CN106179146A - A kind of percussion flow heterophase reactor - Google Patents
A kind of percussion flow heterophase reactor Download PDFInfo
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- CN106179146A CN106179146A CN201510296607.3A CN201510296607A CN106179146A CN 106179146 A CN106179146 A CN 106179146A CN 201510296607 A CN201510296607 A CN 201510296607A CN 106179146 A CN106179146 A CN 106179146A
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Abstract
The present invention is a kind of percussion flow heterophase reactor, relates to Liquid-liquid mixing heterogeneous reaction.This reactor by raw material injection premixed device by high viscosity and low viscosity fluid at lower temperature, be uniformly mixed into low viscous emulsion in the short time, spray ring-shaped liquid film by the nozzle at high speeds of multiple injection knock-on reaction devices again and clash into strengthening reaction mutually, make reaction the most fully carry out.The percussion flow heterophase reactor that the present invention is introduced, simple in construction, there is no mixing component, be difficult to leakage, reaction liquid contact area is big, can realize the rapidly and efficiently hybrid reaction of immiscible fluid in large-scale production, and the selectivity of product is high.Can be applicable to fluid viscosity in the industrial process such as fine chemistry industry, petrochemical industry, pharmaceuticals industry, biochemical industry compared with big, liquid-liquid is immiscible, the reaction unit of quick hybrid reaction between liquid, especially liquid acid catalyzing iso-butane alkane alkylated reaction.
Description
Technical field
The present invention relates to Liquid-liquid mixing heterogeneous reaction, particularly to fluid viscosity compared with big, the immiscible heterogeneous reaction of liquid-liquid, especially
It is concentrated sulphuric acid or the reaction of ionic liquid-catalyzed isobutane alkylation, belongs to the fields such as petrochemical industry, environmental project, pharmaceutical engineering.
Background technology
Along with the quick growth of China's automobile pollution, the impact of atmospheric pollution is increased by exhaust emissions day by day, and oil quality is shadow
Ring the key factor of motor vehicle exhaust emission, accelerate to advance oil quality upgrading, how to produce the environmental protection mark meeting country's increasingly stringent
Accurate clean gasoline blend component, is the Major Strategic Demand of national resources environment/green manufacturing.Alkylate oil and other component phase
Ratio, not olefin-containing and aromatic hydrocarbons, hardly sulfur-bearing, and there is higher octane number and relatively low vapour pressure, it is a kind of ideal
Clean gasoline, advantage is apparent.China's alkylate oil produces and is faced with unprecedented opportunity to develop and space at present.
Mixing of liquid acid catalyzing iso-butane alkane alkylated reaction, concentrated sulphuric acid and the carbon four such as the concentrated sulphuric acid of current commercial Application or ionic liquid
Close effect and directly affect quality and the yield of alkylate oil.Reaction temperature reduction advantageously reduces side reaction, improves octane number.But
It is concentrated sulphuric acid or the increase of ionic liquid viscosity at low temperatures, affects iso-butane to the mass transfer of acid phase so that reaction efficiency drops
Low, the side reaction that polymerization, cracking etc. are complicated can be caused simultaneously.When fast and parallel competitive reaction or company that complexity occurs in liquid phase
During string competitive reaction, product or intermediate product can react further with raw material component, to such an extent as between reaction raw materials
Initial mixing effect greatly affects final products distribution, the yield of product and quality, and affects setting of all round process simultaneously
The indexs such as meter and energy consumption.So designing efficient Liquid-liquid mixing equipment, it is achieved the initial quickly mixing of liquid-liquid, produce for improving
The quality of product, reduce the yield of by-product, optimize whole production process and have great importance.
The mechanism of Liquid-liquid mixing mainly has Laminar flow mixing and turbulent closure scheme.The coefficient of molecular diffusion that general fluid mixes naturally only has
1.0～10cm/s, main body convection current, the diffusion coefficient of eddying motion then can reach its about 100,000 times.For high viscosity liquid it
Between mixed process be usually Laminar flow mixing, its mixing mainly by means of fluid molecule spread, if at low temperatures
The viscosity of high viscosity liquid reduces, then can realize mixed process and be changed into turbulent closure scheme to strengthen the effect of mass transfer.In commercial production
The equipment utilizing turbulent closure scheme mechanism to realize Liquid-liquid mixing mainly have stirred autoclave, jet mixer, impinging streams mixer,
Static mixer, dynamic mixer etc..Wherein, the micromixing corresponding to process of churned mechanically form fluid-mixing is used
Time is longer, and process is mainly by micromixing control, and it is fast that the mixing apparatus of other several forms is usually used between low-viscosity (mobile) liquid
Speed mixing.
In commercial production, modal stirred autoclave is mainly made up of cylinder, baffle plate and stirring system, transmission and sealing device.
For having the alkylated reaction of high viscosity liquid, the most widely used horizontal reactor having band agitating device, patent
ZL200520078557.3 describes the horizontal reactor in a kind of sulfuric acid process alkylation process, and main body is a horizontal pressure vessel,
There are an inner circulating tube, a tube bank taking reaction heat away and a mixing auger oar.Back-mixing in this reactor is relatively big, no
It is beneficial to improve the conversion ratio of reaction.United States Patent (USP) US6194625B1 describes the alkylation reactor of a kind of sectional feeding, reaction
District is divided into the section of several series connection, fresh feed is separated into a few stock and does not introduce each reaction section, and recycle
High viscosity reactant is then series flow, uses churned mechanically mode to mix in each reaction section.Although this structure
Overcome the problem that back-mixing is bigger, but structure is the most complicated.It addition, both structures all have employed fixed rotating speed motor-driven
Stirring paddle, it is easy to leak because of poorly sealed.Static mixer is that the nearest one grown up for 20 years does not has machinery
The mixing apparatus rotated.Fluid, when flowing through static mixer, is mixed the thin slice that element divisions becomes the thinnest, and its quantity presses element
Certain power of number increases, and eventually becomes small drop, thus reaches sufficiently to mix.It is low that static mixer has running cost,
Floor space is little, compact conformation, be difficult to leakage, there is no revolving member and manufacture the advantages such as easy for installation.But, for possible
There is the mixed process that solid produces, easily make static mixer block, be difficult to clear up.Additionally, static mixer there is also
Pressure drop is excessive waits fatal defects.
External loop reactor is a kind of efficient heterophase reactor, and patent US5777189 and CN200410152286.5 describe one
Plant solution-air, gas-liquid-solid external loop reactor, the kinetic energy generation circulation sprayed by gas, but the easy back-mixing of reactant, it is unfavorable for
Improve the conversion ratio of reaction.United States Patent (USP) US3281213 proposes a kind of vertical reactor, and its main body is a riser, carries
Riser and a horizontal tank are connected, and horizontal tank is built with high viscosity reactant, and other two kinds of reactants are by bottom riser
Nozzle sprays into, and the gravitation that injection causes drives the high viscosity reactant in horizontal tank to enter riser together, and reaction is i.e. at this root
Riser reactor is carried out.Riser top connects has a knockout drum, for the separation of product.Height after separation glues
Degree reactant is recycled into the horizontal tank bottom riser.This structure does not use mechanical rotation component, solves built-in spiral
The series of problems that oar brings.But, high viscosity reactant is not satisfactory with the mixing of other reactant, it addition, whole
Individual reactor assembly have employed a riser, two horizontal tanks and a down-comer, and equipment is huge, structure is the compactest.
The vertical reactor of a band particular fillers in United States Patent (USP) US7652187, the mode using allotter and filler to combine realizes acid
Hydrocarbon mixes, it is not necessary to rotating machinery.It utilizes jet mixing device to replace mechanical mixture, (sprays including hydraulic spray nozzle, distributor
The bubbling device of device), venturi-type blender etc..US7435864 patent has carried out the improvement in terms of nozzle, the hydrocarbon of mixing
Class is sprayed in sulphuric acid emulsion by multiple parallel nozzles and is alkylated reaction.But patent is for injection apparatus the most specifically
Bright, inefficient jet mixing device inapplicable and full-bodied sulphuric acid catalysis carbon tetra-alkylation react.
Patent CN101104570 describes a kind of alkylating method of liquid acid, containing fractal orchestration and the reactor of disperser.
Disperser includes liquid liquid coalescer, altogether knitmesh line, glass fiber mesh, porous plate, wire netting, multifilament catalysis material etc..
CN201310140601.8 describes a kind of tower alkylation reactor of filler.Liquid phase C4 alkane and concentrated sulphuric acid utilize outside device and stir
Mixing device fully emulsified, keep temperature to be 2-10 DEG C, enter device through raw material pump from tower top liquid phase feed pipe, gas phase C4 alkene is certainly
Tower top enters device, flows downwardly together with liquid phase, is layered through packing section acid hydrocarbon, uses spray between tower reactor packing section
Hair style feed pipe adds fresh liquid phase C4 alkane alkene.But the back-mixing of this device is serious, and the time of staying is longer, and side reaction increases.
Chinese patent CN200510004936.2 and CN00230326.4 describes a kind of relatively new mixing apparatus, and percussion flow mixes
Device.Its basic conception is to make two streams be sprayed by coaxially arranged nozzle and be clashed into, and due to inertia, granule oozes through striking face
Enter reverse flow, and make convergent oscillation campaign back and forth.Its result is to make the alternate relative velocity of granule high, passes strengthening heat, matter
The transmittance process passing process especially external diffusion control is the most effective.But, impinging streams mixer is easy in the region away from nozzle
Form dead band, make distribution of reaction products uneven, for the reaction between multiply high viscosity liquid, be still difficult to reach good mixing
Close effect.
Summary of the invention
Present invention is primarily targeted at offer to be applicable under large-scale production, liquid-liquid, liquid-liquid-liquid heterogeneous reaction are the highest viscous
Coupled reactor is clashed in the injection quickly mix between degree liquid, reacted, as anti-in concentrated sulphuric acid or ionic liquid-catalyzed isobutane alkylation
Should.High viscosity reaction liquid can be ground into the least drop by raw material injection premixed device by this reactor, makes high viscosity liquid
Body the most uniformly mixes with other low viscosity raw material, is formed as low viscous emulsion, then by multiple injections
The nozzle at high speeds ejection ring-shaped liquid film of knock-on reaction device clashes into mutually, can improve the rapids of course of reaction in further knock-on reaction
Stream, strengthening reaction mixing homogeneity, it is provided that bigger liquid liquid phase contact area, make reaction the most fully carry out, strengthen primary response,
Suppression side reaction, feed stock conversion reaches the highest.Reacted liquid material is in reactor lower part initial gross separation, and catalyst is from instead
Answering and flow out bottom device, enter raw material injection premixed device by circulating pump, alkylate oil and hydrocarbon mixture are from middle part extraction.Gas phase hydrocarbon from
Discharge reactor after reactor head sweat cooling, recirculate after entering compressor assembly or absorption system liquefaction and use.
The present invention has a clear advantage and beneficial effect than prior art:
The percussion flow heterophase reactor that the present invention designs, in strengthening blender dependence change blender, the geometries of passage etc. are square
Method strengthens molecule diffusion and the convection current of fluid, increases the convection current mixing portion of microfluid, thus increases effective contact of microfluid
Area, improves the mixing efficiency of liquid, may be implemented in the Quick uniform mixing of low reynolds number fluid under minute yardstick in the short time.Instead
Answering device simple in construction, liquid liquid contact area is big, does not has mixing component, is difficult to leakage, possesses the biography that reaction temperature is easily-controllable, good
The performances such as matter and heat transfer property, widely adaptability.Rapidly and efficiently mixing of immiscible two kinds of fluids in large-scale production can be realized
Close reaction, suppress side reaction simultaneously, improve the selectivity of product.Can be widely used for petrochemical industry, be particularly well-suited to high viscous
The liquid phase reactor of degree fluid, such as concentrated sulphuric acid or ionic liquid-catalyzed carbon tetra-alkylation reaction etc..
Accompanying drawing explanation
Fig. 1 is the structure chart of percussion flow heterophase reactor；
Fig. 2 is the nozzle arrangements schematic diagram of percussion flow heterophase reactor；
Fig. 3 is the premixer structure schematic diagram of percussion flow heterophase reactor；
Fig. 1 show the schematic diagram of percussion flow heterophase reactor of the present invention, including: nozzle system 1, import 2, demister 3, gas
Export 4 mutually, safety relief mouth 5, coalescing separator 6, premixed device 7, import 8, catalyst inlet 9, reactor 10, catalyst
Outlet 11, coalescing separator 12, products export 13.
Fig. 2 show nozzle system 1 schematic diagram of percussion flow heterophase reactor of the present invention, including working solution entrance 14, injection liquid
Entrance 15, trunnion 16, mixing chamber 17, nozzle 18, perforation 19, cavity 20, and be threaded connection.
Fig. 3 show premixed device 7 schematic diagram of percussion flow heterophase reactor of the present invention, and including working solution entrance 21, injection liquid enters
Mouth 22, trunnion 23, mixing chamber 24, perforation 25, cavity 26, and be threaded connection.
Detailed description of the invention
Below in conjunction with the drawings and specific embodiments, the present invention is described in further detail, but the present invention is the most thus by any
Limit:
The catalyst of accompanying drawing 1 medium-high viscosity enters raw material premixed device 7 from pipeline 9 with active flow, and alkane is from pipeline 8 driven entrance raw material
Blender 7, high viscosity reacting fluid is the most uniformly mixed with other low viscosity, cryogen by premixed device 7,
Be formed as the emulsion of low viscosity, low temperature, enter back into nozzle system 1.The middle part of reactor 10 is the most symmetrical uniform nozzle system
System 1, alkene from pipeline 2 driven entrance nozzle system 1, the nozzle arranged by the port of export after catalyst, alkane, olefin with
Certain angle is cone ejection, and the liquid of each nozzle at high speeds ejection clashes in opposite directions, and liquid phases of reactants drops to reactor bottom,
Product and catalyst are discharged from bottom by gravity settling separation, catalyst, and reactant is discharged in the middle part of reactor.Part
Discharge from reactor head with the form of gas phase after alkane vaporization heat absorption, maintain reaction temperature.
As shown in Figure 2, each nozzle axial centre is relative, and distance is 1～10D, and D is jet expansion outer annular diameter for nozzle system 1.
Jet expansion is annular space, and the area of annular space is the 10～30% of outer shroud area.The a diameter of d of perforation, throat pipe diameter is 1～5d, nozzle
Outer annular diameter D is 10～20d, and mixer length is 10～50d.Premixed device 7 structure as shown in Figure 3, a diameter of d of perforation, trunnion
A diameter of 1～5d, mixer length is 10～50d.Premixed device can also use other liquid liquid mixing arrangements such as static mixer.Produce
The height of product outlet 13 should ensure that the liquid residence time of outlet less than 13 is not less than product and the separation time of catalyst, and passes through
Ring-type coalescing separator 12 separates the catalyst in product further.Coalescing separator 6 and coalescing separator 12 should make oil phase and urge
Agent is sufficiently separated mutually, selects oleophilic drainage material and loads the aniones such as trifluoro sulfonate radical, bisulfate ion or perfluorinated sulfonic acid root
Ionic liquid.
Claims (8)
1. percussion flow heterophase reactor, including: nozzle system 1, import 2, demister 3, gaseous phase outlet 4, safety relief mouth 5,
Coalescing separator 6, premixed device 7, import 8, catalyst inlet 9, reactor 10, catalyst outlet 11, coarse separation
Device 12, products export 13, it is characterised in that: premixed device 7 is fixed on the middle part of reactor, and it connects horizontal positioned
Nozzle system 1, outlet be provided with annular space nozzle, high viscosity fluid by circulating pump with active flow enter raw material premixed device 7,
Low viscosity fluid is from pipeline 8 driven entrance raw material premixed device 7, then mixes with driven pipeline 2, enters symmetrical horizontally towards each other
Uniform nozzle system 1.
Percussion flow heterophase reactor the most according to claim 1, is characterized by that nozzle system 1 includes working solution entrance 14, draws
Penetrate liquid inlet 15, trunnion 16, mixing chamber 17, nozzle 18, perforation 19, cavity 20, and be threaded connection；Respectively
Nozzle axial centre is relative, and distance is 1～10D, and D is jet expansion outer annular diameter；Jet expansion is annular space, annular space
Area is outer shroud area 5～40%；The a diameter of d of perforation, throat pipe diameter is 1～10d, and nozzle outer annular diameter D is
10～30d, mixer length is 5～100d.
Nozzle system 1 the most according to claim 2, area is outer shroud area the 10～30% of its feature preferably annular space；Penetrate
Bore dia is d, and throat pipe diameter is 1～5d, and nozzle outer annular diameter D is 10～20d, and mixer length is 20～40d.
Percussion flow heterophase reactor the most according to claim 1, is characterized by that premixed device 7 structure includes working solution entrance 21,
Injection liquid inlet 22, trunnion 23, mixing chamber 24, perforation 25, cavity 26, and be threaded connection；Perforation diameter
For d, throat pipe diameter is 1～6d, and mixer length is 10～60d.
Premixed device 7 the most according to claim 4, is ground into the least drop by high viscosity reaction liquid, makes high viscosity liquid
The most uniformly mix with other low temperature, low viscosity raw material, be formed as low temperature, low viscous emulsion.
Percussion flow heterophase reactor the most according to claim 1, is characterized by that nozzle system 1 and premixed device 7 are by one or many
Individual similar structures in series uses.
Percussion flow heterophase reactor the most according to claim 1, is characterized by that the height of products export 13 should ensure that outlet 13
Following liquid residence time is not less than product and the separation time of catalyst, and enters one by ring-type coalescing separator
Step separates the catalyst in product.
Percussion flow heterophase reactor the most according to claim 1, is characterized by that coalescing separator 6 and coalescing separator 12 should make
Oil phase is sufficiently separated mutually with catalyst, selects oleophilic drainage material and loads trifluoro sulfonate radical, bisulfate ion or perfluor sulphur
The anion ion liquids such as acid group.
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
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| CN2015102067000 | 2015-04-28 | ||
| CN201510206700 | 2015-04-28 |
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| CN106179146A true CN106179146A (en) | 2016-12-07 |
| CN106179146B CN106179146B (en) | 2019-04-12 |
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| CN201510296607.3A Active CN106179146B (en) | 2015-04-28 | 2015-06-02 | A kind of percussion flow heterophase reactor |
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| CN108439490A (en) * | 2018-04-25 | 2018-08-24 | 深圳市寒暑科技新能源有限公司 | A kind of Preparation equipment and preparation method of ternary material precursor |
| CN109225115A (en) * | 2018-09-17 | 2019-01-18 | 沈阳化工大学 | A kind of impact flow reactor of adjustable nozzle spacing |
| CN110542490A (en) * | 2019-09-18 | 2019-12-06 | 昆明理工大学 | non-isothermal micro-impinging stream reactor testing method and device |
| CN110639445A (en) * | 2019-11-04 | 2020-01-03 | 锦益创典(天津)科技有限责任公司 | Device and method for spray continuous reaction |
| CN111359556A (en) * | 2019-03-15 | 2020-07-03 | 南京延长反应技术研究院有限公司 | Micro-interface enhanced hydrogenation reaction system |
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| CN111686665A (en) * | 2019-03-15 | 2020-09-22 | 南京延长反应技术研究院有限公司 | Micro-interface enhanced reaction system |
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| CN205042452U (en) * | 2015-04-28 | 2016-02-24 | 中国科学院过程工程研究所 | Percussion flow heterogeneous reaction ware |
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| CN108439490A (en) * | 2018-04-25 | 2018-08-24 | 深圳市寒暑科技新能源有限公司 | A kind of Preparation equipment and preparation method of ternary material precursor |
| CN109225115A (en) * | 2018-09-17 | 2019-01-18 | 沈阳化工大学 | A kind of impact flow reactor of adjustable nozzle spacing |
| CN109225115B (en) * | 2018-09-17 | 2024-04-16 | 沈阳化工大学 | Impinging stream reactor with adjustable nozzle spacing |
| CN111482139A (en) * | 2019-01-29 | 2020-08-04 | 南京大学 | Up-down opposite flushing type residual oil hydrogenation fluidized bed micro-interface strengthening reaction device and method |
| CN111359556A (en) * | 2019-03-15 | 2020-07-03 | 南京延长反应技术研究院有限公司 | Micro-interface enhanced hydrogenation reaction system |
| CN111359547A (en) * | 2019-03-15 | 2020-07-03 | 南京延长反应技术研究院有限公司 | Oil-coal co-hydrogenation micro-interface reinforced emulsion bed reaction system |
| CN111686665A (en) * | 2019-03-15 | 2020-09-22 | 南京延长反应技术研究院有限公司 | Micro-interface enhanced reaction system |
| CN111686654A (en) * | 2019-03-15 | 2020-09-22 | 南京延长反应技术研究院有限公司 | Coal tar hydrogenation micro-interface emulsion bed enhanced reaction system |
| CN112169720A (en) * | 2019-07-04 | 2021-01-05 | 南京延长反应技术研究院有限公司 | Nano-micro interface enhanced reaction system |
| CN110542490A (en) * | 2019-09-18 | 2019-12-06 | 昆明理工大学 | non-isothermal micro-impinging stream reactor testing method and device |
| CN110639445A (en) * | 2019-11-04 | 2020-01-03 | 锦益创典(天津)科技有限责任公司 | Device and method for spray continuous reaction |
| CN111471482A (en) * | 2020-04-20 | 2020-07-31 | 华东理工大学 | Method for dehydrating high-emulsification sump oil and device adopted by method |
| CN112569871A (en) * | 2020-11-23 | 2021-03-30 | 中国科学院过程工程研究所 | For CO2Gas-liquid uniform distribution tube type reactor for carbonylation reaction |
| CN114621066A (en) * | 2022-03-23 | 2022-06-14 | 煤炭科学技术研究院有限公司 | Method for synthesizing 2-methyl-6-propionyl naphthalene |
| CN114621066B (en) * | 2022-03-23 | 2024-03-19 | 煤炭科学技术研究院有限公司 | Method for synthesizing 2-methyl-6-propionyl naphthalene |
Also Published As
| Publication number | Publication date |
|---|---|
| CN106179146B (en) | 2019-04-12 |
| CN205042452U (en) | 2016-02-24 |
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