CN103059967B - Mixed hydrogenation method for catalytic cracking gasoline and coking diesel oil - Google Patents
Mixed hydrogenation method for catalytic cracking gasoline and coking diesel oil Download PDFInfo
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Abstract
The invention discloses a mixed hydrogenation method for catalytic cracking gasoline and coking diesel oil. The method comprises: subjecting FCC (fluid catalytic cracking) gasoline to alkali-free deodorization, making the deodorized catalytic gasoline enter a prefractionator to be fractionated into light gasoline and heavy gasoline; mixing the heavy gasoline with coking diesel oil, then performing hydrodesulfurization, separating the desulfurization product to obtain hydrogenated heavy gasoline and treated coking diesel oil, and blending the hydrogenated heavy gasoline with the light gasoline to obtain a clean gasoline product. According to the method provided in the invention, when the coking diesel oil and the heavy gasoline are mixed for hydrogenation, the nitride brought in by the coking diesel oil undergoes competitive adsorption at a catalyst hydrogenation center and causes poisoning of the hydrogenation center, thus reducing olefin hydrogenation selectivity and decreasing the octane number loss of hydrogenation. On the other hand, when the mixed feed flows through a heat exchanger and heating furnace, the raw materials are in a gas-liquid mixed phase in the heating furnace and the heat exchanger, so that a coke material can be dissolved and taken away, coking can be avoided in the heat exchanger and the heating furnace, and the operation cycle of the equipment can be prolonged.
Description
Technical field
The present invention relates to a kind of mixed hydrogenation method of catalytically cracked gasoline and coker gas oil, specifically a kind of combined method improving catalyzed gasoline hydrogenation desulfurization selectivity and extend hydrodesulfurization unit and downstream coker gas oil hydrogenation unit operation period.
Background technology
Along with the development of automotive industry and the increase of automobile pollution, the nuisance of motor vehicle exhaust to the pollution of air day by day by people are paid attention to, various countries to motor spirit specification requirement as the index such as olefin(e) centent, sulphur content improves day by day.Reduce finished product motor spirit sulphur and olefin(e) centent, effectively can reduce the quantity discharged of nuisance in vehicle exhaust.Therefore, country has not only formulated " automobile exhaust emission standard " of increasingly stringent, and has higher requirement to nuisance in motor spirit and correlated quality Con trolling index.In China's gasoline product, the proportion that catalytic cracking (FCC) gasoline accounts for is very large, accounts for greatly 70 ~ 80% of gasoline product, therefore, in this context FCC gasoline clean the key becoming and solve gasoline cleaning problem.
At present, clean in technology in FCC gasoline, selective hydrodesulfurization technology be main, be also the most effective technique means.For the feature of China's catalytic cracking (FCC) gasoline, in recent years, Fushun Petrochemical Research Institute (FRIPP) is devoted to the exploitation of FCC gasoline catalyst for selectively hydrodesulfurizing and Technology always, the OCT-MD FCC gasoline selective hydrogenation desulfurization process of FRIPP exploitation, adopt the FGH-21/FGH-31 combination catalyst of special exploitation and supporting hydrogenation technique, product gasoline sulphur content can reach 50mg/g, and RON loss of octane number is less than 1.5 units.Stablize in OCT-MD technique that FCC gasoline fractionates out gently through the laggard separation column of alkali-free sweetening, heavy constituent, heavy constituent enters after hydrogenator carries out hydrogenation and is mixed to get low sulfur clean gasoline with light constituent after heat exchange and process furnace heating.But, owing to containing more alkene, diolefine in catalytically cracked gasoline, therefore, heavy constituent easy coking when interchanger and process furnace heating, and at reaction conditions, heavy constituent is generally gaseous state, the coking material particle generated is difficult to be pulled away, thus be trapped in interchanger or process furnace, interchanger or process furnace internal drop is caused to increase, and once reaction conditions shakiness causes process furnace and interchanger charging to be liquid phase, the coking materials such as the coke powder of accumulation can enter reactor in the short period of time causes reactor pressure decrease to increase fast, device is caused to be forced to stop work.In addition, along with the increasingly stringent of environmental regulation, desulfurization depth is deepened gradually, has higher requirement to selectivity of catalyst, therefore, has higher requirement to catalytic gasoline selective hydrodesulfurization device selectivity and operation period.
Summary of the invention
For RSDS interchanger and furnace coking problem and selective desulfurization problem, the invention provides a kind of catalytic cracking (FCC) gasoline and coker gas oil mixed hydrogenation method.
Catalytically cracked gasoline of the present invention-coker gas oil mixed hydrogenation method comprises following content:
(1) FCC gasoline enters alkali-free sweetening unit, carries out mercaptan removal process;
(2) FCC gasoline after alkali-free sweetening enters hydrogenation preliminary fractionator, and fractionation is petroleum naphtha and heavy petrol; The cutting temperature of petroleum naphtha and heavy petrol is 40 DEG C ~ 80 DEG C;
(3) step (2) gained heavy petrol mixes with hydrogen after mixing with coker gas oil, enters hydrofining reactor, contacts with Hydrobon catalyst, carry out hydrodesulfurization reaction;
(4) hydrogenation reaction effluent that step (3) obtains enters gas-liquid separator and carries out gas-liquid separation;
(5) liquid phase that step (4) obtains obtains hydrogenated heavy gasoline and pretreated coker gas oil after fractionation, hydrogenated heavy gasoline goes out device as clean gasoline product after mixing with step (2) gained petroleum naphtha, and step (4) gained gas phase recycle hydrogen loops back hydrogenator.
According to catalytically cracked gasoline of the present invention and coker gas oil mixed hydrogenation method, wherein the alkali-free sweetening described in step (1) is the routine operation of this area.Alkali-free sweetening condition is generally: reaction pressure 0.1 ~ 1.0MPa, temperature of reaction 20 DEG C ~ 70 DEG C, Feed space velocities 0.5 ~ 2.0h
-1, air flow quantity/inlet amount volume ratio is 0.1 ~ 1.0.The final boiling point of FCC stable gasoline is generally lower than 205 DEG C.
In step (2), the cutting temperature of petroleum naphtha and heavy petrol is generally 40 DEG C ~ 80 DEG C, is preferably 50 DEG C ~ 70 DEG C.The concrete cutting temperature of petroleum naphtha and heavy petrol should judge depending on the result of alkali-free sweetening.
In step (3), described FCC heavy petrol and coker gas oil form parallel feeding nitrogen content general control be 300 μ g/g ~ 1000 μ g/g.The initial boiling point of wherein said coker gas oil controls to be not less than 205 DEG C, and be preferably 210 DEG C ~ 230 DEG C, final boiling point is 360 DEG C ~ 380 DEG C, and nitrogen content is generally 800 μ g/g ~ 2500 μ g/g.
FCC heavy petrol mixes with coker gas oil and after mixing with hydrogen, first can enter process furnace again after interchanger and hydrogenation reaction effluent heat exchange and heat, the mixing raw material after heating enters hydrofining reactor and reacts in step (3).
In method of hydrotreating of the present invention, in step (3), the operational condition of hydrofining reactor is as follows: temperature of reaction 200 DEG C ~ 320 DEG C, preferably 220 DEG C ~ 300 DEG C; Reaction pressure 1.0 MPa ~ 3.0 MPa, preferably 1.2 MPa ~ 2.5 MPa; Volume space velocity 1.0h during liquid
-1~ 8.0h
-1, preferred 2h
-1~ 6.0h
-1; Hydrogen to oil volume ratio 100: 1 ~ 1000: 1, preferably 200: 1 ~ 500: 1.
In the inventive method, described Hydrobon catalyst can be conventional hydrodesulfurization catalyzer.Preferably there is the catalyst for selectively hydrodesulfurizing of following character: catalyzer take aluminum oxide as carrier, with Mo and Co for active metal component; Catalyzer is containing MoO by weight
33.0 ~ 18.0 w%, preferably 4.0 ~ 16.0 w%, CoO 1.0 ~ 6.0 w%, preferably 2.0 ~ 5.0 w%, Co/Mo atomic ratio 0.1 ~ 1.0; Catalyzer pore volume is 0.3 ~ 1.3mL/g, and specific surface area is 150 ~ 300m
2/ g.Can also potassium and phosphorus be contained in described catalyzer, as containing potassium 0.2 ~ 10.2w%, preferably 0.5 ~ 5.0 w%, P/K atomic ratio 0.1 ~ 10.0, preferably 0.8 ~ 5.0.Compare conventional gasoline hydrogenation catalyst, this catalyzer has higher desulfuration selectivity, and olefin saturated activity is relatively weak, and after hydrogenation, gasoline octane rating loss is less.
Described Hydrobon catalyst can select commercial goods catalyzer, also can be prepared according to the Conventional wisdom of this area.Commercial goods catalyzer can be selected from FGH-21 and the FGH-31 selective hydrogenation catalyst of FRIPP development.Described hydrofining reactor comprises at least two beds, and different bed can grading loading Hydrobon catalyst, has cold hydrogen to inject and arrange between bed.
Wherein in step (4), the hydrogen-rich gas that gas-liquid separator obtains removes after the liquid phase of carrying secretly through cyclone separator and enters desulphurization of recycle hydrogen tower.Desulphurization of recycle hydrogen adopts amine liquid solvent adsorption method, described amine liquid is organic bases, more with alcamines, conventional hydramine is selected from one or more in Monoethanolamine MEA BASF (MEA), diethanolamine (DEA), diisopropanolamine (DIPA) (DIPA) or N methyldiethanol amine (MDEA).In desulphurization of recycle hydrogen tower, inject poor amine liquid from thionizer top, at the bottom of tower, extract rich amine solution carrying device recycling utilization out; Remove the new hydrogen external with device after compressor boosting of the recycle hydrogen after hydrogen sulfide to mix, as mixed hydrogen for device.Hydrogen sulfide content in described desulphurization of recycle hydrogen Posterior circle hydrogen is 0 ~ 300 μ L/L, preferably 0 ~ 50 μ L/L.
Compared with prior art, FCC gasoline of the present invention and coker gas oil mixed hydrogenation method have following characteristics:
1, contain more alkene, diolefine in FCC stable gasoline, in storage process and in alkali-free sweetening process, contact the coke precursor easily producing colloid with oxygen.In conventional FCC gasoline hydrogenation technique, when these coke precursor are through interchanger especially process furnace, at high temperature be easy to coking, gasoline component is being gasified totally through interchanger and process furnace simultaneously, the coking material generated is deposited in interchanger and process furnace, thus the pressure drop that induces reaction increases, device is finally caused to be forced to stop work.In the inventive method, coker gas oil and the parallel feeding of FCC heavy petrol is adopted to enter interchanger and process furnace, make raw material in process furnace and interchanger, be in gas, liquid mixed phase, can dissolve and take away coke precursor, avoid in interchanger and process furnace and coking occurs, extend the operation period of device.
2, on the other hand, nitride especially basic nitrogen compound is the poisonous substance at catalyst hydrogenation center, has very strong absorption and restraining effect to the hydrogenation center of catalyzer.And containing higher nitrogen content and basic nitrogen in coker gas oil.Therefore, when the mixing raw material of FCC gasoline and coker gas oil is by hydrogenator beds, in parallel feeding, the nitride of high-content can play the effect of poisoned catalyst hydrogenation sites, thus suppress the hydrogenation activity of catalyzer, reduce the hydrotreated lube base oil rate of alkene, reduce the loss of octane number of FCC gasoline hydrogenated products.Because the sulfocompound structure contained in catalytic gasoline is comparatively simple, directly can be removed by hydrogenolysis in the heart in hydrogenolysis, therefore the poisoning sweetening effectiveness that can not affect gasoline of the nitride at catalyst hydrogenation center.In addition, unifining process serves the effect of diolefine and colloid in pre-hydrogenation and removing coker gas oil to coker gas oil, thus is also conducive to the long-term operation of downstream coker gas oil hydrogenation unit.
Accompanying drawing explanation
Fig. 1 is the principle process schematic diagram of FCC gasoline of the present invention and coker gas oil mixed hydrogenation method.
Embodiment
Below by specific embodiment, catalytic gasoline of the present invention and coker gas oil mixed hydrogenation method are described in detail.
As shown in Figure 1, FCC gasoline enters alkali-free sweetening unit 2 by pipeline 1 and carries out mercaptan removal process, and the gasoline after deodorization enters hydrogenation preliminary fractionator 3 and fractionates out petroleum naphtha and heavy petrol.Heavy petrol is through pipeline 4, after mixing with the coker gas oil introduced through pipeline 5, after the hydrogen introduced with pipeline 6 again mixes, first after interchanger 7 and hydrogenation reaction effluent carry out heat exchange, enter hydrofining reactor 9 after entering process furnace 8 heating and carry out selective hydrodesulfurization reaction, reaction effluent enters gas-liquid separator 10 and carries out gas-liquid separation after interchanger 7 is lowered the temperature, gas phase can go recycle hydrogen amine to wash tower through pipeline 11 to carry out depriving hydrogen sulphide process, gained liquid phase enters separation column 13 through pipeline 12 and fractionates out coker gas oil after refining heavy petrol and pre-treatment, pretreated coker gas oil flows out to downstream diesel hydrotreating unit through pipeline 14, refining heavy petrol goes out device through pipeline 16, and be in harmonious proportion with the petroleum naphtha after the deodorization of pipeline 17, obtain clean gasoline product.
Below by specific embodiment and comparative example, further illustrate technical scheme of the present invention and effect.
Embodiment 1 ~ 3
Embodiment 1 ~ 3 adopts the technical process shown in Fig. 1.
The AFS-12 prefabrication type catalyzer that the catalyzer that FCC gasoline alkali-free sweetening uses is researched and developed for China University Of Petroleum Beijing.Alkali-free sweetening adopts identical processing condition: reaction pressure 0.6MPa, temperature of reaction 40 DEG C, Feed space velocities 0.9h
-1, air flow quantity/inlet amount volume ratio is 0.7.
After alkali-free sweetening, FCC gasoline carries out fractionation in hydrogenation preliminary fractionator, and the cutting temperature of petroleum naphtha and heavy petrol is 50 DEG C.Heavy petrol enters hydrofining reactor after mixing with coker gas oil, hydrogen and reacts.Hydrotreated product, through to be separated and after fractionation, to obtain refining heavy petrol and petroleum naphtha and is in harmonious proportion and obtains gasoline products.
The FGH-21/FGH-31 combination catalyst that Hydrobon catalyst selects Fushun Petrochemical Research Institute to develop, by 1: 2 grading loading.Stock oil character used is in table 1, and the hydrodesulfurization condition of embodiment 1 ~ 3 lists in table 2, and the character of gained blended gasoline lists in table 3.
Table 1 stock oil character
| Project | FCC gasoline | Coker gas oil 1 | Coker gas oil 2 | Coker gas oil 3 |
| Density (20 DEG C)/gcm -3 | 0.7317 | 0.8632 | 0.8678 | 0.8680 |
| Boiling range (ASTM D 86), DEG C | ? | ? | ? | ? |
| Initial boiling point/ | 34 | 205 | 210 | 214 |
| 10% | 56 | 264 | 271 | 273 |
| 50% | 98 | 291 | 299 | 300 |
| 90% | 171 | 346 | 354 | 355 |
| Final boiling point | 192 | 362 | 365 | 365 |
| Sulphur, μ g/g | 700 | 5600 | 6250 | 7100 |
| Nitrogen, μ g/g | 45 | 1200 | 1800 | 2000 |
| RON | 94.5 | — | — | — |
Table 2 embodiment 1 ~ 3 hydrodesulfurization condition
| ? | Embodiment 1 | Embodiment 2 | Embodiment 3 |
| Stock oil | FCC heavy petrol/coker gas oil 1=2 | FCC heavy petrol/coker gas oil 2=3 | FCC heavy petrol/coker gas oil 3=4 |
| Feed nitrogen content, μ g/g | 425 | 473 | 436 |
| Temperature of reaction, DEG C | 260 | 280 | 300 |
| Reaction pressure, MPa | 1.6 | 1.6 | 1.6 |
| Volume space velocity, h -1 | 3.0 | 3.0 | 2.5 |
| Hydrogen to oil volume ratio | 300 | 300 | 300 |
Table 3 embodiment 1 ~ 3 gained blended gasoline product property
| ? | Embodiment 1 | Embodiment 2 | Embodiment 3 |
| Density (20 DEG C)/gcm -3 | 0.7314 | 0.7312 | 0.7268 |
| Boiling range (ASTM D 86), DEG C | ? | ? | ? |
| Initial boiling point | 35 | 35 | 35 |
| 10% | 55 | 56 | 54 |
| 50% | 98 | 97 | 98 |
| 90% | 170 | 169 | 170 |
| Final boiling point | 191 | 190 | 189 |
| Sulphur, μ g/g | 132 | 27 | 8 |
| RON | 94.1 | 93.8 | 92.8 |
| RON loses | 0.4 | 0.7 | 1.7 |
| The steady running cycle, h | 8000 | 8000 | 8000 |
Known by embodiment 1 ~ 3, during the gasoline products using FCC gasoline raw material in embodiment to produce respectively to meet Europe III, Europe IV, Europe V clean gasoline sulphur content to require, its loss of octane number is respectively 0.4,0.7 and 1.7 unit.Meanwhile, device steady running 1 year reactor pressure decrease is without considerable change, and device can long period steady running.
Comparative example 1 ~ 3
Comparative example 1 ~ 3 is substantially identical with Fig. 1 flow process.FCC gasoline alkali-free sweetening part, petroleum naphtha is corresponding with embodiment 1 ~ 3 with the fractionating section of heavy petrol.In FCC heavy petrol hydrogenating desulfurization part, only have FCC heavy petrol to carry out selective hydrodesulfurization, do not introduce coker gas oil, the volume space velocity of heavy petrol is corresponding.
Used catalyst selects FGH-21/FGH-31 by the combination catalyst of 1: 2 grating.Operational condition is corresponding with embodiment 1 ~ 3 respectively.Test-results lists in table 4.
Table 4 comparative example 1 ~ 3 gained FCC gasoline product property
| ? | Comparative example 1 | Comparative example 2 | Comparative example 3 |
| Density (20 DEG C)/gcm -3 | 0.7314 | 0.7312 | 0.7268 |
| Boiling range (ASTM D 86), DEG C | ? | ? | ? |
| Initial boiling point | 35 | 35 | 35 |
| 10% | 55 | 56 | 54 |
| 50% | 98 | 97 | 98 |
| 90% | 170 | 169 | 170 |
| Final boiling point | 191 | 190 | 189 |
| Sulphur, μ g/g | 108 | 24 | 7 |
| RON | 93.4 | 92.8 | 92.0 |
| RON loses | 1.1 | 1.7 | 2.5 |
Can find from comparative example 1 ~ 3 test-results, under the reaction conditions identical with embodiment 1 ~ 3, desulfurization degree is suitable with embodiment 1 ~ 3, but loss of octane number is apparently higher than embodiment 1 ~ 3.And plant running after two months, reactor pressure decrease rises to more than 300kPa by initial 60kPa, is forced to stop work.
Claims (11)
1. catalytically cracked gasoline and a coker gas oil mixed hydrogenation method, comprises the following steps:
(1) FCC gasoline enters alkali-free sweetening unit, carries out mercaptan removal process;
(2) FCC gasoline after alkali-free sweetening enters hydrogenation preliminary fractionator, and fractionation is petroleum naphtha and heavy petrol; The cutting temperature of petroleum naphtha and heavy petrol is 40 DEG C ~ 80 DEG C;
(3) step (2) gained heavy petrol mixes with hydrogen after mixing with coker gas oil, enters hydrofining reactor, contacts with Hydrobon catalyst, carry out hydrodesulfurization reaction;
(4) hydrogenation reaction effluent that step (3) obtains enters gas-liquid separator and carries out gas-liquid separation;
(5) liquid phase that step (4) obtains obtains hydrogenated heavy gasoline and pretreated coker gas oil after fractionation, and hydrogenated heavy gasoline goes out device as clean gasoline product after mixing with step (2) gained petroleum naphtha.
2. in accordance with the method for claim 1, it is characterized in that, the nitrogen content of the parallel feeding of heavy petrol and coker gas oil described in step (3) is 300 μ g/g ~ 1000 μ g/g.
3. in accordance with the method for claim 1, it is characterized in that, wherein in step (2), the cutting temperature of petroleum naphtha and heavy petrol is 50 DEG C ~ 70 DEG C.
4. according to method of hydrotreating according to claim 1, it is characterized in that, described in step (3), the initial boiling point of coker gas oil is not less than 205 DEG C, and final boiling point is 360 DEG C ~ 380 DEG C, and the final boiling point of described catalytically cracked gasoline is lower than 205 DEG C.
5. according to the method for hydrotreating described in claim 1 or 4, it is characterized in that, the initial boiling point of coker gas oil described in step (3) is 210 DEG C ~ 230 DEG C.
6. according to method of hydrotreating according to claim 1, it is characterized in that, the nitrogen content of coker gas oil described in step (3) is 800 μ g/g ~ 2500 μ g/g.
7. according to method of hydrotreating according to claim 1, it is characterized in that, described in step (3), the condition of hydrodesulfurization reaction is: temperature of reaction 200 DEG C ~ 320 DEG C, reaction pressure 1.0 MPa ~ 3.0 MPa, volume space velocity 1.0h during liquid
-1~ 8.0h
-1, hydrogen to oil volume ratio 100: 1 ~ 1000: 1.
8. according to method of hydrotreating according to claim 1, it is characterized in that, described in step (3), the condition of hydrodesulfurization reaction is: temperature of reaction 220 DEG C ~ 300 DEG C, reaction pressure 1.2MPa ~ 2.5 MPa, volume space velocity 2h
-1~ 6.0h
-1, hydrogen to oil volume ratio 200: 1 ~ 500: 1.
9. according to method of hydrotreating according to claim 1, it is characterized in that, described Hydrobon catalyst take aluminum oxide as carrier, with Mo and Co for active metal component; Catalyzer contains molybdenum with MoO by weight
3count 3.0 ~ 18.0 w%, count 1.0 ~ 6.0 w% containing cobalt with CoO, Co/Mo atomic ratio 0.1 ~ 1.0.
10. according to method of hydrotreating according to claim 1, it is characterized in that, described Hydrobon catalyst, also containing potassium and phosphorus, wherein contains potassium 0.2 ~ 10.2 w%, P/K atomic ratio 0.1 ~ 10.0.
11. in accordance with the method for claim 1, it is characterized in that, the condition of step (1) described alkali-free sweetening is: reaction pressure 0.1 ~ 1.0MPa, temperature of reaction 20 DEG C ~ 70 DEG C, Feed space velocities 0.5 ~ 2.0h
-1, air flow quantity/inlet amount volume ratio is 0.1 ~ 1.0.
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| CN105738244B (en) * | 2014-12-10 | 2018-10-16 | 中国石油天然气股份有限公司 | Method for quantitatively determining dissolution rate of cleaning agent to petroleum sulfonate coked material |
| CN105462607B (en) * | 2016-01-13 | 2017-09-12 | 山东联星能源集团有限公司 | The group technology of catalytically cracked gasoline desulfurization |
| CN107867968B (en) * | 2016-09-23 | 2021-08-03 | 中国石油化工股份有限公司 | Method for reducing side reaction of hydrogenation ring opening of benzene ring |
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| CN101942328A (en) * | 2009-07-09 | 2011-01-12 | 中国石油化工股份有限公司抚顺石油化工研究院 | Hydrogenation method for gasoline and diesel |
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| US6692635B2 (en) * | 1999-02-24 | 2004-02-17 | Institut Francais Du Petrole | Process for the production of gasolines with low sulfur contents |
| CN101307255A (en) * | 2007-05-18 | 2008-11-19 | 中国石油化工股份有限公司 | Process for producing sweet gas for poor-quality gasoline distillate |
| CN101942331A (en) * | 2009-07-09 | 2011-01-12 | 中国石油化工股份有限公司抚顺石油化工研究院 | Gasoline and diesel oil combined hydrogenation method |
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