the heat carrier in the steam or hot water pipeline replaces steam by hot water with a certain temperature until the hot water fills the jacket of the reactor, the hot water has the effects that the temperature gradient of the hot water and the steam is smaller, the material of equipment is not seriously damaged, the temperature of the hot water is close to the reaction temperature, the reaction temperature is not suddenly reduced, and the reaction can be stably carried out; when the reaction releases more heat, the hot water in the reactor jacket can not control the reaction temperature, at the moment, cooling water is needed to be introduced, the reaction temperature measuring meter at the top of the reactor transmits the measured temperature signal to the temperature controller, and the temperature controller controls the valve switch and the switching value on the cooling water of the fourth valve, so that a proper amount of cooling water enters the reactor jacket to be mixed with the hot water, and the temperature is quickly reduced to the required reaction temperature.
Still further, the reactor system for precisely controlling the reaction temperature of the present invention further comprises a water circulation pump, a third valve and a fifth valve; the water circulation pump is arranged between the fourth valve and the second inlet of the reactor jacket, cold water in the cold water pipeline circulates through the water circulation pump and then enters the reactor jacket, and the fifth valve is arranged between the water circulation pump and the second inlet of the reactor jacket and is used for controlling mixed water entering the reactor jacket from the water circulation pump; the pipeline between the second valve and the reactor jacket is communicated with a water circulating pump through a third valve, and is used for conveying the hot water passing through the second valve into the reactor jacket in two ways; one path is directly sent through a pipeline between the second valve and the inlet of the reactor jacket, and the other path is sent through a water circulation pump; and is used for pumping the hot water in the reactor jacket into the water circulation pump for circulation and then sending the hot water into the reactor jacket again so as to ensure that the temperature of the hot water in the reactor jacket is uniform.
The purpose of the water circulation pump is to uniformly mix the cold water with the hot water before entering the reactor jacket and then enter the reactor for heating, so as to avoid the problem that the cold water directly enters the reactor jacket to cause non-uniform water temperature at different positions in the heating jacket; and secondly, hot water in the reactor heating jacket is pumped into a water circulation pump for circulation, so that the problem that the temperature of water in the reactor jacket is not uniform due to the occurrence of reaction hot spots in the reactor is also avoided, in a word, the water circulation pump is used for enabling cold and hot water to be mixed in the circulation to form mixed liquid with uniform temperature and then enter the reactor jacket, and meanwhile, water in the reactor jacket is pumped out for circulation to enable the temperature to be uniform and then enter the reactor jacket, and therefore, the water temperature in the reactor jacket is always uniform, the uniformity of the reaction temperature is ensured, and the occurrence of the reaction hot spots can be prevented to protect the reactor equipment.
Still further, the above-mentioned overflow valve is provided on a water return line of about 5 meters, for example 4 to 6 meters, above the top of the reactor.
The overflow valve is always opened until the reaction is finished after the hot water starts to be conveyed, and the overflow valve is used for keeping the air flow or the water flow passage in the reactor jacket unblocked when the hot water or the cold water is conveyed into the reactor jacket so as to prevent the pressure from being blocked; and simultaneously is used for observing the height of the water level in the jacket of the reactor to prevent overflow.
Still further, the water circulation pump is a hot water type pipeline circulation pump or a hot water type centrifugal pump.
Still further, still include backwater thermoscope, hot water thermoscope, cold water thermoscope, condensate thermoscope, backwater thermoscope set up in the return water pipeline, in order to measure the temperature of backwater that circulates from the reactor jacket; the hot water thermometer is arranged on a steam or hot water pipeline to measure the temperature of hot water provided by a hot water source, and the cold water thermometer is arranged on a cold water pipeline to measure the temperature of cold water fed into the water circulation pump; the condensate thermometer is arranged on the condensate pipeline and is used for measuring the temperature of the steam after condensation during discharge. .
The temperature detector is combined with the flow at the valve to count the heat in the reaction process.
Still further, the first valve, the second valve, the third valve, the fifth valve and the sixth valve are all communication valves; the fourth valve is an adjusting control valve.
The first valve, the second valve, the third valve, the fifth valve and the sixth valve can be opened and closed only; the fourth valve is an adjusting control valve, and the opening and closing degree of the fourth valve can be adjusted to be any value between 0 and 100% under the control of the temperature controller.
The above reactor system for precisely controlling the reaction temperature comprises the following steps by a method for controlling the exothermic reaction temperature by combining steam, hot water and cooling water:
S1, before the reaction, rapidly heating to reach the minimum reaction temperature:
Adding reaction materials into a reactor, opening a second valve and a sixth valve, introducing steam into a jacket of the reactor, quickly heating the reaction materials to the minimum temperature required by the reaction, closing the sixth valve, and cutting off the steam;
and S2, maintaining a proper reaction temperature in the reaction process:
S21, exothermic reaction, wherein the temperature of raw materials in the reactor is increased, and the stable reaction temperature is realized by adopting hot water circulation: keeping the first valve and the second valve in a communication state, changing a steam pipeline into hot water, opening a third valve, communicating the hot water to an inlet of a water circulating pump, dividing the hot water into two paths, enabling one path to enter a jacket of the reactor through the second valve, and enabling the other path to enter the inlet of the water circulating pump through a fifth valve;
S22, when water overflow is observed on a first valve on a water return pipeline, closing a second valve, cutting off a hot water source, opening a fifth valve, starting a water circulation pump, and circulating hot water in a jacket of the reactor to enable the reaction temperature to be in a proper temperature range;
And S23, keeping the first valve in a communication state, when the reaction exotherm is large, and the reaction temperature measured by the reaction temperature measuring meter exceeds the highest proper temperature, transmitting a measured temperature signal to the temperature controller by the reaction temperature measuring meter, controlling the fourth valve to be opened to a proper opening degree, enabling cooling water to enter the circulating pump, mixing with hot water therein, and then entering the reactor jacket, and when the temperature measured by the reaction temperature measuring meter is lower than the lowest reaction temperature, closing the fourth valve, thereby realizing stable control of the reaction temperature.
The invention also provides a reactor system for accurately controlling the thermal reaction temperature by taking oil as a heat carrier, wherein the first pipeline and the second pipeline are integrated heat conduction oil or medium temperature oil pipelines, the third pipeline is a cold oil pipeline, and the reactor system further comprises an oil circulating pump, a second valve, a third valve, a fourth valve, a fifth valve, a reaction temperature meter, a temperature controller, an oil return pipeline, an overflow valve, an oil return temperature meter and a hot oil temperature meter; the second valve is arranged between the heat conduction oil or medium temperature oil pipeline and the reactor jacket, and the heat conduction oil or medium temperature oil of the heat conduction oil source or medium temperature oil source is controlled to enter the reactor jacket through the first inlet of the reactor jacket by the heat conduction oil or medium temperature oil pipeline; the cold oil pipeline, the fourth valve, the circulating pump, the fifth valve and the reactor jacket are sequentially connected, the fourth valve is used for controlling cold oil of a cold oil source to enter the circulating pump through the cold oil pipeline, and the fifth valve is used for controlling oil in the circulating pump to enter the reactor jacket through a second inlet of the reactor jacket; the pipeline between the second valve and the reactor jacket is communicated with the circulating pump through a third valve, and the pipeline is used for conveying the medium-temperature oil passing through the second valve into the reactor jacket in two ways: one path is directly sent through a pipeline between the second valve and the inlet of the reactor jacket, and the other path is sent through a circulating pump; the medium-temperature oil in the reactor jacket is pumped into the circulating pump for circulation and then is sent into the reactor jacket again, so that the temperature of the hot oil in the reactor jacket is uniform; the reaction temperature meter is used for measuring the temperature in the reactor; the temperature controller is respectively connected with the reaction temperature measuring meter and the fourth valve to control the fourth valve to be opened, the flow and closed according to the temperature measured by the reaction temperature measuring meter, so as to realize the regulation of the reaction temperature in the reactor through the cold oil inlet; the oil return pipeline is connected with a second outlet of the reactor jacket; the overflow valve is arranged on the oil return pipeline and is used for preventing pressure build-up and overflow during oil inlet in the reactor jacket; the overflow valve is arranged on a water return pipeline which is about 5 meters, for example 4 to 6 meters, above the top of the reactor; the oil return temperature measuring meter is arranged on the oil return pipeline to measure the temperature of the oil return circulated from the reactor jacket; the thermal oil thermometer is arranged on the thermal oil or medium-temperature oil pipeline to measure the temperature of the thermal oil provided by the thermal oil source or the thermal oil source; the first valve, the second valve, the third valve and the fifth valve are all communicated valves; the fourth valve is an adjusting control valve.
According to another aspect of the present invention, there is provided a process for controlling the reaction temperature by combining steam, hot water and cooling water, wherein the steam, hot water and/or cold water are switched to the outside Zhou Gatao of the reactor as the reaction progresses, so as to rapidly raise the temperature of the materials in the reactor to the reaction temperature and always control the temperature within the range required for the reaction.
Further, the process of controlling the reaction temperature by combining steam, hot water and cooling water is realized by a reactor system for precisely controlling the thermal reaction temperature, which comprises a reactor (R101), a steam or hot water pipeline, a cold water pipeline, a water circulation pump (P101), an overflow valve (V1), a second valve (V2), a third valve (V3), a fourth valve (V4), a fifth valve (V5), a sixth valve (V6), a reaction temperature meter (T3), a temperature controller (TC 01), a return water pipeline, a condensate pipeline, a return water thermometer (T1), a hot water thermometer (T2), a cold water thermometer (T4) and a condensate thermometer (T5); the reactor (R101) is a container for material reaction, and a reactor jacket is arranged on the periphery of the reactor and is used for loading a heat medium; the steam or hot water pipeline is used for conveying steam or hot water into the reactor jacket, and the cold water pipeline is used for conveying cold water into the reactor jacket; the second valve (V2) is arranged between the steam or hot water pipeline and the first inlet of the jacket of the reactor (R101) and controls steam or hot water from a steam source or a hot water source to enter the jacket of the reactor (R101) from the first inlet of the jacket of the reactor (R101) through the steam or hot water pipeline; the cold water pipeline, the fourth valve (V4), the water circulating pump (P101), the fifth valve (V5) and the second inlet of the jacket of the reactor (R101) are sequentially connected, cold water from a cold water source enters the water circulating pump ((P101) after circulating through the fourth valve (V4) and enters the jacket of the reactor (R101) from the second inlet of the jacket of the reactor (R101) through the fifth valve (V5), a pipeline between the second valve (V2) and the jacket of the reactor (R101) is communicated with the water circulating pump (P101) through the third valve (V3), hot water passing through the second valve (V2) is fed into the jacket of the reactor (R101) in two paths, one path is directly fed through the pipeline between the second valve (V2) and the jacket inlet of the reactor (R101), the other path is fed through the water circulating pump (P101), hot water in the jacket of the reactor (R101) is pumped into the water circulating pump (P101) through the cold water pipeline, and then is fed into the reactor (R101) again after being mixed and circulated through the cold water pipeline, the temperature measuring device (T101) is controlled by the temperature measuring valve (T101) to avoid the temperature of the reactor (R101) from being damaged by the temperature measuring equipment (T101) and the temperature of the temperature measuring device (T101) which is not obviously connected with the temperature measuring device (T101) of the temperature (T101) of the reactor (T) in the reactor (R101) respectively, the opening, flow and closing of the fourth valve (V4) are controlled according to the temperature in the reactor (R101) measured by the reaction temperature meter (T3), so that the reaction temperature in the reactor (R101) is regulated by the cold water inlet; the condensate pipeline is connected with a first outlet of a jacket of the reactor (R101), and a sixth valve (V6) is arranged on the condensate pipeline; the water return pipeline is connected with a second outlet of the jacket of the reactor (R101); the overflow valve (V1) is arranged on the water return pipeline and is used for preventing pressure holding or water overflow when water is fed into the jacket of the reactor (R101); the backwater thermometer (T1) is arranged on the backwater pipeline to measure the temperature of backwater circulated from the jacket of the reactor (R101); the hot water thermometer (T2) is arranged on a steam or hot water pipeline to measure the temperature of hot water provided by a hot water source, and the cold water thermometer (T4) is arranged on a cold water pipeline to measure the temperature of cold water fed into the water circulating pump (P101); the condensate thermometer (T5) is arranged on the condensate pipeline and is used for measuring the temperature of the steam after condensation during discharge.
Further, the process for controlling the reaction temperature by combining steam, hot water and cooling water comprises the following steps: s1, before the reaction, rapidly heating to reach the minimum reaction temperature: adding reaction materials into a reactor (R101), opening a second valve (V2) and a sixth valve (V6), leading steam or hot water into the reactor jacket through a first inlet of the reactor jacket by a steam or hot water pipeline, quickly heating the reaction materials to the minimum temperature required by the reaction, closing the sixth valve (V6), and cutting off the steam supply of the steam source to the steam or hot water pipeline; and S2, maintaining a proper reaction temperature in the reaction process: s21, enabling the first valve (V1) and the second valve (V2) to be in a communication state, changing a steam or hot water pipeline into a hot water source, opening the third valve (V3), enabling hot water to directly enter the reactor jacket through a first inlet of the reactor jacket, and enabling the hot water to enter a water circulating pump (P101) through the third valve (V3); s22, when water overflow is observed on a first valve (V1) on a water return pipeline, a second valve (V2) is closed, the supply of a hot water source to a steam or hot water pipeline is cut off, a fifth valve (V5) is opened, a water circulation pump (P101) is started, hot water in a jacket of the reactor enters the circulation pump (P101) for circulation, so that the reaction temperature of each part in the reactor is uniform, and reaction hot spots are avoided; s23, keeping the first valve (V1) in a communication state, when the exothermic amount of the reaction process is large, and the reaction temperature measured by the reaction temperature measuring meter (T3) exceeds the highest proper temperature, transmitting a measured temperature signal to the temperature controller (TC 01) by the reaction temperature measuring meter (T3), controlling the fourth valve (V4) to be opened to a proper opening degree by the temperature controller (TC 01), enabling cold water to enter the circulating pump (P101), mixing with hot water of the circulating pump (P101), enabling the mixed cold water to enter the reactor jacket through a second inlet of the reactor jacket, and enabling the fourth valve (V4) to be closed when the temperature measured by the reaction temperature measuring meter (T3) is lower than the lowest reaction temperature, so that the reaction temperature is stably controlled in the reaction process.
Further, the process for controlling the reaction temperature by combining steam, hot water and cooling water is characterized in that the minimum temperature in step S1 and the suitable temperature in step S2 are not higher than 100 ℃.
Further, the process for controlling the reaction temperature by combining steam, hot water and cooling water is characterized in that the temperature of hot water fed into the reactor jacket through a steam or hot water line in the step S2 is not higher than 10 ℃ than the lowest temperature in the reaction step S1.
Further, the process for controlling the reaction temperature by combining steam, hot water and cooling water is characterized by further comprising the following steps: measuring the temperature of backwater circulated from the jacket of the reactor (R101) in a backwater pipeline by a backwater thermometer (T1); measuring the temperature of hot water provided by a hot water source on a steam or hot water pipeline through a hot water thermometer (T2); measuring the temperature of cold water fed into a water circulation pump (P101) in a cold water pipeline by a cold water thermometer (T4); and measuring the temperature of the condensate pipeline after steam is condensed during discharging by a condensate thermometer (T5), and carrying out heat statistics in the reaction process by combining the flow of the corresponding valve.
Further, the process for controlling the reaction temperature by combining steam, hot water and cooling water is characterized in that the steam in the step S1 or the steam introduced into the hot water pipeline is low-pressure steam, and the pressure is 0.3MPa.
It can be seen that the present invention has the following advantages over the prior art:
1) The reactor system can switch the heat carrier entering the reactor jacket in real time according to the temperature required by specific reaction, so that the materials in the reactor can quickly and accurately reach the required temperature, and the conditions that the temperature is too high, too low and the like and cannot be controlled can not occur;
2) The reactor system can circulate by extracting the hot water in the reactor jacket in real time, and circularly mix the cold water with the hot water before the cold water is sent into the reactor jacket, so that the temperature uniformity of each part in the reactor is ensured, the reaction hot spot is timely discharged, and meanwhile, the damage of temperature mutation to equipment is eliminated.
Drawings
These and/or other aspects and advantages of the present invention will become more apparent and more readily appreciated from the following detailed description of the embodiments of the invention, taken in conjunction with the accompanying drawings, wherein:
FIG. 1 is a schematic diagram of a reactor system for precisely controlling a thermal reaction temperature by combining steam, cooling water and hot water according to an embodiment of the present invention;
Wherein: r101-reactor, P101-water circulating pump, T1-backwater temperature meter, T2-hot water temperature meter, T3-reaction temperature meter, T4-cold water temperature meter, T5-condensate temperature meter, V1-first valve, V2-second valve, V3-third valve, V4-fourth valve, V5-fifth valve, V6-sixth valve, TC 01-temperature controller.
Detailed Description
The present invention will be described in further detail below with reference to the drawings and detailed description for the purpose of enabling those skilled in the art to understand the invention better.
Example 1
The reactor system for precisely controlling exothermic reaction temperature has the structure shown in figure 1, and comprises a reactor R101, a steam or hot water pipeline, a cold water pipeline, an overflow valve V1, a second valve V2, a third valve V3, a fourth valve V4, a fifth valve V5, a water circulation pump P101, a reaction temperature meter T3, a temperature controller TC01, a water return pipeline, a condensate pipeline, a cold water thermometer T4 and a condensate thermometer T5; the reactor R101 is a container for material reaction, and a reactor jacket is arranged on the periphery of the reactor R101; the second valve V2 is arranged between the steam or hot water pipeline and the first inlet of the jacket of the reactor R101, and controls steam or hot water from a steam source or a hot water source to enter the jacket of the reactor R101 from the first inlet of the jacket of the reactor R101 through the steam or hot water pipeline; the cold water pipeline, the fourth valve V4, the water circulating pump P101, the fifth valve V5 and the second inlet of the jacket of the reactor R101 are sequentially connected, so that cold water with the flow controlled by the fourth valve V4 in the cold water pipeline firstly enters the water circulating pump P101 for circulation and then enters the jacket of the reactor R101, and the fifth valve V5 is arranged between the water circulating pump P101 and the second inlet of the jacket of the reactor R101 and is used for controlling mixed water entering the jacket of the reactor R101 from the water circulating pump P101; the pipeline between the second valve V2 and the jacket of the reactor R101 is communicated with the water circulating pump P101 through the third valve V3, and is used for sending the hot water passing through the second valve V2 into the jacket of the reactor R101 in two ways; one path is directly sent through a pipeline between a second valve V2 and a jacket inlet of the reactor R101, and the other path is sent through a water circulating pump P101; the hot water in the jacket of the reactor R101 is pumped into the water circulation pump P101 for circulation and then is sent into the jacket of the reactor R101 again, so that the temperature of the hot water in the jacket of the reactor R101 is uniform; the reaction temperature meter T3 is used for measuring the temperature in the reactor R101; the temperature controller TC01 is respectively connected with the reaction temperature meter T3 and the fourth valve V4, so as to control the opening, the opening degree and the closing degree of the fourth valve V4 according to the temperature in the reactor R101 measured by the reaction temperature meter T3, and realize the adjustment of the reaction temperature in the reactor R101 through the cold water inlet; the condensate pipeline is connected with a first outlet of a jacket of the reactor R101, and a sixth valve V6 is arranged on the condensate pipeline; the water return pipeline is connected with a second outlet of the jacket of the reactor R101; the overflow valve V1 is arranged on the water return pipeline and is used for preventing pressure building and water overflow when water is fed into the jacket of the reactor R101 or steam is fed into the jacket;
Preferably, the overflow valve V1 is provided on a water return line which is located 5 meters, for example 4 to 6 meters, above the top of the reactor R101; the water circulating pump P101 is a hot water type pipeline circulating pump or a hot water type centrifugal pump; the first valve V1, the second valve V2, the third valve V3, the fifth valve V5 and the sixth valve V6 are all communicated valves; the fourth valve V4 is an adjusting control valve
The embodiment also preferably comprises a backwater thermometer T1 and a hot water thermometer T2, wherein the backwater thermometer T1 is arranged on a backwater pipeline to measure the temperature of backwater circulated from the jacket of the reactor R101; the hot water thermometer T2 is arranged on the steam or hot water pipeline to measure the temperature of hot water provided by the hot water source. The cold water thermometer T4 is arranged on the cold water pipeline and is used for measuring the temperature of cold water fed into the water circulation pump; the condensate thermometer T5 is arranged on the condensate pipeline and is used for measuring the temperature of the steam after condensation during discharge. The above temperature measurements are used in conjunction with valve flow for thermal statistics and calculations during the reaction.
Example 2
A method for controlling the reaction temperature in nitromethane synthesis by combining steam, cooling water and hot water, which uses the apparatus of example 1, comprising the steps of: heating sodium carbonate and sodium nitrite into a reactor R101 according to a reaction ratio, starting stirring, continuously introducing 0.3MPa low-pressure steam into a jacket of the reactor R101 through a steam or hot water pipeline, rapidly heating raw materials in the reactor R101 to 90 ℃, starting dropwise adding dimethyl sulfate into the reactor R101, reacting to release heat, cutting off a steam inlet, replacing steam in the steam or hot water pipeline with hot water at 90 ℃, opening a jacket circulation flow, and starting a circulation pump P101 to circulate hot water. When the reaction temperature rises above 95 ℃ due to the heat release of the reaction, 25 ℃ cooling water is connected in a cold water pipeline, and the opening and closing degree of a V4 valve on the cold water pipeline is controlled to control the cooling water inlet through the temperature obtained by a reaction temperature measuring element T3 on a reactor R101 and a temperature controller TC01 connected with the reaction temperature measuring element T3; when the reaction temperature measured by the reaction temperature measuring element T3 is lower than 89 ℃, the temperature controller TC01 controls the fourth valve V4 of the cold water inlet valve to be closed, so that the reaction temperature can be basically ensured to be between 90 and 95 ℃, and the stable control of the temperature of the nitromethane synthesis reaction is realized.
Example 3
A method for controlling the temperature of hydroxylamine hydrochloride synthesis reaction by combining steam, cooling water and hot water, which uses the device in example 1, comprises the following specific operation steps: nitromethane and 36.5% hydrochloric acid are heated into a reactor R101 according to a reaction proportion, mechanical stirring is started, 0.3MPa low-pressure steam is continuously introduced into a jacket of the reactor R101 through a steam or hot water pipeline, and raw materials in the reactor R101 are rapidly heated to 50 ℃. The reaction heat release amount is large, the steam inlet is cut off, the steam or the steam in the hot water pipeline is replaced by hot water at 50 ℃, the jacket circulation flow is opened, and the circulating pump P101 is started to circulate the hot water. When the reaction temperature is higher than 55 ℃, 25 ℃ cooling water is connected in a cold water pipeline and enters a jacket of the reactor after circulating with hot water by a circulating pump P101, and the water circulation and cold water supplement in the jacket ensure that the temperature in the reactor is uniform, the reaction temperature is basically ensured to be 50-55 ℃, and the stable control of the temperature of nitromethane synthesis reaction is realized.
The foregoing description of embodiments of the invention has been presented for purposes of illustration and description, and is not intended to be exhaustive or limited to the embodiments disclosed. Many modifications and variations will be apparent to those of ordinary skill in the art without departing from the scope and spirit of the various embodiments described. Therefore, the protection scope of the present invention should be subject to the protection scope of the claims.
Claims (11)
1. A reactor system for precisely controlling the thermal reaction temperature is characterized by comprising a reactor (R101), wherein the reactor (R101) is a container for material reaction, a reactor jacket is arranged on the periphery of the reactor, the reactor jacket is connected with a plurality of pipelines, the pipelines are used for changing and introducing different phase states or temperature heat mediums into the reactor jacket along with the reaction progress so as to precisely control the reaction temperature,
The pipeline comprises a first pipeline, a second pipeline and a third pipeline, wherein the first pipeline is used for feeding a heat medium with the highest temperature into a jacket of the reactor so as to enable the temperature of materials in the reactor (R101) to reach the temperature required by the materials to start reaction in the shortest time; the second pipeline is used for feeding a heat medium with the temperature lower than that of the heat medium of the first pipeline into the reactor jacket and is used for maintaining the temperature required by the reaction; the third pipeline is used for feeding a heat medium with lower temperature into the reactor jacket so as to absorb heat released by materials in exothermic reaction and prevent the reaction temperature from being too high; the first pipeline and the second pipeline are respectively and independently connected with the reactor jacket, or the first pipeline and the second pipeline are integrated into one pipeline, the same medium with different phase states or temperatures is fed into the pipeline in different time periods of the reaction process,
The first pipeline and the second pipeline are integrated steam or hot water pipelines, the third pipeline is a cold water pipeline,
The reactor system also comprises a second valve (V2), a fourth valve (V4), a reaction temperature meter (T3), a temperature controller (TC 01), a water return pipeline, a condensate pipeline and an overflow valve (V1);
The second valve (V2) is arranged between the steam or hot water pipeline and the first inlet of the reactor jacket, and controls steam or hot water from a steam source or a hot water source to enter the reactor jacket from the first inlet of the reactor jacket through the steam or hot water pipeline;
the cold water pipeline is connected with the second inlet of the reactor jacket through a fourth valve (V4), and the fourth valve (V4) is used for controlling cold water from a cold water source to enter the reactor jacket from the second inlet of the reactor jacket through the cold water pipeline;
The reaction temperature meter (T3) is used for measuring the temperature inside the reactor (R101);
The temperature controller (TC 01) is respectively connected with the reaction temperature meter (T3) and the fourth valve (V4) to control the fourth valve (V4) to be opened, flow and closed according to the temperature in the reactor (R101) measured by the reaction temperature meter (T3) so as to realize the regulation of the reaction temperature in the reactor (R101) through the cold water inlet;
The condensate pipeline is connected with a first outlet of the reactor jacket, and a sixth valve (V6) is arranged on the condensate pipeline; the water return pipeline is connected with a second outlet of the reactor jacket; an overflow valve (V1) is arranged on the water return pipeline and is used for preventing the pressure from being blocked and the water from overflowing when water is fed into the jacket of the reactor or steam is fed into the jacket of the reactor,
The device is characterized by further comprising a water circulating pump (P101), a third valve (V3) and a fifth valve (V5);
The water circulation pump (P101) is arranged between the fourth valve (V4) and the second inlet of the reactor jacket, cold water in the cold water pipeline circulates through the water circulation pump (P101) before entering the reactor jacket, and the fifth valve (V5) is arranged between the water circulation pump (P101) and the second inlet of the reactor jacket and is used for controlling mixed water entering the reactor jacket from the water circulation pump (P101);
The pipeline between the second valve (V2) and the reactor jacket is communicated with a water circulating pump (P101) through a third valve (V3) and is used for sending hot water passing through the second valve (V2) into the reactor jacket in two ways; one path is directly fed through a pipeline between a second valve (V2) and a jacket inlet of the reactor, and the other path is fed through a water circulating pump (P101); and is used for pumping the hot water in the reactor jacket to a water circulation pump (P101) for circulation and then sending the hot water into the reactor jacket again so as to ensure that the temperature of the hot water in the reactor jacket is uniform,
The overflow valve (V1) is arranged on a water return pipeline which is 4 to 6 meters higher than the top of the reactor (R101),
The reactor system also comprises a backwater thermometer (T1), a hot water thermometer (T2), a cold water thermometer (T4) and a condensate thermometer (T5).
2. The reactor system for precisely controlling a thermal reaction temperature according to claim 1, wherein the water circulation pump (P101) is a hot water type pipe circulation pump or a hot water type centrifugal pump.
3. A reactor system for precisely controlling the temperature of a thermal reaction according to claim 1, characterized in that said return water thermometer (T1) is provided on the return water line to measure the temperature of the return water circulated from the reactor jacket; the hot water thermometer (T2) is arranged on a steam or hot water pipeline to measure the temperature of hot water provided by a hot water source, and the cold water thermometer (T4) is arranged on a cold water pipeline to measure the temperature of cold water fed into the water circulating pump (P101); the condensate thermometer (T5) is arranged on the condensate pipeline and is used for measuring the temperature of the steam after condensation during discharge.
4. The reactor system for precisely controlling the temperature of a thermal reaction according to claim 1, wherein the overflow valve (V1), the second valve (V2), the third valve (V3), the fifth valve (V5) and the sixth valve (V6) are all communication valves; the fourth valve (V4) is an adjusting control valve.
5. A reactor system for precisely controlling the thermal reaction temperature is characterized by comprising a reactor (R101), wherein the reactor (R101) is a container for material reaction, a reactor jacket is arranged on the periphery of the reactor, the reactor jacket is connected with a plurality of pipelines, the pipelines are used for changing and introducing different phase states or temperature heat mediums into the reactor jacket along with the reaction progress so as to precisely control the reaction temperature,
The pipeline comprises a first pipeline, a second pipeline and a third pipeline, wherein the first pipeline is used for feeding a heat medium with the highest temperature into a jacket of the reactor so as to enable the temperature of materials in the reactor (R101) to reach the temperature required by the materials to start reaction in the shortest time; the second pipeline is used for feeding a heat medium with the temperature lower than that of the heat medium of the first pipeline into the reactor jacket and is used for maintaining the temperature required by the reaction; the third pipeline is used for feeding a heat medium with lower temperature into the reactor jacket so as to absorb heat released by materials in exothermic reaction and prevent the reaction temperature from being too high; the first pipeline and the second pipeline are respectively and independently connected with the reactor jacket, or the first pipeline and the second pipeline are integrated into one pipeline, the same medium with different phase states or temperatures is fed into the pipeline in different time periods of the reaction process,
The first pipeline and the second pipeline are integrated heat conduction oil or medium temperature oil pipelines, the third pipeline is a cold oil pipeline,
The reactor system also comprises an oil circulating pump, a second valve, a third valve, a fourth valve, a fifth valve, a reaction temperature meter, a temperature controller, an oil return pipeline, an overflow valve, an oil return thermometer and a hot oil thermometer;
The second valve is arranged between the heat conduction oil or medium temperature oil pipeline and the first inlet of the reactor jacket, and controls the heat conduction oil or medium temperature oil from the heat conduction oil source or the medium temperature oil source to enter the reactor jacket through the first inlet of the reactor jacket through the heat conduction oil or the medium temperature oil pipeline;
the cold oil pipeline, the fourth valve, the circulating pump, the fifth valve and the reactor jacket are sequentially connected, the fourth valve is used for controlling cold oil of a cold oil source to enter the circulating pump through the cold oil pipeline, and the fifth valve is used for controlling oil in the circulating pump to enter the reactor jacket through a second inlet of the reactor jacket;
The pipeline between the second valve and the reactor jacket is communicated with the circulating pump through a third valve, and the pipeline is used for conveying the medium-temperature oil passing through the second valve into the reactor jacket in two ways: one path is directly sent through a pipeline between the second valve and the inlet of the reactor jacket, and the other path is sent through a circulating pump; the medium-temperature oil in the reactor jacket is pumped into the circulating pump for circulation and then is sent into the reactor jacket again, so that the temperature of the hot oil in the reactor jacket is uniform;
The reaction temperature meter is used for measuring the temperature in the reactor;
the temperature controller is respectively connected with the reaction temperature measuring meter and the fourth valve to control the fourth valve to be opened, the flow and closed according to the temperature measured by the reaction temperature measuring meter, so as to realize the regulation of the reaction temperature in the reactor through the cold oil inlet;
the oil return pipeline is connected with a second outlet of the reactor jacket; the overflow valve is arranged on the oil return pipeline and is used for preventing pressure build-up and overflow during oil inlet in the reactor jacket; the overflow valve is arranged on a water return pipeline which is 4 to 6 meters higher than the top of the reactor;
The oil return temperature measuring meter is arranged on the oil return pipeline to measure the temperature of the oil return circulated from the reactor jacket; the thermal oil thermometer is arranged on the thermal oil or medium-temperature oil pipeline to measure the temperature of the thermal oil provided by the thermal oil source or the thermal oil source; the overflow valve, the second valve, the third valve and the fifth valve are all communicated valves; the fourth valve is an adjusting control valve.
6. A process for the combined control of the reaction temperature from steam, hot water and cooling water by means of a reactor system according to any one of claims 1 to 4, characterized in that the steam, hot water and/or cold water is switched over outside the reactor Zhou Gatao as the reaction progresses, so that the temperature of the material in the reactor is rapidly raised to the reaction temperature and is always controlled within the desired range for the reaction.
7. The process for controlling the reaction temperature by combining steam, hot water and cooling water according to claim 6, comprising the steps of:
S1, before the reaction, rapidly heating to reach the minimum reaction temperature:
Adding reaction materials into a reactor (R101), opening a second valve (V2) and a sixth valve (V6), leading steam or hot water into the reactor jacket through a first inlet of the reactor jacket by a steam or hot water pipeline, quickly heating the reaction materials to the minimum temperature required by the reaction, closing the sixth valve (V6), and cutting off the steam supply of the steam source to the steam or hot water pipeline;
and S2, maintaining a proper reaction temperature in the reaction process:
S21, enabling the overflow valve (V1) and the second valve (V2) to be in a communication state, changing a steam or hot water pipeline into a hot water source, opening the third valve (V3), enabling hot water to directly enter the reactor jacket through a first inlet of the reactor jacket, and enabling the hot water to enter a water circulating pump (P101) through the third valve (V3);
S22, when water overflow is observed on an overflow valve (V1) on a water return pipeline, a second valve (V2) is closed, the supply of a hot water source to a steam or hot water pipeline is cut off, a fifth valve (V5) is opened, a water circulation pump (P101) is started, hot water in a jacket of the reactor enters the circulation pump (P101) for circulation, so that the reaction temperature of each part in the reactor is uniform, and reaction hot spots are avoided;
S23, keeping the overflow valve (V1) in a communication state, when the exothermic amount of the reaction process is large, and the reaction temperature measured by the reaction temperature measuring meter (T3) exceeds the highest proper temperature, transmitting a measured temperature signal to the temperature controller (TC 01) by the reaction temperature measuring meter (T3), controlling the fourth valve (V4) to be opened to a proper opening and closing degree by the temperature controller (TC 01), enabling cold water to enter the circulating pump (P101), mixing with hot water of the circulating pump (P101), enabling the mixed water to enter the reactor jacket through a second inlet of the reactor jacket, and enabling the fourth valve (V4) to be closed when the temperature measured by the reaction temperature measuring meter (T3) is lower than the lowest reaction temperature, so that the reaction temperature is stably controlled in the reaction process.
8. The process for the combined control of reaction temperature by steam, hot water and cooling water according to claim 7, wherein the minimum temperature in step S1 and the suitable temperature in step S2 are not higher than 100 ℃.
9. The process for the combined control of reaction temperature from steam, hot water and cooling water according to claim 8, wherein the temperature of the hot water fed into the reactor jacket via the steam or hot water line in step S2 is not higher than 10 ℃ than the lowest temperature in the reaction step S1.
10. The process for the combined control of reaction temperature from steam, hot water and cooling water according to claim 7, further comprising the steps of: measuring the temperature of backwater circulated from the reactor jacket in a backwater pipeline by a backwater thermometer (T1); measuring the temperature of hot water provided by a hot water source on a steam or hot water pipeline through a hot water thermometer (T2); measuring the temperature of cold water fed into a water circulation pump (P101) in a cold water pipeline by a cold water thermometer (T4); and measuring the temperature of the condensate pipeline after steam is condensed during discharging by a condensate thermometer (T5), and carrying out heat statistics in the reaction process by combining the flow of the corresponding valve.
11. The process for controlling the reaction temperature by combining steam, hot water and cooling water according to claim 7, wherein the steam introduced into the steam or hot water line in the step S1 is low pressure steam having a pressure of 0.3MPa.
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