CN102464544A - Method for hydrothermally reducing CO2 or CO into methane by using porous nickel catalyst - Google Patents
Method for hydrothermally reducing CO2 or CO into methane by using porous nickel catalyst Download PDFInfo
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- CN102464544A CN102464544A CN2010105548067A CN201010554806A CN102464544A CN 102464544 A CN102464544 A CN 102464544A CN 2010105548067 A CN2010105548067 A CN 2010105548067A CN 201010554806 A CN201010554806 A CN 201010554806A CN 102464544 A CN102464544 A CN 102464544A
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Abstract
The invention relates to a method for hydrothermally reducing CO2 or CO into methane by using a porous nickel catalyst. The method comprises the following steps of: placing the porous nickel catalyst into a hydrothermal reactor, mixing hydrogen and CO2 or CO according to the molar ratio of 1:(1-10) in the hydrothermal reactor, controlling the temperature of the reactor to 200 to 400 DEG C, and adjusting the pressure of the reactor to 6 to 20MPa and the reaction time to 5 to 180 minutes to obtain the reaction product, namely methane. When the method is compared with the prior art, the highest conversion rate of CO2 and CO is 99 percent, the whole reaction is performed under a hydrothermal condition, the defect that the catalyst is inactivated because carbon is easy to accumulate on the surface of the catalyst in a gas-phase reduction process is overcome, and the used catalyst has the characteristics of high strength, good activity, good thermal stability, excellent low-temperature activity and the like.
Description
Technical field
The present invention relates to field of environment engineering technology, especially relate to a kind of nickel porous catalyzer hydrothermal reduction CO that utilizes
2Method for methane.
Background technology
Since the thirties in 20th century, the human fossil oil that uses has discharged a large amount of CO
2Isothermal chamber gas, CO in the atmosphere
2The problem that concentration continues to increase has caused the great attention of national governments, how to limit CO
2Excessive emissions become the global problem of various countries' Sustainable development.Therefore from CO
2Receive the concern of countries in the world to the transformation technology of chemical, and begin to put among the practical application.Produced at present the technological achievement of different stages of development, under directly or indirectly participating in, utilized CO in other chemical substance
2The technology for preparing multi-functional complex metal hydroxide, long-acting ammonium bicarbonate, terepthaloyl moietie and methane has got into the suitability for industrialized production stage.
CO
2Reduction technique mainly contain: electrochemical reducing, photoreduction method and methanation method.Electrochemical reducing is to utilize applied electromotive force to overcome CO
2/ CO
2 -It is the method for methane that the right high redox potential of electricity makes carbon dioxide reduction.
The photoreduction of carbonic acid gas is through the rayed catalyzer; Formation catalyzer radical or excitation electron are accomplished, and used catalystsystem has the enzyme catalysis system of metal complex to catalyze system, semiconductive suspension body system and mimic photosynthesis effect reducing carbon dioxide.Though the research to these two kinds of method of reducing has obtained certain progress, still exist following problem to need to be resolved hurrily.The one, be that basic colloid catalystsystem and noble metal complexes solution catalyzing system all exists the shortcoming that catalytic efficiency (is not high, quantum yield is low with the semi-conductor, and this type catalyzer cost is high, is unfavorable for industrial application.The 2nd, use the mercuryvapour lamp simulated solar irradiation in the laboratory study mostly, and actual sunshine wants dispersive many than the mercuryvapour lamp radiation, therefore needs reaction unit to possess very big light-receiving area and comes the large-scale aggregating sunshine, certainly will increase cost.
The chemical reduction method of carbonic acid gas is meant that utilizing hydrogen is that the catalyst reduction carbonic acid gas generates methane with Fe, Co, Ni, Ru etc. under gas phase condition.Though the existing at present wide industrial of the vapour phase reduction of carbonic acid gas is used, still there are some problems in this method, is embodied in: (1) CO content>0.3% in virgin gas, (CO+CO
2)>0.7% o'clock causes the reaction bed temperature fluctuation easily, is difficult to accurate temperature controlling.(2) methanation reaction carries out in gas phase, and carbon distribution takes place easily, causes catalyst deactivation, reduces transformation efficiency.
The hydro-thermal reaction method is that nearly twenty or thirty rises over year and becomes one of research focus of applied chemistry rapidly; Hydro-thermal reaction (hydrothermal reaction) is meant under high temperature (150~600 ℃) high pressure; With water is the reaction process of solvent, can be divided into supercritical reaction and subcritical reaction.The critical temperature of water is T
C=374.2 ℃, emergent pressure is P
C=22.1MPa.When the temperature and pressure postcritical of system, be called supercritical water (supercriticalwater, SCW), when the temperature of system is in 150~374 ℃, pressure is in 0.4~22.1MPa, be called near-critical water (near-critical water, NCW).Compare with common liquid water and water vapor, wide variation have taken place in the specific inductivity of near-critical water, solvating ability, viscosity, ionic product.The temperature of water is more near criticality, intermolecular hydrogen bond more a little less than, many gases are (like oxygen, hydrogen, CO, CO
2) solubleness increase, therefore reaction is carried out more easily.Numerous characteristics of near-critical water have determined it that the application of a lot of uniquenesses is arranged in chemical reaction.
Research before this research department shows, under hydrothermal condition, and CO
2Can under the catalysis of common nickel powder, be reduced to formic acid, methane and methyl alcohol, but the selectivity of this reaction pair formic acid is good, has only the methane of trace and methyl alcohol to generate.Adopted nickel porous among the present invention, specific surface area is big, makes methane production improve greatly, and near 100%, selectivity is good.In addition, MOX such as FeO also can be reduced to fe by some biomass (like the former product glycerine of biofuel), so the final source of hydrogen are biomass and water among the present invention.
Summary of the invention
The object of the invention be exactly provide a kind of in order to overcome the defective that above-mentioned prior art exists and be convenient to control reaction temperature, technology is simple, facility investment is few, transformation efficiency is high utilizes nickel porous catalyzer hydrothermal reduction CO
2Or CO is the method for methane.
The object of the invention can be realized through following technical scheme:
A kind of nickel porous catalyzer hydrothermal reduction CO that utilizes
2Or CO is the method for methane, it is characterized in that this method may further comprise the steps: the nickel porous catalyzer is placed hydrothermal reactor, then with hydrogen and CO
2Or CO is 1 in molar ratio: mix in hydrothermal reactor (1~10), and the temperature of controlling reactor is 200~400 ℃, and the pressure of conditioned reaction device is 6~20MPa, and the reaction times is 5~180min, promptly obtains reaction product methane.
Described nickel porous catalyzer is prepared by alumino nickel, and the weight ratio of al and ni is 1 in this alumino nickel: (1~2).
Described nickel porous method for preparing catalyst is following: with the aluminium in the sodium hydroxide solution dissolved particles shape alumino nickel, and the dissolving after-filtration, the gained solid is dried in baking oven, promptly gets the nickel porous catalyzer.
Described hydrogen can be pure hydrogen, also can be Fe, Al, Zn or the Mn metal oxidized hydrogen that reduction produces from water under hydrothermal condition.
Described CO
2Or CO can be pure CO
2Or CO, also can be waste gas from the carbon oxide of Coal Chemical Industry, coal-burning power plant, coke-oven plant, the discharging of steelworks highly energy-consuming factory, can also be the virgin gas of city raw gas and synthetic ammonia.
Described reaction product contains and comprises micro-formic acid.
Compared with prior art; Conversion process of the present invention is carried out under hydrothermal condition, is convenient to control reaction temperature, makes reaction system internal temperature uniform distribution; Overcome reaction bed temperature problem of unstable in the existing technology; In addition, under hydrothermal condition, the deficiency of the easy carbon distribution inactivation of catalyzer also is able to solve.The present invention has also that technology is simple, and facility investment is few, and the characteristics that transformation efficiency is high specifically comprise following advantage:
(1) the present invention is with pure CO
2, the CO in CO or the waste gas
2, CO changes into methane, realized CO
2, the CO recycling purpose, have simultaneously that transformation efficiency height, technology are simple, easy to operate, the advantage of non-secondary pollution, to reducing CO
2Discharging and solve energy shortage and be of great immediate significance and be worth with theoretical;
(2) the nickel porous catalyzer is immersed in aqueous phase among the present invention, is reflected at aqueous phase and carries out, and can avoid the carbon oxides reduction not exclusively, at how empty nickel catalyst surface carbon distribution, reduces activity of such catalysts.In the gas-phase reaction, the carbon simple substance particle that reduction not exclusively produces is adsorbed on catalyst surface and forms carbon distribution, causes catalytic activity to reduce;
(3) the nickel porous catalyzer is immersed in aqueous phase among the present invention, can absorb liberated heat in the catalytic conversion reaction, has guaranteed that the temperature of different sites catalyzer in the reactor drum is uniform and stable.In the gas-phase reaction, the reaction liberated heat has little time diffusion, can make the beds local temperature that bigger fluctuation takes place, and is unfavorable for the control to temperature of reaction.
Description of drawings
Fig. 1 is hydrogen reducing CO, CO under the effect of nickel porous catalyzer
2Virgin gas hydro-thermal reaction product gas compares with the TCD collection of illustrative plates of the preceding virgin gas of reaction;
Fig. 2 continuous production processes schematic flow sheet of the present invention.
Embodiment
Below in conjunction with accompanying drawing and specific embodiment the present invention is elaborated.
The waste gas of coal-burning power plant is CO
2One of main source of discharging.At present, the power department of China is to discharge 2,700,000,000 tons of CO every year
2Follow closely after the U.S., occupy the second in the world.The present invention is applied to power department, can be with the useless CO of its discharging
2Collecting the feeding hydrothermal reactor handles.And the used heat in power station can provide some to react needed temperature, and the energy consumption of hydrothermal treatment consists carbonic acid gas is reduced.
The coal-burning power plant adopts suitable hydrothermal reactor by demand, and its suitability for industrialized production can adopt technical process shown in the drawings.Reaction conditions is controlled as follows: the addition of hydrogen is CO
25 times (in molar ratios), 300 ℃ of temperature of reaction, reaction pressure 10MPa, the ratio of catalyzer addition and virgin gas is 1: 1 (mol ratio), 90 minutes reaction times.
Through this reaction, can be with CO
2Change into methane in a large number; And catalyzer can repeat repeatedly to use, and has practiced thrift the cost that transforms.The obnoxious flavour SO in the waste gas under hydrothermal condition in addition
X, NO
XDeng dissolving in the water, therefore, reduced entering the pollutant component in the gaseous component in the atmosphere; SO soluble in water
X, NO
XTo CO
2Reduction effect can not exert an influence.Recycling through to product liquid not only can generate the new energy, also can significantly reduce greenhouse gas emission.Can be to whole Chinese CO
2The reduction of total amount is made contributions.
Embodiment 2
The coal-burned industrial boiler average operating efficiency is merely 60%~65%, about 2,000,000 tons of the flue dust of annual discharging, and about 7,000,000 tons of sulfurous gas, nearly 1,000,000,000 tons of carbonic acid gas are the second largest coal-smoke pollution sources that is only second to thermal power plant.To this present situation, can in each coal fired plant, dispose the hydro-thermal reaction device, its exhaust gas discharged is collected handle.
Coal-burned industrial boiler adopts suitable hydrothermal reactor by sized, and its suitability for industrialized production can adopt technical process shown in the drawings.Reaction conditions is controlled as follows: the addition of hydrogen is CO
25 times (in molar ratios), 350 ℃ of temperature of reaction, reaction pressure 10MPa, the ratio of catalyzer addition and virgin gas is 1: 1 (mol ratio), 60 minutes reaction times.
Through this reaction, can be with CO
2Change into methane in a large number.And catalyzer can repeat repeatedly to use, and has practiced thrift the cost that transforms.Obnoxious flavour in the waste gas can dissolve in the water under hydrothermal condition in addition, therefore, has reduced entering the pollutant component in the gaseous component in the atmosphere; Simultaneously, to CO
2Reduction effect can not exert an influence.Through recycling, also can regard it as considerable economic return to product liquid.This method not only can generate the new energy, also can significantly reduce greenhouse gas emission.And can solve the CO of coal-burned industrial boiler enterprise
2The difficult present situation of administering of concentrating just can be accomplished CO in each coal firing boiler enterprise
2Utilization transform.And the used heat of coal-burned industrial boiler can provide some to react needed temperature, and the energy consumption of hydrothermal treatment consists carbonic acid gas is reduced.
The carbon dioxide isothermal chamber gas emissions of garbage burning factory constantly increases, and it is calculated that, the annual carbon dioxide that produces of most of incineration plant is also more than thermal power plant.For the contained a large amount of carbonic acid gas of flue gas, can build a hydrothermal treatment consists equipment on the spot, collect institute's exhaust gas discharged, it is carried out hydrothermal conversion as raw material.And burn the great amount of heat energy bring and can provide reaction needed temperature fully, the running cost of hydrothermal treatment consists carbonic acid gas is further reduced.
Garbage burning factory adopts suitable hydrothermal reactor by demand, and its suitability for industrialized production can adopt technical process shown in the drawings.Reaction conditions is controlled as follows: the addition of hydrogen is CO
210 times (in molar ratios), 200 ℃ of temperature of reaction, reaction pressure 20MPa, the ratio of catalyzer addition and virgin gas is 1: 1 (mol ratio), 180 minutes reaction times.
Through this reaction, can be with CO
2Change into methane in a large number.And catalyzer can repeat repeatedly to use, and has practiced thrift the cost that transforms.Obnoxious flavour in the waste gas can dissolve in the water under hydrothermal condition in addition, therefore, has reduced entering the pollutant component in the gaseous component in the atmosphere; Simultaneously, to CO
2Reduction effect can not exert an influence.Through recycling, also can regard it as considerable economic return to product liquid.This method not only can generate the new energy, also can significantly reduce greenhouse gas emission.
Steel industry is to use one of fossil oil four big industry, and the amount of carbon dioxide of its annual discharging is quite big, can reach 600,015,000.Worry from greenhouse gases being caused global warming reduces the emphasis that CO2 emissions have also become the efforts at environmental protection of iron and steel enterprise of developed country.CO with its discharging
2Collect feeding hydro-thermal device and handle conversion, to reach the minimizing of carbonic acid gas.
Iron And Steel Plant adopt suitable hydrothermal reactor by demand, and its suitability for industrialized production can adopt technical process shown in the drawings.Reaction conditions is controlled as follows: the addition of hydrogen is CO
21 times (in molar ratio), 400 ℃ of temperature of reaction, reaction pressure 6MPa, the ratio of catalyzer addition and virgin gas is 1: 1 (mol ratio), 5 minutes reaction times.
Through this reaction, can be with CO
2Change into methane in a large number.And catalyzer can repeat repeatedly to use, and has practiced thrift the cost that transforms.Obnoxious flavour in the waste gas can dissolve in the water under hydrothermal condition in addition, therefore, has reduced entering the pollutant component in the gaseous component in the atmosphere; Simultaneously, to CO
2Reduction effect can not exert an influence.Through recycling, also can regard it as considerable economic return to product liquid.This method not only can generate the new energy, also can significantly reduce greenhouse gas emission.
At present, the major part of required hydrogen is to be made by chemical method in the world, as being made by the methods such as partial oxidation process of Sweet natural gas or naphtha steam conversion method, heavy oil or coal with hydrogen industries such as petroleum refining industry, Iron And Steel Industry, petrochemical complex a large amount of.The common defects that adopts these hydrogen production process is the H of preparation
2Contain a certain amount of CO, CO in the product inevitably
2If the not treated direct supply downstream user of this hydrogen product (being commonly called as " thick hydrogen ") is used, and can cause very big negative impact to subsequent process, therefore the purification processes for thick hydrogen is very necessary.Generally, require through H after the purification processes for most downstream user
2CO in the product
2With the total amount of CO less than 5~10 μ g/g, even lower.The main effect of methanation is with the CO that in the gas mixture subsequent process catalyzer is had toxic action
2Be converted into methane with CO, to reach the purpose of purified hydrogen, lifting product gas calorific value, reduction environmental pollution.
Thick hydrogen, nickel porous catalyzer and water are imported hydrothermal reactor, and reaction conditions is controlled as follows: 250 ℃ of temperature of reaction, and reaction pressure 15MPa, the ratio of catalyzer addition and virgin gas is 1: 1 (mol ratio), 100 minutes reaction times.
Through reaction, about 98% CO in the thick hydrogen
2Be converted into methane with CO, removed the influential impurity of downstream application.And catalyzer can repeat repeatedly to use, and practiced thrift the cost that transforms.
Coal occupies special status in the energy strategy of China, coal gasification is one of main path of production city coal gas.The Chinese government has just proposed the town gas development program and has formulated town gas quality standard: calorific value>=14654kJ/m as far back as 1984
3, CO<10%, O
2<1%, H
2S<20mg/m
3But all contain 20~30% CO in the coal gas that most of coal gasifying process (like gasifications such as the ancient stoves of lurgi gasifier or moral soil) are produced, the content of CO is than higher and CH
4The low requirement that does not meet the town gas use of content.Necessary upgrading makes most of CO and H in the coal gas through the part methanation
2Reaction conversion is methane (the calorific value 35258kJ/m of high caloic
3), CO content is reduced to can makes caloric power of gas bring up to 14654kJ/m below 10% again
3More than, can also more effectively utilize existing gasification and transportation equipment, practice thrift the original oil liquefied gas resource that just lacks very much of China, CO concentration reduces in addition, has also improved the security of using.Therefore it is high to need to seek a kind of efficient, and energy consumption is low, the method for transformation of good economy performance.
City raw gas, nickel porous catalyzer and water are imported hydrothermal reactor, and reaction conditions is controlled as follows: 400 ℃ of temperature of reaction, and reaction pressure 9MPa, the ratio of catalyzer addition and virgin gas is 1: 1 (mol ratio), 80 minutes reaction times.
Through reaction, about 98% CO is converted into methane in the raw gas of city, has reduced the content of CO in the coal gas, has improved the calorific value of coal gas simultaneously.And catalyzer can repeat repeatedly to use, and practiced thrift the cost of methanation.
Embodiment 7
A kind of nickel porous catalyzer hydrothermal reduction CO that utilizes
2Or CO is the method for methane, and this method may further comprise the steps: the nickel porous catalyzer is placed hydrothermal reactor, then with hydrogen and CO
2Or CO in hydrothermal reactor mixes at 1: 5, and the temperature of controlling reactor is 300 ℃, and the pressure of conditioned reaction device is 9MPa; Reaction times is 60min, promptly obtains reaction product methane, in addition; The reduzate of reaction is except methane; In reacted liquid, also have a small amount of formic acid to generate, formic acid is important chemical material, can recycle.
Used nickel porous catalyzer is prepared by alumino nickel; The weight ratio of al and ni is 1: 1 in this alumino nickel, and the preparation method is following: with the aluminium in the sodium hydroxide solution dissolved particles shape alumino nickel, and the dissolving after-filtration; The gained solid is dried in baking oven, promptly gets the nickel porous catalyzer.
Hydrogen reducing CO, CO under the effect of nickel porous catalyzer
2Virgin gas hydro-thermal reaction product gas is more as shown in Figure 1 with the TCD collection of illustrative plates of the preceding virgin gas of reaction.CO in the virgin gas
2Content is 49.63%, and CO content is 50.37%.H in the catalyzed reaction
2With the mol ratio of virgin gas gas be 5: 1, temperature is 300 ℃, pressure is 10MPa, the time is 30min, catalyzer and gas mixture mol ratio are 1: 1.Can draw CO and CO through instrumental analysis
2The transformation efficiency of gas mixture is 98.8%.
Fig. 2 is a continuous production processes schematic flow sheet of the present invention.Technical process of the present invention is following: at first will contain CO, CO
2And the virgin gas 1 of hydrogen (containing metal displacement produce hydrogen) compresses in compressor 2, and the virgin gas after the compression gets into hydrothermal reactor 3, CO, CO under the promotion of pressure reduction
2Under the effect of nickel porous catalyzer, be reduced to methane; Reacted gas mixture flows out on the top of high pressure tank 4, high pressure tank 4 in and water generation initial gross separation; The gas mixture that flows out high pressure tank 4 gets into condensing surface 5 through back pressure valve, cooling in condensing surface 5, and water vapour is cooled; Condense, flow back to water tank 6, get into next circulation in the bottom of condensing surface 5; Remaining gas is the product gas after the methanation, flows out from the top of condensing surface.
Claims (6)
1. one kind is utilized nickel porous catalyzer hydrothermal reduction CO
2Or CO is the method for methane, it is characterized in that this method may further comprise the steps: the nickel porous catalyzer is placed hydrothermal reactor, then with hydrogen and CO
2Or CO is 1 in molar ratio: mix in hydrothermal reactor (1~10), and the temperature of controlling reactor is 200~400 ℃, and the pressure of conditioned reaction device is 6~20MPa, and the reaction times is 5~180min, promptly obtains reaction product methane.
2. a kind of nickel porous catalyzer hydrothermal reduction CO2 or CO of utilizing according to claim 1 is characterized in that for the method for methane described nickel porous catalyzer is prepared by alumino nickel, and the weight ratio of al and ni is 1 in this alumino nickel: (1~2).
3. a kind of method of utilizing nickel porous catalyzer hydrothermal reduction CO2 or CO for methane according to claim 2; It is characterized in that; Described nickel porous method for preparing catalyst is following: with the aluminium in the sodium hydroxide solution dissolved particles shape alumino nickel; The dissolving after-filtration, the gained solid is dried in baking oven, promptly gets the nickel porous catalyzer.
4. a kind of method of utilizing nickel porous catalyzer hydrothermal reduction CO2 or CO for methane according to claim 1; It is characterized in that; Described hydrogen can be pure hydrogen, also can be Fe, Al, Zn or the Mn metal oxidized hydrogen that reduction produces from water under hydrothermal condition.
5. a kind of nickel porous catalyzer hydrothermal reduction CO2 or CO of utilizing according to claim 1 is characterized in that described CO for the method for methane
2Or CO can be pure CO
2Or CO, also can be waste gas from the carbon oxide of Coal Chemical Industry, coal-burning power plant, coke-oven plant, the discharging of steelworks highly energy-consuming factory, can also be the virgin gas of city raw gas and synthetic ammonia.
6. a kind of nickel porous catalyzer hydrothermal reduction CO2 or CO of utilizing according to claim 1 is characterized in that for the method for methane described reaction product contains and comprises micro-formic acid.
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Cited By (5)
Publication number | Priority date | Publication date | Assignee | Title |
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CN103464219A (en) * | 2013-09-03 | 2013-12-25 | 四川蜀泰化工科技有限公司 | Temperature-rising reduction method of methanation catalyst |
CN103755548A (en) * | 2013-12-30 | 2014-04-30 | 上海交通大学 | Method for hydrothermally converting CO2 into formic acid by hydrazine hydrate |
CN104888783A (en) * | 2014-03-03 | 2015-09-09 | 中国石油化工股份有限公司 | Methanation catalyst, preparation method and application thereof |
CN104936893A (en) * | 2012-11-29 | 2015-09-23 | 赛尔斯通股份有限公司 | Reactors and methods for producing solid carbon materials |
CN111495378A (en) * | 2020-05-28 | 2020-08-07 | 中建材蚌埠玻璃工业设计研究院有限公司 | Methanation catalyst and preparation method thereof |
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Cited By (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN104936893A (en) * | 2012-11-29 | 2015-09-23 | 赛尔斯通股份有限公司 | Reactors and methods for producing solid carbon materials |
CN103464219A (en) * | 2013-09-03 | 2013-12-25 | 四川蜀泰化工科技有限公司 | Temperature-rising reduction method of methanation catalyst |
CN103464219B (en) * | 2013-09-03 | 2015-06-17 | 四川蜀泰化工科技有限公司 | Temperature-rising reduction method of methanation catalyst |
CN103755548A (en) * | 2013-12-30 | 2014-04-30 | 上海交通大学 | Method for hydrothermally converting CO2 into formic acid by hydrazine hydrate |
CN104888783A (en) * | 2014-03-03 | 2015-09-09 | 中国石油化工股份有限公司 | Methanation catalyst, preparation method and application thereof |
CN111495378A (en) * | 2020-05-28 | 2020-08-07 | 中建材蚌埠玻璃工业设计研究院有限公司 | Methanation catalyst and preparation method thereof |
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Application publication date: 20120523 |