CN113893790B - Temperature control method of organosilicon monomer synthesis fluidized bed - Google Patents
Temperature control method of organosilicon monomer synthesis fluidized bed Download PDFInfo
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- 238000000034 method Methods 0.000 title claims abstract description 39
- 239000000178 monomer Substances 0.000 title claims abstract description 17
- 238000003786 synthesis reaction Methods 0.000 title claims abstract description 12
- 230000015572 biosynthetic process Effects 0.000 title claims abstract description 10
- 230000001105 regulatory effect Effects 0.000 claims abstract description 159
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 30
- 230000008569 process Effects 0.000 claims abstract description 9
- 230000001276 controlling effect Effects 0.000 claims description 15
- 230000002194 synthesizing effect Effects 0.000 claims description 4
- 239000003921 oil Substances 0.000 description 297
- 238000006243 chemical reaction Methods 0.000 description 10
- NEHMKBQYUWJMIP-UHFFFAOYSA-N chloromethane Chemical compound ClC NEHMKBQYUWJMIP-UHFFFAOYSA-N 0.000 description 8
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 7
- 125000004122 cyclic group Chemical group 0.000 description 7
- 238000004519 manufacturing process Methods 0.000 description 6
- YGZSVWMBUCGDCV-UHFFFAOYSA-N chloro(methyl)silane Chemical compound C[SiH2]Cl YGZSVWMBUCGDCV-UHFFFAOYSA-N 0.000 description 5
- 238000012423 maintenance Methods 0.000 description 5
- 239000006227 byproduct Substances 0.000 description 4
- 239000011863 silicon-based powder Substances 0.000 description 4
- LIKFHECYJZWXFJ-UHFFFAOYSA-N dimethyldichlorosilane Chemical compound C[Si](C)(Cl)Cl LIKFHECYJZWXFJ-UHFFFAOYSA-N 0.000 description 3
- 238000005265 energy consumption Methods 0.000 description 3
- 230000007246 mechanism Effects 0.000 description 3
- 229910052710 silicon Inorganic materials 0.000 description 3
- 239000010703 silicon Substances 0.000 description 3
- 230000008859 change Effects 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- WCCJDBZJUYKDBF-UHFFFAOYSA-N copper silicon Chemical compound [Si].[Cu] WCCJDBZJUYKDBF-UHFFFAOYSA-N 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000002427 irreversible effect Effects 0.000 description 1
- 229940050176 methyl chloride Drugs 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000007086 side reaction Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000007790 solid phase Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
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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
- B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
- B01J8/18—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with fluidised particles
- B01J8/24—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with fluidised particles according to "fluidised-bed" technique
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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
- B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
- B01J8/18—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with fluidised particles
- B01J8/1809—Controlling processes
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F7/00—Compounds containing elements of Groups 4 or 14 of the Periodic Table
- C07F7/02—Silicon compounds
- C07F7/08—Compounds having one or more C—Si linkages
- C07F7/12—Organo silicon halides
- C07F7/16—Preparation thereof from silicon and halogenated hydrocarbons direct synthesis
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Combustion & Propulsion (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Control Of Temperature (AREA)
Abstract
The invention discloses a temperature control method of an organosilicon monomer synthesis fluidized bed, which comprises the following steps: firstly, introducing high-temperature heat conduction oil discharged from a heat conduction oil outlet of a reactor into an oil discharge pipe through a heat conduction oil pump; step two: a first three-way temperature regulating valve is arranged at the outlet of the oil discharge pipe, and a high-temperature heat conducting oil temperature signal of an oil inlet of the first three-way temperature regulating valve and a boiler water supply temperature signal of the steam generator are connected to a control module; step three: when the control module detects that the inlet temperature of the high-temperature heat conduction oil is higher than 260-260.5 ℃ in the running process of the reactor, the control module controls the boiler water supply to reduce the temperature of the high-temperature heat conduction oil to 260-260.5 ℃ and then the high-temperature heat conduction oil is introduced into the heat conduction oil inlet; when the control module detects that the inlet temperature of the high-temperature heat conduction oil is equal to 260-260.5 ℃, the control module controls the high-temperature heat conduction oil to be directly introduced into the heat conduction oil inlet. The invention has the advantages of reasonable method, easy implementation and high adjustment precision.
Description
Technical Field
The invention belongs to the technical field of organosilicon production processes, and particularly relates to a temperature control method of an organosilicon monomer synthesis fluidized bed.
Background
At present, the production process of the organic silicon mostly adopts a direct method to synthesize methyl chlorosilane, namely silicon powder and methyl chloride are used as raw materials, ternary copper is used as a catalyst, and gas-solid phase catalytic reaction is carried out in a fluidized bed reactor under the conditions of the temperature of 295-300 ℃ and the pressure of 0.3MPa to generate a mixed monomer mainly containing dimethyl dichlorosilane. The fluidized bed reactor is key equipment in the silicon powder and chloromethane synthesis process, the existing fluidized bed reactor comprises a shell, an internal heat exchange tube bundle, a distribution plate, a chloromethane air inlet, a silico-copper powder inlet, a temperature measuring port, a pressure measuring port, a heat conducting oil inlet, a heat conducting oil outlet, a synthesis gas outlet and the like, when in reaction, chloromethane gas passes through a solid granular silicon powder layer to enable the silicon powder to react in a fluidized state, the reaction is exothermic, the fluidized bed reactor not only needs to be wear-resistant and high-temperature-resistant, but also can rapidly take away heat generated by the reaction in the fluidized bed, and meanwhile, the reaction temperature in the fluidized bed reactor needs to be controlled to be stable. In the prior art, the reaction temperature of the fluidized bed reactor is controlled by mainly controlling the flow of heat conduction oil entering the fluidized bed reactor to control the reaction temperature in the fluidized bed reactor, under the technology, because the temperature control of the fluidized bed reactor is related to the inlet flow of the heat conduction oil and the temperature of the heat conduction oil, in the process of controlling the temperature of the fluidized bed reactor by controlling the flow of the heat conduction oil, the temperature of the heat conduction oil, the heat transfer coefficient and the like are changed along with the change when the flow of the heat conduction oil is changed, the possibility that the temperature fluctuation of the fluidized bed is larger can exist, the maximum temperature fluctuation of the fluidized bed reactor can reach +/-8 ℃, the larger temperature fluctuation of the fluidized bed reactor can have larger influence on the synthesis reaction in the fluidized bed reactor, firstly, the irreversible damage to the combination of the silicon copper contact in the fluidized bed reactor is most likely to occur, the great influence on the mixed monomer with the dimethyl dichlorosilane as a main component, secondly, the occurrence of side reaction in the fluidized bed reactor can be caused, the more in the synthesis reaction process, the mixed monomer content of the dimethyl dichlorosilane is more, the mixed monomer content is lower than 80% of the mixed monomer is required to be more in the subsequent maintenance period of the maintenance of the system, and the maintenance of the system is required to be carried out in the following the maintenance period of the maintenance of the system. Therefore, the development of the temperature control method of the organosilicon monomer synthesis fluidized bed with reasonable method, easy implementation and high temperature regulation precision is objectively required.
Disclosure of Invention
In order to solve the problems in the background art, the invention aims to provide the temperature control method of the organosilicon monomer synthesis fluidized bed, which has the advantages of reasonable method, easy implementation and high temperature regulation precision.
The invention discloses a temperature control method of an organosilicon monomer synthesis fluidized bed, which comprises the following steps:
Step one: introducing high-temperature heat conduction oil discharged from a heat conduction oil outlet of the reactor into an oil discharge pipe through a heat conduction oil pump, wherein the flow rate of the high-temperature heat conduction oil at the heat conduction oil pump outlet is controlled to be 2000-2020 m 3/h, and the temperature of the high-temperature heat conduction oil at the heat conduction oil pump outlet is controlled to be 280-285 ℃;
Step two: the method comprises the steps that a first three-way temperature regulating valve is arranged on an outlet of an oil discharge pipe, a first oil inlet branch pipe communicated with a heat conducting oil inlet of a reactor is arranged on a first oil outlet of the first three-way temperature regulating valve, a steam generator is arranged on the first oil inlet branch pipe, a second oil inlet branch pipe communicated with the heat conducting oil inlet of the reactor is arranged on a second oil outlet of the first three-way temperature regulating valve, a high-temperature heat conducting oil temperature signal of an oil inlet of the first three-way temperature regulating valve and a boiler water supply temperature signal on the steam generator are connected to a control module, and the opening and the closing of the first oil outlet and the second oil outlet of the first three-way temperature regulating valve are controlled by the control module;
Step three: in the running process of the reactor, the temperature of the heat conduction oil entering the reactor from a heat conduction oil inlet is required to be controlled to be 260-260.5 ℃, when the control module detects that the inlet temperature of the high-temperature heat conduction oil at the oil inlet of the first three-way temperature regulating valve is higher than 260-260.5 ℃, the control module controls the first oil outlet of the first three-way temperature regulating valve to be opened, the second oil outlet is closed, the high-temperature heat conduction oil in the oil drain pipe enters the tube side of the steam generator through the first oil outlet of the first three-way temperature regulating valve, at the moment, boiler water is introduced into the shell side of the steam generator, the inlet temperature of the boiler water is 80-82 ℃, the pressure is 1.2-1.25 MPa, the temperature of the high-temperature heat conduction oil in the steam generator is reduced to be 260-260.5 ℃ by using the boiler water, and the high-temperature heat conduction oil is introduced into the heat conduction oil inlet through the first outlet of the first three-way temperature regulating valve and the first oil inlet branch pipe; when the control module detects that the inlet temperature of the high-temperature heat conduction oil at the oil inlet of the first three-way temperature regulating valve is equal to 260-260.5 ℃, the control module controls the first oil outlet of the first three-way temperature regulating valve to be closed, the second oil outlet is opened, and the high-temperature heat conduction oil is led into the heat conduction oil inlet through the second oil outlet and the second oil inlet branch pipe of the first three-way temperature regulating valve.
In the third step, a second three-way temperature regulating valve is arranged on the oil outlet of the first oil inlet branch pipe, the first oil outlet of the second three-way temperature regulating valve is communicated with the heat conducting oil inlet through a first bypass pipe, the second oil outlet of the second three-way temperature regulating valve is communicated with the heat conducting oil inlet through a second bypass pipe, a condenser is arranged on the second bypass pipe, a high-temperature heat conducting oil temperature signal on the oil inlet of the second three-way temperature regulating valve and a temperature signal of a condensing medium of the condenser are also connected to a control module, when the temperature of the high-temperature heat conducting oil discharged from the steam generator and detected by the control module is equal to 260-260.5 ℃, the control module controls the first oil outlet on the second three-way temperature regulating valve to be opened, the second oil outlet is closed, and when the temperature of the high-temperature heat conduction oil discharged from the steam generator and detected by the control module is still higher than 260-260.5 ℃, the control module controls the first oil outlet on the second three-way temperature regulating valve to be closed, the second oil outlet is opened, a condensing medium is introduced into the shell side inlet of the condenser, the condensing medium in the condenser is circulating water, the inlet temperature of the circulating water is 27-28 ℃, the outlet temperature is 32-33 ℃, the high-temperature heat conduction oil in the condenser is reduced to 260-260.5 ℃ by using the condensing medium, and then the high-temperature heat conduction oil discharged from the condenser is introduced into the heat conduction oil inlet through the second bypass pipe, wherein the condensing medium in the condenser is circulating water.
The temperature regulating method is controlled by the first three-way temperature regulating valve and the steam generator, the manufacturing investment cost of the first three-way temperature regulating valve and the steam generator is low, and the inlet temperature of the high-temperature heat-conducting oil can be accurately regulated by using low-cost equipment investment. Compared with the existing temperature regulating method by flow, the invention has the following excellent effects: the invention utilizes the first three-way temperature regulating valve to regulate the control of the high-temperature heat conduction oil entering the reactor, the high-temperature heat conduction oil discharged from the reactor enters between the first three-way temperature regulating valves, the temperature of the high-temperature heat conduction oil can be monitored timely through the control module, a proper temperature regulating pipeline is selected according to the detected actual temperature of the high-temperature heat conduction oil, the high-temperature heat conduction oil is properly regulated and then is fed into the reactor, the invention utilizes the first three-way temperature regulating valve to select a mode of combining an oil inlet pipeline with boiler water supply heat exchange, temperature reduction and heat exchange, thoroughly solves the problem that the temperature, heat transfer coefficient and the like of the heat conduction oil are changed along with the change caused by the flow of the heat conduction oil, the regulated temperature of the high-temperature heat conduction oil is relatively stable, the fluctuation of the high-temperature heat conduction oil is smaller, the temperature fluctuation of the high-temperature heat conduction oil can be controlled within the range of 0.5 ℃, and the temperature regulation precision is high; the control module is introduced, the control module is utilized to realize the temperature control automation of the cyclic utilization of the high-temperature heat conduction oil, the possibility of large fluctuation of the reaction temperature in the reactor is reduced, the running stability of the reactor is greatly increased, the running period of the reactor is prolonged, the generation of byproducts is prevented, the productivity and the quality of the methylchlorosilane are effectively improved, and the method has the advantages of reasonable method, easiness in implementation and high regulation precision, and is easy to popularize and use.
Drawings
FIG. 1 is a schematic diagram of the structure of the present invention;
in the figure: the device comprises a reactor, a 2-heat conducting oil outlet, a 3-heat conducting oil pump, a 4-oil discharge pipe, a 5-first three-way temperature regulating valve, a 6-heat conducting oil inlet, a 7-first oil inlet branch pipe, an 8-steam generator, a 9-second oil inlet branch pipe, a 10-control module, a 11-second three-way temperature regulating valve, a 12-first coil pipe, a 13-second bypass pipe and a 14-condenser.
Detailed Description
The invention is further described below with reference to examples and the accompanying drawings, which are not in any way limiting, but are any changes or substitutions based on the teachings of the invention, all falling within the scope of the invention.
Example 1
The method for controlling the temperature of the fluidized bed for synthesizing the organic silicon monomer according to the embodiment 1 is characterized by comprising the following steps:
Step one: introducing high-temperature heat conduction oil discharged from a heat conduction oil outlet 2 of the reactor 1 into an oil discharge pipe 4 through a heat conduction oil pump 3, controlling the flow rate of the high-temperature heat conduction oil at the outlet of the heat conduction oil pump 3 to be 2000m 3/h, and controlling the temperature of the high-temperature heat conduction oil at the outlet of the heat conduction oil pump to be 280 ℃;
Step two: the outlet of the oil drain pipe 4 is provided with a first three-way temperature regulating valve 5, the first three-way temperature regulating valve 5 is driven by compressed air, an actuating mechanism of the first three-way temperature regulating valve 5 is provided with a position-keeping valve, an electromagnetic valve and a compressed air tank, when the first three-way temperature regulating valve 5 loses control power or compressed air, the electromagnetic valve or the position-keeping valve is automatically closed, so that the first three-way temperature regulating valve 5 keeps the current opening degree, the first three-way temperature regulating valve 5 is prevented from being out of control under the accident state of losing control power or compressed air and the like, further, the oil temperature is prevented from changing greatly, meanwhile, the first three-way temperature regulating valve 5 is provided with a hand wheel, the oil temperature can be manually regulated on site under the accident state, a first oil inlet branch pipe 7 communicated with a heat conducting oil inlet 6 of the reactor 1 is arranged on a first oil outlet of the first three-way temperature regulating valve 5, the first oil inlet branch pipe 7 is provided with a steam generator 8, the steam generator 8 preferably adopts a U-shaped tubular heat exchanger, the second oil outlet of the first three-way temperature regulating valve 5 is provided with a second oil inlet branch pipe 9 communicated with the heat conducting oil inlet 6 of the reactor 1, a high-temperature heat conducting oil temperature signal of an oil inlet of the first three-way temperature regulating valve 5 and a boiler water supply temperature signal on the steam generator 8 are connected to the control module 10, the control module 10 controls the opening and closing of the first oil outlet and the second oil outlet of the first three-way temperature regulating valve 5, the control module 10 can automatically perform function temperature regulating switching according to the actual demand temperature of a client, the automatic control of a system is facilitated, the temperature control of the high-temperature heat conducting oil is reasonably arranged in the control module 10, the temperature control of the cyclic use of the high-temperature heat conducting oil is realized, the heat of the high-temperature heat conducting oil is effectively utilized, the energy consumption is saved, and the high-precision control of the circulation temperature of the high-temperature heat conduction oil is realized;
Step three: in the running process of the reactor 1, the temperature of heat conduction oil entering the reactor 1 from a heat conduction oil inlet 6 is required to be controlled to be 260 ℃, when a control module 10 detects that the inlet temperature of high-temperature heat conduction oil at an oil inlet of a first three-way temperature regulating valve 5 is higher than 260 ℃, the control module 10 controls a first oil outlet of the first three-way temperature regulating valve 5 to be opened, a second oil outlet is closed, the high-temperature heat conduction oil in an oil drain pipe 4 enters a tube pass of a steam generator 8 through the first oil outlet of the first three-way temperature regulating valve 5, boiler feed water is introduced into a shell pass of the steam generator 8 at the moment, the inlet temperature of the boiler feed water is 80 ℃ and the pressure is 1.2MPa, and the high-temperature heat conduction oil in the steam generator 8 is reduced to be 260 ℃ by using boiler feed water, so that the high-temperature heat conduction oil is introduced into the heat conduction oil inlet 6 through a first outlet of the first three-way regulating valve 5 and a first oil inlet branch pipe 7; when the control module 10 detects that the inlet temperature of the high-temperature heat conduction oil at the oil inlet of the first three-way temperature regulating valve 5 is equal to 260 ℃, the control module 10 controls the first oil outlet of the first three-way temperature regulating valve 5 to be closed, the second oil outlet to be opened, and the high-temperature heat conduction oil is led into the heat conduction oil inlet 6 through the second oil outlet of the first three-way temperature regulating valve 5 and the second oil inlet branch pipe 9;
in order to further improve the accuracy of the high-temperature heat-conducting oil inlet temperature, in the third step, a second three-way temperature regulating valve 11 is arranged on the oil outlet of the first oil inlet branch pipe 7, the first oil outlet of the second three-way temperature regulating valve 11 is communicated with the heat-conducting oil inlet 6 through a first bypass pipe 12, the second oil outlet of the second three-way temperature regulating valve 11 is communicated with the heat-conducting oil inlet 6 through a second bypass pipe 13, a condenser 14 is arranged on the second bypass pipe 13, a high-temperature heat-conducting oil temperature signal on the oil inlet of the second three-way temperature regulating valve 11 and a temperature signal of a condensing medium of the condenser 14 are also connected to the control module 10, when the temperature of the high-temperature heat-conducting oil discharged from the steam generator 8 detected by the control module 10 is equal to 260 ℃, the control module 10 controls the first oil outlet on the second three-way temperature regulating valve 11 to be opened, the second oil outlet is closed, high-temperature heat conduction oil is led into the heat conduction oil inlet 6 through the first bypass 12 pipe, when the temperature of the high-temperature heat conduction oil discharged from the steam generator 8 detected by the control module 10 is still higher than 260 ℃, the control module 10 controls the first oil outlet on the second three-way temperature regulating valve 11 to be closed, the second oil outlet is opened, condensing medium is led into the shell side inlet of the condenser 14, the condensing medium in the condenser is circulating water, the inlet temperature of the circulating water is 27 ℃, the outlet temperature is 32 ℃, the temperature of the high-temperature heat conduction oil in the condenser 14 is reduced to 260 ℃, the high-temperature heat conduction oil discharged from the condenser 14 is led into the heat conduction oil inlet 6 through the second bypass pipe 13, and the first three-way temperature regulating valve and the second three-way temperature regulating valve 11 realize the control of two valves in a stepping control mode.
The temperature regulating method is controlled by the first three-way temperature regulating valve and the steam generator, the manufacturing investment cost of the first three-way temperature regulating valve and the steam generator is low, and the inlet temperature of the high-temperature heat-conducting oil can be accurately regulated by using low-cost equipment investment. Compared with the existing temperature regulating method by flow, the temperature regulating method of the invention can thoroughly solve the problems of temperature, heat transfer coefficient and the like of the heat conduction oil caused by the flow of the heat conduction oil, can lead the temperature of the regulated high-temperature heat conduction oil to be relatively stable, has smaller volatility, can control the temperature fluctuation of the high-temperature heat conduction oil within the range of 0.5 ℃ and has high temperature regulating precision; and secondly, the control module is utilized to realize the temperature control automation of the cyclic utilization of the high-temperature heat conduction oil, thereby improving the convenience and accuracy of temperature adjustment, reducing the possibility of large fluctuation of reaction temperature in the reactor, greatly increasing the running stability of the reactor, prolonging the running period of the reactor, preventing the generation of byproducts and effectively improving the productivity and quality of the methylchlorosilane.
Example 2
The method for controlling the temperature of the fluidized bed for synthesizing the organic silicon monomer according to the embodiment 2 is characterized by comprising the following steps:
step one: introducing high-temperature heat conduction oil discharged from a heat conduction oil outlet 2 of the reactor 1 into an oil discharge pipe 4 through a heat conduction oil pump 3, controlling the flow rate of the high-temperature heat conduction oil at the outlet of the heat conduction oil pump 3 at 2010m 3/h, and controlling the temperature of the high-temperature heat conduction oil at the outlet of the heat conduction oil pump at 283 ℃;
Step two: the outlet of the oil drain pipe 4 is provided with a first three-way temperature regulating valve 5, the first three-way temperature regulating valve 5 is driven by compressed air, an actuating mechanism of the first three-way temperature regulating valve 5 is provided with a position-keeping valve, an electromagnetic valve and a compressed air tank, when the first three-way temperature regulating valve 5 loses control power or compressed air, the electromagnetic valve or the position-keeping valve is automatically closed, so that the first three-way temperature regulating valve 5 keeps the current opening degree, the first three-way temperature regulating valve 5 is prevented from being out of control under the accident state of losing control power or compressed air and the like, further, the oil temperature is prevented from changing greatly, meanwhile, the first three-way temperature regulating valve 5 is provided with a hand wheel, the oil temperature can be manually regulated on site under the accident state, a first oil inlet branch pipe 7 communicated with a heat conducting oil inlet 6 of the reactor 1 is arranged on a first oil outlet of the first three-way temperature regulating valve 5, the first oil inlet branch pipe 7 is provided with a steam generator 8, the steam generator 8 preferably adopts a U-shaped tubular heat exchanger, the second oil outlet of the first three-way temperature regulating valve 5 is provided with a second oil inlet branch pipe 9 communicated with the heat conducting oil inlet 6 of the reactor 1, a high-temperature heat conducting oil temperature signal of an oil inlet of the first three-way temperature regulating valve 5 and a boiler water supply temperature signal on the steam generator 8 are connected to the control module 10, the control module 10 controls the opening and closing of the first oil outlet and the second oil outlet of the first three-way temperature regulating valve 5, the control module 10 can automatically perform function temperature regulating switching according to the actual demand temperature of a client, the automatic control of a system is facilitated, the temperature control of the high-temperature heat conducting oil is reasonably arranged in the control module 10, the temperature control of the cyclic use of the high-temperature heat conducting oil is realized, the heat of the high-temperature heat conducting oil is effectively utilized, the energy consumption is saved, and the high-precision control of the circulation temperature of the high-temperature heat conduction oil is realized;
Step three: in the running process of the reactor 1, the temperature of heat conduction oil entering the reactor 1 from a heat conduction oil inlet 6 is required to be controlled to be 260.3 ℃, when the control module 10 detects that the inlet temperature of high-temperature heat conduction oil at an oil inlet of a first three-way temperature regulating valve 5 is higher than 260.3 ℃, the control module 10 controls a first oil outlet of the first three-way temperature regulating valve 5 to be opened, a second oil outlet is closed, the high-temperature heat conduction oil in an oil drain pipe 4 enters a tube side of a steam generator 8 through the first oil outlet of the first three-way temperature regulating valve 5, at the moment, boiler feed water is introduced into a shell side of the steam generator 8, the inlet temperature of the boiler feed water is reduced to 160.3 ℃, and the high-temperature heat conduction oil in the steam generator 8 is introduced into the heat conduction oil inlet 6 through a first outlet of the first three-way temperature regulating valve 5 and a first oil inlet branch pipe 7; when the control module 10 detects that the inlet temperature of the high-temperature heat conduction oil at the oil inlet of the first three-way temperature regulating valve 5 is equal to 260.3 ℃, the control module 10 controls the first oil outlet of the first three-way temperature regulating valve 5 to be closed, the second oil outlet to be opened, and the high-temperature heat conduction oil is led into the heat conduction oil inlet 6 through the second oil outlet of the first three-way temperature regulating valve 5 and the second oil inlet branch pipe 9;
In order to further improve the accuracy of the high-temperature heat-conducting oil inlet temperature, in the third step, a second three-way temperature regulating valve 11 is arranged on the oil outlet of the first oil inlet branch pipe 7, the first oil outlet of the second three-way temperature regulating valve 11 is communicated with the heat-conducting oil inlet 6 through a first bypass pipe 12, the second oil outlet of the second three-way temperature regulating valve 11 is communicated with the heat-conducting oil inlet 6 through a second bypass pipe 13, a condenser 14 is arranged on the second bypass pipe 13, a high-temperature heat-conducting oil temperature signal on the oil inlet of the second three-way temperature regulating valve 11 and a temperature signal of a condensing medium of the condenser 14 are also connected to the control module 10, when the temperature of the high-temperature heat-conducting oil discharged from the steam generator 8 detected by the control module 10 is equal to 260.3 ℃, the control module 10 controls the first oil outlet on the second three-way temperature regulating valve 11 to be opened, the second oil outlet is closed, when the temperature of the high-temperature heat conduction oil discharged from the steam generator 8 detected by the control module 10 is still higher than 260.3 ℃, the control module 10 controls a first oil outlet on the second three-way temperature regulating valve 11 to be closed, a second oil outlet is opened, a condensing medium is introduced into a shell side inlet of the condenser 14, the condensing medium in the condenser is circulating water, the inlet temperature of the circulating water is 27.5 ℃, the outlet temperature is 31 ℃, the temperature of the high-temperature heat conduction oil in the condenser 14 is reduced to 260.3 ℃ by utilizing the condensing medium, the high-temperature heat conduction oil discharged from the condenser 14 is introduced into the heat conduction oil inlet 6 through the second bypass pipe 13, and the first three-way temperature regulating valve and the second three-way temperature regulating valve 11 realize the control of the two valves in a branch control mode.
The temperature regulating method is controlled by the first three-way temperature regulating valve and the steam generator, the manufacturing investment cost of the first three-way temperature regulating valve and the steam generator is low, and the inlet temperature of the high-temperature heat-conducting oil can be accurately regulated by using low-cost equipment investment. Compared with the existing temperature regulating method by flow, the temperature regulating method of the invention can thoroughly solve the problems of temperature, heat transfer coefficient and the like of the heat conduction oil caused by the flow of the heat conduction oil, can lead the temperature of the regulated high-temperature heat conduction oil to be relatively stable, has smaller volatility, can control the temperature fluctuation of the high-temperature heat conduction oil within the range of 0.5 ℃ and has high temperature regulating precision; and secondly, the control module is utilized to realize the temperature control automation of the cyclic utilization of the high-temperature heat conduction oil, thereby improving the convenience and accuracy of temperature adjustment, reducing the possibility of large fluctuation of reaction temperature in the reactor, greatly increasing the running stability of the reactor, prolonging the running period of the reactor, preventing the generation of byproducts and effectively improving the productivity and quality of the methylchlorosilane.
Example 3
The method for controlling the temperature of the fluidized bed for synthesizing the organosilicon monomer according to the embodiment 3 is characterized by comprising the following steps:
Step one: introducing high-temperature heat conduction oil discharged from a heat conduction oil outlet 2 of the reactor 1 into an oil discharge pipe 4 through a heat conduction oil pump 3, controlling the flow rate of the high-temperature heat conduction oil at the outlet of the heat conduction oil pump 3 to 2020m 3/h, and controlling the temperature of the high-temperature heat conduction oil at the outlet of the heat conduction oil pump to 285 ℃;
Step two: the outlet of the oil drain pipe 4 is provided with a first three-way temperature regulating valve 5, the first three-way temperature regulating valve 5 is driven by compressed air, an actuating mechanism of the first three-way temperature regulating valve 5 is provided with a position-keeping valve, an electromagnetic valve and a compressed air tank, when the first three-way temperature regulating valve 5 loses control power or compressed air, the electromagnetic valve or the position-keeping valve is automatically closed, so that the first three-way temperature regulating valve 5 keeps the current opening degree, the first three-way temperature regulating valve 5 is prevented from being out of control under the accident state of losing control power or compressed air and the like, further, the oil temperature is prevented from changing greatly, meanwhile, the first three-way temperature regulating valve 5 is provided with a hand wheel, the oil temperature can be manually regulated on site under the accident state, a first oil inlet branch pipe 7 communicated with a heat conducting oil inlet 6 of the reactor 1 is arranged on a first oil outlet of the first three-way temperature regulating valve 5, the first oil inlet branch pipe 7 is provided with a steam generator 8, the steam generator 8 preferably adopts a U-shaped tubular heat exchanger, the second oil outlet of the first three-way temperature regulating valve 5 is provided with a second oil inlet branch pipe 9 communicated with the heat conducting oil inlet 6 of the reactor 1, a high-temperature heat conducting oil temperature signal of an oil inlet of the first three-way temperature regulating valve 5 and a boiler water supply temperature signal on the steam generator 8 are connected to the control module 10, the control module 10 controls the opening and closing of the first oil outlet and the second oil outlet of the first three-way temperature regulating valve 5, the control module 10 can automatically perform function temperature regulating switching according to the actual demand temperature of a client, the automatic control of a system is facilitated, the temperature control of the high-temperature heat conducting oil is reasonably arranged in the control module 10, the temperature control of the cyclic use of the high-temperature heat conducting oil is realized, the heat of the high-temperature heat conducting oil is effectively utilized, the energy consumption is saved, and the high-precision control of the circulation temperature of the high-temperature heat conduction oil is realized;
Step three: in the running process of the reactor 1, the temperature of heat conduction oil entering the reactor 1 from the heat conduction oil inlet 6 is required to be controlled to be 260.5 ℃, when the control module 10 detects that the inlet temperature of high-temperature heat conduction oil at the oil inlet of the first three-way temperature regulating valve 5 is higher than 260.5 ℃, the control module 10 controls the first oil outlet of the first three-way temperature regulating valve 5 to be opened, the second oil outlet is closed, the high-temperature heat conduction oil in the oil drain pipe 4 enters the tube side of the steam generator 8 through the first oil outlet of the first three-way temperature regulating valve 5, at the moment, boiler feed water is introduced into the shell side of the steam generator 8, the inlet temperature of the boiler feed water is reduced to be 260.5 ℃, and the high-temperature heat conduction oil in the steam generator 8 is introduced into the heat conduction oil inlet 6 through the first outlet of the first three-way temperature regulating valve 5 and the first oil inlet branch pipe 7; when the control module 10 detects that the inlet temperature of the high-temperature heat conduction oil at the oil inlet of the first three-way temperature regulating valve 5 is equal to 260.5 ℃, the control module 10 controls the first oil outlet of the first three-way temperature regulating valve 5 to be closed, the second oil outlet to be opened, and the high-temperature heat conduction oil is led into the heat conduction oil inlet 6 through the second oil outlet of the first three-way temperature regulating valve 5 and the second oil inlet branch pipe 9;
In order to further improve the accuracy of the high-temperature heat conduction oil inlet temperature, in the third step, a second three-way temperature regulating valve 11 is arranged on an oil outlet of the first oil inlet branch pipe 7, a first oil outlet of the second three-way temperature regulating valve 11 is communicated with a heat conduction oil inlet 6 through a first bypass pipe 12, a second oil outlet of the second three-way temperature regulating valve 11 is communicated with the heat conduction oil inlet 6 through a second bypass pipe 13, a condenser 14 is arranged on the second bypass pipe 13, a high-temperature heat conduction oil temperature signal on an oil inlet of the second three-way temperature regulating valve 11 and a temperature signal of a condensing medium of the condenser 14 are also connected to the control module 10, when the temperature of the high-temperature heat conduction oil discharged from the steam generator 8 and detected by the control module 10 is equal to 260.5 ℃, the control module 10 controls the first oil outlet of the second three-way temperature regulating valve 11 to be opened, the second oil outlet of the second three-way temperature regulating valve 11 is closed, the high-temperature heat conduction oil is led into the heat conduction oil inlet 6 through the first bypass pipe 12, when the temperature of the high-temperature heat conduction oil discharged from the steam generator 8 and the heat conduction oil is still higher than 260.5 ℃, the temperature of the control module 10 is controlled to be still higher than 260.5 ℃, the temperature of the high-temperature of the heat conduction oil discharged from the steam generator 8 is controlled by the second three-way temperature regulating valve is controlled by the control module 10, the second three-way temperature regulating valve is controlled to be opened, the temperature of the condensing medium is cooled by the high-temperature of the condensing medium is discharged from the heat conduction medium 14, and the heat conduction medium is cooled by the heat medium, and the heat medium is cooled by the heat medium, and the temperature is cooled by the temperature of the heat medium is cooled by the heat medium, the temperature is cooled medium is cooled by the temperature controller 23, the temperature is cooled by the temperature medium 2 temperature is cooled by the temperature medium 23.
The temperature regulating method is controlled by the first three-way temperature regulating valve and the steam generator, the manufacturing investment cost of the first three-way temperature regulating valve and the steam generator is low, and the inlet temperature of the high-temperature heat-conducting oil can be accurately regulated by using low-cost equipment investment. Compared with the existing temperature regulating method by flow, the temperature regulating method of the invention can thoroughly solve the problems of temperature, heat transfer coefficient and the like of the heat conduction oil caused by the flow of the heat conduction oil, can lead the temperature of the regulated high-temperature heat conduction oil to be relatively stable, has smaller volatility, can control the temperature fluctuation of the high-temperature heat conduction oil within the range of 0.5 ℃ and has high temperature regulating precision; and secondly, the control module is utilized to realize the temperature control automation of the cyclic utilization of the high-temperature heat conduction oil, thereby improving the convenience and accuracy of temperature adjustment, reducing the possibility of large fluctuation of reaction temperature in the reactor, greatly increasing the running stability of the reactor, prolonging the running period of the reactor, preventing the generation of byproducts and effectively improving the productivity and quality of the methylchlorosilane.
Claims (2)
1. The temperature control method of the organosilicon monomer synthesis fluidized bed is characterized by comprising the following steps of:
Step one: introducing high-temperature heat conduction oil discharged from a heat conduction oil outlet (2) of the reactor (1) into an oil discharge pipe (4) through a heat conduction oil pump (3), controlling the flow rate of the high-temperature heat conduction oil at the outlet of the heat conduction oil pump (3) to be 2000-2020 m 3/h, and controlling the temperature of the high-temperature heat conduction oil at the outlet of the heat conduction oil pump to be 280-285 ℃;
Step two: a first three-way temperature regulating valve (5) is arranged on an outlet of the oil discharge pipe (4), a first oil inlet branch pipe (7) communicated with a heat conducting oil inlet (6) of the reactor (1) is arranged on a first oil outlet of the first three-way temperature regulating valve (5), a steam generator (8) is arranged on the first oil inlet branch pipe (7), a second oil inlet branch pipe (9) communicated with the heat conducting oil inlet (6) of the reactor (1) is arranged on a second oil outlet of the first three-way temperature regulating valve (5), a high-temperature heat conducting oil temperature signal of an oil inlet of the first three-way temperature regulating valve (5) and a boiler water supply temperature signal of the steam generator (8) are connected to a control module (10), and the opening and closing of the first oil outlet and the second oil outlet of the first three-way temperature regulating valve (5) are controlled by the control module (10);
Step three: in the running process of the reactor (1), the temperature of heat conduction oil entering the reactor (1) from a heat conduction oil inlet (6) needs to be controlled to be 260-260.5 ℃, when a control module (10) detects that the inlet temperature of high-temperature heat conduction oil at an oil inlet of a first three-way temperature regulating valve (5) is higher than 260-260.5 ℃, the control module (10) controls a first oil outlet of the first three-way temperature regulating valve (5) to be opened, a second oil outlet is closed, the high-temperature heat conduction oil in an oil drain pipe (4) enters a tube pass of a steam generator (8) through a first oil outlet of the first three-way temperature regulating valve (5), at the moment, boiler water is introduced into a shell pass of the steam generator (8), the inlet temperature of the boiler water is 80-82 ℃ and the pressure is 1.2-1.25 MPa, and the high-temperature heat conduction oil in the steam generator (8) is reduced to 260-260.5 ℃ by using boiler water supply, so that the high-temperature heat conduction oil is introduced into the heat conduction oil inlet (6) through a first outlet of the first three-way temperature regulating valve (5); when the control module (10) detects that the inlet temperature of high-temperature heat conduction oil at the oil inlet of the first three-way temperature regulating valve (5) is equal to 260-260.5 ℃, the control module (10) controls the first oil outlet of the first three-way temperature regulating valve (5) to be closed, the second oil outlet is opened, and the high-temperature heat conduction oil is led into the heat conduction oil inlet (6) through the second oil outlet of the first three-way temperature regulating valve (5) and the second oil inlet branch pipe (9); a second three-way temperature regulating valve (11) is arranged on an oil outlet of the first oil inlet branch pipe (7), a first oil outlet of the second three-way temperature regulating valve (11) is communicated with the heat conducting oil inlet (6) through a first bypass pipe (12), a second oil outlet of the second three-way temperature regulating valve (11) is communicated with the heat conducting oil inlet (6) through a second bypass pipe (13), a condenser (14) is arranged on the second bypass pipe (13), a high-temperature heat conducting oil temperature signal on an oil inlet of the second three-way temperature regulating valve (11) and a temperature signal of a condensing medium of the condenser (14) are also connected to the control module (10), when the temperature of the high-temperature heat conducting oil discharged from the steam generator (8) detected by the control module (10) is equal to 260-260.5 ℃, the control module (10) controls a first oil outlet on the second three-way temperature regulating valve (11) to be opened, a second oil outlet is closed, high-temperature heat conduction oil is led into the heat conduction oil inlet (6) through the first bypass pipe (12), when the temperature of the high-temperature heat conduction oil discharged from the steam generator (8) and detected by the control module (10) is still higher than 260-260.5 ℃, the control module (10) controls the first oil outlet on the second three-way temperature regulating valve (11) to be closed, the second oil outlet is opened, then a condensing medium is led into a shell side inlet of the condenser (14), the high-temperature heat conduction oil in the condenser (14) is cooled to 260-260.5 ℃ by the condensing medium, and then the high-temperature heat conduction oil discharged from the condenser (14) is introduced into the heat conduction oil inlet (6) through the second bypass pipe (13).
2. The method for controlling the temperature of a fluidized bed for synthesizing an organosilicon monomer according to claim 1, wherein: the condensing medium in the condenser (14) is circulating water, the inlet temperature of the circulating water is 27-28 ℃, and the outlet temperature is 32-33 ℃.
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CN213334297U (en) * | 2020-10-15 | 2021-06-01 | 苏州奥德高端装备股份有限公司 | Heat conduction oil furnace device capable of achieving steam heating and accurate temperature control |
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JPH09119607A (en) * | 1995-10-24 | 1997-05-06 | Ishikawajima Harima Heavy Ind Co Ltd | Bed temperature control device for fluidized bed boiler |
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