CN103773459B - A kind of vegetable and animals oils and catalytic diesel oil Unionfining technique - Google Patents
A kind of vegetable and animals oils and catalytic diesel oil Unionfining technique Download PDFInfo
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- CN103773459B CN103773459B CN201210408384.1A CN201210408384A CN103773459B CN 103773459 B CN103773459 B CN 103773459B CN 201210408384 A CN201210408384 A CN 201210408384A CN 103773459 B CN103773459 B CN 103773459B
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Abstract
The invention discloses a kind of vegetable and animals oils and catalytic diesel oil combined hydrogenation method.The method comprises following content: enter hydroisomerization reactor after vegetable and animals oils mixes with hydrogen, carries out hydrofining and isomerization-visbreaking reaction; Gained reaction effluent enters the high branch of heat and is separated, after hot high score liquid phase mixes with catalytic cracking diesel oil, enter mixed hydrogen tank and carry out mixed hydrogen, then enter in liquid phase hydrogenation reactor and carry out hydrofining reaction, a part for gained hydrofining diesel oil is circulated to the lower catalyst bed layer of hydroisomerization reactor.Vegetable and animals oils, after hydroisomerizing pour point depression, can improve the molten hydrogen amount of liquid phase hydrogenation reactor on the one hand; Its condensation point is reduced on the other hand, has very high cetane value, with the problem of urging bavin Unionfining can make up catalytic diesel oil cetane value deficiency.The inventive method had both widened raw material sources for refinery's diesel production, provided outlet again to the processing of catalytic diesel oil inferior simultaneously.
Description
Technical field
The present invention relates to a kind of vegetable and animals oils and catalytic diesel oil Unionfining technique, specifically a kind of gas phase circulation hydrogenation and liquid-phase hydrogenatin machinery processing vegetable oil and catalytic diesel oil, produce the hydrogenation process of 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, the ratio of secondary processing diesel oil especially catalytic diesel oil strengthens gradually, and under normal circumstances, containing a large amount of aromatic hydrocarbons in catalytic diesel oil, cetane value is very low, even if by also meeting the requirement of diesel oil to cetane value very slowly 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 triglyceride, and wherein fatty acid chain length is generally C
12~ C
24, and with C
16and C
18in the majority.The Typical fatty acid that animal-plant oil contains comprises saturated acid (palmitinic acid, stearic acid), unitary unsaturated acid (oleic acid) and polyunsaturated polycarboxylic acid (linolic acid, linolenic acid), vegetables oil is based on unsaturated monoenoic acid and diolefinic acid, and Tallow, beef is then based on saturated fatty acid.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 the control of refinery to cost is more and more stricter, to invest the attention that the low liquid phase hydrogenation technology for distinguishing feature is more and more subject to refinery, so-called liquid phase hydrogenation technology is compared to conventional gas-phase circulation hydrogenation technique, liquid-phase hydrogenatin technological reaction part does not arrange hydrogen gas circulating system, liquid-phase product a large amount of circulation time is relied on to carry dissolved hydrogen into reactive system to the hydrogen providing fresh feed to carry out required for hydrogenation reaction, therefore, the key of liquid phase hydrogenation technology is that reaction oil product dissolved hydrogen tolerance meets reaction and needs hydrogen amount.And catalytic diesel oil is owing to containing higher aromaticity content, reaction hydrogen-consuming volume is very high, and meanwhile, compared to alkane, the meltage of hydrogen in aromatic hydrocarbons is lower, therefore, in traditional liquid-phase hydrogenatin technological process, is difficult to be directly used in process 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 method that a kind of gas phase circulation hydrogenation and liquid-phase hydrogenatin machinery processing vegetable oil and catalytic cracking diesel oil produce high hexadecane value clean diesel.
A kind of vegetable and animals oils of the present invention and catalytic diesel oil Unionfining technique comprise following content:
(1) vegetable and animals oils enters hydroisomerization reactor after mixing with hydrogen, first contact with Hydrobon catalyst bed and carry out hydrofining reaction, after refining reaction effluent mixes with the liquid-phase hydrogenatin diesel oil of circulation, by hydro-upgrading isomerization-visbreaking beds, carry out the reaction of hydroisomerizing pour point depression;
(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) the hot high score liquid phase part that step (2) obtains mixes with catalytic cracking diesel oil, enters after mixed hydrogen tank carries out mixed hydrogen, enters liquid phase hydrogenation reactor and carry out hydrofining reaction;
(4) step (3) obtains hydrogenation reaction effluent part bleeder after reducing valve decompression, and obtain high hexadecane value clean diesel product, another part loops back the lower catalyst bed layer of step (1) described hydroisomerization reactor.
According to vegetable and animals oils of the present invention and catalytic diesel oil Unionfining technique, wherein can also comprise step (5), after the gas phase portion that step (2) obtains isolates hydrogen further, after compressor compression, return step (1) recycle.
According to vegetable and animals oils of the present invention and catalytic diesel oil Unionfining technique, wherein the vegetable and animals oils described in step (1) is selected from one or more in vegetables oil, animal oil, vegetable tallow and Tallow, beef.Can be such as one or more of 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, its carbonatoms be generally 12 ~ 24.
In catalytic cracking diesel oil described in step (2), its aromaticity content is generally 40wt% ~ 95wt%, is preferably 50wt% ~ 70wt%.
In present invention process method, described vegetable and animals oils raw material and the mass ratio of fresh catalyst cracked fuel oil are 1:6 ~ 6:1, preferred 1:2 ~ 4:1.
In vegetable and animals oils of the present invention and catalytic cracking diesel oil Unionfining technique, the operational condition of the vegetable and animals oils hydroisomerization reactor in step (1) is as follows: average reaction temperature 300 DEG C ~ 420 DEG C, preferably 340 DEG C ~ 400 DEG C; Reaction pressure 4.0MPa ~ 18.0MPa, preferred 6.0MPa ~ 15.0MPa; Volume space velocity 0.2h during liquid
-1~ 5h
-1, preferred 0.5h
-1~ 3.0h
-1; Hydrogen to oil volume ratio 100: 1 ~ 1000: 1, preferably 200: 1 ~ 500: 1.
Be filled with Hydrobon catalyst and hydro-upgrading isomerization-visbreaking catalyzer in hydroisomerization reactor described in step (1), the volume ratio of Hydrobon catalyst and hydro-upgrading isomerization-visbreaking catalyzer is generally 1: 5 ~ 2: 1, is preferably 1:3 ~ 1:1.Described Hydrobon catalyst is generally the common diesel Hydrobon catalyst in this area, wherein, Hydrobon catalyst generally with VI B race and/or group VIII metal for active ingredient, with aluminum oxide or silicon-containing alumina for carrier.Group VIB metal is generally Mo and/or W, and group VIII metal is generally Co and/or Ni.With the weight of catalyzer for benchmark, group VIB metal content take oxide basis as 8wt% ~ 28wt%, and group VIII metal content take oxide basis as 2wt% ~ 15wt%.Hydro-upgrading isomerization-visbreaking catalyzer is the heterogeneous catalyst containing beta molecular sieve, and catalyzer contains WO by weight
315 ~ 30%, NiO or CoO2 ~ 15%, beta molecular sieve 10 ~ 45%, carrier is aluminum oxide or amorphous aluminum silicide.
In hydroisomerization reactor, Hydrobon catalyst and hydro-upgrading isomerization-visbreaking catalyzer fill in the upper and lower bed of reactor respectively.Hydroisomerization reactor can be single bed reactor, but preferably includes two beds, upper bed layer filling Hydrobon catalyst, lower bed layer filling hydroisomerizing upgrading and pour point reducing catalyzer.The diesel product that Partial Liquid Phase hydrogenator obtains is passed between two beds, one side can carry out deep hydrodesulfurizationof to liquid-phase hydrogenatin diesel cycle oil and the degree of depth takes off arylation reaction, the liquid-phase hydrogenatin diesel oil of circulation can also play the effect of quenching oil on the other hand, can improve the temperature distribution in hydroisomerization reactor and the entrance temperature of charge reducing bottom bed.
The hydroisomerization reactor of the present invention Hydrobon catalyst selecting hydrogenation capability stronger and the isomerization-visbreaking catalyzer with strong hydrogenation isomery function, single dose or two doses of series connection are adopted once to pass through technical process, under medium-pressure or high pressure condition, hydrotreatment is carried out to vegetable and animals oils, while realizing deep desulfuration, denitrogenation, deoxidation, the contour condensation point component of the normal paraffin in vegetable and animals oils can be made to carry out isomerization reaction, thus reduce its condensation point.
In vegetable and animals oils of the present invention and catalytic diesel oil Unionfining technique, the operational condition of the liquid phase hydrogenation reactor in step (3) is as follows: temperature of reaction 300 DEG C ~ 400 DEG C, preferably 320 DEG C ~ 380 DEG C; Reaction pressure 4.0MPa ~ 15.0MPa, preferred 6.0MPa ~ 10.0MPa; Volume space velocity 1.0h during liquid
-1~ 5h
-1, preferred 1.5h
-1~ 3.0h
-1, liquid phase circulation ratio (i.e. liquid-phase hydrogenatin diesel cycle oil/fresh catalyst diesel feed mass ratio) is 1:5 ~ 5:1, preferred 1:2 ~ 3:1.
Be filled with Hydrobon catalyst in liquid phase hydrogenation reactor in step (3), this catalyzer can be commercially available prod, also can prepare by this area Conventional wisdom.Hydrobon catalyst described in step (3) generally with VI race and/or group VIII metal for active ingredient, with aluminum oxide or silicon-containing alumina for carrier.Group VIB metal is generally Mo and/or W, and group VIII metal is generally Co and/or Ni.With the weight of catalyzer for benchmark, group VIB metal content take oxide basis as 8wt% ~ 28wt%, group VIII metal content take oxide basis as 2wt% ~ 15wt%, this catalyzer has stronger hydrotreated lube base oil ability 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 Unionfining technique have following characteristics:
1, vegetable and animals oils is first through hydrofining, then after hydroisomerizing, the main component of gained liquid-phase product is paraffinic hydrocarbons, has higher hydrogen solubility compared to the catalytic cracking diesel oil based on aromatic hydrocarbons.When studying the normal heptane of same molecular amount and toluene in the solubleness to hydrogen, find that the solubleness of hydrogen at normal heptane is close to two in toluene times.Therefore, the vegetable and animals oils after hydroisomerizing and catalytic diesel oil are mixed into the molten hydrogen amount that liquid-phase hydrogenatin device improves mixing oil.Further, this part no longer consumes hydrogen through the reacted vegetable and animals oils of isomerization-visbreaking in liquid phase hydrogenation reactor, provides dissolved hydrogen for catalytic diesel oil hydrofining reaction just merely, solves the problem that catalytic diesel oil dissolved hydrogen can not meet hydrogenation reaction needs.
2, a large amount of unreacting hydrogens has been dissolved in hydroisomerizing pour point depression unit hot high score oil, be equivalent to this part oil and fulfil mixed hydrogen process ahead of schedule, this part oil directly and catalytic cracking diesel oil be mixed into mixed hydrogen tank, reduce the mixed hydrogen amount that saturated mixed hydrogen needs, improve mixed hydrogen effect, thus be conducive to the carrying out of reaction in liquid phase hydrogenation reactor.
3, the vegetable and animals oils after isomerization-visbreaking has higher cetane value and suitable condensation point, by combining the problem of processing and can make up catalytic diesel oil cetane value deficiency with catalytic diesel oil.Therefore, this technique had both widened raw material sources for refinery's diesel production, meanwhile, provided outlet again to the catalytic diesel oil of poor quality.
4, the circulation of liquid phase hydrogenation reactor reaction effluent cyclic part enters hydroisomerization reactor lower catalyst bed layer, the liquid-phase hydrogenatin diesel oil of circulation both can carry out further isomerization-visbreaking and aromatic saturation reaction in the hydroisomerizing pour point depression beds of hydroisomerization reactor, improved quality product; Simultaneously, the refined diesel oil looped back also serves the effect of thermal barrier or quenching oil, which reduce the reaction temperature rising in hydroisomerization reactor, and in isomerizing reactor, enhance molten hydrogen process, decrease liquid phase hydrogenation reactor part and mix mixed hydrogen load in hydrogen tank, the also corresponding reaction effect that improve in liquid phase hydrogenation reactor.
Accompanying drawing explanation
Fig. 1 is a kind of principle process schematic diagram of the inventive method.
Embodiment
Below by specific embodiment, vegetable and animals oils of the present invention and catalytic diesel oil Unionfining technique are described in detail.
As shown in Figure 1, vegetable and animals oils enters hydroisomerization reactor 3 and carries out the reaction of hydroisomerizing pour point depression after being mixed with the recycle hydrogen introduced through pipeline 2 by pipeline 1, reaction effluent enters hot high score 4 and carries out gas, liquid is separated, obtain gas phase and liquid two-phase, gas phase is gone downstream separation system to isolate the laggard circulating hydrogen compressor of hydrogen further through pipeline 13 and is looped back hydroisomerization reactor entrance, liquid phase part is mixed into mixed hydrogen tank 7 through pipeline 5 and the catalytic diesel oil introduced through pipeline 6, molten hydrogen is mixed with the hydrogen introduced through pipeline 8 at mixed hydrogen in-tank mixing oil, the exess of H2 gas 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 enters the lower catalyst bed layer of hydroisomerization reactor through pipeline 11 circulation, another part obtains high hexadecane value clean diesel product through pipeline 12 bleeder.
Below by specific embodiment and comparative example, further illustrate technical scheme of the present invention and effect.
Embodiment 1 ~ 3
Adopt 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 lists in table 2.Feedstock property used is in table 1, and embodiment 1 ~ 3 and comparative example processing condition used list in table 3.The evaluation result of embodiment 1 ~ 3 and comparative example is in table 4.
Comparative example 1
Gas phase circulation hydrogenation technique is utilized to carry out the reaction of hydro-upgrading isomerization-visbreaking to soybean oil; Catalytic cracking diesel oil carries out liquid-phase hydrogenatin reaction, and liquid-phase hydrogenatin reaction effluent circulates, and recycle ratio is 3:1, and isomery upgrading diesel oil and liquid-phase hydrogenatin diesel oil are in harmonious proportion in embodiment 2 ratio.Comparative example 1 used catalyst is with embodiment 1-3.
Table 1 stock oil character.
| Project | Catalytic diesel oil | Soybean oil |
| Density (20 DEG C), g/cm 3 | 0.9028 | 0.8821 |
| Boiling range, DEG C | 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, DEG C | -20 | 17 |
| Condensation point, DEG C | -17 | 14 |
Table 2 catalyst property.
| Project | Hydrobon catalyst | Hydro-upgrading isomerization-visbreaking catalyzer | Hydrobon catalyst |
| Chemical constitution, wt% | |||
| MoO 3 | 9 | — | 24 |
| NiO | 5 | 4 | 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 | Embodiment 3 | Comparative example 1 | |
| Isomerization-visbreaking condition | ||||
| Temperature of reaction, DEG C | 370 | 375 | 390 | 375 |
| Reaction pressure, MPa | 10.0 | 9.0 | 9.0 | 9.0 |
| Volume space velocity, h -1 | 1.0 | 1.5 | 1.0 | 1.5 |
| Hydrogen to oil volume ratio * | 700 | 800 | 800 | 800 |
| Liquid-phase hydrogenatin condition | ||||
| Temperature of reaction, DEG C | 350 | 360 | 350 | 360 |
| Reaction pressure, MPa | 9.0 | 8.0 | 8.0 | 8.0 |
| Urge bavin volume space velocity, h -1 | 1.5 | 1.5 | 1.0 | 1.5 |
| Liquid phase circulation compares * | 2：1 | 1：1 | 2：1 | 3：1 |
| Soybean oil/urge bavin ratio | 1：1 | 2：1 | 1：1 | 2：1 |
* recycle ratio is the mass ratio of liquid-phase hydrogenatin diesel cycle oil and catalytic diesel oil charging.
The test-results of table 4 embodiment 1 ~ 3 and comparative example.
| Embodiment 1 | Embodiment 2 | Embodiment 3 | Comparative example | |
| Sulphur content, μ g/g | 25 | 8 | 18 | 180 |
| Cetane value | 51 | 55 | 52 | 48 |
| Cold filter clogging temperature, DEG C | -16 | -15 | -15 | -21 |
| Condensation point, DEG C | -13 | -12 | -13 | -17 |
Can be found with the comparative test result of comparative example 1 by embodiment 1 ~ 3: vegetable and animals oils of the present invention with urge bavin to combine processing scheme embodiment 1 and embodiment 3 product sulphur content is respectively 25 μ g/g and 18 μ g/g, cetane value reaches 51 and 52 respectively and meets state IV diesel oil standard; Embodiment 2 products obtained therefrom sulphur content is 8 μ g/g, and cetane value 55 meets state V clean diesel standard, and the index such as cold filter point of diesel oil, condensation point all meets the requirements simultaneously.And identical processing condition taked by comparative example 1 and embodiment 2 diesel oil, product sulphur content and cetane value are respectively 180 μ g/g and 48, and reaction effect is obviously not as embodiment 2.This is because being mixed into of isomery vegetables oil in embodiment improves the molten hydrogen amount of liquid phase, makes to urge bavin amounts of hydrogen in liquid phase hydrogenation reactor reaction process more sufficient, improves liquid phase hydrogenation reactor reaction environment, thus is conducive to the carrying out of desulfurization, de-arylation reaction.
Claims (10)
1. vegetable and animals oils and a catalytic diesel oil Unionfining technique, comprises following content:
(1) vegetable and animals oils enters hydroisomerization reactor after mixing with hydrogen, first contact with Hydrobon catalyst bed and carry out hydrofining reaction, after refining reaction effluent mixes with the liquid-phase hydrogenatin diesel oil of circulation, by hydro-upgrading isomerization-visbreaking beds, carry out the reaction of hydroisomerizing pour point depression;
(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) the hot high score liquid phase part that step (2) obtains mixes with catalytic cracking diesel oil, enters after mixed hydrogen tank carries out mixed hydrogen, enters in liquid phase hydrogenation reactor and carry out hydrofining reaction;
(4) step (3) obtains hydrogenation reaction effluent part bleeder after reducing valve decompression, and obtain high hexadecane value clean diesel product, another part loops back the lower catalyst bed layer of step (1) described hydroisomerization reactor.
2. according to technique according to claim 1, it is characterized in that, the vegetable and animals oils described in step (1) is selected from one or more in vegetables oil, animal oil, vegetable tallow and Tallow, beef.
3. according to the technique described in claim 1 or 2, it is characterized in that, described vegetable and animals oils 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 or butter, and its carbonatoms is 12 ~ 24.
4. according to technique according to claim 1, it is characterized in that, the aromaticity content of the catalytic cracking diesel oil described in step (2) is 40wt% ~ 95wt%.
5. according to technique according to claim 1, it is characterized in that, described vegetable and animals oils raw material and the mass ratio of fresh catalyst cracked fuel oil are 1:6 ~ 6:1.
6. according to technique according to claim 1, it is characterized in that, in step (1), the operational condition of hydroisomerization reactor is as follows: average reaction temperature 300 DEG C ~ 420 DEG C, reaction pressure 4.0MPa ~ 18.0MPa, volume space velocity 0.2h during liquid
-1~ 5h
-1, hydrogen to oil volume ratio 100: 1 ~ 1000: 1.
7. according to technique according to claim 1, it is characterized in that, be filled with Hydrobon catalyst and hydro-upgrading isomerization-visbreaking catalyzer in isomerizing reactor described in step (1), the volume ratio of Hydrobon catalyst and hydro-upgrading isomerization-visbreaking catalyzer is 1:5 ~ 2:1.
8. according to technique according to claim 7, it is characterized in that, described Hydrobon catalyst with VI B race and/or group VIII metal for active ingredient, with aluminum oxide or silicon-containing alumina for carrier, with the weight of catalyzer for benchmark, group VIB metal content take oxide basis as 8wt% ~ 28wt%, and group VIII metal content take oxide basis as 2wt% ~ 15wt%; Described hydro-upgrading isomerization-visbreaking catalyzer is the heterogeneous catalyst containing beta molecular sieve, and catalyzer contains WO by weight
315 ~ 30%, NiO or CoO2 ~ 15% and beta molecular sieve 10 ~ 45%, carrier is aluminum oxide or amorphous aluminum silicide.
9. according to technique according to claim 1, it is characterized in that, Hydrobon catalyst is filled with in liquid phase hydrogenation reactor in step (3), with the weight of catalyzer for benchmark, it take oxide basis as 8wt% ~ 28wt% that catalyzer contains group VIB metal content, and group VIII metal content take oxide basis as 2wt% ~ 15wt%.
10. according to technique according to claim 1, it is characterized in that, in step (3), the operational condition of liquid phase hydrogenation reactor is as follows: average reaction temperature 300 DEG C ~ 400 DEG C, reaction pressure 4.0MPa ~ 15.0MPa, volume space velocity 1.0h during liquid
-1~ 5h
-1, liquid phase circulation is than being 1:5 ~ 5:1.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP1741767A1 (en) * | 2005-07-04 | 2007-01-10 | Neste Oil OYJ | Process for the manufacture of diesel range hydrocarbons |
| CN102464998A (en) * | 2010-11-05 | 2012-05-23 | 中国石油化工股份有限公司 | Method by catalyzing and hydrogenating animal and vegetable oil to produce high-quality diesel |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP1741767A1 (en) * | 2005-07-04 | 2007-01-10 | Neste Oil OYJ | Process for the manufacture of diesel range hydrocarbons |
| CN102464998A (en) * | 2010-11-05 | 2012-05-23 | 中国石油化工股份有限公司 | Method by catalyzing and hydrogenating animal and vegetable oil to produce high-quality diesel |
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