CN1429823A - Analogue reactor for olefin hydrocarbon oxidation reaction - Google Patents
Analogue reactor for olefin hydrocarbon oxidation reaction Download PDFInfo
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- CN1429823A CN1429823A CN 01145156 CN01145156A CN1429823A CN 1429823 A CN1429823 A CN 1429823A CN 01145156 CN01145156 CN 01145156 CN 01145156 A CN01145156 A CN 01145156A CN 1429823 A CN1429823 A CN 1429823A
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Abstract
A reactor for simulating the olefine oxidization reaction procedure to evaluate the performance of catalyst features that the hot water evaporation is used to remove reactive heat, the finned radiator is used to condense vapour for returning it bake to reactor, the internal cooling tubes are used to regulate axial and radial temp for reducing temp. different, and more reaction tubes switched flexibly are arranged in it for simulating different reaction conditions.
Description
Technical field
The present invention relates to a kind of reactor that in the experiment of solid alkene oxidation catalysts performance evaluation, is used to simulate oxidation reaction process of olefin hydrocarbon, particularly estimate oxidation of ethylene and produce the reactor that is used for the analog vinyl oxidation reaction process in the experiment of epoxyethane catalyst performance.
Background technology
The industrial reactor that is used for oxidizing reaction mostly is calandria type fixed bed reactor, and catalyzer is filled in the reaction tubes, the shifting out heat-eliminating medium (the mostly being water) evaporation by the reactor shell side or carry out heat exchange with reaction mixture and realize of reaction heat.Usually, the evaluation of the performance of catalyzer is all carried out in the pilot reactor that can simulate the industrial reaction condition or laboratory reaction device.At present, the reactor that is used for evaluating catalyst mostly is single tube reactor, be to have only a reaction tubes in the reactor, adopt thermal oil outer circulation mode to remove reaction heat, therefore a covering device can only be simulated a kind of condition of industrial reactor, and owing to adopt thermal oil to remove hot system, can not simulate the real reaction state of industrial reactor fully, reactor axle, radial temperature difference are all bigger, and reaction is unstable, and the control of temperature of reaction also exists comparatively serious lag phenomenon.And because the heat storage capacity of thermal oil is less, easily makes temperature of reaction out of control, even cause temperature runaway, set off an explosion.In addition, be a kind of experimental installation owing to be used for the reactor of evaluating catalyst, so need on reactor, the multiple spot perforate carry out the measurement and the inspection by sampling of temperature, certainly will produce considerable influence, and then influence the stability and the accuracy of experimental result reaction conditions.
Summary of the invention
The objective of the invention is to propose a kind of novel analogue reactor, to overcome the shortcoming of above-mentioned analogue reactor, and have simple in structure, facility investment is few, stable reaction, temperature of reaction is adjustable, long service life, the condition that can simulate the olefin hydrocarbon oxidation reaction industrial reactor better and result advantage accurately, for Study of Catalyst and exploitation provide reliable basis.
Therefore, the invention provides a kind of reactor that is used at olefin hydrocarbon oxidation reaction catalyst performance evaluation experiment simulation oxidation reaction process of olefin hydrocarbon, it comprises reactor shell; Be arranged on the reaction tubes of described inner barrel; The reaction mass that is arranged on the described reaction tubes is imported and exported and catalyst inlet; Be arranged at the heat-eliminating medium inlet tube and the blow-down pipe on described cylindrical shell top; It is characterized in that also being provided with the vibration damping net in described inner barrel; Be provided with finned radiator at described heat-eliminating medium inlet tube and blow-down pipe; Each needs thermometric and sampling point to be provided with thermometric-thief hole at described cylindrical shell; And described heat-eliminating medium is for removing the hot water of reaction heat with inner loop mode.
Analogue reactor of the present invention is vertical tubular reactor, is made up of reactor shell, reaction tubes, finned radiator, vibration damping net, thermometric-thief hole, reaction mass import and export, catalyst inlet and heat-eliminating medium inlet tube and blow-down pipe.The reactor used cylindrical shell of the present invention can be selected metal material for use, is preferably stainless steel.The catalyzer that is used for olefin hydrocarbon oxidation reaction is housed in the reaction tubes, and the reactor shell side adopts hot water to remove reaction heat.In order to simulate the reactor condition of domestic all olefin hydrocarbon oxidation reaction devices at present flexibly, analogue reactor of the present invention can be provided with many reaction tubess as required, and every reaction tubes can be simulated a cover industrial reactor condition.Reaction tubes can be selected metal material for use, be preferably stainless steel, its length and caliber want the mimic industrial reactor to adapt with it respectively, each reaction tubes parallel connection, be provided with independently on the pipe that reaction mass is imported and exported and catalyst inlet, between can switch (as using the switching between the magnetic valve realization response pipe) flexibly.Can use and want the corresponding reaction tubes of mimic industrial reactor when carrying out the evaluating catalyst experiment, adopt the hot water inner loop mode to shift out reaction heat, the inner cyclic process of hot water is finished by well heater that is arranged on reactor bottom and the finned radiator that is arranged on reactor head: the well heater that is arranged on reactor bottom in the reaction process heats hot water, make its upwards evaporation, and the temperature homogeneous of maintenance hot water, in the hot water evaporating course reaction heat is shifted out, and vapor condensation and Returning reactor shell side that finned radiator produces after with hot water absorption reaction heat are realized the internal recycle of hot water.Well heater of the present invention can adopt far-infrared electric heater or resistance wire electric heater.Adopt inner loop mode can reduce the magnitude of recruitment of hot water.In reaction process, the hot water layer that the reactor tube outside forms one deck boiling state strengthens the transmission of heat by convection effect, and the reactor radial temperature difference is reduced.Finned radiator is distributed in heat-eliminating medium inlet tube on the pipeline axial and separately and the concentric ring fin of blow-down pipe constitutes by fluid line with parallel, is installed on reactor shell hot water inlet and the blow-down pipe, and length is determined by the steam output of hot water.When preventing that a large amount of bubbles that hot water evaporation produces from breaking to the impact of reaction tubes, analogue reactor of the present invention is provided with the vibration damping net in cylindrical shell, the air pocket that produces is broken into tiny bubble, the surging force that produces when reducing it and breaking, and can improve the flow-pattern of hot water, enhance heat transfer effect.The vibration damping net adopts the composite mesh structure, is tied together relatively by hole, multiple tracks single-layer metal silk screen hole to constitute.As required, the quantity of vibration damping net can be together, and twice or multiple tracks generally can be arranged on top, bottom and the middle part of cylindrical shell.When the quantity of vibration damping net was one, it can be arranged on the middle part of cylindrical shell; When the quantity of vibration damping net was twice, they can be separately positioned on the upper and lower of cylindrical shell; And when the quantity of vibration damping net was three roads, they can be separately positioned on top, bottom and the middle part of cylindrical shell.In reaction process, form for monitoring inside reactor temperature variation and material everywhere better, need several temperature-measuring ports and thief hole be set in the appropriate location of reactor shell (as the upper, middle and lower portion of reaction tubes inner catalyst bed).Like this, will increase the interference of extraneous factor to reaction conditions.For avoiding the generation of this situation, just need reduce the open amount on the reactor shell as far as possible.Therefore, in order to reach this purpose, the present invention has thermometric-thief hole on the appropriate location of reactor shell, and the sleeve pipe (being called for short the temperature element sleeve pipe) that will place temperature element is linked in together with the sleeve pipe that is connected stopple coupon (being called for short the stopple coupon sleeve pipe), from the reaction tubes cylindrical shell in the same opening insertion reaction device, thereby form thermometric-thief hole of the present invention.Temperature element telescopic top extend in the reaction tubes, and does not communicate with reaction tubes.Prior art is disclosed to be suitable for placing any temperature element in the sleeve pipe all to can be used for the present invention, as thermopair, hot resistance, thermometer etc., the present invention preferably use thermoelectricity occasionally hot resistance as temperature element.Stopple coupon sleeve pipe of the present invention can be used one-piece construction, also can form by two sections.During structure, an end welds with reaction tubes and reactor shell this stopple coupon sleeve pipe mutually as a whole, and the other end and the welding of temperature element sleeve pipe simultaneously, be welded with stopple coupon on the stopple coupon sleeve pipe, and this stopple coupon sleeve pipe communicate with reaction tubes.When the stopple coupon sleeve pipe is formed by two sections, one section of stopple coupon sleeve pipe welds mutually with reaction tubes and reactor shell, this section stopple coupon sleeve pipe communicates with reaction tubes, another section is welded mutually with the temperature element sleeve pipe, weld together with stopple coupon simultaneously, this two portions stopple coupon overlaps effective cutting ferrule and joins, and this cutting ferrule is a universal cutting ferrule on the market.Stopple coupon can link to each other with online gc by valve, also can take a sample by sampling valve with syringe.The temperature element sleeve pipe of thermometric-thief hole of the present invention and stopple coupon sleeve pipe preference card shell type mode of connection, this mode of connection can make temperature element sleeve pipe and weldering one section stopple coupon sleeve pipe thereon integral body take off, and are convenient to catalyst loading and unloading.The material of temperature element sleeve pipe of the present invention, stopple coupon sleeve pipe and stopple coupon can be selected metal material for use, is preferably stainless steel or is the metal tube identical with the reaction tubes material.
For the temperature of conditioned reaction device better, alleviate the hysteresis phenomenon of temperature of reaction control, analogue reactor of the present invention is realized this purpose by the inner cool tube that insertion reaction device shell side is set.Inner cool tube is the metal tube identical with the reaction tubes material, be arranged in parallel with bundle of reaction tubes, has hot water, water vapor or heat conduction wet goods heat transferring medium to circulate therebetween, can finely tune temperature of reactor by the temperature that changes heat transferring medium.The position of inner cool tube and quantity all can be decided on demand.
These and other purposes of the present invention, feature and advantage will become more clear after reading this specification sheets with reference to the following drawings.
The accompanying drawing summary
Fig. 1 is the synoptic diagram of analogue reactor of the present invention;
Fig. 2 is the enlarged view of analogue reactor finned radiator of the present invention; With
Fig. 3 is the enlarged view of analogue reactor thermometric-thief hole of the present invention.
The specific embodiment of the present invention
The present invention will be further described below in conjunction with accompanying drawing, but scope of the present invention is not restricted to this.
In Fig. 1, reactor shell 1 inside has three reaction tubess 5, and the catalyzer that is used for ethylene oxidation reactions is by catalyst inlet 2 reaction tubes 5 of packing into.There is hot water flow in the space that forms between reactor shell 1 and the reaction tubes 5.Upper and lower in reactor shell 1 respectively is equipped with vibration damping net 4 one, finned radiator 7 is housed on the heat-eliminating medium inlet tube 8, finned radiator 7a also is housed on the blow-down pipe 11, inner cool tube 9 insertion reaction device cylindrical shells 1 inside, parallel with reaction tubes 5, be full of heat transferring medium in the inner cool tube 9.In the reactor operating process, enter the tube side of reactor from reaction tubes top inlet 3 through the reaction mass of preheating and recycle stock, oxidizing reaction is taking place in reaction tubes 5 under the effect of catalyzer and emitting reaction heat, reaction heat is shifted out by the hot water evaporation of reactor shell side.Be provided with well heater (as far-infrared electric heater, resistance wire electric heater) 12 at reactor bottom, be used for hot water is heated, make upwards evaporation of water, in the hot water evaporating course reaction heat is shifted out, and vapor condensation and Returning reactor shell side that finned radiator 7 and 7a produce after with hot water absorption reaction heat are realized the internal recycle of hot water.The loss of hot water is remedied by the hot water that replenishes, and the hot water that replenishes enters the reactor shell side through finned radiator 7 by hot water inlet 8.The mixture of resultant of reaction and unreacted material is discharged by reaction tubes outlet at bottom 6 and is entered subsequent processing.In reaction process, the temperature of reaction tubes inner catalyst bed is arranged on reactor shell 1 by insertion respectively needs thermometric-thief hole 10 interior temperature elements of thermometric sampling point (being generally the upper, middle and lower portion of beds) to measure, and is finely tuned by the heat transferring mediums in the inner cool tube 9.
Thermometric-thief hole 10 is an a preferred embodiment of the present invention, its enlarged view as shown in Figure 3, sleeve pipe (the abbreviation temperature element sleeve pipe) 13 that wherein will place temperature element is linked in together with the sleeve pipe that is connected stopple coupon (being called for short the stopple coupon sleeve pipe) 14, from the reaction tubes cylindrical shell 1 in the same opening insertion reaction device, thereby form thermometric-thief hole 10.The top of the temperature element sleeve pipe 13 of this thermometric-thief hole 10 extend in the reaction tubes 5, and does not communicate with reaction tubes 5.Stopple coupon sleeve pipe 14 is formed by two sections, wherein one section is welded mutually with reaction tubes 5 and reactor shell 1, and this section stopple coupon sleeve pipe communicates with reaction tubes 5, and another section is welded mutually with temperature element sleeve pipe 13, weld together with stopple coupon 15 simultaneously, these two portions stopple coupon sleeve pipe 14 usefulness cutting ferrules 16 join.Stopple coupon 15 can link to each other with the online gc (not shown) by the valve (not shown), also can be with the syringe (not shown) by the sampling of sampling valve (not shown).
Reactor of the present invention can be used as the condition of simulation oxidation reaction process reactor in the evaluation experimental of olefin hydrocarbon oxidation reaction solid catalyst performance, be particularly suitable for being used in the experiment of estimating oxidation of ethylene production oxyethane catalyst system therefor performance the condition of analog vinyl oxidation reactor.
Embodiment
Analogue reactor of the present invention can obtain describing more clearly by following examples.
With analogue reactor shown in Figure 1 oxidation of ethylene being produced ethylene oxide reactor simulates, different is the inner cool tube 9 that does not adopt among Fig. 1, the analogue reactor cylindrical shell adopts stainless steel, its external diameter is 325mm, the reaction tubes of three stainless steels is equipped with in inside, and (nominal diameter is respectively 15mm, 20mm and 25mm, length is 14m), and be provided with the vibration damping net of two road stainless steels respectively in the upper and lower of reactor shell, adopt hot water to remove reaction heat.Reaction conditions is as follows:
Reaction pressure (MPa): 2.1
Temperature of reaction (℃): 220～230
Inlet feed is formed: ethene 0.2905%
Oxygen 0.07732%
Oxyethane 0.00056%
Carbonic acid gas 0.07596%
Water 0.00198%
Nitrogen 0.5523%
Argon 0.00119%
Methane 0.00005%
Ethane 0.00014%
Below all be weight percentage
Air speed (h
-1): 5000
Catalyzer: 5.38 liters of YS-6 type silver catalysts (this catalyzer is to be produced by the Research Institute of Beijing Yanshan Petrochemical Corp)
With caliber is that the reaction tubes of 25mm experimentizes, and the upper, middle and lower portion of beds is provided with 3 thermometric-thief holes respectively in reaction tubes, and wherein upper and lower thermometric-thief hole is 2 meters apart from the reactor two ends.In addition, for the temperature of assaying reaction pipe outer wall, 3 universal temperature-measuring ports with 3 same axial locations of thermometric-thief hole are set also, the top of this universal temperature tube extend in the shell side near the reactor at reaction tubes place.Insert the thermometric-thief hole and the universal temperature-measuring port of setting with hot resistance respectively as temperature element in the reaction process, the temperature data that same axial temperature measurement location records subtracts each other and obtains the reaction tubes inside and outside wall temperature difference, and its value is 5～7 ℃.Comparative Examples 1
(the reactor cylinder body diameter is 50mm with single tube reactor, the reaction tubes caliber is 25mm) oxidation of ethylene production ethylene oxide reactor is simulated, reaction conditions is with embodiment 1, adopt the YD-300 thermal oil that the Research Institute of Beijing Yanshan Petrochemical Corp produces (20 ℃ time proportion be 1.01), Recycle design is removed reaction heat in addition, the upper, middle and lower portion of beds is provided with 3 universal temperature-measuring ports and 3 thief holes in reaction tubes, and wherein upper and lower temperature-measuring port and thief hole are 2 meters apart from the reactor two ends.In addition, for the temperature of assaying reaction pipe outer wall, 3 universal temperature-measuring ports with aforementioned 3 same axial locations of universal temperature-measuring port are set also, the top of this universal temperature tube extend in the shell side near the reactor at reaction tubes place.To obtain the reaction tubes inside and outside wall temperature difference with embodiment 1 same procedure is 15～20 ℃.Embodiment 2
With the analogue reactor of embodiment 1 oxidation of ethylene is produced the ethylene oxide reactor condition and simulate, reaction conditions is with embodiment 1.Use hot resistance to measure the temperature of thermometric-thief hole up and down respectively as temperature element, both subtract each other, and to obtain the reactor axial temperature difference be 2～3 ℃.Comparative Examples 2
With the single tube reactor of Comparative Examples 1 oxidation of ethylene is produced the ethylene oxide reactor condition and simulate, reaction conditions is with embodiment 1.Using hot resistance to measure the temperature of temperature-measuring port up and down respectively as temperature element, is 5～6 ℃ by obtaining the reactor axial temperature difference with embodiment 2 same procedure.
Claims (12)
1. one kind is used for testing the reactor of simulating oxidation reaction process of olefin hydrocarbon in the olefin hydrocarbon oxidation reaction catalyst performance evaluation, and it comprises reactor shell (1); Be arranged on the inner reaction tubes (5) of described cylindrical shell (1); The reaction mass that is arranged on the described reaction tubes (5) imports and exports (3; 6) and catalyst inlet (2); Be arranged at the heat-eliminating medium inlet tube (8) and the blow-down pipe (11) on described cylindrical shell (1) top; It is characterized in that also being provided with the vibration damping net (4) that is used for protective reaction pipe (5) in described cylindrical shell (1) inside; Be provided with finned radiator (7 at described heat-eliminating medium inlet tube (8) and blow-down pipe (11); 7a); Each needs thermometric and sampling point to be provided with thermometric-thief hole (10) at described cylindrical shell (1); And described heat-eliminating medium is for removing the hot water of reaction heat with inner loop mode.
2. reactor according to claim 1 is characterized in that being arranged in parallel many described reaction tubess (5) in described cylindrical shell (1) inside.
3. reactor according to claim 1 is characterized in that described reactor bottom is provided with its well heater that heats (12).
4. reactor according to claim 1 is characterized in that described finned radiator (7; Form 7a) for its fin is and separately heat-eliminating medium inlet tube (8) and the concentric annular of blow-down pipe (11), parallel be distributed in pipe axially on.
5. reactor according to claim 1 is characterized in that being provided with a plurality of described vibration damping nets (4) in described cylindrical shell (1) inside.
6. reactor according to claim 5 is characterized in that described vibration damping net (4) is the composite mesh structure, is tied together relatively by hole, multiple tracks single-layer metal silk screen hole to constitute.
7. reactor according to claim 1, it is characterized in that at the inner inner cool tube (9) that is used for the conditioned reaction temperature that also is provided with of described reactor shell (1), described inner cool tube (9) is and the identical metal tube of described reaction tubes (5) material, and parallel with bundle of reaction tubes.
8. reactor according to claim 7 is characterized in that the heat transferring medium in the described inner cool tube (9) is hot water, water vapor, thermal oil or other media.
9. reactor according to claim 1, it is characterized in that described thermometric-thief hole (10) comprises temperature element sleeve pipe (13) and the stopple coupon sleeve pipe (14) that is linked in together, and described stopple coupon sleeve pipe (14) is one-piece construction, the one end welds mutually with described reaction tubes (5) and described reactor shell (1), the other end welds mutually with described temperature element sleeve pipe (13), simultaneously be welded with stopple coupon (15) on described stopple coupon sleeve pipe (14), described stopple coupon sleeve pipe (14) communicates with described reaction tubes (5).
10. reactor according to claim 1, it is characterized in that described thermometric-thief hole (10) comprises temperature element sleeve pipe (13) and the stopple coupon sleeve pipe (14) that is linked in together, and described stopple coupon sleeve pipe (14) is formed by two sections, wherein one section is welded mutually with described reaction tubes (5) and described reactor shell (1) and this section stopple coupon sleeve pipe communicates with described reactor (5), another section is welded mutually with described temperature element sleeve pipe (13), weld together with described stopple coupon (15) simultaneously, and these two sections stopple coupon sleeve pipes (14) join with cutting ferrule (16).
11., be used for condition at the evaluation experimental simulation olefin oxidation industrial reactor of olefin hydrocarbon oxidation reaction catalyst performance according to each described reactor in the claim 1～10.
12. reactor according to claim 11 is used for the experiment analog vinyl oxidation reaction process of estimating to the performance of the catalyzer of the used various models of ethylene oxidation reactions.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB011451564A CN1194973C (en) | 2001-12-31 | 2001-12-31 | Analogue reactor for olefin hydrocarbon oxidation reaction |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB011451564A CN1194973C (en) | 2001-12-31 | 2001-12-31 | Analogue reactor for olefin hydrocarbon oxidation reaction |
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| Publication Number | Publication Date |
|---|---|
| CN1429823A true CN1429823A (en) | 2003-07-16 |
| CN1194973C CN1194973C (en) | 2005-03-30 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB011451564A Expired - Lifetime CN1194973C (en) | 2001-12-31 | 2001-12-31 | Analogue reactor for olefin hydrocarbon oxidation reaction |
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| Country | Link |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105467062A (en) * | 2015-12-14 | 2016-04-06 | 天津市天环精细化工研究所 | Pilot reactor for catalyst performance evaluation |
| CN107037145A (en) * | 2016-12-02 | 2017-08-11 | 上海化工研究院有限公司 | A kind of multichannel rowed rings purifying vehicle exhaust material property comparison means |
-
2001
- 2001-12-31 CN CNB011451564A patent/CN1194973C/en not_active Expired - Lifetime
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105467062A (en) * | 2015-12-14 | 2016-04-06 | 天津市天环精细化工研究所 | Pilot reactor for catalyst performance evaluation |
| CN107037145A (en) * | 2016-12-02 | 2017-08-11 | 上海化工研究院有限公司 | A kind of multichannel rowed rings purifying vehicle exhaust material property comparison means |
| CN107037145B (en) * | 2016-12-02 | 2019-10-22 | 上海化工研究院有限公司 | A kind of multichannel rowed rings purifying vehicle exhaust material property comparison unit |
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| Publication number | Publication date |
|---|---|
| CN1194973C (en) | 2005-03-30 |
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Granted publication date: 20050330 |