CN103721765A - Catalyst regeneration method capable of reducing carbon dioxide discharge - Google Patents

Catalyst regeneration method capable of reducing carbon dioxide discharge Download PDF

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Publication number
CN103721765A
CN103721765A CN201210385902.2A CN201210385902A CN103721765A CN 103721765 A CN103721765 A CN 103721765A CN 201210385902 A CN201210385902 A CN 201210385902A CN 103721765 A CN103721765 A CN 103721765A
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catalyst
regenerator
reactivator
flue gas
heavy
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CN103721765B (en
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许友好
王新
龚剑洪
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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 invention discloses a catalyst regeneration method capable of reducing carbon dioxide discharge. The catalyst regeneration method is characterized in that a catalyst with coke is subjected to pure oxygen-used partial regeneration in a first regenerator; the partially regenerated catalyst goes through an external circulating pipe, then enters into a second regenerator below the first regenerator and then is subjected to pure oxygen-used residual coke burning; the catalyst discharged from the first regenerator is fed into an external cooler, then is cooled and then is returned to the second regenerator; after cyclone separation, flue gas orderly enters into a flue gas energy recovery system and a carbon dioxide separation system and after carbon dioxide separation, a capturing process is carried out; and the regenerated catalyst is directly returned into a reactor for recycle. The catalyst regeneration method realizes complete regeneration of a catalyst and uniform distribution of catalyst activity so that coke as a catalytic cracking by-product and a dry gas yield are reduced. The catalyst regeneration method greatly reduces carbon emission and even realizes zero emission of carbon.

Description

A kind of catalyst recovery process that reduces CO2 emission
Technical field
The present invention relates to the renovation process containing Pd/carbon catalyst in a kind of hydrocarbon process.More particularly, the present invention relates to realize in mink cell focus catalytic cracking process the catalyst recovery process of carbon dioxide discharge-reduction.
Background technology
Now, whole world petroleum refining industry development faces the lot of challenges such as oil price fluctuation, the aggravation of crude oil in poor quality trend, oil quality specification improve, energy-saving and emission-reduction requirement becomes sternly, bio-fuel develops rapidly, and minimizing CO2 emission, mitigation of climate change have become petroleum refining industry transforms mode of economic growth, keeps the only way of sustainable development.In October, 2009, country has announced the action target of controlling greenhouse gas emission, arrives the year two thousand twenty nationwide units GDP CO 2discharge declined 40% to 45% than 2005, and clearly proposed per GDP carbon dioxide emission reduction 17% during " 12 ", and country likely imposes " carbon tax " during " 12 " in good time simultaneously.Therefore in petroleum refining and chemical process, effectively reduce carbon emission and seem and be even more important, trap, seal up for safekeeping and manage CO 2refinery's vital task in future will be become.Carbon emission in processing of heavy oil process is mainly the carbon emission of catalytic cracking burning, hydrogen production process and the energy consumption of technical process.Catalytic cracking unit is the core process units of refinery, because catalyst burns, becomes CO 2one of main source of discharge.
US2011/0155642A1 discloses a kind of catalytic cracking process process that reduces CO2 emission, adopt coke-burning riser series connection dense bed regenerating unit, pure oxygen and the regeneration techniques in coke-burning riser multiple spot delivery of supplemental oxygen, this technology Special attention will be given to has increased a tank in regeneration and circuit to be generated respectively, it is degassed that the tank of circuit of wherein regenerating adopts nitrogen to carry out regenerated catalyst, and the tank of circuit to be generated burns efficiency by temperature before introducing reclaimable catalyst and regenerated catalyst and mixing to improve reclaimable catalyst regeneration to improve.But the introducing of regeneration circuit nitrogen finally inevitably can make nitrogen play a reversed role in flue gas by regenerator, obviously lost the advantage of pure oxygen regeneration, only burn efficiency and increase, but the recovery of carbon dioxide has increased difficulty.
US4542114 discloses a kind of integral process process that reclaims the flue gas compositions such as carbon dioxide, can realize and in burning process, go back hydrogen manufacturing and carbon dioxide product, eliminate sulphur, the aerial discharge of nitrogen oxide completely, its pure oxygen mist that adopts carbon dioxide to dilute carries out catalyst and burns to produce rich carbonated flue gas simultaneously.But this technique does not increase interior heat collecting device for realizing in regenerator, emphasize wherein the preferred 30-24% of oxygen concentration 60-21% in mist, thereby part has lost the advantage that adopts purity oxygen regeneration, burns efficiency as increased substantially, and reduces regenerator size etc.
US5565089 discloses a kind of catalytic cracking catalyst process of regenerating, first with air, to enter regenerator to carry out catalyst and burn, then the carbon dioxide in reclaiming flue gas, recycled carbon dioxide and be incorporated to gradually oxygen-containing gas stream until in regenerator temperature normal, last direct oxygen injection and carbon dioxide carry out burning of catalyst.This process of regenerating is only paid close attention to the improvement of regenerative process gas handling system aspect and the processing of flue gas, does not consider the problem of the aspects such as regenerator structure or concrete regeneration technology process and catalytic cracking catalyst circulation.
CN1600431A discloses a kind of incomplete regen-eration smoke combustion technology, employing supplements the way of air in the incomplete regen-eration flue gas between catalyst regenerator and flue gas turbine inlet, CO in incomplete regen-eration flue gas is burnt away, thereby make flue-gas temperature be increased to 660-760 ℃, finally make flue gas turbine inlet temperature reach 640-700 ℃, improve cigarette machine organic efficiency, thereby reduce plant energy consumption with recovered flue gas pressure energy to greatest extent.Adopt the present invention, according to the concentration of unit scale and CO and/or entraining hydrocarbon, supplement air capacity 20-300Nm 3/ min, can effectively improve flue-gas temperature 20-80 ℃, improves cigarette engine efficiency.For single hop incomplete regen-eration, in flue, supplement air and also can make flue gas carry hydro carbons secretly fully to burn, eliminate its impact on cigarette machine, but can not effectively reduce CO2 emissions.
Because conventional catalyst coke burning regeneration method is to pass into air or oxygen-containing gas is regenerated in fluid bed, and air is mainly by O 2and N 2composition, contains a large amount of N in the regenerated flue gas therefore producing after catalyst coke burning regeneration 2, CO 2with a small amount of O 2and CO.And the flue gas of this composition is due to CO 2concentration is low, therefore CO 2separating difficulty is large, cost is high, cannot be isolated collection, can only enter directly discharge after energy-recuperation system, thereby cause greenhouse effects.
In addition,, from the development of regenerator, pursue the at utmost recovery that realizes regenerated catalyst activity, to realize the maximum conversion ability of hydro carbons always.But the activity of catalyst is the concept represent of a macroscopical conversion ratio, does not embody the pursuit of object product selectivity.While for example regenerating, can realize regenerated catalyst activation recovering the highest, but this regenerated catalyst may be because its high activity causes high coke and dry gas yied when participating in reaction, this does not wish to see.While therefore regenerating, need to pursue a kind of uniformity that catalyst activity recovers, realize in other words on regenerated catalyst acid one and be uniformly distributed, thereby realize low coke and dry gas yied, high object product selectivity.Therefore, be necessary to develop a kind of reduction CO2 emission and improve optionally catalyst recovery process.
Summary of the invention
The object of the invention is to provide on the basis of existing technology a kind of catalyst recovery process that reduces CO2 emission.
The catalyst recovery process of reduction CO2 emission provided by the invention adopts the regenerating unit pattern of two sections of adverse currents of coaxial-type, the first regenerator, Second reactivator are coaxially arranged, Second reactivator is positioned at the first regenerator below, the first regenerator, Second reactivator are turbulent bed operation, and the method comprises:
(1) from the band Pd/carbon catalyst of catalytic cracking unit stripping section, first in the first regenerator, adopt pure oxygen gas regeneration, coke combustion reaction occurs, the ratio of burning of the first regenerator is 55-70%;
(2) from the first regenerator bottom half regenerated catalyst out, through half regenerated catalyst pipe, enter Second reactivator, in Second reactivator bottom, further supplement pure oxygen gas, the catalyst of incomplete regen-eration is further burnt in dense-phase bed, holomorphosis, the ratio of burning of Second reactivator is 30-45%;
(3) Second reactivator arranges external warmer, and the catalyst of heat enters external warmer from the first regenerator, returns to Second reactivator after cooling, to control the temperature of Second reactivator dense-phase bed, is no more than 750 ℃ and is preferably no more than 720 ℃;
(4) from Second reactivator bottom replenishment cycles flue gas, the oxygen concentration of maintenance from regenerator cyclone separation system flue gas is out not less than 30% and is preferably not less than 40%, Second reactivator flue gas enters the first regenerator through its top macropore distribution grid, and the oxygen in flue gas continues on for burning;
(5) flue gas enters smoke energy recovering system after cyclone separator separates, and enters subsequently carbon dioxide separating system, after separating carbon dioxide, traps, and from the direct Returning reactor of regenerator regenerated catalyst out, recycles.
The operating condition of described the first regenerator is: temperature 550-720 ℃, and catalyst mean residence time is 1.0-5.0 minute preferred 1.0-4.0 minute, the gas superficial linear velocity of the first regenerator is that 0.6-1.0m/s is preferably 0.6-0.9m/s.In the first regenerator, interior heat collector can be set, also can not arrange, depend on whether the temperature of burning tank exceedes 750 ℃.
The operating condition of described Second reactivator is: temperature 580-700 ℃, and catalyst mean residence time is 1.0-4.0 minute preferred 1.0-3.0 minute, gas superficial linear velocity is that 0.6-1.0m/s is preferably 0.7-0.9m/s.The heat collector of Second reactivator setting is interior heat collector or/and external warmer, and heat collector is one or more.
Described catalyst comprises zeolite, inorganic oxide and optional clay, and each component accounts for respectively total catalyst weight and is: the heavy % of the heavy %-50 of zeolite 1, the heavy % of the heavy %-99 of inorganic oxide 5, the heavy % of the heavy %-70 of clay 0.Its mesolite is active component, be selected from mesopore zeolite and/or optional large pore zeolite, mesopore zeolite accounts for the heavy % of 10 heavy %-100 of zeolite gross weight, the preferably heavy % of 20 heavy %-80, large pore zeolite accounts for the heavy % of 0 heavy %-90 of zeolite gross weight, the preferably heavy % of 20 heavy %-80.Mesopore zeolite is selected from one or more mixtures and/or the ZRP zeolite in ZSM series zeolite, also can carry out modification to the transition metal such as the nonmetalloids such as phosphorus and/or iron, cobalt, nickel for above-mentioned mesopore zeolite.Large pore zeolite selects one or more the mixture in this group zeolite that super steady Y, high silicon Y that free Rare Earth Y (REY), rare earth hydrogen Y (REHY), distinct methods obtain form.
Inorganic oxide, as catalyst carrier, is selected from silica and/or alundum (Al2O3) or both mixtures.
Clay, as bonding agent, is selected from one or more in kaolin, imvite, diatomite, saponite, rectorite, sepiolite, hydrotalcite and bentonite.
Compared with existing renovation process, major advantage of the present invention is following two aspects:
1, the method not only can make catalyst holomorphosis, can significantly reduce carbon emission simultaneously, and even zero carbon emission reduces greenhouse effects.
2, the method can significantly reduce especially regenerator reserve of device catalyst inventory, greatly reduces the size of static equipment and moving equipment, reduces investment, reduces floor space.
3, because purity oxygen concentration in regenerative system is high, thereby make to burn efficiency, increase substantially, the recovery time shortens, and reduces fragmentation, the wearing and tearing of catalyst, has improved the service efficiency of catalyst.
Accompanying drawing explanation
Accompanying drawing is the catalyst recovery process schematic flow sheet of reduction CO2 emission provided by the invention.
The specific embodiment
Below in conjunction with accompanying drawing, further illustrate method provided by the present invention, but the present invention is not therefore subject to any restriction.
Accompanying drawing is the catalyst recovery process schematic flow sheet of reduction CO2 emission provided by the invention.
In accompanying drawing, each numbering is described as follows:
1,10,11,12,13,18,20,21,23 all represent pipeline; 2 is Second reactivator; 3 is macropore distribution grid; 4 is the dense-phase bed of the first regenerator; 6 is the first regenerator; 7 and 17 are cyclone separation system; 8 is smoke energy recovering system; 9 is carbon dioxide separating system; 14 is riser reactor; 15 is stripping section; 16 is settler; 19 is oil and gas separating system; 22 is external warmer.
As shown in drawings, reclaimable catalyst enters the dense-phase bed 4 of the first regenerator 6 through inclined tube 1 to be generated, and pure oxygen gas enters the bottom of the first regenerator 6 dense-phase bed 4 through pipeline 21, contact the combustion reaction of concurrent green coke charcoal with reclaimable catalyst.Incomplete regen-eration catalyst enters Second reactivator 2 through half regenerated catalyst pipe 23, and pure oxygen gas enters Second reactivator 2 bottoms through pipeline 20, the remaining coke of burning-off.Second reactivator flue gas enters through the macropore distribution grid 3 at top that the first regenerator is auxiliary to be burnt.The catalyst of heat is drawn from the first regenerator dense-phase bed 4, returns to Second reactivator 2 after external warmer 22 is cooling.The flue gas of the first regenerator leaves the first regenerator through cyclone separation system 7.From the first regenerator flue gas part out, directly entering smoke energy recovering system 8 recovers energy, another part returns to the bottom of Second reactivator 2 through pipeline 10 circulations, can realize the lifting of the carbon dioxide in flue gas concentration that enters carbon dioxide separating system 9.From energy-recuperation system 8 flue gas out, enter carbon dioxide separating system 9, realize the trapping of carbon dioxide.From Second reactivator 2 regenerated catalyst out, through regenerator sloped tube 11, enter riser reactor 14 bottoms, it is up that pre-lift medium enters riser reactor bottom lifting regenerated catalyst through pipeline 12, feedstock oil enters riser reactor through pipeline 13 and contacts with regenerated catalyst and carry out catalytic cracking reaction, and reaction oil gas enters oil and gas separating system 19 through settler 16, cyclone separation system 17 and oil-gas pipeline 18 successively and obtains various products.Reclaimable catalyst enters inclined tube 1 to be generated and turns back to the first regenerator 6 and regenerate after stripping section 15 strippings, thereby realize, recycles.
The following examples will be further described the present invention, but not thereby limiting the invention.The feedstock oil using in embodiment and comparative example is decompression residuum, and its character is listed in table 1.Catalyst is produced by catalyst branch company of Sinopec Group Shandong catalyst plant, and goods number is MLC-500, and its character is listed in table 2.
Embodiment
Embodiment carries out on catalytic cracking demonstration plant, as shown in drawings.Demonstration plant does not have smoke energy recovering system and carbon dioxide separating system.Wherein 60 centimetres of the internal diameters of the first regenerator dense-phase bed, the internal diameter of Second reactivator dense-phase bed is 30 centimetres.According to renovation process proposed by the invention, catalyst is regenerated, at the first regenerator and Second reactivator dense-phase bed, pass into respectively pure oxygen gas, from the first regenerator cyclone separation system flue gas partial out, return to Second reactivator dense-phase bed bottom simultaneously.The bed temperature of the first regenerator is 680 ℃, and Second reactivator dense-phase bed temperature is 670 ℃.Catalyst is 3 minutes in the time of staying of the first regenerator dense-phase bed, at the mean residence time of Second reactivator dense-phase bed, is 2 minutes.The gas superficial linear velocity of the first regenerator is 0.7m/s, and Second reactivator gas superficial linear velocity is 0.8m/s.Catalyst after regeneration enters reactor, and the feedstock oil listed with table 1 contacts, and carries out catalytic cracking reaction, and regeneration condition, reaction condition, regenerated catalyst carbon content and flue gas composition are all listed in table 3.
Comparative example
Comparative example is also to carry out on the catalytic cracking demonstration plant of same structure, but the internal diameter of the first regenerator and Second reactivator dense-phase bed is different with embodiment, 180 centimetres of the internal diameters of the first regenerator dense-phase bed, the internal diameter of Second reactivator dense-phase bed is 120 centimetres, and other physical dimension is identical with embodiment.Pair reclaimable catalyst identical with embodiment of renovation process routinely regenerated, and the first regenerator and Second reactivator dense-phase bed pass into respectively air, and the bed temperature of the first regenerator is 690 ℃, and Second reactivator dense-phase bed temperature is 700 ℃.Catalyst is 10 minutes in the time of staying of the first regenerator dense-phase bed, at the mean residence time of Second reactivator dense-phase bed, is 8 minutes.The gas superficial linear velocity of the first regenerator is 0.7m/s, and Second reactivator gas superficial linear velocity is 0.8m/s.Catalyst after regeneration enters reactor, and the feedstock oil listed with table 1 contacts, and carries out catalytic cracking reaction, and regeneration condition, reaction condition, regenerated catalyst carbon content and flue gas composition are all listed in table 3.
From the result contrast of operating condition and table 3, can find out, compared with comparative example, the present invention significantly reduces, installs general reserve in burning tank size and regeneration dense bed size and significantly reduces, consumes under the obvious prerequisite reducing of wind index, adopt renovation process proposed by the invention, on regenerated catalyst, carbon content reduces more, in addition in the flue gas that, this catalyst recovery process produces, do not contain CO and N 2, gas concentration lwevel, up to 59.52%, is conducive to separation and the trapping of carbon dioxide.
Table 1
Feedstock oil title Decompression residuum
Density (20 ℃), kg/m 3 920.9
Kinematic viscosity, millimeter 2/ second
100℃ 114.4
Carbon residue, heavy % 8.2
Condensation point, ℃ 25
Total nitrogen, heavy % 0.33
Sulphur, heavy % 0.21
Carbon, heavy % 86.91
Hydrogen, heavy % 12.55
Tenor, ppm
Nickel 8.8
Vanadium 0.1
Iron 1.8
Copper <0.1
Sodium 3.0
Boiling range, ℃
HK (initial boiling point) 415
10% 545
30% /
50% /
70% /
KK (end point of distillation) /
Table 2
Catalyst goods number MLC-500
Chemical composition, heavy %
Aluminium oxide 50.2
Sodium oxide molybdena 0.321
Apparent density, kg/m 3 700
Pore volume, mL/g 0.38
Specific area, m 2/g 229
Abrasion index, during heavy % -1 1.9
Size consist, heavy %
0~40 micron 17.3
40~80 microns 49.3
80 microns of > 33.4
Table 3
Embodiment Comparative example
Device catalyst general reserve, ton 1.2 6
Cracking hydrocarbon reaction member
Outlet temperature of riser, ℃ 500 500
Catalyst/feed weight ratio 6 6
Reaction time, second 3 3
Water vapour/raw material weight ratio 0.05 0.05
Regeneration unit
The first regenerator dense bed internal diameter, cm 60 180
Second reactivator dense bed internal diameter, cm 30 120
Consumption wind index, Nm 3/kg 3.6 16.5
Carbon content on regenerated catalyst, heavy % 0.01 0.06
Regenerated flue gas composition, %
N 2 0 78.4
CO 2 59.14 11.34
CO 0 8.39
O 2 40.86 1.87

Claims (9)

1. one kind is reduced the catalyst recovery process of CO2 emission, it is characterized in that the method adopts the regenerating unit pattern of two sections of adverse currents of coaxial-type, the first regenerator, Second reactivator are coaxially arranged, Second reactivator is positioned at the first regenerator below, the first regenerator, Second reactivator are turbulent bed operation, and the method comprises:
(1) from the band Pd/carbon catalyst of catalytic cracking unit stripping section, first in the first regenerator, adopt pure oxygen gas regeneration, coke combustion reaction occurs, the ratio of burning of the first regenerator is 55-70%;
(2) from the first regenerator bottom half regenerated catalyst out, through half regenerated catalyst pipe, enter Second reactivator, in Second reactivator bottom, further supplement pure oxygen gas, the catalyst of incomplete regen-eration is further burnt in dense-phase bed, holomorphosis, the ratio of burning of Second reactivator is 30-45%;
(3) Second reactivator arranges heat collector, and the catalyst of heat enters heat collector from the first regenerator, returns to Second reactivator after cooling, to control the temperature of Second reactivator dense-phase bed, is no more than 750 ℃;
(4) from Second reactivator bottom replenishment cycles flue gas, the oxygen concentration of maintenance from regenerator cyclone separation system flue gas is out not less than 30%, Second reactivator flue gas enters the first regenerator through its top macropore distribution grid, and the oxygen in flue gas continues on for burning;
(5) flue gas enters smoke energy recovering system after cyclone separator separates, and enters subsequently carbon dioxide separating system, after separating carbon dioxide, traps, and from the direct Returning reactor of regenerator regenerated catalyst out, recycles.
2. according to the method for claim 1, it is characterized in that the operating condition of described the first regenerator is: temperature 550-720 ℃, catalyst mean residence time is 1.0-5.0 minute, gas superficial linear velocity is 0.6-1.0m/s.
3. according to the method for claim 2, it is characterized in that the operating condition of described the first regenerator is: catalyst mean residence time is 1.0-4.0 minute, gas superficial linear velocity is 0.6-0.9m/s.
4. according to the method for claim 1, it is characterized in that the operating condition of described Second reactivator is: temperature 580-700 ℃, catalyst mean residence time is 1.0-4.0 minute, gas superficial linear velocity is 0.6-1.0m/s.
5. according to the method for claim 4, it is characterized in that the operating condition of described Second reactivator is: catalyst mean residence time is 1.0-3.0 minute, gas superficial linear velocity is 0.7-0.9m/s.
6. according to the method for claim 1, it is characterized in that the described heat collector of step (3) is interior heat collector or/and external warmer, heat collector is one or more.
7. according to the method for claim 1, it is characterized in that the temperature of step (3) control dense-phase bed is no more than 720 ℃.
8. according to the method for claim 1, it is characterized in that the oxygen concentration in the described flue gas of step (4) is not less than 40%.
9. according to the method for claim 1, it is characterized in that described catalyst comprises zeolite, inorganic oxide and optional clay, each component accounts for respectively total catalyst weight and is: the heavy % of the heavy %-50 of zeolite 1, the heavy % of the heavy %-99 of inorganic oxide 5, the heavy % of the heavy %-70 of clay 0.
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CN105457570A (en) * 2014-09-09 2016-04-06 中国石油化工股份有限公司 Coaxial two-stage regenerative reaction device for preparing low-carbon olefins and aromatic hydrocarbon by converting methanol or dimethyl ether and reaction method for coaxial two-stage regenerative reaction device

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