Production device of electronic-grade hydrogen phosphide

Abstract

The utility model provides a production device of electronic-grade hydrogen phosphide. The production device comprises a full-automatic aluminum phosphide feeding system, a sulfuric acid metering tank, a constant-temperature reaction kettle, a purification cooling system, a heavy component removal purification column, a cold trap collection device, a light component removal purification column, a low-temperature filling system, an inert gas purging system, a vacuum system and a tail gas treatment system. The method comprises the following steps: quantitatively adding aluminum phosphide into a constant-temperature reaction kettle, slowly adding sulfuric acid into the constant-temperature reaction kettle through a metering tank, reacting to generate hydrogen phosphide gas, and removing particulate matters, acid mist, moisture, arsenic hydride, hydrogen sulfide, carbon dioxide, carbon monoxide, alkane, silane and ethylene in the hydrogen phosphide gas through pre-cooling, deep cooling, heavy component removal, cold trap and light component removal to obtain the electronic-grade hydrogen phosphide special gas with the purity of 99.9999%. And feeding tail gas generated in the purification process into a tail gas treatment system, absorbing the tail gas through a two-stage tower, and discharging the tail gas after reaching the standard.

Description

TECHNICAL FIELD

[0001] The application belongs to the technical field of electronic-grade phosphine special gas, and specifically relates to a device for preparing electronic-grade phosphine. BACKGROUND

[0002] Phosphine (PH3) is a high-purity electronic gas, which is widely used in the electronic industry, solar cells, mobile communication, automobile navigation, aerospace, military industry and the like. Common production processes of phosphine include a phosphorous acid thermal decomposition method and an aluminum phosphide acidolysis method.

[0003] 1) The phosphorous acid thermal decomposition method:

[0004] Solid phosphorous acid is put into a jacketed reactor, and heat-conducting oil is used to heat the jacketed reactor to about 260 DEG C under an oxygen-free condition, so that the phosphorous acid is subjected to a disproportionation reaction, PH3 is generated through deoxidation between H3PO4 molecules, and high-purity phosphine gas is obtained through processes such as drying, adsorption and low-temperature cooling. The raw material phosphorous acid used in this method has strong corrosion, and the materials used for the reaction kettle and pipelines are required to be relatively high, and the project investment is very large. The reaction temperature is relatively high, the reaction is relatively violent, and the reaction is not easy to control.

[0005] 2) The aluminum phosphide acidolysis method:

[0006] Aluminum phosphide powder is put into a jacketed reactor, water and sulfuric acid are added dropwise into the reactor after metering, phosphine gas is generated after the aluminum phosphide is subjected to acidolysis, and high-purity phosphine gas is obtained through processes such as condensation, adsorption, cold trap, purification and filling. This method is easy to produce phosphine gas, the reaction conditions are mild, and the reaction is easy to control.

[0007] Patent US3116109 proposes a method for preparing phosphine, which further reacts phosphite and hypophosphite and phosphoric acid to generate phosphine and sodium dihydrogen phosphate. The reaction temperature needs to be between 190 DEG C and 310 DEG C.

[0008] Patent CN114620695 proposes a system and a method for preparing phosphine, which reacts aluminum phosphide and sulfuric acid to obtain phosphine gas, uses mixed alcohol as an extractant, and obtains aluminum phosphate by static layering of the reaction liquid. The mixed alcohol is subjected to distillation to remove water and is recycled.

[0009] Patent CN221267604U proposes an electronic-grade phosphine purification device, which obtains phosphine products through three-stage adsorption, two-stage rectification and cooling, and controls the operating pressure to be between 0.8MPa and 1.0MPa.

[0010] The prior art has a high reaction temperature, a large operating pressure, and simultaneously introduces an extractant to increase the processing cost, so that the equipment investment, operation and maintenance cost of the entire system are high.

[0011] The prior art uses adsorbents for purification, which cannot be regenerated and recycled, and has high operation and treatment costs.

[0012] The prior art uses vacuum and nitrogen to replace the system, and lacks detection measures for system safety, which has hidden dangers for device safety and stability. SUMMARY

[0013] Problems to be solved by the invention

[0014] To solve the above problems, i.e. to solve the problems raised in the above background art, the present application provides a production device for electronic-grade phosphine, and the specific technical solutions are as follows:

[0015] The production device for electronic-grade phosphine comprises: S1, an automatic phosphonium aluminum feeding system; S2, a sulfuric acid metering tank; S3, a constant-temperature reaction kettle; S4, a pre-cooling condenser; S5, a deep cooling condenser; S6, a heavy-purification column; S7, a cold trap collection device; S8, a cold trap transfer tank; S9, a light-purification column; S10, a low-temperature jacketing filling machine; S11, a vacuum buffer tank; S12, a vacuum pump; S13, a first-stage alkali washing tower; S14, a washing circulating pump; S15, a second-stage adsorption tower; S16, an exhaust fan; S17, an exhaust cylinder; S18, a phosphonium aluminum pipeline; S19, a sulfuric acid pipeline; S20, a nitrogen pipeline control valve; S21, a helium pipeline control valve; S22, a phosphine pipeline; S23, an alkali solution pipeline; S24, a phosphonium aluminum quantitative control valve; and S25, a sulfuric acid quantitative control valve.

[0016] Phosphonium aluminum raw materials from a raw material warehouse are stored in the material bin of the automatic phosphonium aluminum feeding system (1) through the automatic phosphonium aluminum feeding system (1), and are quantitatively added to the constant-temperature reaction kettle (S3) through the phosphonium aluminum quantitative control valve (S24) on the phosphonium aluminum pipeline (S18), and the control valve (S24) is closed; the heat conduction oil cooling system in the constant-temperature reaction kettle (S3) is opened to ensure the normal operation of the cooling system; the nitrogen pipeline control valve (S20) connected to the constant-temperature reaction kettle (S3) is opened to replace the air or other gas in the constant-temperature reaction kettle (S3) completely; the helium pipeline control valve (S21) connected to the constant-temperature reaction kettle (S3) is opened to detect whether the equipment, pipeline, instrument, and flange connection are completely sealed; the vacuum pump connected to the constant-temperature reaction kettle (S3) is opened to control the pressure of the reaction kettle at-0.01 MPa (A), and the nitrogen and helium used for purging and detection are sent to the first-stage alkali washing tower (S13) of the exhaust treatment system (11).

[0017] Further, the raw material sulfuric acid is slowly added to the constant-temperature reaction kettle (S3) from the sulfuric acid metering tank (2) through the metering scale and the quantitative control valve (S25) on the sulfuric acid pipeline (S19) configured therein, the addition amount of the sulfuric acid is controlled at 1-10 L / min, and the reaction temperature is controlled at 20-60℃.

[0018] Further, the obtained aluminum sulfate solution is intermittently filled into an aluminum sulfate tank as a water treatment agent for sale.

[0019] Further, the obtained phosphine gas from which the particulate matter and moisture are removed is sent to a heavy component removal column (S6) to remove heavy components such as arsine, metal hydride, hydrogen sulfide, and water from the gas by using an adsorbent.

[0020] Further, the phosphine gas from which the particulate matter and moisture are removed is sent to a heavy component removal column (S6) to remove heavy components such as arsine, metal hydride, hydrogen sulfide, and water from the gas by using an adsorbent.

[0021] Further, helium gas is introduced to replace the gas, and then a vacuum pump (S12) is started, and a pipeline valve connected to the heavy component removal column (S6) after adsorption is opened, and the vacuum degree is controlled to 90 to 99 kPa, so that the components such as arsine, metal hydride, hydrogen sulfide, and water adsorbed are desorbed and sent to a first caustic washing tower (S13) of an exhaust gas treatment system (11), thereby regenerating the adsorbent for recycling.

[0022] Further, the phosphine gas from which the heavy components are removed is sent to a cold trap transfer tank (S8) in a cold trap collection device (S7), and liquid nitrogen is used as a cold trap agent, and the temperature is controlled to -100 to -90°C, so that the phosphine gas is condensed to a liquid state, and light components such as nitrogen and oxygen are separated and sent to the first caustic washing tower (S13) of the exhaust gas treatment system (11) by a vacuum pump.

[0023] Further, the cold trap transfer tank (S8) is taken out of the cold trap collection device (S7) and connected to a light component removal column (S9). The light component removal column is 2 to 10 adsorption towers connected in series, and is filled with adsorbents such as activated carbon, 4A molecular sieve, 5A molecular sieve, and 13X. A heating system of the cold trap transfer tank (S8) is started, and the temperature is controlled to -90 to -80°C, so that the phosphine liquid in the container is gasified to remove carbon monoxide, carbon dioxide, methane, ethane, silane, ethylene, and organic compounds of C3 or more, thereby obtaining 99.9999% (6N) purity electronic grade phosphine special gas, which is sent to a low-temperature jacketed tank filling machine (S10) to be condensed, liquefied, and tanked for storage.

[0024] Further, helium is introduced for replacement, and then a vacuum pump (S12) is started, a vacuum valve connected to the light-purification column (S9) after adsorption is opened, and the vacuum degree is controlled at 90-99 kPa, so that the adsorbed carbon monoxide, carbon dioxide, ethylene, ethane and C3 or more organic components are desorbed and sent to the first alkaline washing tower (S13) of the tail gas treatment system (11), so that the adsorbent is regenerated and recycled.

[0025] Further, the purge tail gas, leakage detection tail gas and desorption tail gas from the aluminum phosphide automatic feeding system (S1), the constant-temperature reaction kettle (S3), the heavy-purification column (S6), the cold trap collection device (S7), the cold trap transfer tank (S8), the light-purification column (S9), the low-temperature jacketed tank filling machine (S10) and the like are connected to the first alkaline washing tower (S13), and the acidic gas in the tail gas is removed by reverse absorption with the alkaline washing liquid sprayed by the washing circulating pump (S14) and sent to the second adsorption tower (S15) to adsorb ethylene and alkane organic components in the tail gas, and the treated tail gas is sent into the exhaust cylinder (S17) through the tail gas fan (S16) for standard emission. The waste liquid generated by washing is collected and treated uniformly.

[0026] Effects of the application

[0027] In summary, the application has the following advantages and beneficial effects:

[0028] 1. The method and system of the application work under negative pressure to normal pressure, and the investment cost of equipment is low.

[0029] 2. The method and system of the application have simple raw materials, do not need extraction and the like, have a short device process, simple operation and low energy consumption.

[0030] 3. The method and system of the application regenerate the adsorbent by using helium and a vacuum system, and the service life of the adsorbent is improved.

[0031] 4. The method and system of the application detect leakage by using helium on the reaction equipment and the connection of pipelines, and ensure safe and stable operation of the device. BRIEF DESCRIPTION OF DRAWINGS

[0032] The present disclosure is described in detail according to one or more embodiments with reference to the following drawings. The provided drawings are for the purpose of facilitating understanding of the present disclosure and should not be considered as a limitation on the breadth, scope, size or applicability of the present disclosure. The drawings are not necessarily drawn to scale for ease of illustration.

[0033] Figure 1 The figure is a schematic diagram of the system of the application.

[0034] Figure labels: S1-Automatic aluminum phosphide feeding system, S2-Sulfuric acid metering tank, S3-Constant temperature reactor, S4-Pre-condenser, S5-Cryogenic condenser, S6-Heavy weight removal purification column, S7-Cold trap collection device, S8-Cold trap transfer tank, S9-Light weight removal purification column, S10-Low temperature jacketed filling machine, S11-Vacuum buffer tank, S12-Vacuum pump, S13-First-stage alkaline washing tower, S14-Washing circulation pump, S15-Second-stage adsorption tower, S16-Tail gas fan, S17-Exhaust stack, S18-Aluminum phosphide pipeline, S19-Sulfuric acid pipeline, S20-Nitrogen pipeline control valve, S21-Helium pipeline control valve, S22-Phosphine phosphate pipeline, S23-Alkali solution pipeline, S-24-Aluminum phosphide metering control valve, S-25-Sulfuric acid metering control valve. Detailed Implementation

[0035] The present invention will be further described in detail below through specific embodiments.

[0036] like Figure 1 As shown, the present invention includes a fully automatic aluminum phosphide feeding system 1, a sulfuric acid metering tank 2, a constant temperature reaction vessel 3, a purification and cooling system 4, a heavy removal purification column 5, a cold trap collection device 6, a light removal purification column 7, a low temperature filling system 8, an inert gas purging system 9, a vacuum system 10, and a tail gas treatment system 11.

[0037] The fully automatic aluminum phosphide feeding system 1 is equipped with a vacuum silo, with a vacuum pump connected to the top and a constant temperature reactor 3 connected to the bottom via a control valve. The system is equipped with nitrogen and helium inert gases for purging and leak testing. The heavy metal removal and purification column 5 consists of 2-4 adsorption towers, with 1-2 used for adsorption and 1-2 for desorption and regeneration. The adsorbent is sodium lime, molecular sieve, or activated carbon. The adsorption tower is connected to a vacuum system 10 and helium pipelines for adsorption and regeneration of the adsorbent.

[0038] The inert gas purging system 9 includes nitrogen and helium. Nitrogen is used for purging and replacing the equipment and pipelines of the entire unit, while helium is used for leak detection and regeneration of the adsorbent in the equipment, pipelines and connections of the entire unit.

[0039] The constant temperature reactor 3 is a jacketed reactor, with an inert gas purging system 9 and a vacuum system 10 connected to the top of the reactor; the jacket of the reactor is equipped with a heat transfer oil cooling system, and a stirrer is installed at the top; an emergency shut-off valve is installed on the material inlet pipe at the top of the reactor; a remote pressure gauge and a remote thermometer are installed at the top of the reactor; the reactor is equipped with an SIS system and a safety relief system.

[0040] The purification cooling system 4 includes pre-cooling and deep cooling, the pre-cooling temperature is controlled at 0-10℃, and the deep cooling temperature is controlled at -30--10℃; the pre-cooling and deep cooling both adopt heat exchangers, and the heat exchanger type is a shell-and-tube heat exchanger, a jacketed heat exchanger or a plate heat exchanger.

[0041] The cold trap collection device 6 adopts liquid nitrogen condensation, and is matched with multiple cold trap transfer tanks; the temperature of the cold trap collection device 6 is controlled at -110--90℃, the cold trap transfer tank is a mobile storage tank, and is configured with an electric heating or hot water heating system.

[0042] The light removal purification column 7 is connected to the cold trap transfer tank through a pipeline, the light removal purification column 7 is composed of multiple adsorption towers in series, the adsorbent is molecular sieve or activated carbon, and the molecular sieve is selected from 4A molecular sieve, 5A molecular sieve or 13X molecular sieve; the light removal purification column 7 is configured with a flow meter and an adjusting valve through a pipeline.

[0043] The vacuum system 10 includes a vacuum buffer tank, a vacuum pump and a pipeline system, and the vacuum degree is controlled at 90-99kPa.

[0044] The tail gas treatment system 11 is a first-stage alkali washing tower and a second-stage adsorption tower; the alkali solution of the first-stage alkali washing tower is calcium hydroxide solution or sodium hydroxide solution or sodium hypochlorite solution; and the second-stage adsorption tower adopts molecular sieve or activated carbon adsorbent.

[0045] Specifically, the aluminum phosphide raw material from the raw material warehouse is stored in the silo through the aluminum phosphide automatic feeding system 1, is quantitatively added to the constant temperature reaction kettle S3 through the aluminum phosphide quantitative control valve S24 on the aluminum phosphide pipeline S18, and the control valve S24 is closed; the heat conduction oil cooling system in the constant temperature reaction kettle S3 is opened to ensure the normal operation of the cooling system; the nitrogen pipeline control valve S20 connected with the constant temperature reaction kettle S3 is opened to replace the air or other gas in the constant temperature reaction kettle S3; the helium pipeline control valve S21 connected with the constant temperature reaction kettle S3 is opened to detect whether the sealing of the equipment, the pipeline, the instrument and the flange connection is perfect; the vacuum pump connected with the constant temperature reaction kettle S3 is opened to control the pressure of the reaction kettle at -0.01MPa(A), and the nitrogen and helium used for purging and detection are sent to the first-stage alkali washing tower S13 of the tail gas treatment system 11.

[0046] Further, the raw material sulfuric acid is slowly added to the constant temperature reaction kettle S3 through the metering scale and the quantitative control valve S25 on the sulfuric acid pipeline S19 configured in the sulfuric acid metering tank 2, the sulfuric acid addition amount is controlled at 1-10L / min, and the reaction temperature is controlled at 20-60℃.

[0047] Further, the aluminum sulfate solution obtained by the reaction is intermittently filled into the aluminum sulfate barrel and sold as a water treatment agent.

[0048] Further, the obtained gas-phase phosphine product of the reaction is connected by pipeline to a pre-condenser S4, the condensing temperature is controlled at 0-20°C, the particulate matter and moisture therein are removed, and then sent to a deep-cooling condenser S5, the cooling temperature is controlled at -30-10°C, and the moisture in the phosphine product is further removed.

[0049] Further, the phosphine gas from which the particulate matter and moisture are removed is sent to a heavy-purification column S6, and the heavy components such as arsine, metal hydride, hydrogen sulfide, and water in the gas are removed completely by the adsorbent.

[0050] Further, the vacuum pump S12 is started, the pipeline vacuum valve connected to the heavy-purification column S6 after adsorption is opened, the vacuum degree is controlled at 90-99 kPa, the adsorbed components such as arsine, metal hydride, hydrogen sulfide, and water are desorbed and sent to the first alkaline washing tower S13 of the tail gas treatment system 11, so that the adsorbent is regenerated and recycled.

[0051] Further, the phosphine gas from which the heavy components are removed is sent to the cold trap transfer tank S8 in the cold trap collection device S7, liquid nitrogen is used as the cold trap agent, the temperature is controlled at -100-90°C, the phosphine gas is condensed to liquid state, the light components such as nitrogen and oxygen are separated, and sent to the first alkaline washing tower S13 of the tail gas treatment system 11 by the vacuum pump.

[0052] Further, the cold trap transfer tank S8 is taken out from the cold trap collection device S7 and connected to the light-purification column S9. The light-purification column is 2-10 adsorption towers connected in series, and is internally filled with adsorbents such as activated carbon, 4A molecular sieve, 5A molecular sieve, and 13X. The heating system of the cold trap transfer tank S8 is started, the temperature is controlled at -90-80°C, the phosphine liquid in the container is gasified, the carbon monoxide, carbon dioxide, methane, ethane, silane, ethylene, and organic matters above C3 therein are removed, so that the electronic-grade phosphine special gas with the purity of 99.9999% (6N) is obtained and sent to the low-temperature jacketed tank filling machine S10 for condensation, liquefaction, tank filling, and storage.

[0053] Further, the vacuum pump S12 is started, the pipeline vacuum valve connected to the light-purification column S9 after adsorption is opened, the vacuum degree is controlled at 90-99 kPa, the adsorbed components such as carbon monoxide, carbon dioxide, ethylene, ethane, and organic matters above C3 are desorbed and sent to the first alkaline washing tower S13 of the tail gas treatment system 11, so that the adsorbent is regenerated and recycled.

[0054] Further, the purging tail gas, leakage detection tail gas, desorption tail gas and the like from the phosphonium aluminum automatic feeding system S1, the constant temperature reaction kettle S3, the heavy component removal column S6, the cold trap collection device S7, the cold trap transfer tank S8, the light component removal column S9, the low-temperature jacketed tank filling machine S10 and the like are connected to the first alkaline washing tower S13, and the acidic gas in the tail gas is removed by countercurrent absorption of the alkaline washing liquid sprayed by the washing circulating pump S14 and is sent to the second adsorption tower S15 to adsorb the organic components such as ethylene and alkanes in the tail gas, and the treated tail gas is sent to the exhaust cylinder S17 through the tail gas fan S16 for standard emission. The waste liquid generated by washing is collected and treated uniformly.

[0055] The technical solutions of the present application are further explained by examples below.

[0056] The phosphonium aluminum raw material is quantitatively added to the constant temperature reaction kettle S3 through the phosphonium aluminum quantitative control valve S24 on the phosphonium aluminum pipeline S18 from the phosphonium aluminum automatic feeding system 1, 230 kg in total, the heat conduction oil cooling system in the constant temperature reaction kettle S3 is opened to ensure the normal operation of the cooling system, the nitrogen pipeline control valve S20 connected to the constant temperature reaction kettle S3 is opened to replace the air or other gas in the constant temperature reaction kettle S3, the helium pipeline control valve S21 connected to the constant temperature reaction kettle S3 is opened to detect whether the equipment, pipeline, instrument and flange connection are sealed perfectly, and the vacuum pump connected to the constant temperature reaction kettle S3 is opened to control the pressure of the reaction kettle at-0.01 MPa(A), and the nitrogen and helium for purging and detection are sent to the first alkaline washing tower S13 of the tail gas treatment system 11.

[0057] 98% concentrated sulfuric acid 98 kg is quantitatively added to the sulfuric acid metering tank 2, and then 25 kg of pure water is slowly added to the sulfuric acid metering tank 2 to prepare a dilute sulfuric acid of a certain concentration for standby use.

[0058] After the constant temperature reaction kettle S3 is detected to be correct, the quantitative control valve S25 on the sulfuric acid pipeline S19 is opened on the DCS to slowly add sulfuric acid into the constant temperature reaction kettle S3, and the addition amount of sulfuric acid is controlled at 1-10 L / min, the reaction temperature is controlled at 20-60°C, and the gas phase outlet pipeline valve of the constant temperature reaction kettle S3 is opened.

[0059] After the reaction is completed, 1346 kg of aluminum sulfate solution is obtained, which is sold as a water treatment agent.

[0060] The gas phase material obtained from the constant temperature reaction kettle S3 is sequentially sent to the pre-cooler S4 (the condensation temperature is controlled at 0-20°C), the deep cooling condenser S5 (the cooling temperature is controlled at-30- -10°C) and the heavy component removal column S6 to remove the heavy components such as particulate matter, moisture, arsine, metal hydride and hydrogen sulfide in the phosphonium hydrogen primary product, and 107.25 kg of phosphonium hydrogen primary product is obtained, and the components are shown in Table-1:

[0061] Table-1 Components of the phosphonium hydrogen primary product

[0062] Component Mole fraction % Notes Phosphine 99.9435 Oxygen + Argon 4.0757 ppm Nitrogen 526.769 ppm Carbon dioxide 1.6118 ppm Methane 1.1227 ppm Carbon monoxide 0.0247 ppm Ethylene 0.0495 ppm Ethane 0.0069 ppm Acetylene 0.0105 ppm Silane 0.0002 ppm Hydrogen sulfide 0.0003 ppm Arsine 31.4638 ppm

[0063] The raw phosphine gas is sent to the cold trap in the cold trap collection device S7, and the cold trap transfer tank S8 is used, liquid nitrogen is used as the cold trap agent, the temperature is controlled at-100 DEG C to-90 DEG C, the phosphine gas is condensed to liquid state, the light components such as nitrogen and oxygen are separated, and the primary pure phosphine 106.25 kg is obtained, and the components are shown in Table-2.

[0064] Table-2 Components of the primary pure phosphine

[0065]

[0066]

[0067] The cold trap transfer tank S8 is taken out from the cold trap collection device S7, connected to the light removal purification column S9, the heating system of the cold trap transfer tank S8 is started, the temperature is controlled at-90 DEG C to-80 DEG C, the phosphine liquid in the container is gasified, and is sequentially adsorbed by activated carbon, 4A molecular sieve, 5A molecular sieve, 13X adsorbent, and the carbon monoxide, carbon dioxide, methane, ethane, silane, ethylene and C3 above organic matters are removed, so that 100 kg of 99.9999% (6N) purity electronic grade phosphine special gas is obtained, and is sent to the low-temperature jacketed tank filling machine S10 to condense and liquefy and tank filling storage, and the components are shown in Table 3.

[0068] Table-3 Components of the 6N phosphine product

[0069]

[0070]

[0071] Therefore, the product purity of the system and method reaches 99.99998%, and meets the requirements of the electronic industry special gas. The whole system flow is short, the operation is simple, the investment, operation and maintenance costs are reduced, the system safety monitoring is strengthened, and the continuous, stable and safe operation of the system is realized.

[0072] Those skilled in the art will understand that other changes can be made to the example embodiments without departing from the spirit of the application. Likewise, various figures can depict example architectures or other configurations for purposes of the present disclosure, which are used to understand features and functionality that can be included in the present disclosure. The present disclosure is not limited to the example architectures or configurations shown, and the breadth and scope of the present disclosure should not be limited by any of the above-described example embodiments.

Claims

1. A production apparatus for electronic-grade phosphine, characterized in that: The system includes a fully automatic aluminum phosphide feeding system (1), a sulfuric acid metering tank (2), a constant temperature reactor (3), a purification and cooling system (4), a heavy removal purification column (5), a cold trap collection device (6), a light removal purification column (7), a low temperature filling system (8), an inert gas purging system (9), a vacuum system (10), and a tail gas treatment system (11). The fully automatic feeding system for raw aluminum phosphide (1) is equipped with a vacuum silo, with a vacuum pump connected to the top and a constant temperature reactor (3) connected to the bottom through a control valve; the fully automatic feeding system for raw aluminum phosphide (1) is equipped with nitrogen and helium inert gases for purging and leak testing; The heavy removal purification column (5) consists of 2 to 4 adsorption towers, 1 to 2 for adsorption and 1 to 2 for desorption and regeneration; the adsorbent is sodium lime, molecular sieve or activated carbon; the adsorption tower is equipped with a vacuum system (10) and helium pipeline for replacement and regeneration of the adsorbent. The inert gas purging system (9) includes nitrogen and helium. Nitrogen is used for purging and replacing the equipment and pipelines of the entire unit, while helium is used for leak detection and regeneration of the adsorbent in the equipment, pipelines and connections of the entire unit.

2. The production apparatus for electronic-grade phosphine according to claim 1, characterized in that: The constant temperature reactor (3) is a jacketed reactor. The top of the reactor is connected to an inert gas purging system (9) and a vacuum system (10). The jacket of the reactor is equipped with a heat transfer oil cooling system, and a stirrer is installed on the top. An emergency shut-off valve is installed on the material inlet pipe at the top of the reactor. A remote pressure gauge and a remote thermometer are installed on the top of the reactor. The reactor is equipped with an SIS system and a safety relief system.

3. The production apparatus for electronic-grade phosphine according to claim 1, characterized in that: The purification cooling system (4) includes precooling and deep cooling. The precooling temperature is controlled at 0 to 10℃ and the deep cooling temperature is controlled at -30 to -10℃. Both precooling and deep cooling use heat exchangers, which are shell-and-tube heat exchangers, jacketed heat exchangers, or plate heat exchangers.

4. The production apparatus for electronic-grade phosphine according to claim 1, characterized in that: The cold trap collection device (6) uses liquid nitrogen condensation and is equipped with multiple cold trap transfer tanks; the temperature of the cold trap collection device (6) is controlled at -110 to -90℃, and the cold trap transfer tank is a mobile storage tank equipped with an electric heating or hot water heating system.

5. The apparatus for producing electronic-grade phosphine according to claim 1, characterized in that: The light-weight removal purification column (7) is connected to the cold trap transfer tank through a pipeline. The light-weight removal purification column (7) is composed of multiple adsorption towers connected in series. The adsorbent is molecular sieve or activated carbon. The molecular sieve is 4A molecular sieve, 5A molecular sieve or 13X molecular sieve. The light-weight removal purification column (7) is equipped with a flow meter and regulating valve through a pipeline.

6. The production apparatus for electronic-grade phosphine according to claim 1, characterized in that: The vacuum system (10) includes a vacuum buffer tank, a vacuum pump and a pipeline system, with the vacuum level controlled at 90 to 99 kPa.

7. The production apparatus for electronic-grade phosphine according to claim 1, characterized in that: The exhaust gas treatment system (11) consists of a primary alkaline scrubbing tower and a secondary adsorption tower. The alkaline solution in the primary alkaline scrubbing tower is calcium hydroxide solution, sodium hydroxide solution, or sodium hypochlorite solution. The secondary adsorption tower uses molecular sieve or activated carbon adsorbent.

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