CN102795958A - Method for producing aromatic hydrocarbon and ethylene through taking naphtha as raw material - Google Patents
Method for producing aromatic hydrocarbon and ethylene through taking naphtha as raw material Download PDFInfo
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Abstract
一种以石脑油为原料生产芳烃和乙烯的方法，包括如下步骤：(1)将石脑油在压力0.15～3.0MPa、温度300～540℃，体积空速为2.1～50h-1的临氢条件下与重整催化剂接触进行浅度催化重整反应，使石脑油中的环烷烃转化率大于85质量％，链烷烃转化为芳烃和C4 -烃的转化率小于30质量％，(2)将催化重整得到的重整生成油送入芳烃分离装置将烷烃与芳烃分离，得到富含芳烃的馏份和富含链烷烃的馏份；(3)将富含烷烃的馏份送入蒸汽裂解装置进行裂解反应生产乙烯。该法通过浅度催化重整，充分利用有限的石脑油资源，在生产芳烃的同时，可以最大化地生产乙烯。A method for producing aromatic hydrocarbons and ethylene using naphtha as a raw material, comprising the following steps: (1) Preheating the naphtha at a pressure of 0.15 to 3.0 MPa, a temperature of 300 to 540° C., and a volume space velocity of 2.1 to 50 h −1 Contacting with a reforming catalyst under hydrogen conditions to carry out a shallow catalytic reforming reaction, so that the conversion rate of naphthenes in naphtha is greater than 85% by mass, and the conversion rate of paraffins into aromatics and C4 - hydrocarbons is less than 30% by mass, ( 2) Send the reformed oil obtained by catalytic reforming to the aromatics separation device to separate alkanes from aromatics, and obtain fractions rich in aromatics and fractions rich in paraffins; (3) send the fractions rich in alkanes to into the steam cracking unit for cracking reaction to produce ethylene. This method makes full use of limited naphtha resources through shallow catalytic reforming, and can maximize the production of ethylene while producing aromatics.
Description
Technical field
The present invention is a kind of method of producing aromatic hydrocarbons and ethene, specifically, be a kind of be the method for raw material production aromatic hydrocarbons and ethene with the petroleum naphtha.
Background technology
CR and steam cracking are the sophisticated industrialization technologies of petrochemical industry, and the main purpose of CR is to produce aromatic hydrocarbons, stop bracket gasoline and hydrogen.In the catforming process; Several competing reactions can take place simultaneously; These reactions comprise that cyclohexane dehydrogenation generates aromatic hydrocarbons, the alkyl cyclopentane dehydroisomerization turns to aromatic hydrocarbons; Paraffin dehydrogenation is cyclized into aromatic hydrocarbons, paraffinic hydrocarbons hydrocracking changes into the light hydrocarbon product outside the gasoline boiling range, and korenyl takes off the isomerizing of alkyl and paraffinic hydrocarbons.In order to obtain high octane value gasoline blending component or aromatic hydrocarbons, hope that not only the naphthenic hydrocarbon dehydrocyclization becomes aromatic hydrocarbons, to paraffinic hydrocarbons be transformed simultaneously, increase the output of aromatic hydrocarbons.
The main purpose of steam cracking is to produce the propylene of ethene and relatively small amount.
The raw material of CR is a petroleum naphtha, and petroleum naphtha is the main ingredient in the steam cracking device raw material formation.Along with the change of crude oil is heavy, naphtha yield reduces, and global continuous increase to ethene and aromatic hydrocarbons demand, and the problem that CR and steam cracking device are contended over raw materials is outstanding all the more.
The mixture that petroleum naphtha is made up of multiple hydrocarbon such as normal paraffin, isomerization alkanes, naphthenic hydrocarbon and aromatic hydrocarbons.Normal paraffin is than isomerization alkanes and naphthenic hydrocarbon, and the yield that ethene is produced in cracking is high, and the phenyl ring of aromatic hydrocarbons is difficult to cracking relatively under typical cracking condition, to the almost not contribution of generation of ethene; Yet naphthenic hydrocarbon is easy to be converted into aromatic hydrocarbons under the CR condition, is the fine catalytic reforming raw material.Therefore, raw material how to optimize CR and steam cracking device is that people very are concerned about and problem demanding prompt solution.
Rectifying is the effective ways that petroleum naphtha are separated into close-cut fraction, but is difficult to reach with normal paraffin and the isolating effect of other hydrocarbon.
Adsorption separation technology can be separated normal paraffin from petroleum naphtha.CN1476474A discloses the ethylene production through steam cracking of normal paraffins, is a kind of method that is used to prepare the feedstream that adds naphtha reforming device and steam cracking device.This method is fractionated into C with petroleum naphtha earlier
5Alkane hydrocarbon stream and C
6～C
9Hydrocarbon stream is with C
6～C
9Hydrocarbon stream carries out fractionation by adsorption, optionally adsorbs normal paraffin, the C that again fractionation is obtained
5The alkane hydrocarbon stream is as strippant, with normal paraffin in the desorption liquid and C
5After paraffinic hydrocarbons separates, feed the steam cracking district and produce ethene, inhale excess oil and then feed reformer section production stop bracket gasoline.
CN101198574A discloses the ethylene production of normal paraffin steam cracking, with 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 the steam cracking district, non-positive structure hydrocarbon feeds reformer section and changes into aromatic hydrocarbons.
The optimization that CN1710030A discloses a kind of petroleum naphtha utilizes method; Use the 5A molecular sieve that petroleum naphtha is carried out fractionation by adsorption; Isolate desorption oil prodn that is rich in positive structure hydrocarbon and the residual oil absorber that is rich in non-positive structure hydrocarbon, the content of positive structure hydrocarbon is 80～100 weight % in the desorption oil.Desorption oil as the fine steam crack material or cut into close-cut fraction through rectifying and produce reagent and high-quality solvent oil product then, is inhaled excess oil as fine catalytic reforming raw material or high-octane rating clean gasoline blend component.
In the above-mentioned technology; Petroleum naphtha is through fractionation by adsorption, although normal paraffin can be improved yield of ethene as steam crack material, because normal paraffin content is lower in the petroleum naphtha; When obtaining identical ethylene yield, the demand of petroleum naphtha is increased considerably.
Summary of the invention
The purpose of this invention is to provide a kind of is the method for raw material production aromatic hydrocarbons and ethene with the petroleum naphtha, and this method can make full use of petroleum naphtha through shallow degree CR and when producing aromatic hydrocarbons, produce ethene substantially.
Provided by the invention is the method for raw material production aromatic hydrocarbons and ethene with the petroleum naphtha, comprises the steps:
(1) with petroleum naphtha 300～540 ℃ of pressure 0.15～3.0MPa, temperature, volume space velocity is 2.1～50h
-1Hydro condition contact down and carry out shallow degree catalytic reforming reaction with reforming catalyst, make naphthenic hydrocarbon transformation efficiency in the petroleum naphtha greater than 85 quality %, paraffin conversion is aromatic hydrocarbons and C
4 -Hydrocarbon conversion rate is less than 30 quality %;
(2) reformed oil that CR is obtained is sent into aromatic hydrocarbons tripping device aromatics separation and paraffinic hydrocarbons, obtains being rich in the fraction and the fraction that is rich in paraffinic hydrocarbons of aromatic hydrocarbons;
The fraction that (3) will be rich in paraffinic hydrocarbons is sent into steam cracking device and is carried out scission reaction and produce ethene.
The inventive method is carried out shallow degree CR with petroleum naphtha; Make the naphthenic hydrocarbon in the petroleum naphtha be converted into aromatic hydrocarbons; The conversion of Quality Initiative alkane simultaneously; Thereby can in reforming process, obtain to maximum paraffinic hydrocarbons, and described CR is separated with aromatic hydrocarbons and the steam cracking process combination, can, CR produce ethene in maximum ground when producing aromatic hydrocarbons.Compare with the CR or the fractionation by adsorption of routine, the inventive method can be produced more light aromatics (BTX), ethene and propylene and 1,3-butadiene under the identical condition of aromatics yield.
Description of drawings
Fig. 1 is the inventive method schematic flow sheet.
Embodiment
In conventional catforming process; In order to reach the reformed oil octane value of expection; When the naphthenic hydrocarbon in the petroleum naphtha almost all is converted into aromatic hydrocarbons; Reaction has also taken place in normal paraffin and isomerization alkanes, comprises that isomerization of paraffinic hydrocarbons generates highly-branched chain isomerous alkane, dehydrocyclization generates aromatic hydrocarbons, hydrogenolysis generation methane, hydrogen cracking generation C
3And C
4Alkane.
The present invention carries out shallow degree CR with petroleum naphtha; Promptly through control reforming reaction condition; The degree of depth that the control reaction takes place; When the naphthenic hydrocarbon in guaranteeing petroleum naphtha is converted into aromatic hydrocarbons basically, the conversion of paraffinic hydrocarbons taking place as few as possible, makes isomerization of paraffinic hydrocarbons generate highly-branched chain isomerous alkane, dehydrocyclization generation aromatic hydrocarbons, hydrogenolysis generation methane, hydrogen cracking generation C
3And C
4It is minimum that the reaction of alkane reduces to, and can make thus to keep most paraffinic hydrocarbons in the reformate.Aromatic hydrocarbons in the reformate is separated with paraffinic hydrocarbons, again paraffinic hydrocarbons is sent into steam cracking device and carry out cracking, can produce ethene, obtain propylene and 1,3-butadiene simultaneously, above-mentioned three kinds of alkene are called for short triolefin.The present invention uses the petroleum naphtha of equal amts than prior art, can produce more light aromatics (benzene, toluene and YLENE are called for short BTX), ethene, propylene and 1,3-butadiene.
The inventive method (1) step is shallow degree CR; Through the degree of depth of control reaction conditions control reforming reaction, mainly be controlled temperature and charging air speed, paraffinic hydrocarbons is transformed as few as possible; Make preferably that the naphthenic hydrocarbon transformation efficiency is greater than 90 quality % in the petroleum naphtha, paraffin conversion is aromatic hydrocarbons and C
4The transformation efficiency of hydrocarbon is less than 10 quality %.
Preferred 0.2～the 2.0MPa of the inventive method (1) described catalytic reforming reaction pressure of step, preferred 350～520 ℃, more preferably 400～500 ℃ of temperature, the preferred 3.0～30h of petroleum naphtha volume space velocity
-1, more preferably 8.0～25.0h
-1
(1) hydrogen/hydrocarbon mol ratio preferred 0.1～20: 1 of described catalytic reforming reaction of step, more preferably 1～8: 1.
CR of the present invention can adopt the technology of (moving-bed) reformation continuously, half regeneration (fixed bed) reformation technology or cyclic regeneration reformation technology.
The inventive method (1) step, described reforming catalyst comprised the VIII family metal of 0.01～5.0 quality %, the halogen of 0.01～5.0 quality % and the inorganic oxide carrier of 90.0～99.97 quality %.
Said reforming catalyst can also comprise the VIII family metal of 0.01～5.0 quality %, the halogen of 0.01～5.0 quality %, the metal that is selected from Re, Sn, Ge, Ir or Rh of 0.01～10.0 quality %, and the inorganic oxide carrier of 80.0～99.97 quality %.
In addition, can also comprise the metal constituent element that one or more are selected from basic metal, earth alkali metal, REE, In, Co, Ni, Fe, W, Mo, Cr, Bi, Sb, Zn, Cd and Cu in the above-mentioned reforming catalyst.
Inorganic oxide carrier in the said reforming catalyst comprises aluminum oxide, Natural manganese dioxide, chromic oxide, B
2O
3, TiO
2, ThO
2, ZnO
2, ZrO
2, silica-alumina, silicon oxide-Natural manganese dioxide, chromic oxide-aluminum oxide, Al
2O
3-B
2O
3, SiO
2-ZrO
2, various potteries, various alumina, various bauxite, SiO
2, silit, synthetic or naturally occurring various silicate and clay, crystalline silico-alumino zeolite; Like X-zeolite, Y-zeolite, mordenite, beta-zeolite, Ω-zeolite or L-zeolite; These crystalline silico-alumino zeolites can be Hydrogens; Preferred non-acid type can have one or more basic metal to occupy the commutative position of positively charged ion in non-acid type crystalline silico-alumino zeolite), non-Si-Al zeolite, like aluminophosphates or silicoaluminophosphates.The preferred aluminum oxide of described inorganic oxide carrier.
Said reforming catalyst adopts the ordinary method preparation, and the preparation shaping carrier can be ball-type or stripe shape earlier; And then dipping is introduced metal constituent element and halogen; If contain second, third metal constituent element in the catalyzer, preferable methods is in carrier, to introduce second, third metal constituent element earlier, introduces VIII family metal and halogen at last again; Carrier behind the introducing metal constituent element is through drying, and 450～650 ℃ of roastings promptly get the oxidation state reforming catalyst.The oxidation state reforming catalyst generally need pass through halogen and regulate, and introduces the preferred chlorine of halogen of catalyzer, and the halogen control method is handled for the water chlorine activation, and treatment temp is 370～600 ℃.The oxidation state reforming catalyst needed in 315～650 ℃ of hydrogen atmospheres, to reduce before using, and obtained going back the ortho states reforming catalyst, also need carry out prevulcanized for reforming Pt-Re catalyst and handle.
Petroleum naphtha of the present invention is that to have ASTM D-86 initial boiling point be that 40～80 ℃, final boiling point are 160～220 ℃ hydrocarbon mixture, is mainly C
5～C
12Hydro carbons, comprise alkane, naphthenic hydrocarbon, aromatic hydrocarbons and alkene.Described petroleum naphtha contains the alkane of 30～85 quality %, the naphthenic hydrocarbon of 10～50 quality % and the aromatic hydrocarbons of 5～30 quality %.
Described petroleum naphtha is virgin naphtha, hydrogen cracking petroleum naphtha, coking naphtha, catalytic cracking petroleum naphtha or field condensate.
Impurity such as the alkene that contains in the petroleum naphtha, sulphur, nitrogen, arsenic, oxygen, chlorine all can have a negative impact to catalytic reforming unit and reforming catalyst; Therefore petroleum naphtha is before carrying out reforming reaction; Preferably carry out unifining; Make alkene generation hydrogenation wherein saturated, remove impurity such as sulphur, nitrogen, arsenic, oxygen, chlorine simultaneously, obtain the unifining petroleum naphtha.
Described petroleum naphtha hydrogenation refining reaction temperature is generally 260～460 ℃, preferred 280～400 ℃, and pressure is 1.0～8.0MPa, preferred 1.6～4.0MPa, and the feed volume air speed is 1～20h
-1, preferred 2～8h
-1, hydrogen during reaction/hydrocarbon volume ratio is 10～1000: 1, preferred 50～600: 1.
Described Hydrobon catalyst should have the hydrogenation saturation of olefins, has the ability of hydrogenating desulfurization, denitrogenation and deoxidation simultaneously.Said Hydrobon catalyst comprises the hydrogenation activity component of 5～49 quality %, the halogen of 0.1～1.0 quality % and the inorganic oxide carrier of 50.0～94.9 quality %; Said 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 the rare earth metal, the preferred aluminum oxide of described inorganic oxide carrier.
Above-mentioned Hydrobon catalyst can adopt conventional method preparation, and with the white lake moulding, roasting makes gamma-aluminium oxide carrier in air or water vapour again like the described elder generation of CN1169337A, and then adopts dipping method to introduce the hydrogenation activity component.
In addition, to the petroleum naphtha after the unifining, can also further adopt following method to remove detrimental impurity.Adopting dechlorinating agent, is that the dechlorinating agent of calcium hydroxide or calcium hydroxide and lime carbonate or yellow soda ash and lime carbonate removes the chlorine in the petroleum naphtha like the disclosed active ingredient of CN1353005A.Adopt suitable sweetening agent, as removing the sulphur in the petroleum naphtha with the disclosed sweetening agent of forming by nickel, zeyssatite, silicon-dioxide and aluminum oxide of CN86100015A; Adopt suitable dearsenic agent, remove the arsenic impurities in the petroleum naphtha like the disclosed dearsenic agent of CN1095749A by the alumina load metallic nickel.
Product after petroleum naphtha hydrogenation is refining; Through separating; Isolate dry gas and liquefied gas, the product liquid that obtains is refining petroleum naphtha, the sulphur content in the refining petroleum naphtha less than 0.5 μ g/g, nitrogen content less than 0.5 μ g/g, arsenic content less than 1.0ng/g, lead content less than 10ng/g.
The inventive method (2) step, described reformed oil was that the catalytic reforming reaction product is obtained with the separation column fractionation.(1) contain hydrogen in the step catalytic reforming reaction product, reforming reaction product cooling back entering knockout drum separates the gas that will be rich in hydrogen and from liquid phase, separates.The knockout drum service temperature is 0～65 ℃, and liquid-phase product is through a separation column, and cat head is isolated C
4Or C
5Following light hydrocarbon component obtains C at the bottom of the tower
5Or C
6Above hydrocarbon mixture is C
5 +Or C
6 +Reformed oil.
(2) step is sent reformed oil into aromatic hydrocarbons tripping device separation aromatic hydrocarbons and paraffinic hydrocarbons wherein, and described aromatic hydrocarbons tripping device is preferably aromatic extraction unit or arene adsorptive separation apparatus.
When separating the aromatic hydrocarbons in the reformed oil with aromatic extraction unit, the preferred tetramethylene sulfone of used extraction solvent, DMSO 99.8MIN., N, N-Methyl pyrrolidone, N-N-formyl morpholine N-, triglycol, Tetraglycol 99, five glycol, methyl alcohol or acetonitrile.
Described aromatic hydrocarbons extracting can be liquid-liquid extraction or extractive distillation process.
The process of liquid-liquid extraction aromatics separation is: reformed oil contacts with the extraction solvent liquid phase in extraction tower, obtains being rich in the rich solvent of aromatic hydroxy compound at the bottom of the tower, and cat head obtains being rich in the raffinate of non-aromatic hydroxy compound.Raffinate can also be purified in washing tower, removes residual trace solvent, obtains being rich in the hydrocarbon mixture of paraffinic hydrocarbons.The rich solvent that is rich in aromatic hydroxy compound gets into the separated from solvent tower, and aromatic hydrocarbons is discharged by reclaiming cat head, and lean solvent is discharged at the bottom of by tower, returns the extraction tower recycle again.
The process of extractive distillation aromatics separation is: reformed oil is sent into extraction distillation column contact under gas phase condition with extraction solvent; Non-aromatic hydroxy compound and a spot of solvent are discharged through cat head; The rich solvent that is rich in aromatic hydrocarbons gets into the separated from solvent tower through discharging at the bottom of the tower; Aromatic hydroxy compound is separated from solvent, and the lean solvent that obtains returns extraction distillation column again and recycles.
The isolated BTX aromatics of aromatic hydrocarbons extracting can be sent into Aromatic Hydrocarbon United Plant and produce benzene, toluene and YLENE, and YLENE is carried out xylene isomerization and fractionation by adsorption production p-Xylol.Aromatic Hydrocarbon United Plant is generally by aromatic hydrocarbons extracting, C
8Several or whole unit in the unit such as aromatics isomerization, fractionation by adsorption, toluene disproportionation and aromatic hydrocarbons transalkylation are formed, and can be used to produce Chemicals such as benzene, toluene, p-Xylol, m-xylene.
Reformate of the present invention separates through aromatic hydrocarbons; The compound that is rich in aromatic hydrocarbons that obtains all is the raw materials as the subsequent reactions device with the hydrocarbon mixture that is rich in paraffinic hydrocarbons, does not therefore make strict restriction for the purity of aromatic hydrocarbons and the content that is rich in aromatic hydrocarbons in the hydrocarbon mixture of paraffinic hydrocarbons.Therefore can adopt the program of more simplifying than conventional aromatic hydrocarbons extracting unit to carry out the extraction of aromatic hydroxy compound.In this case, the separated from solvent tower can have less stage number, and the mass ratio of described extraction solvent and extracting raw material can be 1～10, and preferred 1～5.
Described aromatic hydrocarbons of the inventive method (2) step separates also can adopt fractionation by adsorption.Reformed oil is fed adsorbent bed, aromatic hydrocarbons wherein is adsorbed, and non-aromatic hydrocarbons is then discharged adsorbent bed, in adsorbent bed, feeds desorbing agent then to the adsorbent bed desorption that carries out.In the adsorption separation process, the sorbent material of employing can be any porous mass that aromatic hydrocarbons is had adsorptive power, preferred NaX, NaY zeolite.
The inventive method (3) step is produced ethene for the hydrocarbon mixture that will be rich in paraffinic hydrocarbons as steam crack material, and the reaction conditions of steam cracking is 0.05～0.30MPa, reactant residence time 0.01～0.6 second, water/oil quality than 0.3～1.0,760～900 ℃ of pyrolyzer temperature outs.
Further specify the present invention below in conjunction with accompanying drawing.
Among Fig. 1, from the petroleum naphtha of pipeline 1 with mix from the hydrogen make-up of pipeline 2, get into pre-hydrogenator 3 with circulating hydrogen again from pipeline 9.Hydrogenation products gets into knockout drum 5 by pipeline 4 in advance; Knockout drum 5 tops are isolated the gas that is rich in hydrogen and are got into recycle compressors 8 by pipeline 6 and circulate; The effusive logistics in knockout drum 5 bottoms gets into rectifying tower 10 through pipeline 7, and 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, carries out shallow degree CR of the present invention through pipeline 12 with entering reforming reactor 13 after circulating hydrogen from pipeline 19 mixes.The reforming reaction product gets into reformate knockout drum 15 by pipeline 14; The isolated gas that is rich in hydrogen in top is recycled through recycle compressor 18 by pipeline 16; The effusive liquid ingredient in bottom gets into reformate rectifying tower 20 by pipeline 17, and the liquefaction vapour that rectifying obtains is by upper pipeline 21 discharge systems, and reformed oil is discharged by the bottom; Get into aromatic hydrocarbons disengaging zone 23 by pipeline 22; Aromatic hydrocarbons disengaging zone 23 can be extraction plant or adsorption separation device, through solvent extraction (also can be absorption) aromatic hydrocarbons is separated with non-aromatic hydrocarbons, and the component that is rich in paraffinic hydrocarbons after the separation gets into water wash column 26 by pipeline 24; Through washing; The component that is rich in paraffinic hydrocarbons gets into steam cracking district 32 by pipeline 27 and carries out preparing ethylene by steam cracking, and the mixture that contains extraction solvent and water that discharge water wash column 26 bottoms is discharged by pipeline 28, can return aromatic hydrocarbons disengaging zone 23 and recycle.The rich solvent that contains aromatic hydrocarbons that discharge aromatic hydrocarbons disengaging zone 23 gets into solvent recovery tower 29 aromatics separations and solvent by pipeline 25; The arene stream that solvent recovery tower 29 tops obtain is discharged by pipeline 30; Can send into Aromatic Hydrocarbon United Plant separates aromatic hydrocarbon product such as BTX or carries out treating processess such as follow-up diformazan isomerizing and p-Xylol fractionation by adsorption; The lean solvent that solvent recovery tower 29 bottoms obtain is discharged by pipeline 31, can return aromatic hydrocarbons disengaging zone 23 and recycle.
Pass through instance further explain the present invention below, but the present invention is not limited to this.
Instance 1
This instance carries out unifining to petroleum naphtha.
In 20 milliliters of continuous flow reactor of fixed bed, load 20 milliliters of Hydrobon catalyst A, wherein contain the CoO of 0.03 quality %, the NiO of 2.0 quality %, the WO of 19.0 quality %
3, the F of 0.7 quality % and the Al of 78.27 quality %
2O
3
Is that 1.6MPa, hydrogen/hydrocarbon volume ratio are that 200: 1, feed volume air speed are 8.0h with the petroleum naphtha of listed composition of table 1 and character at 290 ℃, hydrogen dividing potential drop
-1Condition under feed in the reactor drum of above-mentioned loading catalyst A and carry out unifining, reaction product gets into watercooler, is separated into gas-liquid two-phase, measures respectively and carries out compositional analysis, the composition and the character of refining back gained petroleum naphtha are seen table 2.
Table 1
Table 2
Can know that by table 2 result the alkene after unifining in the petroleum naphtha, sulphur, nitrogen, arsenic, lead content all reach the charging requirement of catalytic reforming reaction.
Instance 2～3
Following instance carries out CR by the inventive method.
Adopt PtSn/ γ-Al
2O
3Catalyst B, wherein containing Pt 0.35 quality %, Sn 0.30 quality %, Cl 1.0 quality %, surplus is γ-Al
2O
3
In 100 milliliters of continuous flow reactor of fixed bed; Load 50 milliliters of catalyst B; With the listed refining petroleum naphtha of table 2 is catalytic reforming raw material, is that 500 ℃, reaction pressure are that 0.34MPa, hydrogen/hydrocarbon mol ratio are 6.7, the feed volume air speed is respectively 20.0h in the reaction mass temperature in
-1, 8.0h
-1Condition under carry out reforming reaction, the rectifying of reforming reaction product is obtained C
5 +Reformed oil, reaction result is seen table 3.
Instance 4
Adopt PtRe/ γ-Al
2O
3Catalyzer C, wherein containing Pt 0.26 quality %, Re 0.26 quality %, Cl 1.0 quality %, surplus is γ-Al
2O
3
In 100 milliliters of continuous flow reactor of fixed bed, load 50 milliliters of catalyzer C, catalyzer C adds 0.1 quality % before use in 425 ℃ hydrogen stream hydrogen sulfide carries out prevulcanized, and the sulphur content that makes catalyzer is 0.06 quality %.With the listed refining petroleum naphtha of table 2 is catalytic reforming raw material, is that 475 ℃, reaction pressure are that 1.4MPa, hydrogen/hydrocarbon mol ratio are 6.7, the feed volume air speed is 20.0h in the reaction raw materials temperature in
-1Condition under carry out reforming reaction, the rectifying of reforming reaction product is obtained C
5 +Reformed oil, reaction result is seen table 3.
Adopt Pt/ γ-Al
2O
3Catalyzer D, wherein containing Pt 0.50 quality %, Cl 0.8 quality %, surplus is γ-Al
2O
3
In 100 milliliters of continuous flow reactor of fixed bed; Load 50 milliliters of catalyzer D; With the listed refining petroleum naphtha of table 2 is catalytic reforming raw material, is that 475 ℃, reaction pressure are that 1.4MPa, hydrogen/hydrocarbon mol ratio are 6.7, the feed volume air speed is 18.0h in the reaction mass temperature in
-1Condition under carry out reforming reaction, the rectifying of reforming reaction product is obtained C
5 +Reformed oil, reaction result is seen table 3.
Comparative Examples 1
This Comparative Examples explanation petroleum naphtha is through the effect of conventional CR.
Method his-and-hers watches 2 listed refining petroleum naphthas by instance 2 carry out CR, and different is that the feed volume air speed is 2.0h
-1, the result sees table 3.
Comparative Examples 2
This Comparative Examples explanation petroleum naphtha is inhaled the effect that excess oil carries out CR through after the fractionation by adsorption with gained.
The petroleum naphtha that table 1 is listed feeds the fixed bed that the 5A molecular sieve is housed and carries out fractionation by adsorption, and adsorption temp is 200 ℃, and the charging mass space velocity is 0.3h
-1, 5A molecular sieve bed layer aspect ratio 8: 1, adsorption time 30 minutes.Be not to inhale excess oil after the condensation of the gas of 5A molecular sieve adsorption process, wherein be rich in naphthenic hydrocarbon and aromatic hydrocarbons.Adopt nitrogen to carry out desorption, desorption temperature is 400 ℃, desorbing agent charging air speed 200h
-1, behind the desorption, obtain being rich in the desorption oil of normal paraffin.
The suction excess oil that obtains is carried out CR by the method for Comparative Examples 1, and the result sees table 3.
Table 3
Adopt PtSn/ γ-Al
2O
3Catalyst B; By the inventive method with the listed refining petroleum naphtha of table 2 as catalytic reforming raw material; The investigation reaction pressure is that 0.70MPa, hydrogen/hydrocarbon mol ratio are 2.2 o'clock; Different temperature of reaction and feed volume air speed are to the influence of catalytic reforming reaction, and each instance reaction raw materials temperature in and feed volume air speed and reaction result are seen table 4.
Instance 9
Adopt PtRe/ γ-Al
2O
3Catalyzer C, by the inventive method with the listed refining petroleum naphtha of table 2 as catalytic reforming raw material, be that 1.30MPa, hydrogen/hydrocarbon mol ratio are 4.5 o'clock in reaction pressure, temperature of reaction is 436 ℃, the feed volume air speed is 2.1h
-1Condition under carry out reforming reaction, the result sees table 4.
Table 4
Can know that by table 3 and table 4 adopt the inventive method to reduce temperature of reaction or increase feed volume air speed, than conventional reforming reaction, when guaranteeing that naphthenic hydrocarbon is converted into aromatic hydrocarbons, paraffin conversion is aromatic hydrocarbons and C
4 -The transformation efficiency of lighter hydrocarbons reduces significantly, and most paraffinic hydrocarbonss have kept, and promptly in the inventive method, the naphthenic hydrocarbon transformation efficiency all reaches more than the 85 quality %, and paraffin conversion is aromatic hydrocarbons and C
4 -The transformation efficiency of hydrocarbon is then less than 30 quality %, and in most cases, paraffin conversion is aromatic hydrocarbons and C
4 -The transformation efficiency of hydrocarbon is less than 10 quality %.
Instance 10～11
The C that following instance explanation the inventive method obtains
5 +Effect after reformed oil separates through aromatic hydrocarbons.
Adopting tetramethylene sulfone is the solvent of extracting aromatics separation, the C that instance 2 and instance 3 are obtained
5 +Reformed oil contacts with tetramethylene sulfone in extraction tower, and solvent/raw materials quality ratio is 2, extracting tower top pressure 0.45MPa, and reflux ratio is 0.25, and solvent is gone into 85 ℃ of tower temperature, and raw material is gone into 50 ℃ of tower temperature.
Obtain being rich in the solvent of aromatic hydroxy compound at the bottom of the extraction tower, cat head obtains containing the raffinate of non-aromatic hydroxy compound.The solvent that is rich in aromatic hydroxy compound obtains BTX aromatics through distillation and after extraction solvent separates.Raffinate removes residual trace solvent through washing, obtains being rich in the hydrocarbon mixture of paraffinic hydrocarbons.The hydrocarbon mixture yield (with respect to petroleum naphtha) and the aromatics yield that are rich in paraffinic hydrocarbons are (with respect to C
5 +Aromatic hydrocarbons in the reformed oil) see table 5.
Comparative Examples 3
Press the method for instance 10, the C that Comparative Examples 1 is obtained
5 +Reformed oil is that extraction solvent separates aromatic hydrocarbons and paraffinic hydrocarbons wherein with the tetramethylene sulfone.The hydrocarbon mixture yield (with respect to petroleum naphtha) and the aromatics yield that are rich in paraffinic hydrocarbons are (with respect to C
5 +Aromatic hydrocarbons in the reformed oil) see table 5.
Comparative Examples 4
The petroleum naphtha that table 1 is listed feeds the fixed bed that the 5A molecular sieve is housed and carries out fractionation by adsorption, and the temperature of absorption is 200 ℃, and the charging mass space velocity is 0.3 hour
-1, 5A molecular sieve bed layer aspect ratio 8: 1, adsorption time 30 minutes.Do not obtained inhaling excess oil through after the condensation, wherein be rich in naphthenic hydrocarbon and aromatic hydrocarbons by the gas of 5A molecular sieve adsorption.Adopt nitrogen to carry out desorption, desorption temperature is 400 ℃, desorbing agent charging air speed 200h
-1, behind the desorption, obtaining being rich in the desorption oil of normal paraffin, its yield with respect to petroleum naphtha is seen table 5.
Table 5
| Project | Instance 10 | Instance 11 | Comparative Examples 3 | Comparative Examples 4 |
| Aromatics yield, quality % | 95 | 98 | 98.5 | |
| Be rich in the hydrocarbon mixture yield of paraffinic hydrocarbons, quality % | 65.81 | 48.31 | 20.35 | 29.60 |
Table 5 is the result show, the hydrocarbon mixture yield that is rich in paraffinic hydrocarbons that the inventive method obtains all is improved largely than routine reformation and adsorption separating method.
The steam cracking effect of the hydrocarbon mixture that is rich in paraffinic hydrocarbons that following instance explanation the inventive method obtains.
The hydrocarbon mixture that is rich in paraffinic hydrocarbons that instance 10 is obtained is as steam crack material.The steam cracking reaction condition is: pyrolyzer top hole pressure 0.185MPa, 0.20 second residence time, water/oil quality than 0.55,840 ℃ of pyrolyzer temperature outs, yield of ethene is seen table 6.
The hydrocarbon mixture that is rich in paraffinic hydrocarbons that instance 11 is obtained is as steam crack material.The steam cracking reaction condition is: pyrolyzer top hole pressure 0.185MPa, 0.20 second residence time, water/oil quality than 0.55,840 ℃ of pyrolyzer temperature outs, yield of ethene is seen table 6.
Comparative Examples 5
This instance explains that gained after conventional CR is through the aromatic hydrocarbons extracting is rich in the steam cracking effect of the hydrocarbon mixture of paraffinic hydrocarbons.
The hydrocarbon mixture that is rich in paraffinic hydrocarbons that obtains behind the Comparative Examples 3 extracting aromatics separations as steam crack material, is carried out cracking according to the method for instance 12, and yield of ethene is seen table 6.
Comparative Examples 6
This instance explanation petroleum naphtha is rich in the steam cracking effect of the hydrocarbon mixture of normal paraffin through gained after the fractionation by adsorption.
The desorption oil that is rich in normal paraffin that Comparative Examples 4 fractionation by adsorption are obtained carries out cracking as steam crack material by the method for instance 12, and yield of ethene is seen table 6.
Table 6
*Triolefin is ethene, propylene, 1,3-butadiene.
Table 6 is the result show; Petroleum naphtha increases obviously although be rich in the steam cracking yield of ethene and the triolefin yield of the hydrocarbon mixture of normal paraffin through after the fractionation by adsorption of prior art, and the normal paraffin yield that fractionation by adsorption obtains is low; Therefore can be used for the also corresponding minimizing significantly of raw material of steam cracking; With respect to every 100kg petroleum naphtha, the output of ethene and triolefin is respectively 11.28 and 17.15kg, far below the ethylene yield and the triolefin output of instance 12 of the present invention and 13.And the inventive method is with respect to conventional CR, and the ethene of every 100kg petroleum naphtha and triolefin output also obviously improve.
This instance explanation 100kg petroleum naphtha is with the output of available ethene of the inventive method and aromatic hydrocarbons.
Get the listed refining petroleum naphtha of table 2, carry out CR by the method for instance 2, the C that obtains
5 +Reformed oil is pressed the method extracting aromatics separation of instance 10 again, and the hydrocarbon mixture that is rich in paraffinic hydrocarbons that obtains behind the extracting aromatics separation carries out steam cracking by the method for instance 12, and the output that obtains ethene and aromatic hydrocarbons is seen table 7.
Comparative Examples 8
The explanation of this Comparative Examples is according to the output of available ethene of prior art 100kg petroleum naphtha and aromatic hydrocarbons.
The 100kg petroleum naphtha is divided into two parts, and portion is 62.90kg, and portion is 37.10kg in addition.
The 62.90kg petroleum naphtha is carried out fractionation by adsorption by the method for Comparative Examples 4, the desorption oil that is rich in normal paraffin that obtains after separating is carried out steam cracking by the method for instance 12, inhale excess oil and then carry out CR by the method for Comparative Examples 1.Petroleum naphtha with 37.10kg carries out steam cracking by the method for instance 12 again.The ethene that above-mentioned two kinds of methods obtain and the output of aromatic hydrocarbons are seen table 7.
Table 7
| | Instance | 14 | Comparative Examples 8 |
| Petroleum naphtha, kg | 100 | 100 | |
| Ethylene yield, kg | 22.65 | 18.12 | |
| Triolefin output, kg | 36.14 | 29.29 | |
| Aromatic production, kg | 32.54 | 32.50 | |
| BTX output, kg | 22.12 | 21.24 |
Table 7 is the result show, compare with the Comparative Examples 8 that adopts prior art, when from the 100kg petroleum naphtha, obtaining identical aromatic production, the inventive method compared to prior art, light aromatic hydrocarbons (BTX) output increases 0.88kg, amplification is 4.14%; Ethylene yield increases 4.53kg, and amplification is 25.00%; Triolefin output increases 6.85kg, and amplification is 23.39%.
Claims (17)
1. one kind is the method for raw material production aromatic hydrocarbons and ethene with the petroleum naphtha, comprises the steps:
(1) with petroleum naphtha 300～540 ℃ of pressure 0.15～3.0MPa, temperature, volume space velocity is 2.1～50h
-1Hydro condition contact down and carry out shallow degree catalytic reforming reaction with reforming catalyst, make naphthenic hydrocarbon transformation efficiency in the petroleum naphtha greater than 85 quality %, paraffin conversion is aromatic hydrocarbons and C
4 -The transformation efficiency of hydrocarbon is less than 30 quality %,
(2) reformed oil that CR is obtained is sent into aromatic hydrocarbons tripping device aromatics separation and paraffinic hydrocarbons, obtains being rich in the fraction and the fraction that is rich in paraffinic hydrocarbons of aromatic hydrocarbons;
The fraction that (3) will be rich in paraffinic hydrocarbons is sent into steam cracking device and is carried out scission reaction and produce ethene.
2. according to the described method of claim 1, it is characterized in that described reforming reaction of (1) step makes naphthenic hydrocarbon transformation efficiency in the petroleum naphtha greater than 90 quality %, paraffin conversion is aromatic hydrocarbons and C
4 -The transformation efficiency of hydrocarbon is less than 10 quality %.
3. according to the described method of claim 1, it is characterized in that described catalytic reforming reaction pressure of (1) step is 0.2～2.0MPa, temperature is 350～520 ℃, and the petroleum naphtha volume space velocity is 3.0～30h
-1
4. according to the described method of claim 1, it is characterized in that the hydrogen/hydrocarbon mol ratio of described catalytic reforming reaction of (1) step is 0.1～20: 1.
5. according to the described method of claim 4, it is characterized in that the hydrogen/hydrocarbon mol ratio of described catalytic reforming reaction is 1～8: 1.
6. according to the described method of claim 1, it is characterized in that the temperature that (1) step petroleum naphtha carries out catalytic reforming reaction is 400～500 ℃, the volume space velocity of petroleum naphtha is 8.0～25.0h
-1
7. according to the described method of claim 1, it is characterized in that described reformed oil of (2) step is that the catalytic reforming reaction product liquid is obtained with the separation column fractionation.
8. according to claim 1 or 7 described methods, it is characterized in that described reformed oil of (2) step is C
5 +Or C
6 +Hydrocarbon mixture.
9. according to the described method of claim 1, it is characterized in that described aromatic hydrocarbons tripping device of (2) step is aromatic extraction unit or arene adsorptive separation apparatus.
10. according to the described method of claim 9, it is characterized in that the used extraction solvent of aromatic extraction unit is tetramethylene sulfone, DMSO 99.8MIN., N, N-Methyl pyrrolidone, N-N-formyl morpholine N-, triglycol, Tetraglycol 99, five glycol, methyl alcohol or acetonitrile.
11. according to the described method of claim 10, the mass ratio that it is characterized in that described extraction solvent and extracting raw material is 1～5.
12., it is characterized in that arene adsorptive separation apparatus is sorbent used for NaX or NaY according to the described method of claim 9.
13. according to the described method of claim 1, the condition that it is characterized in that said scission reaction of (3) step is 0.05～0.30MPa, reactant residence time 0.01～0.6 second, water/oil quality than 0.3～1.0,760～900 ℃ of pyrolyzer temperature outs.
14., it is characterized in that described petroleum naphtha is that to have the ASTMD-86 initial boiling point be that 40～80 ℃, final boiling point are 160～220 ℃ hydrocarbon mixture according to the described method of claim 1.
15., it is characterized in that described petroleum naphtha is virgin naphtha, hydrogen cracking petroleum naphtha, coking naphtha, catalytic cracking petroleum naphtha or field condensate according to claim 1 or 7 described methods.
16., it is characterized in that described petroleum naphtha contains the naphthenic hydrocarbon of the alkane of 30～85 quality %, 10～50 quality % and the aromatic hydrocarbons of 5～30 quality % according to the described method of claim 1.
17. according to the described method of claim 1, it is characterized in that described petroleum naphtha is the unifining petroleum naphtha, its sulphur content less than 0.5 μ g/g, nitrogen content less than 0.5 μ g/g, arsenic content less than 1.0ng/g, lead content less than 10ng/g.
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| TW101117875A TWI544067B (en) | 2011-05-27 | 2012-05-18 | A Method for Catalytic Recombination of Naphtha |
| FR1254690A FR2975701B1 (en) | 2011-05-27 | 2012-05-23 | PROCESS FOR CATALYTIC REFORMING NAPHTHA |
| KR1020120056145A KR101882958B1 (en) | 2011-05-27 | 2012-05-25 | A process for catalytically reforming naphtha |
| US13/480,837 US9303217B2 (en) | 2011-05-27 | 2012-05-25 | Processes for catalytically reforming naphtha |
| JP2012119997A JP6032944B2 (en) | 2011-05-27 | 2012-05-25 | Process for catalytic reforming of naphtha |
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