CN101210198A - Hydrogenation method for producing high grade diesel oil and high grade reforming raw material - Google Patents
Hydrogenation method for producing high grade diesel oil and high grade reforming raw material Download PDFInfo
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Abstract
A hydrogenation method for producing high-quality diesel oil and high-quality reforming materials comprises the following steps of: mixing diesel oil and/or a light wax oil material with hydrogen gas, and sequentially contact-reacting with a hydrorefining catalyst and a hydrocracking catalyst without middle separation, cooling the reaction result, and separating to obtain a light naphtha fraction, a heavy naphtha fraction, a kerosene fraction, a diesel oil fraction and a tail oil fraction, wherein the kerosene fraction and/or the tail oil fraction can be directly extracted or partially or completely recycled back to the reaction system. By adopting single-stage once-through process and a non-noble metal catalyst, the invention can produce the reforming materials with high aromatic content and the diesel oil fraction with high cetane number, wherein the yield of the reforming material is larger than 20wt%, and the cetane number of the diesel oil fraction can be improved by more than 15 units. The method provided by the invention has high operation flexibility and can flexibly adjust the technical scheme according to different raw materials and different product scheme requirements.
Description
Technical field
The invention belongs to a kind of is the hydrocarbon ils cleavage method that obtains lower boiling cut existing under the situation of hydrogen, more particularly, is a kind of method of hydrotreating of producing fine-quality diesel oil and high-quality reformer feed.
Background technology
Specification of quality to diesel product is more and more higher in recent years, the clean diesel product requirement of new spec has low sulphur content, nitrogen content and other foreign matter content, except sulphur content in the diesel oil is made the more strict restriction, also aromaticity content and cetane value have been proposed further requirement, cetane value then general requirement is not less than 49.
As everyone knows, catalytic cracking is the important technical of oil product lighting.To be worth lower wax oil (can mix refining part residual oil) is raw material, by catalytic cracking can the production high value liquefied gas, gasoline and diesel product.Because catalytic cracking unit construction cost and process cost are lower, therefore obtained bigger development in China.But the catalytic diesel oil density that catalytic cracking is produced is big, the aromaticity content height, and cetane value is low, and foreign matter contents such as sulphur content, nitrogen content are higher, and character is very poor.The low-quality characteristic of catalytic cracking diesel oil has produced very big contradiction with the diesel product specification that improves day by day.
Catalytic diesel oil is rich in the aromatic hydrocarbons component, increase substantially cetane value must effectively reduce aromatic hydrocarbons particularly polycyclic aromatic hydrocarbons content, increase the particularly content of paraffinic hydrocarbons of stable hydrocarbon.Adopt conventional hydrofining method and highly active Hydrobon catalyst, under middle pressure, can slough foreign matter contents such as sulphur in the catalytic diesel oil, nitrogen effectively, the color of oil product is improved, but be difficult to realize increasing substantially cetane value by hydrofining.Result of study shows: in the hydrogen dividing potential drop is under 6.4MPa and the hydrogenation conditions such as common air speed, temperature, relies on conventional hydrofining technology, urges the multipotency of cetane value of bavin to improve 3～5 units, the density 0.015～0.025g/cm that can only descend
3The cetane value that improves catalytic diesel oil with hydrofinishing process has significant limitation.
In addition, because catalytic reforming unit has obtained bigger development in recent years, some refineries face the insufficient situation of reformer feed.And the heavy naphtha of hydro-upgrading process by-product has low sulphur nitrogen content and high virtue is dived, and is good reformer feed.
CN1234814C discloses a kind of method of hydrotreating of distillate, this patented method adopts a kind of catalytic diesel oil raw material of hydrogenation catalyst processing heavy under middle pressure, the main diesel oil distillate of producing high yield, though present method can obtain than high diesel yield, but naphtha yield is low, and the cetane value increase rate of diesel product is about 10 units.
US 5609752 discloses a kind of method that improves the distillate cetane value, this method can be processed high aromaticity content, the low-cetane distillate that initial boiling point is not less than 204 ℃, the catalyst activity metal that is adopted is selected from one or more among VIII family metal, rare earth metal, Mo, the W, preferred precious metals pt, carrier then is the beta-molecular sieve through hydrothermal treatment consists, make cakingagent with aluminum oxide, this catalyzer before use need be through the preprocessing process of reduction revulcanization, to improve the anti-sulphur nitrogen of noble metal catalyst poisoning capability.This method both can be connected by one section multi-agent, also can adopt the two-stage method flow process.But this method makes that cost increases, flexibility of operation reduces owing to adopted noble metal catalyst.
US 6264827 discloses a kind of method of producing high hexadecane value, low-sulfur diesel-oil, this method by two-stage method with the raw material production of low cetane value, high sulfur content go out high hexadecane value (＞45), low-sulfur (＜350ppm) and the good diesel product of stability in storage.First section adopt acid carrier load Ni, Co, Mo, W one or more as catalyzer, this acid carrier is molecular sieve or multiple oxide mixture, second section employing with porous material such as aluminum oxide as carrier, the catalyzer of load hydrogenation active metals thereon, first section mainly is the sulphur content in reducing raw material and improves its cetane value, and second section purpose is to decolour and improve the stability in storage of product.This method cetane value increase rate is low.
Summary of the invention
The objective of the invention is to provide on the basis of existing technology a kind of method of hydrotreating of producing fine-quality diesel oil and high-quality reformer feed.
Method provided by the invention is: diesel oil and/or light wax oil raw material with after hydrogen mixes successively with Hydrobon catalyst and hydrocracking catalyst contact reacts and without intermediate section from, resultant of reaction is through cooling, obtain hydrogen-rich gas and liquid phase stream after the separation, the gained liquid phase stream obtains light naphtha fraction through fractionation, heavy naphtha fraction, kerosene(oil)fraction, diesel oil distillate and tail oil cut, described kerosene(oil)fraction and/or tail oil cut can directly be extracted out or part circulates or all loop back reactive system, described hydrocracking catalyst is a kind of by zeolite and the carrier loaded at least a group VIII of aluminum oxide composite molding and the metal component of at least a group vib and the catalyzer of organic additive, and described organic additive is selected from and contains in oxygen or the nitrogenous organic compound one or more.
Described reaction conditions is: hydrogen dividing potential drop 5.0～12.0MPa, 330～400 ℃ of temperature of reaction, total liquid hourly space velocity 0.4～2.0h
-1, hydrogen to oil volume ratio 400～1000Nm
3/ m
3
Described diesel raw material is selected from one or more in straight-run diesel oil, catalytic cracking light cycle oil, coker gas oil, thermo-cracking diesel oil, the visbreaking diesel oil.Described light wax oil is that boiling range is 200～450 ℃ normal pressure or a vacuum distillate.Light wax oil mainly is selected from one or more in straight run atmosphere 3rd side cut, straight run vacuum 1st side cut, the heavy catalytic cycle oil.The stock oil that the present invention adopts is the mixing raw material of diesel oil distillate and/or light wax oil, and its sulphur content is preferably in below the 20000 μ g/g, and nitrogen content is preferably in below the 1500 μ g/g.
Cetane value is to weigh the index of fuel ignition quality in self-igniton engine, and the cetane value of regulation n-hexadecane is 100, and the cetane value of alpha-methyl-naphthalene is 0; When carbon number was identical, the cetane value of alkane was the highest, and the cetane value of aromatic hydrocarbon is minimum; In addition, the number of rings of aromatic hydrocarbon is many more, and cetane value is low more.Therefore, effectively improve the diesel product cetane value, need change the hydrocarbon composition structure of diesel oil: increase stable hydrocarbon especially paraffinic hydrocarbons content, reduce the especially content of polycyclic aromatic hydrocarbons of aromatic hydrocarbons.
Although the polycyclic aromatic hydrocarbons in the diesel oil can make it to take off lower level by hydrofinishing process or shallow degree hydrogenation modification method, if do not realize the naphthenic open loop then the cetane value increase rate still is limited.The product cetane value can increase substantially after realizing the naphthenic selective opening on the contrary.For example, the cetane value of naphthane is lower, behind the saturated perhydronaphthalene that obtains of naphthane hydrogenation its to be in harmonious proportion cetane value be 35～38, after opening one of them ring and becoming alkyl cyclopentane, it is in harmonious proportion cetane value and further brings up to 58～62.
In addition, the aromatic hydrogenation saturated reaction is the reaction of a strong heat release, smaller volume, limited by the thermodynamics of reactions equilibrated, so the reaction depth of hydrogenation saturated reaction (1), (2) is more shallow.If the saturated ring of naphthalene class is follow-up with ring-opening reaction (3), then can break the restriction of aromatic hydrogenation conversion reaction thermodynamic(al)equilibrium, promote the generation of reaction (1)-(3)-(4), this reaction scheme can effectively change the diesel oil hydrocarbon composition, increases the content of desirable component in the diesel oil distillate.Following formula has characterized this process:
The Hydrobon catalyst that the present invention adopts is the catalyst for refining with high arene saturating activity, high hydrodesulfurization activity and high hydrodenitrogenationactivity activity, can effectively reduce the nitrogen content in the raw material and carry out the aromatic hydrogenation saturated reaction, for follow-up selective opening cracking reaction creates conditions.The hydrocracking catalyst that the present invention adopts has good open loop selectivity, can break the thermodynamics equilibrium limit that aromatic hydrogenation transforms, and the low cut of boiling point such as mononuclear aromatics is transferred in the naphtha fraction, thereby realize aromatic hydrocarbons favourable conversion, produce high virtue dive reformer feed and high hexadecane value diesel product.
In addition, because the present invention has adopted Hydrobon catalyst and two doses of placed in-line flow processs of hydrocracking catalyst, the lighting function that has possessed heavy feed stock, thus can surpass the light wax oil of diesel oil distillate scope by the processing part boiling point, thus enlarge raw material sources, raising process economy.
Described Hydrobon catalyst is a kind of metal load type catalyst, carrier is unformed aluminum oxide and/or sial, metal component is VIB or VIII family base metal or their combination, and wherein the group vib metal is selected from molybdenum or/and tungsten, and VIII family metal is selected from cobalt or/and nickel.
The composition of preferred Hydrobon catalyst: with the catalyzer is benchmark, nickel oxide 1～10 weight %, and molybdenum oxide and Tungsten oxide 99.999 sum are 10～50 weight %, fluorine 1～10 weight %, Vanadium Pentoxide in FLAKES 0.5～8 weight %, surplus is a silica-alumina; With the carrier is benchmark, and silica content is 2～45 weight %, and alumina content is 55～98 weight %.
Described hydrocracking catalyst is a kind of by zeolite and the carrier loaded at least a group VIII of aluminum oxide composite molding and the metal component of at least a group vib and the catalyzer of organic additive, and described organic additive is selected from and contains in oxygen or the nitrogenous organic compound one or more.
The composition of preferred hydrocracking catalyst: with the catalyzer is benchmark, zeolite 3～60 weight %, and aluminum oxide 10～80 weight %, nickel oxide 1～15 weight %, Tungsten oxide 99.999 5～40 weight %, organic additive content are 0.1～40 weight %.
Described zeolite is selected from one or more in faujusite, Beta zeolite, ZSM-5 zeolite and the mordenite.
Preferred oxygen-containing organic compound is selected from one or more in organic alcohol, the organic acid; Preferred organic compounds containing nitrogen is selected from one or more in organic amine, the organic ammonium salt.For example, oxygenatedchemicals can be ethylene glycol, glycerol, polyoxyethylene glycol (molecular weight is 200-1500), Diethylene Glycol, butyleneglycol, acetate, toxilic acid, oxalic acid, nitrilotriacetic acid, 1,2-CDTA, Alpha-hydroxy tricarballylic acid (citric acid), 2, in 3-dyhydrobutanedioic acid (tartrate), the oxysuccinic acid one or more, organic compounds containing nitrogen can be quadrol, ethylenediamine tetraacetic acid (EDTA) (EDTA) and ammonium salt thereof.
The preparation method of this hydrocracking catalyst is as follows: precursor mixing, moulding, the roasting of zeolite, aluminum oxide and/or aluminum oxide are prepared into carrier.The salts solution of related reactive metal is mixed with mixing solutions with preferred organism, carrier is joined in this mixing solutions, the dipping certain hour, the elimination surplus solution obtains finished catalyst after drying, the activation.
The admission space ratio of described Hydrobon catalyst and hydrocracking catalyst is 30: 70～80: 20.For guaranteeing the long-term operation of full scale plant, in the agent of Hydrobon catalyst top filling hydrogenation protecting, the hydrogenation protecting agent is group vib metal or VIII family non-precious metal catalyst or their combination that loads on unformed aluminum oxide and/or the silica-alumina supports.This type of protective material has bigger pore volume and specific surface area.With the Hydrobon catalyst is benchmark, and the hydrogenation protecting agent accounts for 10%～20% of Hydrobon catalyst volume.
For preventing H
2The issuable alkene of S and cracking process further reacts the generation mercaptan sulfur, can be at a certain amount of catalyst for refining of hydrocracking reactor bottom filling, with the hydrocracking catalyst is benchmark, and this catalyst for refining accounts for 10%～30% of hydrocracking catalyst volume.
Method provided by the invention, not only adaptability to raw material is strong, and it is strong to implement handiness, can be according to different raw materials and different product requirements, flexible adjustment technology scheme is to satisfy different production demands.
Technical scheme one: with diesel oil distillate and/or light wax oil is raw material, is purpose with production high-quality reformer feed, high-quality boat coal and fine-quality diesel oil.
Diesel oil distillate and/or light wax oil with after hydrogen mixes successively with Hydrobon catalyst and hydrocracking catalyst contact reacts and without intermediate section from, resultant of reaction obtains hydrogen-rich gas and liquid phase stream after cooling, separation, the gained liquid phase stream obtains light naphtha fraction, heavy naphtha fraction, kerosene(oil)fraction, diesel oil distillate and tail oil cut through fractionation, perhaps according to demand product is cut into light naphtha fraction, heavy naphtha fraction, diesel oil distillate and tail oil cut.
The heavy naphtha fraction sulphur of gained, nitrogen content are the fine reformer feeds less than 0.5 μ g/g all, and yield is greater than 20 weight %, and the kerosene(oil)fraction of gained is the qualified rocket engine fuel cut of smoke point, and the diesel oil distillate of gained is that cetane value surpasses 51 fine-quality diesel oil.
Technical scheme two: with diesel oil distillate and/or light wax oil is raw material, is purpose with the greatly preparing hihg-quality reformer feed.
Diesel oil distillate and/or light wax oil with after hydrogen mixes successively with Hydrobon catalyst and hydrocracking catalyst contact reacts and without intermediate section from, resultant of reaction obtains hydrogen-rich gas and liquid phase stream after cooling, separation, the gained liquid phase stream obtains light naphtha fraction, heavy naphtha fraction, kerosene(oil)fraction, diesel oil distillate and tail oil cut through fractionation, and described kerosene(oil)fraction can partly circulate or all loop back reactive system.
When polycyclic aromatic hydrocarbons boiling point after hydrogenation is saturated to mononuclear aromatics descends.Studies show that diesel oil distillate mononuclear aromatics behind hydrogenation is enriched in 175～230 ℃ the kerosene(oil)fraction.Therefore, 175～230 ℃ kerosene(oil)fraction is looped back the hydrofining reactor inlet in the present invention or the hydro-upgrading reactor inlet carries out freshening, make the mononuclear aromatics in the kerosene(oil)fraction behind hydrogenation, be enriched in the naphtha fraction, this can not only improve the cetane value of diesel product, can also improve heavy naphtha yield and arene underwater content.The heavy naphtha fraction sulphur of gained, nitrogen content are the fine reformer feeds less than 0.5 μ g/g, and the diesel oil distillate of gained is that cetane value surpasses 51 fine-quality diesel oil.
Technical scheme three: with diesel oil distillate and light wax oil is raw material, is purpose to increase light ends oil yield.
The mixing raw material of diesel oil distillate and light wax oil with after hydrogen mixes successively with Hydrobon catalyst and hydrocracking catalyst contact reacts and without intermediate section from, resultant of reaction obtains hydrogen-rich gas and liquid phase stream after cooling, separation, the gained liquid phase stream obtains light naphtha fraction, heavy naphtha fraction, kerosene(oil)fraction, diesel oil distillate and tail oil cut through fractionation, and described tail oil cut can partly circulate or all loop back reactive system.When containing light wax oil in the raw material, product separation can obtain boiling range greater than 370 ℃ tail oil cut, this part tail oil cut is partly circulated or all loops back reactive system, further carries out hydrocracking, can further increase the yield of light ends oil.In addition, when not needing to produce kerosene and producing reformer feed and be purpose, also described kerosene(oil)fraction partly can be circulated or all loop back reactive system with maximum.
The heavy naphtha fraction sulphur of gained, nitrogen content are the fine reformer feeds less than 0.5 μ g/g, and the kerosene(oil)fraction of gained is the qualified rocket engine fuel cut of smoke point, and the diesel oil distillate of gained is that cetane value surpasses 51 fine-quality diesel oil.
The invention has the advantages that:
1, the present invention adopts single hop connect one-pass flow process and non-precious metal catalyst, and technical process is simple, and processing condition relax, and reaction pressure can be middle pressure, and temperature of reaction is low, the air speed height.
2, the present invention can process high poor ignition quality fuel of aromaticity content and/or light wax oil, produce the reformer feed of Gao Fangqian and the diesel oil distillate of high hexadecane value, wherein resulting heavy naphtha fraction yield is greater than 20 weight %, sulphur, nitrogen content need not promptly to can be used as the reformer charging through making with extra care again all less than 0.5 μ g/g.Resulting diesel oil distillate cetane value increase rate can be greater than 15 units.
3, method provided by the invention, flexibility of operation is strong, can be according to different raw materials and different product requirement, flexible adjustment technology scheme is to satisfy different products scheme demands.
Description of drawings
Accompanying drawing is the schematic flow sheet of the method for hydrotreating of production fine-quality diesel oil provided by the present invention and high-quality reformer feed.
Embodiment
Below in conjunction with accompanying drawing method provided by the present invention is further detailed.
Accompanying drawing is the schematic flow sheet of the method for hydrotreating of production fine-quality diesel oil provided by the present invention and high-quality reformer feed.Some utility appliance among the figure such as interchanger etc. do not mark, but this is known to those of ordinary skills.
The flow process of the method for hydrotreating of production fine-quality diesel oil provided by the present invention and high-quality reformer feed is as follows:
Mix after raw oil pump 3 boosts from the diesel oil distillate of pipeline 1 and/or from the light wax oil of pipeline 21, with mix from the new hydrogen of pipeline 2 and from the recycle hydrogen of pipeline 10, mixture enters hydrofining reactor 4, desulfurization, denitrogenation and aromatic hydrocarbons saturated reaction take place under the Hydrobon catalyst effect, its reaction effluent is without separating through pipeline 16, with enter hydrocracking reactor 5 after recycle hydrogen from pipeline 10 mixes, under the hydrocracking catalyst effect, carry out the reaction of cracking reaction and selective opening.The resultant of reaction of hydrocracking reactor 5 enters high-pressure separator 6 through pipeline 17 and carries out gas-oil separation.High-pressure separator 6 isolated hydrogen-rich gases enter circulating hydrogen compressor 9 through pipeline 18, and hydrogen-rich gas compresses after pipeline 10 extractions recycle as recycle hydrogen; High-pressure separator 6 isolated liquid streams enter light pressure separator 7 through pipeline 19 and carry out further gas-oil separation, light pressure separator 7 isolated gases are through pipeline 11 emptying, light pressure separator 7 isolated liquid enter separation column 8 through pipeline 20, separation column 8 isolated light naphtha fraction, heavy naphtha fraction, kerosene(oil)fraction, diesel oil distillate and tail oil cut are respectively through pipeline 12,13,14,15,26 withdrawing devices, wherein partly or entirely kerosene(oil)fraction can be successively through pipeline 22,23,25 grades loop back hydrofining reactor 4 inlet or successively through pipeline 22,23,24 grades loop back hydrocracking reactor 5 inlets, and wherein partly or entirely the tail oil cut can be successively through pipeline 27,23,25 grades loop back hydrofining reactor 4 inlet or successively through pipeline 27,23,24 grades loop back hydrocracking reactor 5 inlets.
The following examples will give further instruction to the present invention, but therefore not limit the present invention.
The commercial trade mark of used hydrogenation protecting agent, Hydrobon catalyst and hydrocracking catalyst is respectively RG-1, RN-32 and RHC-1 among the embodiment, is the Chang Ling catalyst plant production of Sinopec catalyzer branch office.
Embodiment 1
Present embodiment is stock oil A with a kind of catalytic diesel oil, and its raw material main character is as shown in table 1, and as can be seen from Table 1, the cetane value of this raw material only is 31.
Stock oil A with after hydrogen mixes successively with Hydrobon catalyst and hydrocracking catalyst contact reacts and without intermediate section from, resultant of reaction obtains hydrogen-rich gas and liquid phase stream after cooling, separation, the gained liquid phase stream obtains light naphtha fraction, heavy naphtha fraction and diesel oil distillate through fractionation, and the admission space ratio of Hydrobon catalyst and hydrocracking catalyst is 60: 40.Reaction conditions is as shown in table 2, and the yield and the character of the main products of gained are as shown in table 3.
As can be seen from Table 3, the heavy naphtha fraction sulphur of gained, nitrogen content are less than 0.5 μ g/g, and fragrant potential content is 58 weight %, are the fine reformer feeds, and yield is greater than 20 weight %, the sulphur content of diesel fraction of gained is less than 10 μ g/g, and polycyclic aromatic hydrocarbon content is less than 5.0 weight %, and cetane value is 53, it is the fine-quality diesel oil of high hexadecane value, the low virtue of low-sulfur, in addition, compare with raw material, cetane value has improved 22 units.
Table 1
| Stock oil | A |
| Density (20 ℃), g/cm 3 | 0.8876 |
| Sulphur content, μ g/g | 3480 |
| Nitrogen content, μ g/g | 1030 |
| The bromine valency, gBr/100g | 12.1 |
| Boiling range, ℃ (ASTM D-86) | |
| IBP/5％ | 182/206 |
| 10％/20％ | 219/236 |
| 30％/50％ | 251/275 |
| 70％/80％ | 309/325 |
| 90％/FBP | 346/375 |
| Cetane value | 31 |
Table 2
| Hydrofining reactor | Hydrocracking reactor | |
| The hydrogen dividing potential drop, MPa | 10.0 | 10.0 |
| Volume space velocity, h -1 | 1.17 | 1.75 |
| Temperature of reaction, ℃ | 357 | 364 |
| Hydrogen to oil volume ratio, Nm 3/m 3 | 700 | 700 |
Table 3
| Product cut | Light naphthar | Heavy naphtha | Diesel oil |
| The TBP cut coverage, ℃ | ＜65 | 65～165 | ＞165 |
| Yield, weight % | 3.79 | 20.80 | 75.03 |
| Density (20 ℃), g/cm 3 | 0.667 | 0.765 | 0.835 |
| Sulphur content, μ g/g | - | ＜0.5 | ＜10 |
| Nitrogen content, μ g/g | ＜0.5 | ＜0.5 | ＜1 |
| Polycyclic aromatic hydrocarbon content, weight % | - | - | ＜5.0 |
| Boiling range, ℃ (ASTM D-86) | |||
| IBP | 32 | 74 | 173 |
| 50％ | 47 | 108 | 260 |
| 90％ | 60 | 139 | 330 |
| FBP | 70 | 165 | 366 |
| Virtue is dived, weight % | - | 58 | - |
| Cetane value | - | - | 53 |
Embodiment 2
Stock oil A with after hydrogen mixes successively with Hydrobon catalyst and hydrocracking catalyst contact reacts and without intermediate section from, resultant of reaction obtains hydrogen-rich gas and liquid phase stream after cooling, separation, the gained liquid phase stream obtains light naphtha fraction, heavy naphtha fraction, kerosene(oil)fraction, diesel oil distillate and tail oil cut through fractionation, wherein boiling range is that 175～230 ℃ kerosene(oil)fraction all loops back the hydrofining reactor inlet, by weight, the round-robin kerosene(oil)fraction accounts for 15% of stock oil A.The admission space ratio of Hydrobon catalyst and hydrocracking catalyst is 60: 40.Reaction conditions is as shown in table 4, and the yield and the character of the main products of gained are as shown in table 5.As can be seen from Table 5, the heavy naphtha fraction sulphur of gained, nitrogen content are less than 0.5 μ g/g, and fragrant potential content is 62 weight %, are the fine reformer feeds, and yield is 31.8 weight %, the sulphur content of diesel fraction of gained is less than 10 μ g/g, and polycyclic aromatic hydrocarbon content is less than 5.0 weight %, and cetane value is 59, it is the fine-quality diesel oil of high hexadecane value, the low virtue of low-sulfur, in addition, compare with raw material, cetane value has improved 28 units.
Table 4
| Hydrofining reactor | Hydrocracking reactor | |
| The hydrogen dividing potential drop, MPa | 10.0 | 10.0 |
| Volume space velocity, h -1 | 1.35 | 2.01 |
| Temperature of reaction, ℃ | 357 | 364 |
| Hydrogen to oil volume ratio, Nm 3/m 3 | 700 | 700 |
Table 5
| Product cut | Light naphthar | Heavy naphtha | Diesel oil |
| The TBP cut coverage, ℃ | ＜65 | 65～165 | ＞220 |
| Yield, weight % | 5.86 | 31.80 | 61.34 |
| Density (20 ℃), g/cm 3 | 0.669 | 0.768 | 0.837 |
| Sulphur content, μ g/g | - | ＜0.5 | ＜10 |
| Nitrogen content, μ g/g | ＜0.5 | ＜0.5 | ＜1 |
| Polycyclic aromatic hydrocarbon content, weight % | - | - | ＜5.0 |
| Boiling range, ℃ (ASTM D-86) | |||
| IBP | 30 | 75 | 226 |
| 50％ | 45 | 109 | 310 |
| 90％ | 61 | 141 | 340 |
| FBP | 73 | 170 | 369 |
| Virtue is dived, weight % | - | 62 | - |
| Cetane value | - | - | 59 |
Embodiment 3
With a kind of light wax oil is stock oil B, with a kind of catalytic diesel oil is stock oil C, another kind of catalytic diesel oil is stock oil D, obtains mixing raw material oil E after stock oil B, stock oil C and stock oil D are mixed with weight ratio at 41: 41: 18, and the main character of these several stock oils is as shown in table 6.
Stock oil E with after hydrogen mixes successively with Hydrobon catalyst and hydrocracking catalyst contact reacts and without intermediate section from, resultant of reaction obtains hydrogen-rich gas and liquid phase stream after cooling, separation, the gained liquid phase stream obtains light naphtha fraction, heavy naphtha fraction, diesel oil distillate and tail oil cut through fractionation, reaction conditions is as shown in table 7, and the yield and the character of the main products of gained are as shown in table 8.The admission space ratio of Hydrobon catalyst and hydrocracking catalyst is 56: 44; in the agent of the top of Hydrobon catalyst filling hydrogenation protecting; the hydrogenation protecting agent accounts for 14.4% of Hydrobon catalyst volume; at hydrocracking reactor bottom filling Hydrobon catalyst; with the hydrocracking catalyst is benchmark, and Hydrobon catalyst accounts for 15.2% of hydrocracking catalyst volume.
As can be seen from Table 8, the heavy naphtha fraction sulphur of gained, nitrogen content are less than 0.5 μ g/g, the virtue potential content is 55.2 weight %, it is the fine reformer feed, and yield is 30.35 weight %, the sulphur content of diesel fraction of gained is less than 30 μ g/g, and cetane value is 54, and polycyclic aromatic hydrocarbon content is fine-quality diesel oils of high hexadecane value, low sulfur and low aromatics less than 3.0 weight %.
Table 6
| Stock oil | B | C | D | E |
| 20 ℃ of density, g/cm 3 | 0.8573 | 0.8900 | 0.9150 | 0.8807 |
| Boiling range, ℃ | ASTM D-1160 | ASTM D-86 | ASTM D-86 | ASTM D-1160 |
| Initial boiling point | 351 | 166 | 195 | 248 |
| 10％ | 355 | 266 | 215 | 261 |
| 30％ | 369 | - | - | 288 |
| 50％ | 384 | 281 | 270 | 340 |
| 70％ | 401 | - | 307 | 363 |
| 90％ | 417 | 355 | 351 | 392 |
| Do | 425 | 380 | 375 | 406 |
| Cetane value | - | 28.4 | 30 | - |
| Sulphur content, μ g/g | 2950 | 3500 | 5000 | 3550 |
| Nitrogen content, μ g/g | 472 | 600 | 1000 | 621 |
| Condensation point, ℃ | 33 | -4 | - | - |
Table 7
| Hydrofining reactor | Hydrocracking reactor | |
| The hydrogen dividing potential drop, MPa | 9.5 | 9.5 |
| Volume space velocity, h -1 | 1.44 | 1.82 |
| Temperature of reaction, ℃ | 355 | 366 |
| Hydrogen to oil volume ratio, Nm 3/m 3 | 790 | 790 |
Table 8
| Product cut | Light naphthar | Heavy naphtha | Diesel oil | Tail oil |
| The TBP cut coverage, ℃ | ＜65 | 65～175 | 175～370 | ＞370 |
| Product yield, weight % | 5.34 | 30.35 | 54.61 | 8.29 |
| Density (20 ℃), g/cm 3 | 0.670 | 0.751 | 0.817 | 0.820 |
| Sulphur content, μ g/g | - | ＜0.5 | ＜10 | ＜30 |
| Nitrogen content, μ g/g | ＜0.5 | ＜0.5 | ＜1 | ＜5 |
| 20 ℃ of viscosity, mm 2/s | - | - | 2.3 | 5.8(50℃) |
| Condensation point, ℃ | - | - | -11 | 28 |
| Polycyclic aromatic hydrocarbons, weight % | - | - | ＜3 | - |
| Hydrogen richness, weight % | - | - | - | 14.88 |
| Boiling range, ℃ (ASTM D-86) | ASTM D-1160 | |||
| IBP/10％ | 34/38 | 84/96 | 180/190 | 353/362 |
| 30％/50％ | 41/46 | 104/117 | 212/245 | 369/374 |
| 70％/90％ | 55/60 | 130/147 | 265/311 | 390/401 |
| FBP | 72 | 167 | 347 | 416 |
| Virtue is dived, weight % | - | 55.2 | - | - |
| Cetane value | - | - | 54 | - |
Embodiment 4
Present embodiment is a stock oil with mixing raw material oil E, stock oil E with after hydrogen mixes successively with Hydrobon catalyst and hydrocracking catalyst contact reacts and without intermediate section from, resultant of reaction obtains hydrogen-rich gas and liquid phase stream after cooling, separation, the gained liquid phase stream obtains light naphtha fraction, heavy naphtha fraction, diesel oil distillate and tail oil cut through fractionation, boiling range is looped back the hydrofining reactor inlet greater than 370 ℃ tail oil cut, by weight, round-robin tail oil cut accounts for 12% of stock oil E.Reaction conditions is as shown in table 9, and the yield and the character of the main products of gained are as shown in table 10.The admission space ratio of Hydrobon catalyst and hydrocracking catalyst is 56: 44; in the agent of the top of Hydrobon catalyst filling hydrogenation protecting; the hydrogenation protecting agent accounts for 14.4% of Hydrobon catalyst volume; at hydrocracking reactor bottom filling Hydrobon catalyst; with the hydrocracking catalyst is benchmark, and Hydrobon catalyst accounts for 15.2% of hydrocracking catalyst volume.
As can be seen from Table 10, the heavy naphtha fraction sulphur of gained, nitrogen content are less than 0.5 μ g/g, the virtue potential content is 55.6 weight %, it is the fine reformer feed, and yield is 31.09 weight %, the sulphur content of diesel fraction of gained is less than 10 μ g/g, and cetane value is 55, and polycyclic aromatic hydrocarbon content is fine-quality diesel oils of high hexadecane value, low sulfur and low aromatics less than 3.0 weight %.
Table 9
| Hydrofining reactor | Hydrocracking reactor | |
| The hydrogen dividing potential drop, MPa | 9.5 | 9.5 |
| Volume space velocity, h -1 | 1.64 | 2.07 |
| Temperature of reaction, ℃ | 356 | 366 |
| Hydrogen to oil volume ratio, Nm 3/m 3 | 700 | 700 |
Table 10
| Product cut | Light naphthar | Heavy naphtha | Diesel oil |
| The TBP cut coverage, ℃ | ＜65 | 65～175 | 175～370 |
| Product yield, weight % | 5.95 | 31.09 | 61.92 |
| Density (20 ℃), g/cm 3 | 0.669 | 0.752 | 0.819 |
| Sulphur content, μ g/g | ＜0.5 | ＜10 | |
| Nitrogen content, μ g/g | ＜0.5 | ＜0.5 | ＜1 |
| Viscosity (20 ℃), mm 2/s | - | - | 2.3 |
| Condensation point, ℃ | - | - | -11 |
| Polycyclic aromatic hydrocarbons, weight % | - | - | ＜3 |
| Boiling range, ℃ (ASTM D-86 | |||
| IBP/10％ | 34/38 | 84/96 | 178/192 |
| 30％/50％ | 41/46 | 105/118 | 217/249 |
| 70％/90％ | 55/60 | 132/148 | 273/317 |
| FBP | 72 | 167 | 347 |
| Virtue is dived, weight % | - | 55.6 | - |
| Cetane value | - | - | 55 |
Claims (10)
1. method of hydrotreating of producing fine-quality diesel oil and high-quality reformer feed, after it is characterized in that diesel oil and/or light wax oil raw material and hydrogen mixing successively with Hydrobon catalyst and hydrocracking catalyst contact reacts and without intermediate section from, resultant of reaction is through cooling, obtain hydrogen-rich gas and liquid phase stream after the separation, the gained liquid phase stream obtains light naphtha fraction through fractionation, heavy naphtha fraction, kerosene(oil)fraction, diesel oil distillate and tail oil cut, described kerosene(oil)fraction and/or tail oil cut can directly be extracted out or part circulates or all loop back reactive system, described hydrocracking catalyst is a kind of by zeolite and the carrier loaded at least a group VIII of aluminum oxide composite molding and the metal component of at least a group vib and the catalyzer of organic additive, and described organic additive is selected from and contains in oxygen or the nitrogenous organic compound one or more.
2. in accordance with the method for claim 1, it is characterized in that described reaction conditions is: hydrogen dividing potential drop 5.0～12.0MPa, 330～400 ℃ of temperature of reaction, total liquid hourly space velocity 0.4～2.0h
-1, hydrogen to oil volume ratio 400～1000Nm
3/ m
3
3. in accordance with the method for claim 1, it is characterized in that described diesel raw material is selected from one or more in straight-run diesel oil, catalytic cracking light cycle oil, coker gas oil, thermo-cracking diesel oil, the visbreaking diesel oil.
4. in accordance with the method for claim 1, it is characterized in that described light wax oil is that boiling range is 200～450 ℃ normal pressure or a vacuum distillate.
5. in accordance with the method for claim 1, it is characterized in that described Hydrobon catalyst is a kind of metal load type catalyst, carrier is a silica-alumina, metal component is group vib or VIII family base metal or their combination, wherein the group vib metal is selected from molybdenum or/and tungsten, and VIII family metal is selected from cobalt or/and nickel.
6. according to claim 1 or 5 described methods, it is characterized in that described Hydrobon catalyst, with the catalyzer is benchmark, and it consists of: nickel oxide 1～10 weight %, and molybdenum oxide and Tungsten oxide 99.999 sum are 10～50 weight %, fluorine 1～10 weight %, Vanadium Pentoxide in FLAKES 0.5～8 weight %, surplus is a silica-alumina, is benchmark with the carrier, silica content is 2～45 weight %, and alumina content is 55～98 weight %.
7. in accordance with the method for claim 1, it is characterized in that described hydrocracking catalyst, with the catalyzer is benchmark, it consists of: zeolite 3～60 weight %, aluminum oxide 10～80 weight %, nickel oxide 1～15 weight %, Tungsten oxide 99.999 5～40 weight %, organic additive content are 0.1～40 weight %.
8. according to claim 1 or 7 described methods, it is characterized in that oxygen-containing organic compound in the described organic additive is selected from one or more in organic alcohol, the organic acid; Organic compounds containing nitrogen is selected from one or more in organic amine, the organic ammonium salt.
9. according to claim 1 or 7 described methods, it is characterized in that described zeolite is selected from one or more in faujusite, Beta zeolite, ZSM-5 zeolite and the mordenite.
10. in accordance with the method for claim 1, the admission space ratio that it is characterized in that described Hydrobon catalyst and hydrocracking catalyst is 30: 70～80: 20.
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