CN103102912B - Two-stage hydrogenation method for producing high quality low freezing point motor fuel - Google Patents
Two-stage hydrogenation method for producing high quality low freezing point motor fuel Download PDFInfo
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- CN103102912B CN103102912B CN201110353718.5A CN201110353718A CN103102912B CN 103102912 B CN103102912 B CN 103102912B CN 201110353718 A CN201110353718 A CN 201110353718A CN 103102912 B CN103102912 B CN 103102912B
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- 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 present invention relates to a two-stage hydrogenation method for producing a high quality low freezing point motor fuel. The method is characterized in that a biological oil is adopted as a raw material oil; under a hydrogenation condition, the raw material oil and hydrogen are mixed, and pass through a first stage hydrogenation reaction zone; the stream generated from hydrogenation is separated to obtain hydrogen-rich gas; the hydrogen-rich gas is recycled at the first stage; the separated liquid enters a second stage hydrogenation modification reaction zone; the sub-hydrogen gas separated from the oil generated through second stage hydrogenation is recycled at the second stage; and the separated liquid product is subjected to fractionation to obtain naphtha and a low freezing point diesel oil, wherein hydrogenation activity components of the hydrogenation catalyst used at the first stage are one or a plurality of materials selected from sulfurization state W, Mo, Ni and Co and hydrogenation activity components of the hydrogenation catalyst used at the second stage are reduction state Pt and/or Pd under a reaction state. Compared to the method in the prior art, the two-stage hydrogenation method of the present invention has the following characteristics that: the low freezing point motor fuel can be produced, activity stability of the catalyst can be ensured, and stable and long period device operation can be ensured.
Description
Technical field
The present invention relates to a kind of method of hydrotreating, particularly a kind of is stock oil with bio-oil, the two-stage method method of hydrotreating of direct production high-grade low-freezing point automotive fuel.
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) utilizing transesterify has been 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 bed carbon distribution 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 (the sulphided state hydrogenation catalyst of grating), second segment hydro-upgrading (noble metal hydrogenation catalyst), 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 a kind of two-stage method method of hydrotreating producing high-grade low-freezing point automotive fuel, independent is stock oil with bio-oil, first paragraph uses the sulphided state hydrogenation catalyst of grating, second segment uses noble metal hydrogenation modifying catalyst, 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.
A kind of two-stage method method of hydrotreating producing high-grade low-freezing point automotive fuel of the present invention 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 sulphided state;
C () first paragraph reaction zone hydrogenation effluent is separated into gas phase and liquid phase, recycle in first paragraph reaction zone after gas-phase dehydration process, 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 Pt and/or Pd of reduction-state;
D the gas phase of () second segment reaction zone resultant stream gas-liquid separation recycles at second segment, liquid phase fractionation in separation column of second segment reaction zone resultant stream gas-liquid separation obtains petroleum naphtha and low freezing point diesel fuel;
E () supplements S-contained substance in first paragraph reaction mass, to maintain hydrogen sulfide content in circulation gas.
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 3.0MPa ~ 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), first paragraph reaction zone 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.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 paragraph 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, hydrogenation catalyst such as ICR 179 grade, 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 (b), first paragraph reaction zone hydrogenation active component is the catalyzer of oxidation state, carries out conventional sulfidizing before the use, makes hydrogenation active component be converted into sulphided state, or use the catalyzer that ex situ presulfiding is good.
In the inventive method step (c), the Hydroprocessing conditions of second segment 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 0.3h
-1~ 6.0h
-1, average reaction temperature 180 DEG C ~ 465 DEG C; Preferred operational condition is reaction pressure 3.0MPa ~ 18.0MPa, 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.First paragraph reaction zone hydrogenation effluent does not need cooling to carry out gas-liquid separation, and the water that reaction generates enters in gas phase.The liquid phase entering second segment reaction zone can be the liquid phase material after the gas-liquid separation of first paragraph reaction zone, also can be the diesel oil distillate that the liquid phase material after the gas-liquid separation of first paragraph reaction zone obtains through separation column fractionation.The working pressure of second segment reaction zone can be identical with first paragraph, also can be different.
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.Catalyst for hydro-upgrading is in the element quality of precious metals pt and/or Pd, and the content of noble metal hydrogenation active ingredient is 0.01% ~ 1.5%.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.
In the inventive method step (c), catalyzer uses hydrogen 200 DEG C ~ 500 DEG C temperature before use, reduces under preferably 220 DEG C ~ 450 DEG C conditions.Whenever forbid in second segment reactive system, inject sulfur-bearing, nitrogenous medium, avoid poisoning of catalyst.
The sulfur-containing medium supplemented in reaction mass (optimum is dosed in the liquid phase feeding of first paragraph reaction zone) in the inventive method step (e) can be the compound of sulfur-bearing, as DMDS, CS
2deng, also can be the oil light-end products of sulfur-bearing, as the boat coal etc. of sulfur-bearing.Supplementing by sulphur, can ensure that the hydrogen sulfide content in the circulation gas of first paragraph reaction zone is not less than 0.005v%, preferred 0.01v% ~ 2.0v%.
Accompanying drawing explanation
Fig. 1 is the two-stage method method of hydrotreating principle flow chart that the present invention produces high-grade low-freezing point automotive fuel.
Fig. 2 is the another one principle flow chart that the present invention produces the two-stage method method of hydrotreating of high-grade low-freezing 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 conditions, stock oil and hydrogen are by comprising the first paragraph hydroconversion reaction zone of at least two kinds of hydrogenation catalysts, the hydrogenated oil obtained is separated in high-pressure separator (abbreviation high score) gas obtained and recycles in first paragraph reaction zone, the liquid distillate obtained and hydrogen are mixed into the second segment reaction zone comprising and have isomery performance noble metal hydrogenation modifying catalyst, obtain hydro-upgrading logistics to be separated in high-pressure separator (abbreviation high score) gas obtained and to recycle at second segment, the liquid fractionation obtained obtains following products: gas, petroleum naphtha, one or more in diesel oil, if improve the character of diesel product further or extend the cycle of operation, also consider, at first paragraph, a part of diesel oil and unconverted oil are looped back first paragraph reaction zone.The bio-oil that embodiment uses is commercially available prod, uses front filtering solid impurity.
Particular case of the present invention is further illustrated below by embodiment.
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% | 4.0 | 9.0 | 24.0 | 16.2 | |
| NiO，wt% | 1.5 | 3.5 | 2.5 | ||
| CoO，wt% | 2.6 | ||||
| Pt，wt% | 1.20 | ||||
| Pd，wt% | 0.15 | ||||
| Beta-molecular sieve, wt% | 15.5 | ||||
| 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 reaction zone processing condition | Embodiment 1 | Embodiment 2 | Embodiment 3 |
| Catalyzer | Catalyzer 1/ catalyzer 2 | Catalyzer 1/ catalyzer 3 | Catalyzer 1/ catalyzer 2/ catalyzer 4 |
| Catalyst volume ratio | 20:80 | 40:60 | 20:30:50 |
| Stock oil | Oleum Gossypii semen | Soybean oil | Coconut oil |
| Reaction pressure, MPa | 16.0 | 6.0 | 4.0 |
| Entrance hydrogen to oil volume ratio | 1000:1 | 1000:1 | 1000:1 |
| Cumulative volume air speed, h -1 | 2.0 | 0.8 | 0.5 |
| Average reaction temperature, DEG C | 360 | 320 | 300 |
| Sulfur-containing medium | DMDS | DMDS | CS 2 |
| Hydrogen sulfide content in first paragraph circulation gas, μ L/L | 100 | 2000 | 8000 |
| Second segment reaction zone processing condition | |||
| Catalyzer | Modifying catalyst | Modifying catalyst | Modifying catalyst |
| Reaction pressure, MPa | 16.0 | 12.0 | 4.0 |
| Entrance hydrogen to oil volume ratio | 1500:1 | 500:1 | 800:1 |
| Volume space velocity, h -1 | 1.5 | 3.0 | 4.0 |
| Average reaction temperature, DEG C | 260 | 280 | 310 |
| Diesel product | |||
| Density, g/cm 3 | 0.781 | 0.780 | 0.779 |
| Sulphur content, μ g/g | <1 | <1 | <1 |
| Condensation point, DEG C | -10 | -18 | -35 |
| Cetane value | >80 | >80 | >80 |
Table 3 embodiment processing condition and test-results.
| First paragraph reaction zone processing condition | Embodiment 4 | Comparative example 1 | Comparative example 2 | Comparative example 3 |
| Catalyzer | Catalyzer 1/ catalyzer 4 | Catalyzer 4 | Catalyzer 4 | Catalyzer 4 |
| Catalyst volume ratio | 40:60 | |||
| Stock oil | Rapeseed oil | Rapeseed oil | Rapeseed oil | Rapeseed oil |
| Reaction pressure, MPa | 12.0 | 12.0 | 12.0 | 12.0 |
| Entrance hydrogen to oil volume ratio | 1000:1 | 1000:1 | 1000:1 | 1000:1 |
| Cumulative volume air speed, h -1 | 0.5 | 0.5 | 0.5 | 0.5 |
| Average reaction temperature, DEG C | 320 | 320 | 320 | 330 |
| Sulfur-containing medium | DMDS | DMDS | DMDS | DMDS |
| Hydrogen sulfide content in first paragraph circulation gas, μ L/L | 200 | 200 | 200 | 200 |
| Second segment reaction zone processing condition | ||||
| Catalyzer | Modifying catalyst | Modifying catalyst | Modifying catalyst | Modifying catalyst |
| 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 |
| Volume space velocity, h -1 | 2.0 | 2.0 | 2.0 | 2.0 |
| Average reaction temperature, DEG C | 280 | 280 | 280 | 280 |
| Runtime, h | 1000 | 100 | 300 | 600 |
| Pressure Drop, MPa | 0 | 0.1 | 0.3 | 0.6 |
| Diesel product | ||||
| Density, g/cm 3 | 0.781 | 0.781 | 0.812 | 0.870 |
| Sulphur content, μ g/g | <5 | <5 | <5 | <5 |
| Condensation point, DEG C | -25 | -25 | 0 | 16 |
| Cetane value | >80 | >80 | 75 | 61 |
As can be seen from embodiment, bio-oil can direct production high-grade low-freezing point diesel product by the method for hydrotreating of this technology, or fine-quality diesel oil blending component, and can realize long-period stable operation.
Claims (11)
1. produce a two-stage method method of hydrotreating for high-grade low-freezing 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 sulphided state, Mo, in Ni and Co one or more, 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, follow after gas-phase dehydration process in first paragraph reaction zone
Ring uses, and enter the second segment reaction zone using catalyst for hydro-upgrading after liquid phase mixes with circulation gas, under response behaviour, the active metal component of catalyst for hydro-upgrading is Pt and/or Pd of reduction-state;
D the gas phase of () second segment reaction zone resultant stream gas-liquid separation recycles at second segment, second segment reaction zone resultant
Liquid phase fractionation in separation column of stream gas-liquid separation obtains petroleum naphtha and low freezing point diesel fuel;
E () supplements S-contained substance in first paragraph reaction mass, to maintain hydrogen sulfide content in circulation gas.
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 reaction pressure of first paragraph reaction zone 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 180 DEG C ~ 465 DEG C.
4. in accordance with the method for claim 1, it is characterized in that: in step (b), the reaction pressure 3.0MPa ~ 18.0MPa of first paragraph reaction zone, 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.
5. according to the method described in claim 1 or 3, it is characterized in that: in step (b), first paragraph reaction zone beds arranges 2 ~ 5, and the hydrogenation catalyst bed 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, and 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
For 3.0MPa ~ 20.0MPa, 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℃~465℃。
8. in accordance with the method for claim 7, it is characterized in that: in step (c), the reaction pressure of second segment reaction zone is 3.0MPa ~ 18.0MPa, and hydrogen to oil volume ratio 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. in accordance with the method for claim 1, it is characterized in that: in step (c), the catalyst for hydro-upgrading of second segment reaction zone has isomery function, catalyst for hydro-upgrading contains beta-molecular sieve, SAPO-11 molecular sieve, SAPO-41, NU-10 molecular sieve or ZSM-22 molecular sieve component, catalyst for hydro-upgrading is in the element quality of precious metals pt and/or Pd, and the content of noble metal hydrogenation active ingredient is 0.01% ~ 1.5%.
10. in accordance with the method for claim 1, it is characterized in that: the sulfur-containing medium supplemented in the reaction mass of first paragraph reaction zone is the compound of sulfur-bearing, or the oil light-end products of sulfur-bearing.
11., according to the method described in claim 1 or 10, is characterized in that: in the circulation gas of first paragraph reaction zone, hydrogen sulfide content is not less than 0.005v%.
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