CN101274249A - Novel liquid-liquid heterophase reactor - Google Patents

Novel liquid-liquid heterophase reactor Download PDF

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CN101274249A
CN101274249A CNA2007101522865A CN200710152286A CN101274249A CN 101274249 A CN101274249 A CN 101274249A CN A2007101522865 A CNA2007101522865 A CN A2007101522865A CN 200710152286 A CN200710152286 A CN 200710152286A CN 101274249 A CN101274249 A CN 101274249A
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liquid
reactor
chamber
tedge
riser
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CN101274249B (en
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卢春喜
刘植昌
刘梦溪
范怡平
周建军
徐春明
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China University of Petroleum Beijing
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China University of Petroleum Beijing
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Abstract

The invention provides a novel liquid-liquid multi-phase reactor device, comprising three different structures: an injection-typed circumfluence reactor, an impact flow lifting pipe reactor and a reinforced mass transfer gathering beam fibre filling material reactor; wherein, the injection-typed external circumfluence reactor (shown as figure 1) uses kinetic energy generated by the liquid injection to lead the reaction liquid which can be circulated used to circularly flow in the reactor, to be excellently mixed and reacted; the impact flow lifting pipe reactor (shown in figure 5) leads three reaction liquids to pass through multi-time butt-impact, crushing and mixing and carry out the reaction in the lifting pipe; the reinforced mass transfer gathering beam fibre filling material reactor (shown in picture 9) is internally provided with a plurality of fibre silks, so as to lead the reaction liquid to flow downwards from the surface of the fibre silk and to form two liquid film layer to carry out the reaction. The reactor of the invention has good liquid crushing and mixing effect and large liquid-liquid contact area, is widely applied to the fields of petroleum, chemicals, environments, etc., is especially suitable for the reaction between high viscosity liquid and liquid, such as ion liquid catalysis alkylation, P-noke method oil product catalytic oxidation reaction, etc.

Description

Novel liquid-liquid heterophase reactor
Technical field
The present invention relates to novel liquid-liquid heterophase reactor equipment, the liquid-liquid-liquid heterophase reactor equipment that particularly viscosity is bigger belongs to fields such as oil, chemical environment, biology.
Background technology
The mixed effect of the liquid-liquid two-phase of not dissolving each other has material impact to the conversion ratio and the selectivity of liquid-liquid reactions.At present, realize that the device category of liquid-liquid two-phase mixing is a lot, as: stirred tank, static mixer, percussion flow blender etc.
Common stirred tank mainly is made of teeter chamber, baffle plate, agitating device and sealing device.This device is applied widely, based on intermittently operated.The time scale of mixing a few minutes to several hours between, be usually used in the relatively slow reaction system of reaction rate.But therefore stirred tank, is difficult to the sealing of assurance device owing to introduce mechanical rotation equipment under middle and high press operation condition.
Static mixer is the nearest mixing apparatus that grew up in 20 years, is a kind of fluid circuit structure that does not have mechanical rotation.Fluid is when flowing through static mixer, and mixed element divisions becomes very thin thin slice, and the power power that its quantity is pressed parts number increases, and finally becomes small drop, thereby reaches sufficient mixing.Static mixer has that running cost is low, and floor space is little, compact conformation, is difficult for leaking, not having revolving member and make advantages such as easy for installation.But, for having the mixed process that solid produces, static mixer is stopped up, be difficult to clear up.In addition, also there are fatal shortcomings such as pressure drop is excessive in static mixer.
The percussion flow blender is a kind of novel mixing apparatus.It is conceived substantially makes nozzle ejection and the bump of two bursts of logistics by coaxial arrangement.Infiltrate reverse flow because inertia, particle pass striking face, and do the convergent oscillation campaign back and forth.Consequently make the alternate relative velocity of particle high, especially the transmittance process of external diffusion control is comparatively effective to strengthening heat, matter transmittance process.But the time scale of percussion flow blender is generally less than 1 second, and requires inlet pressure very high, forms the dead band easily in the zone away from nozzle, makes distribution of reaction products inhomogeneous.Present impact flow reactor is the structure that screw is set in guide shell, introduced a kind of submergence circulation impact flow reactor as Chinese patent ZL00230326.4, though the impact flow reactor of this structure has improved mixing efficiency, also comes with some shortcomings.Motor shaft as screw is a cantilever structure, easily causes the vibration of screw and motor shaft during operation, secondly, also is difficult to guarantee the sealing of motor shaft when operating condition is mesohigh.Patent 200510045866.6 has been introduced a kind of impact flow reactor that does not have screw, utilize centrifugal pump energy to be provided, to produce head-on collision for liquid, though this structure has been avoided some shortcomings of traditional impact flow reactor, but, still be difficult to reach the good mixing effect for the reaction between the multiply high viscosity liquid.
External loop reactor is a kind of heterophase reactor efficiently, patent 01272218.2 has been introduced a kind of gas-liquid, the solid external loop reactor of gas-liquid, the kinetic energy that sprays by gas produces circulation, but its tedge adopts inverted cone-shaped structure, reactant is not that the form with piston flow flows in the process that tedge rises, cause back-mixing thus, be unfavorable for improving the conversion ratio of reaction.
For the reaction between the high viscosity liquid liquid, the vertical reactor (as United States Patent (USP) 3281213) of the horizontal reactor (as Chinese patent ZL200520078557.3, United States Patent (USP) 3281213) of the present also promising band agitating device that extensively adopts and band riser, the former is mainly used in the sulfuric acid process alkylation process, and the latter is mainly used in hydrofluoric acid method alkylation process.
Patent ZL200520078557.3 has introduced the horizontal reactor in a kind of sulfuric acid process alkylation process, and main body is a horizontal pressure vessel, and an inner circulating tube, a tube bank and a mixing auger oar of taking reaction heat away are arranged.Reaction feed and recycle acid enter the suction side of screw, and under the driving of screw, reaction mass spreads rapidly and forms emulsion with acid.Emulsion ceaselessly circulates and reacts at a high speed in reactor.In the discharge side of screw, a part of emulsion is drawn into acid settler, carries out the separation of acid.Acid turns back to the screw suction side of reactor then owing to proportion sinks to the settler bottom greatly.Back-mixing in this reactor is bigger, is unfavorable for improving the conversion ratio of reaction.U.S. Pat 6194625B1 has introduced a kind of alkylation reactor of sectional feeding, reaction zone is separated into the section of several series connection, fresh feed is separated into several stocks does not introduce each reaction section, the high viscosity reactant that recycles then is a series flow, adopts churned mechanically mode to mix in each reaction section.Though this structure has overcome the bigger problem of back-mixing, structure is too complicated.In addition, these two kinds of structures have all adopted the electric motor driven paddle of fixed rotating speed, are easy to leak because of poorly sealed.
United States Patent (USP) 3281213 has proposed a kind of vertical reactor, its main body is a riser, riser is connected with a horizontal tank, the high viscosity reactant is housed in the horizontal tank, other two kinds of reactants spray into by the nozzle of riser bottom, the high viscosity reactant that the gravitation that injection causes is driving in the horizontal tank enters riser together, and reaction is promptly carried out in this root riser reactor.The riser top is connected with a knockout drum, is used for the separation of product.High viscosity reactant circulation after the separation enters the horizontal tank of riser bottom.This structure does not adopt the mechanical rotation member, has solved a series of problems that built-in screw brings.But the high viscosity reactant can not be satisfactory with mixing of other reactants, and in addition, the whole reactor system has adopted a riser, two horizontal tanks and a down-comer, and equipment is huge, structure is also compact inadequately.
Summary of the invention
Main purpose of the present invention is to provide the reactor that is applicable to that liquid-liquid, liquid-liquid-liquid heterogeneous reaction are especially reacted between high viscosity liquid.This reactor can will be ground into very little drop or more low viscous reaction liquid be pulled into very thin liquid film than the low viscosity reaction liquid, high viscosity liquid is evenly mixed in a short period of time with other reactants, very big liquid liquid phase contact area is provided, makes reaction reach very high conversion ratio.
The present invention has tangible advantage and useful effect than prior art:
The novel liquid-liquid heterophase reactor that the present invention designs, simple in structure, liquid-liquid contact area is big, does not have mixing component, is difficult for leaking.Can be widely used in petrochemical industry, be specially adapted to full-bodied liquid reactants, as ionic liquid-catalyzed hydro carbons alkylated reaction etc.
Description of drawings
Fig. 1 a is the structural representation of injecting type external loop reactor;
Fig. 1 b is the structural representation of injecting type common loop reactor;
Fig. 2 is the structural representation of fluid injector;
Fig. 3 is layering chamber 5 structural representations;
Fig. 4 is the structural representation of liquid distributing pipe;
Fig. 5 is the structural representation of percussion flow riser reactor
Fig. 9 strengthens mass transfer boundling fiberfill reactor
Figure 10 strengthens in the mass transfer boundling fiberfill reactor two kinds of liquid flows, contact schematic diagram.
The specific embodiment
Novel liquid-liquid heterophase reactor of the present invention is realized by following approach: this reactor comprises three kinds of different structures.(Fig. 1 a), injecting type common loop reactor (Fig. 1 b), percussion flow promote tubular reactor (Fig. 5) and reinforcement mass transfer boundling fiberfill reactor (Fig. 9) to be respectively the injecting type external loop reactor.The present invention is described in further detail below in conjunction with accompanying drawing and specific embodiment:
Accompanying drawing 1a is depicted as embodiment 1 of the present invention, i.e. injecting type external loop reactor schematic diagram.At least comprise: nozzle system 1, tedge 2, downspout 3, liquid distributing pipe 4, layering chamber 5, reacting product outlet 6, liquid distributing pipe import 7, trunnion 8, mixing chamber 9 and liquid-inlet 10.It is characterized in that: mixing chamber 9 is positioned at reactor bottom, and it is provided with liquid-inlet 10; The inlet tube of nozzle system 1 is fixed on mixing chamber 9 walls, and the port of export is provided with nozzle, towards trunnion 8; Mixing chamber 9 links to each other with trunnion 8; Trunnion 8 is connected with tedge 2; Tedge 2 tops are connected with layering chamber 5, and liquid distributing pipe 4 inserts in the tedge 2, and downspout 3 one ends are connected with layering chamber 5, and the other end is connected with the minimum place of trunnion 8 diameters.As shown in Figure 2, nozzle system 1 is made up of inlet tube, surge chamber, nozzle; The axis of nozzle is parallel with the axis of tedge 2; Jet expansion and downspout 3 export center linear distances are less than injection stream length.The nozzle percent opening is 5%~20% (is benchmark with trunnion 8 throat's minimum diameter place sectional areas).The length of trunnion 8 is 1~4D, and wherein D is tedge 2 internal diameters, and trunnion 8 throat diameters are 0.5D~0.9D.Tedge 2 length should guarantee that the time of staying of liquid in tedge 2 is not less than the liquid reactions time.Layering chamber 5 should comprise two kinds of structures shown in accompanying drawing 3a, a kind of is that 5 bottoms, layering chamber awl section directly is connected with tedge 2, another kind of the cylinder lower end is connected with layering chamber 5 in order in the layering chamber 5 cylindrical section to be set, and liquid enters layering chamber 5 by cylinder 2 top overflows.The volume of layering chamber 5 should guarantee that the time of staying of liquid in layering chamber 5 is not less than the time of liquid standing demix.Layering chamber 5 diameters are 1.5~6D, and drum diameter is 0.8~2.5D, and the cylinder top is 0.2~1D apart from layering chamber 5 top spacings, and 5 direct tube section lower edges distance is 0.5~1.5D to downspout 3 center line of suction apart from the layering chamber.Liquid distributing pipe 4 inserts in the tedges 2, and the difference of tedge 2 diameters and liquid distributing pipe 4 diameters is not more than 2L, and wherein L is the jet length of liquid when being sprayed by aperture on the liquid distributing pipe 4; As shown in Figure 4, evenly be furnished with aperture in 360 ° of scopes on the liquid distributing pipe 4, flow out for the third reaction liquid, the percent opening on the liquid distributing pipe 4 is 5%~30% (is benchmark with liquid distributing pipe 4 outer surfaces); Liquid distributing pipe 4 ends are back taper, and the injector spacing of back taper summit and nozzle system 1 is 1~5D.Downspout 3 can be many, and downspout 3 upper ends are connected with layering chamber 5, and 5 direct tube section lower edges distance is 0.5~1.5D apart from the layering chamber in the junction; Downspout 3 lower ends are connected with trunnion 8 throats, and the junction is the minimum place of throat diameter; The cross-sectional area of downspout 3 is 0.5~3 times of tedge 2 cross-sectional areas.Course of reaction is: a kind of reaction liquid is injected by the mixing chamber bottom, and another strand liquid sprays at a high speed in the trunnion 8 by the nozzle of fluid injector 1.In tedge 2, upwards flow after two bursts of liquid premixeds, and with the 3rd burst of liquid rapid mixing by the ejection of the aperture on liquid distributing pipe 4 tube walls.Behind the layering chamber 5 above the mixing material arrival tedge 2, speed reduces, and realizes that liquid-liquid partly separates.High viscosity liquid flows downward by the downspout 3 of tedge 2 arranged outside, reenters tedge 2 circular responses by trunnion 8 throat positions; Another part mixing material (reactant that product and unreacted are intact) by two reacting product outlet 5 outflow reactors that tedge 2 tops are provided with, enters the subsequent treatment unit.
Accompanying drawing 1b is depicted as embodiment 2 of the present invention, i.e. injecting type common loop reactor schematic diagram.At least comprise: nozzle system 1, tedge 2, downspout 3, liquid distributing pipe 4, layering chamber 5, reacting product outlet 6, liquid distributing pipe import 7, mixing chamber 9 and liquid-inlet 10.It is characterized in that: mixing chamber 9 is positioned at reactor bottom, and it is provided with liquid-inlet 10; The inlet tube of nozzle system 1 is fixed on mixing chamber 9 walls, and the port of export is provided with nozzle; Mixing chamber 9 is connected with downspout 3; Tedge 2 with its arranged concentric is arranged in the downspout 3, and downspout 3 tops are connected with layering chamber 5, and liquid distributing pipe 4 is inserted in the tedge 2 by the top.As shown in Figure 2, nozzle system 1 is made up of inlet tube, surge chamber, nozzle; The axis of nozzle is parallel with the axis of tedge 2; Jet expansion and downspout 3 export center linear distances are less than injection stream length.The nozzle percent opening is 5%~20% (is benchmark with mixing chamber 9 top exit cross sections).Tedge 2 length should guarantee that the time of staying of liquid in tedge 2 is not less than the liquid reactions time.Mixing chamber 9 tops are the undergauge structure, and tedge 2 bottoms also are the undergauge structure, are separated with an intersegmental crack mutually between tedge 2 bottoms and mixing chamber 9 tops, and this gap is the outlet of downspout 3; Tedge 2 bottom undergauges, downspout 3 outlets and mixing chamber 9 top undergauges surround a structure that is similar to trunnion.Layering chamber 5 comprises two kinds of structures shown in accompanying drawing 3b, a kind of is without any inner member in the layering chamber 5, another kind of in the layering chamber 5 cylindrical section being set, the cylinder lower end is connected with layering chamber 5, cylinder is divided into 2 parts with layering chamber 5: middle circular space and outside annular space, liquid enters circular space by tedge, enters annular space by cylinder 2 top overflows.The volume of layering chamber 5 should guarantee that the time of staying of liquid in layering chamber 5 be not less than the liquid standing demix time, and layering chamber 5 diameters are 1.5~6D.Liquid distributing pipe 4 inserts in the tedges 2, and the difference of tedge 2 diameters and liquid distributing pipe 4 diameters is not more than 2L, and wherein L is the jet length of liquid when being sprayed by aperture on the liquid distributing pipe 4; As shown in Figure 4, evenly be furnished with aperture in 360 ° of scopes on the liquid distributing pipe 4, flow out for the third reaction liquid, the percent opening on the liquid distributing pipe 4 is 5%~30% (is benchmark with liquid distributing pipe 4 outer surfaces); Liquid distributing pipe 4 ends are back taper, and the injector spacing of back taper summit and nozzle system 1 is 1~5D.The annular space that downspout 3 surrounds for tedge 2 and reactor wall, downspout 3 upper ends are connected with layering chamber 5, and downspout 3 lower ends are connected with mixing chamber 9 tops; Total cross-sectional area of downspout 3 is 0.5~3 times of tedge 2 cross-sectional areas.Course of reaction is: a kind of reaction liquid is injected by the mixing chamber bottom, and another strand liquid sprays at a high speed by the nozzle of fluid injector 1.In tedge 2, upwards flow after two bursts of liquid premixeds, and with the 3rd burst of liquid rapid mixing by the ejection of the aperture on liquid distributing pipe 4 tube walls.Behind the layering chamber 5 above the mixing material arrival tedge 2, speed reduces, and realizes that liquid-liquid partly separates.High viscosity liquid flows downward by downspout 3, reenters tedge 2 circular responses by downspout 3 bottoms; Another part mixing material (reactant that product and unreacted are intact) by two reacting product outlet 5 outflow reactors that tedge 2 tops are provided with, enters the subsequent treatment unit.
Accompanying drawing 5 is depicted as embodiment 2 of the present invention, be the structural representation of percussion flow riser reactor, comprise at least: riser outlet 1 ', riser 2 ', umbrella crown baffle plate 3 ', nozzle system 4 ', liquid distribution trough 5 ', bump chamber 6 ', liquid feed pipe 7 '.At same reactor internal reaction, wherein can distinguish, add in the reactor successively by two or three liquid in two kinds or three kinds of liquid for this reactor adapted.The bump chamber is positioned at the bottom of percussion flow riser reactor, and its effect is that two kinds of reaction liquids are tentatively mixed.Bump chamber 6 ' is provided with two fluid injectors, and two kinds of reaction liquids enter the bump chamber by two nozzle ejection respectively, produce great shearing force during bump, and liquid is ground into minimum drop and makes it mutual mixing.Difference according to mixed effect, the axis of two nozzles can overlap (accompanying drawing 7a), thereby when clashing, reaction liquid produces maximum pulverizing and mixed effect, but the axis of two nozzles also but shape is in an angle, thereby make mixing material after head-on collision circulation mobile (accompanying drawing 7b) or in bump chamber 6 ' along circumferential flow (accompanying drawing 7c), so not only can avoid drop to produce coalescence, and can avoid clashing into chamber 6 ' and the dead band occurs.The axis of two nozzles can with the bump chamber axis vertical certain angle (accompanying drawing 6) that also can form.Fluid injector can flush with bump chamber wall, also can stretch into the bump chamber, and the built-in length of fluid injector can be inconsistent, and distance is less than two bursts of liquid stream jet length sums between fluid injector.Because the flow difference of two strands of reaction liquids, therefore the diameter of two nozzles might not be identical, but should make the spouting velocity of two kinds of liquid identical as far as possible.Bump chamber diameter is 1~5 times of riser diameter, and bump chamber volume should guarantee that mixing material is not more than the time of its standing demix in the indoor time of staying of bump.Be provided with liquid distribution trough 5 ' between bump chamber and the riser flange, so that the liquid that comes out in the bump chamber 6 ' mixes again, the form of its liquid distribution trough 5 ' is a sieve plate, and percent opening is not more than 20%.The riser bottom is provided with fluid injector 4 ' (accompanying drawing 8), the nozzle top is connected with umbrella crown baffle plate 3 ' by supporting leg, reaction liquid impinging jet by the nozzle ejection is ground into tiny drop on umbrella crown baffle plate 3 ', after the jet of the mixing material that drop and liquid distribution trough come out contacts, under the effect of shearing force, pulverized again, and fully mixed with it.The spacing H at umbrella crown baffle plate top and nozzle top 1Jet length less than liquid stream.Umbrella crown baffle plate diameter is 1~5 times of nozzle entrance pipe diameter.For guaranteeing that the annular space space between umbrella crown baffle plate 3 ' and riser 2 ' can guarantee that liquid normally passes through, the caliber that riser 2 ' bottom is provided with is bigger usually.The riser bottom links to each other with the middle and upper part by undergauge.The spacing at undergauge lower edge to umbrella crown baffle plate top is H 10~5 times, undergauge lower edge diameter is 1~3 times of upper edge diameter.The mixing material of three kinds of liquid enters the riser middle and upper part through undergauge, and is upwards mobile with the form of piston flow, meanwhile reacts.Riser length was determined according to the time of staying of liquid reactions.For preventing liquid to the washing away and wear and tear of riser top, the riser outlet flushes with the riser top, but with a certain distance from the riser top H is arranged 3, H 3Be 0~5 times of riser diameter.Need to prove, should make the relatively large reaction liquid of viscosity by bump chamber fluid injector charging, with abundant raising mixed effect.
Accompanying drawing 9 is depicted as embodiment 3 of the present invention, promptly strengthen the structural representation of mass transfer boundling fiberfill reactor, at least comprise: reactor body 6 "; mass transfer space 2 ", boundling filament filler 1 "; cover head 7 ", reaction liquid distributor 10 "; 11 ", liquid re-distributor 12 "; separate and subside jar 3 ", strengthen mass transfer circulation pipe 13 " form; it is characterized in that: reactor body 6 " be divided into, in, the lower part, reactor body 6 " top be provided with reaction liquid import 8 "; 9 ", wherein liquid-inlet 8 " with liquid distribution trough 10 " be connected; Liquid-inlet 9 " be located at fluid distributor 10 " fluid distributor 11 of below " be connected; reactor body 6 " the middle part be mass transfer space 2 "; its inside is provided with a large amount of boundling filament fillers 1 " and fluid redistributor 11 "; reactor body 6 " the bottom be separate and subside jar 3 ", fibre bundle 1 " end 5 " be arranged on separate and subside jar 3 " and two kinds of liquid surfaces 4 " under.At separate and subside jar 3 " on be provided with strengthen mass transfer circulation pipe 13 ", strengthen mass transfer circulation pipe 13 " end 14 " can be arranged on two kinds of liquid surfaces 4 as required " and on or under.
Wherein, described reactor body 6 " draw ratio 1~50.
Wherein, described liquid distribution trough 10 ", 11 " can be the liquid distribution trough of orifice-plate type, overflow-type, three kinds of structures of tubular type.
Wherein, the quantity of described liquid re-distributor 12 is that a cover is above.
Wherein, described boundling filament 1 " packed density 0.1~30%.
Wherein, described boundling filament filler 1 ", every bundle includes 10~50000 of filaments.
Wherein, described boundling filament 1 ", the filament diameter that every bundle comprises is between 3~2500 microns.
Wherein, described boundling filament 1 ", the filament that every bundle comprises can adopt metal material, as non-ferrous metal alloy, stainless steel, carbon steel; or nonmetallic materials comprise glass fibre, staple fibre, nylon, polyester material as fiber in the nonmetallic materials.
Wherein, described boundling filament filler 1 " end can be fixing or freely dangle.
Wherein, described reinforcement mass transfer circulation pipe 13 " end 14 " can be arranged on two kinds of liquid surfaces 4 as required " and on or under.
When two kinds of liquid that participate in reaction from its top feed mouth 8 ", 9 " when flowing into, in boundling fiberfill 1 " each root filament surface, all exist two kinds of liquid that participate in reaction, as shown in figure 10.First kind of liquid is through distributor 11 " enter into mass transfer space 2 " lining, under gravity and capillary effect, along filament 1 " the surface form very thin liquid film, its surface is expanded.Second kind of liquid enters into mass transfer space 2 through another liquid distribution trough 10 ", under gravity and capillary effect, also along filament 1 " the surface form liquid film.Because two kinds of liquid are at filament 1 " the surface tension difference; again because the flow velocity difference (in general; the flow velocity height of first kind of liquid of second kind of flowing fluid ratio) of two-phase, thereby two alternate frictional force draw liquid film extremely thin, for two kinds of liquid provide great contact area.Two kinds of liquid are at filament 1 in addition " the surface constantly flow and upgrade, exist bigger concentration gradient motive force in the mass transport process all the time, therefore strengthening mass transfer boundling fiberfill reactor is mass transfer, a consersion unit efficiently.In mass transfer, course of reaction, the interface of two kinds of liquid remains, the generation of no disperse and emulsion.
At reactor body 6 " the bottom, separate and subside jar 3 " in because two kinds of liquid exist density contrast, thereby both can separate and form the interface of two kinds of liquid rapidly.The higher a kind of liquid of density can be along boundling fiberfill 1 " end 5 " flow directly to separate and subside jar 3 " and the jar end; the separate mode of this cleaning has been avoided the disperse phase separation problem that conventional method ran into; thus two-phase can separate up hill and dale rapidly, fundamentally avoided emulsification and carried the appearance of phenomenon secretly.
Form boundling fiberfill 1 " filament, according to the difference of technological requirement, can adopt metal material, as non-ferrous metal alloy, stainless steel, carbon steel etc.; Perhaps adopt nonmetallic materials as filler, comprise glass fibre, staple fibre, nylon, polyester material etc.The definite of filament material should follow two principles: this filament must soak into easily with two kinds of liquid that participate in reaction; In addition, this material can not cause adverse influence to reaction, simultaneously, can not be destroyed by two kinds of reaction liquid institute burn intos; Boundling fiberfill 1 " packed density (this packed density is defined as: all boundling fiberfill 1 " total sectional area/mass transfer space 2 " area in cross section) should be controlled between 0.1~30%; Boundling fiberfill 1 " the filament diameter should be controlled between 3~2500 microns.For some metallic fibers, for example stainless steel fibre before being fit into reactor, is at first shaken up it again, and purpose is to increase processing area for further, and then draws in reactor; In concrete use, all filaments can be divided into some bundles, every bundle comprises 10~50000 of fibers; Form boundling fiberfill 1 "; In order to improve the membrane effect, boundling fiberfill 1 " end 5 " adopt fixing or freely dangle.
In the present invention, mass transfer space 2 " wall effect be a very important problem because the existence of limit wall, the device mass-transfer efficiency that has even reduce by 40%, especially in the less device of reactor diameter, its influence is even more serious.Therefore, in the present invention, in mass transfer space 2 " inwall array of fluid redistributor 12 is installed ", its objective is and eliminate wall stream, reduce wall effect.
On version, liquid distribution trough 10 ", 11 " can distinguish the difference of two kinds of liquid mediums and the size for the treatment of capacity determines to adopt orifice-plate type, overflow-type and three kinds of forms of tubular type.
As dirt in, the liquid less in opereating specification less and the situation of reactor diameter less (diameter is less than 1m) adopts the orifice-plate type fluid distributor; And in, the liquid less in opereating specification dirt less and the tower diameter reactor diameter situation of big (diameter is greater than 1m) adopts the tubular type fluid distributor.
Otherwise the more and reactor diameter of the dirt situation of big (diameter is greater than 1m) adopts the overflow-type fluid distributor in, the liquid big in opereating specification.
In above-mentioned three kinds of liquid distribution troughs, the density of spray point should remain on 65~90/square metre principle and determine.
In the technical program, in order to promote reaction effect, at separate and subside jar 3 " on be provided with strengthen mass transfer circulation pipe 13 ".If the effect of the contact of two kinds of liquid, reaction is undesirable, can be according to arts demand with settling tank 3 " in wherein a kind of liquid extract out, through strengthening mass transfer circulation pipe 13 " get back to liquid-inlet 8 " or 10 " in, participate in reaction once more.
According to arts demand, if be drawn out of, to participate in the fluid density of reaction once more higher, then strengthens mass transfer circulation pipe 13 " end 14 " be arranged on two kinds of liquid surfaces 4 " under; If instead be drawn out of, to participate in the fluid density of reaction once more lower, then strengthens mass transfer circulation pipe 13 " end 14 " be arranged on two kinds of liquid surfaces 4 " on
It should be noted that at last: above embodiment only in order to the explanation the present invention and and unrestricted technical scheme described in the invention; Therefore, although this specification has been described in detail the present invention with reference to each above-mentioned embodiment,, it will be understood by those of skill in the art that still and can make amendment or be equal to replacement the present invention; And all do not break away from the technical scheme and the improvement thereof of the spirit and scope of the present invention, and it all should be encompassed in the middle of the claim scope of the present invention.

Claims (16)

1, novel liquid-liquid heterophase reactor is characterized in that: this reactor comprises three kinds of different structures.Be respectively injecting type circulation flow reactor (Fig. 1 a, Fig. 1 b), percussion flow lifting tubular reactor (Fig. 5) and strengthen mass transfer boundling fiberfill reactor (Fig. 9).Wherein the injecting type circulation flow reactor is divided into outside circulation (Fig. 1 a) and two kinds of structures of interior circulation (Fig. 1 b).
(see Fig. 1 a), it is characterized in that: described injecting type external loop reactor comprises the novel liquid-liquid heterophase reactor of first kind of structure at least: nozzle system 1, tedge 2, downspout 3, liquid distributing pipe 4, layering chamber 5, reacting product outlet 6, liquid distributing pipe import 7, trunnion 8, mixing chamber 9 and liquid-inlet 10.It is characterized in that: mixing chamber 9 is positioned at reactor bottom, and it is provided with liquid-inlet 10; The inlet tube of nozzle system 1 is fixed on mixing chamber 9 walls, and the port of export is provided with nozzle, towards trunnion 8; Mixing chamber 9 links to each other with trunnion 8 bottoms; Trunnion 8 tops are connected with tedge 2; Tedge 2 tops are connected with layering chamber 5, and liquid distributing pipe 4 is inserted in the tedge 2 by the top, and downspout 3 one ends are connected with layering chamber 5, and the other end is connected with the minimum place of trunnion 8 throat diameters.
Novel liquid-the liquid heterophase reactor of first kind of structure (seeing Fig. 1 b) is characterized in that: described injecting type common loop reactor comprises at least: nozzle system 1, tedge 2, downspout 3, liquid distributing pipe 4, layering chamber 5, reacting product outlet 6, liquid distributing pipe import 7, mixing chamber 9, liquid-inlet 10.It is characterized in that: mixing chamber 9 is positioned at reactor bottom, and it is provided with liquid-inlet 10; The inlet tube of nozzle system 1 is fixed on mixing chamber 9 walls, and the port of export is provided with nozzle; Mixing chamber 9 is connected with downspout 3; Tedge 2 with its arranged concentric is arranged in the downspout 3, and downspout 3 tops are connected with layering chamber 5, and liquid distributing pipe 4 is inserted in the tedge 2 by the top.
Novel liquid-liquid heterophase reactor the (see figure 5) of second kind of structure is characterized in that: described percussion flow riser reactor comprises at least: riser outlet 1 ', riser 2 ', umbrella crown baffle plate 3 ', nozzle system 4 ', liquid distribution trough 5 ', bump chamber 6 ', liquid feed pipe 7 '.It is characterized in that: bump chamber 6 ' is positioned at reactor bottom, it is provided with relative liquid feed pipe 7 ', nozzle system 4 ' is fixed on the bump chamber 6 ', its nozzle makes progress, axis and riser 2 ' dead in line, and umbrella crown baffle plate 3 ' is fixed on the nozzle by supporting leg, be provided with liquid distributor 5 ' between bump chamber 6 ' and riser 2 ' adpting flange, nozzle stretches into riser 2 ' bottom, and riser outlet 1 ' is positioned at riser 2 ' top, adopts T type structure with being connected of riser 2 '.
Novel liquid-liquid heterophase reactor the (see figure 9) of the third structure, it is characterized in that: described reinforcement mass transfer boundling fiberfill reactor comprises at least: reactor body 6 "; mass transfer space 2 ", boundling filament filler 1 "; cover head 7 ", reaction liquid distributor 10 "; 11 ", liquid re-distributor 12 "; separate and subside jar 3 ", strengthen mass transfer circulation pipe 13 " form; it is characterized in that: reactor body 6 " be divided into, in, the lower part, reactor body 6 " top be provided with reaction liquid import 8 "; 9 ", wherein liquid-inlet 8 " with liquid distribution trough 10 " be connected; Liquid-inlet 9 " be located at fluid distributor 10 " fluid distributor 11 of below " be connected; reactor body 6 " the middle part be mass transfer space 2 "; its inside is provided with a large amount of boundling filament fillers 1 " and fluid redistributor 11 "; reactor body 6 " the bottom be separate and subside jar 3 ", fibre bundle 1 " end 5 " be arranged on separate and subside jar 3 " and two kinds of liquid surfaces 4 " under.At separate and subside jar 3 " on be provided with strengthen mass transfer circulation pipe 13 ", strengthen mass transfer circulation pipe 13 " end 14 " can be arranged on two kinds of liquid surfaces 4 as required " and on or under.
2, injecting type external loop reactor according to claim 1 and injecting type common loop reactor is characterized in that: described nozzle system 1 is formed (see figure 2) by inlet tube, surge chamber, nozzle; The axis of nozzle is parallel with the axis of tedge 2; Jet expansion and downspout 3 export center linear distances are less than injection stream length.The nozzle percent opening is 5%~20% (the injecting type external loop reactor is a benchmark with trunnion 8 throat's minimum diameter place sectional areas, and common loop reactor is a benchmark with mixing chamber 9 top exit cross sections); The length of described trunnion 8 is (1~4) D, and wherein D is tedge 2 internal diameters, and trunnion 8 throat diameters are (0.5~0.9) D; Described tedge 2 length should guarantee that the time of staying of liquid in tedge 2 is not less than the liquid reactions time.
3, injecting type external loop reactor according to claim 1 and injecting type common loop reactor, it is characterized in that: described layering chamber 5 comprises two kinds of structures, a kind of is without any inner member in the layering chamber 5, another kind of in the layering chamber 5 cylindrical section (Fig. 3) being set, the cylinder lower end is connected with layering chamber 5, cylinder is divided into 2 parts with layering chamber 5: middle circular space and outside annular space, liquid enters circular space by tedge, enters annular space by cylinder 2 top overflows.The volume of layering chamber 5 should guarantee that the time of staying of liquid in layering chamber 5 is not less than the liquid standing demix time.
4, injecting type external loop reactor according to claim 1 and injecting type common loop reactor, it is characterized in that: described liquid distributing pipe 4 inserts in the tedge 2, the difference of tedge 2 diameters and liquid distributing pipe 4 diameters is not more than 4L, and wherein L is a liquid by the jet length during the aperture ejection on the liquid distributing pipe 4; Percent opening on the liquid distributing pipe 4 is 5%~30% (is benchmark with liquid distributing pipe 4 outer surfaces); Liquid distributing pipe 4 ends are back taper, and the injector spacing of back taper summit and nozzle system 1 is (1~5) D.
5, injecting type circulation flow reactor according to claim 1 is characterized in that: downspout 3 can be many in the described injecting type external loop reactor, and downspout 3 upper ends are connected with layering chamber 5; Downspout 3 lower ends are connected with trunnion 8 throats, and the junction is the minimum place of throat diameter; Total cross-sectional area of downspout 3 is 0.5~3 times of tedge 2 cross-sectional areas.The annular space that downspout 3 surrounds for tedge 2 and reactor wall in the described injecting type common loop reactor, downspout 3 upper ends are connected with layering chamber 5, and downspout 3 lower ends are connected with mixing chamber 9 tops; Total cross-sectional area of downspout 3 is 0.5~3 times of tedge 2 cross-sectional areas.
6, injecting type common loop reactor according to claim 1, it is characterized in that: described mixing chamber 9 tops are the undergauge structure, tedge 2 bottoms also are the undergauge structure, are separated with an intersegmental crack mutually between tedge 2 bottoms and mixing chamber 9 tops, and this gap is the outlet of downspout 3; Tedge 2 bottom undergauges, downspout 3 outlets and mixing chamber 9 top undergauges surround a structure that is similar to trunnion.
7, second kind of structure percussion flow riser reactor according to claim 1, it is characterized in that: described bump chamber is provided with two relative fluid injectors, according to the difference of mixed effect, shape in an angle but the axis of two nozzles can overlap also.The axis of two nozzles can chamber axis be vertical also can form certain angle with bump.Fluid injector can flush with the bump chamber interior walls, also can stretch into the bump chamber, and the built-in length of fluid injector can be inconsistent, and distance should be less than two bursts of liquid stream jet length sums between fluid injector.Bump chamber diameter is 1~5 times of riser diameter, and bump chamber volume should guarantee that mixing material is not more than the time of its standing demix in the indoor time of staying of bump.Be provided with liquid distributor between bump chamber and the riser flange, its form is a sieve plate, and percent opening is not more than 0.5%~10%.
8, second kind of structure percussion flow riser reactor according to claim 1, it is characterized in that: described riser bottom is provided with fluid injector 4 ', the nozzle top is connected with umbrella crown baffle plate 3 ' by supporting leg, the spacing H at umbrella crown baffle plate top and nozzle top 1Jet length less than liquid stream.Umbrella crown baffle plate diameter is 1~5 times of nozzle entrance pipe diameter.
9, second kind of structure percussion flow riser reactor according to claim 1 is characterized in that: described riser bottom is provided with the undergauge structure, and the undergauge lower edge is apart from the spacing H at umbrella crown baffle plate top 2Be H 10~5 times, undergauge lower edge diameter is 1~3 times of upper edge diameter.
10, second kind of structure percussion flow riser reactor according to claim 1 is characterized in that: described riser outlet is apart from the spacing H at riser top 3Be 0~5 times of riser diameter.
11, the third structure-reinforced mass transfer boundling fiberfill reactor according to claim 1 is characterized in that: described reactor body 6 " draw ratio 1~50.Liquid distribution trough 10 ", 11 " can be the liquid distribution trough of orifice-plate type, overflow-type, three kinds of structures of tubular type.
12, the third structure-reinforced mass transfer boundling fiberfill reactor according to claim 1 is characterized in that: the quantity of described liquid re-distributor 12 is that a cover is above.
13, the third structure-reinforced mass transfer boundling fiberfill reactor according to claim 1 is characterized in that: described boundling filament 1 " packed density 0.1~30%; Every bundle includes 10~50000 of filaments; The filament diameter that every bundle comprises is between 3~2500 microns.
14, the third structure-reinforced mass transfer boundling fiberfill reactor according to claim 1, it is characterized in that: described boundling filament 1 "; the filament that every bundle comprises can adopt metal material; as non-ferrous metal alloy, stainless steel, carbon steel; or nonmetallic materials comprise glass fibre, staple fibre, nylon, polyester material as fiber in the nonmetallic materials.
15, the third structure-reinforced mass transfer boundling fiberfill reactor according to claim 1 is characterized in that: described boundling filament filler 1 " end can be fixing or freely dangle.
16, the third structure-reinforced mass transfer boundling fiberfill reactor according to claim 1 is characterized in that: described reinforcement mass transfer circulation pipe 13 " end 14 " can be arranged on two kinds of liquid surfaces 4 as required " and on or under.
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