CN109954510A - A kind of chromium base ammonia synthesis and ammonia decomposition catalyzer and application - Google Patents
A kind of chromium base ammonia synthesis and ammonia decomposition catalyzer and application Download PDFInfo
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- CN109954510A CN109954510A CN201711336922.XA CN201711336922A CN109954510A CN 109954510 A CN109954510 A CN 109954510A CN 201711336922 A CN201711336922 A CN 201711336922A CN 109954510 A CN109954510 A CN 109954510A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/24—Nitrogen compounds
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B3/00—Hydrogen; Gaseous mixtures containing hydrogen; Separation of hydrogen from mixtures containing it; Purification of hydrogen
- C01B3/02—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen
- C01B3/04—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen by decomposition of inorganic compounds, e.g. ammonia
- C01B3/047—Decomposition of ammonia
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01C—AMMONIA; CYANOGEN; COMPOUNDS THEREOF
- C01C1/00—Ammonia; Compounds thereof
- C01C1/02—Preparation, purification or separation of ammonia
- C01C1/04—Preparation of ammonia by synthesis in the gas phase
- C01C1/0405—Preparation of ammonia by synthesis in the gas phase from N2 and H2 in presence of a catalyst
- C01C1/0411—Preparation of ammonia by synthesis in the gas phase from N2 and H2 in presence of a catalyst characterised by the catalyst
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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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- 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
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/52—Improvements relating to the production of bulk chemicals using catalysts, e.g. selective catalysts
Abstract
The present invention relates to a kind of for ammonia synthesis and the chromium-based catalysts of ammonolysis craft, the catalyst include chromium and relevant carrier and additive.The present invention shows good catalytic activity as a kind of novel catalysis material in ammonia synthesis and ammonia decomposition reaction.
Description
Technical field
The present invention relates to catalyst technology, specifically provide a kind of chromium-based catalysts for ammonia synthesis and ammonolysis craft and its
Application in ammonia synthesis and ammonia decomposition reaction.
Background technique
Ammonia is the base stock for producing the important chemical products such as chemical fertilizer, nitric acid, plastics, medicine, while being also that one kind has
The hydrogen source carrier of potential application foreground, thus the synthesis and decomposition of ammonia industrially have a very important significance.Nitrogen and hydrogen
Catalyzed conversion of the gas on transition metal is the major way of industry synthetic ammonia, and the industrial flow mainly used at present is Haber-
Bosch process.The severe reaction conditions (ferrum-based catalyst: 350-525 DEG C, 100-300atm) of the process ammonia synthesis, to equipment
It is required that it is very high, thus energy consumption is very high, the energy consumed every year is the 1% of the annual total energy consumption in the world.It is industrial at present wide
The general catalyst for ammonia synthesis and ammonolysis craft is respectively iron-based, ruthenium-based catalyst and nickel-base catalyst etc. are transition metal-catalyzed
Agent, however in decades, the efficiency for synthesizing ammonia is not significantly improved and improves, and reaction condition still needs high temperature height
Pressure.And for ammonia decomposition reaction, nickel-base catalyst is although cheap but active lower, thus develops new type low temperature low-voltage high-efficiency
Ammonia synthesis and ammonia decomposition catalyzer system be still current highly important research topic.It jumps out iron-based and ruthenium-based catalyst
Limitation, uses for reference the catalyst of existing basic theory and technical research other components, is to develop ammonia synthesis of new generation and ammonolysis craft
The available strategy of catalyst.
About non-ferric (ruthenium) base catalyst of ammonia synthesis and decomposition, the especially research in terms of chromium-based catalysts is considerably less.
The result of study of early stage show the ammonia synthesis of chromium-based catalysts and degrading activity it is lower [A.Mittasch, Adv.Catal.,
1950,2,81-104；C.R.Lotz, F.Sebba, Trans.Faraday Soc., 1957,53,1246-1252.], thus it is long
The concern of researcher is not caused since phase.2009, Zhu etc. reported chromium oxide (Cr2O3) in higher temperature (> 500
DEG C), certain ammonolysis craft catalytic activity can be shown, such as in 600 DEG C and WHSV=60000mlNH3gcat -1h-1Reaction item
Under part, ammonia conversion ratio can reach 43.4% [L.Li, Z.H.Zhu, S.B.Wang, X.D.Yao, Z.F.Yan,
J.Mol.Catal.A,2009,304,71-76.]。
In conclusion the research in terms of the ammonia synthesis of chromium base and ammonia decomposition catalyzer is also seldom, people are to its ammonolysis craft
It is also very unintelligible with the mechanism of action of synthesis.How by the Nomenclature Composition and Structure of Complexes progress modulation to catalyst, to improve catalysis
The Activity and stabill of agent, and catalyst cost is reduced, it needs to be further studied.
Summary of the invention
Alkali (soil) metal amide, such as lithium amide, potassamide, amino magnesium are a kind of with important application prospect
Hydrogen storage material., when studying the property of such material, discovery after being added transition metal chromium thereto, heat point for we
Significant change has occurred in solution property.For example, to lithium amide (LiNH2) in be added Cr after, when reaction temperature be higher than 200 degree when,
A large amount of nitrogen and hydrogen are detected in gaseous product, as shown in Figure 1.Due at 500 degree hereinafter, LiNH2Decomposition product
Mainly ammonia so the presence of Cr may change the decomposition path-ways of lithium amide, and is possible to urging as ammonia decomposition reaction
Agent.
To prove this imagination, we have synthesized CrN/LiNH2Composite catalyst has simultaneously investigated its ammonolysis craft catalytic performance.Such as
Shown in Fig. 2, nitrogen and hydrogen are produced at 300 degree, and ammonia conversion ratio gradually increases as the temperature rises.
Further study showed that the Cr nitrogenous chemical combination with the major elements such as Na, K, Cs, Be, Mg, Ca, Sr, Ba, Al respectively
Object also has similar catalytic activity.Nitrogenous or/and hydrogen-containing compound includes unitary or multicomponent nitride, amino-compound, Asia
The mixture etc. of amino-compound, nitrogen oxides, nitride-hydride and hydride or in which 2 kinds or more.It is formed substantially
For MxNyH3y-nx, wherein M is one of I above-mentioned A, II A, III A race element or several two or more, and n is the chemical valence state of M,
X=1~4, y=0~3.
The nitrogenous or/and hydrogen-containing compound of these major elements can be carried on certain carrier.Carrier can be main group member
The oxide such as Li of element2O、Na2O、K2O、MgO、CaO、SrO、BaO、SiO2、Al2O3Deng or its nitride such as BN, Si3N4、
Mg3N2、Ca3N2, the combination of one or more of AlN and molecular sieve, carbon material, metal-organic framework materials (MOFs).Catalyst
Mass ratio with carrier can be from 1000:1 to 1:500；It can be from 200:1 to 1:100 after optimization.
Other metal nitrides can be added into Cr element.The metal of metal nitride can for IV B, V B, VI B, VII B or
One or more of VIII B race element.The mass ratio of catalyst and metal nitride can be from 1000:1 to 1:500；Optimization
After can be from 200:1 to 1:100.
Metal alloy can be added into Cr element.Metal alloy are as follows: IV B, V B, VI B, VII B or VIII B race element and C, B or
The two-spot or multicomponent alloy formed between N.The mass ratio of catalyst and metal alloy can be from 1000:1 to 1:500；It can after optimization
From 200:1 to 1:100.
In ammonia decomposition reaction, ideal effect: CrN/LiNH can be obtained using catalyst provided by the invention2
(molar ratio 1:0.8) catalyst is significantly improved compared with CrN.In ammonia synthesis reaction, CrN/LiH (molar ratio 1:5) catalysis
Agent (N in nitrogen and hydrogen mixture2: H2=1:3), 10atm, under 350 DEG C of reaction condition, ammonia synthesis reaction rate be can reach
8627umol gcat -1h-1。
Detailed description of the invention
Fig. 1 .CrN/LiNH2The Ar-TPD spectrogram of (molar ratio 1:0.8).
Fig. 2 .CrN and CrN/LiNH2(molar ratio 1:0.8) is in 5%NH3Activity in/Ar.Fig. 3 .CrN/NaNH2It (rubs
You are than being 1:0.4) in 5%NH3Activity in/Ar.
Fig. 4 .CrN and CrN/LiNH2The activity of (molar ratio 1:0.8) in pure ammonia.
Fig. 5 .CrN and CrN/NaNH2The activity of (molar ratio 1:0.4) in pure ammonia.
Fig. 6 .CrN/LiH (molar ratio 1:5) is in N2/H2(1/3) the ammonia synthesis reaction activity in.
Fig. 7 .CrN/CaH2(molar ratio 1:1.3) is in N2/H2(1/3) the ammonia synthesis reaction activity in.
Specific embodiment
To further illustrate the present invention, following specific embodiments are enumerated, but it is not intended to limit each accessory claim and determines
The invention scope of justice.
Embodiment 1:
In argon gas glove box, chromium nitride (CrN) 1.0000g and lithium amide (LiNH are accurately weighed2) 0.2788g, it is placed in
It makes by oneself in stainless steel jar mill.After closing ball grinder, it is packed into planetary ball mill (Fischt PM400), ball milling condition is
150rpm ball milling 3 hours.Up to sample CrN/LiNH2(molar ratio 1:0.8).
In argon gas glove box, CrN/LiNH is accurately weighed2(molar ratio 1:0.8) 0.0300g is placed in fixed bed stainless steel
In reactor.Sample (5%NH in reaction atmosphere3/ Ar gaseous mixture) it is warming up to required temperature, reaction gas flow control exists
1.8L/h and 3.6L/h, sampling analysis after 30 minutes.Test results are shown in figure 2.CrN just starts when temperature is higher than 475 degree
Show a small amount of ammonolysis craft activity, ammonia conversion ratio is only 3% at 500 degree.And CrN/LiNH2At 300 degree, that is, show
Certain ammonolysis craft is active (ammonia conversion ratio is about 7%), and ammonia conversion ratio gradually increases as the temperature rises；?
At 500 degree, ammonia conversion ratio can reach 90%.
Embodiment 2:
In argon gas glove box, chromium nitride (CrN) 1.0000g and Sodamide (NaNH are accurately weighed2) 0.2364g, it is placed in
It makes by oneself in stainless steel jar mill.After closing ball grinder, it is packed into planetary ball mill (Fischt PM400), ball milling condition is
150rpm ball milling 3 hours.Up to sample CrN/LiNH2(molar ratio 1:0.4).
In argon gas glove box, CrN/NaNH is accurately weighed2(molar ratio 1:0.4) 0.0300g is placed in fixed bed stainless steel
In reactor.Sample (5%NH in reaction atmosphere3/ Ar gaseous mixture) it is warming up to required temperature, reaction gas flow control exists
1.8L/h and 3.6L/h, sampling analysis after 30 minutes.Test results are shown in figure 3.Ammonia conversion ratio as the temperature rises and
It gradually increases, at 300 degree, CrN/NaNH2Upper ammonia conversion ratio is about 11%, slightly above CrN/LiNH2Upper ammonia conversion ratio；
At 500 degree, ammonia conversion ratio can reach 82%.
Embodiment 3:
In argon gas glove box, chromium nitride (CrN) 1.0000g and lithium amide (LiNH are accurately weighed2) 0.2788g, it is placed in
It makes by oneself in stainless steel jar mill.After closing ball grinder, it is packed into planetary ball mill (Fischt PM400), ball milling condition is
150rpm ball milling 3 hours.Up to sample CrN/LiNH2(molar ratio 1:0.8).
In argon gas glove box, CrN/LiNH is accurately weighed2(molar ratio 1:0.8) 0.0300g is placed in fixed bed stainless steel
In reactor.Sample is warming up to required reaction temperature in pure ammonia atmosphere, and pressure 1atm, reaction gas flow control is in 2.4L/
H, sampling analysis after 30 minutes.Test results are shown in figure 4.CrN just starts to show a small amount of ammonia when temperature is higher than 500 degree
Degrading activity, ammonia conversion ratio is only 2.4% at 550 degree.And CrN/LiNH2At 300 degree, that is, show certain ammonia point
Active (ammonia conversion ratio is about 2%) is solved, and ammonia conversion ratio gradually increases as the temperature rises；At 550 degree, ammonia
Conversion ratio can reach 38%.
Embodiment 4:
In argon gas glove box, chromium nitride (CrN) 1.0000g and Sodamide (NaNH are accurately weighed2) 0.2364g, it is placed in
It makes by oneself in stainless steel jar mill.After closing ball grinder, it is packed into planetary ball mill (Fischt PM400), ball milling condition is
150rpm ball milling 3 hours.Up to sample CrN/LiNH2(molar ratio 1:0.4).
In argon gas glove box, CrN/NaNH is accurately weighed2(molar ratio 1:0.4) 0.0300g is placed in fixed bed stainless steel
In reactor.Sample is warming up to required reaction temperature in pure ammonia atmosphere, and pressure 1atm, reaction gas flow control is in 2.4L/
H, sampling analysis after 30 minutes.Test results are shown in figure 5.CrN/NaNH2At 300 degree, that is, show certain ammonia point
Active (ammonia conversion ratio is about 1.4%) is solved, and ammonia conversion ratio gradually increases as the temperature rises；But in 300-550
It spends in temperature range, activity is below CrN/LiNH2；At 550 degree, CrN/NaNH2Upper ammonia conversion ratio can reach 22%.
Embodiment 5:
In argon gas glove box, chromium nitride (CrN) 1.0000g and lithium hydride (LiH) 0.6060g are accurately weighed, is placed in certainly
In stainless steel jar mill processed.After closing ball grinder, it is packed into planetary ball mill (Fischt PM400), ball milling condition 150rpm
Ball milling 3 hours.Up to sample CrN/LiH (molar ratio 1:5).
In argon gas glove box, CrN/LiH (molar ratio 1:5) 0.0300g is accurately weighed, fixed bed stainless steel reaction is placed in
In device.Sample is in N2/H2(1/3) required reaction temperature, pressure 10atm are warming up in atmosphere, reaction gas flow control exists
1.8L/h, sampling analysis after at least 1 hour.Test results are shown in figure 6.CrN/LiH has been shown certain at 225 degree
Ammino is Viability, and (generating rate of ammonia is about 437umol gcat -1h-1), and ammonia generating rate is as the temperature rises and gradually
Increase；At 350 degree, the generating rate of the upper ammonia of CrN/LiH can reach 8627umol gcat -1h-1。
Embodiment 6:
In argon gas glove box, chromium nitride (CrN) 1.0000g and calcium hydride (CaH are accurately weighed2) 0.8273g, it is placed in
It makes by oneself in stainless steel jar mill.After closing ball grinder, it is packed into planetary ball mill (Fischt PM400), ball milling condition is
150rpm ball milling 3 hours.Up to sample CrN/CaH2(molar ratio 1:1.3).
In argon gas glove box, CrN/CaH is accurately weighed2(molar ratio 1:1.3) 0.0300g is placed in fixed bed stainless steel
In reactor.Sample is in N2/H2(1/3) required reaction temperature, pressure 10atm are warming up in atmosphere, reaction gas flow control exists
1.8L/h, sampling analysis after at least 1 hour.Test results are shown in figure 7.CrN/CaH2One is just shown at 275 degree or more
Fixed ammino is Viability, and ammonia generating rate gradually increases as the temperature rises；At 350 degree, CrN/CaH2Upper ammonia
Generating rate can reach 3472umol gcat -1h-1, lower than the generating rate of ammonia on CrN/LiH.
Claims (8)
1. a kind of for ammonia synthesis and the chromium-based catalysts of ammonolysis craft, it is characterised in that: the catalyst includes main body and addition
Agent, main body are one of crome metal, chromium nitride or its metal evanohm or two kinds or more, and additive includes containing for major element
One of nitrogen compound or/and hydrogen-containing compound or two kinds or more and carrier；
The range that the mass ratio of the catalyst body and additive is is 1000:1 to 1:500.
2. catalyst as described in claim 1, it is characterised in that:
Nitrogenous or/and hydrogen-containing compound the molecular formula of the major element are as follows: MxNyHm(3y-nx), wherein M is I A, II A, III A
One of race's element or two kinds or more, the chemical valence state that n (can be 1,2,3) is M, m can be 1, -1) chemical valence state that is H, when
When m=1, molecular formula MxNyH3y-nx, x=1~3, y=1~3；As m=-1, molecular formula MxNyHnx-3y, x=1~4, y=
0~1.
3. catalyst as claimed in claim 1 or 2, it is characterised in that: the major element be Li, Na, K, Rb, Cs, Mg,
The mixture of one of Ca, Sr, Ba, Al or two kinds or more.
4. catalyst as described in claim 1, it is characterised in that: the carrier is Li2O、MgO、CaO、SrO、BaO、
Al2O3、SiO2、TiO2、ZrO2、CeO2、BN、Si3N4、Mg3N2、Ca3N2, AlN, molecular sieve, carbon material, metal-organic framework materials
One of (MOFs) or two kinds or more of combination, the quality of carrier is 20-99wt% in catalyst.
5. catalyst as described in claim 1, it is characterised in that: the chromium nitride is CrN, Cr2One in the nitride such as N
Kind or two kinds or more of combination.
6. catalyst as described in claim 1, it is characterised in that: the metal evanohm are as follows: IV B, V B, VI B, VII B or
More than one of VIII B race element or two kinds or more of the binary or ternary being combined into Cr metal alloy or IV B, V B,
VI B, VII B or VIII B race element, preferably such as Ti, Zr, V, Nb, Ta, Mo, W, Mn, Re, Fe, Ru, Os, Co, Rh, Ir, Ni, Pd, Pt
One of or two kinds or more of the binary or ternary being combined into Cr more than metal alloy；Or IV B, V B, VI B, VII B or
Alloy more than one of VIII B race element or two kinds or more of the binary or ternary formed between Cr and C and/or N, preferably
As one of Ti, Zr, V, Nb, Ta, Mo, W, Mn, Re, Fe, Ru, Os, Co, Rh, Ir, Ni, Pd, Pt or two kinds or more and Cr
And the alloy more than binary or ternary formed between C and/or N.
7. catalyst as described in claim 1, it is characterised in that: the mass ratio of the catalyst body and additive it is more excellent
Range is 200:1 to 1:100.
8. a kind of application of any catalyst of claim 1-7, it is characterised in that:
The catalyst is used for operating condition when ammonia synthesis: sample is in nitrogen and hydrogen mixture (volume ratio N2: H2=1:3) in heating
To 200-500 (preferably 300 degrees centigrade), gross pressure 1-30atm, reaction gas flow velocity is 1.8-2.4L/h, with conventional conductance
The generating rate of rate method detection ammonia；
The catalyst is used for operating condition when ammonolysis craft: sample is in reaction atmosphere (volume content 1-100% (preferably 5%)
NH3/ Ar or pure ammonia) in rise to 300-600 degrees Celsius of reaction temperature, product composition is divided online using gas-chromatography
Analysis.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111790420A (en) * | 2020-06-04 | 2020-10-20 | 福州大学 | Catalyst carrier, ammonia decomposition catalyst and preparation method |
| CN112973749A (en) * | 2019-12-13 | 2021-06-18 | 中国科学院大连化学物理研究所 | Catalyst, preparation method and application |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112973749A (en) * | 2019-12-13 | 2021-06-18 | 中国科学院大连化学物理研究所 | Catalyst, preparation method and application |
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| CN111790420B (en) * | 2020-06-04 | 2021-11-16 | 福州大学 | Catalyst carrier, ammonia decomposition catalyst and preparation method |
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