CN108147940B - Device and method for recovering sulfur dioxide and butadiene in sulfolene - Google Patents

Device and method for recovering sulfur dioxide and butadiene in sulfolene Download PDF

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CN108147940B
CN108147940B CN201611103560.5A CN201611103560A CN108147940B CN 108147940 B CN108147940 B CN 108147940B CN 201611103560 A CN201611103560 A CN 201611103560A CN 108147940 B CN108147940 B CN 108147940B
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pressure
butadiene
sulfur dioxide
liquid
reduced
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CN108147940A (en
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赵永祥
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Petrochina Co Ltd
CNPC Northeast Refining and Chemical Engineering Co Ltd
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Petrochina Co Ltd
CNPC Northeast Refining and Chemical Engineering Co Ltd
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    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C7/00Purification; Separation; Use of additives
    • C07C7/005Processes comprising at least two steps in series
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B17/00Sulfur; Compounds thereof
    • C01B17/48Sulfur dioxide; Sulfurous acid
    • C01B17/50Preparation of sulfur dioxide
    • C01B17/56Separation; Purification

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Abstract

The invention discloses a device and a method for recovering sulfur dioxide and butadiene in sulfolene, and belongs to the field of recovery of sulfur dioxide and butadiene in sulfolene. The device is including the decompression flash distillation cauldron, jet pump, condenser, first recovery tank, the circulating pump that communicate in order, and wherein, decompression flash distillation cauldron passes through the pipeline and communicates with the export of sulfolene reactor, is provided with first pressure control valve on this pipeline. The outlet of the circulating pump is simultaneously communicated with the liquid inlet of the jet pump and the inlet of the sulfolene reactor through pipelines. And the second recovery tank is communicated with a liquid outlet of the reduced-pressure flash kettle through a pipeline. And the pressure control system can adjust the flow of the mixture of liquid-phase sulfur dioxide and butadiene input into the jet pump so as to adjust the flow of the mixture of gas-phase sulfur dioxide and butadiene pumped by the jet pump, and further adjust the pressure of the inner cavity of the reduced-pressure flash evaporation kettle within a preset range. The device can automatically realize the continuous and complete recovery of sulfur dioxide and butadiene, and avoids environmental pollution.

Description

Device and method for recovering sulfur dioxide and butadiene in sulfolene
Technical Field
The invention relates to the field of recovery of sulfur dioxide and butadiene in sulfolene, in particular to a device and a method for recovering sulfur dioxide and butadiene in sulfolene.
Background
Sulfolene, also known as butadiene sulfone, 3-thiophenylene dioxide, having the chemical formula C4H6O2S, can be synthesized by sulfur dioxide and butadiene under the action of a polymerization inhibitor (hydroquinone). However, the reaction for synthesizing sulfolene is a reversible reaction, and sulfur dioxide and butadiene cannot be completely converted into sulfolene, so that the waste gas after synthesizing the sulfolene or the liquid-phase sulfolene contains sulfur dioxide and butadiene. However, sulfur dioxide and butadiene are harmful gases, and if the waste gas after synthesizing sulfolene or the gas separated from liquid-phase sulfolene is directly discharged into the atmosphere, environmental pollution is easily causedAnd sulfur dioxide and butadiene used for synthesizing the sulfolene are wasted. Therefore, it is necessary to recycle sulfur dioxide and butadiene after synthesizing sulfolene, so as to improve the utilization rate of sulfur dioxide and butadiene and reduce the emission. Therefore, it is necessary to provide a device and a method capable of recovering sulfur dioxide and butadiene in sulfolene.
The prior art provides a device capable of recovering sulfur dioxide and butadiene in sulfolene, and the recovered sulfur dioxide and butadiene can be reused for synthesizing sulfolene. The device includes stirred tank, polymerization inhibitor jar, compressor, condenser, recovery jar, the pressure retaining valve that communicates in order through the pipeline. The specific recovery method comprises the following steps: firstly, filling nitrogen into a stirring kettle, starting stirring, controlling pressure, inputting a generated mixture of sulfolene, sulfur dioxide and butadiene into the stirring kettle, enabling a mixed gas of sulfur dioxide, butadiene and nitrogen to enter a polymerization inhibitor tank through a pipeline to fully contact with the polymerization inhibitor due to pressure difference, outputting the primarily separated mixed gas from the polymerization inhibitor tank, pressurizing by a compressor, inputting into a condenser to liquefy, and finally inputting into a recovery storage tank. At the moment, the nitrogen gas carries partial sulfur dioxide and butadiene gas, the sulfur dioxide and butadiene gas enter the stirring kettle again through a pressure retaining valve to purge the sulfolene solution in the stirring kettle, the steps are repeated for many times, and finally the nitrogen gas, the sulfur dioxide and the butadiene gas are discharged into the atmosphere after being desulfurized and purified by alkali liquor.
The inventor finds that the prior art has at least the following problems:
the efficiency of recycling sulfur dioxide and butadiene in sulfolene provided by the prior art is low, and the sulfur dioxide and butadiene are finally treated by alkali liquor.
Disclosure of Invention
The technical problem to be solved by the embodiments of the present invention is to provide a device and a method capable of completely recovering and utilizing sulfur dioxide and butadiene in sulfolene. The specific technical scheme is as follows:
in a first aspect, an embodiment of the present invention provides an apparatus for recovering sulfur dioxide and butadiene from sulfolene, the apparatus including a condenser, and a first recovery tank in communication with an outlet of the condenser through a line, the apparatus further including: the inlet of the reduced-pressure flash evaporation kettle is communicated with the outlet of the sulfolene reactor through a pipeline; the first pressure control valve is arranged on a pipeline at the inlet of the reduced-pressure flash kettle; the gas inlet of the jet pump is communicated with the gas outlet of the reduced-pressure flash evaporation kettle through a pipeline, and the gas-liquid outlet is communicated with the inlet of the condenser through a pipeline; the inlet of the circulating pump is communicated with the outlet of the first recovery tank through a pipeline, and the outlet of the circulating pump is simultaneously communicated with the liquid inlet of the jet pump and the inlet of the sulfolene reactor through pipelines; the second recovery tank is communicated with a liquid outlet of the reduced-pressure flash evaporation kettle through a pipeline; and the pressure control system is used for measuring the pressure of the inner cavity of the reduced-pressure flash evaporation kettle, adjusting the flow of the mixture of liquid-phase sulfur dioxide and butadiene input into the jet pump by the circulating pump according to the pressure, further driving the jet pump to suck the flow of the mixture of gas-phase sulfur dioxide and butadiene output by the reduced-pressure flash evaporation kettle, and further adjusting the pressure of the inner cavity of the reduced-pressure flash evaporation kettle within a preset range.
Specifically, as a preference, the device further comprises a hydrocyclone which is arranged in the inner cavity of the decompression flash still at the inlet.
In particular, as a preference, the device further comprises a foam breaking net arranged below the hydrocyclone.
Specifically, preferably, the device further comprises a heat-insulating jacket, circulating hot water at the temperature of 50-85 ℃ is introduced into the heat-insulating jacket, and the heat-insulating jacket is sleeved on the outer surface of the reduced-pressure flash evaporation kettle.
Specifically, preferably, the pressure control system comprises a pressure transmitter for measuring the pressure of the inner cavity of the reduced-pressure flash tank, a second pressure control valve arranged on a connecting pipeline between the jet pump and the circulating pump, and a pressure logic controller electrically connected with the pressure transmitter and the second pressure control valve; and the pressure logic controller receives the pressure information measured by the pressure transmitter, processes the pressure information, sends a pressure control instruction to the second pressure control valve according to a processing result, and adjusts the flow of the mixture of the liquid-phase sulfur dioxide and the butadiene input into the jet pump by the circulating pump according to the pressure control instruction by the second pressure control valve.
Specifically, preferably, the device further comprises a liquid level control system, wherein the liquid level control system comprises a liquid level meter for measuring the liquid level in the decompression flash still, a regulating valve arranged on a connecting pipeline between the decompression flash still and the second recovery tank, and a liquid level logic controller electrically connected with the liquid level meter and the regulating valve; and the liquid level logic controller receives the liquid level information measured by the liquid level meter, processes the liquid level information, sends a liquid level control instruction to the regulating valve according to a processing result, and the regulating valve regulates the flow of the liquid-phase sulfolene output by the reduced-pressure flash evaporation kettle according to the liquid level control instruction.
Particularly, as a preference, liquid level displays are arranged on the first recovery tank and the second recovery tank.
Specifically, preferably, temperature displays are arranged on pipelines at the lower part of the reduced-pressure flash still and the outlet of the condenser.
Specifically, it is preferable that the temperature display provided on the line at the outlet of the condenser is a thermal resistor.
In a second aspect, the present invention also provides a method for recovering sulfur dioxide and butadiene from sulfolene in the above apparatus, including:
the method comprises the following steps of inputting a mixture of sulfolene, sulfur dioxide and butadiene into a reduced-pressure flash evaporation kettle at a preset flow rate by controlling a first pressure control valve, and obtaining a liquid-phase sulfolene and a mixture of gas-phase sulfur dioxide and butadiene through the reduced-pressure flash evaporation treatment of the reduced-pressure flash evaporation kettle; the mixture of the gas-phase sulfur dioxide and the butadiene is input into a jet pump through a pipeline, is input into a condenser through a gas-liquid outlet of the jet pump to be condensed into a mixture of liquid-phase sulfur dioxide and butadiene, and is sequentially input into a first recovery tank and a circulating pump; a part of the mixture of the liquid-phase sulfur dioxide and the butadiene output by the circulating pump is input into a sulfolene reactor through a pipeline, the other part of the mixture of the liquid-phase sulfur dioxide and the butadiene is input into the jet pump through a pipeline under the control of a pressure control system, is mixed with the mixture of the gas-phase sulfur dioxide and the butadiene in the jet pump, is input into the condenser through a gas-liquid outlet of the jet pump for condensation, and is circulated repeatedly, in the process, the pressure control system adjusts the flow rate of the mixture of the liquid-phase sulfur dioxide and the butadiene input into the jet pump according to the pressure of the inner cavity of the reduced-pressure flash kettle so as to adjust the flow rate of the mixture of the gas-phase sulfur dioxide and the butadiene pumped by the jet pump, and further adjust the pressure of the inner cavity of the reduced-pressure flash kettle within; meanwhile, the liquid-phase sulfolene is conveyed into a second recovery tank from a liquid outlet of the reduced-pressure flash kettle through a pipeline.
The technical scheme provided by the embodiment of the invention has the following beneficial effects:
according to the device for recovering sulfur dioxide and butadiene from sulfolene provided by the embodiment of the invention, the pressure of the inner cavity of the sulfolene reactor and the flow of the mixture of sulfolene, sulfur dioxide and butadiene entering the pressure-reducing flash evaporation kettle are conveniently controlled by arranging the pressure-reducing flash evaporation kettle and the first pressure control valve, and after the pressure-reducing flash evaporation treatment of the pressure-reducing flash evaporation kettle, the mixture of liquid-phase sulfolene, gas-phase sulfur dioxide and butadiene is conveniently separated so as to be respectively input into the second recovery tank and the jet pump. Through setting up the jet pump, be convenient for suck the gaseous phase sulfur dioxide in the decompression flash evaporation cauldron and the mist of butadiene under pressure control system's control to the pressure of adjustment decompression flash evaporation cauldron inner chamber, sulfur dioxide and butadiene are retrieved to the later stage of being convenient for, and the gaseous phase and the liquid phase of sulfur dioxide and butadiene in the jet pump are mixed in addition, can avoid getting into the sulfolene emergence desublimation in the condenser, block up equipment and pipeline, retrieve and produce in order to realize the serialization. And the circulating pump is arranged, so that the mixture of the liquid-phase sulfur dioxide and the butadiene can be conveniently recovered and circulated. Through setting up pressure control system, be convenient for adjust the pressure of decompression flash distillation cauldron inner chamber, sulfur dioxide, butadiene, sulfolene gas-liquid separation of being convenient for make whole device realize automatic sulfur dioxide and butadiene of retrieving. Therefore, the device provided by the embodiment of the invention can automatically realize continuous and complete recovery of sulfur dioxide and butadiene, and is used for synthesizing sulfolene, so that environmental pollution caused by emission of sulfur dioxide and butadiene is avoided.
Drawings
In order to more clearly illustrate the technical solutions in the embodiments of the present invention, the drawings needed to be used in the description of the embodiments will be briefly introduced below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art to obtain other drawings based on these drawings without creative efforts.
FIG. 1 is a schematic structural diagram of an apparatus for recovering sulfur dioxide and butadiene from sulfolene provided by an embodiment of the invention.
Wherein the reference numerals denote:
1 a condenser, a condenser and a condenser,
2 a first recovery tank is arranged in the first recovery tank,
3, a pressure reduction flash evaporation kettle is used,
4 a sulfolene reactor, a reactor of sulfolene,
5 a first pressure control valve for controlling the pressure of the gas,
6, a jet pump is arranged on the upper portion of the cylinder,
7 a circulating pump is arranged on the base,
8 of the second recovery tank, and a second recovery tank,
9 a pressure control system for controlling the pressure of the gas,
901 a pressure transmitter for a gas turbine, the pressure transmitter,
902 a second pressure control valve for controlling the flow of fluid,
903 a pressure logic controller for the pressure of the gas,
10 a liquid cyclone separator, wherein the liquid cyclone separator is arranged in the shell,
11 a foam breaking net for removing the foam from the air,
12 a heat-preserving jacket is arranged on the upper portion of the shell,
13 a liquid level control system for the liquid level control system,
1301 a liquid level meter, wherein the liquid level meter is arranged on the liquid level meter,
1302 the valve is adjusted such that,
1303 a logic controller for controlling the liquid level of the liquid,
14 thermal resistance.
Detailed Description
Unless defined otherwise, all technical terms used in the examples of the present invention have the same meaning as commonly understood by one of ordinary skill in the art. In order to make the objects, technical solutions and advantages of the present invention more apparent, embodiments of the present invention will be described in detail with reference to the accompanying drawings.
In a first aspect, the embodiment of the present invention provides an apparatus for recovering sulfur dioxide and butadiene from sulfolene, as shown in fig. 1, the apparatus includes a condenser 1, and a first recovery tank 2 connected to an outlet of the condenser 1 through a pipeline, the apparatus further includes: the system comprises a reduced-pressure flash kettle 3, a first pressure control valve 5, a jet pump 6, a circulating pump 7, a second recovery tank 8 and a pressure control system 9, wherein the inlet of the reduced-pressure flash kettle 3 is communicated with the outlet of a sulfolene reactor 4 through a pipeline; the first pressure control valve 5 is arranged on a pipeline at the inlet of the reduced-pressure flash still 3; an inlet of the jet pump 6 is communicated with an air outlet of the reduced-pressure flash evaporation kettle 3 through a pipeline, and a gas-liquid outlet is communicated with an inlet of the condenser 1 through a pipeline; an inlet of the circulating pump 7 is communicated with an outlet of the first recovery tank 2 through a pipeline, and an outlet of the circulating pump is simultaneously communicated with a liquid inlet of the jet pump 6 and an inlet of the sulfolene reactor 4 through pipelines; the second recovery tank 8 is communicated with a liquid outlet of the reduced-pressure flash kettle 3 through a pipeline; pressure control system 9 for measure the pressure of 3 inner chambers of decompression flash distillation cauldron, and come the adjustment according to pressure and input the flow of the mixture of liquid phase sulfur dioxide and butadiene in jet pump 6 by circulating pump 7, and then drive the flow of adjusting jet pump 6 suction by the gaseous phase sulfur dioxide of 3 outputs in decompression flash distillation cauldron and the mixture of butadiene, and then the pressure of 3 inner chambers of adjustment decompression flash distillation cauldron is in predetermineeing the within range.
The following description is given of the operation principle of the apparatus for recovering sulfur dioxide and butadiene from sulfolene provided in the embodiment of the present invention:
the method comprises the steps of firstly starting a pressure control system 9 to enable the pressure of an inner cavity of a reduced-pressure flash evaporation kettle 3 to be within a preset range (the preset range of the pressure is vacuum or micro-positive pressure to guarantee normal operation of reduced-pressure flash evaporation), then controlling a first pressure control valve 5 to enable a mixture of sulfolene, sulfur dioxide and butadiene output by a sulfolene reactor 4 to enter the reduced-pressure flash evaporation kettle 3, wherein the mixture of liquid-phase sulfolene and gas-phase sulfur dioxide and butadiene is obtained through reduced-pressure flash evaporation treatment of the reduced-pressure flash evaporation kettle 3 because the boiling points of the sulfur dioxide and the butadiene are much lower than that of the sulfolene, the mixture of the gas-phase sulfur dioxide and the butadiene floats upwards to be located at the upper part of the inner cavity of the reduced-pressure flash evaporation kettle 3, and the liquid-phase sulfo. Then the mixture of gas-phase sulfur dioxide and butadiene is pumped into a jet pump 6 through a pipeline from an air outlet of a decompression flash evaporation kettle 3, then the mixture enters a condenser 1 for liquefaction, then the mixture of liquid-phase sulfur dioxide and butadiene enters a first recovery tank 2 through a pipeline from the condenser 1, further enters a circulating pump 7, a part of the mixture of liquid-phase sulfur dioxide and butadiene output by the circulating pump 7 enters a sulfolene reactor 4 to synthesize sulfolene again, and a part of the mixture of liquid-phase sulfur dioxide and butadiene enters the jet pump 6 again under the action of a pressure control system 9 and is mixed with the mixture of gas-phase sulfur dioxide and butadiene, and then enters the condenser 1 again for repeated circulation. In the process, the pressure control system 9 adjusts the flow of the mixture of liquid-phase sulfur dioxide and butadiene input into the jet pump 6 by the circulating pump 7 through a pipeline according to the measured pressure of the inner cavity of the reduced-pressure flash evaporation kettle 3, so as to adjust the flow of the mixture of gas-phase sulfur dioxide and butadiene output by the reduced-pressure flash evaporation kettle 3 sucked by the jet pump 6, and further adjust the pressure of the inner cavity of the reduced-pressure flash evaporation kettle 3, so that the pressure is in a preset range, and the mixture of input sulfolene, sulfur dioxide and butadiene can be subjected to reduced-pressure flash evaporation.
Meanwhile, the liquid-phase sulfolene is conveyed into the second recovery tank 8 from the liquid outlet of the reduced-pressure flash kettle 3 through a pipeline.
It should be noted that the preset range of the pressure in the inner cavity of the reduced-pressure flash evaporation kettle 3 is vacuum or micro-positive pressure, which is smaller than the pressure of the mixture of sulfolene, sulfur dioxide and butadiene input into the reduced-pressure flash evaporation kettle, so that the reduced-pressure flash evaporation of the mixture is realized under the condition of near vacuum degree. The gas outlet and the liquid outlet of the decompression flash evaporation kettle 3 are respectively positioned at the top and the bottom of the decompression flash evaporation kettle 3, so that the mixture of the gas-phase sulfur dioxide and the butadiene after decompression flash evaporation and the liquid-phase sulfolene are respectively input into a downstream pipeline from the upper part and the lower part of the decompression flash evaporation kettle 3. When the flow of the mixture of liquid-phase sulfur dioxide and butadiene in the input jet pump 6 is large, the mixture of a large amount of gas-phase sulfur dioxide and butadiene is wound, so that the flow of the mixture of liquid-phase sulfur dioxide and butadiene entering the jet pump 6 can be adjusted by adjusting the flow of the mixture of liquid-phase sulfur dioxide and butadiene entering the jet pump 6, the pressure of the inner cavity of the reduced-pressure flash kettle 3 is adjusted, the pressure meets the reduced-pressure flash conditions, and the mixture of sulfolene, sulfur dioxide and butadiene is ensured to be separated into the mixture of liquid-phase sulfolene, gas-phase sulfur dioxide and butadiene through reduced-pressure flash treatment.
Based on the above, according to the device for recovering sulfur dioxide and butadiene from sulfolene provided in the embodiment of the present invention, by providing the reduced-pressure flash evaporation kettle 3 and the first pressure control valve 5, it is convenient to control the pressure in the inner cavity of the sulfolene reactor 4 and the flow rate of the mixture of sulfolene, sulfur dioxide and butadiene entering the reduced-pressure flash evaporation kettle 3, and after the reduced-pressure flash evaporation treatment in the reduced-pressure flash evaporation kettle 3, it is convenient to separate the liquid-phase sulfolene from the mixture of gas-phase sulfur dioxide and butadiene, so as to input the mixture into the second recovery tank 8 and the jet pump 6, respectively. Through setting up jet pump 6, be convenient for suck the gaseous phase sulfur dioxide in the decompression flash evaporation cauldron 3 and the mist of butadiene under pressure control system 9's control, with the pressure of 3 inner chambers of adjustment decompression flash evaporation cauldron, sulfur dioxide and butadiene are retrieved to the later stage of being convenient for, and the gaseous phase and the liquid phase of sulfur dioxide and butadiene in jet pump 6 mix, can avoid getting into the sulfolene in condenser 1 and take place the desublimation, block up equipment and pipeline, retrieve and produce in order to realize the serialization. And the circulating pump 7 is arranged, so that the mixture of the liquid-phase sulfur dioxide and the butadiene can be conveniently recovered and circulated. Through setting up pressure control system 9, be convenient for adjust the pressure of 3 inner chambers of decompression flash distillation cauldron, sulfur dioxide and butadiene, sulfolene gas-liquid separation of being convenient for make whole device realize automatic sulfur dioxide and butadiene of retrieving. Therefore, the device provided by the embodiment of the invention can automatically realize continuous and complete recovery of sulfur dioxide and butadiene, and is used for synthesizing sulfolene, so that environmental pollution caused by emission of sulfur dioxide and butadiene is avoided.
Specifically, as shown in fig. 1, the apparatus provided in the embodiment of the present invention further includes a hydrocyclone 10, the hydrocyclone 10 is disposed in an inner cavity of the reduced-pressure flash tank 3 at an inlet, and a foam breaking net 11 is disposed below the hydrocyclone 10, and the hydrocyclone 10 and the foam breaking net 11 cooperate to facilitate efficient gas-liquid separation of sulfur dioxide, butadiene and sulfolene. Wherein, the hydrocyclone 10 can separate out gas-phase sulfur dioxide and butadiene in the liquid-phase sulfolene, and the foam breaking net 11 can completely break up foam in the liquid-phase sulfolene, so that the gas-phase sulfur dioxide and butadiene are completely separated out from the liquid-phase sulfolene, and the recovered liquid-phase sulfolene with high purity is obtained. The hydrocyclone 10 is commercially available, and the foam breaking net 11 may be a net formed by interlacing iron wires.
Specifically, the device provided by the embodiment of the invention further comprises a heat-insulating jacket 12, circulating hot water at 50-85 ℃ is introduced into the heat-insulating jacket 12, the heat-insulating jacket 12 is sleeved on the outer surface of the reduced-pressure flash evaporation kettle 3 to ensure that the temperature of the material in the reduced-pressure flash evaporation kettle 3 is higher than 50 ℃, for example, 50 ℃, 55 ℃, 60 ℃, 65 ℃, 70 ℃, 75 ℃, 80 ℃, 85 ℃ and the like, and the heat-insulating jacket 12 can be arranged to play a role in heat insulation and heat insulation, so that the mixture of the sulfolene, the sulfur dioxide and the butadiene can be efficiently flashed and separated from gas and liquid in the reduced-pressure flash evaporation kettle 3.
Specifically, in the embodiment of the present invention, as shown in fig. 1, the pressure control system 9 includes a pressure transmitter 901 for measuring the pressure in the cavity of the reduced-pressure flash tank 3, a second pressure control valve 902 provided on the connection line between the jet pump 6 and the circulation pump 7, and a pressure logic controller 903 electrically connected to the pressure transmitter 901 and the second pressure control valve 902; the pressure logic controller 903 receives the pressure information measured by the pressure transmitter 901, processes the pressure information, sends a pressure control command to the second pressure control valve 902 according to the processing result, and according to the pressure control command, the second pressure control valve 902 adjusts the flow rate of the mixture of the liquid-phase sulfur dioxide and the butadiene input into the jet pump 6 by the circulating pump 7. Specifically, when the pressure measured by the pressure transmitter 901 is within a preset range, the mixture of gas-phase sulfur dioxide and butadiene input to the jet pump 6 from the reduced-pressure flash tank 3 and the mixture of liquid-phase sulfur dioxide and butadiene input to the jet pump 6 from the circulating pump 7 are kept at the current flow rate; when the existing flow is not within the preset range, the pressure logic controller 903 receives the pressure information measured by the pressure transmitter 901, processes the pressure information, and sends a pressure control instruction to the second pressure control valve 902, according to the pressure control instruction, the second pressure control valve 902 increases (decreases) the flow of the liquid-phase sulfur dioxide and butadiene entering the jet pump 6, and further increases (decreases) the flow of the gas-phase sulfur dioxide and butadiene input into the jet pump 6, so that the pressure in the inner cavity of the reduced-pressure flash evaporation kettle 3 is decreased (increased) to be within the preset pressure range. It should be noted that the pressure logic controller 903 is a computer, and a pressure logic control system is provided on the computer.
Specifically, as shown in fig. 1, the apparatus provided in the embodiment of the present invention further includes a liquid level control system 13, where the liquid level control system 13 includes a liquid level meter 1301 for measuring the liquid level inside the reduced-pressure flash still 3, a regulating valve 1302 arranged on a connecting pipeline between the reduced-pressure flash still 3 and the second recovery tank 8, and a liquid level logic controller 1303 electrically connected to the liquid level meter 1301 and the regulating valve 1302; and the liquid level logic controller 1303 receives the liquid level information measured by the liquid level meter 1301, processes the liquid level information, sends a liquid level control instruction to the regulating valve 1302 according to the processing result, and regulates the flow of the liquid-phase sulfolene output by the decompression flash evaporation kettle 3 by the regulating valve 1302 according to the liquid level control instruction. The liquid level control system 13 is arranged, so that the flow of the liquid-phase sulfolene entering the second recovery tank 8 from the reduced-pressure flash still 3 can be automatically adjusted. Specifically, when the liquid level measured by the liquid level meter 1301 is within a preset range, the measured liquid level information is transmitted to the liquid level logic controller 1303, the liquid level logic controller 1303 processes the liquid level information, sends a liquid level control instruction to the regulating valve 1302 according to the result, and according to the liquid level control instruction, the regulating valve 1302 adjusts to keep the flow rate of the liquid-phase sulfolene input into the second recovery tank 8 unchanged; when the liquid level measured by the liquid level meter 1301 is not within the preset range, the above process is repeated, except that the regulating valve 1302 is adjusted to increase (decrease) the flow rate of the liquid-phase sulfolene fed into the second recovery tank 8, so that the liquid level of the liquid-phase sulfolene in the inner cavity of the reduced-pressure flash tank 3 is within the preset range. In addition, be provided with liquid level display on first recovery tank 2, the second recovery tank 8 to observe the liquid level of liquid in the corresponding device, liquid level display can be for frosting formula liquid level indicator, glass tube formula liquid level indicator, oil pocket formula liquid level indicator, remote liquid level indicator etc. for the liquid level in the corresponding equipment of visual observation.
Specifically, in the embodiment of the present invention, temperature displays are disposed on the pipelines at the lower part of the reduced-pressure flash evaporation kettle 3 and at the outlet of the condenser 1, so as to observe the temperature of the liquid sulfolene in the reduced-pressure flash evaporation kettle 3 and the temperature of the mixture of the liquid-phase sulfur dioxide and butadiene output by the condenser 1, and further adjust the corresponding operating parameters, so that the reduced-pressure flash evaporation kettle 3 and the condenser 1 are in the optimal operating state. As shown in fig. 1, the temperature display device disposed on the pipeline at the outlet of the condenser 1 is a thermal resistor 14, and the thermal resistor 14 measures the temperature based on the characteristic that the resistance value of the metal conductor increases with the increase of the temperature, and the measurement accuracy is high and the performance is stable.
In a second aspect, the embodiments of the present invention also provide a method for recovering sulfur dioxide and butadiene from sulfolene using the above apparatus, the method comprising:
the mixture of the sulfolene, the sulfur dioxide and the butadiene is input into the decompression flash evaporation kettle 3 at a preset flow rate by controlling the first pressure control valve 5, and the mixture of the liquid-phase sulfolene and the gas-phase sulfur dioxide and the butadiene is obtained through decompression flash evaporation treatment of the decompression flash evaporation kettle 3.
Wherein, the mixture of gas-phase sulfur dioxide and butadiene is input into the jet pump 6 through a pipeline, and is input into the condenser 1 through a gas-liquid outlet of the jet pump 6 to be condensed into a mixture of liquid-phase sulfur dioxide and butadiene, and is input into the first recovery tank 2 and the circulating pump 7 in sequence.
A part of the mixture of liquid-phase sulfur dioxide and butadiene output by the circulating pump 7 is input into the sulfolene reactor 4 through a pipeline, the other part of the mixture of liquid-phase sulfur dioxide and butadiene is input into the jet pump 6 through a pipeline under the control of the pressure control system 9 and is mixed with the mixture of gas-phase sulfur dioxide and butadiene in the jet pump 6, then the mixture is input into the condenser 1 through a gas-liquid outlet of the jet pump 6 for condensation and repeated circulation, and in the process, the pressure control system 9 adjusts the flow rate of the mixture of liquid-phase sulfur dioxide and butadiene input into the jet pump 6 according to the pressure in the inner cavity of the reduced-pressure flash kettle 3 so as to adjust the flow rate of the mixture of gas-phase sulfur dioxide and butadiene pumped by the jet pump 6 and further adjust the pressure in the inner cavity of the reduced;
meanwhile, the liquid-phase sulfolene is conveyed into the second recovery tank 8 from the liquid outlet of the reduced-pressure flash kettle 3 through a pipeline.
The process for recycling sulfur dioxide and butadiene in the sulfolene is automatic recycling, can realize the complete recycling of sulfur dioxide and butadiene, can be used for re-synthesizing the sulfolene, and avoids the environmental pollution caused by the discharge of sulfur dioxide and butadiene.
Specifically, in the above method, the pressure control system 9 adjusts the pressure in the inner cavity of the reduced-pressure flash evaporation kettle 3 to be within a preset range, where the preset range may be micro-positive pressure or vacuum, so as to be smaller than the pressure of the mixture of sulfolene, sulfur dioxide and butadiene input into the reduced-pressure flash evaporation kettle 3, so as to ensure that the mixture is flashed into a mixture of gas-phase sulfur dioxide and butadiene and liquid-phase sulfolene. Further, the mixture input into the decompression flash evaporation kettle 3 is input at a preset flow rate by controlling the first pressure control valve 5, so that the decompression flash evaporation effect after the mixture enters the decompression flash evaporation kettle 3 is good. Further, the mixture fed into the vacuum flash still 3 can be separated by the action of the hydrocyclone 10 and the foam breaking net 11, and the gas phase and the liquid phase can be fed into the downstream pipeline through the gas phase outlet at the upper part and the liquid phase outlet at the lower part of the vacuum flash still 3, respectively.
Wherein, the mixture of gas-phase sulfur dioxide and butadiene is inputted into the jet pump 6 and the condenser 1 in sequence through the pipeline to become a mixture of liquid-phase sulfur dioxide and butadiene, further, the mixture of liquid-phase sulfur dioxide and butadiene is inputted into the first recovery tank 2 and the circulating pump 7 in sequence, then a part of the mixture of liquid-phase sulfur dioxide and butadiene is recovered for synthesizing sulfolene, the other part of the mixture of liquid-phase sulfur dioxide and butadiene is inputted into the jet pump 6 under the action of the second pressure control valve 902 to be mixed with the mixture of gas-phase sulfur dioxide and butadiene in the jet pump 6, the mixture of liquid-phase sulfur dioxide and butadiene is adopted as a solvent in the jet pump 6 to be mixed with a trace amount of liquid-phase sulfolene entering the jet pump 6, thereby preventing the trace amount of liquid-phase sulfolene from generating desublimation when being inputted into the condenser 1 and, and the mixture of the partial liquid-phase sulfur dioxide and the butadiene is input into the jet pump 6 again, so that the operating conditions of the jet pump 6 are met.
The present invention will be further described below by way of specific examples.
In the following examples, those whose operations are not subject to the conditions indicated, are carried out according to the conventional conditions or conditions recommended by the manufacturer.
Example 1
The embodiment provides a device for recovering sulfur dioxide and butadiene in sulfolene, and as shown in figure 1, the device comprises a reduced-pressure flash evaporation kettle 3, a jet pump 6, a condenser 1, a first recovery tank 2 and a circulating pump 7 which are communicated in sequence. The liquid outlet of decompression flash cauldron 3 passes through the pipeline and retrieves jar 8 intercommunication with the second, and still is provided with governing valve 1302 on the connecting line between decompression flash cauldron 3 and the second recovery jar 8. The circulating pump 7 is simultaneously communicated with the liquid inlets of the sulfolene reactor 4 and the jet pump 6 through pipelines, and a second pressure control valve 902 is arranged on the pipeline between the jet pump 6 and the circulating pump 7. The inner cavity of the decompression flash evaporation kettle 3 is provided with a hydrocyclone 10, and a foam breaking net 11 is arranged below the hydrocyclone 10. The device also comprises a pressure control system 9, wherein the pressure control system 9 comprises a pressure transmitter 901 on the reduced-pressure flash still 3, a second pressure control valve 902 arranged on a connecting pipeline between the jet pump 6 and the circulating pump 7, and a pressure logic controller 903 electrically connected with the pressure transmitter 901 and the second pressure control valve 902; the pressure logic controller 903 processes the data from the pressure transmitter 901, and then adjusts the flow rate of the mixture of liquid-phase sulfur dioxide and butadiene fed into the jet pump 6 by the circulating pump 7 through the second pressure control valve 902, so as to adjust the flow rate of the mixture of gas-phase sulfur dioxide and butadiene pumped by the jet pump 6 and output from the pressure-reducing flash still 3, and further adjust the pressure in the inner cavity of the pressure-reducing flash still 3.
Example 2
The apparatus provided in example 1 was used to evaluate the vacuum flash evaporation effect of the vacuum flash evaporation vessel 3. Wherein the simulated mixture comprises: the mixture enters a reduced-pressure flash evaporation kettle 3 with different vacuum degrees for reduced-pressure flash evaporation treatment by a flow meter, 1298kg/h of sulfolene, 235.23kg/h of sulfur dioxide and 65.89kg/h of butadiene respectively, wherein the temperature of the mixture is 110 ℃, the pressure of the mixture is 3.6MPa, the mixture is reduced to 1.0MPa through a first pressure control valve 5, reduced-pressure flash evaporation is realized in the reduced-pressure flash evaporation kettle 3, then the liquid-phase sulfolene is collected in a second recovery tank 8 with the temperature of-20 ℃, and the flow rates of the sulfur dioxide and the butadiene in the liquid-phase sulfolene are obtained through simulation, and relevant parameters are shown in the following table 1:
TABLE 1
Pressure/bar in the reduced-pressure flash still 0.05 0.10 0.20 0.30 0.40 0.50 0.60
Sulfur dioxide/(kg/h) 1.86 3.69 7.28 10.82 14.30 17.73 21.12
Butadiene/(kg/h) 0.80 1.57 3.08 4.55 5.97 7.35 8.64
Temperature of liquid phase of reduced pressure flash evaporation kettle/° c 69.1 69.8 70.8 71.7 72.4 73.1 73.8
As can be seen from table 1, as the pressure in the reduced-pressure flash evaporation kettle 3 increases, the flow rates of sulfur dioxide and butadiene in the liquid-phase sulfolene increase, so the lower the pressure in the reduced-pressure flash evaporation kettle 3 is, the better the reduced-pressure flash evaporation effect is, the more complete the separation of sulfur dioxide and butadiene from sulfolene is, the better the recovery effect of sulfur dioxide and butadiene is.
Example 3
The apparatus provided in example 1 was used to evaluate the vacuum flash evaporation effect of the vacuum flash evaporation vessel 3. This example is the same as example 2, except that the simulated mixture comprises: flow meters are used for measuring 1298kg/h of sulfolene, 235.23kg/h of sulfur dioxide and 33kg/h of butadiene, and the flow rates of the sulfur dioxide and the butadiene in the liquid-phase sulfolene after the reduced-pressure flash evaporation in the reduced-pressure flash evaporation kettle 3 are obtained through simulation, wherein the relevant parameters are shown in the following table 2:
TABLE 2
Figure BDA0001170915450000121
As can be seen from table 2, as the pressure in the reduced-pressure flash evaporation kettle 3 increases, the flow rates of sulfur dioxide and butadiene in the liquid-phase sulfolene increase, so the lower the pressure in the reduced-pressure flash evaporation kettle 3 is, the better the reduced-pressure flash evaporation effect is, the more complete the separation of sulfur dioxide and butadiene from sulfolene is, the better the recovery effect of sulfur dioxide and butadiene is.
Example 4
The apparatus provided in example 1 was used to evaluate the vacuum flash evaporation effect of the vacuum flash evaporation vessel 3. This example is the same as example 2, except that the simulated mixture comprises: flow meters are used for measuring 1298kg/h of sulfolene, 200kg/h of sulfur dioxide and 33kg/h of butadiene, and the flow rates of the sulfur dioxide and the butadiene in the liquid-phase sulfolene after the reduced-pressure flash evaporation in the reduced-pressure flash evaporation kettle 3 are obtained through simulation, wherein the relevant parameters are shown in the following table 3:
TABLE 3
Figure BDA0001170915450000122
As can be seen from table 3, as the pressure in the reduced-pressure flash evaporation kettle 3 increases, the flow rates of sulfur dioxide and butadiene in the liquid-phase sulfolene increase, so the lower the pressure in the reduced-pressure flash evaporation kettle 3 is, the better the reduced-pressure flash evaporation effect is, the more complete the separation of sulfur dioxide and butadiene from sulfolene is, the better the recovery effect of sulfur dioxide and butadiene is.
As can be seen from the above examples 2 to 4, the smaller the pressure in the reduced-pressure flash evaporation kettle 3 provided in the embodiment of the present invention is, the better the flash evaporation separation effect of sulfur dioxide and butadiene in the liquid-phase sulfolene is.
The above description is only exemplary of the present invention and should not be taken as limiting the scope of the present invention, as any modifications, equivalents, improvements and the like made within the spirit and principle of the present invention should be included in the scope of the present invention.

Claims (9)

1. An apparatus for recovering sulfur dioxide and butadiene from sulfolene, comprising a condenser (1) and a first recovery tank (2) in communication with the outlet of the condenser (1) through a line, characterized in that it further comprises: the inlet of the reduced-pressure flash evaporation kettle (3) is communicated with the outlet of the sulfolene reactor (4) through a pipeline;
a first pressure control valve (5) arranged on a pipeline at the inlet of the reduced-pressure flash still (3);
the air inlet of the jet pump (6) is communicated with the air outlet of the reduced-pressure flash evaporation kettle (3) through a pipeline, and the gas-liquid outlet is communicated with the inlet of the condenser (1) through a pipeline;
the inlet of the circulating pump (7) is communicated with the outlet of the first recovery tank (2) through a pipeline, and the outlet of the circulating pump is simultaneously communicated with the liquid inlet of the jet pump (6) and the inlet of the sulfolene reactor (4) through pipelines;
the second recovery tank (8) is communicated with a liquid outlet of the reduced-pressure flash kettle (3) through a pipeline;
the pressure control system (9) is used for measuring the pressure of the inner cavity of the reduced-pressure flash evaporation kettle (3), adjusting the flow of the mixture of liquid-phase sulfur dioxide and butadiene input into the jet pump (6) by the circulating pump (7) according to the pressure, further driving and adjusting the flow of the mixture of gas-phase sulfur dioxide and butadiene output by the reduced-pressure flash evaporation kettle (3) sucked by the jet pump (6), and further adjusting the pressure of the inner cavity of the reduced-pressure flash evaporation kettle (3) within a preset range;
the pressure control system (9) comprises a pressure transmitter (901) for measuring the pressure in the inner cavity of the reduced-pressure flash still (3), a second pressure control valve (902) arranged on a connecting pipeline between the jet pump (6) and the circulating pump (7), and a pressure logic controller (903) electrically connected with the pressure transmitter (901) and the second pressure control valve (902);
the pressure logic controller (903) receives the pressure information measured by the pressure transmitter (901), processes the pressure information, sends a pressure control command to the second pressure control valve (902) according to the processing result, and the second pressure control valve (902) adjusts the flow of the mixture of the liquid-phase sulfur dioxide and the butadiene input into the jet pump (6) by the circulating pump (7) according to the pressure control command.
2. The apparatus according to claim 1, further comprising a hydrocyclone (10), the hydrocyclone (10) being arranged in an inner cavity of the reduced-pressure flash vessel (3) at the inlet.
3. The device according to claim 2, characterized in that it further comprises a de-foaming screen (11) arranged below the hydrocyclone (10).
4. The device according to claim 1, further comprising a heat-insulating jacket (12), wherein circulating hot water with the temperature of 50-85 ℃ is introduced into the heat-insulating jacket (12), and the heat-insulating jacket (12) is sleeved on the outer surface of the reduced-pressure flash kettle (3).
5. The apparatus according to claim 1, further comprising a liquid level control system (13), the liquid level control system (13) comprising a liquid level meter (1301) for measuring the liquid level inside the reduced pressure flash tank (3), a regulating valve (1302) provided on a connection line between the reduced pressure flash tank (3) and the second recovery tank (8), and a liquid level logic controller (1303) electrically connected to the liquid level meter (1301) and the regulating valve (1302);
the liquid level logic controller (1303) receives the liquid level information measured by the liquid level meter (1301), processes the liquid level information, sends a liquid level control instruction to the regulating valve (1302) according to a processing result, and according to the liquid level control instruction, the regulating valve (1302) adjusts the flow of the liquid-phase sulfolene output by the reduced-pressure flash kettle (3).
6. The device according to claim 1, characterized in that liquid level displays are arranged on the first recovery tank (2) and the second recovery tank (8).
7. The apparatus according to claim 1, characterized in that the lower part of the vacuum flash still (3) and the pipeline at the outlet of the condenser (1) are provided with temperature displays.
8. The device according to claim 7, characterized in that the temperature display provided on the line at the outlet of the condenser (1) is a thermal resistor (14).
9. A process for the recovery of sulfur dioxide and butadiene from sulfolene using the apparatus of any of claims 1 to 8, wherein said process comprises:
the method comprises the following steps of (1) inputting a mixture of sulfolene, sulfur dioxide and butadiene into a reduced-pressure flash evaporation kettle (3) at a preset flow rate by controlling a first pressure control valve (5), and obtaining a liquid-phase sulfolene and a mixture of gas-phase sulfur dioxide and butadiene through the reduced-pressure flash evaporation treatment of the reduced-pressure flash evaporation kettle (3);
the mixture of the gas-phase sulfur dioxide and the butadiene is input into a jet pump (6) through a pipeline, is input into a condenser (1) through a gas-liquid outlet of the jet pump (6) and is condensed into a mixture of liquid-phase sulfur dioxide and butadiene, and is sequentially input into a first recovery tank (2) and a circulating pump (7);
a part of the liquid-phase mixture of sulfur dioxide and butadiene output by the circulating pump (7) is input into a sulfolene reactor (4) through a pipeline, the other part of the liquid-phase mixture of sulfur dioxide and butadiene is input into the jet pump (6) through a pipeline under the control of a pressure control system (9) and is mixed with the gas-phase mixture of sulfur dioxide and butadiene in the jet pump (6), then the mixture is input into the condenser (1) through a gas-liquid outlet of the jet pump (6) to be condensed, and the circulation is repeated, wherein the pressure control system (9) adjusts the flow rate of the liquid-phase mixture of sulfur dioxide and butadiene input into the jet pump (6) according to the pressure in an inner cavity of the reduced-pressure flash kettle (3) so as to adjust the flow rate of the gas-phase mixture of sulfur dioxide and butadiene pumped by the jet pump (6), further adjusting the pressure of the inner cavity of the reduced-pressure flash evaporation kettle (3) within a preset range;
meanwhile, the liquid-phase sulfolene is conveyed into a second recovery tank (8) from a liquid outlet of the reduced-pressure flash kettle (3) through a pipeline.
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