CN103102896B - Hydro-upgrading method for production of low-condensation point motor fuel from biolipid - Google Patents
Hydro-upgrading method for production of low-condensation point motor fuel from biolipid Download PDFInfo
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- CN103102896B CN103102896B CN201110353377.1A CN201110353377A CN103102896B CN 103102896 B CN103102896 B CN 103102896B CN 201110353377 A CN201110353377 A CN 201110353377A CN 103102896 B CN103102896 B CN 103102896B
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E50/00—Technologies for the production of fuel of non-fossil origin
- Y02E50/10—Biofuels, e.g. bio-diesel
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P30/00—Technologies relating to oil refining and petrochemical industry
- Y02P30/20—Technologies relating to oil refining and petrochemical industry using bio-feedstock
Abstract
The invention relates to a hydro-upgrading method for production of a low-condensation point motor fuel from biolipid. The method comprises the following steps that: biolipid is used as raw oil, and the raw oil and hydrogen pass through a first-stage hydrogenation reaction zone, wherein the first-stage hydrogenation reaction zone comprises at least two hydrogenation catalyst beds in which the content of a hydrogenation active component successively increases; a material flow generated in first-stage hydrogenation is separated, obtained hydrogen-rich gas is recycled, and obtained liquid enters into a second-stage hydro-upgrading reaction zone; and a material flow generated in second-stage hydrogenation is separated, obtained side hydrogen is recycled, and an obtained liquid product is subjected to fractionation so as to obtain naphtha and low-condensation point diesel oil; wherein in a reaction state, the active component of all the hydrogenation catalysts is one or more selected from the group consisting of W, Mo, Ni and Co in a reduction state. Compared with the prior art, the method provided by the invention can produce the low-condensation point motor fuel while guaranteeing activity stability of the catalysts and long-period stable running of an apparatus.
Description
Technical field
The present invention relates to a kind of hydroprocessing process, particularly a kind of is stock oil with bio-oil, the hydrogenation modification method of the low condensation point automotive fuel of direct production.
Background technology
The energy in current global range is mainly derived from fossil energy, and its PetroChina Company Limited. is the main source of automotive fuel.Oil belongs to Nonrenewable energy resources, not only resource is day by day exhausted, and heaviness and in poor quality aggravation, and world economy sustainable development, environmental regulation increasingly stringent need to produce a large amount of light clean fuel, these increase new oil substitutes while all requiring to improve existing oil Refining Technologies, produce satisfactory product with minimum cost.
Bio-oil, as renewable resources, obtains the extensive attention in the world, and each research unit and enterprise are all making great efforts to carry out its research as clean energy.The method production biofuel (being generally fatty acid methyl ester) of transesterify is utilized to be comparatively proven technique, but because fatty acid methyl ester oxygen level is high, although many countries and regions have put into effect the standard of biofuel successively, and are not suitable for all oil engines.Bio-oil produces automotive fuel by the method for hydrogenation, and all remove by oxygen or partly remove the product produced and meet automotive fuel standard, this method directly can meet the requirement of existing market.
Existing animal-plant oil hydrogenation method produces the processing technology of automotive fuel, US20060186020, EP1693432, CN101321847A, CN200710012090.6, CN200680045053.9, CN200710065393.4, CN200780035038.0, CN200710012208.5, CN200780028314.0 and CN101029245A etc. disclose vegetables oil hydroconversion process, adopt coker naphtha, diesel oil distillate (straight-run diesel oil, LCO and coker gas oil), the petroleum hydrocarbon cuts such as wax oil cut and bio-oil are mixed into hydrogenation catalyst bed, produce diesel product or preparing ethylene by steam cracking raw material etc.US5705722 discloses the diesel oil blending component producing diesel oil distillate scope containing the vegetables oil such as unsaturated fatty acids, fat and animal oil mixing back end hydrogenation.
EP1741767 and EP1741768 discloses a kind of method of producing diesel oil distillate with animal-plant oil, be mainly animal-plant oil first through hydrotreatment, then by isomerization catalyst bed layer, obtain low freezing point diesel fuel component, but owing to generating water in hydroprocessing processes, cause very adverse influence to isomerization catalyst, device can not long-period stable operation.
Comprise in the bio-oil hydrogenation process of aforesaid method, one of subject matter run into is that beds carbon deposit causes shorten running period, needs more catalyst changeout of often stopping work.Particularly independent with bio-oil be raw material or bio-oil blending ratio higher time, the running period of hydrogenation catalyst is more subject to obvious impact.
In prior art, bio-oil hydrogenation produces the method for automotive fuel, the petroleum fractions hybrid process of general needs and larger proportion, otherwise can not running period be ensured, or directly by hydrofining-catalyst for hydro-upgrading bed, the component poor stability of cracking catalyst activity.The present invention is by optimizing the grating technology and operational condition that use catalyzer, first paragraph hydrofining (hydrogenation catalyst of grating), second segment hydro-upgrading, it can be directly raw material production high-grade low-freezing point automotive fuel with bio-oil, solving bio-oil hydrogenation unit can not the problem of long period steady running, significantly can reduce the condensation point of diesel oil distillate simultaneously.
Summary of the invention
For the deficiencies in the prior art, the invention provides the hydrogenation modification method that a kind of bio-oil produces low condensation point automotive fuel, independent is stock oil with bio-oil, the method of the low condensation point automotive fuel of direct production under the condition of hydrogenation, can direct production super low sulfur, low density, low freezing point diesel fuel be in harmonious proportion product, the situation that diesel product can not be occurred biofuel that conventional animal-plant oil obtains is gone mouldy, hydrogenation process is stablized, and running period is long.
The hydrogenation modification method that bio-oil of the present invention produces low condensation point automotive fuel comprises following content:
A one or more in () bio-oil are stock oil;
B () is under Hydroprocessing conditions, stock oil and hydrogen are by first paragraph reaction zone, first paragraph reaction zone comprises the hydrogenation catalyst bed that at least two hydrogenation active component content raise successively, first stock oil and hydrogen pass through the low beds of hydrogenation active component content, then the high beds of hydrogenation active component content is passed through, under response behaviour, hydrogenation active component is one or more in W, Mo, Ni and Co of reduction-state;
C () first paragraph reaction zone hydrogenation effluent is separated into gas phase and liquid phase, gas-phase dehydration process Posterior circle uses, the second segment reaction zone using catalyst for hydro-upgrading is entered after liquid phase mixes with circulation gas, under response behaviour, the active metal component of catalyst for hydro-upgrading is one or more in W, Mo, Ni and Co of reduction-state;
D gas phase that () second segment reaction zone generates logistics recycles, and liquid phase fractionation in separation column that second segment reaction zone generates logistics obtains petroleum naphtha and low freezing point diesel fuel.
In the inventive method step (a), the bio-oil used can comprise vegetables oil or animal grease, vegetables oil comprises one or more in soybean oil, peanut oil, Viscotrol C, rapeseed oil, Semen Maydis oil, sweet oil, plam oil, Oleum Cocois, tung oil, oleum lini, sesame oil, Oleum Gossypii semen, sunflower seed oil and rice bran wet goods, and animal grease comprises one or more in butter, lard, sheep oil and fish oil etc.
In the inventive method step (b), the Hydroprocessing conditions of first paragraph reaction zone is generally reaction pressure 3.0MPa ~ 20.0MPa, and hydrogen to oil volume ratio is 200:1 ~ 3000:1, and volume space velocity is 0.1h
-1~ 6.0h
-1, average reaction temperature 180 DEG C ~ 465 DEG C; Preferred operational condition is reaction pressure 4.0MPa ~ 18.0MPa, hydrogen to oil volume ratio 300:1 ~ 2500:1, volume space velocity 0.2h
-1~ 4.0h
-1, average reaction temperature 200 DEG C ~ 445 DEG C.
In the inventive method step (b), beds generally can arrange 2 ~ 5, in the beds that first reaction mass passes through, hydrogenation active component with the weight content of oxide basis for 3% ~ 10%, the hydrogenation catalyst that first reaction mass passes through accounts for 10% ~ 80% of all hydrogenation catalyst volumes in first paragraph reaction zone, preferably 20% ~ 70%, best 30% ~ 60%.The hydrogenation active component of the downstream catalyst that reaction mass passes through increases by 3 ~ 25 percentage points in oxide weight than adjacent upstream catalyzer, preferably increases by 5 ~ 20 percentage points.Beds generally can arrange 2 ~ 5.The carrier of hydrogenation catalyst is generally aluminum oxide, amorphous silicon aluminium, silicon oxide, titanium oxide etc., can contain other auxiliary agent, as P, Si, B, Ti, Zr etc. simultaneously.Can commercial catalyst be adopted, also can by the existing method preparation in this area.The business hydrogenation catalyst that first reaction zone uses mainly contains, as Fushun Petrochemical Research Institute (FRIPP) develop 3926, 3936, CH-20, FF-14, FF-18, FF-24, FF-26, FF-36, FH-98, FH-UDS, the hydrogenation catalysts such as FZC-41, the HR-416 of Inst Francais Du Petrole, the hydrogenation catalysts such as HR-448, the ICR174 of CLG company, ICR178, the hydrogenation catalysts such as ICR179, Uop Inc. is newly developed HC-P, HC-K UF-210/220, the TK-525 of Topsor company, TK-555, the hydrogenation catalysts such as TK-557, the KF-752 of AKZO company, KF-840, KF-848, KF-901, the hydrogenation catalysts such as KF-907.
In the inventive method step (c), the Hydroprocessing conditions of second segment reaction zone is generally reaction pressure 3.0MPa ~ 20.0MPa, usually (pressure rating that identical finger herein identical identical with first paragraph reaction zone, due to the Pressure Drop of Flow of Goods and Materials, second segment reaction zone reaction pressure can a little less than first paragraph reaction zone), hydrogen to oil volume ratio is 200:1 ~ 3000:1, and volume space velocity is 0.3h
-1~ 6.0h
-1, average reaction temperature 180 DEG C ~ 465 DEG C; Preferred operational condition is hydrogen to oil volume ratio 300:1 ~ 2500:1, volume space velocity 0.4h
-1~ 4.0h
-1, average reaction temperature 200 DEG C ~ 445 DEG C.
In the inventive method step (c), the catalyst for hydro-upgrading of second segment reaction zone has isomery function, as containing beta-molecular sieve, and the components such as SAPO-11 molecular sieve, SAPO-41, NU-10 molecular sieve or ZSM-22 molecular sieve.The hydrogenation active metals component of catalyst for hydro-upgrading is generally 10% ~ 40% with the weight content of oxide basis.The massfraction of catalyst for hydro-upgrading Middle molecule sieve is generally 5% ~ 40%.Other component in catalyst for hydro-upgrading is generally the porous refractory oxide such as aluminum oxide, silicon oxide, amorphous aluminum silicide.The commercial catalysts that second segment reaction zone uses mainly contains, as FC-14, FC-16, FC-20 etc. that Fushun Petrochemical Research Institute (FRIPP) develops.
The hydrogenation catalyst of business hydrogenation catalyst or preparation is generally oxidation state, uses hydrogen 200 DEG C ~ 500 DEG C temperature before use, is reduced to reduction-state under preferably 220 DEG C ~ 450 DEG C conditions.Whenever forbid in system, inject sulfur-bearing, nitrogenous medium, avoid poisoning of catalyst.
Accompanying drawing explanation
Fig. 1 is the hydrogenation modification method principle flow chart that bio-oil of the present invention produces low condensation point automotive fuel.
Embodiment
Method of the present invention is specific as follows: with the mixing oil of one or more in bio-oil for stock oil, under hydroprocessing operations condition, stock oil and hydrogen are by comprising the first paragraph reaction zone of at least two kinds of hydrogenation catalysts, the hydrotreatment obtained generates logistics and is separated the gas circulation use obtained in high-pressure separator (abbreviation high score), also system can be gone out, the liquid fractionation obtained and hydrogen are mixed into the second Fan Duanying district comprising and have isomery performance catalyst for hydro-upgrading, obtain hydro-upgrading logistics and be separated the gas circulation use obtained in high-pressure separator (abbreviation high score), also system can be gone out, liquid fractionation obtains following products: gas, petroleum naphtha, one or more in low freezing point diesel fuel.The bio-oil that embodiment uses is commercially available prod, uses front filtering solid impurity.
Further illustrate particular case of the present invention below by embodiment, before formally reacting, catalyzer uses hydrogen reducing 10 hours at 380 DEG C.
The main composition of table 1 hydrogenation catalyst and character.
| Catalyzer | Catalyzer 1 | Catalyzer 2 | Catalyzer 3 | Catalyzer 4 | Modifying catalyst |
| Catalyzer forms | ? | ? | ? | ? | ? |
| MoO 3，wt% | 7.0 | 5.0 | 24.5 | 15.7 | 18.0 |
| NiO，wt% | 2.0 | ? | 3.8 | 2.4 | 2.5 |
| CoO，wt% | ? | 1.6 | ? | ? | ? |
| Beta-molecular sieve, wt% | ? | ? | ? | ? | 10.6 |
| Alumina supporter, wt% | Surplus | Surplus | Surplus | Surplus | Surplus |
| The main character of catalyzer | ? | ? | ? | ? | ? |
| Specific surface, m 2/g | >160 | >160 | >160 | >160 | >160 |
| Pore volume, ml/g | >0.30 | >0.30 | 0.33 | 0.32 | >0.34 |
Table 2 embodiment processing condition and test-results.
| First paragraph processing condition | Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 |
| Catalyzer | Catalyzer 1/ catalyzer 3 | Catalyzer 2/ catalyzer 3 | Catalyzer 2/ catalyzer 3 | Catalyzer 1/ catalyzer 4/ catalyzer 3 |
| Catalyst volume ratio | 10:90 | 20:80 | 40:60 | 25：35：40 |
| Stock oil | Soybean oil | Rapeseed oil | Oleum Gossypii semen | Oleum Gossypii semen |
| Reaction pressure, MPa | 17.0 | 5.0 | 10.0 | 10.0 |
| Entrance hydrogen to oil volume ratio | 2000:1 | 300:1 | 1000:1 | 1000:1 |
| Cumulative volume air speed, h -1 | 2.0 | 1.8 | 0.5 | 0.5 |
| Average reaction temperature, DEG C | 380 | 370 | 330 | 330 |
| Second segment processing condition | ? | ? | ? | ? |
| Catalyzer | Modifying catalyst | Modifying catalyst | Modifying catalyst | Modifying catalyst |
| Reaction pressure, MPa | 17.0 | 5.0 | 10.0 | 10.0 |
| Entrance hydrogen to oil volume ratio | 1500:1 | 500:1 | 800:1 | 1000:1 |
| Volume space velocity, h -1 | 2.0 | 4.5 | 1.5 | 3.0 |
| Average reaction temperature, DEG C | 320 | 350 | 310 | 280 |
| Diesel product | ? | ? | ? | ? |
| Density, g/cm 3 | 0.788 | 0.796 | 0.790 | 0.797 |
| Sulphur content, μ g/g | <5 | <5 | <5 | <5 |
| Condensation point, DEG C | -20 | -35 | -15 | -10 |
| Cetane value | >80 | >80 | >80 | >80 |
Table 3 embodiment processing condition and test-results.
| First paragraph processing condition | Embodiment 5 | Comparative example 1 | Comparative example 2 | Comparative example 3 |
| Catalyzer | Catalyzer 2/ catalyzer 3 | Catalyzer 3/ modifying catalyst | Catalyzer 3/ modifying catalyst | Catalyzer 3/ modifying catalyst |
| Catalyst volume ratio | 40:60 | ? | ? | ? |
| Stock oil | Oleum Gossypii semen | Oleum Gossypii semen | Oleum Gossypii semen | Oleum Gossypii semen |
| Reaction pressure, MPa | 10.0 | 10.0 | 10.0 | 10.0 |
| Entrance hydrogen to oil volume ratio | 1000:1 | 1000:1 | 1000:1 | 1000:1 |
| Cumulative volume air speed, h -1 | 0.6 | 0.48 | 0.48 | 0.48 |
| Average reaction temperature, DEG C | 330 | 330 | 330 | 330 |
| Second segment processing condition | ? | — | — | — |
| Catalyzer | Modifying catalyst | ? | ? | ? |
| Reaction pressure, MPa | 10.0 | ? | ? | ? |
| Entrance hydrogen to oil volume ratio | 1000:1 | ? | ? | ? |
| Cumulative volume air speed, h -1 | 2.4 | ? | ? | ? |
| Average reaction temperature, DEG C | 330 | ? | ? | ? |
| Runtime, h | 1000 | 200 | 300 | 500 |
| Pressure Drop, MPa | 0 | 0.1 | 0.3 | 0.6 |
| Diesel product | ? | ? | ? | ? |
| Density, g/cm 3 | 0.789 | 0.792 | 0.819 | 0.870 |
| Sulphur content, μ g/g | <5 | <5 | <5 | <5 |
| Condensation point, DEG C | -20 | -20 | 0 | 12 |
| Cetane value | >80 | >80 | 76 | 67 |
Comparative example catalyzer 3 consumption is identical with the total consumption of embodiment 5 catalyzer 2 and catalyzer 3, and comparative example modifying catalyst consumption is identical with embodiment 5 modifying catalyst consumption.As can be seen from embodiment, bio-oil can direct production low freezing point diesel fuel product by the method for hydrotreating of this technology, or fine-quality diesel oil blending component, and can realize long-period stable operation.
Claims (10)
1. bio-oil produces a hydrogenation modification method for low condensation point automotive fuel, it is characterized in that comprising following content:
A one or more in () bio-oil are stock oil;
B () is under Hydroprocessing conditions, stock oil and hydrogen are by first paragraph reaction zone, first paragraph reaction zone comprises the hydrogenation catalyst bed that at least two hydrogenation active component content raise successively, first stock oil and hydrogen pass through the low beds of hydrogenation active component content, then the high beds of hydrogenation active component content is passed through, under response behaviour, hydrogenation active component is the W of reduction-state, Mo, one or more in Ni and Co, in the beds that first reaction mass passes through, hydrogenation active component with the weight content of oxide basis for 3% ~ 10%, the hydrogenation active component of the downstream catalyst that reaction mass passes through increases by 3 ~ 25 percentage points in oxide weight than adjacent upstream catalyzer,
C () first paragraph reaction zone hydrogenation effluent is separated into gas phase and liquid phase, gas-phase dehydration process Posterior circle uses, the second segment reaction zone using catalyst for hydro-upgrading is entered after liquid phase mixes with circulation gas, under response behaviour, the active metal component of catalyst for hydro-upgrading is one or more in W, Mo, Ni and Co of reduction-state;
D gas phase that () second segment reaction zone generates logistics recycles, and liquid phase fractionation in separation column that second segment reaction zone generates logistics obtains petroleum naphtha and low freezing point diesel fuel.
2. in accordance with the method for claim 1, it is characterized in that: in step (a), the bio-oil of use comprises vegetables oil or animal grease.
3. in accordance with the method for claim 1, it is characterized in that: in step (b), the Hydroprocessing conditions of first paragraph reaction zone is reaction pressure is 3.0MPa ~ 20.0MPa, and hydrogen to oil volume ratio is 200:1 ~ 3000:1, and volume space velocity is 0.1h
-1~ 6.0h
-1, average reaction temperature is 180 DEG C ~ 465 DEG C.
4. in accordance with the method for claim 1, it is characterized in that: in step (b), the Hydroprocessing conditions of first paragraph reaction zone is reaction pressure is 4.0MPa ~ 18.0MPa, and hydrogen to oil volume ratio is 300:1 ~ 2500:1, and volume space velocity is 0.2h
-1~ 4.0h
-1, average reaction temperature is 200 DEG C ~ 445 DEG C.
5. according to the method described in claim 1,3 or 4, it is characterized in that: in step (b), first paragraph reaction zone beds arranges 2 ~ 5, and the hydrogenation catalyst that first reaction mass passes through accounts for 10% ~ 80% of all hydrogenation catalyst volumes in first paragraph reaction zone.
6. in accordance with the method for claim 5, it is characterized in that: in step (b) first paragraph reaction zone, the hydrogenation catalyst that first reaction mass passes through accounts for 20% ~ 70% of all hydrogenation catalyst volumes in first paragraph reaction zone; The hydrogenation active component of the downstream catalyst that reaction mass passes through increases by 5 ~ 20 percentage points in oxide weight than adjacent upstream catalyzer.
7. in accordance with the method for claim 1, it is characterized in that: in step (c), the reaction pressure of second segment reaction zone is 3.0MPa ~ 20.0MPa, and hydrogen to oil volume ratio is 200:1 ~ 3000:1, and volume space velocity is 0.3h
-1~ 6.0h
-1, average reaction temperature is 180 DEG C ~ 465 DEG C.
8. in accordance with the method for claim 1, it is characterized in that: in step (c), the reaction pressure of second segment reaction zone is 300:1 ~ 2500:1, and volume space velocity is 0.4h
-1~ 4.0h
-1, average reaction temperature is 200 DEG C ~ 445 DEG C.
9. according to the method described in claim 1 or 7, it is characterized in that: in step (c), the catalyst for hydro-upgrading of second segment reaction zone has isomery function, containing beta-molecular sieve, SAPO-11 molecular sieve, SAPO-41 molecular sieve, NU-10 molecular sieve or ZSM-22 molecular sieve in catalyst for hydro-upgrading.
10. in accordance with the method for claim 9, it is characterized in that: the hydrogenation active metals component of catalyst for hydro-upgrading with the weight content of oxide basis for 10% ~ 40%.
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| CN101321847A (en) * | 2005-11-30 | 2008-12-10 | 新日本石油株式会社 | Hydrorefining process and hydrorefined oil |
| CN101617029A (en) * | 2007-02-20 | 2009-12-30 | 国际壳牌研究有限公司 | Produce the method for paraffinic hydrocarbons |
| CN102041023A (en) * | 2009-10-16 | 2011-05-04 | 中国石油化工股份有限公司 | Method for improving residual oil hydrogenation by blending biological grease |
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| BRPI0500591A (en) * | 2005-02-18 | 2006-10-03 | Petroleo Brasileiro Sa | process for hydroconversion of vegetable oils |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101321847A (en) * | 2005-11-30 | 2008-12-10 | 新日本石油株式会社 | Hydrorefining process and hydrorefined oil |
| CN101617029A (en) * | 2007-02-20 | 2009-12-30 | 国际壳牌研究有限公司 | Produce the method for paraffinic hydrocarbons |
| CN102041023A (en) * | 2009-10-16 | 2011-05-04 | 中国石油化工股份有限公司 | Method for improving residual oil hydrogenation by blending biological grease |
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