CN1990832A - Quality modified method for hydrocarbon oil - Google Patents
Quality modified method for hydrocarbon oil Download PDFInfo
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- CN1990832A CN1990832A CN 200510135175 CN200510135175A CN1990832A CN 1990832 A CN1990832 A CN 1990832A CN 200510135175 CN200510135175 CN 200510135175 CN 200510135175 A CN200510135175 A CN 200510135175A CN 1990832 A CN1990832 A CN 1990832A
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- carbon monoxide
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Abstract
The invention discloses a method for modifying quality for hydrocarbon oil. It is characterized in that it comprises mixing reacting material that includes carbon monoxide or synthesized gas containing carbon monoxide, steam and raw hydrocarbon oil with catalyst at 150- 500 Deg. C and 0.1- 1.0 MPa, separting and getting product. The volume of fed carbon monoxide is 3- 40 % of the total fed material, the molar ratio between steam and carbon monoxide is between 0.8- 3, and the weight proportion of raw hydrocarbon oil is 10- 90% of the total fed material. The invention can reduce the cost for hydrogenation for hydrocarbon oil.
Description
Technical field
The invention relates to a kind of method for modifying of hydrocarbon ils, further say so and handle hydrocarbon ils, improve the hydrocarbon ils method for quality about a kind of transition state hydrogen.
Background technology
Hydrogen addition technology can be divided into hydrofining and hydrocracking, and the former is primarily aimed at distillate and carries out upgrading, and the latter is a kind of working method of mink cell focus.Gasoline hydrofinishing is a purpose with desulfurization nitrogen and saturation of olefins mainly, and temperature of reaction is between 250～350 ℃, and under 6.89MPa pressure, volume space velocity can maintain 3h
-1About.Diesel oil hydrofining mainly is with desulfurization nitrogen and to improve cetane value be purpose, and temperature of reaction is between 300～400 ℃, and pressure is in 4～8MPa scope, and air speed can be at 1.0～3.0h
-1Between regulate.Residual hydrocracking is to be purpose to remove metal in the residual oil, sulphur and nitrogen and to reduce its viscosity, can carry out under 16MPa pressure and 402 ℃ of temperature condition.Be that hydrofining or hydrocracking all are the higher technological processs of energy consumption, so energy-saving and cost-reducing significant.
Along with the development of crude oil heaviness trend, the refinery process raw material oil the H/C ratio constantly descend, sulphur nitrogen and metal pollutant content progressively increase.This situation requires the hydrogenation technique scale increasing, and the consumption of hydrogen also rises thereupon.Yet the higher cost of producing hydrogen is one of restraining factors of greatly developing hydrogenation technique.
Summary of the invention
The purpose of this invention is to provide a kind of prior art that is different from, lower-cost novel quality modified method for hydrocarbon oil.
We know that general hydrogen is separated from synthesis gas, and synthetic gas can be by hydrocarbon polymers such as coal, oil, pitch, methane by gasification or steam cracking process production.Contain the CO (carbon monoxide converter) gas suitable in the synthetic gas with amount of hydrogen.Being in the technological process of purpose product with hydrogen, be carbon monodixe conversion to be become hydrogen by water gas shift reaction.In transformationreation, carbon monoxide molecule and water molecules react at catalyst surface, generate carbonic acid gas and hydrogen.
The contriver is by thinking, the active transition state hydrogen that exists in the water gas shift reaction process is suitable in the hydrogenation reaction of hydrocarbon ils, based on this understanding, the contriver unites two into one transformationreation and hydrogenation reaction, in a reaction system, make CO (carbon monoxide converter) gas, water vapour and raw material hydrocarbon ils contact reacts, thereby make the raw material hydrocarbon ils obtain hydrogen atom in molecularity, play saturated, take off heteroatomic hydrocarbon ils upgrading purpose.
Therefore, quality modified method for hydrocarbon oil provided by the invention, it is characterized in that CO (carbon monoxide converter) gas or contain the synthetic gas of carbon monoxide and water vapor and raw material hydrocarbon ils are mixing and contacting reaction under 150～500 ℃ and the 0.1～1.0MPa and in the presence of the catalyzer at reaction conditions, and separate the reaction product obtain, carbon monoxide accounts for 3～40 volume % of combined feed total feed, the molar ratio of water vapor and carbon monoxide is between 0.8～3, and the raw material hydrocarbon oil feed accounts for 10～90 heavy % of combined feed total feed.
Described raw material hydrocarbon grease separation is from vapour, diesel oil distillate.
Method provided by the invention can adopt the reactor types of fluidized-bed, fixed bed or moving-bed.
With the fluidized-bed is example, specific implementation process of the present invention is such: CO (carbon monoxide converter) gas or the synthetic gas, water vapor and the stock oil that contain carbon monoxide are introduced bed from the fluidized-bed lower curtate together, the bed linear gas velocity between 1～20m/s, preferred 2～15m/s; Temperature between 150～500 ℃, preferred 200～400 ℃; Pressure is between 0.1～1.0MPa; Gas residence time between 0.1～15.0s, preferred 0.2～10.0s.
Described reaction mass mixed in mixing tank before entering reactor through preheating, and the mixer outlet temperature is between 120-400 ℃.Described CO (carbon monoxide converter) gas or contain the synthetic gas of carbon monoxide and water vapor enters reactor through nozzle or spraying gun from reactor bottom; Said raw material hydrocarbon ils sprays into reactor from the higher position of reactor.
In the method provided by the invention, the process of the reaction product that said separation obtains normally enters reaction product single-stage or multistage cooling tower, with oil and gas separating process.Described reaction product flows into cooling separation from reactor, and cooling separator is by one or more series connection, and heat-eliminating medium is one or more in the reaction raw materials.It is the preheating that heat energy that product discharges can be used for unstripped gas or oil plant.
Carbonic acid gas in the gas removes by alkaline cleaning procedure, part in the residual gas is returned reaction zone, another part is isolated cumulative C-4-fraction, carbon three and carbon two components through the low temperature separation process system, and hydrogen more than needed can be used for other hydrogenation technique such as hydrocracking etc.
Catalyst system therefor and water gas converting catalyst and hydrotreating catalyst have similarity in the method provided by the invention.But, because the essential distinction that exists with both, so catalyzer is formed the design concept difference that transitivity requires.The reaction system that the present invention relates to contains carbon monoxide or contains the synthetic gas of carbon monoxide, water vapor and pending stock oil, this and pure transformationreation system greatly differ from each other, and need to consider the coupling of the combination of transformationreation and hydrogenation reaction or kinetics, thermodynamics aspect.
We know that in the carbon monodixe conversion reaction, carbon monoxide molecule and water molecules react at catalyst surface, generate carbonic acid gas and hydrogen.The catalyzer of transformationreation has iron-chromium high temperature (300～470 ℃) series, copper-zinc low temperature series (200～260 ℃) and cobalt-molybdenum sulfur-resisting series (150～480 ℃).For example, the catalyzer that is loaded with cobalt, molybdenum element not only is used for the processing treatment of the higher hydrocarbon oil crude material of sulphur content, as the FCC gasoline desulfur, and can be used for the processing of low-sulfur hydrocarbon oil crude material.
For quality modified method for hydrocarbon oil provided by the invention, can correspondingly select to use the above-mentioned activity of such catalysts component that is used for transformationreation according to the height of temperature of reaction.Therefore, in the method provided by the invention, metallic elements such as the active ingredient chosen from Fe of catalyst system therefor, cobalt, nickel, copper, zinc, molybdenum, chromium, preferred cobalt, molybdenum, three kinds of elements of nickel.Metal element content accounts for 5～60% of catalyst weight, and is preferred 8～40%, and all the other are carriers such as kaolin, aluminum oxide.
In the method provided by the invention, when adopting fluidized-bed reactor, catalyzer is through spray shaping, and catalyst particle size is between 10～500 μ m, and median size is between 60～200 μ m; When adopting fixed bed or moving-bed, catalyzer is bar shaped or bead, and the cross section of bar shaped catalyst can be circle or trilobal shape, and maximum diameter is between 1～5mm, and length is between 1～20mm; The spherical catalyst particle diameter is between 0.5～5mm.
In the method provided by the invention, described reaction mass mixed in mixing tank before entering reactor through preheating, and the mixer outlet temperature is between 120～400 ℃.Described CO (carbon monoxide converter) gas or contain the synthetic gas of carbon monoxide and water vapor enters reactor through nozzle or spraying gun from reactor bottom; Said raw material hydrocarbon ils sprays into reactor from the top of reactor.Described reaction product flows into cooling separation from reactor, and cooling separator is by one or more series connection.Heat-eliminating medium is one or more in the reaction raw materials in the cooling separation, i.e. the heat energy of product release is used for the preheating of unstripped gas or oil plant.
Method provided by the invention is characterized in that utilizing transition state hydrogen atom in the reaction process to treat handling oil product and processes, and can finish at atmospheric or low pressure.In addition, compare, adopt carbon monoxide much lower as the cost of reactant gases raw material with hydrogen.Quality modified method for hydrocarbon oil provided by the invention can reduce the cost of vapour, diesel oil hydrofining and residual oil, saves the energy of unnecessary consumption.
Embodiment
Below by embodiment the present invention is further described, but content not thereby limiting the invention.
Embodiment 1
Preparation of Catalyst: get kaolin 60 grams (butt), Xiao Suangu 10 grams, ammonium molybdate 20 grams, nickelous nitrate 10 grams, deionized water 150～200ml, heating, stirring to pulp 1h in there-necked flask, temperature maintenance is between 20～80 ℃.Then slurries are poured in the enamel tray, (102 ℃) oven dry is collected the catalyst debris of drying, (550 ℃) roasting 4h in retort furnace in baking oven.Baked catalyzer grinding is sieved, get granularity and experimentize at the catalyzer of 0.5～3mm.Need before the experiment catalyzer is carried out prevulcanized, the prevulcanized condition is: gas composition: H
270%, N
222%, H
2S8%, 200 ℃ of curing temperatures, normal pressure, gas empty bed speed 0.5m/s, curing time 24 hours.This catalyzer is used for fixing bed.
Above-mentioned catalystic material after mixing making beating on disk spray shaping, mean particle size is controlled at 78 μ m.At 550 ℃ of roasting 4h, prevulcanized is 24 hours in fluidized-bed reactor before the experiment, gas empty bed speed 1.0m/s, and the sulfiding gas composition is identical with the front with service temperature.This catalyzer is used for fluidized-bed.
Stock oil: get catalytic cracking full distillate gasoline, its PIONA consists of: normal paraffin 7%, isoparaffin 11.13%, alkene 40.42%, naphthenic hydrocarbon 5.62%, aromatic hydrocarbons 35.85%.
At normal pressure, fixed bed (20g catalyzer) linear gas velocity is that 1.2m/s, steam and carbon monoxide ratio are that 1.2: 1, carbon monoxide feeding rate are that 300ml/min, feed gasoline feeding rate are 1.0g/min, under the condition of different temperatures, and product liquid (C
5 +) PIONA value and yield be shown in table 1.
Table 1
| Service temperature, ℃ | Normal paraffin, % | Isoparaffin, % | Alkene, % | Naphthenic hydrocarbon, % | Aromatic hydrocarbons, % | Yield of gasoline, % |
| 160 | 11.21 | 15.22 | 32.22 | 6.85 | 34.5 | 98.3 |
| 200 | 12.60 | 20.33 | 26.43 | 7.08 | 33.56 | 97.1 |
| 260 | 14.94 | 23.15 | 20.23 | 8.92 | 32.76 | 96.7 |
| 400 | 14.22 | 23.91 | 19.56 | 9.21 | 33.1 | 95.9 |
| 460 | 13.24 | 25.45 | 18.35 | 9.35 | 33.61 | 95.2 |
Embodiment 2
260 ℃ of service temperature maintenances are constant, and other operational condition is tested under 0.5MPa and 1.0MPa pressure respectively with embodiment 1, and the PONA value and the yield of product liquid are shown in table 2.
Table 2
| Working pressure, MPa | Normal paraffin, % | Isoparaffin, % | Alkene, % | Naphthenic hydrocarbon, % | Aromatic hydrocarbons, % | Yield of gasoline, % |
| 0.1 | 14.94 | 23.15 | 20.23 | 8.92 | 32.76 | 96.7 |
| 0.5 | 13.51 | 23.75 | 19.57 | 9.38 | 33.79 | 97.2 |
| 1.0 | 13.32 | 23.96 | 19.78 | 9.09 | 33.85 | 97.1 |
Embodiment 3
260 ℃ of service temperature maintenances are constant, and other operational condition is tested under different gasoline feeding rate conditions with embodiment 1, and the PONA value and the yield of product liquid are shown in table 3.
Table 3
| The gasoline flow rate, g/min | Normal paraffin, % | Isoparaffin, % | Alkene, % | Naphthenic hydrocarbon, % | Aromatic hydrocarbons, % | Yield of gasoline, % |
| 0.1 | 16.12 | 24.25 | 16.16 | 8.95 | 34.52 | 95.3 |
| 1.0 | 14.94 | 23.15 | 20.23 | 8.92 | 32.76 | 96.7 |
| 2.0 | 13.75 | 20.02 | 25.63 | 8.78 | 31.82 | 97.4 |
Embodiment 4
260 ℃ of service temperature maintenances are constant, and other operational condition is tested under different carbon monoxide and water vapor ratio with embodiment 1, and the PONA value and the yield of product liquid are shown in table 4.
Table 4
| H 2O/CO | Normal paraffin, % | Isoparaffin, % | Alkene, % | Naphthenic hydrocarbon, % | Aromatic hydrocarbons, % | Yield of gasoline, % |
| 0.8 | 14.09 | 23.38 | 19.06 | 8.89 | 34.58 | 96.5 |
| 1.2 | 14.94 | 23.15 | 20.23 | 8.92 | 32.76 | 96.7 |
| 2.7 | 14.73 | 23.03 | 20.64 | 8.78 | 32.82 | 97.1 |
Embodiment 5
Adopt the full cut diesel oil of catalyst treatment of embodiment 1 preparation, the front and back of processing the results are shown in Table 5.
Operational condition: 310 ℃ of temperature, normal pressure, bed linear gas velocity are that 2m/s, steam and carbon monoxide ratio are that 1.2: 1, diesel feed account for 70% of combined feed total feed.Use fixed bed, catalyzer loading amount 20g.
Table 5
| Character | Raw material | Product |
| Density, g/cm 3 | 0.8332 | 0.8141 |
| Sulphur, ppm | 6759 | 42.6 |
| Nitrogen, ppm | 1907 | 96 |
| Colloid, mg/ (100ml) | 195 | 9.3 |
| Bromine number, g/ (100g) | 45 | 1.3 |
| Yield, % | -- | 99.2 |
Embodiment 6
Get the full cut FCC gasoline sample of sulfur-bearing 832ppm, utilize the catalyzer of embodiment 1 to handle.Under 230 ℃ of service temperatures and condition of normal pressure, the bed linear gas velocity is that 1.5m/s, steam and carbon monoxide ratio are that 1.2: 1, gasoline feeding account for 80% of combined feed total feed, fixed bed catalyst loading amount 20g.The total sulfur content of sampling analysis product is 30ppm behind the steady state operation, and desulfurization degree reaches 96%.
Embodiment 7
With high temperature conversion catalyst (iron is transformation catalyst, trade mark FB123) 100g grinding powder, mix with 50g kaolin, 10g aluminium colloidal sol, add appropriate amount of deionized water and mix pasty state, insert baking oven then, under 110 ℃ of temperature, dry.Taking-up oven dry thing makes and fragmentates, and inserts retort furnace, at 550 ℃ of roasting temperature 4h.Then baked catalyzer is ground and sieve, get granularity and experimentize at the catalyzer of 0.5～3mm.In reactor, the ferric oxide in the catalyzer is reduced into Z 250 before the experiment.
Adopt the full cut diesel oil of catalyst treatment of preparation, the front and back of processing the results are shown in Table 6.
Operational condition: 350 ℃ of temperature, normal pressure, bed linear gas velocity are that 2m/s, steam and carbon monoxide ratio are that 1.2: 1, diesel feed account for 70% of combined feed total feed.Use fixed bed, catalyzer loading amount 20g.
Table 6
| Character | Raw material | Product |
| Density, g/cm 3 | 0.8321 | 0.8153 |
| Sulphur, ppm | 200 | 37 |
| Nitrogen, ppm | 632 | 56 |
| Colloid, mg/ (100ml) | 121 | 4.1 |
| Bromine number, g/ (100g) | 63 | 1.5 |
| Yield, % | -- | 99.0 |
Embodiment 8
Adopt the full cut low-sulphur oil of catalyst treatment of embodiment 7 preparations:
Operational condition: 300 ℃ of temperature, normal pressure, bed linear gas velocity are that 3m/s, steam and carbon monoxide ratio are that 1.2: 1, gasoline feeding account for 80% of combined feed total feed.Use fixed bed, catalyzer loading amount 20g.
The PONA value of feed gasoline is: alkane 16.03%, alkene 59.16%, naphthenic hydrocarbon 4.77%, aromatic hydrocarbons 20.05%.Product liquid yield 98%, olefin(e) centent 27.3%, alkene decreases by 54%.
Embodiment 9
Adopt the full cut diesel oil of the catalyst treatment that is used for fluidized-bed of embodiment 1 preparation.Operational condition: 280 ℃ of temperature, working pressure 0.3MPa, steam and carbon monoxide ratio are that 1.2: 1, gasoline feeding account for 60% of combined feed total feed.Fluid catalyst loading amount 60g.Under different carbon monoxide flow rates, test, the results are shown in table 7.
Table 7
| The CO flow rate, ml/min | Normal paraffin, % | Isoparaffin, % | Alkene, % | Naphthenic hydrocarbon, % | Aromatic hydrocarbons, % | Yield of gasoline, % |
| 100 | 14.12 | 23.25 | 23.1 | 8.25 | 31.28 | 96.5 |
| 300 | 14.12 | 23.11 | 22.43 | 8.32 | 32.02 | 96.7 |
| 600 | 14.23 | 22.32 | 22.03 | 8.73 | 32.69 | 96.4 |
Claims (10)
1. quality modified method for hydrocarbon oil, it is characterized in that this method comprise with CO (carbon monoxide converter) gas or contain the synthetic gas of carbon monoxide and the reaction mass of water vapor and raw material hydrocarbon ils under 150～500 ℃ and 0.1～1.0MPa, with the catalyzer contact reacts and separate the product that obtains, wherein carbon monoxide accounts for 3～40 volume % of combined feed total feed, the mol ratio of water vapor and carbon monoxide is 0.8～3, and the raw material hydrocarbon oil feed accounts for 10～90 heavy % of combined feed total feed.
2. according to the method for claim 1, it is characterized in that described raw material hydrocarbon grease separation is from gasoline or diesel oil distillate.
3. according to the method for claim 1, one or more of activity of such catalysts component chosen from Fe, cobalt, nickel, copper, zinc, molybdenum, chromium.
4. according to the method for claim 1, the activity of such catalysts component is selected from one or more mixture of cobalt, molybdenum, nickel.
5. according to the method for claim 3 or 4, said metal element content accounts for 5～60% of catalyst weight.
6. according to the method for claim 5, said metal element content accounts for 8～40% of catalyst weight.
7. according to the method for claim 1, it is characterized in that described reaction mass through preheating, mixed before entering reactor in mixing tank, the mixer outlet temperature is between 120～400 ℃.
8. according to the method for claim 1, the synthetic gas and the water vapor that it is characterized in that described CO (carbon monoxide converter) gas or contain carbon monoxide enter reactor through nozzle or spraying gun from reactor bottom; Said raw material hydrocarbon ils sprays into reactor from the top of reactor.
9. according to the method for claim 1, it is characterized in that described reaction product flows into cooling separation from reactor, cooling separator is by one or more series connection.
10. according to the method for claim 5, it is characterized in that heat-eliminating medium in the cooling separation is one or more in the reaction raw materials.
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|---|---|---|---|
| CN 200510135175 CN1990832A (en) | 2005-12-29 | 2005-12-29 | Quality modified method for hydrocarbon oil |
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| CN 200510135175 CN1990832A (en) | 2005-12-29 | 2005-12-29 | Quality modified method for hydrocarbon oil |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102433153A (en) * | 2011-10-21 | 2012-05-02 | 华东理工大学 | Method for refining biological oil |
| CN107810252A (en) * | 2015-06-24 | 2018-03-16 | 卡尔·维尔纳·迪特里希 | Boudouard reaction for the hydrolysis of the combination water that manufactures methane |
| CN109355098A (en) * | 2018-09-19 | 2019-02-19 | 北京三聚环保新材料股份有限公司 | A kind of low grade oils multi-stage conversion process |
| CN110408420A (en) * | 2018-04-28 | 2019-11-05 | 北京三聚环保新材料股份有限公司 | A kind of organic matter transformation technique |
| US11492563B2 (en) | 2018-04-28 | 2022-11-08 | Beijing Sanju Environmental Protection & New Materials Co., Ltd | Conversion process for an inferior oil |
-
2005
- 2005-12-29 CN CN 200510135175 patent/CN1990832A/en active Pending
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102433153A (en) * | 2011-10-21 | 2012-05-02 | 华东理工大学 | Method for refining biological oil |
| CN107810252A (en) * | 2015-06-24 | 2018-03-16 | 卡尔·维尔纳·迪特里希 | Boudouard reaction for the hydrolysis of the combination water that manufactures methane |
| CN110408420A (en) * | 2018-04-28 | 2019-11-05 | 北京三聚环保新材料股份有限公司 | A kind of organic matter transformation technique |
| CN110408420B (en) * | 2018-04-28 | 2021-07-30 | 北京三聚环保新材料股份有限公司 | Organic matter conversion process |
| US11492563B2 (en) | 2018-04-28 | 2022-11-08 | Beijing Sanju Environmental Protection & New Materials Co., Ltd | Conversion process for an inferior oil |
| CN109355098A (en) * | 2018-09-19 | 2019-02-19 | 北京三聚环保新材料股份有限公司 | A kind of low grade oils multi-stage conversion process |
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