CN103861544B - A kind of impact flow reactor and application thereof - Google Patents
A kind of impact flow reactor and application thereof Download PDFInfo
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- CN103861544B CN103861544B CN201210427702.9A CN201210427702A CN103861544B CN 103861544 B CN103861544 B CN 103861544B CN 201210427702 A CN201210427702 A CN 201210427702A CN 103861544 B CN103861544 B CN 103861544B
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Abstract
Disclosure one impact flow reactor, groove, liquid delivery pump is clashed into including shell of reactor, reaction, described reaction is clashed into groove and is arranged on the inside of shell of reactor, it is uncovered for clashing into groove, clashing in groove and be symmetrically installed guide shell, guide shell is connected with liquid delivery pump by the fluid-carrying lines through shell of reactor, described shell of reactor covers and is provided with air inlet, lower cover is the liquid collection trough of pyramidal structure, and collecting tank is provided with extraction mouth.In impact flow reactor of the present invention, collecting tank is provided with oil phase extraction mouth, aqueous phase extraction mouth and circulation fluid extraction mouth, is separately positioned on the vertex of a cone place of the oil phase district of collecting tank, aqueous phase district and collecting tank.Temperature and the pressure of this impact flow reactor are easily controllable, the reactor vibrations caused after reducing knock-on reaction, it is adaptable in oxidation sweetening of oil product reaction.
Description
Technical field
The present invention relates to a kind of impact flow reactor and application thereof, relate in particular to a kind of impact flow reactor suitable in oxidation sweetening of oil product and application thereof.
Background technology
Along with the enhancing of human environment consciousness and perfecting gradually of environmental regulation, produce low-sulfur and super-low sulfur vapour, diesel oil are concerned just gradually, especially the restriction of motor vehicle fuel is more and more stricter, it is embodied in the restriction to Sulfur content in Fuel Oil, nitrogen, alkene, benzene and arene content, existing technique is constantly improved, innovates by this ball Oil Refining Industry of will demanding perfection, and develops some advanced technologies and produces cleaning fuel.Therefore the development trend of petroleum refining industry in cleaning fuel is current or even is long-time from now on is produced.
At present, vapour, Diesel fuel desulfurization technologies are divided into hydrodesulfurization and non-hydrodesulfurization, and hydrodesulfurization is relatively difficult for the elimination of condensed ring thiophene class sulfur-containing compound and derivant thereof, and need higher temperature and pressure and catalytic hydroprocessing environment.Non-hydrodesulfurization mainly includes absorption desulfurization, biological desulphurization, oxidation sweetening, pickling caustic wash desulfuration and membrane separation technique etc..
Generally described oxidative desulfurization techniques is using hydrogen peroxide, formic acid as oxidant, phosphomolybdic acid quaternary ammonium salt is catalyst, thiophene-type sulfide in oil product is oxidized to sulfone class, then according to similar compatibility principle, employing furfural is extractant, sulfone class in oil product being extracted, thus reaching the purpose of desulfurization, achieving reasonable effect.
Organic sulfur in coker gasoline is mainly alkyl benzothiophenes, dibenzothiophenes and methyldibenzothiophene, and possibly together with a small amount of condensed ring organic sulfur, these are all the organosulfur compounds of extremely difficult elimination in hydrodesulfurization.Compared with traditional hydrodesulfurizationprocess process, novel oxidation desulfurizing method can carry out under low-temp low-pressure, does not expend hydrogen, and equipment investment is less, the oil-source rock correlation being difficult to remove for catalytic hydrogenation has good desulfurized effect, is a very practical desulfurization technology.Compared with conventional hydrodesulfurization method, the method has that principle is simple, invest little, desulfuration efficiency high, is suitable for medium-sized and small enterprises or the enterprise of no hydrogen resource.
CN200510045867.X, CN200610146027.7 individually disclose the oxidation desulfurizing method of distillate and diesel oil.The method includes distillate feedstock or diesel raw material and hydrogen peroxide and deposits in case including rudimentary organic acid catalyst, reacts in the efficient mass transfer reactor such as impact flow reactor with strengthening turbulent flow inner member.In this efficient mass transfer reactor, reactant can be sufficiently mixed uniformly and at short notice owing to intermolecular effective collision quickly reacts, improve reaction efficiency significantly, when obtaining identical desulfurization results, the more conventional stirring reactor of reaction condition relaxes more.Compared with existing distillate or diesel oxidation desulfurizing technology, this technique adopts impact flow reactor can process more high sulfur content and raw material more inferior, obtains low-sulphur fuel.But the impact flow reactor adopted in said method is the same with most of published impact flow reactors, commonly used liquid phase controls pressure, Stress control is relatively difficult, and material after shock and reactor wall collision cause reactor to shake, and converts kinetic energy into heat energy and elevate the temperature.
Summary of the invention
For the deficiencies in the prior art, the present invention provides a kind of impact flow reactor and application thereof.Temperature and the pressure of this impact flow reactor are easily controllable, the reactor vibrations caused after reducing knock-on reaction, it is adaptable in oxidation sweetening of oil product reaction.
A kind of impact flow reactor, groove, liquid delivery pump is clashed into including shell of reactor, reaction, described reaction is clashed into groove and is arranged on the inside of shell of reactor, it is uncovered for clashing into groove, clashing in groove and be symmetrically installed guide shell, guide shell is connected with liquid delivery pump by the fluid-carrying lines through shell of reactor, described shell of reactor covers and is provided with air inlet, lower cover is the liquid collection trough of pyramidal structure, and collecting tank is provided with extraction mouth.
In impact flow reactor of the present invention, collecting tank is provided with oil phase extraction mouth, aqueous phase extraction mouth and circulation fluid extraction mouth, is separately positioned on the vertex of a cone place of the oil phase district of collecting tank, aqueous phase district and collecting tank.
In impact flow reactor of the present invention, fluid-carrying lines is provided with heat exchanger for controlling reaction temperature.
The application in oxidation sweetening of oil product reacts of the above-mentioned impact flow reactor, reaction temperature 30～300 DEG C, it is preferable that 50～150 DEG C, reaction pressure 0.01～10MPa, preferably 0.3～1.0MPa, reaction time (to clash into the stereometer of groove) 1.5～30min, it is preferable that 5～10min.
The impact flow reactor of the present invention application in oxidation sweetening of oil product reacts, described oil product is diesel oil, gasoline, solvent wet goods.
The impact flow reactor of the present invention application in oxidation sweetening of oil product reacts, adopts intermittent operation or continuous operation, it is preferable that continuous way operates.
The impact flow reactor of the present invention application in oxidation sweetening of oil product reacts, first with a liquid delivery pump, appropriate oil product, hydrogen peroxide-formic acid mixed liquor are squeezed in reactor during intermittent operation, raw material is made to be warming up to reaction temperature by the heat exchanger on fluid-carrying lines, air inlet passes into after gas adjusts pressure and opens double pump, reactant liquor is sent into shock groove from circulation fluid extraction mouth through liquid delivery pump and is reacted, and reaction takes out product from oil phase extraction mouth, aqueous phase extraction mouth after terminating standing.During intermittent cyclic operation, improve pressure before pump, it is possible to adopt low-power pump, reduce energy consumption.
The impact flow reactor of the present invention application in oxidation sweetening of oil product reacts, during continuous operation, first air inlet passes into gas and adjusts pressure, open double pump oil product, hydrogen peroxide-formic acid mixed liquor are squeezed into shock groove by heat exchanger and reacted, reactant liquor overflows shock groove and falls into liquid collection trough, from the continuous extraction oil-phase product of oil phase extraction mouth clashing into groove, aqueous phase extraction mouth interval extraction water-phase product (measuring fewer), water-phase product can also recirculate back to clash into groove through circulation fluid extraction mouth.
Compared with prior art, one impact flow reactor of the present invention and application thereof have the advantage that
(1) knock-on reaction district is separated by impact flow reactor of the present invention with liquid collection region, and uncovered knock-on reaction groove is placed in a sealing container, achieve gas phase and control reaction pressure, reduce in course of reaction because of liquid and reactor directly clash into pressure, the fluctuation of temperature and device vibrations, improve collision efficiency；
(2) impact flow reactor of the present invention is applied in oxidation sweetening of oil product reaction that to have reaction condition easily controllable, and desulfuration efficiency is high, and reaction unit can the operation of long-term smooth.
Accompanying drawing explanation
Fig. 1 is impact flow reactor structural representation and flow process used by the present invention.
Detailed description of the invention
As shown in Figure 1, a kind of impact flow reactor (some has symmetrical structure and does not mark completely), including shell of reactor 1, groove 2 is clashed in reaction, liquid delivery pump 4, described reaction is clashed into groove 2 and is arranged on the inside of shell of reactor 1, it is uncovered for clashing into groove 2, clash in groove 2 and be symmetrically installed guide shell 3, guide shell 3 is connected with liquid delivery pump 4 by the fluid-carrying lines 5 through shell of reactor 1, fluid-carrying lines 6 is provided with heat exchanger 6, described shell of reactor 1 covers and is provided with air inlet 7, liquid collection trough 8 collecting tank 8 that lower cover is pyramidal structure is provided with oil phase extraction mouth 13, aqueous phase extraction mouth 14 and circulation fluid extraction mouth, it is separately positioned on the oil phase district 11 of collecting tank, the vertex of a cone place of aqueous phase district 12 and collecting tank 8.
The impact flow reactor of the present invention application effect in oxidation sweetening reacts is illustrated below in conjunction with embodiment.It is 6L that the impact flow reactor adopted clashes into sump volume (reaction effective volume)；Experimental raw is northern Suzhou blended diesel, and the mass ratio urging bavin and straight bavin is 1:1.5, and miscella sulfur-bearing is 1600 μ g/g；Formic acid: Tianjin great Mao chemical reagent factory, purity is 85%；Hydrogen peroxide: Tianjin great Mao chemical reagent factory, purity is 35%.Squeezing into hydrogen peroxide in the oil product in reactor, hydrogen peroxide-formic acid mixed liquor is 6 times of sulfur molal quantity in diesel oil, and in hydrogen peroxide-formic acid system, the mass fraction of hydrogen peroxide is 2.5%, and all the other are the formic acid of 85% for mass concentration；The reaction pressure nitrogen being filled with maintains.
Embodiment 1 ~ 5(operates continuously)
From the continuous extraction product of oil phase extraction mouth, it is cooled to room temperature, it is sequentially carried out washing, alkali cleaning, washing, absorption desulfurization process, to slough the polarity sulfide (mainly the thiophenes corresponding sulfone compound of oxidized generation in diesel oil) that oxidation generates, sample analysis, in oil sample, sulfur content is coulometry quantitative analysis.The condition of reaction and result are in Table 1.In whole course of reaction, reactor is shockproof, and reaction pressure and temperature can realize stable control.
Table 1
| Sequence number | Reaction pressure/MPa | The time of staying time/min | Reaction temperature (T)/DEG C | Sulphur concentration (Cs)/μ g g in oil after reaction-1 |
| Embodiment 1 | 0.2 | 5 | 60 | 514 |
| Embodiment 2 | 0.4 | 8 | 70 | 499 |
| Embodiment 3 | 0.6 | 9 | 80 | 460 |
| Embodiment 4 | 0.8 | 7 | 90 | 388 |
| Embodiment 5 | 1.0 | 6 | 100 | 318 |
Comparative example 1
Adopt the reactor disclosed in CN200510045867.X and method, reactor vibrations are substantially, reaction pressure and reaction temperature fluctuation are bigger, control that cannot be relatively accurate, when average response pressure is 1.5MPa, average reaction temperature 92.5 DEG C, when the time of staying is similarly 7min, sulphur concentration 425 μ g g in oil after reaction-1。
Claims (9)
1. an impact flow reactor, it is characterized in that: this reactor includes shell of reactor, groove, liquid delivery pump are clashed in reaction, described reaction is clashed into groove and is arranged on the inside of shell of reactor, it is uncovered for clashing into groove, clashing in groove and be symmetrically installed guide shell, guide shell is connected with liquid delivery pump by the fluid-carrying lines through shell of reactor, described shell of reactor covers and is provided with air inlet, lower cover is the liquid collection trough of pyramidal structure, and collecting tank is provided with extraction mouth.
2. impact flow reactor according to claim 1, it is characterized in that: collecting tank is provided with oil phase extraction mouth, aqueous phase extraction mouth and circulation fluid extraction mouth, oil phase extraction mouth is arranged on the oil phase district of collecting tank, aqueous phase extraction mouth is arranged on aqueous phase district and circulation fluid extraction mouth is arranged on the vertex of a cone place of collecting tank.
3. impact flow reactor according to claim 1, it is characterised in that: fluid-carrying lines is provided with heat exchanger for controlling reaction temperature.
4. the application in oxidation sweetening of oil product reacts of the impact flow reactor described in claim 1, it is characterised in that: reaction temperature 30～300 DEG C, reaction pressure 0.01～10MPa, reaction time 1.5～30min.
5. application according to claim 4, it is characterised in that: reaction temperature 30～150 DEG C, reaction pressure 0.3～1.0MPa, reaction time 5～10min.
6. application according to claim 4, it is characterised in that: described oil product is diesel oil, gasoline, solvent naphtha.
7. application according to claim 4, it is characterised in that: adopt intermittent operation or continuous operation.
8. the application according to claim 4 or 7, it is characterized in that: first with a liquid delivery pump, appropriate oil product, hydrogen peroxide-formic acid mixed liquor are squeezed in reactor during intermittent operation, raw material is made to be warming up to reaction temperature by the heat exchanger on fluid-carrying lines, air inlet passes into after gas adjusts pressure and opens double pump, reactant liquor is sent into shock groove from circulation fluid extraction mouth through liquid delivery pump and is reacted, and reaction takes out product from oil phase extraction mouth, aqueous phase extraction mouth after terminating standing.
9. the application according to claim 4 or 7, it is characterized in that: during continuous operation, first air inlet passes into gas and adjusts pressure, open double pump oil product, hydrogen peroxide-formic acid mixed liquor are squeezed into shock groove by heat exchanger and reacted, reactant liquor overflows shock groove and falls into liquid collection trough, from clash into groove the continuous extraction oil-phase product of oil phase extraction mouth, aqueous phase extraction mouth interval extraction water-phase product or through circulation fluid extraction mouth recirculate back to clash into groove.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1914123A (en) * | 2004-02-03 | 2007-02-14 | 松江土建株式会社 | Gas-liquid dissolution apparatus |
| CN2772612Y (en) * | 2005-02-05 | 2006-04-19 | 中国石油化工股份有限公司 | Impact fluid reactor for liquid-phase reaction |
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| CN1951915A (en) * | 2006-11-10 | 2007-04-25 | 中国日用化学工业研究院 | Sulfur trioxide gas jet sulfonation process and device for bisalkyl benzene |
| CN1973989A (en) * | 2006-11-10 | 2007-06-06 | 中国日用化学工业研究院 | SO3 gas jetting sulfonation reactor and process |
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