CN101724457B - Hydrogenation combined method for diesel oil - Google Patents
Hydrogenation combined method for diesel oil Download PDFInfo
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- CN101724457B CN101724457B CN 200810228411 CN200810228411A CN101724457B CN 101724457 B CN101724457 B CN 101724457B CN 200810228411 CN200810228411 CN 200810228411 CN 200810228411 A CN200810228411 A CN 200810228411A CN 101724457 B CN101724457 B CN 101724457B
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Abstract
The invention discloses a hydrogenation combined method for diesel oil, which comprises the following steps: dividing a straight-run diesel oil raw material and/or a coking diesel oil raw material into two parts of materials, performing hydro-upgrading reaction on one part of the material after being mixed with a catalytically cracked diesel oil raw material, and performing hydro-refining reaction on the other part of the material. The hydro-refining reaction and the hydro-upgrading reaction share a set of hydrogen recycling system. The combined method of the invention meets the requirement of products with different amounts and quality by flexibly adjusting raw oil ratio of two reaction zones, reduces operating severity of a hydro-upgrading reaction zone and prolongs the operation cycle at the same time. In addition, the method of the invention simplifies the process flow, can decrease equipment and reduces investment and operation cost. The method is suitable for hydro-processes of various inferior-quality distillate raw materials.
Description
Technical field
The present invention relates to a kind of hydrogenation combined method for diesel oil, particularly different properties diesel oil carries out hydrofining and hydro-upgrading by the technical process of optimizing, and obtains the combined hydrogenation method of quality products.
Background technology
Light materialization of heavy oil is that refiner's benefit increases point.The heavy oil lighting device that process cost such as coking and catalytic cracking and construction cost are low worldwide extensively exists.Because China market demand and refiner require to increase the benefit, secondary processing such as coking and catalytic cracking technology is extensive use of at each refinery, and the light ends oil that these devices are produced, especially diesel oil distillate need reach the requirement of product specification by further hydrogenation.Particularly catalytic cracking technology develops to voluminous high added value alkene direction, causes the further poor qualityization of diesel oil character of catalytic cracking, shows that mainly density is big, and cetane value is low.And environmental regulation requires production high-quality, light clean fuel, need carry out the deep hydrogenation upgrading to catalytic cracking diesel oil.Along with the diesel product specification of quality is more and more higher, straight-run diesel oil also just can reach specification of quality according to further hydrogenating desulfurization of practical situation needs or hydro-upgrading in addition.
Existing secondary processing distillate improves the quality of products and mainly finishes by hydrogenation process, mainly comprises hydrofining technology and hydro-upgrading technology for diesel oil distillate.
The hydrofining technology mainly contains two kinds: a kind of is with the single hop hydrofining under middle pressure or low pressure of secondary processing diesel oil cut, as FR2764902, RU2058371, US5068025, US5543036, US5817594, US5035793, CN1205312C etc., disclose diesel oil fraction hydrogenating purified technology, this technology adopts single hydrofinishing process to improve the quality of diesel oil distillate.Can be easy to make the sulphur content in the cut to reach low-down level, but the cetane value increase rate is less, generally can only improves 3～6 units.
Another kind of hydrofining technology is to use two sections purification techniquess of noble metal catalyst, it can guarantee that sulphur, nitrogen in the diesel oil remove fully with aromatic hydrocarbons and removes in a large number in second section in first section, make sulphur in the product, nitrogen and aromaticity content reach requirement, as US5556824 and US5651878 etc., but the one-time investment of its catalyzer and device is very huge, divide two sections operations again, operation is very complicated, and the stability of catalyzer awaits further to verify.
Adopt the middle pressure hydrocracking technology, as US5611912, US4985134, US4971680 and US4483760 etc., although can increase substantially every index of diesel oil distillate, but liquid yield is lower, especially the purpose product---diesel yield reduces manyly, and the gasoline fraction octane value that cracking obtains is low, also needs the reformation technology further to process.
Adopt the diesel oil fraction hydrogenating modification technology, as CN1156752A and CN1289832A etc., although can increase substantially diesel-fuel cetane number and reduce foreign matter contents such as sulphur, nitrogen, this technology is only applicable to the diesel raw material that cetane value is low, aromaticity content is high.
In the refining of petroleum enterprise, catalytic cracking and coking be two kinds most important, the heavy oil lighting technological process of amount of finish maximum, the quality of the distillates such as diesel oil that two kinds of processes obtain all can not satisfy the quality product requirement, especially catalytic cracking diesel oil density is big, the aromaticity content height, cetane value is low, prior art adopts the hybrid process mode usually to the diesel oil distillate that these two kinds of processes obtain, or with diesel raw material (as straight-run diesel oil etc.) the hybrid process mode in other source, though hybrid process has the simple advantage of technological process, but be unfavorable for carrying out the product upgrading targetedly, comprehensively improve the quality of products at the characteristics of different material.
Summary of the invention
At the deficiencies in the prior art, the invention provides a kind of hydrogenation combined method for diesel oil, flexible operation, by adjusting that material distributes and operational condition reaches the market requirement of variant production, and the cycle of operation is long.
It is wide that the diesel oil distillate that catalytic cracking process obtains has boiling range, aromaticity content height, characteristics such as cetane value is low.Straight-run diesel oil has the saturated hydrocarbon content height, sulphur content height, characteristics such as nitrogen content is low.It is wide that the vapour that coking obtains, diesel oil distillate have boiling range, sulphur, nitrogen content height, characteristics such as aromaticity content is relatively low, olefin(e) centent height.The present invention is directed to the inferior distillate oil of different sources, determine following combination hydrogenation modified technological process, specifically comprise the steps:
A, straight-run diesel oil raw material and/or coker gas oil raw material are divided into two strands of materials;
B, under the hydro-upgrading operational condition, one mixing of materials among catalytic cracking diesel oil raw material and a is through catalyst for hydro-upgrading bed, described catalyst for hydro-upgrading contains Modified Zeolite Y;
C, under the hydrofining operational condition, other one material among a is through Hydrobon catalyst bed;
D, step b and step c reaction effluent enter gas-liquid separator separately, perhaps enter same gas-liquid separator jointly, liquid phase enters the fractionating system fractionation and obtains the hydrogenated hydrocarbons series products, and gas phase is used for the hydro-upgrading process of step b and the unifining process of step c after adopting a cover recycle system supercharging.
The diesel oil distillate that obtains for atmospheric unit of the described straight-run diesel oil raw material of step a, the coker gas oil raw material is the diesel oil distillate that coker obtains.In two strands of materials that mixing oil is divided into, entering hydrofining reactor is 50:50～90:10 with the part by weight that enters the hydro-upgrading reactor content.
The described catalytic diesel oil raw material of step b is the diesel oil distillate that catalytic unit obtains, and the part by weight that enters hydro-upgrading reaction zone material among this material and the step a is 20:80～80:20.
The described catalyst for hydro-upgrading of step b is the catalyst for hydro-upgrading that contains Modified Zeolite Y, and catalyzer contains MoO by weight
3Or WO
315%～30%, NiO or CoO2%～15%, Modified Zeolite Y 10%～45% can contain auxiliary agent such as B simultaneously, and B content is 1%～9% by weight, and carrier is aluminum oxide and/or amorphous aluminum silicide.Wherein Modified Zeolite Y has following character: lattice constant is 2.436～2.444nm, and infrared total acid (160 ℃) is 0.5～1.1mmol/g.The hydro-upgrading process can adopt catalyst for hydro-upgrading separately, also can before catalyst for hydro-upgrading, use Hydrobon catalyst, Hydrobon catalyst can account for 10%～50% of total catalyst volume, and Hydrobon catalyst is the common Hydrobon catalyst in this area.
The described hydro-upgrading operational condition of step b is: reaction pressure 4.0MPa～15.0MPa, average reaction temperature is 300 ℃～420 ℃, volume space velocity 0.3h during liquid
-1～4.0h
-1, hydrogen to oil volume ratio is 100:1～2000:1.
The Hydrobon catalyst that the described Hydrobon catalyst of step c can adopt this area generally to adopt.The described hydrofining operational condition of step c is generally: reaction pressure 4.0MPa～15.0MPa, average reaction temperature is 260 ℃～420 ℃, volume space velocity 0.3h during liquid
-1～6.0h
-1, hydrogen to oil volume ratio is 100:1～2000:1.
During two serial parallel operations (recycle hydrogen enters hydrofining reactor and hydro-upgrading reactor respectively), the hydrogenation process of step a and step b adopts same pressure rating, common gas-liquid separator easy to use and common recycle hydrogen compressor.During two serial serial operations (the hydrogen series connection is used: recycle hydrogen is introduced into hydrofining reactor, enters the hydro-upgrading reactor then), step a is than the high 0.1～3.0MPa of step b, so that gas flow.Recycle hydrogen generally needs recirculation use behind depriving hydrogen sulphide.
The present invention is by optimizing the poor-quality diesel-oil by cut fraction oil raw material of different sources, adopt suitable technical process and optimize suitable catalyzer and operational condition, the inferior raw material of different sources is improved the quality of products under suitable operational condition, finally obtained ideal comprehensive process effect.In technical process, the inventive method and two kinds of raw materials add have saving equipment man-hour (gas-liquid separation equipment, stripping apparatus, hydrogen gas circulating system etc., particularly hydrogen gas circulating system are invested and accounted for higher proportion), advantage such as technical process is short, facility investment is low, process cost is low respectively in hydrogenation unit.The catalyzer that the upgrading of poor-quality diesel-oil by cut fraction need suit, the catalyzer that contains Modified Zeolite Y of optimized choice of the present invention has characteristics such as upgrading is deep, purpose product (diesel oil) yield height, is suitable for technological process of the present invention.Saturated hydrocarbon content height in the straight-run diesel oil, nitrogen content is low, and nitrogen and unsaturated hydrocarbons in the fraction of coker gas oil are easy to hydrogenation and removing, design this stock oil and catalytic cracking diesel oil and process simultaneously, can reduce the coking of catalyzer, thereby improve catalyzer work-ing life.The inventive method can be adjusted as required flexibly, at utmost satisfies the requirement in market.
Description of drawings
Fig. 1 is a kind of embodiment schematic flow sheet in parallel of the present invention.
Fig. 2 is a kind of series connection embodiment schematic flow sheet of the present invention.
Wherein: 1 is straight-run diesel oil, the mixing oil of coker gas oil or wherein a kind of, a is the raw material that enters reactor 2, b is the raw material that enters reactor 11, and 2 is hydrofining reactor, and 3 are the hydrofining resultant, 4 are the hydrofining high-pressure separator, 5 are the hydrofining hydrogen-rich gas, and 6 for hydrofining generates oil, and 7 is stripping tower or separation column, 8 are hydrofining raw gasline or petroleum naphtha, 9 is hydrofining diesel oil, and 10 is catalytic diesel oil, and 11 is the hydro-upgrading reactor, 12 is the hydro-upgrading resultant, 13 is the hydro-upgrading high-pressure separator, and 14 is the hydro-upgrading hydrogen-rich gas, and 15 are hydro-upgrading generation oil, 16 is separation column, 17 is the hydro-upgrading light naphthar, and 18 is hydro-upgrading heavy naphtha, and 19 is hydro-upgrading diesel oil, 20 is the circulation gas desulphurization system, 21 is recycle gas compressor, and 22 is new hydrogen, and 23 are the circulation gas after the supercharging, c is the circulation gas that enters reactor 2, and d is the circulation gas that enters reactor 11.
Embodiment
The described catalyst for hydro-upgrading of step a can basis the feedstock property difference, adjust accordingly, if raw material sulphur nitrogen impurity content is lower, can use catalyst for hydro-upgrading separately, if raw material sulphur nitrogen impurity is higher or raw material in be mixed with fraction of coker gas oil, can be before catalyst for hydro-upgrading, raw material contacts with Hydrobon catalyst earlier, removes impurity such as part sulphur nitrogen wherein.Hydrobon catalyst can be conventional Hydrobon catalyst, as the extensive stock Hydrobon catalyst, FH-5, the FH-5A that produces as Fushun Petrochemical Research Institute's development tissue, FH-98, FH-DS, FH-UDS, 3936, Hydrobon catalysts such as 3996, the function class that also can be other catalyst Co. exploitation is like catalyzer, HC-K, HC-P as Uop Inc., KF-847, the KF-848 etc. of the TK-555 of Topsor company, TK-565 catalyzer and AKZO company.Catalyst for hydro-upgrading can root character require to select commercial catalyst for hydro-upgrading, as 3963 of Fushun Petrochemical Research Institute's development tissue production, FC-18, FC-24, FC-26 etc.
The described conventional Hydrobon catalyst of step b can be identical with the Hydrobon catalyst that step a uses, also can be different.Can select the commodity Hydrobon catalyst, FH-5, the FH-5A that produces as Fushun Petrochemical Research Institute's development tissue, FH-98, FH-DS, FH-UDS, 3936, Hydrobon catalysts such as 3996, the function class that also can be other catalyst Co. exploitation is like catalyzer, HC-K, HC-P as Uop Inc., KF-847, the KF-848 etc. of the TK-555 of Topsor company, TK-565 catalyzer and AKZO company.
The present invention can adopt suitable technical process, catalyzer and processing condition according to the difference of feedstock property and product requirement.The percentage composition that relates among the present invention is a weight percentage.
Figure 1 shows that one embodiment of the present invention principle flow chart.
Figure 2 shows that another embodiment principle flow chart of the present invention.
Among Fig. 1, at first raw material a and hydrogen c are mixed into hydrofining reactor 2, obtain hydrofining generation oil 3 and enter hydrofining high-pressure separator 4, in hydrofining high-pressure separator 4, separate the hydrofining hydrogen-rich gas 5 that obtains and remove hydrogen sulfide through desulphurization system 20, and recycle after obtaining 23 through mixing with new hydrogen 22 after circulating hydrogen compressor 21 superchargings, the liquid that separation obtains in 4 obtains petroleum naphtha 9 and diesel oil 9 in separation column; Raw material 10, raw material b and hydrogen d are mixed into hydro-upgrading reactor 11, through series reaction, the hydro-upgrading that obtains generates oil 12 and enters hydro-upgrading high-pressure separator 13, in 13, separate the gas and the hydrofining hydrogen-rich gas 5 that obtain and be mixed into desulphurization system 20, separate the liquid 15 that obtains and enter separation column 16, and further fractionation obtains light naphthar 17, heavy naphtha 18 and diesel oil 19.
Fig. 2 is another kind of embodiment principle flow chart.The difference of Fig. 2 and Fig. 1 is that the logistics that the refining reaction district obtains directly enters upgrading reaction zone 11 through hydrogen-rich gas 5 bodies that gas-liquid separation obtains, and d can reduce the load of circulating hydrogen compressor like this as the hydrogen make-up of upgrading reaction zone, thereby reduces process cost.
Embodiment uses the main character of stock oil to list in table 1.Hydrofining operational condition and the results are shown in table 2.Hydro-upgrading operational condition and the results are shown in table 3.
Table 1 stock oil character
| The stock oil title | Stock oil-1 | Stock oil-2 | Stock oil-3 | Stock oil-4 |
| The source | Catalytic cracking diesel oil | Straight-run diesel oil | Coker gas oil | Coking gasoline and diesel |
| Density (20 ℃)/gcm -3 | 0.9534 | 0.8465 | 0.8672 | 0.8122 |
| The boiling range scope/℃ | 165～375 | 230～365 | 185～363 | 65～360 |
| Sulphur content, wt% | 0.88 | 2.10 | 1.30 | 0.90 |
| Nitrogen content, wt% | 0.12 | 0.04 | 0.13 | 0.07 |
| Cetane value | 16.9 | 52.8 | 45.1 |
Table 2 hydrofining operational condition and result
| Numbering | |
Embodiment 2 | |
| Stock oil | Stock oil-2 and stock oil-3 mixing oils | Stock oil-2 and stock oil-3 mixing oils | Stock oil-2 and stock oil-4 mixing oils |
| Stock oil ratio (mass ratio) | 50:50 | 40:60 | 30:70 |
| Catalyzer | FH-UDS | FH-DS | FH-98 |
| Reaction pressure/MPa | 12.0 | 10.0 | 8.0 |
| Temperature of reaction/℃ | 350 | 340 | 330 |
| LHSV/h -1 | 1.5 | 2.0 | 3.0 |
| Hydrogen to oil volume ratio (v/v) | 300:1 | 600:1 | 800:1 |
| ＜145 ℃ of gasoline fractions | |||
| Product yield, wt% | 1.3 | 1.8 | 10.2 |
| Sulphur content/μ gg -1 | <10 | 25 | 15 |
| 〉=145 ℃ of diesel oil distillates | 98.5 | 98.1 | 88.3 |
| Density (20 ℃)/gcm -3 | 0.8312 | 0.8362 | 0.8369 |
| Sulphur content/μ gg -1 | <10 | 80 | 50 |
| Cetane value | 53.2 | 51.9 | 51.3 |
Table 3 hydro-upgrading operational condition and result
| Numbering | |
Embodiment 2 | |
|||
| Stock | Stock oil | 1, stock oil-2 and stock oil-3 mixing | Stock oil | 1, stock oil-2 and stock oil-3 mixing | Stock oil | 1, stock oil-2 and stock oil-4 mixing oil |
| Stock oil ratio (mass ratio) | 50:25:25 | 60:16:24 | 70:9:21 | |||
| Catalyzer | FH-98/3963 | FC-18 | FF-26/FC-24 | |||
| Catalyst ratio (v/v) | 40/60 | / | 50/50 |
| Reaction pressure/MPa | 12.0 | 9.5 | 8.0 |
| Average reaction temperature/℃ | 375 | 360 | 355 |
| LHSV/h -1 | 1.0 | 1.5 | 0.7 |
| Hydrogen to oil volume ratio (v/v) | 500:1 | 700:1 | 1300:1 |
| ＜65 ℃ of petroleum naphthas | |||
| Yield, wt% | 2.8 | 2.1 | 4.0 |
| Sulphur content/μ gg -1 | <10 | <10 | <10 |
| 65～165 ℃ of petroleum naphthas | |||
| Yield, wt% | 10.3 | 5.4 | 8.3 |
| Virtue is dived, quality % | 68.4 | 72.3 | 59.5 |
| Sulphur content/μ gg -1 | <10 | <10 | <10 |
| 〉=165 ℃ of diesel oil distillates | |||
| Yield, wt% | 85.0 | 92.5 | 86.8 |
| Density (20 ℃)/gcm -3 | 0.8326 | 0.8368 | 0.8437 |
| Sulphur content/μ gg -1 | <10 | <10 | 12 |
| Cetane value | 52.8 | 51.2 | 49.1 |
From above embodiment, come as can be seen, the maximum characteristics of this combination process are, rationally utilize the characteristics separately of hydrogenation modifying process and hydrofining technology, when keeping higher diesel oil distillate yield and higher product, increased the handiness of operation.
Claims (9)
1. hydrogenation combined method for diesel oil comprises following process:
A, straight-run diesel oil raw material and/or coker gas oil raw material are divided into two strands of materials;
B, under the hydro-upgrading operational condition, one mixing of materials among catalytic cracking diesel oil raw material and a is through catalyst for hydro-upgrading bed, described catalyst for hydro-upgrading contains Modified Zeolite Y;
C, under the hydrofining operational condition, other one material among a is through Hydrobon catalyst bed;
D, step b and step c reaction effluent enter gas-liquid separator separately, perhaps enter same gas-liquid separator jointly, liquid phase enters the fractionating system fractionation and obtains the hydrogenated hydrocarbons series products, and gas phase is used for the hydro-upgrading process of step b and the unifining process of step c after adopting a cover recycle system supercharging;
In two strands of materials that step a raw material is divided into, entering hydrofining reactor is 50: 50～90: 10 with the part by weight that enters the hydro-upgrading reactor content; The described catalytic cracking diesel oil raw material of step b is the diesel oil distillate that catalytic unit obtains, and the part by weight that enters hydro-upgrading reaction zone material among this material and the step a is 50: 50～80: 20.
2. in accordance with the method for claim 1, it is characterized in that: the described straight-run diesel oil raw material of step a is the diesel oil distillate that atmospheric unit obtains, and the coker gas oil raw material is the diesel oil distillate that coker obtains.
3. in accordance with the method for claim 1, it is characterized in that: the described catalyst for hydro-upgrading of step b is the catalyst for hydro-upgrading that contains Modified Zeolite Y, and catalyzer contains MoO by weight
3Or WO
315%～30%, NiO or CoO2%～15%, Modified Zeolite Y 10%～45%.
4. according to claim 1 or 3 described methods, it is characterized in that: contained Modified Zeolite Y has following character in the catalyst for hydro-upgrading: lattice constant is 2.436～2.444nm, and 160 ℃ of infrared total acids are 0.5～1.1mmol/g.
5. in accordance with the method for claim 1, it is characterized in that: the hydro-upgrading process adopts catalyst for hydro-upgrading separately, perhaps uses Hydrobon catalyst before catalyst for hydro-upgrading, and Hydrobon catalyst accounts for 10%～50% of total catalyst volume.
6. in accordance with the method for claim 1, it is characterized in that: the described hydro-upgrading operational condition of step b is: reaction pressure 4.0MPa～15.0MPa, average reaction temperature is 300 ℃～420 ℃, volume space velocity 0.3h during liquid
-1～4.0h
-1, hydrogen to oil volume ratio is 100: 1～2000: 1.
7. in accordance with the method for claim 1, it is characterized in that: the described hydrofining operational condition of step c is: reaction pressure 4.0MPa～15.0MPa, average reaction temperature is 260 ℃～420 ℃, volume space velocity 0.3h during liquid
-1～6.0h
-1, hydrogen to oil volume ratio is 100: 1～2000: 1.
8. in accordance with the method for claim 1, it is characterized in that: two serial parallel operations of hydrofining and hydro-upgrading, recycle hydrogen enters hydrofining reactor and hydro-upgrading reactor respectively, and the hydrogenation process of step a and step b adopts same pressure rating.
9. in accordance with the method for claim 1, it is characterized in that: two serial serial operations of hydrofining and hydro-upgrading, recycle hydrogen is introduced into hydrofining reactor, enters the hydro-upgrading reactor then, and step a is than the high 0.1～3.0MPa of step b working pressure.
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| CN109988604B (en) * | 2017-12-29 | 2021-10-08 | 中国石油化工股份有限公司 | Hydrogenation coupling process for producing low-freezing-point diesel oil |
| CN109988627B (en) * | 2017-12-29 | 2021-07-09 | 中国石油化工股份有限公司 | Flexible paraffin hydrogenation process |
| CN109988601B (en) * | 2017-12-29 | 2021-07-09 | 中国石油化工股份有限公司 | Hydrogenation process for flexibly producing low-condensation-point diesel oil |
| CN109988628B (en) * | 2017-12-29 | 2021-07-09 | 中国石油化工股份有限公司 | Flexible single-stage hydrocracking process |
| CN109988603B (en) * | 2017-12-29 | 2021-07-09 | 中国石油化工股份有限公司 | Hydrogenation coupling process for producing low-freezing-point diesel oil |
| CN109988605B (en) * | 2017-12-29 | 2021-07-09 | 中国石油化工股份有限公司 | Flexible hydrocracking process for producing lubricating oil base oil |
| CN109988599B (en) * | 2017-12-29 | 2021-07-09 | 中国石油化工股份有限公司 | Flexible hydrogenation modification process for inferior diesel oil |
| CN109988600B (en) * | 2017-12-29 | 2021-07-09 | 中国石油化工股份有限公司 | Flexible hydrogenation modification process for poor diesel oil |
| CN109988645B (en) * | 2017-12-29 | 2021-06-04 | 中国石油化工股份有限公司 | Hydrogenation modification and hydrofining combined process for inferior diesel oil |
| CN109988643B (en) * | 2017-12-29 | 2021-06-04 | 中国石油化工股份有限公司 | Hydrogenation modification and hydrofining combined process for poor diesel oil |
| CN109988647B (en) * | 2017-12-29 | 2021-07-09 | 中国石油化工股份有限公司 | Flexible single-stage two-agent hydrocracking process |
| CN109988638B (en) * | 2017-12-29 | 2021-07-09 | 中国石油化工股份有限公司 | Hydrogenation process for flexibly producing low-condensation-point diesel oil |
| CN110041964B (en) * | 2019-05-21 | 2021-03-12 | 山东京博石油化工有限公司 | Production method of crude white oil product |
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| CN101003750A (en) * | 2006-01-19 | 2007-07-25 | 中国石油化工股份有限公司 | Method for producing high grade of diesel oil from charking full distillate oil |
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