CN105368485B - Catalytic conversion method for directly processing high chlorine raw material - Google Patents

Catalytic conversion method for directly processing high chlorine raw material Download PDF

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Publication number
CN105368485B
CN105368485B CN201410407655.0A CN201410407655A CN105368485B CN 105368485 B CN105368485 B CN 105368485B CN 201410407655 A CN201410407655 A CN 201410407655A CN 105368485 B CN105368485 B CN 105368485B
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reaction
oil
catalyst
raw material
temperature
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CN105368485A (en
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宋宝梅
魏晓丽
陈学峰
谢朝钢
毛安国
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Sinopec Research Institute of Petroleum Processing
China Petroleum and Chemical Corp
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Sinopec Research Institute of Petroleum Processing
China Petroleum and Chemical Corp
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Abstract

The present invention relates to a catalytic conversion method for directly processing a high chlorine raw material. The method comprises that a pre-heated high chlorine raw material and a first catalytic conversion catalyst are subjected to a first contact reaction at the initial reaction zone of a riser reactor, the oil agent mixture produced in the initial reaction zone enters the main reaction zone of the riser reactor, and the oil agent mixture and a complementally-injected second catalytic conversion catalyst are continuously subjected to a catalytic conversion reaction, wherein the reaction temperature of the initial reaction zone is higher than the reaction temperature of the main reaction zone, and the reaction time of the original reaction zone is shorter than the reaction time of the main reaction zone. With the method of the present invention, the high chlorine raw material can be directly processed while the high dechlorination rate can be obtained, the high chlorine raw material conversion rate can be improved, the product selectivity can be improved, and the dry gas yield and the coke yield can be reduced.

Description

A kind of catalysis conversion method for directly processing high-chlorine raw material
Technical field
The present invention relates to a kind of catalysis conversion method of hydrocarbon ils, in particular it relates to a kind of direct processing high-chlorine raw material is urged Change method for transformation.
Background technology
The petroleum resources relative shortage of China, the Global Oil field status report middle finger of Swiss Bank's issue in 2012 Go out, about 15,000,000,000 barrels of CNPC's reserves account for the 1.1% of world oil reserves, only enough 10 years.Crude oil is inferior in world wide Change tendency increasingly serious, especially nearly ten years, based on water flooding recovery, the application of various oil recovery techniques makes crude oil and reinjected water In complicated component, the not only treatment to crude oil and sewage causes difficulty, and stable operation to oil refining apparatus, equipment are rotten Erosion, product quality are brought and are had a strong impact on, and wherein chlorine compound has very big harm to Crude Oil Processing.Chlorine compound point in crude oil It is inorganic chloride and organochlorine compound.When organochlorine compound content is higher in crude oil, it is difficult to by conventional water wash Method removing and enter Atmospheric vacuum steam unit.Undecomposed organic chloride enters in each distillate during Atmospheric vacuum, In distillate secondary processing process, organochlorine issues biochemical reaction generation chlorination in HTHP and hydrogen existence condition Hydrogen, easily causes equipment corrosion.It is usually de- using electricity in order to prevent organic chloride that hydrogen chloride is converted into Crude Oil Processing The technologies such as salt, catalytic hydrogenation, adsorbing separation remove organic chloride.CN200910180772.7 discloses a kind of electro-desalting removing The method of organic chloride in crude oil, the method mixes demulsifier, alkali compounds, consisting of phase-transferring agent, water filling and hydrocarbon ils, in heat And/or in the presence of electric field, water-oil separating being carried out, organic chloride is converted to butter, is mutually excluded with water, reaches de- Except the purpose of organochlorine.
CN200310102941.8 provides a kind of method that catalytic hydrogenation removes organochlorine compound, with calcium oxide and oxygen Change iron mixture or calcium iron compound oxide as antichlor, the temperature more than 200 DEG C carries out reacting the purpose for reaching dechlorination.
CN200710057240.5 discloses a kind of method of chlorinated aromatic hydrocarbons catalytic hydrogenation and dechlorination, using fixed bed reaction Device, support type catalyst of phosphatizing nickel, the wherein mass fraction of nickel are 5-25%, and the catalyst can be with chlorobenzene, dichloro-benzenes or three Chlorobenzene carries out catalytic hydrogenation and dechlorination reaction, reaches the purpose of removing organic chloride.
CN201110006489.X discloses a kind of method of the catalysis dechlorination for chloride aromatic hydrocarbons organic compound, with Amorphous cobalt carried noble metal is catalyst, produces hydrogen as reducing agent using amorphous cobalt and water reaction are in situ, will be contained Chlorine arene organic compound conversions turn into corresponding arene organic compound.
CN200910010151.4 provides a kind of nickel and is catalyzed chlorinated aromatic hydrocarbons dechlorination method.In the condition that room temperature and alkali are present Under, with low-carbon alcohols as solvent, with divalence nickel complex as catalyst, it is catalyzed the dechlorination reaction of chlorinated aromatic hydrocarbons.Product is easy to Separate, yield is high, selectivity is good.With low, the cheap and easy to get low-carbon alcohols of toxicity as solvent in the patent application, nickelous used is matched somebody with somebody Compound its preparation method is easy, catalysis activity is high, selectivity is good, stable in the air.
US3864243 discloses a kind of method for removing chloride in hydrocarbon ils, and the method utilizes zeolite molecular sieve by hydrocarbon ils Middle chloride is removed by adsorption method.
US5928500 provide it is a kind of use porous, the tripoli of bigger serface is carrier, with nickel, cobalt or iron and its Mixture or metal oxide be active component as adsorbent, organic chloride is converted into metal chloride and is removed.
US7476374 discloses a kind of halogenated hydrocarbons decomposition method, in the range of 200-350 DEG C of reaction temperature, is steamed in water Under conditions of gas is present, halogenated hydrocarbons is decomposed reaction on lanthanum modified solid acid catalyst.
However, when organic chloride content is higher in raw material, above-mentioned electro-desalting method is still unable to reach preferable dechlorination Effect, although absorption method removing chloride process is simple, the poor selectivity of adsorbent, adsorption capacity is relatively low, adsorbent reactivation The problem of recycling is difficult to solve, and hydrogenation is the technology path of ideal removing organic chloride, and what the method was present asks Topic is that plant investment and operating cost are higher, while being likely to result in equipment corrosion and environmental pollution.Therefore, it is necessary to develop one The method that high-chlorine raw material is directly catalyzed processing is planted, process economy benefit and petroleum resources utilization rate is improved.
The content of the invention
The invention aims to overcome when the organic chloride content in raw material is higher using existing method without Method effectively removes the defect of chloride, there is provided a kind of catalysis conversion method for directly processing high-chlorine raw material.
The invention provides a kind of catalysis conversion method for directly processing high-chlorine raw material, the method includes:After preheating High-chlorine raw material and the first catalytic converting catalyst carry out catalytic conversion reaction in the initial reaction area of riser reactor, and make The oil agent mixture produced by the initial reaction area enters the main reaction region of riser reactor, and second with supplement injection is urged Change reforming catalyst and proceed catalytic conversion reaction, wherein, the reaction temperature in the initial reaction area is higher than the main reaction The reaction temperature in area, the reaction time of the reaction time less than the main reaction region in the initial reaction area.
In the catalysis conversion method of the direct processing high-chlorine raw material that the present invention is provided, by the catalyzed conversion mistake of high-chlorine raw material Journey is divided into two stages of reaction, and first stage of reaction is absorption phase, is carried out in the initial reaction area of riser reactor, is made High-chlorine raw material contacts the shorter time with catalytic converting catalyst, the chlorine-containing compound in high-chlorine raw material is adsorbed in catalyst Acid centre is simultaneously reacted;Second stage of reaction is decomposition reaction stage, is carried out in the main reaction region of riser reactor, Catalyst is added by supplementing, makes to continue to be catalyzed under oil ratio higher by the oil plant obtained after first stage of reaction Conversion reaction such that it is able to the chlorine-containing compound effectively in removing high-chlorine raw material, while turning for high-chlorine raw material can be significantly improved Rate.And, the method that the present invention is provided can be effectively improved the selectivity of product, particularly can occasionally improve liquefied gas, gasoline With the yield of diesel oil, the yield of coke, heavy oil and dry gas is reduced.
In addition, the methods described that the present invention is provided is simple to operate, letter is carried out on the basis of conventional catalytic cracking unit Single transformation is just operable.
Other features and advantages of the present invention will be described in detail in subsequent specific embodiment part.
Brief description of the drawings
Accompanying drawing is, for providing a further understanding of the present invention, and to constitute the part of specification, with following tool Body implementation method is used to explain the present invention together, but is not construed as limiting the invention.In the accompanying drawings:
Fig. 1 is that the flow of the catalysis conversion method of the processing high-chlorine raw material according to one embodiment of the present invention is illustrated Figure;
Fig. 2 is that the flow of the catalysis conversion method of the processing high-chlorine raw material according to a kind of preferred embodiment of the invention is shown It is intended to.
Description of reference numerals
1- riser reactors;2- regenerators;3- settlers;
4- stripping sections;5- degassing tanks;
6- (port of export of riser reactor 1) cyclone separator;
7- (gas vent and main oil gas piping 20 of connection cyclone separator 6) collection chamber;
8- guiding valves to be generated;9- reclaimable catalyst inclined tube pipelines;
10- (catalyst outlet and degassing tank 5 of connection regenerator 2) pipeline;
11- (the connection gas vent of degassing tank 5 and regenerator 2) pipeline;
12- (bottom of connection degassing tank 5 and riser reactor 1) pipeline;
13- regenerates guiding valve;
14- is the pipeline that riser reactor 1 conveys pre-lift medium;
15- is the pipeline of the transferring raw material of riser reactor 1;
16- is the pipeline of the conveying atomizing steam of riser reactor 1 and transferring raw material;
The initial reaction area of 17- riser reactors;
The main reaction region of 18- riser reactors;
19- is the pipeline that stripping section 4 conveys atomizing steam;
20- main oil gas pipings;
The pipeline of the main wind entrances of 21- (regenerator 2);
22- air distributors;
23- is the pipeline that degassing tank 5 conveys atomizing steam;
24- regenerator cyclone separators;
25- (being connected with the gas vent of cyclone separator 24) flue;
26- (main reaction region of connection degassing tank 5 and riser reactor 1) pipeline;
27- regenerates guiding valve;
The addition reaction area of 28- riser reactors.
Specific embodiment
Specific embodiment of the invention is described in detail below in conjunction with accompanying drawing.It should be appreciated that this place is retouched The specific embodiment stated is merely to illustrate and explain the present invention, and is not intended to limit the invention.
All ranges disclosed herein can all be combined comprising end points and independently.Scope presently disclosed End points and any value are not limited to the accurate scope or value, these scopes or value should be understood to include close to these scopes or The value of value.
The invention provides a kind of catalysis conversion method for directly processing high-chlorine raw material, the method includes:After preheating High-chlorine raw material and the first catalytic converting catalyst carry out catalytic conversion reaction in the initial reaction area of riser reactor, and make The oil agent mixture produced by the initial reaction area enters the main reaction region of riser reactor, and second with supplement injection is urged Change reforming catalyst and proceed catalytic conversion reaction, wherein, the reaction temperature in the initial reaction area is higher than the main reaction The reaction temperature in area, the reaction time of the reaction time less than the main reaction region in the initial reaction area.
In the methods described that the present invention is provided, it is preferable that the reaction temperature in the initial reaction area is than the main reaction The reaction temperature in area is high 5-100 DEG C, more preferably 10-80 DEG C, further preferred 30-60 DEG C.
In the methods described that the present invention is provided, it is preferable that the reaction time in the initial reaction area is than the main reaction The reaction time in area is short 0.5-5 seconds, more preferably 0.6-4 seconds, further preferred 0.7-3.8 seconds.
In the methods described that the present invention is provided, the reaction condition in the initial reaction area can include:Reaction temperature is 500-750 DEG C, preferably 550-700 DEG C;Oil ratio (i.e. the weight ratio of catalyst and high-chlorine raw material) is 5-50: 1, preferably 10-30∶1;Reaction time is 0.1-1.9 seconds, preferably 0.2-1.5 seconds.
In the methods described that the present invention is provided, the agent weight of oil ratio of the main reaction region is 15-80: 1, preferably 15- 60∶1;Reaction time is 1-8 seconds, preferably 1.5-6 seconds.The agent weight of oil ratio of the main reaction region refers to that the first catalyzed conversion is urged Agent and the total amount of the second catalytic converting catalyst and the weight ratio of high-chlorine raw material.
In the present invention, the reaction temperature of riser reactor refers to certain of riser reactor or riser reactor The outlet temperature of individual reaction zone.
In the methods described that the present invention is provided, the main reaction region in the riser reactor for being used can be provided with one Individual or multiple.In order that high-chlorine raw material can fully react, and according to different purpose product quality requirements, the riser The quantity of main reaction region could be arranged to 2-8, preferably 2-3 in reactor.
A kind of implementation method of the invention, as shown in figure 1, the riser reactor is included in advance successively from bottom to top Raising section, initial reaction area and main reaction region.In the riser reactor, the pre lift zone, the initial reaction area Can in a conventional manner distribute or connect with the main reaction region.Under preferable case, the initial reaction area is relative to institute Main reaction region is stated for undergauge, and the ratio between the initial reaction area and the riser diameter of the main reaction region can be 0.5- 0.8:1.The junction of the initial reaction area and the main reaction region can be truncated cone-shaped, and the preferably vertical profile of the truncated cone-shaped The drift angle of face isosceles trapezoid can be 45-75 °.In this embodiment, first catalytic converting catalyst is preferably described Pre lift zone injects, and second catalytic converting catalyst preferably injects in the bottom of the main reaction region.Specifically, first urge Change reforming catalyst after pre lift zone is injected, initial reaction area is flowed up into the presence of pre-lift medium, in advance High-chlorine raw material after heat injects in the bottom in initial reaction area, with the first catalytic converting catalyst haptoreaction, the oil for being formed Agent composition (namely first product of contact) is advanced into main reaction region on continuing, the second catalytic converting catalyst with supplement injection Continue to react.
Another embodiment of the invention, as shown in Fig. 2 in the riser reactor, described initial Addition reaction area is additionally provided between reactor and the main reaction region, the riser reactor includes pre- successively from bottom to top Raising section, initial reaction area, addition reaction area and main reaction region.It is the pre lift zone, described in the riser reactor Initial reaction area, the addition reaction area and the main reaction region can in a conventional manner be distributed or connect.Preferable case Under, the initial reaction area is undergauge relative to the addition reaction area, and the main reaction region is additional anti-relative to described It is also undergauge to answer area.It is highly preferred that the ratio between the initial reaction area and riser diameter of the main reaction region can be 0.5-0.8:1, the ratio between the addition reaction area and riser diameter of the main reaction region can be 1.05-1.8:1.It is described first Connect between beginning reaction zone and the addition reaction area and by truncated cone-shaped between the addition reaction area and the main reaction region Connect, and preferably the drift angle of the vertical section isosceles trapezoid of the truncated cone-shaped can be 30-75 °.In this embodiment, described first Catalytic converting catalyst preferably injects in the pre lift zone, and second catalytic converting catalyst is preferably in the addition reaction The bottom injection in area.Specifically, the first catalytic converting catalyst inject pre lift zone after, in the presence of pre-lift medium Initial reaction area is flowed up into, the high-chlorine raw material after preheating injects in the bottom in initial reaction area, with the first catalyzed conversion Catalyst haptoreaction, addition reaction area is advanced into the oil agent mixture for being formed (namely first product of contact) continuation, with The second catalytic converting catalyst haptoreaction of injection is supplemented, and it is subsequent by the oil agent mixture of addition reaction area generation Proceed catalytic conversion reaction into main reaction region.The reaction condition in the addition reaction area can include:Reaction temperature is 500-750 DEG C, preferably 550-700 DEG C;Agent weight of oil ratio is 15-80: 1, preferably 15-60: 1;Reaction time is 0.5-4 Second, preferably 1-3 seconds.
For the main reaction region of riser reactor, its structure can be conventional equal diameter riser reactor, and its is straight Footpath can be 0.2-5 meters, and length can be 10-50 meters.For the initial reaction area of riser reactor, its structure can also be Conventional equal diameter riser reactor, its length can be 0.5-5 meters.For the addition reaction area of riser reactor, its Structure can also be conventional equal diameter riser reactor, and its length can be 0.5-5 meters.
In the present invention, the pre-lift medium and the weight ratio of high-chlorine raw material can be 0.01-2:1, preferably 0.05- 1:1.The pre-lift medium can be selected from least one in vapor, dry gas and nitrogen.
In the methods described that the present invention is provided, first catalytic converting catalyst is catalyzed with second catalyzed conversion Agent can be preferably identical with identical or different.It is highly preferred that the two is respectively high-temperature regenerated catalyst.The high temperature regeneration is urged Regenerated catalyst, or itself work that the reclaimable catalyst regeneration that agent can be derived from other catalytic conversion process is obtained The regenerated catalyst that reclaimable catalyst regeneration during skill is obtained.When first catalytic converting catalyst and described second is urged When changing reforming catalyst from high-temperature regenerated catalyst, first catalytic converting catalyst and second catalyzed conversion are catalyzed The temperature of agent can be each 620-750 DEG C, preferably 650-720 DEG C.
In the present invention, the catalysis conversion method can also include:To be discharged by the outlet of the riser reactor Reaction mass carry out gas solid separation, the solid catalyst that will be isolated is stripped, coke burning regeneration and optional degassing process To obtain high-temperature regenerated catalyst, a part of high-temperature regenerated catalyst is recycled as first catalytic converting catalyst, will Another part high-temperature regenerated catalyst is recycled as second catalytic converting catalyst.The process of the gas solid separation can be Carried out in cyclone separator.For the reaction oil gas isolated during gas solid separation, subsequent separation system is generally injected into, Separate and obtain the cuts such as dry gas, liquefied gas, gasoline and diesel oil.
The process of the regeneration can be implemented according to the conventional catalyst recovery process in this area, for example, the regeneration side Method can include:Oxygen-containing gas (such as air) is introduced from the bottom of regenerator, after oxygen-containing gas introduces regenerator, reclaimable catalyst Coke burning regeneration is contacted with oxygen, in regenerator top gas solid separation, flue gas can enter the flue gas generated after catalyst coke burning regeneration Enter subsequent power recovery system.The regeneration condition of the reclaimable catalyst can be the conventional operating condition in this area, for example may be used To include:Temperature is 550-750 DEG C, more preferably preferably 600-730 DEG C, 650-700 DEG C;Gas superficial linear speed is 0.5-3 meter per seconds, preferably 0.8-2.5 meter per seconds, more preferably 1-2 meter per seconds;Reclaimable catalyst mean residence time is 0.6-3 Minute, preferably 0.8-2.5 minutes, more preferably 1-2 minutes.
It is to slough the impurity such as the gas wherein carried secretly by the purpose that regenerated catalyst is de-gassed treatment.The degassing The process for the treatment of can be stripped using vapor.
In the methods described that the present invention is provided, whole high-chlorine raw materials can be introduced into reactor in a feed entrance point It is interior, it is also possible to high-chlorine raw material is introduced in reactor according to identical or different ratio at least two different feed entrance points. However, either one or more than two feed entrance points, all feed entrance points of preferably high-chlorine raw material are respectively positioned on described carrying The initial reaction area of riser reactors, is more preferably respectively positioned on the bottom in the initial reaction area.
In the methods described that the present invention is provided, before the high-chlorine raw material is contacted with catalytic converting catalyst, will The high-chlorine raw material is preheated, such as reactor is introduced after high-chlorine raw material being preheated into 150-400 DEG C and is catalyzed with catalyzed conversion Agent is contacted, and is preferably preheated to 220-380 DEG C.
In the present invention, the high-chlorine raw material is that chloride content is more than 50ppm (such as 60-1000ppm) or organic chloride Catalytic cracking of hydrocarbon oil raw material of the content more than 10ppm (such as 50-950ppm).Chloride in the high-chlorine raw material includes inorganic chlorine Compound and organic chloride, the butter for example can be NaCl, MgCl2、CaCl2Deng the organic chloride is for example Can be chloralkane, chlorinated aromatic hydrocarbons, hydroxyl chloralkane etc..The butter generally can be in Desalting and Dewatering from Crude Oil mistake Removed with the removing of water in journey, and the organic chloride is generally difficult removing using conventional method.
The high-chlorine raw material can be selected from crude oil and heavy oil, and the heavy oil is not less than 250 DEG C of hydrocarbon oil cut for initial boiling point. Preferably, the high-chlorine raw material be selected from wax tailings, decompressed wax oil, decompression residuum, deasphalted oil, extract oil, recycle oil inferior, At least one in crude oil, shale oil and oil-sand.
In the methods described that the present invention is provided, the catalytic converting catalyst can be the conventional selection of this area, pin To the present invention, the catalytic converting catalyst is preferably solid acid catalyst.The solid acid catalyst contain active component and Carrier.The active component can be selected from Y or HY types zeolite, the zeolite with MFI structure, faujasite with or without rare earth With at least one in alumina silicate, the ultrastable with or without rare earth, the zeolite with MFI structure and dilute are preferably selected from At least one in the faujasite of native ion exchange.The carrier can be selected from inorganic oxide (as artificial synthesized) and day At least one in right clay.
In the present invention, each component accounts for total catalyst weight respectively in the catalytic converting catalyst:Zeolite 1-50 weights Amount %, inorganic oxide 5-99 weight %, clay 0-70 weight %.Wherein zeolite as active component, selected from mesopore zeolite and/ Or optional large pore zeolite, mesopore zeolite accounts for the 0-100 weight % of zeolite gross weight, preferably 0-50 weight %, more preferably 0-20 Weight %, large pore zeolite accounts for the 0-100 weight % of zeolite gross weight, preferably 20-80 weight %.Mesopore zeolite is selected from ZSM series Zeolite and/or ZRP zeolites, also can be to the nonmetalloid and/or iron, cobalt, nickel etc. such as above-mentioned mesopore zeolite phosphorus transition metal unit Element is modified, and relevant ZRP is more described referring to US5 in detail, 232,675, ZSM series zeolites be selected from ZSM-5, ZSM-11, At least one among the zeolite of ZSM-12, ZSM-23, ZSM-35, ZSM-38, ZSM-48 and other similar structures, relevant ZSM- 5 more detailed descriptions are referring to US3,702,886.Large pore zeolite is selected from by Rare Earth Y (REY), not rare earth hydrogen Y (REHY), Tongfang At least one in this group of zeolite that super steady Y, the silicon Y high that method is obtained are constituted.
In the present invention, the inorganic oxide is preferably selected from silica (SiO as bonding agent2) and/or three oxidations two Aluminium (Al2O3)。
In the present invention, described clay is preferably selected from kaolin and/or halloysite as matrix (i.e. carrier).
A kind of implementation method of the invention, the riser reactor for being used includes pre-lift successively from bottom to top Section, initial reaction area and main reaction region, the catalysis conversion method comprise the following steps:
By the pre lift zone of high-temperature regenerated catalyst injecting lift pipe reactor, to upstream in the presence of pre-lift medium The dynamic initial reaction area for entering riser reactor bottom, the high-chlorine raw material after preheating enters initial by riser reactor bottom In reaction zone, contacted with high-temperature regenerated catalyst, reacted and be up;The oil agent mixture for being formed enters riser reactor Main reaction region, the high-temperature regenerated catalyst with the bottom supplement injection in main reaction region proceeds hydrocarbon conversion reactions, reacts Into gas solid separation is carried out in the cyclone separator in settler, the solid catalyst isolated is treated through stripping for logistics afterwards Raw catalyst, and the reclaimable catalyst is injected into coke burning regeneration in regenerator, the high-temperature regenerated catalyst of activity recovery is returned respectively Return riser reactor pre lift zone and main reaction region in recycle;The reaction oil gas isolated deliver to subsequent product separation System isolates the cuts such as dry gas, liquefied gas, gasoline and diesel oil.
A kind of more preferably implementation method of the invention, the riser reactor for being used includes successively from bottom to top Pre lift zone, initial reaction area, addition reaction area and main reaction region, the catalysis conversion method comprise the following steps:
By the pre lift zone of high-temperature regenerated catalyst injecting lift pipe reactor, to upstream in the presence of pre-lift medium The dynamic initial reaction area for entering riser reactor bottom, the high-chlorine raw material after preheating enters initial by riser reactor bottom In reaction zone, contacted with high-temperature regenerated catalyst, reacted and be up;The oil agent mixture for being formed enters riser reactor Addition reaction area, the high-temperature regenerated catalyst with the bottom supplement injection in addition reaction area continues to react, then by additional anti- The oil agent mixture for answering area to be formed proceeds hydrocarbon conversion reactions into the main reaction region of riser reactor, logistics after reaction Gas solid separation is carried out into the cyclone separator in settler, the solid catalyst isolated obtains catalysis to be generated through stripping Agent, and the reclaimable catalyst is injected into coke burning regeneration in regenerator, the high-temperature regenerated catalyst of activity recovery returns to lifting respectively Recycled in the pre lift zone of pipe reactor and addition reaction area;The reaction oil gas isolated deliver to subsequent product piece-rate system Isolate the cuts such as dry gas, liquefied gas, gasoline and diesel oil.In the preferred embodiment, in addition reaction area, because supplement is noted The high-temperature regenerated catalyst for entering, is improved the reaction temperature reduced because initial reaction area reacts, and makes the addition reaction area Maintain reaction temperature higher, and the addition reaction area enlarged-diameter, bed speed slows down, density of catalyst increase, Oil gas increases in this section of residence time, so as to be conducive to improving dechlorination effect and improve high-chlorine raw material conversion ratio.
Specific embodiment of the invention is described in detail below in conjunction with accompanying drawing.It should be appreciated that this place is retouched The specific embodiment stated is merely to illustrate and explain the present invention, and is not intended to limit the invention.
A kind of flow of implementation method of the catalysis conversion method of the direct processing high-chlorine raw material that Fig. 1 is provided for the present invention is shown It is intended to.
The technological process of the method for present invention offer is provided referring to Fig. 1:As shown in figure 1, pre-lift medium is passed through Pipeline 14 is entered by the bottom of riser reactor 1, and the high-temperature regenerated catalyst from pipeline 12 adjusts laggard through regenerating guiding valve 13 Enter the bottom of riser reactor 1, accelerated upwards along riser under the castering action of pre-lift medium, the chlorine high of preheating Feedstock oil and is carried through the initial reaction area 17 of the injecting lift pipe reactor 1 together with the atomizing steam from pipeline 16 of pipeline 15 The existing logistics of riser reactors 1 mixing, high-chlorine raw material oil and high-temperature regenerated catalyst haptoreaction, and accelerate upwards, Into the main reaction region 18 of riser reactor, and from pipeline 26 and through regenerating the high temperature for supplementing injection after guiding valve 27 is adjusted again Raw catalyst continues haptoreaction.The whirlwind that the product oil gas of generation and the reclaimable catalyst of inactivation enter in settler 3 Separator 6, realizes that reclaimable catalyst is separated with product oil gas, and product oil gas enters collection chamber 7, catalyst fines Settler 3 is returned to by dipleg.Reclaimable catalyst in settler 3 flows to stripping section 4, is contacted with the steam from pipeline 19.From The product oil gas being stripped off in reclaimable catalyst enters collection chamber 7 after cyclone separator.Reclaimable catalyst after stripping Regenerator 2 is injected by pipeline 9 after being adjusted through guiding valve to be generated 8, the air from pipeline 21 distributes laggard through air distributor 22 Enter regenerator 2, coke of the burning-off on reclaimable catalyst in the dense-phase bed of the bottom of regenerator 2 makes the catalysis to be generated of inactivation Agent regenerates, and flue gas enters subsequent power recovery system through the upper gas flue 25 of cyclone separator 24.Wherein, it is described pre- Lifting medium can be dry gas, vapor or their mixture.
Catalyst after regeneration passes through the entrance degassing tank 5 of pipeline 10 connect with the catalyst outlet of regenerator 2, and from degassing The stripping fluid contact of the pipeline 23 of the bottom of tank 5, the flue gas of removing regenerated catalyst entrainment, the high-temperature regenerated catalyst after degassing A part is recycled to the bottom of riser reactor 1 through pipeline 12, can control catalyst internal circulating load by regenerating guiding valve 13, separately A part is recycled to the main reaction region 18 of riser reactor 1 through pipeline 26, and it can control catalyst by regenerating guiding valve 27 Internal circulating load;The gas produced after degassing is returned in regenerator 2 through pipeline 11, and the product oil gas in collection chamber 7 is through excessive oil Gas pipeline 20 enters subsequent separation system.
A kind of stream of the preferred embodiment of the catalysis conversion method of the direct processing high-chlorine raw material that Fig. 2 is provided for the present invention Journey schematic diagram.
Preferred embodiment shown in Fig. 2 is to be had made some improvements on the basis of the implementation method shown in Fig. 1 and obtained , specifically, addition reaction area 28 is set up between the initial reaction area 17 and main reaction region 18 of riser reactor 1, this is attached Plus reaction zone is expanding, its internal diameter is about 1.2 times of the internal diameter of main reaction region 18.In the addition reaction area 28, because of new benefit The high-temperature regenerated catalyst of addition is filled, the reaction temperature for making lifting bottom of the tube be fallen by cracking reaction is improved, and makes this Reaction zone maintains the internal diameter in reaction temperature higher, the addition reaction area to expand, and bed speed slows down, density of catalyst increase, Oil gas increases in this section of residence time, and dechlorination effect is more preferable.
The advantage of catalysis conversion method of the processing high-chlorine raw material that the present invention is provided is:
First in the initial reaction area of riser reactor, high-chlorine raw material is contacted with high-temperature regenerated catalyst, is conducive to Carbon-chlorine cleavage reaction;One high-temperature regenerated catalyst is added in the bottom of riser reactor, there is provided agent oil higher Than that for high-chlorine raw material cracking provides a large amount of acid centres, high-chlorine raw material can be made to carry out converting instead under acid centre effect Should, so as to improve the reaction conversion ratio of high-chlorine raw material.Simultaneously as initial reaction area employs undergauge structure substantially reducing In the reaction time, so as to reduce absorption of the coke precursor on acid centre in raw material, reduce coke yield.
Secondly, high-temperature regenerated catalyst is divided to two strands can be caused entirely to react in a ratio for relative equilibrium into reactor Carried out at temperature higher, be so more beneficial for the carrying out of high-chlorine raw material dechlorination reaction so that high-chlorine raw material is further converted to Liquefied gas and gasoline, improve feed stock conversion, meanwhile, high-temperature regenerated catalyst is added at twice, which reduces coke product Rate, while also slow down the generation of dry gas during crack materials.
Below will by embodiment, the invention will be further described, it is but not thereby limiting the invention.
In the following Examples and Comparative Examples, dechlorination rate and conversion ratio are calculated according to below equation:
Dechlorination rate=(in the chloride content-gasoline in raw material in chlorinity-diesel oil in chlorinity-heavy oil chlorinity) Chloride content × 100% in ÷ feedstock oils
Conversion ratio=dry gas yield+yield of liquefied gas+yield of gasoline+coking yield
The property of high-chlorine raw material oil used in following examples and comparative example as shown in table 1, urge by catalyzed conversion used As shown in table 2, the catalyst is by catalyst branch company of Sinopec Group Shandong catalyst for the property of agent Factory produces, product designation MLC-500.
Table 1
Project Raw material oil nature
Density (20 DEG C), g/cm3 0.926
Viscosity (80 DEG C), mm/s 43.65
Freezing point, DEG C -12
Carbon residue, weight % 6.49
Basic nitrogen, weight % 0.161
Chloride content, ppm 53
Element is constituted, weight %
Carbon 85.61
Hydrogen 12.05
Sulphur 0.79
Nitrogen 0.41
Table 2
Project MLC-500
Quality composition/weight %
RE2O3 2.7
Al2O3 55.9
Na2O 0.29
Specific surface area/(m2·g-1) 153
Pore volume/(cm3·g-1) 0.174
Tenor/(μ gg-1)
Fe 0.19
Ca 0.052
Sb 0.037
Hydrothermal conditions
Temperature/DEG C 800
Time/h 17
Micro-activity/% 65
Embodiment 1
The present embodiment is used to illustrate the catalysis conversion method of direct processing high-chlorine raw material of the present invention.
Tested according to the flow shown in Fig. 2, tested on kitty cracker, high-chlorine raw material oil preheating To 380 DEG C of initial reaction areas through the injecting lift pipe reactor of pipeline 15, with the high-temperature regenerated catalyst lifted by vapor (660 DEG C) in initial reaction area haptoreaction, wherein, agent weight of oil ratio be 15:1, the reaction time is 0.8 second, and reaction temperature is 560 DEG C, vapor is 0.05 with the weight ratio of high-chlorine raw material oil:1.The oil agent mixture of initial reaction area generation is advanced on continuing Enter addition reaction area, (660 DEG C) are continued haptoreactions with the high-temperature regenerated catalyst injected by pipeline 26, wherein, agent oil weight Amount is than being 30:1, the reaction time is 1.5 seconds, and reaction temperature is 545 DEG C.The oil agent mixture of addition reaction area generation continues up Reacted into main reaction region, wherein, reaction temperature is 505 DEG C, and the reaction time is 1.5 seconds, initial reaction area and main reaction The ratio between the riser diameter in area is 0.6:1, the ratio between riser diameter of addition reaction area and main reaction region is 1.2:1.Then will The reaction mass generated through main reaction region carries out gas solid separation, and the oil gas isolated enters rear portion after being separated through cyclone separator Fractionating system, isolates dry gas, liquefied gas, gasoline, diesel oil, heavy oil, coke etc., and the reclaimable catalyst with carbon deposit isolated enters Enter stripping section to be stripped, then go regenerator coke burning regeneration and degassing tank degassing process to obtain high-temperature regenerated catalyst, and A part of high-temperature regenerated catalyst is controlled internal circulating load and the bottom of riser reactor is returned to by pipeline 12 through regenerating guiding valve 13 Portion is recycled, and another part high-temperature regenerated catalyst is controlled internal circulating load and returned by pipeline 26 additional through regenerating guiding valve 27 Reaction zone is recycled.Operating condition and result of the test are as shown in table 3.
Comparative example 1
It is in place of the test method that this comparative example is used and the main difference of embodiment 1, the riser of this comparative example Reactor is not provided with initial reaction area and addition reaction area, and other operating conditions are same as Example 1, specifically, high-chlorine raw material Oil is preheated to 220 DEG C of bottoms through pipeline injecting lift pipe reactor, with the high-temperature regenerated catalyst (660 lifted by vapor DEG C) haptoreaction, wherein, reaction temperature is 560 DEG C, and the reaction time is 3.8 seconds, and agent weight of oil ratio is 30:1.Then will generation Material carry out gas solid separation, the oil gas isolated through cyclone separator separate after enter rear portion fractionating system, isolate dry Air-liquid gas, gasoline, diesel oil, heavy oil, coke etc., the reclaimable catalyst with charcoal isolated enter stripping section, treating after stripping Raw catalyst goes regenerator to regenerate and degassing tank degassing process, and enters riser reactor by high-temperature regenerated catalyst is obtained Bottom cycle is used.Operating condition and result of the test are as shown in table 3.
Embodiment 2
The present embodiment is used to illustrate the catalysis conversion method of direct processing high-chlorine raw material of the present invention.
The test method that the present embodiment is used is with the main difference part of embodiment 1, as shown in figure 1, this implementation The riser reactor of example is not provided with addition reaction area, and other operating conditions are same as Example 1, specifically, high-chlorine raw material oil 380 DEG C of initial reaction areas through the injecting lift pipe reactor of pipeline 15 are preheated to, are catalyzed with the high temperature regeneration lifted by vapor Agent (660 DEG C) in initial reaction area haptoreaction, wherein, agent weight of oil ratio be 15:1, the reaction time is 0.8 second, reaction temperature It it is 560 DEG C, vapor is 0.05 with the weight ratio of high-chlorine raw material oil:1.The oil agent mixture of initial reaction area generation continues up Into main reaction region, (660 DEG C) are continued haptoreactions with the high-temperature regenerated catalyst injected by pipeline 26, wherein, agent oil weight Amount is than being 30:1, the reaction time is 3 seconds, and reaction temperature is 505 DEG C, the ratio between riser diameter of initial reaction area and main reaction region It is 0.6:1.Then the reaction mass that will be generated through main reaction region carries out gas solid separation, and the oil gas isolated is through cyclone separator point From the fractionating system at rear entrance rear portion, dry gas, liquefied gas, gasoline, diesel oil, heavy oil, coke etc. are isolated, the band carbon deposit isolated Reclaimable catalyst stripped into stripping section, then go regenerator coke burning regeneration and degassing tank degassing process to obtain high temperature Regenerated catalyst, and a part of high-temperature regenerated catalyst is controlled internal circulating load and return to lifting by pipeline 12 through regenerating guiding valve 13 The bottom cycle of pipe reactor is used, and through regenerating guiding valve 27 another part high-temperature regenerated catalyst is controlled into internal circulating load and by pipe Line 26 returns to main reaction region and recycles.Operating condition and result of the test are as shown in table 3.
Embodiment 3
The present embodiment is used to illustrate the catalysis conversion method of direct processing high-chlorine raw material of the present invention.
Tested according to the flow shown in Fig. 2, tested on kitty cracker, high-chlorine raw material oil preheating To 220 DEG C of initial reaction areas through the injecting lift pipe reactor of pipeline 15, with the high-temperature regenerated catalyst lifted by vapor (650 DEG C) in initial reaction area haptoreaction, wherein, agent weight of oil ratio be 30:1, the reaction time is 0.2 second, and reaction temperature is 550 DEG C, vapor is 0.05 with the weight ratio of high-chlorine raw material oil:1.The oil agent mixture of initial reaction area generation is advanced on continuing Enter addition reaction area, (650 DEG C) are continued haptoreactions with the high-temperature regenerated catalyst injected by pipeline 26, wherein, agent oil weight Amount is than being 40:1, the reaction time is 3 seconds, and reaction temperature is 545 DEG C.The oil agent mixture of addition reaction area generation is advanced on continuing Enter main reaction region to be reacted, wherein, reaction temperature is 520 DEG C, and the reaction time is 4 seconds, initial reaction area and main reaction region The ratio between riser diameter is 0.6:1, the ratio between riser diameter of addition reaction area and main reaction region is 1.2:1.Then will be through master The reaction mass of reaction zone generation carries out gas solid separation, and the oil gas isolated enters the fractionation at rear portion after being separated through cyclone separator System, isolates dry gas, liquefied gas, gasoline, diesel oil, heavy oil, coke etc., and the reclaimable catalyst with carbon deposit isolated enters vapour Put forward section to be stripped, then go regenerator coke burning regeneration and degassing tank degassing process to obtain high-temperature regenerated catalyst, and by one Part high-temperature regenerated catalyst is through regenerating the control internal circulating load of guiding valve 13 and being followed by the bottom that pipeline 12 returns to riser reactor Ring is used, and internal circulating load is controlled and return to addition reaction by pipeline 26 another part high-temperature regenerated catalyst through regenerating guiding valve 27 Area recycles.Operating condition and result of the test are as shown in table 3.
Embodiment 4
The present embodiment is used to illustrate the catalysis conversion method of direct processing high-chlorine raw material of the present invention.
Tested according to the flow shown in Fig. 2, tested on kitty cracker, high-chlorine raw material oil preheating To 300 DEG C of initial reaction areas through the injecting lift pipe reactor of pipeline 15, with the high-temperature regenerated catalyst lifted by vapor (670 DEG C) in initial reaction area haptoreaction, wherein, agent weight of oil ratio be 25:1, the reaction time is 1.5 seconds, and reaction temperature is 600 DEG C, vapor is 0.05 with the weight ratio of high-chlorine raw material oil:1.The oil agent mixture of initial reaction area generation is advanced on continuing Enter addition reaction area, (660 DEG C) are continued haptoreactions with the high-temperature regenerated catalyst injected by pipeline 26, wherein, agent oil weight Amount is than being 60:1, the reaction time is 2 seconds, and reaction temperature is 585 DEG C.The oil agent mixture of addition reaction area generation is advanced on continuing Enter main reaction region to be reacted, wherein, reaction temperature is 540 DEG C, and the reaction time is 3 seconds, initial reaction area and main reaction region The ratio between riser diameter is 0.6:1, the ratio between riser diameter of addition reaction area and main reaction region is 1.2:1.Then will be through master The reaction mass of reaction zone generation carries out gas solid separation, and the oil gas isolated enters the fractionation at rear portion after being separated through cyclone separator System, isolates dry gas, liquefied gas, gasoline, diesel oil, heavy oil, coke etc., and the reclaimable catalyst with carbon deposit isolated enters vapour Put forward section to be stripped, then go regenerator coke burning regeneration and degassing tank degassing process to obtain high-temperature regenerated catalyst, and by one Part high-temperature regenerated catalyst is through regenerating the control internal circulating load of guiding valve 13 and being followed by the bottom that pipeline 12 returns to riser reactor Ring is used, and internal circulating load is controlled and return to addition reaction by pipeline 26 another part high-temperature regenerated catalyst through regenerating guiding valve 27 Area recycles.Operating condition and result of the test are as shown in table 3.
Table 3
Embodiment 1 Comparative example 1 Embodiment 2 Embodiment 3 Embodiment 4
Raw material preheating temperature, DEG C 380 220 380 220 300
Reaction temperature, DEG C
Initial reaction area 560 - 560 550 600
Addition reaction area 545 - - 545 585
Main reaction region 505 560 505 520 540
Reaction time, second
Initial reaction area 0.8 - 0.8 0.2 1.5
Addition reaction area 1.5 - - 3 2
Main reaction region 1.5 3.8 3.0 4 3
Agent weight of oil ratio
Initial reaction area 15 - 15 30 25
Addition reaction area 30 - - 40 60
Main reaction region 30 30 30 40 60
Vapor and raw material weight ratio 0.05 0.05 0.05 0.05 0.05
Product slates, weight %
Dry gas 1.83 1.99 1.90 1.87 2.56
Liquefied gas 25.31 9.92 24.73 25.14 24.51
Gasoline 43.11 39.81 42.89 42.81 41.39
Diesel oil 16.22 16.81 15.73 15.59 14.75
Heavy oil 8.15 25.34 9.52 9.42 9.81
Coke 4.98 6.13 5.23 5.17 6.98
Dechlorination rate, weight % 70.4 40.2 72.1 72.5 74.1
Conversion ratio, weight % 75.63 57.85 74.75 74.99 75.44
Be can be seen that by the result of above-described embodiment and comparative example can directly process height according to method of the present invention Chlorine raw material simultaneously obtains dechlorination rate higher, but also can improve the conversion ratio of high-chlorine raw material, improves product selectivity, reduces Dry gas and coke yield.

Claims (20)

1. a kind of catalysis conversion method for directly processing high-chlorine raw material, the method includes:By the high-chlorine raw material after preheating and first Catalytic converting catalyst carries out catalytic conversion reaction in the initial reaction area of riser reactor, and makes by the initial reaction Area produce oil agent mixture enter riser reactor main reaction region, with supplement injection the second catalytic converting catalyst after It is continuous to carry out catalytic conversion reaction, wherein, the reaction temperature of the reaction temperature higher than the main reaction region in the initial reaction area, institute State the reaction time of reaction time in initial reaction area less than the main reaction region, first catalytic converting catalyst with it is described Second catalytic converting catalyst is identical or different, and the two is respectively high-temperature regenerated catalyst;
Wherein, the high-chlorine raw material is catalytic cracking of hydrocarbons of the chloride content more than 50ppm or organic chloride content more than 10ppm Oily raw material.
2. method according to claim 1, wherein, the reaction temperature in the initial reaction area is more anti-than the main reaction region Answer temperature high 5-100 DEG C.
3. method according to claim 2, wherein, the reaction temperature in the initial reaction area is more anti-than the main reaction region Answer temperature high 10-80 DEG C.
4. method according to claim 1, wherein, the reaction time in the initial reaction area is more anti-than the main reaction region It is short 0.5-5 seconds between seasonable.
5. the method according to any one in claim 1-4, wherein, the reaction condition in the initial reaction area includes: Reaction temperature is 500-750 DEG C, and agent weight of oil ratio is 5-50: 1, and the reaction time is 0.1-1.9 seconds.
6. method according to claim 5, wherein, the reaction condition in the initial reaction area includes:Reaction temperature is 550-700 DEG C, agent weight of oil ratio is 10-30: 1, and the reaction time is 0.2-1.5 seconds.
7. the method according to any one in claim 1-4, wherein, the agent weight of oil ratio of the main reaction region is 15- 80: 1, the reaction time is 1-8 seconds.
8. method according to claim 7, wherein, the agent weight of oil ratio of the main reaction region is 15-60: 1, reaction time It is 1.5-6 seconds.
9. method according to claim 1, wherein, in the riser reactor, the initial reaction area with it is described The ratio between riser diameter of main reaction region is 0.5-0.8:1.
10. the method according to claim 1 or 9, wherein, in the riser reactor, in the initial reaction area Addition reaction area is additionally provided with and the main reaction region between.
11. methods according to claim 10, wherein, the reaction condition in the addition reaction area includes:Reaction temperature is 500-750 DEG C, agent weight of oil ratio is 15-80: 1, and the reaction time is 0.5-4 seconds.
12. methods according to claim 11, wherein, the reaction condition in the addition reaction area includes:Reaction temperature is 550-700 DEG C, agent weight of oil ratio is 15-60: 1, and the reaction time is 1-3 seconds.
13. methods according to claim 10, wherein, in the riser reactor, the addition reaction area and institute The ratio between riser diameter of main reaction region is stated for 1.05-1.8:1.
14. methods according to claim 1, wherein, first catalytic converting catalyst and second catalyzed conversion The temperature of catalyst is respectively 620-750 DEG C.
15. method according to claim 1 or 14, wherein, methods described also includes:Will be by the riser reactor Outlet discharge reaction mass carry out gas solid separation, the solid catalyst that will be isolated is stripped, coke burning regeneration and optionally Degassing process to obtain high-temperature regenerated catalyst, a part of high-temperature regenerated catalyst is recycled as first catalyzed conversion Catalyst, second catalytic converting catalyst is recycled as by another part high-temperature regenerated catalyst.
16. method according to claim 1 or 14, wherein, catalytic converting catalyst is to contain active component and carrier Solid acid catalyst, the active component is selected from Y or HY types zeolite, the zeolite with MFI structure, octahedral with or without rare earth At least one in zeolite and alumina silicate, the carrier is selected from least one in inorganic oxide and natural clay.
17. methods according to claim 1, wherein, the temperature after the high-chlorine raw material preheating is 150-400 DEG C.
18. methods according to claim 17, wherein, the temperature after the high-chlorine raw material preheating is 220-380 DEG C.
19. methods according to claim 1, wherein, the high-chlorine raw material is selected from crude oil and heavy oil, and the heavy oil is fore-running Point is not less than 250 DEG C of hydrocarbon oil cut.
20. methods according to claim 19, wherein, the high-chlorine raw material is selected from wax tailings, decompressed wax oil, decompression slag At least one in oil, deasphalted oil, extract oil, recycle oil inferior, crude oil, shale oil and oil-sand.
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CN103031147A (en) * 2011-09-29 2013-04-10 中国石油化工股份有限公司 Catalytic conversion method for processing high-nitrogen raw material
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