CN205042452U - Percussion flow heterogeneous reaction ware - Google Patents

Percussion flow heterogeneous reaction ware Download PDF

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Publication number
CN205042452U
CN205042452U CN201520372727.2U CN201520372727U CN205042452U CN 205042452 U CN205042452 U CN 205042452U CN 201520372727 U CN201520372727 U CN 201520372727U CN 205042452 U CN205042452 U CN 205042452U
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liquid
reaction
nozzle
diameter
reactor
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张锁江
周志茂
赵国英
李海方
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Institute of Process Engineering of CAS
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Abstract

The utility model relates to a percussion flow heterogeneous reaction ware relates to the mixed heterogeneous reaction of liquid - liquid. This reactor pass through the raw materials spray mix in advance the ware with high viscosity and low viscosity fluid at the lower temperature, the homogeneous mixing be low viscous emulsion in the short time, the high -speed cyclic annular liquid films of blowing out of nozzles of a plurality of injection knock -on reaction wares of rethread clash into mutually strengthens the reaction, makes to react and fully goes on fast. The utility model discloses the percussion flow heterogeneous reaction ware who introduces, simple structure does not stir the part, the difficult leakage, reaction fluid contact area is big, can realize that immiscible fluid's high efficiency mixes the reaction in the large -scale production, and the selectivity of product is high. Can be applied to reaction unit, the especially liquid acid catalysis isobutane alkylation reaction that the fluid viscosity is great, liquid - liquid does not dissolve each other, a liquid flash mixed reacts among the industrial process such as fine chemistry industry, petrochemical, pharmaceutical industry, biochemical industry.

Description

A kind of percussion flow heterophase reactor
Technical field
The utility model relates to Liquid-liquid mixing heterogeneous reaction, particularly comparatively large, the immiscible heterogeneous reaction of liquid-liquid of fluid viscosity, and especially the concentrated sulfuric acid or the reaction of ionic liquid-catalyzed isobutane alkylation, belong 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 exhaust emissions on atmosphere pollution increases day by day, oil quality is the key factor affecting motor vehicle exhaust emission, accelerate to advance oil quality upgrading, how producing the clean gasoline blend component of the environmental protection standard meeting national increasingly stringent, is the Major Strategic Demand of national resources environment/green manufacturing.Alkylate oil is compared with other component, and not containing alkene and aromatic hydrocarbons, hardly sulfur-bearing, and have higher octane number and lower vapour pressure, be a kind of ideal clean gasoline, advantage is apparent.Current China alkylate oil is produced and is faced with unprecedented opportunity to develop and space.
The liquid acid catalyzing iso-butane alkane alkylated reactions such as the concentrated sulfuric acid of current commercial Application or ionic liquid, the mixed effect of the concentrated sulfuric acid and carbon four directly affects quality and the yield of alkylate oil.Reaction temperature reduction is conducive to reducing side reaction, improves octane number.But the concentrated sulfuric acid or ionic liquid at low temperatures viscosity increase, affect iso-butane to the mass transfer of sour phase makes reaction efficiency reduce, and to cause the side reaction of the complexity such as polymerization, cracking simultaneously.When there is complicated fast and parallel competitive reaction or consecutive competitive reaction in liquid phase, product or intermediate product and raw material component can be reacted further, to such an extent as to the initial mixing effect between reaction raw materials greatly affects the distribution of final product, the yield of product and quality, and affect the indexs such as the design of all round process and energy consumption simultaneously.So design efficient Liquid-liquid mixing equipment, realize the initial rapid mixing of liquid-liquid, for improve product quality, reduce accessory substance yield, optimize whole production process and have great importance.
The mechanism of Liquid-liquid mixing mainly contains Laminar flow mixing and turbulent closure scheme.The coefficient of molecular diffusion that general fluid mixes naturally only has 1.0 ~ 10cm/s, and the diffusion coefficient of main body convection current, eddying motion then can reach its about 100,000 times.Laminar flow mixing is generally for the mixed process between high viscosity liquid, its mixing is mainly by means of the molecular diffusion of fluid, if at low temperatures the viscosity of high viscosity liquid is reduced, then can realize mixed process and change turbulent closure scheme into strengthen the effect of mass transfer.The equipment utilizing turbulent closure scheme mechanism to realize Liquid-liquid mixing in industrial production mainly contains stirred autoclave, jet mixer, impinging streams mixer, static mixer, dynamic mixer etc.Wherein, adopt the macroscopic mixing time corresponding to process of churned mechanically form fluid-mixing longer, process mainly controls by micromixing, and the mixing apparatus of other several form is usually used in the rapid mixing between low-viscosity (mobile) liquid.
In industrial production, modal stirred autoclave is formed primarily of cylindrical shell, baffle plate and stirring system, transmission and sealing device.For the alkylated reaction with high viscosity liquid, the horizontal reactor having band agitating device extensively adopted at present, patent ZL200520078557.3 describes the horizontal reactor in a kind of sulfuric acid process alkylation process, main body is a horizontal pressure vessel, has an inner circulating tube, tube bank and a mixing auger oar taking reaction heat away.Back-mixing in this reactor is comparatively large, is unfavorable for the conversion ratio improving reaction.US Patent No. 6194625B1 describes a kind of alkylation reactor of sectional feeding, reaction zone is separated into the section of several series connection, fresh feed is separated into a few stock and does not introduce each reaction section, the high viscosity reactant recycled is then series flow, adopts churned mechanically mode to mix in each reaction section.Although this structure overcomes the larger problem of back-mixing, structure is too complicated.In addition, these two kinds of structures all have employed the paddle that fixed rotating speed motor drives, and are easy to leak because of poorly sealed.Static mixer is a kind of mixing apparatus not having mechanical rotation grown up for nearest 20 years.Fluid is when flowing through static mixer, and mixed element divisions becomes very thin thin slice, and certain power that its quantity presses parts number increases, and finally becomes small drop, thus reaches sufficient mixing.It is low that static mixer has running cost, and floor space is little, compact conformation, not easily leak, the advantage such as do not have revolving member and making and installation convenient.But, for the mixed process that solid may be had to produce, easily make static mixer block, be difficult to clear up.In addition, also there is fatal defects such as pressure drop excessive grade in static mixer.
External loop reactor is a kind of heterophase reactor efficiently, patent US5777189 and CN200410152286.5 describes a kind of solution-air, gas-liquid-solid external loop reactor, the kinetic energy sprayed by gas produces circulation, but the easy back-mixing of reactant, be unfavorable for the conversion ratio improving reaction.US Patent No. 3281213 proposes a kind of vertical reactor, its main body is a riser, riser is connected with a horizontal tank, horizontal tank is built with high viscosity reactant, other two kinds of reactants are sprayed into by the nozzle bottom riser, spraying the gravitation caused drives the high viscosity reactant in horizontal tank to enter riser together, and namely reaction is carried out in this root riser reactor.Riser top is connected with a knockout drum, for the separation of product.High viscosity reactant after separation circulates the horizontal tank entered bottom riser.This structure does not adopt mechanical rotation component, solves the series of problems that built-in screw brings.But high viscosity reactant can not be satisfactory with mixing of other reactant, in addition, whole reactor assembly have employed a riser, two horizontal tanks and a down-comer, and equipment is huge, structure is also compact not.The vertical reactor of a band particular fillers in US Patent No. 7652187, the mode adopting distributor and filler to combine realizes the mixing of sour hydrocarbon, without the need to rotating machinery.It utilizes jet mixing device to replace mechanical mixture, comprises hydraulic spray nozzle, distributor (bubbling device of sprinkler), venturi-type blender etc.US7435864 patent has carried out the improvement of nozzle aspect, and the hydro carbons of mixing is sprayed in sulfuric acid emulsion by multiple parallel nozzle and carries out alkylated reaction.But patent does not illustrate for injection apparatus, 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, the reactor containing fractal orchestration and disperser.Disperser comprises liquid liquid coalescer, altogether knitmesh line, glass fiber mesh, porous plate, wire netting, multifilament catalysis material etc.CN201310140601.8 describes the tower alkylation reactor of a kind of filler.Liquid phase C4 alkane and the concentrated sulfuric acid utilize agitating device fully emulsified outside device, maintenance temperature is 2-10 DEG C, through feedstock pump from tower top liquid phase feed pipe access to plant, gas phase C4 alkene is from tower top access to plant, flow downward with liquid phase, through the layering of packing section acid hydrocarbon, spray nozzle type feed pipe between tower reactor packing section, is adopted to add 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 more novel mixing apparatus, impinging streams mixer.Its basic conception makes two bursts of logistics be sprayed by coaxially arranged nozzle and clash into, and due to inertia, particle infiltrates reverse flow through striking face, and does convergent oscillation campaign back and forth.Consequently make the alternate relative velocity of particle high, the transmittance process controlled strengthening heat, matter transmittance process especially external diffusion is comparatively effective.But impinging streams mixer easily forms dead band in the region away from nozzle, make distribution of reaction products uneven, for the reaction between multiply high viscosity liquid, be still difficult to reach good mixed effect.
Summary of the invention
Under main purpose of the present utility model is to provide and is applicable to large-scale production, liquid-liquid, liquid-liquid-liquid heterogeneous reaction especially rapid mixing, reaction between high viscosity liquid injection clash into coupled reactor, as the concentrated sulfuric acid or ionic liquid-catalyzed isobutane alkylation reaction.This reactor can spray premixed device by raw material and high viscosity reaction liquid is ground into very little drop, make high viscosity liquid and other low viscosity raw material Homogeneous phase mixing in a short period of time, be formed as low viscous emulsion, then clashed into mutually by the nozzle at high speeds ejection ring-shaped liquid film of multiple injection knock-on reaction device, the turbulent flow of course of reaction can be improved in further knock-on reaction, strengthening reaction mixture homogeneity, larger liquid liquid phase contact area is provided, reaction is fully carried out fast, strengthening main reaction, suppress side reaction, feed stock conversion reaches very high.Reacted liquid material is in reactor lower part initial gross separation, and catalyst flows out from reactor bottom, and enter raw material by circulating pump and spray premixed device, alkylate oil and hydrocarbon mixture are from middle part extraction.Gas phase hydrocarbon discharges reactor after reactor head sweat cooling, enters compressor assembly or absorption system post liquefaction recycles again.
The technical solution of the utility model is:
Percussion flow heterophase reactor comprises: nozzle system 1, first material inlet 2, demister 3, gaseous phase outlet 4, safety relief mouth 5, first coalescing separator 6, premixed device 7, second material inlet 8, catalyst inlet 9, reactor 10, catalyst outlet 11, second coalescing separator 12, products export 13.Premixed device 7 is fixed on the middle part of reactor, it connects the nozzle system 1 of horizontal positioned, outlet is provided with annular space nozzle, high viscosity fluid enters raw material premixed device 7 with active flow from catalyst inlet 9 by circulating pump, low viscosity fluid enters raw material premixed device 7 from the second material inlet 8 is driven, high viscosity reacting fluid is by premixed device 7 and other low viscosity, cryogen Homogeneous phase mixing in a short period of time, be formed as the emulsion of low viscosity, low temperature, mix with driven pipeline 2 again, the symmetrical in opposite directions uniform nozzle system 1 of the level that enters.The nozzle arranged by the port of export after catalyst, alkane, olefin is conically sprayed at a certain angle, the liquid of each nozzle at high speeds ejection clashes in opposite directions, liquid phases of reactants drops to reactor bottom, product and catalyst pass through gravity settling separation, catalyst is discharged from bottom, and reactant is discharged in the middle part of reactor.Discharge from reactor head with the form of gas phase after part alkane vaporization heat absorption, maintain reaction temperature.
Nozzle system 1 comprises working solution entrance 14, injection liquid inlet 15, trunnion 16, mixing chamber 17, nozzle 18, perforation 19, cavity 20, and by screw thread or Flange joint.In reactor, each nozzle axial centre is relative, and distance is 1 ~ 10D, D is jet expansion outer annular diameter.Jet expansion is annular space, and jet expansion is annular space, and the area of annular space is 5 ~ 40% of outer shroud area, and the area of preferred annular space is 10 ~ 30% of outer shroud area.Perforation diameter is d, and throat pipe diameter is 1 ~ 10d, and optimizing choke diameter is 1 ~ 5d; Nozzle outer annular diameter D is 10 ~ 30d, and preferred nozzle outer annular diameter D is 10 ~ 20d; Mixer length is 5 ~ 100d, and preferred mixer length is 10 ~ 50d.Premixed device 7 comprises working solution entrance 21, injection liquid inlet 22, trunnion 23, mixing chamber 24, perforation 25, cavity 26, and is threaded connection.The perforation diameter of premixed device 7 is d, and throat pipe diameter is 1 ~ 6d, and optimizing choke diameter is 1 ~ 5d; Mixer length is 10 ~ 60d, and preferred mixer length is 10 ~ 50d.Nozzle system 1 is used by one or more similar structures in series with premixed device 7.Premixed device also can adopt other liquid liquid mixing arrangements such as static mixer.The height of products export 13 should ensure that the liquid residence time of outlet less than 13 is not less than the separation time of product and catalyst, and by the catalyst in the further products of separated of the second coalescing separator 12 of ring-type.First coalescing separator 6 should make oil phase fully be separated mutually with catalyst with the second coalescing separator 12, selects oleophilic drainage material and the anion ion liquids such as load trifluoro sulfonate radical, bisulfate ion or perfluorinated sulfonic acid root.
The utility model has obvious advantage and useful effect than prior art:
The percussion flow heterophase reactor that the utility model is designed, strengthening blender relies on the methods such as the geometries changing passage in blender to come molecular diffusion and the convection current of enhance fluid, increase the convection current mixing portion of microfluid, thus increase effective contact area of microfluid, improve the mixing efficiency of liquid, the Quick uniform mixing of low reynolds number fluid under minute yardstick at short notice can be realized.Structure of reactor is simple, and liquid liquid contact area is large, does not have mixing component, not easily leaks, possess the performances such as reaction temperature is easily controlled, good heat and mass transport performance, widely adaptability.The rapidly and efficiently hybrid reaction of immiscible two kinds of fluids in large-scale production can be realized, suppress side reaction simultaneously, improve the selective of product.Can petrochemical industry be widely used in, be specially adapted to the liquid phase reactor of high viscosity fluid, as the concentrated sulfuric acid or the reaction of ionic liquid-catalyzed carbon tetra-alkylation 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;
Figure 1 shows that the schematic diagram of the utility model percussion flow heterophase reactor, comprising: nozzle system 1, first material inlet 2, demister 3, gaseous phase outlet 4, safety relief mouth 5, first coalescing separator 6, premixed device 7, second material inlet 8, catalyst inlet 9, reactor 10, catalyst outlet 11, second coalescing separator 12, products export 13.
Figure 2 shows that nozzle system 1 schematic diagram of the utility model percussion flow heterophase reactor, comprise working solution entrance 14, injection liquid inlet 15, trunnion 16, mixing chamber 17, nozzle 18, perforation 19, cavity 20, and be threaded connection.
Figure 3 shows that premixed device 7 schematic diagram of the utility model percussion flow heterophase reactor, comprise working solution entrance 21, injection liquid inlet 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 utility model is described in further detail, but the utility model is not subject to any restriction thus:
The schematic diagram of percussion flow heterophase reactor in accompanying drawing 1, comprising: nozzle system 1, first material inlet 2, demister 3, gaseous phase outlet 4, safety relief mouth 5, first coalescing separator 6, premixed device 7, second material inlet 8, catalyst inlet 9, reactor 10, catalyst outlet 11, second coalescing separator 12, products export 13.Premixed device 7 is fixed on the middle part of reactor, it connects the nozzle system 1 of horizontal positioned, outlet is provided with annular space nozzle, high viscosity fluid enters raw material premixed device 7 with active flow from catalyst inlet 9 by circulating pump, low viscosity fluid enters raw material premixed device 7 from the second material inlet 8 is driven, high viscosity reacting fluid is by premixed device 7 and other low viscosity, cryogen Homogeneous phase mixing in a short period of time, be formed as the emulsion of low viscosity, low temperature, mix with driven pipeline 2 again, the symmetrical in opposite directions uniform nozzle system 1 of the level that enters.The nozzle arranged by the port of export after catalyst, alkane, olefin is conically sprayed at a certain angle, the liquid of each nozzle at high speeds ejection clashes in opposite directions, liquid phases of reactants drops to reactor bottom, product and catalyst pass through gravity settling separation, catalyst is discharged from bottom, and reactant is discharged in the middle part of reactor.Discharge from reactor head with the form of gas phase after part alkane vaporization heat absorption, maintain reaction temperature.
As shown in Figure 2, each nozzle axial centre is relative, and distance is 1 ~ 10D, D is jet expansion outer annular diameter for nozzle system 1.Jet expansion is annular space, and the area of annular space is 10 ~ 30% of outer shroud area.Perforation diameter is d, and throat pipe diameter is 1 ~ 5d, and nozzle outer annular diameter D is 10 ~ 20d, and mixer length is 10 ~ 50d.As shown in Figure 3, perforation diameter is d to premixed device 7 structure, and throat pipe diameter is 1 ~ 5d, and mixer length is 10 ~ 50d.Premixed device also can adopt other liquid liquid mixing arrangements such as static mixer.The height of products export 13 should ensure that the liquid residence time of outlet less than 13 is not less than the separation time of product and catalyst, and by the catalyst in the further products of separated of the second coalescing separator 12 of ring-type.First coalescing separator 6 should make oil phase fully be separated mutually with catalyst with the second coalescing separator 12, selects oleophilic drainage material and the anion ion liquids such as load trifluoro sulfonate radical, bisulfate ion or perfluorinated sulfonic acid root.

Claims (6)

1. percussion flow heterophase reactor, comprise: nozzle system (1), first material inlet (2), demister (3), gaseous phase outlet (4), safety relief mouth (5), first coalescing separator (6), premixed device (7), second material inlet (8), catalyst inlet (9), reactor (10), catalyst outlet (11), second coalescing separator (12), products export (13), it is characterized in that: premixed device 7 is fixed on the middle part of reactor, it connects the nozzle system (1) of horizontal positioned, outlet is provided with annular space nozzle, high viscosity fluid enters raw material premixed device (7) by circulating pump with active flow, low viscosity fluid enters raw material premixed device (7) from the second material inlet (8) is driven, mix with driven pipeline first material inlet (2) again, the symmetrical in opposite directions uniform nozzle system (1) of the level that enters.
2. percussion flow heterophase reactor according to claim 1, it is characterized by described nozzle system (1) and comprise working solution entrance (14), injection liquid inlet (15), trunnion (16), mixing chamber (17), nozzle (18), perforation (19), cavity (20), and be threaded connection; Each nozzle axial centre is relative, and distance is 1 ~ 10D, D is jet expansion outer annular diameter; Jet expansion is annular space, and the area of annular space is 5 ~ 40% of outer shroud area; Perforation diameter is d, and throat pipe diameter is 1 ~ 10d, and nozzle outer annular diameter D is 10 ~ 30d, and mixer length is 5 ~ 100d.
3. percussion flow heterophase reactor according to claim 1, it is characterized by described premixed device (7) structure and comprise working solution entrance (21), injection liquid inlet (22), trunnion (23), mixing chamber (24), perforation (25), cavity (26), and be threaded connection; Perforation diameter is d, and throat pipe diameter is 1 ~ 6d, and mixer length is 10 ~ 60d.
4. nozzle system according to claim 2 (1), the area that its feature is preferably annular space is 10 ~ 30% of outer shroud area; Perforation diameter is d, and throat pipe diameter is 1 ~ 5d, and nozzle outer annular diameter D is 10 ~ 20d, and mixer length is 20 ~ 40d.
5. percussion flow heterophase reactor according to claim 1, is characterized by nozzle system (1) and is used by one or more similar structures in series with premixed device (7).
6. percussion flow heterophase reactor according to claim 1, it is characterized by the first coalescing separator (6) should make oil phase fully be separated mutually with catalyst with the second coalescing separator (12), selects oleophilic drainage material and the anion ion liquids such as load trifluoro sulfonate radical, bisulfate ion or perfluorinated sulfonic acid root.
CN201520372727.2U 2015-04-28 2015-06-02 Percussion flow heterogeneous reaction ware Expired - Fee Related CN205042452U (en)

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