CA2527443A1 - Method for sulfur compounds removal from contaminated gas and liquid streams - Google Patents

Method for sulfur compounds removal from contaminated gas and liquid streams Download PDF

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Publication number
CA2527443A1
CA2527443A1 CA002527443A CA2527443A CA2527443A1 CA 2527443 A1 CA2527443 A1 CA 2527443A1 CA 002527443 A CA002527443 A CA 002527443A CA 2527443 A CA2527443 A CA 2527443A CA 2527443 A1 CA2527443 A1 CA 2527443A1
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CA
Canada
Prior art keywords
zeolite
anyone
desorption
sulfur compounds
temperature
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.)
Granted
Application number
CA002527443A
Other languages
French (fr)
Other versions
CA2527443C (en
Inventor
Peter Hawes
Andreas Scheuble
Beat Kleeb
Armin Pfenninger
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Zeochem AG
Original Assignee
Peter Hawes
Andreas Scheuble
Beat Kleeb
Armin Pfenninger
Zeochem Ag
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Application filed by Peter Hawes, Andreas Scheuble, Beat Kleeb, Armin Pfenninger, Zeochem Ag filed Critical Peter Hawes
Publication of CA2527443A1 publication Critical patent/CA2527443A1/en
Application granted granted Critical
Publication of CA2527443C publication Critical patent/CA2527443C/en
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Classifications

    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D15/00Separating processes involving the treatment of liquids with solid sorbents; Apparatus therefor
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D53/00Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
    • B01D53/02Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by adsorption, e.g. preparative gas chromatography
    • B01D53/04Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by adsorption, e.g. preparative gas chromatography with stationary adsorbents
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/10Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
    • B01J20/16Alumino-silicates
    • B01J20/18Synthetic zeolitic molecular sieves
    • B01J20/183Physical conditioning without chemical treatment, e.g. drying, granulating, coating, irradiation
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/10Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
    • B01J20/16Alumino-silicates
    • B01J20/18Synthetic zeolitic molecular sieves
    • B01J20/186Chemical treatments in view of modifying the properties of the sieve, e.g. increasing the stability or the activity, also decreasing the activity
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/30Processes for preparing, regenerating, or reactivating
    • B01J20/34Regenerating or reactivating
    • B01J20/3408Regenerating or reactivating of aluminosilicate molecular sieves
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10GCRACKING 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
    • C10G25/00Refining of hydrocarbon oils in the absence of hydrogen, with solid sorbents
    • C10G25/02Refining of hydrocarbon oils in the absence of hydrogen, with solid sorbents with ion-exchange material
    • C10G25/03Refining of hydrocarbon oils in the absence of hydrogen, with solid sorbents with ion-exchange material with crystalline alumino-silicates, e.g. molecular sieves
    • C10G25/05Removal of non-hydrocarbon compounds, e.g. sulfur compounds
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D2253/00Adsorbents used in seperation treatment of gases and vapours
    • B01D2253/10Inorganic adsorbents
    • B01D2253/106Silica or silicates
    • B01D2253/108Zeolites
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D2257/00Components to be removed
    • B01D2257/30Sulfur compounds
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D2257/00Components to be removed
    • B01D2257/30Sulfur compounds
    • B01D2257/306Organic sulfur compounds, e.g. mercaptans
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D2259/00Type of treatment
    • B01D2259/40Further details for adsorption processes and devices
    • B01D2259/40083Regeneration of adsorbents in processes other than pressure or temperature swing adsorption
    • B01D2259/40088Regeneration of adsorbents in processes other than pressure or temperature swing adsorption by heating
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D53/00Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
    • B01D53/02Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by adsorption, e.g. preparative gas chromatography

Abstract

Abstract Described is a desorption process and a process for producing a catalytically deactivated formed zeolitic adsorbent, whereby both processes are suitable to improve the lifetime of a formed zeolithic adsorbant in the removal of sulfur compounds from sulfur contaminated gas and liquid feed streams. The adsorbent is in particular a synthetic 13X or LSX faujasite with a silica to alumina ratio from 1.9 : 1.0 to about 3.0 : 1Ø The cations of the faujasite include alkali and alkaline earth metals. The formed zeolite mixture is preferably catalytically deactivated due to a phosphate treatment.
The desorption is carried out thermally, wherein the heat treatment is done at different temperature stages to avoid decomposition of the organic sulfur compounds.

Claims (25)

1. A process to produce a formed zeolite for adsorption purposes with improved adsorption and desorp-tion properties comprising the following steps a) mixing of at least one faujasite zeolite powder, in particular a zeolite 13X powder or a zeolite LSX powder, with a clay type binder, an inorganic phos-phorous salt, water and, optionally, with an organic ad-ditive b) production of a formed zeolitic body out of the mixture of step a), and c) drying and calcination of said zeolitic body produced in step b) to fix the binder and to get the active adsorption reagent.
2. The process of claim 1, comprising after step c) a step of ion exchange.
3. The process of anyone of the preceding claims, wherein the amount of clay binder is between 5 and 30 weight percent of the formed body weight.
4. The process of anyone of the preceding claims, wherein the amount of clay binder is between 5 and 20 weight percent of the formed body weight.
5. The process of anyone of the preceding claims, wherein the zeolite powder is at least 70 % in its sodium form.
6. The process of anyone of the preceding claims, wherein the zeolite powder is at least 90% in its sodium form.
7. The process of anyone of the preceding claims, wherein the zeolite powder is at maximum 30 % in its potassium form.
8. The process of anyone of the preceding claims, wherein a pore forming agent is added to the zeo-lite and binder mixture, in particular a pore forming agent selected from the group consisting of Rayon fibers, Nylon fibers, Sisal fibers and flax, as well as organic polymers, such as starch, starch derivatives, ligninsul-fonates, polyacrylamides, polyacrylic acids, cellulose and cellulose derivatives.
9. The process of anyone of the preceding claims, wherein the pore forming agent amounts to 2 to 15 weight percent based on the formed body weight.
10. The process of anyone of the preceding claims, wherein the inorganic phosphorous salt used in step b) is a water soluble phosphorous salt, in particu-lar a phosphorous salt selected from the group consisting of tetrasodium diphosphate, tetrasodium polyphosphate, trisodium phosphate, disodium hydrogen phosphate, sodium dihydrogen phosphate, tripotassium phosphate, dipotassium hydrogen phosphate, potassium dihydrogen phosphate or a mixture of two or more of said phosphorous salts.
11. The process of anyone of the preceding claims, where the amount of inorganic phosphorous salt is between 0.3 and 5.0 weight percent based on the formed body weight.
12. The process of anyone of the preceding claims, where the amount of inorganic phosphorous salt is between 0.3 and 3.0 weight percent based on the formed body weight.
13. A zeolitic adsorption compound obtainable according to the process of anyone of the preceding claims.
14. A process to remove by adsorption one or more low molecular weight organic sulfur compounds from a gaseous or liquid stream, wherein the feed stream is passed through a bed of formed zeolitic molecular sieve according to claim 13.
15. The process of claim 14, wherein the or-ganic sulfur compounds are one or more low molecular weight mercaptans or sulfides.
16. The process of claim 14 or 15, wherein the adsorption temperature is at most 60°C.
17. A desorption process for the desorption of organic sulfur compounds from a formed faujasite zeo-lite, in particular formed zeolite 13X or formed zeolite LSX, or a mixture of formed zeolite 13X and formed zeo-lite LSX, wherein the desorption is done by a heating profile allowing the organic sulfur compounds to reach their equilibrium adsorption capacity at each tempera-ture.
18. A desorption process, in particular ac-cording to claim 17, for the desorption of organic sulfur compounds from a formed faujasite zeolite, in particular formed zeolite 13X or formed zeolite LSX, or a mixture of formed zeolite 13X and formed zeolite LSX, wherein the desorption is done by fast heating to a basic temperature of at most 200°C, preferably 100 to 150°C, in particular about 150°C, and then using a temperature halt at differ-ent temperature levels starting at the basic temperature.
19. A process according to claim 18, wherein the halt time is at least 10 minutes at each temperature level.
20. A process according to claim 18 or 19, wherein the temperature levels are at least 5°C and at most 50°C apart from each other.
21. A desorption process, in particular ac-cording to claim 17, of organic sulfur compounds from a formed faujasite zeolite, in particular a formed zeolite 13X or formed zeolite LSX, or a mixture of formed zeolite 13X and LSX, wherein the desorption is done by fast heat-ing to a basic temperature of at most 200°C, preferably 100 to 150°C, in particular about 150°C, and then heating using a small temperature increase rate at temperature levels above the basic temperature.
22. A process of claim 21, wherein the tem-perature increase rate is less than 3°C/min.
23. The process of anyone of claims 17 to 22, wherein the zeolite is a zeolite of claim 13.
24. The process of anyone of claims 17 to 23, wherein the maximum regeneration temperature is about 320°C.
25. The process of anyone of claims 17 to 24, wherein the regeneration gas is a dry natural gas, meth-ane, natural gas liquids, hydrogen, nitrogen or hydrocar-bons.
CA2527443A 2003-06-06 2003-06-06 Method for sulfur compounds removal from contaminated gas and liquid streams Expired - Fee Related CA2527443C (en)

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
PCT/IB2003/002541 WO2004108273A1 (en) 2003-06-06 2003-06-06 Method for sulfur compounds removal from contaminated gas and liquid streams

Publications (2)

Publication Number Publication Date
CA2527443A1 true CA2527443A1 (en) 2004-12-16
CA2527443C CA2527443C (en) 2011-03-15

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ID=33495837

Family Applications (1)

Application Number Title Priority Date Filing Date
CA2527443A Expired - Fee Related CA2527443C (en) 2003-06-06 2003-06-06 Method for sulfur compounds removal from contaminated gas and liquid streams

Country Status (7)

Country Link
US (1) US7651550B2 (en)
EP (1) EP1633475B1 (en)
AU (1) AU2003239295A1 (en)
CA (1) CA2527443C (en)
DE (1) DE60333129D1 (en)
NO (1) NO20055679L (en)
WO (1) WO2004108273A1 (en)

Families Citing this family (11)

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US8323603B2 (en) 2004-09-01 2012-12-04 Sud-Chemie Inc. Desulfurization system and method for desulfurizing a fuel stream
US20060283780A1 (en) * 2004-09-01 2006-12-21 Sud-Chemie Inc., Desulfurization system and method for desulfurizing a fuel stream
GB0619396D0 (en) 2006-10-02 2006-11-08 M I Drilling Fluids Uk Ltd Porous articles
JP5706126B2 (en) * 2010-10-07 2015-04-22 出光興産株式会社 Adsorbent regeneration method
CN101982232B (en) * 2010-10-29 2013-03-13 烟台大学 Deaminizing agent and preparation method thereof
US20140088334A1 (en) * 2011-01-14 2014-03-27 Uop Llc Process for removing one or more sulfur compounds from a stream
US9150471B2 (en) * 2011-10-28 2015-10-06 Uop Llc Methods and apparatuses for treating a hydrocarbon-containing feed stream
CN103721668B (en) * 2012-10-10 2016-07-13 中国科学院大连化学物理研究所 A kind of Gasoline ultra-deep desulfurization adsorbent and application thereof
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CN110627090A (en) * 2018-06-25 2019-12-31 中国石油化工股份有限公司 Preparation method and application of sulfydryl functionalized SBA molecular sieve

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Also Published As

Publication number Publication date
DE60333129D1 (en) 2010-08-05
NO20055679D0 (en) 2005-12-01
EP1633475A1 (en) 2006-03-15
WO2004108273A1 (en) 2004-12-16
US7651550B2 (en) 2010-01-26
CA2527443C (en) 2011-03-15
AU2003239295A1 (en) 2005-01-04
EP1633475B1 (en) 2010-06-23
NO20055679L (en) 2006-01-04
US20070193939A1 (en) 2007-08-23

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