Gas-liquid separator for separating diazomethane from diazomethane mixed solution

Abstract

The utility model provides a gas-liquid separator for separating diazomethane from a diazomethane mixed solution, which comprises an upper cylinder body, a middle cylinder body and a lower cylinder body which are sequentially connected from top to bottom, a gas moisture detection port, a diazomethane content detection port, a gas temperature detection port and an upper cylinder explosion venting port are formed around the gas outlet, and a pressure detection port is formed in the side surface; a refrigerant inlet and a refrigerant outlet are formed in the upper portion of the middle barrel, a refrigerant coil is arranged in the middle barrel, an inlet of the refrigerant coil is connected with the refrigerant inlet, and an outlet of the refrigerant coil is connected with the refrigerant outlet. A liquid level upper gas inlet and a liquid level lower gas inlet are formed in the upper portion of the lower barrel, the liquid level upper gas inlet is connected with the liquid level upper gas distributor through a pipeline, the liquid level lower gas inlet is connected with the liquid level lower gas distributor through a pipeline, and a feeding port is formed in the side wall of the middle of the lower barrel. The gas-liquid separator disclosed by the utility model is high in gas-liquid separation efficiency, safe and explosion-proof, and can be used for continuous automatic production.

Description

Technical Field

[0001] The utility model belongs to the technical field of gas-liquid separation, and in particular relates to a multi-stage feeding micro-interface enhanced mass transfer reactor. Background Art

[0002] Diazomethane is an important chemical raw material. Due to the addition of water phase in the preparation process of diazomethane, a large amount of liquid droplets and water vapor are entrained in the diazomethane gas, which affects the subsequent chemical reaction. Therefore, it is necessary to separate the diazomethane gas from gas and liquid. The gas-liquid separator is an important equipment in the modern process industry. The gas-liquid separator currently used in the industrial process is generally a single-stage separator, which is provided with a gas-liquid separator cylinder. The top of the gas-liquid separator cylinder is provided with a gas phase outlet pipe, the lower part is provided with a liquid phase outlet pipe, the middle part is provided with an inlet diffuser, and the top of the inlet diffuser is provided with a defoaming net. During operation, the gas-liquid two-phase fluid enters the gas-liquid separator from the inlet diffuser for flash separation, a large amount of liquid phase flows to the bottom of the separator, and a large amount of gas phase carries the droplets upward, relying on the gravity of the droplets and separating droplets of different sizes according to the different heights of the gas phase space between the inlet diffuser and the defoamer. At the same time, the defoaming net can coalesce the droplets entrained in the remaining gas phase. However, for special gases such as diazomethane, the existing gas-liquid separators cannot meet the requirements of sufficient liquid removal, safety and explosion protection, and automated continuous production. Utility Model Content

[0003] In view of the above problems, the utility model provides a gas-liquid separator for separating diazomethane from a diazomethane mixed solution, which has the advantages of high gas-liquid separation efficiency, safety and explosion-proof, and continuous automated production.

[0004] In order to achieve the above purpose, the utility model adopts the following technical solutions:

[0005] A gas-liquid separator for separating diazomethane from a diazomethane mixed solution, comprising an upper cylinder, a middle cylinder and a lower cylinder, wherein the upper part of the middle cylinder is connected to the upper cylinder through a flange, and the lower part is connected to the lower cylinder through a flange, an air outlet is provided at the center of the top of the upper cylinder, a gas moisture detection port, a diazomethane content detection port, a gas temperature detection port, an upper cylinder explosion vent are provided around the air outlet, and a pressure detection port is provided on the side; a refrigerant inlet and a refrigerant outlet are provided at the upper part of the middle cylinder, a refrigerant coil is provided inside the middle cylinder, the refrigerant coil inlet is connected to the refrigerant inlet, the refrigerant coil outlet is connected to the refrigerant outlet, and the refrigerant coil is connected to the refrigerant outlet through a support plate It is fixedly connected to the inner wall of the middle cylinder; an upper gas inlet for liquid level and a lower gas inlet for liquid level are provided on the upper part of the lower cylinder, the upper gas inlet for liquid level is connected to the gas distributor on the liquid surface through a pipeline, and the lower gas inlet for liquid level is connected to the gas distributor below the liquid surface through a pipeline, an upper tuning fork liquid level gauge port, a lower cylinder explosion relief port and a lower cylinder pressure sensor port are respectively provided on the upper part of the side wall of the lower cylinder, a lower tuning fork liquid level gauge port and a lower cylinder temperature detection port are provided on the lower part of the side wall of the lower cylinder, a feed port is provided on the middle side wall of the lower cylinder, a drain port is provided in the middle position of the bottom, a jacket is provided on the outside of the lower cylinder, a jacket inlet is provided at the bottom of the jacket, and a jacket outlet is provided at the upper part.

[0006] Furthermore, the gas distributor above 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 port is installed in a tangential direction to the wall of the lower cylinder, and an exhaust port is also opened on the upper part of the side wall of the lower cylinder.

[0008] Furthermore, the support plate is cylindrical, and its outer wall is 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 a plurality of support frames.

[0009] Furthermore, an upper support is provided on the upper portion of the outer wall of the middle cylinder, and a lower support is provided on the upper portion of the outer wall of the jacket, and the number of the upper supports is the same as that of the lower supports, both of which are 2-5.

[0010] Furthermore, the lower cylinder temperature detection port and the tuning fork level gauge port are arranged opposite to each other, and the angle between the lower cylinder temperature detection port and the outer side wall of the lower cylinder is 60°.

[0011] Furthermore, a spare port is opened at 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, and the two spare ports are connected through 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 through a one-way ring loop.

[0012] By adopting the gas-liquid separator of the utility model, diazomethane containing droplets enters along the tangent direction of the lower cylinder at a relatively low temperature, and the liquid enters the lower cylinder. The lower cylinder is provided with a jacket, and cooling water can be introduced into the jacket to reduce the temperature of the lower cylinder and reduce the evaporation amount of the liquid entering the lower cylinder. The lower cylinder is provided with a temperature detection port for installing a temperature sensor, and the temperature of the lower cylinder can be automatically monitored. After the temperature of the lower cylinder is set, the flow rate of cooling water introduced into the jacket can be feedback-controlled by the control system; the lower cylinder is provided with two nitrogen inlets, and the nitrogen inlets are respectively connected to the gas distributors, one of which is introduced into the bottom of the lower cylinder and immersed in the liquid. After the nitrogen is introduced, the gas distributor can disperse the nitrogen into micron-level bubbles, take out the diazomethane gas in the liquid, and reduce the gas content in the liquid. The other gas distributor is located above the liquid surface, and the nitrogen entering the lower cylinder is dispersed to make it fully mixed with the diazomethane. The diazomethane diluted by the nitrogen enters the middle cylinder for deep condensation and liquid removal. In order to ensure that the lower cylinder maintains a certain liquid level, tuning fork level gauges are installed at the upper and lower tuning fork level gauge ports of the lower cylinder to monitor the liquid level of the lower cylinder. When the liquid level is too high, the battery valve installed at the drain port can be fed back to open to discharge the liquid. In order to prevent ice blockage during the deep cooling of the middle cylinder, which may cause the pressure in the lower cylinder to increase and cause risks, a pressure sensor is installed at the pressure sensor port of the lower cylinder to monitor the pressure in the lower cylinder in real time. When the pressure exceeds the set value, the lower cylinder explosion vent is opened to reduce the pressure in the lower cylinder. After the middle cylinder is deep cooled and deliquated, the diazomethane enters the upper cylinder. A pressure sensor is installed at the pressure detection port of the upper cylinder to monitor the pressure in the upper cylinder. When the pressure exceeds the set value, the upper cylinder explosion vent is opened to reduce the pressure in the upper cylinder. At the same time, a gas temperature sensor and a diazomethane content detection sensor are installed on the upper cylinder to monitor the quality of diazomethane in real time. When the quality of diazomethane is qualified, it is passed into the subsequent reaction equipment for chemical reaction. When the quality of diazomethane is unqualified, it is acid quenched.

[0013] The diazomethane mixed gas saturated with water vapor was obtained through a gas-liquid separation, and the water content was about 10g / m 3 The water content of the gas is greatly reduced, and the water content is further reduced to 0.5g / m 3This amount of water can fully meet the requirements for anhydrous reaction systems, avoiding the cumbersomeness of water removal and the difficulty of industrialization in existing processes; the introduction of nitrogen dilutes diazomethane to 14.7% within the safety range, and the actual operation is controlled within 12%, and real-time monitoring is adopted to ensure the safety of the system; the automatic control device (online monitoring of pressure, temperature, diazomethane concentration, etc., the signal enters the PLC control cabinet on site, and the signal is transmitted to the central control room at the same time) ensures that after the pressure exceeds a certain range, the upper and lower pressure relief valves can automatically open to relieve the pressure, and if the concentration is too high, the system will be automatically stopped and nitrogen will be replenished in time, further ensuring safety.

[0014] In order to further improve the safety and continuity of the reaction, the two gas-liquid separators described in the utility model can be used in series, and the two sets of separators are connected together through the spare port of the middle cylinder, and a safety valve is added. When the upper part of the first set of separators is cooled and blocked, and exceeds a certain pressure, the safety valve from the first set of separators to the second set of separators is opened, that is, the diazomethane mixed gas separated from the gas and liquid in the first set of separators cannot enter the upper cylinder, and instead enters the middle cylinder of the second set through the safety valve connected to the spare port for gas-liquid separation. When the blockage of the upper section of the first set is melted and the pipeline is cleared, it is switched back to the first set for use. In this way, the problem of overpressure inside the separator caused by the blockage of the ultra-low temperature ice-water mixture in the cylinder of the separator is avoided, and at the same time, the raw materials and the generated diazomethane are not wasted. Through the conversion of the two sets of separators, continuous production is facilitated.

[0015] In order to increase the safety and continuity of the production process, two sets of gas-liquid separators can also be used in parallel. When used in parallel, the cooling of the cylinder in the first set of separators is blocked. When a certain pressure is exceeded, the feed port of the first set of separators is closed, and the mixed liquid feed liquid of diazomethane is automatically cut into the feed port of the second set to continue separation. Clean the blockage of the cylinder in the first set of separators in time, clear the pipeline, and circulate it for standby use. In order to further enhance the gas-liquid separation effect, the two sets of separators can also be used in series, connecting the gas outlet of the first set with the feed port of the second set, and performing secondary gas-liquid separation on diazomethane to reduce the water content in diazomethane.

[0016] The gas-liquid separator of the utility model adopts the technical means of gas-liquid separation combined with deep cooling to solve the anhydrous problem of diazomethane, and solves the safe, automated and continuous industrial solution of the existing technology for immediate production; and solves the problem of ensuring the safety of diazomethane by diluting it with protective gas nitrogen or air. BRIEF DESCRIPTION OF THE DRAWINGS

[0017] Figure 1 It is a structural schematic diagram of the gas-liquid separator described in the utility model;

[0018] Figure 2is a top view of the gas-liquid separator;

[0019] Figure 3 It is a top view of the AA surface of the gas-liquid separator;

[0020] Figure 4 This is a schematic diagram of the use of the gas-liquid separators connected in series;

[0021] Figure 5 It is a schematic diagram of the gas-liquid separators used in parallel.

[0022] 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-coil inlet, 202-coil outlet, 203-refrigerant coil, 204-support plate, 205-spare port, 206-upper support, 301-liquid level nitrogen inlet, 302-liquid surface gas distributor, 3 03-nitrogen inlet below liquid level, 304-gas distributor below liquid surface, 305-upper tuning fork liquid level gauge port, 306-lower tuning fork liquid level gauge port, 307-feeding port, 308-drain port, 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 ring loop. DETAILED DESCRIPTION

[0023] The utility model is further described below in conjunction with the accompanying drawings and specific embodiments.

[0024] Example 1

[0025] like Figure 1-Figure 3 As shown, a gas-liquid separator for separating diazomethane from a diazomethane mixed solution comprises an upper cylinder 1, a middle cylinder 2, and a lower cylinder 3. The upper portion of the middle cylinder 2 is connected to the upper cylinder 1 through a flange, and the lower portion is connected to the lower cylinder 3 through a flange. A gas outlet 101 is provided at the center of the top of the upper cylinder 1, and a gas moisture detection port 102, a diazomethane content detection port 103, a gas temperature detection port 104, and an upper cylinder explosion vent 105 are provided around the gas outlet 101, and a pressure detection port 106 is provided on the side.

[0026] A refrigerant inlet 201 and a refrigerant outlet 202 are provided at the upper part of the side wall of the middle cylinder 2, a spare port 205 is provided at the lower part of the 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, and the refrigerant coil 203 is welded and fixed to the inner wall of the middle cylinder 2 through a support plate 204;

[0027] The upper part of the lower cylinder 3 is provided with an upper liquid level gas inlet 301 and a lower liquid level gas inlet 303, the upper liquid level gas inlet 301 is connected to the gas distributor 302 on the liquid surface through a pipeline, the lower liquid level gas inlet 303 is connected to the gas distributor 304 below the liquid surface through a pipeline, the gas distributor 302 on the liquid surface is located at the upper 1 / 3 of the lower cylinder 3, and the gas distributor 304 below the liquid surface extends into the bottom of the lower cylinder 3; the upper side walls of the lower cylinder 3 are respectively provided with an upper tuning fork liquid level gauge port 305, a lower cylinder explosion venting port 311, a lower cylinder pressure sensor port 312, and a lower cylinder exhaust port 313, the lower side walls of the lower cylinder are provided with a lower tuning fork liquid level gauge port 306 and a lower cylinder temperature detection port 310, the middle side wall of the lower cylinder is provided with a feed port 307, a drain port 308 is provided in the middle position of the bottom, and a lower cylinder temperature detection port 310 is provided. 310 is arranged opposite to the lower tuning fork level gauge port 306, 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 in a tangential direction 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 in the same vertical plane; the outer sleeve of the lower cylinder 3 is provided with a jacket 309, the bottom of the jacket 309 is provided with a jacket inlet 3091, and the upper part is provided with a jacket outlet 3092; an upper support 205 is provided at the upper part of the outer wall of the middle cylinder 2, and a lower support 3093 is provided at the upper part of the outer wall of the jacket 309, and the number of the upper support 205 and the lower support 3093 is the same, both of which are 2; the support plate 204 is cylindrical, and its outer wall is 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.

[0028] The method for separating diazomethane from a diazomethane mixture by using the gas-liquid separator in this embodiment specifically comprises the following steps:

[0029] Step 1: Cooling water is introduced from the jacket inlet 3091, and low-temperature refrigerant is introduced from the coil inlet 201. After the temperature inside the separator is stable, proceed to step 2;

[0030] Step 2: The diazomethane mixed solution enters the lower cylinder 3 from the feed port 307 along the tangential direction;

[0031] Step 3: gas-liquid primary separation, nitrogen or air is introduced simultaneously from the nitrogen inlet 301 above the liquid level and the nitrogen inlet 303 below the liquid level, under the action of the gas distributor 304 below the liquid surface, the nitrogen or air takes the diazomethane dissolved in the liquid out of the liquid, and the nitrogen and mixed gas coming out of the gas distributor 303 above the liquid surface are mixed and diluted with the above nitrogen and the overflowed diazomethane, so as to obtain a preliminary gas-liquid separation to obtain a water-saturated diazomethane and nitrogen mixed gas, which enters the upper cylinder; during the primary separation of gas and liquid, the tuning fork level gauge installed at the upper tuning fork level gauge port 305 and the lower tuning fork level gauge port 306 measures and monitors the liquid level of the lower cylinder, and when the liquid level is exceeded, 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 from the nitrogen inlet 303 below the liquid level;

[0032] Step 3: Secondary separation of gas and liquid. The diazomethane and nitrogen mixed gas entering the middle cylinder 2 is condensed deeply by the refrigerant coil 203. The water vapor in the gas is liquefied and flows down along the coil 203 to enter the lower cylinder 3. The diazomethane after deep condensation and liquid removal enters the upper cylinder 1.

[0033] Step 4: The upper cylinder 1 detects the water content, diazomethane content, gas temperature and pressure in the diazomethane gas. The qualified diazomethane gas enters the subsequent reaction equipment for reaction, and the unqualified diazomethane gas is subjected to acid quenching treatment.

[0034] In step 1, ice water at a temperature of 0-10°C is introduced into the jacket 309 to maintain the temperature in the lower cylinder 3 at 5-15°C. The refrigerant temperature introduced into the coil 203 is -35-20°C to maintain the temperature in the middle cylinder 2 at less than -25°C. The pressure in 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 3, the water content of diazomethane in the upper cylinder 1 is less than 0.5 g / m 3 .

[0035] The gas is nitrogen or air, wherein the volume content of diazomethane does not exceed 14.7%, the nitrogen flow rate is 39-624 L / min, the volume content of diazomethane in air does not exceed 3.9%, and the air flow rate is 377-2352 L / min.

[0036] Example 2

[0037] like Figure 4 As shown, the two gas-liquid separators in Example 1 are connected in series through a spare port, and the two spare ports are connected through a straight pipeline, and a safety pressure relief valve is provided on the straight pipeline.

[0038] Example 3

[0039] like Figure 5As shown, the two gas-liquid separators in Example 1 are connected in parallel through a spare port, and the two spare ports are connected through a one-way ring loop.

[0040] A person skilled in the art should understand that the above description is only 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 in the protection scope of the present invention.

Claims

1. A gas-liquid separator for separating diazomethane from a diazomethane mixed solution, characterized in that: It includes an upper cylinder, a middle cylinder and a lower cylinder. The upper part of the middle cylinder is connected to the upper cylinder through a flange, and the lower part is connected to the lower cylinder through a flange. An air outlet is opened at the center of the top of the upper cylinder, and a gas moisture detection port, a diazomethane content detection port, a gas temperature detection port, an upper cylinder explosion vent are opened around the air outlet, and a pressure detection port is opened on the side; a refrigerant inlet and a refrigerant outlet are arranged on the upper part of the middle cylinder, and a refrigerant coil is arranged inside the middle cylinder, the refrigerant coil inlet is connected to the refrigerant inlet, the refrigerant coil outlet is connected to the refrigerant outlet, and the refrigerant coil is fixedly connected to the inner wall of the middle cylinder through a support plate; An upper gas inlet for liquid level and a lower gas inlet for liquid level are provided on the upper part of the lower cylinder. The upper gas inlet for liquid level is connected to the gas distributor above the liquid surface through a pipeline, and the lower gas inlet for liquid level is connected to the gas distributor below the liquid surface through a pipeline. An upper tuning fork liquid level gauge port, a lower cylinder explosion relief port and a lower cylinder pressure sensor port are respectively provided on the upper part of the side wall of the lower cylinder, a lower tuning fork liquid level gauge port and a lower cylinder temperature detection port are provided on the lower part of the side wall of the lower cylinder, a feed port is provided on the middle side wall of the lower cylinder, and a drain port is provided in the middle position of the bottom. The outer cover of the lower cylinder is provided with a jacket, a jacket inlet is provided at the bottom of the jacket, and a jacket outlet is provided at the upper part.

2. A gas-liquid separator for separating diazomethane from a diazomethane mixed solution according to claim 1, characterized in that: The gas distributor above 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.

3. A gas-liquid separator for separating diazomethane from a diazomethane mixed solution according to claim 1, characterized in that: The feed port is installed in a tangential direction to the wall of the lower cylinder, and an exhaust port is also opened on the upper part of the side wall of the lower cylinder.

4. A gas-liquid separator for separating diazomethane from a diazomethane mixed solution according to claim 1, characterized in that: The support plate 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 a plurality of support frames.

5. A gas-liquid separator for separating diazomethane from a diazomethane mixed solution according to claim 1, characterized in that: An upper support is provided at the upper portion of the outer wall of the middle cylinder, and a lower support is provided at the upper portion of the outer wall of the jacket. The number of the upper supports is the same as that of the lower supports, which are both 2-5.

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

7. A gas-liquid separator for separating diazomethane from a diazomethane mixed solution according to claim 1, characterized in that: A spare port is provided at 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, and the two spare ports are connected through 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 through a one-way ring loop.

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