Phosphine preparation system, preparation method, equipment and medium
By designing a phosphine preparation system and utilizing real-time monitoring data and intelligent control technology, the problems of low intelligence and unstable purity in phosphine preparation were solved, achieving efficient and stable phosphine preparation and reducing by-products, thereby lowering labor costs and operational errors.
Patent Information
- Application Number
- CN202511078655.5
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-08-01
- Publication Date
- 2025-10-31
AI Technical Summary
The current industrial production of phosphine is characterized by low levels of automation, low reaction efficiency, low purity, and instability, failing to meet the high-quality material requirements of specific industrial sectors.
A phosphine preparation system was designed, including a controller, a reaction unit, a dehydration unit, a gas collection and compression unit, a purification unit, and a post-processing unit. By dynamically adjusting the reaction parameters through real-time monitoring data, the entire process can be intelligently controlled, improving reaction efficiency and removing impurities to obtain high-purity and stable phosphine.
The system achieves efficient preparation of phosphine with high purity and stability, reduces byproducts, lowers labor costs and operational errors, and can operate stably without human intervention, with a response speed improved to the second level.
Smart Images
Figure CN120860947A_ABST
Abstract
Description
Technical Field
[0001] This application relates to the field of industrial production control technology, and more specifically, to a phosphine preparation system, preparation method, equipment, and medium. Background Technology
[0002] Phosphine, as an important chemical raw material, is widely used in semiconductor doping, organic synthesis, and food fumigation. Currently, the industrial production of phosphine suffers from low levels of automation, low reaction efficiency, and excessive byproducts. Furthermore, the purity and quality of the obtained phosphine are not high, failing to meet the demands of specific industrial sectors for high-quality materials. Summary of the Invention
[0003] The purpose of this application is to provide a phosphine preparation system, preparation method, equipment and medium to solve the above-mentioned problems existing in the prior art, to intelligently control the phosphine preparation process and improve reaction efficiency, and to obtain phosphine with high purity and stable quality.
[0004] In a first aspect, a phosphine preparation system is provided, comprising a controller, a reaction unit, a dehydration unit, a gas collection and compression unit, a purification unit, and a post-treatment unit; the controller is connected to the reaction unit, the dehydration unit, the gas collection and compression unit, the purification unit, and the post-treatment unit respectively; a first inlet of the reaction unit is connected to a first outlet of the dehydration unit; a first outlet of the reaction unit is connected to the inlet of the dehydration unit; a second outlet of the dehydration unit is connected to the inlet of the gas collection and compression unit; a first outlet of the gas collection and compression unit is connected to a first inlet of the purification unit; and a second outlet of the gas collection and compression unit and a first outlet of the purification unit are respectively connected to the first inlet and the second inlet of the post-treatment unit. The controller is used to generate control parameters for each unit based on the real-time monitoring data of different units, and to send the corresponding control parameters to the corresponding units. The reaction unit is used to control the reaction of different materials to generate crude phosphine according to corresponding control parameters; The dehydration unit is used to remove water from crude phosphine according to corresponding control parameters to obtain dehydrated phosphine. The gas collection and compression unit is used to temporarily store dehydrated phosphine according to the corresponding control parameters. The refining unit is used to remove impurities from the dehydrated phosphine according to the corresponding control parameters to obtain the target phosphine. The post-processing unit is used to process the target phosphine and intermediate products obtained in the phosphine production process according to corresponding control parameters.
[0005] In an optional implementation, the system further includes: a liquid yellow phosphorus inlet, a lime slurry suspension inlet, a sodium hydroxide solution inlet, and a pretreatment unit; the first, second, and third inlets of the pretreatment unit are respectively connected to the liquid yellow phosphorus inlet, the lime slurry suspension inlet, and the sodium hydroxide solution inlet; the first, second, and third outlets of the pretreatment unit are respectively connected to the second, third, and fourth inlets of the reaction unit. The pretreatment unit is used to pretreat liquid yellow phosphorus, lime milk suspension and sodium hydroxide solution respectively; The reaction unit is specifically used to react pretreated liquid yellow phosphorus, lime milk suspension and sodium hydroxide solution to generate crude phosphine.
[0006] In an optional implementation, the pretreatment unit includes: an atomizing component, a homogenizing component, and a preheating component; wherein, the inlet of the atomizing component is the first inlet of the pretreatment unit; the inlet of the homogenizing component is the second inlet of the pretreatment unit; the inlet of the preheating component is the third inlet of the pretreatment unit; the outlet of the atomizing component is the first outlet of the pretreatment unit; the outlet of the homogenizing component is the second outlet of the pretreatment unit; and the outlet of the preheating component is the third outlet of the pretreatment unit. Atomizing component for continuously atomizing liquid yellow phosphorus according to configured atomizing parameters; A homogenizing component is used to homogenize a lime slurry suspension according to configured homogenizing parameters; A preheating component is used to preheat the sodium hydroxide solution to a first preset temperature.
[0007] In an optional implementation, the post-processing unit includes: a filling unit, a spraying unit, an exhaust gas treatment unit, and a tailings salt unit; The first inlet of the spray unit is the first inlet of the post-treatment unit; the second inlet of the spray unit is the second inlet of the post-treatment unit; the second outlet of the refining unit is connected to the inlet of the filling unit; the second inlet of the refining unit is connected to the outlet of the filling unit; the first outlet of the spray unit is connected to the inlet of the exhaust gas treatment unit; the second outlet of the spray unit is connected to the third inlet of the tailings salt unit; the first outlet of the exhaust gas treatment unit is connected to the first inlet of the tailings salt unit; the second outlet of the exhaust gas treatment unit is used to discharge the exhaust gas to be emitted into the atmosphere. The second outlet of the reaction unit is connected to the second inlet of the tailings unit.
[0008] In an optional implementation, the reaction unit is further configured to: transport the salt solution generated by the reaction to the tailings unit; The filling unit is used to compress and store the target phosphine into a phosphine container; The spraying unit is used to treat the phosphine tail gas emitted from the refining unit and the gas collection and compression unit to obtain tail gas to be treated and an oxidized salt solution; and to transport the tail gas to be treated to the tail gas treatment unit and the oxidized salt solution to the tail salt unit. The exhaust gas treatment unit is used to decompose and oxidize the exhaust gas to be treated, and absorb it with an alkaline solution to obtain a salt solution; and to transport the salt solution to the tail salt unit. The tailings unit is used to process the oxidized salt solution delivered by the reaction unit, the spray unit, and the tail gas treatment unit to obtain reaction byproducts.
[0009] In an optional implementation, the water removal unit includes: a separation component, a first adsorption tower, a second adsorption tower, and a three-stage membrane permeate dewatering device; the inlet of the separation component is the inlet of the water removal unit; the outlet of the separation component is connected to the inlet of the first adsorption tower; the outlet of the first adsorption tower is connected to the inlet of the second adsorption tower; the outlet of the second adsorption tower is connected to the inlet of the three-stage membrane permeate dewatering device; and the outlet of the three-stage membrane permeate dewatering device is the inlet of the water removal unit. The separation component is used to separate crude phosphine to obtain first phosphine; The first adsorption tower is used to perform initial water removal on the first phosphine to obtain the second phosphine. The second adsorption tower is used to perform secondary dehydration on the second phosphine to obtain the third phosphine; The three-stage membrane permeate dewatering device is used to perform deep dewatering of the third phosphine to obtain dewatered phosphine.
[0010] In an optional implementation, the tailings unit includes: a first filtration device, a drying device, a second filtration device, a calcium removal reactor, a sulfur removal reactor, and a filtrate intermediate tank. The first filtration device is used to filter the salt solution to obtain filtrate and filter cake; The drying device is used to dry the filter cake to obtain a mixed byproduct of calcium carbonate and calcium phosphite; The second filtration device is used to filter the filtrate to obtain a primary purified liquid; The calcium removal reactor is used to add sodium carbonate solution to the primary purification liquid to obtain calcium carbonate precipitate and secondary purification liquid; The desulfurization reactor is used to oxidize the secondary purified filtrate with compressed air to obtain the tertiary purified filtrate after removing sulfur ions. The intermediate filtrate tank is used to heat and concentrate sodium hypophosphite crystals in the tertiary purified liquid.
[0011] Secondly, a method for preparing phosphine is provided, applied in a controller of a phosphine preparation system. The system further includes: a reaction unit, a dehydration unit, a gas collection and compression unit, a purification unit, and a post-treatment unit. The controller is connected to the reaction unit, the dehydration unit, the gas collection and compression unit, the purification unit, and the post-treatment unit, respectively. A first inlet of the reaction unit is connected to a first outlet of the dehydration unit. The first outlet of the reaction unit is connected to the inlet of the dehydration unit. A second outlet of the dehydration unit is connected to the inlet of the gas collection and compression unit. The first outlet of the gas collection and compression unit is connected to the first inlet of the purification unit. The second outlet of the gas collection and compression unit and the first outlet of the purification unit are respectively connected to the first inlet and the second inlet of the post-treatment unit. The method may include: Based on the real-time monitoring data of different units, control parameters for each unit are generated. The corresponding control parameters are sent to the corresponding units to control the reaction unit to react different materials to generate crude phosphine according to the corresponding control parameters, to control the dehydration unit to remove water from the crude phosphine to obtain dehydrated phosphine according to the corresponding control parameters, to control the gas collection and compression unit to temporarily store the dehydrated phosphine according to the corresponding control parameters, to control the refining unit to remove impurities from the dehydrated phosphine to obtain the target phosphine according to the corresponding control parameters, and to control the post-processing unit to process the target phosphine and the intermediate products obtained in the phosphine production process according to the corresponding control parameters.
[0012] Thirdly, an electronic device is provided, which includes a processor, a communication interface, a memory, and a communication bus, wherein the processor, the communication interface, and the memory communicate with each other through the communication bus; Memory, used to store computer programs; When a processor executes a program stored in memory, it implements the method steps in the second aspect described above.
[0013] Fourthly, a computer-readable storage medium is provided, wherein a computer program is stored therein, and when executed by a processor, the computer program implements the method steps of the second aspect described above.
[0014] This application dynamically adjusts reaction parameters based on real-time monitoring data from each unit, minimizing fluctuations in the target phosphine purity, improving reaction efficiency, and reducing byproducts. Through global collaborative control, it avoids over-processing, resulting in high-purity and stable phosphine. It achieves full-process intelligence: replacing traditional manual intervention, the system can operate stably without human intervention by calculating and distributing unit parameters in real time through the controller. The response speed is improved to the second level (for sudden disturbances, such as fluctuations in feed flow), significantly reducing labor costs and operational errors. Attached Figure Description
[0015] To more clearly illustrate the technical solutions of the embodiments of this application, the accompanying drawings used in the embodiments of this application will be briefly introduced below. It should be understood that the following drawings only show some embodiments of this application and should not be regarded as a limitation of the scope. For those skilled in the art, other related drawings can be obtained based on these drawings without creative effort.
[0016] Figure 1 A schematic diagram of the architecture of a phosphine preparation system provided in an embodiment of this application; Figure 2 A schematic flowchart illustrating a method for preparing phosphine provided in this application embodiment; Figure 3 A schematic diagram of a phosphine preparation apparatus provided in an embodiment of this application; Figure 4 This is a schematic diagram of the structure of an electronic device provided in an embodiment of this application. Detailed Implementation
[0017] The technical solutions of the embodiments of this application will be clearly and completely described below with reference to the accompanying drawings. Obviously, the described embodiments are only a part of the embodiments of this application, and not all of the embodiments. Based on the embodiments of this application, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of this application. Unless otherwise defined, the technical or scientific terms used in this application should have the ordinary meaning understood by those skilled in the art. The words "first," "second," and similar terms used in this application do not indicate any order, quantity, or importance, but are only used to distinguish different components. The words "comprising" or "including," etc., mean that the element or object preceding the word covers the element or object listed after the word and its equivalents, but do not exclude other elements or objects. The words "connected," "coupled," or "connected," etc., are not limited to physical or mechanical connections, but can include electrical connections, whether direct or indirect. "Up," "down," "left," "right," etc., are only used to indicate relative positional relationships. When the absolute position of the described object changes, the relative positional relationship may also change accordingly.
[0018] The method for preparing phosphine provided in this application embodiment can be applied to... Figure 1 In the system architecture shown, such as Figure 1 As shown, the system may include: a controller, a reaction unit, a dehydration unit, a gas collection and compression unit, a purification unit, and a post-treatment unit; the controller is connected to the reaction unit, the dehydration unit, the gas collection and compression unit, the purification unit, and the post-treatment unit respectively; the first inlet of the reaction unit is connected to the first outlet of the dehydration unit; the first outlet of the reaction unit is connected to the inlet of the dehydration unit; the second outlet of the dehydration unit is connected to the first inlet of the gas collection and compression unit, and the third outlet of the dehydration unit is connected to the second inlet of the gas collection and compression unit; the first outlet of the gas collection and compression unit is connected to the first inlet of the purification unit; the second outlet of the gas collection and compression unit and the first outlet of the purification unit are respectively connected to the first inlet and the second inlet of the post-treatment unit. The controller is used to control the reaction unit, dehydration unit, gas collection and compression unit, purification unit and post-treatment unit to perform corresponding processes according to different configured control parameters; The reaction unit comprises multiple reactors connected in parallel. Each reactor is a vertical, continuous-flow rotating packed bed reactor, constructed primarily of duplex stainless steel. It has an overall height of 6.5 meters, a diameter of 1.8 meters, an effective reaction volume of 8 cubic meters, a design working pressure of 3.5 MPa, and a working temperature range of 50-120℃. The reactor is externally equipped with a jacketed heat exchange assembly and an explosion-proof safety protection layer. The reactor features a bottom swirling flow and a central baffle mixing structure to achieve efficient mixing of materials in turbulent conditions. A variable frequency drive is connected to the central shaft of the reactor. This reactor is used to react various materials to produce crude phosphine, including liquid yellow phosphorus, lime slurry suspension, and sodium hydroxide solution. The dehydration unit includes a separation component, a first adsorption tower, a second adsorption tower, and a three-stage membrane permeate dehydrator. The separation component separates liquid alkaline droplets and yellow phosphorus microparticles from crude phosphine to obtain the first phosphine. The first phosphine is then heated using an electric heating sleeve and transported to the first adsorption tower. The first adsorption tower is internally filled with three layers of mesoporous silica-based adsorbent, with porous sieve plates between the layers, for primary dehydration of the first phosphine to obtain the second phosphine. The second adsorption tower is filled with 3A molecular sieves for secondary dehydration of the second phosphine to obtain the third phosphine. The three-stage membrane permeate dehydrator uses a polyimide hollow fiber membrane module for deep dehydration of the third phosphine to obtain dehydrated phosphine. A compressed air collection unit includes a collection component and a compression component. The collection component comprises a first buffer tank, a second buffer tank, an automatic pressure regulation component, and a temperature regulation component. The inlets of the first and second buffer tanks are the inlets of the compressed air collection unit. The first outlets of the first and second buffer tanks are connected to the inlet of the compression component. The first outlet of the compression component is the first outlet of the compressed air collection unit. The second outlets of the first and second buffer tanks and the second outlet of the compression component are the second outlets of the compressed air collection unit. The first and second buffer tanks are made of stainless steel. The interior of the first and second buffer tanks... The system maintains a slight positive pressure; a first buffer tank is used to temporarily store the dehydrated phosphine gas; a second buffer tank serves as a backup, used to temporarily store the dehydrated phosphine gas when the first buffer tank fails; an automatic pressure regulating component is used to regulate the pressure of the first and second buffer tanks respectively; a temperature regulating component is used to regulate the temperature of the first and second buffer tanks respectively; the compression component may include: a cyclone separator, an explosion-proof screw compressor, and a cooling component; the cyclone separator is located at the inlet of the compression component and is used to separate droplets with a particle size of not less than 5μm; the cooling component is located at the first outlet of the compression component and is used to cool the dehydrated phosphine. The refining unit includes: a deweighting tower, a multi-stage adsorption assembly, and a cryogenic distillation unit; wherein, the feed inlet of the deweighting tower is the first feed inlet of the refining unit; the discharge outlet of the deweighting tower is connected to the feed inlet of the multi-stage adsorption assembly; the discharge outlet of the multi-stage adsorption assembly is connected to the feed inlet of the cryogenic distillation unit; the feed inlet of the cryogenic distillation unit is the first discharge outlet of the refining unit; the deweighting tower is used to separate the heavy components in the cooled dehydrated phosphine to obtain deweighted phosphine, wherein the heavy components have a boiling point higher than that of phosphine; the multi-stage adsorption assembly is used to deeply remove trace amounts of low-boiling-point or... The process involves removing polar impurities to obtain purified phosphine; a cryogenic distillation unit is used to finely separate the purified phosphine by utilizing the boiling point differences of different substances under low-temperature conditions, obtaining the target phosphine; the multi-stage adsorption components include: a modified ZSM-5 molecular sieve adsorption tower, used to remove acidic sulfide impurities such as hydrogen sulfide from the deweighted phosphine; a metal-organic framework material adsorption tower for precise adsorption of organophosphorus compounds, the metal-organic framework material being HKUST-1; and a hydroxyapatite nanofiber adsorption tower employing a fixed bed and pulse backwashing structure for deep removal of alkaline gas impurities. The post-treatment unit is used to process the target phosphine and intermediate products obtained during the phosphine production process. Specifically, the post-treatment unit includes: a filling unit, a spraying unit, a tail gas treatment unit, and a tailings unit. The first inlet of the spraying unit is the first inlet of the post-treatment unit; the second inlet of the spraying unit is the second inlet of the post-treatment unit; the first outlet of the spraying unit is connected to the inlet of the tail gas treatment unit; the first outlet of the tail gas treatment unit is connected to the first inlet of the tailings unit; the second outlet of the spraying unit is connected to the third inlet of the tailings unit; the second outlet of the refining unit is connected to the inlet of the filling unit; the second inlet of the refining unit is connected to the outlet of the filling unit; the second outlet of the reaction unit is connected to the second inlet of the tailings unit; and the second outlet of the tail gas treatment unit is used to discharge the tail gas to be emitted into the atmosphere. A filling unit is used to compress and store the target phosphine into phosphine containers; the phosphine containers are multiple stainless steel high-pressure storage tanks stored in a liquid nitrogen pool; each stainless steel high-pressure storage tank corresponds to a storage number and volume; The spray unit is used to treat the phosphine tail gas emitted from the refining unit and the gas collection and compression unit to obtain tail gas to be treated and an oxidized salt solution; and to transport the tail gas to be treated to the tail gas treatment unit and the oxidized salt solution to the tail salt unit; the spray unit adopts a multi-stage spray tower structure, including: a low-temperature plasma oxidation component, a hydroxyl radical advanced oxidation component, and a circulating spray device. The low-temperature plasma oxidation component is used to decompose unreacted yellow phosphorus vapor; the hydroxyl radical advanced oxidation component is used to generate hydroxyl radicals by exciting hydrogen peroxide with 185-254nm ultraviolet light; the circulating spray device is used to achieve chemical absorption of phosphine using a 10% sodium hydroxide solution as an absorbent; The exhaust gas treatment unit includes a photocatalytic oxidation device or a plasma decomposition device and a spray assembly. The photocatalytic oxidation device or plasma decomposition device is used to decompose and oxidize the exhaust gas to be treated to obtain exhaust gas to be emitted. The spray assembly is used to absorb the exhaust gas to be emitted with an alkaline solution to obtain a salt solution. The salt solution is then transported to the tail salt unit to discharge the exhaust gas to be emitted that has not been absorbed by the alkaline solution into the atmosphere. The tailings unit processes the oxidized salt solution supplied by the reaction unit, spray unit, and tail gas treatment unit to obtain reaction byproducts. The tailings unit may include: a first filtration device, a drying device, a second filtration device, a calcium removal reactor, a desulfurization reactor, a filtrate intermediate tank, and a residue harmless treatment tank. The first filtration device uses a large rotary drum vacuum filter to filter the salt solution, obtaining filtrate and filter cake. The drying device uses a spiral dryer to dry the filter cake, obtaining a mixed byproduct of calcium carbonate and calcium phosphite. The second filtration device uses a ceramic membrane filter to filter the filtrate using cross-flow filtration, obtaining a primary purified liquid. Every 8 hours, it is automatically reacted with 5% dilute hydrochloric acid. The second filtration unit is rinsed; the calcium removal reactor is a vertical fluidized bed reactor; the calcium removal reactor is used to add sodium carbonate solution to the primary purified liquid to obtain calcium carbonate precipitate and secondary purified liquid; the desulfurization reactor is a packed tower used to introduce a large amount of compressed air into the secondary purified filtrate, using oxygen in the air to oxidize soluble sulfur ions to obtain tertiary purified liquid after sulfur ion removal; the intermediate filtrate tank is used to heat and concentrate the tertiary purified liquid using MVR evaporation technology, increasing the sodium hypophosphite concentration from 15% to 45%, and then it enters the crystallizer to form sodium hypophosphite crystals. After centrifugation and drying, high-purity solids are obtained; the residue harmless disposal tank is used to store various solids obtained.
[0019] In some embodiments of this application, the reaction unit further includes an injection component, a first temperature monitoring component, a first pressure monitoring component, and a concentration monitoring component. The injection component is used to continuously introduce supercritical carbon dioxide, accounting for 8-15% of the reaction volume, into the reaction system to form a homogeneous reaction environment, and to monitor the flow rate of the introduced supercritical carbon dioxide. The temperature monitoring component is used to monitor the temperature inside the reactor. The pressure monitoring component is used to monitor the pressure inside the reactor. The concentration monitoring component is used to monitor the concentration of different gases inside the reactor in real time using a laser gas analyzer, and to monitor the concentration of different gases at the first outlet in real time using a laser gas analyzer and a gas chromatograph. Specifically, the controller is also used to determine the reaction control parameters of the reactor based on various parameters monitored within the reaction unit. The reaction control parameters include: the input ratio of reactants, the rotation speed of the rotating packed bed, the injection amount of supercritical carbon dioxide, and the reaction temperature and reaction pressure inside the reactor adjusted by the jacketed heat exchange component.
[0020] In some embodiments of this application, the dewatering unit and the air collection and compression unit are connected by dual branches, that is, the dewatering unit has two outlets and the air collection and compression unit has two inlets; the two outlets of the dewatering unit are respectively connected to the two inlets of the air collection and compression unit; the dual-branch configuration allows the other branch to be used when one branch fails.
[0021] In some embodiments of this application, the system further includes: a liquid yellow phosphorus inlet, a lime slurry suspension inlet, a sodium hydroxide solution inlet, and a pretreatment unit; the first, second, and third inlets of the pretreatment unit are respectively connected to the liquid yellow phosphorus inlet, the lime slurry suspension inlet, and the sodium hydroxide solution inlet; the first, second, and third outlets of the pretreatment unit are respectively connected to the second, third, and fourth inlets of the reaction unit. A pretreatment unit is used to pretreat liquid yellow phosphorus, lime slurry suspension, and sodium hydroxide solution, respectively. The pretreatment unit includes an atomizing component, a homogenizing component, and a preheating component. The inlet of the atomizing component is the first inlet of the pretreatment unit; the inlet of the homogenizing component is the second inlet; the inlet of the preheating component is the third inlet; the outlet of the atomizing component is the first outlet; the outlet of the homogenizing component is the second outlet; and the outlet of the preheating component is the third outlet. Specifically, the atomizing component employs an array-type ultra-high pressure system. The atomizing device continuously atomizes liquid yellow phosphorus into 20-50 μm droplets according to the configured atomization parameters, maintaining the liquid yellow phosphorus in a dispersed state at the reaction temperature. The homogenizing component includes a series-connected ultrasonic disperser and an online laser particle size analyzer. The ultrasonic disperser homogenizes the lime slurry suspension according to the configured homogenization parameters, and the online laser particle size analyzer detects the dispersion of the lime slurry suspension. When the detected dispersion meets the configured dispersion threshold, the homogenized lime slurry suspension is delivered to the reaction unit. The preheating component preheats the sodium hydroxide solution to a first preset temperature. A combination of jacketed microwave heating and a plate heat exchanger is used to control the sodium hydroxide solution temperature at 40-60℃, with temperature fluctuations not exceeding ±0.5℃, and the feed metering accuracy reaches ±0.1%.
[0022] In some further embodiments of this application, the dehydration unit further includes: a humidity monitoring component, a second temperature monitoring component, and a second pressure monitoring component; the humidity monitoring component is installed at the inlet of the first adsorption tower, the inlet and outlet of the second adsorption tower, and the outlet of the tertiary membrane permeate dehydrator, and is used to monitor the humidity of phosphine at each stage; the second temperature monitoring component is installed at the outlet of the separation component, inside the first adsorption tower and the second adsorption tower, respectively, and is used to monitor the temperature of the first phosphine after heating and the temperature inside the adsorption tower; the second pressure monitoring component is installed at the inlet and outlet of the tertiary membrane permeate dehydrator and is used to monitor the pressure difference across the membrane module; The gas collection and compression unit also includes: a third pressure monitoring component, a third temperature monitoring component, a first flow rate monitoring component, and a droplet monitoring component. The third pressure monitoring component is installed inside the first and second buffer tanks and at the inlet and outlet of the compression component to monitor the pressure inside the buffer tanks and the pressure at the inlet and outlet of the compressor. The third temperature monitoring component is installed inside the buffer tanks, at the outlet of the compression component, and at the outlet of the cooling component to monitor the temperature inside the buffer tanks, the temperature of the compressed phosphine, and the temperature after cooling. The flow rate monitoring component is installed in the feed pipe of the gas collection and compression unit to monitor the inlet flow rate of the dehydrated phosphine. The droplet monitoring component is installed at the outlet of the cyclone separator to monitor the residual amount of droplets with a particle size of not less than 5 μm using a laser particle size analyzer. The refining unit also includes: a first component monitoring component, a second component monitoring component, a third component monitoring component, a fourth pressure monitoring component, and a fourth temperature monitoring component; the first component monitoring component is installed at the inlet and outlet of the deweighting tower and is used to monitor the content of heavy components by gas chromatography; the second component monitoring component is installed at the inlet and outlet of the multi-stage adsorption unit and is used to monitor the concentration of impurities such as hydrogen sulfide, organophosphorus compounds, and alkaline gases; the third component monitoring component is installed at the outlet of the cryogenic distillation unit and is used to monitor the purity of the target phosphine; the fourth temperature monitoring component is installed at the bottom and top of the deweighting tower and at each section of the distillation column of the cryogenic distillation unit and is used to monitor the operating temperature of the deweighting tower and the cryogenic ambient temperature of the distillation column; the fourth pressure monitoring component is installed at the inlet and outlet of the deweighting tower and the cryogenic distillation unit and is used to monitor the pressure inside the tower; The filling unit also includes: a fifth pressure monitoring component, a fifth temperature monitoring component, a second flow monitoring component, and a first phosphine concentration monitoring component; the fifth pressure monitoring component and the fifth temperature monitoring component are installed in a stainless steel high-pressure storage tank and are used to monitor the pressure in the storage tank and the temperature of the liquid nitrogen pool, respectively; the second flow monitoring component and the phosphine concentration monitoring component are installed in the filling pipeline of the filling unit and are used to monitor the filling flow rate and purity of the target phosphine. The spray unit also includes: a second phosphine concentration monitoring component and a pH value monitoring component; the second phosphine concentration monitoring component and the pH value monitoring component are installed at the inlet and outlet of the spray tower to monitor the phosphine concentration in the tail gas and the pH value of the oxidized salt solution, respectively. The exhaust gas treatment unit also includes a gas monitoring component installed at the outlet of the exhaust gas treatment unit to monitor the concentration of phosphine and other pollutants in the exhaust gas to be emitted.
[0023] The preferred embodiments of this application are described below with reference to the accompanying drawings. It should be understood that the preferred embodiments described herein are for illustration and explanation only and are not intended to limit this application. Furthermore, the embodiments and features in the embodiments of this application can be combined with each other without conflict.
[0024] Figure 2 This is a schematic flowchart illustrating a method for preparing phosphine, provided as an embodiment of this application. Figure 2 As shown, the method may include: Step S210: Generate control parameters for each unit based on the real-time monitoring data of the different units.
[0025] In this embodiment, the real-time monitoring data of different units is achieved using multiple monitoring components set in different units. The real-time monitoring data of different units include: the temperature, pressure and concentration of different gases in the reaction vessel of the reaction unit; the humidity of phosphine at each stage of the dehydration unit, the temperature of the first phosphine after heating and the temperature in the adsorption tower, and the pressure difference across the membrane module; the pressure in the buffer tank and the inlet and outlet pressure of the compressor in the gas collection and compression unit, the temperature in the buffer tank, the temperature of the compressed phosphine and the temperature after cooling, the inlet flow rate and droplet residue of the dehydrated phosphine; the content of heavy components in the refining unit, the concentration of impurities such as hydrogen sulfide, organophosphorus compounds and alkaline gases, the purity of the target phosphine, the operating temperature of the deweighting tower and the low-temperature ambient temperature and pressure in the distillation tower; the pressure in the storage tank and the temperature of the liquid nitrogen pool in the filling unit, the filling flow rate and purity of the target phosphine; the concentration of phosphine in the tail gas of the spraying unit and the pH value of the oxidized salt solution; and the concentration of phosphine and other pollutants in the tail gas to be discharged in the tail gas treatment unit.
[0026] Specifically, based on the real-time monitoring data of different units, control parameters for each unit are generated, including: inputting the real-time monitoring data of different units into a pre-trained multimodal intelligent cooperative control model to generate control parameters for each unit; wherein, the multimodal intelligent cooperative control model includes: reaction unit sub-model, water removal unit sub-model, gas collection and compression unit sub-model, purification unit sub-model, filling unit sub-model, spraying unit sub-model, exhaust gas treatment unit sub-model and cooperative model; The reaction unit sub-model employs an improved temporal attention mechanism and LSTM to capture the correlation between different monitoring data of the reaction unit through the temporal attention mechanism, and outputs reaction control parameters in combination with reaction mechanism constraints (stoichiometry of yellow phosphorus disproportionation reaction). Among these, the reaction control parameters include: the input ratio of reactants, the rotation speed of the rotating packed bed, the injection rate of supercritical carbon dioxide, and the reaction temperature and reaction pressure in the reactor adjusted by the jacketed heat exchange components. The water removal unit sub-model adopts an adaptive fuzzy reinforcement learning architecture; it uses fuzzy logic to process the phosphine humidity, the first phosphine heating temperature, the temperature inside the adsorption tower, and the pressure difference across the membrane module at each stage to generate water removal control parameters. The water removal control parameters include: the heating power of the separation module, the switching signal between the first adsorption tower and the second adsorption tower, the inlet pressure of the three-stage membrane permeate dewatering unit, and the cooling water flow rate of the adsorption tower cooling jacket. The sub-model of the gas collection and compression unit adopts a hybrid architecture of PID and reinforcement learning. It is used to optimize and dynamically adjust the gas collection and compression control parameters based on different real-time monitoring data of the gas collection and compression unit. The gas collection and compression control parameters include: the opening degree of the nitrogen replenishment or exhaust valve of the buffer tank, the flow rate of the heat exchange medium in the jacket of the buffer tank, the frequency of the explosion-proof screw compressor, the cooling water flow rate of the cooling component, and the angle of the inlet guide plate of the cyclone separator. The refining unit sub-model employs multi-objective genetic optimization and a GNN architecture to model the relationship between the heavy removal tower, adsorption components, and distillation tower based on different real-time monitoring data of the refining unit. The genetic algorithm optimizes multiple objectives (highest purity, lowest energy consumption) to generate refining control parameters, including: the heating power of the heavy removal tower bottom, the purging frequency of the modified ZSM-5 molecular sieve adsorption tower, the feed flow rate of the HKUST-1 adsorption tower, the liquid nitrogen flow rate of the cryogenic distillation unit, and the reflux ratio of the distillation tower. The filling unit sub-model adopts adaptive PID and fuzzy fusion to perform fuzzy logic judgment and dynamic adjustment based on real-time monitoring data of the filling unit to generate filling control parameters, including: filling valve opening, liquid nitrogen replenishment flow rate and storage tank pressure relief valve threshold. The spray unit sub-model uses a hybrid approach of reinforcement learning and rules to perform reinforcement learning optimization based on real-time monitoring data of the spray unit, generating spray control parameters, including: pump frequency of the circulating spray equipment and power of the low-temperature plasma oxidation component; The exhaust gas treatment unit sub-model uses feedback correction and PID to generate exhaust gas treatment control parameters based on real-time monitoring data of the exhaust gas treatment unit, including: the number of ultraviolet lamps in the photocatalytic oxidation device, the concentration of alkaline solution in the spray assembly, and the fan air volume. The collaborative model employs deep reinforcement learning combined with a global optimization architecture to coordinate the control parameters of each unit in order to avoid local optimization conflicts. The optimization objective of the collaborative model is a global reward function = purity compliance rate (40%) + energy consumption reduction rate (30%) + equipment life extension (20%) + by-product recovery rate (10%). The collaborative mechanism is that when the control parameters of a certain unit exceed the safety threshold, the collaborative model forcibly reduces the load of the associated units to prioritize system safety.
[0027] Step S220: The corresponding control parameters are sent to the corresponding units to control the reaction unit to react different materials to generate crude phosphine according to the corresponding control parameters, to control the dehydration unit to remove water from the crude phosphine according to the corresponding control parameters to obtain dehydrated phosphine, to control the gas collection and compression unit to temporarily store the dehydrated phosphine according to the corresponding control parameters, to control the purification unit to remove impurities from the dehydrated phosphine according to the corresponding control parameters to obtain the target phosphine, and to control the post-processing unit to process the target phosphine and the intermediate products obtained in the phosphine production process according to the corresponding control parameters.
[0028] Specifically, reaction control parameters are sent to the reaction unit to control the reaction of different materials to produce crude phosphine according to the corresponding control parameters; The dehydration control parameters are sent to the dehydration unit to control it to remove moisture from the crude phosphine according to the corresponding control parameters to obtain dehydrated phosphine; the collection and compression control parameters are sent to the collection and compression unit to control it to temporarily store the dehydrated phosphine according to the corresponding control parameters; the refining control parameters are sent to the refining unit to control it to remove impurities from the dehydrated phosphine according to the corresponding control parameters to obtain the target phosphine; the filling control parameters are sent to the fine filling unit, the spraying control parameters are sent to the spraying unit, and the exhaust gas treatment control parameters are sent to the exhaust gas treatment unit to control the filling unit, the spraying unit, and the exhaust gas treatment unit to perform the corresponding post-treatment.
[0029] Corresponding to the above method, this application also provides an apparatus for preparing phosphine, such as... Figure 3 As shown, the device includes: The generation unit 310 is used to generate control parameters for each unit based on the real-time monitoring data of different units. The distribution unit 320 is used to distribute the corresponding control parameters to the corresponding units, so as to control the reaction unit to react different materials to generate crude phosphine according to the corresponding control parameters, to control the dehydration unit to remove water from the crude phosphine to obtain dehydrated phosphine according to the corresponding control parameters, to control the gas collection and compression unit to temporarily store the dehydrated phosphine according to the corresponding control parameters, to control the refining unit to remove impurities from the dehydrated phosphine to obtain the target phosphine according to the corresponding control parameters, and to control the post-processing unit to process the target phosphine and the intermediate products obtained in the phosphine production process according to the corresponding control parameters.
[0030] The functions of each functional unit in the phosphine preparation apparatus provided in the above embodiments of this application can be realized through the above method steps. Therefore, the specific working process and beneficial effects of each unit in the phosphine preparation apparatus provided in the embodiments of this application will not be repeated here.
[0031] This application also provides an electronic device, such as... Figure 4 As shown, it includes a processor 410, a communication interface 420, a memory 430, and a communication bus 440, wherein the processor 410, the communication interface 420, and the memory 430 communicate with each other through the communication bus 440.
[0032] Memory 430 is used to store computer programs; When the processor 410 executes the program stored in the memory 430, it performs the following steps: Based on the real-time monitoring data of different units, control parameters for each unit are generated. The corresponding control parameters are sent to the corresponding units to control the reaction unit to react different materials to produce crude phosphine, to control the dehydration unit to remove water from the crude phosphine to obtain dehydrated phosphine, to control the gas collection and compression unit to temporarily store the dehydrated phosphine according to the corresponding control parameters, to control the purification unit to remove impurities from the dehydrated phosphine to obtain the target phosphine, and to control the post-processing unit to process the target phosphine and intermediate products obtained in the phosphine production process according to the corresponding control parameters.
[0033] The communication bus mentioned above can be a Peripheral Component Interconnect Standard (PCI) bus or an Extended Industry Standard Architecture (EISA) bus, etc. This communication bus can be divided into address bus, data bus, control bus, etc. For ease of illustration, only one thick line is used to represent it in the diagram, but this does not mean that there is only one bus or one type of bus.
[0034] The communication interface is used for communication between the aforementioned electronic devices and other devices.
[0035] The memory may include random access memory (RAM) or non-volatile memory (NVM), such as at least one disk storage device. Optionally, the memory may also be at least one storage device located remotely from the aforementioned processor.
[0036] The processors mentioned above can be general-purpose processors, including central processing units (CPUs), network processors (NPs), etc.; they can also be digital signal processors (DSPs), application-specific integrated circuits (ASICs), field-programmable gate arrays (FPGAs), or other programmable logic devices, discrete gate or transistor logic devices, or discrete hardware components.
[0037] The implementation methods and beneficial effects of the various components of the electronic device in the above embodiments for solving the problem can be found in [reference needed]. Figure 2 The steps in the illustrated embodiments are used to implement the electronic device. Therefore, the specific working process and beneficial effects of the electronic device provided in this application will not be repeated here.
[0038] In another embodiment provided in this application, a computer-readable storage medium is also provided, which stores instructions that, when executed on a computer, cause the computer to perform any of the above-described methods for preparing phosphine.
[0039] In another embodiment provided in this application, a computer program product containing instructions is also provided, which, when run on a computer, causes the computer to execute any of the above-described methods for preparing phosphine.
[0040] Those skilled in the art will understand that the embodiments in this application can be provided as methods, systems, or computer program products. Therefore, the embodiments in this application can take the form of a completely hardware embodiment, a completely software embodiment, or an embodiment combining software and hardware aspects. Furthermore, the embodiments in this application can take the form of a computer program product implemented on one or more computer-usable storage media (including but not limited to disk storage, CD-ROM, optical storage, etc.) containing computer-usable program code.
[0041] This application describes embodiments of methods, apparatus (systems), and computer program products according to embodiments of this application with reference to flowchart illustrations and / or block diagrams. It will be understood that each block of the flowchart illustrations and / or block diagrams, and combinations of blocks in the flowchart illustrations and / or block diagrams, can be implemented by computer program instructions. These computer program instructions can be provided to a processor of a general-purpose computer, special-purpose computer, embedded processor, or other programmable data processing apparatus to produce a machine, such that the instructions, which execute via the processor of the computer or other programmable data processing apparatus, generate instructions for implementing the flowchart illustrations. Figure 1 One or more processes and / or boxes Figure 1 A device that provides the functions specified in one or more boxes.
[0042] These computer program instructions may also be stored in a computer-readable storage medium that can direct a computer or other programmable data processing device to function in a particular manner, such that the instructions stored in the computer-readable storage medium produce an article of manufacture including instruction means, which are implemented in a process Figure 1 One or more processes and / or boxes Figure 1 The function specified in one or more boxes.
[0043] These computer program instructions may also be loaded onto a computer or other programmable data processing equipment to cause a series of operational steps to be performed on the computer or other programmable equipment to produce a computer-implemented process, thereby providing instructions that execute on the computer or other programmable equipment for implementing the process. Figure 1 One or more processes and / or boxes Figure 1 The steps of the function specified in one or more boxes.
[0044] Although preferred embodiments have been described in this application, those skilled in the art, upon learning the basic inventive concept, can make other changes and modifications to these embodiments. Therefore, the appended claims are intended to be interpreted as including the preferred embodiments as well as all changes and modifications falling within the scope of the embodiments of this application.
[0045] Obviously, those skilled in the art can make various modifications and variations to the embodiments of this application without departing from the spirit and scope of the embodiments of this application. Therefore, if these modifications and variations to the embodiments of this application fall within the scope of this application and its equivalents, then these modifications and variations are also intended to be included in the embodiments of this application.
Claims
1. A phosphine preparation system, characterized in that, The system includes: a controller, a reaction unit, a dehydration unit, a gas collection and compression unit, a purification unit, and a post-treatment unit; the controller is connected to the reaction unit, the dehydration unit, the gas collection and compression unit, the purification unit, and the post-treatment unit respectively; the first inlet of the reaction unit is connected to the first outlet of the dehydration unit; the first outlet of the reaction unit is connected to the inlet of the dehydration unit; the second outlet of the dehydration unit is connected to the inlet of the gas collection and compression unit; the first outlet of the gas collection and compression unit is connected to the first inlet of the purification unit; the second outlet of the gas collection and compression unit and the first outlet of the purification unit are respectively connected to the first inlet and the second inlet of the post-treatment unit. The controller is used to generate control parameters for each unit based on the real-time monitoring data of different units, and to send the corresponding control parameters to the corresponding units. The reaction unit is used to control the reaction of different materials to generate crude phosphine according to corresponding control parameters; The dehydration unit is used to remove water from crude phosphine according to corresponding control parameters to obtain dehydrated phosphine. The gas collection and compression unit is used to temporarily store dehydrated phosphine according to the corresponding control parameters. The refining unit is used to remove impurities from the dehydrated phosphine according to the corresponding control parameters to obtain the target phosphine. The post-processing unit is used to process the target phosphine and intermediate products obtained in the phosphine production process according to corresponding control parameters.
2. The system as described in claim 1, characterized in that, The system further includes: a liquid yellow phosphorus inlet, a lime slurry suspension inlet, a sodium hydroxide solution inlet, and a pretreatment unit; the first, second, and third inlets of the pretreatment unit are respectively connected to the liquid yellow phosphorus inlet, the lime slurry suspension inlet, and the sodium hydroxide solution inlet; the first, second, and third outlets of the pretreatment unit are respectively connected to the second, third, and fourth inlets of the reaction unit. The pretreatment unit is used to pretreat liquid yellow phosphorus, lime milk suspension and sodium hydroxide solution respectively; The reaction unit is specifically used to react pretreated liquid yellow phosphorus, lime milk suspension and sodium hydroxide solution to generate crude phosphine.
3. The system as described in claim 2, characterized in that, The pretreatment unit includes: an atomizing component, a homogenizing component, and a preheating component; wherein, the inlet of the atomizing component is the first inlet of the pretreatment unit; the inlet of the homogenizing component is the second inlet of the pretreatment unit; the inlet of the preheating component is the third inlet of the pretreatment unit; the outlet of the atomizing component is the first outlet of the pretreatment unit; the outlet of the homogenizing component is the second outlet of the pretreatment unit; and the outlet of the preheating component is the third outlet of the pretreatment unit. Atomizing component for continuously atomizing liquid yellow phosphorus according to configured atomizing parameters; Homogenization component, used to homogenize lime slurry suspension according to configured homogenization parameters; A preheating component is used to preheat the sodium hydroxide solution to a first preset temperature.
4. The system as described in claim 1, characterized in that, The post-processing unit includes: a filling unit, a spraying unit, an exhaust gas treatment unit, and a tailings salt unit; The first inlet of the spray unit is the first inlet of the post-treatment unit; the second inlet of the spray unit is the second inlet of the post-treatment unit; the second outlet of the refining unit is connected to the inlet of the filling unit; the second inlet of the refining unit is connected to the outlet of the filling unit; the first outlet of the spray unit is connected to the inlet of the exhaust gas treatment unit; the second outlet of the spray unit is connected to the third inlet of the tailings salt unit; the first outlet of the exhaust gas treatment unit is connected to the first inlet of the tailings salt unit; the second outlet of the exhaust gas treatment unit is used to discharge the exhaust gas to be emitted into the atmosphere. The second outlet of the reaction unit is connected to the second inlet of the tailings unit.
5. The system as described in claim 4, characterized in that, The reaction unit is also used to: transport the salt solution generated by the reaction to the tailings unit; The filling unit is used to compress and store the target phosphine into a phosphine container; The spraying unit is used to treat the phosphine tail gas emitted from the refining unit and the gas collection and compression unit to obtain tail gas to be treated and an oxidized salt solution; and to transport the tail gas to be treated to the tail gas treatment unit and the oxidized salt solution to the tail salt unit. The exhaust gas treatment unit is used to decompose and oxidize the exhaust gas to be treated, and absorb it with an alkaline solution to obtain a salt solution. And the salt solution is transported to the tailings unit; The tailings unit is used to process the oxidized salt solution delivered by the reaction unit, the spray unit, and the tail gas treatment unit to obtain reaction byproducts.
6. The system as described in claim 1, characterized in that, The water removal unit includes a separation component, a first adsorption tower, a second adsorption tower, and a three-stage membrane permeate dewatering unit. The inlet of the separation component is the inlet of the water removal unit. The outlet of the separation component is connected to the inlet of the first adsorption tower. The outlet of the first adsorption tower is connected to the inlet of the second adsorption tower. The outlet of the second adsorption tower is connected to the inlet of the three-stage membrane permeate dewatering unit. The outlet of the three-stage membrane permeate dewatering unit is the inlet of the water removal unit. The separation component is used to separate crude phosphine to obtain first phosphine; The first adsorption tower is used to perform initial water removal on the first phosphine to obtain the second phosphine. The second adsorption tower is used to perform secondary dehydration on the second phosphine to obtain the third phosphine; The three-stage membrane permeate dewatering device is used to perform deep dewatering of the third phosphine to obtain dewatered phosphine.
7. The system as described in claim 5, characterized in that, The tailings unit includes: a first filtration device, a drying device, a second filtration device, a calcium removal reactor, a sulfur removal reactor, and a filtrate intermediate tank; The first filtration device is used to filter the salt solution to obtain filtrate and filter cake; The drying device is used to dry the filter cake to obtain a mixed byproduct of calcium carbonate and calcium phosphite; The second filtration device is used to filter the filtrate to obtain a primary purified liquid; The calcium removal reactor is used to add sodium carbonate solution to the primary purification liquid to obtain calcium carbonate precipitate and secondary purification liquid; The desulfurization reactor is used to oxidize the secondary purified filtrate with compressed air to obtain the tertiary purified filtrate after removing sulfur ions. The intermediate filtrate tank is used to heat and concentrate sodium hypophosphite crystals in the tertiary purified liquid.
8. A method for preparing phosphine, characterized in that, In a controller for a phosphine preparation system, the system further includes: a reaction unit, a dehydration unit, a gas collection and compression unit, a purification unit, and a post-treatment unit; the controller is connected to the reaction unit, the dehydration unit, the gas collection and compression unit, the purification unit, and the post-treatment unit respectively; the first inlet of the reaction unit is connected to the first outlet of the dehydration unit; the first outlet of the reaction unit is connected to the inlet of the dehydration unit; the second outlet of the dehydration unit is connected to the inlet of the gas collection and compression unit; the first outlet of the gas collection and compression unit is connected to the first inlet of the purification unit; the second outlet of the gas collection and compression unit and the first outlet of the purification unit are respectively connected to the first inlet and the second inlet of the post-treatment unit, and the method includes: Based on the real-time monitoring data of different units, control parameters for each unit are generated. The corresponding control parameters are sent to the corresponding units to control the reaction unit to react different materials to generate crude phosphine according to the corresponding control parameters, to control the dehydration unit to remove water from the crude phosphine to obtain dehydrated phosphine according to the corresponding control parameters, to control the gas collection and compression unit to temporarily store the dehydrated phosphine according to the corresponding control parameters, to control the refining unit to remove impurities from the dehydrated phosphine to obtain the target phosphine according to the corresponding control parameters, and to control the post-processing unit to process the target phosphine and the intermediate products obtained in the phosphine production process according to the corresponding control parameters.
9. An electronic device, characterized in that, The electronic device includes a processor, a communication interface, a memory, and a communication bus, wherein the processor, the communication interface, and the memory communicate with each other through the communication bus; Memory, used to store computer programs; A processor, when executing a program stored in memory, implements the method of claim 8.
10. A computer-readable storage medium, characterized in that, The computer-readable storage medium stores a computer program that, when executed by a processor, implements the method of claim 8.