CN106179146B - A kind of percussion flow heterophase reactor - Google Patents
A kind of percussion flow heterophase reactor Download PDFInfo
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- CN106179146B CN106179146B CN201510296607.3A CN201510296607A CN106179146B CN 106179146 B CN106179146 B CN 106179146B CN 201510296607 A CN201510296607 A CN 201510296607A CN 106179146 B CN106179146 B CN 106179146B
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Abstract
The present invention is a kind of percussion flow heterophase reactor, is related to Liquid-liquid mixing heterogeneous reaction.The reactor by raw material spray premixed device by high viscosity and low viscosity fluid in lower temperature, the emulsion of low viscosity is uniformly mixed into the short time, ring-shaped liquid film is sprayed by the nozzle at high speeds of multiple injection knock-on reaction devices again and mutually hits reinforcing reaction, carries out rapid reaction sufficiently.The percussion flow heterophase reactor introduced of the present invention, structure is simple, without mixing component, is not easy to leak, reaction liquid contact area it is big, it can be achieved that in large-scale production immiscible fluid rapidly and efficiently hybrid reaction, the selectivity of product is high.Can be applied to fluid viscosity in the industrial process such as fine chemistry industry, petrochemical industry, pharmaceuticals industry, biochemical industry is larger, liquid-liquid is immiscible, between liquid quick hybrid reaction reaction unit, especially liquid acid catalyzing iso-butane alkane alkylated reaction.
Description
Technical field
The present invention relates to Liquid-liquid mixing heterogeneous reactions, in particular to fluid viscosity is larger, the immiscible multiphase of liquid-liquid is anti-
It answers, especially the concentrated sulfuric acid or the reaction of ionic liquid-catalyzed isobutane alkylation, belongs to petrochemical industry, environmental project, pharmaceutical engineering
Equal fields.
Background technique
With the rapid growth of China's car ownership, influence of the exhaust emissions to atmosphere pollution increasingly increases, oil quality
Amount be influence motor vehicle exhaust emission an important factor for, accelerate promote oil quality upgrading, how to produce meet country it is increasingly strict
Environmental protection standard clean gasoline blend component, be national resources environment/green manufacturing Major Strategic Demand.Alkylate oil with
Other components are compared, not olefin-containing and aromatic hydrocarbons, hardly sulfur-bearing, and octane number with higher and lower vapour pressure, are
A kind of ideal clean gasoline, advantage are apparent.China's alkylate oil production at present is faced with unprecedented development
Opportunity and space.
The liquid acids such as concentrated sulfuric acid or ionic liquid of industrial application catalyzing iso-butane alkane alkylated reaction at present, the concentrated sulfuric acid and carbon
Four mixed effect directly affects the quality and yield of alkylate oil.Reaction temperature reduction advantageously reduces side reaction, improves pungent
Alkane value.But the concentrated sulfuric acid or ionic liquid at low temperatures viscosity increase, influence iso-butane to the mass transfer of sour phase so that
Reaction efficiency reduces, while can cause the complicated side reactions such as polymerization, cracking.When the fast and parallel competition that complexity occurs in liquid phase
Reaction product or intermediate product are further reacted with raw material group branch when reacting perhaps consecutive competitive reaction, so that instead
It answers the initial mixing effect between raw material greatly to influence final product distribution, the yield of product and quality, and influences simultaneously
The indexs such as the design and energy consumption of all round process.So designing efficient Liquid-liquid mixing equipment, the initial quick of liquid-liquid is realized
Mixing has great importance for the quality for improving product, the yield for reducing by-product, the entire production process of optimization.
The mechanism of Liquid-liquid mixing mainly has Laminar flow mixing and turbulent closure scheme.The molecule diffusion system that general fluid mixes naturally
Number only has 1.0~10cm/s, and the diffusion coefficient of main body convection current, eddying motion then can reach its 100,000 times or so.It is viscous for height
The mixed process spent between liquid is usually Laminar flow mixing, and the molecule mixed mainly by means of fluid is spread, such as can be low
The viscosity of high viscosity liquid is reduced in warm situation, then mixed process can be achieved and be changed into turbulent closure scheme to strengthen the effect of mass transfer
Fruit.Mainly there are stirred autoclave, jet stream injection mixing using the equipment that turbulent closure scheme mechanism realizes Liquid-liquid mixing in industrial production
Device, impinging streams mixer, static mixer, dynamic mixer etc..Wherein, using the process of churned mechanically form fluid-mixing
Corresponding macroscopic mixing time is longer, and process is mainly controlled by micromixing, and the mixing apparatus of other several forms is usually used in
Quick mixing between low-viscosity (mobile) liquid.
The most common stirred autoclave is mainly by cylinder, baffle and stirring system, transmission and sealing device in industrial production
It constitutes.For the alkylated reaction with high viscosity liquid, what is be widely used at present has the horizontal reactor with agitating device, specially
Sharp ZL200520078557.3 describes the horizontal reactor in a kind of sulfuric acid process alkylation process, and main body is a Horizontal pressure
Container has an inner circulating tube, a tube bank for taking reaction heat away and a mixing auger paddle.Back-mixing in this reactor compared with
Greatly, it is unfavorable for improving the conversion ratio of reaction.United States Patent (USP) US6194625B1 describes a kind of alkylated reaction of sectional feeding
Device, reaction zone are divided into several concatenated sections, and fresh feed is separated into several stocks and does not introduce each reaction section, and follow
The high viscosity reactant that ring uses is then series flow, is mixed in each reaction section using churned mechanically mode.This
Although kind structure overcomes the larger problem of back-mixing, but structure is excessively complicated.In addition, both structures all use fixed rotating speed
The agitating paddle of motor drive, it is easy to be leaked because poorly sealed.Static mixer is to grow up for nearest 20 years
A kind of mixing apparatus without machinery rotation.Fluid is mixed element divisions into very thin thin slice when flowing through static mixer,
Its quantity is increased by certain power of parts number, small drop is eventually become, to reach sufficient mixing.Static mixing utensil
There is operating cost low, occupied area is small, compact-sized, the advantages that being not easy to leak, is easy for installation without revolving member and manufacture.But
It is, for the mixed process that may there is solid to generate, to be easy to block static mixer, be difficult to be cleared up.In addition, static mixed
There is also the excessive equal fatal defects of pressure drop for clutch.
External loop reactor is a kind of efficient heterophase reactor, and patent US5777189 and CN200410152286.5 are situated between
Continued a kind of solution-air, gas-liquid-solid external loop reactor, generates circulation, but the easy back-mixing of reactant by the kinetic energy of gas injection,
It is unfavorable for improving the conversion ratio of reaction.United States Patent (USP) US3281213 proposes a kind of vertical reactor, and main body is a promotion
Pipe, riser are connected with a horizontal tank, and horizontal tank is provided with high viscosity reactant, and in addition two kinds of reactants pass through riser
The nozzle of bottom sprays into, and gravitation caused by injection drives the high viscosity reactant in horizontal tank to enter riser together, reacts
Carried out in this root riser reactor.Riser top is connected with a knockout drum, the separation for reaction product.Separation
High viscosity reactant afterwards is recycled into the horizontal tank for promoting bottom of the tube.This structure does not use mechanical revolving member, solves
Built-in propeller bring a series of problems.But the mixing of high viscosity reactant and other reactants can not make us full
Meaning, in addition, entire reactor assembly uses a riser, two horizontal tanks and a down-comer, equipment is huge, structure
It is not compact enough.A vertical reactor with particular fillers in United States Patent (USP) US7652187 is combined using distributor and filler
Mode realizes sour hydrocarbon mixing, is not necessarily to rotating machinery.Its using jet mixing device replace mechanical mixture, including hydraulic spray nozzle, point
Cloth device (bubbling device of sprinkler), venturi-type mixer etc..US7435864 patent has carried out the improvement in terms of nozzle,
Mixed hydro carbons is sprayed into sulfuric acid emulsion by multiple parallel nozzles and is alkylated reaction.But patent is for injection apparatus
It does not illustrate, inefficient jet mixing device simultaneously not applicable is reacted with highly viscous sulphuric acid catalysis carbon tetra-alkylation.
Patent CN101104570 describes a kind of alkylated method of liquid acid, containing fractal orchestration and disperser
Reactor.Disperser includes liquid liquid coalescer, altogether knitmesh line, glass fiber mesh, porous plate, metal mesh, multifilament catalysis material etc..
CN201310140601.8 describes a kind of tower alkylation reactor of filler.Liquid phase C4 alkane and the concentrated sulfuric acid utilize outside device
Agitating device is fully emulsified, and keeping temperature is 2-10 DEG C, pumps through raw material from tower top liquid phase feed pipe and enters device, gas phase C4 alkene
Enter device from tower top, flowed downwardly together with liquid phase, is layered by packing section acid hydrocarbon, is used between tower reactor packing section
Fresh liquid phase C4 alkane alkene is added in spray nozzle type feed pipe.But the back-mixing of the device is serious, the residence time is longer, and side reaction increases
It is more.
Chinese patent CN200510004936.2 and CN00230326.4 describe a kind of relatively new mixing apparatus, hit
Flow mixer.Its basic conception is that two streams is made to be sprayed and be hit by coaxially arranged nozzle, and due to inertia, particle is passed through and hit
It hits face and penetrates into reverse flow, and make convergent oscillation campaign back and forth.As a result, keeping the alternate relative velocity of particle high, to reinforcing
The transmittance process of heat, matter transmittance process especially external diffusion control is more effective.But impinging streams mixer is in separate nozzle
Region dead zone easy to form, keeps distribution of reaction products uneven, for the reaction between multiply high viscosity liquid, is still difficult to reach
To good mixed effect.
Summary of the invention
Under being suitable for being mass produced, liquid-liquid, liquid-liquid-liquid heterogeneous reaction are especially
Be quickly mix between high viscosity liquid, coupled reactor is hit in the injection reacted, such as the concentrated sulfuric acid or ionic liquid-catalyzed iso-butane
Alkylated reaction.This reactor can spray the drop that high viscosity reaction liquid is ground into very little by premixed device by raw material,
It mixes high viscosity liquid uniformly in a short period of time with other low viscosity raw materials, is formed as the emulsion of low viscosity, then
Ring-shaped liquid film is sprayed by the nozzle at high speeds of multiple injection knock-on reaction devices mutually to hit, and can be mentioned in further knock-on reaction
The turbulent flow of high reaction process, strengthen reaction mixture homogeneity, biggish liquid liquid phase contact area is provided, make rapid reaction sufficiently into
Row strengthens main reaction, inhibits side reaction, and feed stock conversion reaches very high.Liquid material after reaction is preliminary in reactor lower part
Separation, catalyst are flowed out from reactor bottom, are entered raw material by circulating pump and are sprayed premixed device, alkylate oil and hydrocarbon mixture are therefrom
Portion's extraction.Reactor is discharged after reactor head sweat cooling in gas phase hydrocarbon, into after compressor assembly or absorption system liquefaction
It recirculates and uses.
The present invention has clear advantage and beneficial effect than the prior art:
The percussion flow heterophase reactor that the present invention designs strengthens mixer by the set shape for changing channel in mixer
The methods of shape come enhance fluid molecule diffusion and convection current, increase the convection current mixing portion of microfluid, to increase microfluid
Effective contact area, improve the mixing efficiency of liquid, it can be achieved that in a short time under minute yardstick low reynolds number fluid it is quick
Even mixing.Structure of reactor is simple, and liquid liquid contact area is big, without mixing component, is not easy to leak, have reaction temperature it is easily-controllable,
The performances such as good heat and mass transport performance, extensive adaptability.Immiscible two kinds of fluids in large-scale production can be achieved
Rapidly and efficiently hybrid reaction, while inhibiting side reaction, improve the selectivity of product.It can be widely used for petrochemical industry, especially
Suitable for the liquid phase reactor of high viscosity fluid, such as the concentrated sulfuric acid or the reaction of ionic liquid-catalyzed carbon tetra-alkylation.
Detailed description of the invention
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, comprising: 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 go out
Mouth 11, coalescing separator 12, products export 13.
Fig. 2 show 1 schematic diagram of nozzle system of percussion flow heterophase reactor of the present invention, including working solution entrance 14, draws
Liquid inlet 15, trunnion 16, mixing chamber 17, nozzle 18, perforation 19, cavity 20 are penetrated, and is connected through a screw thread.
Fig. 3 show 7 schematic diagram of premixed device of percussion flow heterophase reactor of the present invention, including working solution entrance 21, injection
Liquid inlet 22, trunnion 23, mixing chamber 24, perforation 25, cavity 26, and be connected through a screw thread.
Specific embodiment
Below in conjunction with the drawings and specific embodiments, the present invention is described in further detail, but the present invention not thus by
To any restrictions:
The catalyst of 1 medium-high viscosity of attached drawing from pipeline 9 with active flow enter raw material premix device 7, alkane from pipeline 8 it is driven into
Enter material mixer 7, high viscosity reacting fluid is equal in a short period of time by premixed device 7 and other low viscosities, cryogen
Even mixing is formed as the emulsion of low viscosity, low temperature, enters back into nozzle system 1.The middle part of reactor 10 is opposite symmetrical uniformly distributed
Nozzle system 1, alkene enters nozzle system 1 from pipeline 2 is driven, passes through outlet end setting after catalyst, alkane, olefin
Nozzle be at a certain angle in conical ejection, the liquid that each nozzle at high speeds sprays is hit in opposite directions, and liquid phases of reactants drops to instead
Answer device bottom, reaction product and catalyst by gravity settling separation, catalyst is discharged from bottom, and reactant is in the middle part of reactor
Discharge.It is discharged in the form of gas phase from reactor head after the vaporization heat absorption of part alkane, maintaining reaction temperature.
As shown in Fig. 2, each nozzle axial centre is opposite for nozzle system 1, and distance is 1~10D, and D is jet expansion outer ring
Diameter.Jet expansion is annular space, and the area of annular space is the 10~30% of outer ring area.Perforation diameter be d, throat pipe diameter be 1~
5d, nozzle outer annular diameter D are 10~20d, and mixer length is 10~50d.7 structure of premixed device is as shown in Fig. 3, perforation diameter
For d, throat pipe diameter is 1~5d, and mixer length is 10~50d.Premixed device can also be using other liquid liquid such as static mixers
Mixing arrangement.The height of products export 13 should ensure that point of 13 liquid residence times below of outlet not less than product and catalyst
The layer time, and pass through the catalyst in cricoid coalescing separator 12 further separation product.Coalescing separator 6 and coarse separation
Device 12 should be such that oily phase is mutually sufficiently separated with catalyst, and oleophilic drainage material is selected simultaneously to load trifluoro sulfonate radical, bisulfate ion or complete
The anion ion liquids such as fluosulfonic acid root.
Claims (5)
1. percussion flow heterophase reactor, comprising: 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), coalescing separator (12), products export (13), it is characterised in that: premixed device (7)
It is fixed on the middle part of reactor, connects horizontal positioned nozzle system (1) thereon；
Nozzle system (1) includes working solution entrance (14), injection liquid inlet (15), trunnion (16), mixing chamber (
17), nozzle (18), perforation (19), cavity (20), and be connected through a screw thread；Each nozzle axial centre is opposite, distance
It is jet expansion outer annular diameter for 1~10D, D；Jet expansion is annular space, and the area of annular space is the 5~40% of outer ring area；It penetrates
Bore dia is d, and throat pipe diameter is 1~10d, and nozzle outer annular diameter D is 10~30d, and mixer length is 5~100d；
Outlet is equipped with annular space nozzle, and high viscosity fluid, which is flowed by circulating pump with active, enters raw material premix device (7), low viscosity stream
Body enters raw material premix device (7) from pipeline (8) is driven, then mixes with driven pipeline (2), and entrance is symmetrical equal horizontally towards each other
The nozzle system (1) of cloth；
The area of annular space is the 10~30% of outer ring area；Perforation diameter is d, and throat pipe diameter is 1~5d, nozzle outer annular diameter D
For 10~20d, mixer length is 20~40d；
Premixed device (7) structure includes working solution entrance (21), injection liquid inlet (22), trunnion (23), mixing chamber
(24), perforation (25), cavity (26), and be connected through a screw thread；Perforation diameter is d, and throat pipe diameter is 1~6d, mixing
Room length is 10~60d.
2. percussion flow heterophase reactor according to claim 1, high viscosity reaction liquid is ground into very by premixed device (7)
Small drop mixes high viscosity liquid uniformly in a short period of time with other low temperature, low viscosity raw material, be formed as low temperature,
The emulsion of low viscosity.
3. percussion flow heterophase reactor according to claim 1, it is characterized in that nozzle system (1) and premixed device (7)
It is used by one or more similar structures in series.
4. percussion flow heterophase reactor according to claim 1, it is characterized in that the height of products export (13) should ensure that
The separation time that (13) liquid residence time below is not less than product and catalyst is exported, and passes through cricoid coarse separation
Device further separates the catalyst in product.
5. percussion flow heterophase reactor according to claim 1, it is characterized in that coalescing separator (6) and coalescing separator
(12) should make it is oily be mutually mutually sufficiently separated with catalyst, selection oleophilic drainage material and load trifluoro sulfonate radical, bisulfate ion or
Perfluorinated sulfonic acid root anion ion liquid.
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510206700 | 2015-04-28 | ||
| CN2015102067000 | 2015-04-28 |
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| CN106179146A CN106179146A (en) | 2016-12-07 |
| CN106179146B true 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 |
| CN201520372727.2U Expired - Fee Related CN205042452U (en) | 2015-04-28 | 2015-06-02 | Percussion flow heterogeneous reaction ware |
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| CN106179146B (en) * | 2015-04-28 | 2019-04-12 | 中国科学院过程工程研究所 | A kind of percussion flow heterophase reactor |
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| 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 |
| CN114425260B (en) * | 2020-10-29 | 2023-05-30 | 中国石油化工股份有限公司 | Liquid-liquid mixing device and mixing 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 |
| CN112755926B (en) * | 2021-01-05 | 2022-09-02 | 华东理工大学 | Device and method for enhancing liquid-liquid reaction |
| 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 |
| CN117258743B (en) * | 2023-11-17 | 2024-03-19 | 山东天力科技工程有限公司 | Para-aramid continuous polymerization system and method |
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| CN2057116U (en) * | 1989-10-13 | 1990-05-16 | 罗德勤 | Unitary corrosion-resistant jet pump |
| CN1047815A (en) * | 1989-06-03 | 1990-12-19 | 全苏铝镁电气工业科学研究所设计院 | Device for atomizing liquid |
| CN103611487A (en) * | 2013-12-18 | 2014-03-05 | 华东理工大学 | Impinging stream reactor |
| 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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- 2015-06-02 CN CN201510296607.3A patent/CN106179146B/en active Active
- 2015-06-02 CN CN201520372727.2U patent/CN205042452U/en not_active Expired - Fee Related
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1047815A (en) * | 1989-06-03 | 1990-12-19 | 全苏铝镁电气工业科学研究所设计院 | Device for atomizing liquid |
| CN2057116U (en) * | 1989-10-13 | 1990-05-16 | 罗德勤 | Unitary corrosion-resistant jet pump |
| CN103611487A (en) * | 2013-12-18 | 2014-03-05 | 华东理工大学 | Impinging stream reactor |
| 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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| CN205042452U (en) | 2016-02-24 |
| CN106179146A (en) | 2016-12-07 |
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