CN105013519A - Catalyst for ammonia decomposition and application of catalyst - Google Patents
Catalyst for ammonia decomposition and application of catalyst Download PDFInfo
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- CN105013519A CN105013519A CN201410171613.1A CN201410171613A CN105013519A CN 105013519 A CN105013519 A CN 105013519A CN 201410171613 A CN201410171613 A CN 201410171613A CN 105013519 A CN105013519 A CN 105013519A
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/30—Hydrogen technology
- Y02E60/36—Hydrogen production from non-carbon containing sources, e.g. by water electrolysis
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Abstract
The invention relates to a catalyst for ammonia decomposition. The catalyst comprises a nitrogen-containing compound of a main group metal as a carrier and an additive. The catalyst is a novel catalytic material, and has high catalytic activity in ammonia decomposition reaction.
Description
Technical field
The present invention relates to catalyst technology, specifically provide a kind of for the catalyst of ammonolysis craft and the application in ammonia decomposition reaction thereof.
Background technology
Ammonolysis craft is not only widely used in environmental improvement, as process oven gas, fuel gas, petroleum refinery's waste gas and NO
xnH in reduction treatment tail gas
3remove, also for industrial hydrogen productions such as chemical industry, iron and steel, glass, electronics.In recent years; the hydrogen of cheap sustainable production is considered to the matter of utmost importance realizing Proton Exchange Membrane Fuel Cells (PEMFC) scale application, because ammonia has higher hydrogen-storage density, complete production technology and transportation technology, cheap price, decomposes afterwards without CO
xpoison the advantages such as fuel cell, its decomposing hydrogen-production technology is paid close attention to more and more widely.But the hydrogen production efficiency of existing ammonia decomposition catalyzer can't meet the application of on-vehicle fuel, therefore, design and the stable ammonia decomposition catalyzer of synthesizing efficient have important practical significance.
The mid-90, the catalyst based second generation catalyst becoming synthetic ammonia of Ru/AC catalyst replaced Fe, therefore, the catalyst based research being also widely used in ammonia decomposition reaction of Ru.In the ammonia decomposition catalyzer reported at present, K Ru/CNTs MgO has the highest catalytic activity [S.F.Yin, B.Q.Xu, S.J.Wang, C.F.Ng, C.T.Au, Catal.Lett.96 (2004) 113.].But the thermodynamics calculation results shows, under 673K, the equilibrium conversion of ammonolysis craft can reach 99.1%, and this illustrates that the activity of catalyst has further room for promotion.
In sum, the research of ruthenium base ammonia decomposition catalyzer has obtained some progress, but still has further room for promotion.How by carrying out modulation to the Nomenclature Composition and Structure of Complexes of catalyst, thus improving the Activity and stabill of catalyst, needing further research.
Summary of the invention
The present invention, as a kind of novel catalysis material, shows good catalytic activity in ammonia decomposition reaction.
For a catalyst for ammonolysis craft, described catalyst comprises main body and additive; Main body is transition metal, and additive comprises amino-compound or the imino-compound of unitary or binary main group metal.
Body loads is in the surface of additive, and the quality of catalyst body and additive is 1:100 to 30:100 than scope.
Main body is transition metal, and additive is amino-compound or the imino-compound of unitary or binary main group metal, and main body and additive mutual load are in ammonolysis craft common carrier;
The quality of main body and carrier is 1:100 to 30:100 than scope.The atomic ratio scope of main body and additive is 1:1 to 1:10.
Described common carrier is MgO, SiO
2, Al
2o
3, molecular sieve, the one in CNT (CNTs).
The amino-compound of described unitary or binary main group metal or imino-compound are amino-compound or the imino-compound of a kind of in alkali metal or alkaline-earth metal or two kinds;
Alkali metal or alkaline-earth metal comprise in Li, Na, K, Cs, Mg, Ca, Ba element one or more.
Described transition metal is the one in Ru, Mn, Fe, Co, Ni.
Described additive is Mg (NH
2)
2, Ca (NH
2)
2, Ba (NH
2)
2, CaNH, BaNH, Li
2mg (NH)
2, Li
2ca (NH)
2in one.
Described catalyst is that in reaction gas, ammonia concentration is volume content more than 5% for operating condition during ammonolysis craft.
Reaction gas is pure NH
3or NH
3with the gaseous mixture of Ar.
Adopt fixed bed reactors, reaction tube sample bed height is 0.5-2cm, and mass space velocity is 30000-180000h
-1;
Reaction temperature is 200 DEG C to 550 DEG C, and the optimum interval of reaction temperature is 300 DEG C to 350 DEG C.
The present invention relates to two ammonia decomposition catalyzers altogether, and one is that metal Ru load is at Li
2mg (NH)
2on composite catalyst, another is that Ru load is at Ba (NH
2)
2on composite catalyst.In ammonia decomposition reaction, if the reaction gas used is 5%NH
3/ Ar gaseous mixture, the temperature range of catalytic reaction is between 300 DEG C to 350 DEG C, adopts catalyst provided by the invention than the catalytic activity of the catalyst of the Ru load reported in the past on CNT (CNTs) to be significantly improved.
Advantage of the present invention
1. catalyst of the present invention is easily prepared, without the need to the reduction of heat pre-treatment in reaction gas atmosphere transition metal active centres.
2. catalyst preparation time of the present invention is short, and the present invention uses ball-milling method just can prepare catalyst in 3 hours, and the infusion process that catalysis is in the past commonly used takes one day, and even a couple of days could prepare a catalyst.
3. catalyst raw material of the present invention is cheap, and the raw material that catalyst of the present invention uses is RuCl
3, relative to Ru conventional in the past
3(CO)
12cheap a lot.
4. catalyst raw material of the present invention is easy to get, activated centre presoma RuCl used in the present invention
3be commercial reagents, can directly buy.Additive Li used in the present invention
2mg (NH)
2with Ba (NH
2)
2comparatively CNTs is easily prepared.
5. at identical reaction gas composition 5%NH
3under the prerequisite of/Ar, reaction gas flow velocity 30mL/min, activated centre content of metal 5wt%Ru, catalyst sample-loading amount 30mg, catalyst of the present invention in the catalytic activity of low-temperature space apparently higher than the activity of Ru/CNTs catalyst.Specifically see Fig. 1,2,3.
Accompanying drawing explanation
Fig. 1 is that 5wt%Ru CNTs is at 5%NH
3catalytic activity in/Ar gaseous mixture;
Fig. 2 is 5wt%Ru Li
2mg (NH)
2at 5%NH
3catalytic activity in/Ar gaseous mixture;
Fig. 3 is 5wt%Ru Ba (NH
2)
2at 5%NH
3catalytic activity in/Ar gaseous mixture.
Specific embodiment
For further illustrating the present invention, enumerate following specific embodiment, but it does not limit the invention scope that each accessory claim defines.
Comparative example
In argon gas glove box, accurately take ruthenium trichloride (RuCl
3) 41.5mg and commercial CNT (CNTs) 300mg (mass ratio of metal Ru and CNTs is 5:100), be placed in self-control stainless steel jar mill.After closure ball grinding jar, put into planetary ball mill (Fischt PM400), ball milling 3 hours under 150rpm rotating speed.Ball grinder after ball milling is opened in argon gas glove box, and take out sample, this sample is the composite catalyst of metal Ru load on CNTs, is hereafter being abbreviated as 5wt%Ru CNTS for convenience of this catalyst.
In argon gas glove box, accurately take 5wt%Ru CNTs catalyst 30mg, be placed in fixed bed SiO
2in reactor.Sample is at pure NH
3400 DEG C are heated to, by RuCl in atmosphere
3be reduced into metal Ru.And then temperature is adjusted to probe temperature, reaction gas flow speed control is built in 30mL/min, and sample analysis (analytical method use electrical conductivity method) after this temperature stabilization 30min, test result is as shown in Figure 1.
Embodiment 1
In argon gas glove box, accurately take lithium hydride (LiH) 0.44g and amino magnesium (Mg (NH
2)
2) 1.56g (LiH and Mg (NH
2)
2mol ratio be 2:1), be placed in self-control stainless steel jar mill.After closure ball grinding jar, put into planetary ball mill (Fischt PM400), ball milling 12 hours under 200rpm rotating speed.Ball grinder after ball milling is opened in argon gas glove box, and take out sample, found time to be heated to 300 DEG C in enclosed system by this sample, in argon gas glove box, take out sample, this sample is Li
2mg (NH)
2.
In argon gas glove box, accurately take ruthenium trichloride (RuCl
3) 41.5mg and homemade imino group lithium magnesium (Li
2mg (NH)
2) 300mg (metal Ru and Li
2mg (NH)
2mass ratio be 5:100), be placed in self-control stainless steel jar mill.After closure ball grinding jar, put into planetary ball mill (Fischt PM400), ball milling 3 hours under 150rpm rotating speed.Ball grinder after ball milling is opened in argon gas glove box, and take out sample, this sample is metal Ru load at Li
2mg (NH)
2on composite catalyst, be hereafter abbreviated as 5wt%Ru Li for convenience of this catalyst
2mg (NH)
2.
In argon gas glove box, accurately take 5wt%Ru Li
2mg (NH)
2catalyst 30mg, is placed in fixed bed SiO
2in reactor.Sample is (5%NH in reaction atmosphere
3/ Ar gaseous mixture) be heated to temperature required, reaction gas flow speed control is built in 30mL/min, and sample analysis (analytical method use electrical conductivity method) after this temperature stabilization 30min, test result is as shown in Figure 2.The conversion ratio of ammonia increases gradually along with the rising of temperature, and 300 DEG C time, the conversion ratio of ammonia is 8%, and 325 DEG C time, the conversion ratio of ammonia is 30%, and 350 DEG C time, the conversion ratio of ammonia is 53%.Compared with 5wt%Ru CNTs catalyst, ammonia conversion ratio is all significantly improved at the same temperature.Specifically see Fig. 1 and Fig. 2.
Embodiment 2
In argon gas glove box, a block of metal barium is put into self-control stainless steel jar mill, after closure ball grinding jar, add liquefied ammonia, at room temperature leave standstill three months.In glove box, open ball grinder after three months, sample is Powdered.This powdered samples is placed in self-control stainless steel reactor, liquefied ammonia is added after closing, 200 DEG C are heated in enclosed system, keep 12 hours at 200 DEG C, for guaranteeing abundant reaction, repeatedly reaction gas being replaced as ammonia therebetween, after cooling, stainless steel reactor being opened in glove box, take out sample, be Ba (NH
2)
2.
In argon gas glove box, accurately take ruthenium trichloride (RuCl
3) 41.5mg and barium amide (Ba (NH
2)
2) 300mg (metal Ru and Ba (NH
2)
2mass ratio be 5:100), be placed in self-control stainless steel jar mill.After closure ball grinding jar, put into planetary ball mill (Fischt PM400), ball milling 3 hours under 150rpm rotating speed.Ball grinder after ball milling is opened in argon gas glove box, and take out sample, this sample is metal Ru load at Ba (NH
2)
2on composite catalyst, be hereafter abbreviated as 5wt%Ru Ba (NH for convenience of this catalyst
2)
2.
In argon gas glove box, accurately take 5wt%Ru Ba (NH
2)
2catalyst 30mg, is placed in fixed bed SiO
2in reactor.Sample is (5%NH in reaction atmosphere
3/ Ar gaseous mixture) be heated to temperature required, reaction gas flow speed control is built in 30mL/min, and sample analysis (analytical method use electrical conductivity method) after this temperature stabilization 30min, test result is as shown in Figure 3.The conversion ratio of ammonia increases gradually along with the rising of temperature, and 300 DEG C time, the conversion ratio of ammonia is 20%, and 325 DEG C time, the conversion ratio of ammonia is 35%, and 350 DEG C time, the conversion ratio of ammonia is 42%.Compared with 5wt%Ru CNTs catalyst, ammonia conversion ratio is all significantly improved at the same temperature.Specifically see Fig. 1 and Fig. 3.
Embodiment 3
In argon gas glove box, accurately take ruthenium trichloride (RuCl
3) 41.5mg and amino magnesium (Mg (NH
2)
2) 300mg (metal Ru and Mg (NH
2)
2mass ratio be 5:100), be placed in self-control stainless steel jar mill.After closure ball grinding jar, put into planetary ball mill (Fischt PM400), ball milling 3 hours under 150rpm rotating speed.Ball grinder after ball milling is opened in argon gas glove box, and take out sample, this sample is metal Ru load at Mg (NH
2)
2on composite catalyst, be hereafter abbreviated as 5wt%Ru Mg (NH for convenience of this catalyst
2)
2.
In argon gas glove box, accurately take 5wt%Ru Mg (NH
2)
2catalyst 30mg, is placed in fixed bed SiO
2in reactor.Sample is (5%NH in reaction atmosphere
3/ Ar gaseous mixture) be heated to temperature required, reaction gas flow speed control built in 30mL/min, sample analysis (analytical method use electrical conductivity method) after this temperature stabilization 30min.Its catalytic activity is suitable with embodiment 1.
Embodiment 4
In argon gas glove box, accurately take ruthenium trichloride (RuCl
3) 41.5mg and amino calcium (Ca (NH
2)
2) 300mg (metal Ru and Ca (NH
2)
2mass ratio be 5:100), be placed in self-control stainless steel jar mill.After closure ball grinding jar, put into planetary ball mill (Fischt PM400), ball milling 3 hours under 150rpm rotating speed.Ball grinder after ball milling is opened in argon gas glove box, and take out sample, this sample is metal Ru load at Ca (NH
2)
2on composite catalyst, be hereafter abbreviated as 5wt%Ru Ca (NH for convenience of this catalyst
2)
2.
In argon gas glove box, accurately take 5wt%Ru Ca (NH
2)
2catalyst 30mg, is placed in fixed bed SiO
2in reactor.Sample is (5%NH in reaction atmosphere
3/ Ar gaseous mixture) be heated to temperature required, reaction gas flow speed control built in 30mL/min, sample analysis (analytical method use electrical conductivity method) after this temperature stabilization 30min.Its catalytic activity is suitable with embodiment 1.
Embodiment 5
In argon gas glove box, accurately take ruthenium (Ru
3(CO)
12) 52.7mg and commercial magnesia (MgO) 500mg (mass ratio of metal Ru and MgO is 5:100), add THF solvent, ultrasonic process 20min, stir dry for THF volatilization under condition is swept in Ar air-blowing, take out this sample, add barium amide (Ba (NH
2)
2) 41.9mg, (atomic ratio of metal Ru and metal Ba is 1:1), adds THF solvent, stirs dry for THF volatilization, take out this catalyst precursor, at 150 DEG C of 2h reducing metal Ru that find time under condition is swept in Ar air-blowing.This sample is the composite catalyst of metal Ru load on MgO that Ba promotes.Hereafter Ba-Ru/MgO is being abbreviated as convenience of this catalyst.
In Ar gas glove box, accurately take Ba-Ru/MgO catalyst 30mg, be placed in fixed bed SiO2 reactor.Sample is (5%NH in reaction atmosphere
3/ Ar gaseous mixture) be heated to temperature required, reaction gas flow speed control built in 30mL/min, sample analysis (analytical method use electrical conductivity method) after this temperature stabilization 30min.Its catalytic activity is suitable with embodiment 1.
Claims (10)
1. for a catalyst for ammonolysis craft, it is characterized in that: described catalyst comprises main body and additive; Main body is transition metal, and additive comprises amino-compound or the imino-compound of unitary or binary main group metal.
2. catalyst as claimed in claim 1, is characterized in that: body loads is in the surface of additive, and the quality of catalyst body and additive is 1:100 to 30:100 than scope.
3. catalyst as claimed in claim 1, it is characterized in that: main body is transition metal, additive is amino-compound or the imino-compound of unitary or binary main group metal, and main body and additive mutual load are in ammonolysis craft common carrier;
The quality of main body and carrier is 1:100 to 30:100 than scope.The atomic ratio scope of main body and additive is 1:1 to 1:10.
4. catalyst as claimed in claim 3, is characterized in that: described common carrier is MgO, SiO
2, Al
2o
3, molecular sieve, the one in CNT (CNTs).
5. catalyst as claimed in claim 1, is characterized in that: the amino-compound of described unitary or binary main group metal or imino-compound are amino-compound or the imino-compound of a kind of in alkali metal or alkaline-earth metal or two kinds;
Alkali metal or alkaline-earth metal comprise in Li, Na, K, Cs, Mg, Ca, Ba element one or more.
6. catalyst as claimed in claim 1, is characterized in that: described transition metal is the one in Ru, Mn, Fe, Co, Ni.
7. catalyst as claimed in claim 1, is characterized in that:
Described additive is Mg (NH
2)
2, Ca (NH
2)
2, Ba (NH
2)
2, CaNH, BaNH, Li
2mg (NH)
2, Li
2ca (NH)
2in one.
8. the application of catalyst as claimed in claim 1, is characterized in that: operating condition when described catalyst is used for ammonolysis craft is that in reaction gas, ammonia concentration is volume content more than 5%.
9. the application of catalyst as claimed in claim 8, is characterized in that: reaction gas is pure NH
3or NH
3with the gaseous mixture of Ar.
10. the application of catalyst as claimed in claim 1, is characterized in that:
Adopt fixed bed reactors, reaction tube sample bed height is 0.5-2cm, and mass space velocity is 30000-180000h
-1;
Reaction temperature is 200 DEG C to 550 DEG C, and the optimum interval of reaction temperature is 300 DEG C to 350 DEG C.
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|---|---|---|---|
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|---|---|---|---|
| CN201410171613.1A CN105013519B (en) | 2014-04-25 | 2014-04-25 | A kind of catalyst and its application for ammonolysis craft |
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| CN105013519B CN105013519B (en) | 2018-06-29 |
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Cited By (6)
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| CN107206363A (en) * | 2014-12-05 | 2017-09-26 | 国立研究开发法人科学技术振兴机构 | Complex, the manufacture method of complex, ammonia synthesis catalyst and ammonia synthesis |
| CN108080014A (en) * | 2016-11-22 | 2018-05-29 | 中国科学院大连化学物理研究所 | A kind of vanadium base ammonia synthesis and ammonia decomposition catalyzer and application |
| CN108607609A (en) * | 2016-12-10 | 2018-10-02 | 中国科学院大连化学物理研究所 | A kind of cobalt-based ammonia synthesis catalyst and its application |
| CN111229213A (en) * | 2018-11-28 | 2020-06-05 | 中国科学院大连化学物理研究所 | Preparation method of ruthenium-based catalyst |
| CN112973679A (en) * | 2019-12-17 | 2021-06-18 | 中国科学院大连化学物理研究所 | Alkaline earth metal oxide supported ruthenium catalyst, preparation method and application |
| JPWO2021172109A1 (en) * | 2020-02-26 | 2021-09-02 |
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Cited By (14)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107206363A (en) * | 2014-12-05 | 2017-09-26 | 国立研究开发法人科学技术振兴机构 | Complex, the manufacture method of complex, ammonia synthesis catalyst and ammonia synthesis |
| US20170355607A1 (en) * | 2014-12-05 | 2017-12-14 | Japan Science And Technology Agency | Composite, method for producing composite, ammonia synthesis catalyst, and ammonia synthesis method |
| EP3228386A4 (en) * | 2014-12-05 | 2018-08-01 | Japan Science and Technology Agency | Composite body, method for producing composite body, ammonia synthesis catalyst, and ammonia synthesis method |
| US10322940B2 (en) * | 2014-12-05 | 2019-06-18 | Japan Science And Technology Agency | Composite, method for producing composite, ammonia synthesis catalyst, and ammonia synthesis method |
| CN108080014A (en) * | 2016-11-22 | 2018-05-29 | 中国科学院大连化学物理研究所 | A kind of vanadium base ammonia synthesis and ammonia decomposition catalyzer and application |
| CN108607609A (en) * | 2016-12-10 | 2018-10-02 | 中国科学院大连化学物理研究所 | A kind of cobalt-based ammonia synthesis catalyst and its application |
| CN111229213A (en) * | 2018-11-28 | 2020-06-05 | 中国科学院大连化学物理研究所 | Preparation method of ruthenium-based catalyst |
| CN112973679A (en) * | 2019-12-17 | 2021-06-18 | 中国科学院大连化学物理研究所 | Alkaline earth metal oxide supported ruthenium catalyst, preparation method and application |
| CN112973679B (en) * | 2019-12-17 | 2022-04-29 | 中国科学院大连化学物理研究所 | Alkaline earth metal oxide supported ruthenium catalyst, preparation method and application |
| JPWO2021172109A1 (en) * | 2020-02-26 | 2021-09-02 | ||
| WO2021172109A1 (en) * | 2020-02-26 | 2021-09-02 | 国立研究開発法人科学技術振興機構 | Oxynitride-hydride, metal carrier containing oxynitride-hydride, and ammonia synthesis catalyst |
| CN115379896A (en) * | 2020-02-26 | 2022-11-22 | 国立研究开发法人科学技术振兴机构 | Oxynitride-nitrogen hydride, metal carrier containing oxynitride-nitrogen hydride, and catalyst for ammonia synthesis |
| JP7388776B2 (en) | 2020-02-26 | 2023-11-29 | 国立研究開発法人科学技術振興機構 | Catalyst for ammonia synthesis and method for producing ammonia |
| EP4112166A4 (en) * | 2020-02-26 | 2024-04-03 | Japan Science and Technology Agency | Oxynitride-hydride, metal carrier containing oxynitride-hydride, and ammonia synthesis catalyst |
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| CN105013519B (en) | 2018-06-29 |
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