CN102686294A - Process and apparatus for online rejuvenation of contaminated sulfolane solvent - Google Patents
Process and apparatus for online rejuvenation of contaminated sulfolane solvent Download PDFInfo
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- CN102686294A CN102686294A CN2009801618117A CN200980161811A CN102686294A CN 102686294 A CN102686294 A CN 102686294A CN 2009801618117 A CN2009801618117 A CN 2009801618117A CN 200980161811 A CN200980161811 A CN 200980161811A CN 102686294 A CN102686294 A CN 102686294A
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- Prior art keywords
- regenerator
- sulfolane
- contaminated
- solvent
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- HXJUTPCZVOIRIF-UHFFFAOYSA-N sulfolane Chemical class O=S1(=O)CCCC1 HXJUTPCZVOIRIF-UHFFFAOYSA-N 0.000 title claims abstract description 94
- 239000002904 solvent Substances 0.000 title claims abstract description 43
- 238000000034 method Methods 0.000 title claims abstract description 27
- 230000008569 process Effects 0.000 title abstract description 7
- 230000003716 rejuvenation Effects 0.000 title abstract 2
- 229910001220 stainless steel Inorganic materials 0.000 claims abstract description 24
- 239000010935 stainless steel Substances 0.000 claims abstract description 24
- 230000008929 regeneration Effects 0.000 claims description 19
- 238000011069 regeneration method Methods 0.000 claims description 19
- 239000012530 fluid Substances 0.000 claims description 12
- 239000003344 environmental pollutant Substances 0.000 claims description 6
- 231100000719 pollutant Toxicity 0.000 claims description 6
- 238000012545 processing Methods 0.000 claims description 6
- 238000005260 corrosion Methods 0.000 abstract description 56
- 230000007797 corrosion Effects 0.000 abstract description 56
- 238000000605 extraction Methods 0.000 abstract description 12
- 238000012423 maintenance Methods 0.000 abstract description 6
- 239000000356 contaminant Substances 0.000 abstract description 4
- 230000005291 magnetic effect Effects 0.000 abstract description 4
- 238000010276 construction Methods 0.000 abstract 1
- 239000000047 product Substances 0.000 description 50
- 150000004945 aromatic hydrocarbons Chemical class 0.000 description 17
- 239000002253 acid Substances 0.000 description 13
- 238000004140 cleaning Methods 0.000 description 11
- 238000009825 accumulation Methods 0.000 description 10
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 9
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 9
- 230000001172 regenerating effect Effects 0.000 description 7
- 239000000284 extract Substances 0.000 description 6
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 5
- 239000003463 adsorbent Substances 0.000 description 5
- 238000011084 recovery Methods 0.000 description 5
- 238000012360 testing method Methods 0.000 description 5
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 4
- 238000004026 adhesive bonding Methods 0.000 description 4
- 150000001768 cations Chemical class 0.000 description 4
- 239000002245 particle Substances 0.000 description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 150000001412 amines Chemical class 0.000 description 3
- 230000008859 change Effects 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 229910052742 iron Inorganic materials 0.000 description 3
- 239000011347 resin Substances 0.000 description 3
- 229920005989 resin Polymers 0.000 description 3
- 238000010998 test method Methods 0.000 description 3
- -1 tetramethyl sulfone Chemical class 0.000 description 3
- 239000002699 waste material Substances 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- LSNNMFCWUKXFEE-UHFFFAOYSA-M Bisulfite Chemical compound OS([O-])=O LSNNMFCWUKXFEE-UHFFFAOYSA-M 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 150000001450 anions Chemical class 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 238000005844 autocatalytic reaction Methods 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- BTANRVKWQNVYAZ-UHFFFAOYSA-N butan-2-ol Chemical compound CCC(C)O BTANRVKWQNVYAZ-UHFFFAOYSA-N 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 239000000460 chlorine Substances 0.000 description 2
- 229910052801 chlorine Inorganic materials 0.000 description 2
- 238000006731 degradation reaction Methods 0.000 description 2
- 238000013461 design Methods 0.000 description 2
- 238000005194 fractionation Methods 0.000 description 2
- 230000008676 import Effects 0.000 description 2
- 238000009434 installation Methods 0.000 description 2
- 238000005342 ion exchange Methods 0.000 description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 230000003472 neutralizing effect Effects 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 230000005298 paramagnetic effect Effects 0.000 description 2
- 230000005408 paramagnetism Effects 0.000 description 2
- 238000000746 purification Methods 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 238000001179 sorption measurement Methods 0.000 description 2
- 238000012546 transfer Methods 0.000 description 2
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- 239000005864 Sulphur Substances 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 125000001931 aliphatic group Chemical group 0.000 description 1
- 150000001336 alkenes Chemical class 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 230000000903 blocking effect Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 150000001732 carboxylic acid derivatives Chemical class 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 239000003518 caustics Substances 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000004927 clay Substances 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000001186 cumulative effect Effects 0.000 description 1
- 125000004122 cyclic group Chemical group 0.000 description 1
- 230000001351 cycling effect Effects 0.000 description 1
- 150000001924 cycloalkanes Chemical class 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 150000001993 dienes Chemical class 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 230000003628 erosive effect Effects 0.000 description 1
- 238000005530 etching Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000003345 natural gas Substances 0.000 description 1
- 239000012188 paraffin wax Substances 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 description 1
- 238000010926 purge Methods 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 239000004576 sand Substances 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 239000013049 sediment Substances 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 125000000383 tetramethylene group Chemical group [H]C([H])([*:1])C([H])([H])C([H])([H])C([H])([H])[*:2] 0.000 description 1
- 238000005292 vacuum distillation Methods 0.000 description 1
- 238000009834 vaporization Methods 0.000 description 1
- 230000008016 vaporization Effects 0.000 description 1
- 239000008096 xylene Substances 0.000 description 1
- 150000003738 xylenes Chemical class 0.000 description 1
Images
Classifications
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
- C10G21/00—Refining of hydrocarbon oils, in the absence of hydrogen, by extraction with selective solvents
- C10G21/28—Recovery of used solvent
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D35/00—Filtering devices having features not specifically covered by groups B01D24/00 - B01D33/00, or for applications not specifically covered by groups B01D24/00 - B01D33/00; Auxiliary devices for filtration; Filter housing constructions
- B01D35/06—Filters making use of electricity or magnetism
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D37/00—Processes of filtration
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B03—SEPARATION OF SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS; MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
- B03C—MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
- B03C1/00—Magnetic separation
- B03C1/02—Magnetic separation acting directly on the substance being separated
- B03C1/025—High gradient magnetic separators
- B03C1/031—Component parts; Auxiliary operations
- B03C1/033—Component parts; Auxiliary operations characterised by the magnetic circuit
- B03C1/0332—Component parts; Auxiliary operations characterised by the magnetic circuit using permanent magnets
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B03—SEPARATION OF SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS; MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
- B03C—MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
- B03C1/00—Magnetic separation
- B03C1/02—Magnetic separation acting directly on the substance being separated
- B03C1/28—Magnetic plugs and dipsticks
- B03C1/284—Magnetic plugs and dipsticks with associated cleaning means, e.g. retractable non-magnetic sleeve
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B03—SEPARATION OF SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS; MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
- B03C—MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
- B03C1/00—Magnetic separation
- B03C1/02—Magnetic separation acting directly on the substance being separated
- B03C1/28—Magnetic plugs and dipsticks
- B03C1/286—Magnetic plugs and dipsticks disposed at the inner circumference of a recipient, e.g. magnetic drain bolt
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
- C10G21/00—Refining of hydrocarbon oils, in the absence of hydrogen, by extraction with selective solvents
- C10G21/06—Refining of hydrocarbon oils, in the absence of hydrogen, by extraction with selective solvents characterised by the solvent used
- C10G21/12—Organic compounds only
- C10G21/22—Compounds containing sulfur, selenium, or tellurium
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B03—SEPARATION OF SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS; MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
- B03C—MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
- B03C2201/00—Details of magnetic or electrostatic separation
- B03C2201/18—Magnetic separation whereby the particles are suspended in a liquid
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B03—SEPARATION OF SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS; MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
- B03C—MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
- B03C2201/00—Details of magnetic or electrostatic separation
- B03C2201/20—Magnetic separation whereby the particles to be separated are in solid form
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B03—SEPARATION OF SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS; MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
- B03C—MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
- B03C2201/00—Details of magnetic or electrostatic separation
- B03C2201/28—Parts being easily removable for cleaning purposes
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
- C10G2300/00—Aspects relating to hydrocarbon processing covered by groups C10G1/00 - C10G99/00
- C10G2300/40—Characteristics of the process deviating from typical ways of processing
- C10G2300/44—Solvents
Abstract
A continuous online process for rejuvenating whole stream of contaminated lean sulfolane in an extraction system is provided. In particular, a rejuvenator is installed in the solvent circulation loop to remove the contaminants continuously to keep the solvent clean, effective and less corrosive. Specifically, the rejuvenator comprises a high pressure vessel with a removable cover and a round rack with vertical stainless steel tubes fitted in the high pressure vessel. A magnetic bar is placed in each stainless steel tube. A screen cylinder is installed inside the ring of stainless steel tubes. As the contaminated sulfolane is passed through the rejuvenator, the rejuvenator picks up its contaminants. The rejuvenator can be dissembled to remove the contaminants periodically. The rejuvenator is characterized by simple in construction, reliable in operation, and low in operation and maintenance costs. With this rejuvenator, the extraction system can be operated at high efficiency and high capacity without the dreaded corrosion.
Description
Technical field
The present invention relates to a kind of method that is used for the contaminated sulfolane solvent of online regeneration aromatic hydrocarbon extracting system, be used for constantly solvent being maintained the quality level of expection.More specifically; The present invention relates to a kind of method that in cyclic process, adopts novel regenerator; Be used to remove sulfolane degraded and corrosion product; Comprise acid, polymer, little iron and husky solids, thereby solvent is maintained high quality level, and obtain the extracting system of high operational efficiency and low corrosion successively.In addition, through removing these pollutants, the degradation speed of sulfolane is greatly reduced, and then makes the consumption of sulfolane drop to minimum.Characteristic of the present invention is to remove the efficient height of pollutant, and simple in structure, operation and maintenance cost is low.
Background technology
Sulfolane, chemical formula are C
4H
8O
2S has another name called tetramethylene sulfone-1,1-dioxide and tetramethyl sulfone.Sulfolane is as extraction and reaction dissolvent; Be used for separating aromatic hydrocarbon (for example benzene, toluene and xylenes) from non-aromatic hydrocarbon (for example paraffin wax and cycloalkane); Also be used to separate normal propyl alcohol and sec-butyl alcohol, and be used for refining natural gas stream and the aliphatic acid fractionation is become saturated component and unsaturated component.
The sulfolane unit usually mixes with the aromatic hydrocarbon compound, is used for from reformate and drippolene highly purified benzene of recovery and toluene products.In the aromatic hydrocarbon compound in modern times, the sulfolane unit is arranged on the downstream of reformate knockout tower.
In the sulfolane extraction tower, aromatic hydrocarbon is dissolved in the sulfolane, and this mixture is an extraction attitude (bottom), and remaining non-aromatic hydrocarbon counter current contacting, through with butterfly for example rotating disc column RDC mix and can improve stage efficient.
At first in coalescent filter, from extract, reclaim sulfolane, in water scrubber, reclaim then.Final extract is injected into blending naphtha as gasoline component.
With after other sulfolane contacts again, extract is stripped from and in aromatic hydrocarbon, is concentrated.Solvent is recovered through from extract, distilling under vacuum; Through cooling and clay treatment, remove alkene and diolefins, from water, isolate extract; Deliver to aromatic hydrocarbon fractionation unit separation of benzene and toluene then.
In the sulfolane extracting system, serious etching problem is often arranged.The corrosion of sulfolane that keeper has often been polluted, keeper comprise that the rich solvent pipeline, the extraction that are connected to stripper peel off tower, reboiler, transmission pipeline and solvent recovery tower.Along with the quickening of corrosion rate, keyhole progressively shows, and causes about safety problem and dangerous concern.
The root of corrosion mainly is the accumulation of the acidic materials in the circulating solvent.Contaminated sulfolane is from the colourless black that becomes, become more thickness with become acidity (pH value step-down to 4), have corrosivity.Generally speaking, below four be regarded as cause in the sulfolane extraction cells corrosion the main cause of erosion problem.
Oxygen in the equipment (porch or via the input fluid)
Chlorine in the circulating solvent
The accumulation of degraded and corrosion product in the equipment
High temperature in the reboiler
Degraded and corrosion product are gluing, gluey, bonding, frowzy, tedious and intractable.Through the several years, degraded and corrosion product are accumulated in equipment.These degradeds and corrosion product deposit in system, blocking filter, carbon adsorbent bed, thus make pressure drop increase, and the more important thing is the heat transfer coefficient that reduces heat exchanger, cause operational efficiency low.In addition, the dirt of accumulating in the equipment normally corrosive substance and or produce more catabolite as catalyst.A kind of makeshift of controlling corrosion is through interpolation MEA (MEA) thereby neutralizing acid, and this can bring extra pollution to sulfolane solvent.Operating experience shows that equipment needs once in a while clean completely.In commercial sulfolane extraction cells, approximately the dirt of 10-15 cubic meter is taken out from the unit.Thoroughly cleaning the sulfolane extraction cells is a large order really.
There are a lot of methods to keep the sulfolane cleaning in the cycling element, comprise:
1) filter bed or cross filter core is arranged on and is used for catching degraded and corrosion product in the poor sulfolane transfer tube.Yet filter bed or mistake filter core can be covered by a large amount of degradeds and corrosion product in a short period of time.Most of commercial are equipped with this filter course, but this filter course major part is all got around because of operating difficulties.
2) fill up two adsorption towers of adsorbent (for example active carbon), be used for removing degraded and corrosion product.Commercial experience shows that this adsorption tower is impracticable, because will soon be blocked, be difficult to cleaning and change adsorbent.
3) sulfolane reclaims: a small gangs of sulfolane shunting that is mounted with degraded and corrosion product is extracted out from the circulatory system, and is charged in the vacuum distillation unit.The top is the sulfolane of cleaning, be used for recycling in the circulatory system, and the bottom is degraded and corrosion product that being regarded waste disposal falls.This operating efficiency is not high, because have only a fraction of solvent to be recovered in the system.In addition, can produce the waste material of the needs processing of a lot of danger.
4) utilize cation and resin anion (R.A.) to remove acid contaminant, comprise sulfonic acid and a spot of carboxylic acid and hydrochloric acid.The application people be Lai and Bhat the 5th, 053, No. 137 US patent teaches a kind of through making a small gangs of fluid contaminated or spent sulfolane flow through the method for the purifications of two towers or regenerate contaminated or spent sulfolane successively.First tower fills up cation exchanger, and second tower fills up anion exchanger.Liu and Li show that the acid in degraded and the corrosion product can be effectively by resin cation ion-exchange [Liu lingchi and Li Dong-sheng; Petrochemical Design; 2002,19 (2) 31-33], thus the sulfolane solvent of cleaning more obtained.Resin cation with NaOH regeneration load acid.In this method, have only a small gangs of fluid by ion-exchange, the effect of therefore improving the sulfolane quality is limited.This method is very dirty and can produce the waste material of the needs processing of a large amount of danger.
In order to control rate of corrosion, can be through using the for example amine neutralizing acid of MEA (MEA).Yet the degraded and the corrosion product that remain in the circulatory system can silt heat exchanger up, cause obstruction and cause pressure drop to increase.In addition, the accumulation meeting of degraded and corrosion product is because autocatalysis promotes the degraded of sulfolane, and accelerated corrosion is degraded and the accumulation of corrosion product can cause vicious circle.Therefore, need a large amount of cleanings to maintain the level of allowing with the quality that guarantees sulfolane.
The prior art of the corrosion of control sulfolane and regeneration sulfolane has a lot of shortcomings in the circulatory system, comprising:
1) system's rate of corrosion is high, because the degraded of accumulation and corrosion product promote the degraded of sulfolane, and accelerated corrosion, and the accumulation of degraded and corrosion product can cause vicious circle.
2) owing to autocatalysis, the accumulation of degraded and corrosion product can be quickened.
3) operation tedium, the danger and expensive of replacing filter and/or adsorbent.
4) can't maintain when being equal to or higher than the expection level when the quality of sulfolane, service ability and efficient can reduce.
5) because shunting moves, the regeneration efficiency of sulfolane solvent is low.
6) operation and maintenance cost is high.
Clearly, need a kind of effective, safe, economic method contaminated sulfolane of regenerating in the industry, safety, efficiently, the operation aromatic hydrocarbon extracting system of ability, and operation and maintenance cost is low.
Summary of the invention
The present invention provides a kind of method of the contaminated sulfolane of in aromatic hydrocarbon extracting system closed circuit, regenerating continuously, and the quality of the sulfolane after the regeneration sulfolane with new in fact is the same.Special, this method adopts a kind of novel regenerator, through removing degraded and the corrosion product contaminated sulfolane of regenerating in the fluids all from the loop, keeps that the aromatic hydrocarbon extracting system is efficient, ability is moved.
A kind of novel regenerator is used to remove degraded and corrosion product, is arranged in the contaminated sulfolane solvent system all fluid in the cycle of treatment system.The preferred location of regenerator is in poor sulfolane section, the position that the cooler back is the coldest, and getting into extraction tower is most preferred position before.Two regenerator parallel connections are provided with, and therefore online regenerator can switch to subsequent use regenerator, thereby discharge degraded and the corrosion product of assembling.Special, regenerator comprises a high-pressure bottle with a dismountable lid and a circular support with vertical stainless steel tube, said circular support is assemblied in the high-pressure bottle.A bar magnet is set in each stainless steel tube.A screen drum, the cylindrical cavity that is installed in stainless steel tube is inner.When contaminated sulfolane was flowed through regenerator, regenerator was collected pollutant.Regenerator can be disassembled out regularly to remove pollutant.
Along with contaminated sulfolane gets into regenerator, degraded and corrosion product are attracted and stick on the vertical stainless steel tube that is filled with strong bar magnet, thereby from solvent system, are removed.The existence of inner screen drum has strengthened the ability that bar magnet is removed degraded and corrosion product.When the degraded of remnants and corrosion product will maintain very low level, this enhancing became most important.Through inner screen drum, sulfolane regeneration, cleaning leaves regenerator, is recycled back into extraction tower.After the running certain hour, for example fortnight, regenerator has been filled degraded and corrosion product, and the pressure drop of regenerator both sides increases.Fluid switches to subsequent use regenerator, and the regenerator of filling degraded and corrosion product is opened, dismounting disk and bar magnet.The disk that has magnetic in the VERTICAL TUBE is set in the container, and the magnetic of pipe is removed.In case the dismounting bar magnet, because the dismounting bar magnet loses its reliss, degraded and corrosion product drop from VERTICAL TUBE.The characteristic of this system is to remove the efficient height of pollutant, and simple in structure, operation and maintenance cost is low.
Therefore, objects and advantages of the present invention are following:
1) owing to having removed corrosive acid, degraded and corrosion product, so rate of corrosion is low;
2) owing to removed autocatalyst, degraded and corrosion product cumulative percentage are low;
3) purging system with change filter and/or adsorbent can tedium, danger, move also not expensive;
4) maintain near fresh level through quality, make service ability and stabilised efficiency sulfolane;
5) owing to all sulfolane fluids in the closed circuit all obtain regeneration, sulfolane solvent is regenerated effectively;
6) operation and maintenance cost is low.
According to following description and accompanying drawing, further purpose and advantage become obvious.
Description of drawings
Fig. 1 is a sketch map of representing the vertical section of regenerator according to a preferred embodiment of the present invention;
Fig. 2 is a sketch map of representing the STRUCTURE DECOMPOSITION of regenerator according to a preferred embodiment of the present invention;
Fig. 3 is the sketch map of the section of expression 3-3 shown in Figure 1;
Fig. 4 is an indicative flowchart that comprises the extracting system of regenerator of the present invention.
The specific embodiment
According to the present invention, the fluid of all contaminated poor sulfolane solvents flows through regenerator of the present invention continuously, thereby removes disacidify and degraded and corrosion product, and the quality of keeping sulfolane solvent is in fact with fresh identical.Novel regenerator is a core of the present invention.The installation and operation of regenerator also is critical.
Regenerator
Regenerator is a core of the present invention.The invention of regenerator and design are to be based upon on the basis of the character of finding degraded and corrosion product.The degraded and the corrosion product of accumulation have been considered to following several kinds usually:
1, the acid that produces owing to the oxidation of sulfolane, for example sulfonic acid and sulfuric acid;
2, the acid of chlorine generation, for example hydrochloric acid;
3, the oxidation of sulfolane and catabolite thereof the sulfolane oligomer that condenses and produce.
These products are acid, and pH value is low, and black in color is a viscosity, are deposited on easily in the system, for example in pipeline, filter and the heat exchanger, cause the reduction of service ability and efficient.These products are difficult to from solvent circuit and process equipment, remove.From solvent system, removing these products and system equipment is cleaned is the problem of whole world oil and petrochemical industry industrial research.
In our research, but we find to comprise the tiny black particles that contains sand in the product of viscosity.Above-mentioned product characteristic further shows that these products have natural paramagnetism, can be adsorbed onto on the magnet.The discovery that we are surprised, through using magnet, these products are removed, and contaminated sulfolane solvent becomes totally, and its character has obtained recovery.We believe that in processing procedure, equipment is corroded by acid byproduct, and iron ion is released.Iron ion further reacts with sulphur, oxygen and water, produces tiny paramagnetic particles, FeS for example, FeO and Fe (OH)
2Deng.These tiny black particles sulfolane solvents become black just.These tiny paramagnetic particles are stayed in the organic catabolite by envelope then, make all degradeds and corrosion product have paramagnetism.Therefore, through utilizing magnet, all degradeds and corrosion product can miraculously be removed from the solvent that has polluted, thereby make used solvent obtain regeneration.Through experiment and test, a kind of novel regenerator is devised, and its effect has obtained proof.
Fig. 1 to Fig. 3 is respectively the sketch map of expression regenerator.Regenerator 30 comprises a high-pressure bottle 37, and high-pressure bottle 37 has a dismountable lid 36, is used to bear the pressure of aromatic hydrocarbon extracting system.Regenerator 30 is provided with import 31 and outlet 32.Be provided with screen drum 80 in high-pressure bottle 37 inside.The mesh size of screen drum is 1 to 200 sieve mesh, preferred 10 to 100 sieve meshes.In screen drum 80 inside, three circular supports 33,34,35 are set from the top to the bottom.A plurality of stainless steel tubes 40 are connected on the circular support 33,34,35.The number of stainless steel tube 40 is 2 to 30, and is perhaps more.In the present embodiment, 12 stainless steel tubes are arranged attached on the circular support 33,34,35.The inner bar magnet 60 that inserts of each stainless steel tube.
Process configuration
Fig. 4 shows a kind of indicative flowchart of typical aromatic hydrocarbon extracting system.Extractor 10 is introduced in charging 11.Lean solvent 22 is introduced from extractor 10 tops.Raffinate 13 is removed from extractor 10 tops mutually; Thereby the recovery non-aromatic hydrocarbon, and extraction phase 12 extracts and charges into recovery tower 20 out from the bottom, reclaim the aromatic hydrocarbon as overhead 21; And reclaim lean solvent 22 as basic sediment, be used to get back to extractor 10 recirculation.Lean solvent 22 utilizes heat exchanger or aerial cooler 23 to be cooled, and the regenerator 30 of before returning extractor 10, at first flowing through.
Keeping regenerator 30 is vital effectively and efficiently.In order to realize this goal, we find that the best way is to handle all fluids rather than handle shunting.Therefore, regenerator 30 is arranged on all fluids of processing on the closed circuit.
For the continuous operation that realizes that regenerator is real, two regenerator 30A, 30B parallel connection are provided with, so one of them regeneration operation the time, another one is cleaned.
See also Fig. 1 and Fig. 4.Lean solvent 22 is introduced regenerator 30 through import 31, flows downward along the stainless steel tube that includes bar magnet 60 40, and is final through outlet 32 outflows.Screen drum 80 is used for the short circuit of the lean solvent 22 in the regenerator 30 is minimized.
Along with regenerator 30A, the 30B increase of the duration of runs, degraded continues to assemble with corrosion product, and around the stainless steel tube that includes bar magnet 60 40, accumulates.The pressure at regenerator 30 two ends increases, and must clean.The time cycle that regenerator 30A, 30B clean is 2 to 30 days even more, depends on the clean level of sulfolane.
For cleaning and regeneration device 30A, lean solvent 22 is switched to regenerator 30B and continues operation.Dismounting top cover 36, circular support and stainless steel tube 40, bar magnet 60 are dismantled from regenerator 30 together then.Space between the surface of stainless steel tube 40 and the stainless steel tube 40 has been full of the degraded and the corrosion product of accumulation now.After bar magnet 60 was dismantled from stainless steel tube 40, the degraded of accumulation and corrosion product had dropped totally owing to the gravity effect.Bar magnet 60 is reinstalled stainless steel tube 40, and circular support 33,34,35 is put back to regenerator 30, and is last, loads onto top cover 36, accomplishes cleaning process.Regenerator 30A is ready to come into operation once more now.
Process conditions
For effective operation, with regard to superficial velocity, the fluid velocity that flows through regenerator 30 is 10 to 10000v/v/Hr, and preferred 50 to 5000v/v/Hr.
The pressure drop of regenerator 30 both sides is indicators of cleannes or regenerator 30 residual capacities.When the pressure drop (Δ P) of regenerator 30 both sides is 1 to 5Kg/Cm
2Or higher the time, regenerator 30 should clean according to above-described program.
Instance
Instance 1
Build two regenerators, appearance and size is that diameter is 33Cm, highly is 65Cm, and volume is 55 liters.Bar magnet is inserted in the stainless steel tube on the circular support.Screen drum is of a size of 80 sieve meshes.Regenerator is installed in below the cooler abreast, in the poor sulfolane loop of the front of extractor.
Instance 2
Regenerator is to be tested in the aromatic hydrocarbon extracting system of oil plant.This extractor has moved 3 years, and poor sulfolane solvent is dirty, corrosive, has been full of gluing degraded and corrosion product.Extractor is 3600mm ID x 42000mm T-T.The charging of extractor is the reformate of 42531Kg/Hr.Contaminated poor sulfolane is 138602Kg/Hr through the circulation rate that regenerator gets into extractor.Therefore, the ratio of the solvent of this test and charging is about 3.Pressure drop when the regenerator both sides reaches 2Kg/Cm
2The time, the cleaning and regeneration device.In test at first, poor sulfolane solution is so dirty, to such an extent as to regenerator has to when finishing once week, clean.But along with poor sulfolane solution is reproduced the purification that device continues, the cycle of cleaning and regeneration device a from week was increased to for 2 week, to 4 week, up to 3 months.When support when regenerator is dismantled, the surface of stainless steel tube and the space between the stainless steel tube have been full of degraded black, gluing and corrosion product.Along with bar magnet is removed, black, gluing degraded and corrosion product fall down, and stainless steel tube becomes totally, can reuse.
The effectiveness of having showed regenerator of the present invention with the character that 3 months samples afterwards are installed before the installation regenerator.These character are:
1) amount of the poor sulfolane solvent to 288 of distillation ℃ remaining residue.Because sulfolane is 285 ℃ of boiling vaporizations, residue is degraded and corrosion product certainly.Therefore, residue content is low more, and poor sulfolane solvent is cleaner.
2) color of poor sulfolane solution: because degraded and corrosion product color are very dark, so the color of sulfolane solution is shallow more clean more.
3) ratio of amine (MEA): because acid produces in the sulfolane degradation process, thus be a constant in order to keep pH value, for example 8, the ratio that needs to add amine is low more, and sulfolane solution is clean more.
4) ratio of the supplementary rate of sulfolane: because sulfolane is degraded in processing procedure, a certain amount of poor sulfolane solvent need be eliminated, thereby keeps the quality of sulfolane.Therefore, fresh sulfolane need be added, and is used for the capacity that replenishes.So the supplementary rate of fresh sulfolane is low more, sulfolane solution is clean more.
Table 1 shows test result.
Table 1
The level of residue of the sample that records according to the ASTM86 method of testing is 1.0% before the regeneration, and regenerating after 3 months is 0.4%.Notice that extracting system is very dirty, have a large amount of degradeds and corrosion product.Therefore, the sample that test is specifically chosen does not have representativeness, and actual residue quantity originally can be far above 1% of demonstration.As a comparison, surprising clean of the extracting system after 3 months of regenerating, 0.4% residue content is the abundant performance of the poor sulfolane in the system.
Sample before the regeneration has significant difference with the color of the sample of regeneration after 3 months.This observation is consistent with the color code that records based on ASTM D1500 method of testing, and the color code of the sample before the regeneration that records based on ASTM D1500 method of testing is 3, and the color code of the sample after 3 months of regenerating is 0.5.
Above the result clearly show the regenerator of the present invention sulfolane solution contaminated or that lost efficacy of effectively regenerating.
More than describing is the preferred embodiments of the present invention, is used for exemplary explanation the present invention.Yet this is not to be used to limit protection scope of the present invention.The distortion of any equivalence of doing according to spirit of the present invention or change also all is included in protection scope of the present invention.
Claims (16)
1. the device of the contaminated sulfolane solvent of online regeneration comprises:
Limit the shell of compartment;
Be arranged at least one magnet of compartment interior; And
Guide contaminated sulfolane to flow through the mechanism of said at least one magnet.
2. device as claimed in claim 1, wherein said shell comprises pressure vessel, this pressure vessel is equipped with dismountable lid, and wherein a plurality of bar magnet is arranged in the said compartment.
3. device as claimed in claim 2; Wherein said pressure vessel is equipped with the inlet that is used for contaminated sulfolane; The outlet of the sulfolane after being used to handle; Said device also comprises sieve, and said sieve surrounds at least a portion of above-mentioned a plurality of bar magnets, flows and flows through said a plurality of bar magnet towards said a plurality of bar magnets from the contaminated sulfolane of said inlet with guiding.
4. device as claimed in claim 1 comprises:
High-pressure bottle with dismountable lid;
The bearing of a plurality of bar magnets in the fixed container;
Sieve, said sieve surrounds at least a portion of said a plurality of bar magnets.
5. device as claimed in claim 4, each in wherein said a plurality of bar magnets is all packed in the stainless steel tube.
6. device as claimed in claim 5 comprises 2 to 30 bar magnets.
7. device as claimed in claim 4, wherein pressure vessel be equipped with the inlet that is used for contaminated sulfolane and be used to handle after the outlet of sulfolane.
8. device as claimed in claim 4, wherein the mesh size of sieve is 10 to 100 sieve meshes.
9. method that is used for online regeneration from the contaminated sulfolane solvent of the extractor of extracting system comprises:
Regenerator is arranged in the poor sulfolane closed circuit, and wherein said regenerator comprises the shell that limits compartment, and this compartment interior is provided with at least one magnet;
Guiding gets into regenerator from the poor sulfolane solvent of extracting system through the inlet in the shell, and pollutant is removed by at least one magnet whereby;
Outlet discharge from shell comprises the effluent of the sulfolane solvent after the processing; And
Making effluent get into extractor once more recycles.
10. method as claimed in claim 9, wherein said shell comprises the pressure vessel of being equipped, wherein a plurality of bar magnets are arranged in the compartment.
11. method as claimed in claim 10, each in wherein said a plurality of bar magnets is all packed in the stainless steel tube.
12. method as claimed in claim 9, wherein said extracting system comprises aerial cooler or heat exchanger, is used for before contaminated sulfolane solvent gets into regenerator, changing its temperature.
13. method as claimed in claim 9, the running temperature of wherein said regenerator are 20 to 150 ℃.
14. method as claimed in claim 9, the fluid velocity that wherein flows through said regenerator are 50 to 5000v/v/Hr.
15. method as claimed in claim 9; Further comprise: in poor sulfolane closed circuit, second regenerator is set, wherein said second regenerator comprises second shell, and this second shell limits second compartment; This second compartment has at least one magnet that is arranged at wherein; And wherein first regenerator and the second regenerator parallel running, thereby the same time both can a regenerator isolated operation, also can move simultaneously by two regenerators.
16. method as claimed in claim 15 comprises that the pressure drop when the initial regenerator both sides of moving reaches 1 to 5kg/cm
2In the time of perhaps higher, switch to the step of operation another one regenerator from the regenerator that moves initial operation.
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| PCT/US2009/005672 WO2011049544A1 (en) | 2009-10-19 | 2009-10-19 | Process and apparatus for online rejuvenation of contaminated sulfolane solvent |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN102686294A true CN102686294A (en) | 2012-09-19 |
| CN102686294B CN102686294B (en) | 2015-05-20 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN200980161811.7A Expired - Fee Related CN102686294B (en) | 2009-10-19 | 2009-10-19 | Process and apparatus for online rejuvenation of contaminated sulfolane solvent |
Country Status (5)
| Country | Link |
|---|---|
| EP (1) | EP2490787A4 (en) |
| JP (1) | JP5521049B2 (en) |
| KR (1) | KR101570901B1 (en) |
| CN (1) | CN102686294B (en) |
| WO (1) | WO2011049544A1 (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106957297A (en) * | 2016-12-31 | 2017-07-18 | 光华（营口）化工技术服务有限公司 | A kind of renovation process of inferior sulfolane solvent |
| CN109622221A (en) * | 2018-12-26 | 2019-04-16 | 樊振 | Discarded metal collecting device in a kind of sewage |
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|---|---|---|---|---|
| JP6912911B2 (en) * | 2017-03-21 | 2021-08-04 | トリニティ工業株式会社 | Magnet filter |
| CN107262275A (en) * | 2017-05-16 | 2017-10-20 | 合肥市瀚坤机械有限公司 | A kind of electronic isolated machining waste water oil-water separation tank Magnetic filtration device frame |
| JP7079105B2 (en) * | 2018-01-22 | 2022-06-01 | ヤマシンフィルタ株式会社 | Filter device |
| KR102629120B1 (en) * | 2020-11-09 | 2024-01-24 | 주식회사 엘지화학 | Method for removing metalic material in petrochemical product |
| KR102620509B1 (en) * | 2023-06-15 | 2024-01-03 | (주)동진테크 | Strainer |
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- 2009-10-19 CN CN200980161811.7A patent/CN102686294B/en not_active Expired - Fee Related
- 2009-10-19 JP JP2012535172A patent/JP5521049B2/en not_active Expired - Fee Related
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| CN109622221A (en) * | 2018-12-26 | 2019-04-16 | 樊振 | Discarded metal collecting device in a kind of sewage |
Also Published As
| Publication number | Publication date |
|---|---|
| WO2011049544A1 (en) | 2011-04-28 |
| CN102686294B (en) | 2015-05-20 |
| KR101570901B1 (en) | 2015-11-20 |
| EP2490787A4 (en) | 2014-03-19 |
| KR20120083482A (en) | 2012-07-25 |
| EP2490787A1 (en) | 2012-08-29 |
| JP2013508501A (en) | 2013-03-07 |
| JP5521049B2 (en) | 2014-06-11 |
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