CN104316556A - Visual fluidized bed reaction analysis system - Google Patents
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- CN104316556A CN104316556A CN201410594385.9A CN201410594385A CN104316556A CN 104316556 A CN104316556 A CN 104316556A CN 201410594385 A CN201410594385 A CN 201410594385A CN 104316556 A CN104316556 A CN 104316556A
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Abstract
The invention relates to a visual fluidized bed reaction analysis system. The system comprises a visual heating furnace and a fluidized reactor placed in the visual heating furnace; a gas inlet of the fluidized bed reactor is connected with a gas flowmeter, a gas outlet is connected with a gas online analysis device; the visual heating furnace comprises a furnace body, the furnace body is orderly provided with an inner tube and an outer pipe from inside to outside; the outer wall of the inner tube is provided with a heating element, the outer wall of the outer tube is provided with an insulation coating, and an observation window is formed on a longitudinal middle part of the insulation coating; the outer tube is capable of rotating along a round groove to facilitate the view angle adjusting. The analysis system disclosed by the invention is simple in structure, small in volume, can be applied to measuring a reaction kinetic parameter of a multi-phase complex system, and approaches to intrinsic kinetics; and the system can be used for the fluidization field to observe the flowing and fluidization behavior of multi-scale structure such as particles and bubbles under the heating state.
Description
Technical field
The present invention relates to the visual fluidized-bed reaction analytic system of the ambit scientific researches such as a kind of energy, chemical industry, metallurgy, biology, material, be specifically related to a kind of visual fluidized-bed reaction analytic system being applied to fluidization field.
Background technology
Fluidized-bed reactor based on particle fluidization technology has the features such as mass transfer, rate of heat transfer is fast, bed temperature is even, tradition and the emerging industry such as be widely used in Coal Chemical Industry, prepared by petrochemical complex, Ferrous Metallurgy, biological medicine, nano material, becomes the important technical of research gas-solid reaction and materials synthesis.But in gas-solid bubbling fluidized bed, gas can form bubble, particle because of the adhesion in course of reaction of intergranular inelastic collision, particle, liquid bridge and fine particle strong Van der Waals force and form agglomerate.The existence of these uneven textures such as bubble and particle agglomeration (being commonly referred to Jie's mesostructure), greatly reduces gas-solid contact efficiency and the back-mixing degree increasing the weight of gas or solid in fluidized bed, thus reduces the selectivity of reaction rate and reaction.In gas-solid fluidized bed, size, motion state and the fluidization quality of the uneven textures (Jie's mesostructure) such as bubble, particle and particle agglomeration are the important factor in order affecting gas-solid reaction in fluidized bed.The acquisition of the dynamic fluidized feature of its bubble and the particle agglomeration process intensification to the design of gas-solid fluidized bed reactor and amplification, gas-solid reaction plays a key effect.
Gas-solid fluidized bed amplification test research is normally by organic glass fluidized bed, particle, the flowing of bubble and flowing situation (cold mould) under research normal temperature condition, again the successful experience of cold work die is applied in hot reaction, and then at high temperature studies particle, the flowing of bubble and flowing situation (hot-die).Because industrial fluidized-bed process is commonly hot reaction (>150 DEG C), particle flow rule under cold conditions pattern, under transferring to hot pattern, by the impact of temperature and reaction, the character of particle or composition will change in hot or course of reaction, and these changes can not directly be obtained by the mode of cold mould.Also need on Cold simulating test basis, further under research heated condition, the flowing of particle (catalyzer) and bubble produce, grow up and rupture process, particularly emerging nano material preparation process.
Usually the method adopted under hot conditions, namely by assaying reaction process the off-line characterization technique of solid particle structure and size after overflow tail gas composition and reaction, the formation of Jie such as bubble and particle agglomeration mesostructure in fluidized-bed reaction process can not be reflected comprehensively, grow up and the dynamic image data intuitively such as fragmentation.In gas-solid fluidized bed, the acquisition of the dynamic fluidized feature such as size and motion state of the flow behavior of individual particle and particle agglomeration, fluidization quality, the bubble research to gas-solid fluidized bed design and amplification, reaction mechanism plays a key effect.By the direct observation to fluidized bed endoparticle fluidized state, bubbly flow and course of reaction, high-speed camera, In-situ Infrared scanning etc., the visual image of the generation of the Multi-scale models such as Granules in Fluidized Bed agglomerate, bubble, growth and rupture process and the reaction mechanism mechanism of reaction can be obtained.These dynamic visual images are of great significance gas-solid fluidized bed " transport " tool of research.Therefore, the visual of fluidization process is amplified becoming gas-solid reaction and fluidized-bed reactor and even technological means very important in industrial scale experimental study.
But the operating temperature under hot pattern, considerably beyond the tolerable temperature of organic glass, needs by means of stainless steel reactor or quartz tube reactor and supporting heating arrangement.The resistance furnace that it is heater element that its heating arrangement is generally with the heating element such as resistance wire or Elema.Since the 19th-century nickel-chrome twenties (as Cr20Ni80) invention, resistance furnace is in laboratory study and be industrially widely used.And the electric furnace of existing scientific research is made up of heating element, burner hearth, metal shell, insulation filler, control system etc. usually.The burner hearth material adopted is aluminium oxide ceramics, insulation material is alumina silicate or heat-preservation cotton, stainless steel or iron sheet outer casing, cannot observe directly the grain fluidized of inside reactor and reactiveness.
Massachusetts Institute Technology patent US3626154 discloses a kind of transparent electric furnace, mainly comprises gold-plated vitreosil pipe, high temperature resistant resistance silk, quartz ampoule burner hearth and cooling jacket.The infrared radiation heat that one deck gold coating of outer quartz ampoule inwall can make resistance wire send reflexes to burner hearth center, serves insulation effect.When guaranteeing heating-up temperature more than 700 DEG C, the variable condition of burner hearth materials inside clearly can be seen.
Patent CN 202281506U discloses a kind of visual high temperature process furnances, body of heater is sealed by inside and outside layer quartz ampoule and forms vacuum double quartz ampoule, and gold film is coated with on outer quartz ampoule inwall, the inwall of the layered quartz tube around quartz ampoule burner hearth is provided with heater element.
Patent CN 102829631A discloses a kind of visual tubular furnace, and this tubular furnace device is made up of frame, gold-plated quartz tube furnace and coaxial crystal reaction tube, left and right water cooled seal assembly, vacuum measurement and acquisition system, air inlet system and exhaust system and power-supply system.Its principle utilizes when the heating-up temperature of object is greater than more than 500 DEG C, and the mode of the heat trnasfer in relative confined space mainly relies on infrared radiation, utilizes gold-plated film to realize heating to the reflex of infrared radiation.But its resistance wire used comparatively thick (5-8mm), the resistance value of its resistance per unit length silk is very low, obtain high heating power, certainly will will increase the wound convolution number density of resistance wire, and this will reduce the area of watch window.And from instructions and accompanying drawing, except the two ends that quartz ampoule support is used for fixed resistance silk, instructions does not illustrate how center section resistance wire is fixed.If unfixed words, reaction tube is easy to cause resistance wire short circuit accident at moving process, causes complete problem.
Patent CN 103285786A discloses a kind of visual high temperature fluidized bed, and fluidized bed body is offered the anti-infrared radiation shield of high quartz glass window and outside.Fluidized bed body adopts high temperature resistant quartz glass, and periphery is bed body electric heater, heat-preservation cotton and bed body case.But from accompanying drawing, its quartz ampoule fluidized bed and heating arrangement are integrated, and result in quartz ampoule fluidized bed cannot disassembly, cleaning, and due to quartz ampoule belong to frangible, delicate materials, in this patent, quartzy fluidized bed damages and whole device will be caused to use, and maintenance cost is high.
CN 101210916A discloses a kind of analyser that can be used for measuring gas-solid reaction kinetic parameter, disclose one and can add trace solid particle instantaneously online, solid is made to reach setting temperature of reaction instantaneously, miniature fluidized bed is utilized to realize the function of differential reaction, and by measuring crucial gaseous product relation over time, determine rate constant and reaction activity.But the technological deficiency that this analyser exists is fine grained to overflow reactor with gas, likely causes pipeline and detecting device blocking, the normal running of impact analysis instrument; And miniature fluidized bed used is difficult to the normal fluidisation realizing ultra-fine grain (<30um) or nano particle (<100nm), causes gas short circuit and wild effect.
CN 103364521A discloses a kind of isothermal micronized response analysis instrument, and described analyser comprises miniature fluidized bed, temperature and control pressurer system, gas purification and detection system and data collection and transmission; Described gas-solid reaction analyser also comprises transient pulse sampling system; Described transient pulse sampling system, comprising: gas-solid sample sample feeding pipe, impulse electromagnetic valve and gas bomb; Sample introduction gas in gas bomb controls transient pulse by impulse electromagnetic valve and injects solid sample sample feeding pipe, realizes transient pulse sample introduction.Although overcome fine grain effusion reaction flat-temperature zone by two sections of beds, but still be difficult to the normal fluidisation realizing ultra-fine grain (<30um) or nano particle (<100nm), cause gas short circuit and wild effect.
In addition, fluidized-bed reactor disclosed in CN 101210916A and CN 103364521A is miniature quartz or metal flow fluidized bed reactor, electrothermal furnace is reactor heat supply, electrothermal furnace is not described in detail, but be seen as laboratory conventional resistive stove from accompanying drawing, cannot granule-morphology, flowing situation and Air Bubble Size under observing response state.
The visual heating furnace that above patent proposes all have employed gold-plated quartz ampoule, and gold-plated quartz ampoule has insulation effect, simultaneously visible light-transmissive.Its disadvantage is to only have when operating temperature is greater than 700 DEG C, and the material of electric furnace inside could be high-visible.Thus, it cannot meet the demand of less than 700 DEG C visualized experiments.And run off in order to avoid the high temperature of gold coating, need to arrange cooling jacket, structure relative complex.
Patent CN 103673607A and CN 103675013A discloses a kind of visual heating furnace device and visual micro fluidized-bed reaction analyser, by being provided with heat insulation coating at middle pipe outer wall, longitudinal center section of heat insulation coating leaves watch window, observe the Gas-particle Flows state in reactor under can be implemented in arbitrary temp, widen the application of transparent electric furnace.But the body of heater of this patent by interior, in, outer three quartz ampoules and bell and furnace bottom form, complex structure.On the one hand, furnace diameter is large, and inner and outer tubes distance, is unfavorable for closely visual observation.On the other hand, furnace bottom is connected as a whole with bell by support bar, and its outer tube cannot rotate, and is unfavorable for the angle adjusting watch window, affects the practicality of product.And thermopair, heating furnace silk and power cord connector are located at bell inside, cause the easily-consumed products such as thermopair, heating furnace silk and intraware to change, thus affect the serviceable life of visual heating furnace.In addition, when supporting the use with field coil, because the diameter of outer tube is large, in order to ensure the normal use of field coil, requires the field coil of more large diameter, causing the weight and volume of field coil suddenly to increase, cost improves.The feature of its miniature fluidized-bed reaction analyser is the analysis of reactive kinetics parameters, cannot be applied to the grain fluidized behavior of research major diameter fluidized-bed reactor and the impact of gas-solid reactiveness and fluidized-bed reactor enlarge-effect.The present invention on this basis, proposes the visual fluidized bed reaction system that a kind of structure is simple, practicality is stronger, not only can be used for research reactive kinetics parameters and measures, and can also pass through to change intraware, for scaling-up effect study.
Summary of the invention
The object of the invention is to propose a kind of visual fluidized-bed reaction analytic system that can be used for realizing the multi-functionals such as visual, Kinetic analysis and scaling-up law study.The present invention not only can be used for measuring gas-solid reaction kinetic parameter, also can be observed the Gas-particle Flows mode in reactor, for the simulation of Gas-particle Flows under the condition of high temperature and reaction provides online observation evidence.Watch window adjustable angle, is conducive to studying the impact on gas-solid fluidized state and reaction of fluidized-bed reactor size.Meanwhile, the intraware of heating furnace is easy to install and change, and improves the practicality of heating furnace, extends the serviceable life of heating furnace.
For reaching this object, the present invention by the following technical solutions:
A kind of visual fluidized-bed reaction analytic system, described system comprises visual heating furnace and is placed in the fluidized-bed reactor of visual heating furnace; The air intake opening of described fluidized-bed reactor connects gas meter, and gas outlet connects online gas analyzing apparatus;
Described visual heating furnace comprises body of heater, and described body of heater is provided with inner and outer tubes from inside to outside successively; Described outer wall of inner tube is equipped with heating element; Described outer tube outer wall is provided with heat insulation coating, and longitudinal center section of heat insulation coating leaves watch window;
Described inner and outer tubes are fixed respectively by the outer annular recess on bell and furnace bottom and inner annular recess; Described outer tube can rotate along inner annular recess.
In the present invention, unstripped gas is entered by the air intake opening of fluidized-bed reactor, and reacted tail gas is discharged from fluidized-bed reactor gas outlet; The tail gas of discharging passes into on-line gas analysis device after dehydration, purification, carries out the quantitative and qualitative analysis such as gas chromatography, mass spectrum and measures, to obtain the composition of tail gas.
Longitudinal center section of described heat insulation coating maintains an equal level mutually with the soaking zone of inside heating furnace, is convenient to observe.
Watch window of the present invention be on outer tube outer wall without heat insulation coating region.The remainder of outer tube outer wall is evenly coated with heat insulation coating.
When heating-up temperature rises to more than 700 DEG C, heating element can send ruddiness, can observe the endocorpuscular flowing of reactor and fluidized state through heat insulation coating; When lower than 700 DEG C, the endocorpuscular flowing of reactor and fluidized state can be observed by watch window.
Heat insulation coating of the present invention is used for infrared reflecting, prevents thermal loss.Because the heat transfer type of (more than 500 DEG C) under the condition of high temperature is based on infrared radiation, the heat insulation coating of outer pipe surface effectively can reflex to reaction tube center the infrared radiation from heating element, realizes the object of insulation.
Described outer tube can rotate along inner annular recess, is conducive to adjusting viewing angle.
Described bell has thermocouple jack, makes thermopair insert the inner side of described interior pipe with measuring tempeature, in order to control the heating-up temperature of heating furnace.
Described bell and furnace bottom side are provided with screw recess, are fixed on stainless steel stent by supporting screw.
Watch window of the present invention vertically or radial distribution.
The length of described watch window is 20 ~ 1000mm, and width is 5 ~ 100mm.Its length optional selects 20.01 ~ 998mm, 23 ~ 985mm, 40 ~ 946mm, 116 ~ 820mm, 80 ~ 804mm, 204 ~ 700mm, 337 ~ 586mm, 460 ~ 472mm etc.; Its selectable width selects 5.03 ~ 99.6mm, 7 ~ 92mm, 12 ~ 84mm, 20 ~ 76mm, 34 ~ 64mm, 43 ~ 55mm, 52mm etc.Preferably, the length of described watch window is 100 ~ 500mm, and width is 10 ~ 30mm.
Described inner and outer tubes are quartz ampoule.The present invention selects resistant to elevated temperatures quartz ampoule as tubing, can tolerate the heating-up temperature in stove to a great extent.
Described furnace bottom and bell are refractory ceramics, high purity aluminium oxide, high-purity magnesium oxide, the one of metallic aluminium or potpourri.Furnace bottom and bell smooth surface.
Described analytic system also comprises high speed video system, and its height maintains an equal level mutually with the watch window of visual heating furnace.
Described visual heating furnace outside is provided with field coil, thus can form the visual fluidized-bed reaction analytic system of magnetic field environment.On the one hand, magnetic field environment can strengthen the fluidizing performance of magnetic-particle, makes the flowing of gas close to laminar flow, is conducive to the function realizing differential reaction; On the other hand its magnetic field environment is that the fluidisation of strengthening ultra-fine grain provides a kind of effective means, makes analytic system of the present invention become possibility for the flowing situation of Studies of The Superfine or nano particle and reactivity worth.
The magnetic field intensity scope of described field coil is 20 Gausses (Gs) ~ 1 tesla (T), and its magnitude of field intensity is relevant with the diameter of copper wire with the number of turn of field coil.Described field coil is made up of 2 ~ 20 coils, is connected between coil by copper wire; The two ends of field coil are connected with magnetic field control unit.
The outside of described visual heating furnace is also provided with jacking gear, for regulating the relative axial position of visual heating furnace and field coil.The elevation rate of described jacking gear is 0 ~ 100mm/min.Described jacking gear load capacity is not less than 50kg.
The heating element that outer wall of inner tube of the present invention is provided with has two kinds of fixed forms:
Described outer wall of inner tube is provided with helical groove, for supporting heating element; Or described outer wall of inner tube arranges bracing frame, and bracing frame is provided with draw-in groove, for supporting heating element.
The two ends of described heating element are drawn from furnace bottom, connection control power supply.
The diameter of described interior pipe is 30 ~ 180mm, such as, can select 30.02 ~ 178mm, 58 ~ 150mm, 70 ~ 132mm, 81 ~ 110mm, 100mm etc., preferred 80mm.
The diameter of described outer tube is 50 ~ 200mm, such as, can select 50.2 ~ 198.6mm, 68 ~ 142mm, 83 ~ 120mm, 90 ~ 108mm, 100mm etc., preferred 110mm.
The height of described inner and outer tubes is 100 ~ 1000mm, such as, can select 100.3 ~ 995mm, 190 ~ 880mm, 260 ~ 765mm, 328 ~ 660mm, 364 ~ 604mm, 390 ~ 570mm, 420 ~ 527mm, 456 ~ 500mm etc., preferably 300 ~ 400mm.
Described heating element is nickel-chrome resistance wire, Elema or Si-Mo rod.The diameter of nickel-chrome resistance wire is 0.5 ~ 5mm, such as, can select 0.51 ~ 4.96mm, 0.6 ~ 3.8mm, 0.72 ~ 2.64mm, 0.9 ~ 1.4mm, 1.5mm etc., preferred 1-3mm.
The diameter of described Elema or Si-Mo rod is 3-8mm, is preferably 5mm.
Described heat insulation coating is the alloy coat of a kind of in silver, tin, titanium, gold, copper, magnesium, manganese, molybdenum, tungsten or zirconium or at least two kinds.Typical but non-limiting example comprises: silver, gold, copper, tungsten, magnesium, the combination of tin and titanium, the combination of titanium and molybdenum, the combination of gold and zirconium, the combination of tin and manganese, the combination of gold, copper and tungsten, the combination of tin, titanium and manganese, the combination of silver, tungsten, manganese and molybdenum, the combination etc. of tungsten, zirconium, titanium and gold, all can be used for implementing the present invention.
Or described heat insulation coating is the mixture coating of a kind of in the oxide of titanium, zirconium, manganese, magnesium, copper, nickel or iron or at least two kinds.Typical but non-limiting example comprises: titanium dioxide, cupric oxide, iron oxide, zirconia and magnesian combination, the combination of titanium dioxide and nickel oxide, the combination of zirconia, magnesium oxide and manganese oxide, the combination of titanium dioxide, manganese oxide and iron oxide, the combination etc. of zirconia, magnesium oxide, nickel oxide and titanium dioxide, all can be used for implementing the present invention.
The thickness of described heat insulation coating is 5 ~ 500nm, such as, can select 5.02 ~ 496nm, 8 ~ 460nm, 15 ~ 421nm, 40 ~ 400nm, 53 ~ 375nm, 80 ~ 340nm, 120 ~ 318nm, 148 ~ 300nm, 180 ~ 264nm, 234nm etc., more preferably 20 ~ 100nm.
The heating power of described visual heating furnace is 500 ~ 5000W, and heating temperature range is 100 ~ 1100 DEG C, and heating rate is 5 ~ 50 DEG C/min.Described maximum heating temperature and heating rate and diameter of inner pipe and highly relevant, simultaneously also relevant with length with the diameter of heating element.
Described fluidized-bed reactor comprises pipe and fluidized bed outer tube in fluidized bed, is sealed in described fluidized bed between pipe and fluidized bed outer tube by ground; Described fluidized bed outer tube top is provided with gas access; In described fluidized bed, the bottom of pipe is gas distributor, and its top is gas vent.
Described gas distributor is sintered plate distributor or perforated-plate distributor.
In described fluidized bed, pipe and fluidized bed outer tube are quartz ampoule.In described fluidized bed, pipe is divided into the fluidisation section of bottom and the expanding reach on top.In described fluidized bed, pipe is preheating zone with the middle part annular space of fluidized bed outer tube.
Unstripped gas is entered by fluidized bed outer tube upper gas entrance, successively through reactor outer shroud preheating zone, gas distributor, fully contacts with the particle in pipe in fluidized bed, and makes it be in fluidized state; Reacted tail gas is discharged from the gas vent at pipe top in fluidized bed.
Fluidized-bed reactor structure simple and flexible of the present invention, can put into rapidly the heating furnace of high temperature, also can take out from the heating furnace of high temperature rapidly; The unstripped gas passed into contacts with solid material and reacts after preheating.
Compared with prior art scheme, the present invention has following beneficial effect:
Visual fluidized-bed reaction analytic system structure of the present invention is simple, volume is little, is easy to change the key component such as fluidized-bed reactor and visual heating furnace, can be applicable to the nearly Kinetic parameter measuring multi-phase complex system; Directly can observe flowing and the flowing situation of the Multi-scale model such as multi-phase complex course of reaction particle, bubble under heated condition simultaneously.Magnetic field environment not only can strengthen the fluidizing performance of magnetic-particle, makes the flowing of gas close to laminar flow, is conducive to the function realizing differential reaction; Can also be used for studying magnetic field environment or without the flowing of the Multi-scale models such as heterogeneous reaction process particle, bubble under magnetic field condition and flowing situation, changes in crystal structure etc.And, the more important thing is, this analytic system is easy to change visual heating furnace and fluidized-bed reactor, in order to study the impact of fluidized-bed reactor size on gas-solid fluidized behavior and reaction, and studies gas-solid reaction and fluidized bed state etc. in extensive fluidized-bed reactor.Especially, the outer tube with watch window can rotate along inner annular recess, the angle of adjustment watch window, is conducive to flowing and the fluidized state of the particle studying diverse location in fluidized bed.
Accompanying drawing explanation
Fig. 1 is the structural representation of visual fluidized-bed reaction analytic system of the present invention;
Fig. 2 is the structural representation of fluidized-bed reactor of the present invention;
Fig. 3 is the structural representation of visual heating furnace of the present invention;
Fig. 4 is the fluidized state of methanation catalyst in embodiment 2; Wherein, (a) is under not adding magnetic field condition; B () is under adding magnetic field condition;
Fig. 5 is that in embodiment 3, nano oxidized Fe3+ reduction prepares fluidisation photo in nanometer iron powder process
In figure: 1-1: visual heating furnace; 1-2: fluidized-bed reactor; 1-3: field coil; 1-4: jacking gear; 1-5: temperature control system; 1-6: magnetic field control system; 1-7: gas meter; 1-8: gas on-line analysis device; 1-9: high speed video system;
2-1: pipe in fluidized bed; 2-2: fluidized bed outer tube; 2-3: gas distributor; 2-4: fluidisation section; 2-5: expanding reach; 2-6: gas access; 2-7: gas vent; 2-8: preheating zone;
Pipe in 1-; 2-outer tube; 3-bell; 4-furnace bottom; 5-heating element; 6-heat insulation coating; 7-thermocouple jack; 8-thermopair; 9-protective casing; 10-control device.
The present invention is described in more detail below.But following example is only simple and easy example of the present invention, and do not represent or limit the scope of the present invention, protection scope of the present invention is as the criterion with claims.
Embodiment
Technical scheme of the present invention is further illustrated by embodiment below in conjunction with accompanying drawing.
For better the present invention being described, be convenient to understand technical scheme of the present invention, typical but non-limiting embodiment of the present invention is as follows:
Figure 1 show the structural representation of visual fluidized-bed reaction analytic system of the present invention, comprise visual heating furnace 1-1 and be placed in the fluidized-bed reactor 1-2 of visual heating furnace 1-1; The air intake opening of described fluidized-bed reactor 1-2 connects gas meter 1-7, and gas outlet connects gas on-line analysis device 1-8; Also comprise high speed video system 1-9, its height maintains an equal level mutually with the watch window of visual heating furnace 1-1.Described visual heating furnace 1-1 outside is provided with field coil 1-3 and jacking gear 1-4, and jacking gear 1-4 can be used for the relative axial position regulating visual heating furnace 1-1 and field coil 1-3.The two ends of field coil 1-3 are connected with magnetic field control unit 1-6.Heating element 5 in visual heating furnace 1-1 is connected with attemperating unit 1-5.
Attemperating unit 1-5, the jacking gear 1-4 of visual heating furnace 1-1, magnetic field control device 1-6, the gas meter 1-7 of field coil 1-3, gas on-line analysis device 1-8 are connected with computing machine by signal wire with high speed video system 1-9, unified by computing machine PLC software control and output.
Figure 2 illustrate a kind of fluidized-bed reactor structural representation of the present invention, comprise pipe 2-1 and fluidized bed outer tube 2-2 in fluidized bed, sealed by ground between pipe 2-1 and fluidized bed outer tube 2-2 in described fluidized bed; Described fluidized bed outer tube 2-2 top is provided with gas access 2-6; In described fluidized bed, the bottom of pipe 2-1 is gas distributor 2-3, and its top is gas vent 2-7.In described fluidized bed, pipe 2-1 and fluidized bed outer tube 2-2 is quartz ampoule; In described fluidized bed, pipe 2-1 is divided into the fluidisation section 2-4 of bottom and the expanding reach 2-5 on top; In described fluidized bed, the middle part annular space of pipe 2-1 and fluidized bed outer tube 2-2 is preheating zone 2-8.Unstripped gas is entered by fluidized bed outer tube 2-2 upper gas entrance 2-6, successively through preheating zone 2-8, the gas distributor 2-3 of reactor outer shroud, fully contacts, and make it be in fluidized state with the particle in pipe 2-1 in fluidized bed; Reacted tail gas is discharged from the gas vent 2-7 at pipe 2-1 top in fluidized bed.
With reference to accompanying drawing 3, the visual heating furnace of one of the present invention is made up of interior pipe 1, outer tube 2, bell 3 and furnace bottom 4 four part.Interior pipe 1 of the present invention, outer tube 2, bell 3 and furnace bottom 4 be fixedly be fixed on supporting stainless steel stent by bell 3 and furnace bottom 4 side screw recess and screw.Interior pipe 1, outer tube 2 are fixed by the circular groove of bell 3 and furnace bottom 4, by regulating the distance between bell 3 and furnace bottom 4, outer tube 2 can be made to rotate along circular groove, being conducive to the angle regulating watch window.
Interior pipe 1 outer wall is equipped with heating element 5, and outer tube 2 outer wall is provided with heat insulation coating 6.On bell 3, have thermocouple jack 7, make thermopair 8 insert the inner side of interior pipe 1 with measuring tempeature, the outside of thermopair 8 is wrapped up by protective casing 9, and its output terminal is connected with control device 10, and object is the heating-up temperature controlling heating furnace.
The basic operation process of visual fluidized-bed reaction analytic system of the present invention is:
Appropriate solid particle is loaded in pipe 2-1 in the fluidized bed of fluidized-bed reactor 1-2; Unstripped gas enters fluidized-bed reactor 1-2 by gas meter 1-7 from the upper gas entrance 2-6 of fluidized-bed reactor 1-2, particle contacts above preheating zone 2-8, the gas distributor 2-3 and gas distributor 2-3 of reactor outer shroud reacts, and makes an endoparticle be in fluidized state.Reacted tail gas is discharged from the top gas outlet 2-7 of pipe 2-1 in fluidized bed; The tail gas of discharging passes into gas on-line analysis device 1-8 after dehydration, purification, primarily of gas chromatography, mass spectrometry system, can on-line measurement reacting gas production concentration, form variation relation with temperature or time.Like this, according to the concentration change of gaseous product, the reaction rate under this reaction conditions can be determined, and go out the reactive kinetics parameters such as reaction activity according to Arrhenus formulae discovery further.
By the position regulating the lifting distance of jacking gear 1-4 to regulate visual heating furnace 1-1 and field coil 1-3; The size of magnetic field intensity regulates the size of current of field coil 1-3 to realize by magnetic field control system 1-6; Meanwhile, open high speed video system 1-9, regulate the position that the relative axial position of high speed video system 1-9 and visual heating furnace 1-1 is extremely suitable, make high speed video system 1-9 clearly can observe material in fluidized-bed reactor 1-2; The gas flow of adjusting gas flow meter 1-7, makes the material in bed be in fluidized state, utilizes high speed video system 1-9 to observe the particle agglomeration of material and size, the fluidized state of bubble in bed.By software process, the significant data such as the ascending velocity of bubble, particle moving speed can be obtained.
Analytic system structure of the present invention is simple, volume is little; The grain fluidized quality of magnetic field-intensification is good, makes measured reactive kinetics parameters close to intrinsic kinetics; Directly can observe flowing and the flowing situation of the Multi-scale model such as particle, bubble within the scope of room temperature ~ 1000 DEG C under arbitrary temp simultaneously.
Embodiment 1
For CH4 production process, set forth the embodiment of visual fluidized-bed reaction analytic system of the present invention further.
The present embodiment is using the visual heating furnace of the plated film with watch window as the heating arrangement of CH4 production.The outer wall of inner tube of visual heating furnace is provided with helical groove, and heating element adopts Cr20Ni80 high temperature resistant resistance silk, and its diameter is 1.0mm, and the heat insulation coating of outer tube outer wall is gold coatings, coating thickness 50nm; The watch window without the coat of metal is radially provided with at heating furnace core.The heating power of heating furnace is 2000W, maximum heating temperature 950 DEG C.
Methane reforming catalyst used is Ni-Co-Al
2o
3bimetallic catalyst (Ni and Co massfraction is 20wt%), particle diameter is 10 ~ 50 μm; Fluidized-bed reactor internal diameter used is 30mm; The fluidizing gas velocity of fluidizing gas used is 0.05m/s, and fluidizing gas consists of methane: the mol ratio of carbon dioxide is 1:1; Before reaction, in advance from room temperature temperature programme to 800 DEG C, used time 20min, at 800 DEG C of constant temperature reduction activation 4h, being then warming up to temperature of reaction is 900 DEG C; Be can be observed the fluidized state of reforming catalyst by watch window in course of reaction.
Reacted gas is by Inficon portable gas chromatograph analytical gas product composition, and calculating titanium dioxide charcoal percent conversion is 96%, and the conversion ratio of methane is 93%, hydrogen selective 92%, CO selectivity 99%.
Embodiment 2
For the methanation of carbon monoxide reaction, set forth the embodiment of visual fluidized-bed reaction analytic system of the present invention further.
The heating arrangement that the present embodiment reacts using the visual heating furnace of the plated film with watch window as the methanation of carbon monoxide.The outer wall of inner tube of visual heating furnace is provided with helical groove, and heating element is Cr20Ni80 high temperature resistant resistance silk, and its diameter is 1.0mm, and the heat insulation coating of outer tube outer wall is silver-plated coating, coating thickness 100nm.The watch window without the coat of metal is provided with vertically at heating furnace core.The heating power of heating furnace is 500W, maximum heating temperature 600 DEG C.
Methanation catalyst used is Ni-Al
2o
3catalyzer (the massfraction 20wt% of Ni), particle diameter is 30 ~ 70 μm; Fluidized-bed reactor internal diameter used is 20mm; The fluidizing gas velocity of fluidizing gas used is 0.01m/s, and fluidizing gas consists of nitrogen: hydrogen: carbon monoxide=1:3:1; Before reaction, in advance from room temperature temperature programme to 800 DEG C, used time 40min, at 800 DEG C of constant temperature reduction activation 2h, being then cooled to temperature of reaction is 350 DEG C; Reacted gas is by Inficon portable gas chromatograph analytical gas product composition, and the conversion ratio calculating carbon monoxide is 96%, and the selectivity of methane is 83%, methane yield 80%.As shown in Figure 4.Can obviously find out, poor in the fluidized state not adding methanation catalyst under magnetic field condition, bubble is comparatively large, there is Biased flow phenomenon; And under adding magnetic field condition (300Gs), the fluidized state of methanation catalyst presents the steady bed state of magnetic, catalyst granules is that needle-like is dispersed in bed.
Embodiment 3
For hydrogen reducing nano-sized iron oxide, set forth the embodiment of visual fluidized-bed reaction analytic system of the present invention further.
The heating arrangement that the present embodiment reacts using the visual heating furnace of the plated film with watch window as hydrogen reducing nano-sized iron oxide.Outer wall of inner tube arranges bracing frame, and support frame as described above has draw-in groove, and heating element is Si-Mo rod, and its diameter is 5.0mm, and the heat insulation coating of outer tube outer wall is nickel-tungsten coating, coating thickness 20nm.The watch window without the coat of metal is radially provided with at heating furnace core.The heating power of heating furnace is 4000W, maximum heating temperature 1050 DEG C.
Nano-sized iron oxide used is the brown iron oxide (iron oxide purity 99%, particle diameter is 240nm) that traditional Chinese medicines group company produces; Fluidized-bed reactor internal diameter used is 30mm; The fluidizing gas velocity 0.05m/s of fluidizing gas used, fluidizing gas consists of nitrogen: hydrogen=1:1; Reduction reaction temperature is 600 DEG C; Even fluidizing by watch window observable nanometer iron powder in course of reaction, see Fig. 5, after 600 DEG C of reduction reaction 15min, observe defluidization, the average particulate diameter of nanometer iron powder agglomerate during defluidization is 10 μm, and the massfraction of product iron is 95.5wt%.
Embodiment 4
The heating arrangement of the present embodiment using the visual heating furnace of the plated film with watch window as preparation carbon nano-tube.Outer wall of inner tube arranges bracing frame, and support frame as described above has draw-in groove, and heating element is Cr20Ni80 high temperature resistant resistance silk, and its diameter is 2.0mm, and the heat insulation coating of outer tube outer wall is magnesium oxide coating, coating thickness 100nm.The watch window without the coat of metal is radially provided with at heating furnace core.The heating power of heating furnace is 2000W, maximum heating temperature 1000 DEG C.
Used catalyst is FeMo catalyzer; Fluidized-bed reactor internal diameter used is 20mm; Carbon source used be 5% methane Balance Air be helium; Temperature of reaction is 900 DEG C; Magnetic field intensity 0.2T, can be observed the growth course of carbon pipe by watch window in course of reaction.Uniform length, loose array carbon nano tube can be obtained after reaction 3h.
Embodiment 5
To remove NO in catalytic cracking (FCC) regenerator flue gas
xfor example, set forth the embodiment of visual fluidized-bed reaction analytic system of the present invention further.
The present embodiment is using the visual heating furnace of the plated film with watch window as removing NO in catalytic cracking (FCC) regenerator flue gas
xthe heating arrangement of reaction.The outer wall of inner tube of visual heating furnace is provided with draw-in groove, and heating element is Elema, and its diameter is 8mm, and the heat insulation coating of middle pipe outer wall is gold coatings, coating thickness 50nm.The watch window without the coat of metal is provided with vertically at heating furnace core.The heating power of heating furnace is 5000W, maximum heating temperature 1100 DEG C.
Denitrating catalyst used is the FCC Cracking catalyst of carbon distribution, and fluidized-bed reactor internal diameter used is 20mm; The fluidizing gas velocity 0.01m/s of fluidizing gas used, fluidizing gas is the combination gas (volume fraction of CO is 4%) of CO and argon gas; Because FCC catalyst fluidization quality is good, without the need to magnetic field-intensification.Regulate jacking gear during experiment, make heating furnace raise 300mm, rate travel 100mm/min.Denitration reaction temperature is 700 DEG C; Gaseous product passes into NO/NO after processed
2/ NO
xon-line checkingi NO, NO
2effusion behavior.
Applicant states, the present invention illustrates detailed construction feature of the present invention by above-described embodiment, but the present invention is not limited to above-mentioned detailed construction feature, does not namely mean that the present invention must rely on above-mentioned detailed construction feature and could implement.Person of ordinary skill in the field should understand, any improvement in the present invention, to equivalence replacement and the increase of accessory, the concrete way choice etc. of parts selected by the present invention, all drops within protection scope of the present invention and open scope.
More than describe the preferred embodiment of the present invention in detail; but the present invention is not limited to the detail in above-mentioned embodiment, within the scope of technical conceive of the present invention; can carry out multiple simple variant to technical scheme of the present invention, these simple variant all belong to protection scope of the present invention.
It should be noted that in addition, each concrete technical characteristic described in above-mentioned embodiment, in reconcilable situation, can be combined by any suitable mode, in order to avoid unnecessary repetition, the present invention illustrates no longer separately to various possible array mode.
In addition, also can carry out combination in any between various different embodiment of the present invention, as long as it is without prejudice to thought of the present invention, it should be considered as content disclosed in this invention equally.
Claims (10)
1. a visual fluidized-bed reaction analytic system, is characterized in that, described analytic system comprises visual heating furnace (1-1) and is placed in the fluidized-bed reactor (1-2) of visual heating furnace (1-1); The air intake opening of described fluidized-bed reactor (1-2) connects gas meter (1-7), and gas outlet connects gas on-line analysis device (1-8);
Described visual heating furnace (1-1) comprises body of heater, and described body of heater is provided with interior pipe (1) and outer tube (2) from inside to outside successively; Described interior pipe (1) outer wall is equipped with heating element (5); Described outer tube (2) outer wall is provided with heat insulation coating (6), and longitudinal center section of heat insulation coating (6) leaves watch window (22);
Described interior pipe (1) and outer tube (2) are fixed respectively by the outer annular recess on bell (3) and furnace bottom (4) and inner annular recess; Described outer tube (2) can rotate along inner annular recess.
2. analytic system as claimed in claim 1, is characterized in that, described bell (3) has thermocouple jack (7), make thermopair (8) insert the inner side of described interior pipe (1) with measuring tempeature;
Preferably, described bell (3) and furnace bottom (4) side are provided with screw recess, are fixed on stainless steel stent by supporting screw;
Preferably, described interior pipe (1) and outer tube (2) are quartz ampoule.
3. analytic system as claimed in claim 1 or 2, it is characterized in that, described analytic system also comprises high speed video system (1-9), and its height maintains an equal level mutually with the watch window (22) of visual heating furnace (1-1).
4. the analytic system as described in one of claim 1-3, is characterized in that, described visual heating furnace (1-1) outside is provided with field coil (1-3);
Preferably, described field coil (1-3) is made up of 2-20 coil, is connected between coil by copper wire, and magnetic field intensity scope is 20Gs ~ 1T;
Preferably, the outside of described visual heating furnace (1-1) is also provided with jacking gear (1-4), for regulating the relative axial position of visual heating furnace (1-1) and field coil (1-3);
Preferably, the elevation rate of described jacking gear (1-4) is 0 ~ 100mm/min;
Preferably, described jacking gear (1-4) load capacity is not less than 50kg.
5. the analytic system as described in one of claim 1-4, is characterized in that, described interior pipe (1) outer wall is provided with helical groove, for supporting heating element (5); Or described interior pipe (1) outer wall arranges bracing frame, and bracing frame is provided with draw-in groove, for supporting heating element (5);
Preferably, the two ends of described heating element (5) are drawn from bell (3) and furnace bottom (4), connection control power supply.
6. the analytic system as described in one of claim 1-5, is characterized in that, described heating element (5) is nickel-chrome resistance wire, Elema or Si-Mo rod; Preferably, the diameter of nickel-chrome resistance wire is 0.5 ~ 5mm, further preferred 1-3mm.
7. the analytic system as described in one of claim 1-6, is characterized in that, described heat insulation coating (6) is the alloy coat of a kind of in silver, tin, titanium, gold, copper, magnesium, manganese, molybdenum, tungsten or zirconium or at least two kinds; Or described heat insulation coating (6) is titanium, the mixture coating of a kind of in the oxide of zirconium, manganese, magnesium, copper, nickel or iron or at least two kinds;
Preferably, the thickness of described heat insulation coating (6) is 5 ~ 500nm, more preferably 20 ~ 100nm.
8. the analytic system as described in one of claim 1-7, is characterized in that, the heating power of described visual heating furnace (1-1) is 500 ~ 5000W, and heating temperature range is 100 ~ 1100 DEG C, and heating rate is 5 ~ 50 DEG C/min.
9. the analytic system as described in one of claim 1-8, it is characterized in that, described fluidized-bed reactor (1-2) comprises pipe (2-1) and fluidized bed outer tube (2-2) in fluidized bed, is sealed in described fluidized bed between pipe (2-1) and fluidized bed outer tube (2-2) by ground; Described fluidized bed outer tube (2-2) top is provided with gas access (2-6); In described fluidized bed, the bottom of pipe (2-1) is gas distributor (2-3), and its top is gas vent (2-7).
10. analytic system as claimed in claim 9, is characterized in that, in described fluidized bed, pipe (2-1) and fluidized bed outer tube (2-2) are quartz ampoule;
Preferably, in described fluidized bed, pipe (2-1) is divided into the fluidisation section (2-4) of bottom and the expanding reach (2-5) on top;
Preferably, in described fluidized bed, pipe (2-1) is preheating zone (2-8) with the middle part annular space of fluidized bed outer tube (2-2).
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| CN111841453A (en) * | 2020-06-18 | 2020-10-30 | 西北大学 | Be applied to thermogravimetric analysis's miniature fluidized bed reaction unit |
| CN113509896A (en) * | 2021-07-26 | 2021-10-19 | 东南大学 | Online measurement device and method for gasification total flow field temperature of organic solid waste bubbling fluidized bed |
| CN115285976A (en) * | 2022-07-15 | 2022-11-04 | 深圳烯湾科技有限公司 | Carbon nano tube and carbon nano tube fluidized bed preparation process |
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