CN108147940A - 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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Publication number
CN108147940A
CN108147940A CN201611103560.5A CN201611103560A CN108147940A CN 108147940 A CN108147940 A CN 108147940A CN 201611103560 A CN201611103560 A CN 201611103560A CN 108147940 A CN108147940 A CN 108147940A
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China
Prior art keywords
butadiene
kettle
sulfur dioxide
pressure
vacuum flashing
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CN201611103560.5A
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CN108147940B (en
Inventor
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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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Analytical Chemistry (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Water Supply & Treatment (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)

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

The device and method of sulfur dioxide and butadiene in a kind of recycling cyclobufene sultone
Technical field
The present invention relates to the recycling field of sulfur dioxide in cyclobufene sultone and butadiene, more particularly to a kind of recycling cyclobutane The device and method of sulfur dioxide and butadiene in sulfone.
Background technology
Cyclobufene sultone, also known as butadiene sulfone, 3- dioxide thiophene alkene, chemical molecular formula C4H6O2S can pass through titanium dioxide Sulphur and butadiene synthesize under the action of polymerization inhibitor (hydroquinone).But the reaction of cyclobufene sultone is synthesized as reversible reaction, dioxy Cyclobufene sultone cannot be completely converted by changing sulphur and butadiene, therefore be synthesized in the exhaust gas after cyclobufene sultone or in liquid phase cyclobufene sultone Contain sulfur dioxide and butadiene.But sulfur dioxide and butadiene are pernicious gas, if after will directly synthesizing cyclobufene sultone Exhaust gas or the gas that is detached from liquid phase cyclobufene sultone be discharged into air, be easy to cause environmental pollution, and waste and use In the sulfur dioxide and butadiene of synthesis cyclobufene sultone.It is therefore desirable to pairings into the sulfur dioxide and butadiene after cyclobufene sultone It is recycled, to improve the utilization rate of sulfur dioxide and butadiene, reduces discharge.Therefore cyclobutane can be recycled by providing one kind The device and method of sulfur dioxide and butadiene in sulfone is very necessary.
The prior art provides the device of a kind of sulfur dioxide that can be recycled in cyclobufene sultone and butadiene, and can incite somebody to action Sulfur dioxide and butadiene after recycling are reused for synthesis cyclobufene sultone.The device includes the stirring sequentially connected by pipeline Kettle, polymerization inhibitor tank, compressor, condenser, recycling can, pressure retaining valve.Specifically recovery method is:Nitrogen is full of first in stirred tank Gas starts stirring, control pressure, and makes in the mixture input stirred tank of the cyclobufene sultone of generation, sulfur dioxide, butadiene, Due to pressure difference, sulfur dioxide, butadiene, nitrogen mixed gas enter polymerization inhibitor tank through pipeline and polymerization inhibitor comes into full contact with, so The mixed gas of initial gross separation pressurizes through compressor from the output of polymerization inhibitor tank and inputs condenser liquefaction afterwards, recently enters recycling storage Tank.At this point, then entrainment portions sulfur dioxide and butadiene gas are again introduced into stirred tank through pressure retaining valve in stirred tank nitrogen Cyclobufene sultone solution purged, repeat the above steps repeatedly, last nitrogen, sulfur dioxide and butadiene are net through lye desulfurization Air is discharged into after change.
Inventor has found that the prior art has at least the following problems:
The prior art provide recycle cyclobufene sultone in sulfur dioxide and butadiene efficiency it is low, sulfur dioxide and Butadiene is finally also needed through base extraction.
Invention content
Technical problem to be solved of the embodiment of the present invention is that providing one kind can recycle and utilize cyclobutane completely The device and method of sulfur dioxide and butadiene in sulfone.Specific technical solution is as follows:
In a first aspect, an embodiment of the present invention provides the device of sulfur dioxide and butadiene in a kind of recycling cyclobufene sultone, Described device includes condenser and the first recycling being connected by pipeline with the condensator outlet, and described device is also Including:Vacuum flashing kettle, import pass through pipeline and the outlet of cyclobufene sultone reactor;First pressure control valve, is arranged on On the pipeline of the vacuum flashing kettle entrance;Jet pump, air inlet are connected by the gas outlet of pipeline and the vacuum flashing kettle Logical, gas liquid outlet passes through pipeline and the inlet communication of the condenser;Circulating pump, import pass through pipeline and first recycling can Outlet, outlet is connected by pipeline with the import of the inlet of the jet pump and the cyclobufene sultone reactor simultaneously It is logical;Second recycling can is connected by pipeline with the liquid outlet of the vacuum flashing kettle;Control pressurer system, it is described for measuring The pressure of vacuum flashing kettle inner cavity, and liquid phase dioxy in the jet pump is inputted by the circulating pump to adjust according to the pressure Change the flow of the mixture of sulphur and butadiene, and then the gas that the adjustment injection pumping is driven to be exported by the vacuum flashing kettle The flow of the mixture of phase sulfur dioxide and butadiene, and then the pressure of the vacuum flashing kettle inner cavity is adjusted in preset range It is interior.
Specifically, preferably, described device further includes cyclone hydraulic separators, the cyclone hydraulic separators is arranged on the decompression Flash vaporization kettle is located in the inner cavity of entrance.
Specifically, preferably, described device further includes the demister being arranged below the cyclone hydraulic separators.
Specifically, preferably, described device further includes insulation jacket, 50-85 DEG C is connected in the insulation jacket and is followed Ring hot water, the insulation jacket are sleeved on the outer surface of the vacuum flashing kettle.
Specifically, preferably, the control pressurer system includes measuring the vacuum flashing kettle chamber pressure Second pressure control valve on pressure transmitter, the connecting pipeline being arranged between the jet pump and the circulating pump and The pressure logic controller being electrically connected with the pressure transmitter and the second pressure control valve;The pressure logic controller The pressure information of the pressure transmitter measurement is received, and the pressure information is handled, and according to handling result to institute It states second pressure control valve and sends pressure control instruction, according to the pressure control instruction, the second pressure control valve adjustment The flow of the mixture of liquid phase sulfur dioxide and butadiene in the jet pump is inputted by the circulating pump.
Specifically, preferably, described device further includes tank level control system, the tank level control system includes surveying Measure the liquid level gauge of the vacuum flashing kettle inside liquid level, the company being arranged between the vacuum flashing kettle and second recycling can Regulating valve on take over line and the liquid level logic controller being electrically connected with the liquid level gauge and the regulating valve;The liquid level Logic controller receives the liquid level information that the liquid level gauge measures, and the liquid level information is handled, and is tied according to processing Fruit sends Liquid level instruction to the regulating valve, is instructed according to the Liquid level, and the regulating valve adjustment is by the decompression The flow of the liquid phase cyclobufene sultone of flash vaporization kettle output.
Specifically, preferably, being provided with liquid level display on first recycling can, second recycling can.
Specifically, preferably, being all provided on pipeline at the lower part of the vacuum flashing kettle and the condensator outlet It is equipped with temperature indicator.
Specifically, preferably, the temperature indicator set on pipeline at the condensator outlet is thermal resistance.
Second aspect, the embodiment of the present invention additionally provide sulfur dioxide and butadiene in above device recycling cyclobufene sultone Method, the method includes:
By controlling first pressure control valve, the mixture for making cyclobufene sultone, sulfur dioxide, butadiene is defeated with predetermined amount of flow Enter in vacuum flashing kettle, handle to obtain liquid phase cyclobufene sultone and gas phase titanium dioxide by the vacuum flashing of the vacuum flashing kettle The mixture of sulphur and butadiene;The mixture of the gas phase sulfur dioxide and butadiene inputs jet pump by pipeline, through described The mixture of liquid phase sulfur dioxide and butadiene is condensed into, and sequentially input first in the gas liquid outlet input condenser of jet pump Recycling can, circulating pump;A part of liquid phase sulfur dioxide and the mixture of butadiene exported by the circulating pump passes through pipe In line input cyclobufene sultone reactor, the mixture of liquid phase sulfur dioxide and butadiene described in another part is in control pressurer system Control under inputted in the jet pump by pipeline, and with the mixture of gas phase sulfur dioxide and butadiene in the jet pump Then mixing condenses in the gas liquid outlet input condenser through the jet pump, repetitive cycling is in the process, described Control pressurer system adjusts the liquid phase titanium dioxide inputted in the jet pump according to the pressure of the vacuum flashing kettle inner cavity The flow of the mixture of sulphur and butadiene, to adjust the injection gas phase sulfur dioxide of pumping and butadiene mixture Flow, and then adjust the pressure of the vacuum flashing kettle inner cavity within a preset range;At the same time, the liquid phase cyclobufene sultone It is inputted in the second recycling can by the liquid outlet of the vacuum flashing kettle by pipeline.
The advantageous effect that technical solution provided in an embodiment of the present invention is brought is:
The device of sulfur dioxide and butadiene in recycling cyclobufene sultone provided in an embodiment of the present invention, by the way that decompression is set to dodge Kettle and first pressure control valve are steamed, convenient for the ring fourth in the pressure of control cyclobufene sultone reactor inner cavity and entrance vacuum flashing kettle Alkene sulfone, sulfur dioxide, butadiene mixture flow, after vacuum flashing kettle vacuum flashing processing, convenient for by liquid phase cyclobutane Sulfone is detached with the mixture of gas phase sulfur dioxide and butadiene, to input respectively in the second recycling can and jet pump.Pass through setting Jet pump, convenient for aspirating the mixing of gas phase sulfur dioxide and butadiene in vacuum flashing kettle under the control of control pressurer system To adjust the pressure of vacuum flashing kettle inner cavity, sulfur dioxide and butadiene are recycled, and in jet pump convenient for the later stage for gas The gas phase of sulfur dioxide and butadiene is mixed with liquid phase, and the cyclobufene sultone that can be avoided enter into condenser is sublimated, and blocking is set Standby and pipeline, to realize serialization recycling and production.By setting circulating pump, convenient for the mixing of liquid phase sulfur dioxide and butadiene The recycling of object and cycle.By setting control pressurer system, the pressure of vacuum flashing kettle inner cavity is conveniently adjusted, convenient for titanium dioxide Sulphur, butadiene, cyclobufene sultone gas-liquid separation make whole device realize automation recycling sulfur dioxide and butadiene.As it can be seen that this hair Bright embodiment, which provides device, can automate the continuous and complete recycling for realizing sulfur dioxide and butadiene, and for synthesizing cyclobutane Sulfone, avoids discharge sulfur dioxide and butadiene causes environmental pollution.
Description of the drawings
To describe the technical solutions in the embodiments of the present invention more clearly, make required in being described below to embodiment Attached drawing is briefly described, it should be apparent that, the accompanying drawings in the following description is only some embodiments of the present invention, for For those of ordinary skill in the art, without creative efforts, other are can also be obtained according to these attached drawings Attached drawing.
Fig. 1 is the structural representation of the device of sulfur dioxide and butadiene in recycling cyclobufene sultone provided in an embodiment of the present invention Figure.
Wherein, reference numeral represents respectively:
1 condenser,
2 first recycling cans,
3 vacuum flashing kettles,
4 cyclobufene sultone reactors,
5 first pressure control valves,
6 jet pumps,
7 circulating pumps,
8 second recycling cans,
9 control pressurer systems,
901 pressure transmitters,
902 second pressure control valves,
903 pressure logic controllers,
10 cyclone hydraulic separators,
11 demisters,
12 insulation jackets,
13 tank level control systems,
1301 liquid level gauges,
1302 regulating valves,
1303 liquid level logic controllers,
14 thermal resistances.
Specific embodiment
Unless otherwise defined, all technical terms used in the embodiment of the present invention are respectively provided with usual with those skilled in the art The identical meaning understood.To make the object, technical solutions and advantages of the present invention clearer, below in conjunction with attached drawing to this hair Bright embodiment is described in further detail.
In a first aspect, an embodiment of the present invention provides the device of sulfur dioxide and butadiene in a kind of recycling cyclobufene sultone, As shown in Figure 1, which includes condenser 1 and exports the first recycling can 2 being connected with condenser 1 by pipeline, should Device further includes:Vacuum flashing kettle 3, first pressure control valve 5, jet pump 6, circulating pump 7, the second recycling can 8, pressure control system System 9, wherein, the import of vacuum flashing kettle 3 passes through pipeline and the outlet of cyclobufene sultone reactor 4;First pressure control valve 5 It is arranged on the pipeline of 3 entrance of vacuum flashing kettle;The import of jet pump 6 is connected by the gas outlet of pipeline and vacuum flashing kettle 3 Logical, gas liquid outlet passes through pipeline and the inlet communication of condenser 1;The import of circulating pump 7 is gone out by pipeline and the first recycling can 2 Mouthful connection, outlet by pipeline simultaneously with the inlet of jet pump 6 and the inlet communication of cyclobufene sultone reactor 4;Second recycling Tank 8 is connected by pipeline with the liquid outlet of vacuum flashing kettle 3;Control pressurer system 9, for measuring 3 inner cavity of vacuum flashing kettle Pressure, and the stream of the mixture of liquid phase sulfur dioxide and butadiene in jet pump 6 is inputted by circulating pump 7 to adjust according to pressure Amount, so drive adjustment jet pump 6 aspirate the gas phase sulfur dioxide exported by vacuum flashing kettle 3 and butadiene mixture stream Amount, and then adjust the pressure of 3 inner cavity of vacuum flashing kettle within a preset range.
Just the work of the device of sulfur dioxide and butadiene is former in recycling cyclobufene sultone provided in an embodiment of the present invention below Reason, which is given, to be described:
Start control pressurer system 9 first so that the pressure of 3 inner cavity of vacuum flashing kettle within a preset range (pressure Preset range is vacuum or micro-positive pressure, to ensure being normally carried out for vacuum flashing), first pressure control valve 5 is then controlled, is made The cyclobufene sultone that is exported by cyclobufene sultone reactor 4, sulfur dioxide, butadiene mixture enter in vacuum flashing kettle 3, due to The boiling point of sulfur dioxide and butadiene is more much lower than cyclobufene sultone, and the vacuum flashing processing through vacuum flashing kettle 3 can obtain liquid Trim on the mixture of phase cyclobufene sultone and the mixture of gas phase sulfur dioxide and butadiene, gas phase sulfur dioxide and butadiene In the top of 3 inner cavity of vacuum flashing kettle, liquid phase cyclobufene sultone is located at the lower part of 3 inner cavity of vacuum flashing kettle due to gravity.So The mixture of gas phase sulfur dioxide and butadiene is sucked up to by the gas outlet of vacuum flashing kettle 3 in jet pump 6 by pipeline afterwards, It liquefies later into condenser 1, then the mixture of liquid phase sulfur dioxide and butadiene enters first by pipeline by condenser 1 Recycling can 2, further into circulating pump 7, a part of liquid phase sulfur dioxide and the mixture of butadiene exported by circulating pump 7 Into in cyclobufene sultone reactor 4, to synthesize cyclobufene sultone again, the mixture of a part of liquid phase sulfur dioxide and butadiene exists It under the action of control pressurer system 9, is again introduced into jet pump 6, and is mixed with the mixture of gas phase sulfur dioxide and butadiene, Then it is again introduced into condenser 1, repetitive cycling.In the process, the vacuum flashing that control pressurer system 9 is obtained according to measurement The pressure of 3 inner cavity of kettle, adjustment input liquid phase sulfur dioxide and the mixture of fourth two in jet pump 6 by pipeline by circulating pump 7 Flow, to adjust the flow that jet pump 6 aspirates the gas phase sulfur dioxide exported by vacuum flashing kettle 3 and butadiene mixture, into And adjust the pressure of 3 inner cavity of vacuum flashing kettle, be in preset range, with ensure input cyclobufene sultone, sulfur dioxide, Vacuum flashing can occur for the mixture of butadiene.
At the same time, liquid phase cyclobufene sultone is inputted by the liquid outlet of vacuum flashing kettle 3 in the second recycling can 8 by pipeline.
It should be noted that the preset range of the chamber pressure of vacuum flashing kettle 3 be vacuum or micro-positive pressure, less than to its The cyclobufene sultone of interior input, sulfur dioxide, butadiene mixture pressure, so as to be realized under conditions of nearly vacuum degree to mixed Close the vacuum flashing of object.The gas outlet of vacuum flashing kettle 3 and liquid outlet are located at the top and bottom of vacuum flashing kettle 3 respectively, with Convenient for the gas phase sulfur dioxide after vacuum flashing and the mixture of butadiene and liquid phase cyclobufene sultone respectively by vacuum flashing kettle 3 Top and lower part input downstream line in.The flow for inputting the mixture of liquid phase sulfur dioxide and butadiene in jet pump 6 is big When, by a large amount of gas phase sulfur dioxide of winding and the mixture of butadiene, therefore can be by adjusting the liquid phase two of entrance jet pump 6 The flow of the mixture of sulfur oxide and butadiene is adjusted into the gas phase sulfur dioxide of jet pump 6 and mixing for butadiene to drive The flow of object is closed, and then adjusts the pressure of 3 inner cavity of vacuum flashing kettle, the pressure is made to meet vacuum flashing condition, ensures cyclobutane Sulfone, sulfur dioxide, butadiene mixture through vacuum flashing processing be divided into liquid phase cyclobufene sultone, gas phase sulfur dioxide and butadiene Mixture.
Based on it is above-mentioned it is found that it is provided in an embodiment of the present invention recycling cyclobufene sultone in the device of sulfur dioxide and butadiene, By setting vacuum flashing kettle 3 and first pressure control valve 5, pressure and entrance convenient for 4 inner cavity of control cyclobufene sultone reactor The flow of cyclobufene sultone, sulfur dioxide, butadiene mixture in vacuum flashing kettle 3 is handled through 3 vacuum flashing of vacuum flashing kettle Afterwards, convenient for liquid phase cyclobufene sultone is detached with the mixture of gas phase sulfur dioxide and butadiene, to input the second recycling can 8 respectively And in jet pump 6.By setting jet pump 6, convenient for aspirating the gas in vacuum flashing kettle 3 under the control of control pressurer system 9 To adjust the pressure of 3 inner cavity of vacuum flashing kettle, sulfur dioxide is recycled convenient for the later stage for the mixed gas of phase sulfur dioxide and butadiene And butadiene, and sulfur dioxide in jet pump 6 and the gas phase of butadiene are mixed with liquid phase, can avoid enter into condenser 1 Interior cyclobufene sultone is sublimated, occluding device and pipeline, to realize serialization recycling and production.By setting circulating pump 7, just Recycling and cycle in liquid phase sulfur dioxide and the mixture of butadiene.By setting control pressurer system 9, it is conveniently adjusted decompression The pressure of 3 inner cavity of flash vaporization kettle convenient for sulfur dioxide and butadiene, cyclobufene sultone gas-liquid separation, makes whole device realize automation Recycle sulfur dioxide and butadiene.It can automate as it can be seen that the embodiment of the present invention provides device and realize sulfur dioxide and butadiene Continuous and recycling completely, and for synthesizing cyclobufene sultone, avoid discharge sulfur dioxide and butadiene causes environmental pollution.
Specifically, as shown in Figure 1, device provided in an embodiment of the present invention further includes cyclone hydraulic separators 10, rotary filter press Device 10 is arranged on the demister 11 that vacuum flashing kettle 3 is located in the inner cavity of entrance and is arranged on 10 lower section of cyclone hydraulic separators, Cyclone hydraulic separators 10 is convenient for efficiently making sulfur dioxide, butadiene and cyclobufene sultone gas-liquid separation with 11 mating reaction of demister. Wherein, cyclone hydraulic separators 10 can go out the gas phase sulfur dioxide in liquid phase cyclobufene sultone and separate butadiene, and demister 11 can Foam in liquid phase cyclobufene sultone is smashed completely, so that gas phase sulfur dioxide and butadiene divide completely from liquid phase cyclobufene sultone It separates out, with the liquid phase cyclobufene sultone of the recycling of high-purity.Wherein, cyclone hydraulic separators 10 can pass through commercially available acquisition, demister 11 Can be iron wire it is interlaced into mesh.
Specifically, device provided in an embodiment of the present invention further includes insulation jacket 12, and 50-85 DEG C is connected in insulation jacket 12 Circulating hot water, insulation jacket 12 is sleeved on the outer surface of vacuum flashing kettle 3, to ensure the temperature of material in vacuum flashing kettle 3 Degree is more than 50 DEG C, such as can be 50 DEG C, 55 DEG C, 60 DEG C, 65 DEG C, 70 DEG C, 75 DEG C, 80 DEG C, 85 DEG C etc., sets insulation jacket 12 The adiabatic effect of heat preservation can be played, convenient for cyclobufene sultone, sulfur dioxide and butadiene mixture in vacuum flashing kettle 3 efficiently Flash simultaneously gas-liquid separation.
Specifically, in embodiments of the present invention, as shown in Figure 1, control pressurer system 9 includes measuring vacuum flashing Second pressure control on the pressure transmitter 901 of 3 chamber pressure of kettle, the connecting pipeline being arranged between jet pump 6 and circulating pump 7 Valve 902 processed and the pressure logic controller 903 being electrically connected with pressure transmitter 901 and second pressure control valve 902;Pressure Logic controller 903 receives the pressure information that pressure transmitter 901 measures, and pressure information is handled, and according to processing As a result pressure control instruction is sent to second pressure control valve 902, according to pressure control instruction, second pressure control valve 902 is adjusted The whole flow that the mixture of liquid phase sulfur dioxide and butadiene in jet pump 6 is inputted by circulating pump 7.Specifically, work as pressure inverting The pressure that device 901 measures within a preset range when, the gas phase sulfur dioxide and butadiene of jet pump 6 are inputted by vacuum flashing kettle 3 Mixture and existing flow is kept i.e. by the mixture of liquid phase sulfur dioxide and butadiene that circulating pump 7 inputs jet pump 6 It can;When existing flow not within a preset range when, pressure logic controller 903 receive pressure transmitter 901 measure pressure letter Breath, and after processing, pressure control instruction is sent to second pressure control valve 902, according to pressure control instruction, second pressure control Valve 902 makes the flow of the liquid phase sulfur dioxide and butadiene entered in jet pump 6 become larger (small), and then inputs in jet pump 6 The flow of gas phase sulfur dioxide and butadiene becomes larger (small), so that the pressure of 3 inner cavity of vacuum flashing kettle becomes smaller (big), to be in pre- If in pressure limit.It should be noted that pressure logic controller 903 is computer, which is equipped with pressure logic control System processed.
Specifically, as shown in Figure 1, device provided in an embodiment of the present invention further includes tank level control system 13, liquid level control System 13 processed includes measuring the liquid level gauge 1301 of 3 inside liquid level of vacuum flashing kettle, being arranged on vacuum flashing kettle 3 and second time Regulating valve 1302 in connecting pipeline between closed cans 8 and the liquid level being electrically connected with liquid level gauge 1301 and regulating valve 1302 are patrolled Collect controller 1303;Liquid level logic controller 1303 receives the liquid level information that liquid level gauge 1301 measures, and liquid level information is carried out Processing, and Liquid level instruction is sent to regulating valve 1302 according to handling result, it is instructed according to Liquid level, regulating valve 1302 is adjusted The whole flow of liquid phase cyclobufene sultone exported by vacuum flashing kettle 3.Setting tank level control system 13, it can be achieved that automatically adjust by Vacuum flashing kettle 3 enters the flow of the liquid phase cyclobufene sultone of the second recycling can 8.Specifically, when the liquid level that liquid level gauge 1301 measures When within a preset range, the liquid level information of measurement is sent to liquid level logic controller 1303, liquid level logic controller 1303 is right Liquid level information is handled, and sends Liquid level instruction to regulating valve 1302 according to the result, is instructed, adjusted according to Liquid level The flow that section valve 1302 adjusts the liquid phase cyclobufene sultone for making the second recycling can of input 8 remains unchanged;It is measured when liquid level gauge 1301 Liquid level not within a preset range when, repeat the above process, the difference is that only regulating valve 1302 adjustment recycle input second The flow of the liquid phase cyclobufene sultone of tank 8 becomes larger (small), so that the liquid level of the liquid phase cyclobufene sultone of 3 inner cavity of vacuum flashing kettle is default In the range of.In addition, liquid level display is provided on the first recycling can 2, the second recycling can 8, in order to observe liquid in related device The liquid level of body, liquid level display can be frosting formula fluid level indicator, glass pipe type fluid level indicator, oily packet mode liquid level instruction Device, remote fluid level indicator etc., for intuitively observing the liquid level in relevant device.
Specifically, in embodiments of the present invention, on the pipeline in 1 exit of the lower part of vacuum flashing kettle 3 and condenser Temperature indicator is provided with, in order to observe the temperature of liquid cyclobufene sultone and the liquid phase exported by condenser 1 in vacuum flashing kettle 3 The temperature of the mixture of sulfur dioxide and butadiene in order to further adjust corresponding running parameter, makes vacuum flashing kettle 3 And condenser 1 is in optimum Working.Wherein, as shown in Figure 1, the temperature set on the pipeline in 1 exit of condenser is shown Show device for thermal resistance 14, thermal resistance 14 increases this characteristic to carry out temperature based on the resistance value of metallic conductor with the increase of temperature Degree measures, and the accuracy measured is high, performance is stablized.
Second aspect, the embodiment of the present invention is additionally provided recycles sulfur dioxide and fourth two in cyclobufene sultone using above device The method of alkene, this method include:
By controlling first pressure control valve 5, make the mixture of cyclobufene sultone, sulfur dioxide, butadiene with predetermined amount of flow It inputs in vacuum flashing kettle 3, handles to obtain liquid phase cyclobufene sultone and gas phase titanium dioxide by the vacuum flashing of vacuum flashing kettle 3 The mixture of sulphur and butadiene.
Wherein, the mixture of gas phase sulfur dioxide and butadiene inputs jet pump 6, the gas-liquid through jet pump 6 by pipeline The mixture of liquid phase sulfur dioxide and butadiene is condensed into, and sequentially input the first recycling can 2, follow in outlet input condenser 1 Ring pump 7.
A part of liquid phase sulfur dioxide and the mixture of butadiene exported by circulating pump 7 inputs cyclobufene sultone by pipeline In reactor 4, the mixture of another part liquid phase sulfur dioxide and butadiene passes through pipeline under the control of control pressurer system 9 It inputs in jet pump 6, and is mixed with the mixture of gas phase sulfur dioxide and butadiene in jet pump 6, the gas then through jet pump 6 It is condensed in liquid outlet input condenser 1, repetitive cycling, in the process, control pressurer system 9 is according to 3 inner cavity of vacuum flashing kettle Pressure, adjustment input jet pump 6 in liquid phase sulfur dioxide and butadiene mixture flow, taken out with adjusting jet pump 6 The gas phase sulfur dioxide of suction and the flow of butadiene mixture, and then the pressure of 3 inner cavity of vacuum flashing kettle is adjusted in preset range It is interior;
At the same time, liquid phase cyclobufene sultone is inputted by the liquid outlet of vacuum flashing kettle 3 in the second recycling can 8 by pipeline.
The process of sulfur dioxide and butadiene in above-mentioned recycling cyclobufene sultone is automation recycling, it can be achieved that sulfur dioxide It is recycled with the whole of butadiene, and available for synthesizing cyclobufene sultone again, avoids sulfur dioxide and butadiene discharge causes ring It pollutes in border.
Specifically, in the above-mentioned methods, the pressure of 3 inner cavity of vacuum flashing kettle is adjusted to default by control pressurer system 9 In the range of, which can be micro-positive pressure or vacuum, in order to be less than the cyclobufene sultone inputted in vacuum flashing kettle 3, two The pressure of the mixture of sulfur oxide and butadiene, to ensure mixture flash distillation for gas phase sulfur dioxide and the mixture of butadiene With liquid phase cyclobufene sultone.Further, by controlling first pressure control valve 5, make the mixture in input vacuum flashing kettle 3 with Predetermined amount of flow inputs, to ensure that it is good that the mixture enters the vacuum flashing effect after vacuum flashing kettle 3.Further, input should Mixture in vacuum flashing kettle 3 can separate under the action of cyclone hydraulic separators 10 and demister 11, and gas phase and liquid phase can Downstream line is inputted by the gaseous phase outlet on 3 top of vacuum flashing kettle and the liquid-phase outlet of lower part respectively respectively.
Wherein, after the mixture of gas phase sulfur dioxide and butadiene sequentially inputs jet pump 6, condenser 1 by pipeline, into For liquid phase sulfur dioxide and the mixture of butadiene, further, the mixture of liquid phase sulfur dioxide and butadiene sequentially inputs First recycling can 2, circulating pump 7, then the mixture of a part of liquid phase sulfur dioxide and butadiene be recycled for synthesis ring fourth The mixture of alkene sulfone, another part liquid phase sulfur dioxide and butadiene inputs injection under the action of second pressure control valve 902 It in pump 6, is mixed with the gas phase sulfur dioxide in jet pump 6 and the mixture of butadiene, liquid phase sulfur dioxide is used in jet pump 6 Mixture with butadiene, to be mixed with the micro liquid phase cyclobufene sultone into jet pump 6, prevents input from condensing as solvent Micro liquid phase cyclobufene sultone is sublimated during device 1, blocks condenser 1 and pipeline, and the Partial Liquid Phase sulfur dioxide and fourth two The mixture of alkene is inputted again in jet pump 6, meets the service condition of jet pump 6.
To the present invention be further described through by specific embodiment below.
In specific examples below, condition person is not specified in involved operation, according to normal condition or manufacturer It is recommended that condition carry out.
Embodiment 1
The device of sulfur dioxide and butadiene in a kind of recycling cyclobufene sultone is present embodiments provided, it as shown in Figure 1, should Device includes the vacuum flashing kettle 3, jet pump 6, condenser 1, the first recycling can 2, the circulating pump 7 that sequentially connect.Vacuum flashing kettle 3 Liquid outlet connected by pipeline with the second recycling can 8, and in the connecting pipeline between 3 and second recycling can 8 of vacuum flashing kettle It is additionally provided with regulating valve 1302.Circulating pump 7 is connected by pipeline with the inlet of cyclobufene sultone reactor 4 and jet pump 6 simultaneously, Second pressure control valve 902 is provided on pipeline between jet pump 6 and circulating pump 7.The inner cavity of vacuum flashing kettle 3 is provided with rotation Liquid/gas separator 10 is provided with demister 11 in the lower section of cyclone hydraulic separators 10.The device further includes control pressurer system 9, pressure The connection that control system 9 is included in pressure transmitter 901 on vacuum flashing kettle 3, is arranged between jet pump 6 and circulating pump 7 Second pressure control valve 902 on pipeline and the pressure being electrically connected with pressure transmitter 901 and second pressure control valve 902 Logic controller 903;Pressure logic controller 903 is handled according to the reading of pressure transmitter 901, then passes through the second pressure Force control valve 902 adjusts the flow that the mixture of liquid phase sulfur dioxide and butadiene in jet pump 6 is inputted by circulating pump 7, to adjust Whole jet pump 6 aspirates the flow of the gas phase sulfur dioxide exported by vacuum flashing kettle 3 and butadiene mixture, and then adjusts decompression The pressure of 3 inner cavity of flash vaporization kettle.
Embodiment 2
The device provided using embodiment 1, evaluates the vacuum flashing effect of vacuum flashing kettle 3.Wherein, simulation is mixed Object is closed to include:With flowmeter, cyclobufene sultone 1298kg/h, sulfur dioxide 235.23kg/h, butadiene 65.89kg/h, the mixing Object, which respectively enters, carries out vacuum flashing processing in the vacuum flashing kettle 3 of different vacuum degrees, wherein, the temperature of the mixture is 110 DEG C, pressure 3.6MPa after first pressure control valve 5 is decompressed to 1.0MPa, realizes that decompression is dodged into vacuum flashing kettle 3 is interior It steams, is then collected in liquid phase cyclobufene sultone in the second recycling can 8 that temperature is -20 DEG C, and pass through simulation and obtain liquid phase ring fourth The flow of sulfur dioxide and butadiene in alkene sulfone, relevant parameter are as shown in table 1 below:
Table 1
Pressure/bar in vacuum flashing kettle 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
The temperature of vacuum flashing kettle liquid phase/DEG C 69.1 69.8 70.8 71.7 72.4 73.1 73.8
As can be seen from Table 1, with the increase of pressure in vacuum flashing kettle 3, sulfur dioxide in liquid phase cyclobufene sultone and The flow of butadiene increases, therefore the pressure in vacuum flashing kettle 3 is lower, and vacuum flashing effect is better, sulfur dioxide and butadiene Detached with cyclobufene sultone more complete, sulfur dioxide and butadiene recovering effect are better.
Embodiment 3
The device provided using embodiment 1, evaluates the vacuum flashing effect of vacuum flashing kettle 3.The present embodiment with Embodiment 2 is identical, the difference is that only that simulation mixture includes:With flowmeter, cyclobufene sultone 1298kg/h, sulfur dioxide 235.23kg/h, butadiene 33kg/h, and pass through simulation and obtain in the liquid phase cyclobufene sultone after 3 vacuum flashing of vacuum flashing kettle The flow of sulfur dioxide and butadiene, relevant parameter are as shown in table 2 below:
Table 2
As can be seen from Table 2, with the increase of pressure in vacuum flashing kettle 3, sulfur dioxide in liquid phase cyclobufene sultone and The flow of butadiene increases, therefore the pressure in vacuum flashing kettle 3 is lower, and vacuum flashing effect is better, sulfur dioxide and butadiene Detached with cyclobufene sultone more complete, sulfur dioxide and butadiene recovering effect are better.
Embodiment 4
The device provided using embodiment 1, evaluates the vacuum flashing effect of vacuum flashing kettle 3.The present embodiment with Embodiment 2 is identical, the difference is that only that simulation mixture includes:With flowmeter, cyclobufene sultone 1298kg/h, sulfur dioxide 200kg/h, butadiene 33kg/h, and pass through simulation and obtain two in the liquid phase cyclobufene sultone after 3 vacuum flashing of vacuum flashing kettle The flow of sulfur oxide and butadiene, relevant parameter are as shown in table 3 below:
Table 3
As can be seen from Table 3, with the increase of pressure in vacuum flashing kettle 3, sulfur dioxide in liquid phase cyclobufene sultone and The flow of butadiene increases, therefore the pressure in vacuum flashing kettle 3 is lower, and vacuum flashing effect is better, sulfur dioxide and butadiene Detached with cyclobufene sultone more complete, sulfur dioxide and butadiene recovering effect are better.
It can be obtained by above-described embodiment 2-4, the pressure in vacuum flashing kettle 3 provided in an embodiment of the present invention is smaller, liquid The flash separation effect of sulfur dioxide and butadiene in phase cyclobufene sultone is better.
The foregoing is merely presently preferred embodiments of the present invention, the protection domain being not intended to limit the invention, all in this hair Within bright spirit and principle, any modification, equivalent replacement, improvement and so on should be included in protection scope of the present invention Within.

Claims (10)

1. the device of sulfur dioxide and butadiene in a kind of recycling cyclobufene sultone, described device include condenser (1) and pass through The first recycling can (2) that pipeline is connected with the condenser (1) outlet, which is characterized in that described device further includes:Decompression is dodged Kettle (3) is steamed, import passes through pipeline and the outlet of cyclobufene sultone reactor (4);
First pressure control valve (5) is arranged on the pipeline of vacuum flashing kettle (3) entrance;
Jet pump (6), air inlet are connected by pipeline with the gas outlet of the vacuum flashing kettle (3), and gas liquid outlet passes through pipeline With the inlet communication of the condenser (1);
Circulating pump (7), import by the outlet of pipeline and first recycling can (2), outlet by pipeline simultaneously with institute State the inlet of jet pump (6) and the inlet communication of the cyclobufene sultone reactor (4);
Second recycling can (8) is connected by pipeline with the liquid outlet of the vacuum flashing kettle (3);
Control pressurer system (9) for measuring the pressure of vacuum flashing kettle (3) inner cavity, and is adjusted according to the pressure The flow of the mixture of the interior liquid phase sulfur dioxide of the jet pump (6) and butadiene is inputted by the circulating pump (7), and then is driven Adjust the mixture of gas phase sulfur dioxide that the jet pump (6) suction exported by the vacuum flashing kettle (3) and butadiene Flow, and then adjust the pressure of vacuum flashing kettle (3) inner cavity within a preset range.
2. the apparatus according to claim 1, which is characterized in that described device further includes cyclone hydraulic separators (10), the rotation Liquid/gas separator (10) is arranged on the vacuum flashing kettle (3) in the inner cavity of entrance.
3. the apparatus of claim 2, which is characterized in that described device, which further includes, is arranged on the cyclone hydraulic separators (10) demister (11) below.
4. the apparatus according to claim 1, which is characterized in that described device further includes insulation jacket (12), the heat preservation 50-85 DEG C of circulating hot water is connected in chuck (12), the insulation jacket (12) is sleeved on the appearance of the vacuum flashing kettle (3) On face.
5. the apparatus according to claim 1, which is characterized in that the control pressurer system (9) is described including being used to measure The pressure transmitter (901) of vacuum flashing kettle (3) chamber pressure is arranged between the jet pump (6) and the circulating pump (7) Connecting pipeline on second pressure control valve (902) and controlled with the pressure transmitter (901) and the second pressure The pressure logic controller (903) of valve (902) electrical connection;
The pressure logic controller (903) receives the pressure information that the pressure transmitter (901) measures, and to the pressure Information is handled, and sends pressure control instruction to the second pressure control valve (902) according to handling result, according to described Pressure control instruction, second pressure control valve (902) adjustment input the interior liquid of the jet pump (6) by the circulating pump (7) The flow of the mixture of phase sulfur dioxide and butadiene.
6. the apparatus according to claim 1, which is characterized in that described device further includes tank level control system (13), described Tank level control system (13) is including being used to measure the liquid level gauge (1301) of vacuum flashing kettle (3) inside liquid level, being arranged on institute State regulating valve (1302) in the connecting pipeline between vacuum flashing kettle (3) and second recycling can (8) and with the liquid Position meter (1301) and the liquid level logic controller (1303) of the regulating valve (1302) electrical connection;
The liquid level logic controller (1303) receives the liquid level information that the liquid level gauge (1301) measures, and the liquid level is believed Breath is handled, and sends Liquid level instruction to the regulating valve (1302) according to handling result, according to the Liquid level Instruction, the flow of liquid phase cyclobufene sultone that regulating valve (1302) adjustment is exported by the vacuum flashing kettle (3).
7. the apparatus according to claim 1, which is characterized in that first recycling can (2), second recycling can (8) On be provided with liquid level display.
8. the apparatus according to claim 1, which is characterized in that the lower part of the vacuum flashing kettle (3) and the condensation Temperature indicator is both provided on the pipeline in device (1) exit.
9. device according to claim 8, which is characterized in that the institute set on the pipeline in condenser (1) exit Temperature indicator is stated as thermal resistance (14).
10. using the method for sulfur dioxide and butadiene in claim 1-9 any one of them device recycling cyclobufene sultone, It is characterized in that, the method includes:
By controlling first pressure control valve (5), the mixture for making cyclobufene sultone, sulfur dioxide, butadiene is defeated with predetermined amount of flow Enter in vacuum flashing kettle (3), handle to obtain liquid phase cyclobufene sultone and gas phase by the vacuum flashing of the vacuum flashing kettle (3) The mixture of sulfur dioxide and butadiene;
The mixture of the gas phase sulfur dioxide and butadiene inputs jet pump (6), the gas through the jet pump (6) by pipeline The mixture of liquid phase sulfur dioxide and butadiene is condensed into, and sequentially input the first recycling can in liquid outlet input condenser (1) (2), circulating pump (7);
Ring is inputted by pipeline by a part of liquid phase sulfur dioxide of the circulating pump (7) output and the mixture of butadiene In butylene sulfone reactor (4), the mixture of liquid phase sulfur dioxide and butadiene described in another part is in control pressurer system (9) Control is lower to be inputted by pipeline in the jet pump (6), and is mixed with gas phase sulfur dioxide in the jet pump (6) and butadiene Object mixing is closed, then the gas liquid outlet through the jet pump (6) is inputted in the condenser (1) and condensed, repetitive cycling, herein mistake Cheng Zhong, the control pressurer system (9) is according to the pressure of vacuum flashing kettle (3) inner cavity, the adjustment input jet pump (6) The interior liquid phase sulfur dioxide and the flow of the mixture of butadiene, to adjust the gas phase of the jet pump (6) suction The flow of sulfur dioxide and butadiene mixture, and then adjust the pressure of vacuum flashing kettle (3) inner cavity within a preset range;
At the same time, the liquid phase cyclobufene sultone is recycled by pipeline by the liquid outlet input second of the vacuum flashing kettle (3) In tank (8).
CN201611103560.5A 2016-12-05 2016-12-05 Device and method for recovering sulfur dioxide and butadiene in sulfolene Active CN108147940B (en)

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