CN105017210B - Regeneration method of sulfolane - Google Patents
Regeneration method of sulfolane Download PDFInfo
- Publication number
- CN105017210B CN105017210B CN201410165929.XA CN201410165929A CN105017210B CN 105017210 B CN105017210 B CN 105017210B CN 201410165929 A CN201410165929 A CN 201410165929A CN 105017210 B CN105017210 B CN 105017210B
- Authority
- CN
- China
- Prior art keywords
- solvent
- water
- sulfolane
- tower
- lean solvent
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Classifications
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Production Of Liquid Hydrocarbon Mixture For Refining Petroleum (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a sulfolane regeneration method, which comprises the steps of enabling a circulating solvent containing sulfolane to be in reverse contact with mixed aromatic hydrocarbon in an extraction tower, obtaining a rich solvent rich in the aromatic hydrocarbon at the bottom of the extraction tower in a gas-liquid extraction mode, sending the rich solvent into a recovery tower, obtaining a lean solvent without the mixed aromatic hydrocarbon at the bottom of the recovery tower in a distillation mode under a vacuum condition, using 95% of the total amount of the lean solvent for system circulation, sending 3% of the total amount of the lean solvent into the regeneration tower, mixing 2% of the total amount of the lean solvent with desalted water, sending the mixture into an oil-water separation tank for static separation, intermittently discharging an oil phase at the top of the oil-water separation tank into a heavy benzene product, automatically flowing a water phase at the bottom of the tank into a steam extraction water heat exchanger for heat exchange with the lean solvent, and sending the sulfolane in the circulating solvent back to the bottom of the recovery tower through a pump. The method solves the problem of deterioration of the sulfolane, ensures that the purity of the sulfolane in the poor solvent in the circulating process reaches more than 97 percent, and meets the process production requirement.
Description
Technical field
The present invention relates to triphen extract and separate field, specifically a kind of sulfolane regeneration technology.
Background technology
Crude benzol obtains qualified hydrogenated oil, hydrogenated oil feeding after hydrofinishing removes the impurity such as unsaturates, S and N
Extraction tower carries out the separation of non-aromatics and aromatic hydrocarbons, and extractant (sulfolane) dissolves each other with aromatic hydrocarbons in extraction tower, and with non-aromatic alkyl
Originally can not dissolve, the boiling temperature of sulfolane reaches more than 220 DEG C, after aromatic hydrocarbons is dissolved into sulfolane, improves the boiling point of itself
Temperature, then the method by distilling, propose non-aromatics from tower top, and sulfolane (rich solvent) feeding of the bottom of towe rich in aromatic hydrocarbons is reclaimed
Tower, using aromatic hydrocarbons and the boiling-point difference of sulfolane, realizes that aromatic hydrocarbons is separated with sulfolane, the sulfolane of bottom of towe by the method distilled
(lean solvent) sends extraction tower back to, and sulfolane is recycled, and in whole technological process, the purity of the sulfolane for recycling is true
The key factor of non-aromatics quality and aromatics quality is protected, generally requiring ensures its purity more than 97%, so in order to ensure ring
The purity of fourth sulfone, extension sulfolane feeding regenerator, sulfolane is removed by way of stripping distillation on pipeloop
In trace impurity.
The refined sector application of crude benzole hydrogenation extensively, can be real using this technique at home for above sulfolane gas-liquid extraction process
Existing triphen carries out extract and separate simultaneously, relative to two benzene extraction process, can lack a step benzene, toluene and dimethylbenzene and tails
Separate, be conducive to energy-conservation.But, due to constituting the non-aromatic of complicated, close with sulfolane boiling point C8 and the above in crude benzol raw material
Hydrocarbon content is high, constantly can be enriched with sulfolane, and sulfolane is regenerated by existing regenerator distillation technique, is only capable of
Except the solid impurity in lean solvent, it is impossible to lift the purity of lean solvent sulfolan, according to practical condition, sulfolane circulation
After 2 months, concentration drops to 92% by 99%, and non-aromatics concentration drops to 50%, ring fourth by 85% in non-aromatic hydrocarbon product
After sulfone is recycled 4 months, Production requirement cannot be met substantially.
The content of the invention
It is an object of the present invention to provide one kind it is easy to operate and economical and practical, and can effectively remove circulation solvent in
Impurity, it is ensured that the regeneration technology flow of circulation solvent sulfolan purity.
To achieve the above object, the technical solution adopted by the present invention is as follows：
A kind of renovation process of sulfolane, it comprises the following steps：By circulation solvent and BTX aromatics containing sulfolane
Inversely contacted in extraction tower, gas-liquid extract by way of, the tower top of extraction tower obtain purity be not less than 85% it is non-aromatic
Hydrocarbon, the bottom of towe of extraction tower obtains the rich solvent rich in aromatic hydrocarbons, and the rich solvent is sent into recovery tower, under vacuum, leads to
Distillation mode is crossed, the BTX aromatics that non-aromatic hydrocarbon content is not more than 3.5% are obtained in the tower top of recovery tower, the bottom of towe of recovery tower is obtained
The lean solvent of BTX aromatics is eliminated, system circulation is used for by the 95% of the lean solvent total amount, send extraction column overhead back to, it is poor molten
3% feeding regenerator of agent total amount carries out steam stripping regeneration, and the 2% of lean solvent total amount is mixed with demineralized water, feeding profit point
Static separation is carried out from groove, the oil phase interval at the top of the oil-water separation tank is entered in heavy benzol product, and bottom land water is mutually from inflow
In stripping water- to-water heat exchanger, the lean solvent with feeding tower top part is exchanged heat, and water is sent into regenerator and steamed as stripping after being gasified
Vapour, the sulfolane in circulation solvent is transmitted back to recovery tower bottom of towe by pump.
Preferably, when solvent content of impurities is low, it is also possible to stop regenerator, the 5% of lean solvent total amount
Directly mix with demineralized water, send into oil-water separation tank, oil phase interval in top is entered in heavy benzol product, and bottom aqueous phase passes through water stripping
Water to be directly entered recovery tower after heat exchanger exchanges heat with lean solvent, the sulfolane in circulation solvent is delivered to recovery by pump
Tower bottom of towe.
Preferably, the composition of the demineralized water is the pure water of deionization.
Preferably, the weight ratio of circulation solvent and BTX aromatics is 5：1~7：1, more preferably 6.5：1.
Preferably, the demineralized water and the volume ratio of lean solvent are 1：0.5~1：3, more preferably 1：2.
The present invention solves the problems, such as that sulfolane deteriorates, it is ensured that lean solvent reaches in cyclic process sulfolan purity
More than 97%, technique productions demand is met, while non-aromatic content has reached 95% or so, the first in toluene product in non-aromatics
Benzene content reaches more than 99.7%.
Brief description of the drawings
Fig. 1 is process chart of the invention.
Specific embodiment
The present invention is further elaborated with reference to embodiment and accompanying drawing.
A kind of renovation process of sulfolane, it comprises the following steps：By circulation solvent and BTX aromatics containing sulfolane
Inversely contacted in extraction tower, gas-liquid extract by way of, the tower top of extraction tower obtain purity be not less than 85% it is non-aromatic
Hydrocarbon, the bottom of towe of extraction tower obtains the rich solvent rich in aromatic hydrocarbons, and the rich solvent is sent into recovery tower, under vacuum, leads to
Distillation mode is crossed, the BTX aromatics that non-aromatic hydrocarbon content is not more than 3.5% are obtained in the tower top of recovery tower, the bottom of towe of recovery tower is obtained
The lean solvent of BTX aromatics is eliminated, system circulation is used for by the 95% of the lean solvent total amount, send extraction column overhead back to, it is poor molten
3% feeding regenerator of agent total amount carries out steam stripping regeneration, and the 2% of lean solvent total amount is mixed with demineralized water, feeding profit point
Static separation is carried out from groove, the oil phase interval at the top of the oil-water separation tank is entered in heavy benzol product, and bottom land water is mutually from inflow
In stripping water- to-water heat exchanger, the lean solvent with feeding tower top part is exchanged heat, and water is sent into regenerator and steamed as stripping after being gasified
Vapour, the sulfolane in circulation solvent is transmitted back to recovery tower bottom of towe by pump.
Preferably, when solvent content of impurities is low, it is also possible to stop regenerator, the 5% of lean solvent total amount
Directly mix with demineralized water, send into oil-water separation tank, oil phase interval in top is entered in heavy benzol product, and bottom aqueous phase passes through water stripping
Water to be directly entered recovery tower after heat exchanger exchanges heat with lean solvent, the sulfolane in circulation solvent is delivered to recovery by pump
Tower bottom of towe.
Preferably, the weight ratio of circulation solvent and BTX aromatics is 5：1~7：1, more preferably 6.5：1.
Preferably, the demineralized water and the volume ratio of lean solvent are 1：0.5~1：3, more preferably 1：2.
Embodiment 1
As shown in figure 1, qualified hydrogenated oil sends into extraction tower from bottom, circulation solvent enters from extraction tower top, tower top
The qualified non-aromatics of extraction, bottom of towe rich solvent feeding recovery tower, the qualified aromatic hydrocarbons of overhead extraction, bottom of towe lean solvent is by water stripping
After heat exchanger heat exchange, major part feeding extraction tower is mixed into oil-water separation tank, oil-water separation tank top with demineralized water on a small quantity
The oil of extraction is respectively fed in crude benzol or heavy benzol product according to the height of water content, and bottom liquid phases send stripping water- to-water heat exchanger back to, remove
Salt solution major part is gasified, and the demineralized water after gasification can be sent directly into recovery tower according to production needs, can also send into regenerator
Stripped vapor for regenerating sulfolane, the liquid phase of water stripping exchanger base enters in dashpot, and material passes through in dashpot
Conveying pumped back recovery tower bottom.When solvent content of impurities is low, it is also possible to stop regenerator, the 5% of lean solvent total amount
Directly mix with demineralized water, send into oil-water separation tank, oil phase interval in top is entered in heavy benzol product, and bottom aqueous phase passes through water stripping
Water to be directly entered recovery tower after heat exchanger exchanges heat with lean solvent, the sulfolane in circulation solvent is delivered to recovery by pump
Tower bottom of towe.Using the present invention, can solve the problems, such as to circulate solvent sulfolan deterioration well, it is ensured that in circulation solvent
Sulfolane purity reaches more than 97%, and the non-aromatics purity produced ensure that more than 85%, while pure benzene and toluene
Quality reaches industry-leading level.
In the technical program, recovery tower bottom of towe part lean solvent is mixed by regenerating pipeline with the demineralized water of system requirements,
In mixed feeding gun barrel, realize that C8 and the non-aromatics of the above are separated with sulfolane in gun barrel, point
The non-aromatics of C8 and the above after is entered in heavy benzol product, bottom liquid phases feeding stripping water- to-water heat exchanger, water to return to recovery
Tower or regenerator, unvaporized sulfolane feeding recovery tower bottom, process above flow is what prior art did not possessed.This technology side
Case has following advantage compared with original technology：1st, it is washings to need the demineralized water of injection using system, without increase
Wastewater flow rate；2nd, the mixed proportion of demineralized water and lean solvent is 1：2, this is the ratio that is most economical and ensureing regeneration effect found out
Example；3rd, it is 45min that demineralized water needs the separate time after mixing with lean solvent, and a water-oil separating is devised according to disengaging time
Tank, specially knockout drum charging aperture to bottom discharge outlet are decanting zone, and charging aperture to top oil discharge outlet is oily Disengagement zone, decanting zone
Volume with feed flux matched, the sedimentation time is about 2 times of disengaging time, and top oil Disengagement zone volume is about decanting zone
25%；4th, original water stripping/lean solvent heat exchanger is make use of, heat has both been reclaimed, recovery tower bottom of towe load energy is in turn ensured that
Enough bear the caused impact of sulfolane backflow after regeneration；5th, the function that original regenerator removes solid impurity is remained.
The present invention solves the problems, such as that sulfolane deteriorates, it is ensured that lean solvent reaches in cyclic process sulfolan purity
More than 97%, technique productions demand is met, while non-aromatic content has reached 95% or so, the first in toluene product in non-aromatics
Benzene content reaches more than 99.7%.
Finally be necessary explanation be：Above example is served only for making technical scheme further details of theory
Bright, it is impossible to be interpreted as limiting the scope of the invention, those skilled in the art's the above of the invention is made
Some nonessential modifications and adaptations belong to protection scope of the present invention.
Claims (5)
1. a kind of renovation process of sulfolane, it is characterised in that comprise the following steps：
A) the circulation solvent containing sulfolane is inversely contacted with BTX aromatics in extraction tower, by way of gas-liquid is extracted,
The non-aromatics that purity is not less than 85% is obtained in the tower top of extraction tower, the bottom of towe of extraction tower obtains the rich solvent rich in aromatic hydrocarbons；
B) rich solvent is sent into recovery tower, under vacuum, by the mode of distilling, obtains non-in the tower top of recovery tower
Arene content is not more than 3.5% BTX aromatics, and the bottom of towe of recovery tower obtains eliminating the lean solvent of BTX aromatics；
C) it is used for system circulation by the 94%~97% of the lean solvent gross weight, sends extraction column overhead, lean solvent gross weight back to
1%~3% feeding regenerator carry out steam stripping regeneration, the 3%~5% of lean solvent gross weight is mixed with demineralized water, send into
Oil-water separation tank carries out static separation, and the oil phase interval at the top of the oil-water separation tank is entered in heavy benzol product, bottom land water phase
From in flowing into water stripping heat exchanger, the lean solvent with tower top part is exchanged heat, and water sends into regenerator as stripping after being gasified
Steam, the sulfolane in circulation solvent is transmitted back to recovery tower bottom of towe by pump.
2. renovation process as claimed in claim 1, it is characterised in that when solvent content of impurities is low, stop regenerator,
The 3%~5% of the lean solvent gross weight is directly mixed with demineralized water, oil-water separation tank, the oil-water separation tank top is sent into
Portion's oil phase interval is entered in heavy benzol product, and bottom aqueous phase is water directly to enter after stripping water- to-water heat exchanger and lean solvent heat exchange
Enter recovery tower, the sulfolane in circulation solvent is delivered to recovery tower bottom of towe by pump.
3. renovation process as claimed in claim 1, it is characterised in that the composition of the demineralized water is the pure water of deionization.
4. renovation process as claimed in claim 1, it is characterised in that circulation solvent and BTX aromatics described in step a)
Weight ratio is 5：1~7：1.
5. renovation process as claimed in claim 1, it is characterised in that the demineralized water is 1 with the volume ratio of lean solvent:0.5
~1：3.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410165929.XA CN105017210B (en) | 2014-04-23 | 2014-04-23 | Regeneration method of sulfolane |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410165929.XA CN105017210B (en) | 2014-04-23 | 2014-04-23 | Regeneration method of sulfolane |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN105017210A CN105017210A (en) | 2015-11-04 |
| CN105017210B true CN105017210B (en) | 2017-06-06 |
Family
ID=54407560
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201410165929.XA Active CN105017210B (en) | 2014-04-23 | 2014-04-23 | Regeneration method of sulfolane |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN105017210B (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106632236A (en) * | 2016-09-30 | 2017-05-10 | 马鞍山钢铁股份有限公司 | Method for continuously removing heavy aromatics from solvent online |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5053137A (en) * | 1989-08-21 | 1991-10-01 | Indian Petrochemicals Corporation Limited | Process for the purification or regeneration of contaminated or spent process sulfolane |
| CN1230545A (en) * | 1998-03-26 | 1999-10-06 | 中国石油化工总公司 | Regeneration process of inferior sulfolane |
| CN102659758A (en) * | 2012-06-01 | 2012-09-12 | 唐山中润煤化工有限公司 | Regeneration and purification method of sulfolane in crude benzene hydrofining |
-
2014
- 2014-04-23 CN CN201410165929.XA patent/CN105017210B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5053137A (en) * | 1989-08-21 | 1991-10-01 | Indian Petrochemicals Corporation Limited | Process for the purification or regeneration of contaminated or spent process sulfolane |
| CN1230545A (en) * | 1998-03-26 | 1999-10-06 | 中国石油化工总公司 | Regeneration process of inferior sulfolane |
| CN102659758A (en) * | 2012-06-01 | 2012-09-12 | 唐山中润煤化工有限公司 | Regeneration and purification method of sulfolane in crude benzene hydrofining |
Also Published As
| Publication number | Publication date |
|---|---|
| CN105017210A (en) | 2015-11-04 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN106145426B (en) | Carbolic oil joint removing system and treatment process in a kind of coal chemical industrial waste water | |
| CN106588579B (en) | A method of extracting phenolic compound from carbolic oil | |
| CN103520945B (en) | The refining plant of crude benzole hydrogenation product and method | |
| CN105296135B (en) | A kind of regeneration method of waste lubricating oil | |
| CN103073383B (en) | Method and device for separating isohexane, n-hexane and benzene | |
| CN105016554B (en) | Semi-coke wastewater treatment process | |
| CN111954654A (en) | Method for separating aromatic hydrocarbon by extractive distillation | |
| CN105907452B (en) | A kind of combined technical method making waste lubricant oil regeneration by being heat-treated | |
| CN105316018A (en) | Pretreatment method for deep processing of coal tar | |
| CN104276926B (en) | By drippolene C8The discoloration method of the crude styrene that fraction extracting rectifying obtains | |
| CN102391064B (en) | Process for recovering and refining extracting agent in production procedure of hexanolactam | |
| CN110015949B (en) | Method for extracting phenolic substances from raw oil containing phenol | |
| CN101081993B (en) | Method for recovering aromatic hydrocarbons from hydrocarbons mixture with high content of aromatic hydrocarbons | |
| CN105017210B (en) | Regeneration method of sulfolane | |
| CN102731243A (en) | Method for separating benzene/toluene and methanol-alkylated reaction product | |
| CN108203595A (en) | A kind of method of aromatic hydrocarbons and alkane in extracting separation diesel oil distillate | |
| CN101955410B (en) | From containing the cinnamic method and system of cinnamic raw materials recovery | |
| CN104312620B (en) | One removes catalyst fines and the solvent-extracted combined method of slurry oil in slurry oil | |
| CN102432423B (en) | Method for refining crude dimethylbenzenes by extraction and rectification | |
| CN105419859A (en) | Reverse back extraction refining method for petroleum reduced pressure distillation distillate and application thereof | |
| CN205759806U (en) | A kind of solvent extraction refining plant of added solvent side reflux | |
| CN110003939A (en) | A kind of efficient carbolic oil dephenolization method | |
| CN105295989A (en) | Dehydrating and desalinizing method of high-temperature coal tar | |
| CN106398745B (en) | A kind of coarse raw materials oil treatment process | |
| CN105085152A (en) | Novel extraction process for aromatic hydrocarbons |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| CP03 | Change of name, title or address | ||
| CP03 | Change of name, title or address |
Address after: Weisan Road Chemical Office Building, Baoshan District, Shanghai, 2004 Patentee after: Baowu Carbon Material Technology Co., Ltd. Address before: No. 3501 Tongji Road, Baoshan District, Shanghai 201900 Patentee before: Chemical Co., Ltd. of Baoshan Iron and Steel Group, Shanghai |
|
| CP01 | Change in the name or title of a patent holder | ||
| CP01 | Change in the name or title of a patent holder |
Address after: Weisan Road Chemical Office Building, Baoshan District, Shanghai, 2004 Patentee after: Baowu Carbon Technology Co.,Ltd. Address before: Weisan Road Chemical Office Building, Baoshan District, Shanghai, 2004 Patentee before: BAOWU CARBON MATERIAL TECHNOLOGY Co.,Ltd. |