A gas-liquid separator for separating diazomethane from a diazomethane mixed solution

Abstract

This invention provides a gas-liquid separator for separating diazonium methane from a diazonium methane mixture. The separator comprises an upper cylinder, a middle cylinder, and a lower cylinder connected sequentially from top to bottom. The upper cylinder has a gas outlet at its top center, surrounded by gas moisture detection ports, diazonium methane content detection ports, gas temperature detection ports, and an explosion vent. A pressure detection port is located on the side. The middle cylinder has a refrigerant inlet and a refrigerant outlet at its upper part, and a refrigerant coil is installed inside the middle cylinder. The refrigerant coil inlet is connected to the refrigerant outlet, and the refrigerant coil outlet is connected to the refrigerant outlet. The lower cylinder has a liquid level-above gas inlet and a liquid level-below gas inlet at its upper part. The liquid level-above gas inlet is connected to a gas distributor above the liquid level via a pipe, and the liquid level-below gas inlet is connected to a gas distributor below the liquid level via a pipe. A feed inlet is located on the middle side wall of the lower cylinder. This gas-liquid separator offers high gas-liquid separation efficiency, is explosion-proof, and can be used for continuous automated production.

Description

Technical Field

[0001] This invention belongs to the field of gas-liquid separation technology, and specifically relates to a gas-liquid separator for separating diazonium methane from a diazonium methane mixed solution. Background Technology

[0002] Diazomethane is an important chemical raw material. During its preparation, the addition of an aqueous phase results in the diazonethane gas carrying a large amount of liquid droplets and water vapor, affecting subsequent chemical reactions. Therefore, gas-liquid separation of diazonethane gas is necessary. Gas-liquid separators are crucial equipment in modern process industries. Currently, industrial gas-liquid separators are generally single-stage separators with a gas-liquid separator cylinder. The top of the cylinder has a gas phase outlet pipe, the bottom has a liquid phase outlet pipe, and the middle has an inlet diffuser. A demister is installed above the inlet diffuser. During operation, the gas and liquid phases enter the gas-liquid separator through the inlet diffuser for flash evaporation separation. A large amount of liquid phase flows to the bottom of the separator, while a large amount of gas phase carries liquid droplets upwards. Depending on the gravity of the droplets and the different heights of the gas phase space between the inlet diffuser and the demister, droplets of different sizes are separated. Simultaneously, the demister can coalesce the remaining droplets entrained in the gas phase. However, for special gases such as diazomethane, existing gas-liquid separators cannot meet the requirements of sufficient liquid removal, explosion-proof safety, and automated continuous production. Summary of the Invention

[0003] To address the aforementioned problems, this invention provides a gas-liquid separator for separating diazonium methane from a diazonium methane mixed solution, which has advantages such as high gas-liquid separation efficiency, safety and explosion protection, and continuous automated production capability.

[0004] To achieve the above objectives, the present invention adopts the following technical solution:

[0005] A gas-liquid separator for separating diazonium methane from a mixed solution includes an upper cylinder, a middle cylinder, and a lower cylinder. The upper part of the middle cylinder is connected to the upper cylinder via a flange, and the lower part is connected to the lower cylinder via a flange. An outlet is located at the center of the top of the upper cylinder, and around the outlet are gas moisture detection ports, diazonium methane content detection ports, gas temperature detection ports, and an upper cylinder explosion vent. A pressure detection port is located on the side. A refrigerant inlet and a refrigerant outlet are located at the upper part of the middle cylinder, and a refrigerant coil is installed inside the middle cylinder. The refrigerant coil inlet is connected to the refrigerant inlet, and the refrigerant coil outlet is connected to the refrigerant outlet. The refrigerant coil is supported by a support plate. The lower cylinder is fixedly connected to the inner wall of the middle cylinder. The upper part of the lower cylinder has a liquid level gas inlet and a liquid level gas inlet. The liquid level gas inlet is connected to the liquid level gas distributor through a pipe, and the liquid level gas inlet is connected to the liquid level gas distributor through a pipe. The upper part of the side wall of the lower cylinder is provided with an upper tuning fork level gauge port, a lower cylinder explosion vent, and a lower cylinder pressure sensor port. The lower part of the side wall of the lower cylinder is provided with a lower tuning fork level gauge port and a lower cylinder temperature detection port. The middle side wall of the lower cylinder is provided with a feed port, and the bottom middle position is provided with a drain port. The lower cylinder is fitted with a jacket, with a jacket inlet at the bottom and a jacket outlet at the top.

[0006] Furthermore, the gas distributor on the liquid surface is located at the upper 1 / 3 of the lower cylinder, and the gas distributor below the liquid surface extends into the bottom of the lower cylinder.

[0007] Furthermore, the feed inlet is installed tangentially to the lower cylinder wall, and an exhaust port is also provided on the upper part of the side wall of the lower cylinder.

[0008] Furthermore, the support plate is cylindrical, with its outer wall fixedly connected to the inner wall of the middle cylinder, and the refrigerant coil is fixedly connected to the inner side of the support plate through multiple support brackets.

[0009] Furthermore, an upper support is provided on the upper part of the outer side wall of the middle cylinder, and a lower support is provided on the upper part of the outer side wall of the jacket. The number of upper and lower supports is the same, both being 2-5.

[0010] Furthermore, the temperature detection port of the lower cylinder is positioned opposite to the port of the lower tuning fork level gauge, and the included angle between the temperature detection port of the lower cylinder and the outer wall of the lower cylinder is 60°.

[0011] Furthermore, a spare port is provided on the lower part of the side wall of the middle cylinder, and the two gas-liquid separators are connected in series through the spare port. The two spare ports are connected by a straight pipe, and a safety pressure relief valve is provided on the straight pipe; or the gas-liquid separators are connected in parallel through the spare port, and the two spare ports are connected by a one-way loop.

[0012] The method for separating diazonium methane from a diazonium methane mixture using the above-mentioned gas-liquid separator includes the following steps:

[0013] Step 1: Refrigerant introduction. Cooling water is introduced through the jacket inlet, and low-temperature refrigerant is introduced through the refrigerant coil inlet. After the internal temperature of the gas-liquid separator stabilizes, proceed to Step 2.

[0014] Step 2: The diazomethane mixture solution is introduced into the lower cylinder tangentially from the feed inlet;

[0015] Step 3: Gas-liquid primary separation. Nitrogen gas is simultaneously introduced through both the gas inlet above and below the liquid level. Under the action of the gas distributor below the liquid surface, the nitrogen gas carries the diazonium methane dissolved in the liquid out of the liquid. The nitrogen mixture exiting through the gas distributor above the liquid surface mixes and dilutes with the nitrogen gas and the overflowing diazonium methane, resulting in a water-saturated mixture of diazonium methane and nitrogen gas from the initial gas-liquid separation. This mixture enters the upper cylinder. During the gas-liquid primary separation, the liquid level in the lower cylinder is measured and monitored by tuning fork level gauges installed at the upper and lower tuning fork level gauge ports. If the liquid level exceeds the limit, the liquid is discharged through the drain outlet. When the liquid level in the lower cylinder rises to 1 / 3-2 / 3 of the lower cylinder height, nitrogen gas is introduced through the nitrogen inlet below the liquid level.

[0016] Step 4: Secondary gas-liquid separation. The diazonium methane and nitrogen mixture entering the middle cylinder liquefies the water vapor in the gas under the deep condensation of the refrigerant coil. The water vapor flows down along the refrigerant coil and enters the lower cylinder. The diazonium methane after deep condensation and liquid removal enters the upper cylinder.

[0017] Step 5: The water content, diazonium content, gas temperature, and pressure in the diazonium gas are tested inside the upper cylinder. Qualified diazonium gas enters the subsequent reaction equipment for reaction, while unqualified diazonium gas undergoes acid quenching treatment.

[0018] Furthermore, in step one, the temperature of the cooling water flowing into the jacket is -10 to 15°C, maintaining the temperature inside the lower cylinder at 0 to 20°C. The temperature of the refrigerant flowing into the refrigerant coil is -40 to 25°C, maintaining the temperature inside the middle cylinder at less than -30°C. The pressure inside the lower, middle, and upper cylinders is controlled to be less than 2 kg. If the pressure exceeds the limit, the explosion vent in the upper or lower cylinder is opened. In step four, the moisture content of diazonium methane inside the upper cylinder is less than 0.5 g / m³.

[0019] Furthermore, the volume content of diazonium methane in the nitrogen gas exiting the gas-liquid separator does not exceed 14.7%, and the nitrogen gas flow rate is 39-624 L / min; the volume content of diazonium methane in the air does not exceed 3.9%, and the air flow rate is 377-2352 L / min.

[0020] Using the gas-liquid separator described in this invention, diazomethane containing droplets enters the lower cylinder tangentially at a lower temperature. The liquid enters the lower cylinder, which is equipped with a jacket to allow cooling water to be introduced, reducing the temperature of the lower cylinder and decreasing the evaporation of the liquid entering the lower cylinder. The lower cylinder is equipped with a temperature detection port with a temperature sensor for automatic temperature monitoring. After setting the temperature of the lower cylinder, the flow rate of cooling water entering the jacket can be controlled via feedback from the control system. The lower cylinder has two nitrogen inlets, each connected to a gas distributor. One gas distributor is introduced into the bottom of the lower cylinder and immersed in the liquid. After nitrogen is introduced, the gas distributor disperses the nitrogen into micron-sized bubbles, carrying away the diazomethane gas in the liquid and reducing the gas content in the liquid. The other gas distributor is located above the liquid surface, dispersing the nitrogen entering the lower cylinder to ensure thorough mixing with the diazomethane. The dilute diazomethane then enters the middle cylinder for deep condensation and deliquescence. To maintain a constant liquid level in the lower cylinder, tuning fork level gauges are installed at both the upper and lower tuning fork level gauge ports to monitor the liquid level. If the level is too high, a solenoid valve installed at the drain outlet will open to discharge the liquid. To prevent ice buildup and blockage during the cryogenic treatment of the middle cylinder, which could lead to increased pressure and potential risks in the lower cylinder, a pressure sensor is installed at the lower cylinder pressure sensor port to monitor the pressure in real time. When the pressure exceeds a set value, a feedback control mechanism opens the lower cylinder's explosion vent to reduce the pressure. Diazomethane, after cryogenic treatment in the middle cylinder, enters the upper cylinder. A pressure sensor is installed at the upper cylinder's pressure detection port to monitor the pressure. If the pressure exceeds a set value, a feedback control mechanism opens the upper cylinder's explosion vent to reduce the pressure. Simultaneously, a gas temperature sensor and a diazonium methane content sensor are installed in the upper cylinder to monitor the diazonium methane quality in real time. If the diazonium methane quality is acceptable, it is introduced into subsequent reaction equipment for chemical reaction; if the quality is unacceptable, acid quenching is performed.

[0021] A saturated water vapor diazomethane mixture was obtained through a single gas-liquid separation process, with a water content of approximately 10 g / m³, significantly reducing the moisture content. Further moisture reduction was achieved by using ultra-low temperatures in the refrigerant coil and controlling the flow rate of the generated nitrogen or air-diazomethane mixture, further reducing the moisture content to 0.5 g / m³. This moisture content is perfectly adequate for an anhydrous reaction system, avoiding the cumbersome and industrially unsustainable nature of existing dehydration processes. Nitrogen gas was introduced to dilute the diazomethane to a safe level of 14.7%, with actual operation controlled within 12%. Real-time monitoring ensured system safety. An automated control system (monitoring pressure, temperature, and diazomethane concentration online, with signals transmitted to the PLC control cabinet in the field and simultaneously to the central control room) ensured that pressure exceeding a certain range was automatically released by both upper and lower pressure relief valves, and that the system automatically shut down and replenished nitrogen when the concentration was too high, further guaranteeing safety.

[0022] To further improve safety and reaction continuity, two gas-liquid separators as described in this invention can be used in series. The two separators are connected via a spare port on the middle cylinder and a safety valve is added. When the upper part of the first separator becomes blocked due to cooling, exceeding a certain pressure, the safety valve from the first separator to the second separator opens. This prevents the diazonium methane mixture from the first gas-liquid separation in the first separator from entering the upper cylinder, instead allowing it to enter the middle cylinder of the second separator through the safety valve connected to the spare port for gas-liquid separation. Once the blockage in the upper section of the first separator melts and clears the pipeline, the system switches back to the first separator. This avoids the problem of overpressure inside the separator caused by blockage from the ultra-low temperature ice-water mixture in the middle cylinder, while also preventing waste of raw materials and the generated diazonium methane. The conversion through the two separators facilitates continuous production.

[0023] To enhance production safety and continuity, two gas-liquid separators can be used in parallel. In parallel operation, if the cylinder of the first separator becomes clogged due to cooling and exceeds a certain pressure, the inlet of the first separator closes, and the diazonium methane mixture feed liquid automatically switches to the inlet of the second separator for further separation. Promptly clean the blockage in the cylinder of the first separator, unclog the pipelines, and ensure smooth flow before use. To further enhance gas-liquid separation, the two separators can also be used in series, connecting the outlet of the first separator to the inlet of the second separator for secondary gas-liquid separation of the diazonium methane, thereby reducing its water content.

[0024] The gas-liquid separator of this invention solves the anhydrous problem of diazonium methane by combining gas-liquid separation with deep cryogenic technology, and solves the problem of safe, automated and continuous industrialization of on-site production and use in existing technologies; it also solves the problem of ensuring the safety of diazonium methane by using protective nitrogen or air dilution. Attached Figure Description

[0025] Figure 1 This is a schematic diagram of the gas-liquid separator described in this invention;

[0026] Figure 2 This is a top view of the gas-liquid separator.

[0027] Figure 3 This is a top view of surface AA of the gas-liquid separator.

[0028] Figure 4 This is a schematic diagram showing the series connection of the gas-liquid separator.

[0029] Figure 5 This is a schematic diagram of the gas-liquid separators used in parallel.

[0030] Among them, 1-upper cylinder, 2-middle cylinder, 3-lower cylinder, 101-gas outlet, 102-gas moisture detection port, 103-diazomethane content detection port, 104-gas temperature detection port, 105-upper cylinder explosion vent, 106-pressure detection port, 201-refrigerant inlet, 202-coil outlet, 203-refrigerant coil, 204-support plate, 205-spare port, 206-upper support, 301-gas inlet above liquid level, 302-gas distributor above liquid level, 3 03-Gas inlet below liquid level, 304-Gas distributor below liquid level, 305-Upper tuning fork level gauge port, 306-Lower tuning fork level gauge port, 307-Feed inlet, 308-Drain outlet, 309-Jacket, 310-Lower cylinder temperature detection port, 311-Lower cylinder explosion vent, 312-Pressure sensor port, 313-Lower cylinder exhaust port, 3091-Jacket inlet, 3092-Jacket outlet, 3093-Lower support, 4-Safety valve, 5-Three-way valve, 6-One-way loop circuit. Detailed Implementation

[0031] The present invention will be further described below with reference to the accompanying drawings and specific embodiments. Example

[0032] like Figures 1-3 As shown, a gas-liquid separator for separating diazonium from a diazonium mixed solution includes an upper cylinder 1, a middle cylinder 2, and a lower cylinder 3. The upper part of the middle cylinder 2 is connected to the upper cylinder 1 via a flange, and the lower part is connected to the lower cylinder 3 via a flange. An outlet 101 is opened at the center of the top of the upper cylinder 1. Around the outlet 101 are a gas moisture detection port 102, a diazonium content detection port 103, a gas temperature detection port 104, an upper cylinder explosion vent 105, and a pressure detection port 106 on the side.

[0033] The upper side wall of the middle cylinder 2 is provided with a refrigerant inlet 201 and a refrigerant outlet 202. A spare port 205 is opened at the lower side wall of the middle cylinder 2. A refrigerant coil 203 is provided inside the middle cylinder 2. The inlet of the refrigerant coil 203 is connected to the refrigerant inlet 201, and the outlet is connected to the refrigerant outlet 202. The refrigerant coil 203 is welded and fixed to the inner wall of the middle cylinder 2 through a support plate 204. The lower cylinder 3 has an upper gas inlet 301 and a lower gas inlet 303. The upper gas inlet 301 is connected to a gas distributor 302 above the liquid level via a pipe, and the lower gas inlet 303 is connected to a gas distributor 304 below the liquid level via a pipe. The gas distributor 302 above the liquid level is located at the upper 1 / 3 of the lower cylinder 3, and the gas distributor 304 below the liquid level extends into the bottom of the lower cylinder 3. The upper sidewall of the lower cylinder 3 is provided with an upper tuning fork level gauge port 305, a lower cylinder explosion vent 311, a lower cylinder pressure sensor port 312, and a lower cylinder exhaust port 313. The lower sidewall of the lower cylinder is provided with a lower tuning fork level gauge port 306 and a lower cylinder temperature detection port 310. The middle sidewall of the lower cylinder is provided with a feed inlet 307, and a drain outlet 308 is located at the middle of the bottom. The lower tuning fork level gauge port 306 is positioned opposite to the lower cylinder temperature detection port 310. The angle between the lower cylinder temperature detection port 310 and the outer wall of the lower cylinder 3 is 60°. The feed port 307 is installed tangentially to the cylinder wall of the lower cylinder 3. The upper tuning fork level gauge port 305 and the lower tuning fork level gauge port 306 are located on the same vertical plane. The lower cylinder 3 is fitted with a jacket 309. The jacket 309 has a jacket inlet 3091 at the bottom and a jacket outlet 3092 at the top. The upper support 205 is provided on the upper part of the outer wall of the middle cylinder 2. The lower support 3093 is provided on the upper part of the outer wall of the jacket 309. The number of upper supports 205 and lower supports 3093 is the same, both being two. The support plate 204 is cylindrical, and its outer wall is fixedly connected to the inner wall of the middle cylinder. The refrigerant coil is fixedly connected to the inner side of the support plate through multiple support frames.

[0034] The method for separating diazonium methane from a diazonium methane mixture using the gas-liquid separator in this embodiment specifically includes the following steps:

[0035] Step 1: Refrigerant introduction. Cooling water is introduced through jacket inlet 3091, and low-temperature refrigerant is introduced through refrigerant inlet 201. After the internal temperature of the gas-liquid separator stabilizes, proceed to Step 2.

[0036] Step 2: The diazomethane mixed solution is introduced into the lower cylinder 3 tangentially through the feed inlet 307;

[0037] Step 3: Gas-liquid primary separation. Nitrogen or air is simultaneously introduced through the gas inlet 301 above the liquid level and the gas inlet 303 below the liquid level. Under the action of the gas distributor 304 below the liquid level, the nitrogen or air carries the diazonium methane dissolved in the liquid out of the liquid. The nitrogen and mixed gas coming out of the gas distributor 303 above the liquid level are mixed and diluted with the nitrogen and overflowing diazonium methane to obtain a water-saturated mixture of diazonium methane and nitrogen obtained from the initial gas-liquid separation. This mixture enters the upper cylinder. During the gas-liquid primary separation, the level of the lower cylinder is measured and monitored by the tuning fork level gauges installed at the upper tuning fork level gauge port 305 and the lower tuning fork level gauge port 306. When the level exceeds the limit, the liquid is discharged from the drain port 308 for acid quenching. When the liquid level in the lower cylinder 3 rises to 1 / 3-2 / 3 of the height of the lower cylinder 3, nitrogen is introduced through the gas inlet 303 below the liquid level.

[0038] Step 4: Secondary gas-liquid separation. The diazomethane and nitrogen mixture entering the middle cylinder 2 undergoes deep condensation in the refrigerant coil 203. The water vapor in the gas liquefies and flows down the refrigerant coil 203 into the lower cylinder 3. The diazomethane after deep condensation and liquid removal enters the upper cylinder 1.

[0039] Step 5: The water content, diazonium content, gas temperature, and pressure in the diazonium gas are detected inside the upper cylinder 1. Qualified diazonium gas enters the subsequent reaction equipment for reaction, while unqualified diazonium gas is subjected to acid quenching treatment.

[0040] In step one, the temperature of the cooling water flowing into the jacket 309 is 0-10℃, so that the temperature inside the lower cylinder 3 is maintained at 5-15℃. The temperature of the refrigerant flowing into the refrigerant coil 203 is -35-20℃, so that the temperature inside the middle cylinder 2 is maintained below -25℃. The pressure inside the upper cylinder 1, the middle cylinder 2 and the lower cylinder 3 is controlled to be less than 2 kg. When the pressure exceeds the standard, the explosion vent 311 of the lower cylinder is opened. In step four, the moisture content of diazonium methane in the upper cylinder 1 is less than 0.5 g / m3.

[0041] The volume content of diazonium methane exiting the gas-liquid separator does not exceed 14.7%, and the nitrogen flow rate is 39-624 L / min. The volume content of diazonium methane in the air does not exceed 3.9%, and the air flow rate is 377-2352 L / min. Example

[0042] like Figure 4 As shown, in Example 1, two gas-liquid separators are connected in series through a spare port, and the two spare ports are connected by a straight pipe with a safety relief valve on the straight pipe. Example

[0043] like Figure 5As shown, in Example 1, two gas-liquid separators are connected in parallel through a spare port, and the two spare ports are connected through a one-way loop.

[0044] Those skilled in the art should understand that the above description is merely a specific embodiment of the present invention and is not intended to limit the present invention. Any modifications, equivalent substitutions, improvements, etc., made within the spirit and principles of the present invention should be included within the protection scope of the present invention.

Claims

1. A gas-liquid separator for separating diazonium methane from a mixed solution of diazonium methane, characterized in that, The system comprises an upper cylinder, a middle cylinder, and a lower cylinder. The upper part of the middle cylinder is connected to the upper cylinder via a flange, and the lower part is connected to the lower cylinder via a flange. The upper cylinder has a gas outlet at its top center, surrounded by gas moisture detection ports, diazomethane content detection ports, gas temperature detection ports, and an upper cylinder explosion vent. A pressure detection port is located on the side. The upper part of the middle cylinder has a refrigerant inlet and a refrigerant outlet. A refrigerant coil is installed inside the middle cylinder, with its inlet and outlet connected to the refrigerant outlet. The refrigerant coil is fixedly connected to the inner wall of the middle cylinder via a support plate. The upper part of the lower cylinder has a gas inlet above the liquid level and a gas inlet below the liquid level. The gas inlet above the liquid level is connected to a gas distributor on the liquid surface via a pipe, and the gas inlet below the liquid level... The gas distributor is connected to the submerged gas distributor via a pipe. The submerged gas distributor is located at the upper 1 / 3 of the lower cylinder and extends into the bottom of the lower cylinder. The upper side wall of the lower cylinder is provided with an upper tuning fork level gauge port, a lower cylinder explosion vent, and a lower cylinder pressure sensor port. The lower side wall of the lower cylinder is provided with a lower tuning fork level gauge port and a lower cylinder temperature detection port. The middle side wall of the lower cylinder is provided with a feed inlet, and the bottom center is provided with a drain outlet. The lower cylinder is fitted with a jacket with a jacket inlet at the bottom and a jacket outlet at the top. The jacket inlet is connected to cooling water. The submerged gas inlet is used to introduce gas to carry the diazonium methane dissolved in the liquid out of the liquid. The upper gas inlet is used to introduce gas to dilute the diazonium methane.

2. A gas-liquid separator for separating diazonium methane from a diazonium methane mixed solution according to claim 1, characterized in that, The feed inlet is installed tangentially to the lower cylinder wall, and an exhaust port is also provided on the upper part of the side wall of the lower cylinder.

3. A gas-liquid separator for separating diazonium methane from a diazonium methane mixed solution according to claim 1, characterized in that, The support plate is cylindrical, with its outer wall fixedly connected to the inner wall of the middle cylinder, and the refrigerant coil is fixedly connected to the inner side of the support plate through multiple support frames.

4. A gas-liquid separator for separating diazonium methane from a diazonium methane mixed solution according to claim 1, characterized in that, The upper part of the outer wall of the middle cylinder is provided with an upper support, and the upper part of the outer wall of the jacket is provided with a lower support. The number of upper and lower supports is the same, which is 2-5 each.

5. A gas-liquid separator for separating diazonium methane from a diazonium methane mixed solution according to claim 1, characterized in that, The temperature detection port of the lower cylinder is set opposite to the port of the lower tuning fork level gauge, and the included angle between the temperature detection port of the lower cylinder and the outer wall of the lower cylinder is 60°.

6. A gas-liquid separator for separating diazonium methane from a diazonium methane mixed solution according to claim 1, characterized in that, A spare port is provided on the lower part of the side wall of the middle cylinder. The two gas-liquid separators are connected in series through the spare port and are connected by a straight pipe. A safety pressure relief valve is provided on the straight pipe. Alternatively, the gas-liquid separators are connected in parallel through the spare port and the two spare ports are connected by a one-way loop.

7. A method for separating diazonium methane from a mixed solution of diazonium methane using the gas-liquid separator according to any one of claims 1-6, characterized in that, Includes the following steps: Step 1: Refrigerant introduction. Cooling water is introduced through the jacket inlet, and low-temperature refrigerant is introduced through the refrigerant inlet. After the internal temperature of the gas-liquid separator stabilizes, proceed to Step 2. Step 2: The diazomethane mixture solution is introduced into the lower cylinder tangentially from the feed inlet; Step 3: Gas-liquid primary separation. Nitrogen gas is simultaneously introduced through both the upper and lower gas inlets. Under the action of the gas distributor below the liquid surface, the nitrogen gas carries the diazonium methane dissolved in the liquid out of the liquid. The nitrogen mixture exiting through the gas distributor above the liquid surface is mixed and diluted with the nitrogen gas and the overflowing diazonium methane to obtain a water-saturated diazonium methane and nitrogen mixture obtained from the initial gas-liquid separation. This mixture enters the middle cylinder. During the gas-liquid primary separation, the liquid level in the lower cylinder is measured and monitored by tuning fork level gauges installed at the upper and lower tuning fork level gauge ports. If the liquid level exceeds the limit, the liquid is discharged through the drain port. When the liquid level in the lower cylinder rises to 1 / 3-2 / 3 of the lower cylinder height, nitrogen gas is introduced through the lower gas inlet. Step 4: Secondary gas-liquid separation. The diazonium methane and nitrogen mixture entering the middle cylinder liquefies the water vapor in the gas under the deep condensation of the refrigerant coil. The water vapor flows down along the refrigerant coil and enters the lower cylinder. The diazonium methane after deep condensation and liquid removal enters the upper cylinder. Step 5: The upper cylinder detects the water content, diazonium content, gas temperature, and pressure in the diazonium gas. Qualified diazonium gas enters the subsequent reaction equipment for reaction, while unqualified diazonium gas undergoes acid quenching treatment.

8. The method for separating diazonium methane from a mixed solution of diazonium methane according to claim 7, characterized in that, In step one, the cooling water temperature introduced into the jacket is -10 to 15°C, maintaining the temperature inside the lower cylinder at 0 to 20°C. The low-temperature refrigerant temperature introduced into the refrigerant coil is -40 to 25°C, maintaining the temperature inside the middle cylinder below -30°C. The pressure inside the lower, middle, and upper cylinders is controlled to be less than 2 kg. If the pressure exceeds the limit, the explosion vent in the upper or lower cylinder is opened. In step four, the moisture content of diazonium methane in the upper cylinder is less than 0.5 g / m³. 3 .

9. The method for separating diazonium methane from a mixed solution of diazonium methane according to claim 7, characterized in that, The nitrogen gas exiting the gas-liquid separator contains no more than 14.7% diazonium methane by volume, and the nitrogen flow rate is 39-624 L / min. The air contains no more than 3.9% diazonium methane by volume, and the air flow rate is 377-2352 L / min.

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