CN100439238C - Production of hydrogen by catalyzed decomposing magnesium and its mixture doped with other metals - Google Patents

Production of hydrogen by catalyzed decomposing magnesium and its mixture doped with other metals Download PDF

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CN100439238C
CN100439238C CNB2005100325470A CN200510032547A CN100439238C CN 100439238 C CN100439238 C CN 100439238C CN B2005100325470 A CNB2005100325470 A CN B2005100325470A CN 200510032547 A CN200510032547 A CN 200510032547A CN 100439238 C CN100439238 C CN 100439238C
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hydrogen
reaction
carbon
metal catalyst
methane
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CNB2005100325470A
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CN1982204A (en
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王科
刘振
李文生
周小平
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微宏科技(湖州)有限公司
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J21/00Catalysts comprising the elements, oxides, or hydroxides of magnesium, boron, aluminium, carbon, silicon, titanium, zirconium, or hafnium
    • B01J21/10Magnesium; Oxides or hydroxides thereof
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B3/00Hydrogen; Gaseous mixtures containing hydrogen; Separation of hydrogen from mixtures containing it; Purification of hydrogen
    • C01B3/02Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen
    • C01B3/22Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen by decomposition of gaseous or liquid organic compounds
    • C01B3/24Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen by decomposition of gaseous or liquid organic compounds of hydrocarbons
    • C01B3/26Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen by decomposition of gaseous or liquid organic compounds of hydrocarbons using catalysts

Abstract

A method for producing hydrogen and carbon with mixture of metal magnesium and other metals as catalyst by catalytic decomposition is carried out by reacting at 0.01-10Pa and 200-1500degree and separating catalyst from products. It can re-used and not contain CO and CO2 impurities.

Description

The mixture through catalytic of MAGNESIUM METAL and other metals that mix thereof decomposes hydrocarbon polymer hydrogen manufacturing

Technical field

The present invention relates to a kind of method of using catalyzer from hydrocarbon polymer hydrogen manufacturing, especially relate to a kind of method of using the hydrogen manufacturing of metal catalyst catalyzed decomposing thing.

Background technology

As efficient, clean secondary energy, hydrogen is widely used in space flight, oil refining, metallurgy and the Minute Organic Synthesis industry; In ammonia synthesizing industry, hydrogen is one of important synthesis material.In recent years, along with the rise of fuel cell, caused extensive interest as the preparation of the high-purity hydrogen of battery fuel.At present, industrial hydrogen manufacturing has a variety of flow processs, wherein the natural gas hydrogen preparation method is cheap and easy to get because of raw material, technical process is simple relatively, become main hydrogen production process, specifically comprise methods such as methane steam reforming method, partial oxidation process, CO 2 reformation method and direct breakdown method, wherein most widely used with steam reformation again.

In the steam reforming flow process of methane, methane under High Temperature High Pressure with steam reaction, generate synthetic gas, i.e. carbon monoxide and hydrogen, the carbon monoxide of generation continues and steam reaction, generates carbonic acid gas and hydrogen.By separating and purification procedures, obtain hydrogen.At present, a lot of patents and bibliographical information are arranged about this Study on process flow progress, for example U.S. Pat 5496859, and US6312658 is the patent of relevant hydrogen manufacturing aspect with US6328945.Keiichi Tomishige[Energy ﹠amp; Fuels2001,15,571-574] reported that Ni reacts hydrogen manufacturing with methane and water vapour on aluminium sesquioxide, generate carbon monoxide and hydrogen at 800~1100 ℃.Giuseppe Barbieri[Ind.Eng.Chem.Res.2001,40,2017-2026] reported and on palladium film reactor, carried out steam reformation, and the model of reaction has been carried out theoretical analysis.

In the partial oxidation flow process of methane, methane and oxygen reaction generate carbon compound and hydrogen.It is 600~900 ℃ that U.S. Pat 5149516 and US5447705 have introduced in temperature, and pressure is successfully to have realized this reaction under the 0.1MPa on uhligite.U.S. Pat 4973486 has reported with hydrogen bromide that as catalyzer methane and oxygen generate carbon monoxide, hydrogen, ethene and acetylene 850 ℃ of reactions, and after reaction finished, the amount of hydrogen bromide remained unchanged.Korada Supat[Ind.Eng.Chem.Res.2003,42,1654-1661] use the ring current energy supply, partial oxidation reaction and steam reforming reaction are taken place simultaneously, and obtain good result.

In the CO 2 reformation flow process of methane, carbonic acid gas and methane reaction generate carbon monoxide and hydrogen.Usually this reforming reaction that does not have water vapor to participate in is called dry gas and reforms.U.S. Pat 5753143 has been reported on the Si-Al molecular sieve catalyzer of rhodium load, methane and carbonic acid gas generate synthetic gas 500 ℃, 1 normal atmosphere reaction, methane conversion is between 10%~34%, and the ratio that hydrogen and carbon monoxide are the highest in the product reaches 0.92: 1.Another piece U.S. Pat 6355219 is carried out the CO 2 reformation of methane on nickel-alumina catalyst, the peak rate of conversion of methane can reach 70%, and life of catalyst was above 30 hours.Mahesh V.lyer[Ind.Eng.Chem.Res.2003,42,2712-2721] carbide [Co that reported at cobalt tungsten 6W 6C] on, the reaction under 500~600 ℃ temperature and 5 normal atmosphere of methane and carbonic acid gas generates synthetic gas.TatsuakiYamaguchi[Energy﹠amp; Fuels 2001,15,571-574] reported on the cylindrical reactor of aluminum, be catalyzer with the gac of nickel-loaded, carry out CO 2 reforming reaction, methane conversion surpasses 65%.

But all these are produced by methane in the flow process of hydrogen, and product unavoidably contains the hydrocarbon of contaminate environment, particularly carbon monoxide, though through separating, be difficult to remove clean.And carbon monoxide concentration can not surpass 20ppm in the needed high-purity hydrogen of fuel cell, therefore, the hydrogen that methane reforming makes can not be directly used in fuel cell, must remove carbon monoxide through secondary separation, and carbon monoxide is reduced to 20ppm level level, need complicated step and lot of energy.

In addition, also have some other flow process to produce hydrogen.U.S. Pat 4064740 discloses a kind of method of direct heat splitting water, and this method raw material is simple, directly water of decomposition at high temperature.But, the high temperature of reaction needed more than 2000 ℃, this needs huge energy consumption.It is catalyzer that United States Patent (USP) U84024230 has introduced with Z 250 and chlorine, through a catalytic cycle, water is finally resolved into hydrogen and oxygen, and this method has successfully reduced the temperature of water decomposition, but the reactor that needs the resistance to chlorine corrosion to involve great expense.U.S. Pat 6017425, US6077497, US6300274 and US6297190 disclose a kind of method, this method is a catalyzer with the zinc sulphide or the Cadmium Sulfide of metals such as load iron nickel ruthenium platinum, water of decomposition comes hydrogen manufacturing under ultraviolet lighting or visible light condition, reaction can be carried out at normal temperatures, but conversion rate is very low.U.S. Pat 5958297 and US6673270 are catalyzer with the metal such as the nickel cobalt of the 8th family, catalytic hydrocarbon such as kerosene and oxygen reaction are produced hydrogen, it is wider that this method can be handled hydrocarbon context, different hydrocarbons all can be reacted hydrogen manufacturing compound from carbon one compound methane to carbon ten such as the naphthalene, but there is the product complexity, selectivity is lower, the drawback of separation difficulty.U.S. Pat 6059995 and US5837217 have then introduced dme or methyl alcohol is that raw material carries out steam reforming, produces hydrogen.Because cost of material is more expensive relatively, not remarkable from economic benefit, in addition, this method needs oxidized portion hydrogen that carry out of heat for reforming reaction is provided, and the efficient of hydrogen manufacturing is reduced.U.S. Pat 4372833 and US4507185 then use visible light decompose formic acid salt and water to produce hydrogen, but are subjected to the restriction of raw material sources equally, and this method application prospect is little.

In recent years, alkane particularly methane decomposition hydrogen manufacturing caused extensive interest.Because do not have the participation of oxygen element in the whole flow process, the product of reaction does not contain hydrocarbon, the hydrogen after flash liberation can be directly used in fuel cell, therefore greatly reduces production cost, has expanded gas chemical industry's Application Areas.For example, U.S. Pat 6315977 utilizes hydrocarbons decompose to produce hydrogen, and U.S. Pat 5028307 has then been introduced usually to decompose with organic fibre and produced hydrogen.It is that catalyzer is at 400~700 ℃ of methane decompositions that the Lv Yuan of the Dalian Chemistry and Physics Institute has introduced in Chinese patent CN1179878 with Fe, Co, Ni; It is the hydrogen manufacturing of thermal source cracking methane that people such as the Cao Xuewu of Shanghai Communications University have adopted sodium-cooled fast reactor at patent CN1193927.Aspect document, people such as Huffman [Energy﹠amp; Fuels 2001,15,1528-1534] reported that (M=Pd, Mo Ni) are catalyzer, and methane decomposes generation hydrogen and carbon at 400~1200 ℃ with bimetal system Fe-M; Mohamed[Ind.Eng.Chem.Res.2004,43,4864-4870] employing loaded catalyst Ni/TiO 2Methane decomposition is also succeedd.R.Terry[J.Phys.Chem.B2004,108,20273-20277] etc. reported that methane is to decompose on 665~725 ℃ of three component catalyst Ni-Cu-MgO to have obtained hydrogen and nano level carbon dust in temperature.

But in these traditional reaction process, along with the decomposition of alkane, generating more and more many carbon can not remove at any time, and residual buildup is at catalyst surface, and the active centre of covering catalyst makes it isolated with reactant gradually, cause the catalytic activity of catalyzer to decline to a great extent, finally cause inactivation.Therefore, the life of catalyst of these flow processs is generally shorter, generally is no more than 10 hours, even has only several minutes.In addition, because the carbon supported catalyst surface that generates is very firm, easy-clear brings great trouble for the regeneration and the repeated use of catalyzer.

Summary of the invention

The present invention adopts MAGNESIUM METAL or magnesium and Ca, Li, Na, Al, K, Ti, V, Cr, Mn, Fe, Co, Ni, Cu, Ge, Rb, Sr, Y, Zr, Nb, Mo, Ru, Rh, Pd, Ag, Cd, In, Sn, Sb, Cs, Ba, Tl, Pb, Bi, La, Ce and Sm, and wherein one or more mixture is as catalyzer, and directly the catalyzed decomposing thing is produced hydrogen and carbon.Described hydrocarbon polymer can be wherein one or several a mixture of alkane, alkene, alkynes, isocyclic compound, aromatics, waste or used plastics, waste old and pitch.The temperature of reaction of this catalyzed reaction is between 200 to 1500 ℃, and temperature of reaction is between 300 to 1100 ℃ preferably, and best temperature of reaction is between 600 to 900 ℃; Working pressure is between 0.01 to 10 normal atmosphere, and working pressure is between 0.02 to 8 normal atmosphere preferably, and best working pressure is between 0.1 to 5 normal atmosphere; Used reactor is a kind of bubbling reactor.

Because directly adopting the mixture of MAGNESIUM METAL and other metals that mix thereof is catalyzer, can directly add in the reactor, thereby significantly reduce pretreated operation, has saved expense and time.The condition range of choice of reaction is wide, especially obtains higher yield under gentle relatively condition.For example when adopting methane as raw material, react maximum per pass conversion and can reach 35%, the product of reaction is hydrogen and powdered carbon.Characteristic of the present invention is the catalyzer of life of catalyst much larger than report, can reach more than 120 hours.In addition, after reaction finished, catalyzer separated automatically with product, be convenient to very much separate, and the catalyzer that reclaims was reusable, and activity does not reduce.

Description of drawings

Fig. 1 is a hydrocarbon oxidation catalyst decomposer synoptic diagram

Fig. 2 is a hydrocarbon polymer two-stage cartalytic decomposition effect device synoptic diagram

Embodiment

Embodiment 1~5 takes by weighing a certain amount of metal catalyst and promotor, in the reactor 14 of the stainless steel inner core 15 of being furnished with end sealing of packing into (as shown in Figure 1), makes inlet pipe 7, thermopair 11, catalyzer keep excellent contact, and good seal.Then reactor is put into process furnace 19, adjusted the height of reactor, to guarantee that heat transfer evenly.Connect methane steel cylinder 1 and reaction pipeline, jam-pack soft rubber ball 9, device leak detection.Adjust reducing valve 2 through charging, make air pressure reach 0.1MPa, open control valve under meter 3 and display instrument 4 dominant discharge 5ml/min.Ventilated 20 minutes, and guaranteed to wash down other gases in the reactor.Heating unit comprises temperature controller 5, thermopair 11, heater block 12,13, lagging material 17,18 etc., open temperature controller 5, temperature is risen to 700 ℃, treat after the temperature-stable, sampling spot 8 samplings on sampling spot 6 and escape pipe 10 are analyzed with the gas phase chromatograph mass spectrometer.After the reaction, close temperature controller, stop heating.Continue ventilating methane until the temperature cool to room temperature, stop ventilation.In stainless steel, overlap 15 taking-up reactors 14, pour out the carbon dust of generation, weigh.Changing different Primary Catalysts and promotor reacts.Reaction result is as shown in table 1.

Table 1 is methane conversion under different catalysts

Embodiment 6~9 reaction units, working method, reaction pressure and flow are identical with embodiment 1, take by weighing 4 gram catalyzer, change temperature of reaction and react at 300 ℃, 400 ℃, 500 ℃, 600 ℃, and reaction result is as shown in table 2.

Table 2 is methane conversion under differing temps

Embodiment 10 takes by weighing 4 gram MAGNESIUM METAL catalyzer, and reaction unit, working method, reaction pressure and flow are identical with embodiment 1, and temperature of reaction is 680 ℃, reacts 20 hours post analysis results and shows that methane conversion still is stabilized in 22.0%.

Embodiment 11 takes by weighing 4 gram MAGNESIUM METAL catalyzer, and reaction unit, working method and flow are identical with embodiment 1, and temperature of reaction is 700 ℃, and reaction is carried out 20 hours post analysis results and shown that methane conversion still is stabilized in 23.0%.

Embodiment 12 takes by weighing 4 gram MAGNESIUM METAL catalyzer, and reaction unit, working method and flow are identical with embodiment 1, and temperature of reaction is 720 ℃, and reaction is carried out 25 hours post analysis results and shown that methane conversion still is stabilized in 27%.

Embodiment 13 takes by weighing 4 gram MAGNESIUM METAL catalyzer, and reaction unit, working method and flow are identical with embodiment 1, and temperature of reaction is 740 ℃, and reaction is carried out 25 hours post analysis results and shown that methane conversion still is stabilized in 32.0%.

Embodiment 14 takes by weighing 4 gram MAGNESIUM METAL catalyzer, and reaction unit, working method and flow are identical with embodiment 1, and temperature of reaction is 760 ℃, and reaction is carried out 20 hours post analysis results and shown that methane conversion still is stabilized in 31%.

Embodiment 15 takes by weighing 4 gram MAGNESIUM METAL catalyzer, and reaction unit, working method and flow are identical with embodiment 1, and temperature of reaction is 700 ℃, and reaction is carried out 15 hours post analysis results and shown that ethane conversion still is stabilized in 62.0%.

Embodiment 16 takes by weighing 4 gram MAGNESIUM METAL catalyzer, and reaction unit, working method, reaction pressure and flow are identical with embodiment 1, and temperature of reaction is 700 ℃.Conversion of propane is stabilized in 90.0%, and hydrogen selective 80.0%, by product are methane.

Embodiment 17 takes by weighing 2 gram MAGNESIUM METAL catalyzer and 1 gram pitch, for making the pitch complete decomposition, what adopt is two-stage reactor (as shown in Figure 2, each reacting appliance volume description is seen embodiment 1), connects second stage reactor and further carry out decomposition reaction behind first step reactor.Connect the reaction pipeline, the device leak detection.Logical rare gas element 20 minutes guarantees to wash down other gases in the reactor.Open temperature controlling system, preceding stage reactor is warming up to 700 ℃ with the speed program of 1 ℃ of per minute, constantly carries out quantitative analysis in analytical port 1,2 samplings and with gas chromatograph in the temperature-rise period, pitch decomposes fully, hydrogen selective is more than 80.0%, and by product is a methane.

Embodiment 18 takes by weighing 2 gram MAGNESIUM METAL catalyzer and 1 gram plastics rice, packs into and is furnished with in the reactor of stainless steel inner core, makes inlet pipe, thermopair, catalyzer keep excellent contact, and good seal.Then reactor, heating muff are put into process furnace, adjust the height of reactor, to guarantee that heat transfer evenly.For making plastics rice complete decomposition, employing be two-stage reactor (as shown in Figure 2), behind first step reactor, connect second stage reactor and further carry out decomposition reaction.Connect the reaction pipeline, the device leak detection.Logical rare gas element 20 minutes guarantees to wash down other gases in the reactor.Open temperature controlling system, preceding stage reactor is warming up to 700 ℃ with the speed program of 1 ℃ of per minute, constantly carries out quantitative analysis in analytical port 1,2 samplings and with gas chromatograph in the temperature-rise period, plastics rice decomposes fully, hydrogen selective is more than 90.0%, and by product is a methane.

Embodiment 19 takes by weighing the rubber of 2 gram MAGNESIUM METAL catalyzer and 1 gram, packs into and is furnished with in the reactor of stainless steel inner core, makes into inlet pipe, thermopair, catalyzer maintenance excellent contact, and good seal.Then reactor, heating muff are put into process furnace, adjust the height of reactor, to guarantee that heat transfer evenly.For making the rubber complete decomposition, employing be two-stage reactor (as shown in Figure 2), behind first step reactor, connect second stage reactor and further carry out decomposition reaction.Connect the reaction pipeline, the device leak detection.Logical rare gas element 20 minutes guarantees to wash down other gases in the reactor.Open temperature controlling system, preceding stage reactor is warming up to 700 ℃ with the speed program of 1 ℃ of per minute, constantly carries out quantitative analysis in analytical port 1,2 samplings and with gas chromatograph in the temperature-rise period, rubber decomposes fully, hydrogen selective is more than 90.0%, and by product is a methane.

Claims (11)

1. a method of using thing hydrogen manufacturing of metal catalyst catalyzed decomposing and carbon is characterized in that described metal catalyst is the mixture of MAGNESIUM METAL or magnesium and other metals.
2. the method for use metal catalyst catalyzed decomposing according to claim 1 thing hydrogen manufacturing and carbon is characterized in that described hydrocarbon polymer is wherein one or several a mixture of alkane, alkene, alkynes, isocyclic compound, aromatics, waste or used plastics, waste old and pitch.
3. the method for use metal catalyst catalyzed decomposing according to claim 1 thing hydrogen manufacturing and carbon is characterized in that described other metals are wherein one or more mixtures of Ca, Li, Na, Al, K, Ti, V, Cr, Mn, Fe, Co, Ni, Cu, Ge, Rb, Sr, Y, Zr, Nb, Mo, Ru, Rh, Pd, Ag, Cd, In, Sn, Sb, Cs, Ba, Tl, Pb, Bi, La, Ce and Sm.
4. the method for use metal catalyst catalyzed decomposing according to claim 3 thing hydrogen manufacturing and carbon is characterized in that described other metals are Rh.
5. according to the method for thing hydrogen manufacturing of arbitrary described use metal catalyst catalyzed decomposing and carbon in the claim 1~4, the temperature of reaction that it is characterized in that this method is between 200 to 1500 ℃.
6. the method for use metal catalyst catalyzed decomposing according to claim 5 thing hydrogen manufacturing and carbon, the temperature of reaction that it is characterized in that this method are between 300 to 1100 ℃.
7. the method for use metal catalyst catalyzed decomposing according to claim 6 thing hydrogen manufacturing and carbon, the temperature of reaction that it is characterized in that this method are between 600 to 900 ℃.
8. according to the method for thing hydrogen manufacturing of arbitrary described use metal catalyst catalyzed decomposing and carbon in the claim 1~4, the working pressure that it is characterized in that this method is between 0.01 to 10 normal atmosphere.
9. the method for use metal catalyst catalyzed decomposing according to claim 8 thing hydrogen manufacturing and carbon, the working pressure that it is characterized in that this method are between 0.02 to 8 normal atmosphere.
10. the method for use metal catalyst catalyzed decomposing according to claim 9 thing hydrogen manufacturing and carbon, the working pressure that it is characterized in that this method are between 0.1 to 5 normal atmosphere.
11., it is characterized in that the employed reactor of this method is a kind of bubbling reactor according to the method for thing hydrogen manufacturing of arbitrary described use metal catalyst catalyzed decomposing and carbon in the claim 1~4.
CNB2005100325470A 2005-12-14 2005-12-14 Production of hydrogen by catalyzed decomposing magnesium and its mixture doped with other metals CN100439238C (en)

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PCT/CN2006/003390 WO2007068202A1 (en) 2005-12-14 2006-12-13 Production of hydrogen by pyrolysis of hydrocarbon under catalysts of metal magnesium and metal magnesium doped with other metals

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Cited By (2)

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WO2017136205A1 (en) * 2016-02-01 2017-08-10 West Virginia University Research Corporation Methods for production of carbon and hydrogen from natural gas and other hydrocarbons
US10494264B2 (en) 2013-03-15 2019-12-03 West Virginia University Research Corporation Process for pure carbon production, compositions, and methods thereof

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CN106556637A (en) * 2016-11-11 2017-04-05 上海理工大学 A kind of photoelectrocatalysis reaction experiment device

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CN1533981A (en) * 2000-06-16 2004-10-06 打矢恒温器株式会社 Oxygen supply device

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CN1533981A (en) * 2000-06-16 2004-10-06 打矢恒温器株式会社 Oxygen supply device
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Cited By (4)

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Publication number Priority date Publication date Assignee Title
US10494264B2 (en) 2013-03-15 2019-12-03 West Virginia University Research Corporation Process for pure carbon production, compositions, and methods thereof
US10696555B2 (en) 2013-03-15 2020-06-30 West Virginia University Research Corporation Process for pure carbon production
WO2017136205A1 (en) * 2016-02-01 2017-08-10 West Virginia University Research Corporation Methods for production of carbon and hydrogen from natural gas and other hydrocarbons
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