CN107474875A - A kind of method of hypergravity diesel oil and gasoline hydrofinishing - Google Patents
A kind of method of hypergravity diesel oil and gasoline hydrofinishing Download PDFInfo
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- CN107474875A CN107474875A CN201710865181.8A CN201710865181A CN107474875A CN 107474875 A CN107474875 A CN 107474875A CN 201710865181 A CN201710865181 A CN 201710865181A CN 107474875 A CN107474875 A CN 107474875A
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
- C10G45/00—Refining of hydrocarbon oils using hydrogen or hydrogen-generating compounds
- C10G45/02—Refining of hydrocarbon oils using hydrogen or hydrogen-generating compounds to eliminate hetero atoms without changing the skeleton of the hydrocarbon involved and without cracking into lower boiling hydrocarbons; Hydrofinishing
- C10G45/04—Refining of hydrocarbon oils using hydrogen or hydrogen-generating compounds to eliminate hetero atoms without changing the skeleton of the hydrocarbon involved and without cracking into lower boiling hydrocarbons; Hydrofinishing characterised by the catalyst used
- C10G45/06—Refining of hydrocarbon oils using hydrogen or hydrogen-generating compounds to eliminate hetero atoms without changing the skeleton of the hydrocarbon involved and without cracking into lower boiling hydrocarbons; Hydrofinishing characterised by the catalyst used containing nickel or cobalt metal, or compounds thereof
- C10G45/08—Refining of hydrocarbon oils using hydrogen or hydrogen-generating compounds to eliminate hetero atoms without changing the skeleton of the hydrocarbon involved and without cracking into lower boiling hydrocarbons; Hydrofinishing characterised by the catalyst used containing nickel or cobalt metal, or compounds thereof in combination with chromium, molybdenum, or tungsten metals, or compounds thereof
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J3/00—Processes of utilising sub-atmospheric or super-atmospheric pressure to effect chemical or physical change of matter; Apparatus therefor
- B01J3/04—Pressure vessels, e.g. autoclaves
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
- C10G45/00—Refining of hydrocarbon oils using hydrogen or hydrogen-generating compounds
- C10G45/02—Refining of hydrocarbon oils using hydrogen or hydrogen-generating compounds to eliminate hetero atoms without changing the skeleton of the hydrocarbon involved and without cracking into lower boiling hydrocarbons; Hydrofinishing
- C10G45/04—Refining of hydrocarbon oils using hydrogen or hydrogen-generating compounds to eliminate hetero atoms without changing the skeleton of the hydrocarbon involved and without cracking into lower boiling hydrocarbons; Hydrofinishing characterised by the catalyst used
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
- C10G2300/00—Aspects relating to hydrocarbon processing covered by groups C10G1/00 - C10G99/00
- C10G2300/10—Feedstock materials
- C10G2300/1037—Hydrocarbon fractions
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
- C10G2300/00—Aspects relating to hydrocarbon processing covered by groups C10G1/00 - C10G99/00
- C10G2300/20—Characteristics of the feedstock or the products
- C10G2300/201—Impurities
- C10G2300/202—Heteroatoms content, i.e. S, N, O, P
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- Chemical & Material Sciences (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- General Chemical & Material Sciences (AREA)
- Production Of Liquid Hydrocarbon Mixture For Refining Petroleum (AREA)
Abstract
The invention discloses a kind of method of hypergravity diesel oil and gasoline hydrofinishing, comprise the following steps：The first order and second level supergravity reactor from series connection；Efficiently mixed gas-liquid two-phase is carried out in hydrogen and feedstock oil input feed cavity, make slightly solubility hydrogen be dispersed into feedstock oil it is substantial amounts of receive micron bubble, hydrogen reaches supersaturation in feedstock oil, forms gas-liquid mixture；Gas-liquid mixture is delivered into progress hydrogenation desulfurization and denitrogenation reaction in the rotor containing catalyst by liquid distribution trough, obtains removing the feedstock oil of sulfur-bearing nitrogen impurity；The feedstock oil input second level supergravity reactor of hydrogen and removing sulfur-bearing nitrogen impurity is subjected to hydrogenation reaction of unsaturated hydrocarbon；Reactor of the present invention can make slightly solubility hydrogen reach supersaturation in liquid phase dissolved degree, efficiently using reductive hydrogen, strengthen gas-liquid-solid phase mass transfer, feedstock oil desulfurization rate≤90% of this method；Denitrogenation Shuai≤80%；Compared with existing high-gravity technology, unsaturated hydrocarbons conversion ratio improves 15%.
Description
Technical field
The invention belongs to feedstock oil hydrofinishing field, more particularly, to a kind of hypergravity diesel oil and gasoline hydrofinishing
Method.
Background technology
Increasingly strict with environmental regulation, low-sulfur, low aromatic hydrocarbons, the diesel oil of high cetane number and gasoline have turned into the world and sent out
Up to the development trend of countries and regions diesel oil and gasoline new spec.The discharge mark that European Union member countries came into effect Europe V from 2009
Diesel oil sulfur content is reduced to below 10 μ g/g by standard, the standard.The developed countries such as the U.S., Japan have also promulgated respective diesel oil mark
Standard, the standard of sulfur content is down to 15 μ g/g and below 10 μ g/g respectively.Implement state in 1 day January in 2017, in the whole nation in China
V discharge standard.
At present, traditional trickle bed hydrogen addition technology is ripe, reliably, is widely used in oil plant hydrogenation plant.But the work
Skill needs gas separated by high pressure separator to be circulated by circulating hydrogen compressor, and hydrogen-oil ratio is more than 300, and high pressure line is more, and reactor is larger.Conventional
Bavin/gasoline hydrogenation is designed according to old plant, can not meet the requirement of product quality upgrading from now on.
If the requirement needs that existing common diesel and gasoline hydrogenation technology will adapt to bavin/quality of gasoline upgrading are done a lot
Work：
(1) it is one trickle bed reactor of series connection after trickle bed reactor that conventional process techniques, which are improved, to reduce diesel oil
Feed space velocities, so as to realize production the low-sulfur even needs of super-low sulfur quality.But the cost of construction can greatly increase.
(2) designed using existing hydrogenation conventional processing technique, in order to produce the low-sulfur even needs of the product of super-low sulfur,
By changing new catalyst.But a kind of new catalyst of research and development needs substantial amounts of experiment to complete, it is difficult in the short cycle
Interior completion.
Therefore, it is particularly important by the improvement or the other hydrogen addition technology process routes of searching of engineering technology.It is conventional
The reactions such as desulfurization, denitrogenation in trickle bed reactor mainly from gas phase diffusion and are dissolved into feedstock oil with hydrogen mass transfer, i.e. hydrogen
In speed be whole hydrogenation reaction rate-determining steps.Therefore, hydrogen is dissolved in feedstock oil with the state of saturation, eliminates hydrogen
Mass transfer influences, and subsequently enters reactor and catalyst and carries out catalytic reaction and can yet be regarded as a kind of efficient hydrofinishing process.
High-gravity technology obtains more impressive progress, CN103102942A in the application study of field of chemical engineering in recent years
Feedstock oil is successfully passed through the supergravity reactor equipped with non-precious metal catalyst, desulfurization is carried out with hydrogen counter current contacting, takes off
Nitrogen and part aromatic hydrocarbons saturated reaction, but by the way of catalyst is loaded, operating process is difficult, and course of reaction pressure drop is larger, urges
Agent easily inactivates；Metal-polymer catalyst is fixed on the rotor of rotating packed bed reactor by CN104419454A,
Drippolene and hydrogen carry out selective hydrogenation reaction by the beds being rotating, but not specific proposition monoblock type is urged
The raw material proportioning and fixing means of agent fixation procedure.And in existing high-gravity technology, diesel oil and gasoline hydrogenation reaction are because of hydrogen
The solubility of gas so that hydrogenation efficiency is relatively low, and hydrogenation cost is higher.
The content of the invention
The technical problem to be solved in the present invention is to provide a kind of method of hypergravity diesel oil and gasoline hydrofinishing.This method
The reactor used can make slightly solubility hydrogen reach supersaturation in liquid phase dissolved degree, efficiently using reductive hydrogen, strengthen gas-liquid
Solid phase mass transfer, feedstock oil desulfurization Shuai≤90% of this method；Denitrogenation Shuai≤80%；Compared with existing supergravity reactor, insatiable hunger
With hydrocarbon conversion rate Ti Gao≤15%.
Term " feedstock oil " in the present invention refers to common diesel or regular price gasoline.
In order to solve the above technical problems, invention adopts the following technical scheme that：
A kind of method of hypergravity diesel oil and gasoline hydrofinishing, comprises the following steps：
S1, selection supergravity reactor
From the first order supergravity reactor and second level supergravity reactor of series connection, the supergravity reactor includes
Motor, main shaft, rotor, housing and liquid distribution trough；The main shaft of the motor output end is extend into housing through housing bottom,
The rotor is fixed on main shaft top；The super-gravity device also includes secondary axes, speed increaser, output shaft of the speed increaser and feed cavity；
The feed cavity is arranged on the top of housing, the bottom connection liquid distribution trough of feed cavity；The main shaft passes through secondary axes and speedup
Device is fixedly connected, and the output shaft of the speed increaser is extend into feed cavity through feed cavity bottom；The output shaft of the speed increaser enters
Material intracavitary part is provided with agitator；The feed cavity is provided with first gas entrance, liquid inlet and catalyst inlet, described
Lower housing portion is provided with gas liquid outlet；The housing upper is provided with gas inlet-outlet, and the housing side is provided with second gas entrance；
S2, first order supergravity reactor motor is started, speed increaser rotation is driven, so as to drive the agitator in feed cavity
Ultrahigh speed rotates；Efficiently mixed gas-liquid two-phase is carried out in hydrogen and feedstock oil input feed cavity, make slightly solubility hydrogen in raw material
Be dispersed into oil it is substantial amounts of receive micron bubble, solubility of the hydrogen in feedstock oil reaches supersaturation, forms gas-liquid mixture；Will
Gas-liquid mixture delivers into progress hydrogenation desulfurization and denitrogenation reaction in the rotor containing catalyst by liquid distribution trough, is taken off
Except the feedstock oil of sulfur-bearing nitrogen impurity；
S3, second level supergravity reactor motor is started, speed increaser rotation is driven, so as to drive the agitator in feed cavity
Ultrahigh speed rotates；Efficiently mix, make by gas-liquid two-phase is carried out in the feedstock oil input feed cavity of hydrogen and removing sulfur-bearing nitrogen impurity
Slightly solubility hydrogen be dispersed into the feedstock oil of removing sulfur-bearing nitrogen impurity it is substantial amounts of receive micron bubble, hydrogen is molten in feedstock oil
Xie Du reaches supersaturation, forms gas-liquid mixture；Gas-liquid mixture is delivered into containing catalyst by liquid distribution trough
Hydrogenation reaction of unsaturated hydrocarbon is carried out in rotor；
S4, reaction product and unreacted hydrogen leave reactor by liquid outlet and gas inlet-outlet respectively.
As the further improvement of technical scheme, the speed increasing ratio of the speed increaser is 1：2-500；Preferably, speed increaser
Speed increasing ratio is 1：4-25；It is highly preferred that the speed increasing ratio of speed increaser is 1：5-15.
As the further improvement of technical scheme, the material of the agitator include titanium alloy, chromium-base alloy, dual phase steel or
Ceramics etc..
As the further improvement of technical scheme, the catalyst includes structured packing catalyst or intends homogeneous catalyst.
Preferably, the structured packing catalyst includes basic framework, active component and Second support；The basic framework
For cordierite structured packing, the active component is combined into by molybdenum or the testing sulphide of tungsten and cobalt or nickel, and Second support is
γ-Al2O3。
Preferably, the plan homogeneous catalyst is DNAcarrier free Ni-Mo sulfide catalysts；The plan homogeneous catalyst can
To be transported to feed cavity together with feedstock oil and hydrogen.
As the further improvement of technical scheme, in step S2, in first order supergravity reactor, reaction pressure is
0.3-0.5MPa, temperature are 230-350 DEG C, hydrogen-oil ratio 100:1-800:1；In step S3, in second level supergravity reactor
In, reaction pressure 0.1-2MPa, temperature is 360-480 DEG C, hydrogen-oil ratio 20:1-200:1.Aforementioned condition is adapted so that with regular
The situation of filler catalyst.
As the further improvement of technical scheme, in step S2, in first order supergravity reactor, reaction pressure is
0.3-0.4MPa, temperature are 200-320 DEG C, hydrogen-oil ratio 50:1-600:1；In step S3, in second level supergravity reactor
In, reaction pressure 0.1-1.5MPa；Temperature is 360-420 DEG C, hydrogen-oil ratio 20:1-100.
As the further improvement of technical scheme, in step S2 and S3, the micron bubble size Control of receiving is in 30nm-
300μm。
As the further improvement of technical scheme, in step S3, the control of gas-liquid-solid catalytic hydrogenation reaction residence time is
Realized by regulating and controlling supergravity reactor rotating speed, the rotating speed of supergravity reactor can be controlled in 200-2700rpm, and liquid phase exists
The residence time can be controlled in 50-2000ms in rotor.
In the case where the one way course of reaction residence time is shorter, catalytic hydroconversion rate is relatively low, can be by material outside
The mode of portion's circulation improves reaction conversion ratio.Realized by the rotating speed for regulating and controlling supergravity reactor to molecular mixing efficiency and material
The control of residence time, side reaction can be reduced.
Any scope described in the present invention includes any numerical value and end value or end value between end value and end value
Between any subrange for being formed of any number.
Unless otherwise specified, each raw material in the present invention can be obtained by commercially available purchase, equipment used in the present invention
The conventional equipment in art or the prior art with reference to art can be used to carry out.
Compared with prior art, the present invention has the advantages that：
1) bubble in the liquid phase grow by existence time：Common gas-liquid is simply mixed after bubble produces in the liquid phase in device, meeting
Rapidly rise to liquid phase surface and rupture disappearance, existence time is very short；And pass through micro-nano caused by gas liquid high-efficiency pre-mixing apparatus
Rice bubble is once generation, and the rate of climb in water is slower, and the course from producing rupture generally reaches tens seconds even rather
Clock, and volume is constantly shunk in uphill process and final dissolving disappears in water, and volume smaller gas ducks in drink
The rate of climb is slower；
2) gas-liquid mass transfer efficiency high, when bubble diameter is smaller, the surface tension of microbubble interface is to Bubble Characteristics
The more notable of performance is influenceed, surface tension at this moment produces compression to internal gas so that micron bubble was rising
Constantly shunk in journey and show itself supercharging.With the unlimited diminution of bubble diameter, the specific surface area of bubble interface is also therewith
Unlimited increase, finally because itself pressurized effect causes air pressure inside to increase to infinity.Therefore, have so that more gases
It is dissolved into through gas-liquid interface in water, may be such that mass-transfer efficiency persistently strengthens at gas-liquid interface, and micro- gas that this characteristic makes
Even if the gas content of bubble in the liquid phase reaches supersaturated condition, it may continue to carry out the mass transport process of gas and keep efficient
Mass-transfer efficiency.Reaction and the dissolving of gas are simultaneous, and while vapor-phase reactant is consumed, micron bubble of receiving crushes
Dissolving and macroscopical gas phase the mass transfer dissolving into liquid phase are carried out simultaneously, and gas can be supplemented within the very first time；
3) in terms of reducing reaction pressure：As improved hydrogen using the method for improving pressure mostly in hydrogenation plant at this stage
The dissolving of gas in the solution, such as reached before entering the reactor using the gas liquid high-efficiency mixing arrangement of the present invention, liquid phase
Supersaturation, and due to high efficient gas and liquid mixing arrangement Gas content in liquid phase can be made to be up to 90%, micron even nano bubble exists
The redissolution for carrying out gas phase is crushed in liquid phase, therefore the partial pressure of hydrogen can be reduced suitably in actual reactor, reduce investment into
This；
4) flow is simplified, it is not necessary to circulating hydrogen compressor, reduces investment and energy consumption, the production cost of device substantially drop
It is low；
5) supergravity reactor can greatly strengthen gas-liquid/liquid-liquid mass transfer, improve the solubility of hydrogen, fortifying catalytic hydrogenation
Reaction, reaction velocity is high, reactor volume is small；
6) desulfurization removing nitric significant effect, super-low sulfur nitrogen oil product can be produced；
7) reaction temperature rising is small, hot localised points is not present in reactor, catalyst is not easy coking；
8) catalyst has preferable stability and selectivity under the conditions of Continuous Liquid Phase feedstock oil hydrogen addition technology, can meet
The needs of industrial long-term operation；
9) integer catalyzer active component dosage is less, typically not over 30%.
In summary, feedstock oil desulfurization Shuai≤90% of method of the invention；Denitrogenation Shuai≤80%；With existing hypergravity phase
Than unsaturated hydrocarbons conversion ratio Ti Gao≤15%.
Brief description of the drawings
The embodiment of the present invention is described in further detail below in conjunction with the accompanying drawings
Fig. 1 shows supergravity reactor structural representation of the present invention；
Fig. 2 shows that the present invention carries out the technological process of hypergravity diesel oil and gasoline hydrofinishing using structured packing catalyst
Figure；
Fig. 3 shows that the present invention uses the technological process for intending homogeneous catalyst progress hypergravity diesel oil and gasoline hydrofinishing
Figure.
Embodiment
In order to illustrate more clearly of the present invention, with reference to preferred embodiment, the present invention is described further.Ability
Field technique personnel should be appreciated that following specifically described content is illustrative and be not restrictive, and this should not be limited with this
The protection domain of invention.
Narration is intended merely to using noun of locality " upper and lower, left and right " etc. conveniently, those skilled in the art can in the present invention
Know, these orientation are relative, may be changed by modes such as rotations.
First supergravity reactor and second level supergravity reactor shown in Figure 1, being used in the present invention, including electricity
Machine 1, main shaft 2, rotor 3, housing 4 and liquid distribution trough 14；The main shaft 2 of the motor output end extend into shell through housing bottom
In body 4, the rotor 3 is fixed on the top of main shaft 2；It is defeated that the supergravity reactor also includes secondary axes 17, speed increaser 15, speed increaser
Shaft 6 and feed cavity 7；The feed cavity 7 is arranged on the top of housing 4, the bottom connection liquid distribution trough 14 of feed cavity 7；Institute
Main shaft 2 is stated to be fixedly connected with speed increaser 15 by secondary axes 17, the output shaft of the speed increaser 6 through the bottom of feed cavity 7 extend into
Expect in chamber 7；The feed cavity inside points of the output shaft of the speed increaser 6 are provided with agitator 11；The feed cavity 7 is provided with the first gas
Body entrance 10, liquid inlet 8 and catalyst inlet 9, the bottom of housing 4 are provided with gas liquid outlet 16；The top of housing 4 is provided with
Gas inlet-outlet 12, the housing side are provided with second gas entrance 13；Sealing 5 is provided between rotor 3 and housing 4；
Fig. 2 show the process chart that structured packing catalyst carries out hypergravity diesel oil and gasoline hydrofinishing.
The implication that each several part represents in figure as：
18- gas bombs；19- pressure-regulating valves；20- mass flowmenters；21- gas bombs；22- pressure is adjusted
Valve；
23- mass flowmenters；24- main valves；25- check-valves；26- divides valve；27- mass flowmenters；
28- mass flowmenters；29- divides valve；30- mass flowmenters；31- ball valves；32- pumps；
33- liquid supplementation pipes；34- mass flowmenters；35- ball valves；36- ball valves；37- ball valves；
38- storage tanks；39- cooling agents；40- ball valves；41- ball valves；42- ball valves；
43- mass flowmenters；44- mass flowmenters；45- ball valves；46- divides valve；47- main valves；48- check-valves.
As shown in Fig. 2 hydrogen gas pass through needed for the level pressure of pressure-regulating valve 22 to reaction system from raw material gas cylinder 21
Pressure, enter first order supergravity reactor after then being measured by mass flowmenter 23, while be passed through feedstock oil with pump 32
In one-level supergravity reactor, because agitator 11 and rotor 3 rotate strengthen gas-liquid mass transfer at a high speed, the dissolving of hydrogen is improved
Degree, hydrogen is set in feedstock oil be in saturation state, the feedstock oil of saturation reacts with the catalyst being supported on rotor 3, removes
Sulfur-bearing nitrogen impurity in feedstock oil；Then, the feedstock oil of sulfur-bearing nitrogen impurity is removed by entering two after the metering of mass flowmenter 44
Level supergravity reactor；At the same time, the hydrogen feed gas of purification from raw material gas cylinder 18 by the level pressure of pressure-regulating valve 19 to
Pressure needed for reaction system, enter two level supergravity reactor after then being measured by mass flowmenter 20, carry out catalysis and add
Hydrogen reacts；A hydrogenated products part is sampled detection by valve 41, and liquid is delivered to storage tank 38 by pump 36 and entered by another
Row Matter Transfer, fresh feed oil product is supplemented by liquid supplementation pipe 33.
In certain embodiments of the present invention, the catalyst is structured packing catalyst, the structured packing catalyst
Including basic framework, active component and Second support；The basic framework is cordierite structured packing, and the active component is by molybdenum
Or tungsten and the testing sulphide of cobalt or nickel are combined into, Second support is γ-Al2O3。
In certain embodiments of the present invention, in step S2, in first order supergravity reactor, reaction pressure 0.3-
0.5MPa, temperature are 230-350 DEG C, hydrogen-oil ratio 100:1-800:1、100:1-700:1、100:1-600:1、100:1-500:
1、100:1-400:1、100:1-300:1、100:1-200:1、200:1-800:1、200:1-700:1、200:1-600:1、
200:1-500:1、200:1-400:1、200:1-300:1、300:1-800:1、300:1-700:1、300:1-600:1、300:
1-500:1、300:1-400:1、500:1-800:1、600:1-800:1 or 700:1-800:1.
In certain embodiments of the present invention, in step S3, in the supergravity reactor of the second level, reaction pressure 0.1-
2MPa, temperature are 360-480 DEG C, hydrogen-oil ratio 20:1-200:1、20:1-180:1、20:1-160:1、20:1-140:1、20:1-
120:1、20:1-100:1、20:1-80:1、20:1-60:1、20:1-40:1、50:1-200:1、50:1-180:1、50:1-
160:1、50:1-140:1、50:1-120:1、50:1-100:1、50:1-80:1、80:1-200:1、80:1-180:1、80:1-
160:1、80:1-140:1、80:1-120:1、80:1-100:1、100:1-200:1、100:1-180:1、100:1-160:1、
100:1-140:1 or 100:1-120:1.
In certain embodiments of the present invention, the speed increasing ratio of the speed increaser is 1：2-500；Preferably, the increasing of speed increaser
Speed is than being 1：4-25；It is highly preferred that the speed increasing ratio of speed increaser is 1：5-15.
By the regulation to speed increaser, it can make it that the bubble in feed cavity 7 in the liquid phase grow by existence time：Common gas-liquid
It is simply mixed after bubble produces in the liquid phase in device, liquid phase surface can be rapidly risen to and rupture disappearance, existence time is very short；
And it is slower once generation, the rate of climb in water by micro-nano bubble caused by gas liquid high-efficiency pre-mixing apparatus, from generation
Course to rupture generally reaches tens seconds even a few minutes, and volume is constantly shunk and final in water in uphill process
Dissolving disappears, and the rate of climb that the smaller gas of volume ducks in drink is slower.
When bubble diameter is smaller, the surface tension of microbubble interface influences the more aobvious of performance to Bubble Characteristics
Write, surface tension at this moment produces compression to internal gas so that micron bubble is constantly shunk in uphill process and table
Reveal itself supercharging；With the unlimited diminution of bubble diameter, the specific surface area also unlimited increase therewith of bubble interface, finally due to
Itself pressurized effect causes air pressure inside to increase to infinity；Therefore, have so that more gases dissolve through gas-liquid interface
Into water, may be such that mass-transfer efficiency persistently strengthens at gas-liquid interface, even and if this characteristic microbubble that makes in the liquid phase
When gas content reaches supersaturated condition, it may continue to carry out the mass transport process of gas and keep efficient mass-transfer efficiency.Reaction
Dissolving with gas is simultaneous, while vapor-phase reactant is consumed, the broken dissolving of micron bubble of receiving and macroscopical gas phase
Into liquid phase, mass transfer dissolving is carried out simultaneously, and gas can be supplemented within the very first time；
The dissolving of hydrogen in the solution is improved using the method for improving pressure mostly in hydrogenation plant at this stage, and adopted
With gas liquid high-efficiency mixing arrangement (motor 1, main shaft 2, secondary axes 17, speed increaser 15, output shaft of the speed increaser 6, the agitator of the present invention
11st, feed cavity 7 etc. is collectively referred to as), liquid phase has reached supersaturation before rotor is entered, and micron even nano bubble is in liquid phase
In crush the redissolution for carrying out gas phase, therefore the partial pressure of hydrogen can be reduced suitably in actual reactor, reduce cost of investment.
In certain embodiments of the present invention, the material of the agitator includes titanium alloy, chromium-base alloy, dual phase steel or pottery
Porcelain etc..
Shown in Fig. 3, to intend the process chart that homogeneous catalyst carries out hypergravity diesel oil and gasoline hydrofinishing.
The implication that each several part represents in figure as：
49- separators；50- catalyst feeds；51- pumps；52- fluid storage tanks；
53- intends homogeneous catalyst separation supplementary device；54- separators；55- catalyst feeds；56- pumps；
57- fluid storage tanks；58- intends homogeneous catalyst separation supplementary device.
As shown in Figure 3：Hydrogen from raw material gas cylinder by pressure-regulating valve level pressure to the pressure needed for reaction system, then
Enter one-level supergravity reactor after being measured by mass flowmenter, at the same time with pump by feedstock oil with add desulfurization removing nitric
Intend homogeneous catalyst to be together passed through in one-level supergravity reactor, because agitator and rotor rotate strengthen gas-liquid biography at a high speed
Matter, the solubility of hydrogen is improved, make hydrogen in feedstock oil be in saturation state, the catalyst in the feedstock oil and solution of saturation occurs
Reaction, remove the impurity of the sulfur-bearing nitrogen in feedstock oil；Then, reaction product is by separator 49, by primary product oil and catalysis
Agent separates, and is sent in fluid storage tanks 52；Aromatic hydrocarbons saturation intends homogeneous catalytic hydrogenation catalyst and passes through catalyst feeds
50 be added in fluid storage tanks 52 mixed with product oil be sent into second level hypergravity catalytic reactor in, at the same time, hydrogen
Then measured from raw material gas cylinder by pressure-regulating valve level pressure to the pressure needed for reaction system by mass flowmenter laggard
Enter second level supergravity reactor, carry out catalytic hydrogenation reaction.Reaction product is by separator 54, by secondary products oil and catalysis
Agent separates；A product part is sampled detection by bypass, and another part enters fluid storage tanks 57；Desulfurization removing nitric is intended homogeneous
Catalyst is added in fluid storage tanks 57 by catalyst feeds 55 and mixed with product oil by being pumped into fluid storage tanks
In 59, and fresh feed oil product is supplemented by liquid supplementation pipe；Then liquid is delivered in fluid storage tanks 52 by pump and carried out
Matter Transfer.
In certain embodiments of the present invention, the plan homogeneous catalyst is DNAcarrier free Ni-Mo sulfide catalysts.
In certain embodiments of the present invention, in first order supergravity reactor, reaction pressure 0.3-0.4MPa, temperature
Spend for 200-320 DEG C, hydrogen-oil ratio 50:1-600:1、50:1-550:1、50:1-500:1、50:1-450:1、50:1-400:1、
50:1-350:1、50:1-300:1、50:1-250:1、50:1-200:1、50:1-150:1、50:1-100:1、100:1-600:
1、100:1-550:1、100:1-500:1、100:1-450:1、100:1-400:1、100:1-350:1、100:1-300:1、
100:1-250:1、100:1-200:1 or 100:1-150:1；
In the supergravity reactor of the second level, reaction pressure 0.1-1.5MPa；Temperature is 360-420 DEG C, hydrogen-oil ratio 20:
1-100、20:1-80、20:1-60、20:1-40 or 20:1-20.
In certain embodiments of the present invention, the speed increasing ratio of the speed increaser is 1：2-7；Preferably, the speedup of speed increaser
Than for 1：2-5；It is highly preferred that the speed increasing ratio of speed increaser is 1：3-4.
In some preferred embodiments of the present invention, the micron bubble size Control of receiving is at 30nm-300 μm, or 30nm-
250 μm, or 30nm-200 μm, or 30nm-150 μm, or 30nm-100 μm, or 30nm-50 μm, or 30nm-10 μm, or 30nm-1
μm, or 100nm-300 μm, or 100nm-250 μm, or 100nm-200 μm, or 100nm-100 μm, or 100nm-1 μm.
In certain embodiments of the present invention, the control of catalytic hydrogenation reaction residence time is reacted by regulating and controlling hypergravity
What device rotating speed was realized, the rotating speed of supergravity reactor can be controlled in 200-2700rpm, or 200-2500rpm, or 200-
2000rpm, or 200-1500rpm, or 200-1000rpm, or 200-500rpm, or 400-2500rpm, or 400-2000rpm,
Or 400-1500rpm, or 400-1000rpm.Liquid phase residence time in rotor can be controlled in 50-2000ms.
Embodiment 1
As shown in Fig. 2 a kind of method of hypergravity straight-run diesel oil hydrofinishing, comprises the following steps：
Containing derivatives such as substantial amounts of sulfur impurity, nitrogen in straight-run diesel oil, sulphur removal, nitrogen are removed by way of Hydrobon
It is as follows Deng impurity, step：Structured packing catalyst and filler are loaded in the rotor of rotating packed bed reactor, its gravity
The basic framework of integer catalyzer in rotary drill reactor is foam γ-Al2O3.Rotating packed bed reactor is opened, is passed through
Frequency converter adjusts speed increaser (speed increasing ratio 1：3) reacted with rotating packed bed reactor rotating speed, reinforcing hydrogenation catalyst；
The structured packing catalyst includes basic framework, active component and Second support；The basic framework is that violet is blue or green
Stone structured packing, the active component are combined into by molybdenum or the testing sulphide of tungsten and cobalt or nickel, Second support be γ-
Al2O3；
Reaction condition is：The pressure of one-level supergravity reactor is 0.4MPa；Temperature is 300 DEG C；Hydrogen-oil ratio is 300:1.
The pressure of two level supergravity reactor is 1.5MPa；Temperature is 400 DEG C, hydrogen-oil ratio 100:1；
Under the above-described reaction conditions, gasoline parameter is as shown in table 1 before and after hypergravity hydrogenation, and the magazine derivative such as sulphur, nitrogen has
Higher removal efficiency, Cetane number improve 4 indexes；And as the magazine derivative such as the increase of rotating speed, sulphur, nitrogen removal efficiency becomes
Greatly, referring to table 2.When rotating speed exceedes maximum (top) speed in table, extrusion rate change is smaller.
Table 1：Straight-run diesel oil parameter comparison before and after hydrogenation
| Oil product title | Feedstock oil 1 | Refined oil 1 | Feedstock oil 2 | Refined oil 2 |
| Density g/cm3 | 0.8248 | 0.8145 | 0.8233 | 0.8127 |
| Sulfur content m (%) | 0.711 | 0.13 | 0.860 | 0.18 |
| Nitrogen content m (%) | 0.078 | 0.008 | 0.0646 | 0.004 |
| Cetane number | 50.7 | 54.6 | 51.0 | 55.1 |
Table 2：The influence that RPB rotating speeds are hydrogenated with to straight-run diesel oil
Contrasted with existing published supergravity reactor, such as the reactor that CN103102942A is used, its material are defeated
Send and catalyst surface is directly entered by liquid distribution trough, carry out gas-liquid-solid three-phase haptoreaction, due to the alternate mixing effect of gas-liquid
Fruit is poor, and hydrogen largely escapes, and final desulfurization degree is 65% under 1600rpm operating conditions；Denitrification percent is 50%；Unsaturated hydrocarbons
Conversion ratio 60%.
Embodiment 2
As shown in Fig. 2 a kind of method that hypergravity pyrolysis gasoline hydrogenation is refined, comprises the following steps：
Drippolene (C5—C9Component) in containing the aromatic hydrocarbons composition such as substantial amounts of benzene,toluene,xylene, be to obtain aromatic hydrocarbons
Valable starting materials；But the presence that will have unsaturated hydrocarbons in gasoline in gasoline, its cracking is simultaneously unstable, by way of catalytic hydrogenation
Unsaturated hydrocarbons in gasoline (monoolefine, diolefin and alkenyl arene) is become saturated hydrocarbons, while remove the impurity such as sulphur removal, nitrogen.
Reaction condition is：The pressure of one-level supergravity reactor is 0.42MPa；Temperature is 320 DEG C；Hydrogen-oil ratio is 300:1；
The pressure of two level supergravity reactor is 1.8MPa；Temperature is 400 DEG C, hydrogen-oil ratio 100:1.
The structured packing catalyst includes basic framework, active component and Second support；The basic framework is that violet is blue or green
Stone structured packing, the active component are combined into by molybdenum or the testing sulphide of tungsten and cobalt or nickel, Second support be γ-
Al2O3；
Under the above-described reaction conditions, gasoline parameter is as shown in table 3 before and after hypergravity hydrogenation, and hydrogenation of unsaturated hydrocarbons is converted into full
And hydrocarbon, sulphur nitrogen have higher removal efficiency；High-gravity rotating bed rotating speed is to the conversion ratio of unsaturated hydrocarbons, and the impurity such as sulphur nitrogen are taken off
The affecting laws removed, as a result as shown in table 4；With the raising of RPB rotating speeds, unsaturated conversion ratio increase, the removal efficiency of sulphur nitrogen increase
Greatly.When rotating speed exceedes maximum (top) speed in table, extrusion rate change is smaller.
Table 3 is hydrogenated with front and rear feed gasoline parameter comparison
The influence that the RPB rotating speeds of table 4 are hydrogenated with to feed gasoline
Contrasted with traditional supergravity reactor, such as the reactor that CN104419454A is used, operated in 1600rpm
Under the conditions of final desulfurization degree be 70%；Denitrification percent is 60%；Unsaturated hydrocarbons conversion ratio 65%.
Embodiment 3
As shown in figure 3, a kind of method of hypergravity straight-run diesel oil hydrofinishing, comprises the following steps：
Containing derivatives such as substantial amounts of sulfur impurity, nitrogen in straight-run diesel oil, sulphur removal, nitrogen are removed by way of Hydrobon
It is as follows Deng impurity, step：
Homogeneous catalyst will be intended and be passed through revolving bed；Rotating packed bed reactor is opened, speed increaser is adjusted by frequency converter
(speed increasing ratio 1：5) reacted with rotating packed bed reactor rotating speed, reinforcing hydrogenation catalyst；
Reaction condition is：The pressure of one-level supergravity reactor is 0.3MPa；Temperature is 280 DEG C；Hydrogen-oil ratio is 200:1.
The pressure of two level supergravity reactor is 1.2MPa；Temperature is 320 DEG C, hydrogen-oil ratio 90:1；
The plan homogeneous catalyst is DNAcarrier free Ni-Mo sulfide catalysts；
Under the above-described reaction conditions, gasoline parameter is as shown in table 5 before and after hypergravity hydrogenation, and the magazine derivative such as sulphur, nitrogen has
Higher removal efficiency, Cetane number improve 4 indexes；And as the magazine derivative such as the increase of rotating speed, sulphur, nitrogen removal efficiency becomes
Greatly, referring to table 6.When rotating speed exceedes maximum (top) speed in table, extrusion rate change is smaller.
Table 5 is hydrogenated with front and rear straight-run diesel oil parameter comparison
Table 6：The influence that RPB rotating speeds are hydrogenated with to straight-run diesel oil
| Rotating speed/rpm | S extrusion rates (%) | N extrusion rates (%) |
| 400 | 60.8 | 70.4 |
| 800 | 87.2 | 85.8 |
| 1200 | 95.7 | 92.3 |
| 1600 | 99.5 | 99.6 |
Contrasted with traditional supergravity reactor, such as the reactor that CN103102942A is used, operate bar in 1600rpm
Final desulfurization degree is 58% under part；Denitrification percent is 56%；Unsaturated hydrocarbons conversion ratio 62%.
Embodiment 4
As shown in figure 3, a kind of method of hypergravity straight-run diesel oil hydrofinishing, comprises the following steps：
Drippolene (C5—C9Component) in containing the aromatic hydrocarbons composition such as substantial amounts of benzene,toluene,xylene, be to obtain aromatic hydrocarbons
Valable starting materials.But the presence that will have unsaturated hydrocarbons in gasoline in gasoline, its cracking is simultaneously unstable, by way of catalytic hydrogenation
Unsaturated hydrocarbons in gasoline (monoolefine, diolefin and alkenyl arene) is become saturated hydrocarbons, while remove the impurity such as sulphur removal, nitrogen；It will intend
Homogeneous catalyst is passed through revolving bed；
Reaction condition is：The pressure of one-level supergravity reactor is 0.22MPa；Temperature is 270 DEG C；Hydrogen-oil ratio is 180:1.
The pressure of two level supergravity reactor is 1.4MPa；Temperature is 320 DEG C, hydrogen-oil ratio 50:1；
The plan homogeneous catalyst is DNAcarrier free Ni-Mo sulfide catalysts；
Under the above-described reaction conditions, gasoline parameter is as shown in table 7 before and after hypergravity hydrogenation, and hydrogenation of unsaturated hydrocarbons is converted into full
And hydrocarbon, sulphur nitrogen have higher removal efficiency；High-gravity rotating bed rotating speed is to the conversion ratio of unsaturated hydrocarbons, and the impurity such as sulphur nitrogen are taken off
The affecting laws removed, as a result as shown in table 8.With the raising of RPB rotating speeds, unsaturated conversion ratio increase, the removal efficiency of sulphur nitrogen increase
Greatly.When rotating speed exceedes maximum (top) speed in table, extrusion rate change is smaller.
Table 7：Feed gasoline parameter comparison before and after hydrogenation
Table 8：The influence that RPB rotating speeds are hydrogenated with to feed gasoline
Contrasted with traditional supergravity reactor, such as the reactor that CN104419454A is used, operate bar in 1600rpm
Final desulfurization degree is 72% under part；Denitrification percent is 62%；Unsaturated hydrocarbons conversion ratio 68%.
Obviously, the above embodiment of the present invention is only intended to clearly illustrate example of the present invention, and is not pair
The restriction of embodiments of the present invention.For those of ordinary skill in the field, may be used also on the basis of the above description
To make other changes in different forms.Here all embodiments can not be exhaustive.It is every to belong to this hair
Row of the obvious changes or variations that bright technical scheme is extended out still in protection scope of the present invention.
Claims (10)
1. a kind of method of hypergravity diesel oil and gasoline hydrofinishing, it is characterised in that comprise the following steps：
S1, selection supergravity reactor
From the first order supergravity reactor and second level supergravity reactor of series connection；The supergravity reactor includes electricity
Machine, main shaft, rotor, housing and liquid distribution trough；The main shaft of the motor output end is extend into housing through housing bottom, institute
State rotor and be fixed on main shaft top；The super-gravity device also includes secondary axes, speed increaser, output shaft of the speed increaser and feed cavity；Institute
State the top that feed cavity is arranged on housing, the bottom connection liquid distribution trough of feed cavity；The main shaft passes through secondary axes and speed increaser
It is fixedly connected, the output shaft of the speed increaser is extend into feed cavity through feed cavity bottom；The charging of the output shaft of the speed increaser
Intracavitary part is provided with agitator；The feed cavity is provided with first gas entrance, liquid inlet and catalyst inlet, the shell
Body bottom is provided with gas liquid outlet；The housing upper is provided with gas inlet-outlet, and the housing side is provided with second gas entrance；
S2, first order supergravity reactor motor is started, speed increaser rotation is driven, so as to drive the agitator superelevation in feed cavity
Speed rotation；Efficiently mixed gas-liquid two-phase is carried out in hydrogen and feedstock oil input feed cavity, make slightly solubility hydrogen in feedstock oil
Be dispersed into it is substantial amounts of receive micron bubble, solubility of the hydrogen in feedstock oil reaches supersaturation, forms gas-liquid mixture；By gas-liquid
Mixture delivers into progress hydrogenation desulfurization and denitrogenation reaction in the rotor containing catalyst by liquid distribution trough, obtains removing and contains
The feedstock oil of sulphur nitrogen impurity；
S3, second level supergravity reactor motor is started, speed increaser rotation is driven, so as to drive the agitator superelevation in feed cavity
Speed rotation；Efficiently mixed gas-liquid two-phase is carried out in the feedstock oil input feed cavity of hydrogen and removing sulfur-bearing nitrogen impurity, make indissoluble
Property hydrogen be dispersed into the feedstock oil of removing sulfur-bearing nitrogen impurity it is substantial amounts of receive micron bubble, solubility of the hydrogen in feedstock oil
Reach supersaturation, form gas-liquid mixture；Gas-liquid mixture is delivered into the rotor containing catalyst by liquid distribution trough
Middle carry out hydrogenation reaction of unsaturated hydrocarbon；
S4, reaction product and unreacted hydrogen leave reactor by liquid outlet and gas inlet-outlet respectively.
2. the method for hypergravity diesel oil and gasoline hydrofinishing according to claim 1, it is characterised in that：The speed increaser
Speed increasing ratio is 1：2-500；Preferably, the speed increasing ratio of speed increaser is 1：4-25；It is highly preferred that the speed increasing ratio of speed increaser is 1：5-
15。
3. the method for hypergravity diesel oil and gasoline hydrofinishing according to claim 1, it is characterised in that：The agitator
Material includes titanium alloy, chromium-base alloy, dual phase steel or ceramics.
4. the method for hypergravity diesel oil and gasoline hydrofinishing according to claim 1, it is characterised in that：The catalyst bag
Include structured packing catalyst or intend homogeneous catalyst.
5. the method for hypergravity diesel oil and gasoline hydrofinishing according to claim 4, it is characterised in that：The structured packing
Catalyst includes basic framework, active component and Second support；The basic framework is cordierite structured packing, the activearm
Divide and be combined into by molybdenum or the testing sulphide of tungsten and cobalt or nickel, Second support is γ-Al2O3。
6. the method for hypergravity diesel oil and gasoline hydrofinishing according to claim 1, it is characterised in that：The plan is homogeneously urged
Agent is DNAcarrier free Ni-Mo sulfide catalysts.
7. the method for hypergravity diesel oil and gasoline hydrofinishing according to claim 5, it is characterised in that：In step S2,
In first order supergravity reactor, reaction pressure 0.3-0.5MPa, temperature is 230-350 DEG C, hydrogen-oil ratio 100:1-800:
1、100:1-700:1、100:1-600:1、100:1-500:1、100:1-400:1、100:1-300:1、100:1-200:1、
200:1-800:1、200:1-700:1、200:1-600:1、200:1-500:1、200:1-400:1、200:1-300:1、300:
1-800:1、300:1-700:1、300:1-600:1、300:1-500:1、300:1-400:1、500:1-800:1、600:1-
800:1 or 700:1-800:1；
In step S3, in the supergravity reactor of the second level, reaction pressure 0.1-2MPa, temperature is 360-480 DEG C, hydrogen-oil ratio
20:1-200:1、20:1-180:1、20:1-160:1、20:1-140:1、20:1-120:1、20:1-100:1、20:1-80:1、
20:1-60:1、20:1-40:1、50:1-200:1、50:1-180:1、50:1-160:1、50:1-140:1、50:1-120:1、
50:1-100:1、50:1-80:1、80:1-200:1、80:1-180:1、80:1-160:1、80:1-140:1、80:1-120:1、
80:1-100:1、100:1-200:1、100:1-180:1、100:1-160:1、100:1-140:1 or 100:1-120:1.
8. the method for hypergravity diesel oil and gasoline hydrofinishing according to claim 6, it is characterised in that：In step S2,
In first order supergravity reactor, reaction pressure 0.3-0.4MPa, temperature is 200-320 DEG C, hydrogen-oil ratio 50:1-600:1、
50:1-550:1、50:1-500:1、50:1-450:1、50:1-400:1、50:1-350:1、50:1-300:1、50:1-250:1、
50:1-200:1、50:1-150:1、50:1-100:1、100:1-600:1、100:1-550:1、100:1-500:1、100:1-
450:1、100:1-400:1、100:1-350:1、100:1-300:1、100:1-250:1、100:1-200:1 or 100:1-150:
1；
In step S3, in the supergravity reactor of the second level, reaction pressure 0.1-1.5MPa；Temperature is 360-420 DEG C, hydrogen oil
Than 20:1-100、20:1-80、20:1-60、20:1-40 or 20:1-20.
9. the method for hypergravity diesel oil and gasoline hydrofinishing according to claim 1, it is characterised in that：Micron gas of receiving
Size Control is steeped at 30nm-300 μm, or 30nm-250 μm, or 30nm-200 μm, or 30nm-150 μm, or 30nm-100 μm, or
30nm-50 μm, or 30nm-10 μm, or 30nm-1 μm, or 100nm-300 μm, or 100nm-250 μm, or 100nm-200 μm, or
100nm-100 μm, or 100nm-1 μm.
10. the method for hypergravity diesel oil and gasoline hydrofinishing according to claim 1, it is characterised in that：Hypergravity reacts
The rotating speed of device can be controlled in 200-2700rpm, or 200-2500rpm, or 200-2000rpm, or 200-1500rpm, or 200-
1000rpm, or 200-500rpm, or 400-2500rpm, or 400-2000rpm, or 400-1500rpm, or 400-1000rpm；
Liquid phase residence time in rotor can be controlled in 50-2000ms.
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| CN114849595A (en) * | 2021-02-04 | 2022-08-05 | 北京化工大学 | Hypergravity heterogeneous catalytic reactor device and application thereof |
| CN116790285A (en) * | 2022-03-15 | 2023-09-22 | 中国石油天然气股份有限公司 | Hypergravity enhanced diesel hydrofining method and device |
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