CN106366066A - Method of recycling SO2 through compression/condensation during production process of sulfolane - Google Patents
Method of recycling SO2 through compression/condensation during production process of sulfolane Download PDFInfo
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- CN106366066A CN106366066A CN201610712136.4A CN201610712136A CN106366066A CN 106366066 A CN106366066 A CN 106366066A CN 201610712136 A CN201610712136 A CN 201610712136A CN 106366066 A CN106366066 A CN 106366066A
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D333/00—Heterocyclic compounds containing five-membered rings having one sulfur atom as the only ring hetero atom
- C07D333/02—Heterocyclic compounds containing five-membered rings having one sulfur atom as the only ring hetero atom not condensed with other rings
- C07D333/46—Heterocyclic compounds containing five-membered rings having one sulfur atom as the only ring hetero atom not condensed with other rings substituted on the ring sulfur atom
- C07D333/48—Heterocyclic compounds containing five-membered rings having one sulfur atom as the only ring hetero atom not condensed with other rings substituted on the ring sulfur atom by oxygen atoms
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- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B17/00—Sulfur; Compounds thereof
- C01B17/48—Sulfur dioxide; Sulfurous acid
- C01B17/50—Preparation of sulfur dioxide
- C01B17/56—Separation; Purification
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
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- C07C7/005—Processes comprising at least two steps in series
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Abstract
The invention relates to a method of recycling SO2 through compression/condensation during a production process of sulfolane. During production of the sulfolane, the residual pressure of an intermediate product sulfolene reactor is reduced, so that SO2 and 1,3-butadiene, which are not reacted during the production process, are recycled in a step-by-step compression/condensation manner. The method has excellent desulfurization effect no matter on an intermediate production process or a continuous production process of the sulfolane. The method reduces emission concentration of the SO2 and reaches national environment protection requirement.
Description
Technical field
The present invention relates in sulfolane production process, using the method for compression/condensation process recovery sulfur dioxide.
Background technology
Sulfolane, as the extractant of Aromatics Extractive Project, has important application in petrochemical industry.At present, synthesize sulfolane
There are three kinds of methods, one kind is Tetramethylene sulfide oxidizing process, with potassium permanganate or hydrogen peroxide as oxidant, oxidation product benzene extracts
Afterwards, carry out fractional distillation, can get the sulfolane close to 100%.Second method is ethylene and sulfur dioxide synthetic method.The third side
Method is cyclobufene sultone hydrogenization method, that is, adopt liquid 1,3 butadiene and sulfur dioxide to react generation cyclobutane in the presence of polymerization inhibitor
Sulfone, then by cyclobufene sultone hydrogenated after, produce sulfolane.First two method in the Technological Economy due to, up to the present
Not yet realize real industrialization, cyclobufene sultone hydrogenization method is currently the only to realize industrialized method.
Four parts mostly can be divided into for cyclobufene sultone hydrogenization method technical process, (1) composite part, using liquid 1,3
Butadiene and sulfur dioxide react generation cyclobufene sultone in the presence of polymerization inhibitor；(2) disengagement section, removing synthetic reaction process is not
The sulfur dioxide of reaction and butadiene, and the concentration of sulfur dioxide in liquid phase is down to below 50ppm, it is beneficial to hydrogenation reaction
It is smoothed out；(3) it is hydrogenated with part, after desulfurization is qualified, add hydrogenation solvent to be configured to cyclobufene sultone solution, in the presence of a catalyst
Carry out hydrogenation reaction with hydrogen, generate sulfolane；(4) product purification part, at the coarse sulfolane product process obtaining after hydrogenation
Become finished product sulfolane after reason.
In cyclobufene sultone synthesis technique, because reaction reacts generation ring fourth for 1,3 butadiene and excessive sulfur dioxide
Alkene sulfone, excessive sulfur dioxide can lead to the catalyst poisoning of cyclobufene sultone hydrogenation, so the sulfur dioxide of excess is necessary
Removing.Disengagement section has obtained increasing concern at present, and chief reason derives from 2 points., reduce material consumption at first point.Cause
For sulfur dioxide inherently reactant, if so life can be reduced superfluous sulfur dioxide recovery it is possible to save material consumption
Produce cost.Domestic and international at present adopted desulfurization all refers to chemical absorbing, such as Shell technology, Philips's technique and Jinzhou
, all there is chemical reaction using sodium hydroxide solution and sulfur dioxide, reach removing titanium dioxide in the sulfolane production technology of petrochemical industry
The purpose of sulfur.Second point, is the requirement based on environmental conservation.Current sulfolane produces to adopt batch production process more, due to
Sulfur dioxide is excessive, and after the completion of reaction, sulfur dioxide surpluses are larger, after Dilution air purging, the discharge initial stage due to
Moment sulfur dioxide concentration too high it is difficult to all reach the standard of environmental emission in whole moment of discharge.With both at home and abroad to big
The attention in compression ring border, especially China propose increasingly stricter control standard recently to sulfur dioxide (SO2) emissions, lead to ring fourth
Sulfone manufacturer is faced with huge survival pressure.Therefore desulfurization is carried out using new process route it is ensured that enterprise's sulfur dioxide
Airborne release meets national standard, is very urgent task.In view of sulfur dioxide and 1,3 butadiene are all reactants, institute
With the new thinking of sulfur removal technology it should be can on the one hand to recycle unreacted material, thus reducing material consumption, pass through simultaneously
Reclaim unreacted sulfur dioxide and reduce the emission reduction of follow-up sulfur dioxide.The present invention is under such thinking, right
Desulfurization during sulfolane produces has carried out new technological design.
Content of the invention
Goal of the invention:
For sulfur dioxide emissioning concentration in sulfur removal technology in interval sulfolane production technology it cannot be guaranteed that whole period reaches
Target situation, the present invention redesigns to sulfur removal technology, by the compression/condensation process of novelty, one side maximum
Recovery reactant sulfur dioxide, reduce reaction material consumption, reduce the pressure of follow-up caustic wash desulfuration it is ensured that sulfur dioxide exists simultaneously
Concentration in discharge gas meets the discharge standard of current atmospheric environment；And the sweetening process to continuous sulfolane production process,
It is also proposed the process program of compression/condensation, to reach the dual purpose of environmental protection and reduces cost.
Technical scheme:
In a kind of sulfolane production process compression/condensation reclaim sulfur dioxide method it is characterised in that: sulfolane life
In product, using intermediate product cyclobufene sultone reactor overbottom pressure blood pressure lowering, sulfolane production process is reclaimed in compression condensation mode step by step
Unreacted sulfur dioxide and 1,3 butadiene.
Sulfolane produces and is divided into continuous production and two kinds of modes of production of Batch Process.
Overbottom pressure blood pressure lowering using sulfolane reactor refers to: the material going out cyclobufene sultone reactor bears more than 0.6mpa's
Pressure, carries out blood pressure lowering to this partial high pressure material, and when pressure drops to below 0.6mpa, liquid phase material starts to gasify.
Compression condensation refers to: carries out gradually pressure drop stage to the cyclobufene sultone reacting rear material more than 0.6mpa, presses from initial
When power is reduced to below 0.6mpa, cyclobufene sultone liquid mixture gasifies, when material is dropping to from the pressure that gasification occurs
During this pressure stage of 0.4mpa, vaporized gas is directly entered condenser, is condensed, and is mainly titanium dioxide in condensed fluid
Sulfur and 1,3 butadiene and a small amount of cyclobufene sultone, then material continue blood pressure lowering, when material pressure be less than below 0.4mpa
When, after vaporized gas will boost after compressor compresses, more condensed recovery sulfur dioxide and 1,3 butadiene.
Compression condensation refers to: carries out gradually pressure drop stage to the cyclobufene sultone reacting rear material more than 0.6mpa, presses from initial
When power is reduced to below 0.6mpa, cyclobufene sultone liquid mixture gasifies, when material is dropping to from the pressure that gasification occurs
During this pressure stage of 0.4mpa, vaporized gas is directly entered condenser, is condensed, and is mainly titanium dioxide in condensed fluid
Sulfur and 1,3 butadiene and a small amount of cyclobufene sultone, then material continue blood pressure lowering, when material pressure be less than below 0.4mpa
When, after vaporized gas will boost after compressor compresses, more condensed recovery sulfur dioxide and 1,3 butadiene.
Compression condensation refers to step by step, after the material having reacted in cyclobufene sultone reactor gasifies in pressure reduction, when
In more than 0.4mpa, gas is directly entered condenser to pressure, is condensed, and is mainly sulfur dioxide and 1,3 in condensed fluid
Butadiene and a small amount of cyclobufene sultone, and when material is depressurized to less than below 0.4mpa, the gas being flashed out will be through
After the compression of overcompression machine, then condense recovery sulfur dioxide and 1,3 butadiene.
The material having reacted in cyclobufene sultone reactor is between the temperature conditionss in pressure reduction are 90-110 DEG C.
Blood pressure lowering, compression condensation sulfur removal technology reclaim most liquid sulfur dioxide and 1, after 3 butadiene, then with follow-up
Alkali washing process combines, and controls tail gas sulphur dioxide concentration of emission.
Advantage and effect:
The present invention proposes a kind of method that in sulfolane production process, sulfur dioxide is reclaimed in compression/condensation, has following
Advantage:
The present invention, to the reaction mass in the sulfolane reactor that subject high pressure, carries out blood pressure lowering process, is down to liquid phase thing
Material starts the state of gasification, and when pressure is in more than 0.4mpa, the gas of gasification is directly entered condenser, by all cold
Solidifying, it is mainly sulfur dioxide and 1,3 butadiene and a small amount of cyclobufene sultone in condensed fluid, and work as pressure and be less than below 0.4mpa
When, gas then will be condensed through compressor compresses again, reclaims sulfur dioxide and 1,3 butadiene, the sulfur dioxide of recovery
Again it is utilized as reactant with 1,3 butadiene.The present invention passes through to produce sweetening process increase compression/condensation work in sulfolane
Skill, has reclaimed most sulfur dioxide, reduces the pressure of the follow-up desulfurization of device, compression/condensation desulfurization recovery process and after
Continuous alkali washing process combines, and sulfur dioxide in tail gas concentration of emission can be controlled to reach the emission request of National Environmental air.
At present, the corporate boss's Technology to be adopted being engaged in sulfolane production both at home and abroad has Britain's Philips's technique, shell
Board technique, SUMITOMO CHEMICAL technique, Chinese Jinzhou Petrochemical Company technique.These technical processs all include sweetening process.Philips's technique is adopted
It is Vacuum Desulfurization and alkali liquor desulfurization combines, Sumitomo technique adopts air stripping and alkali liquor desulfurization, the employing of Jinzhou Petrochemical Company
Be that warm air blowoff and alkali liquor desulfurization combine, the above technique is all not carried out the recycling to raw material sulfur dioxide,
And adopt substantial amounts of alkali liquor absorption sulfur dioxide, on the one hand increased cost, on the one hand cause the ring that sulfur dioxide (SO2) emissions cause
Border is polluted.Shell technology is only had to carry out cycling and reutilization to sulfur dioxide in existing process, this technique passes through absorption-rectification
Desorption process achieves the recovery of sulfur dioxide, but due to absorption and desorption cyclic process, feed liquid circulates in a large number, so power consumption is very
High.And the present invention relates to the compression condensation method mentioned, using original overbottom pressure, carry out compression condensation step by step, energy expenditure is down to
Minimum, pass through to reclaim most sulfur dioxide simultaneously, reduce the pressure of follow-up alkali liquor, both decreased the consumption of alkali liquor, and
Achieve the reduction of discharging of sulfur dioxide, there is save energy, save material consumption and more environmentally friendly triple advantages.
Brief description
Fig. 1 is mass fraction in gas phase mixture for the different pressures condition sulfur dioxide at 100 DEG C.
Show from Fig. 1, when the material going out cyclobufene sultone reactor is 100 DEG C in temperature, pressure is 0.1-0.5mpa scope
Interior, sulfur dioxide gas phase mass fraction with pressure variation tendency.According to Phase Diagram Analysis, only pressure is less than 0.6mpa
When, at existing temperature, liquid material could gasify, therefore it is 0.1- that the effective pressure of compression/condensation process adjusts interval
Between 0.5mpa.Fig. 1 shows the reduction with pressure, and in gas phase, content of sulfur dioxide increases, and this is conducive to reclaiming more two
Sulfur oxide.But be depressurized to which kind of degree is limited by condenser liquid-phase outlet temperature, when pressure low to certain degree after, to handle
Gas is condensed into liquid phase, needs condensation to lower temperature, is cooling water to be used as cooling medium, its condensation temperature is cooled down
The restriction of coolant-temperature gage is it is impossible to be less than 20 DEG C.So compression/condensation scheme that will be reasonable in design, the operating mode meeting actual production will
Ask.
Fig. 2 Batch Process sulfur dioxide removal/compression/condensation process flow chart.
1,3 butadiene and sulfur dioxide drain in devulcanizing pan 2 in reactor 1 after completion of the reaction, then start to system
Blood pressure lowering.When discharging pressure and being higher, the gaseous mixture of gasification is directly condensed by condenser 4, and condensed liquid enters into dioxy
Change sulfur and 1, in the measuring tank 5 of 3 butadiene, when discharging reduced pressure to below 0.4mpa, open diaphragm type compressor 6, pass through
The sulfur dioxide and 1 of compression high concentration, 3 butadiene mixed gas, enter condenser, after condensation, enter measuring tank 5.By dioxy
Change the liquidometer on sulfur recovery measuring tank 5, measure the recuperable sulfur dioxide of above-mentioned two steps and 1,3 butadiene.Solution
In remaining sulfur dioxide and 1,3 butadiene, after air compressor 7 compressed air stripping, air inlet storage tank 8, then warp
Cross air heater 9 to cool down mixed gas, then pass through the remaining sulfur dioxide of absorption tower alkali liquor absorption.
Compression condensation desulfurization flow chart in Fig. 3 continuous flow procedure.
1,3 butadiene and sulfur dioxide drain in devulcanizing pan 2 in reactor 1 after completion of the reaction, excess in devulcanizing pan
High Temperature High Pressure high-concentration sulfur dioxide gas first passes around condenser 4 and condenses, and subsequently into measuring tank 5, has gas-liquid two here
Phase, liquid phase is the sulfur dioxide and 1 reclaiming, 3 butadiene, after uncooled gas compresses through diaphragm type compressor 6 again, by condensation
Device, enters into measuring tank 5 after condensation, reclaim sulfur dioxide and 1,3 butadiene further.By sulfur dioxide recovery measuring tank 5
On liquidometer, measure the recuperable sulfur dioxide of above-mentioned two steps and 1,3 butadiene.Remaining sulfur dioxide in solution
With 1,3 butadiene, after air compressor 7 compressed air stripping, first pass around condenser, mixed gas are cooled to 20
DEG C, then pass through absorption tower alkali liquor absorption.
The equilibrium of ternary system in the range of table 1 pressure 0.1-0.5mpa.
Table 1 lists the equilibrium that pressure is respectively the ternary system under 0.1mpa, 0.3mpa and 0.5mpa.Left side
First is classified as different pressure, and second is classified as corresponding different temperatures under different pressures, after several row represent different temperatures and
Under pressure, sulfur dioxide/1,3 butadiene/cyclobufene sultone ternary system mass fraction in gas phase and liquid phase respectively.From table 1
Know, cyclobufene sultone content in the gas phase seldom, can be ignored substantially, so being mainly sulfur dioxide and 1,3 fourths two in gas phase
Alkene；With the reduction of pressure, sulfur dioxide mass fraction in the gas phase increases；At the same pressure, temperature is higher, titanium dioxide
Sulfur mass fraction in the gas phase is bigger.
Table 2 compresses step by step/condensation scheme condensation yield and condensation temperature.
The change of condensation yield and condensation temperature under step pressure reducing scheme given in table 2.The blood pressure lowering side being given in table
Case is, when devulcanizing pan temperature of charge out is 110 DEG C, to be first once depressurized to 0.5mpa, be then depressurized to 0.4mpa again, so
It is down to 0.3mpa afterwards again, be finally down to 0.2mpa.After pressure is down to 0.4mpa, condensed chilling temperature can be less than cooling
Water, therefore high pressure will be risen to gas phase and then condense, so after pressure is for 0.4mpa, gas will enter compressibility boosting, complete
Become condensation removal process.Secondary series in table 2 lists the amount of sulfur dioxide, 1,3 butadiene and cyclobufene sultone, and this tittle is different
It is because reducing step by step pressure, after blood pressure lowering, had liquid phase output to reclaim each time, so the raw material of ensuing blood pressure lowering system
Composition will do corresponding subtraction, deducts condensed material, and remaining material is depressurized generation gas phase again, then gas phase warp again
The liquid phase that compression/condensation is recycled.After every grade of blood pressure lowering, or adjoint compression, obtain condensed sulfur dioxide, 1,3 fourths two
Alkene and cyclobufene sultone are listed in table 2, through the blood pressure lowering of whole process, compress/condensation, the total each material finally obtaining
Yield list in table 2.Every grade of condensed liquidus temperature is also listed in table, from data, goes out condenser
Temperature is all higher than 20 DEG C.The response rate of the sulfur dioxide that can calculate from table 2 is 65.5%, and the response rate of 1,3 butadiene is
90.6%, overall recovery is 68.5%.
Description of reference numerals:
1st, reactor, 2, devulcanizing pan, 3, coil heat exchanger, 4, condenser, 5, measuring tank, 6, diaphragm type compressor, 7, air
Compressor, 8, air reservoir, 9, air heater.
Specific embodiment
For in sulfolane production technology, sulfur dioxide emissioning concentration after desulfurization is it cannot be guaranteed that all the period of time feelings up to standard
Condition, the sulfur removal technology that the present invention is directed in interval sulfolane and the production of continuous sulfolane is designed, by the pressure of novelty
Contracting/condensation process, on the one hand the maximum amount of can reclaim reactant sulfur dioxide, reduce the material consumption reacted, simultaneously because part
The recovery of sulfur dioxide reactant, reduces the pressure of follow-up caustic wash desulfuration, so that it is guaranteed that concentration in discharge gas for the sulfur dioxide
Meet the discharge standard of current atmospheric environment, reach the dual purpose of environmental protection and reduces cost.
The method that in sulfolane production process proposed by the present invention, sulfur dioxide is reclaimed in compression/condensation, is in sulfolane life
In product, using intermediate product cyclobufene sultone reactor overbottom pressure blood pressure lowering, sulfolane production process is reclaimed in compression condensation mode step by step
Unreacted sulfur dioxide and 1,3 butadiene.
Sulfolane produces and is divided into continuous production and two kinds of modes of production of Batch Process.
Overbottom pressure blood pressure lowering using sulfolane reactor refers to: the material going out cyclobufene sultone reactor bears more than 0.6mpa's
Pressure, carries out blood pressure lowering to this partial high pressure material, and when pressure drops to below 0.6mpa, liquid phase material starts to gasify.
Compression condensation refers to: carries out gradually pressure drop stage to the cyclobufene sultone reacting rear material more than 0.6mpa, presses from initial
When power is reduced to below 0.6mpa, cyclobufene sultone liquid mixture gasifies, when material is dropping to from the pressure that gasification occurs
During this pressure stage of 0.4mpa, vaporized gas is directly entered condenser, is condensed, and is mainly titanium dioxide in condensed fluid
Sulfur and 1,3 butadiene and a small amount of cyclobufene sultone, then material continue blood pressure lowering, when material pressure be less than below 0.4mpa
When, after vaporized gas will boost after compressor compresses, more condensed recovery sulfur dioxide and 1,3 butadiene.
Compression condensation refers to step by step, after the material having reacted in cyclobufene sultone reactor gasifies in pressure reduction, when
In more than 0.4mpa, gas is directly entered condenser to pressure, is condensed, and is mainly sulfur dioxide and 1,3 in condensed fluid
Butadiene and a small amount of cyclobufene sultone, and when material is depressurized to less than below 0.4mpa, the gas being flashed out will be through
After the compression of overcompression machine, then condense recovery sulfur dioxide and 1,3 butadiene.
The principle of compression condensation refers to that as needed, pressure change can be divided into during implementing compression condensation step by step
Multistage, the final value after first order blood pressure lowering is 0.4mpa, and in this stage, the gas phase of generation is directly entered condensing units below,
Then continue blood pressure lowering, blood pressure lowering below can have multiple blood pressure lowerings to select.Multiple blood pressure lowerings select to refer to: the first order, to liquid phase material,
0.4mpa is dropped to by the pressure of cyclobufene sultone reactor outlet, under this pressure, the gas after liquid-phase vaporization is directly entered cold
Condenser is condensed into liquid phase, realizes reclaiming.Blood pressure lowering is continued liquid phase material in the second level, and first pressing is 0.4mpa, and end of a period pressure can be
Value between 0.4mpa to 0.2mpa, delivers to compressor boosting again, then enters back into condenser cold to the gas phase generating after blood pressure lowering
Solidifying, the liquid phase being recycled.Thus only has two stages of compression condensation.Because from the beginning of the second level, the scope of final pressure is 0.4mpa
To between 0.2mpa, so according to practice in factory, any pressure value in this interval can be selected to do final pressure, so selection can
With multiformity.
If starting to continue blood pressure lowering to liquid phase material from 0.4mpa, final pressure can be the pressure between 0.4mpa to 0.2mpa
Power, under the pressure in this stage, may proceed to gasification is gas to material, then compresses boosting to this portion gas, and boosting to can
Pressure under making this portion gas all condense, realizes the purpose that compression condensation reclaims gas phase.
Three-level scheme can also be selected, material pressure is dropped to 0.3mpa as the second level from 0.4mpa, is down to 0.3mpa
The gas phase that process produces is sent to compressor and is compressed boosting, and then enters condenser condensation, the liquid phase being recycled.So
Next just have the third level, pressure is down to 0.2mpa by 0.3mpa, the gas phase generating after blood pressure lowering delivered to compressor boosting again,
Then condenser condensation, the liquid phase being recycled are entered back into.
The material having reacted in cyclobufene sultone reactor is between the temperature conditionss in pressure reduction are 90-110 DEG C.
Blood pressure lowering, compression condensation sulfur removal technology reclaim most liquid sulfur dioxide and 1, after 3 butadiene, then with follow-up
Alkali washing process combines, and controls tail gas sulphur dioxide concentration of emission.
During using Batch Process mode, the method reclaiming sulfur dioxide is as follows:
Using compression/condensation process step by step, 1,3 butadiene and sulfur dioxide drain into de- in reactor 1 after completion of the reaction
In sulfur kettle 2, in devulcanizing pan excessive High Temperature High Pressure high-concentration sulfur dioxide gas after blood pressure lowering, under a certain pressure, liquid phase
Can vaporize, be the sulfur dioxide and 1 of high-load in gas phase, 3 butadiene.When gas phase is discharged in elevated pressures, be directly
Enter condenser 4 to condense, reclaim sulfur dioxide and 1,3 butadiene.When discharging reduced pressure to below 0.4mpa, open barrier film
Compressor 6, using compression/condensation process, reclaims the sulfur dioxide under low-pressure vapor phase.By on sulfur dioxide recovery measuring tank 5
Liquidometer, measure the recuperable sulfur dioxide of above-mentioned two steps and 1,3 butadiene, account for unreacted residue sulfur dioxide
55-70% with 1,3 butadiene amounts.Remaining sulfur dioxide and 1 in solution, 3 butadiene, compress sky by air compressor 7
After air-blowing takes off, air inlet storage tank 8, then through air heater 9, mixed gas are cooled down, then pass through absorption tower alkali liquor absorption
Remaining sulfur dioxide.
During using the continuous mode of production, the method reclaiming sulfur dioxide is as follows:
For the material out from cyclobufene sultone devulcanizing pan, using the compression condensation desulfurization program of secondary recovery, one-level is straight
Connected condensation and reclaimed sulfur dioxide and 1,3 butadiene, two grades of employings were first compressed and condensed it is achieved that farthest reclaiming two again
Sulfur oxide and 1,3 butadiene.1,3 butadiene and sulfur dioxide drain in devulcanizing pan 2 after completion of the reaction in reactor 1, through fall
After pressure 0.2mpa, the High Temperature High Pressure high-concentration sulfur dioxide gas in devulcanizing pan first passes around condenser 4 and is cooled to 25 DEG C, returns
Receiving portions liquid phase sulfur dioxide and 1,3 butadiene enter into storage tank 5, and uncooled gas is compressed to through diaphragm type compressor 6
After 0.4mpa, then 25 DEG C of recovery sulfur dioxide and 1 further, 3 butadiene are cooled to by condenser condensation 4.Secondary recovery mistake
Cheng Lianxu stable state is carried out.By on sulfur dioxide recovery measuring tank 5 liquidometer, measure above-mentioned two steps recuperable two
Sulfur oxide and 1,3 butadiene, yield accounts for reacting total surplus sulfur dioxide and 1, the 55-70% of 3 butadiene amounts.Surplus in solution
Remaining sulfur dioxide and 1,3 butadiene, after air compressor 7 compressed air stripping, air inlet storage tank 8, then through sky
Mixed gas are cooled down by hot-air heater 9, then pass through the remaining sulfur dioxide of absorption tower alkali liquor absorption.
With reference to specific embodiment, the present invention is described further, but protection scope of the present invention is not implemented
The restriction of example.
Embodiment 1
For a batch production process, enter reactor material liquid and consist of, liquid 1,3 butadiene 1070kg, liquid two
Sulfur oxide 1400kg, together enters reactor, produces cyclobufene sultone again through hydrogenation, rectification obtains sulfolane product.Cyclobutane
After sulfone reaction completely, consist of from the kettle material that goes out of reactor, cyclobufene sultone 2290.411kg, reacting remaining sulfur dioxide is
158.064kg, 1,3 butadiene is 21.4kg, sulfur dioxide and 1, and 3 butadiene are dissolved in cyclobufene sultone liquid phase.Go out reactor
Material pressure be 1.0mpa, temperature be 110 DEG C.Kettle material is gone out to this composition, carries out step pressure reducing.Depressurization step: to liquid
Phase materials directly drop to 0.4mpa, and by condensing recovery section sulfur dioxide and 1,3 butadiene, then again to remaining liquid phase material
It is depressured to 0.2mpa, for the continuous gas producing, be compressed to after 0.4mpa through diaphragm type compressor, then again through condenser
Condensation, the sulfur dioxide and 1 reclaiming after obtaining compressed/condensation process, 3 butadiene.The sulfur dioxide being recycled is
104.597kg, 1,3 butadiene is 18.895kg, the response rate 66.17% of sulfur dioxide, and the response rate of 1,3 butadiene is
88.13%, yield accounts for and reacts total surplus sulfur dioxide and 1, and the 68.81% of 3 butadiene amounts.
Embodiment 2:
For a batch production process, enter reactor material liquid and consist of, liquid 1,3 butadiene 1070kg, liquid two
Sulfur oxide 1400kg, together enters reactor, produces cyclobufene sultone again through hydrogenation, rectification obtains sulfolane product.Cyclobutane
After sulfone reaction completely, consist of from the kettle material that goes out of reactor, cyclobufene sultone 2290.411kg, reacting remaining sulfur dioxide is
158.064kg, 1,3 butadiene is 21.4kg, sulfur dioxide and 1, and 3 butadiene are dissolved in cyclobufene sultone liquid phase.Go out reactor
Material pressure be 1.0mpa, temperature be 110 DEG C.Kettle material is gone out to this composition, carries out step pressure reducing, depressurization step: to liquid
Phase materials directly drop to 0.5mpa, and by condensing recovery section sulfur dioxide and 1,3 butadiene, then again to remaining liquid phase material
It is depressured to 0.4mpa, then by condensing recovery section sulfur dioxide and 1,3 butadiene, more remaining liquid phase material is depressured to is down to
0.2mpa, for the continuous gas producing, after diaphragm type compressor compressor compresses to 0.4mpa, then entered condenser again
Condensation, the sulfur dioxide and 1 reclaiming after obtaining compression/condensation process, 3 butadiene.The sulfur dioxide of the recovery obtaining is
103.5kg, 1,3 butadiene is 19.3kg, the response rate 65.5% of sulfur dioxide, and the response rate of 1,3 butadiene is 90.6%, returns
Receipts amount accounts for the 68.5% of reaction total surplus sulfur dioxide and 1,3 butadiene amounts.
Embodiment 3
For a batch production process, enter reactor material liquid and consist of, liquid 1,3 butadiene 1070kg, liquid two
Sulfur oxide 1400kg, together enters reactor, produces cyclobufene sultone again through hydrogenation, rectification obtains sulfolane product.Cyclobutane
After sulfone reaction completely, consist of from the kettle material that goes out of reactor, cyclobufene sultone 2290.411kg, reacting remaining sulfur dioxide is
158.064kg, 1,3 butadiene is 21.4kg, sulfur dioxide and 1, and 3 butadiene are dissolved in cyclobufene sultone liquid phase.Go out reactor
Material pressure be 1.0mpa, temperature be 90 DEG C.Kettle material is gone out to this composition, carries out step pressure reducing, depressurization step: to liquid phase
Material is directly depressurized to 0.4mpa, and by condensing recovery section sulfur dioxide and 1,3 butadiene, then again to remaining liquid phase material
It is depressured to 0.2mpa, for the continuous gas producing, be compressed to after 0.4mpa through diaphragm type compressor, then entered condenser again
Condensation, the sulfur dioxide and 1 reclaiming after obtaining compression/condensation process, 3 butadiene.The sulfur dioxide of the recovery obtaining is
82.414kg, 1,3 butadiene is 17.27kg, the response rate 52.14% of sulfur dioxide, and the response rate of 1,3 butadiene is
80.7%, yield accounts for and reacts total surplus sulfur dioxide and 1, and the 55.55% of 3 butadiene amounts.
Embodiment 4:
For a tandem reaction sequence, enter reactor material liquid and consist of, liquid 1,3 butadiene 1070kg/hr, liquid
Sulfur dioxide 1400kg/hr, together enters reactor, produces cyclobufene sultone again through hydrogenation, rectification obtains sulfolane product.Ring
After the reaction completely of butylene sulfone, consist of from the kettle material that goes out of reactor, cyclobufene sultone 2290.411kg/hr, react remaining two
Sulfur oxide is 158.064kg/hr, and 1,3 butadiene is 21.4kg/hr, sulfur dioxide and 1, and 3 butadiene are dissolved in cyclobufene sultone liquid
Xiang Zhong.The material pressure going out reactor is 1.0mpa, and temperature is 110 DEG C.Tower material is gone out to this, is directly depressurized to
0.2mpa, is then condensed to the gas phase of gasification by condenser again, controls outlet temperature to be 25 DEG C, then passes through one again
Play the measuring tank of flash distillation effect, liquid phase is recovered, solidifying gas phase is compressed to after 0.4mpa through diaphragm type compressor and condenses, reclaims
Two parts liquid-phase mixing together.The sulfur dioxide of the recovery obtaining is 103.5kg/hr, and 1,3 butadiene is 19.3kg/hr,
The response rate 67.63% of sulfur dioxide, the response rate of 1,3 butadiene is 85.02%, and yield accounts for reaction total surplus sulfur dioxide
With 1,3 butadiene amounts 69.7%.
Implement row 5
For a tandem reaction sequence, enter reactor material liquid and consist of, liquid 1,3 butadiene 1070kg/hr, liquid
Sulfur dioxide 1400kg/hr, together enters reactor, produces cyclobufene sultone again through hydrogenation, rectification obtains sulfolane product.Ring
After the reaction completely of butylene sulfone, consist of from the tower material that goes out of reactor, cyclobufene sultone 290.411kg/hr, react remaining dioxy
Change sulfur is 158.064kg/hr, and 1,3 butadiene is 21.4kg/hr, and they are partially dissolved in cyclobufene sultone liquid phase.Go out reactor
Material pressure be 1.0mpa, temperature be 90 DEG C.Kettle material is gone out to this composition, is directly depressurized to 0.2mpa, Ran Houzai
Condensed by condenser, control outlet temperature to be 25 DEG C, then again by a measuring tank playing flash distillation effect, liquid phase reclaims,
Solidifying gas phase is compressed to after 0.4mpa through diaphragm type compressor and condenses, and two parts liquid-phase mixing of recovery is together.Obtain
The sulfur dioxide reclaiming is 84.635kg/hr, and 1,3 butadiene is 16.684kg/hr, the response rate 53.54%, 1 of sulfur dioxide,
The response rate of 3 butadiene is 77.96%, and yield accounts for and reacts total surplus sulfur dioxide and 1, the 56.46% of 3 butadiene amounts.
Embodiment 6
For a batch production process, enter reactor material liquid and consist of, liquid 1,3 butadiene 1670kg, liquid two
Sulfur oxide 2200kg, together enters reactor, produces cyclobufene sultone again through hydrogenation, rectification obtains sulfolane product.Cyclobutane
After sulfone reaction completely, consist of from the kettle material that goes out of reactor, cyclobufene sultone 3581.1kg, reacting remaining sulfur dioxide is
260.39kg, 1,3 butadiene is 33.4kg, and they are dissolved in cyclobufene sultone liquid phase.The material pressure going out reactor is
1.0mpa, temperature is 110 DEG C.Kettle material is gone out to this composition, carries out step pressure reducing, step will be pressed: direct to liquid phase material
0.3mpa, by condensing recovery section sulfur dioxide and 1,3 butadiene, is then depressured to 0.2mpa to remaining liquid phase material again,
For the continuous gas producing, it is compressed to after 0.4mpa through diaphragm type compressor, then entered condenser condensation again, and pressed
The sulfur dioxide reclaiming after contracting/condensation process and 1,3 butadiene.The sulfur dioxide of the recovery obtaining is 175.89kg, 1,3 fourth two
Alkene is 29.75kg, the response rate 67.55% of sulfur dioxide, and the response rate of 1,3 butadiene is 88.96%, and it is total that yield accounts for reaction
Remaining sulfur dioxide and the 69.99% of 1,3 butadiene amounts.
Embodiment 7:
For a tandem reaction sequence, reaction raw materials liquid 1,3 butadiene 1670kg/hr, liquid sulfur dioxide
2200kg/hr, together enters reactor, produces cyclobufene sultone again through hydrogenation, rectification obtains sulfolane product.Cyclobufene sultone is anti-
After answering completely, consist of from the kettle material that goes out of reactor, cyclobufene sultone 3581.1kg/hr, reacting remaining sulfur dioxide is
260.39kg/hr, 1,3 butadiene is 33.4kg/hr, and they are dissolved in cyclobufene sultone liquid phase.Go out the material pressure of reactor
For 1.0mpa, temperature is 110 DEG C.Kettle material is gone out to this composition, is directly depressurized to 0.2mpa, then pass through condenser again
Condensation, controls outlet temperature to be 25, and then again by a measuring tank playing flash distillation effect, liquid phase reclaims, and gas phase is through barrier film
Compressor compresses condense to after 0.4mpa again, and two parts liquid-phase mixing of recovery is together.The sulfur dioxide of the recovery obtaining is
179.53kg/hr, 1,3 butadiene is 28.85kg/hr, the response rate 68.95% of sulfur dioxide, and the response rate of 1,3 butadiene is
86.37%, yield accounts for and reacts total surplus sulfur dioxide and 1, and the 70.92% of 3 butadiene amounts.
Embodiment 8:
For a batch production process, enter reactor material liquid and consist of, liquid 1,3 butadiene 1070kg, liquid two
Sulfur oxide 1400kg, together enters reactor, produces cyclobufene sultone again through hydrogenation, rectification obtains sulfolane product.Cyclobutane
After sulfone reaction completely, consist of from the kettle material that goes out of reactor, cyclobufene sultone 2290.411kg, reacting remaining sulfur dioxide is
158.064kg, 1,3 butadiene is 21.4kg, sulfur dioxide and 1, and 3 butadiene are dissolved in cyclobufene sultone liquid phase.Go out reactor
Material pressure be 1.0mpa, temperature be 100 DEG C.Kettle material is gone out to this composition, carries out step pressure reducing, depressurization step: to liquid
Phase materials are directly depressurized to 0.4mpa, and by condensing recovery section sulfur dioxide and 1,3 butadiene, then again to remaining liquid phase thing
Material is depressured to 0.2mpa, for the continuous gas producing, is compressed to after 0.4mpa through diaphragm type compressor, then entered condensation again
Device condenses, the sulfur dioxide and 1 reclaiming after obtaining compression/condensation process, 3 butadiene.The sulfur dioxide of the recovery obtaining is
94.702kg, 1,3 butadiene is 18.249kg, the response rate 59.91% of sulfur dioxide, and the response rate of 1,3 butadiene is
85.27%, yield accounts for and reacts total surplus sulfur dioxide and 1, and the 62.94% of 3 butadiene amounts.
Embodiment 9:
For a tandem reaction sequence, reaction raw materials liquid 1,3 butadiene 1670kg/hr, liquid sulfur dioxide
2200kg/hr, together enters reactor, produces cyclobufene sultone again through hydrogenation, rectification obtains sulfolane product.Cyclobufene sultone is anti-
After answering completely, consist of from the kettle material that goes out of reactor, cyclobufene sultone 3581.1kg/hr, reacting remaining sulfur dioxide is
260.39kg/hr, 1,3 butadiene is 33.4kg/hr, and they are dissolved in cyclobufene sultone liquid phase.Go out the material pressure of reactor
For 1.0mpa, temperature is 100 DEG C.Kettle material is gone out to this composition, is directly depressurized to 0.2mpa, then pass through condenser again
Condensation, controls outlet temperature to be 25, and then again by a measuring tank playing flash distillation effect, liquid phase reclaims, and gas phase is through barrier film
Compressor compresses condense to after 0.4mpa again, and two parts liquid-phase mixing of recovery is together.The sulfur dioxide of the recovery obtaining is
163.92kg/hr, 1,3 butadiene is 27.74kg/hr, the response rate 62.95% of sulfur dioxide, and the response rate of 1,3 butadiene is
83.05%, yield accounts for and reacts total surplus sulfur dioxide and 1, and the 65.23% of 3 butadiene amounts.
The equilibrium of ternary system under table 1 0.1～0.5mpa
Table 2 batch process procedures compress step by step/condensation scheme condensation yield and condensation temperature
Conclusion: the present invention provides more preferable sulfur removal technology and selects to the production of sulfolane, no matter for the production of interval
Technique or continuous sulfolane production technology, both provide good sulfur method so as to sweetening process is more perfect, reduce by two
Sulfur oxide emissions concentration, reaches national requirements for environmental protection.
Claims (8)
1. in a kind of sulfolane production process compression/condensation reclaim sulfur dioxide method it is characterised in that: sulfolane produce
In, using intermediate product cyclobufene sultone reactor overbottom pressure blood pressure lowering, sulfolane production process is reclaimed not in compression condensation mode step by step
The sulfur dioxide of reaction and 1,3 butadiene.
2. the method that in sulfolane production process, sulfur dioxide is reclaimed in compression/condensation according to claim 1, its feature exists
In: sulfolane produces and is divided into continuous production and two kinds of modes of production of Batch Process.
3. the method that in sulfolane production process according to claim 1 or claim 2, sulfur dioxide is reclaimed in compression/condensation, its feature
It is: the overbottom pressure blood pressure lowering using sulfolane reactor refers to: the material going out cyclobufene sultone reactor bears the pressure more than 0.6mpa
Power, carries out blood pressure lowering to this partial high pressure material, and when pressure drops to below 0.6mpa, liquid phase material starts to gasify.
4. the method that in sulfolane production process according to claim 1 or claim 2, sulfur dioxide is reclaimed in compression/condensation, its feature
It is: compression condensation refers to: gradually pressure drop stage is carried out to the cyclobufene sultone reacting rear material more than 0.6mpa, from initial pressure fall
Low to below 0.6mpa when, cyclobufene sultone liquid mixture gasifies, when material from occur gasification pressure dropping to
During this pressure stage of 0.4mpa, vaporized gas is directly entered condenser, is condensed, and is mainly titanium dioxide in condensed fluid
Sulfur and 1,3 butadiene and a small amount of cyclobufene sultone, then material continue blood pressure lowering, when material pressure be less than below 0.4mpa
When, after vaporized gas will boost after compressor compresses, more condensed recovery sulfur dioxide and 1,3 butadiene.
5. the method that in sulfolane production process, sulfur dioxide is reclaimed in compression/condensation according to claim 3, its feature exists
In: compression condensation refers to: carries out gradually pressure drop stage to the cyclobufene sultone reacting rear material more than 0.6mpa, reduces from initial pressure
During to below 0.6mpa, cyclobufene sultone liquid mixture gasifies, when material is dropping to 0.4mpa from the pressure that gasification occurs
During this pressure stage, vaporized gas is directly entered condenser, is condensed, and is mainly sulfur dioxide and 1 in condensed fluid,
3 butadiene and a small amount of cyclobufene sultone, then material continue blood pressure lowering, when material pressure be less than below 0.4mpa when, by gas
After the gas changed will boost after compressor compresses, more condensed recovery sulfur dioxide and 1,3 butadiene.
6. the method that in sulfolane production process according to claim 1 or claim 2, sulfur dioxide is reclaimed in compression/condensation, its feature
It is: compression condensation refers to step by step, after the material having reacted in cyclobufene sultone reactor gasifies in pressure reduction, work as pressure
In more than 0.4mpa, gas is directly entered condenser, is condensed, and is mainly sulfur dioxide and 1,3 fourths two in condensed fluid
Alkene and a small amount of cyclobufene sultone, and when material is depressurized to less than below 0.4mpa, the gas being flashed out will be through overvoltage
After the compression of contracting machine, then condense recovery sulfur dioxide and 1,3 butadiene.
7. the method that in sulfolane production process according to claim 1 or claim 2, sulfur dioxide is reclaimed in compression/condensation, its feature
It is: the material having reacted in cyclobufene sultone reactor is between the temperature conditionss in pressure reduction are 90-110 DEG C.
8. the method that in sulfolane production process according to claim 1 or claim 2, sulfur dioxide is reclaimed in compression/condensation, its feature
Be: blood pressure lowering, compression condensation sulfur removal technology reclaim most liquid sulfur dioxide and 1, after 3 butadiene, then with follow-up alkali
Wash technique to combine, control tail gas sulphur dioxide concentration of emission.
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| CN109232522A (en) * | 2018-09-30 | 2019-01-18 | 辽阳辽东精细化工有限公司 | Sulfolane continuous process system and technique |
| CN109833637A (en) * | 2017-11-27 | 2019-06-04 | 中国石油天然气股份有限公司 | Recyclable device |
| CN112239454A (en) * | 2019-07-17 | 2021-01-19 | 中国石油天然气股份有限公司 | System and method for producing sulfolane |
| CN112742179A (en) * | 2020-12-11 | 2021-05-04 | 安徽金禾实业股份有限公司 | Method for treating chlorination tail gas in sucralose production |
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| CN112239454A (en) * | 2019-07-17 | 2021-01-19 | 中国石油天然气股份有限公司 | System and method for producing sulfolane |
| CN112239454B (en) * | 2019-07-17 | 2022-08-05 | 中国石油天然气股份有限公司 | System and method for producing sulfolane |
| CN112742179A (en) * | 2020-12-11 | 2021-05-04 | 安徽金禾实业股份有限公司 | Method for treating chlorination tail gas in sucralose production |
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