CN106221734A - A kind of straight-run naphtha hydrofining technology - Google Patents

A kind of straight-run naphtha hydrofining technology Download PDF

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Publication number
CN106221734A
CN106221734A CN201610659469.5A CN201610659469A CN106221734A CN 106221734 A CN106221734 A CN 106221734A CN 201610659469 A CN201610659469 A CN 201610659469A CN 106221734 A CN106221734 A CN 106221734A
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kit
fixed bed
bed reactors
straight
hydrofining technology
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朱忠良
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Xishan Lvchun Plastic Products Factory
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Xishan Lvchun Plastic Products Factory
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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
    • C10G45/00—Refining of hydrocarbon oils using hydrogen or hydrogen-generating compounds
    • C10G45/02—Refining of hydrocarbon oils using hydrogen or hydrogen-generating compounds to eliminate hetero atoms without changing the skeleton of the hydrocarbon involved and without cracking into lower boiling hydrocarbons; Hydrofinishing
    • C10G45/04—Refining of hydrocarbon oils using hydrogen or hydrogen-generating compounds to eliminate hetero atoms without changing the skeleton of the hydrocarbon involved and without cracking into lower boiling hydrocarbons; Hydrofinishing characterised by the catalyst used
    • C10G45/06—Refining of hydrocarbon oils using hydrogen or hydrogen-generating compounds to eliminate hetero atoms without changing the skeleton of the hydrocarbon involved and without cracking into lower boiling hydrocarbons; Hydrofinishing characterised by the catalyst used containing nickel or cobalt metal, or compounds thereof
    • C10G45/08—Refining of hydrocarbon oils using hydrogen or hydrogen-generating compounds to eliminate hetero atoms without changing the skeleton of the hydrocarbon involved and without cracking into lower boiling hydrocarbons; Hydrofinishing characterised by the catalyst used containing nickel or cobalt metal, or compounds thereof in combination with chromium, molybdenum, or tungsten metals, or compounds thereof
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J29/00—Catalysts comprising molecular sieves
    • B01J29/03—Catalysts comprising molecular sieves not having base-exchange properties
    • B01J29/0308—Mesoporous materials not having base exchange properties, e.g. Si-MCM-41
    • B01J29/0341—Mesoporous materials not having base exchange properties, e.g. Si-MCM-41 containing arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2229/00—Aspects of molecular sieve catalysts not covered by B01J29/00
    • B01J2229/10—After treatment, characterised by the effect to be obtained
    • B01J2229/18—After treatment, characterised by the effect to be obtained to introduce other elements into or onto the molecular sieve itself
    • B01J2229/183—After treatment, characterised by the effect to be obtained to introduce other elements into or onto the molecular sieve itself in framework positions
    • 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
    • C10G2300/20—Characteristics of the feedstock or the products
    • C10G2300/201—Impurities
    • C10G2300/202—Heteroatoms content, i.e. S, N, O, P
    • 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
    • C10G2300/70—Catalyst aspects

Abstract

The invention discloses a kind of straight-run naphtha hydrofining technology, described technique uses fixed bed reactors, is filled with hydrogenation desulfurization and denitrogenation catalyst in fixed bed reactors, and described catalyst includes carrier and active component；Described carrier is incorporation hetero atom Cu in synthetic bone shelf structure2+KIT 1；Described active component is nitridation two molybdenum MO2N, tungsten nitride W2N, molybdenum carbide Mo2C and the mixture of tungsten carbide wc；The reaction condition of described fixed bed reactors is: reaction temperature is 250 300 DEG C, and hydrogen dividing potential drop is 1.5 2.0MPa, hydrogen to oil volume ratio 80 150, volume space velocity 9 14h‑1.Straight-run naphtha total sulfur content can be controlled less than 0.5ppm by this technique.

Description

A kind of straight-run naphtha hydrofining technology
Technical field
The present invention relates to straight-run naphtha hydrodesulfurization process for refining, be specifically related to a kind of use special catalyst to carry out Straight-run naphtha hydrofining technology.
Background technology
Petroleum (chemical industry light oil) is all a kind of main raw material in oil refining and petroleum chemical industry.Petroleum is a kind of Do the refinery less than 200-250 DEG C once or the petroleum distillate of secondary operations gained, be typically derived from refinery's atmospheric and vacuum distillation Straight-run naphtha and refinery catalytic cracking, be hydrocracked, coking plant secondary operations Petroleum, some condensates are also a kind of Naphtha cut.Here it should be stressed that because Chinese Crude Oils is generally laid particular stress on, its straight-run naphtha ends content is the lowest, so Making good use of secondary operations Petroleum as petrochemical material is a critically important problem, the most also pays much attention to the degree of depth of crude oil Processing, gained secondary Petroleum is used as petroleum products blending component, replaces the raw material for petrochemical industry industry by many refineries.Therefore, First oil refining, petrochemical industry resource over all Integration are the integrated of Petroleum (including secondary operations Petroleum).
The purposes of Petroleum is many, is the primary raw material manufacturing clean gasoline, at oil in terms of petroleum refining Chemical industry aspect is to manufacture ethylene, aromatic hydrocarbons/polyester, synthesis ammonia/chemical fertilizer and the raw material of hydrogen manufacturing.In terms of quantitative relation, Petroleum makes Maximum for the quantity of oil product, secondly, aromatic hydrocarbons is less for feed ethylene.Oil product, feed ethylene, aromatic hydrocarbons material three substantially quantity ratio in the world Example is: 6.82:1:0.36.
And in an important use of straight-run naphtha, such as time as reforming raw oil, due to reforming catalyst pair Sulfur poisoning, it is therefore necessary to the sulfur content in raw material is reduced to below 0.5ppm.
Along with heaviness, the in poor quality of world's crude oil are deepened day by day, crude oil sulfur content is more and more higher, and the lightweight of high-quality is former Oil is constantly reducing.The crude oil of refinery's processing in recent years mostly is imported crude oil, and relative density increases year by year, in several years of the beginning of this century The average density of whole world refinery processing crude oil rises to about 0.8633.The problem that sulfur content is high is the most extremely serious, the current world The yield of upper sour crude oil and sour crude accounts for more than the 75% of world's crude oil total output.20th century the mid-90 whole world refinery The crude oil average sulfur content of processing is 0.9%, and the beginning of this century has increased to 1.6%.
But existing straight-run naphtha hydrofining technology for be all low sulfur product, treat with Venezuelan crude (oil) The straight-run naphtha produced for the sour crude represented, sulfur content is too high, causes desulphurizing ability limited, and catalysqt deactivation is fast. The most how straight-run naphtha process for refining is provided, can effectively the sulfur content in high-sulfur straight-run naphtha be controlled at 0.5ppm Hereinafter, to meet burning and exhausting standard, it it is a difficult problem facing of this area.
Summary of the invention
It is an object of the invention to propose a kind of straight-run naphtha hydrodesulfurization process for refining, this technique can be by straight run stone Total sulfur content in cerebrol is reduced to below 0.5ppm, to meet following process requirement and to meet burning and exhausting standard.
For reaching this purpose, the present invention by the following technical solutions:
A kind of straight-run naphtha hydrofining technology, described technique uses fixed bed reactors, fills in fixed bed reactors Being filled with hydrogenation catalyst, described catalyst includes carrier and active component.
Described carrier is incorporation hetero atom Cu in synthetic bone shelf structure2+KIT-1.
Described active component is nitridation two molybdenum MO2N, tungsten nitride W2N, molybdenum carbide Mo2C and the mixture of tungsten carbide wc.
The reaction condition of described fixed bed reactors is: reaction temperature is 250-300 DEG C, and hydrogen dividing potential drop is 1.5-2.0MPa, Hydrogen to oil volume ratio 80-150, volume space velocity 9-14h-1。
High-sulfur straight-run naphtha of the present invention refers to the straight-run naphtha that sulfur content is more than 1000ppm, such as breathes out The smooth straight-run naphtha of saxophone, its sulfur content is up to 2400ppm.
KIT-1 molecular sieve has one-dimensional channels and crosses each other to form three-dimensional disordered structure, and this structure is conducive to catalysis, absorption During material transmission.Pure silicon mesopore molecular sieve KIT-1 has heat stability more more preferable than MCM-241, HMS and hydrothermally stable Property.The present invention through in numerous mesoporous materials, such as KIT-1, KIT-6, MCM-22, MCM-36, MCM-48, MCM-49, MCM56 etc., carry out contrast test selection, find that only KIT-1 can reach the goal of the invention of the present invention, and other mesoporous materials are all Having such-and-such defect, there is the technical difficulty being difficult to overcome when being applied in the present invention, therefore the present invention selects to use KIT-1 is as carrier basis.
Although pure silicon KIT-1 mesopore molecular sieve hydro-thermal performance is outstanding, but inventor's research is later discovered that, it adds Hetero atom or surface are after chemical modification, and its hydrothermal stability obtains bigger raising.Therefore, it is modified by the present invention, with Increase its catalysis activity.The approach that KIT-1 mesopore molecular sieve is modified is by the present invention: to the total silicon KIT-1 mesoporous molecular of finished product Sieve inner surfaces of pores introduces Cu2+, this approach can be exchanged Cu by ion2+It is supported on the inner surface of KIT-1, thus Improve catalysis activity, absorption and the Thermodynamically stable performance etc. of KIT-1 mesopore molecular sieve on the whole.
Although the method being modified KIT-1 mesopore molecular sieve or approach are a lot, inventor finds, the catalysis of the present invention Agent can only use doping Cu2+KIT-1 as carrier could realize sulfur content control effect, inventor has attempted in KIT-1 Doping: Al3+、Fe3+、Zn2+、Ga3+In the ion at generation anionic surface center, find all to realize described effect.Although institute State mechanism current and unclear, but this have no effect on the enforcement of the present invention, inventor according to well-known theory with it is experimentally confirmed that its with Cooperative effect is there is between the active component of the present invention.
Described Cu2+Doping in KIT-1 must control within specific content range, and its doping is with weight Meter, for the 0.56%-0.75% of KIT-1 weight, such as 0.57%, 0.58%, 0.59%, 0.6%, 0.61%, 0.62%, 0.63%, 0.64%, 0.65%, 0.66%, 0.67%, 0.68%, 0.69%, 0.7%, 0.71%, 0.72%, 0.73%, 0.74 etc..
Inventor finds, outside this range, can cause drastically reducing of straight-run naphtha desulfurized effect.More pleasurable , work as Cu2+When doping in KIT-1 controls in the range of 0.63%-0.72%, its desulphurizing ability is the strongest, works as drafting With Cu2+Doping is transverse axis, and during curve chart with target desulfurized effect as the longitudinal axis, in this content range, sulfur content can control in pole Within the scope of low, its desulfurized effect produced, far beyond expection, belongs to unforeseeable technique effect.
The total content of described active component is the 1%-15% of carrier KIT-1 weight, preferably 3-12%, further preferred 5- 10%.Such as, described content can be 2%, 2.5%, 3%, 3.5%, 4%, 4.5%, 5%, 5.5%, 6%, 6.5%, 7%, 7.5%, 8%, 8.5%, 9%, 9.5%, 10%, 10.5%, 11%, 11.5%, 12%, 12.5%, 13%, 13.5%, 14%, 14.5% etc..
In the present invention, it is particularly limited to active component for nitridation two molybdenum MO2N, tungsten nitride W2N, molybdenum carbide Mo2C and tungsten carbide wc Mixed proportion, inventor find, the effect that different mixed proportions reaches is entirely different.Inventor finds, nitrogenizes two molybdenums MO2N, tungsten nitride W2N, molybdenum carbide Mo2The mixed proportion (mol ratio) of C and tungsten carbide wc is 1:(0.4-0.6): (0.28- 0.45): (0.8-1.2), nitridation two molybdenum MO are only controlled2N, tungsten nitride W2N, molybdenum carbide Mo2The mol ratio of C and tungsten carbide wc exists In the range of Gai, sulfur content in straight-run naphtha can be realized and control at below 10ppm and denitrification ability notable.It is to say, Four kinds of active components of the present invention are only 1:(0.4-0.6 in mol ratio): (0.28-0.45): time (0.8-1.2), just possess Cooperative effect.Outside this molar ratio range, or omit or replace any one component, all can not realize collaborative effect Should.
Preferably, two molybdenum MO are nitrogenized2N, tungsten nitride W2N, molybdenum carbide Mo2The mol ratio of C and tungsten carbide wc is 1:(0.45- 0.5): (0.35-0.45): (0.8-1.0), more preferably 1:(0.45-0.48): (0.4-0.45): (0.9-1.0), Preferably 1:0.48:0.42:0.95.
The preparation method of described catalyst can take infusion process and other alternative methods, the people in the art of routine The prior art unrestricted choice that member can grasp according to it, the present invention repeats no more.The typical but non-limiting example of the present invention As follows:
Sodium silicate, cetyl trimethylammonium bromide (CTAB), sodium ethylene diamine tetracetate (EDTA) and distilled water are massaged You mix the ratio than 1:0.25:1:60, load with in teflon-lined autoclave pressure, after stirring under 373K Constant temperature 24h, the pH of re-adjustments mixture are 10.5, after constant temperature 4 times, take out product, with distilled water cyclic washing to filtrate PH=7, then under 373K, constant temperature overnight, obtains the KIT-1 with surfactant.KIT-1 with surfactant is existed Roasting 1.5h under 523K, then roasting 6h in air atmosphere under 813K, obtains KIT-1 powder body.By this powder body 0.1mol/L Salpeter solution carry out pickling (control solid-to-liquid ratio is 1:10), under room temperature stir 0.5h, filter, be washed with distilled water to filtrate Dry under pH=7,373K and obtain matrix KIT-1 molecular sieve.
Preferably, the reaction condition of described fixed bed reactors is: reaction temperature is 260-280 DEG C, and hydrogen dividing potential drop is 1.8- 2.0MPa, hydrogen to oil volume ratio 100-150, volume space velocity 9-12h-1。
Preferably, described technological process includes, raw material, after filter, surge tank, is pumped into heat exchanger by feed pump and become Product heat exchange, is mixed to form hydrogen oil mixture, again enters heating furnace with after product heat exchange with recycle hydrogen and new hydrogen after heat exchange, Being heated to reaction temperature and enter hydrofining reactor (fixed bed reactors), hydrogen oil mixture is made at catalyst in the reactor Under with, carrying out the reaction such as hydrodesulfurization, denitrogenation, product is through heat exchange more water cooled to predetermined temperature, enters high pressure and separates Device, high-pressure separator top gas phase returns recycle hydrogen surge tank as recycle hydrogen, and oil phase enters low pressure separator, low pressure separator The generation oil that bottom is drawn enters stripper after product heat exchange, and tower top oil gas enters separatory tank after air cooling, water-cooled and obtains To lighter hydrocarbons, stripping tower bottom obtains straight-run naphtha.
Preferably, described fixed bed reactors include 1-5 beds, further preferred 2-3 beds.
The hydrofining technology of the present invention is by choosing specific catalyst, and described catalyst is by mixing hetero atom Cu2+ KIT-1 as carrier, and choose the nitridation two molybdenum MO of special ratios2N, tungsten nitride W2N, molybdenum carbide Mo2C and tungsten carbide wc As active component so that this catalyst produces cooperative effect, and the hydrodesulfurization to straight-run naphtha can control at total sulfur content Less than 0.5ppm, the total nitrogen content in straight-run naphtha is controlled within 10ppm simultaneously.
Detailed description of the invention
The hydrofining technology of the present invention is illustrated by the present invention by following embodiment.
Embodiment 1
Preparing catalyst by infusion process, carrier is doping Cu2+KIT-1, Cu2+Doping control in KIT-1 System is at the 0.65% of carrier quality.Described active component nitrogenizes two molybdenum MO2N, tungsten nitride W2N, molybdenum carbide Mo2C and tungsten carbide wc Total content is the 10% of carrier quality, and its mol ratio is 1:0.4:0.3:0.8.
Described Catalyst packing enters fixed bed reactors, and the reaction tube of described reactor is by the stainless steel of internal diameter 50mm Become, beds is set to 3 layers, reaction bed temperature with UGU808 type temp controlled meter measure, raw material straight-run naphtha by The double plunger micro pump that Beijing Satellite Manufacturing Factory manufactures carries continuously, and hydrogen is supplied by gas cylinder and uses Beijing Sevenstar-HC D07-11A/ZM mass-flow gas meter coutroi velocity, loaded catalyst is 2kg.Reacted product cools down through water-bath room temperature Laggard row gas-liquid separation.
Raw materials used for Kazakhstan's straight-run naphtha, its sulfur content is up to 2400ppm.
Controlling reaction condition is: temperature 270 DEG C, hydrogen dividing potential drop 2.0MPa, hydrogen to oil volume ratio 150, volume space velocity 10h-1。
Testing final product, total sulfur content is reduced to 0.4ppm.
Embodiment 2
Preparing catalyst by infusion process, carrier is doping Cu2+KIT-1, Cu2+Doping control in KIT-1 System is at the 0.7% of carrier quality.Described active component nitrogenizes two molybdenum MO2N, tungsten nitride W2N, molybdenum carbide Mo2C and tungsten carbide wc Total content is the 10% of carrier quality, and its mol ratio is 1:0.6:0.45): 1.2.
Remaining condition is same as in Example 1.
Testing final product, total sulfur content is reduced to 0.3ppm.
Comparative example 1
The carrier of embodiment 1 is replaced with γ-Al2O3, remaining condition is constant.
Testing final product, total sulfur content is reduced to 21ppm.
Comparative example 2
The carrier of embodiment 1 is replaced with unadulterated KIT-1, and remaining condition is constant.
Testing final product, total sulfur content is reduced to 26ppm.
Comparative example 3
Cu by embodiment 12+Replace with Zn2+, remaining condition is constant.
Testing final product, total sulfur content is reduced to 19ppm.
Comparative example 4
By the Cu in embodiment 12+Doping in KIT-1 controls at the 0.5% of carrier quality, and remaining condition is constant.
Testing final product, total sulfur content is reduced to 14ppm.
Comparative example 5
By the Cu in embodiment 12+Doping in KIT-1 controls at the 0.8% of carrier quality, and remaining condition is constant.
Testing final product, total sulfur content is reduced to 18ppm.
Embodiment 1 shows with comparative example 1-5, certain content scope that the application uses and certain loads metal ion KIT-1 carrier, when replacing with other known carriers of this area, or carrier is identical but Cu2+During doping difference, all reach not To the technique effect of the present invention, the therefore Cu of the certain content scope of the present invention2+Doping KIT-1 carrier and other components of catalyst Between possess cooperative effect, described hydrofining technology creates unforeseeable technique effect.
Comparative example 6
Omit the MO in embodiment 12N, remaining condition is constant.
Testing final product, total sulfur content is reduced to 21ppm.
Comparative example 7
Omitting the WC in embodiment 1, remaining condition is constant.
Testing final product, total sulfur content is reduced to 22ppm.
Above-described embodiment and comparative example 6-7 explanation, several active component of catalyst of the hydrofining technology of the present invention it Between there is specific contact, be omitted or substituted one of which or several, all can not reach the certain effects of the application, it was demonstrated that it produces Give birth to cooperative effect.
Applicant states, the present invention illustrates the technique of the present invention by above-described embodiment, but the invention is not limited in Above-mentioned technique, does not i.e. mean that the present invention has to rely on above-mentioned detailed catalysts and could implement.Those of skill in the art Member is it will be clearly understood that any improvement in the present invention, and the equivalence of raw material each to product of the present invention is replaced and the interpolation of auxiliary element, tool Body way choice etc., within the scope of all falling within protection scope of the present invention and disclosure.

Claims (6)

1. a high-sulfur straight-run naphtha hydrofining technology, described technique uses fixed bed reactors, in fixed bed reactors Being filled with hydrogenation catalyst, described catalyst includes carrier and active component, it is characterised in that
Described carrier is incorporation hetero atom Cu in synthetic bone shelf structure2+KIT-1,
Described active component is nitridation two molybdenum MO2N, tungsten nitride W2N, molybdenum carbide Mo2C and the mixture of tungsten carbide wc,
The reaction condition of described fixed bed reactors is: reaction temperature is 250-300 DEG C, and hydrogen dividing potential drop is 1.5-2.0MPa, hydrogen oil Volume ratio 80-150, volume space velocity 9-14h-1。
2. hydrofining technology as claimed in claim 1, it is characterised in that hetero atom Cu2+Doping be KIT-1 weight 0.63%-0.72%.
3. hydrofining technology as claimed in claim 1, it is characterised in that the total content of described active component is carrier KIT- The 3-12% of 1 weight, preferably 5-10%.
4. hydrofining technology as claimed in claim 1, it is characterised in that nitrogenize two molybdenum MO2N, tungsten nitride W2N, molybdenum carbide Mo2The mol ratio of C and tungsten carbide wc is 1:(0.45-0.5): (0.35-0.45): (0.8-1.0), more preferably 1: (0.45-0.48): (0.4-0.45): (0.9-1.0), most preferably 1:0.48:0.42:0.95.
5. hydrofining technology as claimed in claim 1, it is characterised in that the reaction condition of described fixed bed reactors is: Reaction temperature is 260-280 DEG C, and hydrogen dividing potential drop is 1.8-2.0MPa, hydrogen to oil volume ratio 100-150, volume space velocity 9-12h-1。
6. hydrofining technology as claimed in claim 1, it is characterised in that described fixed bed reactors include 1-5 catalysis Agent bed, preferably includes 2-3 beds.
CN201610659469.5A 2016-08-11 2016-08-11 A kind of straight-run naphtha hydrofining technology Pending CN106221734A (en)

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Application publication date: 20161214