EP0239687A1 - Désulfuration d'hydrocarbures - Google Patents
Désulfuration d'hydrocarbures Download PDFInfo
- Publication number
- EP0239687A1 EP0239687A1 EP86302463A EP86302463A EP0239687A1 EP 0239687 A1 EP0239687 A1 EP 0239687A1 EP 86302463 A EP86302463 A EP 86302463A EP 86302463 A EP86302463 A EP 86302463A EP 0239687 A1 EP0239687 A1 EP 0239687A1
- Authority
- EP
- European Patent Office
- Prior art keywords
- sulfur
- catalyst
- percent
- sorbent
- wppm
- 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.)
- Ceased
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Classifications
-
- 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
- C10G61/00—Treatment of naphtha by at least one reforming process and at least one process of refining in the absence of hydrogen
- C10G61/02—Treatment of naphtha by at least one reforming process and at least one process of refining in the absence of hydrogen plural serial stages only
- C10G61/06—Treatment of naphtha by at least one reforming process and at least one process of refining in the absence of hydrogen plural serial stages only the refining step being a sorption process
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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
- C10G25/00—Refining of hydrocarbon oils in the absence of hydrogen, with solid sorbents
- C10G25/003—Specific sorbent material, not covered by C10G25/02 or C10G25/03
Definitions
- a process for the desulfurization of sulfur-containing hydrocarbon feedstocks, especially reformer feedstocks relates to a process for the removal of sulfur from hydrofined reformer feedstocks, without reduction in the temperature of the feedstock as received from the hydrofiner, via the use of an adsorbent, or sorbent.
- sorbents for the removal of sulfur from process streams, including particularly hydrocarbon process streams.
- the nature and quality of such sorbents varies widely, particularly as relates to this capacity to remove a wide variety of sulfur species, viz., mercaptans, thiophenes, disulfides, thioethers, hydrogen sulfide, carbonyl sulfide, and the like.
- Such sorbents are not especially suitable for the essentially complete removal of sulfur from process streams, as required in some operations, e.g., catalytic reforming, or hydroforming, a well-known and important process employed in the petroleum refining industry for improving the octane quality of naphthas and straight run gasolines.
- a series of reactors of the reforming unit are each provided with fixed beds of sulfided catalyst which are sequentially contacted with a naphtha feed, and hydrogen at high severities, e.g., at high temperatures and low pressures.
- Each reactor is provided with a preheater, or interstage heater, because the reactions which take place are endothermic, and the temperature between the several reactors is progressively increased.
- a sulfur-containing straight run gasoline, or naphtha is first hydrofined (or hydrodesufurized) to remove a preponderance of the sulfur, and the desulfurized feed then reformed.
- a sulfur-containing straight-run gasoline, or naphtha is contacted with hydrogen, over a Group VIB and/or Group VIII metal catalyst, e.g., cobalt molybdate or nickel molybdate supported on alumina, at conditioners sufficient to remove a preponderance of the sulfur as hydrogen sulfide, and the liquid product recovered for use as feed to the reformer.
- a Group VIB and/or Group VIII metal catalyst e.g., cobalt molybdate or nickel molybdate supported on alumina
- the hydrofiner cannot reduce the sulfur levels to the amounts that are desired, or required; which may be of the order of 2 wppm, 0.5 wppm, or even 0.1 wppm, or less. Moreover, even if hydrofiners were capable of such effective operation, they are not capable of such operation 100 percent of the time. Upsets can and do occur. Typically, the naphtha feed will contain as much as 5 wppm to about 50 wppm, or more, of sulfur; and, if upsets occur, the feed during some portions of an operating cycle will contain even higher amounts of sulfur.
- Sorbent or catalyst packed guard chambers, or vessels filled with sorbents or catalysts consequently have been used to remove additional sulfur from hydrofined products prior to their use as reformer feeds.
- Massive nickel catalysts e.g., nickel on a silica-alumina support, have been particularly effective in removing sulfur from hydrofined products, or naphthas at temperatures ranging below about 350°F. Higher temperatures than about 350°F cannot be used for the removal of sulfur from naphthas with massive nickel catalysts, however, because the production of fused multi-ring aromatics or polynuclear aromatic compounds (PNA's) in the naphtha becomes excessive.
- PNA's fused multi-ring aromatics or polynuclear aromatic compounds
- ORI octane requirement increase
- PNA's are undesirable, not only in that they cause deactivation of reformer catalysts, but they are also primarily responsible for the octane requirement increase (ORI) known to occur in automobile engines.
- ORI is caused by the build-up of carbonaceous deposits in internal combustion engines (particularly old engines) which, by limiting heat transfer from the combustion chamber, leads to preignition. Preignition causes the phenomenon known as engine knock or ping which is "cured" by burning higher octane gasolines.
- the PNA's are major contributors to the build-up of carbon deposits over the lifetime of an engine, which leads to ORI.
- the ORI can be as small as 1-2 octane numbers or as great as 10-12 octane numbers.
- the naphtha feed from the hydrofiner is available at temperatures far in excess of 350°F, e.g., 500°F and higher, and whereas expensive heat exchange processes might be employed to reduce the temperature to 350°F, or less, the naphtha, after such treatment, would have to be reheated to the temperature required for reforming.
- This step is obviously quite burdensome, particularly in these times of increasing fuel costs.
- a sorbent, or catalyst useful for removing sulfur at temperatures above about 350°F, or at temperatures ranging about above 350°F up to reforming temperatures; temperatures which normally produce excessive PNA's.
- a particular object is to provide a novel, and improved nickel sorbent, or catalyst, and process for the use of such sorbent, or catalyst, to effectively remove sulfur from naphthas at temperatures above about 350°F without the significant production of PNA's.
- a particulate mass of the sulfur sorbent is charged, or packed into a guard chamber, or plurality of guard chambers and employed downstream of a hydrofiner for removing sulfur from a naphtha hydrofiner product.
- the guard chambers are employed in series, one behind the other in tandem relationship, or in parallel downstream of the hydrofiner.
- the sulfur-containing naphtha product from the hydrofiner, constituting a reformer feed, is introduced into the guard chamber, or guard chambers, the sulfur-containing naphtha product from the hydrofiner being passed therethrough, the naphtha being thereby denuded of sulfur, and the sulfur-denuded naphtha product then employed as feed to the reforming, or hydroforming unit.
- sulfur can be effectively removed from a hydrofined naphtha containing up to about 20 wppm sulfur, or even up to about 50 wppm sulfur, and higher, to provide a naphtha reformer feed containing less than about 2 wppm sulfur, or less than about 0.5 wppm sulfur, and even less than about 0.1 wppm sulfur, by contacting the hydrofined naphtha product with the contact mass at temperatures ranging above about 350°F, preferably from about 500°F to about 850°F, more preferably from about 700°F to about 800°F.
- the sulfur is effectively removed from the hydrofined naphtha, and at the same time there is a minimum of polynuclear aromatics produced, and transported with the naphtha feed to the catalyst packed reactors of the reforming unit.
- the FIGURE depicts, by means of a simplified flow diagram, the use of a nickel/iron sorbent packed guard chamber or "sulfur trap" downstream of a hydrofiner, between said hydrofiner and reforming unit.
- a hydrofiner, H/F, and reforming unit inclusive of multiple on-stream reactors R1, R2, and R3 each of which is provided with a fixed bed of a sulfur sensitive polymetallic platinum catalyst.
- a separate furnace, or heater F1, F2, and F3, respectively, is connected in series with the reactors, R1, R2, and R3 so that feed can be passed in seratim through F1R1, F2R2, and F3R3. Pumps, compressors and other auxiliary equipment are omitted for clarity.
- a deisomerizer, debutanizer, and guard chamber, or sulfur trap are located between the hydrofiner H/F and the reforming unit.
- a hydrofined petroleum or synthetic naphtha feed from hydrofiner H/F is passed serially through the deisomerizer and debutanizer, and the partiallyd desulfurized feed then passed through the sulfur trap wherein essentially the balance of the sulfur is removed. Then, the desulfurized naphtha feed, with hydrogen, is passed through the F1R1, F2R2, and F3R3 with the products from the reactions being passed to a high pressure separator HPS.
- a portion of the hydrogen-rich make gas can be taken from the top of the high pressure separator HPS and, after passage through a make gas compressor, recycled to the hydrofiner, H/F, and another portion recycled through gas driers to the lead furnace and reactor F1R1.
- Substantially all, or a major portion of the moisture and sulfur can be scrubbed and removed from the recycle gas by the recycle gas drier to maintain a dry, low-sulfur system.
- C5+ liquids from the bottom of high pressure separator HPS are sent to a stabilizer, or to tankage.
- the feed which is hydrofined to provide the reformer feedstock is constituted of a naphtha, whether a virgin naphtha, straight run gasoline, thermally or catalytically cracked naphtha or the like, or blends thereof, which boils within a range for about 80°F to about 450°F, preferably from about 150°F to about 430°F.
- the predominant hydrocarbons have from about 5 to 12 carbon atoms, more typically from about 6 to about 9 carbon atoms per molecule.
- such a gasoline will contain from about 15 vol. % to about 20 vol.
- % paraffins, naphthenes, and branched paraffins which fall within a range of from about C5+ to about C12, from about 15 vol. % to about 20 vol. % of olefins which fall within a range of from about C6 to about C12, and from about 60 vol. % to about 70 vol. % of aromatics, the preponderance of which fall within a range of from about C6 to about C12.
- Most of the gasoline that are used for motor vehicles are derived from petroleum, but may also be derived in whole or in part from hydrocarbons obtained for synthetic sources.
- Such feeds, prior to hydrofining generally contain from about 300 wppm to about 10,000 wppm sulfur, or more typically from about 300 wppm to about 2000 wppm sulfur, as organo sulfur compounds.
- the hydrofining operation is typically conducted at conditions of temperature, pressure, hydrogen flow rate, and liquid hourly space velocities correlated to provide the desired amount of conversion to convert the organo sulfur compounds to hydrogen sulfide.
- the sulfur-containing naphtha is introduced, with hydrogen, into a reactor provided with a catalyst comprised of a Group VIB metal, or metals, of the Periodic Table of the Elements (E. H. Sargent & Co., Copyright 1964 Dyna-Slide Co.), or a Group VIII metal, or metals, or both; inclusive patricularly of the oxides and/or sulfides of such metals, and admixtures of Group VIB and Group VIII metals.
- the metals are preferably supported on a porous, refractory inorganic oxide base, e.g., alumina, silica, zirconia, titania, bauxite, or the like.
- a catalyst suitably ranges from between about 2 to 25 weight percent.
- Suitable catalysts include cobalt-molybdate, chromic acid, nickel, iron, etc., which are deposited on carriers, such as alumina, or various other oxides, or gels.
- a suitable catalyst for the hydrofining process is, for example, an alumina-containing support with a minor proportion of molybdenum oxide and cobalt oxide.
- Sulfided nickel and tungsten on alumina as well as nickel-molybdenum on alumina can also be used.
- the hydrofining runs are conducted by adjusting the hydrogen and feed rates, and the temperature and pressure to the conditions desired to remove the desired amount of sulfur from the feed.
- the run is made by adjustment of the major process variables within the ranges described below:
- the effluent from the hydrofining zone is treated to remove hydrogen sulfide and ammonia from the hydrofined naphtha.
- Removal of hydrogen sulfide and ammonia may be accomplished, for example, by injecting water or alkylized water into the hydrofiner effluent and passing the resulting mixture into a separator operating under such conditions that a water phase containing essentially all the hydrogen sulfide and ammonia present in the effluent can be removed.
- purification of the hydrofined feed can be accomplished by a stripper or a distillation column.
- the hydrogen sulfide and ammonia can be removed by passing the hydrofiner effluent to a separator at a temperature and pressure whereby substantially only hydrogen sulfide, ammonia, and hydrogen are in the gaseous state.
- the liquid naphtha is thus easily separated from the gases. While it is essential to free the naphtha of hydrogen sulfide and ammonia, hydrogen dissolved in the naphtha presents no problem, but is desirable.
- the guard chamber, or guard chambers containing the nickel-iron catalyst of this invention, viz., at temperature ranging from about 300°F to about 600°F, preferably from about 350°F to about 500°F.
- substantially all hydrofined products contain some PNA's, substantially no new PNA formation occurs in the desulfurization reaction produced by the nickel-iron sorbent of this invention.
- the desulfurization reaction can be conducted with or without the addition of hydrogen to the nickel-iron sorbent-containing guard chamber, or guard chambers.
- the reforming catalyst is constituted of composite particles which contain, besides a carrier or support material, a hydrogenation-dehydrogenation component, or components, and a halide component.
- the support material is constituted of a porous, refractory inorganic oxide, particularly alumina.
- the support can contain, e.g., one or more of alumina, bentonite, clay, diatomaceous earth, zeolite, silica, activated carbon, magnesia, zirconia, thoria, an the like; though the most preferred support is alumina to which, if desired, can be added a suitable amount of other refractory carrier materials such as silica, zirconia, magnesia, titania, etc., usually in a range of about 1 to 20 percent, based on the weight of the support.
- a preferred support is one having a surface area of more than 50 m2/g, a bulk density of about 0.3 to 1.0 g/ml, preferably about 0.4 to 0.8 g/ml, an average pore volume of about 0.2 to 1.1 ml/g, preferably about 0.3 to 0.8 ml/g, and an average pore diameter of about 30 to 300°A.
- the metal hydrogenation-dehydrogenation component can be composited with or otherwise intimately associated with the porous inorganic oxide support or carrier by various techniques known to the art such as ion-exchange, coprecipitation with the alumina in the sol or gel form, and the like.
- the catalyst composite can be formed by adding together suitable reagents such as a salt of platinum and ammonium hydroxide or carbonate, and a salt of aluminum such as aluminum chloride or aluminum sulfate to form aluminum hydroxide.
- suitable reagents such as a salt of platinum and ammonium hydroxide or carbonate
- a salt of aluminum such as aluminum chloride or aluminum sulfate
- the aluminum hydroxide containing the salts or platinum can then be heated, dried, formed into pellets or extruded, and then calcined in nitrogen or other non-agglomerating atmosphere.
- Other metal hydrogenation components can also be added to the catalyst in similar manner, or by impregnation.
- platinum, or platinum and rhenium metals, or other metal or metals used as promoters are preferred to deposit the platinum, or platinum and rhenium metals, or other metal or metals used as promoters, if any, on a previously pilled, pelleted, beaded, extruded, or sieved particulate support material by the impregnation method.
- porous refractory inorganic oxides in dry or solvated state are contacted, either alone or admixed, or otherwise incorporated with a metal or metals-containing solution, or solutions, and thereby impregnated by either the "incipient wetness” technique, or a technique embodying absorption from a dilute or concentrated solution, or solutions, with subsequent filtration or evaporation to effect total uptake of the metallic components.
- Platinum in absolute amount is usually supported on the carrier within the range of from about 0.01 to 3 percent, preferably from about 0.2 to 1 percent, based on the weight of the catalyst (dry basis).
- Rhenium, in absolute amount is also usually supported on the carrier in concentration ranging form about 0.1 to about 3 percent, preferably from about 0.2 to about 1 percent, based on the weight of the catalyst (dry basis).
- the absolute concentration of each for use in reactors is preselected to provide the desired ration of rhenium:platinum for a respective reactor of the unit.
- any soluble compound can be used, but a soluble compound which can be easily subjected to thermal decomposition and reduction is preferred, for example, inorganic salts such as halide, nitrate, inorganic complex compounds, or organic salts such as the complex salt of acetylacetone, amine salt, and the like.
- inorganic salts such as halide, nitrate, inorganic complex compounds, or organic salts such as the complex salt of acetylacetone, amine salt, and the like.
- platinum chloride, platinum nitrate, chloroplatinic acid, ammonium chloroplatinate, potassium chloroplatinate, platinum polyamine, platinum acetylacetonate, and the like are preferably used.
- a promoter metal is added in concentration ranging from about 0.01 to 3 percent, preferably from about 0.05 to about 1 percent, based on the weight of the catalyst.
- halogen component to the catalysts, fluorine and chlorine being preferred halogen components.
- the halogen is contained on the catalyst within the range of 0.1 to 3 percent, preferably within the range of about 0.6 to about 1.5 percent, based on the weight of the catalyst.
- chlorine when using chlorine as a halogen component, it is added to the catalyst within the range of about 0.2 to 2 percent, preferably within the range of about 0.6 to 1.5 percent, based on the weight of the catalyst.
- the introduction of halogen into the catalyst can be carried out by any method at any time.
- It can be added to the catalyst during catalyst preparation, for example, prior to, following or simultaneously with the incorporation of the metal hydrogenation-dehydrogenation component, or components. It can also be introduced by contacting a carrier material with a vapor phase or liquid phase containing a halogen compound such as hydrogen fluoride, hydrogen chloride, ammonium chloride, or the like.
- a halogen compound such as hydrogen fluoride, hydrogen chloride, ammonium chloride, or the like.
- the reforming operation is carried out by adjusting the hydrogen and feed rates, and the temperature and pressure to operating conditions.
- the run is made at optimum reforming conditions by adjustment of the major process variables, within the ranges described below:
- Catalyst A, B, and C were prepared by the techniques described above. These are listed as Catalyst A, B, and C in the table. Nickel to the extent of 50% by weight was supported on a silica/alumina base (15% SiO2) and designated as Catalyst A. The same amount of nickel was then impregnated on a pure alumina base and designated Catalyst B. A portion of this latter catalyst was then impregnated with iron nitrate to produce an adsorbent containing 5% Fe in addition to the nickel already impregnated. This is designated as Catalyst C.
- Catalysts of existing art are represented by Catalysts A and B.
- Catalyst A has a higher adsorption capacity of 14.5% sulfur but also produces a larger amount of PNA's as shown by the higher UV absorbance.
- the UV absorbance is decreased but also a substantial loss in sulfur capacity is incurred as illustrated by the results with Catalyst B.
- the material of this invention is that shown by Catalyst C.
- the extent of PNA production is greatly inhibited.
- the ability of the material to adsorb sulfur is substantially increased to the extent of 18.8% by weight.
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- Chemical & Material Sciences (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Production Of Liquid Hydrocarbon Mixture For Refining Petroleum (AREA)
Priority Applications (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
US06/686,453 US4592829A (en) | 1984-12-26 | 1984-12-26 | Desulfurization of hydrocarbons |
EP86302463A EP0239687A1 (fr) | 1986-04-03 | 1986-04-03 | Désulfuration d'hydrocarbures |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
EP86302463A EP0239687A1 (fr) | 1986-04-03 | 1986-04-03 | Désulfuration d'hydrocarbures |
Publications (1)
Publication Number | Publication Date |
---|---|
EP0239687A1 true EP0239687A1 (fr) | 1987-10-07 |
Family
ID=8195953
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
EP86302463A Ceased EP0239687A1 (fr) | 1984-12-26 | 1986-04-03 | Désulfuration d'hydrocarbures |
Country Status (1)
Country | Link |
---|---|
EP (1) | EP0239687A1 (fr) |
Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
DE3822132A1 (de) * | 1987-07-02 | 1989-01-12 | Inst Francais Du Petrole | Verfahren zur entfernung von arsen und/oder phosphorverbindungen aus fluessigen kohlenwasserstoffen |
EP0412862A1 (fr) * | 1989-08-08 | 1991-02-13 | Institut Français du Pétrole | Masse de captation à base de nickel pour l'élimination de l'arsenic et du phosphore contenus dans les coupes d'hydrocarbures liquides, sa préparation et son utilisation |
US8308848B1 (en) | 2009-11-27 | 2012-11-13 | Tda Research, Inc. | High temperature gas desulfurization sorbents |
Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
GB1333666A (en) * | 1971-04-23 | 1973-10-10 | Kazak Khmiko T I | Method of producing polyhydric alcohols |
US4089809A (en) * | 1976-03-01 | 1978-05-16 | The United States Of America As Represented By The United States Department Of Energy | Regenerable sorbent and method for removing hydrogen sulfide from hot gaseous mixtures |
US4336130A (en) * | 1980-11-28 | 1982-06-22 | Union Oil Company Of California | Desulfurization of hydrocarbons |
US4446005A (en) * | 1982-09-17 | 1984-05-01 | Exxon Research And Engineering Co. | Guard bed for the removal of sulfur and nickel from feeds previously contacted with nickel containing sulfur adsorption catalysts |
-
1986
- 1986-04-03 EP EP86302463A patent/EP0239687A1/fr not_active Ceased
Patent Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
GB1333666A (en) * | 1971-04-23 | 1973-10-10 | Kazak Khmiko T I | Method of producing polyhydric alcohols |
US4089809A (en) * | 1976-03-01 | 1978-05-16 | The United States Of America As Represented By The United States Department Of Energy | Regenerable sorbent and method for removing hydrogen sulfide from hot gaseous mixtures |
US4336130A (en) * | 1980-11-28 | 1982-06-22 | Union Oil Company Of California | Desulfurization of hydrocarbons |
US4446005A (en) * | 1982-09-17 | 1984-05-01 | Exxon Research And Engineering Co. | Guard bed for the removal of sulfur and nickel from feeds previously contacted with nickel containing sulfur adsorption catalysts |
Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
DE3822132A1 (de) * | 1987-07-02 | 1989-01-12 | Inst Francais Du Petrole | Verfahren zur entfernung von arsen und/oder phosphorverbindungen aus fluessigen kohlenwasserstoffen |
EP0412862A1 (fr) * | 1989-08-08 | 1991-02-13 | Institut Français du Pétrole | Masse de captation à base de nickel pour l'élimination de l'arsenic et du phosphore contenus dans les coupes d'hydrocarbures liquides, sa préparation et son utilisation |
FR2650759A1 (fr) * | 1989-08-08 | 1991-02-15 | Inst Francais Du Petrole | Masse de captation a base de nickel pour l'elimination de l'arsenic et du phosphore contenus dans les coupes d'hydrocarbures liquides, sa preparation et son utilisation |
US8308848B1 (en) | 2009-11-27 | 2012-11-13 | Tda Research, Inc. | High temperature gas desulfurization sorbents |
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