CN202246046U - Deep removing device for CO in hydrogen-rich gas - Google Patents

Deep removing device for CO in hydrogen-rich gas Download PDF

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CN202246046U
CN202246046U CN2011203249893U CN201120324989U CN202246046U CN 202246046 U CN202246046 U CN 202246046U CN 2011203249893 U CN2011203249893 U CN 2011203249893U CN 201120324989 U CN201120324989 U CN 201120324989U CN 202246046 U CN202246046 U CN 202246046U
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bed reactor
water vapor
fixed
reactor
lower flange
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解东来
王子良
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South China University of Technology SCUT
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Abstract

The utility model discloses a deep removing device for CO in a hydrogen-rich gas. A fixed bed reactor of the deep removing device comprises a reactor cylinder body, an upper flange and a lower flange, wherein the reactor cylinder body is respectively connected with the upper flange and the lower flange through bolts; the upper flange is provided with a raw material gas inlet pipe; the lower flange is provided with a product gas outlet pipe; a Pt/gamma-Al2O3 catalyst and gamma-Al2O3 particles are filled into the reactor cylinder body sequentially layer by layer; the fixed bed reactor is provided with an air distribution device; an opening of the air distribution device is formed in a bed layer of the Pt/gamma-Al2O3 catalyst; temperature measuring points of multipoint thermocouples are positioned in the Pt/gamma-Al2O3 catalyst; and the reactor cylinder body is surrounded by a water vapor jacket. The deep removing device can be directly butted with a hydrogen-rich synthetic gas which is produced by hydrogen production of fossil fuel reformation and has the advantages of high starting speed, convenience and feasibility for assembly and disassembly, small device volume and small occupied area.

Description

CO deep removal device in a kind of hydrogen-rich gas
Technical field
The utility model relates to the method and the device of the CO preferential oxidation of CO in a kind of deep removal hydrogen-rich gas, is used to Proton Exchange Membrane Fuel Cells the hydrogen-rich synthetic gas of CO content below 10ppm is provided.
Background technology
Fuel cell is the high efficient energy sources transfer equipment that a kind of chemical energy with fuel is converted into electric energy.At present, the Proton Exchange Membrane Fuel Cells of technical development comparative maturity has strict requirement to CO content in the fuel in application process, and general requirement is less than 10ppm.Therefore, need the CO in the hydrogen rich gas is carried out deep removal (＜10ppm) just can the act as a fuel fuel of battery.The CO preferential oxidation is one of most effectual way of removing at present CO in the hydrogen-rich gas, and the CO preferential oxidation is one of gordian technique of fuel cell virgin gas preparation in the hydrogen-rich gas.
Employing preferential oxidation technology is removed to the CO in the reformed gas below the 10ppm, reduces air feeding amount, improves hydrogen yield, and the design of preferential oxidation reactor is gordian technique wherein.At present, preferential oxidation reactor mainly contains following several kinds: multistage adds oxygen reactor, membrane reactor and micro passage reaction.The structure that multistage advances oxygen reactor is simple relatively, and reactivity worth is better, but still needs further to optimize configuration, oxygen feeding amount and the heat transfer structure that enters the oxygen zone, improves the selectivity of catalysts, improves the performance that multistage advances oxygen reactor.Membrane reactor has its unique advantage, promptly obtains target product with high purity, but the power resources of reaction gas through film are gas pressure differences in the film both sides, need virgin gas that higher pressure is arranged.Micro passage reaction can enhanced reactor heat transfer, mass-transfer performance, with respect to traditional fixed-bed reactor, be applied to the reaction of CO preferential oxidation and have certain advantage.
The principle of work of CO preferential oxidation is in reformed gas, to feed O 2, O 2With respect to hydrogen preferential oxidation CO, so both removed CO, avoided the consumption of hydrogen simultaneously.CO preferential oxidation process can be reduced to the concentration of CO below the 10ppm through the reactor design of optimization and the catalyzer of highly selective, in oxidation CO, reduces H as far as possible 2Oxidation, guarantee the efficient of whole fuel cell system.Its main reaction process is:
Figure BDA0000088142760000011
ΔH (298)＝-283kJ/mol (1)
Issuable side reaction is:
Figure BDA0000088142760000012
ΔH (298)＝-242kJ/mol (2)
Figure BDA0000088142760000021
ΔH (298)＝-41.1kJ/mol (3)
The utility model content
The purpose of the utility model is to overcome the shortcoming of existing fixed bed bioreactor; CO deep removal method and device in a kind of hydrogen-rich gas are provided, the utlity model has efficient, quick and safe advantage, the hydrogen-rich synthetic gas that this device adopts the fossil oil reformation to obtain is a virgin gas; Compact construction; Handled easily, volume is little, is easy to install.
The purpose of the utility model realizes through following technical scheme:
CO deep removal device in a kind of hydrogen-rich gas comprises fixed-bed reactor, Pt/ γ-Al 2O 3Catalyzer, γ-Al 2O 3Particle, air-distributor, multiple spot thermopair, water vapor chuck and thermal insulation layer; Fixed-bed reactor comprise reactor shell, upper flange and lower flange, and reactor shell is connected through bolt with lower flange with upper flange respectively, and upper flange is equipped with the virgin gas inlet pipe; Lower flange is equipped with product gas fairlead; Pt/ γ-Al 2O 3Catalyzer and γ-Al 2O 3Particle layering successively fills in the reactor shell; Air-distributor is installed on the fixed-bed reactor, and the air-distributor opening is arranged at Pt/ γ-Al 2O 3In the beds, be used for air being provided to reaction; The multiple spot thermopair is installed on the fixed-bed reactor, and the point for measuring temperature of multiple spot thermopair is positioned at Pt/ γ-Al 2O 3In the catalyzer, be used to monitor temperature of reaction; Reactor shell is surrounded by the water vapor chuck, and water vapor chuck bottom is connected with the water vapor inlet tube, and water vapor chuck top is connected with the water vapor fairlead, and the water vapor inlet tube is provided with valve; Lower flange covers with thermal insulation layer on water vapor chuck and the fixed-bed reactor.
Further, described Pt/ γ-Al 2O 3Catalyzer is for being carried on γ-Al 2O 3Pt catalyzer on the particle, the mass loading amount of Pt is 0.5%～2.0%; γ-Al 2O 3The particle diameter of carrier is 2～5mm, and the micropore size in the particle is 5～10nm, and micropore specific area is greater than 270m 2/ g, Pt/ γ-Al 2O 3The CO air speed of catalyzer is 20～100h -1The CO air speed be meant the ratio of volume of CO flow and the catalyzer in the treatable virgin gas;
Said Pt/ γ-Al 2O 3Loaded catalyst
Figure BDA0000088142760000022
Wherein: F is the volumetric flow rate (m of CO in the virgin gas 3/ h), v is the CO air speed (h of catalyzer -1).
Described γ-Al 2O 3Particle is selected γ-Al with Pt/ for use 2O 3The particle that support of the catalyst is same; γ-Al 2O 3Particle packing amount V 2=0.5V 1～V 1
Described fixed-bed reactor are drum, fixed-bed reactor cavity volume V=V 1+ V 2
Fixed-bed reactor cylinder internal diameter D 1=(15～30) d; Wherein d is γ-Al 2O 3The particle diameter of carrier;
Fixed-bed reactor height
Figure BDA0000088142760000023
V is the fixed-bed reactor cavity volume.
Pt/ γ-Al in the said fixed-bed reactor 2O 3Catalyzer and γ-Al 2O 3The particulate type of feed is: press 0.25V from top to bottom successively 1Pt/ γ-Al 2O 3Catalyzer, 0.5V 2γ-Al 2O 3Particle, 0.5V 1Pt/ γ-Al 2O 3Catalyzer, 0.5V 2γ-Al 2O 3Particle, 0.25V 1Pt/ γ-Al 2O 3Catalyzer loads.
Said air-distributor is the stainless steel tube of a diameter 3～6mm, and the air that is drilled with 3 diameter 0.4mm～1.0mm on the tube wall is introduced the hole, and the position in three holes lays respectively at three Pt/ γ-Al 2O 3The top of beds; Air-distributor inserts fixed-bed reactor through the air-distributor access tube of lower flange, and adopts cutting ferrule to connect and sealing.
Said multiple spot thermopair is the thermopair that contains 3 points for measuring temperature, is K type, Type B, E or S type thermopair; The position of 3 points for measuring temperature lays respectively at three Pt/ γ-Al 2O 3The middle part of beds; The multiple spot thermopair inserts fixed-bed reactor through the thermopair access tube of lower flange, and adopts cutting ferrule to connect and sealing.
The material of said thermal insulation layer is the ceramic fiber of heatproof more than 150 ℃.
CO deep removal method comprises the steps: in a kind of hydrogen-rich gas
The first step, the preheating fixed-bed reactor, superheated vapour is incorporated in the water vapor chuck in the future, the Pt/ γ-Al of heating fixed-bed reactor 2O 3Catalyzer and γ-Al 2O 3Particle is up to temperature-averaging value to 115～125 that three points for measuring temperature of multiple spot thermopair record ℃;
Second step was passed into the hydrogen-rich gas that needs the degree of depth to remove CO in the fixed-bed reactor through the virgin gas inlet pipe on the upper flange, and air is incorporated in the fixed-bed reactor through air-distributor; The ratio of the molar flow of the aerial oxygen of flow control of air and the molar flow of the CO in the hydrogen containing synthesis gas is 1.5～2.8: 1;
The 3rd step; In the water vapor chuck, feed the normal pressure saturated vapor; The temperature-averaging value that three points for measuring temperature of flow control multiple spot thermopair through the adjustment water vapor record is between 115～125 ℃; CO is oxidation removal in fixed-bed reactor, and the gas that removes CO is derived through the product gas fairlead on the lower flange.
The utility model compared with prior art has the following advantages:
1) Pt/ γ-Al in the fixed-bed reactor 2O 3Catalyzer adopts the segmentation filling, has overcome the reaction local superheating, has reduced the generation in channel and dead band;
2) use air-distributor, alleviated reaction local superheating and Pt/ γ-Al 2O 3Problems such as reaction bed temperature skewness;
3) use the water vapour chuck to help heat and get rid of timely, help fixed-bed reactor and maintain a metastable temperature;
4) be reflected at operation under the normal pressure, safe and reliable to operation;
5) fixed-bed reactor is simple in structure, and installation and removal are convenient and easy, and device volume is little, and floor space is few.
Description of drawings
Fig. 1 is the structural representation of CO deep removal device in a kind of hydrogen-rich gas.
Embodiment
Below in conjunction with accompanying drawing and embodiment the utility model is described further; Following embodiment only is schematic rather than determinate; Other staff are under the enlightenment of the utility model; Under the utility model aim and claim, can make multiple similar expression, such conversion all falls within the protection domain of the utility model.
CO deep removal device comprises fixed-bed reactor 22 in a kind of hydrogen-rich gas, Pt/ γ-Al 2O 3Catalyzer 14, γ-Al 2O 3 Particle 15, air-distributor 3, multiple spot thermopair 5, water vapor chuck 11 and thermal insulation layer 12 etc.Fixed-bed reactor 22 comprise reactor shell 10, upper flange 17 and lower flange 18, and reactor shell is fixedly connected through bolt 19 nuts 20 with lower flange with upper flange respectively.Upper flange 17 is equipped with virgin gas inlet pipe 1; Lower flange 18 is equipped with product gas fairlead 2, air-distributor access tube 4 and thermopair access tube 6; Be lined with Graphite pad 21 between upper flange 17, lower flange 18 and the fixed-bed reactor cylindrical shell 10, adopt bolt 19, nut 20 to be fixedly connected.Pt/ γ-Al 2O 3Catalyzer 14 and γ-Al 2O 3Particle 15 layerings fill in fixed-bed reactor 22 cylindrical shells.Air-distributor 3 is installed on the fixed-bed reactor, and the opening 16 of air-distributor 3 is positioned at Pt/ γ-Al 2O 3In catalyzer 14 beds, be used for air being provided to reaction.Multiple spot thermopair 5 is installed on the fixed-bed reactor, and the point for measuring temperature 13 of multiple spot thermopair 5 is positioned at Pt/ γ-Al 2O 3In the beds 14, be used to monitor temperature of reaction.Reactor shell 10 is surrounded by water vapor chuck 11, is used for fixing when bed bioreactor 22 starts to utilize the superheated vapour preheating, and in reaction is carried out, utilizes saturated vapor to remove the heat that reaction produces.Water vapor chuck 11 and fixed-bed reactor 22 upper flange 17, lower flange 18 usefulness thermal insulation layers 12 coat, to reduce the heat lost by radiation of reaction pair surrounding environment; The material of thermal insulation layer is the ceramic fiber of heatproof more than 150 ℃.Air-distributor 3 is the stainless steel tube of a diameter 3～6mm, and the air that is drilled with 3 diameter 0.4mm～1.0mm on the tube wall is introduced the hole, and the position in three holes lays respectively at three Pt/ γ-Al 2O 3The top of beds; Air-distributor 3 inserts fixed-bed reactor through the air-distributor access tube 4 of lower flange, and adopts cutting ferrule to connect and sealing.Pt/ γ-Al in the fixed-bed reactor 2O 3Catalyzer and γ-Al 2O 3The particulate type of feed is: press 0.25V from top to bottom successively 1Pt/ γ-Al 2O 3Catalyzer, 0.5V 2γ-Al 2O 3Particle, 0.5V 1Pt/ γ-Al 2O 3Catalyzer, 0.5V 2γ-Al 2O 3Particle, 0.25V 1Pt/ γ-Al 2O 3Catalyzer loads.
Pt/ γ-Al 2O 3Catalyzer is for being carried on γ-Al 2O 3Pt catalyzer on the particle, the mass loading amount of Pt is 0.5%～2.0%; γ-Al 2O 3The particle diameter of carrier is 2～5mm, and the micropore size in the particle is 5～10nm, and micropore specific area is greater than 270m 2/ g, Pt/ γ-Al 2O 3The CO air speed of catalyzer is 20～100h -1The CO air speed be meant the ratio of volume of CO flow and the catalyzer in the treatable virgin gas; Pt/ γ-Al 2O 3Loaded catalyst
Figure BDA0000088142760000041
Wherein: F is the volumetric flow rate (m of CO in the virgin gas 3/ h), v is the CO air speed (h of catalyzer -1).
γ-Al 2O 3Particle is selected γ-Al with Pt/ for use 2O 3The particle that support of the catalyst is same; γ-Al 2O 3Particle packing amount V 2=0.5V 1～V 1
Preferably, fixed-bed reactor 22 are drum, fixed-bed reactor cavity volume V=V 1+ V 2
Fixed-bed reactor cylinder internal diameter D 1=(15～30) d; Wherein d is γ-Al 2O 3The particle diameter of carrier; The fixed-bed reactor height
Figure BDA0000088142760000051
V is the fixed-bed reactor cavity volume.
Multiple spot thermopair 5 is K type, Type B, E or S type thermopair for containing the thermopair of 3 points for measuring temperature; The position of 3 points for measuring temperature lays respectively at three Pt/ γ-Al 2O 3The middle part of beds; The multiple spot thermopair inserts fixed-bed reactor through the thermopair access tube 6 of lower flange, and adopts cutting ferrule to connect and sealing.
Embodiment
In the hydrogen-rich gas in the CO deep removal device, Pt/ γ-Al 2O 3Catalyzer 14 is for being carried on γ-Al 2O 3Pt catalyzer on the carrier, the mass loading amount of Pt is 1.0%.γ-Al 2O 3Carrier is chemical research institute's buying from Tianjin, and particle diameter d is 2.6mm, and the micro-pore diameter in the particle is 7nm, and micropore specific area is 280m 2/ g, (application number: 201010191716.6), the suitable CO air speed of the prepared catalyzer ratio of volume of CO flow and the catalyzer in the treatable virgin gas () is 30h to the Preparation of catalysts method with reference to Chinese utility model -1Pt/ γ-Al that fixed-bed reactor 22 are equipped with 2O 3Catalyzer 14 volumes are 500ml.
γ-Al 2O 3Particle 15 is chemical research institute's buying from Tianjin, and particle diameter d is 2.6mm, and the aperture in the particle is 7nm, and micropore specific area is 280m 2/ g, loadings is 300ml.
Fixed-bed reactor 22 adopt drum, comprise reactor shell 10, upper flange 17, lower flange 18 3 parts composition, and design temperature is 150 ℃; Pressure is a normal pressure.Reactor shell 10 adopts the processing of SS316 stainless steel, volume 800ml, high 200mm, internal diameter 70mm, wall thickness 3mm.
Air-distributor 3 is the stainless steel tube of a diameter 3mm; The air that is drilled with 3 diameter 0.8mm on the tube wall is introduced hole 16; Three air are introduced adjacent two interval, hole and are respectively 70mm and 115mm, make three air introduce hole 16 during installation and lay respectively at three Pt/ γ-Al 2O 3The top of catalyzer 14 beds.Air-distributor inserts fixed-bed reactor 22 through the air-distributor access tube 4 of lower flange, and adopts cutting ferrule to connect and sealing.
Multiple spot thermopair 5 for containing the thermopair of 3 points for measuring temperature 13, is the K type, adjacent 2 position of 3 points for measuring temperature
Put interval 90mm and 90mm respectively, make three points for measuring temperature lay respectively at three Pt/ γ-Al during installation 2O 3The middle part of catalyzer 14 beds.The multiple spot thermopair inserts fixed-bed reactor 22 through the thermocouple access tube 6 of lower flange, and adopts cutting ferrule to connect and sealing.
Water vapor chuck 11 is peripheral for being surrounded on fixed-bed reactor 22 cylindrical shells, the inside diameter D of said water vapor chuck 2With D outer diameter than reactor shell 1Big 2mm～5mm.The ring-like gas communication passage that the SS316 stainless steel tube that is 80mm by the wall and the another one internal diameter of fixed-bed reactor 22 cylindrical shells is formed; 150 ℃ of design temperatures; Pressure is a normal pressure.The water vapor inlet tube 7 of diameter 8mm is established in the bottom of stainless steel tube, and the water vapor fairlead 8 of diameter 8mm is established on top, establishes the valve 9 of a nominal diameter 8mm on the water vapor inlet tube, is used for drainage water steam jacket 11 issuable water of condensation.
The material of thermal insulation layer 12 is resistant to elevated temperatures ceramic fiber, is coated on the upper flange 17, lower flange 18 of water vapor chuck 11 outer walls and fixed-bed reactor 22, and the thickness of thermal insulation layer is 40mm.
The device setting up procedure is following:
The first step, preheating fixed-bed reactor 22, the superheated vapour (150 ℃, normal pressure) that will come from other technological processs is incorporated in the water vapor chuck 11, the Pt/ γ-Al of heating fixed-bed reactor 22 2O 3Beds and γ-Al 2O 3Particle, the temperature-averaging value that records up to three points for measuring temperature of multiple spot thermopair is between 115～125 ℃;
Second step was passed into the hydrogeneous virgin gas 60L/min that needs the degree of depth to remove CO in the fixed-bed reactor 22, and virgin gas consists of (percent by volume): 0.45%CO, 0.34%CH 4, 16.55%CO 2, 50.25%H 2, N 2Balance is incorporated into air in the fixed-bed reactor 22 through air-distributor 3.The ratio of the molar flow of the aerial oxygen of flow control of air and the molar flow of the CO in the hydrogen containing synthesis gas is 2.5, and flow is 0.675L/min.
The 3rd step fed the normal pressure saturated vapor in water vapor chuck 11, the temperature-averaging value that three points for measuring temperature of the flow control multiple spot thermopair through the adjustment water vapor record is between 115～125 ℃.CO is oxidation removal in fixed-bed reactor, and the gas that removes CO is derived through the product gas fairlead on the lower flange.
Before the reaction beginning, earlier beds being preheating to medial temperature is 120 ℃, and this moment, the beds upper temp was more even, and there is about 10 ℃ the temperature difference in the middle part, and fixed-bed reactor 22 temperature of lower are about 130 ℃.Reaction is carried out 20min rear catalyst bed upper temp and is on average risen 20 ℃, and beds radially maximum temperature difference has only 4 ℃, and radially heat transfer property is fine.The beds middle portion temperature difference further dwindles, and average the rising has only 15 ℃, and radial temperature difference is less than 10 ℃, and the temperature at bed middle part still will be lower than fixed-bed reactor 22 tops.Through detecting, the CO transformation efficiency is 99.9%, and CO concentration is 6ppm.
When reaction finishes, first stop supplies air, stop supplies hydrogen containing synthesis gas then stops the saturated vapor supply at last.After treating that fixed-bed reactor 22 temperature are reduced to room temperature, reduce the water coolant of the water vapor that produces through Yin Wendu in the valve drainage water steam jacket on the water vapor fairlead 8.

Claims (1)

1. CO deep removal device in the hydrogen-rich gas is characterized in that, comprises fixed-bed reactor, Pt/ γ-Al 2O 3Catalyzer, γ-Al 2O 3Particle, air-distributor, multiple spot thermopair, water vapor chuck and thermal insulation layer; Fixed-bed reactor comprise reactor shell, upper flange and lower flange, and reactor shell is connected through bolt with lower flange with upper flange respectively, and upper flange is equipped with the virgin gas inlet pipe; Lower flange is equipped with product gas fairlead; Pt/ γ-Al 2O 3Catalyzer and γ-Al 2O 3Particle layering successively fills in the reactor shell; Air-distributor is installed on the fixed-bed reactor, and the air-distributor opening is arranged at Pt/ γ-Al 2O 3In the beds; The multiple spot thermopair is installed on the fixed-bed reactor, and the point for measuring temperature of multiple spot thermopair is positioned at Pt/ γ-Al 2O 3In the catalyzer; Reactor shell is surrounded by the water vapor chuck, and water vapor chuck bottom is connected with the water vapor inlet tube, and water vapor chuck top is connected with the water vapor fairlead, and the water vapor inlet tube is provided with valve; Lower flange covers with thermal insulation layer on water vapor chuck and the fixed-bed reactor.
CN2011203249893U 2011-08-31 2011-08-31 Deep removing device for CO in hydrogen-rich gas Withdrawn - After Issue CN202246046U (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102424361A (en) * 2011-08-31 2012-04-25 华南理工大学 Deep removal method for CO in hydrogen-rich gas, and apparatus thereof

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102424361A (en) * 2011-08-31 2012-04-25 华南理工大学 Deep removal method for CO in hydrogen-rich gas, and apparatus thereof
CN102424361B (en) * 2011-08-31 2013-05-08 华南理工大学 Deep removal method for CO in hydrogen-rich gas, and apparatus thereof

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