CN101376840B - Heavy fraction oil hydrotreating method - Google Patents
Heavy fraction oil hydrotreating method Download PDFInfo
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- CN101376840B CN101376840B CN 200710012688 CN200710012688A CN101376840B CN 101376840 B CN101376840 B CN 101376840B CN 200710012688 CN200710012688 CN 200710012688 CN 200710012688 A CN200710012688 A CN 200710012688A CN 101376840 B CN101376840 B CN 101376840B
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- hydrotreatment
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- 238000000034 method Methods 0.000 title claims abstract description 32
- 238000006243 chemical reaction Methods 0.000 claims abstract description 64
- 239000001257 hydrogen Substances 0.000 claims abstract description 29
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 29
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 25
- 239000007789 gas Substances 0.000 claims abstract description 25
- 239000007788 liquid Substances 0.000 claims abstract description 10
- 229910052717 sulfur Inorganic materials 0.000 claims abstract description 9
- 239000011593 sulfur Substances 0.000 claims abstract description 9
- 238000000926 separation method Methods 0.000 claims abstract description 5
- 239000003054 catalyst Substances 0.000 claims description 29
- 239000002994 raw material Substances 0.000 claims description 8
- RWSOTUBLDIXVET-UHFFFAOYSA-N Dihydrogen sulfide Chemical compound S RWSOTUBLDIXVET-UHFFFAOYSA-N 0.000 claims description 7
- 239000012263 liquid product Substances 0.000 claims description 4
- 238000009835 boiling Methods 0.000 claims description 3
- 239000002283 diesel fuel Substances 0.000 claims description 3
- 239000011280 coal tar Substances 0.000 claims description 2
- 239000003208 petroleum Substances 0.000 claims description 2
- 239000003245 coal Substances 0.000 claims 1
- 239000003921 oil Substances 0.000 abstract description 35
- 239000000463 material Substances 0.000 abstract description 7
- 239000000295 fuel oil Substances 0.000 abstract description 3
- 238000004523 catalytic cracking Methods 0.000 description 12
- 239000000047 product Substances 0.000 description 11
- 238000005984 hydrogenation reaction Methods 0.000 description 7
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 6
- 239000005864 Sulphur Substances 0.000 description 6
- 230000000694 effects Effects 0.000 description 5
- 238000006477 desulfuration reaction Methods 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- 150000002431 hydrogen Chemical class 0.000 description 4
- 239000012535 impurity Substances 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- 230000003197 catalytic effect Effects 0.000 description 3
- 239000007795 chemical reaction product Substances 0.000 description 3
- 238000011161 development Methods 0.000 description 3
- 238000012545 processing Methods 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 230000023556 desulfurization Effects 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 239000003974 emollient agent Substances 0.000 description 2
- 239000000446 fuel Substances 0.000 description 2
- 239000003502 gasoline Substances 0.000 description 2
- 229910000037 hydrogen sulfide Inorganic materials 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 description 1
- 239000004215 Carbon black (E152) Substances 0.000 description 1
- 108010010803 Gelatin Proteins 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 150000004945 aromatic hydrocarbons Chemical class 0.000 description 1
- 238000000975 co-precipitation Methods 0.000 description 1
- 239000000571 coke Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 229920000159 gelatin Polymers 0.000 description 1
- 239000008273 gelatin Substances 0.000 description 1
- 235000019322 gelatine Nutrition 0.000 description 1
- 235000011852 gelatine desserts Nutrition 0.000 description 1
- 229930195733 hydrocarbon Natural products 0.000 description 1
- 150000002430 hydrocarbons Chemical class 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- TVMXDCGIABBOFY-UHFFFAOYSA-N octane Chemical compound CCCCCCCC TVMXDCGIABBOFY-UHFFFAOYSA-N 0.000 description 1
- 238000005504 petroleum refining Methods 0.000 description 1
- 238000005554 pickling Methods 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 238000002203 pretreatment Methods 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 230000003245 working effect Effects 0.000 description 1
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- Production Of Liquid Hydrocarbon Mixture For Refining Petroleum (AREA)
Abstract
The invention relates to a hydrotreatment method of heavy diesel fractions. The heavy diesel fractions are used as material oil; under the hydrotreatment conditions, the material oil and circulated hydrogen are mixed and pass through a first hydrotreatment reaction area; gas and liquid are obtained through the high pressure separation of the oil generated by the hydrotreatment; the gas after being desulfurized is mixed with the liquid and then passes through a second hydrotreatment reaction area; the oil generated by the hydrotreatment is separated in a high pressure separator; the gas obtained through separation after passing through a compressor enters the first hydrotreatment reaction area; the liquid obtained through separation obtains a low-sulfur light oil product and a heavy oil product in a fractionating tower. Compared with the prior art, the method can effectively improve the hydrotreatment depth of the material oil; besides, the two hydrotreatment reaction areas only need one set of hydrogen circulating system; the device investment and the operation cost are low.
Description
Technical field
The present invention relates to a kind of hydroprocessing process, particularly a kind of low-sulfur recycle hydrogen that makes full use of carries out heavy distillate inferior the method for Deep Hydrotreating.
Background technology
Oil property becomes heavy gradually, becomes bad in the our times scope, the increasingly stringent of the sustainable development of world economy and environmental regulation in addition, need to produce a large amount of light clean fuels, these all require existing oil Refining Technologies is improved, and produce satisfactory product with minimum cost.
Produce in the working method of light-end products at heavy feed stock, catalytic cracking (FCC) still accounts for critical role.The light-end products of catalytic cracking technology direct production are second-rate, and especially the sulphur content of catalytic gasoline is than higher, and catalytic diesel oil sulphur content and aromaticity content height, cetane value are low.Therefore, the catalytic cracking product does not meet the requirement of clean fuel.In order to improve the quality of catalytic cracking product, need certain processing means, topmost approach generally has two kinds, i.e. and catalytic cracking generates the pre-treatment that oil subsidy fills hydrofining and catalytically cracked material.FCC raw material hydrogenation preconditioning technique can be avoided loss of octane number in the catalytic gasoline hydrogenation treating process, and has following advantage: the replacing speed that can reduce the FCC catalyzer; Reduce the FCC coke yield; Improving the FCC product distributes, improves the purpose product yield, reduces non-purpose product yield; Directly improve the FCC quality product, reduce the product sulphur content; Reduce the quantity discharged of FCC revivifier SOx, NOx etc., so FCC raw material hydrogenation pretreatment technology is widely used in modern refineries.
The catalytically cracked material preconditioning technique is that the stock oil with catalytic cracking carries out hydrotreatment earlier, remove impurity such as wherein most of sulphur, nitrogen, aromatic hydrocarbons has obtained fractional saturation, thereby improved the stock oil quality of catalytic cracking, can effectively reduce the operating severity of catalytic cracking unit, and improved the catalytic cracking quality product, and can directly obtain the purpose product, perhaps reduced back purified difficulty.
Existing catalytically cracked material preconditioning technique mainly contains: US3983029 and US6793804 disclose hydroprocessing technique and catalyzer, CN1313379 discloses a kind of hydroprocessing process of poor-quality raw material for catalytic cracking, and CN1646665 discloses the hydrotreatment of hydrocarbon raw material.These patents use conventional hydrotreating catalyst to carry out hydrotreatment under the common process condition, adopt usually and once pass through flow process, owing to be subjected to the influence that stock oil becomes heavy variation day by day, only could reduce the sulphur content of resultant under the critical operation condition.
Summary of the invention
At the deficiencies in the prior art, the invention provides a kind of catalytically cracked material Deep Hydrotreating method, can under than the demulcent operational condition, effectively improve the hydrotreatment degree of depth, production low-sulfur catalytic cracking stock, have the operating severity that reduces the hydrogenation pretreatment unit, reduce the operating operation expense, reduce temperature of reaction, increase the device processing power and prolong characteristics such as catalyzer work-ing life.
Heavy-oil hydrogenation treatment process of the present invention comprises following content:
A) with the heavy distillate be stock oil, under the hydrotreatment operational condition, stock oil and hydrogen-rich gas are by the first hydrotreatment reaction zone;
B) hydrotreatment that obtains of step a is flowed out thing and is entered Separate System of Water-jet, separates obtaining gas and liquid;
C) gas that obtains of step b carries out depriving hydrogen sulphide and handles;
D) liquid that obtains of gas phase behind the depriving hydrogen sulphide that obtains of step c and step b is by the second hydrotreatment reaction zone;
E) hydrotreatment that obtains of steps d is flowed out thing and is entered separation system, separates obtaining gas and liquid product;
F) gas that obtains of step e enters the first hydrotreatment reaction zone behind circulating hydrogen compressor, and as the hydrogen source of the first hydrotreatment reaction zone, the liquid product that step e obtains comprises low-sulfur petroleum naphtha and low-sulfur diesel-oil, and the low-sulfur wax oil;
The operational condition of the wherein said first hydrotreatment reaction zone is reaction pressure 3.0～20.0MPa, and hydrogen to oil volume ratio is 200: 1～2500: 1, and volume space velocity is 0.1～8.0h
-1, 260 ℃～455 ℃ of temperature of reaction; The operational condition of the described second hydrotreatment reaction zone is reaction pressure 3.0～20.0MPa, and hydrogen to oil volume ratio is 200: 1～2500: 1, and volume space velocity is 0.1～8.0h
-1, 260 ℃～455 ℃ of temperature of reaction; Described first reaction zone is than the second reaction zone pressure height, the high 0.01～2.0MPa of pressure.
It is 350～620 ℃ heavy ends that the heavy distillate raw material that the inventive method is used generally comprises boiling range, as being in the various vacuum gas oils (VGO) that obtain in the petroleum refining process, deasphalted oil (DAO), coker gas oil (CGO), heavy cycle oil (HCO) etc. one or more, also can be from coal tar, gelatin liquefaction wet goods.
The operational condition of the first hydrotreatment reaction zone is generally reaction pressure 3.0～20.0MPa, and hydrogen to oil volume ratio is 200: 1～2500: 1, and volume space velocity is 0.1～8.0h
-1, 260 ℃～455 ℃ of temperature of reaction; Preferred operational condition is reaction pressure 4.0～18.0MPa, hydrogen to oil volume ratio 300: 1～2000: 1, volume space velocity 0.2～6.0h
-1, 280～444 ℃ of temperature of reaction.The operational condition of the second hydrotreatment reaction zone is generally reaction pressure 3.0～20.0MPa, and hydrogen to oil volume ratio is 200: 1～2500: 1, and volume space velocity is 0.1～8.0h
-1, 260 ℃～455 ℃ of temperature of reaction; Preferred operational condition is reaction pressure 4.0～18.0MPa, hydrogen to oil volume ratio 300: 1～2000: 1, volume space velocity 0.2～6.0h
-1, 280～444 ℃ of temperature of reaction.First reaction zone is than the second reaction zone pressure height, the high 0.01～2.0MPa of pressure.
Two hydrotreatment reaction zones of the present invention can use identical hydrotreating catalyst, also can use different hydrotreating catalysts.Hydrotreating catalyst can all be conventional hydrotreating catalyst, also can be the combination of conventional hydrotreating catalyst and bulk phase catalyst.During combination loading, bulk phase catalyst can be seated in the top of reaction zone, also can be seated in the bottom of reaction zone, and perhaps two types catalyzer loads at interval, the volume ratio of bulk phase catalyst and conventional catalyst is 90: 10～10: 90, preferred 20: 80～80: 20.During combination loading, preferred feed by the bulk phase catalyst bed, helps bringing into play the catalyzer overall activity most then at first by common hydrotreating catalyst bed.Wherein conventional hydrotreating catalyst can be various commercial catalysts, as Fushun Petrochemical Research Institute (FRIPP) development and production 3926,3936, hydrotreating catalyst such as CH-20,3996, FF-14, FF-16, FF-18, FF-26, catalyzer such as the HR-416 of Inst Francais Du Petrole, HR-448, the TK-525 of Topsor company, TK-557 catalyzer, the KF-752 of AKZO company, KF-840, KF-901, KF-907 or the like.The FH-FS of bulk phase catalyst such as Fushun Petrochemical Research Institute (FRIPP) development and production etc.Above-mentioned hydrotreating catalyst also can be prepared by this area knowledge, common hydrotreating catalyst (loaded catalyst, active metallic content is relatively low, generally count 20%～45% with oxide compound) the general support of the catalyst of preparation earlier, use pickling process supported active metal component then, bulk phase catalyst (the active metallic content height generally counts 50%～85% with oxide compound) generally adopts the coprecipitation method preparation.
Compared with prior art, characteristics of the present invention are: because the present invention has increased a reactor, first section hydrotreatment generates oil in this reactor, under hydrogen and the low in hydrogen sulphide atmosphere, can reach the effect of deep desulfuration, perhaps reach identical when desulphurizing activated, improved the treatment capacity of device.Particularly the impurity that is easy in the heavy oil feed remove is being removed under the demulcent condition relatively, and carrying out under the difficult impurity employing favourable condition that reaction pressure is higher relatively, concentration of hydrogen sulfide is relatively low that removes, making that comprehensively taking off the impurity effect obviously improves.Owing to only use a circulating hydrogen compressor and a cover product fractionating system, and the circulating hydrogen compressor load reduces by 50% when reaching identical hydrogen-oil ratio, therefore can significantly reduce facility investment and process cost.
Description of drawings
Fig. 1 is a kind of process flow diagram of the present invention.
Fig. 2 is an another kind of process flow diagram of the present invention.
Embodiment
Shown in Figure 1, at first poor heavy raw material oil 1 and second reaction zone obtains hydrogen-rich gas 3 and is mixed into first reaction zone 2, the first hydrotreatment logistics 4 that obtains separates in separator 5, separate the gas 6 and the liquid 7 that obtain, wherein gas 6 after thionizer 8 desulfurization as the hydrogen 10 of second reaction zone, liquid 7 is mixed into second reaction zone 11 with hydrogen 10, obtains the second hydrotreatment logistics 12 after the reaction and separates in separator 13, separates obtaining gas, light ends 14 and hydrogenation wax oil 15.Light ends 14 can be used as light-end products, and hydrogenation wax oil 15 is as the catalytic cracking unit charging, and gas mixes the hydrogen source as first reaction zone with new hydrogen 16 after circulating hydrogen compressor 9 superchargings.
Fig. 2 and Fig. 1 difference only is: new hydrogen 16 mixes with processed gas 10 and directly enters second reaction zone 11.
Below by embodiment the present invention program and effect are described.
Table 1 stock oil character
| The stock oil title | Stock oil-1* | Stock oil-2** |
| Density (20 ℃)/gcm -3 | 0.931 | 0.902 |
| The boiling range scope/℃ | 360～600 | 360～560 |
| Sulphur content, wt% | 3.10 | 1.60 |
| Aromaticity content, wt% | 58 | 43 |
* stock oil-1 is mixing oil (VGO: CGO: DAO=50 wherein: 25: 25 weight ratios)
* stock oil-2 is mixing oil (VGO: CGO=60 wherein: 40 weight ratios)
The main composition and the character of table 2 Hydrobon catalyst
| Catalyzer | 3936 | FF-14 |
| Catalyzer is formed | ||
| MoO 3，wt％ | 24.5 | 24.0 |
| NiO，wt％ | 3.8 | 2.0 |
| CoO，wt％ | - | 1.6 |
| Carrier, wt% | Surplus | Surplus |
| The main character of catalyzer | ||
| Specific surface, m 2/g | ＞160 | ＞160 |
| Pore volume ml/g | 0.33 | ＞0.30 |
Table 3 embodiment 5 processing condition and test-results
By top embodiment as can be seen, because hydrogen sulfide content is low in second reaction zone, the liquid that first reaction zone obtains continues further reaction under optimized conditions in second reaction zone, can reach the effect of deep desulfuration, when perhaps reaching identical desulfurization depth, can increase the treatment capacity of device, perhaps reduce catalyst consumption, reduce facility investment and process cost.
Claims (7)
1. heavy distillate oil hydrotreating method comprises:
A) with the heavy distillate be stock oil, under the hydrotreatment operational condition, stock oil and hydrogen-rich gas are by the first hydrotreatment reaction zone;
B) hydrotreatment that obtains of step a is flowed out thing and is entered Separate System of Water-jet, separates obtaining gas and liquid;
C) gas that obtains of step b carries out depriving hydrogen sulphide and handles;
D) liquid that obtains of gas phase behind the depriving hydrogen sulphide that obtains of step c and step b is by the second hydrotreatment reaction zone;
E) hydrotreatment that obtains of steps d is flowed out thing and is entered separation system, separates obtaining gas and liquid product;
F) gas that obtains of step e enters the first hydrotreatment reaction zone behind circulating hydrogen compressor, and as the hydrogen source of the first hydrotreatment reaction zone, the liquid product that step e obtains comprises low-sulfur petroleum naphtha and low-sulfur diesel-oil, and the low-sulfur wax oil;
The operational condition of the wherein said first hydrotreatment reaction zone is reaction pressure 3.0～20.0MPa, and hydrogen to oil volume ratio is 200: 1～2500: 1, and volume space velocity is 0.1～8.0h
-1, 260 ℃～455 ℃ of temperature of reaction; The operational condition of the described second hydrotreatment reaction zone is reaction pressure 3.0～20.0MPa, and hydrogen to oil volume ratio is 200: 1～2500: 1, and volume space velocity is 0.1～8.0h
-1, 260 ℃～455 ℃ of temperature of reaction; Described first reaction zone is than the second reaction zone pressure height, the high 0.01～2.0MPa of pressure.
2. in accordance with the method for claim 1, it is characterized in that described heavy distillate raw material comprises that boiling range is 350～620 ℃ a heavy ends.
3. according to claim 1 or 2 described methods, it is characterized in that described heavy distillate raw material is one or more in vacuum gas oil, deasphalted oil, coker gas oil, the heavy cycle oil, perhaps from coal tar or liquefied coal coil.
4. in accordance with the method for claim 1, the operational condition that it is characterized in that the described first hydrotreatment reaction zone is reaction pressure 4.0～18.0MPa, hydrogen to oil volume ratio 300: 1～2000: 1, volume space velocity 0.2～6.0h
-1, 280 ℃～444 ℃ of temperature of reaction.
5. in accordance with the method for claim 1, the operational condition that it is characterized in that the described second hydrotreatment reaction zone is reaction pressure 4.0～18.0MPa, hydrogen to oil volume ratio 300: 1～2000: 1, volume space velocity 0.2～6.0h
-1, 280～444 ℃ of temperature of reaction.
6. in accordance with the method for claim 1, it is characterized in that the described first hydrotreatment reaction zone uses identical hydrotreating catalyst with the second hydrotreatment reaction zone, perhaps uses different hydrotreating catalysts.
7. in accordance with the method for claim 6, it is characterized in that described hydrotreating catalyst is conventional hydrotreating catalyst, perhaps is the combination of conventional hydrotreating catalyst and bulk phase catalyst.
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|---|---|---|---|
| CN 200710012688 CN101376840B (en) | 2007-08-27 | 2007-08-27 | Heavy fraction oil hydrotreating method |
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|---|---|---|---|
| CN 200710012688 CN101376840B (en) | 2007-08-27 | 2007-08-27 | Heavy fraction oil hydrotreating method |
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| CN101376840B true CN101376840B (en) | 2011-10-12 |
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Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101798527B (en) * | 2009-12-11 | 2013-03-13 | 深圳市兖能环保科技有限公司 | Treatment method for liquid products in garbage microwave pyrolysis treatment system and distillation equipment used by same |
| CN102453537B (en) * | 2010-10-14 | 2014-07-23 | 中国石油化工股份有限公司 | Method for maximum production of clean diesel oil by shale oil whole fraction hydrogenation |
| CN102465027B (en) * | 2010-11-05 | 2015-04-15 | 中国石油化工股份有限公司 | Hydrotreating method of heavy distillate oil |
| CN102465011B (en) * | 2010-11-05 | 2015-07-22 | 中国石油化工股份有限公司 | Hydrotreatment method of heavy distillate oil |
| CN110499190B (en) * | 2018-05-17 | 2022-02-01 | 中国石油天然气集团有限公司 | Residual oil hydrotreating system and residual oil hydrotreating method |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6190542B1 (en) * | 1996-02-23 | 2001-02-20 | Hydrocarbon Technologies, Inc. | Catalytic multi-stage process for hydroconversion and refining hydrocarbon feeds |
| US20030035765A1 (en) * | 2001-03-01 | 2003-02-20 | Intevep, S.A. | Hydroprocessing process |
| CN1646665A (en) * | 2002-04-05 | 2005-07-27 | 英格哈得公司 | Hydroprocessing of hydrocarbon feedstock |
| 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 |
-
2007
- 2007-08-27 CN CN 200710012688 patent/CN101376840B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6190542B1 (en) * | 1996-02-23 | 2001-02-20 | Hydrocarbon Technologies, Inc. | Catalytic multi-stage process for hydroconversion and refining hydrocarbon feeds |
| US20030035765A1 (en) * | 2001-03-01 | 2003-02-20 | Intevep, S.A. | Hydroprocessing process |
| CN1646665A (en) * | 2002-04-05 | 2005-07-27 | 英格哈得公司 | Hydroprocessing of hydrocarbon feedstock |
| 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 |
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