CN115025742B - Continuous phosphorus pentachloride preparation device - Google Patents
Continuous phosphorus pentachloride preparation device Download PDFInfo
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- CN115025742B CN115025742B CN202210743220.8A CN202210743220A CN115025742B CN 115025742 B CN115025742 B CN 115025742B CN 202210743220 A CN202210743220 A CN 202210743220A CN 115025742 B CN115025742 B CN 115025742B
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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
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F33/00—Other mixers; Mixing plants; Combinations of mixers
- B01F33/80—Mixing plants; Combinations of mixers
- B01F33/83—Mixing plants specially adapted for mixing in combination with disintegrating operations
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F33/00—Other mixers; Mixing plants; Combinations of mixers
- B01F33/80—Mixing plants; Combinations of mixers
- B01F33/836—Mixing plants; Combinations of mixers combining mixing with other treatments
- B01F33/8361—Mixing plants; Combinations of mixers combining mixing with other treatments with disintegrating
- B01F33/83612—Mixing plants; Combinations of mixers combining mixing with other treatments with disintegrating by crushing or breaking
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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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- Y—GENERAL 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
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Physical Or Chemical Processes And Apparatus (AREA)
Abstract
The invention belongs to the field of phosphorus pentachloride production, and particularly relates to a continuous phosphorus pentachloride preparation device which comprises a machine base and a shell assembly, wherein the shell assembly comprises a double-layer jacket structure double-screw cylinder body and a reaction port cylinder body vertically fixedly connected with the double-layer jacket structure double-screw cylinder body, a hollow left-screw assembly and a hollow right-screw assembly are arranged in the double-screw cylinder body, the front ends of two rotary main shafts are provided with heat conducting medium cavity inlets, the rear ends of the two rotary main shafts are connected with solid transmission shafts, the top of the reaction port cylinder body is provided with an upper end cover, a phosphorus trichloride spray port and a chlorine inlet are arranged on the upper end cover, a phosphorus trichloride spray nozzle is arranged in the reaction port cylinder body, and a phosphorus pentachloride discharge port is arranged below the front end of the double-screw cylinder body. The full-closed continuous reaction, crystallization, stirring and crushing integrated structural design is adopted, the traditional batch feeding, discharging and pouring crushing production mode is thoroughly changed, the material reaction is more complete, the discharging blockage is avoided, the leakage risk is reduced, the equipment corrosion resistance is strong, and the temperature and pressure regulation and control are more timely and accurate.
Description
Technical Field
The invention belongs to the field of phosphorus pentachloride production, and particularly relates to a continuous phosphorus pentachloride preparation device.
Background
Phosphorus pentachloride is used as an important production raw material of lithium hexafluorophosphate, and is generally prepared by injecting phosphorus trichloride into a reactor, carrying out a liquid contact synthesis reaction with chlorine introduced into the reactor, strictly controlling the temperature and the pressure in the reaction process, stirring, stopping the reaction when no solid matters are generated, and obtaining solid phosphorus pentachloride. Phosphorus pentachloride is easy to sublimate, has strong corrosiveness and strong irritation, and gas and smoke dust generated by sublimate have serious threat to human health, can cause eye conjunctiva irritation symptoms, can stimulate throat to cause burning pain, aphonia or dysphagia, and can cause diseases such as bronchitis, pneumonia, pulmonary edema and the like.
The traditional phosphorus pentachloride preparation is carried out in a sealed reaction kettle, and has the problems that 1, a batch production mode is adopted, production raw materials and preparation products are fed or discharged in batches, feeding and discharging operations are troublesome, production efficiency is low, 2, phosphorus pentachloride is easy to solidify and condense in the reaction kettle to form hard large blocks, discharging is difficult, equipment is easy to corrode and damage, the service life of the equipment is influenced, 3, reaction materials are insufficient in reaction, reaction temperature and pressure are not controlled timely and accurately, 4, phosphorus pentachloride crystals are crushed again, crystals are required to be poured into a crushing device in batches, the operation of the material pouring process is complex, a certain leakage risk exists, and the operation danger is high.
Disclosure of Invention
Aiming at the situation, the invention provides a continuous phosphorus pentachloride preparation device, which adopts the production modes of fully-closed continuous feeding, reaction, crystallization, crushing and discharging, thereby improving the production efficiency and safety of phosphorus pentachloride preparation.
In order to achieve the above purpose, the present invention adopts the following technical scheme:
The utility model provides a continuous phosphorus pentachloride preparation facilities, includes frame and fixed mounting in the casing assembly of frame top, the casing assembly includes double helix barrel and reaction mouth barrel, the perpendicular rigid coupling of reaction mouth barrel is in double helix barrel rear portion top, double helix barrel inside is provided with left helix assembly and right helix assembly along its length direction parallel arrangement, double helix barrel is double-deck jacket structure, double helix barrel's intermediate layer is provided with the intermediate layer entry and the intermediate layer export of leading-in heat-conducting medium, double helix barrel's front and back end is provided with front end housing and rear end cap respectively, two helix assemblies are by hollow rotatory main shaft and hollow helical blade constitution, and rotatory main shaft's cavity and rather than corresponding helical blade's cavity intercommunication each other, two helical blade crisscross interlock, two rotatory main shaft's front end all is provided with the cavity entry of pouring into heat-conducting medium into to the cavity, be connected with rotary joint on two cavity entry respectively, two rotatory main shaft's rear ends all are connected with solid transmission shaft through mechanical seal and two end caps rotatable coupling, the rear end cap is provided with driving motor, two transmission shafts are connected with driving motor transmission through drive assembly and reaction mouth top, the spout is provided with the top of the barrel, spout is provided with the phosphorus pentachloride, spout is connected with the top of the barrel, spout is provided with the top of the barrel is connected with the top of the barrel.
Further, the transmission assembly comprises transmission gears which are respectively arranged at the rear ends of the two transmission shafts, the two transmission gears are meshed with each other, a motor shaft of the driving motor is connected with a speed reducer, one of the two rotation shafts is connected with an output shaft of the speed reducer through a coupler, and the coupler is an elastic pin coupler.
Further, the speed reducer is a cycloidal pin gear speed reducer, the bottom of the speed reducer is fixedly connected with the machine base, a protective cover is arranged on the periphery of the transmission gear and the coupler, and the mechanical seal is an inner rotary mechanical seal with a support.
Further, a replacement gas inlet and a standby interface are also arranged on the upper end cover, the replacement gas is nitrogen, and before the reaction starts, the nitrogen is introduced to completely replace and discharge the air in the shell assembly, so that the phosphorus trichloride spray and the chlorine carry out liquid contact synthesis reaction under the protection of the nitrogen; after the reaction is finished, introducing nitrogen to replace and discharge all the residual reaction waste gas in the shell assembly.
Further, an exhaust gas outlet, a first temperature measuring port, a pressure measuring port and a second temperature measuring port are sequentially arranged above the double-spiral cylinder body from front to back. The waste gas outlet is mainly used for discharging gas in the shell assembly during nitrogen replacement, the first temperature measuring port and the second temperature measuring port are respectively provided with temperature sensors for detecting the reaction temperature of the barrel body of the rear reaction port and the discharge temperature of the discharge port of the front phosphorus pentachloride, and the pressure measuring port is provided with a pressure sensor for timely and accurately detecting the reaction pressure in the shell assembly on line.
Further, heat conducting media introduced into the interlayer of the double-spiral cylinder and the cavities of the two rotary spindles are heat conducting oil. The heat conducting oil is mainly used as a heat conducting medium, quick flow update is not needed in the fixed volume cavity, and heat conduction and heat exchange can be promoted to be completed through uneven heat conducting oil heating and cooling of different parts. The traditional reaction kettle generally only has an outer interlayer for heat exchange, but the device can exchange heat for materials in two directions through the outer interlayer and the inner stirring, and can rapidly and accurately control the temperature of the materials in the container.
Further, the shell assembly, the left screw assembly, the right screw assembly, the front end cover, the rear end cover and the upper end cover are all made of 316L stainless steel, so that the surfaces of all parts, which are in contact with the reaction materials, inside the device are smooth, high in hardness, strong in corrosion resistance and difficult to wear.
Further, the front end cover, the rear end cover and the upper end cover are all in a detachable connection mode of flange connection, the flange sealing gaskets are arranged at the positions of the flange connection in a matched mode, and the flange sealing gaskets are made of polytetrafluoroethylene, so that the sealing performance is good, and the corrosion resistance is strong.
The invention also includes other components that enable normal use thereof, all as is conventional in the art, and in addition, the devices or components not defined in the invention are all well known in the art.
The beneficial effects of the invention are as follows:
The continuous phosphorus pentachloride preparation device provided by the invention adopts a fully-closed and continuous production concept, and thoroughly changes the traditional production mode of batch feeding, discharging and material pouring and crushing through the structural design of integration of reaction, crystallization, stirring and crushing, so that the operation flow is simpler, the working strength is reduced, the production efficiency is improved, the leakage risk is reduced, the working safety is improved, the discharging blockage is avoided, the equipment failure is reduced, the corrosion resistance and the wear resistance of the equipment are better, the service life of the equipment is prolonged, the material reaction contact area is improved, the reaction temperature and the pressure are regulated more timely and more accurately, and the material reaction is more complete and thorough.
Drawings
FIG. 1 is a schematic diagram showing the front view of the apparatus for producing phosphorus pentachloride in the example.
Fig. 2 is a schematic top view of the continuous phosphorus pentachloride production apparatus of fig. 1.
Fig. 3 is a schematic side view of the continuous phosphorus pentachloride production apparatus of fig. 1.
Fig. 4 is a schematic structural view of the housing assembly of fig. 1.
Fig. 5 is a schematic cross-sectional view of fig. 4 along A-A.
Fig. 6 is a schematic cross-sectional view of fig. 4 along the direction B-B.
Fig. 7 is a schematic view of the right screw assembly of fig. 2.
Fig. 8 is a schematic cross-sectional view of fig. 7 along the direction C-C.
Detailed Description
The technical solutions of the present invention will be clearly and completely described below in connection with specific embodiments, and it is obvious that the described embodiments are only some embodiments of the present invention, not all embodiments.
The terms "upper", "lower", "front", "rear", "left", "right", "inner", "outer", and the like refer to the directions or positional relationships shown in the drawings, and are merely for convenience of description.
Examples
As shown in fig. 1-8, a continuous phosphorus pentachloride preparation device comprises a machine base 1 and a shell assembly fixedly arranged above the machine base, wherein the shell assembly comprises a double-screw cylinder 2 and a reaction port cylinder 3, the reaction port cylinder is vertically and fixedly connected above the rear part of the double-screw cylinder, a left screw assembly 4 and a right screw assembly 5 are arranged in the double-screw cylinder in parallel along the length direction of the double-screw cylinder, the double-screw cylinder is of a double-layer jacket structure, an interlayer 31 of the double-screw cylinder is provided with an interlayer inlet 6 and an interlayer outlet 7 which are communicated with heat conducting media, the front end and the rear end of the double-screw cylinder are respectively provided with a front end cover 8 and a rear end cover 9, the two screw assemblies are respectively formed by hollow rotary spindles 10 and hollow screw blades 11, cavities of the rotary spindles are mutually communicated with cavities of the corresponding screw blades, the front ends of the two rotary spindles are respectively provided with a cavity inlet 30 for injecting heat conducting media into the cavities, the two cavity inlets are respectively connected with rotary joints 12, the rear ends of the two rotary spindles are respectively connected with a solid transmission shaft 13, the two rotary spindles are respectively correspondingly connected with a mechanical seal 14 and can be rotatably connected with two end covers, the two rotary spindles are respectively provided with a back end cover 15, the spray nozzle is connected with a spray nozzle 18, the spray nozzle is arranged on the spray nozzle is connected with the bottom of the spray nozzle, the spray nozzle is arranged on the spray nozzle, the spray nozzle is connected with the spray nozzle is provided with the bottom a spray nozzle, and the spray nozzle is provided with a spray nozzle is connected with a top with a spray nozzle with a top, and the spray nozzle 18, and the spray nozzle is connected with the spray nozzle.
The transmission assembly comprises transmission gears 20 which are respectively arranged at the rear ends of two transmission shafts, the two transmission gears are meshed with each other, a motor shaft of the driving motor is connected with a speed reducer 21, one of the two rotation shafts is connected with an output shaft of the speed reducer through a coupler 22, and the coupler is an elastic pin coupler.
The speed reducer is a cycloidal pin gear speed reducer, the bottom of the speed reducer is fixedly connected with the machine base, a protective cover 23 is arranged on the periphery of the transmission gear and the coupler, and the mechanical seal is an internal rotary mechanical seal with a support.
The upper end cover is also provided with a replacement gas inlet 24 and a standby interface, the standby interface is provided with a flange blank 25, and the replacement gas is obtained easily by adopting nitrogen, so that the economy is good.
An exhaust gas outlet 26, a first temperature measuring port 27, a pressure measuring port 28 and a second temperature measuring port 29 are sequentially arranged above the double-spiral cylinder body from front to back.
The interlayer of the double-spiral cylinder body and the heat conducting medium introduced into the cavities of the two rotary spindles are heat conducting oil. The heat conduction oil can be recycled by utilizing the production line, so that the heat energy of the heat conduction oil is recycled, the heat transfer efficiency is high, and the energy-saving effect is good.
The shell assembly, the left screw assembly, the right screw assembly, the front end cover, the rear end cover and the upper end cover are all made of 316L stainless steel.
The front end cover, the rear end cover and the upper end cover are all in a detachable connection mode of flange connection, flange sealing gaskets are arranged at all the flange connection positions in a matched mode, and the flange sealing gaskets are made of polytetrafluoroethylene.
The technical solution of the present invention is not limited to the above-described specific embodiments, and many modifications and variations will be apparent to those skilled in the art without departing from the scope and spirit of the described embodiments, and any technical modifications made within the spirit and principles of the present invention fall within the scope of the present invention.
Claims (6)
1. The continuous phosphorus pentachloride preparation device comprises a machine base and a shell assembly fixedly arranged above the machine base, and is characterized in that the shell assembly comprises a double-screw cylinder body and a reaction port cylinder body, the reaction port cylinder body is vertically and fixedly connected above the rear part of the double-screw cylinder body, a left screw assembly and a right screw assembly are arranged in the double-screw cylinder body in parallel along the length direction of the double-screw cylinder body, the double-screw cylinder body is of a sandwich structure, and a sandwich inlet and a sandwich outlet which are communicated with a heat conducting medium are arranged in the sandwich of the double-screw cylinder body;
The device comprises a double-spiral cylinder body, a waste gas outlet, a first temperature measuring port, a pressure measuring port and a second temperature measuring port, wherein the waste gas outlet, the first temperature measuring port, the pressure measuring port and the second temperature measuring port are sequentially arranged above the double-spiral cylinder body from front to back;
The front end and the rear end of the double-screw cylinder body are respectively provided with a front end cover and a rear end cover, the two screw assemblies are composed of hollow rotating main shafts and hollow screw blades, the cavities of the rotating main shafts are communicated with the cavities of the corresponding screw blades, the two screw blades are engaged in a staggered way, the front ends of the two rotating main shafts are respectively provided with a cavity inlet for injecting heat-conducting medium into the cavities, and the two cavity inlets are respectively connected with a rotary joint;
The rear ends of the two rotary spindles are connected with solid transmission shafts, the two rotary spindles are respectively and rotatably connected with the two end covers through mechanical seals, a driving motor is arranged behind the rear end cover, the two transmission shafts are in transmission connection with the driving motor through a transmission assembly, an upper end cover is arranged at the top of the reaction port cylinder, and the bottom of the reaction port cylinder is communicated with the double-spiral cylinder;
The upper end cover is provided with a phosphorus trichloride spray opening, a chlorine inlet and a replacement gas inlet, the replacement gas adopts nitrogen, a spray nozzle connected with the phosphorus trichloride spray opening is arranged in the reaction port cylinder, and a phosphorus pentachloride discharge port is arranged below the front end of the double-spiral cylinder.
2. The device for preparing continuous phosphorus pentachloride according to claim 1, wherein the transmission assembly comprises transmission gears respectively arranged at the rear ends of two transmission shafts, the two transmission gears are meshed with each other, a motor shaft of the driving motor is connected with a speed reducer, and one of the two rotation shafts is connected with an output shaft of the speed reducer through a coupler.
3. The device for preparing continuous phosphorus pentachloride according to claim 2, wherein the bottom of the speed reducer is fixedly connected with the machine base, and a protective cover is arranged on the periphery of the transmission gear and the coupling.
4. The continuous phosphorus pentachloride preparing device according to claim 1, wherein heat conducting media introduced into the interlayer of the double-screw cylinder and the cavities of the two rotary spindles are heat conducting oil.
5. The device for preparing continuous phosphorus pentachloride according to claim 1, wherein the shell assembly, the left screw assembly, the right screw assembly, the front end cover, the rear end cover and the upper end cover are all made of 316L stainless steel.
6. The device for preparing continuous phosphorus pentachloride according to claim 1, wherein the front end cover, the rear end cover and the upper end cover are all detachably connected in a flange connection mode, and flange sealing gaskets are arranged at all flange connection positions in a matched mode.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210743220.8A CN115025742B (en) | 2022-06-28 | 2022-06-28 | Continuous phosphorus pentachloride preparation device |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210743220.8A CN115025742B (en) | 2022-06-28 | 2022-06-28 | Continuous phosphorus pentachloride preparation device |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN115025742A CN115025742A (en) | 2022-09-09 |
| CN115025742B true CN115025742B (en) | 2025-07-08 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN202210743220.8A Active CN115025742B (en) | 2022-06-28 | 2022-06-28 | Continuous phosphorus pentachloride preparation device |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102091551A (en) * | 2004-09-28 | 2011-06-15 | 巴斯夫欧洲公司 | Kneader mixer and method for the production of poly(meth)acrylates using said kneader mixer |
| CN103420349A (en) * | 2012-05-21 | 2013-12-04 | 何猛 | Production method of phosphorus pentachloride |
| WO2017043232A1 (en) * | 2015-09-07 | 2017-03-16 | 水ｉｎｇ株式会社 | Dehydration device, dehydration system, and dehydration method |
| CN112374059A (en) * | 2020-11-30 | 2021-02-19 | 北京鑫泽清源植物秸杆技术有限公司 | Energy-saving environment-friendly double-screw unit |
| CN217450184U (en) * | 2022-06-28 | 2022-09-20 | 焦作市合鑫机械有限公司 | Continuous phosphorus pentachloride preparation facilities |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN209501689U (en) * | 2018-12-20 | 2019-10-18 | 南通利奥化工科技有限公司 | A kind of chlorination tank convenient for discharging |
| CN112919439B (en) * | 2021-03-10 | 2023-03-21 | 焦作多氟多实业集团有限公司 | Method and device for continuously preparing high-purity phosphorus pentachloride |
-
2022
- 2022-06-28 CN CN202210743220.8A patent/CN115025742B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102091551A (en) * | 2004-09-28 | 2011-06-15 | 巴斯夫欧洲公司 | Kneader mixer and method for the production of poly(meth)acrylates using said kneader mixer |
| CN103420349A (en) * | 2012-05-21 | 2013-12-04 | 何猛 | Production method of phosphorus pentachloride |
| WO2017043232A1 (en) * | 2015-09-07 | 2017-03-16 | 水ｉｎｇ株式会社 | Dehydration device, dehydration system, and dehydration method |
| CN112374059A (en) * | 2020-11-30 | 2021-02-19 | 北京鑫泽清源植物秸杆技术有限公司 | Energy-saving environment-friendly double-screw unit |
| CN217450184U (en) * | 2022-06-28 | 2022-09-20 | 焦作市合鑫机械有限公司 | Continuous phosphorus pentachloride preparation facilities |
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| CN115025742A (en) | 2022-09-09 |
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