Device for separating dehydrohalogenation product of alkali liquor

By designing devices such as automatic pressure reactors, flash evaporators and flow coupling plates in the liquid phase dehydrogenation device, the problems of uneven material distribution and insufficient reaction are solved, and more efficient reaction and product separation are achieved, and failure rate and maintenance costs are reduced.

CN222766256UActive Publication Date: 2025-04-18山东东岳绿冷科技有限公司
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Patent Information

Application Number
CN202520274119.1
Authority / Receiving Office
CN · China
Patent Type
Utility models(China)
Current Assignee / Owner
Filing Date
2025-02-20
Publication Date
2025-04-18
Estimated Expiration
2035-02-20

AI Technical Summary

Technical Problem

The existing liquid phase dehydrogenation devices have problems such as uneven material distribution, insufficient reaction, low product separation efficiency, high equipment material requirements, and high failure rate.

Method used

A device for separating alkaline dehydrogenated products is designed, using a high-pressure reactor and a flash evaporator, and a flow-sharing plate and a disturbance device are installed above it, combining a static mixer, a filler distillation tower, a condenser and an alkaline washing tower to achieve uniform distribution of materials and sufficient reaction.

Benefits of technology

By evenly distributing materials and promoting reactions, the reaction efficiency and product separation efficiency are improved, the equipment failure rate and maintenance cost are reduced, the gas-liquid phase mixing is enhanced, and the efficiency of the defogging device is improved.

✦ Generated by Eureka AI based on patent content.

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Abstract

The utility model relates to the technical field of liquid phase dehydrohalogenation, in particular to a device for separating a dehydrohalogenation product of alkali liquor. An alkali liquor storage tank and a raw material storage tank are respectively connected with a static mixer, the static mixer is connected with a high-pressure reaction kettle, the top of the high-pressure reaction kettle is connected with a first filler rectifying tower, the top of the first filler rectifying tower is connected with a first condenser, the first condenser is connected with an alkali washing tower through a first buffer tank, and the alkali washing tower is connected with a product rectifying tower. The bottom of the high-pressure reaction kettle is connected with a first disturbance pump, an outlet of the first disturbance pump is divided into three paths, one path is connected with a first disturbance device at the bottom in the high-pressure reaction kettle, the other path is connected with a first spraying device at the upper part in the high-pressure reaction kettle, a first demister and a first flow equalizing plate are sequentially arranged below the first spraying device, and the last path is connected with a flash evaporation kettle. Disturbance devices are arranged in the high-pressure reaction kettle and the flash evaporation kettle, so that the phenomena of crystallization and overhigh local concentration caused by dead zones, insufficient reaction and material aggregation in the kettle are reduced while the reaction is promoted and the reaction rate is increased.
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Description

Technical Field

[0001] The utility model relates to the technical field of liquid phase dehydrohalogenation, in particular to a device for separating alkali liquid dehydrohalogenation products. Background Art

[0002] In industry, gas phase reactions are mostly used in dehydrohalogenation reactions. Dehydrohalogenation processes occupy a pivotal position in the field of fluorine chemical industry. At present, there are mainly two types of dehydrohalogenation reactions, one is gas phase dehydrohalogenation, and the other is liquid phase dehydrohalogenation. Among them, CN103664508A discloses a process for producing vinylidene fluoride by high temperature cracking of HCFC-142b (monofluorodichloroethane) as a raw material. This method cracks and removes HCl at a high temperature of 600-900°C, and then undergoes a series of post-processing steps, including carbon removal, water washing, alkali washing, compression, cooling, and finally obtains vinylidene fluoride by distillation. This method has the disadvantages of expensive catalysts, low catalyst conversion efficiency, and short life. At the same time, the gas phase method also has the disadvantages of large equipment investment, high reaction temperature, high energy consumption, easy coking of the reaction tube, many impurities, and difficult separation.

[0003] The liquid phase dehydrohalogenation devices in the prior art generally have problems such as uneven material distribution, insufficient reaction, low product separation efficiency, high equipment material requirements, and high failure rate. First, the distribution of materials in the reactor is often uneven, resulting in insufficient reaction and forming the so-called "dead zone". The materials in these areas cannot effectively participate in the reaction, which not only reduces the overall reaction efficiency, but also may cause local excessive concentration and material aggregation, increasing the risk of crystallization. At the same time, the gas phase materials produced by the reaction also lack an effective uniform distribution mechanism during the rising process, affecting the full contact and reaction between the gas phase and the liquid phase. Furthermore, traditional liquid phase dehydrohalogenation devices mostly use high-pressure mechanical stirring devices to promote the reaction, but these devices often fail frequently due to high-load operation. Once a failure occurs, the entire production system needs to be shut down for maintenance, which not only seriously affects the production efficiency, but also increases additional maintenance costs. At the same time, there are also certain problems with the airtightness of the mechanical stirring device, which may cause material leakage and environmental pollution. Utility Model Content

[0004] The utility model provides a device for separating alkali liquid dehydrohalogenation products in order to solve the problems of uneven material distribution, insufficient reaction, low product separation efficiency, high equipment material requirements, high failure rate, etc. commonly found in liquid phase dehydrohalogenation devices in the prior art.

[0005] In order to solve the above problems, the technical solution of the utility model is:

[0006] The utility model discloses a device for separating alkali liquid dehydrohalogenation products, comprising an alkali liquid storage tank and a raw material storage tank, wherein the alkali liquid storage tank and the raw material storage tank are respectively connected to a static mixer, the static mixer is connected to a high-pressure reactor, the top of the high-pressure reactor is connected to a first packing distillation tower, the top of the first packing distillation tower is connected to a first condenser, a first buffer tank is provided at a discharge port at the bottom of the first condenser, a reflux pipe and a discharge pipe are provided at the lower end of the first buffer tank, the reflux pipe is connected to the top of the first packing distillation tower, the discharge pipe is connected to an alkali washing tower, the alkali washing tower is connected to a product distillation tower, the bottom of the high-pressure reactor is connected to a first disturbance pump through a pipeline, the outlet of the first disturbance pump is divided into three routes, one route is connected to the first disturbance device at the bottom of the high-pressure reactor, and the other route is connected to the high-pressure A first spray device is provided at the upper part of the reactor, and a first demister and a first flow equalizing plate are provided below the first spray device in sequence, and the last one is connected to a flash kettle, and the top of the flash kettle is connected to a second packed distillation tower, and the top of the second packed distillation tower is connected to a second condenser, and a second buffer tank is provided at the bottom discharge port of the second condenser, and a reflux pipe and a discharge pipe are provided at the lower end of the second buffer tank, and the reflux pipe is connected to the top of the second packed distillation tower, and the discharge pipe is connected to an alkali washing tower, and the bottom of the flash kettle is connected to a second disturbance pump through a pipeline, and the outlet of the second disturbance pump is divided into two ways, one way is connected to the second disturbance device at the bottom of the flash kettle, and the other way is connected to the second spray device at the upper part of the flash kettle, and a second demister and a second flow equalizing plate are provided below the second spray device in sequence.

[0007] A plurality of first disturbance pumps and second disturbance pumps are arranged in parallel as backup pumps.

[0008] The outlet of the first disturbance pump is divided into three routes, one route goes to the bottom of the high-pressure reactor for disturbance, one route goes to the upper part of the high-pressure reactor for spraying, and the last route goes to the next-stage flash reactor.

[0009] The outlet of the second disturbance pump is divided into two paths, one path goes to the bottom of the flash kettle for disturbance, and the other path goes to the upper part of the flash kettle for spraying.

[0010] High-pressure mechanical stirring devices are prone to failure, and if a failure occurs, they must be shut down, seriously affecting production. Setting up a disturbance device has better air tightness and can use a spare pump after a failure, which does not affect production and is easy to operate. In addition, multiple units can be used to increase the disturbance efficiency and improve the reaction efficiency.

[0011] The first flow equalizing plate and the second flow equalizing plate are arranged at about 2 / 3 of the position above the high-pressure reactor and the flash reactor respectively, and their functions are as follows: to evenly distribute the liquid materials flowing down from the top; to evenly distribute the gas materials flowing upward from the bottom; to slow down the flow rate of the gas and liquid phases to improve the efficiency of the demister; to further mix and react the gas and liquid phases in the gas phase space above the high-pressure reactor and the flash reactor to make the reaction more complete.

[0012] A layer of demister is arranged above the equalizing plate to remove most of the water and alkali solution, which then flows back to the bottom of the reactor through the equalizing plate via the spray device above. This not only saves materials, but also reduces the risk of crystallization in the packed distillation tower, while promoting the full progress of the reaction.

[0013] The pipelines connecting the alkali solution storage tank, the raw material storage tank and the static mixer are respectively provided with an alkali solution feed pump and a raw material feed pump, and are also provided with a feed control valve; the high-pressure reactor is provided with a first temperature transmitter, a first pressure transmitter, a reactor pH meter, and a quartz tube level gauge; the flash reactor is provided with a second temperature transmitter, a second pressure transmitter, and a quartz tube level gauge.

[0014] The reactor pH meter is used to detect the pH value of the liquid phase material in the high-pressure reactor. An automatic adjustment device is set on the DCS. When the pH drops to the lower limit of 7.5, the regulating valve automatically opens. When the pH rises to the upper limit of 8.5, the regulating valve automatically closes. The upper and lower limits can be set on the DCS according to the actual operating conditions. This realizes the automatic control of the reaction feed, which not only saves costs, but also reduces the loss of manpower and material resources and reduces the possibility of misoperation.

[0015] The high-pressure reactor and the flash reactor are heated by hot water or steam.

[0016] The packings of the first packed distillation tower and the second packed distillation tower are one or two of θ-ring packings made of stainless steel or ceramic; the packing height is at least 0.1m.

[0017] The first spray device and the second spray device are both composed of a return pipe, a tubular distributor and a spray head.

[0018] A reflux pipe, a tubular distributor and a spray head are arranged above the demister and below the flange connected to the packed distillation tower to form a spray, which is connected to the outlet of the disturbance pump to allow the gas phase material to further react and absorb, and the demister can also be flushed at the same time.

[0019] The first spray device is arranged above the first demister and below the flange connected to the first packed distillation tower; the second spray device is arranged above the second demister and below the flange connected to the second packed distillation tower.

[0020] The first disturbance device includes a pipeline arranged about 0.1 m below the lowest liquid level of the high-pressure reactor, and nozzles are evenly arranged downward on the pipeline; the second disturbance device includes a pipeline arranged about 0.1 m below the lowest liquid level of the flash reactor, and nozzles are evenly arranged downward on the pipeline.

[0021] A disturbance device is installed in the high-pressure reactor and flash reactor to promote the reaction and increase the reaction rate, while reducing the dead zone in the reactor, insufficient reaction and material aggregation causing crystallization and local excessive concentration.

[0022] The top of the product distillation tower is connected to the third condenser, the bottom outlet of the third condenser is provided with a third buffer tank, the lower end of the third buffer tank is provided with a reflux pipe and a discharge pipe, the reflux pipe is connected to the top of the product distillation tower, and the discharge pipe is connected to the product storage tank.

[0023] The upper ends of the first condenser, the second condenser and the third condenser are provided with interconnected air pressure balance pipes; the tops of the air pressure balance pipes are provided with pressure regulating exhaust pipes.

[0024] Working principle:

[0025] The prepared NaOH solution in the alkali liquid storage tank is pumped into the high-pressure reactor by the alkali liquid feed pump. During normal operation, the NaOH solution is automatically fed according to the pH change. The HCFC-142b raw material is continuously fed from the raw material storage tank through the raw material feed pump. After being uniformly mixed by a static mixer under the control of a feed control valve and an electromagnetic valve on the feed pump pipeline, the high-pressure reactor is pumped into the high-pressure reactor, wherein the feed molar ratio of NaOH to HCFC-142b is controlled at 1:1, the temperature in the high-pressure reactor is controlled at 50-200° C., the pressure is controlled at 0.2-1 MPa, and the reactor is continuously disturbed. The reactor is refluxed and purified by a first packing distillation tower and a first condenser. The temperature of the first packing distillation tower is controlled at 10-60° C., the temperature of the first condenser is controlled at -5-30° C., part of the non-condensable gas is discharged from the top of the first condenser, and the purified product enters an alkali washing tower to remove HCl gas generated by the reaction. The temperature of the alkali washing tower is controlled at 30-45° C. Finally, the product is separated by a product distillation tower. The feed ratio of NaOH solution and HCFC-142b raw material is adjusted by the reactor pH meter, the first temperature transmitter, the second temperature transmitter, the quartz tube level gauge, the first pressure transmitter and the second pressure transmitter to achieve continuous operation.

[0026] All the unreacted materials in the high-pressure reactor are pumped into a flash reactor, the temperature is controlled between 50-100°C, the pressure is controlled between 0.2-1MPa, and the disturbance is continued. The product is refluxed and purified through a second packed distillation tower and a second condenser. The temperature of the second packed distillation tower is controlled between 10-60°C, the temperature of the second condenser is controlled between -5-30°C, and part of the non-condensable gas is discharged from the top of the second condenser. The purified product enters an alkali washing tower to remove HCl gas generated by the reaction. The temperature of the alkali washing tower is controlled between 30-45°C. Finally, the product is separated out through a product distillation tower.

[0027] The beneficial effects of the utility model are as follows:

[0028] (1) The utility model arranges the first flow equalizing plate and the second flow equalizing plate at about 2 / 3 of the upper part of the high-pressure reactor and the flash reactor, respectively, to have the following functions: to evenly distribute the liquid phase material flowing down from the upper part; to evenly distribute the gas phase material flowing upward from the lower part; to slow down the flow rate of the gas phase and the liquid phase to improve the efficiency of the demister; and to further mix and react the gas and liquid phases in the gas phase space above the high-pressure reactor and the flash reactor to make the reaction more complete.

[0029] (2) The utility model arranges a layer of demister above the equalizing plate to remove most of the water and alkali solution, and then refluxes to the bottom of the reactor through the equalizing plate following the spray device above, which not only saves materials but also reduces the risk of crystallization of the packed distillation tower, while promoting the full progress of the reaction.

[0030] (3) The utility model arranges a reflux pipe, a tubular distributor and a spray head above the demister and below the flange connected to the packed distillation tower to form a spray, which is connected to the outlet of the disturbance pump to allow the gas phase material to further react and absorb, and the demister can also be flushed at the same time.

[0031] (4) The utility model sets a disturbance device in the high-pressure reactor and the flash reactor, which promotes the reaction and increases the reaction rate, while reducing the dead zone in the reactor, insufficient reaction and material aggregation causing crystallization and local excessive concentration.

[0032] (5) The high-pressure mechanical stirring device in the prior art is prone to failure, and must be shut down when a failure occurs, seriously affecting production. The utility model has better air tightness by setting a disturbance device, and a spare pump can be used after a failure, which does not affect production and is easy to operate. In addition, multiple units can be used to increase the disturbance efficiency and improve the reaction efficiency.

[0033] (6) The utility model adopts a high-pressure reaction kettle connected to a first packed distillation tower for reactive distillation, which can purify while reacting, and can increase the purity of the product to more than 99.9%. The purity of the product can also be changed by controlling the reflux ratio. The operation is convenient and the process is simple. BRIEF DESCRIPTION OF THE DRAWINGS

[0034] The accompanying drawings described herein are used to provide a further understanding of the present invention and constitute a part of the present invention. In the accompanying drawings:

[0035] Figure 1 This is a schematic diagram of the structure of the device for separating the alkali solution dehydrohalogenation products of the utility model;

[0036] In the figure: 1, alkali liquid storage tank; 2, raw material storage tank; 3, alkali liquid feed pump; 4, raw material feed pump; 5, feed control valve; 6, static mixer; 7, high pressure reactor; 701, first temperature transmitter; 702, first pressure transmitter; 703, first flow equalizer; 704, first demister; 705, first spray device; 706, reactor pH meter; 707, first disturbance device; 8, first packed distillation tower; 801, first condenser; 802, first buffer tank; 9 , the first disturbance pump; 10, the flash kettle; 1001, the second temperature transmitter; 1002, the second pressure transmitter; 1003, the second flow equalizing plate; 1004, the second demister; 1005, the second spray device; 1006, the second disturbance device; 11, the second packed distillation tower; 1101, the second condenser; 1102, the second buffer tank; 12, the second disturbance pump; 13, the alkali washing tower; 14, the product distillation tower; 1401, the third condenser; 1402, the third buffer tank. DETAILED DESCRIPTION

[0037] The present invention will be described in detail below in conjunction with the embodiments.

[0038] Example 1

[0039] like Figure 1As shown, the device for separating the alkali liquid dehydrohalogenation product comprises an alkali liquid storage tank 1 and a raw material storage tank 2, wherein the alkali liquid storage tank 1 and the raw material storage tank 2 are respectively connected to a static mixer 6, the static mixer 6 is connected to a high-pressure reactor 7, the top of the high-pressure reactor 7 is connected to a first packing distillation tower 8, the top of the first packing distillation tower 8 is connected to a first condenser 801, a first buffer tank 802 is provided at the bottom discharge port of the first condenser 801, a reflux pipe and a discharge pipe are provided at the lower end of the first buffer tank 802, the reflux pipe is connected to the top of the first packing distillation tower 8, the discharge pipe is connected to an alkali washing tower 13, the alkali washing tower 13 is connected to a product distillation tower 14, the bottom of the high-pressure reactor 7 is connected to a first disturbance pump 9 through a pipeline, the outlet of the first disturbance pump 9 is divided into three routes, one route is connected to a first disturbance device 707 at the bottom of the high-pressure reactor 7, one route is connected to a first spray device 705 at the upper part of the high-pressure reactor 7, and the third route is connected to a first perturbation device 707 at the bottom of the high-pressure reactor 7. A first demister 704 and a first flow equalizer 703 are sequentially arranged below a spray device 705, and the last one is connected to a flash kettle 10. The top of the flash kettle 10 is connected to a second packed distillation tower 11. The top of the second packed distillation tower 11 is connected to a second condenser 1101. A second buffer tank 1102 is arranged at the bottom discharge port of the second condenser 1101. A reflux pipe and a discharge pipe are arranged at the lower end of the second buffer tank 1102. The reflux pipe is connected to the top of the second packed distillation tower 11. The discharge pipe is connected to an alkali washing tower 13. The bottom of the flash kettle 10 is connected to a second disturbance pump 12 through a pipeline. The outlet of the second disturbance pump 12 is divided into two ways, one of which is connected to a second disturbance device 1006 at the bottom of the flash kettle 10, and the other is connected to a second spray device 1005 at the upper part of the flash kettle 10. A second demister 1004 and a second flow equalizer 1003 are sequentially arranged below the second spray device 1005.

[0040] A plurality of first disturbance pumps 9 and second disturbance pumps 12 are arranged in parallel as backup pumps.

[0041] The outlet of the first disturbance pump 9 is divided into three paths, one path goes to the bottom of the high-pressure reactor 7 for disturbance, one path goes to the upper part of the high-pressure reactor 7 for spraying, and the last path goes to the next-stage flash reactor 10.

[0042] The outlet of the second disturbance pump 12 is divided into two paths, one path goes to the bottom of the flash kettle 10 for disturbance, and the other path goes to the upper part of the flash kettle 10 for spraying.

[0043] High-pressure mechanical stirring devices are prone to failure, and if a failure occurs, they must be shut down, seriously affecting production. Setting up a disturbance device has better air tightness and can use a spare pump after a failure, which does not affect production and is easy to operate. In addition, multiple units can be used to increase the disturbance efficiency and improve the reaction efficiency.

[0044] The first flow equalizing plate 703 and the second flow equalizing plate 1003 are respectively arranged at about 2 / 3 of the position above the high-pressure reactor 7 and the flash reactor 10, and their functions are as follows: to evenly distribute the liquid phase material flowing down from the top; to evenly distribute the gas phase material flowing upward from the bottom; to slow down the flow rate of the gas and liquid phases to improve the efficiency of the demister; to further mix and react the gas and liquid phases in the gas phase space above the high-pressure reactor 7 and the flash reactor 10 to make the reaction more complete.

[0045] A layer of demister is arranged above the equalizing plate to remove most of the water and alkali solution, which then flows back to the bottom of the reactor through the equalizing plate via the spray device above. This not only saves materials, but also reduces the risk of crystallization in the packed distillation tower, while promoting the full progress of the reaction.

[0046] The pipelines connecting the alkali solution storage tank 1, the raw material storage tank 2 and the static mixer 6 are respectively provided with an alkali solution feed pump 3 and a raw material feed pump 4, and are also provided with a feed control valve 5. The high-pressure reactor 7 is provided with a first temperature transmitter 701, a first pressure transmitter 702, a reactor pH meter 706, and a quartz tube level gauge. The flash reactor 10 is provided with a second temperature transmitter 1001, a second pressure transmitter 1002, and a quartz tube level gauge.

[0047] Reactor pH meter 706 is used to detect the pH value of the liquid phase material in the high-pressure reactor 7. An automatic adjustment device is set on the DCS. When the pH drops to the lower limit of 7.5, the regulating valve automatically opens. When the pH rises to the upper limit of 8.5, the regulating valve automatically closes. The upper and lower limits can be set on the DCS according to the actual operating conditions. This realizes the automatic control of the reaction feed, which not only saves costs, but also reduces the loss of manpower and material resources and reduces the possibility of misoperation.

[0048] The high-pressure reactor 7 and the flash reactor 10 are heated by hot water or steam.

[0049] The packings of the first packed distillation tower 8 and the second packed distillation tower 11 are one or both of θ-ring packings made of stainless steel or ceramics; the packing height is at least 0.1 m.

[0050] The first spray device 705 and the second spray device 1005 are both composed of a return pipe, a tubular distributor and a spray head.

[0051] A reflux pipe, a tubular distributor and a spray head are arranged above the demister and below the flange connected to the packed distillation tower to form a spray, which is connected to the outlet of the disturbance pump to allow the gas phase material to further react and absorb, and the demister can also be flushed at the same time.

[0052] The first spray device 705 is arranged above the first demister 704 and below the flange connected to the first packed distillation tower 8 ; the second spray device 1005 is arranged above the second demister 1004 and below the flange connected to the second packed distillation tower 11 .

[0053] The first disturbance device 707 includes a pipeline arranged about 0.1 m below the lowest liquid level of the high-pressure reactor 7, and nozzles are evenly arranged downward on the pipeline; the second disturbance device 1006 includes a pipeline arranged about 0.1 m below the lowest liquid level of the flash reactor 10, and nozzles are evenly arranged downward on the pipeline.

[0054] Disturbance devices are arranged in the high-pressure reactor 7 and the flash reactor 10 to promote the reaction and increase the reaction rate while reducing the dead zone in the reactor, insufficient reaction and material aggregation causing crystallization and local excessive concentration.

[0055] The top of the product distillation tower 14 is connected to the third condenser 1401. The bottom outlet of the third condenser 1401 is provided with a third buffer tank 1402. The lower end of the third buffer tank 1402 is provided with a reflux pipe and a discharge pipe. The reflux pipe is connected to the top of the product distillation tower 14, and the discharge pipe is connected to the product storage tank.

[0056] The upper ends of the first condenser 801, the second condenser 1101, and the third condenser 1401 are provided with interconnected air pressure balance pipes; and the tops of the air pressure balance pipes are provided with pressure regulating exhaust pipes.

[0057] Working principle:

[0058] The prepared NaOH solution in the alkali liquid storage tank 1 is pumped into the high-pressure reactor 7 by the alkali liquid feed pump 3. During normal operation, the NaOH solution is automatically fed according to the pH change. The HCFC-142b raw material is continuously fed from the raw material storage tank 2 by the raw material feed pump 4. After being uniformly mixed by the static mixer 6 under the control of the feed control valve 5 and the solenoid valve on the feed pump pipeline, it is pumped into the high-pressure reactor 7, wherein the feed molar ratio of NaOH to HCFC-142b is controlled at 1:1, and the temperature in the high-pressure reactor 7 is controlled at 1:1. The temperature is between 50-200°C, the pressure is controlled at 0.2-1MPa, and the disturbance is continued. The first packing distillation tower 8 and the first condenser 801 are used for reflux purification. The temperature of the first packing distillation tower 8 is controlled between 10-60°C, and the temperature of the first condenser 801 is controlled between -5-30°C. Part of the non-condensable gas is discharged from the top of the first condenser 801. The purified product enters the alkali washing tower 13 to remove the HCl gas generated by the reaction. The temperature of the alkali washing tower 13 is controlled between 30-45°C. Finally, the product is separated by the product distillation tower 14. The feed ratio of the NaOH solution and the HCFC-142b raw material is adjusted by the reactor pH meter 706, the first temperature transmitter 701, the second temperature transmitter 1001, the quartz tube level gauge, the first pressure transmitter 702 and the second pressure transmitter 1002 to achieve continuous operation.

[0059] All the unreacted materials in the high-pressure reactor 7 are pumped into the flash reactor 10, the temperature is controlled between 50-100°C, the pressure is controlled at 0.2-1MPa, and the disturbance is continued. The materials are refluxed and purified through the second packed distillation tower 11 and the second condenser 1101. The temperature of the second packed distillation tower 11 is controlled between 10-60°C, the temperature of the second condenser 1101 is controlled between -5-30°C, and part of the non-condensable gas is discharged from the top of the second condenser 1101. The purified product enters the alkali washing tower 13 to remove the HCl gas generated by the reaction. The temperature of the alkali washing tower 13 is controlled between 30-45°C. Finally, the product is separated out through the product distillation tower 14.

Claims

1. A device for separating alkali solution dehydrohalogenation products, characterized in that: The invention comprises an alkali liquid storage tank (1) and a raw material storage tank (2), wherein the alkali liquid storage tank (1) and the raw material storage tank (2) are respectively connected to a static mixer (6), the static mixer (6) is connected to a high-pressure reactor (7), the top of the high-pressure reactor (7) is connected to a first packing distillation tower (8), the top of the first packing distillation tower (8) is connected to a first condenser (801), a first buffer tank (802) is provided at a discharge port at the bottom of the first condenser (801), and a reflux pipe and a discharge port are provided at the lower end of the first buffer tank (802). The reflux pipe is connected to the top of the first packing distillation tower (8), the discharge pipe is connected to the alkali washing tower (13), the alkali washing tower (13) is connected to the product distillation tower (14), the bottom of the high-pressure reactor (7) is connected to the first disturbance pump (9) through a pipeline, and the outlet of the first disturbance pump (9) is divided into three paths, one of which is connected to the first disturbance device (707) at the bottom of the high-pressure reactor (7), the other is connected to the first spray device (705) at the upper part of the high-pressure reactor (7), and the first spray device (70 5) is provided with a first demister (704) and a first flow equalizing plate (703) in sequence at the bottom, and the last one is connected to a flash kettle (10), the top of the flash kettle (10) is connected to a second packed distillation tower (11), the top of the second packed distillation tower (11) is connected to a second condenser (1101), a second buffer tank (1102) is provided at the bottom outlet of the second condenser (1101), a reflux pipe and a discharge pipe are provided at the lower end of the second buffer tank (1102), and the reflux pipe is connected to the second packed distillation tower (11 ) tower top, the discharge pipe is connected to the alkali washing tower (13), the bottom of the flash kettle (10) is connected to the second disturbance pump (12) through a pipeline, the outlet of the second disturbance pump (12) is divided into two paths, one is connected to the second disturbance device (1006) at the bottom of the flash kettle (10), and the other is connected to the second spray device (1005) at the upper part of the flash kettle (10), and a second demister (1004) and a second flow equalizing plate (1003) are arranged in sequence below the second spray device (1005).

2. The device for separating alkali solution dehydrohalogenation products according to claim 1, characterized in that: The pipelines connecting the alkali solution storage tank (1), the raw material storage tank (2) and the static mixer (6) are respectively provided with an alkali solution feed pump (3) and a raw material feed pump (4), and are also provided with a feed control valve (5); the high-pressure reactor (7) is provided with a first temperature transmitter (701), a first pressure transmitter (702), a reactor pH meter (706), and a quartz tube level gauge; and the flash reactor (10) is provided with a second temperature transmitter (1001), a second pressure transmitter (1002), and a quartz tube level gauge.

3. The device for separating alkali solution dehydrohalogenation products according to claim 1, characterized in that: The first spray device (705) and the second spray device (1005) are both composed of a return pipe, a tubular distributor and a spray head.

4. The device for separating alkali solution dehydrohalogenation products according to claim 1, characterized in that: The first disturbance device (707) comprises a pipeline arranged below the lowest liquid level of the high-pressure reactor (7), and nozzles are evenly arranged downward on the pipeline; the second disturbance device (1006) comprises a pipeline arranged below the lowest liquid level of the flash reactor (10), and nozzles are evenly arranged downward on the pipeline.

5. The device for separating alkali solution dehydrohalogenation products according to claim 1, characterized in that: The top of the product distillation tower (14) is connected to the third condenser (1401), and a third buffer tank (1402) is provided at the bottom discharge port of the third condenser (1401). A reflux pipe and a discharge pipe are provided at the lower end of the third buffer tank (1402), the reflux pipe is connected to the top of the product distillation tower (14), and the discharge pipe is connected to the product storage tank.

6. The device for separating alkali solution dehydrohalogenation products according to claim 5, characterized in that: The upper ends of the first condenser (801), the second condenser (1101), and the third condenser (1401) are provided with interconnected air pressure balance pipes; and the tops of the air pressure balance pipes are provided with pressure regulating exhaust pipes.

Citation Information

Patent Citations

  • Production method of vinylidene fluoride monomer

    CN103664508A