CN112808192A - Heat recoverable high-efficient phosphorus trichloride apparatus for producing - Google Patents

Heat recoverable high-efficient phosphorus trichloride apparatus for producing Download PDF

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Publication number
CN112808192A
CN112808192A CN202011533673.5A CN202011533673A CN112808192A CN 112808192 A CN112808192 A CN 112808192A CN 202011533673 A CN202011533673 A CN 202011533673A CN 112808192 A CN112808192 A CN 112808192A
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China
Prior art keywords
phosphorus
pipeline
reaction kettle
phosphorus trichloride
heat
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CN202011533673.5A
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Chinese (zh)
Inventor
张坤
王化建
殷浩
刘锦辉
张伟
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Shandong Hanfeng New Material Technology Co ltd
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Xuzhou Jianping Chemical Co ltd
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Priority to CN202011533673.5A priority Critical patent/CN112808192A/en
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/0006Controlling or regulating processes
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/0006Controlling or regulating processes
    • B01J19/0013Controlling the temperature of the process
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J4/00Feed or outlet devices; Feed or outlet control devices
    • B01J4/001Feed or outlet devices as such, e.g. feeding tubes
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J4/00Feed or outlet devices; Feed or outlet control devices
    • B01J4/008Feed or outlet control devices
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B25/00Phosphorus; Compounds thereof
    • C01B25/10Halides or oxyhalides of phosphorus
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2204/00Aspects relating to feed or outlet devices; Regulating devices for feed or outlet devices
    • B01J2204/005Aspects relating to feed or outlet devices; Regulating devices for feed or outlet devices the outlet side being of particular interest
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2204/00Aspects relating to feed or outlet devices; Regulating devices for feed or outlet devices
    • B01J2204/007Aspects relating to the heat-exchange of the feed or outlet devices
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00049Controlling or regulating processes
    • B01J2219/00051Controlling the temperature
    • B01J2219/00074Controlling the temperature by indirect heating or cooling employing heat exchange fluids
    • B01J2219/00087Controlling the temperature by indirect heating or cooling employing heat exchange fluids with heat exchange elements outside the reactor
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00049Controlling or regulating processes
    • B01J2219/00051Controlling the temperature
    • B01J2219/00074Controlling the temperature by indirect heating or cooling employing heat exchange fluids
    • B01J2219/00105Controlling the temperature by indirect heating or cooling employing heat exchange fluids part or all of the reactants being heated or cooled outside the reactor while recycling
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P20/00Technologies relating to chemical industry
    • Y02P20/10Process efficiency

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Inorganic Chemistry (AREA)
  • Physical Or Chemical Processes And Apparatus (AREA)

Abstract

The invention discloses a high-efficiency phosphorus trichloride production device with recoverable heat, which comprises a reaction kettle, a chlorine gas buffer tank, a phosphorus washing tower, a heat exchanger, a vapor-liquid separator and a hot water tank, wherein the reaction kettle is of a double-layer hollow structure, one side of the reaction kettle is provided with a phosphorus trichloride content detection device, the phosphorus trichloride content detection device comprises liquid separation tanks arranged on one side of the reaction kettle side by side, the bottom ends of the liquid separation tanks are connected with the bottom end of the reaction kettle through a first communicating pipe, the top ends of the liquid separation tanks are connected with the top end of the reaction kettle through a second communicating pipe, and control valves are arranged on the first communicating pipe and the second communicating pipe respectively. The method has the characteristics of high detection efficiency and strong practicability.

Description

Heat recoverable high-efficient phosphorus trichloride apparatus for producing
Technical Field
The invention belongs to the technical field of phosphorus trichloride production, and particularly relates to a high-efficiency phosphorus trichloride production device with a recyclable heat quantity.
Background
The phosphorus chemical industry is a new fine chemical industry which is rapidly developed since the 70 s, and the difference between the phosphorus chemical industry and the phosphorus chemical industry is large in product variety and quality compared with the international level when China starts to move late. Because the phosphorus chemical products have respective excellent performances, the phosphorus chemical products replace the original non-phosphorus functional chemical products in a plurality of fields, and take phosphorus trichloride as the phosphorus product of the raw material as an example; such as efficient and low-toxicity organic phosphorus pesticide, novel water treatment agent, flame retardant, plasticizer, stabilizer and the like, the demand increases with the development of national economy, and the plasticizer industry needs to keep pace as soon as possible under the current situation of rapid development of the material industry, so that the scale is improved, and the process is developed to meet the needs of the material industry. As a big support of agriculture, the production of pesticides is a big life for China with billions of population, phosphorus trichloride is an important raw material of organophosphorus pesticides, the optimization of the phosphorus trichloride process becomes a first task for developing organophosphorus pesticides, and the production of high-quality and low-cost phosphorus trichloride and downstream products thereof has important significance.
At present, the domestic phosphorus trichloride production device is still in a small-scale, low-level and repeated construction mode, and the existing problems are as follows:
1. the gas-liquid separator is operated under micro negative pressure, a breathing port is reserved, acidic smoke is frequently emitted outwards from the breathing port, and the heat exchanger is seriously corroded under the environment of cold-hot alternation and dry-wet circulation; the spraying water meets acid mist which is often emitted, more serious acid corrosion occurs, even a heat exchanger with the thickness of 5mm has the service life of only 2-3 years, the emptying pipeline is operated under the pressure of a micro kettle, a large amount of humid air enters from a breathing port, the pipeline is often blocked, and a large amount of phosphoric acid and hydrochloric acid are generated;
2. the capacity of single equipment is low; the reaction of yellow phosphorus and chlorine gas gives off a large amount of heat, but is not recycled.
3. The monitoring of the content of bottom phosphorus in the existing phosphorus trichloride preparation process is difficult;
4. the existing phosphorus trichloride has poor cooling effect on a reaction kettle in the production process.
Disclosure of Invention
The invention aims to provide a high-efficiency phosphorus trichloride production device with recoverable heat, so as to solve the problems in the background technology.
In order to achieve the purpose, the invention provides the following technical scheme:
a high-efficiency phosphorus trichloride production device with recoverable heat comprises a reaction kettle, wherein the reaction kettle is of a double-layer hollow structure, one side of the reaction kettle is provided with a phosphorus trichloride content detection device, the phosphorus trichloride content detection device comprises liquid separation tanks arranged on one side of the reaction kettle side by side, the bottom ends of the liquid separation tanks are connected with the bottom end of the reaction kettle through a first communicating pipe, the top ends of the liquid separation tanks are connected with the top end of the reaction kettle through a second communicating pipe, and the first communicating pipe and the second communicating pipe are both provided with control valves;
the front side of the liquid separation tank is provided with a scale bar, a guide rod is arranged in the liquid separation tank in the vertical direction, the bottom end of the guide rod is connected with a floating ball, the top end of the guide rod penetrates through a guide sleeve and is arranged at the outer end of the liquid separation tank, an insulating L-shaped poking rod is arranged at the top end of the guide rod, the tail end of the L-shaped poking rod is connected with a resistance poking sheet, the resistance poking sheet is connected with an adjustable resistor, the adjustable resistor, an ammeter and a storage battery form a series circuit through conducting wires, and one side of the top of the side surface of the liquid separation tank is provided;
the reaction kettle is characterized in that cooling mechanisms are fixedly arranged on two sides of the top surface of the reaction kettle, each cooling mechanism comprises a pipeline installation box, each pipeline installation box is of a cavity structure, a first motor is arranged on the outer bottom surface of each pipeline installation box, an output shaft of the first motor penetrates through the pipeline installation box and is connected with a first bevel gear, a fastening pipe is fixedly arranged inside the pipeline installation box, a ring groove is formed in the fastening pipe, a water-cooling pipeline is arranged inside the pipeline installation box, a ring block matched with the ring groove is arranged on the water-cooling pipeline, the water-cooling pipeline is rotatably connected into the ring groove of the fastening pipe through the ring block, one end of the water-cooling pipeline penetrates through the outer side wall of the reaction kettle and is arranged inside the hollow structure of the reaction kettle, the water-cooling pipeline is located inside the hollow structure of the reaction kettle and, the other end of the water cooling pipeline penetrates through the side wall of the pipeline installation box and is connected with a booster pump.
As a still further scheme of the invention: and a second motor is arranged at the bottom of the liquid separation tank, an output shaft of the second motor is arranged in the liquid separation tank, and a stirring blade is arranged on the output shaft of the second motor.
As a still further scheme of the invention: and an annular guide block for limiting the guide rod is arranged in the guide sleeve.
As a still further scheme of the invention: the output end of the chlorine buffer tank is connected with the input end of the reaction kettle through a first connecting bent pipe, the first connecting bent pipe is inserted into the reaction kettle, the top output end of the reaction kettle is connected with the input end of one side of the bottom of the phosphorus washing tower through a second connecting bent pipe, the output end of the top end of the phosphorus washing tower is connected with the input end of the front end of the heat exchanger through a third connecting bent pipe, the output end of the rear end of the heat exchanger is provided with a fourth connecting bent pipe and a fifth connecting bent pipe, the other end of the fourth connecting bent pipe is connected with the input end of the top end of the hot water tank, the other end of the fifth connecting bent pipe is connected with the input end of the top;
the output end of the bottom end of the gas-liquid separator is provided with a connecting bent pipe seventh, the other end of the connecting bent pipe seventh is connected with a bypass pipeline I and a bypass pipeline II, the other end of the bypass pipeline I is connected to an output port at the top of the side wall of the phosphorus washing tower, and the other end of the bypass pipeline II is connected with the input end of a finished product buffer tank;
one side of the bottom of the hot water tank is fixedly provided with an eighth connecting elbow, the other end of the eighth connecting elbow is connected with one end of a first pump, and the other end of the first pump is connected with an output port at the bottom of the front end of the heat exchanger through a ninth connecting elbow.
As a still further scheme of the invention: the heat exchanger is a tube type heat exchanger.
As a still further scheme of the invention: and a control valve is arranged on a sixth connecting elbow pipe which is connected with the vapor-liquid separator and the tail gas absorption device.
As a still further scheme of the invention: the tail end of the connecting elbow pipe seven is connected with a three-way joint, and the other two access ports of the three-way joint are respectively connected with a bypass pipeline I and a bypass pipeline II.
As a still further scheme of the invention: the reaction kettle is characterized in that a phosphorus removal pipeline is connected to the input port at the top of the reaction kettle, the phosphorus removal pipeline is of a totally-enclosed structure, and a check valve is arranged on the phosphorus removal pipeline.
As a still further scheme of the invention: the other side of the bottom of the hot water tank is fixedly provided with a first external pipeline, the other end of the first external pipeline is connected with one end of a second pump, and the other end of the second pump is fixedly connected with a thermal equipment input port through the second external pipeline.
As a still further scheme of the invention: the top end of the heat utilization equipment is fixedly provided with a return pipe, and the other end of the return pipe is connected to the hot water tank.
As a still further scheme of the invention: and an output port at the bottom of the phosphorus washing tower is connected with a phosphorus return pipeline, and the other end of the phosphorus return pipeline is connected to an input port at the top end of the reaction kettle.
As a still further scheme of the invention: the phosphorus trichloride production device comprises the following working steps: supplying yellow phosphorus into a reaction kettle through a phosphorus pumping pipeline, supplying chlorine into the reaction kettle through a chlorine buffer tank, reacting the yellow phosphorus and the chlorine to generate phosphorus trichloride, injecting the phosphorus trichloride into a phosphorus washing tower through a connecting bent pipe two for phosphorus washing, leading the phosphorus washing tower into a heat exchanger through a connecting bent pipe three for cooling, keeping the pressure of the reaction kettle, the phosphorus washing tower and the heat exchanger at 0.45Mpa all the time under the action of a control valve, feeding the unreacted yellow phosphorus into the reaction kettle again through a phosphorus return pipeline at the top end of the reaction kettle, simultaneously, cooling the phosphorus trichloride passing through the phosphorus washing tower through the heat exchanger, dividing the phosphorus trichloride into two paths, wherein one path is a steam path, the other path is a liquid path, separating the steam path through a steam-liquid separator, feeding the steam into a tail gas absorption device for treatment, feeding most of the liquid into a finished product buffer tank, feeding a small amount of the phosphorus washing tower again for phosphorus washing treatment, leading the liquid path into a hot water tank through a connecting bent pipe, the tube side is used for feeding materials, the shell side is used for feeding circulating water, the circulating water absorbs heat of the materials in the tube side and then flows into the hot water tank, the temperature of water in the hot water tank can reach 95-98 ℃, and the hot water tank is communicated with heat utilization equipment through a second pump, so that heat is provided for the heat utilization equipment.
Compared with the prior art, the invention has the beneficial effects that:
1. the phosphorus removing pipeline has a fully-closed structure, so that the safety is high, and the pollution to the environment is reduced;
2. the heat exchanger is operated under positive pressure, corrosion is reduced, the service life of the heat exchanger is prolonged, materials are removed on the tube side after circulating water in the shell side of the heat exchanger is condensed, circulating water is removed on the shell side, the circulating water absorbs heat of the materials in the tube side and flows into a hot water tank, the hot water tank is communicated with a heat utilization device through a pump II, heat is provided for the heat utilization device, the circulating water supplies heat to the hot water tank and is communicated with the heat utilization device, heat is recycled, heat energy is conveyed into a cavity of the reaction kettle through a steam backflow pipeline, the heat demand in the reaction process of the reaction kettle is guaranteed, multiple utilization of the heat is realized, and the utilization efficiency is high;
3. according to the invention, along with the reaction process of chlorine and yellow phosphorus in the reaction kettle, the change of the phosphorus trichloride content in the reaction process in the liquid separating tank is realized, so that the change of the buoyancy of the floating ball is realized by changing the phosphorus trichloride concentration in the reaction, the real-time detection of the phosphorus trichloride content in the reaction is realized, the traditional method of monitoring the phosphorus trichloride content by stopping the reaction of the reaction kettle is abandoned, and the characteristics of high detection efficiency and strong practicability are provided;
4. in the process of cooling the reaction kettle, cold water is conveyed into the hollow interior of the reaction kettle through the water cooling pipeline, and the bevel gear I and the bevel gear II are driven to be meshed for transmission through the motor I, so that the water cooling pipeline rotates in the fastening pipe, the hemispherical spray head rotates and sprays in the hollow interior of the reaction kettle to finish water cooling on the whole surface of the reaction kettle, and the water cooling of the reaction kettle is realized.
Drawings
In order to facilitate understanding for those skilled in the art, the present invention will be further described with reference to the accompanying drawings.
FIG. 1 is a schematic structural diagram of a reaction kettle in a high-efficiency phosphorus trichloride production device with recoverable heat.
FIG. 2 is a schematic structural diagram of a cooling mechanism in a high-efficiency phosphorus trichloride production device with recoverable heat.
FIG. 3 is a schematic structural view of a hemispherical nozzle in a high-efficiency phosphorus trichloride production device with recoverable heat.
FIG. 4 is a schematic structural view of a guide sleeve in a high-efficiency phosphorus trichloride production device with recoverable heat.
FIG. 5 is a schematic structural view of a fastening pipe in a heat-recoverable high-efficiency phosphorus trichloride production device.
FIG. 6 is a schematic view of the overall structure of a heat-recoverable high-efficiency phosphorus trichloride production apparatus.
FIG. 7 is a schematic structural diagram of a reaction kettle in a high-efficiency phosphorus trichloride production device with recoverable heat.
In the figure: 1. a reaction kettle; 101. connecting a bent pipe II; 102. a phosphorus removal pipeline; 103. a rephosphorization pipeline; 104. a steam return line; 105. a cooling mechanism; 1051. a pipeline installation box; 1052. a first motor; 1053. a first bevel gear; 1054. fastening the tube; 1055. a second bevel gear; 1056. a water-cooled pipeline; 1057. a booster pump; 1058. a hemispherical nozzle; 1059. a ring block; 106. liquid separating tank; 1061. a scale bar; 1062. a floating ball; 1063. a guide bar; 1064. a guide sleeve; 1065. an L-shaped poke rod; 1066. a first communicating pipe; 1067. a second communicating pipe; 1068. a nitrogen inlet pipe; 1069. a second motor; 107. an adjustable resistor; 1071. an ammeter; 2. a chlorine buffer tank; 201. connecting a first bent pipe; 3. washing a phosphorus tower; 301. connecting a bent pipe III; 4. a heat exchanger; 401. connecting a bent pipe IV; 402. connecting a bent pipe V; 5. a vapor-liquid separator; 501. connecting a bent pipe six; 502. a connecting bent pipe seventh; 5021. a bypass pipeline I; 5022. a bypass pipeline II; 6. a finished product buffer tank; 7. a tail gas absorption device; 8. a hot water tank; 801. connecting a bent pipe eighth; 802. a ninth connecting bend; 803. a first external pipeline; 804. a second external pipeline; 9. a heat-using device; 901. a return pipe; 10. a control valve; 11. a first pump; 12. and a second pump.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Referring to fig. 1-2, in an embodiment of the present invention, an efficient phosphorus trichloride production apparatus with recoverable heat includes a reaction kettle 1, the reaction kettle 1 is a double-layer hollow structure, one side of the reaction kettle 1 is provided with a phosphorus trichloride content detection device, the phosphorus trichloride content detection device comprises a liquid separating tank 106 which is arranged on one side of the reaction kettle 1 side by side, the bottom end of the liquid separation tank 106 is connected with the bottom end of the reaction kettle 1 through a first communicating pipe 1066, the top end of the liquid separation tank 106 is connected with the top end of the reaction kettle 1 through a second communicating pipe 1067, control valves are arranged on the first communicating pipe 1066 and the second communicating pipe 1067, a communicating structure is formed between the liquid separation tank 106 and the reaction kettle 1 through a communicating pipe I1066, so that the detection of the content of the phosphorus trichloride in the reaction kettle 1 is facilitated, and a heat conduction structure is formed between the liquid separation tank 106 and the reaction kettle 1 through the communicating pipe II 1067.
The front surface of the liquid separation tank 106 is provided with a scale bar 1061, which is convenient for observing the amount of the phosphorus trichloride solution in the reaction kettle 1.
The inside of branch fluid reservoir 106 is provided with guide bar 1063 in the vertical direction, the bottom of guide bar 1063 is connected with floater 1062, guide sleeve 1064 is run through at the outer end of branch fluid reservoir 106 at the top of guide bar 1063, and is provided with insulating L type poker rod 1065 at the top of guide bar 1063, the end connection of L type poker rod 1065 has the resistance plectrum, and the resistance plectrum is connected with adjustable resistor 107, adjustable resistor 107 forms a series circuit with ampere meter 1071, battery through the wire, along with the reaction process of reation kettle 1 chlorine and yellow phosphorus, through the change of phosphorus trichloride content in the reaction process in branch fluid reservoir 106, thereby realize the change of phosphorus trichloride concentration in the reaction to floater 1062 buoyancy, change the resistance of adjustable resistor 107, thereby realize the change of electric current, thereby realize the real-time detection to phosphorus trichloride content in the reaction, the traditional method for monitoring the phosphorus trichloride content through stopping the reaction of the reaction kettle is abandoned, and the method has the characteristics of high detection efficiency and strong practicability.
A nitrogen inlet pipe 1068 is arranged on one side of the top of the side surface of the liquid separation tank 106, so that the gas in the liquid separation tank 106 and the reaction kettle 1 can be discharged conveniently in the reaction process.
The two sides of the top surface of the reaction kettle 1 are fixedly provided with cooling mechanisms 105, each cooling mechanism 105 comprises a pipeline installation box 1051, each pipeline installation box 1051 is of a cavity structure, a first motor 1052 is arranged on the outer bottom surface of each pipeline installation box 1051, an output shaft of each first motor 1052 penetrates through the pipeline installation box 1051 and is connected with a first bevel gear 1053, a fastening pipe 1054 is fixedly arranged inside each pipeline installation box 1051, an annular groove is formed in each fastening pipe 1054, a water cooling pipeline 1056 is arranged inside each pipeline installation box 1051, an annular block 1059 matched with the annular groove is arranged on each water cooling pipeline 1056, each water cooling pipeline 1056 is rotatably connected into the annular groove of each fastening pipe 1054 through an annular block 4059, one end of each water cooling pipeline 1056 penetrates through the outer side wall of the reaction kettle 1 and is arranged inside the hollow structure of the reaction kettle 1, each water cooling pipeline 1056 is positioned inside the hollow structure of the reaction kettle 1 and is connected with a hemispherical, the apopore has been seted up on hemispherical shower nozzle 1058, the lateral wall that the other end of water-cooling pipeline 1056 runs through pipeline installation case 1051 is connected with booster pump 1057, carry cold water to reation kettle 1's cavity inside through water-cooling pipeline 1056, drive bevel gear 1053 and the meshing transmission of bevel gear two 1055 through motor 1052 to make water-cooling pipeline 1056 at fastening pipe 1054 internal rotation, realize hemispherical shower nozzle 1058 and accomplish the water-cooling to reation kettle 1 whole surface at reation kettle 1 cavity inside rotation spraying, realize the water-cooling to reation kettle 1.
The bottom of the liquid separation tank 106 is provided with a second motor 1069, an output shaft of the second motor 1069 is arranged inside the liquid separation tank 106, and a stirring blade is arranged on the output shaft of the second motor 1069, so that precipitation in the liquid separation tank 106 is avoided, and the rapid dispersion in the liquid separation tank 106 of heat is improved.
An annular guide block for limiting the guide rod 1063 is arranged inside the guide sleeve 1064.
The output end of the chlorine buffer tank 2 is connected with the input end of the reaction kettle 1 through a first connecting elbow 201, the first connecting bent pipe 201 is inserted into the reaction kettle 1, the top output end of the reaction kettle 1 is connected with the input end of one side of the bottom of the phosphorus washing tower 3 through a second connecting bent pipe 101, the output end of the top end of the phosphorus washing tower 3 is connected with the input end of the front end of the heat exchanger 4 through a connecting bent pipe III 301, the output end of the rear end of the heat exchanger 4 is provided with a connecting elbow pipe four 401 and a connecting elbow pipe five 402, the other end of the fourth connecting elbow 401 is connected with the input end of the top end of the hot water tank 8, the other end of the fifth connecting elbow 402 is connected with the input end of the top end of the vapor-liquid separator 5, the top end output end of the gas-liquid separator 5 is connected with a tail gas absorption device 7 through a connecting elbow six 501, the tail gas generated in the gas-liquid separator 5 is absorbed by the tail gas absorption device 7.
The output of 5 bottoms ends of vapour and liquid separator is provided with connecting bent pipe seven 502, the other end of connecting bent pipe seven 502 is connected with bypass pipeline one 5021 and bypass pipeline two 5022, the other end of bypass pipeline one 5021 is connected on the output port at the lateral wall top of phosphorus washing tower 3, the other end of bypass pipeline two 5022 is connected with the input of finished product buffer tank 6, and the steam circuit separates the back through vapour and liquid separator 5, and the steam enters into tail gas absorbing device 7 through connecting bent pipe six 501 and handles, and liquid major part enters into finished product buffer tank 6 through bypass pipeline two 5022, and a small amount of process bypass pipeline one 5021 gets into again and washes the phosphorus in the phosphorus washing tower 3 and handles.
One side of the bottom of the hot water tank 8 is fixedly provided with a connecting elbow eight 801, the other end of the connecting elbow eight 801 is connected with one end of a pump I11, and the other end of the pump I11 is connected with an output port at the bottom of the front end of the heat exchanger 4 through a connecting elbow nine 802.
The heat exchanger 4 is a tube type heat exchanger, materials are fed through a tube pass, circulating water is fed through a shell pass, and the circulating water absorbs heat of the materials in the tube pass and then flows into the hot water tank 8.
And a control valve 10 is arranged on a connecting elbow six 501 connected with the vapor-liquid separator 5 and the tail gas absorption device 7, and the pressure of the reaction kettle 1, the phosphorus washing tower 3 and the heat exchanger 4 is controlled to be always kept at 0.45 Mpa.
The tail end of the connecting elbow seventh 502 is connected with a three-way joint, and the other two access ports of the three-way joint are respectively connected with the first bypass pipeline 5021 and the second bypass pipeline 5022, so that the connecting elbow seventh 502 is connected with the first bypass pipeline 5021 and the second bypass pipeline 5022 more simply, conveniently and rapidly.
The input port at the top of the reaction kettle 1 is connected with a phosphorus removal pipeline 102, the phosphorus removal pipeline 102 is of a totally enclosed structure, a check valve is arranged on the phosphorus removal pipeline 102, and the safety is high while the pollution to the environment is reduced.
The other side of the bottom of the hot water tank 8 is fixedly provided with a first external pipeline 803, the other end of the first external pipeline 803 is connected with one end of a second pump 12, the other end of the second pump 12 is fixedly connected with an input port of the heat utilization equipment 9 through a second external pipeline 804, the top end of the heat utilization equipment 9 is fixedly provided with a return pipe 901, the other end of the return pipe 901 is connected to the hot water tank 8, the temperature of water in the hot water tank 8 can reach 95-98 ℃, and the hot water tank 8 is communicated with the heat utilization equipment 9 through the second pump 12 to supply heat for the heat utilization equipment 9.
And the output port at the bottom of the phosphorus washing tower 3 is connected with a phosphorus return pipeline 103, and the other end of the phosphorus return pipeline 103 is connected with the input port at the top end of the reaction kettle 1.
The phosphorus trichloride production device comprises the following working steps: supplying yellow phosphorus into a reaction kettle 1 through a phosphorus pumping pipeline 102, supplying chlorine into the reaction kettle 1 through a chlorine buffer tank 2, reacting the yellow phosphorus and the chlorine to generate phosphorus trichloride, injecting the phosphorus trichloride into a phosphorus washing tower 3 through a connecting bent pipe II 101 for phosphorus washing, leading the phosphorus washing tower 3 into a heat exchanger 4 through a connecting bent pipe III 301 for cooling, keeping the pressure of the reaction kettle 1, the phosphorus washing tower 3 and the heat exchanger 4 at 0.45Mpa all the time under the action of a control valve 10, enabling the unreacted yellow phosphorus to enter the reaction kettle 1 from a phosphorus return pipeline 103 at the top end of the reaction kettle 1 again, simultaneously, cooling the phosphorus trichloride passing through the phosphorus washing tower 3 through the heat exchanger 4 and dividing the phosphorus trichloride into two paths, one path being a steam path and the other path being a liquid path, separating the steam path through a steam-liquid separator 5, enabling the steam to enter a tail gas absorption device 7 for processing, enabling most of the liquid to enter a finished product buffer tank 6, and enabling a small amount of the liquid to enter the, the liquid path is led into a hot water tank 8 through a connection elbow pipe four 401, a shell-and-tube heat exchanger is adopted as a heat exchanger 4, materials are fed in a pipe pass, circulating water is fed in a shell pass, the circulating water absorbs heat of the materials in the pipe pass and then flows into the hot water tank 8, the water temperature in the hot water tank 8 can reach 95-98 ℃, the hot water tank 8 is communicated with a heat utilization device 9 through a pump two 12, heat is provided for the heat utilization device 9, and meanwhile heat energy is conveyed into the cavity of the reaction kettle (1) through a steam backflow pipeline (104), so that multiple utilization of the heat is realized;
along with the reaction process of reation kettle 1 chlorine and yellow phosphorus, through the change of the phosphorus trichloride content among the reaction process in knockout drum 106, thereby realize the change of phosphorus trichloride concentration change realization to floater 1062 buoyancy in the reaction, change adjustable resistor 107's resistance, thereby realize the change of electric current, thereby realize the real-time detection to phosphorus trichloride content in the reaction, simultaneously behind phosphorus trichloride apparatus for producing's preparation, carry cold water to reation kettle 1's cavity inside through water-cooling pipeline 1056, drive bevel gear 1053 and bevel gear two 1055 meshing transmission through motor 1052, thereby make water-cooling pipeline 1056 at the internal rotation of fastening pipe 1054, realize that hemispherical shower nozzle 1058 sprays in reation kettle 1 cavity inside rotation, realize the water-cooling to reation kettle 1.
Although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that various changes in the embodiments and/or modifications of the invention can be made, and equivalents and modifications of some features of the invention can be made without departing from the spirit and scope of the invention.

Claims (10)

1. The high-efficiency phosphorus trichloride production device with the recoverable heat comprises a reaction kettle (1) and is characterized in that the reaction kettle (1) is of a double-layer hollow structure, a phosphorus trichloride content detection device is arranged on one side of the reaction kettle (1), the phosphorus trichloride content detection device comprises liquid separation tanks (106) which are arranged on one side of the reaction kettle (1) side by side, the bottom ends of the liquid separation tanks (106) are connected with the bottom end of the reaction kettle (1) through a first communicating pipe (1066), the top ends of the liquid separation tanks (106) are connected with the top end of the reaction kettle (1) through a second communicating pipe (1067), and control valves are arranged on the first communicating pipe (1066) and the second communicating pipe (1067);
the front surface of the liquid separation tank (106) is provided with a scale strip (1061), the inside of the liquid separation tank (106) is provided with a guide rod (1063) in the vertical direction, the bottom end of the guide rod (1063) is connected with a floating ball (1062), the top end of the guide rod (1063) penetrates through a guide sleeve (1064) and is arranged at the outer end of the liquid separation tank (106), the top end of the guide rod (1063) is provided with an insulating L-shaped poking rod (1065), the tail end of the L-shaped poking rod (1065) is connected with a resistance poking sheet, the resistance poking sheet is connected with an adjustable resistor (107), the adjustable resistor (107), an ammeter (1071) and a storage battery form a series circuit through conducting wires, and one side surface top side of the liquid separation tank (106) is provided with a nitrogen;
fixed cooling mechanism (105) that is provided with in reation kettle (1) top surface both sides, cooling mechanism (105) include pipeline installation case (1051), pipeline installation case (1051) are the cavity structure, be provided with motor (1052) on the outside bottom surface of pipeline installation case (1051), the output shaft of motor (1052) runs through pipeline installation case (1051) and is connected with bevel gear (1053), the fixed fastening pipe (1054) that is provided with in inside of pipeline installation case (1051), the ring channel has been seted up in the inside setting of fastening pipe (1054), the inside of pipeline installation case (1051) is provided with water-cooling pipeline (1056), be provided with on water-cooling pipeline (1056) with ring channel looks adaptation ring block (1059), water-cooling pipeline (1056) rotate to be connected in the ring channel of fastening pipe (1054) through ring block (4059), the one end of water-cooling pipeline (1056) runs through the lateral wall setting of reation kettle (1) in the hollow structure of reation kettle (1) Portion, water-cooling pipeline (1056) are located reation kettle (1) hollow structure internal connection and have hemispherical shower nozzle (1058), the apopore has been seted up on hemispherical shower nozzle (1058), the lateral wall that the other end of water-cooling pipeline (1056) runs through pipeline install bin (1051) is connected with booster pump (1057).
2. The high-efficiency phosphorus trichloride production device capable of recycling heat according to claim 1, wherein a second motor (1069) is arranged at the bottom of the liquid separation tank (106), an output shaft of the second motor (1069) is arranged inside the liquid separation tank (106), and an output shaft of the second motor (1069) is provided with a stirring blade.
3. The high-efficiency phosphorus trichloride production apparatus capable of recovering heat according to claim 1, wherein an annular guide block for limiting the guide rod (1063) is provided inside the guide sleeve (1064).
4. The high-efficiency phosphorus trichloride production device capable of recovering heat according to claim 1, wherein an input end of the reaction kettle (1) is connected with an output end of the chlorine buffer tank (2) through a first connecting elbow (201), the first connecting elbow (201) is inserted into the reaction kettle (1), an output end of the top of the reaction kettle (1) is connected with an input end of one side of the bottom of the phosphorus washing tower (3) through a second connecting elbow (101), an output end of the top of the phosphorus washing tower (3) is connected with an input end of the front end of the heat exchanger (4) through a third connecting elbow (301), an output end of the rear end of the heat exchanger (4) is provided with a fourth connecting elbow (401) and a fifth connecting elbow (402), the other end of the fourth connecting elbow (401) is connected with an input end of the top of the tank (8), the other end of the fifth connecting elbow (402) is connected with an input end of the vapor-liquid separator (5), the top end output end of the gas-liquid separator (5) is connected with a tail gas absorption device (7) through a connecting elbow six (501);
a connecting bent pipe seven (502) is arranged at the output end of the bottom end of the vapor-liquid separator (5), the other end of the connecting bent pipe seven (502) is connected with a bypass pipeline one (5021) and a bypass pipeline two (5022), the other end of the bypass pipeline one (5021) is connected to an output port at the top of the side wall of the phosphorus washing tower (3), and the other end of the bypass pipeline two (5022) is connected with the input end of a finished product buffer tank (6);
a connecting elbow eight (801) is fixedly arranged on one side of the bottom of the hot water tank (8), the other end of the connecting elbow eight (801) is connected with one end of a pump I (11), and the other end of the pump I (11) is connected with an output port at the bottom of the front end of the heat exchanger (4) through a connecting elbow nine (802);
a steam backflow pipeline (104) is arranged on the top surface of the interior of the hot water tank (8), and the other end of the steam backflow pipeline (104) is connected to the interior of the double-layer hollow structure of the reaction kettle (1).
5. The high-efficiency phosphorus trichloride production device capable of recovering heat according to claim 4, wherein the heat exchanger (4) is a tubular heat exchanger, and a control valve (10) is arranged on a connecting elbow six (501) of the vapor-liquid separator (5) and the tail gas absorption device (7).
6. The high-efficiency phosphorus trichloride production device capable of recovering heat according to claim 4, wherein a tee joint is connected to the end of the connecting elbow pipe seven (502), and the other two inlets of the tee joint are respectively connected with a bypass pipeline one (5021) and a bypass pipeline two (5022).
7. The high-efficiency phosphorus trichloride production device capable of recovering heat according to claim 4, wherein a phosphorus removal pipeline (102) is connected to an input port at the top of the reaction kettle (1), the phosphorus removal pipeline (102) is of a fully-closed structure, and a check valve is arranged on the phosphorus removal pipeline (102).
8. The high-efficiency phosphorus trichloride production device capable of recycling heat according to claim 4, wherein a first external pipeline (803) is fixedly arranged on the other side of the bottom of the hot water tank (8), the other end of the first external pipeline (803) is connected with one end of a second pump (12), the other end of the second pump (12) is fixedly connected with an input port of a heat utilization device (9) through a second external pipeline (804), a return pipe (901) is fixedly arranged at the top end of the heat utilization device (9), and the other end of the return pipe (901) is connected to the hot water tank (8).
9. The high-efficiency phosphorus trichloride production device capable of recovering heat according to claim 4, wherein a phosphorus return pipeline (103) is connected to an output port at the bottom of the phosphorus washing tower (3), and the other end of the phosphorus return pipeline (103) is connected to an input port at the top end of the reaction kettle (1).
10. The heat-recoverable high-efficiency phosphorus trichloride production device according to claim 1, which comprises the following working steps: yellow phosphorus is supplied into a reaction kettle (1) through a phosphorus pumping pipeline (102), chlorine is supplied into the reaction kettle (1) through a chlorine buffer tank (2), the yellow phosphorus reacts with the chlorine to generate phosphorus trichloride, the phosphorus trichloride is injected into a phosphorus washing tower (3) through a connecting bent pipe II (101) to wash phosphorus, the phosphorus trichloride is guided into a heat exchanger (4) through the phosphorus washing tower (3) through a connecting bent pipe III (301) to be cooled, the pressure of the reaction kettle (1), the phosphorus washing tower (3) and the heat exchanger (4) is always kept at 0.45Mpa through the action of a control valve (10), the unreacted yellow phosphorus can enter the reaction kettle (1) from a phosphorus return pipeline (103) at the top end of the reaction kettle (1), meanwhile, the phosphorus trichloride passing through the phosphorus washing tower (3) is cooled through the heat exchanger (4) and then divided into two paths, one path is a vapor path, the other path is a liquid path, the vapor enters a tail gas absorption device (7) to be treated after being separated by a vapor-liquid separator (5), most of liquid enters a finished product buffer tank (6), a small amount of liquid enters a phosphorus washing tower (3) again for phosphorus washing treatment, a liquid path is guided into a hot water tank (8) through a connecting bent pipe IV (401), a heat exchanger (4) adopts a tubular heat exchanger, materials are conveyed through a tube pass, circulating water is conveyed through a shell pass, the circulating water absorbs heat of the materials in the tube pass and flows into the hot water tank (8), the temperature of the water in the hot water tank (8) can reach 95-98 ℃, the hot water tank (8) is communicated with a heat utilization device (9) through a pump II (12), heat is provided for the heat utilization device (9), meanwhile, heat energy is conveyed into a cavity of a reaction kettle (1) through a steam backflow pipeline (104), and multiple utilization of the heat is realized;
along with the reaction process of chlorine and yellow phosphorus in the reaction kettle (1), the change of the concentration of phosphorus trichloride in the reaction and the change of the buoyancy of the floating ball (1062) are realized through the change of the content of phosphorus trichloride in the reaction process in the liquid separation tank (106), so that the real-time detection of the content of phosphorus trichloride in the reaction is realized;
meanwhile, after the phosphorus trichloride production device is prepared, cold water is conveyed to the hollow interior of the reaction kettle (1) through a water cooling pipeline (1056), and a motor I (1052) drives a bevel gear I (1053) and a bevel gear II (1055) to be in meshing transmission, so that the water cooling pipeline (1056) rotates in a fastening pipe (1054), a hemispherical spray head (1058) is rotationally sprayed in the hollow interior of the reaction kettle (1), and the water cooling of the reaction kettle (1) is realized.
CN202011533673.5A 2020-12-22 2020-12-22 Heat recoverable high-efficient phosphorus trichloride apparatus for producing Pending CN112808192A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113694852A (en) * 2021-09-30 2021-11-26 南京佳华工程技术有限公司 Continuous synthesis process and equipment for phosphorus trichloride

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CN201397313Y (en) * 2009-05-06 2010-02-03 河南清水源科技股份有限公司 Phosphorus content tester
CN104787737A (en) * 2014-01-17 2015-07-22 泰兴市申龙化工有限公司 Packaged technology and equipment technology for continuously producing phosphorus trichloride
US20200087146A1 (en) * 2017-03-13 2020-03-19 Kanto Denka Kogyo Co., Ltd. Method for producing phosphorus pentafluoride
CN110898455A (en) * 2019-11-29 2020-03-24 富彤化学有限公司 Phosphorus trichloride refining equipment and process thereof
CN111377420A (en) * 2018-12-29 2020-07-07 江苏灵创工程设计有限公司 Phosphorus trichloride production process

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Publication number Priority date Publication date Assignee Title
CN201397313Y (en) * 2009-05-06 2010-02-03 河南清水源科技股份有限公司 Phosphorus content tester
CN104787737A (en) * 2014-01-17 2015-07-22 泰兴市申龙化工有限公司 Packaged technology and equipment technology for continuously producing phosphorus trichloride
US20200087146A1 (en) * 2017-03-13 2020-03-19 Kanto Denka Kogyo Co., Ltd. Method for producing phosphorus pentafluoride
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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113694852A (en) * 2021-09-30 2021-11-26 南京佳华工程技术有限公司 Continuous synthesis process and equipment for phosphorus trichloride

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