CN101875858A - Method for treating solid particles of deposited carbon-containing compound - Google Patents
Method for treating solid particles of deposited carbon-containing compound Download PDFInfo
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- CN101875858A CN101875858A CN2009101358817A CN200910135881A CN101875858A CN 101875858 A CN101875858 A CN 101875858A CN 2009101358817 A CN2009101358817 A CN 2009101358817A CN 200910135881 A CN200910135881 A CN 200910135881A CN 101875858 A CN101875858 A CN 101875858A
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Abstract
The invention relates to a method for treating solid particles of a deposited carbon-containing compound, which is characterized by comprising the following steps: the solid particles of the deposited carbon-containing compound generated by a reactor contact and react with a gasifying agent in a gasification furnace at 700-900 DEG C, thus the conversion rate of the deposited carbon-containing compound is 60-90wt%, and coarse synthetic gas rich in H2 and CO and semi-regenerative solid particles are obtained; and the semi-regenerative solid particles contact with an oxygen-containing gas in a regenerator and are combusted to be fully regenerated, and then the combusted solid particles are delivered into the reactor for cycle use, wherein the gasifying agent is a mixed gas of vapor and oxygen.
Description
Technical field
The present invention relates to a kind of treatment process of solid particulate of deposited carbon-containing compound, more particularly, be the method that a kind of solid particulate of the carbon compound that will form is used for vaporizing system synthetic gas or hydrogen and solid particulate regeneration is used in the mink cell focus course of processing.
Background technology
Along with world wide oil property heaviness, the aggravation of inferiorization degree, market is to the increase in demand of lightweight, clean fuel oil simultaneously, and the environmental requirement increasingly stringent proposes requirements at the higher level to petroleum refining industry.Mink cell focus processing is nothing more than decarburization and hydrogenation two classes.Decarbonization process is the main method of heavy oil upgrading, mainly comprises heavy oil fluid catalytic cracking, solvent deasphalting, coking etc.Catalytic cracking is because catalyzer is comparatively strict to ingredient requirement, and the rational Application of carbon distribution on the spent agent is acquired a certain degree of difficulty, and is especially true when especially coke content is high on the spent agent.
Coking is a kind of heavy oil thermal processing method, and external 60% residual oil adopts this method now, and its shortcoming is that liquid product yield is low.Catalytic cracking technology is used for residual oil pyrolysated fluid coking technology, hard and volatile matter is low because of coke breeze, be difficult to handle, make its development be absorbed in stagnant condition.In order to solve the problem of coke breeze, developed the flexicoking processing method of fluid coking and gasification combination again, can significantly reduce coke output and produce synthesis gas, but owing to use air and water vapour as vaporized chemical, contain a large amount of nitrogen in the synthesis gas of producing, feasible wherein available gas (H
2+ CO) content is lower, and calorific value is also very low.In addition, for carrying the charcoal particle, solid particles flowing is a coke granule to this technology between coking reactor, interchanger, vapourizing furnace with Jiao's nuclear.Since the coke granule out-of-shape, and easily form larger particles in the coking reactor, and so coke needs high pressure water to smash larger particles before going out coking reactor, the size-grade distribution of carbon granule changes greatly like this, makes fluidization be difficult to keep stable.
The hydrogenation process of oil refining for improve the level of crude oil processing, improve quality product, to improve yield of light oil significant, but hydrogenation technique needs a large amount of hydrogen, the hydrogen amount of original refinery by-product can not satisfy the demands.Prior art also provides multiple other hydrogen manufacturing modes such as Methane Steam Reforming, heavy oil hydrogen manufacturing, gasification hydrogen manufacturing, but it is higher that these methods are produced the cost of hydrogen, in whole hydrogenation cost, occupy sizable ratio, thereby influence the economic benefit of hydrogenation process, make hydrogen come source problem perplexing oil refining industry always.
Therefore, seeking the route that oil refining combines with hydrogen manufacturing is paid close attention to by people.For example: USP5362380 discloses a kind of catalytic cracking hydrogen production process, and this method is that reclaimable catalyst is at first reacted the sufficiently long time down at 537～649 ℃ with water vapor under the environment of anaerobic, contains H with generation
2, CO
2, CO, CH
4Gas stream, make the carbon content on the reclaimable catalyst reduce to 0.3～0.8w% simultaneously; Separate above-mentioned gas logistics and catalyzer, further isolate the hydrogen-rich stream that contains 90～97v% hydrogen after the gas stream cooling.Catalyzer contacts, regenerates with oxygen-containing gas, and the catalyst recirculation after the regeneration is used.Adopt this method hydrogen manufacturing, the duration of contact of water vapor and reclaimable catalyst is long, speed of reaction is slow, not only influences the economy of this method, and hydrothermal aging that also can accelerator activator is affected activity of such catalysts and life-span, so practicality is very low.
The disclosed a kind of method of utilizing regeneration fume from catalytic cracking hydrogen manufacturing of CN1400159A mainly may further comprise the steps: (1). and hydrocarbon oil crude material contacts with catalytic cracking catalyst and reacts; (2). the catalyzer of separating reaction oil gas and carbon deposit, oil gas is sent into subsequent separation system, and the catalyzer of carbon deposit is delivered to first revivifier behind stripping; (3). in first revivifier, the catalyzer of carbon deposit and oxygen-containing gas contact 2～25 seconds under 500～660 ℃, the condition of gas empty bed speed 0.2～0.8m/s after, regenerated flue gas is delivered to follow-up hydrogen production process; (4). separate from the CO in the regenerated flue gas of step (3), make CO and water vapor carry out transformationreation, and from the gas products that is generated separating hydrogen gas; (5). half regenerated catalyst from step (3) enters second revivifier, contacts with oxygen-containing gas, and regenerates under the catalytic cracked regenerated condition of routine, and the catalyzer Returning reactor after the regeneration recycles.This method not only can make the CO in the regenerated flue gas rationally be utilized, and the superfluous problem of heat of FCC apparatus is eased.
CN 1504404A has proposed a kind of oil refining and gasification process combined method, this method is to make petroleum hydrocarbon contact in reactor, react with coke transfer agent, isolating carbon deposit coke transfer agent is delivered to vapourizing furnace behind stripping, in vapourizing furnace, the coke transfer agent of carbon deposit and water vapour and oxygen-containing gas contact 0.5-25 second under 800～1100 ℃, the condition of 0.2～5.0m/s, to produce synthetic gas, make the coke transfer agent of carbon deposit obtain regeneration simultaneously, recycle in the coke transfer agent Returning reactor after the regeneration.In the method, the coke transfer agent of carbon deposit is all regenerated in vapourizing furnace, is not suitable for the regeneration of the high coke transfer agent of carbon distribution content, and the coke transfer agent behind the high temperature regeneration can recycle by Returning reactor after need cooling off, and capacity usage ratio is low.
Summary of the invention
The treatment process that the purpose of this invention is to provide a kind of solid particulate of the deposited carbon-containing compound that is different from prior art.
The treatment process of the solid particulate of deposited carbon-containing compound provided by the invention, it is characterized in that this method comprises: the solid particulate of the deposited carbon-containing compound that produces by reactor in vapourizing furnace with a kind of vaporized chemical 700～900 ℃, gas empty bed speed 0.05～5.0 meter per second, contact reacts 0.5～30 second, making sedimentary carbon compound transformation efficiency is 60～90 weight %, obtains being rich in H
2, the crude synthesis gas body of CO and the solid particulate of partly regenerating, the solid particulate of partly regenerating contacts with oxygen-containing gas in revivifier, burning is able to holomorphosis, sends into reactor cycles then and uses, wherein said vaporized chemical is the mixed gas of water vapour and oxygen.
Treatment process provided by the invention has following characteristics:
1, described gasification is carried out under 700～900 ℃, and gasification temperature is moderate, and is less demanding to equipment material, less investment; In addition, this gasification temperature is higher than conventional catalytic cracking catalyst regeneration temperature again, and speed of response is very fast relatively, CO+H in the crude synthesis gas that is generated
2Content will can provide the higher-grade raw material for follow-up hydrogen production process greater than 60 volume % (table 1), be that prior art is difficult to realize.
2, sedimentary carbon compound on the solid particulate is carried out non-being gasified totally in vapourizing furnace, the control efficiency of carbon conversion is between 60～90 weight %, again remaining carbon compound is burnt at revivifier, can reduce vapourizing furnace load, flexible operation, and regenerator temperature is no more than 800 ℃, can not produce NO in combustion processes
x, environmentally friendly.
3, method provided by the invention, can be at the solid particulate of carbon compound content between 1～5 weight %, be applicable to the regenerative process of the thermal barrier/catalyzer of fluid coking, slight catalytic cracking, hydrotreatment demetalization etc., the refinery opened up new refinery combined process a practical way is provided.
Embodiment
In the method provided by the invention, described reactor can be fluid coking reactor or slight catalyst cracker, and type of reactor of the two and reaction conditions have been conventionally known to one of skill in the art, do not give unnecessary details here.
Described solid particulate can be one or more the mixture in quartz sand, kaolin, pickling carclazyte, amorphous silicon aluminium, semi-synthetic sial, aluminum oxide, titanium dioxide, the waste cracking catalyst.For the ease of the operation of fluidization system, described solid particulate is the microballoon of spray-dried moulding, median size 50～100 μ m, and the particle abrasion resistance index is at 0.5～4.0%h
-1Said solid particulate can contain the mixture that is selected from basic metal, alkaline-earth metal and the rare earth metal one or more of the no more than 10 weight % of content, preferred 2～8 weight %, for example Na or Ce.In reactor, solid particulate is with after heavy oil contacts, surface deposition the carbon compound of 1～5 weight %, the principal element of carbon compound consists of C, H, S, N, wherein the content of carbon is at 86～96 weight %.On solid particulate, the distribution of said carbon compound can be eggshell type (being wrapped in the outside surface of solid particulate) or sponge-type (being deposited on the duct internal surface of solid particulate) or two kinds of distribution forms and deposit.
Method provided by the invention, in the said vaporized chemical, the mol ratio of water vapor and oxygen is (1～10): 1, preferred (2～6): 1.
The solid particulate of deposited carbon-containing compound in vapourizing furnace with the catalytic optimum condition of vaporized chemical is: temperature 700-860 ℃, pressure 100～500kPa, gas empty bed speed 0.2～2.0 meter per second, reaction times is 1～15 second, and making sedimentary carbon compound transformation efficiency is 75～85 weight %.
Described vapourizing furnace is preferably fluidized-bed reactor, and the bed of vapourizing furnace is preferably gas-solid and fluidized bed layer.
In the treatment process provided by the invention, the solid particulate of deposited carbon-containing compound is after gasification, and the crude synthesis gas body that obtains is rich in H
2, CO, also contain carbonic acid gas and a small amount of methane and hydrogen sulfide, above-mentioned crude synthesis gas body can be become produce clean hydrogen by unit such as heat exchange, dedusting, converter unit, desulfurization and decarburizations successively, such process is the processing mode of routine, this no longer numerous stating.
In the treatment process provided by the invention, the solid particulate of deposited carbon-containing compound is after gasification, the solid particulate of partly regenerating that obtains, be admitted in the revivifier, under 500～700 ℃ of temperature of reaction, gas empty bed speed 0.5～5.0m/s, the condition in 0.5～25 second reaction times, contact and remove remaining carbon compound with oxygen-containing gas, be able to holomorphosis, deliver to fluidized reactor and recycle; And regenerated flue gas is delivered to follow-up heat reclaiming system, enters atmosphere after treatment.Said oxygen-containing gas is meant a kind of in air, oxygen-rich air or the oxygen, wherein preferred air.
The invention will be further described below by embodiment, but content not thereby limiting the invention.
Embodiment 1
In the present embodiment, solid particulate is the microballoon that kaolin is made, median size 65 μ m.
The content of carbon distribution is 2.1w% on the kaolin microsphere particle.
Reaction product is separated with carbon distribution kaolin, kaolin particle is sent into vapourizing furnace then, mol ratio is that 5: 1 water vapors and oxygen add from the vapourizing furnace bottom, temperature of reaction is 700 ℃, gas empty bed speed is 0.2m/s, reaction times is 12 seconds, and the transformation efficiency of the carbon compound on the solid particulate in vapourizing furnace is controlled at 62w%.
The crude synthesis gas body is with after the kaolin particle of partly regenerating separates, and the crude synthesis gas body is through the cooling sampling, and the promoting the circulation of qi analysis of hplc of going forward side by side the results are shown in Table 1.
The kaolin particle of partly regenerating is sent into revivifier, and air joins in the revivifier.The reaction conditions of revivifier comprises: temperature of reaction is 680 ℃, and pressure is 150 kPas, about 10 seconds of gas mean residence time.The regeneration kaolin particle with enter reactor cycles after flue gas separates and use.
Embodiment 2
In the present embodiment, solid particulate the has been load kaolin microsphere particle of Ce of 5w%, median size 78 μ m.
Through behind the reactor, the carbon distribution content of the kaolin particle of 5w%Ce is 3.5w%.Gasification reaction conditions is: temperature of reaction is 860 ℃, and gas empty bed speed is 1.0m/s, and the reaction times is 5 seconds, and water vapour and oxygen mol ratio are 2: 1.The transformation efficiency of carbon compound on the solid particulate in vapourizing furnace is controlled at 85w%.
The composition of operational condition and crude synthesis gas body sees Table 1.
The kaolin particle of partly regenerating is sent into revivifier, and air joins in the revivifier.The reaction conditions of revivifier comprises: temperature of reaction is 680 ℃, and pressure is 150 kPas, about 10 seconds of gas mean residence time.The regeneration kaolin particle with enter reactor cycles after flue gas separates and use.
Embodiment 3
In the present embodiment, solid particulate the has been load kaolin microsphere particle of Na of 5w%, median size 80 μ m.
Through behind the reactor, the carbon distribution content of the kaolin particle of 5wNa% is 5.0w%.Gasification reaction conditions is: temperature of reaction is 800 ℃, and gas empty bed speed is 2.0m/s, and the reaction times is 20 seconds, and water vapour and oxygen mol ratio are 4: 1.The transformation efficiency of carbon compound on the solid particulate in vapourizing furnace is controlled at 78w%.
The composition of operational condition and crude synthesis gas body sees Table 1.
The kaolin particle of partly regenerating is sent into revivifier, and air joins in the revivifier.The reaction conditions of revivifier comprises: temperature of reaction is 680 ℃, and pressure is 150 kPas, about 10 seconds of gas mean residence time.The regeneration kaolin particle with enter reactor cycles after flue gas separates and use.
Table 1
Annotate: hydrogen yield is that carbon distribution transforms the speed of producing hydrogen in vapourizing furnace, and the amount of hydrogen has comprised that CO equivalent is transformed to H
2Amount.
The composition of crude synthesis gas as can be seen from table 1: oxygen-free gas component in the reaction product gas that embodiment 1～3 obtains; Available gas (CO and H
2) total content is greater than 75 volume %.
If the result with embodiment 2 is as the criterion, then use method of the present invention, year treatment capacity is the device of 1,000,000 tons in residual oil, solid particulate is 5: 1 with the residual oil ratio, advance that carbon distribution content is 3.5 weight % on the solid particulate of vapourizing furnace, the transformation efficiency of carbon distribution in vapourizing furnace is 85 weight %, and the crude synthesis gas of generation goes out clean hydrogen through process for producing, then annual amount of producing hydrogen is 2.4 ten thousand tons, amounts to 26,980 ten thousand Nm
3/ year.If the hydrogen consumption of decompressed wax oil hydrocracking is 190Nm
3/ ton, then the hydrogen of this device of 1,000,000 tons/year production can satisfy the hydrogen of using of 1,400,000 tons of/year hydroeracking units.
Claims (10)
1. the treatment process of the solid particulate of a deposited carbon-containing compound is characterized in that this method comprises:
The solid particulate of the deposited carbon-containing compound that produces by reactor in vapourizing furnace with a kind of vaporized chemical 700～900 ℃, gas empty bed speed 0.05～5.0 meter per second, contact reacts 0.5～30 second, making sedimentary carbon compound transformation efficiency is 60～90 weight %, obtains being rich in H
2, the crude synthesis gas body of CO and the solid particulate of partly regenerating, the solid particulate of partly regenerating contacts with oxygen-containing gas in revivifier, burning is able to holomorphosis, sends into reactor cycles then and uses, wherein said vaporized chemical is the mixed gas of water vapour and oxygen.
2. according to the method for claim 1, it is characterized in that described solid particulate is selected from one or more the mixture in refinery coke, quartz sand, kaolin, pickling carclazyte, amorphous silicon aluminium, semi-synthetic sial, aluminum oxide, titanium dioxide, the waste cracking catalyst.
3. according to the method for claim 1, it is characterized in that the content of carbon compound in the solid particulate of said deposited carbon-containing compound is 1～5 weight %.
4. according to the method for claim 1, it is characterized in that said solid particulate contains one or more the mixture in basic metal, alkaline-earth metal or the rare earth metal of being selected from of no more than 10 weight %.
5. according to the method for claim 1, it is characterized in that said basic metal is Na, rare earth metal is Ce.
6. according to the method for claim 1, it is characterized in that the mol ratio of water vapor and oxygen is (1～10) in the said vaporized chemical: 1.
7. according to the method for claim 1, it is characterized in that described vapourizing furnace is a fluidized-bed reactor.
8. according to the method for claim 7, the bed that it is characterized in that described fluidized-bed reactor is gas-solid and fluidized bed layer.
9. according to the method for claim 1, the condition that the solid particulate of said deposited carbon-containing compound contacts with vaporized chemical in vapourizing furnace is: temperature 700-860 ℃, pressure 100～500kPa, gas empty bed speed 0.2～2.0 meter per second, reaction times is 1～15 second, and making sedimentary carbon compound transformation efficiency is 75～85 weight %.
10. according to the method for claim 1, the said solid particulate of partly regenerating is 500～700 ℃ of temperature, gas empty bed speed 0.5～5.0m/s, 0.5～25 second reaction times with the oxygen-containing gas contact conditions in revivifier.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103055960A (en) * | 2011-10-19 | 2013-04-24 | 中国石油化工股份有限公司 | Catalyst regeneration method with characteristic of discharge reduction |
| CN103382401A (en) * | 2012-05-02 | 2013-11-06 | 新奥科技发展有限公司 | Gasification raw material, preparation method of the gasification raw material, and catalytic gasification method adopting the gasification raw material |
| CN103933995A (en) * | 2014-04-12 | 2014-07-23 | 深圳市绿野清风环保工程有限公司 | Rubbish gasification catalyst and preparation method thereof |
| CN106669710A (en) * | 2015-11-11 | 2017-05-17 | 中国石油化工股份有限公司 | Regenerating method for catalyst for catalyzing diesel oil hydrocracking |
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| CN1400159A (en) * | 2001-07-31 | 2003-03-05 | 中国石油化工股份有限公司 | Hydrogen-making method by utilizing catalytic cracked regenerated flue gas |
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| CN1608972A (en) * | 2004-09-20 | 2005-04-27 | 东南大学 | Biomass-gasifying hydrogen generating serial fluid bed apparatus and method |
| CN1626622A (en) * | 2004-04-07 | 2005-06-15 | 石油大学(北京) | Method of combined catalytic cracking regeneration technology and equipment |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103055960A (en) * | 2011-10-19 | 2013-04-24 | 中国石油化工股份有限公司 | Catalyst regeneration method with characteristic of discharge reduction |
| CN103055960B (en) * | 2011-10-19 | 2015-05-20 | 中国石油化工股份有限公司 | Catalyst regeneration method with characteristic of discharge reduction |
| CN103382401A (en) * | 2012-05-02 | 2013-11-06 | 新奥科技发展有限公司 | Gasification raw material, preparation method of the gasification raw material, and catalytic gasification method adopting the gasification raw material |
| CN103382401B (en) * | 2012-05-02 | 2015-01-28 | 新奥科技发展有限公司 | Gasification raw material, preparation method of the gasification raw material, and catalytic gasification method adopting the gasification raw material |
| CN103933995A (en) * | 2014-04-12 | 2014-07-23 | 深圳市绿野清风环保工程有限公司 | Rubbish gasification catalyst and preparation method thereof |
| CN106669710A (en) * | 2015-11-11 | 2017-05-17 | 中国石油化工股份有限公司 | Regenerating method for catalyst for catalyzing diesel oil hydrocracking |
| CN106669710B (en) * | 2015-11-11 | 2019-02-22 | 中国石油化工股份有限公司 | A kind of regeneration method of catalytic diesel oil hydrocracking catalyst |
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