CN212141944U - Tail gas separation device in acrylonitrile electrochemical synthesis adiponitrile technology - Google Patents
Tail gas separation device in acrylonitrile electrochemical synthesis adiponitrile technology Download PDFInfo
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- CN212141944U CN212141944U CN202020397780.9U CN202020397780U CN212141944U CN 212141944 U CN212141944 U CN 212141944U CN 202020397780 U CN202020397780 U CN 202020397780U CN 212141944 U CN212141944 U CN 212141944U
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Abstract
The utility model relates to a tail gas separator in acrylonitrile electrochemistry synthesis adiponitrile technology utilizes gas-liquid separation, water oil separating, water washing, active carbon adsorption principle, makes the gas-liquid after the reaction through analytic principle, with the release of a large amount of oxygen that the synthetic phase generated, separates in the liquid phase entering oil water separator simultaneously, and the water phase is as electrolysis carrier cyclic utilization, and the oil phase gets into next process purification. Compared with the existing three-phase separator technology, the equipment avoids the standing separation process of oxygen in the water phase and the oil phase, thereby reducing the amount of organic gas carried in the oxygen release process, and carrying out secondary recovery on tail gas through a trap, a washing tower and an absorption tower, greatly reducing the content of organic matters in the tail gas, reducing the loss of acrylonitrile, and greatly reducing the treatment and recovery cost of subsequent tail gas.
Description
Technical Field
The utility model relates to a tail gas separation device in acrylonitrile electrochemical synthesis adiponitrile technology belongs to separator technical field.
Background
In the prior art for electrochemically synthesizing adiponitrile by acrylonitrile, after a circulating carrier reacts with raw and auxiliary materials in a reactor, a product oil phase and a gas phase can be separated from the circulating carrier only after standing separation, most of equipment adopted for separation is a three-phase separator, after the circulating carrier enters the three-phase separation, gas-phase product oxygen can be separated and escaped in the carrier, a large amount of acrylonitrile gas and other organic gas can be carried in the oil phase in the escaping process, a large amount of loss of acrylonitrile is caused for a moment, and the load of tail gas treatment in the post-process is increased for the second time.
SUMMERY OF THE UTILITY MODEL
The utility model overcomes prior art exists not enough, and the technical problem that solve provides a tail gas separator in acrylonitrile electrochemical synthesis adiponitrile technology, content of organic matter in the reducible tail gas reduces the loss of acrylonitrile.
In order to solve the technical problem, the utility model discloses the technical scheme who adopts is:
a tail gas separation device in a process for electrochemically synthesizing adiponitrile by acrylonitrile, which comprises a gas-liquid separation unit, an oil-water separation unit, a condenser, a tail gas washing tower and an absorption tower,
the gas-liquid separation unit is introduced with a gas-liquid mixed circulation carrier through a circulation carrier inlet, the gas-liquid separation unit is provided with a circulation carrier outlet and a separated tail gas outlet, the circulation carrier outlet is connected with the oil-water separation unit, the separated tail gas outlet is connected with a condenser through a separated tail gas pipe, a condensate outlet of the condenser is connected with the oil-water separation unit, and a condensed tail gas outlet of the condenser is connected with a tail gas washing tower; the washing liquid outlet of the tail gas washing tower is communicated with the rectifying tower of the rectifying section, the washing tail gas outlet of the tail gas washing tower is connected with the absorption tower, the absorption tower is provided with a nitrogen inlet pipe, a nitrogen outlet pipe and an adsorption tail gas outlet, the adsorption tail gas outlet is connected with the catalytic conversion device, the nitrogen inlet pipe is filled with nitrogen, and the nitrogen outlet pipe is connected with the separation tail gas pipe.
The gas-liquid separation unit comprises a cavity, a gas-liquid trap is arranged at the upper part of the cavity, a gas-liquid separation device is arranged at the lower part of the cavity, and a cavity is arranged in the middle of the cavity; the circulation carrier inlet is connected with an inlet pipe, the inlet pipe is positioned in the cavity, a spiral spray type spray head is arranged on the inlet pipe, a circulation carrier outlet is arranged at the bottom of the cavity, and a separation tail gas outlet is arranged at the top of the cavity.
The oil-water separation unit comprises a separation tank, the separation tank is provided with a first liquid feed inlet and a second liquid feed inlet, the first liquid feed inlet and the second liquid feed inlet are respectively connected with a condensate outlet of a circulating carrier and a condenser through pipelines, the separation tank is provided with a water phase outlet and an oil phase outlet, the water phase outlet is positioned at the lower part or the bottom of the separation tank, the oil phase outlet is positioned at the upper part of the separation tank, the outer side of the oil phase outlet is provided with a regulating valve, and the oil phase tank is connected through a pipeline.
The oil phase outlet is characterized in that an overflow partition plate is arranged in the separating tank on the inner side of the oil phase outlet and is of an L shape, holes are formed in the overflow partition plate, the overflow partition plate and the inner wall of the separating tank form an oil phase collecting cavity, the oil phase outlet is located on one side of the oil phase collecting cavity, a liquid level meter is further arranged in the oil phase collecting cavity, and the liquid level meter is electrically connected with the regulating valve.
And cooling circulating water is introduced into the condenser.
Be provided with the washing filler in the tail gas washing tower, tail gas washing tower bottom is connected condensation tail gas export, top are provided with the washing tail gas export, and upper portion is provided with the washing pipe, is provided with washing shower nozzle on the washing pipe, and tail gas washing tower lower part is provided with the washing liquid export, and the washing union coupling has washing liquid pond and tail gas washing tower lower part, is provided with the circulating pump on the washing pipe.
The absorption tower comprises two absorption towers which are arranged in parallel: the absorption tower is characterized in that the top of the absorption tower is provided with an air inlet, the bottom of the absorption tower is provided with an adsorbed tail gas outlet, the adsorbed tail gas outlet is also connected with a nitrogen inlet pipe, the air inlet is connected with a washing tail gas outlet, and the air inlet is also connected with a nitrogen outlet pipe; and the air inlet, the adsorbed tail gas outlet, the nitrogen inlet pipe and the nitrogen outlet pipe of the absorption tower are all provided with switch valves.
The tail gas separation treatment method in the process of electrochemically synthesizing adiponitrile by acrylonitrile by using the device comprises the following steps:
gas-liquid separation is carried out on the gas-liquid mixed circulating carrier of the electrochemical synthesis unit in a gas-liquid separation unit, the obtained separated tail gas is condensed by a condenser, desalted water washing is carried out on the tail gas washing tower, and the active carbon adsorption step of an absorption tower is carried out;
the absorption tower comprises two absorption towers which are connected in parallel, one absorption tower is used for absorbing, the other absorption tower is used for regenerating, and the two absorption towers are switched to use in turn at regular time;
the absorption tower is regenerated by nitrogen, and regenerated gas containing acrylonitrile generated by regeneration returns to the separation tail gas pipe to be used as tail gas make-up gas.
The tail gas is washed by desalted water, enters a tail gas washing tower from the bottom and passes through a washing packing layer from bottom to top to be in countercurrent contact with washing water from top to bottom, part of acrylonitrile in the tail gas is absorbed by the desalted water, the washing tail gas leaves the washing tower from the top, the washing water at the bottom of the washing tower is recycled, the temperature is controlled to be 10-30 ℃, when the washing water is saturated, the concentration of acrylonitrile in the washing water is 2-7%, continuous water inlet and drainage are adopted, the saturated washing water is sent to a rectification working section for distillation, and the acrylonitrile and the desalted water generated after distillation are recycled.
Compared with the prior art, the utility model following beneficial effect has:
the device utilizes the principles of gas-liquid separation, oil-water separation, water washing and activated carbon adsorption to ensure that gas and liquid after reaction release a large amount of oxygen generated in the synthesis stage through the analytic principle, simultaneously liquid phase enters an oil-water separator for separation, water phase is recycled as an electrolytic carrier, and oil phase enters the next procedure for purification. Compared with the existing three-phase separator technology, the equipment avoids the standing separation process of oxygen in the water phase and the oil phase, thereby reducing the amount of organic gas carried in the oxygen release process, and carrying out secondary recovery on tail gas through a trap, a washing tower and an absorption tower, greatly reducing the content of organic matters in the tail gas, reducing the loss of acrylonitrile, and greatly reducing the treatment and recovery cost of subsequent tail gas.
Drawings
Fig. 1 is a schematic structural diagram of an apparatus according to embodiment 1 of the present invention.
In the figure: 1-a gas-liquid separation unit, 2-an oil-water separation unit, 3-a condenser, 4-an absorption tower, 5-an exhaust gas washing tower, 7-a rectification tower, 8-a catalytic conversion device, 11-a circulating carrier inlet, 12-a circulating carrier outlet, 13-a separated exhaust gas outlet, 14-a separated exhaust gas pipe, 15-a gas-liquid trap, 16-a gas-liquid separation device, 18-a spiral spray type spray nozzle, 21-a first liquid feed inlet, 22-a second liquid feed inlet, 23-a water phase outlet, 24-an oil phase outlet, 25-a regulating valve, 26-an oil phase tank, 27-an overflow clapboard, 28-an oil phase collection cavity, 29-a liquid level meter, 41-a nitrogen inlet pipe, 42-a nitrogen outlet pipe and 43-an adsorbed exhaust gas outlet, 51-washing liquid outlet, 52-washing tail gas outlet, 53-washing pipe and 55-washing liquid pool.
Detailed Description
The present invention will be further explained with reference to the accompanying drawings.
Example 1
A tail gas separation device in a process for electrochemically synthesizing adiponitrile by acrylonitrile, which comprises a gas-liquid separation unit 1, an oil-water separation unit 2, a condenser 3, a tail gas washing tower 5 and an absorption tower 4,
the gas-liquid separation unit 1 is provided with a circulating carrier outlet 12 and a separated tail gas outlet 13, the circulating carrier outlet 12 is connected with the oil-water separation unit 2, the separated tail gas outlet 13 is connected with the condenser 3 through a separated tail gas pipe 14, a condensate outlet 31 of the condenser 3 is connected with the oil-water separation unit 2, and a condensed tail gas outlet 32 of the condenser 3 is connected with the tail gas washing tower 5; the washing liquid outlet 51 of the tail gas washing tower 5 is communicated with the rectifying tower 7 of the rectifying section, the washing tail gas outlet 52 of the tail gas washing tower 5 is connected with the absorption tower 4, the absorption tower is provided with a nitrogen inlet pipe 41, a nitrogen outlet pipe 42 and an adsorption tail gas outlet 43, the adsorption tail gas outlet 43 is connected with the catalytic conversion device 8, the nitrogen inlet pipe 41 is filled with nitrogen, and the nitrogen outlet pipe 42 is connected with the separation tail gas pipe 14.
The gas-liquid separation unit 1 comprises a cavity, a gas-liquid trap 15 is arranged at the upper part of the cavity, a gas-liquid separation device 16 is arranged at the lower part of the cavity, and a cavity is arranged in the middle of the cavity; the gas-liquid trap 15 adopts a stainless steel stepped ring of DN15, and is filled with a filler layer for trapping organic phases in a gas phase; the gas-liquid separation device 16 adopts a stainless steel step ring, and is filled with a packing layer, and the function is to enable liquid to pass through the packing layer, so that oxygen in the liquid is better released.
The circulating carrier inlet 11 is connected with an inlet pipe, the inlet pipe is positioned in the cavity, the inlet pipe is connected with a spiral spray type spray head 18, the bottom of the cavity is provided with a circulating carrier outlet 12, and the top of the cavity is provided with a separated tail gas outlet 13.
The oil-water separation unit 2 includes the knockout drum, and the knockout drum is provided with first liquid feed inlet 21 and second liquid feed inlet 22, and first liquid feed inlet 21 and second liquid feed inlet 22 are respectively through the condensate outlet 31 of pipe connection circulation carrier export 12 and condenser, the knockout drum is provided with aqueous phase export 23 and oil phase export 24, aqueous phase export 23 is located knockout drum lower part or bottom, oil phase export 24 is located knockout drum upper portion, the oil phase export outside is provided with governing valve 25 to through pipe connection oil phase jar 26.
Be provided with overflow baffle 27 in the separator tank of oil phase export 24 inboard, the overflow baffle is the L type, be provided with porosely on the overflow baffle, overflow baffle and separator tank inner wall form oil phase and gather chamber 28, oil phase export is located oil phase and gathers chamber one side, the intracavity is gathered to the oil phase still is provided with level gauge 29, level gauge and governing valve electricity are connected.
And cooling circulating water is introduced into the condenser 3.
Be provided with the washing filler in the tail gas washing tower 5, tail gas washing tower bottom is connected condensation tail gas outlet 32, the top is provided with washing tail gas export 52, and upper portion is provided with washing pipe 53, is provided with the washing shower nozzle on the washing pipe, and 5 lower parts of tail gas washing tower are provided with washing liquid export 51, and washing pipe 53 connects washing liquid pond 55 and 5 lower parts of tail gas washing tower, is provided with the circulating pump on the washing pipe 53.
The absorption tower 4 includes two units arranged in parallel: the top of the absorption tower 4 is provided with an air inlet, the bottom of the absorption tower 4 is provided with an adsorbed tail gas outlet 43, the adsorbed tail gas outlet 43 is also connected with a nitrogen inlet pipe 41, the air inlet is connected with a washing tail gas outlet 52, and the air inlet is also connected with a nitrogen outlet pipe 42; and the air inlet, the adsorbed tail gas outlet, the nitrogen inlet pipe and the nitrogen outlet pipe of the absorption tower 4 are all provided with switch valves.
Example 2
In the apparatus described in embodiment 1, a plurality of distribution plates may be further disposed below the inlet pipe of the gas-liquid separation unit 1, and the distribution plates are provided with distribution holes, so that the gas-liquid mixture has sufficient time and sufficient path for separation.
A tail gas separation treatment method in a process for electrochemically synthesizing adiponitrile by acrylonitrile comprises the following steps:
gas-liquid separation is carried out on the gas-liquid mixed circulating carrier of the electrochemical synthesis unit in a gas-liquid separation unit, the obtained separated tail gas is condensed by a condenser, desalted water washing is carried out on the tail gas washing tower, and the active carbon adsorption step of an absorption tower is carried out;
the mixed fluid distributor in the gas-liquid separation unit is in a spiral spray type spray head, gas release is facilitated, the pressure is 0.1-0.4 MPa, the gas-liquid separation unit is arranged in a double-layer mode, the upper portion is a gas-phase collecting device, and the lower portion is a gas-liquid separation device. Spraying a gas-liquid mixed circulating carrier in the gas-liquid separation unit, allowing the liquid to downwards pass through a filler to fully release oxygen, allowing the liquid after gas release to enter an oil-water separator through a pipeline at the bottom of the gas-liquid separation unit, allowing an oil phase to float upwards, allowing the oil phase to enter an oil phase collection cavity through an overflow partition plate, and discharging the oil phase into an oil phase tank through a valve; the gas phase rises in the gas-liquid separation unit and passes through water vapor and acrylonitrile carried in the filler-captured gas phase, and the gas phase is mixed with nitrogen in a separation tail gas pipe and then enters a condenser.
The condenser condenses the gas at low temperature, condenses the organic phase in the tail gas, the condensed organic phase enters an oil-water separator, and the tail gas enters a tail gas washing tower; and tail gas enters from the bottom of the condenser, countercurrent flows in the condenser to exchange heat to 5 to-45 ℃, acrylonitrile gas carried in the tail gas is further condensed, and the condensate is discharged into the oil-water separator through a liquid discharge pipe.
Oil-water separator, liquid feed inlet are located the device bottom, and the aqueous phase export is located the bottom of device opposite side, for the increase dwell time, reduces the fluid disturbance, avoids the fluid short circuit condition, sets up the baffle in the device, and baffle upper portion punches, when the oil phase highly is higher than oil phase collection chamber overflow baffle, flows into the oil phase and gathers the chamber, and the oil phase height of oil phase collection intracavity is adjusted through level gauge and governing valve interlocking, keeps the liquid level at invariable liquid level, and the oil phase is gathered in succession.
Washing acrylonitrile in the tail gas by using industrial soft water in a tail gas washing tower, feeding the washed tail gas into an absorption tower, and feeding washing water into a rectifying tower of a rectifying section to separate and recycle the acrylonitrile; the tail gas is washed by desalted water, enters a tail gas washing tower from the bottom and passes through a washing packing layer from bottom to top to be in countercurrent contact with washing water from top to bottom, part of acrylonitrile in the tail gas is absorbed by the desalted water, the washing tail gas leaves the washing tower from the top, the washing water at the bottom of the washing tower is recycled, the temperature is controlled to be 10-30 ℃, when the washing water is saturated, the concentration of acrylonitrile in the washing water is 2-7%, continuous water inlet and drainage are adopted, the saturated washing water is sent to a rectification working section for distillation, and the acrylonitrile and the desalted water generated after distillation are recycled.
The absorption tower comprises two absorption towers which are connected in parallel, one absorption tower is used for absorbing, the other absorption tower is used for regenerating, and the two absorption towers are switched to use in turn at regular time; after the absorption tower runs for a period of time and is saturated, the absorption tower needs to be isolated and regenerated by nitrogen, at the moment, tail gas is switched to another tower for absorption and operation, nitrogen is introduced into the isolated absorption tower at the bottom for regeneration, and regenerated gas containing acrylonitrile at the top is returned to a tail gas pipeline and used as tail gas make-up gas.
Tail gas gets into at the absorption tower top, through the active carbon bed in the absorption tower, partial acrylonitrile adsorbs in the tail gas, tail gas after the absorption gets into next workshop section catalytic conversion further processing, after operation a period, active carbon reaches the saturation in the absorption tower, switches over tail gas to another absorption tower operation, the saturation tower is then regenerated with nitrogen gas, nitrogen gas gets into from the absorption tower bottom, the top goes out, carries partial acrylonitrile, use as the tail gas make-up gas, two absorption towers regularly switch over the use.
The method utilizes the principles of gas-liquid separation, oil-water separation, water washing and activated carbon adsorption, so that the gas-liquid after reaction releases a large amount of oxygen generated in the synthesis stage by the analytic principle, meanwhile, the liquid phase enters an oil-water separator for separation, the water phase is recycled as an electrolytic carrier, and the oil phase enters the next procedure for purification. Compared with the existing three-phase separator technology, the equipment avoids the standing separation process of oxygen in the water phase and the oil phase, thereby reducing the amount of organic gas carried in the oxygen release process, and carrying out secondary recovery on tail gas through a trap, a washing tower and an absorption tower, greatly reducing the content of organic matters in the tail gas, reducing the loss of acrylonitrile, and greatly reducing the treatment and recovery cost of subsequent tail gas.
The embodiments of the present invention have been described in detail with reference to the accompanying drawings, but the present invention is not limited to the above embodiments, and various changes can be made without departing from the spirit of the present invention within the knowledge of those skilled in the art.
Claims (7)
1. A tail gas separation device in a process for electrochemically synthesizing adiponitrile by acrylonitrile comprises a gas-liquid separation unit (1), an oil-water separation unit (2), a condenser (3), a tail gas washing tower (5) and an absorption tower (4),
the gas-liquid separation unit (1) is introduced with a gas-liquid mixed circulation carrier through a circulation carrier inlet (11), the gas-liquid separation unit is provided with a circulation carrier outlet (12) and a separation tail gas outlet (13), the circulation carrier outlet (12) is connected with the oil-water separation unit (2), the separation tail gas outlet (13) is connected with a condenser (3) through a separation tail gas pipe (14), a condensate outlet (31) of the condenser (3) is connected with the oil-water separation unit (2), and a condensation tail gas outlet (32) of the condenser (3) is connected with a tail gas washing tower (5); the washing liquid outlet (51) of tail gas scrubbing tower (5) accesss to rectifying column (7) of rectification workshop section, and absorption tower (4) are connected in washing tail gas outlet (52) of tail gas scrubbing tower (5), and the absorption tower is provided with nitrogen gas and advances pipe (41), nitrogen gas exit tube (42) and adsorbs tail gas export (43), catalytic conversion device (8) are connected in adsorption tail gas outlet (43), nitrogen gas advances pipe (41) and lets in nitrogen gas, and separation tail gas pipe (14) are connected in nitrogen gas exit tube (42).
2. The tail gas separation device in the process of electrochemically synthesizing adiponitrile by acrylonitrile according to claim 1, wherein the gas-liquid separation unit (1) comprises a cavity, a gas-liquid trap (15) is arranged at the upper part of the cavity, a gas-liquid separation device (16) is arranged at the lower part of the cavity, and a cavity is arranged in the middle of the cavity; the circulating carrier inlet (11) is connected with a feeding pipe, the feeding pipe is positioned in the cavity, a spiral spray type spray head (18) is arranged on the feeding pipe, a circulating carrier outlet (12) is arranged at the bottom of the cavity, and a separated tail gas outlet (13) is arranged at the top of the cavity.
3. The tail gas separation device in the process of electrochemically synthesizing adiponitrile by acrylonitrile according to claim 1, wherein the oil-water separation unit (2) comprises a separation tank, the separation tank is provided with a first liquid feed inlet (21) and a second liquid feed inlet (22), the first liquid feed inlet (21) and the second liquid feed inlet (22) are respectively connected with the circulating carrier outlet (12) and the condensate outlet (31) of the condenser through pipelines, the separation tank is provided with a water phase outlet (23) and an oil phase outlet (24), the water phase outlet (23) is positioned at the lower part or the bottom of the separation tank, the oil phase outlet (24) is positioned at the upper part of the separation tank, the outer side of the oil phase outlet is provided with a regulating valve (25), and the oil phase outlet is connected with the oil phase tank (26) through a pipeline.
4. The device for separating the tail gas in the process of electrochemically synthesizing adiponitrile according to claim 3, wherein an overflow partition plate (27) is arranged in the separation tank inside the oil phase outlet (24), the overflow partition plate is L-shaped, a hole is formed in the overflow partition plate, the overflow partition plate and the separation tank inner wall form an oil phase collection cavity (28), the oil phase outlet is located on one side of the oil phase collection cavity, a liquid level meter (29) is further arranged in the oil phase collection cavity, and the liquid level meter and the regulating valve are interlocked.
5. The device for separating the tail gas in the process of electrochemically synthesizing adiponitrile by acrylonitrile according to claim 1, wherein the condenser (3) is internally filled with cooling circulating water.
6. The tail gas separation device in the process of electrochemically synthesizing adiponitrile by acrylonitrile according to claim 1, wherein a washing filler is arranged in the tail gas washing tower (5), the bottom of the tail gas washing tower is connected with the condensed tail gas outlet (32), the top of the tail gas washing tower is provided with a washing tail gas outlet (52), the upper part of the tail gas washing tower is provided with a washing pipe (53), the washing pipe is provided with a washing nozzle, the lower part of the tail gas washing tower (5) is provided with a washing liquid outlet (51), the washing pipe (53) is connected with a washing liquid tank (55) and the lower part of the tail gas washing tower (5), and the washing pipe (53) is provided with a circulating pump.
7. The tail gas separation device in the process of electrochemically synthesizing adiponitrile by acrylonitrile according to claim 1, wherein the absorption tower (4) comprises two units arranged in parallel: the top of the absorption tower (4) is provided with an air inlet, the bottom of the absorption tower is provided with an adsorption tail gas outlet (43), the adsorption tail gas outlet (43) is also connected with a nitrogen inlet pipe (41), the air inlet is connected with a washing tail gas outlet (52), and the air inlet is also connected with a nitrogen outlet pipe (42); and the air inlet, the adsorbed tail gas outlet, the nitrogen inlet pipe and the nitrogen outlet pipe of the absorption tower (4) are all provided with switch valves.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202020397780.9U CN212141944U (en) | 2020-03-25 | 2020-03-25 | Tail gas separation device in acrylonitrile electrochemical synthesis adiponitrile technology |
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| Application Number | Priority Date | Filing Date | Title |
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| CN202020397780.9U CN212141944U (en) | 2020-03-25 | 2020-03-25 | Tail gas separation device in acrylonitrile electrochemical synthesis adiponitrile technology |
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| CN212141944U true CN212141944U (en) | 2020-12-15 |
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| CN202020397780.9U Active CN212141944U (en) | 2020-03-25 | 2020-03-25 | Tail gas separation device in acrylonitrile electrochemical synthesis adiponitrile technology |
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| PE01 | Entry into force of the registration of the contract for pledge of patent right |
Denomination of utility model: A kind of tail gas separation device in acrylonitrile electrochemical synthesis of adiponitrile process Effective date of registration: 20220804 Granted publication date: 20201215 Pledgee: Changzhi Tonghui Branch Equity Investment Partnership (Limited Partnership) Pledgor: Shanxi runheng Chemical Co.,Ltd. Registration number: Y2022980011968 |
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| PE01 | Entry into force of the registration of the contract for pledge of patent right |