A method and apparatus for improving the detoxification displacement efficiency of a material containing carbonyl groups

By using alternating hot and cold nitrogen passivation and pulsed pressure boosting-depressurization replacement processes, the problems of low material replacement efficiency and safety hazards of carbonyl compounds in carbonyl metallurgy have been solved, achieving efficient and safe material detoxification.

CN122256701APending Publication Date: 2026-06-23JINCHUAN GROUP NICKEL COBALT CO LTD

Patent Information

Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
JINCHUAN GROUP NICKEL COBALT CO LTD
Filing Date
2026-03-19
Publication Date
2026-06-23

AI Technical Summary

Technical Problem

Existing technologies for the displacement and detoxification of carbonyl materials in carbonyl metallurgy are inefficient and incomplete, posing safety hazards and failing to simultaneously balance displacement efficiency and production safety.

Method used

The process employs alternating hot and cold nitrogen passivation and pulsed pressurization-depressurization replacement technology, combined with a gas distribution structure and interlocking control system. By alternating the use of hot and cold nitrogen for multiple pulsed operations, the material is completely replaced.

Benefits of technology

It significantly improves the efficiency and thoroughness of replacement, shortens the replacement time, avoids material caking and high-temperature scalding problems, and reduces production costs and safety risks.

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Abstract

The application discloses a method and device for improving detoxification replacement efficiency of materials containing carbonyl substances, and belongs to the technical field of carbonylation metallurgy safety production. The application adopts the mode of hot nitrogen gas and cold nitrogen gas alternately passivating replacement, replaces the traditional single cold nitrogen gas continuous purging process, and adopts multiple pressure increase-pressure release pulse type operation for each round of replacement; the supporting device is provided with a parallel hot nitrogen gas supply unit and a cold nitrogen gas supply unit, a DCS interlocking control system and an annular tangent air inlet pipeline at the bottom of a storage bin. The application greatly improves the replacement efficiency and completeness of the materials containing carbonyl substances, shortens the replacement time by more than 80%, avoids problems such as material hardening, channeling and burning of material bags caused by continuous high temperature, guarantees continuous, stable and safe operation of carbonylation metallurgy production, and reduces production cost.
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Description

Technical Field

[0001] This invention belongs to the field of carbonyl metallurgical safety production technology, specifically relating to a method and apparatus for improving the detoxification and replacement efficiency of materials containing carbonyl groups. Background Technology

[0002] Carbonyl metallurgy is a core metallurgical technology that utilizes metal carbonyl compounds for metal extraction and purification. The production of nickel carbonyl is a typical application of this technology. During the production of nickel carbonyl products, incomplete decomposition inevitably leads to the product carrying carbonyl compounds (such as nickel carbonyl) and carbon monoxide. These substances are highly toxic, flammable, and explosive. If detoxification is incomplete, it can easily cause serious safety accidents such as poisoning of personnel on the production site and material fires and explosions.

[0003] Currently, the industry commonly employs a long-term, continuous purging process with cold nitrogen for the displacement and detoxification of materials containing carbonyl compounds. This process has core drawbacks: extremely low displacement efficiency, incomplete displacement, requiring tens of hours of continuous purging, high nitrogen consumption, high production costs, and even after prolonged purging, it is still impossible to completely remove carbonyl compounds from the pores of the material, thus posing a persistent safety hazard.

[0004] To improve the displacement effect, some processes have attempted to use continuous hot nitrogen purging to promote the volatilization and decomposition of carbonyl compounds and improve removal efficiency. However, in actual industrial production, it has been found that this process introduces new production risks: continuous high-temperature purging can cause the powder material to clump together due to heat. The clumped material forms gaps, and the purging gas preferentially flows along the gaps, forming a channeling phenomenon. The carbonyl compounds inside the clumped material cannot be completely displaced and removed. At the same time, continuous high temperature can cause the surface temperature of the material to be too high and the viscosity to increase, leading to problems such as scorching of the material bag and blockage during subsequent discharge, which further affects the continuity and safety of production.

[0005] In summary, existing displacement detoxification technologies for carbonyl-containing materials cannot simultaneously achieve displacement efficiency, thoroughness, and production safety, and have failed to address long-standing pain points in the industry. There is an urgent need to develop an efficient, safe, and stable displacement detoxification technology. Summary of the Invention

[0006] To address the aforementioned deficiencies in existing technologies, the present invention aims to provide a method and apparatus for improving the detoxification and replacement efficiency of materials containing carbonyl compounds. Through core processes of alternating hot and cold nitrogen passivation and pulsed pressure boosting-depressurization replacement, combined with a matching gas distribution structure and interlocking control system, the method significantly improves replacement efficiency and thoroughness while completely avoiding problems such as material caking, gas channeling, and high-temperature scorching. This ensures continuous, stable, and safe operation of carbonyl metallurgical production and significantly reduces production costs.

[0007] To achieve the above-mentioned objectives, the technical solution adopted by the present invention is as follows: This invention provides a method for improving the detoxification and replacement efficiency of materials containing carbonyl groups, applicable to the carbonyl metallurgical industry, comprising the following steps: (1) Gas source preparation: Prepare cold nitrogen gas with stable pressure, and hot nitrogen gas heated to a preset temperature with stable pressure; (2) Alternating passivation and replacement: The material in the storage silo is passivated and replaced by alternating hot nitrogen replacement stage and cold nitrogen replacement stage; the hot nitrogen replacement stage and the cold nitrogen replacement stage both adopt multiple repeated pressure increase-depressurization pulse operation to replace the traditional continuous purging. (3) Automatic interlock control: The DCS control system is used to interlock control the switching of hot nitrogen and cold nitrogen, the pressure in the storage silo, and the heating temperature of hot nitrogen to achieve automatic replacement throughout the process.

[0008] Furthermore, the heating temperature of the hot nitrogen is controlled at 120℃~140℃. This temperature range can effectively promote the volatilization and decomposition of carbonyl compounds, greatly improve the replacement efficiency, and avoid the rapid caking of materials due to excessively high temperatures. The inlet pressure of the hot nitrogen is controlled at 80KPa, and the inlet pressure of the cold nitrogen is controlled at 80KPa to ensure stable inlet pressure and avoid pressure fluctuations from impacting the material bed.

[0009] Furthermore, in the pressurization-depressurization pulse operation, the target pressure for a single pressurization is 50 kPa, and the target pressure for a single depressurization is 10 kPa. That is, in each pulse operation, the corresponding amount of nitrogen is injected into the storage silo until the pressure inside reaches 50 kPa, then the gas intake stops, and the pressure is depressurized until the pressure inside the silo drops to 10 kPa, completing one pulse operation. This pulse operation, through the periodic alternation of pressure, allows nitrogen to fully penetrate into the pores of the material, thoroughly breaking the gas channels formed by continuous purging, eliminating displacement dead zones inside the caking material, and significantly improving the thoroughness of displacement.

[0010] Furthermore, in the hot nitrogen replacement stage, the pressurization-depressurization pulse operation is repeated 20 times; in the cold nitrogen replacement stage, the pressurization-depressurization pulse operation is repeated 20 times. Through multiple rounds of pulse alternation, the carbonyl compounds and carbon monoxide are fully removed.

[0011] Furthermore, the alternation sequence of the hot nitrogen replacement stage and the cold nitrogen replacement stage is as follows: first, the complete hot nitrogen replacement stage is completed, and then the cold nitrogen replacement stage is switched to complete the replacement. First, through pulse replacement with hot nitrogen, more than 95% of carbonyl compounds and carbon monoxide in the material are rapidly removed, significantly shortening the total replacement time; then, through pulse replacement with cold nitrogen, the material is rapidly cooled while deep replacement is completed, ensuring replacement efficiency and fundamentally solving the problems of caking and scalding caused by high material temperatures.

[0012] On the other hand, the present invention provides an apparatus for improving the detoxification and replacement efficiency of carbonyl-containing materials by implementing the above method, which is applied in the carbonyl metallurgical industry. It includes a storage silo for holding carbonyl-containing materials and a gas source pipeline for supplying nitrogen to the storage silo. The gas source pipeline includes a hot nitrogen supply unit and a cold nitrogen supply unit arranged in parallel. The outlet of the hot nitrogen supply unit and the cold nitrogen supply unit are both connected to the air inlet of the storage silo. The device also includes a DCS control system, which is connected to the hot nitrogen supply unit and the cold nitrogen supply unit respectively, and is used to control the alternating introduction of hot nitrogen and cold nitrogen, as well as the interlocking regulation of pressure and temperature in the pipeline and storage silo. The bottom of the storage silo is provided with an annular air inlet pipe, which is connected to the outlet of the hot nitrogen supply unit and the cold nitrogen supply unit. The annular air inlet pipe is provided with multiple air inlet contacts that are tangent to the outer wall of the storage silo and extend upward.

[0013] Furthermore, the hot nitrogen supply unit includes a first pressure-reducing valve group, a nitrogen heater, a second pressure-reducing valve group, a hot nitrogen buffer tank, a hot nitrogen inlet regulating valve, and a hot nitrogen inlet check valve arranged sequentially along the inlet direction. The inlet end of the first pressure-reducing valve group is connected to a 0.6MPa nitrogen source, and the outlet end is connected to the inlet end of the nitrogen heater through a pipeline, which is used to reduce the pressure of the source nitrogen to 0.4MPa before sending it into the nitrogen heater. The nitrogen heater is used to heat the nitrogen to 120℃~140℃, and the second pressure-reducing valve group is used to reduce the pressure of the heated hot nitrogen to 80KPa before sending it into the hot nitrogen buffer tank. The hot nitrogen inlet regulating valve is connected to the DCS control system signal and is used to control the on / off and flow regulation of hot nitrogen to the storage silo.

[0014] Furthermore, the cold nitrogen supply unit includes a third pressure reducing valve group, a cold nitrogen buffer tank, a cold nitrogen inlet regulating valve, and a cold nitrogen inlet check valve arranged sequentially along the inlet direction; the inlet end of the third pressure reducing valve group is connected to a 0.6MPa nitrogen source, which is used to reduce the pressure of the source nitrogen to 80KPa before sending it into the cold nitrogen buffer tank; the cold nitrogen inlet regulating valve is connected to the DCS control system signal, which is used to control the on / off of cold nitrogen to the storage silo and to regulate the flow rate.

[0015] Furthermore, the annular air inlet pipe is arranged in a single layer, circumferentially surrounding the bottom of the storage silo; the number of air inlet contacts is n, with four air inlet contacts configured at angle intervals α, where α = 360° / n. This annular tangential air inlet structure allows nitrogen to form a uniform swirling flow along the inner wall of the storage silo, fully covering the entire cross-section of the storage silo, completely avoiding local displacement dead zones caused by air inlet deviation, and further enhancing the displacement effect.

[0016] Furthermore, the hot nitrogen buffer tank is equipped with a hot nitrogen pressure relief valve assembly and an emptying pipeline, and the cold nitrogen buffer tank is equipped with a cold nitrogen pressure relief valve assembly and an emptying pipeline, for automatic release in case of overpressure, ensuring safe operation of the device; the storage silo is equipped with a remote pressure gauge, which is connected to the DCS control system. The DCS control system, based on the pressure detection signal from the storage silo, interlocks and controls the opening and closing of the hot nitrogen inlet regulating valve and the cold nitrogen inlet regulating valve, to achieve precise closed-loop pressure control.

[0017] Compared with the prior art, the present invention has the following significant advantages: 1. This invention pioneers a core process of alternating hot and cold nitrogen passivation and replacement, combined with a pulsed pressurization-depressurization operation mode, which completely solves the two-way pain points of existing technologies: First, through hot nitrogen pulse replacement, the high temperature promotes the volatilization and decomposition of carbonyl compounds, quickly removing most of the toxic media and significantly shortening the replacement time; then, through cold nitrogen pulse replacement, the material is cooled down while deep replacement is completed, which avoids problems such as material caking, channeling, and scorching of material bags caused by continuous high temperature, and also solves the defects of low efficiency and incompleteness of single cold nitrogen replacement. It achieves simultaneous improvement in replacement efficiency, replacement thoroughness and production safety, and the total replacement time is reduced by more than 80% in industrial applications.

[0018] 2. The pulsed pressurization-depressurization operation of the present invention, through the periodic alternation of pressure, allows nitrogen to fully penetrate into the pores of the material, completely breaking the gas channel formed by continuous purging, eliminating the displacement dead zone inside the material, making the displacement and detoxification more thorough, and fundamentally reducing production safety hazards.

[0019] 3. The device of the present invention is equipped with a DCS full-process interlocking control system, which realizes automatic switching between hot and cold nitrogen and precise closed-loop regulation of pressure and temperature without manual intervention, ensuring continuous and stable operation of the replacement process, reducing the safety risks of manual operation, and significantly improving the accuracy and stability of process control.

[0020] 4. The present invention designs a single-layer annular tangential air inlet gas distribution structure at the bottom of the storage silo, which makes nitrogen form a uniform swirling flow in the storage silo, greatly improving the uniformity of gas distribution, avoiding the problem of incomplete local replacement caused by air inflow deviation, further enhancing the replacement effect and improving the replacement efficiency.

[0021] 5. The process and apparatus of the present invention are not only applicable to the displacement detoxification of carbonyl-containing materials in the carbonyl metallurgical industry, but also provide a general solution for the efficient displacement treatment of other volatile, toxic and harmful media, and have broad application value. Attached Figure Description

[0022] Figure 1 This is a schematic diagram of the device for improving the detoxification and replacement efficiency of materials containing carbonyl groups according to the present invention.

[0023] In the diagram: 1-First pressure reducing valve assembly, 2-0.4MPa nitrogen pipeline, 3-Nitrogen heater, 4-Local pressure gauge, 5-Remote temperature gauge, 6-Remote pressure gauge, 7-0.4MPa hot nitrogen pipeline, 8-Control valve assembly connecting heater and buffer tank, 9-Second pressure reducing valve assembly, 10-Hot nitrogen pressure relief valve assembly and venting pipeline, 11-Hot nitrogen buffer tank, 12-Hot nitrogen pipeline to storage silo, 13-Storage silo inlet ring pipeline, 14-Hot nitrogen inlet regulating valve. 15-Hot nitrogen inlet check valve, 16-Storage silo, 17-Storage silo remote pressure gauge, 18-Cold nitrogen inlet check valve, 19-Cold nitrogen inlet regulating valve, 20-Cold nitrogen to storage silo pipeline, 21-Cold nitrogen buffer tank remote pressure gauge, 22-Cold nitrogen buffer tank, 23-Cold nitrogen pressure relief valve assembly and venting pipeline, 24-0.6MPa pressure reduction to 0.08MPa nitrogen pipeline, 25-Cold nitrogen to buffer tank pipeline inlet regulating valve, 26-Third pressure reducing valve assembly. Detailed Implementation

[0024] The present invention will be further described in detail below with reference to the accompanying drawings and specific embodiments. It should be noted that the following embodiments are only used to explain the technical solutions of the present invention and are not intended to limit the scope of protection of the present invention. Any equivalent substitutions or conventional modifications based on the technical solutions of the present invention shall fall within the scope of protection of the present invention.

[0025] The device for improving the detoxification and replacement efficiency of materials containing carbonyl groups provided in this embodiment has the following structure: Figure 1 As shown, this is a displacement and detoxification process for nickel carbonyl powder materials used in the production of nickel carbonyl.

[0026] The device includes a storage silo 16 for holding carbonyl-containing materials, a gas supply pipeline for supplying nitrogen to the storage silo 16, and a DCS control system.

[0027] The gas supply pipeline includes a hot nitrogen supply unit and a cold nitrogen supply unit arranged in parallel. The outlets of both the hot nitrogen supply unit and the cold nitrogen supply unit are connected to the air inlet annular pipeline 13 at the bottom of the storage silo 16.

[0028] The hot nitrogen supply unit includes, in sequence along the air inlet direction, a first pressure reducing valve group 1, a 0.4MPa nitrogen pipeline 2, a nitrogen heater 3, a 0.4MPa hot nitrogen pipeline 7, a heater-buffer tank connection control valve group 8, a second pressure reducing valve group 9, a hot nitrogen buffer tank 11, a hot nitrogen to storage silo pipeline 12, a hot nitrogen inlet regulating valve 14, and a hot nitrogen inlet check valve 15.

[0029] The inlet of the first pressure-reducing valve group 1 is connected to the factory's 0.6MPa utility nitrogen source, and the outlet is connected to the inlet of the nitrogen heater 3 via a 0.4MPa nitrogen pipeline 2. The first pressure-reducing valve group 1 is used to reduce the pressure of the 0.6MPa source nitrogen to 0.4MPa before sending it to the nitrogen heater 3. The nitrogen heater 3 uses electric heating to heat the 0.4MPa nitrogen to 120℃~140℃. The heated nitrogen is then sent to the second pressure-reducing valve group 9 via the 0.4MPa hot nitrogen pipeline 7 and the control valve group 8. The second pressure-reducing valve group 9 reduces the pressure of the hot nitrogen to 80KPa before sending it to the hot nitrogen buffer tank 11. The hot nitrogen buffer tank 11 is used to stabilize the pressure and flow rate of the hot nitrogen. The outlet of the hot nitrogen buffer tank 11 is connected to the hot nitrogen to the storage silo pipeline 12, which is then connected in sequence to the hot nitrogen inlet regulating valve 14 and the hot nitrogen inlet check valve 15, and finally connected to the inlet annular pipeline 13 of the storage silo 16.

[0030] The hot nitrogen supply unit is also equipped with a local pressure gauge 4, a remote pressure gauge 6, and a remote temperature gauge 5. The local pressure gauge 4 and the remote pressure gauge 6 are installed on the outlet pipeline of the nitrogen heater 3 to monitor the pressure of the heated nitrogen in real time. The remote temperature gauge 5 is installed at the outlet of the nitrogen heater 3 and is interlocked with the heating module of the nitrogen heater 3 to automatically adjust the heating power and stably control the outlet temperature of the hot nitrogen at 130℃±5℃. The top of the hot nitrogen buffer tank 11 is equipped with a hot nitrogen pressure relief valve assembly and a venting pipeline 10 for automatic release in case of overpressure, ensuring system safety.

[0031] The cold nitrogen supply unit includes a third pressure reducing valve group 26 arranged sequentially along the air inlet direction, a 0.6MPa pressure-reducing nitrogen pipeline 24, a cold nitrogen to buffer tank pipeline inlet regulating valve 25, a cold nitrogen buffer tank 22, a cold nitrogen to storage silo pipeline 20, a cold nitrogen inlet regulating valve 19, and a cold nitrogen inlet check valve 18.

[0032] The inlet of the third pressure reducing valve assembly 26 is connected to the plant's 0.6MPa utility nitrogen source, used to directly reduce the pressure of the 0.6MPa source nitrogen to 80KPa, and then send it to the cold nitrogen buffer tank 22 via nitrogen pipeline 24 and inlet regulating valve 25. The cold nitrogen buffer tank 22 is used to stabilize the pressure and flow rate of the cold nitrogen. The outlet of the cold nitrogen buffer tank 22 is connected to the cold nitrogen to the storage silo pipeline 20, and then sequentially connected to the cold nitrogen inlet regulating valve 19 and the cold nitrogen inlet check valve 18, finally connecting to the inlet annular pipeline 13 of the storage silo 16.

[0033] The cold nitrogen buffer tank 22 is equipped with a remote pressure gauge 21, which is interlocked with the inlet regulating valve 25 to stably control the pressure inside the cold nitrogen buffer tank 22 at 80 kPa. The top of the cold nitrogen buffer tank 22 is equipped with a cold nitrogen pressure relief valve assembly and an venting pipeline 23 for overpressure relief to ensure system safety.

[0034] A single-layer annular air inlet pipe 13 is provided at the bottom of the storage silo 16. The annular air inlet pipe 13 is arranged circumferentially around the bottom of the storage silo 16, and multiple air inlet contacts are provided on the annular air inlet pipe 13 that are tangential to the outer wall of the storage silo 16 and extend upward. In this embodiment, there are a total of 16 air inlet contacts, with 4 air inlet contacts arranged at 90° intervals, so that nitrogen gas forms a swirling flow along the inner wall of the storage silo 16 and is evenly distributed throughout the entire cross-section of the storage silo, avoiding air inlet deviation.

[0035] The storage silo 16 is equipped with a remote pressure gauge 17, which is connected to the DCS control system. The DCS control system is connected to the hot nitrogen inlet regulating valve 14, the cold nitrogen inlet regulating valve 19, the nitrogen heater 3, and the signals of each remote instrument to realize automatic interlocking control of the entire process.

[0036] The method for improving the detoxification and replacement efficiency of materials containing carbonyl groups in this embodiment is implemented using the above-mentioned apparatus, and the specific steps are as follows: 1. System Preprocessing The starting device first reduces the pressure of 0.6MPa nitrogen to 0.4MPa through the first pressure reducing valve group 1 and sends it into the nitrogen heater 3. The nitrogen heater 3 is started to heat the nitrogen to 130℃. The heated hot nitrogen is then reduced to 80KPa through the second pressure reducing valve group 9 and sent into the hot nitrogen buffer tank 11. The pressure of the hot nitrogen buffer tank 11 is stabilized at 80KPa through interlock control. At the same time, the nitrogen gas pressure of 0.6MPa is reduced to 80KPa through the third pressure reducing valve group 26 and sent into the cold nitrogen buffer tank 22. The pressure of the cold nitrogen buffer tank 22 is stabilized at 80KPa through interlock control. After the pressure and temperature of the hot and cold nitrogen gases stabilize, the carbonyl nickel powder material to be processed is sent into the storage silo 16, and the automatic replacement program is started.

[0037] 2. Hot nitrogen replacement stage The DCS control system automatically opens the hot nitrogen inlet regulating valve 14 to fill the storage silo 16 with hot nitrogen at 130°C. When the remote pressure gauge 17 of the storage silo detects that the pressure inside the silo has risen to 50 kPa, the DCS control system automatically closes the hot nitrogen inlet regulating valve 14 to stop the gas intake. After maintaining the pressure for 10 seconds, the pressure relief valve of the storage silo is opened to release the pressure inside the silo to 10 kPa, thus completing a single hot nitrogen pulse operation. Repeat the pressurization-holding-depressurization pulse operation 20 times to complete the hot nitrogen replacement stage. In this stage, the high temperature of hot nitrogen rapidly removes more than 95% of the carbonyl nickel and carbon monoxide from the material. At the same time, the pulsed pressure changes allow the hot nitrogen to fully penetrate into the pores of the material, avoiding the channeling problem caused by continuous purging.

[0038] 3. Cold nitrogen replacement stage After the hot nitrogen replacement stage is completed, the DCS control system automatically closes the hot nitrogen inlet regulating valve 14 and switches to open the cold nitrogen inlet regulating valve 19 to fill the storage silo 16 with room temperature cold nitrogen. When the remote pressure gauge 17 of the storage silo detects that the pressure inside the silo has risen to 50 kPa, the DCS control system automatically closes the cold nitrogen inlet regulating valve 19 to stop the gas intake. After maintaining the pressure for 10 seconds, the pressure relief valve of the storage silo is opened to release the pressure inside the silo to 10 kPa, thus completing a single cold nitrogen pulse operation. Repeat the pressurization-holding-depressurization pulse operation 20 times to complete the cold nitrogen replacement stage. In this stage, the material is rapidly cooled down to room temperature using cold nitrogen, while simultaneously removing residual carbonyl compounds, thus avoiding the problems of high-temperature caking and scalding during discharge.

[0039] 4. Replacement complete After the cold nitrogen purging stage is completed, the system automatically stops running and tests the material in the storage silo. The residual amount of carbonyl nickel in the material is lower than the industry safety limit, and the material temperature is room temperature, so it can be directly discharged and packaged.

[0040] Compared with the traditional cold nitrogen continuous purging process, this embodiment reduces the total replacement time from 12 hours to 2 hours, increases the replacement efficiency by 83%, reduces nitrogen consumption by 75%, and eliminates material caking and residue. There are no scalding or blockage problems during the discharge process, which completely eliminates safety hazards in the production process and significantly reduces production costs.

Claims

1. A method for improving the detoxification and replacement efficiency of materials containing carbonyl compounds, applied in the carbonyl metallurgical industry, comprising introducing nitrogen gas into a storage silo containing materials containing carbonyl compounds to detoxify and replace the materials, characterized in that... Includes the following steps: (1) Gas source preparation: Prepare cold nitrogen gas with stable pressure, and hot nitrogen gas heated to a preset temperature with stable pressure; (2) Alternating passivation and replacement: The material in the storage silo is passivated and replaced by alternating hot nitrogen replacement stage and cold nitrogen replacement stage; the hot nitrogen replacement stage and the cold nitrogen replacement stage both adopt multiple repeated pressure increase-depressurization pulse operation to replace continuous purging. (3) Automatic interlock control: The DCS control system is used to interlock control the switching of hot nitrogen and cold nitrogen, the pressure in the storage silo, and the heating temperature of hot nitrogen to achieve automatic replacement throughout the process.

2. The method according to claim 1, characterized in that, The heating temperature of the hot nitrogen is controlled at 120℃~140℃, and the inlet pressure of the hot nitrogen is controlled at 80KPa; the inlet pressure of the cold nitrogen is controlled at 80KPa.

3. The method according to claim 1, characterized in that, In the pressurization-depressurization pulse operation, the target pressure for a single pressurization is 50 kPa, and the target pressure for a single depressurization is 10 kPa. That is, in each pulse operation, the corresponding nitrogen gas is injected into the storage silo until the pressure inside the silo reaches 50 kPa, then the gas intake is stopped, and the pressure is depressurized until the pressure inside the silo drops to 10 kPa, thus completing a single pulse operation.

4. The method according to claim 3, characterized in that, During the hot nitrogen purging phase, the pressure boosting-depressurization pulse operation is repeated 20 times; during the cold nitrogen purging phase, the pressure boosting-depressurization pulse operation is repeated 20 times.

5. The method according to claim 1, characterized in that, The alternation sequence between the hot nitrogen replacement stage and the cold nitrogen replacement stage is as follows: first, complete the hot nitrogen replacement stage, and then switch to the cold nitrogen replacement stage to complete the replacement.

6. A device for improving the detoxification and replacement efficiency of carbonyl-containing materials, applied in the carbonyl metallurgical industry, comprising a storage silo for holding carbonyl-containing materials and a gas source pipeline for supplying nitrogen to the storage silo, characterized in that, The gas supply pipeline includes a hot nitrogen supply unit and a cold nitrogen supply unit arranged in parallel, and the outlets of the hot nitrogen supply unit and the cold nitrogen supply unit are connected to the air inlet of the storage silo. The device also includes a DCS control system, which is connected to the hot nitrogen supply unit and the cold nitrogen supply unit respectively, and is used to control the alternating introduction of hot nitrogen and cold nitrogen, as well as the interlocking regulation of pressure and temperature in the pipeline and storage silo. The bottom of the storage silo is provided with an annular air inlet pipe, which is connected to the outlet of the hot nitrogen supply unit and the cold nitrogen supply unit. The annular air inlet pipe is provided with multiple air inlet contacts that are tangent to the outer wall of the storage silo and extend upward.

7. The apparatus according to claim 6, characterized in that, The hot nitrogen supply unit includes a first pressure reducing valve group, a nitrogen heater, a second pressure reducing valve group, a hot nitrogen buffer tank, a hot nitrogen inlet regulating valve, and a hot nitrogen inlet check valve arranged sequentially along the inlet direction. The inlet end of the first pressure reducing valve group is connected to a 0.6MPa nitrogen source, and the outlet end is connected to the inlet end of the nitrogen heater through a pipeline, which is used to reduce the pressure of the source nitrogen to 0.4MPa before sending it into the nitrogen heater. The nitrogen heater is used to heat the nitrogen to 120℃~140℃. The second pressure reducing valve group is used to reduce the pressure of the heated hot nitrogen to 80KPa before sending it into the hot nitrogen buffer tank. The hot nitrogen inlet regulating valve is connected to the DCS control system signal and is used to control the on / off and flow rate regulation of hot nitrogen to the storage silo.

8. The apparatus according to claim 6, characterized in that, The cold nitrogen supply unit includes a third pressure reducing valve group, a cold nitrogen buffer tank, a cold nitrogen inlet regulating valve, and a cold nitrogen inlet check valve arranged sequentially along the inlet direction. The inlet end of the third pressure reducing valve group is connected to a 0.6MPa nitrogen source, which is used to reduce the pressure of the source nitrogen to 80KPa before sending it into the cold nitrogen buffer tank. The cold nitrogen inlet regulating valve is connected to the DCS control system and is used to control the on / off of cold nitrogen to the storage silo and to regulate the flow rate.

9. The apparatus according to claim 6, characterized in that, The annular air intake pipe is arranged in a single layer and is set around the bottom of the storage silo in a circumferential manner; the number of air intake contacts is n, and 4 air intake contacts are configured at an angle interval α, where α=360° / n.

10. The apparatus according to claim 7 or 8, characterized in that, The hot nitrogen buffer tank is equipped with a hot nitrogen pressure relief valve assembly and an emptying pipeline, and the cold nitrogen buffer tank is equipped with a cold nitrogen pressure relief valve assembly and an emptying pipeline; the storage silo is equipped with a remote pressure gauge, which is connected to the DCS control system. The DCS control system interlocks and controls the opening and closing of the hot nitrogen inlet regulating valve and the cold nitrogen inlet regulating valve based on the pressure detection signal from the storage silo.