CN102974344A - Dehydrogenation catalyst applicable to raw gas rich in carbon monoxide, and preparation and application thereof - Google Patents
Dehydrogenation catalyst applicable to raw gas rich in carbon monoxide, and preparation and application thereof Download PDFInfo
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- CN102974344A CN102974344A CN2012104252854A CN201210425285A CN102974344A CN 102974344 A CN102974344 A CN 102974344A CN 2012104252854 A CN2012104252854 A CN 2012104252854A CN 201210425285 A CN201210425285 A CN 201210425285A CN 102974344 A CN102974344 A CN 102974344A
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Abstract
The invention relates to gas purification techniques and specifically to a dehydrogenation catalyst applicable to raw gas rich in carbon monoxide and preparation and application thereof. Palladium is used as an active component of the catalyst, auxiliary agents for the catalyst are two to four selected from the group consisting of silver, zinc, lanthanum, cerium, samarium, praseodymium, iron, stannum, manganese, calcium, magnesium, tungsten and molybdenum, and a carrier of the catalyst is alumina. The catalyst realizes selective catalytic oxidation removal of hydrogen in the raw gas rich in carbon monoxide by directing using synergism of palladium and oxides of a plurality of the auxiliary agents. Components of the catalyst comprise, based on the weight of the carrier, 0.05 to 1% of the active component and 0.5 to 5% of the total auxiliary agents. According to the invention, the catalyst has high activity and stability even when the application amount of a precious metal is small; through usage of the catalyst in a gas source rich in carbon monoxide, outlet hydrogen content is less than 100 ppm, outlet oxygen content is less than 0.1%, and purifying indexes of hydrogen and oxygen in reaction tail gas still accord with requirements after continuous operation for 1000 hours.
Description
Technical field
The present invention relates to gas purification technique, relate in particular to a kind of dehydrogenation and preparation and application that is applicable to be rich in the unstrpped gas of carbon monoxide.
Background technology
As everyone knows, precious metal palladium, platinum are industrial common dehydrogenations, can be used for the purification dehydrogenation in the non-reducing gas such as CO 2 raw material gas in purity nitrogen, pure oxygen and the urea compound probability.But purify in the dehydrogenating technology at feed gas containing carbon monoxide, carbonomonoxide concentration exceeds three orders of magnitude of hydrogen concentration, conventional palladium or platinum/aluminium oxide catalyst are because more approaching to the oxidation reaction selectivity ratios of hydrogen and carbon monoxide, meeting when finishing catalytic oxidation is so that most oxygen and carbon monoxide reacts rather than react with hydrogen, can't realize the selective oxidation removal to hydrogen, the concentration of carbon monoxide is higher, and is also higher to the selective and anti-carbon monoxide absorption property requirement of dehydrogenation.
CN1054765A discloses continuous process for synthesis of oxalic ester by gaseous catalysis, wherein the hydrogen in the carbon monoxide source of the gas, oxygen removal catalyst are as carrier take aluminium oxide, Pt and/or Pd are active component, and this catalyst can remove the hydrogen of 10% following content in being rich in feed gas containing carbon monoxide.But in this patent carbonomonoxide concentration be limited in below 95% and among the embodiment the highest of carbonomonoxide concentration reach 80%, whether can not process for the carbon monoxide of higher concentration and mention; This patent is mainly the technique patent simultaneously, and the aspects such as the preparation of dehydrogenation and use are not described in detail.
CN101543776A discloses a kind of dehydrogenation catalyst for feed gas containing carbon monoxide and methods for making and using same thereof, this catalyst is take aluminium oxide as carrier, Pt and/or Pd are active component, select 2～4 kinds to be auxiliary agent from sodium, potassium, magnesium, titanium, zirconium, vanadium, manganese, iron, nickel, cobalt, copper, molybdenum, tungsten or cerium, this catalyst can remove the hydrogen of 5% following content in the feed gas containing carbon monoxide of 10%～99% content.But this catalyst need carry out activation process before using, and activation method is that hydrogeneous hydrogen-nitrogen mixed gas or pure hydrogen more than 10% was passed through beds at least 8 hours under 450～650 ℃.This catalyst just can pass into unstripped gas after need to finishing online activation in device, need build facility and the high temperature reduction equipment that supplies hydrogen in industry spot, and aftertreatment technology is numerous and diverse, and energy consumption is high, makes troubles to execute-in-place.
Summary of the invention
The objective of the invention is for the problems referred to above, a kind of high-concentration carbon monoxide unstripped gas dehydrogenation dehydrogenation catalyst and its preparation method and application is provided.
For achieving the above object, the technical solution used in the present invention is:
A kind of dehydrogenation that is applicable to be rich in the unstrpped gas of carbon monoxide, catalyst is take palladium as active component, and auxiliary agent is 2-4 kind in silver, zinc, lanthanum, cerium, samarium, praseodymium, iron, tin, manganese, calcium, magnesium, tungsten, the molybdenum, and carrier is aluminium oxide; The described catalyst directly synergy by palladium and multiple auxiliary agent oxide realizes being rich in that the selective catalytic oxidation of hydrogen removes in the feed gas containing carbon monoxide; Wherein the composition of catalyst is counted take vehicle weight: active component is 0.05～1%, and the total amount of auxiliary agent is 0.5-5%.
Described alumina catalyst support can use silica, molecular sieve or silica-alumina supports to replace.
Be applicable to be rich in the preparation method of dehydrogenation of the unstrpped gas of carbon monoxide: palladium salt and builder salts adopt impregnation method with carrier impregnation wherein after dissolving, dry after in 300～600 ℃ of lower roastings 2～5 hours; Hydrazine hydrate solution with concentration 0.5～10% after the roasting reduced 4～12 hours, cleaned and drying, was catalyst.
Mix as maceration extract after described active component palladium salt and the builder salts dissolving and adopt impregnation method with carrier impregnation wherein, realize a step dipping.
Described active component palladium salt and builder salts dissolving adopt impregnation method that carrier is progressively flooded wherein as maceration extract, realize step impregnation.
Described alumina catalyst support can use silica, molecular sieve or silica-alumina supports to replace.
Described active component palladium salt is the acid of chlorine palladium, palladium bichloride or palladium nitrate; Described builder salts is the nitrate of promoter metal, the acetate of promoter metal, the chloride of promoter metal or the hydrochlorate of metal promoter metal.
Be applicable to be rich in the application of dehydrogenation of the unstrpped gas of carbon monoxide, described catalyst directly passes into the selective catalytic oxidation that unstripped gas carries out hydrogen and removes.
It is that serviceability temperature is 130 ℃～250 ℃ in 10～99% the feed gas containing carbon monoxide that described catalyst is directly passed into concentration, and reaction velocity is 800～4000h
-1, the hydrogen in the unstripped gas is carried out selective oxidation removal; The outlet hydrogen content is less than 100ppm, and the outlet oxygen content is less than 0.1%.
It is that serviceability temperature is 150 ℃～230 ℃ in 10～99% the feed gas containing carbon monoxide that described catalyst is directly passed into concentration, and reaction velocity is 800～3000h
-1, the hydrogen in the unstripped gas is carried out selective oxidation removal.
The invention has the advantages that:
1. the catalyst of the present invention's preparation is simple to operation, need not prereduction before the use.
2. still has high activity and stable when catalyst noble metal use amount of the present invention is less, in being rich in the source of the gas of carbon monoxide, by use this catalyst can so that the outlet hydrogen content less than 100ppm, the outlet oxygen content is less than 0.1%, and after moving continuously 1000 hours, the hydrogen-oxygen decontamination index still meets the requirements in the reaction end gas.
3. catalyst of the present invention can be used for concentration removing up to Microamounts of Hydrogen in 99% the carbon monoxide.
4. catalyst of the present invention has good start-stop car performance, the observability decay that experience is stopped for several times and do not caused the hydrogen-oxygen conversion ratio.
5. catalyst cost of the present invention is lower, and adaptability is stronger, removes applicable to the deep oxidation of hydrogen in the industrialization feed gas containing carbon monoxide.
The specific embodiment
A kind of high-concentration carbon monoxide dehydrogenation, this catalyst is realized the oxidation removal of hydrogen in the high-concentration carbon monoxide unstripped gas by the concerted catalysis effect of precious metal palladium and multiple non-noble metal oxide auxiliary agent, wherein promoter metal is selected from 2-4 kind in silver, zinc, lanthanum, cerium, samarium, praseodymium, iron, tin, manganese, calcium, magnesium, tungsten or the molybdenum, carrier is aluminium oxide, Pd content is 0.05～1wt%, and the auxiliary agent total content is 0.5%-5%wt%.
The catalyst of the present invention's preparation need not preliminary treatment before the use, can directly pass into unstripped gas, and the hydrogen in the feed gas containing carbon monoxide of variable concentrations is carried out selective oxidation removal, and its service condition is: reaction temperature is 130～250 ℃, preferred 150～230 ℃; Reaction velocity is 500～4000h
-1, preferred 800～3000h
-1, the outlet hydrogen content is less than 100ppm, and the outlet oxygen content is less than 0.1%.
Embodiment 1
First with 0.3 gram palladium bichloride with 10m (hydrochloric acid be concentrated hydrochloric acid with deionized water by volume 1:1 mix, be the hydrochloric acid that concentrated hydrochloric acid and deionized water are made into equal volume) dissolving with hydrochloric acid, add again 4.6 gram ammonium molybdates, 2.5 gram cerous nitrates and 2.5 gram lanthanum nitrates, the water dissolving is made into 70 gram dipping solutions, 100 gram alumina balls are poured in this solution and flooded, dry rear in 600 ℃ of lower roastings 3 hours, at room temperature with 1% hydrazine hydrate solution reduction 10 hours, abundant cleaning, drying namely obtain this catalyst after the reduction.
Described catalyst directly passes into and consists of: the 0.5%(percent by volume) H
2, 0.5%O
2, 0.5%CO
2, 15%CO, remaining is N
2Unstripped gas, 140 ℃ of temperature, air speed 2650h
-1, pressure 0.5MPa, export H this moment
2Content is 85ppm, outlet O
2Content is 600ppm.
Embodiment 2
First with 0.4 gram palladium bichloride 10m (1:1) dissolving with hydrochloric acid, add again 5 gram ammonium paratungstates and 10 gram magnesium nitrates, the water dissolving is made into 70 gram dipping solutions, 100 gram alumina balls are poured in this solution and flooded, dry rear in 500 ℃ of lower roastings 3 hours, at room temperature with 1% hydrazine hydrate solution reduction 10 hours, and dry after fully cleaning, namely obtain this catalyst.
Described catalyst directly passes into and consists of: 6.2%H
2, 3.6%O
2, 0.5%CO
2, 32%CO, remaining is N
2Unstripped gas, 220 ℃ of temperature, air speed 2000h
-1, pressure 0.5MPa, export H this moment
2Content is 66ppm, outlet O
2Content is 300ppm.
Embodiment 3
First with 0.4 gram palladium nitrate 10m (1:1) nitric acid dissolve, add again 0.45 gram silver nitrate, 3 gram zinc acetates and 2.5 gram praseodymium nitrates, the water dissolving is made into 70 gram dipping solutions, 100 gram alumina balls are poured in this solution and flooded, dry rear in 550 ℃ of lower roastings 3 hours, at room temperature with 1% hydrazine hydrate solution reduction 10 hours, and dry after fully cleaning, namely obtain this catalyst.
Described catalyst directly passes into and consists of: 0.3%H
2, 0.3%O
2, remaining be the unstripped gas of CO, 220 ℃ of temperature, air speed 1500h
-1, pressure 0.5MPa, export H this moment
2Content is 66ppm, outlet O
2Content is 550ppm.
Embodiment 4
First with 0.6 gram palladium nitrate 10m (1:1) nitric acid dissolve, add again 0.45 gram silver nitrate, 6 gram ferric nitrates and 4.2 gram samaric nitrates, the water dissolving is made into 70 gram dipping solutions, 100 gram alumina balls are poured in this solution and flooded, dry rear in 550 ℃ of lower roastings 3 hours, at room temperature with 1% hydrazine hydrate solution reduction 10 hours, and dry after fully cleaning, namely obtain this catalyst.
Described catalyst directly passes into and consists of: 3.5%H
2, 2.5%O
2, 0.5%CO
2, remaining be the unstripped gas of CO, 150 ℃ of temperature, air speed 800h
-1, pressure 0.5MPa, export H this moment
2Content is 65ppm, outlet O
2Content is 900ppm.
Embodiment 5
First with 0.17 gram palladium nitrate 10m (1:1) nitric acid dissolve, add again 5.6 gram ammonium molybdates, 0.5 gram silver nitrate, 3 gram manganese nitrates, the water dissolving is made into 70 gram dipping solutions, 100 gram alumina balls are poured in this solution and flooded, dry rear in 600 ℃ of lower roastings 3 hours, at room temperature with 1% hydrazine hydrate solution reduction 10 hours, and dry after fully cleaning, namely obtain this catalyst.
Described catalyst directly passes into and consists of: 6.2%H
2, 3.5%O
2, 0.5%CO
2, remaining be the unstripped gas of CO, 220 ℃ of temperature, air speed 2500h
-1, pressure 0.5MPa, export H this moment
2Content is 75ppm, outlet O
2Content is 585ppm.
Embodiment 6
First with 0.7 gram palladium bichloride 10m (1:1) dissolving with hydrochloric acid, add again 5.6 gram ammonium paratungstates, 5.6 gram magnesium nitrates and 4.5 gram cerous nitrates, the water dissolving is made into 70 gram dipping solutions, 100 gram alumina balls are poured in this solution and flooded, dry rear in 550 ℃ of lower roastings 3 hours, at room temperature with 1% hydrazine hydrate solution reduction 10 hours, and dry after fully cleaning, namely obtain this catalyst.
Described catalyst directly passes into and consists of: 0.2%H
2, 0.3%O, remaining be the unstripped gas of CO, 200 ℃ of temperature, air speed 1500h
-1, pressure 0.5MPa, export H this moment
2Content is 75ppm, outlet O
2Content is 800ppm.
Embodiment 7
First with 0.3 gram palladium bichloride 10m (1:1) dissolving with hydrochloric acid, add again 4.9 gram manganese nitrates, 2.3 gram ferric nitrates, 1.5 gram samaric nitrates and 2.5 gram calcium nitrate, the water dissolving is made into 70 gram dipping solutions, 100 gram alumina balls are poured in this solution and flooded, dry rear in 600 ℃ of lower roastings 3 hours, at room temperature with 1% hydrazine hydrate solution reduction 10 hours, and dry after fully cleaning, namely obtain this catalyst.
Described catalyst directly passes into and consists of: 0.1%H
2, 0.1%O
2, 0.5%CO
2, remaining be the unstripped gas of CO, 150 ℃ of temperature, air speed 2800h
-1, pressure 0.5MPa, export H this moment
2Content is 75ppm, outlet O
2Content is 320ppm.
Embodiment 8
With 0.45 gram palladium bichloride and 1.5 gram stannous chlorides 15m (1:1) dissolving with hydrochloric acid, add again 0.35 gram samaric nitrate and 6 gram ammonium molybdates, the water dissolving is made into 70 gram dipping solutions, 100 gram alumina balls are poured in this solution and flooded, dry rear in 600 ℃ of lower roastings 3 hours, at room temperature with 1% hydrazine hydrate solution reduction 10 hours, and dry after fully cleaning, namely obtain this catalyst.
Described catalyst directly passes into and consists of: 3.1%H
2, 2.1%O
2, 0.5%CO
2, remaining be the unstripped gas of CO, 220 ℃ of temperature, air speed 2500h
-1, pressure 0.5MPa, export H this moment
2Content is 78ppm, outlet O
2Content is 770ppm.
Embodiment 9
The catalyst of similarly to Example 2 preparation is passed into and consists of: 0.5%H
2, 0.5%O
2, 0.5%CO
2, remaining be the unstripped gas of CO, at 180 ℃ of temperature, air speed 1100h
-1, continuously operation 45 days under the pressure 0.5MPa, outlet H
2Content exports O less than 100ppm
2Content is less than 1000ppm.
Embodiment 10
Identical with embodiment 2 active components and content, be divided into two step dippings during enforcement: first 0.4 gram palladium bichloride is made into 70 gram solution with 10m (1:1) dissolving with hydrochloric acid, 100 gram alumina balls carriers are poured in this solution flood, dry rear in 550 ℃ of lower roastings 3 hours, pour into again in the 70 gram mixed solutions that are made into 5 gram ammonium paratungstates and 10 gram magnesium nitrates and flood, dry rear in 500 ℃ of lower roastings 3 hours, at room temperature process with 1% hydrazine hydrate solution reduction, and dry after fully cleaning, namely obtain this catalyst.
Described catalyst directly passes into and consists of: 1.9%H
2, 1.25%O
2, 0.5%CO
2, remaining be the unstripped gas of CO, 190 ℃ of temperature, air speed 1100h
-1, pressure 0.5MPa, export H this moment
2Content is 68ppm, outlet O
2Content is 56ppm.
Embodiment 11
Identical with embodiment 2 active components and content, be divided into three step dippings during enforcement: 100 gram alumina balls carriers are poured in the 70 gram solution that are made into 5 gram ammonium paratungstates flooded first, dry rear in 550 ℃ of lower roastings 3 hours, pouring 70 grams that 10 gram magnesium nitrates are made into into floods in the solution again, dry rear in 500 ℃ of lower roastings 3 hours, pour at last in the 70 gram solution that use 10m (1:1) dissolving with hydrochloric acid to be made into 0.4 gram palladium bichloride and flood, dry rear in 500 ℃ of lower roastings 3 hours, at room temperature process with 1% hydrazine hydrate solution reduction, and dry after fully cleaning, namely obtain this catalyst.
Described catalyst directly passes into and consists of: 1.0%H
2, 0.8%O
2, 0.5%CO
2, remaining be the unstripped gas of CO, 195 ℃ of temperature, air speed 1000h
-1, pressure 0.5MPa, export H this moment
2Content is 89ppm, outlet O
2Content is 128ppm.
Claims (10)
1. dehydrogenation that is applicable to be rich in the unstrpped gas of carbon monoxide, it is characterized in that: catalyst is take palladium as active component, and auxiliary agent is 2-4 kind in silver, zinc, lanthanum, cerium, samarium, praseodymium, iron, tin, manganese, calcium, magnesium, tungsten, the molybdenum, and carrier is aluminium oxide; The described catalyst directly synergy by palladium and multiple auxiliary agent oxide realizes being rich in that the selective catalytic oxidation of hydrogen removes in the feed gas containing carbon monoxide; Wherein the composition of catalyst is counted take vehicle weight: active component is 0.05～1%, and the total amount of auxiliary agent is 0.5-5%.
2. by the dehydrogenation that is applicable to be rich in the unstrpped gas of carbon monoxide claimed in claim 1, it is characterized in that: described alumina catalyst support can use silica, molecular sieve or silica-alumina supports to replace.
3. the preparation method of the dehydrogenation of a unstrpped gas that is applicable to be rich in carbon monoxide claimed in claim 1, it is characterized in that: palladium salt and builder salts are after dissolving, adopt impregnation method with carrier impregnation wherein, dry rear in 300～600 ℃ of lower roastings 2～5 hours; Hydrazine hydrate solution with concentration 0.5～10% after the roasting reduced 4～12 hours, cleaned and drying, was catalyst.
4. by the preparation method of the dehydrogenation of the unstrpped gas that is applicable to be rich in carbon monoxide claimed in claim 3, it is characterized in that: mix as maceration extract after described active component palladium salt and the builder salts dissolving and adopt impregnation method with carrier impregnation wherein, realize a step dipping.
5. by the preparation method of the dehydrogenation of the unstrpped gas that is applicable to be rich in carbon monoxide claimed in claim 3, it is characterized in that: described active component palladium salt and builder salts dissolving adopt impregnation method that carrier is progressively flooded wherein as maceration extract, realize step impregnation.
6. by the preparation method of the dehydrogenation of the unstrpped gas that is applicable to be rich in carbon monoxide claimed in claim 3, it is characterized in that: described alumina catalyst support can use silica, molecular sieve or silica-alumina supports to replace.
7. by the preparation method of the dehydrogenation of the unstrpped gas that is applicable to be rich in carbon monoxide claimed in claim 3, it is characterized in that: described active component palladium salt is the acid of chlorine palladium, palladium bichloride or palladium nitrate; Described builder salts is the nitrate of promoter metal, the acetate of promoter metal, the chloride of promoter metal or the hydrochlorate of metal promoter metal.
8. the application of the dehydrogenation of a unstrpped gas that is applicable to be rich in carbon monoxide claimed in claim 1 is characterized in that: described catalyst directly passes into the selective catalytic oxidation that unstripped gas carries out hydrogen and removes.
9. by the application of the dehydrogenation of the unstrpped gas that is applicable to be rich in carbon monoxide claimed in claim 8, it is characterized in that: it is in 10～99% the feed gas containing carbon monoxide that described catalyst is directly passed into concentration, serviceability temperature is 130 ℃～250 ℃, and reaction velocity is 800～4000h
-1, the hydrogen in the unstripped gas is carried out selective oxidation removal; The outlet hydrogen content is less than 100ppm, and the outlet oxygen content is less than 0.1%.
10. by the application of the dehydrogenation of the unstrpped gas that is applicable to be rich in carbon monoxide claimed in claim 9, it is characterized in that: it is in 10～99% the feed gas containing carbon monoxide that described catalyst is directly passed into concentration, serviceability temperature is 150 ℃～230 ℃, and reaction velocity is 800～3000h
-1, the hydrogen in the unstripped gas is carried out selective oxidation removal.
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| CN103223339A (en) * | 2013-04-09 | 2013-07-31 | 中国科学院福建物质结构研究所 | Method for preparing supported Pd-based catalysts |
| CN104492443A (en) * | 2014-12-02 | 2015-04-08 | 西南化工研究设计院有限公司 | Dehydrogenation catalyst for preparing high-purity carbon monoxide as well as preparation method and application of dehydrogenation catalyst |
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| CN104888768A (en) * | 2014-03-03 | 2015-09-09 | 中国石油化工股份有限公司 | Oxidation catalyst, preparation method and application thereof |
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| CN104925808B (en) * | 2014-03-17 | 2017-03-15 | 中国石油化工股份有限公司 | The method of hydrogen in removal of carbon monoxide gaseous mixture |
| CN104925808A (en) * | 2014-03-17 | 2015-09-23 | 中国石油化工股份有限公司 | Method of removing hydrogen in carbon monoxide mixed gas |
| CN104492443A (en) * | 2014-12-02 | 2015-04-08 | 西南化工研究设计院有限公司 | Dehydrogenation catalyst for preparing high-purity carbon monoxide as well as preparation method and application of dehydrogenation catalyst |
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| CN105771983B (en) * | 2014-12-24 | 2018-12-07 | 大连凯特利催化工程技术有限公司 | Hydrogenation of unsaturated hydrocarbons is the catalyst and its preparation method and application of saturated hydrocarbons in a kind of carbon monoxide industrial gasses |
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| CN110721707A (en) * | 2019-10-30 | 2020-01-24 | 大连凯特利催化工程技术有限公司 | Low-temperature deoxidation catalyst for synthesis gas and preparation and application thereof |
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| CN111905729A (en) * | 2020-07-30 | 2020-11-10 | 成都龙飞科技有限公司 | Organic hydrocarbon deoxidation catalyst and preparation method thereof |
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