CN101456783A - Method for improving light olefins output during catalytic cracking process - Google Patents
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Abstract
The invention relates to a method for improving the yield of low-carbon olefin during catalytic cracking, which comprises: low-carbon alkane is injected into the middle lower part of a riser and/or a fluidized bed reactor, contacts a reduced catalytic cracking catalyst with dehydrogenation activity, and is subjected to catalytic dehydrogenation reaction; the catalyst after dehydrogenation reaction, hydrocarbon streams which are rich in the low-carbon olefin, and a reducing medium contact raw oil from a raw oil nozzle, and complete normal catalytic cracking reaction; and after subsequent oil gas and a spent catalyst are separated, target products are obtained after oil-gas separation, and the spent catalyst is subjected to steam stripping, regeneration and reduction in turn, returned to the reactor, and contacts the low-carbon alkane and the raw oil in turn. The method adopts the catalytic cracking catalyst with the dehydrogenation activity, and can improve the yield of the low-carbon olefin between C2 and C4 of a catalytic cracking unit by 3 to 5 percent.
Description
Technical field
The invention belongs to a kind of under the situation that does not have hydrogen the catalysis conversion method of hydrocarbon ils, more particularly, belong to a kind of catalysis conversion method that improves light olefins output.
Background technology
In the catalytic cracking process process, can generate the bigger lower low-carbon alkanes of added value of quantity, as propane, Trimethylmethane etc., both volume content sums can reach 25% of liquefied gas yield, 8 heavy % of catalytic cracking unit charging, these low-carbon alkanes can only be as the low liquefied gas of added value.If these low-carbon alkanes are converted into corresponding alkene, then its added value increases greatly.As liquefied gas price per ton is 4500 yuan, and propylene price per ton is about 10000 yuan, and the price of iso-butylene is also about 8000 yuan.As seen low-carbon alkanes is converted into corresponding low-carbon alkene and has good market outlook.For this reason, the researchist has carried out a large amount of research to improving light olefins output during catalytic cracking process.
CN1148865A discloses a kind of method and apparatus that a kind of short contact circulating fluid bed reactor system is catalytically conveted to hydro carbons light olefin.This method may further comprise the steps: a kind of hydrocarbon feed feed is given the reaction zone (1) that contains a kind of solid catalyst; Allow this hydrocarbon feed in reaction zone (1), be catalytically conveted under the light olefin condition helping hydro carbons, contact with catalyzer; Separate the reaction product that obtains behind the catalyzed conversion by reaction zone (1); Reclaim catalyzer and the catalyzer of regeneration of deactivated in revivifier (3).This method is used habitual or improved FCC catalyzer, and the catalyzed conversion by LGO, HGO, VGO or petroleum naphtha prepares propylene, butylene and amylene and high-octane rating, low benzoline fraction.This method also can be used habitual or improved fluidized-bed dehydrogenation catalyst, prepares the product that is rich in propylene, iso-butylene or isopentene respectively by propane, Trimethylmethane or petroleum naphtha catalytic dehydrogenation.But this method needs a newly-built cover short contact circulating fluid bed reactor, and the effect of increased low carbon olefine output and not obvious.
CN1102431A discloses a kind of catalysis conversion method that low-carbon alkene hold concurrently to produce stop bracket gasoline of producing, and is that the petroleum hydrocarbon of preheating is contacted with the five-ring high silica zeolite catalyst of rare earth with phosphorous, is that 480～680 ℃, pressure are 1.2～4.0 * 10 in temperature
5Handkerchief, reaction times are that the weight ratio of 0.1～6 second, catalyzer and stock oil is that the weight ratio of 4～20:1, water vapor and stock oil is to carry out catalytic conversion reaction under the condition of 0.01～0.5:1, the product logistics obtains low-carbon alkene and liquid product through separation, and reclaimable catalyst recycles after regeneration.This method needs character good raw material oil, and the productive rate of low-carbon alkanes such as while propane is still higher.
CN1403540A discloses a kind of catalysis conversion method of producing ethene and propylene, be that the hydrocarbon oil crude material A after the preheating is injected Mi Xiangfanyingqu, contact, react with the catalyzer that contains the five-ring supersiliceous zeolite, temperature of reaction is 630～750 ℃, reaction pressure is 0.15～0.40MPa, reaction times is 0.2-3 second, and the weight ratio of catalyzer and stock oil is 15～40:1, and the weight ratio of water vapor and stock oil is 0.3～1.2:1; Reactant flow enters Mi Xiangfanyingqu, and contact, react with the hydrocarbon oil crude material B that injects wherein, temperature of reaction is 500～600 ℃, reaction pressure is 0.15～0.40MPa, reaction times is 3-30 second, the weight ratio of catalyzer and stock oil is 7-20:1, and the weight ratio of water vapor and stock oil is 0.15～0.6:1; The catalyzer of separating reaction oil gas and reaction back carbon deposit, oil gas is sent into subsequent separation system, and the catalyzer of carbon deposit Returning reactor after stripping, regeneration recycles; Hydrocarbon oil crude material A is 0.5～2:1 with the ratio of the mass rate of hydrocarbon oil crude material B.This method has the total recovery of higher ethene, propylene and butylene.But still have a large amount of small molecules alkane in the process of this method.
USP3,541,179, USP3,647,682 aluminum oxide, silicon oxide or other oxide compounds that disclose metal components such as working load IIB, VB, VIIB and VIII family are produced low-carbon alkene as catalyzer.Because the metal of institute's load still has dehydrogenation activity when carrying out cracking reaction, thereby in the cracking reaction process, quickened condensation and green coke reaction, distribute to product and bring detrimentally affect, so this class catalyzer only has been applicable to the processing lightweight material.
USP3,758,403 disclose ZSM-5 and the two zeolite activity component catalysts of REY, under the condition of catalytic cracking, improve the octane value and the productive rate of product gasoline, obtaining than the single zeolite activity component catalyst of REY simultaneously is high productivity of low carbon olefin hydrocarbon, gas oil with 220～510 ℃ in example is former section, is 4h in about 483 ℃ of temperature of reaction, feed volume air speed
-1, agent-oil ratio is under 1.5 the condition, the overall yield of propylene and butylene can reach 10～15 heavy %.
CN1317467A discloses and has a kind ofly produced the processing method of light olefin by the low-carbon alkanes catalyzed conversion, and this method comprises that the low-carbon alkanes that will contain C4～C6 alkane contacts with a kind of dehydrogenation catalyst and carries out the dehydrogenation pre-treatment in the catalytic dehydrogenating reaction device; Then with dehydrogenation product a kind of with the y-type zeolite be in the presence of the catalytic cracking catalyst of main active component routinely condition carry out catalytic cracking.This processing method is applicable to that being difficult to cracked low-carbon alkanes catalyzed conversion under conventional catalytic cracking process condition produces light olefin, is characterized in that transformation efficiency height, ethene and propylene selectivity are good, can utilize existing catalytic cracking reaction-regeneration system rapidly.But the method that this invention provides need increase dehydrogenation reactor, and is not easy to operate.Simultaneously, because raw material is the gasoline light constituent, therefore can reduce the productive rate of gasoline to a certain extent.
Though above-mentioned prior art can a large amount of low-carbon alkene of direct production, but also can produce a considerable number of low-carbon alkanes simultaneously, these methods of producing low-carbon alkene are then powerless for producing low-carbon alkanes in the process so, based on this present invention is proposed, the present invention can be used for any type of catalytic cracking of hydrocarbon process, with the light olefins output of further this process of raising.
Summary of the invention
The objective of the invention is to provide on the basis of existing technology a kind of method that improves light olefins output during catalytic cracking process.
Technical scheme of the present invention is as follows:
With the middle and lower part of low-carbon alkanes injecting lift pipe and/or fluidized-bed reactor, at 600～750 ℃ of temperature of reaction, air speed 1～20 h
-1Condition under, contact with the catalytic cracking catalyst that has a dehydrogenation activity through reductive and carry out catalytic dehydrogenating reaction, finish the catalyzer of dehydrogenation reaction and be rich in the hydrocarbon stream of low-carbon alkene and reducing medium 500～650 ℃ of temperature of reaction, 0.5～2 second reaction times, the weight ratio of catalyzer and stock oil (hereinafter to be referred as agent-oil ratio) is under the condition of 3～15:1, contact and finish conventional catalytic cracking reaction with stock oil from the stock oil nozzle, follow-up oil gas is with after reclaimable catalyst separates, wherein oil gas obtains the purpose product further the separation, reclaimable catalyst is successively through stripping, regeneration, reduction back Returning reactor is successively with low-carbon alkanes, the stock oil contact.
Described low-carbon alkanes is from one or more gases in the C2～C4 alkane of this device or other device.
Described stock oil is selected from one or more in gasoline, diesel oil, decompressed wax oil, residual oil, wax tailings, the deasphalted oil.
It is that carry out bottom or bottom at riser tube or fluidized-bed reactor that catalyzer after the regeneration is reduced, and the reductive medium can be water vapour, hydrogen or other reducing gas, and reduction temperature is 600～750 ℃, and the recovery time is 0.5～5 second.
Described catalytic cracking catalyst with dehydrogenation activity comprises that (each component ratio is the per-cent that accounts for catalyst weight) is as follows:
The Y zeolite of 10～40 heavy %,
The modification mesopore zeolite of 5～30 heavy %,
The carrier of 5～75 heavy %,
The binding agent of 5～30 heavy %,
Wherein said y-type zeolite is selected from one or more among HY, REHY, REY and the USY, described mesopore zeolite is selected from ZSM series zeolite and/or ZRP zeolite, and the modified metal of mesopore zeolite is selected from one or more in nickel, palladium, platinum, cobalt, iron, chromium, molybdenum, tungsten, the vanadium.
The more detailed description of relevant ZRP is referring to US5,232,675, the ZSM series zeolite is selected from one or more the mixture among the zeolite of ZSM-5, ZSM-11, ZSM-12, ZSM-23, ZSM-35, ZSM-38, ZSM-48 and other similar structures, the more detailed description of relevant ZSM-5 is referring to US3,702,886.The modified metal of mesopore zeolite is selected from one or more in nickel, palladium, platinum, cobalt, iron, chromium, molybdenum, tungsten, the vanadium, and modified metal accounts for 5～30 heavy % of modification mesopore zeolite weight, and these metals all are arranged in the duct of mesopore zeolite.
Described carrier is selected from kaolin and/or halloysite.
Described caking agent is selected from silicon-dioxide (SiO
2) and/or aluminium sesquioxide (Al
2O
3).
Said catalytic cracking catalyst with dehydrogenation activity is the catalytic cracking catalyst that contains Y type and two kinds of zeolites of ZSM-5 in the method provided by the present invention, and wherein y-type zeolite is responsible for finishing the cracking reaction of catalytic cracking process process; The ZSM-5 zeolite is responsible for finishing the dehydrogenation reaction of low-carbon alkanes.
This method adopts the catalytic cracking catalyst with dehydrogenation activity, and the low-carbon alkene that can make C2～C4 improves 3～5 percentage points to the productive rate of catalytic cracking unit charging, and the product of full device is distributed to have no adverse effects.
Provided by the present inventionly directly produce the processing method of corresponding low-carbon alkene owing to realize, thereby have the characteristics of the enforcement of being very easy in catalytic cracking unit itself by the low-carbon alkanes catalytic dehydrogenation.
Embodiment
To be described further effect of the present invention by embodiment below, but not limit range of application of the present invention.
It is 20 heavy % that the used catalytic cracking catalyst with dehydrogenation activity of the present invention contains metal-modified ZSM-5 zeolite (Qilu Petrochemical company catalyst plant), and modified metal is a molybdenum, and content accounts for 20 heavy % of ZSM-5 zeolite; The content of USY zeolite is 20 heavy %, and all the other are kaolin and Al
2O
3Its preparation process is as follows: the ZSM-5 zeolite be impregnated in the deionized water saturated solution of oxalic acid, add the nitric acid molybdenum, stir, put into the baking oven baking, put into the muffle furnace roasting after the taking-up, make metal-modified ZSM-5 zeolite.(the Chang Ling catalyst plant is produced to get above-mentioned metal-modified ZSM-5 zeolite and USY zeolite, trade names SRY), with add the water making beating after kaolin, silica sol mix, conventional catalytic cracking catalyst step of preparation process such as spray-dried, roasting are made the good microspheric catalytic cracking catalyst with dehydrogenation activity of physical properties.
Embodiment 1
The test of present embodiment is carried out on small fixed flowing bed.
The low-carbon alkanes raw material is an ethane, and cracking stock oil is mixed the vacuum residuum of 30 heavy % for decompressed wax oil.Test conditions is: the catalyst reduction medium after the regeneration is water vapour, recovery time to be 650 ℃ of 2 seconds, reduction temperature; The temperature of dehydrogenation reaction is that 650 ℃, air speed are 10h
-1The cracked temperature is that 500 ℃, agent-oil ratio are 6, weight hourly space velocity is 10h-1.Test conditions and experimental result are listed in the table 1.As can be seen from Table 1, conversion rate of dehydrogenation is 95 heavy %, and the selectivity of alkene is 90 heavy %.
Embodiment 2
The test of present embodiment is carried out on medium-sized riser reactor.
The low-carbon alkanes raw material is a propane, and cracking stock oil is decompressed wax oil.Test conditions is: the catalyst reduction medium after the regeneration is hydrogen, recovery time to be 600 ℃ of 2 seconds, reduction temperature; The temperature of dehydrogenation reaction is that 600 ℃, air speed are 15h
-1The cracked temperature is that 500 ℃, agent-oil ratio are 6, air speed is 10h
-1Test conditions and experimental result are listed in the table 1.As can be seen from Table 1, conversion rate of dehydrogenation is 96 heavy %, and the selectivity of alkene is 89 heavy %.
Embodiment 3
The test of present embodiment is carried out on medium-sized riser tube+fluidized-bed reactor.
The low-carbon alkanes raw material is a butane, and cracking stock oil is mixed the deasphalted oil of 30 heavy % for decompressed wax oil.Test conditions is: the catalyst reduction medium after the regeneration is water vapour, recovery time to be 700 ℃ of 2 seconds, reduction temperature; The temperature of dehydrogenation reaction is that 700 ℃, air speed are 20h
-1The cracked temperature is that 500 ℃, agent-oil ratio are 6, air speed is 10h-1.Test conditions and experimental result are listed in the table 1.As can be seen from Table 1, conversion rate of dehydrogenation is 95 heavy %, and the selectivity of alkene is 91 heavy %.
Table 1
| The embodiment numbering | 1 | 2 | 3 |
| The catalyst reduction condition | |||
| Reduction temperature, ℃ | 650 | 600 | 700 |
| Reducing medium | Water | Hydrogen | Water |
| Recovery time, second | 2 | 0.5 | 5 |
| Dehydrogenation condition | |||
| The low-carbon alkanes raw material | Ethane | Propane | Butane |
| Desorption temperature, ℃ | 650 | 600 | 700 |
| The dehydrogenation air speed, h -1 | 10 | 15 | 20 |
| Conversion rate of dehydrogenation, heavy % | 95 | 96 | 95 |
| Olefine selective, heavy % | 90 | 89 | 91 |
| Cracking conditions | |||
| The cracking temperature, ℃ | 500 | 500 | 500 |
| The cracking agent-oil ratio | 6 | 6 | 6 |
| The cracking air speed, h -1 | 10 | 10 | 10 |
| Cracked product distributes, heavy % | |||
| Dry gas | 2.51 | 2.50 | 2.52 |
| Liquefied gas | 15.26 | 15.24 | 15.25 |
| Gasoline | 40.65 | 40.66 | 40.65 |
| Diesel oil | 30.21 | 30.19 | 30.2 |
| Heavy oil | 3.81 | 3.86 | 3.82 |
| Coke | 7.56 | 7.55 | 7.56 |
Claims (7)
1, a kind of method that improves light olefins output during catalytic cracking process is characterized in that the middle and lower part with low-carbon alkanes injecting lift pipe and/or fluidized-bed reactor, at 600～750 ℃ of temperature of reaction, air speed 1～20h
-1Condition under, contact with the catalytic cracking catalyst that has a dehydrogenation activity through reductive and carry out catalytic dehydrogenating reaction, finish the catalyzer of dehydrogenation reaction and be rich in the hydrocarbon stream of low-carbon alkene and reducing medium 500～650 ℃ of temperature of reaction, 0.5～2 second reaction times, the weight ratio of catalyzer and stock oil is under the condition of 3～15:1, contact and finish conventional catalytic cracking reaction with stock oil from the stock oil nozzle, follow-up oil gas is with after reclaimable catalyst separates, wherein oil gas obtains the purpose product further the separation, reclaimable catalyst is successively through stripping, regeneration, reduction back Returning reactor is successively with low-carbon alkanes, the stock oil contact.
2,, it is characterized in that described low-carbon alkanes is selected from one or more in C2～C4 alkane according to the method for claim 1.
3,, it is characterized in that described stock oil is selected from one or more in gasoline, diesel oil, decompressed wax oil, residual oil, wax tailings, the deasphalted oil according to the method for claim 1.
4, according to the method for claim 1, it is characterized in that the catalyzer after the regeneration is reduced is that carry out bottom or bottom at riser tube or fluidized-bed reactor, the reductive medium is water vapour or hydrogen, and reduction temperature is 600～750 ℃, and the recovery time is 0.5～5 second.
5, according to the method for claim 1, it is characterized in that described catalytic cracking catalyst with dehydrogenation activity serves as to calculate benchmark with the gross weight of catalyzer, comprise 10～40 heavy Y zeolite, the modification mesopore zeolite of 5～30 heavy %, the binding agent of the carrier of 5～75 heavy % and 5～30 heavy %.
6,, it is characterized in that described y-type zeolite is selected from one or more among Y, HY, REHY, REY and the USY according to the method for claim 5.
7, according to the method for claim 5, it is characterized in that described mesopore zeolite is selected from ZSM series zeolite and/or ZRP zeolite, the modified metal of mesopore zeolite is selected from one or more in nickel, palladium, platinum, cobalt, iron, chromium, molybdenum, tungsten, the vanadium.
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| CN102274751A (en) * | 2010-06-11 | 2011-12-14 | 中国石油化工股份有限公司 | Steam stripping method for spent catalyst in process for preparing olefins by oxygenated chemicals |
| CN103361115A (en) * | 2012-04-05 | 2013-10-23 | 中国石油天然气股份有限公司 | Method for producing high-octane gasoline by using raw material rich in C4, C5 and C6 alkanes |
| CN103772260A (en) * | 2012-10-25 | 2014-05-07 | 中国石油化工股份有限公司 | Indole production method |
| CN106083509A (en) * | 2016-06-20 | 2016-11-09 | 中国石油大学(北京) | The method of crome metal skeleton doped molecular sieve catalytic pyrolysis normal butane producing light olefins |
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| CN114426857B (en) * | 2020-10-29 | 2023-11-10 | 中国石油化工股份有限公司 | Method and device for increasing yield of low-carbon olefin and catalyzing hydrocarbon oil of gasoline for catalytic conversion |
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