A continuous phosphorus pentachloride preparation device

Abstract

The present invention belongs to the field of phosphorus pentachloride production, and specifically relates to a continuous phosphorus pentachloride preparation device, which includes a machine base and a housing assembly. The housing assembly includes a double-layer jacketed double-helix cylinder and a reaction port cylinder vertically fixed thereto. A hollow left helix assembly and a right helix assembly are provided inside the double-helix cylinder. The front ends of the two rotating main shafts are provided with heat transfer medium cavity inlets, and the rear ends are connected to solid transmission shafts. The top of the reaction port cylinder is provided with an upper end cover, and the upper end cover is provided with a phosphorus trichloride spray port and a chlorine inlet. A phosphorus trichloride spray nozzle is provided inside the reaction port cylinder. A phosphorus pentachloride discharge port is provided below the front end of the double-helix cylinder. The structure design of the fully enclosed, continuous reaction, crystallization, stirring, and pulverization integration completely changes the traditional production method of batch feeding and discharging and pouring and pulverizing. The material reaction is more sufficient, the discharge blockage is avoided, the leakage risk is reduced, the equipment has strong corrosion resistance, and the temperature and pressure regulation are more timely and accurate.

Description

Technical Field

[0001] The present invention belongs to the field of phosphorus pentachloride production, and particularly relates to a continuous phosphorus pentachloride preparation device. Background Art

[0002] Phosphorus pentachloride, as an important raw material for the production of lithium hexafluorophosphate, is generally prepared by injecting phosphorus trichloride into a reactor and carrying out a liquid-contact synthesis reaction with chlorine gas introduced into the reactor. During the reaction process, the temperature and pressure need to be strictly controlled, and stirring is also required. When no more solid substances are formed, the reaction is stopped to obtain solid phosphorus pentachloride; then the solid phosphorus pentachloride is loaded into a sublimation tank for vacuum sublimation, the sublimated gas is collected and cooled for recrystallization, and the crystals are crushed to obtain high-purity solid phosphorus pentachloride. Phosphorus pentachloride is easy to sublimate, and also has strong corrosiveness and strong irritation. The gas and dust generated during sublimation pose a serious threat to human health, can cause eye conjunctival irritation symptoms, irritate the throat to cause burning pain, aphonia or difficulty in swallowing, and can cause diseases such as bronchitis, pneumonia and pulmonary edema.

[0003] Traditional phosphorus pentachloride preparation is carried out in a sealed reaction kettle, and there are the following problems: 1. The batch production method is adopted, and the production raw materials and preparation products are fed or discharged in batches. The feeding and discharging operations are troublesome and the production efficiency is low; 2. Phosphorus pentachloride is easy to solidify and condense in the reaction kettle, forming hard large pieces, resulting in difficult discharging, easy corrosion and damage to the equipment, and affecting the service life of the equipment; 3. The reaction materials do not react sufficiently, and the reaction temperature and pressure are not controlled in a timely and accurate manner; 4. The phosphorus pentachloride crystals need to be crushed in batches and poured into the crushing device again. The pouring process is cumbersome and there is also a certain risk of leakage, and the operation is highly dangerous. Summary of the Invention

[0004] In view of the above situation, the present invention provides a continuous phosphorus pentachloride preparation device, which adopts a fully enclosed continuous production method of feeding, reacting, crystallizing, crushing and discharging, improving the production efficiency and safety of phosphorus pentachloride preparation.

[0005] In order to achieve the above object, the present invention adopts the following technical solutions:

[0006] A continuous phosphorus pentachloride preparation device comprises a machine base and a shell assembly fixedly installed above the machine base, wherein the shell assembly comprises a double-helix cylinder and a reaction port cylinder, wherein the reaction port cylinder is vertically fixedly connected to the upper rear part of the double-helix cylinder, wherein a left-helix assembly and a right-helix assembly are arranged in parallel along the length direction of the double-helix cylinder, wherein the double-helix cylinder is a double-layer jacket structure, wherein the interlayer of the double-helix cylinder is provided with an interlayer inlet and an interlayer outlet for introducing a heat-conducting medium, wherein the front and rear ends of the double-helix cylinder are respectively provided with a front cover and a rear cover, wherein both the two spiral assemblies are composed of a hollow rotating main shaft and a hollow spiral blade, wherein the cavity of the rotating main shaft and the cavity of the spiral blade corresponding thereto are communicated with each other, and the two spiral assemblies are connected to each other. The blades are staggered and interlocked, and the front ends of the two rotating main shafts are each provided with a cavity inlet for injecting a heat-conducting medium into the cavity, and the two cavity inlets are respectively connected with rotating joints, and the rear ends of the two rotating main shafts are each connected with a solid transmission shaft, and the two rotating main shafts are rotatably connected with the two end covers through mechanical seals respectively, and a driving motor is arranged behind the rear end cover, and the two transmission shafts are connected with the driving motor through a transmission assembly, and an upper end cover is arranged on the top of the reaction port cylinder, and the bottom of the reaction port cylinder is connected with the double helix cylinder, and a phosphorus trichloride spray port and a chlorine gas inlet are arranged on the upper end cover, and a spray nozzle connected with the phosphorus trichloride spray port is arranged in the reaction port cylinder, and a phosphorus pentachloride discharge port is arranged below the front end of the double helix cylinder.

[0007] Furthermore, the transmission assembly includes transmission gears respectively arranged at the rear ends of the two transmission shafts, the two transmission gears are meshed with each other, the motor shaft of the drive motor is connected to a reducer, one of the two rotating shafts is connected to the output shaft of the reducer through a coupling, and the coupling is an elastic pin coupling.

[0008] Furthermore, the reducer is a cycloidal pinwheel reducer, the bottom of the reducer is fixedly connected to the base, a protective cover is arranged around the transmission gear and the coupling, and the mechanical seal is a supported internal rotating mechanical seal.

[0009] Furthermore, the upper end cover is also provided with a replacement gas inlet and a spare interface, and the replacement gas is nitrogen. Before the reaction starts, nitrogen is introduced to completely replace and discharge the air inside the shell assembly, so that the phosphorus trichloride spray and chlorine gas undergo a liquid contact synthesis reaction under nitrogen protection conditions; after the reaction is completed, nitrogen is introduced to completely replace and discharge the residual reaction waste gas inside the shell assembly.

[0010] Furthermore, the double-helix cylinder is provided with an exhaust gas outlet, a first temperature measuring port, a pressure measuring port and a second temperature measuring port from front to back. The exhaust gas outlet is mainly used for discharging the gas inside the shell assembly during nitrogen replacement; the first temperature measuring port and the second temperature measuring port are respectively equipped with temperature sensors, which are respectively used to detect the reaction temperature at the rear reaction port cylinder and the discharge temperature at the front phosphorus pentachloride discharge port; the pressure measuring port is equipped with a pressure sensor to timely and accurately detect the reaction pressure inside the shell assembly online.

[0011] Further, the heat-conducting medium introduced into the interlayer of the double-helix cylinder and the cavities of the two rotating main shafts is heat-conducting oil. The heat-conducting oil mainly serves as a heat conduction medium. In a fixed-volume cavity, it does not need to flow and be updated quickly, and can also promote heat conduction and heat exchange through the uneven temperature of the heat-conducting oil at different parts. Generally, traditional reaction kettles only conduct heat exchange through the outer interlayer, while this device can conduct heat exchange on the material bidirectionally from the outer interlayer and the inner stirring, and can quickly and accurately control the temperature of the material in the container.

[0012] Further, the housing assembly, the left helix assembly, the right helix assembly, the front end cover, the rear end cover, and the upper end cover are all made of 316L stainless steel, ensuring that the surfaces of all parts in contact with the reaction material inside the device are smooth, have high hardness, strong corrosion resistance, and are not easily worn.

[0013] Further, the front end cover, the rear end cover, and the upper end cover all adopt a detachable connection method of flange connection. Flange gaskets are arranged in cooperation at each flange connection. The flange gaskets are all made of polytetrafluoroethylene, with good sealing performance and strong corrosion resistance.

[0014] The present invention also includes other components that enable its normal use, which are all conventional means in the art. In addition, for the devices or components not defined in the present invention, the existing technologies in the art are adopted.

[0015] The beneficial effects of the present invention are as follows:

[0016] A continuous phosphorus pentachloride preparation device provided by the present invention adopts a fully enclosed and continuous production concept. Through the integrated structural design of reaction, crystallization, stirring, and pulverization, it has completely changed the traditional production methods of batch feeding and discharging and pouring and pulverizing. The operation process is simpler, the work intensity is reduced, the production efficiency is improved, the leakage risk is reduced, the work safety is improved, the discharge blockage is avoided, the equipment failure is reduced, the equipment has better corrosion resistance and wear resistance, the service life of the equipment is prolonged, the reaction contact area of the material is increased, the reaction temperature and pressure can be regulated more timely and accurately, and the material reaction is more sufficient and thorough. BRIEF DESCRIPTION OF THE DRAWINGS

[0017] Figure 1 It is a front view structural schematic diagram of the continuous phosphorus pentachloride preparation device in the embodiment.

[0018] Figure 2 For Figure 1 It is a top view structural schematic diagram of the continuous phosphorus pentachloride preparation device in

[0019] Figure 3 For Figure 1 It is a side view structural schematic diagram of the continuous phosphorus pentachloride preparation device in

[0020] Figure 4 is Figure 1 the structural schematic diagram of the middle housing assembly.

[0021] Figure 5 is Figure 4 the sectional structural schematic diagram along the A-A direction in.

[0022] Figure 6 is Figure 4 the sectional structural schematic diagram along the B-B direction in.

[0023] Figure 7 is Figure 2 the structural schematic diagram of the right helical assembly in.

[0024] Figure 8 is Figure 7 the sectional structural schematic diagram along the C-C direction in. Specific embodiments

[0025] Next, the technical solutions of the present invention will be clearly and completely described in conjunction with specific embodiments. Obviously, the described embodiments are only part of the embodiments of the present invention, rather than all embodiments.

[0026] It should be noted that the orientation or positional relationship indicated by the terms "upper", "lower", "front", "rear", "left", "right", "inner", "outer", etc. is based on the drawings shown, only for the convenience of description.

[0027] Embodiment

[0028] Such as Figures 1-8As shown, a continuous phosphorus pentachloride preparation device comprises a machine base 1 and a shell assembly fixedly mounted above the machine base, wherein the shell assembly comprises a double helix cylinder 2 and a reaction port cylinder 3, wherein the reaction port cylinder is vertically fixedly connected to the upper rear portion of the double helix cylinder, wherein a left helix assembly 4 and a right helix assembly 5 are arranged in parallel along the length direction of the double helix cylinder, wherein the double helix cylinder is a double-layer jacket structure, wherein an interlayer inlet 6 and an interlayer outlet 7 for introducing a heat-conducting medium are arranged in the interlayer 31 of the double helix cylinder, wherein a front end cover 8 and a rear end cover 9 are arranged at the front and rear ends of the double helix cylinder respectively, wherein both the two helix assemblies are composed of a hollow rotating main shaft 10 and a hollow spiral blade 11, wherein the cavity of the rotating main shaft and the cavity of the spiral blade corresponding thereto are communicated with each other, and the two spiral assemblies are connected to each other. The blades are staggered and interlocked. The front ends of the two rotating main shafts are each provided with a cavity inlet 30 for injecting a heat-conducting medium into the cavity. The two cavity inlets are respectively connected with a rotating joint 12. The rear ends of the two rotating main shafts are each connected with a solid transmission shaft 13. The two rotating main shafts are rotatably connected to the two end covers through a mechanical seal 14 respectively. A driving motor 15 is arranged behind the rear end cover. The two transmission shafts are connected to the driving motor through a transmission assembly. An upper end cover 16 is arranged on the top of the reaction port cylinder. The bottom of the reaction port cylinder is connected with the double spiral cylinder. A phosphorus trichloride spray port and a chlorine gas inlet 18 are arranged on the upper end cover. A spray nozzle 17 connected with the phosphorus trichloride spray port is arranged in the reaction port cylinder. A phosphorus pentachloride discharge port 19 is arranged below the front end of the double spiral cylinder.

[0029] The transmission assembly includes transmission gears 20 respectively arranged at the rear ends of the two transmission shafts, the two transmission gears are meshed with each other, the motor shaft of the drive motor is connected to a reducer 21, and one of the two rotating shafts is connected to the output shaft of the reducer through a coupling 22, and the coupling is an elastic pin coupling.

[0030] The reducer is a cycloidal pinwheel reducer, the bottom of which is fixedly connected to the base, a protective cover 23 is arranged around the transmission gear and the coupling, and the mechanical seal is a supported internal rotating mechanical seal.

[0031] The upper end cover is also provided with a replacement gas inlet 24 and a spare interface, and the spare interface is provided with a flange plate 25. The replacement gas is nitrogen, which is relatively easy to obtain and has good economic efficiency.

[0032] 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 on the top of the double spiral cylinder from front to back.

[0033] The heat transfer medium introduced into the interlayer of the double helical cylinder and the cavity of the two rotating main shafts is heat transfer oil. The heat transfer oil can be circulated in the production line to recycle the heat energy of the heat transfer oil, with high heat transfer efficiency and good energy saving effect.

[0034] The housing assembly, left spiral assembly, right spiral assembly, front end cover, rear end cover, and upper end cover are all made of 316L stainless steel.

[0035] The front end cover, rear end cover, and upper end cover all adopt a detachable connection method of flange connection. Flange gaskets are provided at each flange connection, and the flange gaskets are all made of polytetrafluoroethylene.

[0036] The technical solution of the present invention is not limited to the limitations of the above specific embodiments. Many modifications and changes are obvious to those of ordinary skill in the art without departing from the scope and spirit of the described embodiments. Any technical deformation made within the spirit and principle of the present invention falls within the protection scope of the present invention.

Claims

1. A continuous phosphorus pentachloride preparation device, comprising a machine base and a housing assembly fixedly installed above the machine base, characterized in that: The housing assembly includes a double - helix cylinder and a reaction - port cylinder. The reaction - port cylinder is vertically and fixedly connected above the rear part of the double - helix cylinder. Inside the double - helix cylinder, a left - helix assembly and a right - helix assembly are arranged in parallel along its length direction. The double - helix cylinder has a structure with a sandwich layer. The sandwich layer of the double - helix cylinder is provided with a sandwich - layer inlet and a sandwich - layer outlet for introducing a heat - conducting medium. Above the double - helix cylinder, an exhaust - gas outlet, a first temperature - measuring port, a pressure - measuring port, and a second temperature - measuring port are arranged in sequence from front to back. Temperature sensors are respectively installed on the first temperature - measuring port and the second temperature - measuring port, and a pressure sensor is installed on the pressure - measuring port. The front and rear ends of the double - helix cylinder are respectively provided with a front end - cover and a rear end - cover. Both helix assemblies are composed of a hollow rotating main shaft and a hollow helical blade. The cavity of the rotating main shaft and the cavity of the corresponding helical blade communicate with each other. The two helical blades are staggered and engaged. At the front ends of the two rotating main shafts, cavity inlets for injecting a heat - conducting medium into the cavity are provided. Rotary joints are respectively connected to the two cavity inlets. At the rear ends of the two rotating main shafts, solid transmission shafts are connected. Each rotating main shaft is rotatably connected to the end - covers through mechanical seals. A driving motor is arranged behind the rear end - cover. The two transmission shafts are connected to 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 communicates with the double - helix cylinder. The upper end - cover is provided with a phosphorus trichloride spray port, a chlorine gas inlet, and a replacement - gas inlet. The replacement gas is nitrogen. A spray nozzle connected to the phosphorus trichloride spray port is arranged inside the reaction - port cylinder. A phosphorus pentachloride discharge port is arranged below the front end of the double - helix cylinder.

2. The continuous phosphorus pentachloride preparation device according to claim 1, characterized in that: The transmission assembly includes transmission gears respectively arranged at the rear ends of the two transmission shafts. The two transmission gears mesh with each other. The motor shaft of the driving motor is connected to a speed reducer. One of the two rotating shafts is connected to the output shaft of the speed reducer through a coupling.

3. A continuous phosphorus pentachloride preparation device according to claim 2, characterized in that: The bottom of the speed reducer is fixedly connected to the machine base. A protective cover is arranged outside the transmission gears and the coupling.

4. A continuous phosphorus pentachloride preparation device according to claim 1, characterized in that: The heat - conducting medium introduced into the sandwich layer of the double - helix cylinder and the cavities of the two rotating main shafts is heat - conducting oil.

5. A continuous phosphorus pentachloride preparation device according to claim 1, characterized in that: The housing assembly, the left - helix assembly, the right - helix assembly, and the front end - cover, rear end - cover, and upper end - cover are all made of 316L stainless steel.

6. The continuous phosphorus pentachloride preparation device according to claim 1, characterized in that: The front end - cover, rear end - cover, and upper end - cover all adopt a detachable connection method of flange connection. Flange gaskets are respectively arranged at each flange connection.

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