CN102309947A - On-line filling method for boiling bed catalyst - Google Patents
On-line filling method for boiling bed catalyst Download PDFInfo
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Abstract
The invention relates to an on-line filling method for a boiling bed catalyst. According the method, only the conventional on-line filling device is changed little, a catalyst filling tank is set as a fluidized bed, the catalyst in the catalyst filling tank is vulcanized by using system recycle hydrogen, and the catalyst is filled into a reactor by means of pressure difference of the catalyst filling tank and the reactor and under hydrogen delivery and gravity action. Compared with the prior art, the method has the advantages of reducing investment and simplifying the operation; meanwhile, the system recycle hydrogen is used as the hydrogen of the boiling bed catalyst, so the hydrogen has wide source and is convenient to treat; and because the catalyst is heated to the temperature of the reactor before filling, on-line filling disturbance to the reaction temperature of the boiling bed and influence of instable operation of the device on the product quality in the prior art are reduced. The on-line filling method for the catalyst is particularly suitable for a boiling bed hydrogenation process.
Description
Technical field
The present invention relates to the online charging method of a kind of boiling-bed catalyst.
Background technology
Along with the variation of oil product demand structure in the exploitation energetically of heavy crude and the world wide; Market maintains sustained and rapid growth to the demand of light-weight fuel oil and the demand of heavy oil is reduced rapidly, and heavy, deep processing technology residual oil has become the emphasis of petroleum refining industry's exploitation.As one of main processing of heavy oil means; The boiling bed residual oil hydrogen addition technology has good air-teturning mixed characteristic, have be convenient to control reaction temperature, adapt to different raw materials, to can onlinely the replacing of constant, the catalyst of the suit property of feedstock oil, catalyst activity, the mass transfer constant, that reactor temperature is even, good falls in pressure and heat transfer, characteristics such as service cycle is long, bottoms conversion is high, catalyst utilization is high, device flexible operation, investment are lower.
The boiling bed residual oil hydrogen addition technology, cycle of operation length is one of its important feature.Through catalyst in reactor being carried out periodic online displacement, guaranteed the activity of catalyst in reactor, reduced the increase that reactor pressure falls, thus the prolongation of the realization response device cycle of operation.Therefore, the online replacement technique of catalyst is one of guardian technique of boiling bed residual oil hydrogenation technique technology.
US3547809 introduces a kind of technology of the online adding of catalyst of fluidized bed reactor, and this patent joins a part of drawing from raw material with catalyst to be added and forms slurries, slurry mixture is joined in the fluidized bed reactor again.Because raw material and catalyst form slurries and just react easily outside reactor, coking influences the performance of catalyst, simultaneously not to the wetting and vulcanizing treatment of catalyst.
US4398852 introduces a kind of online adding mode of catalyst of fluidized bed reactor.This method is at first to join catalyst in the container of high voltage bearing Sheng catalyst; Then it is filled hydrogen pressure to reaction pressure; To be positioned at the valve open on catalyst container and the reactor connecting line thereupon, and make catalyst lean on gravity to get into fluidized bed reactor and participate in reaction.This process directly joins catalyst in the fluidized bed reactor for leaning on gravity, because the preheat temperature of catalyst and hydrogen is lower than reaction temperature, so can cause the ebullating bed reactor temperature fluctuation, the device operation is not steady, influences product quality.The variation of simultaneous temperature brings certain influence for the character of catalyst.And do not comprise in this patent the wetting of catalyst and vulcanizing treatment process.
Summary of the invention
To the deficiency of prior art, the present invention provides a kind of boiling-bed catalyst online charging method.
When ebullated bed main reaction flow process is normally carried out, if need a certain amount of catalyst of online filling.With need the catalyst of a certain amount of filling to be filled to jar at every turn; Then according to the purging of routine, airtight, drying etc.; Heat up then, boost, vulcanize, the dry method sulfuration is adopted in sulfuration, can lead in/out from the gas of reactor gaseous phase outlet or the portion of hot material of hot high score gaseous phase outlet.Keep certain pressure reduction that required catalyst is filled in the reactor with reactor in catalyst filling jar, realize the stable long-term operation of technological process.
The online charging method of catalyst provided by the invention may further comprise the steps:
(1) fresh catalyst is added the catalyst storage tank, feed nitrogen protection;
(2) fresh catalyst in the catalyst storage tank joins catalyst filling jar under the gravity effect, and is warmed up to 200 ℃～250 ℃, pressure is risen to reactor pressure equate basically, vacuumizes drying;
(3) feed nitrogen in the hydrogen exchange catalyst filling jar, and catalyst is heated to 280～340 ℃, constant temperature 4～10h according to 10～15 ℃/h programming rate;
(4) after sulfuration finishes, the pressure of catalyst filling jar risen to be higher than reactor pressure 10～700kPa, temperature rises to temperature of reactor and equates;
(5) get through catalyst filling jar a catalyst and add pipeline, catalyst is joined in the reactor, realize the online filling of catalyst to reactor head.
According to method provided by the invention; It is characterized in that; Said method also comprises step (6): all catalyst are all discharged in catalyst filling jar, and continuation is closed catalyst filling pipeline with the hydrogen purge catalyst filling jar filling pipeline to reactor after affirmation pipeline purging is clean.
According to method provided by the invention, it is characterized in that said method also comprises step (7): catalyst filling jar is handled the subsequent use filling of catalyst next time.
Wherein the hydrogen described in the step (3) can be systemic circulation hydrogen, also can be to install like the new hydrogen of reforming, hydrogen manufacturing comes from other, preferably adopts systemic circulation hydrogen.Said hydrogen can also be that the gas of extension reactor gaseous phase outlet gets in the catalyst filling jar, because of it contains certain density hydrogen sulfide, and is gases at high pressure, helps to realize the sulfuration of catalyst.
Described boiling-bed catalyst can preferably use presulfurization type catalyst for oxidation catalyst or presulfurization type catalyst.Described presulfurization type catalyst is meant the catalyst of metal oxysulfide.
Boiling-bed catalyst described in the present invention can adopt conventional catalyst.The shape of boiling-bed catalyst can be shapes such as elliposoidal, sphere, clover, bunge bedstraw herb, four impeller shapes, Raschig ring.Boiling-bed catalyst consist of reactive metal Mo-Ni, bulk density is 0.5～0.9g/cm
3, particle diameter is 0.01～10mm, specific area is 80～300m
2/ g, average pore size 5-35nm.
In the present invention, in boiling bed hydrogenation unit normal run process, boiling-bed catalyst filling frequency is generally 0.1～5.0kg catalyst/t heavy oil feedstock.Can also in time pass through kind, kind ratio and the quantity that filling apparatus is adjusted the filling catalyst according to raw material in the operation process and product change.
Catalyst charging method of the present invention is applicable to the boiling bed hydrogenation processing procedure of reduced crude and decompression residuum, is particularly useful for the boiling bed hydrogenation processing procedure of the residual oil of high metal, high carbon residue, high condensed ring material and high nitrogen-containing.In the inventive method, described heavy oil feedstock can be the normal pressure and the decompression residuum of various crude oil, and various oil-sand, pitch, oli oil or synthetic crude etc., also can be the mixture of two or more above-mentioned raw materials.
Utilize the online charging method of catalyst of the present invention; Can carry out the online filling of catalyst to single reactor; Can also carry out the online filling of catalyst to the reactor of a plurality of series connection, can also adopt the method that the catalyst of follow-up online discharge is filled in the reactor of front.
In the method for the present invention, the once adding of required whole boiling-bed catalysts in the time of can realizing going into operation.Can realize that also the online filling of catalyst in the ebullated bed process unit normal operation process replenishes.
According to method provided by the invention; Wherein said boiling bed hydrogenation reactor refers to conventional fluidized bed reactor; Like the fluidized bed reactor of band gas, liquid, solid three phase separator in the reactor, wherein the gas phase of reaction back generation can be discharged from reactor respectively through same outlet or different outlet with liquid phase.The form of described fluidized bed reactor can be with reference to the record of patents such as CN 02109404.7, CN 200810012191.8, CN 200810228414.4, CN 200810228413.X or CN200810228412.5.
According to method provided by the invention, when adopting the fluidized bed reactor of built-in three phase separator, described boiling-bed catalyst filler is arranged on the baffling section in the separator region usually.Can utilize the advantage that flows downward of fluid here, make catalyst well get into the reactor body zone, can reduce from other position adding and bring the disturbance that air pocket causes flow regime into along flowing downward of fluid.According to the requirement of raw material and processing scheme and product property, it is distributor top in the reactor that described catalyst filler also can be arranged on the reactor middle and lower part.
In the catalyst filling process, the pressure of deduction pipeline (comprising static pressure) and valve falls, and the pressure reduction between catalyst filling jar and the reactor should remain on 10～700kPa.The Level Detection of boiling-bed catalyst filling jar should satisfy the detection requirement at solid material level interface.
The inventive method only needs existing online filling apparatus is done very little change; Can be before the online filling of catalyst; At first boiling-bed catalyst to be added is vulcanized; Then catalyst temperature is risen to the fluidized bed reactor isothermal, pressure is higher than reactor pressure 0.01～0.7MPa, the online filling of the catalyst of presulfurization realization catalyst under the conveying of the pressure reduction of catalyst filling jar and reactor, hydrogen and gravity effect.
Compared with prior art, the inventive method has following effect:
(1) owing to adopts the hydrogen of this device that catalyst is vulcanized; The hydrogen that uses can be systemic circulation hydrogen; Also can be to use hydrogen like the new hydrogen of reforming, hydrogen manufacturing came as sulfuration from other device; Therefore need not newly-built special vulcanization plant is used for the sulfuration of online filling catalyst, thereby has reduced investment.
(2) adopt recycle hydrogen to carry out boiling-bed catalyst sulfuration and filling etc., because wide material sources, convenient processing has been avoided employing residual oil or the heavy oil feedstock possibility in the pipeline coking.
(3) the inventive method before filling with catalyzer temperature-elevating to temperature of reactor, reduced in the prior art online filling to the disturbance of ebullating bed reactor temperature, reduced the device operation not steadily to the influence of product quality.
(4) if adopt pre-sulfide catalyst; Activation only need heat up before using; Needn't be equipped with in addition vulcanizing agent, and since in the hole of the outer presulfurization type catalyst of device the filling and vulcanization thing be difficult for the moisture absorption, also needn't carry out special drying steps before the use; Can directly at the uniform velocity heat up when going into operation until the introducing raw material that goes into operation, simplify operation greatly.
Description of drawings
Fig. 1 is a kind of schematic flow sheet of the online charging method of catalyst of the present invention.
Low cold low minute 9-Disengagement zone of the 7-washing 8-10-baffling section of dividing of the cold high score 6-heat of the 1-catalyst storage tank 2-catalyst filling jar hot high score 5-of 3-fluidized bed reactor 4-.
The specific embodiment
Below in conjunction with accompanying drawing the online charging method of catalyst of the present invention is further described.
At first get into fresh catalyst storage tank 1 after fresh catalyst measured 200L, extract air, use N again with the catalyst pumped vacuum systems
2Vacuum breaker is also protected.Open valve A, the fresh catalyst in the catalyst storage tank 1 joins catalyst filling jar 2 by gravity, feeds nitrogen replacement and is warmed up to 200 ℃～250 ℃ gradually, vacuumizes drying.Use from the gas of partial reaction device gaseous phase outlet or the portion of hot material of hot high score gaseous phase outlet and introduce in the catalyst filling jar 2, catalyst is heated to about 350 ℃, because of it contains finite concentration H
2S, and be gases at high pressure, can help inner catalyst to vulcanize.Open valve C, the gas that the gas vent at gas after the sulfuration and fluidized bed reactor top is discharged merges, and incorporates hot high score 4 into.The pressure of catalyst filling jars 2 risen to be higher than reactor pressure 0.05MPa, temperature rises to consistent with temperature of reactor, programming rate ≯ 15 of catalyst filling jar ℃/h, the rate of rise ≯ 1.5MPa/h.
Foundation is from catalyst filling jar 2 proper flow to reactor 3: open the adding valve B of catalyst filling jar 2 bottoms, the catalyst of getting through reactor head adds pipeline, and catalyst joins in the reactor.The all catalyst of radiological monitor demonstration in catalyst filling jar 2 are all discharged; Continue to be purged to the catalyst filling pipeline of reactor; Confirm that pipeline purges the catalyst adding valve B at off-response device top, clean back; Stop to introduce the gas in the catalyst filling jar 2, the catalyst adding finishes.
Regularly adopt this catalyst charging method, prolonged the operation cycle of boiling bed residual oil hydrogenation, system can even running, and product property is stable.
Heavy oil feedstock carries out boiling bed hydrogenation to be handled, and condition is conventional process operation condition, as temperature: 350-450 ℃, and pressure 11～30MPa, air speed 0.1～5.0h
-1, hydrogen to oil volume ratio 300: 1～1800: 1.Reacted product gets into separator.
Through specific embodiment the advantage of technical scheme of the present invention and scheme is done further to describe below.
Heavy oil feedstock carries out boiling bed hydrogenation to be handled, the process operation condition, and temperature: 385 ℃, pressure 15MPa, air speed 2.0h
-1, hydrogen to oil volume ratio 600: 1.The result sees table 1.
The online charging method of catalyst is with reference to Fig. 1 among the embodiment 1.Conditions of vulcanization wherein, the H 2 S-containing gas air speed is at 350 ℃ of constant temperature sulfuration 6h.Sulfuration finishes, and catalyst filling jar is warming up to 385 ℃, and pressure rises to 15.5MPa, gets through pipeline, carries out online filling.Catalyst filling frequency is 1.5kg catalyst/t heavy oil feedstock.
Catalyst adopts presulfurization type catalyst, and consisting of reactive metal is Mo-Ni, and wherein Mo is with MoO
3Meter content is 13.62%, and Ni is 2.83% with NiO content.Catalyst particle size is 0.2mm, and bulk density is 0.60gcm
-3, specific area is 260m
2/ g, average pore size 16nm.
The fluidized bed reactor operating condition is: temperature is 385 ℃, pressure 15MPa, air speed 2.0h
-1, hydrogen to oil volume ratio 600: 1.The result sees table 1.
Comparative example 1
Do not carry out presulfurization before the online filling of catalyst, be about to catalyst and directly be filled in the ebullated bed, its result sees table 1.
Table 1
| | Embodiment | 1 | Comparative example | |
| Density (20 ℃), kg.m -3 | 1001.8 | - | - | |
| Carbon residue, quality % | 17.3 | 11.7 | 15.7 | |
| Viscosity (100 ℃) mm 2.s -1 | 576.7 | |||
| S, quality % | 2.5 | 1.6 | 2.0 | |
| N, quality % | 0.4 | 0.25 | 0.37 | |
| Ni，μg.g -1 | 38.6 | 14.4 | 19.7 | |
| V，μg.g -1 | 187.4 | 117.7 | 127.1 | |
| Colloid, quality % | 24.5 | 13.0 | 19.8 | |
| Asphalitine, quality % | 13.4 | 8.1 | 10.5 | |
| 500℃ +Conversion ratio, % | 52 | 43 |
Can find out by table 1, adopt effect of the present invention obviously to be superior to the scheme that does not adopt we bright from impurity extrusion rate, conversion ratio etc.Feasibility of the present invention and effect have also been verified.
Claims (8)
1. online charging method of catalyst may further comprise the steps:
(1) fresh catalyst is added the catalyst storage tank, feed nitrogen protection;
(2) fresh catalyst in the catalyst storage tank joins catalyst filling jar under the gravity effect, and is warmed up to 200 ℃～250 ℃, pressure is risen to reactor pressure equate basically, vacuumizes drying;
(3) feed nitrogen in the hydrogen exchange catalyst filling jar, and catalyst is heated to 280～340 ℃, constant temperature 4～10h according to 10～15 ℃/h programming rate;
(4) after sulfuration finishes, the pressure of catalyst filling jar risen to be higher than reactor pressure 10～700kPa, temperature rises to temperature of reactor and equates;
(5) get through catalyst filling jar a catalyst and add pipeline, catalyst is joined in the reactor, realize the online filling of catalyst to reactor head.
2. according to the described method of claim 1, it is characterized in that said method also comprises step (6), all catalyst are all discharged in catalyst filling jar, continue with the hydrogen purge catalyst filling jar filling pipeline to reactor.
3. according to the described method of claim 1, it is characterized in that the hydrogen described in the step (3) is systemic circulation hydrogen or new hydrogen.
4. according to the described method of claim 3, it is characterized in that the hydrogen described in the step (3) is systemic circulation hydrogen.
5. according to the described method of claim 1, it is characterized in that described boiling-bed catalyst is oxidation catalyst or presulfurization type catalyst.
6. according to the described method of claim 5, it is characterized in that described boiling-bed catalyst is a presulfurization type catalyst.
7. according to the described method of claim 1, it is characterized in that the volume space velocity that feeds hydrogen is 300: 1～1800: 1.
8. according to the described method of claim 1, it is characterized in that the filling frequency of said boiling-bed catalyst is 0.1～5.0kg catalyst/t heavy oil feedstock.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108148620A (en) * | 2018-02-02 | 2018-06-12 | 上海英保能源化工科技有限公司 | Boiling bed hydrogenation consersion unit and boiling bed hydrogenation method |
| CN109999731A (en) * | 2019-04-26 | 2019-07-12 | 河南百优福生物能源有限公司 | The online charging method of the catalyst of biomass pyrolysis liquid fluidized bed reactor and device |
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| US4398852A (en) * | 1980-04-21 | 1983-08-16 | Hri, Inc. | Process and apparatus for adding and removing particles from pressurized reactors |
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| US6291391B1 (en) * | 1998-11-12 | 2001-09-18 | Ifp North America, Inc. | Method for presulfiding and preconditioning of residuum hydroconversion catalyst |
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| CN1702147A (en) * | 1999-12-16 | 2005-11-30 | 切夫里昂美国公司 | Presulfiding ocr catalyst replacement batches |
| CN101733114A (en) * | 2008-11-20 | 2010-06-16 | 中国石油化工股份有限公司 | Superfine powder composite metallic oxide catalyst and application thereof |
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2010
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| US3873441A (en) * | 1973-09-06 | 1975-03-25 | Universal Oil Prod Co | Catalyst transfer method for moving-bed reactors |
| US4398852A (en) * | 1980-04-21 | 1983-08-16 | Hri, Inc. | Process and apparatus for adding and removing particles from pressurized reactors |
| US4664782A (en) * | 1986-01-09 | 1987-05-12 | Intevep, S.A. | Method for withdrawing particulate solid from a high pressure vessel |
| CN1059164A (en) * | 1989-07-19 | 1992-03-04 | 切夫里昂研究和技术公司 | Change in the packed bed particulate method and apparatus in the operation with liquid gas feedstream counter current contact |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108148620A (en) * | 2018-02-02 | 2018-06-12 | 上海英保能源化工科技有限公司 | Boiling bed hydrogenation consersion unit and boiling bed hydrogenation method |
| CN108148620B (en) * | 2018-02-02 | 2023-08-15 | 上海竣铭化工工程设计有限公司 | Ebullated bed hydrogenation reaction equipment and ebullated bed hydrogenation method |
| CN109999731A (en) * | 2019-04-26 | 2019-07-12 | 河南百优福生物能源有限公司 | The online charging method of the catalyst of biomass pyrolysis liquid fluidized bed reactor and device |
| CN109999731B (en) * | 2019-04-26 | 2022-04-12 | 河南百优福生物能源有限公司 | Online catalyst filling method and device for biomass pyrolysis liquid fluidized bed reactor |
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Application publication date: 20120111 |