CN106732202B - 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
CN106732202B
CN106732202B CN201611210358.2A CN201611210358A CN106732202B CN 106732202 B CN106732202 B CN 106732202B CN 201611210358 A CN201611210358 A CN 201611210358A CN 106732202 B CN106732202 B CN 106732202B
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reaction tube
reaction
fixed bed
reactor
cylinder
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CN106732202A (en
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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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    • 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)
  • Organic Chemistry (AREA)
  • Devices And Processes Conducted In The Presence Of Fluids And Solid Particles (AREA)
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  • Oil, Petroleum & Natural Gas (AREA)
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Abstract

The invention discloses a kind of single tube structure fixed bed reactors for teaching experiment, the fixed bed reactors are that a reaction tube is provided in cylinder, and a stainless (steel) wire and the filler are provided with below reaction tube, and heating reaction is carried out by the heating device of cylinder two sides.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 progress, improves the conversion ratio of raw material.

Description

A kind of single tube structure fixed bed reactors for teaching experiment
Technical field
The present invention relates to a kind of fixed bed reactors, especially a kind of to be used for methane-CO 2 reformation and coal/coke gas The teaching experiment fixed bed reactors of the high-temperature high-voltage reaction process of change.
Background technique
It is in the incubation of chemical undergraduate and postgraduate to be related to reactor and reaction unit, especially fixed bed more Reactor.Fixed bed reactors are in the laboratory development phase of Chemical Engineering Technology, industrialization amplification and industrialized production stage tool It plays an important role.The fixed bed reactors of existing experiment are mostly external pressure-bearing and the internal fabricated structure for holding heat, general volume Huge, structure is complicated for inside reactor, and manufacture and maintenance cost are higher.In addition, during reaction under high pressure, due in reactor Portion's pressure is higher, causes the extended residence time of reaction raw materials and product in reactor to a certain extent, and side reaction is tight Weight, reduces the conversion ratio of raw material, extends test period, increase experiment fees.Therefore, student in learning process often Fixed bed reactors can only be understood by way of picture or animation, operate cannot be achieved on the spot substantially.
Existing literature CN201558692U discloses " reactor of a kind of high temperature resistant, high pressure handling convenient catalyst ", should Reactor is mainly by portions such as cylinder, upper lower end cap, upper-lower compacting module, locking nut, catalyst bracket and aluminum radiating gaskets It is grouped as.Its structure is more complicated, is equipped with cooling fin and material import and export in reactor cylinder body portion, external for reactor Heating part Structural Design Requirement it is higher;It needs to vibrate entire reactor when catalyst filling, it cannot be guaranteed that catalyst Filling uniformly, causes catalytic effect to be affected.In addition, the reactor maximum temperature be 450 DEG C, cannot meet the requirements temperature compared with The reaction process such as high methane-CO 2 reformation and coal/semicoke hydrogasification.Due to the above reasons, one in teaching process As do not use the type reactor.
Existing literature CN101537327A is disclosed " a kind of fixed bed reactors ", which specifically includes that shell, protects The parts such as adiabator, crystal reaction tube.The reactor is a kind of high temperature resistant, high-pressure reactor, structure and shell-and-tube reactor Similar, the reactor is mainly heat-resisting by inner quartz tube, and the phase seperated reactor of heat-resisting and pressure-bearing of shell pressure-bearing causes Structure of reactor is complicated, manufacturing cost increases;Since the reactor heating part is located inside reactor, match in dismounting and replacement It needs to partially open reactor body when part, operation is more inconvenient.It is generally fixed using this type during teaching experiment Bed, but since the general volume of the reactor is larger, more people's cooperations are generally required during actually behaviour could complete operation, take When it is laborious.Since its manufacturing cost is higher, and internal cavities volume is larger, and instruction cost is caused to increase.
Summary of the invention
The object of the present invention is to provide a kind of single tube structure fixed bed reactors for teaching experiment, to solve at present In the incubation of chemical undergraduate and postgraduate, structure is complicated, experiment for the high temperature and pressure fixed bed reactors of experiment The higher problem of overlong time, experimental cost, the especially fixed bed reactors in 900 DEG C of high temperature and 10MPa pressure.
The present invention, which 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 heating device;It is characterized in that:
It is provided with a reaction tube in the cylinder, a stainless (steel) wire is provided with below the reaction tube And the filler, and heating reaction is carried out by the heating device of the cylinder two sides;
The overall structure of the reaction tube is in T-shape structure, and is 0.4 ~ 0.6: 1 and cylinder with the length of cylinder ratio The outer diameter ratio of body is 1: 1.3 ~ 3;Reaction tube horizontal component and vertical component are connected by way of being fully welded;
The internal cavities of the reaction tube are in funnel-shaped structure from bottom to top, the height of lower inner wall account for tube length of reaction tube 5 ~ 50%;The internal diameter ratio of upper inner wall and lower inner wall is 1:1 ~ 10;Middle inner wall and the angle of lower inner wall (11) are 100 ~ 180 °, convenient anti- Remaining solid raw material or catalyst should be poured out after the completion.
The reaction tube is inserted directly into the cylinder when built-in, and the inner wall of the outside wall surface of reaction tube and cylinder Interval≤5mm, and pass through 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 bottom face of the upper surface and reaction tube of the filler away from From being 2 ~ 5mm, to reduce inside reactor cavity volume, 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 and is fixed by upper flange, then will through material inlet The nitrogen of 10MPa pressure or other inert gases input reaction tube, and 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, at this point, gas raw material and the solid material or catalyst that react bottom of the tube merging Contact is reacted, and is generated product gas and is flowed through reactor lower part filler, export by reactor outlet, after the reaction was completed, from anti- It answers device top to take out reaction tube and pours out remaining solid sample or catalyst, tested again.
A kind of single tube structure fixed bed reactors for teaching experiment provided by the present invention is above-mentioned, in current ground quadrangle In the case that teaching and scientific research funds in school are very nervous, it is used for experimental teaching, structure to be simple, easily fills readily removable, and occupied area is small, experiment At 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.
Detailed description of the invention
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 inner wall;10: middle inner wall;11: lower inner wall;12: stainless (steel) wire;13: heating device.
Specific embodiment
A specific embodiment of the invention is further illustrated below.
Implement a kind of single tube structure fixed bed reactors for teaching experiment, which is by material inlet 1, upper flange 2, cylinder 3, reaction tube 4, filler 5, lower flange 6, material outlet 7, thermocouple 8, upper inner wall 9, middle inner wall 10, it is lower in Wall 11, stainless (steel) wire 12 and its heating device 13 carry out configuration assembling using the prior art and constitute.
Specific embodiment is a reaction tube 4 to be arranged in cylinder 3, and one 10 ~ 600 mesh are arranged below reaction tube 4 Stainless (steel) wire 12 and merging filler 5, filler 5 can be the broken of broken tile, 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 at a distance from the bottom face of reaction tube 4;Anti- It answers the setting of 3 two sides of device cylinder that heating device 13 is installed, and thermocouple 8 is installed between cylinder 3 and heating device 13, to solid Fixed bed reactor carries out heating reaction 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, horizontal component and vertical component are connected by way of being fully welded, 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;The length ratio of reaction tube 4 and cylinder is designed as 0.4 ~ 0.6: 1 and cylinder 3 Outer diameter ratio be designed as 1: 1.3 ~ 3;The inner cavity of reaction tube 4 is funnel-shaped structure from bottom to top, and the height of lower inner wall 11 is anti- Answer the 5 ~ 50% of length of tube;The internal diameter ratio of upper inner wall 9 and lower inner wall 11 is designed as 1:1 ~ 10;The folder of middle inner wall 10 and lower inner wall 11 Angle is designed as 100 ~ 180 °;Reaction tube 4 is inserted directly into reactor in built-in installation, by 4 lower end of reaction tube of T-shape structure Cylinder in, the spaced design of the inner wall of the outside wall surface and reactor shell 3 of reaction tube 4 is≤5mm, and passes through 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 12 horizontal position of stainless (steel) wire and is close to the outer wall of cylinder 3;Afterwards by the solid material of certain particle size or catalysis Agent is placed in reaction tube 4, then reaction tube 4 is disposed from upper flange 2 into reactor shell, by 2 fixing seal of upper flange, finally The inert gas that pressure is 10MPa is inputted in reaction tube 4 through material inlet 1,900 DEG C are risen to temperature, by indifferent gas structural reform For unstrpped gas, the solid material or catalyst that unstripped gas and 4 bottom of reaction tube are placed in are contacted and are reacted, and generate product air-flow Reacted device lower part filler 5 after the reaction was completed, takes out reaction tube 4 from reactor top by 7 output of reactor content outlet And remaining solid sample or catalyst are poured out.The above process is the operating procedure of thermostatic process reaction, when investigation temperature-rise period When the response characteristic of middle material, it is passed directly into the unstripped gas of specified pressure and does not have to be passed through inert gas, other steps and constant temperature Process is identical.
This reactor is simple using flange and gasket combination sealing, 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 it is thermocouple is external and reduce reaction pipe outer wall and reactor shell inner wall Distance, ensure that the accurate of inside reactor temperature while greatly simplifying the structure of reactor built in original thermocouple Property.Reaction tube can be dismounted from reactor top, and hollow space is in funnel shaped, after the reaction was completed can be smoothly by remaining solid original Material or catalyst are poured out, easy to operate.Do not have to mobile reactor main part during the experiment, largely reduces reality Human factor destruction caused by reactor during testing.In addition, 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 reaction process, reduces the progress of side reaction, is conducive to reaction Forward direction carries out and the Efficient Conversion of material.
It is solid with regard to illustrating a kind of single tube structure for teaching experiment of the present invention for semicoke hydrogasification reaction below A kind of structure and experimentation of fixed bed reactor.
The concrete specification of experimental reactor are as follows: the outer diameter of reaction tube 4 is 24mm, a length of 300mm, and the height of lower inner wall 11 is The internal diameter of 100mm, upper inner wall 9 and lower inner wall 11 is 5mm and 20mm respectively, and the angle of middle inner wall 10 and lower inner wall 11 is 150 °; The outer diameter of cylinder 3 is 44, thickness 5mm, a length of 600mm;The inner wall of 4 outer wall of reaction tube and cylinder 3 distance is 5mm;Stainless (steel) wire For 200 mesh, broken tile (5 ~ 10 mesh of granularity) is placed in the lower section of reaction tube 4 and is used as filler, the upper end identity distance reaction tube bottom face For 3mm.
Attached drawing 2 is temperature comparisons' figure of 4 bottom temp of this reaction tube and reactor shell 3, and measuring method is: opening heating The temperature of reactor shell 3 is risen to 900 DEG C and keeps constant temperature by device, then inserts an other thermocouple from reaction tube top Enter to react at bottom of the tube stainless (steel) wire and measure reaction tube temperature herein, finds out that the bottom temp of reaction tube 4 is basic from attached drawing 2 Stablize at 900 DEG C, meets requirement of experiment.
Specific experiment process: first by 5.0g granularity be 20 ~ 40 mesh drying semicoke pour into reaction tube 4, after will reaction In 4 intercalation reaction device cylinder 3 of pipe, and the sealing for completing upper flange is fixed, and is then passed to the nitrogen that pressure is 10MPa and is used as protection Gas controls heating device afterwards, and temperature is risen to 900 DEG C and keeps constant temperature, and the nitrogen of 10MPa is then changed to hydrogen and is passed through reaction In device, reaction stops heating after sixty minutes, and hydrogen is changed to nitrogen, is down to room temperature to reactor, stops ventilation and by reactor It is down to normal pressure, opens reactor upper flange 2, take out reaction tube 4 and remaining semicoke is poured out into weighing, remaining 0.53g, through gas phase color After spectrum detection and calculating, the raw methane 6.12L of common property, semicoke conversion ratio is 89.4%, efficiency of carbon con version 95.5%.After the completion of experiment, It opens reactor lower flange and filler is poured out into sieving (200 mesh), do not find semicoke particle or powder, illustrate that semicoke granularity is 20 When ~ 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 realizing the experiment of high temperature and pressure with succinct operating procedure in simple structure Condition meets some experiments reaction needs more demanding to temperature and pressure, enormously simplifies the master of existing fixture bed experiment Body structure, while the cavity volume inside experimental reactor is smaller, preferably avoids experiment material and stops in inside reactor The problem of time length, reduces the waste of experimental raw.This reactor manufacturing cost is low, experimental cost is 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 heating device;It is characterized in that:
A reaction tube (4) is provided in the cylinder (3), be provided with one below the reaction tube (4) described in not Become rusty steel mesh (12) and the filler (5), and heat instead by the heating device (13) of the cylinder (3) two sides It answers;
The overall structure of the reaction tube (4) is in T-shape structure, and with the length ratio of the cylinder (3) be 0.4 ~ 0.6: 1, with The outer diameter ratio of cylinder (3) is 1: 1.3 ~ 3;
The internal cavities of the reaction tube (4) are in funnel-shaped structure from bottom to top, and the height of lower inner wall (11) accounts for tube length of reaction tube 5 ~ 50%;The internal diameter ratio of upper inner wall (9) and lower inner wall (11) is 1:4 ~ 10;The angle of middle inner wall (10) and lower inner wall (11) is 100~150°;
The reaction tube (4) is inserted directly into the cylinder (3) when built-in, and the outside wall surface of reaction tube (4) and cylinder (3) Inner wall interval≤5mm, and by upper flange (2) compress sealing fix.
2. the single tube structure fixed bed reactors of teaching experiment are used for as described in claim 1, it is characterized in that: the stainless steel Net (12) is the stainless (steel) wire of 10 ~ 600 mesh.
3. the single tube structure fixed bed reactors of teaching experiment are used for as described 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 described in claim 1, it is characterized in that: the filler (5) upper surface is 2 ~ 5mm at a distance from the bottom face of reaction tube (4).
5. it is used for the single tube structure fixed bed reactors of teaching experiment as described in claim 1, it is characterized in that:
Solid material or solid catalyst are placed in reaction tube (4) by the single tube structure fixed bed reactors in experiment, and Reaction tube (4) is installed in reactor, by upper flange (2) fixing seal, then by the inert gas of 10MPa pressure through object Expect import (1) input reaction tube (4), when reaction temperature rises to 900 DEG C, inert gas be changed to the unstrpped gas of 10MPa pressure, The solid material or catalyst that unstrpped gas and reaction tube (4) bottom are placed in are contacted and are reacted, and are generated product gas and are flowed through reaction Device lower part filler (5) is exported by material outlet (7), after the reaction was completed, is taken out reaction tube (4) from reactor top and will be remained 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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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
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Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1817436A (en) * 2006-01-16 2006-08-16 华东理工大学 Double-pipe reactor
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

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1817436A (en) * 2006-01-16 2006-08-16 华东理工大学 Double-pipe reactor
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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