CN102533313B - Method for preparing ethylene and propylene through catalytic cracking - Google Patents
Method for preparing ethylene and propylene through catalytic cracking Download PDFInfo
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- CN102533313B CN102533313B CN201010591015.1A CN201010591015A CN102533313B CN 102533313 B CN102533313 B CN 102533313B CN 201010591015 A CN201010591015 A CN 201010591015A CN 102533313 B CN102533313 B CN 102533313B
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- propylene
- zeolite
- catalyst
- ethene
- catalyzer
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/52—Improvements relating to the production of bulk chemicals using catalysts, e.g. selective catalysts
Abstract
The invention discloses a method for preparing ethylene and propylene through catalytic cracking, wherein average particle diameter range of catalyst particles is 1-500 nm; and the method comprises the following steps of: uniformly dispersing the catalyst particles into a reactant; and reacting in a reactor to produce low-carbon-number olefin. The reactant is at least one of naphtha, diesel oil and hydrocarbon mixtures containing C4-C8 olefin; and the catalyst is preferably zeolite, more preferably at last one of ZSM-5 series zeolite, mordenite, beta zeolite and Y zeolite or a product obtained by modifying alkali metal oxide or rare earth metal oxide. By using the method, the yield of ethylene and propylene can be increased, the using amount of the catalyst can be reduced, and the cost can be reduced.
Description
Technical field
The present invention relates to organic chemical industry field, say further, relate to a kind of method that catalytic pyrolysis is prepared ethene and propylene.
Background technology
The catalyzer that petrochemical complex is used in producing, mainly contains heterogeneous catalyst and the large type of homogeneous catalyst two.Homogeneous catalyst is owing to being difficult to separate with product, and it is the method for homogeneous catalysis heterogenize that people attempt homogeneous catalyst to load on carrier, through research and probe for many years, unrealized industrialization so far, is mainly that the problem of loss of active component is difficult to solve.Because homogeneous catalyst exists above-mentioned shortcoming, therefore most industry catalyzer is heterogeneous catalyst.Use the following problem of heterogeneous catalyst ubiquity: 1, catalyst levels is large, and utilization ratio is low, and life cycle is short; 2, easily coking, need frequent regeneration; 3, in the catalyzer of inactivation, still have a lot of active ingredients not play a role, cause the wasting of resources etc.
Industrial catalytic cracking reaction mainly contains fixed bed reaction technique and fluidized-bed reaction technique.Fixed bed reaction technique is as disclosed methods such as CN1274342A, CN1313268A, WO 00/26163; Fluidized-bed reaction technique method as disclosed in CN1069016, CN1383448.
CN1274342A discloses by catalyzed conversion to contain 20% (weight) or higher (with the weighing scale of hydrocarbon feed) at least one C
4-C
12the straight chain hydrocarbon of alkene is the method for waste ethene and propylene.Zeolite in the zeolite catalyst that the method is used is substantially not containing proton, SiO
2/ Al
2o
3the zeolite that mol ratio is 200-5000, contain at least one IB family metal, intermediate pore size, the preferably zeolite of ZSM-5 family.Reaction at the temperature of 400-700 ℃, a 0.1-10 normal atmosphere and 1-1000h
-1weight hourly space velocity under carry out, the diluent gas of use comprises hydrogen, methane, steam and rare gas element, can obtain and be up to 6.5% ethylene yield and 22.7% productivity of propylene.
CN1313268A discloses with C
2-C
5hydrocarbon gas, if Sweet natural gas, liquefied petroleum gas (LPG) or catalytic cracked gas are the method for waste ethene.WO 00/26163 discloses to contain C
4and C
5the mixture of alkene is raw material, prepares the method for ethene and propylene under zeolite catalyst exists.
CN1069016 discloses a kind of method of preparing ethene by direct conversion of heavy hydrocarbon, the method is in fluidized-bed or plug flow reactor, adopt solid particulate contact substance and stock oil to carry out conversion reaction, in reaction zone, can add water vapour or including other gas containing hydrogen, methane etc.CN1383448 discloses one selectivity in fluid catalytic cracking process and has produced C
3the method of alkene, the method is used feed naphtha logistics to contact with catalyzer in reaction zone, this catalyzer is less than the crystalline zeolite of about 0.7nm containing the 10-50% weighted average bore dia of having an appointment, reaction conditions comprises that temperature of reaction is about 500-650 ℃, and the dividing potential drop of hydrocarbon is about 10-40psia.
Because fixed bed reaction technique is used heterogeneous catalyst, main drawback is exactly that catalyzer is easily coking, and life cycle is short, needs frequent regeneration; The main drawback of fluidized-bed reaction technique is not only to invest greatly, and in product, contains nitrogen and oxygen, causes and the difficulty that gently component separates such as hydrogen, methane, ethene.Therefore, in order to reduce the production cost of heterogeneous catalyst, give full play to the effect of active ingredient, need solve with a kind of new catalytic cracking method the shortcoming of existing fixed bed and fluidized-bed process existence.
Summary of the invention
For solving problems of the prior art, the invention provides a kind of method that catalytic pyrolysis is prepared ethene and propylene, can improve selectivity of catalyst, reduce catalyst levels, reduce costs, give full play to the effect of active ingredient.
The object of this invention is to provide a kind of catalytic pyrolysis and prepare the method for ethene and propylene.
Wherein the average particle size range of granules of catalyst is 1～500nm, preferably 10～100nm;
Said method comprising the steps of:
Granules of catalyst is dispersed in reactant, in reactor, reacts, generate olefine in low carbon number, separating, make ethene and propylene.
Wherein reactant is preferably petroleum naphtha, diesel oil and contains C
4-C
8at least one in the hydrocarbon mixture of alkene;
The catalyzer adopting in the method for the invention can be all catalyzer for catalytic cracking reaction in prior art, and its particle size range meets particle size range of the present invention.Catalyzer preferred zeolite, more preferably at least one in ZSM-5 series zeolite, mordenite, β zeolite and Y zeolite or its product with alkalimetal oxide or rare-earth oxide modification; The ZSM-5 series zeolite that particularly preferably silica alumina ratio is 10～500, mordenite, β zeolite and Y zeolite that silica alumina ratio is 5～60.
Described reactor can be suspension bed, fluidized-bed or tubular reactor.
Described catalyzer is dispersed in reactant, and the content of catalyzer is 1～1000ppm, makes catalyzer and reactant evenly under admixture, carry out catalytic cracking reaction, generates olefine in low carbon number; Preferably described zeolite catalyst is dispersed in reactant, and the content of catalyzer is 10～500ppm.
Catalytic cracking method of the present invention can carry out under the condition of common catalytic cracking reaction, is that 450～750 ℃, pressure are 0.01～0.5MPa, 3～30h in temperature
-1the condition of volume hourly space velocity under react.
The method of the invention is heterogeneous catalyst under homogeneously dispersed state and reacts in reaction process, and after reaction product is cooling, catalyzer is present in liquid-phase product, can from liquid phase composition, reclaim by distillation.
In specific embodiments, can be used for C
5-C
8the catalytic pyrolysis of conversion of olefines, petroleum naphtha or diesel oil, can adopt steam cracking boiler tube or fixed-bed reactor, and detailed process is as follows:
Catalyzer is dispersed in containing C
5-C
8in the raw material of the hydrocarbon mixture of alkene, the median size of catalyzer is 10～100nm, and the content in raw material is 10～500ppm, at pressure and the 3～30h of the temperature of 450～650 ℃, 0.01～0.5MPa
-1the processing condition of volume hourly space velocity under, in reactor, react, generate the reaction mixture that contains propylene and ethene, after refrigerated separation, obtain ethene and propylene;
Catalyzer is dispersed in the raw materials such as petroleum naphtha, the median size of catalyzer is 10～300nm, and the content in raw material is 10～500ppm, at pressure and the 3～30h of the temperature of 450～750 ℃, 0.01～0.5MPa
-1the processing condition of volumctric hourly space velocity under, in reactor, react, generate and contain C
1, C
2, C
3, C
4, C
5deng reaction mixture, after refrigerated separation, obtain ethene and propylene.
Method provided by the invention can be used as the method for preparing separately ethene and propylene, also can combine use with the device of preparing ethylene by steam cracking.
It is the reaction of gas that method of the present invention is applicable to reaction product, is applicable to the heterogeneous catalytic reaction in petrochemical complex and fine chemistry industry, as the reaction of solar oil or mink cell focus catalytic pyrolysis preparing ethylene, propylene; C
2～C
5high unsaturated hydrocarbons select the reaction of Hydrogenation for monoolefine or full hydrogenation; The catalyzed reaction such as gasoline hydrodesulfurizationmethod, denitrogenation.
Effect of the present invention is as follows:
1, due to nanoscale molecular sieve catalyst is dispersed in reactant, greatly strengthen mass transfer process, reduced the impact on catalyzed reaction of diffusion process between reaction mass and catalyzer and between reaction product and catalyzer, therefore by product obviously reduces, selectivity significantly improves.
2, use method of the present invention, by simplifying the preparation method of catalyzer in prior art, reduce catalyst levels, reduce costs, give full play to the effect of active ingredient.
3, method of the present invention makes catalyzer homogeneously dispersed state in reaction process, and the cooling rear catalyst of reaction product is present in liquid phase, can conveniently reclaim or reuse, and reduces environmental pollution.
Accompanying drawing explanation
Fig. 1 is the schematic flow sheet of catalytic cracking method of the present invention.
Description of reference numerals
1 peristaltic pump 2 process furnace 3 fixed-bed reactor 4 water cooler 5 gas-liquid separators
Embodiment
Below in conjunction with embodiment, further illustrate the present invention.
As shown in Figure 1:
Fixed-bed reactor 3 are installed, after logical N2 leak test, opening process furnace 2 heats, temperature is opened peristaltic pump 1 after rising to temperature of reaction, raw material enters fixed-bed reactor 3 through peristaltic pump 1 after mixing under high-speed stirring with catalyzer, reaction product after water cooler 4, gas-liquid separator 5 separates, gas phase wet test meter measurement volumes, liquid phase is collected with Erlenmeyer flask.Catalyzer is present in liquid phase, pours out supernatant liquid, filtration, collection catalyst by fractionation by distillation or after leaving standstill.The catalyzer of collecting is dried, reusable after 580 ℃ of burnings in retort furnace.Analyze the composition of gas phase and liquid phase with gas chromatograph.
Embodiments of the invention and comparative example are all used small fixed reactor to react, and reactor is the stainless steel tube of internal diameter ф 16mm, wall thickness 2mm, isothermal section volume 20ml.
In embodiment and comparative example, the source of used catalyst is commercially available.
Embodiment 1
Carbon five hydrocarbon mixtures that do not contain diolefin take oil of SPC chemical institute are as raw material, and it consists of (wt%):
Iso-pentane 6.79, Skellysolve A 46.12, trans-2-amylene 8.60,1-amylene 7.75,
2-methyl-2-butene 7.17,2-methyl-1-butene alkene 17.33, cis-2-amylene 5.07.
By 0.3g ZSM-5 zeolite (SiO
2/ Al
2o
3mol ratio is 200, median size 30nm) add in 1kg carbon five hydrocarbon mixtures, catalyst content 300ppm, under agitation in peristaltic pump 1 enters fixed-bed reactor 3; At pressure 0.1MPa, 550 ℃ of temperature, volume hourly space velocity 5h
-1under react.Reaction product after water cooler 4, gas-liquid separator 5 refrigerated separation, gas phase wet test meter measurement volumes, liquid product is collected with Erlenmeyer flask, leave standstill after pour out supernatant liquid, filter, collection catalyst.The catalyzer of collecting is dried, reusable after 580 ℃ of burnings in retort furnace.The composition of analyzing gas phase with gas chromatograph, the composition of gas phase primary product is listed in table 1.
Comparative example 1
By the ZSM-5 zeolite 50g identical with embodiment 1 and 10g specific surface area > 200m
2the high-purity silicon oxide of/g, 2g sesbania powder mix, and add 5% the about 80ml of nitric acid after mixing, and are squeezed into the cylindrical type of 2mm after stirring evenly, and can obtain the catalyzer of 2 × 2.5mm after dry, roasting.In the fixed-bed reactor identical with embodiment 1, filling 20ml catalyzer reacts under the condition identical with embodiment 1.The composition of analyzing gas phase with gas chromatograph, the composition of gas phase primary product is listed in table 1.
The petroleum naphtha used take Yanshan Petrochemical ethylene plant is as raw material, and the boiling range of petroleum naphtha is 32-156 ℃, (wt%) composed as follows:
By 0.3g ZSM-5 zeolite (SiO
2/ Al
2o
3mol ratio is 200, and median size is 100nm) add in 1kg petroleum naphtha, catalyst content 300ppm, at pressure 0.1MPa, 650 ℃ of temperature, volume hourly space velocity 5h
-1condition under react, other step is identical with embodiment 1.The composition of gas phase primary product is listed in table 1.
Comparative example 2
By the preparation method of the catalyzer described in comparative example 1, by the ZSM-5 zeolite 50g identical with embodiment 2 and silicon oxide 10g mixing moulding, obtain the catalyzer of 2 × 2.5mm.
In the fixed-bed reactor identical with embodiment 2, the catalyzer of the above-mentioned preparation of filling 20ml reacts under the condition identical with embodiment 2.The composition of gas phase primary product is listed in table 1.
Take Yanshan Petrochemical refinery solar oil as raw material, its boiling range is 193-384 ℃, (wt%) composed as follows:
Paraffinic hydrocarbons 59.7, naphthenic hydrocarbon 30.3, aromatic hydrocarbons 10.0.
By 0.2g mordenite (SiO
2/ Al
2o
3mol ratio is 30, and median size is 200nm) add in 1kg solar oil, catalyst content 200ppm, at pressure 0.1MPa, 650 ℃ of temperature, volume hourly space velocity 5h
-1condition under react, other step is identical with embodiment 1.The composition of gas phase primary product is listed in table 1.
Comparative example 3
By the preparation method of the catalyzer described in comparative example 1, by the mordenite 50g identical with embodiment 3 and silicon oxide 10g mixing moulding, obtain the catalyzer of 2 × 2.5mm.
In the fixed-bed reactor identical with embodiment 3, the catalyzer of the above-mentioned preparation of filling 20ml reacts under the condition identical with embodiment 3.The composition of gas phase primary product is listed in table 1.
Embodiment 4
Take Yanshan Petrochemical refinery 101 diesel oil as raw material, its boiling range is 199.3-436.5 ℃, (wt%) composed as follows:
Paraffinic hydrocarbons 52.1, naphthenic hydrocarbon 42.4, aromatic hydrocarbons 5.5.
By 0.2g mordenite (SiO
2/ Al
2o
3mol ratio is 30, and median size is 400nm) add in 1kg diesel oil, catalyst content 200ppm, at pressure 0.2MPa, 650 ℃ of temperature, volume hourly space velocity 5h
-1condition under react, other step is identical with embodiment 1.The composition of gas phase primary product is listed in table 1.
Comparative example 4
By the preparation method of the catalyzer described in comparative example 1, by the mordenite 50g identical with embodiment 4 and silicon oxide 10g mixing moulding, obtain the catalyzer of 2 × 2.5mm.In the fixed-bed reactor identical with embodiment 4, the catalyzer of the above-mentioned preparation of filling 20ml reacts under the condition identical with embodiment 4.The composition of gas phase primary product is listed in table 1.
Take petroleum naphtha as raw material (identical with embodiment 2), by 0.1g ZSM-5 zeolite (SiO
2/ Al
2o
3mol ratio is 200, and median size is 100nm) and 0.1g mordenite (SiO
2/ Al
2o
3be 30, median size is 200nm) mix, add in 1kg petroleum naphtha, catalyst content 200ppm, at pressure 0.1MPa, 650 ℃ of temperature, volume hourly space velocity 5h
-1condition under react, other step is identical with embodiment 1.The composition of gas phase primary product is listed in table 1.
Comparative example 5
By the preparation method of the catalyzer described in comparative example 1, by the ZSM-5 zeolite 25g identical with embodiment 5 and mordenite 25g and silicon oxide 10g mixing moulding, obtain the catalyzer of 2 × 2.5mm.
In the fixed-bed reactor identical with embodiment 5, the catalyzer of the above-mentioned preparation of filling 20ml reacts under the condition identical with embodiment 5.The composition of gas phase primary product is listed in table 1.
Embodiment 6
Take petroleum naphtha as raw material (identical with embodiment 2), by 0.2g ZSM-5 zeolite (SiO
2/ Al
2o
3mol ratio is 200, median size 100nm) and 0.2g mordenite (SiO
2/ Al
2o
3mol ratio is 30, and median size is 200nm) mix, add in 1kg petroleum naphtha, catalyst content 400ppm, at pressure 0.1MPa, 650 ℃ of temperature, volume hourly space velocity 5h
-1condition under react, other step is identical with embodiment 1.The composition of gas phase primary product is listed in table 1.
Embodiment 7
Take petroleum naphtha as raw material (identical with embodiment 2), by 0.2g SAPO-34 zeolite (SiO
2/ P
2o
5/ Al
2o
3mol ratio is 1: 1: 1, and median size is 100nm), add in 1kg petroleum naphtha, catalyst content 200ppm, at pressure 0.1MPa, 650 ℃ of temperature, volume hourly space velocity 5h
-1condition under react, other step is identical with embodiment 1.The composition of gas phase primary product is listed in table 1.
The composition (wt%) of table 1 gas-phase reaction product
| Raw material | Temperature of reaction (℃) | Factor of created gase (wt%) | Ethene | Propylene | |
| Embodiment 1 | Carbon five hydrocarbon mixtures | 550 | 65 | 15.58 | 35.22 |
| |
Petroleum naphtha | 650 | 75 | 18.16 | 30.05 |
| |
Solar oil | 650 | 72 | 16.32 | 28.15 |
| Embodiment 4 | Diesel oil | 650 | 70 | 15.36 | 27.46 |
| |
Petroleum naphtha | 650 | 78 | 18.65 | 32.56 |
| Embodiment 6 | Petroleum naphtha | 650 | 82 | 18.95 | 33.98 |
| Embodiment 7 | Petroleum naphtha | 650 | 80 | 18.12 | 33.21 |
| Comparative example 1 | Carbon five hydrocarbon mixtures | 550 | 62 | 13.02 | 34.16 |
| Comparative example 2 | Petroleum naphtha | 650 | 72 | 17.06 | 28.39 |
| Comparative example 3 | Solar oil | 650 | 70 | 15.52 | 27.86 |
| Comparative example 4 | Diesel oil | 650 | 65 | 13.85 | 26.25 |
| Comparative example 5 | Petroleum naphtha | 650 | 75 | 17.32 | 30.27 |
Data from table 1 can find out, under identical reaction conditions, in embodiment of the present invention, the content of ethene and propylene is apparently higher than comparative example, and in embodiment, the consumption of catalyzer is far smaller than the consumption of catalyzer in comparative example.Therefore, method of the present invention can improve the productive rate of ethene and propylene, reduces the consumption of catalyzer, reduces costs.
Claims (7)
1. catalytic pyrolysis is prepared a method for ethene and propylene, it is characterized in that:
Granules of catalyst is dispersed in reactant, in reactor, reacts, generate olefine in low carbon number;
Described catalyzer is at least one or its product with alkalimetal oxide or rare-earth oxide modification in mordenite, β zeolite and Y zeolite;
The average particle size range of granules of catalyst is 1～500nm.
2. catalytic pyrolysis as claimed in claim 1 is prepared the method for ethene and propylene, it is characterized in that:
The particle size range of described granules of catalyst is 10～100nm.
3. catalytic pyrolysis as claimed in claim 1 is prepared the method for ethene and propylene, it is characterized in that:
Described reactant is petroleum naphtha, diesel oil and contains C
4-C
8at least one in the hydrocarbon mixture of alkene.
4. catalytic pyrolysis as claimed in claim 1 is prepared the method for ethene and propylene, it is characterized in that:
Silica alumina ratio in described mordenite, β zeolite and Y zeolite is 5～60.
5. catalytic pyrolysis as claimed in claim 1 is prepared the method for ethene and propylene, it is characterized in that:
Described reactor is suspension bed, fluidized-bed or tubular reactor.
6. catalytic pyrolysis as claimed in claim 1 is prepared the method for ethene and propylene, it is characterized in that:
The content of described catalyzer in reactant is 1～1000ppm.
7. catalytic pyrolysis as claimed in claim 6 is prepared the method for ethene and propylene, it is characterized in that:
The content of described catalyzer in reactant is 10～500ppm;
Temperature is 450～750 ℃, and pressure is 0.01～0.5MPa;
The volume space velocity of reactant is 3～30h
-1.
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|---|---|---|---|
| CN201010591015.1A CN102533313B (en) | 2010-12-16 | 2010-12-16 | Method for preparing ethylene and propylene through catalytic cracking |
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| CN102533313B true CN102533313B (en) | 2014-05-28 |
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| CN108238837B (en) * | 2016-12-27 | 2021-04-30 | 中国石油天然气股份有限公司 | Method for producing low-carbon olefin by catalytic cracking |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1796491A (en) * | 2004-12-23 | 2006-07-05 | 中国石油化工股份有限公司 | Catalytic cracking method |
| CN101584991A (en) * | 2008-05-23 | 2009-11-25 | 中国石油化工股份有限公司 | Catalyst for olefin catalytic cracking to produce propylene and ethylene and application thereof |
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- 2010-12-16 CN CN201010591015.1A patent/CN102533313B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1796491A (en) * | 2004-12-23 | 2006-07-05 | 中国石油化工股份有限公司 | Catalytic cracking method |
| CN101584991A (en) * | 2008-05-23 | 2009-11-25 | 中国石油化工股份有限公司 | Catalyst for olefin catalytic cracking to produce propylene and ethylene and application thereof |
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