CN1796491A - Catalytic cracking method - Google Patents
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Abstract
This invention describes a process for catalytic pyrolysis, comprising the steps of: (1) introducing the reactants into a pre-heater, wherein the reactants are vaporized into gases; (2) introducing the mixed solutions containing ultrafine or nanoscale catalyst into the pipeline between the pre-heater and the reactor, or directly into the reactor, wherein the said ultrafine or nanoscale catalyst is uniformly mixed with the process (1) wherein said gaseous reactants; (3) pyrolysis of the said uniform mixture in the reactor. The average diameter of the said ultrafine or nanoscale catalyst is in the range of 1nm-100mum. This invention resolves such problems existing in the present fixed-bed reaction process as easy carbonization of the catalyst, a short service periodic and frequent need for recovery. The process of this invention is easy to operate, and suitable for a wide variety of catalytic pyrolysis reactions. Compared with the present pyrolytic process, the process of this invention can increase the weight yield rate of ethylene+propylene+butadiene by at least 5%, while the equipment remains the same with only a feeding pipeline added.
Description
Technical field
The present invention relates to a kind of catalytic thermal cracking method, more specifically, relate to the method that a kind of petroleum hydrocarbon catalytic pyrolysis is produced olefine in low carbon number.
Background technology
The catalyzer that uses during petrochemical complex is produced mainly contains heterogeneous catalyst and homogeneous catalyst two major types.Homogeneous catalyst is owing to be difficult to separate with product, and people explored homogeneous catalyst is loaded on the carrier is the method for homogeneous catalysis heterogenize, explores through research for many years, and the industrialization of being unrealized so far mainly is that the problem of loss of active component is difficult to solve.Have above-mentioned shortcoming just because of homogeneous catalyst, therefore most of commercial catalystss are heterogeneous catalysts.Use the following problem of heterogeneous catalyst ubiquity: 1, catalyst levels is big, and utilization ratio is low, and life cycle is short; 2, easily tie charcoal, need frequent regeneration; 3, still have a lot of active ingredients not play a role etc. in the catalyzer of inactivation.
Industrial catalytic cracking reaction mainly contains fixed bed reaction technology and fluidized-bed reaction technology.Disclosed methods such as fixed bed reaction technology such as CN1274342A, CN1313268A, WO 00/26163; Fluidized-bed reaction technology such as CN1069016, the disclosed method of CN1383448.
It is the method that raw material is produced ethene and propylene in the straight chain hydrocarbon that contains 20% (weight) or higher (with the weight of hydrocarbon feed) at least a C4-C12 alkene that CN1274342A discloses by catalyzed conversion.Zeolite in the zeolite catalyst that this method is used be do not contain substantially proton, SiO2/Al203 mol ratio as 200-5000, contain the zeolite of at least a IB family metal, intermediate pore size, the zeolite of preferred ZSM-5 family.Be reflected under 400-700 ℃ the temperature, carry out under the weight hourly space velocity of a 0.1-10 normal atmosphere and 1-1000h-1, the diluent gas that uses comprises hydrogen, methane, steam and rare gas element, can obtain to be up to 6.5% ethylene yield and 22.7% productivity of propylene.
CN1313268A discloses the hydrocarbon gas with C2-C5, is the method that raw material is produced ethene as Sweet natural gas, liquefied petroleum gas (LPG) or catalytic cracked gas.It is raw material that WO00/26163 discloses with the mixture that contains C4 and C5 alkene, prepares the method for ethene and propylene in the presence of zeolite catalyst.
CN1069016 discloses a kind of method of preparing ethene by direct conversion of heavy hydrocarbon, this method is in fluidized-bed or plug flow reactor, adopt solid particulate contact substance and stock oil to carry out conversion reaction, can add water vapour in the reaction zone or comprise other gas that contains hydrogen, methane etc.CN1383448 discloses a kind of method that selectivity is produced C3 alkene in fluid catalytic cracking process, this method uses the feed naphtha logistics to contact with catalyzer at reaction zone, this catalyzer contains the crystalline zeolite of 10-50% weighted average bore dia less than about 0.7nm 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 technology is used heterogeneous catalyst, main drawback is exactly that catalyzer is easily tied charcoal, and life cycle is short, needs frequent regeneration; The main drawback of fluidized-bed reaction technology is not only to invest greatly, and contains nitrogen and oxygen in the product, causes and the light isolating difficulty of component such as hydrogen, methane, ethene.Therefore,, give full play to the effect of active ingredient, need a kind of new catalytic cracking method to solve the shortcoming of existing fixed bed and fluidized-bed process existence in order to reduce the production cost of heterogeneous catalyst.
Summary of the invention
The purpose of this invention is to provide a kind of catalytic thermal cracking method.
Catalytic cracking method of the present invention, it may further comprise the steps:
(1) reactant is introduced preheater, this reactant is vaporizated into gas through preheater;
(2) mixed solution that will contain super-refinement or nanocatalyst is introduced in the reactor without preheater ground, and the gas reactant in described super-refinement or nanocatalyst and the step (1) forms uniform mixture;
(3) described uniform mixture carries out catalytic cracking reaction in reactor;
Wherein, the median size of described super-refinement or nanocatalyst is 1nm-100 μ m.
In the inventive method, described reactant is selected from petroleum naphtha, diesel oil and contains at least a in the hydrocarbon mixture of C4-C8 alkene.
Described catalyzer is selected from least a in molecular sieve series, metal oxide, nonmetal oxide and nano-sized carbon, the nanometer iron.Wherein preferred molecular sieve series is selected from ZSM-5 series, SAPO (aluminosilicophosphate) series and their product by oxide modifyings such as magnesium, molybdenum or zirconiums, and the molecular sieve of preferred high silica alumina ratio, as silica alumina ratio is 50-500, more preferably the ZSM-5 of the high silica alumina ratio of 150-300 series molecular sieve.Described metal oxide concrete as: aluminum oxide, cerium oxide, ferric oxide, zinc oxide etc., wherein preferred aluminum oxide, described nonmetal oxide concrete as: silicon oxide.
In the inventive method, described super-refinement or nanocatalyst are meant that the particulate median size is the solid catalyst of 1nm-100 μ m, and preferred median size is 1-1000nm, more preferably 10-100nm.
The described mixed solution that contains super-refinement or nanocatalyst is with super-refinement or nanocatalyst homodisperse or is suspended in the liquid phase medium and the mixing solutions that obtains, and wherein said liquid phase medium is selected from least a in the liquid phase mediums such as water, hydrocarbon ils and aliphatic hydrocarbon.Described hydrocarbon ils is for example: petroleum naphtha, solar oil etc.Described aliphatic hydrocarbon is meant straight or branched hydrocarbon or its mixture of C6-C25.The concentration of described catalyzer in liquid does not have particular determination, decides on catalyst activity and downstream separation.
The used catalyzer of the inventive method can use the catalyst raw powder of the catalytic cracking reaction that is useful in the prior art, not moulding.Generally, the median size of catalyst raw powder satisfies the particle diameter of granules of catalyst of the present invention; If the median size of catalyst raw powder exceeds the particle size range of granules of catalyst of the present invention, be used further to method of the present invention after the disposal methods such as available grinding.
In existing thermal cracking process, as pyrolyzer etc., hydrocarbons needs through preheater its vaporizationization before entering reactor, and preheater is made of a plurality of U-shaped pipes or bend pipe, if therefore reactant liquid and solid catalyst are introduced preheater simultaneously, after reactant liquid is vaporized in preheater, just have in the bend that granules of catalyst is deposited on preheater, not only influence the utilising efficiency of catalyzer, and after the cracker long-time running, solid deposits will be unfavorable for the proper flow of liquid in preheater.
Therefore, method of the present invention is implemented by existing thermal cracker improves.Below will have thermal cracker now and be called main line, the equipment such as pipe connecting, valve that comprises preheater, reactor, chiller, condenser, wet test meter and connect them.The inventive method adds the mixed solution that contains the super-refinement catalyzer specially by a side line is set on main line, described side line is sent in the cracker main line as long as can will contain the mixed solution of super-refinement or nanocatalyst, do not have particular determination, can implement with the device that comprises mixed solution stirring storage tank, peristaltic pump or ram pump, pipe connecting, valve etc.Deposit in the preheater bend pipe for fear of solid catalyst, the opening for feed that described side line links to each other with main line should be arranged on after the outlet of preheater.In the inventive method, the described mixed solution that contains super-refinement or nanocatalyst can be introduced in the pipeline between preheater and the reactor, also directly in the injecting reactor.Because of the adding of cold material considerable change takes place for fear of reactor temperature, the opening for feed that described side line links to each other with main line is preferably disposed on before the reactor inlet, and described opening for feed and reactor inlet are preferably separated by a distance, the benefit of She Zhiing is to enter reactor by the catalyzer that side line enters main line again after reactant gas and pipeline preheating like this, can reduce the fluctuation of temperature in the reactor.
Method of the present invention is with reactant and the mixed solution that contains super-refinement or nanocatalyst charging respectively, reactant is vaporizated into gas through preheater, after the mixed solution that contains super-refinement or nanocatalyst enters the main line pipeline from the side line pipeline, the vaporization of also being heated, and form uniform mixture with gas reactant in the main line, this uniform mixture carries out catalytic cracking reaction in reactor, generate olefine in low carbon number.Olefine in low carbon number of the present invention refers to that carbon number is 2～4 alkene.
For the described mixed solution liquid that contains super-refinement or nanocatalyst that side line is injected is easy to vaporization, in the step (2) of the inventive method, can also adopt an atomized spray device that described mixed solution is vaporific and spray in the cracker main line, form uniform mixture with gas reactant.Described atomized spray device is preferably disposed on the opening for feed place that side line is connected with main line.Described atomized spray device does not have particular determination, uses conventional atomized spray device to get final product.
In the step (2) of the inventive method, can also under heated condition, add the mixed solution that contains super-refinement or nanocatalyst in the cracker, the temperature of heating can be decided according to the boiling point of described mixed solution liquid, be generally 20-400 ℃, as long as can make the mixed solution that contains the super-refinement catalyzer be flow state, be convenient to carry and add get final product.
In the inventive method, described reactor can be suspension bed, fluidized-bed or tubular reactor.
Catalytic cracking method of the present invention can carry out under the condition of common catalytic cracking reaction, is that 300-850 ℃, pressure are 0.1-0.5MPa, 1-15h in temperature preferably
-1The condition of volumctric hourly space velocity under react.
In the method for the present invention, catalyzer and reactant react under the state that forms uniform mixture, after the reaction product cooling, catalyzer is present in the liquid product, can solid catalyst be separated with liquid product by solid-liquid separating method such as filtering, centrifugal, look whether reclaiming of catalyzer cost determination.
Method provided by the invention can be used as the independent method for preparing low-carbon alkene (as ethene and propylene), also can combine use with the device of preparing ethylene by steam cracking.This method is applicable to some heterogeneous catalytic reactions in petrochemical complex and the fine chemistry industry, as the reaction of solar oil or mink cell focus catalytic pyrolysis preparing ethylene, propylene; The unsaturated hydrocarbon selective hydrogenation of C2-C5 prepares the reaction of monoolefine or full hydrogenation; Catalyzed reaction such as gasoline hydrodesulfurizationmethod, denitrogenation.
Method of the present invention can be used for various catalytic cracking reactions, only needs to add a reinforced side line pipeline on existing pyrolysis reaction device, just can make ethene+propylene+divinyl weight yield improve 5% at least.
Beneficial effect of the present invention is as follows:
1, in the inventive method, the heterogeneous catalyst of super-refinement or nanometer and reactant react forming under the state of uniform mixture, have solved in the fixed bed reaction technology catalyzer and have easily tied charcoal, and life cycle is short, needs the problem of frequent regeneration.
2, use method of the present invention, behind the heterogeneous catalyst super-refinement or nanometer that catalytic cracking reaction in the prior art is required, catalyst levels reduces, and utilization ratio improves, thereby can reduce the cost of catalyzer, gives full play to the effect of active ingredient.
3, the inventive method is simple, easy to operate, is suitable for various catalytic cracking reactions.As long as adding feeding pipe on existing pyrolysis reaction device can realize.Compare with the heat scission reaction method, can make ethene+propylene+divinyl weight yield improve 5% at least.
Description of drawings
Fig. 1 is a cat-cracker schematic flow sheet of the present invention.
1 main line valve, 2 preheaters, 3 mixed solutions stir storage tank 4 peristaltic pumps or ram pump 5 side line valves 6 reactors 7 chillers 8 condensers 9 wet test meters
Below in conjunction with accompanying drawing method of the present invention is described.
Main line valve 1, preheater 2, reactor 6, chiller 7, condenser 8,9 banded pipelines of wet test meter are called main line, and this main line is existing pipeline.Side line valve 5, peristaltic pump or ram pump 4, mixed solution stir 3 connecting pipelines of storage tank and are called side line, implement adding method of the present invention by this side line pipeline.
Fixed-bed reactor 6 are installed, and behind the logical N2 leak test, heating is treated to open main line valve 1 after temperature rises to assigned temperature, and stock oil and water enter reactor 6 after preheater 2 preheatings gasification.Simultaneously, open side line valve 5, the solid catalyst mixed solution that contains in the storage tank 3 is under agitation sent into reactor 6 through peristaltic pump 4, reaction product after chiller 7 and condenser 8 condensations and cooling, gas-liquid separation.Get the gas sample at regular intervals, analyze its composition with gas chromatograph.The cumulative volume of gas measures with wet test meter 9.Behind the reaction certain hour, collect accumulation liquid sample.Filter, separate solid particulate wherein, weighing.Calculate productive rate.
Embodiment
Below example will illustrate further the present invention, but not thereby limiting the invention.
Embodiments of the invention and Comparative Examples are all carried out in the small stationary bed bioreactor.Reactor is the stainless steel tube of 16mm * 2mm, isothermal section～400mm.(w% is that the gross weight with raw material is the weight percent of benchmark)
Embodiment 1
With swallow fossil cerebrol is raw material, its (w%) composed as follows:
C4-1.85，C5 6.96，C6 21.29，C7 19.29，C8 23.66，C9 16.04，C10 7.40，C11 2.61，C12 0.64。Wherein, normal paraffin 26.18, isoparaffin 33.66, naphthenic hydrocarbon 27.35, alkene 0.20, aromatic hydrocarbons 12.35, unknown material 0.26.
To make water-oil ratio be 1 petroleum naphtha enters preheater 2 with the flow of 0.3g/min, the water liquid that contains the 700ppm alumina in Nano level under agitation with the flow of 0.3g/min in the pipeline that peristaltic pump 4 adds between preheaters 2 and the reactor 6.Catalytic cracking reaction carries out under 785 ℃, gets the gas sample every 0.5hr and analyzes its composition.React after about 1 hour semi-invariant metering to gas phase and liquid product.Reaction result and gas phase primary product productive rate see Table 1.
Comparative Examples 1
To make water-oil ratio be 1 petroleum naphtha enters preheater 2 with the flow of 0.3g/min, pure water liquid with the flow of 0.3g/min in the pipeline that peristaltic pump 4 adds between preheaters 2 and the reactor 6.In addition, other reaction conditionss are with embodiment 1.Reaction result and gas phase primary product productive rate see Table 1.
Table 1
| Factor of created gase (w%) | Primary product productive rate (w%) | ||
| Ethene+propylene | Ethene+propylene+divinyl | ||
| The embodiment Comparative Examples | 75.82 62.78 | 38.46 31.27 | 43.28 38.46 |
Except that catalytic cracking reaction carried out under 790 ℃, other reaction conditionss were with embodiment 1, and reaction result and gas phase primary product productive rate see Table 2.
Comparative Examples 2
Except catalytic cracking reaction carries out under 790 ℃, other reaction conditionss are with Comparative Examples 1, and reaction result and gas phase primary product productive rate see Table 2.
Table 2
| Factor of created gase (w%) | Primary product productive rate (w%) | ||
| Ethene+propylene | Ethene+propylene+divinyl | ||
| The embodiment Comparative Examples | 78.68 70.97 | 41.83 38.02 | 47.07 38.47 |
With swallow fossil cerebrol is raw material, its (weight %) composed as follows:
C4-1.85，C5 6.96，C6 21.29，C7 19.29，C8 23.66，C9 16.04，C10 7.40，C11 2.61，C12 0.64。Wherein, normal paraffin 26.18, isoparaffin 33.66, naphthenic hydrocarbon 27.35, alkene 0.20, aromatic hydrocarbons 12.35, unknown material 0.26.
To make water-oil ratio be 1 petroleum naphtha enters preheater 2 with the flow of 0.3g/min, contain the alkali-earth metal modified ZSM-5 molecular sieve of 700ppm (particle diameter＜160 orders) water liquid under agitation with the flow of 0.-1g/min in the pipeline that peristaltic pump 4 adds between preheaters 2 and the reactor 6.Catalytic cracking reaction carries out under 750 ℃ respectively, gets the gas sample every 0.5hr and analyzes its composition.React after about 1 hour semi-invariant metering to gas phase and liquid product.Reaction result and gas phase primary product productive rate see Table 3 respectively.
Comparative Examples 3
To make water-oil ratio be 1 petroleum naphtha enters preheater 2 with the flow of 0.3g/min, pure water liquid with the flow of 0.1g/min in the pipeline that peristaltic pump 4 adds between preheaters 2 and the reactor 6.In addition, other reaction conditionss are with embodiment 3.Reaction result and gas phase primary product productive rate see Table 3.
Table 3
| Factor of created gase (w%) | Primary product productive rate (w%) | ||
| Ethene+propylene | Ethene+propylene+divinyl | ||
| The embodiment Comparative Examples | 70.92 62.12 | 36.66 31.33 | 41.03 34.95 |
Embodiment 4
Except catalytic cracking reaction carries out under 730 ℃, other reaction conditionss are with embodiment 3, and reaction result and gas phase primary product productive rate see Table 4.
Comparative Examples 4
Except catalytic cracking reaction carries out under 730 ℃, other reaction conditionss are with Comparative Examples 3, and reaction result and gas phase primary product productive rate see Table 4.
Table 4
| Factor of created gase (w%) | Primary product productive rate (w%) | ||
| Ethene+propylene | Ethene+propylene+divinyl | ||
| The embodiment Comparative Examples | 68.25 60.88 | 33.71 29.12 | 37.62 32.52 |
From table 1-table 4 as can be seen, catalytic cracking method of the present invention is compared with thermal-cracking method, and the weight yield of ethene+propylene+divinyl has improved 5% at least.
Claims (11)
1. catalytic thermal cracking method, it may further comprise the steps:
(1) reactant is introduced preheater, this reactant is vaporizated into gas through preheater;
(2) mixed solution that will contain super-refinement or nanocatalyst is introduced in the reactor without preheater ground, and the gas reactant in described super-refinement or nanocatalyst and the step (1) forms uniform mixture;
(3) described uniform mixture carries out catalytic cracking reaction in reactor;
Wherein, the median size of described super-refinement or nanocatalyst is 1nm-100 μ m.
2. the method for claim 1 is characterized in that, adopts the mixed solution that the atomized spray device will contain super-refinement or nanocatalyst to be in the vaporific introducing reactor.
3. the method for claim 1 is characterized in that, the mixed solution that will contain super-refinement or nanocatalyst is introduced in the reactor under heated condition.
4. the method for claim 1 is characterized in that, the median size of described super-refinement or nanocatalyst is 1-1000nm.
5. method as claimed in claim 4 is characterized in that, the median size of described super-refinement or nanocatalyst is 10-100nm.
6. the method for claim 1 is characterized in that described catalyzer is selected from least a in molecular sieve series, metal oxide, nonmetal oxide, nano-sized carbon and the nanometer iron.
7. method as claimed in claim 6, it is characterized in that described molecular sieve catalyst series is selected from ZSM-5 series molecular sieve, aluminosilicophosphate SAPO series molecular sieve, a kind of by among the ZSM-5 molecular sieve of magnesium, molybdenum or Zirconium oxide modification and the SAPO molecular sieve.
8. method as claimed in claim 7 is characterized in that, described molecular sieve is that silica alumina ratio is the ZSM-5 series molecular sieve of the high silica alumina ratio of 20-500.
9. method as claimed in claim 8 is characterized in that, described molecular sieve is that silica alumina ratio is the ZSM-5 series molecular sieve of 70-300.
10. method as claimed in claim 6 is characterized in that, described metal oxide is an aluminum oxide, and described nonmetal oxide is a silicon oxide.
11. the method for claim 1 is characterized in that, the liquid phase medium in the described mixed solution that contains super-refinement or nanocatalyst is selected from least a in water, hydrocarbon ils and the aliphatic hydrocarbon.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101450883B (en) * | 2007-12-06 | 2012-05-30 | 中国石油化工股份有限公司 | Method for increasing light olefins through vacuum catalytic cracking |
| CN102533313A (en) * | 2010-12-16 | 2012-07-04 | 中国石油化工股份有限公司 | Method for preparing ethylene and propylene through catalytic cracking |
| CN108238837A (en) * | 2016-12-27 | 2018-07-03 | 中国石油天然气股份有限公司 | The method of producing low-carbon alkene by catalytic pyrolysis |
| CN110869762A (en) * | 2017-06-29 | 2020-03-06 | 沙特阿拉伯石油公司 | Pyrolysis for determining hydrocarbon expulsion efficiency of source rock |
| CN112570019A (en) * | 2019-09-29 | 2021-03-30 | 中国石油化工股份有限公司 | Catalytic cracking method |
| CN113322093A (en) * | 2020-02-28 | 2021-08-31 | 中国石油化工股份有限公司 | Catalytic cracking method |
| US11518941B2 (en) | 2015-05-20 | 2022-12-06 | Saudi Arabian Oil Company | Pyrolysis to determine hydrocarbon expulsion efficiency of hydrocarbon source rock |
Family Cites Families (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0818756B2 (en) * | 1992-10-15 | 1996-02-28 | 村田機械株式会社 | Automatic winder |
| CN1035775C (en) * | 1994-03-28 | 1997-09-03 | 中国石油化工总公司 | Rifining method for catalylic cracking gasoline by adding hydrogen |
| US6093867A (en) * | 1998-05-05 | 2000-07-25 | Exxon Research And Engineering Company | Process for selectively producing C3 olefins in a fluid catalytic cracking process |
| US6569316B2 (en) * | 2000-04-17 | 2003-05-27 | Exxonmobil Research And Engineering Company | Cycle oil conversion process incorporating shape-selective zeolite catalysts |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101450883B (en) * | 2007-12-06 | 2012-05-30 | 中国石油化工股份有限公司 | Method for increasing light olefins through vacuum catalytic cracking |
| CN102533313A (en) * | 2010-12-16 | 2012-07-04 | 中国石油化工股份有限公司 | Method for preparing ethylene and propylene through catalytic cracking |
| CN102533313B (en) * | 2010-12-16 | 2014-05-28 | 中国石油化工股份有限公司 | Method for preparing ethylene and propylene through catalytic cracking |
| US11518941B2 (en) | 2015-05-20 | 2022-12-06 | Saudi Arabian Oil Company | Pyrolysis to determine hydrocarbon expulsion efficiency of hydrocarbon source rock |
| CN108238837A (en) * | 2016-12-27 | 2018-07-03 | 中国石油天然气股份有限公司 | The method of producing low-carbon alkene by catalytic pyrolysis |
| CN110869762A (en) * | 2017-06-29 | 2020-03-06 | 沙特阿拉伯石油公司 | Pyrolysis for determining hydrocarbon expulsion efficiency of source rock |
| CN112570019A (en) * | 2019-09-29 | 2021-03-30 | 中国石油化工股份有限公司 | Catalytic cracking method |
| CN113322093A (en) * | 2020-02-28 | 2021-08-31 | 中国石油化工股份有限公司 | Catalytic cracking method |
| CN113322093B (en) * | 2020-02-28 | 2023-06-09 | 中国石油化工股份有限公司 | Catalytic cracking method |
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