CN106732202A - A kind of single tube structure fixed bed reactors for teaching experiment - Google Patents

A kind of single tube structure fixed bed reactors for teaching experiment Download PDF

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Publication number
CN106732202A
CN106732202A CN201611210358.2A CN201611210358A CN106732202A CN 106732202 A CN106732202 A CN 106732202A CN 201611210358 A CN201611210358 A CN 201611210358A CN 106732202 A CN106732202 A CN 106732202A
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reaction tube
fixed bed
reaction
reactor
bed reactors
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CN201611210358.2A
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CN106732202B (en
Inventor
张天开
武爱莲
王琪
吕学枚
张永发
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Taiyuan University of Technology
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Taiyuan University of Technology
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J8/00Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
    • B01J8/02Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with stationary particles, e.g. in fixed beds
    • B01J8/06Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with stationary particles, e.g. in fixed beds in tube reactors; the solid particles being arranged in tubes
    • B01J8/067Heating or cooling the reactor
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10JPRODUCTION OF PRODUCER GAS, WATER-GAS, SYNTHESIS GAS FROM SOLID CARBONACEOUS MATERIAL, OR MIXTURES CONTAINING THESE GASES; CARBURETTING AIR OR OTHER GASES
    • C10J3/00Production of combustible gases containing carbon monoxide from solid carbonaceous fuels
    • C10J3/02Fixed-bed gasification of lump fuel
    • C10J3/20Apparatus; Plants
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2208/00Processes carried out in the presence of solid particles; Reactors therefor
    • B01J2208/06Details of tube reactors containing solid particles
    • B01J2208/065Heating or cooling the reactor
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10JPRODUCTION OF PRODUCER GAS, WATER-GAS, SYNTHESIS GAS FROM SOLID CARBONACEOUS MATERIAL, OR MIXTURES CONTAINING THESE GASES; CARBURETTING AIR OR OTHER GASES
    • C10J2300/00Details of gasification processes
    • C10J2300/09Details of the feed, e.g. feeding of spent catalyst, inert gas or halogens
    • C10J2300/0913Carbonaceous raw material
    • C10J2300/093Coal
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P20/00Technologies relating to chemical industry
    • Y02P20/50Improvements relating to the production of bulk chemicals
    • Y02P20/52Improvements relating to the production of bulk chemicals using catalysts, e.g. selective catalysts

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  • Chemical & Material Sciences (AREA)
  • Devices And Processes Conducted In The Presence Of Fluids And Solid Particles (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Combustion & Propulsion (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Chemical Kinetics & Catalysis (AREA)

Abstract

The invention discloses a kind of single tube structure fixed bed reactors for teaching experiment, the fixed bed reactors are that reaction tube described in is provided with cylinder, and it is provided with a stainless (steel) wire and described filler below reaction tube, and heater by cylinder both sides carries out heating response.This reactor is used for teaching experimental equipment, enormously simplify structure of reactor, easy assembling disassembling, reduce the cost of instructional response device experiment, and inside reactor cavity volume is small, the residence time of phase feed and product in reactor is reduced, while reducing side reaction and carry out, the conversion ratio of raw material is improve.

Description

A kind of single tube structure fixed bed reactors for teaching experiment
Technical field
It is especially a kind of to be used for methane-CO 2 reformation and coal/Jiao's gas the present invention relates to a kind of fixed bed reactors The teaching experiment fixed bed reactors of the high-temperature high-voltage reaction process of change.
Background technology
It is in the incubation of chemical undergraduate and postgraduate to be related to reactor and reaction unit, particularly fixed bed more Reactor.Fixed bed reactors Chemical Engineering Technology laboratory development, industrialization amplify and the industrialized production stage tool Play an important role.The fixed bed reactors of existing experiment, are outside pressure-bearing and the internal fabricated structure for holding heat, general volume mostly Huge, inside reactor complex structure, manufacture and maintenance cost are higher.Additionally, during reaction under high pressure, due in reactor Portion's pressure is higher, and the extended residence time of reaction raw materials and product in reactor is caused to a certain extent, and side reaction is tight Weight, reduces the conversion ratio of raw material, extends test period, increased experiment fees.Therefore, student in learning process often Fixed bed reactors can only be understood by way of picture or animation, operation on the spot is not realized substantially.
Existing document CN201558692U discloses " reactor that a kind of high temperature resistant, high pressure load and unload convenient catalyst ", should Reactor is main by portions such as cylinder, upper lower end cap, upper-lower compacting module, locking nut, catalyst bracket and aluminum radiating gaskets It is grouped into.Its structure is more complicated, and fin and material import and export are provided with reactor cylinder body portion, external for reactor Heating part Structural Design Requirement it is higher;Need to vibrate whole reactor during catalyst filling, it is impossible to ensure catalyst Filling is uniform, causes catalytic effect to be affected.In addition, the reactor maximum temperature be 450 DEG C, it is impossible to satisfaction require temperature compared with The course of reaction such as methane-CO 2 reformation high and coal/semicoke hydrogasification.For these reasons, one in teaching process As do not use the type reactor.
Existing document CN101537327A discloses " a kind of fixed bed reactors ", and the reactor mainly includes:Housing, guarantor The parts such as adiabator, crystal reaction tube.The reactor is a kind of high temperature resistant, high-pressure reactor, its structure and shell-and-tube reactor Similar, the reactor is mainly, the heat-resisting and pressure-bearing phase seperated reactor of shell pressure-bearing heat-resisting by inner quartz tube, causes Structure of reactor is complicated, manufacturing cost increases;Because the reactor heating part is located inside reactor, match somebody with somebody in dismounting and replacing Need to partially open reactor body during part, operation more inconvenience.It is general during teaching experiment to be fixed using this type Bed, but because the general volume of the reactor is larger, many people's cooperations are generally required during actually behaviour could complete operation, take When it is laborious.Because its manufacturing cost is higher, and internal cavities volume is larger, causes instruction cost to increase.
The content of the invention
It is an object of the invention to provide a kind of single tube structure fixed bed reactors for teaching experiment, it is used to solve at present In the incubation of chemical undergraduate and postgraduate, the HTHP fixed bed reactors complex structure of experiment, experiment Overlong time, experimental cost problem higher, especially in 900 DEG C of high temperature and the fixed bed reactors of 10MPa pressure.
The present invention solves the above problems to be realized by following scheme.
A kind of single tube structure fixed bed reactors for teaching experiment, including material inlet, upper flange, cylinder, reaction Pipe, filler, lower flange, material outlet, stainless (steel) wire and its heater;It is characterized in that:
Reaction tube described in one is provided with the cylinder, be provided with below the reaction tube stainless (steel) wire described in one and Described filler, and the heater by the cylinder both sides carries out heating response;
The reaction tube is monolithically fabricated in T-shape structure, and is 0.4 ~ 0.6: 1 and cylinder with the length ratio of the cylinder External diameter ratio is 1: 1.3 ~ 3;Reaction tube horizontal component is connected with vertical component by way of full weld;
The internal cavities of the reaction tube are in from bottom to top funnel-shaped structure, and the height of lower inwall accounts for the 5 ~ 50% of tube length of reaction tube; Upper inwall is 1 with the internal diameter ratio of lower inwall:1~10;Middle inwall and lower inwall(11)Angle be 100 ~ 180 °, it is convenient to have reacted Remaining solid raw material or catalyst are poured out after.
The reaction tube is inserted directly into the cylinder when built-in, and outside wall surface and the cylinder of reaction tube internal face Interval≤5mm, and by upper flange compress sealing fix.
In the above-mentioned technical solutions, the stainless (steel) wire is the stainless (steel) wire of 10 ~ 600 mesh;The single tube structure fixed bed The reaction temperature of reactor is 900 DEG C, and reaction pressure is 10MPa;The upper surface of described filler and the bottom face of reaction tube away from From being 2 ~ 5mm, to reduce inside reactor cavity volume, so as to reduce inside reactor gas raw material total amount and residence time.
A kind of single tube structure fixed bed reactors for teaching experiment, in experiment, by solid material or solid catalysis Agent is placed in reaction tube, and reaction tube is installed in reactor, is sealed by upper flange and fixed, then will through material inlet The nitrogen of 10MPa pressure or other inert gases input reaction tube, when unit temp rises to 900 DEG C, by nitrogen or other are lazy Property gas be changed to the gas raw material of 10MPa pressure, now, solid material or catalyst that gas raw material is inserted with reaction bottom of the tube Contact is reacted, and generation product gas flow through reactor lower part filler, are exported by reactor outlet, after the completion of reaction, from anti- Answer device top to take out reaction tube and pour out remaining solid sample or catalyst, tested again.
Above-mentioned the provided a kind of single tube structure fixed bed reactors for teaching experiment of the present invention, in current ground quadrangle In the case that teaching and scientific research funds in school are very nervous, for experimental teaching, simple structure easily fills readily removable, and floor space is small, experiment Low cost, experimental period is short, achieves preferable experiment effect, and easy to operate, meet Chemical Engineering Specialty undergraduate and Postgraduate's experimental teaching demand.
Brief description of the drawings
Fig. 1 is the experimental configuration schematic diagram of fixed bed reactors of the present invention.
Fig. 2 is the comparison diagram of present invention reaction tube bottom temp and reactor cylinder temperature in experiment.
In figure:1:Material inlet;2:Upper flange;3:Cylinder;4:Reaction tube;5:Filler;6:Lower flange;7:Material outlet; 8:Thermocouple;9:Upper inwall;10:Middle inwall;11:Lower inwall;12:Stainless (steel) wire;13:Heater.
Specific embodiment
Specific embodiment of the invention is further illustrated below.
Implement a kind of single tube structure fixed bed reactors for teaching experiment, the fixed bed reactors are by material inlet 1st, upper flange 2, cylinder 3, reaction tube 4, filler 5, lower flange 6, material outlet 7, thermocouple 8, upper inwall 9, middle inwall 10, it is lower in Wall 11, stainless (steel) wire 12 and its heater 13, carry out configuration assembling and constitute using prior art.
Specific embodiment is that a reaction tube 4 is set in cylinder 3, and one 10 ~ 600 mesh are set below reaction tube 4 Stainless (steel) wire 12 and insert filler 5, filler 5 can be the broken of broken ceramics, alumina balls, silicon oxide particle or metal material Any one of bits, bar or tubing;The upper surface of filler 5 is designed as 2 ~ 5mm with the distance of the bottom face of reaction tube 4;Anti- Answer the both sides of device cylinder 3 to set and heater 13 is installed, and thermocouple 8 is installed between cylinder 3 and heater 13, to solid Fixed bed reactor carries out heating response experiment.
Wherein, the material of reactor shell 3 is nickel-base alloy, and reaction tube 4 is metal material, the overall structure of reaction tube 4 T-shape structure, its horizontal component is connected with vertical component by way of full weld, and its horizontal component be located at upper flange 2 it Between, the bottom of reaction tube 4 is located at the centre of cylinder 3;Reaction tube 4 is designed as 0.4 ~ 0.6: 1 and cylinder 3 with the length ratio of cylinder External diameter ratio be designed as 1: 1.3 ~ 3;The inner chamber of reaction tube 4 is from bottom to top funnel-shaped structure, and the height of its lower inwall 11 is anti- Answer the 5 ~ 50% of length of tube;Upper inwall 9 is designed as 1 with the internal diameter ratio of lower inwall 11:1~10;The folder of middle inwall 10 and lower inwall 11 Angle is designed as 100 ~ 180 °;The lower end of reaction tube 4 of T-shape structure is inserted directly into reactor by reaction tube 4 in built-in installation Cylinder in, the spaced design of the outside wall surface of reaction tube 4 and the internal face of reactor shell 3 is≤5mm, and by upper flange 2 Sealing is compressed to fix.
The above-mentioned single tube structure fixed bed reactors for teaching experiment, when being tested, first by the survey of thermocouple 8 Wen Duan is moved to the horizontal level of stainless (steel) wire 12 and is close to the outer wall of cylinder 3;Afterwards by the solid material of certain particle size or catalysis Agent is inserted in reaction tube 4, then reaction tube 4 is inserted into reactor shell from upper flange 2, by the fixing seal of upper flange 2, finally By pressure for the inert gas of 10MPa is input into reaction tube 4 through material inlet 1, treat that temperature rises to 900 DEG C, by indifferent gas structural reform It is unstrpped gas, the solid material or catalyst that unstripped gas is inserted with the bottom of reaction tube 4 are contacted and reacted, generates product air-flow Reacted device bottom filler 5, exports by reactor content outlet 7, after the completion of reaction, reaction tube 4 is taken out from reactor top And pour out remaining solid sample or catalyst.Said process is the operating procedure of thermostatic process reaction, when investigation temperature-rise period During the response characteristic of middle material, the unstripped gas of specified pressure is passed directly into and without being passed through inert gas, other steps and constant temperature Process is identical.
This reactor uses flange and pad combination sealing, simple structure.Shell portion uses nickel-base alloy material, can be real Existing single tube holds high temperature and holds the effect of high pressure.Meanwhile, by thermocouple it is external and reduce reaction pipe outer wall and reactor shell inwall Distance, ensure that the accurate of inside reactor temperature while original thermocouple built-in structure of reactor is greatly simplified Property.Reaction tube can be dismounted from reactor top, and its hollow space is in funnel shaped, can be smoothly former by remaining solid after the completion of reaction Material or catalyst are poured out, easy to operate.Without mobile reactor main part in experimentation, reality is largely reduced The destruction that human factor is caused to reactor during testing.Additionally, being equipped with packing material in reactor lower part, inside reactor is empty Cavity volume is smaller, greatly reduces the residence time of material in course of reaction, reduces the carrying out of side reaction, is conducive to reaction Forward direction carries out the Efficient Conversion with material.
A kind of single tube structure for teaching experiment of the invention is illustrated as a example by being reacted with regard to semicoke hydrogasification below to consolidate A kind of structure and experimentation of fixed bed reactor.
The The concrete specification of experimental reactor is:The external diameter of reaction tube 4 is 24mm, a length of 300mm, and the height of lower inwall 11 is 100mm, upper inwall 9 is respectively 5mm and 20mm with the internal diameter of lower inwall 11, and middle inwall 10 is 150 ° with the angle of lower inwall 11; The external diameter of cylinder 3 is 44, and thickness is 5mm, a length of 600mm;The outer wall of reaction tube 4 is 5mm with the inwall distance of cylinder 3;Stainless (steel) wire It is 200 mesh, broken ceramics is inserted in the lower section of reaction tube 4(The mesh of granularity 5 ~ 10)Used as filler, its upper surface is away from reaction tube bottom face It is 3mm.
Accompanying drawing 2 is that the bottom temp of this reaction tube 4 is schemed with the temperature comparisons of reactor shell 3, and assay method is:Open heating The temperature of reactor shell 3 is risen to 900 DEG C and keeps constant temperature by device, and then an other thermocouple is inserted from reaction tube top Enter to react at bottom of the tube stainless (steel) wire and determine reaction tube temperature herein, find out that the bottom temp of reaction tube 4 is basic from accompanying drawing 2 Stabilization meets requirement of experiment at 900 DEG C.
Specific experiment process:First by 5.0g granularities for the semicoke that dries of 20 ~ 40 mesh is poured into reaction tube 4, after will reaction In the intercalation reaction device cylinder 3 of pipe 4, and complete the sealing of upper flange and fix, then pass to nitrogen that pressure is 10MPa as protection Gas, controls heater afterwards, and temperature is risen into 900 DEG C and constant temperature is kept, and the nitrogen of 10MPa then is changed into hydrogen is passed through reaction In device, reaction stops heating after 60 minutes, and hydrogen is changed into nitrogen, and question response device is down to room temperature, stops ventilation and by reactor Normal pressure is down to, reactor upper flange 2 is opened, reaction tube 4 is taken out and is poured out remaining semicoke and weigh, remaining 0.53g, through gas phase color After spectrum detection and calculating, common property life methane 6.12L, semicoke conversion ratio is 89.4%, and efficiency of carbon con version is 95.5%.After the completion of experiment, Open reactor lower flange and filler is poured out into sieving(200 mesh), semicoke particle or powder are not found, illustrate that semicoke granularity is 20 During ~ 40 mesh, 200 mesh stainless (steel) wires can realize the effect that semicoke particle does not fall, and above-mentioned experimentation result is accurately credible.
This experimental reactor is characterized in, with simple structure and succinct operating procedure, to realize the experiment of HTHP Condition, meets some experiments reaction needs higher to temperature and pressure requirement, enormously simplify the master of existing fixture bed experiment Body structure, while the cavity volume inside experimental reactor is smaller, preferably avoids experiment material and is stopped in inside reactor Time problem long, reduces the waste of experimental raw.This reactor low cost of manufacture, experimental cost are low, experiment effect is good, full The foot requirement of Chemical Engineering Specialty experimental teaching at this stage.

Claims (5)

1. a kind of single tube structure fixed bed reactors for teaching experiment, including material inlet, upper flange, cylinder, reaction tube, Filler, lower flange, material outlet, stainless (steel) wire and its heater;It is characterized in that:
In the cylinder(3)Inside it is provided with reaction tube described in(4), in the reaction tube(4)Below be provided with described in one not Rust steel mesh(12)And described filler(5), and by the cylinder(3)The heater of both sides(13)Heat instead Should;
The reaction tube(4)Be monolithically fabricated in T-shape structure, and with the cylinder(3)Length ratio be 0.4 ~ 0.6: 1 and Cylinder(3)External diameter ratio be 1: 1.3 ~ 3;
The reaction tube(4)Internal cavities from bottom to top be in funnel-shaped structure, lower inwall(11)Height account for tube length of reaction tube 5 ~ 50%;Upper inwall(9)With lower inwall(11)Internal diameter ratio be 1:1~10;Middle inwall(10)With lower inwall(11)Angle be 100~180°;
The reaction tube(4)When built-in, the cylinder is inserted directly into(3)It is interior, and reaction tube(4)Outside wall surface and cylinder(3) Internal face interval≤5mm, and by upper flange(2)Sealing is compressed to fix.
2. the single tube structure fixed bed reactors of teaching experiment are used for as claimed in claim 1, it is characterized in that:The stainless steel Net(12)It is the stainless (steel) wire of 10 ~ 600 mesh.
3. the single tube structure fixed bed reactors of teaching experiment are used for as claimed in claim 1, it is characterized in that:The single tube knot The reaction temperature of structure fixed bed reactors is 900 DEG C, and reaction pressure is 10MPa.
4. the single tube structure fixed bed reactors of teaching experiment are used for as claimed in claim 1, it is characterized in that:Described filler (5)Upper surface and reaction tube(4)The distance of bottom face be 2 ~ 5mm.
5. the single tube structure fixed bed reactors of teaching experiment are used for as claimed in claim 1, it is characterized in that:
Solid material or solid catalyst are placed in reaction tube by the single tube structure fixed bed reactors in experiment(4)In, and By reaction tube(4)It is installed in reactor, by upper flange(2)Fixing seal, then by the inert gas of 10MPa pressure through thing Material import(1)Input reaction tube(4), when reaction temperature rises to 900 DEG C, by inert gas be changed to the unstripped gas of 10MPa pressure Body, unstrpped gas and reaction tube(4)The solid material or catalyst contact that bottom is inserted are reacted, and generation product gas are flowed through instead Answer device bottom filler(5), by material outlet(7)Output, after the completion of reaction, reaction tube is taken out from reactor top(4)And will Remaining solid sample or catalyst are poured out, and are tested again.
CN201611210358.2A 2016-12-24 2016-12-24 A kind of single tube structure fixed bed reactors for teaching experiment Expired - Fee Related CN106732202B (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110444096A (en) * 2019-08-15 2019-11-12 长江师范学院 A kind of high-efficiency environment friendly senior chemistry paraffin oil decomposition experimental device and its application method
GB2598579A (en) * 2020-09-02 2022-03-09 Unisa Tubular reactors

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CN104667740A (en) * 2013-11-29 2015-06-03 宇星科技发展(深圳)有限公司 Micro ozone washing device and air quality monitoring system

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CN104667740A (en) * 2013-11-29 2015-06-03 宇星科技发展(深圳)有限公司 Micro ozone washing device and air quality monitoring system

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110444096A (en) * 2019-08-15 2019-11-12 长江师范学院 A kind of high-efficiency environment friendly senior chemistry paraffin oil decomposition experimental device and its application method
CN110444096B (en) * 2019-08-15 2021-08-17 长江师范学院 Efficient environment-friendly high-school chemical paraffin oil decomposition experimental device and using method thereof
GB2598579A (en) * 2020-09-02 2022-03-09 Unisa Tubular reactors

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