CN103773456A - Animal and vegetable oil-catalytic diesel oil combined hydrogenation method - Google Patents
Animal and vegetable oil-catalytic diesel oil combined hydrogenation method Download PDFInfo
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Abstract
The invention discloses an animal and vegetable oil-catalytic diesel oil combined hydrogenation method. The animal and vegetable oil-catalytic diesel oil combined hydrogenation method comprises following steps: animal and vegetable oil is mixed with hydrogen, and an obtained mixture is delivered into a hydrogenation heterogeneous reactor for hydrofinishing and heterogeneous condensation point reducing reaction; an obtained reaction effluent is subjected to hot high pressure separating so as to obtain a gas phase material and a liquid phase material via separation; the liquid phase material is mixed with catalytically cracked diesel oil and recycled hydrofined diesel oil, and an obtained mixed material is delivered into a hydrogen mixing tank for hydrogen mixing, and then is delivered into a liquid hydrogenation reactor for hydrofinishing. After heterogeneous condensation point reducing reaction of the animal and vegetable oil, on the one hand, hydrogen dissolving amount of the liquid phase hydrogenation reactor is increased, and on the other hand, condensation point of the animal and vegetable oil is reduced, the animal and vegetable oil is high in cetane value, and a problem that catalytic diesel oil cetane value is too low can be solved via combined hydrogenation with catalytic diesel oil. The animal and vegetable oil-catalytic diesel oil combined hydrogenation method is capable of widening raw material sources for refinery diesel oil production, and also providing a method for processing of low-quality catalytic diesel oil.
Description
Technical field
The present invention relates to a kind of vegetable and animals oils and catalytic diesel oil combined hydrogenation method, a kind of gas phase circulation hydrogenation and liquid phase circulation hydrogenation machinery processing vegetable and animals oils and catalytic diesel oil specifically, the hydrogenation process of production high hexadecane value clean diesel.
Background technology
Along with petering out of petroleum resources, the ratio of refinery's processing heavy and crude oil with poor quality increases year by year, therefore, in refinery's work flow secondary processing diesel oil especially the ratio of catalytic diesel oil strengthen gradually, and under normal circumstances, in catalytic diesel oil, contain a large amount of aromatic hydrocarbons, cetane value is very low, even by also meeting very slowly the requirement of diesel oil to cetane value after hydrofining.Meanwhile, along with world oil reserves are fewer and feweri, the utilization of animals and plants wet goods renewable resources also more and more comes into one's own.The main component of animal-plant oil is straight chain fatty acid tri-glyceride, and wherein fatty acid chain length is generally C
12～C
24, and with C
16and C
18in the majority.The typical lipid acid that animal-plant oil contains comprises saturated acid (palmitinic acid, stearic acid), monobasic unsaturated acid (oleic acid) and polyunsaturated polycarboxylic acid (linolic acid, linolenic acid), vegetables oil is take unsaturated monoenoic acid and diolefinic acid as main, and Tallow, beef is take saturated fatty acid as main.This part oil generates in oil and is mainly straight-chain paraffin after hydrogenation, and therefore, condensation point is higher, can not meet the requirement of condensation point of diesel oil, but cetane value is very high.Therefore, vegetable and animals oils and catalytic diesel oil mixing oil can improve diesel-fuel cetane number significantly.
In addition, along with refinery is more and more stricter to the control of cost, lowly more and more be subject to the attention of refinery as the liquid phase circulation hydrogen addition technology of distinguishing feature to invest, so-called liquid phase circulation hydrogen addition technology is than conventional gas-phase circulation hydrogenation technique, liquid phase circulation hydrogenation technique reactive moieties does not arrange hydrogen gas circulating system, and relying on a large amount of circulation times of liquid-phase product to carry into the dissolved hydrogen of reactive system provides fresh feed to carry out the needed hydrogen of hydrogenation reaction.Therefore, the key of liquid phase circulation hydrogen addition technology is to react the satisfied reaction of oil product dissolved hydrogen tolerance and needs hydrogen amount.And catalytic diesel oil is owing to containing higher aromaticity content, reaction hydrogen-consuming volume is very high, and meanwhile, than alkane, the meltage of hydrogen in aromatic hydrocarbons is lower.Therefore,, at traditional liquid phase circulation hydrogenation process, be difficult to be directly used in processing catalytic cracking diesel oil.
Summary of the invention
For the features of vegetable and animals oils and catalytic diesel oil, the invention provides the hydrogenation process of a kind of gas phase circulation hydrogenation and liquid phase circulation hydrogenation machinery processing vegetable oil and catalytic diesel oil production high hexadecane value clean diesel.
A kind of vegetable and animals oils of the present invention and catalytic diesel oil combined hydrogenation method, comprise following content:
(1) vegetable and animals oils enters hydroisomerization reactor after mixing with hydrogen, carries out hydrofining and isomerization-visbreaking reaction;
(2) reaction effluent that step (1) obtains enters high pressure hot separator and carries out gas-liquid separation, obtains gas phase and liquid phase;
(3) hydrofining diesel oil of the hot high score liquid phase part that step (2) obtains and catalytic cracking diesel oil and circulation mixes, and enters and mix hydrogen tank and mix after hydrogen, enters and in liquid phase hydrogenation reactor, carries out hydrofining reaction;
(4) step (3) obtains hydrogenation reaction effluent part bleeder after reducing valve decompression, obtains high hexadecane value clean diesel, and the mixed hydrogen tank that another part loops back step (3) mixes hydrogen.
According to vegetable and animals oils of the present invention, catalytic diesel oil combined hydrogenation method method, wherein can also comprise step (5), the gas phase part that step (2) obtains is further isolated after hydrogen, returns to step (1) and recycle after compressor compression.
According to vegetable and animals oils of the present invention, catalytic diesel oil combined hydrogenation method method, wherein the vegetable and animals oils (bio-oil) described in step (1) is selected from one or more in vegetables oil, animal oil, vegetable tallow and Tallow, beef.Can be specifically one or more in the animal-plant oil stock oil cuts such as soybean oil, Trisun Oil R 80, rapeseed oil, plam oil, sweet oil, oleum lini, Oleum Gossypii semen, Viscotrol C, fish oil, butter.The carbonatoms of described vegetable and animals oils is generally 12～24.
In catalytic cracking diesel oil described in step (2), aromaticity content is generally 40 quality %～95 quality %, is preferably 50 quality %～70 quality %.
In step (3), described hot high score liquid phase part take vegetable and animals oils raw material with the mass ratio of fresh catalytic cracking diesel oil as 1: 6～6: 1, preferably 1: 2～4: 1.
In vegetable and animals oils of the present invention and catalytic cracking diesel oil combined hydrogenation method, the operational condition of the vegetable and animals oils hydroisomerization reactor in step (1) is as follows: 300 ℃～420 ℃ of temperature of reaction, preferably 340 ℃～400 ℃; Reaction pressure 4.0 MPa～18.0 MPa, preferably 6.0 MPa～15.0MPa; Volume space velocity 0.2h when liquid
-1～5h
-1, preferably 0.5h
-1～3.0h
-1; Hydrogen to oil volume ratio 100: 1～1000: 1, preferably 200: 1～500: 1.
In isomerizing reactor described in step (1), be filled with Hydrobon catalyst and Hydrodewaxing catalyst, the volume ratio of Hydrobon catalyst and Hydrodewaxing catalyst is generally 1:5～2:1, is preferably 1:3～1:1.Described Hydrobon catalyst is generally the conventional diesel oil hydrofining catalyst in this area, and wherein, Hydrobon catalyst is generally take VI B family and/or group VIII metal as active ingredient, take aluminum oxide or silicon-containing alumina as carrier.Group VIB metal is generally Mo and/or W, and group VIII metal is generally Co and/or Ni.Take the weight of catalyzer as benchmark, group VIB metal content is counted 8wt% ~ 28wt% with oxide compound, and group VIII metal content is counted 2wt% ~ 15wt% with oxide compound.The catalyzer that isomerization-visbreaking catalyzer adopts is the heterogeneous catalyst that contains beta molecular sieve, and catalyzer contains WO by weight
315 ~ 30%, NiO or CoO 2 ~ 15%, beta molecular sieve 5 ~ 45%.Carrier is aluminum oxide or amorphous aluminum silicide.
Hydroisomerization reactor comprises at least two beds, and Hydrobon catalyst and hydro-upgrading pour point depression catalyzer can fill in respectively top bed and the bottom bed of reactor; Or employing grading loading, the top filling Hydrobon catalyst of each bed, bottom filling hydroisomerizing pour point depression catalyzer, preferably adopts this grading loading method; Also can selective finishing agent and pour point depressant mixed packing mode according to feedstock property, be the equal mixed packing finishing agent of upper bed layer and lower bed layer catalyzer and pour point depressant, according to identical or different ratio, catalyst for refining and isomerization-visbreaking catalyst mix filled in respectively to upper bed layer and lower bed layer.
Hydroisomerization reactor of the present invention is selected the Hydrobon catalyst that hydrofining ability is stronger and the isomerization-visbreaking catalyzer with strong hydrogenation isomery function, adopt once by technical process, under medium-pressure or high pressure condition, vegetable and animals oils is carried out to hydrotreatment, in realizing degree of depth deoxidation, desulfurization and denitrogenation, can make the contour condensation point component of normal paraffin in vegetable and animals oils carry out isomerization reaction, thereby reduce its condensation point.
In vegetable and animals oils of the present invention and catalytic diesel oil combined hydrogenation method, in step (3), the operational condition of liquid phase circulation hydrogenator is as follows: 300 ℃～400 ℃ of temperature of reaction, preferably 320 ℃～380 ℃; Reaction pressure 4.0 MPa～15.0 MPa, preferably 6.0 MPa～10.0MPa; Volume space velocity 1.0h when liquid
-1～5h
-1, preferably 1.5h
-1～3.0h
-1, liquid phase circulation is 1:5～5:1 than (being treated oil/fresh catalytic diesel oil charging mass ratio), preferential 1:2～3:1.
In liquid phase hydrogenation reactor in step (3), be filled with Hydrobon catalyst, this catalyzer can be commercially available prod, also can be by the conventional knowledge preparation in this area.Hydrobon catalyst described in step (3) is generally take VI family and/or group VIII metal as active ingredient, take aluminum oxide or silicon-containing alumina as carrier.Group VIB metal is generally Mo and/or W, and group VIII metal is generally Co and/or Ni.Take the weight of catalyzer as benchmark, group VIB metal content is counted 8wt% ~ 28wt% with oxide compound, group VIII metal content is counted 2wt% ~ 15wt% with oxide compound, this catalyzer has stronger hydrogenation saturability and ultra-deep desulfurization ability, completes deep desulfuration and the part aromatic saturation of catalytic diesel oil in liquid phase hydrogenation reactor.
Compared with prior art, vegetable and animals oils of the present invention and catalytic diesel oil combined hydrogenation method have following characteristics:
1, vegetable and animals oils is first through hydrofining, then the main component of gained liquid-phase product is paraffinic hydrocarbons after hydroisomerizing pour point depression, than having higher hydrogen solubility take aromatic hydrocarbons as main catalytic cracking diesel oil.At the normal heptane of research to same molecular amount with toluene during in the solubleness to hydrogen, discovery hydrogen in the solubleness of normal heptane close to two times in toluene.Therefore, the vegetable and animals oils after hydro-isomerization pour point depression and catalytic diesel oil are mixed into liquid phase circulation hydrogenation unit and can improve the molten hydrogen amount of mixing oil.And, this part substantially no longer consumes hydrogen through the reacted vegetable and animals oils of isomerization-visbreaking in liquid phase hydrogenation reactor, just merely for urging bavin hydrofining reaction that dissolved hydrogen is provided, solve catalytic diesel oil dissolved hydrogen and can not meet the problem of hydrogenation reaction needs.
2, in the hot high score oil in hydroisomerizing pour point depression unit, be dissolved with a large amount of unreacting hydrogens, be equivalent to this part oil and fulfiled mixed hydrogen process ahead of schedule, this part hot high score oil directly and catalytic cracking diesel oil be mixed into hydrogen tank, can reduce the mixed hydrogen amount that saturated mixed hydrogen needs, improve mixed hydrogen effect, thereby be conducive to the carrying out of hydrofining reaction in liquid phase hydrogenation reactor.
3, the vegetable and animals oils after hydroisomerizing pour point depression has higher cetane value and suitable condensation point, can make up the problem of catalytic diesel oil cetane value deficiency by combining processing with catalytic diesel oil.Therefore, this technique had both been widened raw material sources for refinery's diesel production, meanwhile, provided outlet again to the processing and utilization of catalytic diesel oil inferior.
Accompanying drawing explanation
Fig. 1 is the principle process schematic diagram of vegetable and animals oils of the present invention and catalytic diesel oil combined hydrogenation method.
Embodiment
Below by specific embodiment, vegetable and animals oils of the present invention and catalytic diesel oil combined hydrogenation method are described in detail.
As shown in Figure 1, vegetable and animals oils enters isomerization-visbreaking reactor 3 after being mixed with the circulation gas of introducing through pipeline 2 by pipeline 1 and carries out hydroisomerizing reaction, reaction effluent enters hot high score 4 and carries out gas, liquid is separated into gas, liquid two-phase, gas phase is gone downstream separation system further to isolate the laggard circulating hydrogen compressor of hydrogen through pipeline 13 and is looped back isomerizing reactor entrance, liquid phase part is mixed into hydrogen tank 7 through pipeline 5 and the bavin of urging of introducing through pipeline 6, mix molten hydrogen at mixed hydrogen in-tank mixing oil with the hydrogen of introducing through pipeline 8, residual hydrogen is discharged through pipeline 9, saturated molten hydrogen mixing oil enters liquid phase hydrogenation reactor 10 and carries out hydrodesulfurization reaction, a liquid phase hydrogenation reactor effluent part continues mixed hydrogen through pipeline 11 and pipeline 5 circulation back-mixing hydrogen tanks 7, another part obtains high hexadecane value clean diesel product through pipeline 12 bleeders.
Below by specific embodiment and comparative example, further illustrate technical scheme of the present invention and effect.
Embodiment 1 ~ 3 adopts flow process shown in Fig. 1.In embodiment 1 ~ 3, isomerization-visbreaking catalyzer used and Hydrobon catalyst are commercial catalyst, and its physico-chemical property is listed in table 2.Feedstock property used is in table 1, and embodiment 1 ~ 3 and comparative example processing condition used are listed in table 3.The evaluation result of embodiment 1 ~ 3 and comparative example is in table 4.
Comparative example adopts conventional liquid-phase hydrogenatin flow process, processes separately catalytic diesel oil raw material, and selected catalytic diesel oil is identical with embodiment with liquid phase hydrogenation reactor catalyzer.
Table 1 stock oil character.
| Project | Catalytic diesel oil | Soybean oil |
| Density (20 ℃), g/cm 3 | 0.9028 | 0.8821 |
| Boiling range, ℃ | 165~362 | 200~340 |
| Sulphur content, μ g/g | 6800 | 120 |
| Nitrogen content, μ g/g | 350 | 3 |
| Aromaticity content, wt % | 60 | 0 |
| Cetane value | 21 | 78 |
| Cold filter clogging temperature, ℃ | -20 | 17 |
| Condensation point, ℃ | -17 | 14 |
Table 2 catalyst property.
| Project | Hydrobon catalyst | Isomerization-visbreaking catalyzer | Hydrobon catalyst |
| Chemical constitution, quality % | ? | ? | ? |
| MoO 3 | 9 | — | 24 |
| NiO | 5 | 6 | 4 |
| CoO | — | — | — |
| WO 3 | 18 | 25 | — |
| Beta molecular sieve | — | 12 | — |
| Carrier | Silicon-containing alumina | Aluminum oxide | Silicon-containing alumina |
Table 3 operational condition.
| ? | Embodiment 1 | Embodiment 2 | |
Comparative example |
| Isomerization-visbreaking condition | ? | ? | ? | ? |
| Temperature of reaction, ℃ | 370 | 375 | 390 | — |
| Reaction pressure, MPa | 10.0 | 9.0 | 9.0 | — |
| Volume space velocity, h -1 | 1.0 | 1.5 | 1.0 | — |
| Hydrogen to oil volume ratio * | 700 | 800 | 800 | — |
| Liquid-phase hydrogenatin condition | ? | ? | ? | ? |
| Temperature of reaction, ℃ | 350 | 360 | 350 | 360 |
| Reaction pressure, MPa | 9.0 | 8.0 | 8.0 | 8.0 |
| Volume space velocity, h -1 | 1.5 | 1.5 | 1.0 | 1.0 |
| Recycle ratio * | 2：1 | 1：1 | 2：1 | 3：1 |
| Urge bavin/soybean oil ratio | 1：1 | 1：2 | 1：1 | — |
* recycle ratio is the liquid phase of circulation and the volume ratio of catalytic diesel oil charging.
The test-results of table 4 embodiment 1 ~ 3 and comparative example.
| ? | Embodiment 1 | Embodiment 2 | |
Comparative example |
| Sulphur content, μ g/g | 25 | 8 | 18 | 320 |
| Cetane value | 51 | 55 | 52 | 23 |
| Cold filter clogging temperature, ℃ | -16 | -15 | -15 | -21 |
| Condensation point, ℃ | -13 | -12 | -13 | -17 |
Can find with the comparative test result of comparative example by embodiment 1～3: vegetable and animals oils of the present invention with urge the embodiment 1 of bavin combined hydrogenation method and embodiment 3 product sulphur contents to be respectively 25 μ g/g and 18 μ g/g, cetane value reaches respectively 51 and 52 and meets state's IV diesel oil standard.Embodiment 2 product sulphur content products obtained therefrom sulphur content 8 μ g/g, cetane value 55 meets state's V clean diesel standard, and the indexs such as while cold filter point of diesel oil, condensation point all meet the requirements.And comparative example adopts identical processing condition with embodiment 2 diesel oil, product sulphur content and cetane value are respectively 320 μ g/g and 23, even the diluting effect of hydroisomerizing vegetables oil in deduction embodiment, merely from liquid phase hydrogenation reactor reaction effect, comparative example separately processing is pure while urging bavin reaction effect is obviously not as embodiment 2, this may be because sneaking into of isomery vegetables oil in embodiment improved the molten hydrogen amount of liquid phase, make to urge bavin amounts of hydrogen in liquid phase hydrogenation reactor reaction process more sufficient, improve liquid phase hydrogenation reactor reaction environment, thereby be conducive to desulfurization, de-arylation reaction carries out.
Claims (10)
1. vegetable and animals oils, a catalytic diesel oil combined hydrogenation method, comprises following content:
(1) vegetable and animals oils enters hydroisomerization reactor after mixing with hydrogen, carries out hydrofining and isomerization-visbreaking reaction;
(2) reaction effluent that step (1) obtains enters high pressure hot separator and carries out gas-liquid separation, obtains gas phase and liquid phase;
(3) hydrofining diesel oil of the hot high score liquid phase part that step (2) obtains and catalytic cracking diesel oil and circulation mixes, and enters and mix hydrogen tank and mix after hydrogen, enters and in liquid phase hydrogenation reactor, carries out hydrofining reaction;
(4) step (3) obtains hydrogenation reaction effluent part bleeder after reducing valve decompression, obtains high hexadecane value clean diesel, and the mixed hydrogen tank that another part loops back step (3) mixes hydrogen.
2. in accordance with the method for claim 1, it is characterized in that, the carbonatoms of the vegetable and animals oils described in step (1) is 12～24.
3. according to the method described in claim 1 or 2, it is characterized in that, the described vegetable and animals oils of step (1) is selected from one or more in soybean oil, Trisun Oil R 80, rapeseed oil, plam oil, sweet oil, oleum lini, Oleum Gossypii semen, Viscotrol C, fish oil and butter.
4. in accordance with the method for claim 1, it is characterized in that, in the catalytic cracking diesel oil described in step (2), aromaticity content is 40 quality %～95 quality %.
5. in accordance with the method for claim 1, it is characterized in that, the hot high score liquid phase described in step (3) take vegetable and animals oils raw material with the mass ratio of fresh catalytic cracking diesel oil as 1:6～6:1.
6. in accordance with the method for claim 1, it is characterized in that, described in step (1), the operational condition of hydroisomerization reactor is: 300 ℃～420 ℃ of temperature of reaction, reaction pressure 4.0 MPa～18.0 MPa, volume space velocity 0.2h when liquid
-1～5h
-1, hydrogen to oil volume ratio 100: 1～1000: 1.
7. in accordance with the method for claim 1, it is characterized in that, the operational condition of the liquid phase hydrogenation reactor described in step (3) is, 300 ℃～400 ℃ of temperature of reaction, reaction pressure 4.0 MPa～15.0 MPa, volume space velocity 1.0h when liquid
-1～5h
-1, liquid phase circulation is than being 1:5～5:1.
8. in accordance with the method for claim 1, it is characterized in that, in hydroisomerization reactor described in step (1), be filled with Hydrobon catalyst and isomerization-visbreaking catalyzer, the volume ratio of Hydrobon catalyst and isomerization-visbreaking catalyzer is generally 1:5～2:1.
9. in accordance with the method for claim 7, it is characterized in that, described Hydrobon catalyst is take VI B family and/or group VIII metal as active ingredient, take aluminum oxide or silicon-containing alumina as carrier, take the weight of catalyzer as benchmark, group VIB metal content is counted 8wt% ~ 28wt% with oxide compound, and group VIII metal content is counted 2wt% ~ 15wt% with oxide compound.
10. in accordance with the method for claim 7, it is characterized in that, described isomerization-visbreaking catalyzer is the heterogeneous catalyst that contains beta molecular sieve, and catalyzer contains WO by weight
315 ~ 30%, NiO or CoO 2 ~ 15% and beta molecular sieve 5 ~ 45%, carrier is aluminum oxide or amorphous aluminum silicide.
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| WO2017101274A1 (en) * | 2015-12-18 | 2017-06-22 | 中国石油天然气股份有限公司 | Liquid-phase hydroisomerization system and process therefor and use thereof |
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