CN104031679A - Method for production of olefin and aromatic hydrocarbon from naphtha - Google Patents

Method for production of olefin and aromatic hydrocarbon from naphtha Download PDF

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Publication number
CN104031679A
CN104031679A CN201310069505.9A CN201310069505A CN104031679A CN 104031679 A CN104031679 A CN 104031679A CN 201310069505 A CN201310069505 A CN 201310069505A CN 104031679 A CN104031679 A CN 104031679A
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petroleum naphtha
oil
naphthenic hydrocarbon
quality
extraction
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CN201310069505.9A
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CN104031679B (en
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马爱增
田龙胜
龙军
王杰广
唐文成
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Sinopec Research Institute of Petroleum Processing
China Petroleum and Chemical Corp
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Sinopec Research Institute of Petroleum Processing
China Petroleum and Chemical Corp
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Priority to CN201310069505.9A priority Critical patent/CN104031679B/en
Priority to TW103107242A priority patent/TWI544068B/en
Priority to RU2014108327A priority patent/RU2615160C2/en
Priority to KR1020140026118A priority patent/KR101760356B1/en
Publication of CN104031679A publication Critical patent/CN104031679A/en
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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
    • 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
    • C10G61/04—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 an extraction
    • 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
    • C10G57/00—Treatment of hydrocarbon oils, in the absence of hydrogen, by at least one cracking process or refining process and at least one other conversion process
    • 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
    • C10G63/00—Treatment of naphtha by at least one reforming process and at least one other conversion process
    • C10G63/06—Treatment of naphtha by at least one reforming process and at least one other conversion process plural parallel stages only
    • C10G63/08—Treatment of naphtha by at least one reforming process and at least one other conversion process plural parallel stages only including at least one cracking step

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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)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)

Abstract

The invention relates to a method for production of olefin and aromatic hydrocarbon from naphtha. The method comprises the steps of: (1) subjecting the naphtha to extraction separation so as to obtain raffinate oil containing alkane and cycloalkane and extract oil containing cycloalkane and aromatic hydrocarbon, with the mass ratio of cycloalkane contained in the raffinate oil to cycloalkane contained in naphtha being 4-40%, (2) contacting the extract oil rich in aromatic hydrocarbon with a reforming catalyst to undergo catalytic reforming reaction under the condition of 0.2-3.0MPa, 300-550DEG C, a hydrogen/hydrocarbon mole ratio of 0.5-20, and a volume space velocity of 0.1-50h<-1>, thus obtaining reformate rich in aromatic hydrocarbon, and (3) subjecting the raffinate oil rich in alkane and cycloalkane to cracking reaction so as to generate olefin. The method adopts naphtha as the raw material and can produce a lot of light olefin and light aromatic hydrocarbon.

Description

A kind of method of being produced alkene and aromatic hydrocarbons by petroleum naphtha
Technical field
The present invention is a kind of combination process, specifically, is a kind of method taking petroleum naphtha as raw material production light olefin and light aromatics.
Background technology
Catalytic reforming and steam cracking are the industrialization technologies of petrochemical industry maturation, and the main purpose of catalytic reforming is to produce aromatic hydrocarbons, stop bracket gasoline and hydrogen.In catforming process, several competing reactions can occur simultaneously, these reactions comprise that cyclohexane dehydrogenation generates aromatic hydrocarbons, alkyl cyclopentane dehydroisomerization turns to aromatic hydrocarbons, paraffin dehydrogenation is cyclized into aromatic hydrocarbons, paraffinic hydrocarbons hydrocracking changes into the light hydrocarbon product outside gasoline boiling range, the isomerization of the de-alkyl of alkylbenzene and paraffinic hydrocarbons.In order to obtain high octane value gasoline blending component or aromatic hydrocarbons, not only wish that naphthenic hydrocarbon dehydrocyclization becomes aromatic hydrocarbons, to make to greatest extent paraffinic hydrocarbons transform simultaneously, increase the output of aromatic hydrocarbons.
Petroleum naphtha catalytic reforming is during for the production of aromatic hydrocarbons, due in aromatic hydrocarbons except being worth higher BTX(benzene, toluene and dimethylbenzene) light aromatics, also contain the lower C of value of significant proportion 9 +heavy arene.The main purpose of steam cracking is to produce ethene, propylene and divinyl.Along with the increase of Chemical market to propylene and the divinyl market requirement.How to be the problem that people are very concerned about from limited naphtha resource volume increase BTX light aromatics, propylene and divinyl.
The raw material of catalytic reforming is petroleum naphtha, and petroleum naphtha is also the main ingredient that steam cracking device raw material forms simultaneously.Along with the change weight of crude oil, naphtha yield reduces, and the continuous increase of the whole world to light olefin and aromatic hydrocarbons demand, and the problem that catalytic reforming and steam cracking device are contended over raw materials is outstanding all the more.
The mixture that petroleum naphtha is made up of hydrocarbons such as normal paraffin, isoparaffin, naphthenic hydrocarbon and aromatic hydrocarbons.Normal paraffin is than isoparaffin and naphthenic hydrocarbon, the yield that ethene is produced in cracking is high, when naphthenic hydrocarbon cracking, there is relatively high propylene and divinyl productive rate, and the phenyl ring of aromatic hydrocarbons is relatively difficult to cracking under typical cracking condition, and the generation of ethene is not almost contributed; But naphthenic hydrocarbon is easy to be converted into aromatic hydrocarbons under catalytic reforming condition, it is the catalytic reforming raw material of high-quality.Therefore raw material, how to optimize catalytic reforming and steam cracking device is that people are very concerned about and problem demanding prompt solution.
From petroleum naphtha, the method for separation of alkane and aromatic hydrocarbons has fractionation by adsorption and extracting and separating.
Fractionation by adsorption can be separated normal paraffin from stone brain.As CN1476474A discloses the ethylene production by steam cracking of normal paraffins, first petroleum naphtha is fractionated into C 5alkane hydrocarbon stream and C 6～C 9hydrocarbon stream, by C 6～C 9hydrocarbon stream carries out fractionation by adsorption, optionally adsorbs normal paraffin, then the C that fractionation is obtained 5alkane hydrocarbon stream is as strippant, by the normal paraffin in desorption liquid and C 5after paraffinic hydrocarbons separates, pass into steam cracking district and produce ethene, inhale excess oil and pass into reformer section production stop bracket gasoline.
CN101198574A discloses the ethylene production of normal paraffin steam cracking, by C 5～C 9hydrocarbon carry out fractionation by adsorption, normal paraffin is separated with non-n-alkane, use C 10～C 16hydrocarbon and composition thereof as strippant, the normal paraffin that fractionation by adsorption is gone out circulates and produces ethene into steam cracking district, non-positive structure hydrocarbon passes into reformer section and changes into aromatic hydrocarbons.
The optimization that CN1710030A discloses a kind of petroleum naphtha utilizes method, use 5A molecular sieve to carry out fractionation by adsorption to petroleum naphtha, isolate the desorption oil production that is rich in positive structure hydrocarbon and the residual oil absorber that is rich in non-positive structure hydrocarbon, in desorption oil, the content of positive structure hydrocarbon is 80～100 % by weight.Steam crack material using desorption oil as high-quality or cut into close-cut fraction by rectifying and then produce reagent and high-quality solvent oil product, inhales catalytic reforming raw material or the clean gasoline with high octane blend component of excess oil as high-quality.
CN1292050C disclose a kind of from full fraction naphtha the method for separating normal alkane, first the aromatic hydrocarbons in full fraction naphtha is removed from raw material with adsorption method of separation, then the normal paraffin in the full fraction naphtha after de-aromatic hydrocarbons is separated with non-n-alkane with adsorption method of separation.The component that is rich in normal paraffin after fractionation by adsorption in naphtha fraction can be used as the charging of steam cracking device, improves the yield of ethene of steam cracking device; The component that is rich in isoparaffin can be used as the raw material of catalytic reforming unit, increases reformed gasoline or aromatics yield; The component that is rich in aromatic hydrocarbons can be used as the charging of coking or reformer.In addition, two kinds of fractionation by adsorption of the present invention have all been selected effective desorbing agent, can make to adsorb the sorbent material effective regeneration after saturated, re-use.
CN1277907C discloses a kind of petroleum naphtha recombinant processing method, comprises the steps: that (1) first carry out extracting and separating by petroleum naphtha, isolates and raffinates oil and extract oil out; (2) raffinate oil and enter ethene steam cracking device; (3) extract oil out and enter reformer reformation.This invention extracting and separating used is actually liquid-liquid extraction, in given embodiment, solvent ratio taking tetramethylene sulfone as extraction solvent as 11,95～128 DEG C of service temperatures, working pressure 0.6～1.0MPa, pressing given operating parameters can only separate alkane with aromatic hydrocarbons, its main ingredient in raffinating oil is alkane.
In above-mentioned adsorption separation technology, although can improve yield of ethene using normal paraffin as steam crack material, because normal paraffin content in petroleum naphtha is lower, while obtaining identical ethylene yield, the demand of petroleum naphtha is increased considerably.Above-mentioned extraction and separation technology carries out petroleum naphtha after extracting and separating, obtain taking alkane as raffinating oil and the extraction oil as leading taking aromatic hydrocarbons and naphthenic hydrocarbon of leading, although what separate can improve yield of ethene using alkane as main raffinating oil as steam crack material, but heavy naphthenic hydrocarbon is not utilized effectively, cause propylene and divinyl yield to decline; And in the time that in petroleum naphtha, Determination of Alkane Content is lower, while obtaining identical triolefin output, the demand of petroleum naphtha is increased considerably.
Summary of the invention
The object of this invention is to provide is a kind of method of being produced alkene and aromatic hydrocarbons by petroleum naphtha, and this method, taking petroleum naphtha as raw material, can be produced more light olefin and light aromatics.
Method of being produced alkene and aromatic hydrocarbons by petroleum naphtha provided by the invention, comprises the steps:
(1) petroleum naphtha is carried out to extracting and separating, obtain containing raffinating oil and containing the extraction oil of naphthenic hydrocarbon and aromatic hydrocarbons of alkane and naphthenic hydrocarbon, the mass ratio of the naphthenic hydrocarbon containing in the naphthenic hydrocarbon containing in raffinating oil and petroleum naphtha is 4～40%,
(2) by the extraction oil containing naphthenic hydrocarbon and aromatic hydrocarbons 0.2～3.0MPa, 300～550 DEG C, hydrogen/hydrocarbon mol ratio 0.5～20, volume space velocity is 0.1～50h -1condition under contact and carry out catalytic reforming reaction with reforming catalyst, obtain being rich in the reformed oil of aromatic hydrocarbons,
(3) produce alkene by carrying out scission reaction containing raffinating oil of alkane and naphthenic hydrocarbon.
The inventive method is first carried out extracting and separating to petroleum naphtha, by extracting and separating by the heavy naphthenic hydrocarbon (C in petroleum naphtha 7 +naphthenic hydrocarbon) incision raffinates oil, and carries out cracking can obtain more propylene and divinyl to raffinating oil, and increases light olefin (ethene, propylene and the divinyl) output in split product, and reform and can obtain light aromatics extracting oil out.The inventive method, by the appropriate separation to aromatic hydrocarbons, naphthenic hydrocarbon and alkane, has improved the utilization ratio of petroleum naphtha.
Brief description of the drawings
Fig. 1 is that the inventive method is taking hydrofining petroleum naphtha as olefin production with the schematic flow sheet of aromatic hydrocarbons.
Fig. 2 is that the inventive method petroleum naphtha is the schematic flow sheet of olefin production and aromatic hydrocarbons.
Embodiment
Petroleum naphtha is carried out extracting and separating by the inventive method, naphthenic hydrocarbon is wherein cut, obtain extraction oil and raffinating oil containing alkane and naphthenic hydrocarbon containing naphthenic hydrocarbon and aromatic hydrocarbons, naphthenic hydrocarbon is distributed in and raffinates oil and extract out in oil with certain proportion according to the difference of carbon number, during part heavy naphthenic hydrocarbon is cut and raffinates oil, more lightweight naphthenic hydrocarbon (C 6～C 8naphthenic hydrocarbon) be cut and extract out in oil, the heavy naphthenic hydrocarbon containing in raffinating oil has increased the productive rate of propylene and divinyl in split product, and extracting the lightweight naphthenic hydrocarbon containing in oil out has increased the productive rate of light aromatics BTX in reformate.Compared with prior art, the inventive method can be converted into petroleum naphtha more light olefin (ethene, propylene and 1,3-butadiene) and light aromatics (BTX).
The inventive method (1) step is that petroleum naphtha is carried out to extracting and separating, so that naphthenic hydrocarbon is wherein cut, a part of naphthenic hydrocarbon and alkane is entered and raffinate oil, and another part naphthenic hydrocarbon and aromatic hydrocarbons enter extracts oil out.Described extraction separating method can be liquid-liquid extraction separation or extractive distillation.
(1) in step, obtain through extracting and separating raffinate oil in preferably 10～35 quality % of mass ratio of the naphthenic hydrocarbon that contains in the naphthenic hydrocarbon that contains and petroleum naphtha.In the present invention, in raffinating oil, contain less C 6～C 8naphthenic hydrocarbon, the C containing in extracting and separating gained is raffinated oil 6～C 8the C containing in naphthenic hydrocarbon and petroleum naphtha 6～C 8the mass ratio of naphthenic hydrocarbon is preferably 3～40%, and more preferably 3～30%, the C containing in raffinating oil 9 +the C containing in naphthenic hydrocarbon and petroleum naphtha 9 +the mass ratio of naphthenic hydrocarbon is preferably 1～48%.
(1) in step, can in liquid-liquid extraction tower, carry out liquid-liquid extraction to petroleum naphtha, the operational condition of liquid-liquid extraction tower is: entering the extraction solvent of liquid-liquid extraction tower and the mass ratio of petroleum naphtha is 3～8:1, and the temperature of liquid-liquid extraction tower top is 130～190 DEG C, and pressure is 1.1～2.0MPa.Also can in extraction distillation column, carry out extractive distillation to petroleum naphtha, the operational condition of extraction distillation column is: entering the extractive distillation solvent of extraction distillation column and the mass ratio of petroleum naphtha is 3～8:1, the temperature of extractive distillation tower top is 70～190 DEG C, and pressure is 0.1～0.3MPa.
In the present invention, the pressure of extraction distillation column represents by absolute pressure, and other pressure is gauge pressure.
(1) step is carried out liquid-liquid extraction or extractive distillation solvent used by petroleum naphtha and is selected from any two or more the mixture in tetramethylene sulfone, furfural, N-Methyl pyrrolidone, N-N-formyl morpholine N-, triglycol, Tetraglycol 99, five glycol, ditane, alpha-methyl-naphthalene or above-mentioned substance.If extractive distillation, extractive distillation solvent used preferably includes tetramethylene sulfone, the solubility promoter of 30～63 quality % and the water of 0.2～2.0 quality % of 35～68 quality %, and described solubility promoter is selected from alkylnaphthalene, biphenyl, ditan, diphenylethane or dialkyl benzene methane.
Particularly, the process that liquid-liquid extraction of the present invention separates is: petroleum naphtha contacts with extraction solvent liquid phase in liquid-liquid extraction tower, obtains being rich in the rich solvent of aromatic hydrocarbons and naphthenic hydrocarbon at the bottom of tower, and tower top obtains the raffinate containing alkane and naphthenic hydrocarbon.Raffinate is preferably purified in washing tower, removes residual trace solvent, obtains raffinating oil containing alkane and naphthenic hydrocarbon.The rich solvent that is rich in aromatic hydrocarbons and naphthenic hydrocarbon enters solvent recovery tower, and aromatic hydrocarbons and naphthenic hydrocarbon are discharged by reclaiming tower top, and lean solvent is discharged at the bottom of by tower, then the recycle of rework solution liquid extraction tower.
The process that extractive distillation separates is: petroleum naphtha is sent into extraction distillation column and contact under liquid phase condition with extraction solvent, utilize the solvent ultimate principle different with the impact of naphthenic hydrocarbon relative volatility on alkane, being rich in alkane and part naphthenic hydrocarbon and a small amount of solvent discharges by tower top, the rich solvent that is rich in aromatic hydrocarbons and naphthenic hydrocarbon is discharged at the bottom of by tower and is entered solvent recovery tower, aromatic hydrocarbons and naphthenic hydrocarbon are separated from solvent, and the lean solvent obtaining returns to extraction distillation column again and recycles.
Because the impurity such as the alkene containing in reforming reaction raw material, sulphur, nitrogen, arsenic, oxygen, chlorine all can have a negative impact to catalytic reforming unit and reforming catalyst, therefore catalytic reforming feedstock is carrying out before reforming reaction, preferably carry out hydrofining, make alkene generation hydrogenation wherein saturated, remove the impurity such as sulphur, nitrogen, arsenic, oxygen, chlorine simultaneously, obtain hydrofining reformer feed.
In the inventive method, (1) the extraction oil of the petroleum naphtha of step and (2) step all preferably carries out hydrofining, specifically, (1) petroleum naphtha described in step preferably carries out hydrofining before extracting and separating, or by the extraction oil described in (2) step carrying out carrying out hydrofining before reforming reaction, make olefin saturated wherein and remove impurity wherein, making refining petroleum naphtha or refining sulphur content of extracting out in oil be less than 0.5 μ g/g, nitrogen content and be less than that 0.5 μ g/g, arsenic content are less than 1.0ng/g, lead content is less than 10ng/g.
Described hydrofining reaction temperature is 260～460 DEG C, preferably 280～400 DEG C, and pressure is 1.0～8.0MPa, preferred 1.6～4.0MPa, and feed volume air speed is 1～20h -1, preferred 2～8h -1, when reaction, hydrogen/hydrocarbon volume ratio is 10～1000:1, preferred 50～600:1.
Described Hydrobon catalyst should have hydrogenation saturation of olefins, has the ability of hydrogenating desulfurization, denitrogenation and deoxidation simultaneously.Described Hydrobon catalyst comprises hydrogenation activity component, the halogen of 0.1～1.0 quality % and the inorganic oxide carrier of 50.0～94.9 quality % of 5～49 quality %, described hydrogenation activity component is selected from the oxide compound of one or more metals in Co, Ni, Fe, W, Mo, Cr, Bi, Sb, Zn, Cd, Cu, In and rare earth metal, described inorganic oxide carrier, preferential oxidation aluminium.
The inventive method (2) step is the process to carry out catalytic reforming containing the extraction oil of aromatic hydrocarbons and naphthenic hydrocarbon, preferably 0.2～2.0MPa of the pressure of catalytic reforming reaction, preferably 350～520 DEG C, more preferably 400～500 DEG C of temperature, preferably 1.0～30h of petroleum naphtha volume space velocity -1, more preferably 2.0～25.0h -1.
(2) the preferably 1～8:1 of hydrogen/hydrocarbon mol ratio of catalytic reforming reaction described in step.
Catalytic reforming of the present invention can adopt continuously (moving-bed) reformation technology, half regeneration (fixed bed) reformation technology or cyclic regeneration reformation technology.
The catalyzer that catalytic reforming described in the inventive method (2) step adopts comprises VIII family metal, the halogen of 0.01～5.0 quality % and the inorganic oxide carrier of 90.0～99.97 quality % of 0.01～5.0 quality %.
If described reforming reaction adopts moving-bed CONTINUOUS REFORMER, catalyzer preferably includes the VIII family metal of 0.01～3.0 quality %, the halogen of 0.01～5.0 quality %, the Sn of 0.01～5.0 quality %, the inorganic oxide carrier of 87.0～99.97 quality %.If adopt fixed bed half generative reforming, catalyzer preferably includes the VIII family metal of 0.01～3.0 quality %, the halogen of 0.01～5.0 quality %, the Re of 0.01～5.0 quality %, the inorganic oxide carrier of 87.0～99.97 quality %.Described Sn or Re are the second metal constituent element.
In above-mentioned CONTINUOUS REFORMER or half generative reforming catalyzer, can also comprise the 3rd metal constituent element that one or more are selected from basic metal, alkaline-earth metal, rare earth element, In, Co, Ni, Fe, W, Mo, Cr, Bi, Sb, Zn, Cd or Cu.
In above-mentioned catalyzer, the described preferred platinum of VIII family metal, inorganic oxide carrier preferential oxidation aluminium.
Described reforming catalyst adopts ordinary method preparation, first prepare shaping carrier, can be ball-type or stripe shape, and then dipping is introduced metal constituent element and halogen, if contain second, third metal constituent element in catalyzer, preferably first in carrier, introduce second, third metal constituent element, finally introduce again VIII family metal and halogen, introduce the carrier drying after metal constituent element, 450～650 DEG C of roastings obtain oxidation state reforming catalyst.Oxidation state reforming catalyst need reduce before using in 315～650 DEG C of hydrogen atmospheres, obtained reduction-state reforming catalyst, also needed to carry out prevulcanized processing for reforming Pt-Re catalyst.
The inventive method (3) step is to carry out cracking to raffinating oil, and crack reacting condition is: pressure 0.05～0.30MPa, reactant residence time 0.01～0.6 second, water/oil quality than 0.3～1.0,760～900 DEG C of pyrolyzer temperature outs.
Petroleum naphtha of the present invention is that to have ASTM D-86 initial boiling point be that 40～80 DEG C, final boiling point are the hydrocarbon mixture of 160～220 DEG C.
Described petroleum naphtha is selected from virgin naphtha, hydrocracking petroleum naphtha, coking naphtha, catalytic cracking petroleum naphtha or field condensate.
Described petroleum naphtha is containing alkane, the naphthenic hydrocarbon of 10～50 quality % and the aromatic hydrocarbons of 5～30 quality % of 30～85 quality %.C in described petroleum naphtha 6～C 8the content of naphthenic hydrocarbon is 12～20 quality %.
Further illustrate the present invention below in conjunction with accompanying drawing.
In Fig. 1, from the petroleum naphtha of pipeline 1 with mix from the hydrogen make-up of pipeline 2, then enter hydrofining reactor 3 with together with circulating hydrogen from pipeline 9.Hydrotreated product enters knockout drum 5 by pipeline 4, the isolated gas that is rich in hydrogen in knockout drum 5 tops enters recycle compressor 8 by pipeline 6 and circulates, the logistics that flow out knockout drum 5 bottoms enters rectifying tower 10 through pipeline 7, through rectifying, liquefied gas is by the pipeline 11 discharge systems on rectifying tower 10 tops, refining petroleum naphtha is flowed out by rectifying tower 10 bottoms, enters extracting and separating district 13 through pipeline 12.Extracting and separating district 13 can be liquid liquid extraction plant or extractive distillation device, through extracting and separating, alkane is separated with aromatic hydrocarbons, a part for naphthenic hydrocarbon is segregated into alkane component simultaneously, and another part segregates into aromatic component.If entering water wash column 16(extractive distillation by pipeline 14, the component that is rich in alkane and naphthenic hydrocarbon after extracting and separating can directly enter steam cracking district 22 without washing), the rear component of washing enters steam cracking district 22 by pipeline 17 and carries out steam cracking, the mixture that contains extraction solvent and water that discharge water wash column 16 bottoms is discharged by pipeline 18, can return to extracting and separating district 13 and recycle.The rich solvent containing naphthenic hydrocarbon and aromatic hydrocarbons that extracting and separating district 13 discharges enters solvent recovery tower 19 by pipeline 15 and separates solvent, and the lean solvent that solvent recovery tower 19 bottoms obtain is discharged by pipeline 21, can return to extracting and separating district 13 and recycle.The logistics containing aromatic hydrocarbons and naphthenic hydrocarbon that solvent recovery tower 19 tops obtain enters reforming reactor 23 and carries out catalytic reforming after pipeline 20 mixes with the reformation circulating hydrogen from pipeline 29.Reforming reaction product enters reformate knockout drum 25 by pipeline 24, the isolated gas that is rich in hydrogen in top is recycled through recycle compressor 28 by pipeline 26, the liquid ingredient that flow out bottom enters reformate rectifying tower 30 by pipeline 27, the liquefied gas tank that rectifying obtains is by upper pipeline 31 discharge systems, and reformed oil is discharged and entered aromatic hydrocarbons disengaging zone by bottom line 32.
Fig. 2, for first petroleum naphtha being carried out to extracting and separating, carries out hydrofining by extraction oil, then carries out the scheme of catalytic reforming.Petroleum naphtha enters extracting and separating district 13 from pipeline 1, and extracting and separating district 13 can be liquid liquid extraction plant or extractive distillation device, through extracting and separating, alkane is separated with aromatic hydrocarbons, a part for naphthenic hydrocarbon is segregated into alkane component simultaneously, and another part segregates into aromatic component.If entering water wash column 16(extractive distillation by pipeline 14, the component that is rich in alkane and naphthenic hydrocarbon after separation can directly enter steam cracking district 22 without washing), the rear component of washing enters steam cracking district 22 by pipeline 17 and carries out preparing ethylene by steam cracking, the mixture that contains extraction solvent and water that discharge water wash column 16 bottoms is discharged by pipeline 18, can return to extracting and separating district 13 and recycle.The rich solvent containing naphthenic hydrocarbon and aromatic hydrocarbons that extracting and separating district 13 discharges enters solvent recovery tower 19 by pipeline 15 and separates solvent.The lean solvent that solvent recovery tower 19 bottoms obtain is discharged by pipeline 21, can return to extracting and separating district 13 recycles, the logistics containing aromatic hydrocarbons and naphthenic hydrocarbon that solvent recovery tower 19 tops obtain, extract out oil through pipeline 20 with mix from the hydrogen make-up of pipeline 2, then enter hydrofining reactor 3 with together with circulating hydrogen from pipeline 9.Hydrotreated product enters knockout drum 5 by pipeline 4, the isolated gas that is rich in hydrogen in knockout drum 5 tops enters recycle compressor 8 by pipeline 6 and circulates, the logistics that flow out knockout drum 5 bottoms enters rectifying tower 10 through pipeline 7, through rectifying, liquefied gas is by the pipeline 11 discharge systems on rectifying tower 10 tops, the refining oil of extracting out is flowed out by rectifying tower 10 bottoms, enters reforming reactor 23 and carry out catalytic reforming after pipeline 12 mixes with the reformation circulating hydrogen from pipeline 29.Reforming reaction product enters reformate knockout drum 25 by pipeline 24, the isolated gas that is rich in hydrogen in top is recycled through recycle compressor 28 by pipeline 26, the liquid ingredient that flow out bottom enters reformate rectifying tower 30 by pipeline 27, the liquefied gas tank that rectifying obtains is by upper pipeline 31 discharge systems, and reformed oil is discharged and entered aromatic hydrocarbons disengaging zone by bottom line 32.
Further describe the present invention below by example, but the present invention is not limited to this.
Example 1
This example carries out hydrofining to petroleum naphtha.
In 20 milliliters of continuous flow reactor of fixed bed, load 20 milliliters of Hydrobon catalyst A, wherein contain NiO, the WO of 19.0 quality % of CoO, the 2.0 quality % of 0.03 quality % 3, the F of 0.7 quality % and the Al of 78.27 quality % 2o 3.
Be that 1.6MPa, hydrogen/hydrocarbon volume ratio are that 200:1, feed volume air speed are 8.0h by the petroleum naphtha of listed table 1 composition and character at 290 DEG C, hydrogen dividing potential drop -1condition under pass in the reactor of above-mentioned loading catalyst A and carry out hydrofining, reaction product enters watercooler, is separated into gas-liquid two-phase, measures respectively and carries out compositional analysis, refining after the composition of gained petroleum naphtha and character in table 2.
Table 1
Table 2
As seen from the results in Table 2, after hydrofining, the alkene in petroleum naphtha, sulphur, nitrogen, arsenic, lead content all reach the charging requirement of catalytic reforming reaction.
Example 2
By the inventive method, refining petroleum naphtha is carried out to extracting and separating.
Taking tetramethylene sulfone as solvent, adopt liquid-liquid extraction separation method, by listed table 2 petroleum naphtha with double centner/hour flow in liquid-liquid extraction tower, contact with tetramethylene sulfone, solvent/raw materials quality ratio is 5, liquid-liquid extraction tower top pressure 1.2MPa, reflux ratio is 0.25, and liquid-liquid extraction column overhead temperature is 140 DEG C.From obtaining being rich in the rich solvent of naphthenic hydrocarbon and aromatic hydrocarbons at the bottom of liquid-liquid extraction tower, tower top obtains being rich in the raffinate of alkane and naphthenic hydrocarbon.Be rich in the rich solvent of naphthenic hydrocarbon and aromatic hydrocarbons after fractionation by distillation tetramethylene sulfone, obtain being rich in the extraction oil of naphthenic hydrocarbon and aromatic hydrocarbons.Raffinate removes residual trace solvent through washing, obtains being rich in raffinating oil of alkane and naphthenic hydrocarbon.The allocation proportion of extraction flow, group composition and the various hydro carbons of extracting oil out and raffinate oil in extracting oil out and raffinating oil is in table 3.
Example 3
Taking five glycol as solvent, adopt liquid-liquid extraction separation method, by listed table 2 petroleum naphtha with double centner/hour flow in liquid-liquid extraction tower, contact with five glycol, solvent/raw materials quality ratio is 7, liquid-liquid extraction tower top pressure 0.8MPa, reflux ratio is 0.2,150 DEG C of liquid-liquid extraction column overhead temperature.From obtaining being rich in the rich solvent of naphthenic hydrocarbon and aromatic hydrocarbons at the bottom of liquid-liquid extraction tower, tower top obtains being rich in the raffinate of alkane and naphthenic hydrocarbon.Be rich in the rich solvent of naphthenic hydrocarbon and aromatic hydrocarbons after fractionation by distillation five glycol, obtain being rich in the extraction oil of naphthenic hydrocarbon and aromatic hydrocarbons.Raffinate removes residual trace solvent through washing, obtains being rich in raffinating oil of alkane and naphthenic hydrocarbon.The allocation proportion of extraction flow, group composition and the various hydro carbons of extracting oil out and raffinate oil in extracting oil out and raffinating oil is in table 3.
Example 4
Taking the mixture of tetramethylene sulfone, the ditane of 49.8 quality % and the water of 0.2 quality % that consists of 50 quality % as solvent, adopt extractive distillation separation method, by listed table 2 petroleum naphtha with double centner/hour flow in extraction distillation column, contact and carry out extractive distillation and separate with mixed solvent, solvent/raw materials quality ratio is 3.5, extractive distillation tower top pressure 0.15MPa, reflux ratio is 0.25, and extractive distillation tower top temperature is 100 DEG C.From obtaining being rich in the rich solvent of naphthenic hydrocarbon and aromatic hydrocarbons at the bottom of extraction distillation column, tower top obtains being rich in raffinating oil of alkane and naphthenic hydrocarbon.Be rich in the rich solvent of naphthenic hydrocarbon and aromatic hydrocarbons after fractionation by distillation mixed solvent, obtain being rich in the extraction oil of naphthenic hydrocarbon and aromatic hydrocarbons.The allocation proportion of extraction flow, group composition and the various hydro carbons of extracting oil out and raffinate oil in extracting oil out and raffinating oil is in table 3.
Comparative example 1
By listed table 2 petroleum naphtha with double centner/hour feed rate by CN1277907C example 3(taking tetramethylene sulfone as solvent) method carry out liquid-liquid extraction aromatics separation and alkane, what obtain is rich in raffinating oil and being rich in the extraction oil of aromatic hydrocarbons of alkane, extract oil out and extraction flow, group composition and the various hydro carbons of the raffinating oil allocation proportion in extracting oil out and raffinating oil in table 3.
Table 3
As shown in Table 3, comparative example 1, after aromatic hydrocarbons separates, is mainly alkane in raffinating oil, and extracts out in oil and is mainly naphthenic hydrocarbon and aromatic hydrocarbons, and during the naphthenic hydrocarbon in petroleum naphtha has 3.62 quality % to enter to raffinate oil, 96.16 quality % enter and extract out in oil, the C in petroleum naphtha 6～C 8during naphthenic hydrocarbon has 3.01 quality % to enter to raffinate oil, 96.99 quality % enter and extract out in oil, the C in petroleum naphtha 9 +during naphthenic hydrocarbon has 5.02 quality % to enter to raffinate oil, 94.98 quality % enter and extract out in oil, and during the aromatic hydrocarbons in petroleum naphtha has 9.59 quality % to enter to raffinate oil, 90.25 quality % enter and extract out in oil.
Adopt liquid-liquid extraction at the inventive method example 2, during the naphthenic hydrocarbon in petroleum naphtha has 33.77 quality % to enter to raffinate oil, 66.23 quality % enter and extract out in oil, the C in petroleum naphtha 6～C 8during naphthenic hydrocarbon has 28.10 quality % to enter to raffinate oil, 71.90 quality % enter and extract out in oil, the C in petroleum naphtha 9 +during naphthenic hydrocarbon has 46.83 quality % to enter to raffinate oil, 53.17 quality % enter and extract out in oil, and during the aromatic hydrocarbons in petroleum naphtha has 0.49 quality % to enter to raffinate oil, 99.51 quality % enter and extract out in oil.
Example 3 adopts liquid-liquid extraction, and during the naphthenic hydrocarbon in petroleum naphtha has 10.64 quality % to enter to raffinate oil, 89.36 quality % enter and extract out in oil, the C in petroleum naphtha 6～C 8during naphthenic hydrocarbon has 6.33 quality % to enter to raffinate oil, 93.67 quality % enter and extract out in oil, the C in petroleum naphtha 9 +during naphthenic hydrocarbon has 40 quality % to enter to raffinate oil, 60 quality % enter and extract out in oil, and during the aromatic hydrocarbons in petroleum naphtha has 1.71 quality % to enter to raffinate oil, 98.29 quality % enter and extract out in oil.
Example 4 adopts extractive distillation, and during the naphthenic hydrocarbon in petroleum naphtha has 10 quality % to enter to raffinate oil, 90 quality % enter and extract out in oil, the C in petroleum naphtha 6～C 8during naphthenic hydrocarbon has 19 quality % to enter to raffinate oil, 81 quality % enter and extract out in oil, the C in petroleum naphtha 9 +during naphthenic hydrocarbon has 1.00 quality % to enter to raffinate oil, 99.00 quality % enter and extract out in oil, and during the aromatic hydrocarbons in petroleum naphtha has 0.8 quality % to enter to raffinate oil, 99.2 quality % enter and extract out in oil.
Example 5
The steam cracking effect of raffinating oil of alkane and naphthenic hydrocarbon is carried out gained after extracting and separating and is rich in this example explanation by the inventive method.
Get the listed petroleum naphtha double centner of table 2, carry out extracting and separating by the method for example 2, gained is raffinated oil as steam crack material.Steam cracking reaction condition is: pyrolyzer top hole pressure 0.185MPa, 0.20 second residence time, water/oil quality than 0.55,840 DEG C of pyrolyzer temperature outs, selectivity of light olefin hydrocarbon and output are in table 4.
Comparative example 2
Get the listed petroleum naphtha double centner of table 2, carry out aromatic hydrocarbons extraction by the method for comparative example 1, using raffinating oil as steam crack material of obtaining, steam cracking reaction condition is: pyrolyzer top hole pressure 0.185MPa, 0.20 second residence time, water/oil quality than 0.55,840 DEG C of pyrolyzer temperature outs, selectivity of light olefin hydrocarbon and output are in table 4.
Table 4
Triolefin is ethene, propylene and divinyl
As shown in Table 4, than comparative example, to carry out by obtaining raffinating oil after the inventive method extracting and separating steam cracking, triolefin yield reaches 62.52 quality %, triolefin yield has improved 3.78%, and wherein propene yield has improved 10.67%, and divinyl yield has improved 16.64%, raffinating oil as steam crack material that extracting and separating of the present invention is obtained is described, is more conducive to propylene enhancing and divinyl.
Example 6
The effect of alkene and aromatic hydrocarbons is produced in the explanation of this example by petroleum naphtha by the inventive method.
Get the listed petroleum naphtha double centner of table 2, carry out extracting and separating by the method for example 2, gained is raffinated oil as steam crack material.Steam cracking reaction condition is: pyrolyzer top hole pressure 0.185MPa, 0.20 second residence time, water/oil quality than 0.55,840 DEG C of pyrolyzer temperature outs, light olefins production is in table 5.
Extract gained out oil as catalytic reforming charging, adopt PtSn/ γ-Al 2o 3catalyst B is wherein γ-Al containing Pt0.35 quality %, Sn0.30 quality %, Cl1.0 quality %, surplus 2o 3.In 100 milliliters of continuous flow reactor of fixed bed, load 50 milliliters of catalyst B, be that 514 DEG C, reaction pressure are that 0.34MPa, hydrogen/hydrocarbon mol ratio are 2.5, feed volume air speed is 2.0h in reaction mass temperature in -1condition under carry out catalytic reforming reaction, C 5 +the RON of reformed oil is 102.The rectifying of reforming reaction product is obtained to C 5 +reformed oil, aromatic production is in table 5.
Example 7
Press the method for example 6 and produce alkene and aromatic hydrocarbons by petroleum naphtha, different is used raffinating oil and extract oil out according to the method preparation of example 3, and the aromatic production of the light olefins production of cracking gained and reformation gained is in table 5.
Example 8
Press the method for example 6 and produce alkene and aromatic hydrocarbons by petroleum naphtha, different is used raffinating oil and extract oil out according to the method preparation of example 4, and the aromatic production of the light olefins production of cracking gained and reformation gained is in table 5.
Comparative example 3
Listed table 2 petroleum naphtha double centner is divided into 78.7 kilograms and 21.3 kilograms, 78.7 kilograms of petroleum naphthas are carried out to aromatic hydrocarbons extraction by the method for comparative example 1, using raffinating oil as steam crack material of obtaining, steam cracking reaction condition is: pyrolyzer top hole pressure 0.185MPa, 0.20 second residence time, water/oil quality than 0.55,840 DEG C of pyrolyzer temperature outs, selectivity of light olefin hydrocarbon is in table 5.
The extraction oil that above-mentioned aromatic hydrocarbons is obtained mixes with 21.3 kilograms of petroleum naphthas, as catalytic reforming charging.In 100 milliliters of continuous flow reactor of fixed bed, load 50 milliliters of catalyst B, be that 506 DEG C, reaction pressure are that 0.34MPa, hydrogen/hydrocarbon mol ratio are 2.5, feed volume air speed is 2.0h in reaction mass temperature in -1condition under carry out reforming reaction, C 5 +the RON of reformed oil is 102.The rectifying of reforming reaction product is obtained to C 5 +reformed oil, aromatic production is in table 5.
Table 5
Project Example 6 Example 7 Example 8 Comparative example 3
BTX output, kilogram 24.17 26.40 24.77 20.43
Benzene yield, kilogram 2.14 2.30 2.17 1.24
Toluene output, kilogram 8.51 9.48 8.80 5.73
C 8Aromatic production, kilogram 13.52 14.62 13.80 13.47
Triolefin output, kilogram 32.89 31.96 33.98 31.32
Propone output, kilogram 9.82 9.46 9.20 8.78
Divinyl output, kilogram 3.50 3.48 3.22 2.98
As shown in Table 5, compared with comparative example 3, example 6 of the present invention is being controlled C 8under the essentially identical condition of aromatic production, in split product, triolefin output increases by 5.01%, and wherein propylene increase by 11.85%, divinyl increase by 17.45%, and in reformate, light aromatics BTX output increases by 18.31%; The method of example 7 of the present invention, at C 8in the situation of aromatic production increase by 8.54%, in split product, triolefin output increases by 2.04%, and wherein propylene increase by 7.74%, divinyl increase by 16.78%, and in reformate, light aromatics BTX output increases by 29.22%; The method of example 8 of the present invention, at C 8in the situation of aromatic production increase by 2.45%, in split product, triolefin output increases by 8.49%, and wherein propylene increase by 4.78%, divinyl increase by 8.05%, and in reformate, light aromatics BTX output increases by 21.24%.
From table 5, the inventive method is compared with comparative example 3, and in BTX light aromatics output and split product, triolefin yield all increases to some extent, and wherein propylene and divinyl output amplification are higher.

Claims (15)

1. a method of being produced alkene and aromatic hydrocarbons by petroleum naphtha, comprises the steps:
(1) petroleum naphtha is carried out to extracting and separating, obtain containing raffinating oil and containing the extraction oil of naphthenic hydrocarbon and aromatic hydrocarbons of alkane and naphthenic hydrocarbon, the mass ratio of the naphthenic hydrocarbon containing in the naphthenic hydrocarbon containing in raffinating oil and petroleum naphtha is 4～40%,
(2) by the extraction oil containing naphthenic hydrocarbon and aromatic hydrocarbons 0.2～3.0MPa, 300～550 DEG C, hydrogen/hydrocarbon mol ratio 0.5～20, volume space velocity is to contact and carry out catalytic reforming reaction with reforming catalyst under the condition of 0.1～50h-1, obtains being rich in the reformed oil of aromatic hydrocarbons
(3) produce alkene by carrying out scission reaction containing raffinating oil of alkane and naphthenic hydrocarbon.
2. the mass ratio that in accordance with the method for claim 1, it is characterized in that the naphthenic hydrocarbon containing in naphthenic hydrocarbon that (1) step contains in raffinating oil and petroleum naphtha is 10～35 quality %.
3. in accordance with the method for claim 1, it is characterized in that the C that in (1) step, gained contains in raffinating oil 6～C 8the C containing in naphthenic hydrocarbon and petroleum naphtha 6～C 8the mass ratio of naphthenic hydrocarbon is 3～40%, the C containing in raffinating oil 9 +the C containing in naphthenic hydrocarbon and petroleum naphtha 9 +the mass ratio of naphthenic hydrocarbon is 1～48%.
4. according to the method described in claim 1 or 3, it is characterized in that (1) step by petroleum naphtha carry out extracting and separating solvent used be selected from tetramethylene sulfone, furfural, N-Methyl pyrrolidone, N-N-formyl morpholine N-, triglycol, Tetraglycol 99, five glycol, ditane, alpha-methyl-naphthalene or above-mentioned substance any two or more.
5. in accordance with the method for claim 1, it is characterized in that the method that petroleum naphtha is carried out extracting and separating by (1) step is liquid-liquid extraction or extractive distillation.
6. in accordance with the method for claim 5, it is characterized in that, in liquid-liquid extraction tower, petroleum naphtha is carried out to liquid-liquid extraction, the operational condition of liquid-liquid extraction tower is: entering the extraction solvent of liquid-liquid extraction tower and the mass ratio of petroleum naphtha is 3～8:1, the temperature of liquid-liquid extraction tower top is 130～190 DEG C, and pressure is 1.1～2.0MPa.
7. in accordance with the method for claim 5, it is characterized in that (1) step carries out extractive distillation to petroleum naphtha in extraction distillation column, the operational condition of extraction distillation column is: entering the extractive distillation solvent of extraction distillation column and the mass ratio of petroleum naphtha is 3～8:1, the temperature of extractive distillation tower top is 70～190 DEG C, and pressure is 0.1～0.3MPa.
8. according to the method described in claim 5 or 7, it is characterized in that extractive distillation extractive distillation solvent used comprises tetramethylene sulfone, the solubility promoter of 30～63 quality % and the water of 0.2～2.0 quality % of 35～68 quality %, described solubility promoter is selected from alkylnaphthalene, biphenyl, ditan, diphenylethane or dialkyl benzene methane.
9. in accordance with the method for claim 1, it is characterized in that the petroleum naphtha described in (1) step carries out hydrofining before extracting and separating, make olefin saturated wherein and remove impurity wherein.
10. the sulphur content that in accordance with the method for claim 9, it is characterized in that described refining petroleum naphtha is less than 0.5 μ g/g, nitrogen content and is less than that 0.5 μ g/g, arsenic content are less than 1.0ng/g, lead content is less than 10ng/g.
11. in accordance with the method for claim 1, it is characterized in that the extraction oil described in (2) step is carrying out carrying out hydrofining before reforming reaction, make olefin saturated wherein and remove impurity wherein, making sulphur content in refined products be less than 0.5 μ g/g, nitrogen content and be less than that 0.5 μ g/g, arsenic content are less than 1.0ng/g, lead content is less than 10ng/g.
12. in accordance with the method for claim 1, it is characterized in that (3) step carries out the reaction conditions of cracking and be to raffinating oil: pressure 0.05～0.30MPa, reactant residence time 0.01～0.6 second, water/oil quality than 0.3～1.0,760～900 DEG C of pyrolyzer temperature outs.
13. in accordance with the method for claim 1, it is characterized in that described petroleum naphtha is that to have ASTMD-86 initial boiling point be that 40～80 DEG C, final boiling point are the hydrocarbon mixture of 160～220 DEG C.
14. according to the method described in claim 1 or 13, it is characterized in that described petroleum naphtha is selected from virgin naphtha, hydrocracking petroleum naphtha, coking naphtha, catalytic cracking petroleum naphtha or field condensate.
15. according to the method described in claim 1 or 13, it is characterized in that alkane, the naphthenic hydrocarbon of 10～50 quality %s and the aromatic hydrocarbons of 5～30 quality %s of described petroleum naphtha containing 30～85 quality %.
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