CN115382492A - Continuous preparation device and preparation method of phosphorus pentachloride - Google Patents
Continuous preparation device and preparation method of phosphorus pentachloride Download PDFInfo
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- CN115382492A CN115382492A CN202211013701.XA CN202211013701A CN115382492A CN 115382492 A CN115382492 A CN 115382492A CN 202211013701 A CN202211013701 A CN 202211013701A CN 115382492 A CN115382492 A CN 115382492A
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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
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/18—Stationary reactors having moving elements inside
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D46/00—Filters or filtering processes specially modified for separating dispersed particles from gases or vapours
- B01D46/66—Regeneration of the filtering material or filter elements inside the filter
- B01D46/70—Regeneration of the filtering material or filter elements inside the filter by acting counter-currently on the filtering surface, e.g. by flushing on the non-cake side of the filter
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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
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/0053—Details of the reactor
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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
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/18—Stationary reactors having moving elements inside
- B01J19/20—Stationary reactors having moving elements inside in the form of helices, e.g. screw reactors
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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
- B01J4/00—Feed or outlet devices; Feed or outlet control devices
- B01J4/001—Feed or outlet devices as such, e.g. feeding tubes
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B25/00—Phosphorus; Compounds thereof
- C01B25/10—Halides or oxyhalides of phosphorus
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Abstract
The invention discloses a continuous preparation device and a preparation method of phosphorus pentachloride, which comprises a reaction kettle, wherein the top of the reaction kettle is connected with a phosphorus trichloride feeding pipeline, the bottom side of the reaction kettle is connected with a chlorine feeding pipeline, a rotating shaft is vertically arranged in the reaction kettle, a spiral belt for extruding materials to form a compact isolation layer is arranged at the lower side of the rotating shaft close to the chlorine feeding pipeline, a material level meter is arranged at the bottom side of the reaction kettle, and an electric rotary valve is arranged at a discharge pipe at the bottom of the reaction kettle; the invention can continuously discharge the product during the continuous production of the phosphorus pentachloride, and does not cause the chlorine to escape downwards during the discharge of the product.
Description
Technical Field
The invention relates to the technical field of phosphorus pentachloride production, in particular to a continuous preparation device and a preparation method of phosphorus pentachloride.
Background
At present, the production of phosphorus pentachloride mostly adopts the traditional kettle type production process, namely, phosphorus trichloride and chlorine are taken as raw materials,
injecting a certain amount of liquid phosphorus trichloride into a stirring type reaction kettle, and then introducing chlorine gas to react in a gas-liquid contact mode. The process has the defects of incomplete reaction, poor working condition environment, large viscous stirring resistance of a reaction system, low impurity wrapping purity of a product, low yield, intermittent production and the like, and cannot meet the requirement of industrial continuous production.
For this reason, relevant researchers have also developed corresponding equipment and process for continuously producing phosphorus pentachloride, for example, CN112919439A, a method and apparatus for continuously preparing high-purity phosphorus pentachloride, disclosed in the following contents: an apparatus for continuously preparing high purity phosphorus pentachloride, comprising: the device comprises a reactor and a buffer tank, wherein a phosphorus trichloride feed inlet and a mixed gas inlet are formed in the middle of the reactor, a phosphorus pentachloride discharge port is formed in the bottom of the reactor, a tail gas outlet is formed in the top of the reactor, a closed circulation loop is formed between the tail gas outlet and the mixed gas inlet, and a circulating fan is connected in series on the circulation loop; the buffer tank is respectively provided with a chlorine inlet, a tail gas recovery port and a mixed gas outlet, and the buffer tank is connected in series on the circulating loop through the tail gas recovery port and the mixed gas outlet. When the preparation device is used, mixed gas enters the reactor through the mixed gas inlet through the circulating fan, phosphorus trichloride enters the reactor through the phosphorus trichloride feeding hole, the phosphorus trichloride feeding hole and the mixed gas inlet are both positioned in the middle of the reactor, phosphorus trichloride in the reactor reacts with chlorine in the mixed gas to form fine phosphorus pentachloride crystal grains which float on the upper part in the reactor to form a fluidized reaction system, the phosphorus pentachloride crystal grains gradually grow into particles along with the reaction, the particles are settled on the inner bottom of the reactor under the action of gravity, and after the reaction is finished, a high-purity phosphorus pentachloride product is collected through the phosphorus pentachloride discharging hole. In the process, phosphorus pentachloride can be continuously produced by continuously introducing phosphorus trichloride and chlorine, but the process has the following problems that cannot be ignored:
firstly, the high-purity phosphorus pentachloride is discharged through a phosphorus pentachloride discharge port after the reaction is finished every time, so that the production of the phosphorus pentachloride is carried out batch by batch, and the so-called continuous preparation process also has a process of stopping the production in a gap of discharging, so that the degree of continuous production is undoubtedly reduced, and the production efficiency is reduced; secondly, the reason that the product of high-purity phosphorus pentachloride is discharged through a phosphorus pentachloride discharge port after the reaction of each batch is finished is as follows: chlorine gas is easy to escape from a phosphorus pentachloride discharge port, and if the continuous production is carried out while discharging, the chlorine gas inevitably escapes downwards along with the discharge of the phosphorus pentachloride, thereby causing serious safety threat to the factory environment; in addition, it should be noted that: because phosphorus pentachloride grains generated by continuous reaction gradually grow into particles and are settled at the inner bottom of the reactor under the action of gravity, and the phosphorus pentachloride particles are in a fluffy state, chlorine gas is easy to escape downwards from gaps among the phosphorus pentachloride particles in the continuous production and discharge process even if the phosphorus pentachloride particles are in a certain thickness.
Disclosure of Invention
The invention aims to overcome the defects and provide a continuous preparation device and a preparation method of phosphorus pentachloride, which can continuously discharge products simultaneously in the process of continuously producing the phosphorus pentachloride and can not cause chlorine to escape downwards in the process of discharging the products.
In order to solve the technical problems, the invention adopts the technical scheme that: the utility model provides a phosphorus pentachloride continuous preparation device, includes reation kettle, reation kettle top and phosphorus trichloride feed line connection, reation kettle bottom side and chlorine feed line connection, the vertical rotation axis that is equipped with in the reation kettle, the downside position that the rotation axis is close to chlorine feed line is equipped with the spiral shell area that is used for the extrusion material to form closely knit isolation layer, and the reation kettle bottom side is equipped with the charge level indicator, and reation kettle bottom discharging pipe position is equipped with electric rotary valve.
Preferably, the signal output end of the level indicator is connected with the input end of a controller, and the control signal output end of the controller is connected with the signal input end of the electric rotary valve.
Preferably, the upper side of the rotating shaft is connected with the scraper through a connecting rod, and the top of the rotating shaft is connected with an output shaft of the rotating motor.
Preferably, the discharge pipe at the bottom of the reaction kettle is connected with the spiral belt product tank through a spiral conveyer; the spiral belt is a double spiral belt structure.
Preferably, an air outlet at the top of the reaction kettle is connected with an air inlet end of a chlorine cooler through an air outlet pipeline, and an air outlet end of the chlorine cooler is connected with a chlorine feeding pipeline through an air return pipeline; the phosphorus trichloride feeding pipeline is connected with the phosphorus trichloride metering tank, and a magnetic pump is arranged on the phosphorus trichloride feeding pipeline.
Preferably, be equipped with first chlorine buffer tank, chlorine circulator and second chlorine buffer tank on the muffler line in proper order, first chlorine buffer tank still is connected with chlorine air supply line.
Preferably, a filter is further arranged at an air outlet in the top of the reaction kettle, and an electric heating belt is arranged outside the filter.
Preferably, a chlorine back-blowing pipeline is further arranged between the outlet of the filter and the chlorine feeding pipeline, a first valve is arranged on the chlorine back-blowing pipeline, a second valve is arranged on the position, close to the bottom side of the reaction kettle, of the chlorine feeding pipeline, and a third valve is arranged on the air outlet pipeline.
In addition, the invention also discloses a preparation method of the continuous preparation device of the phosphorus pentachloride, which comprises the following steps:
s1: the phosphorus trichloride liquid in the phosphorus trichloride feeding pipeline is continuously sprayed downwards through an atomizing nozzle at the top of the reaction kettle;
s2: chlorine in the chlorine feeding pipeline continuously enters the reaction kettle from the bottom side of the reaction kettle and then is mixed with the phosphorus trichloride liquid for reaction to obtain a solid phosphorus pentachloride material;
s3: the phosphorus pentachloride material is deposited at the bottom of the reaction kettle, and after the rotating motor is started, the rotating motor drives the rotating shaft to rotate, so that the spiral belt rotates to extrude the phosphorus pentachloride material to form a compact isolation layer, and at the moment, chlorine introduced from the chlorine feeding pipeline cannot be discharged downwards from a discharge port at the bottom of the reaction kettle due to the obstruction of the compact isolation layer of the phosphorus pentachloride material and only can upwards pass through the inside of the reaction kettle and be mixed with the phosphorus trichloride liquid for reaction;
s4: after the electric rotary valve is opened, the phosphorus pentachloride material moves downwards under the rotation action of the spiral belt and is continuously discharged downwards at a certain flow rate under the control of the electric rotary valve to enter the spiral conveyor, at the moment, the compact isolation layer of the phosphorus pentachloride material at the bottom of the reaction kettle is always kept at a certain thickness, the lower surface of the compact isolation layer of the phosphorus pentachloride material is continuously discharged from a discharge hole at the bottom of the reaction kettle, and the upper surface of the compact isolation layer of the phosphorus pentachloride material always separates the introduced chlorine gas to prevent the chlorine gas from escaping from the discharge hole;
s5: and the phosphorus pentachloride material entering the spiral conveyer is sent into a spiral belt product tank, and then is packaged by a packaging machine and then is delivered out of the warehouse.
Further, the method also comprises the step of back flushing a filter arranged at a gas outlet at the top of the reaction kettle by using a chlorine gas feeding pipe line:
s6: and closing a second valve on the chlorine feeding pipeline and a third valve on the air outlet pipeline at regular intervals, opening a first valve on the chlorine back flushing pipeline, and allowing the chlorine to reversely pass through the filter from the chlorine back flushing pipeline to perform a back flushing process.
The invention has the beneficial effects that:
1. the invention can continuously discharge the product during the continuous production of the phosphorus pentachloride, and does not cause the chlorine to escape downwards during the discharge of the product.
2. According to the invention, the rotating spiral belt is additionally arranged, so that the phosphorus pentachloride material can be extruded to form a compact isolation layer, and at the moment, chlorine introduced from the chlorine feeding pipeline can not be discharged downwards from a discharge hole at the bottom of the reaction kettle due to the isolation of the compact isolation layer of the phosphorus pentachloride material, and can only upwards pass through the interior of the reaction kettle and be mixed and reacted with the phosphorus trichloride liquid, so that the chlorine can not be downwards escaped and discharged in the process of continuously discharging a product.
3. The spiral belt can also play a role in pushing the discharging of the phosphorus pentachloride material, and can push the whole dense isolation layer of the phosphorus pentachloride material to move downwards so as to promote the lower surface of the dense isolation layer of the phosphorus pentachloride material to be continuously discharged from a discharge hole at the bottom of the reaction kettle.
4. Under the regulation of an electric rotary valve, phosphorus pentachloride materials can be discharged downwards continuously at a certain flow rate and enter a spiral conveyer, the discharge flow rate of the electric rotary valve is controlled, so that a compact isolation layer of the phosphorus pentachloride materials at the bottom of a reaction kettle can be always kept at a certain thickness, the lower surface of the compact isolation layer of the phosphorus pentachloride materials is continuously discharged from a discharge hole at the bottom of the reaction kettle, and the upper surface of the compact isolation layer of the phosphorus pentachloride materials is always used for isolating introduced chlorine gas to prevent the chlorine gas from being discharged downwards from the discharge hole;
5. the invention can introduce chlorine to reversely flush the filter by additionally arranging the chlorine reverse blowing pipeline, thereby ensuring the filtering performance of the filter.
Drawings
FIG. 1 is a schematic structural diagram of a continuous preparation apparatus for phosphorus pentachloride;
FIG. 2 is an enlarged schematic view of the region where the reaction vessel is located in FIG. 1.
Detailed Description
The invention is described in further detail below with reference to the figures and specific embodiments.
As shown in figures 1 and 2, a phosphorus pentachloride continuous preparation device, including reation kettle 1, reation kettle 1 top and phosphorus trichloride feed line 2 are connected, and reation kettle 1 bottom side and chlorine feed line 3 are connected, the vertical rotation axis 4 that is equipped with in reation kettle 1, rotation axis 4 are close to the downside position of chlorine feed line 3 and are equipped with the spiral shell area 5 that is used for the extrusion material to form closely knit isolation layer, and reation kettle 1 bottom side is equipped with charge level indicator 6, and reation kettle 1 bottom discharging pipe position is equipped with electric rotary valve 7.
Preferably, the signal output end of the level indicator 6 is connected with the input end of a controller, and the control signal output end of the controller is connected with the signal input end of the electric rotary valve 7. In this embodiment, in order to make the closely knit isolation layer of phosphorus pentachloride material bottom of reation kettle 1 remain at certain thickness throughout, can monitor through charge level indicator 6, when monitoring closely knit isolation layer of phosphorus pentachloride material thickness thin, the blowing flow of controller control electric rotary valve 7 reduces, make closely knit isolation layer of phosphorus pentachloride material thickness increase to normal scope, when monitoring closely knit isolation layer of phosphorus pentachloride material thickness thick, the blowing flow of controller control electric rotary valve 7 increases, make closely knit isolation layer of phosphorus pentachloride material thickness reduce to normal scope till. Preferably, the controller in this embodiment may be a siemens S7-300 PLC controller.
Preferably, the upper side of the rotating shaft 4 is connected with the scraper 9 through a connecting rod 8, and the top of the rotating shaft 4 is connected with an output shaft of a rotating motor 10. In order to prevent the material from being attached to the side wall of the reaction kettle 1, after the connecting rod 8 and the scraper 9 are additionally arranged, when the rotating shaft 4 rotates, the scraper 9 can be driven to rotate along with the rotating shaft, so that the side wall of the reaction kettle 1 is continuously scraped, and phosphorus pentachloride crystals are effectively prevented from being attached to the side wall of the reaction kettle 1.
Preferably, a discharge pipe at the bottom of the reaction kettle 1 is connected with a spiral belt product tank 12 through a spiral conveyer 11; the spiral belt 5 is a double-spiral belt structure. The phosphorus pentachloride material continuously discharged from a discharge pipe at the bottom of the reaction kettle 1 can be directly and continuously conveyed into a spiral belt product tank 12 through a spiral conveyor 11, is stirred through a spiral belt of the material, can be discharged into a packaging machine below, and is discharged out of a warehouse after being packaged. The double-spiral belt structure is more uniform, the range of the extrusion surface of the material is larger, and the material can be extruded more uniformly.
Preferably, an air outlet at the top of the reaction kettle 1 is connected with an air inlet end of a chlorine cooler 14 through an air outlet pipeline 13, and an air outlet end of the chlorine cooler 14 is connected with a chlorine feeding pipeline 3 through an air return pipeline 15; phosphorus trichloride feed line 2 is connected with phosphorus trichloride metering tank 16, is equipped with magnetic drive pump 17 on the phosphorus trichloride feed line 2. The liquid phosphorus trichloride in the phosphorus trichloride metering tank 16 can be pumped into the chlorine gas feeding pipeline 3 by the magnetic pump 17 and then is sent to the top of the reaction kettle 1.
Preferably, a first chlorine buffer tank 18, a chlorine circulator 19 and a second chlorine buffer tank 20 are sequentially arranged on the gas return line 15, and the first chlorine buffer tank 18 is further connected with a chlorine gas supply line 21. The first chlorine buffer tank 18 is arranged, so that the pressure of chlorine can be effectively buffered, the chlorine circulator 19 is protected, the second chlorine buffer tank 20 is arranged, so that the chlorine can be effectively buffered, the impact on the reaction kettle 1 caused by overlarge pressure is prevented, and the chlorine circulator 19 plays a role of a circulating pump, so that the chlorine can circularly enter the reaction kettle 1 for reaction; in addition, a part of the chlorine gas lost by the reaction in the reaction vessel 1 can be supplemented through the chlorine gas supply line 21.
Preferably, a filter 22 is further arranged at an air outlet at the top of the reaction kettle 1, and an electric heating belt 23 is arranged outside the filter 22. When chlorine gas rises and leaves from an air outlet at the top of the reaction kettle 1, solid phosphorus pentachloride is mixed in the chlorine gas, so that in order to avoid material loss, a filter 22 is arranged to filter out the solid phosphorus pentachloride in the gas, and in addition, an electric heating belt 23 can heat the filter 22, so that materials attached to a filter screen of the filter 22 can more easily leave in the back flushing process of the filter 22, and the back flushing effect is improved.
Preferably, a chlorine back-blowing pipeline 24 is further arranged between the outlet of the filter 22 and the chlorine feeding pipeline 3, a first valve 25 is arranged on the chlorine back-blowing pipeline 24, a second valve 26 is arranged at a position of the chlorine feeding pipeline 3 close to the bottom side of the reaction kettle 1, and a third valve 27 is arranged on the gas outlet pipeline 13. The filter 22 can be backwashed by introducing chlorine through the chlorine blowback line 24, so as to ensure the filtering performance of the filter 22.
In addition, the invention also discloses a preparation method of the continuous preparation device of the phosphorus pentachloride, which comprises the following steps:
s1: the phosphorus trichloride liquid in the phosphorus trichloride feeding pipeline 2 is continuously sprayed downwards through an atomizing nozzle at the top of the reaction kettle 1;
s2: chlorine in the chlorine feeding pipeline 3 continuously enters the reaction kettle 1 from the bottom side of the reaction kettle 1, and then is mixed with the phosphorus trichloride liquid for reaction to obtain a solid phosphorus pentachloride material;
s3: the phosphorus pentachloride material is deposited at the bottom of the reaction kettle 1, and after the rotating motor 10 is started, the rotating shaft 4 is driven to rotate, so that the spiral belt 5 rotates to extrude the phosphorus pentachloride material to form a compact isolation layer, and at the moment, chlorine introduced from the chlorine feeding pipeline 3 cannot be discharged downwards from a discharge port at the bottom of the reaction kettle 1 due to the obstruction of the compact isolation layer of the phosphorus pentachloride material, and only can upwards pass through the inside of the reaction kettle 1 to be mixed and reacted with the phosphorus trichloride liquid;
s4: after the electric rotary valve 7 is opened, the phosphorus pentachloride material moves downwards under the rotation action of the spiral belt 5 and is continuously discharged downwards at a certain flow rate under the control of the electric rotary valve 7 to enter the spiral conveyor 11, at the moment, the dense isolation layer of the phosphorus pentachloride material at the bottom of the reaction kettle 1 is always kept at a certain thickness, the lower surface of the dense isolation layer of the phosphorus pentachloride material is continuously discharged from a discharge port at the bottom of the reaction kettle 1, and the upper surface of the dense isolation layer of the phosphorus pentachloride material always isolates the introduced chlorine gas to prevent the chlorine gas from being discharged from the discharge port;
s5: the phosphorus pentachloride material entering the screw conveyor 11 is sent into the spiral belt product tank 12, and then is packaged by a packaging machine and then is delivered out of a warehouse.
Further, the method also comprises the step of back flushing a filter 22 arranged at an air outlet at the top of the reaction kettle 1 by using a chlorine gas feeding pipeline 3:
s6: at regular intervals, the second valve 26 on the chlorine gas feeding pipeline 3 and the third valve 27 on the gas outlet pipeline 13 are closed, the first valve 25 on the chlorine gas back flushing pipeline 24 is opened, and at the moment, the chlorine gas reversely passes through the filter 22 from the chlorine gas back flushing pipeline 24 to carry out the back flushing process on the chlorine gas.
The above-described embodiments are merely preferred embodiments of the present invention, and should not be construed as limiting the present invention, and features in the embodiments and examples in the present application may be arbitrarily combined with each other without conflict. The protection scope of the present invention is defined by the claims, and includes equivalents of technical features of the claims. I.e., equivalent alterations and modifications within the scope hereof, are also intended to be within the scope of the invention.
Claims (10)
1. The utility model provides a phosphorus pentachloride continuous preparation device, includes reation kettle (1), and reation kettle (1) top is connected with phosphorus trichloride feed line (2), and reation kettle (1) bottom side is connected with chlorine feed line (3), its characterized in that: vertical rotation axis (4) that are equipped with in reation kettle (1), the downside position that rotation axis (4) are close to chlorine feed line (3) is equipped with spiral shell area (5) that are used for the extrusion material to form closely knit isolation layer, and reation kettle (1) bottom side is equipped with charge level indicator (6), and reation kettle (1) bottom discharging pipe position is equipped with electric rotary valve (7).
2. The continuous preparation device of phosphorus pentachloride as recited in claim 1, characterized in that: the signal output end of the charge level indicator (6) is connected with the input end of a controller, and the control signal output end of the controller is connected with the signal input end of an electric rotary valve (7).
3. The continuous preparation device of phosphorus pentachloride as recited in claim 1, characterized in that: the upper side of the rotating shaft (4) is connected with a scraper (9) through a connecting rod (8), and the top of the rotating shaft (4) is connected with an output shaft of a rotating motor (10).
4. The continuous preparation device of phosphorus pentachloride as recited in claim 1, characterized in that: a discharge pipe at the bottom of the reaction kettle (1) is connected with a spiral belt product tank (12) through a spiral conveyer (11); the spiral belt (5) is of a double-spiral belt structure.
5. The continuous preparation device of phosphorus pentachloride as recited in claim 1, characterized in that: a gas outlet at the top of the reaction kettle (1) is connected with a gas inlet end of a chlorine gas cooler (14) through a gas outlet pipeline (13), and a gas outlet end of the chlorine gas cooler (14) is connected with a chlorine gas feeding pipeline (3) through a gas return pipeline (15); the phosphorus trichloride feeding pipeline (2) is connected with a phosphorus trichloride metering tank (16), and a magnetic pump (17) is arranged on the phosphorus trichloride feeding pipeline (2).
6. The continuous preparation device of phosphorus pentachloride as recited in claim 5, wherein: be equipped with first chlorine buffer tank (18), chlorine circulator (19) and second chlorine buffer tank (20) on return gas pipeline (15) in proper order, first chlorine buffer tank (18) still are connected with chlorine gas supply pipeline (21).
7. The continuous preparation device of phosphorus pentachloride as recited in claim 5, characterized in that: a filter (22) is further arranged at an air outlet in the top of the reaction kettle (1), and an electric heating belt (23) is arranged on the outer side of the filter (22).
8. The continuous preparation device of phosphorus pentachloride as recited in claim 7, wherein: still be equipped with chlorine blowback pipeline (24) between filter (22) export and chlorine charging pipeline (3), be equipped with first valve (25) on chlorine blowback pipeline (24), be equipped with second valve (26) on chlorine charging pipeline (3) the position that is close to reation kettle (1) bottom side, be equipped with third valve (27) on outlet pipeline (13).
9. A method for preparing the phosphorus pentachloride continuous preparation device of any one of the claims 1 to 8, which is characterized in that: it comprises the following steps:
s1: the phosphorus trichloride liquid in the phosphorus trichloride feeding pipeline (2) is continuously sprayed downwards through an atomizing nozzle at the top of the reaction kettle (1);
s2: chlorine in the chlorine feeding pipeline (3) continuously enters the reaction kettle (1) from the bottom side of the reaction kettle (1), and then is mixed with the phosphorus trichloride liquid for reaction to obtain a solid phosphorus pentachloride material;
s3: phosphorus pentachloride material is deposited at the bottom of the reaction kettle (1), when a rotating motor (10) is started, the rotating motor drives a rotating shaft (4) to rotate, so that a spiral belt (5) rotates to extrude the phosphorus pentachloride material to form a compact isolation layer, and at the moment, chlorine introduced from a chlorine gas feeding pipeline (3) can not be discharged downwards from a discharge port at the bottom of the reaction kettle (1) due to the obstruction of the compact isolation layer of the phosphorus pentachloride material and can only upwards pass through the inside of the reaction kettle (1) and be mixed with phosphorus trichloride liquid for reaction;
s4: after the electric rotary valve (7) is opened, the phosphorus pentachloride material moves downwards under the rotating action of the spiral belt (5) and is continuously discharged downwards at a certain flow rate under the control of the electric rotary valve (7) to enter the spiral conveyor (11), at the moment, the dense isolation layer of the phosphorus pentachloride material at the bottom of the reaction kettle (1) is always kept at a certain thickness, the lower surface of the dense isolation layer of the phosphorus pentachloride material is continuously discharged from a discharge port at the bottom of the reaction kettle (1), and the upper surface of the dense isolation layer of the phosphorus pentachloride material always isolates the introduced chlorine gas to prevent the chlorine gas from being dissipated from the discharge port;
s5: the phosphorus pentachloride material entering the screw conveyor (11) is then sent into a spiral belt product tank (12), and then is packaged by a packaging machine and then is delivered out of a warehouse.
10. The method for preparing the continuous preparation device of phosphorus pentachloride as claimed in claim 9, which is characterized in that: the method also comprises a step of back flushing a filter (22) arranged at an air outlet at the top of the reaction kettle (1) by using a chlorine gas feeding pipeline (3):
s6: at regular intervals, a second valve (26) on the chlorine feeding pipeline (3) and a third valve (27) on the air outlet pipeline (13) are closed, a first valve (25) on the chlorine back-flushing pipeline (24) is opened, and at the moment, chlorine reversely passes through the filter (22) from the chlorine back-flushing pipeline (24) to carry out the back-flushing process on the chlorine.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202211013701.XA CN115382492A (en) | 2022-08-23 | 2022-08-23 | Continuous preparation device and preparation method of phosphorus pentachloride |
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| Application Number | Priority Date | Filing Date | Title |
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| CN202211013701.XA CN115382492A (en) | 2022-08-23 | 2022-08-23 | Continuous preparation device and preparation method of phosphorus pentachloride |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116237006A (en) * | 2023-03-30 | 2023-06-09 | 徐州宏达新能源科技有限公司 | Energy-saving production device and production method for high-purity phosphorus pentachloride |
| CN116492970A (en) * | 2023-06-25 | 2023-07-28 | 泰兴市申龙化工有限公司 | Phosphorus pentachloride processing device for continuous production |
-
2022
- 2022-08-23 CN CN202211013701.XA patent/CN115382492A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116237006A (en) * | 2023-03-30 | 2023-06-09 | 徐州宏达新能源科技有限公司 | Energy-saving production device and production method for high-purity phosphorus pentachloride |
| CN116492970A (en) * | 2023-06-25 | 2023-07-28 | 泰兴市申龙化工有限公司 | Phosphorus pentachloride processing device for continuous production |
| CN116492970B (en) * | 2023-06-25 | 2023-09-01 | 泰兴市申龙化工有限公司 | Phosphorus pentachloride processing device for continuous production |
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