CN100503427C - Purification of a mixture of H*/CO by catalysis of the NO* - Google Patents

Purification of a mixture of H*/CO by catalysis of the NO* Download PDF

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Publication number
CN100503427C
CN100503427C CNB2004800164256A CN200480016425A CN100503427C CN 100503427 C CN100503427 C CN 100503427C CN B2004800164256 A CNB2004800164256 A CN B2004800164256A CN 200480016425 A CN200480016425 A CN 200480016425A CN 100503427 C CN100503427 C CN 100503427C
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catalyzer
air
volume
flow
mixture
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CN1805900A (en
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N·艾克-贝劳德
S·莫雷乌
A·穆兰
F·让特
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LAir Liquide SA pour lEtude et lExploitation des Procedes Georges Claude
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LAir Liquide SA pour lEtude et lExploitation des Procedes Georges Claude
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
    • B01D53/34—Chemical or biological purification of waste gases
    • B01D53/74—General processes for purification of waste gases; Apparatus or devices specially adapted therefor
    • B01D53/86—Catalytic processes
    • B01D53/8621—Removing nitrogen compounds
    • B01D53/8625—Nitrogen oxides
    • B01D53/8628—Processes characterised by a specific catalyst
    • 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
    • C01B3/50—Separation of hydrogen or hydrogen containing gases from gaseous mixtures, e.g. purification
    • C01B3/56—Separation of hydrogen or hydrogen containing gases from gaseous mixtures, e.g. purification by contacting with solids; Regeneration of used solids
    • 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
    • C01B3/50—Separation of hydrogen or hydrogen containing gases from gaseous mixtures, e.g. purification
    • C01B3/56—Separation of hydrogen or hydrogen containing gases from gaseous mixtures, e.g. purification by contacting with solids; Regeneration of used solids
    • C01B3/58—Separation of hydrogen or hydrogen containing gases from gaseous mixtures, e.g. purification by contacting with solids; Regeneration of used solids including a catalytic reaction
    • 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
    • B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
    • B01J23/38—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals
    • B01J23/40—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals of the platinum group metals
    • B01J23/44—Palladium
    • 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
    • B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
    • B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
    • B01J23/72—Copper
    • 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
    • B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
    • B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
    • B01J23/76—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
    • B01J23/84—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36 with arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
    • B01J23/85—Chromium, molybdenum or tungsten
    • B01J23/86—Chromium
    • B01J23/868—Chromium copper and chromium
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B2203/00—Integrated processes for the production of hydrogen or synthesis gas
    • C01B2203/04—Integrated processes for the production of hydrogen or synthesis gas containing a purification step for the hydrogen or the synthesis gas
    • C01B2203/042—Purification by adsorption on solids
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B2203/00—Integrated processes for the production of hydrogen or synthesis gas
    • C01B2203/04—Integrated processes for the production of hydrogen or synthesis gas containing a purification step for the hydrogen or the synthesis gas
    • C01B2203/042—Purification by adsorption on solids
    • C01B2203/043—Regenerative adsorption process in two or more beds, one for adsorption, the other for regeneration
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B2203/00—Integrated processes for the production of hydrogen or synthesis gas
    • C01B2203/04—Integrated processes for the production of hydrogen or synthesis gas containing a purification step for the hydrogen or the synthesis gas
    • C01B2203/0435—Catalytic purification
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B2203/00—Integrated processes for the production of hydrogen or synthesis gas
    • C01B2203/04—Integrated processes for the production of hydrogen or synthesis gas containing a purification step for the hydrogen or the synthesis gas
    • C01B2203/0465—Composition of the impurity
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B2203/00—Integrated processes for the production of hydrogen or synthesis gas
    • C01B2203/04—Integrated processes for the production of hydrogen or synthesis gas containing a purification step for the hydrogen or the synthesis gas
    • C01B2203/0465—Composition of the impurity
    • C01B2203/0495—Composition of the impurity the impurity being water

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Combustion & Propulsion (AREA)
  • Environmental & Geological Engineering (AREA)
  • Inorganic Chemistry (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Health & Medical Sciences (AREA)
  • Biomedical Technology (AREA)
  • General Chemical & Material Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Catalysts (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
  • Exhaust Gas Treatment By Means Of Catalyst (AREA)
  • Hydrogen, Water And Hydrids (AREA)
  • Industrial Gases (AREA)

Abstract

The invention relates to a method for purifying a gas flow containing hydrogen (H2) and carbon monoxide (CO), in addition to at least one nitrogen oxide (NOx), as impurities. According to said method, the gaseous flow is brought into contact with at least one catalyst containing copper and/or palladium, at a temperature between 100 DEG C and 200 DEG C, in such a way as to eliminate at least part of the nitrogen oxide.

Description

Pass through NO XThe H of catalyzed reaction 2/ CO mixture purifies
The present invention relates to the gaseous mixture that polluted by NOx type impurity, particularly mainly contain hydrogen and carbon monoxide (alleged H usually 2/ CO mixture or " synthetic gas ") and can contain methane (CH 4) the purifying method of gaseous mixture.
H 2/ CO gaseous mixture can obtain by several different methods, particularly:
-by partial oxidation with water vapor or CO 2Reform,
-by blending means (as ATR (self-heating recapitalization) method), it is the combination of steam reformation and partial oxidation, uses the gas as methane or ethane, or
-reclaim as waste gas by coal gasification or in acetylene device downstream.
According to operational condition, at these H 2The ratio of CO is usually between about 5 and 30 volume % in/the CO mixture.In addition, except hydrogen and CO, also usually contain the CH of various ratios in the mixture 4, CO 2And H 2O.
At present, there is several method to be used for the H that upgrades 2/ CO mixture, or rather, particularly by producing following method upgrading H 2/ CO mixture:
-pure hydrogen, it has many purposes,
-pure CO, it is used in synthesizing of acetic acid and carbonyl chloride especially, and in the production of polycarbonate, it is a reaction intermediate, or
-oxygen containing gas, its CO (〉 45 volume % that have been enrichment) purification H 2/ CO mixture can be used for the synthetic of butanols.
For this reason, be necessary at first to purify H 2/ CO mixture.
But, also have necessary purification H 2/ CO mixture is to satisfy the needs of its downstream use, and this can rely on special reaction, uses special catalyzer and/or sorbent material to realize at specific impurity, or realizes by other any suitable chemical treatments.
In addition, it is difficult removing some impurity that is present in the air-flow on the technical grade level.
In fact, the catalyzed reaction of removing impurity must or not cause H to be clean as much as possible 2/ CO gaseous mixture reacts.
H 2The reactivity of/CO mixture is well-known.
Thus, in the past few years Fischer-Tropsch synthesis has been used to obtain hydro carbons by following reaction mechanism (I):
(m/2+n)H 2+nCO→C nH m+nH 2O (I)
Be related to methane formation (so-called methanation) scheme as by people such as G.A.Mills at Catalysis Review, vol.8, No.2,1973, p.159-210 describe, this scheme is expressed by following reaction (II):
CO+3H 2→CH 4+H 2O (II)
In addition, the also available following excessively Boudouard reaction of carbon monoxide (III) is decomposed:
2CO→C+CO 2 (III)
Generally can use many metals to come catalysis from CO and H 2Formation reaction to hydro carbons.Example has following metal: Ru, Ir, Rh, Ni, Co, Os, Pt, Fe, Mo, Pd or Ag, as by F.Fischer, H.Tropsch and P.Dilthey at Brennst-Chem, vol.6,1925, p.265 described in.
Methyl alcohol forms reaction and also can carry out in the presence of many metals, is included under the copper existence to carry out:
CO+2H 2→CH 3OH (IV)
Thereby; usually caused the Fischer-Tropsch reaction (top reaction (I)) of formation hydrocarbon (particularly ethene) based on the ethylene hydrogenation catalyzer that is deposited on the platinum on the aluminum oxide, described hydrocarbon is higher in inlet (just in the gas before reaction) concentration at reaction outlet ratio.
Similarly, some oxide catalyst has caused the formation of methyl alcohol, and methyl alcohol must be removed in the downstream of catalyst bed subsequently.
In other words, these assisted reactions cause the generation of other reaction product, these other reaction product are not present in the gas to be clean, and must remove by the absorption in downstream, in being present in initial gas, in fact inevitably the pollutent.
Undesirable impurity comprises the oxynitride that usually is known as NOx.
NOx comprises following compounds: N 2O, NO, N 2O 3, NO 2, N 2O 5Back three is very active, can be spontaneously and reductive agent such as H 2With the CO reaction, form N 2, CO 2And H 2O.NO and N 2O (they may be more stable) can be present in H 2In/CO the mixture.If must handle this mixture in cryostat (low-temperature distillation method), their existence can cause potential danger.In fact, at trace O 2Under the existence of unsaturated hydro carbons, NOx can form the product that is easy to gather in cryogenic distillation, thereby damages device.Therefore definitely be necessary as far as possible effectively they to be removed.
In other words, industrial, in the undesirable production of by-products of restriction, obtain oxynitride (often being known as Nox) from air-flow, particularly from H 2Effective removal in the/CO stream is very important but also difficult the acquisition.
The problem of Chu Xianing is production and reclaims a kind of air-flow thus, has particularly sloughed the also H of its preferred whole contained NOx impurity of great majority 2/ CO air-flow.
In other words, the objective of the invention is to purify H by proposing one 2The effective ways of the NOx impurity that/CO mixture is contained improve the gaseous mixture of prior art, particularly H 2The purifying method of/CO type gaseous mixture is concentrated in the cryogenic distillation to prevent them.
Terms of settlement of the present invention thus is to purify to contain at least a air-flow that contains oxynitride (NOx) as impurity, wherein with air-flow and at least a catalyzer that contains copper or palladium 100 ℃ with 200 ℃ between temperature under contact, with catalysis at least a portion oxynitride.
According to every kind of situation, method of the present invention can comprise one or more following technical characterstics:
-temperature between 120 ℃ and 180 ℃ and/or pressure between 10 and 80 crust, preferred about 40 to 55 crust,
-gas space-time speed is 1000 and 10000Sm 3/ h gas/m 3Between the catalyzer, preferred 2000 and 6000Sm 3/ h gas/m 3(1Sm under 0 ℃ and 1atm between the catalyzer 3=1m 3),
-air-flow contacts with copper bearing catalyzer,
-air-flow contains hydrogen (H 2) and carbon monoxide (CO), and can contain methane (CH 4),
-oxynitride is converted to water (H 2O), O 2, NH 3And/or nitrogen,
-from the water (H that catalysis got of oxynitride 2O) and NH 3Be removed by one or more adsorption steps,
-at least one adsorption step uses one or more sorbent materials that are selected from exchange or not exchanging zeolite, activatory aluminum oxide, silica gel or its mixture or combination to carry out,
-gas to be separated contains the H of 10 volume % to 90 volume % 2, 10 volume % are to the CO of 90 volume %, and can contain methane,
-catalyzer can be protected by at least a protection bed that is positioned at above-mentioned catalyzer upstream.The protection bed plays guard catalyst and is not subjected to be easy to be present in the gas except oxynitride and is easy to degradation catalyst or the infringement of the chemical substance of reduction catalyst activity, for example mercury (Hg), arsenic (AsH 3), sulfide (H 2S, mercaptan, thioether), halogenide (HBr, HCl, Organohalogen compounds), HCN, iron carbonyl Fe (CO) 5With carbonyl nickel (CO) 4The protection bed can contain one or more sorbent materials,
The product P ICATOX Cu/Ag of PICA for example,
The structure of-catalyst system therefor of the present invention can be that size is 0.2 to 1cm particle.
The catalyst system therefor volume depends on the impurity concentration to be removed and the character of specific product.
The volume that provides sorbent material and catalyzer is as standard, because they depend on the impurity concentration to be removed and the character of specific product.General for given situation, can think will with the amount of sorbent material and the amount of pollutent to be removed roughly be directly proportional, the amount of catalyzer roughly is directly proportional with duration of contact or with the inverse of gas space-time speed (GHSV) (with respect to the per hour pending gas volume of catalyst volume) simultaneously.Gas volume can relevant with reactor inlet pressure (so GHSV depends on pressure), or can explain under specified condition, for example 1 crust and 0 ℃ (so GHSV does not rely on pressure); Select to be suitable on the reference conditions of each application possible to make changes.Duration of contact and GHSV -1Only roughly be directly proportional,, also depend on that the variation and the pressure of mole number in temperature along tower, the reaction process falls duration of contact because except pressure.But for one group of given reaction conditions, two parameters can be selected arbitrarily.
Another parameter that will take in is an impurity concentration to be removed in the gaseous effluent of outlet.Substantially, the concentration that needs is low more, and the amount of catalyzer is just big more.
Embodiment is described
In order to check the effect of the inventive method, according to invention, with H 2/ CO gaseous mixture contacts with catalyzer (just copper catalyst and palladium catalyst).
Catalyzer based on copper is the benchmark product 0860T of Engelhard.
Catalyzer based on palladium is the benchmark product 4586 of Engelhard.
In each test, be 47 crust and be about catalyst nox under 120 to 180 ℃ the temperature at pressure.
Initial gas contains hydrogen and the CO of the 80 volume % that have an appointment, and remaining is made up of methane and NOx impurity (about 0.15 volume %) to be removed.
In these tests, the space velocity that is adopted is 5000 to 2500Sm 3/ h/m 3Catalyzer (for example, 6 to 12m 3Catalyst treatment 30000Sm 3The gas of/h).
Following table shows that the use of copper or palladium catalyst can be catalyzed into NOx reaction product such as NH effectively 3, N 2, O 2And H 2O, the easier subsequently material of removing or can not having problems to downstream unit.
Copper catalyst than palladium catalyst allow more effectively remove NOx (after in each test, purifying residual quantity＜10ppb), because if CO concentration height, the latter's catalytic activity reduces a little.
Even now, the CO concentration in the air-flow is low but when containing dienes, it is more favourable than using copper catalyst to use palladium catalyst, because palladium can play the effect that transforms dienes, and copper can not obtain these effectively.
Table
Figure C200480016425D00081

Claims (10)

1, purification contains hydrogen and carbon monoxide, and contain the method for at least a oxynitride in addition as the air-flow of impurity, wherein air-flow is contacted under the temperature between 100 ℃ to 200 ℃ with at least a catalyzer that contains copper and/or palladium, to remove at least a portion oxynitride.
2, the method for claim 1, it is characterized in that temperature between 120 ℃ and 180 ℃ and/or pressure 10 and 80 the crust between.
3, claim 1 or 2 method is characterized in that gas space-time speed is 1000 and 10000Sm 3/ h gas/m 3Between the catalyzer.
4, claim 1 or 2 method is characterized in that air-flow contacts with the catalyzer that contains copper.
5, claim 1 or 2 method is characterized in that air-flow contains hydrogen, carbon monoxide and methane.
6, claim 1 or 2 method is characterized in that oxynitride is converted to water, O 2, NH 3And/or N 2
7, the method for claim 6 is characterized in that the water and the NH that obtain from the catalysis of NOx 3Be removed by one or more adsorption steps.
8, the method for claim 7 is characterized in that at least one adsorption step is selected from the sorbent material enforcement of exchange or not zeolite, activatory aluminum oxide, silica gel or its mixture or the combination of exchange with one or more.
9, claim 1 or 2 method is characterized in that air-flow to be separated contains the H of 10 volume % to 90 volume % 2, 10 volume % are to the CO of 90 volume %, and the optional methane that contains.
10, claim 1 or 2 method is characterized in that catalyzer protected by the protection bed that at least one is positioned at above-mentioned catalyzer upstream.
CNB2004800164256A 2003-06-11 2004-06-10 Purification of a mixture of H*/CO by catalysis of the NO* Expired - Fee Related CN100503427C (en)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
FR0307006A FR2856048B1 (en) 2003-06-11 2003-06-11 PURIFICATION OF A H2 / CO MIXTURE BY CATALYSIS OF NOx
FR03/07006 2003-06-11

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EP1836283B1 (en) * 2004-12-30 2019-03-27 Air Products and Chemicals, Inc. Improvements relating to coal to liquid processes
JP2011504196A (en) 2007-11-20 2011-02-03 シエル・インターナシヨネイル・リサーチ・マーチヤツピイ・ベー・ウイ Process for producing purified syngas stream
KR101011830B1 (en) * 2009-09-30 2011-01-31 상명대학교 산학협력단 Mixed metal oxide catalyst for decomposition of nitrogen oxide
CN106606927B (en) * 2015-10-22 2019-08-20 中国石油化工股份有限公司 Steam cracking produces the method for denitration and its denitrating system for the cracking flue gas that low-carbon alkene generates

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WO2004110924A1 (en) 2004-12-23
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