CN102108307B - Method for lowering contents of impurities and polycyclic aromatic hydrocarbons in catalytic-cracking heavy oil - Google Patents
Method for lowering contents of impurities and polycyclic aromatic hydrocarbons in catalytic-cracking heavy oil Download PDFInfo
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- CN102108307B CN102108307B CN2009102600767A CN200910260076A CN102108307B CN 102108307 B CN102108307 B CN 102108307B CN 2009102600767 A CN2009102600767 A CN 2009102600767A CN 200910260076 A CN200910260076 A CN 200910260076A CN 102108307 B CN102108307 B CN 102108307B
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Abstract
The invention relates to a method for lowering contents of impurities and polycyclic aromatic hydrocarbons in catalytic-cracking heavy oil, which comprises steps as follows: catalytic-cracking heavy oil and circulating hydrogen are mixed, enter a first hydrogenation reaction zone, and sequentially contact a hydrogenation protective agent and a hydrofining catalyst to react; the reaction product of the first hydrogenation reaction zone and new hydrogen are mixed, enter a second hydrogenation reaction zone, and contact a hydrotreating catalyst to react; the reaction product of the second hydrogenation reaction zone is cooled and separated to obtain a hydrogen-rich gas and a liquid product; and the hydrogen-rich gas is circulated back to the inlet of the first hydrogenation reaction zone, and the liquid product enters a fractionating system. The second reaction zone is operated at low temperature, thereby greatly lowering the content of the polycyclic aromatic hydrocarbons. By using the invention, the contents of sulfur, nitrogen and polycyclic aromatic hydrocarbons in the catalytic-cracking heavy oil can be simultaneously lowered.
Description
Technical field
The invention belongs to a kind of method made from extra care hydrocarbon ils under the existence of hydrogen, more particularly, is a kind of method of coming sulphur, nitrogen and polycyclic aromatic hydrocarbon content in the decrease catalytic cracking heavy oil by hydrotreatment.
Background technology
Former oil quality along with the continuous increase of Oil extraction amount worse and worse, is mainly manifested in oil density and becomes large, and viscosity uprises, and heavy metal, sulphur, nitrogen, resin and asphalt equal size uprise.At present, the price difference of crude oil with poor quality and high-quality crude is along with the shortage of petroleum resources is also increasing, cause cheap crude oil with poor quality exploitation and working method more and more to receive publicity, that is to say, from crude oil with poor quality, improving as much as possible the yield of lightweight oil, this has brought huge challenge for the processing technology of traditional crude oil.
In the work flow of refinery, realize that the technical way of heavy oil conversion has the technology such as catalytic cracking (FCC), hydrocracking and coking.In China, catalytic cracking is because flexibility of operation is good, gasoline yield is high, the low broader applications that obtain of one-time investment.Transformation efficiency and the yield of light oil of existing catalytic cracking unit in order to increase catalytic cracking, usually heavy oil catalytic unit produced (heavy cycle oil) self circulates in catalytic cracking unit, but because the hydrogen richness of catalytic cracking heavy oil is low, polycyclic aromatic hydrocarbon content is high, and its cracking effect is unsatisfactory.A big chunk of catalytic cracking heavy oil is converted into coke, has increased the revivifier load, has reduced treatment capacity and the petrol and diesel oil product yield of catalytic cracking unit.
Catalytic cracking heavy oil is similar to the wax oil cut, and than common faulty wax oil, the catalytic cracking heavy oil aromaticity content is high, and polycyclic aromatic hydrocarbon content is especially high.Existing faulty wax oil hydrotreatment technology mainly be take and is removed the impurity such as sulphur in faulty wax oil, nitrogen and be leading indicator, and, for the hydrotreatment of catalytic cracking heavy oil, except removing the impurity such as sulphur, nitrogen, also will reduce polycyclic aromatic hydrocarbon content.
Chinese patent CN1100122C discloses a kind of hydroprocessing process of poor-quality raw material for catalytic cracking; the mixture of coker gas oil, deasphalted oil and vacuum gas oil to be carried out to the method for hydrotreatment production catalytic cracking charging; the method adopts the combination of a kind of hydrogenation protecting agent/hydrodemetallation (HDM) agent/Hydrobon catalyst; make metal content, sulphur content, the nitrogen content decrease of gas oil feedstocks inferior, meet the requirement of catalytic cracking unit to charging.
U.S. Pat 4780193 has been announced a kind of technology, and this technology adopts hydrorefined method to improve the quality of catalytically cracked material, and the temperature of reaction of hydro-refining unit is lower than 390 ℃, and reaction pressure should be more than 10.0MPa, more than being preferably in 12.0MPa.By the hydrofining meeting, reduce significantly catalytically cracked material sulphur and nitrogen content, thereby, can reduce significantly the content of SOx in catalytic cracking flue gas, the cracking catalyst deactivation rate also can reduce due to the minimizing of nitrogen content in raw material.
Chinese patent CN101007964A discloses a kind of technology that catalyst combination processing decompressed wax oil, wax tailings, the low nitrogen content fine quality catalytic cracking charging of diasphaltene wet goods production low-sulfur are set.The catalyst activity that this technology adopts is high, and flow process is simple, and working pressure is lower.
Summary of the invention
The objective of the invention is on the basis of existing technology, a kind of method of coming sulphur, nitrogen and polycyclic aromatic hydrocarbon content in the decrease catalytic cracking heavy oil by hydrotreatment is provided.
Method provided by the invention comprises:
(1) catalytic cracking heavy oil with enter the first hydroconversion reaction zone after recycle hydrogen mixes, with the hydrogenation protecting agent, contact and react with Hydrobon catalyst successively,
(2) first hydroconversion reaction zone resultant of reaction with enter the second hydroconversion reaction zone after new hydrogen mixes, with hydrotreating catalyst, contact and react,
(3) second hydroconversion reaction zone resultant of reaction obtain hydrogen-rich gas and product liquid after refrigerated separation, hydrogen-rich gas loops back the first hydroconversion reaction zone entrance, and product liquid enters fractionating system;
The temperature of reaction of the second hydroconversion reaction zone is lower 10 ℃～50 ℃ than the temperature out of the first reaction zone.
Catalytic cracking heavy oil of the present invention refers in the catalytic cracking charging and in catalytic cracking unit, is converted into unconverted part outside gas, light-end products (gasoline and diesel oil), slurry oil (initial boiling point is greater than 560 ℃) and coke.The catalytic cracking heavy oil aromaticity content is high, and is mainly polycyclic aromatic hydrocarbons, and polycyclic aromatic hydrocarbon content is greater than 30%, is preferably greater than 35%.The boiling range of described catalytic cracking heavy oil is 350 ℃～550 ℃.Here said polycyclic aromatic hydrocarbons refers to the thick and polynuclear aromatic compound that contains 2 or 3 above aromatic rings.
Catalytic cracking heavy oil can also reduce sulphur, nitrogen content after hydrotreatment.The reduction of sulphur content can reduce the sulphur content of catalytically cracked gasoline, reduces revivifier SO
xDischarge.Because nitrogen compound can make the active centre of FCC catalyzer poisoning and improve the coking behavior of catalyzer, so the reduction of nitrogen content can improve transformation efficiency and the product yield of catalytic cracking heavy oil.
In addition, adopt method provided by the invention, catalytic cracking heavy oil is carried out to hydrotreatment, make the saturated generation naphthenic hydrocarbon of polycyclic aromatic hydrocarbons wherein, will greatly improve the cracking performance of catalytic cracking heavy oil, thereby improve transformation efficiency and yield of light oil.And, after the polycyclic aromatic hydrocarbons hydrogenation, also can some generate mononuclear aromatics, mononuclear aromatics is difficult for cracking in FCC apparatus, but can lose side chain, produces high-octane gasoline.
Hydrogenating desulfurization and hydrodenitrification reaction belong to thermo-negative reaction, in actual hydrogenation process, mainly are subjected to kinetic control, raise with temperature, and desulfurization and denitrification reaction are accelerated.The saturated reaction of polycyclic aromatic hydrocarbons belongs to strong exothermal reaction, and at a lower temperature, the polycyclic aromatic hydrocarbons saturated reaction mainly is subjected to kinetic control, raises and improves with temperature.Along with the raising of temperature of reaction, the saturated meeting of polycyclic aromatic hydrocarbons reaches a maximum value, and along with the further raising of temperature, the polycyclic aromatic hydrocarbons saturated reaction mainly is subjected to thermodynamic (al) restriction and reduces gradually afterwards.In the hydrotreatment process of catalytic cracking heavy oil, if take desulfurization and denitrogenation is major objective, just must need to improve constantly the loss that temperature is carried out the compensate for catalyst activity.When temperature improves to a certain degree, will have influence on the polycyclic aromatic hydrocarbons saturated reaction.
The polycyclic aromatic hydrocarbons saturated reaction is the reaction that volume reduces, and improves the hydrogen dividing potential drop and is conducive to equally the carrying out of polycyclic aromatic hydrocarbons saturated reaction.
The present invention includes two reaction zones, the first hydroconversion reaction zone mainly carries out hydrogenating desulfurization and hydrodenitrification reaction, and the second hydroconversion reaction zone mainly carries out the hydrogenation saturated reaction of polycyclic aromatic hydrocarbons.The present invention sneaks into new hydrogen at the second hydroconversion reaction zone entrance, can reduce the temperature of reaction of the second hydroconversion reaction zone, is conducive to the hydrogenation saturated reaction of polycyclic aromatic hydrocarbons.At the second hydroconversion reaction zone entrance, sneak into the hydrogen dividing potential drop that new hydrogen can also significantly improve the second hydroconversion reaction zone, be conducive to equally the carrying out of the second hydroconversion reaction zone polycyclic aromatic hydrocarbons hydrogenation reaction.
The first hydroconversion reaction zone of the present invention and the second hydroconversion reaction zone can form by two beds in fixed-bed reactor, also can by two independently fixed-bed reactor form.
The hydrogenation conditions of the present invention's the first hydroconversion reaction zone is, hydrogen dividing potential drop 4.0MPa～12.0MPa, 330 ℃～420 ℃ of temperature of reaction, volume space velocity 0.4h
-1～2.0h
-1, hydrogen to oil volume ratio 100Nm
3/ m
3～1000Nm
3/ m
3.The hydrogenation conditions of the second hydroconversion reaction zone is: hydrogen dividing potential drop 4.0MPa～12.0MPa, 300 ℃～390 ℃ of temperature of reaction, volume space velocity 1.0h
-1～10h
-1, hydrogen to oil volume ratio 100Nm
3/ m
3～1000Nm
3/ m
3.Preferably the temperature of reaction of the second hydroconversion reaction zone is lower 20 ℃～40 ℃ than the temperature out of the first reaction zone.
The present invention's the first hydroconversion reaction zone loads hydrogenation protecting agent and hydrofining agent from top to bottom successively.Due to the fine powder of the catalytic cracking catalyst of carrying secretly in catalytic cracking heavy oil, be easy to be deposited between granules of catalyst, cause bed pressure drop to rise.This will cause full scale plant frequent shutdowns and catalyst changeout more, greatly reduce the utilization ratio of full scale plant, cause larger financial loss to enterprise.For the above-mentioned characteristic of catalytic cracking heavy oil, the present invention has loaded large, the active low hydrogenation protecting agent of voidage on the top of the first reaction zone, can remove the foulant in raw material, reaches the purpose of protection Primary Catalysts.Described hydrogenation protecting agent contains a kind of alumina supporter and loads on molybdenum and/or the tungsten on this alumina supporter, and nickel and/or cobalt.This hydrogenation protecting agent is the Raschig ring type, and voidage is not less than 0.60, preferably is not less than 0.65.This hydrogenation protecting agent has high voidage, low hydrogenation activity and high activity stability.
The Hydrobon catalyst that the present invention adopts at the first hydroconversion reaction zone rear portion can be for the known any catalyzer of hydrofining petroleum fractions.The reactive metal of described Hydrobon catalyst is selected from least a group VIII metal and at least a group vib metal.Preferred catalyzer is the Co-Mo of load on aluminum oxide, Ni-Mo and Ni-W type catalyzer.The carrier of described Hydrobon catalyst is one or more in aluminum oxide, silica-alumina, amorphous silicon aluminium, molecular sieve.
The hydrotreating catalyst that the present invention's the second hydroconversion reaction zone adopts can be identical with the Hydrobon catalyst of the first hydroconversion reaction zone, also can be different.Can be for the known any catalyzer of hydrotreatment petroleum fractions.The reactive metal of described hydrotreating catalyst is selected from least a group VIII metal and at least a group vib metal.Preferred catalyzer is the Co-Mo of load on aluminum oxide, Ni-Mo and Ni-W type catalyzer.The hydrotreating catalyst that more preferably hydrogenation activity is high, the aromatic saturation rate is high.The carrier of described hydrotreating catalyst is one or more in aluminum oxide, silica-alumina, amorphous silicon aluminium, molecular sieve.
The integer catalyzer of take is benchmark, and by volume, the filling ratio of hydrogenation protecting agent is 5%～20%, and the filling ratio of Hydrobon catalyst is 40%～90%, and the filling ratio of hydrotreating catalyst is 5%～40%.
Advantage of the present invention is:
1, the present invention adopts two reaction zones, and first reaction zone operates at higher temperature, can reduce catalytic cracking heavy oil sulphur, nitrogen content, improves the character of catalytic cracking heavy oil catalytic cracking product.Second reaction zone operates at lower temperature, content that can the decrease polycyclic aromatic hydrocarbons.By the present invention, can realize reducing simultaneously the purpose of sulphur in catalytic cracking heavy oil, nitrogen and polycyclic aromatic hydrocarbon content.
2, the present invention sneaks into new hydrogen at second reaction zone, can improve the hydrogen dividing potential drop of second reaction zone, thereby improves the saturation exponent of polycyclic aromatic hydrocarbons.
3, flow process of the present invention is simple, easy to operate, be applicable to newly-built, building or built hydrogenation unit.
The accompanying drawing explanation
Accompanying drawing is the method simple flow schematic diagram of impurity and polycyclic aromatic hydrocarbon content in reduction catalytic cracking heavy oil provided by the invention.
Embodiment
Below in conjunction with accompanying drawing, method of the present invention is further described, but not thereby limiting the invention.
In reduction catalytic cracking heavy oil provided by the invention, the method flow of impurity and polycyclic aromatic hydrocarbon content is as follows: catalytic cracking heavy oil 1 mixes laggard process furnace 4 through raw oil pump 2 pressurizations with recycle hydrogen 12 by pipeline 3; heating enters the first hydroconversion reaction zone 6 by pipeline 5, with the hydrogenation protecting agent, contacts and reacts with Hydrobon catalyst successively from top to bottom.The first hydroconversion reaction zone resultant of reaction the entrance of the second hydroconversion reaction zone 7 with enter the second hydroconversion reaction zone after new hydrogen 14 mixes, with hydrotreating catalyst, contact and react, the second hydroconversion reaction zone resultant of reaction enters high-pressure separator 9 through pipeline 8, after separation, obtain hydrogen-rich gas and product liquid, hydrogen-rich gas 10 loops back process furnace 4 entrances by circulating hydrogen compressor 11 compressions by pipeline 12 after removing hydrogen sulfide and ammonia, product liquid enters fractionating system through pipeline 13.
The following examples will be further described the present invention, but therefore not limit the present invention.
Catalytic cracking heavy oil raw material main character used in embodiment is in Table 1.
The catalyzer trade names that in embodiment, the first reaction zone adopts are respectively RG-10B and RSN-1, and the catalyzer trade names that second reaction zone adopts are RSN-1, produce by Sinopec catalyzer branch office Chang Ling catalyst plant.
The stock oil that this embodiment adopts is catalytic cracking heavy oil A, and main character is in Table 1.Stock oil with enter the first hydroconversion reaction zone after recycle hydrogen mixes, with the hydrogenation protecting agent, contact with Hydrobon catalyst successively from top to bottom.The first hydroconversion reaction zone resultant of reaction the entrance of the second hydroconversion reaction zone with enter second reaction zone after new hydrogen mixes, the second reaction zone resultant of reaction obtains hydrogen-rich gas and product liquid after refrigerated separation, hydrogen-rich gas loops back the first reaction zone entrance after removing hydrogen sulfide and ammonia, product liquid enters fractionating system.The present embodiment catalyst loading ratio, operational condition and hydrogenated products character are in Table 2.
As can be seen from Table 2, catalytic cracking heavy oil is after hydrotreatment, and sulphur, nitrogen content are reduced to 0.026% and 0.039% by 0.68% and 0.14% respectively.The content of polycyclic aromatic hydrocarbons is reduced to 18.8% by 41.5%, has reduced 22.7 percentage points.
Embodiment 2
The stock oil that this embodiment adopts is catalytic cracking heavy oil B, and main character is in Table 1.Stock oil with enter the first hydroconversion reaction zone after recycle hydrogen mixes, with the hydrogenation protecting agent, contact with Hydrobon catalyst successively from top to bottom.The first reaction zone resultant of reaction the entrance of the second hydroconversion reaction zone with enter second reaction zone after new hydrogen mixes, the second reaction zone resultant of reaction obtains hydrogen-rich gas and product liquid after refrigerated separation, hydrogen-rich gas loops back the first reaction zone entrance after removing hydrogen sulfide and ammonia, product liquid enters fractionating system.The catalyst loading ratio of the present embodiment, operational condition and hydrogenated products character are in Table 2.
As can be seen from Table 2, catalytic cracking heavy oil is after hydrotreatment, and sulphur, nitrogen content are reduced to 0.024% and 0.123% by 0.56% and 0.43% respectively.The content of polycyclic aromatic hydrocarbons is reduced to 19.0% by 31.3%, has reduced 12.3 percentage points.
Table 1
| Stock oil character | Catalytic cracking heavy oil A | Catalytic cracking heavy oil B |
| Density (20 ℃), g/cm 3 | 0.9517 | 0.9364 |
| Sulphur, heavy % | 0.68 | 0.56 |
| Nitrogen, heavy % | 0.14 | 0.43 |
| The mass spectrum quality forms, heavy % | ||
| Paraffinic hydrocarbons | 11.5 | 16.8 |
| Naphthenic hydrocarbon | 25.8 | 32.9 |
| Mononuclear aromatics | 15.8 | 14.3 |
| Polycyclic aromatic hydrocarbons | 41.5 | 31.3 |
| Total aromatic hydrocarbons | 57.3 | 45.6 |
| Colloid | 5.4 | 4.7 |
| Gross weight | 100.0 | 100.0 |
Table 2
Claims (9)
1. method that reduces impurity and polycyclic aromatic hydrocarbon content in catalytic cracking heavy oil comprises:
(1) catalytic cracking heavy oil with enter the first hydroconversion reaction zone after recycle hydrogen mixes; with the hydrogenation protecting agent, contact and react with Hydrobon catalyst successively; in described catalytic cracking heavy oil, the content of polycyclic aromatic hydrocarbons is greater than 30%, and the boiling range of described catalytic cracking heavy oil is 350 ℃～550 ℃
(2) first hydroconversion reaction zone resultant of reaction with enter the second hydroconversion reaction zone after new hydrogen mixes, with hydrotreating catalyst, contact and react,
(3) second hydroconversion reaction zone resultant of reaction obtain hydrogen-rich gas and product liquid after refrigerated separation, hydrogen-rich gas loops back the first hydroconversion reaction zone entrance, and product liquid enters fractionating system;
The temperature of reaction of the second hydroconversion reaction zone is than low 10～50 ℃ of the temperature out of the first reaction zone.
2. in accordance with the method for claim 1, it is characterized in that, the hydrogenation conditions of the first hydroconversion reaction zone is: hydrogen dividing potential drop 4.0MPa～12.0MPa, 330 ℃～420 ℃ of temperature of reaction, volume space velocity 0.4h
-1～2.0h
-1, hydrogen to oil volume ratio 100Nm
3/ m
3～1000Nm
3/ m
3.
3. in accordance with the method for claim 1, it is characterized in that, the hydrogenation conditions of the second hydroconversion reaction zone is: hydrogen dividing potential drop 4.0MPa～12.0MPa, 300 ℃～390 ℃ of temperature of reaction, volume space velocity 1.0h
-1～10h
-1, hydrogen to oil volume ratio 100Nm
3/ m
3～1000Nm
3/ m
3.
4. in accordance with the method for claim 1, it is characterized in that, the temperature of reaction of the second hydroconversion reaction zone is lower 20 ℃～40 ℃ than the temperature out of the first reaction zone.
5. in accordance with the method for claim 1, it is characterized in that, the integer catalyzer of take is benchmark; by volume; the filling ratio of hydrogenation protecting agent is 5%～20%, and the filling ratio of Hydrobon catalyst is 40%～90%, and the filling ratio of hydrotreating catalyst is 5%～40%.
6. in accordance with the method for claim 1, it is characterized in that, described hydrogenation protecting agent contains a kind of alumina supporter and loads on molybdenum and/or the tungsten on this alumina supporter, and nickel and/or cobalt.
7. in accordance with the method for claim 1, it is characterized in that, the reactive metal of described Hydrobon catalyst is selected from least a group VIII metal and at least a group vib metal.
8. in accordance with the method for claim 1, it is characterized in that, the reactive metal of described hydrotreating catalyst is selected from least a group VIII metal and at least a group vib metal.
9. in accordance with the method for claim 1, it is characterized in that, the carrier of described Hydrobon catalyst and hydrotreating catalyst is one or more in aluminum oxide, silica-alumina, amorphous silicon aluminium, molecular sieve.
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| CN102899081B (en) * | 2011-07-28 | 2015-03-18 | 中国石油化工股份有限公司 | Wax oil hydrotreating method |
| CN103160317B (en) * | 2011-12-15 | 2015-07-01 | 中国石油化工股份有限公司 | Production method of propylene and gasoline with high-octane rating |
Citations (4)
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|---|---|---|---|---|
| CN1335366A (en) * | 2000-07-24 | 2002-02-13 | 中国石油化工股份有限公司 | Heavy oil and residual oil hydrogenating conversion process |
| CN1997724A (en) * | 2004-06-17 | 2007-07-11 | 埃克森美孚研究工程公司 | Catalyst combination and two-step hydroprocessing method for heavy hydrocarbon oil |
| CN101020845A (en) * | 2006-02-14 | 2007-08-22 | 中国石油化工股份有限公司 | Gas oil and residual oil hydrotreating process for producing catalytically cracked material |
| CN101360808A (en) * | 2005-12-16 | 2009-02-04 | 雪佛龙美国公司 | Process for upgrading heavy oil using a highly active slurry catalyst composition |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1335366A (en) * | 2000-07-24 | 2002-02-13 | 中国石油化工股份有限公司 | Heavy oil and residual oil hydrogenating conversion process |
| CN1997724A (en) * | 2004-06-17 | 2007-07-11 | 埃克森美孚研究工程公司 | Catalyst combination and two-step hydroprocessing method for heavy hydrocarbon oil |
| CN101360808A (en) * | 2005-12-16 | 2009-02-04 | 雪佛龙美国公司 | Process for upgrading heavy oil using a highly active slurry catalyst composition |
| CN101020845A (en) * | 2006-02-14 | 2007-08-22 | 中国石油化工股份有限公司 | Gas oil and residual oil hydrotreating process for producing catalytically cracked material |
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