CN102876347B - Preparation method of biological naphtha - Google Patents
Preparation method of biological naphtha Download PDFInfo
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- CN102876347B CN102876347B CN201110192755.2A CN201110192755A CN102876347B CN 102876347 B CN102876347 B CN 102876347B CN 201110192755 A CN201110192755 A CN 201110192755A CN 102876347 B CN102876347 B CN 102876347B
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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
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Abstract
The invention discloses a preparation method of biological naphtha, comprising the following steps of: hydrofinishing plant oil and/or animal oil, allowing a hydrofinished effluent to enter a gas-liquid separation device in a hydrocracking reactor for separation, allowing obtained refined oil and hydrogen to pass through a hydrocracking catalyst bed in a countercurrent way, and separating cracking oil to obtain a gas, the biological naphtha and tail oil. According to the method, the gas-liquid separation device is arranged in a countercurrent reactor, thus minimizing internal and external pressure difference of a high-pressure separator, reducing wall thickness and decreasing equipment investment and operational cost. In the meantime, the separator fits with a tray which is arranged below the separator such that it is ensured that ammonia and steam in the refined product will not enter the cracking catalyst bed and will not influence a cracking catalyst so as to help perform the activity of the cracking catalyst. By the adoption of the preparation method, the purpose of preparing naphtha from biological resources is realized, and the raw material range of basic organic chemicals is widened.
Description
technical field
The present invention relates to a kind of preparation method of biolith cerebrol, specifically a kind of method that adopts one-stage serial hydroprocessing technique to produce biolith cerebrol.
Background technology
In order to tackle the day by day exhausted of petroleum resources and to solve the pollution problem producing in oil use procedure, clean environment firendly, reproducible substitute energy are being tried to explore in countries in the world.In numerous raw materials, vegetables oil has good characteristic (sulfur-bearing, nitrogen, metal etc. hardly) because of it, and becomes 21 century most important production synthol and one of the source of chemical.
Utilize animal oil and/or preparation of biodiesel with vegetable oils, petroleum naphtha, can widen the raw material range of diesel oil and petroleum naphtha.Animal oil and/vegetables oil prepares the reaction path that diesel component can adopt transesterify, its product is fatty acid methyl ester, it is a kind of clean renewable energy source, is the petroleum diesel surrogate of high-quality.In addition, utilize vegetable and animals oils to prepare diesel component, can also adopt the method for hydrotreatment.
US5705722 discloses a kind of method of preparing high hexadecane value hydro carbons, and the method comprises that (1), under hydrotreating catalyst exists, is that 4.0～15.0MPa, liquid hourly space velocity are 0.5～5.0h in 350～450 ℃ of temperature, hydrogen dividing potential drop
-1condition under by the mixture of the liquid hydrocarbon that makes vegetable oil raw materials contact pure vegetables oil is carried out to hydrotreatment with gaseous hydrogen, vegetable oil raw materials is converted into contain diesel oil boiling spread; (2) separating obtained mixture; And (3) isolate the cut of diesel oil boiling spread from mixture, as diesel oil, add component.
US4300009 discloses a kind of method of preparing liquid hydrocarbon with animal oil and/or vegetables oil, and the method is included in 300～650 ℃ of temperature, pressure is that 1～50 normal atmosphere, liquid hourly space velocity are 0.2～20h
-1condition under, use crystalline silico-alumino molecular sieve catalytic animal oil and/vegetables oil is cracked into liquid hydrocarbon, product mid-boiling point is greater than 170 ℃ of components and at least accounts for 40%.This animal oil and/or vegetables oil catalytic cracking production can be used for preparing fuel as gasoline, chemical.Described crystalline silico-alumino molecular sieve is a kind of cracking catalyst component.
US20060186020 discloses a kind of hydroprocessing process of bio-oil, and the vegetables oil comprising 1～75% carries out hydrotreatment together with mineral oil, and treatment condition are 320～400 ℃, pressure 4.0～10.0MPa, liquid hourly space velocity 0.5～2.0h
-1, adopted a kind of hydrotreating catalyst containing CoMo, NiMo.
Petroleum naphtha is the raw material of steam cracking alkene processed, is mainly derived from present the straight run distillation of oil.As previously mentioned, due to the continuous minimizing of petroleum resources, in the urgent need to opening up a kind of method of efficiently preparing biolith cerebrol.
Summary of the invention
Deficiency for existing complete processing, the invention provides a kind of improved one-stage serial hydrocracking processing method, vegetables oil and/or animal oil are after hydrofining, with the reverse hydrocracking reactor that enters of hydrogen, the yield that can increase light-weight fuel oil, improves the quality of products.Wherein, the gas-liquid separator that hydrofining effluent enters hydrocracking reactor top carries out separation, beds top is provided with the column plate of some layers, play the effect of fluid-tight and reinforcing mass transfer, avoid water vapour to contact with hydrocracking catalyst, reduce the activity of catalyzer, column plate has the effect of reallocation to treated oil simultaneously, makes treated oil enter uniformly beds.
Biolith cerebrol preparation method of the present invention, comprises following content:
(1) vegetables oil and/or animal oil enter hydrofining reactor after mixing with hydrogen, carry out the refining reactions such as hydrogenation is saturated, hydrogenation deoxidation under the existence of Hydrobon catalyst;
(2) hydrofining reaction resultant enters the gas-liquid separator of hydrocracking reactor top, carries out gas-liquid separation, then in the enterprising step of column plate of reactor top setting, carries out gas-liquid separation with the hydrogen making progress, and carries out the distribution of mass transfer and treated oil;
(3) through the equally distributed treated oil of column plate and hydrogen adverse current, pass through hydrocracking catalyst bed, carry out cracking reaction;
(4) step (3) gained cracking generates oil and enters separation column, through fractionation, obtains gas, petroleum naphtha and tail oil.
According to the preparation method of biolith cerebrol of the present invention, wherein the vegetables oil described in step (1) is one or more in rapeseed oil, soybean oil, peanut oil, Semen Maydis oil, Oleum Gossypii semen, Jatropha oil, tung oil, plam oil, Oleum Cocois and sunflower seed oil; Animal oil is one or more in lard, butter, sheep oil, chicken fat and fish oil.Above-mentioned animal oil and vegetables oil can mix and use with arbitrary proportion.
In some embodiments, also need to add part sulfocompound in described reaction raw materials animal oil and/or vegetables oil.Described sulfocompound is liquid at normal temperatures and pressures, and the add-on of described sulfocompound is counted 0.0005～3wt% of animal oil and/or vegetables oil weight with sulphur.Described sulfocompound is one or more in dithiocarbonic anhydride, thiophene and derivatives, mercaptan and derivative thereof and thioether and derivative thereof.The general sulphided state catalyzer that uses in vegetable and animals oils hydrocracking process, due to sulfur-bearing not substantially in vegetable and animals oils, catalyzer can cause catalyst activity to reduce in life-time service process because of the loss of sulphur, in reaction raw materials, add appropriate sulfocompound can maintain hydrogen sulfide content suitable in recycle hydrogen, prevent catalyzer rapid deactivation, thereby improve the work-ing life of catalyzer.
The described hydrofining reactor of step (1) adopts conventional hydrofining technology.The operational condition of described hydrofining reaction is: reaction pressure is 3.0MPa～19.0 MPa, is preferably 4.0MPa～16.0 MPa; Average reaction temperature is 280 ℃～460 ℃, is preferably 300 ℃～420 ℃; Volume space velocity 0.1～6.0 h
-1, be preferably 0.3～4.0 h
-1; Hydrogen to oil volume ratio 300: 1～3000: 1, is preferably 500: 1～2500: 1.
Gas-liquid separator described in step (2) is identical with conventional in the art structure of gas liquid separator, because it is arranged in the upper space of hydrodewaxing reactor, the external and internal pressure that can reduce high-pressure separator is poor, reduces its wall thickness, thereby reduces facility investment and process cost.In the present invention, preferably adopt centrifuge separator, as wet cyclone.Described column plate is positioned at the below of gas-liquid separator, the top of beds.1～10 layer of calotte column plate can be installed separately, also can arrange in pairs or groups 1～6 layer of calotte column plate and 1～5 layer of sieve tray are installed.Described calotte column plate and sieve tray can play the effect of treated oil reallocation, fluid-tight and further gas-liquid separation and mass transfer, and wherein the column plate number of plies is preferably 2～3 layers of calotte column plate and 1～2 layer of sieve tray.
The operational condition of the hydrocracking reaction that step (3) is described is: reaction pressure is 3.0MPa～19.0 MPa, is preferably 4.0MPa～18.0 MPa; Average reaction temperature is 290 ℃～460 ℃, is preferably 320 ℃～440 ℃; Volume space velocity 0.1～5.0 h
-1, be preferably 0.3～4.0 h
-1; Hydrogen to oil volume ratio 300: 1～3000: 1, is preferably 500: 1～2500: 1.
In step (3), reacted hydrogen-rich gas is discharged from the top of hydrocracking reactor, enters cold high pressure separator, through separation, obtains liquid hydrocarbon streams, can generate after oil mixes and further process with cracking.Described cold high pressure separator working pressure and reacting system pressure are basic identical, and temperature is generally 10～90 ℃, preferably 35～65 ℃.
The tail oil that step (4) separation obtains can be circulated to hydrofining reactor or hydrocracking catalyst bed.
Compared with prior art, method of the present invention has the following advantages:
1, hydrofined oil and hydrogen adverse current are by hydrocracking reactor, and the gas phase gas separated with refining effluent that cracking reaction generates is together discharged from reactor top, and after washing separation, hydrogen recycle is used; Hydrocracking generates oil and discharges from reactor bottom, enters separation column.The gas-liquid separator arranging in counter-current reactor in the inventive method, the external and internal pressure that can reduce high-pressure separator is poor, reduces its wall thickness, thereby reduces facility investment and process cost.
2, the centrifuge separator that cracking case top arranges can make generation oil and the gas delivery in refining reaction effluent, avoids water vapour to contact with catalyzer downwards; Treated oil after separation carries out mass transfer with hydrogen from bottom to top on column plate, and further realizes gas-liquid separation.
3, on the calotte column plate arranging due to separator bottom and sieve tray, there is certain height of liquid layer treated oil to exist, play " fluid-tight " effect, guarantee that ammonia and water vapour in hydrotreated product can not enter hydrocracking catalyst bed, can not exert an influence to the performance of cracking catalyst and acid sites.Be conducive to the performance of cracking catalyst activity, increase the yield of light-end products, the work-ing life of extending catalyst.
4, cracking case top arranges column plate, particularly sieve tray, reallocate to entering the treated oil of reactor, makes the treated oil state of being evenly distributed enter beds.Be conducive to making full use of of catalyst activity, effectively avoided channel and local reaction too violent.
5, refining generation oil is downward along cracking catalyst bed, and the hydrogen contact reacts with making progress, because density of hydrogen increases to bottom gradually from beds top, is conducive to the carrying out of hydrogenation reaction, is also conducive to the smooth operation of hydrocracking reactor.
6, the present invention has realized by Biological resources animal oil and/or vegetables oil and has substituted the object that the petroleum resources that gradually reduce are prepared petroleum naphtha, has widened the raw material range of basic organic chemicals.
7, the present invention is by saturated to the hydrogenation of stock oil, while having avoided animal oil and/or vegetables oil to be heated to high temperature, because interchanger or heating furnace tube are stopped up in coking, and can extend the life-span of hydrocracking catalyst.
Accompanying drawing explanation
Fig. 1 is the preparation method's of biolith cerebrol of the present invention schematic flow sheet.
Embodiment
In the inventive method, wherein the described Hydrobon catalyst of step (1) can be conventional Hydrobon catalyst, and catalyzer comprises the hydrogenation active metals of carrier and institute's load.The weight of catalyzer of take is benchmark, generally includes metal component of group VIB in the periodic table of elements, as tungsten and/or molybdenum, with oxide compound, counts 10wt%～35wt%, is preferably 15wt%～30wt%; Group VIII metal is counted 1wt%～7wt% as nickel and/or cobalt with oxide compound, is preferably 1.5wt%～6wt%.Carrier is inorganic refractory oxide, is generally selected from aluminum oxide, amorphous silicon aluminium, silicon-dioxide or titanium oxide etc.Can select existing various commercial catalysts, the Hydrobon catalysts such as FF-14, the FF-24,3936,3996 developing such as Fushun Petrochemical Research Institute (FRIPP), FF-16, FF-26, FF-36, FF-46; HC-K, HC-P catalyzer that Uop Inc. produces; TK-555, TK-565 catalyzer that Topsoe company produces, also can be prepared by the general knowledge of this area as required.
The described hydrocracking catalyst of step (3) comprises cracking component and hydrogenation component.Cracking component generally includes amorphous aluminum silicide and/or molecular sieve, as Y type or USY molecular sieve.Tackiness agent is generally aluminum oxide or silicon oxide.Hydrogenation component is selected from metal, metal oxide or the metallic sulfide of VI family, VIIZu Huo VIII family, more preferably one or more in iron, chromium, molybdenum, tungsten, cobalt, nickel or its sulfide or oxide compound.The weight of catalyzer of take is benchmark, and the content of hydrogenation component is 5 wt%～40 wt%.Conventional hydrocracking catalyst can be selected existing various commercial catalysts, FC-12, the FC-14 developing such as FRIPP, FC-16, FC-24, FC-26, ZHC-02, FC-28 etc.; The catalyzer such as the HC-12 of Uop Inc., HC-14, HC-24, HC-39, also can prepare specific hydrocracking catalyst by the general knowledge of this area as required.
Below in conjunction with accompanying drawing, method of the present invention is elaborated.
As shown in Figure 1, a kind of biolith cerebrol of the present invention preparation method's technical process is as follows:
Stock oil 1 enters hydrofining reactor 2 with recycle hydrogen 16 and carries out hydrofining reaction; Refining reaction device effluent 3, with the reverse hydrocracking reactor 6 that enters of hydrogen 5, refining reaction device effluent 3 enters the separator 4 of reactor top, carries out gas-liquid separation, then on calotte column plate 7 and sieve tray 9, carries out further gas-liquid separation and mass transfer with the hydrogen making progress.Treated oil and hydrogen adverse current, by hydrocracking catalyst bed 10, are carried out hydrocracking reaction; Hydrogen-rich gas 11 is discharged from the top of hydrocracking reactor, enter cold high pressure separator 13, the liquid 17 that separation obtains enters separation column 18 together with generating oil 12 with cracking, fractionation obtains gas 19, petroleum naphtha 20 and tail oil 21, and tail oil 21 can be circulated to hydrofining reactor 2 or hydrocracking reactor 6.Through cold high pressure separator, obtaining gas 14 recycles through compressor 15.
Next by specific embodiment, the preparation method of a kind of biolith cerebrol of the present invention is further described.
Embodiment 1～3
Raw materials used is refined soybean oil, allocates the dithiocarbonic anhydride in sulphur 0.02wt% in refined soybean oil into.Hydrobon catalyst used is FF-36, and hydrocracking catalyst used is FC-24, by Sinopec Fushun catalyst plant, produces, and its character is in Table 1.Reactor used is fixed-bed reactor, and reaction conditions and the product property that obtains are in Table 2.
The main physico-chemical property of table 1 catalyzer
| Project | FF-36 | FC-24 |
| Physical properties | Trifolium bar | Cylindrical bars |
| Particle diameter, mm | 1.1~1.3 | 1.5~1.7 |
| Bar is long, mm | 3~8 | 3~8 |
| Chemical constitution, wt% | ? | ? |
| NiO | 3.7~4.2 | 5.0~6.0 |
| MoO 3 | 23.0~26.0 | 14.0~16.0 |
| SiO 2 | — | 35.0~42.0 |
Table 2 embodiment 1～3 data
| Reaction conditions | Embodiment 1 | Embodiment 2 | Embodiment 3 |
| Temperature of reaction, ℃ | 370/380 | 370/370 | 370/360 |
| Pressure, MPa | 6/6 | 8/8 | 8/8 |
| Volume space velocity, h -1 | 1.0/1.5 | 1.0/1.5 | 1.0/1.5 |
| Hydrogen to oil volume ratio *, v/v | 1000/1000 | 1000/500 | 1000/600 |
| Water production rate, wt% | 5.9 | 6.1 | 6.3 |
| Liquid hydrocarbon yield, wt% | 82.6 | 84.2 | 83.4 |
| Naphtha fraction (C 6～C 12），wt% | 79.6 | 82.1 | 80.7 |
| Petroleum naphtha character | ? | ? | ? |
| Sulphur content, μ g/g | <0.5 | <0.5 | <0.5 |
| Nitrogen content, μ g/g | <0.5 | <0.5 | <0.5 |
| Bromine valency, gBr100g -1 | 0.05 | 0.06 | 0.06 |
| Aromatic hydrocarbons, v% | 4.8 | 5.6 | 5.5 |
* the volume ratio that refers to hydrogen and animal oil and/or vegetables oil.
Embodiment 4～6
Raw materials used for refining plam oil and lard with the mixture of weight ratio 1:1, in raw material, allocate the DMDS in sulphur 0.03wt% into.Hydrobon catalyst used is FF-36, and hydrocracking catalyst used is FC-24, by Sinopec catalyzer Fushun branch office, produces, and its character is in Table 1.Reactor used is fixed-bed reactor, and reaction conditions and the product property that obtains are in Table 3.
Table 3 embodiment 4～6 data
| Reaction conditions | Embodiment 4 | Embodiment 5 | Embodiment 6 |
| Temperature of reaction, ℃ | 370/380 | 370/370 | 370/360 |
| Pressure, MPa | 6/6 | 8/8 | 8/8 |
| Volume space velocity, h -1 | 1.0/1.5 | 1.0/1.5 | 1.0/1.5 |
| Hydrogen to oil volume ratio *, v/v | 1000/1000 | 1000/500 | 1000/600 |
| Water production rate, wt% | 4.3 | 5.8 | 5.2 |
| Liquid hydrocarbon yield, wt% | 81.7 | 83.2 | 82.8 |
| Naphtha fraction (C 6～C 12），wt% | 77.0 | 79.5 | 78.2 |
| Petroleum naphtha character | ? | ? | ? |
| Sulphur content, μ g/g | <0.5 | <0.5 | <0.5 |
| Nitrogen content, μ g/g | <0.5 | <0.5 | <0.5 |
| Bromine valency, gBr100g -1 | 0.05 | 0.07 | 0.07 |
| Aromatic hydrocarbons, v% | 5.7 | 6.3 | 6.4 |
* refer to the volume ratio of hydrogen and animal oil and/or vegetables oil.
Claims (9)
1. a preparation method for renewable petroleum naphtha, comprises the following steps:
(1) vegetables oil and/or animal oil enter hydrofining reactor after mixing with hydrogen, carry out that hydrogenation is saturated, hydrogenation deoxidation reaction under the existence of Hydrobon catalyst;
(2) hydrofining reaction resultant enters the gas-liquid separator of hydrocracking reactor top, carries out gas-liquid separation, then in the enterprising step of column plate of reactor top setting, carries out gas-liquid separation with the hydrogen making progress, and carries out the distribution of mass transfer and treated oil; Described column plate is positioned at the below of gas-liquid separator, the top of beds, and column plate comprises 1～10 layer of calotte column plate or comprises 1～6 layer of calotte column plate and 1～5 layer of sieve tray;
(3) through the equally distributed treated oil of column plate and hydrogen adverse current, pass through hydrocracking catalyst bed, carry out cracking reaction;
(4) step (3) gained cracking generates oil and enters separation column, through fractionation, obtains gas, petroleum naphtha and tail oil.
2. according to preparation method claimed in claim 1, it is characterized in that, the vegetables oil described in step (1) is one or more in rapeseed oil, soybean oil, peanut oil, Semen Maydis oil, Oleum Gossypii semen, Jatropha oil, tung oil, plam oil, Oleum Cocois and sunflower seed oil; Animal oil is one or more in lard, butter, sheep oil, chicken fat and fish oil.
3. according to preparation method claimed in claim 1, it is characterized in that, in described animal oil and/or vegetables oil, add the sulfocompound in sulphur 0.0005～3wt%, described sulfocompound is selected from one or more in dithiocarbonic anhydride, thiophene and derivatives, mercaptan and derivative thereof and thioether and derivative thereof.
4. according to preparation method claimed in claim 1, it is characterized in that, the operational condition of described hydrofining reaction is: reaction pressure is 3.0MPa～19.0 MPa, and average reaction temperature is 280 ℃～460 ℃, and volume space velocity is 0.1～6.0 h
-1, hydrogen to oil volume ratio 300: 1～3000: 1.
5. according to preparation method claimed in claim 1, it is characterized in that, the operational condition of described hydrocracking reaction is: reaction pressure is 3.0MPa～19.0 MPa, and average reaction temperature is 290 ℃～460 ℃, volume space velocity 0.1～5.0 h
-1, hydrogen to oil volume ratio 300: 1～3000: 1.
6. according to preparation method claimed in claim 1, it is characterized in that, described column plate comprises 2～3 layers of calotte column plate and 1～2 layer of sieve tray.
7. according to preparation method claimed in claim 1, it is characterized in that, Hydrobon catalyst described in step (1) comprises carrier and hydrogenation active metals, the weight of catalyzer of take is benchmark, comprise that tungsten and/or molybdenum count 10wt%～35wt% with oxide compound, nickel and/or cobalt are counted 1wt%～7wt% with oxide compound.
8. according to preparation method claimed in claim 1, it is characterized in that, the described hydrocracking catalyst of step (3) comprises cracking component and hydrogenation component, cracking component comprises amorphous aluminum silicide and/or molecular sieve, and hydrogenation component is selected from metal, metal oxide or the metallic sulfide of VI family, VIIZu Huo VIII family.
9. according to preparation method claimed in claim 1, it is characterized in that, the tail oil described in step (4) is circulated to step (1) or step (3).
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| CN101942333A (en) * | 2009-07-09 | 2011-01-12 | 中国石油化工股份有限公司抚顺石油化工研究院 | Shale oil single-stage serial hydrocracking technology method |
| CN102027098A (en) * | 2008-03-17 | 2011-04-20 | 环球油品公司 | Production of transportation fuel from renewable feedstocks |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102027098A (en) * | 2008-03-17 | 2011-04-20 | 环球油品公司 | Production of transportation fuel from renewable feedstocks |
| CN101942333A (en) * | 2009-07-09 | 2011-01-12 | 中国石油化工股份有限公司抚顺石油化工研究院 | Shale oil single-stage serial hydrocracking technology method |
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