CN103861544A - Impinging stream reactor and application thereof - Google Patents
Impinging stream reactor and application thereof Download PDFInfo
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- CN103861544A CN103861544A CN201210427702.9A CN201210427702A CN103861544A CN 103861544 A CN103861544 A CN 103861544A CN 201210427702 A CN201210427702 A CN 201210427702A CN 103861544 A CN103861544 A CN 103861544A
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Abstract
The invention discloses an impinging stream reactor, which comprises a reactor housing, a reaction impinging tank, and a liquid transfer pump. The reaction impinging tank is arranged in the reactor housing, the impinging tank is openmouthed, the guide cylinders are symmetrically arranged in the impinging tank, the guide cylinder is passed through a liquid feed line of the reactor housing and is connected to the liquid transfer pump, an air intake is arranged on a top cover of the reactor housing, a lower cover is a liquid holding tank with a taper structure, and an extraction port is arranged on the holding tank. In the impinging stream reactor, an oil phase extraction port, a water phase extraction port and a circulation solution extraction port are arranged on the holding tank, and are respectively arranged at an oil phase zone of the holding tank, a water phase zone and a tone top position of the holding tank. The temperature and pressure in the impinging stream reactor is easy to be controlled, the shocking of the reactor due to impinging reaction is reduced, and the impinging stream reactor is suitable for oil product oxidation desulphurization 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 and application thereof that is applicable to oxidation sweetening of oil product.
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 just gradually by people are paid close attention to, especially more and more stricter to the restriction of motor vehicle fuel, be embodied in the restriction to Sulfur content in Fuel Oil, nitrogen, alkene, benzene and arene content, this ball Oil Refining Industry of will demanding perfection constantly improves, innovates existing technique, develops some advanced technologies and produces clean fuel.Therefore produce clean fuel and be at present so long-time from now in the development trend of petroleum refining industry.
At present, vapour, Diesel fuel desulfurization technologies are divided into hydrodesulfurization and non-hydrodesulfurization, and hydrodesulfurization is more difficult for removing of condensed ring thiophene class sulfur-containing compound and derivative thereof, and need higher temperature and pressure and catalytic hydroprocessing environment.Non-hydrodesulfurization mainly comprises adsorption desulfurize, biological desulphurization, oxidation sweetening, pickling caustic wash desulfuration and membrane separation technique etc.
Conventionally 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 is extracted, thereby reach the object of desulfurization, obtained reasonable effect.
Organic sulfur in coker gasoline is mainly alkylbenzene bithiophene, dibenzothiophenes and methyldibenzothiophene, also contains a small amount of condensed ring organic sulfur, and these are all the extremely difficult organosulfur compounds removing 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 that is difficult to remove for catalytic hydrogenation has good desulfurized effect, is a very practical desulfur technology.Compared with traditional hydrodesulfurizationprocess process, the method have principle simple, invest little, desulfuration efficiency high, be suitable for the enterprise of medium-sized and small enterprises or no hydrogen resource.
CN200510045867.X, CN200610146027.7 disclose respectively the oxidation desulfurizing method of distillate and diesel oil.The method comprises that distillate feedstock or diesel raw material and hydrogen peroxide are in the situation that comprising that rudimentary organic acid catalyst exists, and reacts in as impact flow reactor at the efficient mass transfer reactor with strengthening turbulent flow inner member.In this efficient mass transfer reactor, reactant can fully mix and at short notice because intermolecular effective collision reacts fast, improved significantly reaction efficiency, in the time obtaining identical desulfurization result, the more conventional stirring reactor of reaction condition relaxes more.Compared with existing distillate or diesel oxidation desulfurizing technology, this process using impact flow reactor can be processed more high sulfur content and raw material more inferior, obtains low-sulphur fuel.But the impact flow reactor adopting in said method is the same with most of published impact flow reactors, generally adopt liquid phase to carry out controlled pressure, pressure control ratio is more difficult, and the material after shock and reactor wall collision cause reactor vibrations, and are that heat energy elevates the temperature by kinetic transformation.
Summary of the invention
For the deficiencies in the prior art, the invention provides a kind of impact flow reactor and application thereof.The temperature of this impact flow reactor and pressure are easy to control, and have reduced the reactor vibrations that cause after knock-on reaction, are applicable in oxidation sweetening of oil product reaction.
A kind of impact flow reactor, comprise shell of reactor, reaction shock groove, liquid delivery pump, described reaction shock groove is arranged on the inside of shell of reactor, it is uncovered clashing into groove, clash into the symmetrical guide shell of installing in groove, guide shell, by being connected with liquid delivery pump through the fluid-carrying lines of shell of reactor, covering on described shell of reactor and is provided with air inlet, lower cover is the liquid collection trough of pyramidal structure, and feeder is provided with extraction mouth.
In impact flow reactor of the present invention, feeder is provided with oil phase extraction mouth, water extraction mouth and circulation fluid extraction mouth, is separately positioned on the vertex of a cone place of oil phase district, water district and the feeder of feeder.
In impact flow reactor of the present invention, fluid-carrying lines is provided with heat exchanger and is used for controlling reaction temperature.
The application of above-mentioned impact flow reactor in oxidation sweetening of oil product reaction, 30～300 DEG C of reaction temperatures, preferably 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, preferably 5～10min.
The application of impact flow reactor of the present invention in oxidation sweetening of oil product reaction, described oil product is diesel oil, gasoline, solvent wet goods.
The application of impact flow reactor of the present invention in oxidation sweetening of oil product reaction, adopt intermittent operation or continued operation all can, preferably continous way operation.
The application of impact flow reactor of the present invention in oxidation sweetening of oil product reaction, when intermittent operation, first with a liquid delivery pump, appropriate oil product, hydrogen peroxide-formic acid mixed liquor are squeezed in reactor, make raw material be warming up to reaction temperature by the heat exchanger on fluid-carrying lines, air inlet passes into after gas is adjusted 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 after reaction finishes to leave standstill, takes out product from oil phase extraction mouth, water extraction mouth.When intermittent cyclic operation, improve the front pressure of pump, can adopt low-power pump, reduced energy consumption.
The application of impact flow reactor of the present invention in oxidation sweetening of oil product reaction, when continued operation, first air inlet passes into gas and adjusts pressure, unlatching double pump is squeezed into shock groove by oil product, hydrogen peroxide-formic acid mixed liquor by heat exchanger and is reacted, reactant liquor overflows shock groove and falls into liquid collection trough, from clashing into the continuous extraction oil-phase product of oil phase extraction mouth of groove, water extraction mouth is extraction water-phase product (measuring fewer) intermittently, and water-phase product also can be through the salty shock groove that newly loops back of circulation fluid extraction.
Compared with prior art, a kind of impact flow reactor of the present invention and application tool thereof have the following advantages:
(1) impact flow reactor of the present invention distinguishes knock-on reaction district and liquid collection, and uncovered knock-on reaction groove is placed in an airtight container, realize gas phase control reaction pressure, reduced in course of reaction because of liquid and reactor directly clash into pressure, the fluctuation of temperature and the vibrations of device, improved collision efficiency;
(2) impact flow reactor of the present invention is applied to and in oxidation sweetening of oil product reaction, has reaction condition and be easy to control, and desulfuration efficiency is high, and reaction unit can move for a long time stably.
Brief description of the drawings
Fig. 1 is the present invention's impact flow reactor structural representation used and flow process.
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), comprise shell of reactor 1, groove 2 is clashed in reaction, liquid delivery pump 4, described reaction shock groove 2 is arranged on the inside of shell of reactor 1, it is uncovered clashing into groove 2, clash into the interior symmetrical guide shell 3 of installing of groove 2, 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, on described shell of reactor 1, cover and be provided with air inlet 7, lower cover is that liquid collection trough 8 feeders 8 of pyramidal structure are provided with oil phase extraction mouth 13, water extraction mouth 14 and circulation fluid extraction mouth, be separately positioned on the oil phase district 11 of feeder, the vertex of a cone place of water district 12 and feeder 8.
Illustrate the effect of impact flow reactor of the present invention in oxidation desulfur reaction below in conjunction with embodiment.It is 6L that the impact flow reactor adopting clashes into cell body long-pending (reaction effective volume); Experimental raw is northern Suzhou blended diesel, and urging bavin and the mass ratio of 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%.Squeeze into hydrogen peroxide in oil product in reactor, hydrogen peroxide-formic acid mixed liquor and be sulphur molal quantity in diesel oil 6 times, in hydrogen peroxide-formic acid system, the mass fraction of hydrogen peroxide is 2.5%, all the other formic acid that are 85% for mass concentration; Reaction pressure maintains with the nitrogen being filled with.
Embodiment 1 ~ 5(continued operation)
From the continuous extraction product of oil phase extraction mouth, by its cool to room temperature, to its wash successively, alkali cleaning, washing, adsorption desulfurize processing, to slough the polarity sulfide (being mainly the corresponding sulfone compound of the oxidized generation of thiophenes in diesel oil) that oxidation generates, sample analysis, in oil sample, sulfur content is coulometry quantitative analysis.Reaction condition and the results are shown in Table 1.In whole course of reaction, reactor is shockproof, and reaction pressure and temperature can realize stably and controlling.
Table 1
| Sequence number | Reaction pressure/MPa | Time of staying time/min | Reaction temperature (T)/DEG C | Sulphur concentration (Cs)/μ gg 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 disclosed reactor of CN200510045867.X and method, reactor vibrations obviously, reaction pressure and reaction temperature fluctuation are larger, control that cannot be relatively accurate, when average response pressure is 1.5 MPa, 92.5 DEG C of average reaction temperature, the time of staying, while being similarly 7min, is reacted sulphur concentration 425 μ gg in rear oil
-1.
Claims (9)
1. an impact flow reactor, it is characterized in that: this reactor comprises shell of reactor, reaction shock groove, liquid delivery pump, described reaction shock groove is arranged on the inside of shell of reactor, it is uncovered clashing into groove, clash into the symmetrical guide shell of installing in groove, guide shell, by being connected with liquid delivery pump through the fluid-carrying lines of shell of reactor, covering on described shell of reactor and is provided with air inlet, lower cover is the liquid collection trough of pyramidal structure, and feeder is provided with extraction mouth.
2. impact flow reactor according to claim 1, is characterized in that: feeder is provided with oil phase extraction mouth, water extraction mouth and circulation fluid extraction mouth, is separately positioned on the vertex of a cone place of oil phase district, water district and the feeder of feeder.
3. impact flow reactor according to claim 1, is characterized in that: fluid-carrying lines is provided with heat exchanger and is used for controlling reaction temperature.
4. the application of impact flow reactor in oxidation sweetening of oil product reaction described in claim 1, is characterized in that: 30～300 DEG C of reaction temperatures, reaction pressure 0.01～10MPa, reaction time 1.5～30min.
5. application according to claim 4, is characterized in that: reaction temperature, reaction pressure 0.3～1.0MPa, reaction time 5～10min.
6. application according to claim 4, is characterized in that: described oil product is diesel oil, gasoline, solvent wet goods.
7. application according to claim 4, is characterized in that: adopt intermittent operation or continued operation all can.
8. according to the application described in claim 4 or 7, it is characterized in that: when intermittent operation, first with a liquid delivery pump, appropriate oil product, hydrogen peroxide-formic acid mixed liquor are squeezed in reactor, make raw material be warming up to reaction temperature by the heat exchanger on fluid-carrying lines, air inlet passes into after gas is adjusted 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 after reaction finishes to leave standstill, takes out product from oil phase extraction mouth, water extraction mouth.
9. according to the application described in claim 4 or 7, it is characterized in that: when continued operation, first air inlet passes into gas and adjusts pressure, unlatching double pump is squeezed into shock groove by oil product, hydrogen peroxide-formic acid mixed liquor by heat exchanger and is reacted, reactant liquor overflows shock groove and falls into liquid collection trough, from clashing into the continuous extraction oil-phase product of oil phase extraction mouth of groove, intermittently extraction water-phase product or through the salty shock groove that newly loops back of circulation fluid extraction of water extraction mouth.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110882673A (en) * | 2018-09-07 | 2020-03-17 | 上海工程技术大学 | Chemical reaction method and device based on impinging stream |
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| CN101235136A (en) * | 2008-02-28 | 2008-08-06 | 宁波万华聚氨酯有限公司 | Process for preparing polycarbonate |
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- 2012-12-17 CN CN201210427702.9A patent/CN103861544B/en active Active
Patent Citations (10)
| 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 |
| CN1814344A (en) * | 2005-02-05 | 2006-08-09 | 中国石油化工股份有限公司 | Impact flow reactor for liquid-phase reaction |
| CN1814709A (en) * | 2005-02-05 | 2006-08-09 | 中国石油化工股份有限公司 | Cut-fracted oil oxidation desulfurizing method |
| WO2007038605A2 (en) * | 2005-09-27 | 2007-04-05 | Greenfuel Technologies Corporation | Flue gas scrubbing with a multifunction impinging stream gas-liquid reactor |
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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 |
| CN101235136A (en) * | 2008-02-28 | 2008-08-06 | 宁波万华聚氨酯有限公司 | Process for preparing polycarbonate |
| CN201182916Y (en) * | 2008-04-30 | 2009-01-21 | 伍沅 | Irrotational impact-flow heat exchange type crystallizer |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110882673A (en) * | 2018-09-07 | 2020-03-17 | 上海工程技术大学 | Chemical reaction method and device based on impinging stream |
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