CN102399589B - Method for reducing content of olefin in reformate - Google Patents
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- CN102399589B CN102399589B CN201010283118.1A CN201010283118A CN102399589B CN 102399589 B CN102399589 B CN 102399589B CN 201010283118 A CN201010283118 A CN 201010283118A CN 102399589 B CN102399589 B CN 102399589B
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Abstract
A method for reducing the content of olefin in reformate comprises steps of: connecting olefin saturated segments in series in a continuous reforming reaction system, using a continuous reforming catalyst as an olefin saturated catalyst, and converting olefin in the reforming product into saturated hydrocarbon. Calculated by using an inorganic oxide support as the reference, the continuous reforming catalyst contains, by weight, 0.1-5.0% of group VIII metal, 0.1-5.0% of group IV A metal and 0.1-5.0% of halogen. According to the method, the continuous reforming and olefin saturated catalysts are integrated as a whole such that the reforming catalyst is used for olefin saturation under the olefin saturation reaction condition, thus avoiding additional catalyst regeneration process of single use of alkene saturation catalyst with other compositions and simplifying operation steps of the technology.
Description
Technical field
The present invention is a kind of method that reduces content of olefin in reformate, specifically, is a kind of method that reduces olefin(e) centent in CONTINUOUS REFORMER reaction product.
Background technology
Catalytic reforming is the reformate that petroleum naphtha is converted into stop bracket gasoline by catalyzed reaction or is rich in aromatic hydrocarbons, simultaneously rich important refining of petroleum technique of producing cheap hydrogen.In catforming process, be rich in the petroleum naphtha of paraffinic hydrocarbons and naphthenic hydrocarbon, contact with the reforming catalyst of platiniferous under certain condition, main generation reacted as follows: naphthenic hydrocarbon dehydrogenation is converted into aromatic hydrocarbons, paraffin dehydrogenation cyclisation becomes aromatic hydrocarbons, the isomerization of paraffinic hydrocarbons and naphthenic hydrocarbon, paraffinic hydrocarbons hydrocracking.
According to the difference of catalyst regeneration mode, catalytic reforming process mainly contains three types: half generative reforming, cyclic regeneration are reformed and (regeneration) reformation continuously.CONTINUOUS REFORMER, because its liquid yield is high, hydrogen productive rate is high and aromatics yield advantages of higher, is developed rapidly in recent years, in modern times oil refining, occupies more and more consequence.
In recent years, the reaction conditions of continuous reforming process is constantly towards future development favourable to thermodynamic(al)equilibrium and that total energy consumption is minimum.At present, CONTINUOUS REFORMER reaction pressure has dropped to 0.35MPa, and hydrogen/hydrocarbon mol ratio drops to 1～3, and the RON of reformed oil can be up to 105.Along with the raising of CONTINUOUS REFORMER reaction severity, in reformed oil, the content of alkene also obviously improves.
For the reformer of producing gasoline, C
6cut need to enter the de-benzene of extraction plant; For the reformer C that produces aromatic hydrocarbons
6, C
7cut all needs extracting separated.Because the selectivity of extraction solvent is limited, extract the alkene that contains some amount in aromatic hydrocarbons out.In extracting charging, olefin(e) centent is higher, and the olefin(e) centent of extracting out in aromatic hydrocarbons is also higher, also there will be alkene accumulation in backflow aromatic hydrocarbons, has influence on aromaticity content when serious.In addition, alkene also easily produces polymerization and pollutes extraction solvent in extractive process, and alkene generation oxidizing reaction generates the heavy corrosion that organic acid causes extraction system equipment simultaneously.If do not remove alkene wherein, also may cause the bromine index of aromatic hydrocarbon product and pickling color defective, bromine index and the copper strip test of solvent oil are defective.
At present, the Technology of company's exploitation both at home and abroad mainly, by part cut in reformed oil or full cut being carried out to selective hydrogenation or non-hydrogen reaction as post-treating methods such as bleaching earth adsorptions, reaches the object of reduction content of olefin in reformate.The type of used catalyst is different with regeneration, and technical process is also corresponding has different forms.
CN1152605A discloses a kind of process for selective hydrogenation of removing alkene from reformed oil, is in magnetically stabilized bed reactor, makes liquid reformate generate oil and contacts with a kind of ferromegnetism hydrogenation catalyst with hydrogen.Its reaction conditions is: 50～220 ℃ of temperature of reaction, reaction pressure 0.1～3MPa, reaction velocity 2～40 hours
-1, hydrogen/oil ratio 40～150.
CN1250799A discloses a kind of reformed oil olefine saturation hydrogenation method, is included under catalyzer existence, and reformed oil is contacted with hydrogen, and the condition of contact is 50～200 ℃ of temperature, and pressure is greater than 0.1MPa, liquid hourly space velocity 0.1～20 hour
-1, hydrogen/oil ratio is greater than 30; Described catalyzer contains a kind of porous carrier materials, a kind of group VIII metal and is selected from one or both the element in boron, phosphorus, described group VIII metal exists and is carried in porous carrier materials with the form of amorphous alloy, the content of group VIII metal and boron and/or phosphorus is 0.1～60 quality %, and the atomic ratio of group VIII metal element and boron and/or phosphorus is 0.5～10.
CN1394937A discloses a kind of reformed oil olefine saturation hydrogenation method, is included under a kind of catalyzer existence, and reformed oil is contacted with hydrogen, and the temperature of contact is 200～320 ℃, and pressure is not less than 0.7MPa, and liquid hourly space velocity is 1～8 hour
-1, hydrogen/oil volume ratio is not less than 30.Described catalyzer contains Tungsten oxide 99.999 and/or molybdenum oxide, nickel oxide and the cobalt oxide loading on alumina supporter.
CN1448474A discloses a kind of reformed oil selective hydrogenation and olefin hydrocarbon removal catalyzer.This catalyzer, containing the precious metal of 0.1～1.0 quality %, is active ingredient, and the basic metal of 0.05～0.50 quality % or alkaline-earth metal, be auxiliary agent, and support of the catalyst is refractory inorganic oxides.The surface-area of catalyzer is 150～250m
2/ g, pore volume is 0.3～0.8ml/g.150～250 ℃ of temperature of reaction, pressure 1.5～3.0MPa, volume space velocity 2.0～4.0 hours
-1under condition, the bromine index of product is less than 100mgBr/100g oil, and aromatic hydrocarbons loss is less than 0.5 quality %.
CN101260320A discloses a kind of CONTINUOUS REFORMER gasoline selective hydrogenation and olefin hydrocarbon removal catalyzer and preparation method.The distinguishing feature of this catalyzer is that noble metal active component is eggshell type distribution on carrier, and its advantage is to have significantly improved on the one hand the utilization ratio of noble metal active component, has reduced content and the catalyzer cost of noble metal active component; Significantly reduce on the other hand the activity of aromatic hydrogenation, improved the selectivity of hydrogenation of olefins, reduced aromatic hydrogenation loss.
CN1618932A disclose a kind of under conditions of non-hydrogen the method for catalytic refining reforming aromatic oil.It is carrier that the catalyzer adopting be take aluminum oxide or kaolin, and molecular sieve is active component.Molecular sieve can be used β, Y, SAPO, ZSM-5, SRCY and super stable molecular sieve.Adopt the method catalytic treatment reforming aromatic oil, 100～300 ℃ of temperature of reaction, reaction pressure 1.0～2.0MPa, air speed 0.5～4.0 hour
-1under condition, can effectively remove the trace amounts of olefin in aromatic hydrocarbons.
CN101474568A discloses a kind of selective hydrogenation and olefin hydrocarbon removal double-metal phosphide Catalysts and its preparation method.The auxiliary agent of this catalyzer is TiO
2or rare-earth oxide, Primary Catalysts is the phosphide of a kind of transition metal in Mo, W, Fe, Co or Ni, catalyzer is by preparing its oxidation state precursor temperature programmed reduction(TPR).When promotor and Primary Catalysts mol ratio are 0.01～0.5, can realize the selection hydrogenation to alkene in aromatic hydrocarbons, the basic free of losses of aromatic hydrocarbons.
CN1163879A discloses a kind of method of being produced pure aromatics by reformed gasoline, and reformed gasoline selective hydrogenation in the first process steps, is mainly that non-aromatics, particularly alkene, diolefine and alkatrienes are by hydrogenation.Thereafter in the second process steps, the product separation containing aromatic hydrocarbons of the selection hydrogenation the first process steps being obtained by extractive distillation and/or liquid-liquid extraction becomes aromatic hydrocarbons and non-aromatics.
US7304193B1 discloses a kind of method of producing the aromatic hydrocarbons such as benzene and p-Xylol, feed naphtha first passes through hydrotreatment, enter again reforming reactor and carry out catalytic reforming reaction, recapitalization generating oil hydrogenation reactor is undertaken saturated by alkene wherein, be mixed into separating unit with the product of isomerization unit again, separated benzene and dimethylbenzene wherein.Olefin saturated is wherein processed can adopt carclazyte, preferably uses olefins hydrogenation, and this catalyzer be take highly purified aluminum oxide as carrier, nickel-loaded or platinum metals, and content is about 2～40 quality %.Olefins hydrogenation reaction conditions is 20～200 ℃, 0.5～7.0MPa, and the stoichiometric ratio of hydrogen and alkene is 1～5: 1.
USP5817227 discloses a kind of method of benzene and lightweight unsaturated compound in elective reduction hydrocarbon fraction, this method passes into reformed oil in the catalytic distillation tower that has a hydrogenation catalyst bed at least, make lightweight unsaturated compound hydrogenation in the process of rectifying separation saturated, from distillation tower top, discharge C together with benzene
7 +component is discharged from bottom.This method also can increase saturated section of hydrogenation at distillation tower side line, so that from lateral line withdrawal function distillation component, carries out hydrogenation and sends distillation tower back to after saturated again and continue separated weight component.Hydrogenation catalyst used is nickel catalyzator or the aluminium oxide catalyst that carries platinum.
Summary of the invention
The object of this invention is to provide a kind of method that reduces content of olefin in reformate, this method is used conventional petroleum naphtha continuous reforming catalyst as the catalyzer of olefin saturated in reformed oil, save the independent regenerative process of olefins hydrogenation, can effectively reduce the olefin(e) centent in reformed oil.
The method of reduction content of olefin in reformate provided by the invention, be included in serial connection olefin saturated section in CONTINUOUS REFORMER reactive system, take continuous reforming catalyst as olefins hydrogenation, making the conversion of olefines in reformate is stable hydrocarbon, and described continuous reforming catalyst comprises take the VIII family metal that content that inorganic oxide carrier is benchmark is 0.1～5.0 quality %, the IV A family metal of 0.1～5.0 quality %, the halogen of 0.1～5.0 quality %.
The inventive method is integrated CONTINUOUS REFORMER and olefins hydrogenation, make reforming catalyst be used to olefin saturated under olefin saturation condition, avoid the additional catalyst regeneration process of olefins hydrogenation of independent other composition of use, simplified the operation steps of technique.
Embodiment
The inventive method is connected in series olefin saturation device in continuous reformer reactive system, and loads continuous reforming catalyst.During reforming reaction, first petroleum naphtha is passed into continuous reforming reactor, the product that last reactor flows out is taken away after part heat by interchanger, enter olefin saturation device, under continuous reforming catalyst effect and olefin saturation condition, carry out olefin saturation, and then through heat exchange, send into the device of gas-liquid separator and postorder, production object product.
The inventive method is used continuous reforming catalyst as the catalyzer of olefin saturated in reformate, the VIII family metal content of described olefins hydrogenation is 0.1～1.0 quality % preferably, IV A family metal content is 0.1～2.0 quality % preferably, and content of halogen is 0.5～3.0 quality % preferably.Outside described metal HeⅣ A family of olefins hydrogenation Chu Han VIII family metal, the 3rd metal constituent element that also contains 0.01～5.0 quality %, and can further contain the 4th metal constituent element of 0.01～5.0 quality %, the 3rd, preferred 0.1～2.0 quality % of the content of the 4th metal constituent element.
The preferred platinum of VIII family metal of the reforming catalyst for olefin saturation described in the inventive method, the preferred tin of IV A family metal, the preferred chlorine of halogen.The described preferred europium of the 3rd, the 4th metal constituent element, cerium or titanium.Described inorganic oxide carrier preferential oxidation aluminium, more preferably gama-alumina.
The preparation method of continuous reforming catalyst can be referring to CN1039917C, CN1234455C, CN100338189C, CN1715370A, CN101294102A, CN1696253A etc.
Described continuous reforming catalyst needs to process through super-dry, reduction before contact stock oil.The reduction of catalyzer can be carried out before catalyzer packs reactor into, also can after catalyzer packs reactor into, carry out.
Described in the inventive method, the reaction pressure of olefin saturated section is 0.3～1.0MPa, preferred 0.35～0.8MPa, and temperature is 100～400 ℃, preferably 200～350 ℃.The volume space velocity of olefin saturated section is 10～50 hours
-1, preferably 10～40 hours
-1, hydrogen/hydrocarbon mol ratio is 1～20: 1, preferably 2～8: 1.
The present invention's olefin saturation device used can be moving-bed, and the catalyzer of olefin saturated section participates in circulation and the regeneration of reforming catalyst; Also can be fixed bed, after the catalyst deactivation of olefin saturated section, be cemented out, the online feeding equipment by continuous reformer continues to use after joining the activity recovery of regenerating in the recycle system of continuous reforming catalyst.
Olefin saturated section of the present invention can be gone here and there after the last reactor of reforming reactor, use is olefins hydrogenation without the reforming catalyst of regeneration, also can go here and there before first reactor, using the reforming catalyst through regeneration is olefins hydrogenation.
The inventive method is utilized continuous reformer own resources and equipment, only need to increase an olefin saturation device, and interchanger before and after corresponding according to the condition configuration of olefin saturation, while needing, can increase catalyzer lift technique.
The inventive method is applicable to the olefine saturation hydrogenation of CONTINUOUS REFORMER product, therefore, coordinates continuous reforming process to use.The stock oil of described CONTINUOUS REFORMER can be that virgin naphtha, hydrocracking heavy naphtha, hydrotreated coker gasoline, cracking of ethylene gasoline are raffinated oil, catalytically cracked gasoline, can be also the mixture of several raw materials wherein.The initial boiling point of described stock oil is generally 60～95 ℃, and final boiling point is generally 135～180 ℃.The impurity of reforming raw oil requires: sulphur < 0.5 μ g/g, nitrogen < 0.5 μ g/g, arsenic < 1ng/g, plumbous < 10ng/g, copper < 10ng/g, water < 5 μ g/g.
The temperature of described reforming reaction is 430～560 ℃, preferably 490～530 ℃; Feed volume air speed 0.1～10.0 hour
-1, preferably 0.5～2.0 hour
-1; Pressure is 0.3～1.0MPa, preferred 0.35～0.8MPa; Hydrogen/hydrocarbon mol ratio is 1.5～9.0: 1, preferably 1.5～6.0: 1.
Below by example, further illustrate the present invention, but the present invention is not limited to this.
Comparative example 1
By four fixed-bed reactor series connection, load conventional continuous reforming catalyst A in first three reactor according to a conventional method, loading amount is followed successively by 60ml, 90ml, 150ml, and catalyzer is super-dry and reduction processing before packing reactor into.Petroleum naphtha shown in table 1 is passed into three reforming reactors successively, the material flowing out from reforming reactor enters high-pressure gas-liquid separator and carries out gas-liquid separation through overcooling is laggard, and the part in isolated gas is returned to the first reactor inlet and circulated after compressor boost.Reforming catalyst composition used, reaction conditions and reformation product liquid form in Table 2, and wherein aromatics yield is C
5 +liquid product yield and the wherein product of aromaticity content, catalyst A active component content is with carrier γ-Al
2o
3for benchmark.
Comparative example 2
By the method for example 1, carry out reforming reaction, different is to change reforming reaction condition, and reaction conditions and reformation product liquid form in Table 2.
Comparative example 3
Adopt the testing apparatus in comparative example 1, wherein first three reactor loads the reforming catalyst B of load list platinum on chloride alumina supporter successively, and its platinum content is 0.5 quality %, and cl content is 1.0 quality % (all take alumina supporter as calculating benchmark).Loading amount is followed successively by 60ml, 90ml, 150ml, and last reactor is as olefin saturation device, and filling 15ml catalyst B is as olefin saturation catalyzer.Petroleum naphtha shown in table 1 is passed into four reactors successively, the material flowing out from the 4th reactor enters high-pressure gas-liquid separator and carries out gas-liquid separation through overcooling is laggard, and the part in isolated gas is returned to the first reactor inlet and circulated after compressor boost.The reaction conditions of reformation and olefin saturated and final product liquid form in Table 3.
Example 1
Adopt the testing apparatus in comparative example 1, wherein first three reactor loads conventional continuous reforming catalyst A 60ml, 90ml, 150ml successively, and the 4th reactor is as olefin saturation device, and filling 15ml catalyst A is as olefin saturation catalyzer.The reaction conditions of reformation and olefin saturated and final product liquid form in Table 3.
Example 2～3
By the method for example 1, carry out catalytic reforming and olefin saturation, different is that the olefins hydrogenation loading in the 4th reactor of example 2 is 60ml, and olefin saturation temperature is different from example 1; Example 3 first three reforming reactor reaction conditions are identical with comparative example 2, and the olefins hydrogenation loading in the 4th reactor is 15ml.The reaction conditions of reformation and olefin saturated and final product liquid form in Table 3.
Example 4
By the method for example 1, carry out catalytic reforming and olefin saturation, different is that the catalyzer loading in four reactors is reforming catalyst C, and its platinum content is 0.35 quality %, and tin content is 0.30 quality %, titanium content is 0.10 quality %, and cl content is that 1.0 quality % are (all with carrier γ-Al
2o
3for benchmark).The reaction conditions of reformation and olefin saturated and final product liquid form in Table 3.
Example 5
By the method for example 1, carry out catalytic reforming and olefin saturation, different is that the catalyzer loading in four reactors is reforming catalyst D, its platinum content is 0.33 quality %, tin content is 0.30 quality %, europium content is 0.33 quality %, cerium content is 1.17 quality %, and cl content is that 1.20 quality % are (all with carrier γ-Al
2o
3for benchmark).The reaction conditions of reformation and olefin saturated and final product liquid form in Table 3.
Table 1
Table 2
Table 3
Claims (10)
1. a method that reduces content of olefin in reformate, be included in serial connection olefin saturated section in CONTINUOUS REFORMER reactive system, take continuous reforming catalyst as olefins hydrogenation, making the conversion of olefines in reformate is stable hydrocarbon, and described continuous reforming catalyst comprises take the VIII family metal that content that inorganic oxide carrier is benchmark is 0.1～5.0 quality %, the IV A family metal of 0.1～5.0 quality %, the halogen of 0.1～5.0 quality %.
2. in accordance with the method for claim 1, it is characterized in that described continuous reforming catalyst also contains the 3rd metal constituent element of 0.01～5.0 quality %.
3. in accordance with the method for claim 2, it is characterized in that described continuous reforming catalyst further contains the 4th metal constituent element of 0.01～5.0 quality %.
4. in accordance with the method for claim 1, it is characterized in that described VIII family metal is platinum, IV A family metal is tin, and halogen is chlorine.
5. according to the method described in claim 2 or 3, it is characterized in that the 3rd, the 4th described metal constituent element is selected from europium, cerium or titanium.
6. in accordance with the method for claim 1, it is characterized in that described inorganic oxide carrier is aluminum oxide.
7. the reaction pressure that in accordance with the method for claim 1, it is characterized in that olefin saturated section is that 0.2～1.0MPa, temperature are 200～350 ℃.
8. in accordance with the method for claim 1, the volume space velocity that it is characterized in that olefin saturated section is 10～40 hours-1, and hydrogen/hydrocarbon mol ratio is 2～8: 1.
9. in accordance with the method for claim 1, the olefin saturated section described in it is characterized in that is gone here and there after the last reactor of reforming reactor, and using the reforming catalyst without regeneration is olefins hydrogenation.
10. in accordance with the method for claim 1, the olefin saturated section described in it is characterized in that is gone here and there before first reactor, and using the reforming catalyst through regeneration is olefins hydrogenation.
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| CN110064421B (en) * | 2018-01-23 | 2021-11-30 | 中国石油天然气股份有限公司 | Reforming catalyst and preparation method thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1152605A (en) * | 1995-12-20 | 1997-06-25 | 中国石油化工总公司石油化工科学研究院 | Saturation hydrogenating process for removing olefines from reforming produced oil |
| CN1250799A (en) * | 1998-10-13 | 2000-04-19 | 中国石油化工集团公司 | Saturated hydrogenation of olefin of reforming oil |
| CN1394937A (en) * | 2001-07-10 | 2003-02-05 | 中国石油化工股份有限公司 | Reformed oil olefine saturation hydrogenation method |
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2010
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1152605A (en) * | 1995-12-20 | 1997-06-25 | 中国石油化工总公司石油化工科学研究院 | Saturation hydrogenating process for removing olefines from reforming produced oil |
| CN1250799A (en) * | 1998-10-13 | 2000-04-19 | 中国石油化工集团公司 | Saturated hydrogenation of olefin of reforming oil |
| CN1394937A (en) * | 2001-07-10 | 2003-02-05 | 中国石油化工股份有限公司 | Reformed oil olefine saturation hydrogenation method |
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