CN101745391A - A kind of catalyst of removing traces of oxygen in catalytic cracking dry gas - Google Patents
A kind of catalyst of removing traces of oxygen in catalytic cracking dry gas Download PDFInfo
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- CN101745391A CN101745391A CN 200810227655 CN200810227655A CN101745391A CN 101745391 A CN101745391 A CN 101745391A CN 200810227655 CN200810227655 CN 200810227655 CN 200810227655 A CN200810227655 A CN 200810227655A CN 101745391 A CN101745391 A CN 101745391A
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Abstract
A kind of catalyst of removing traces of oxygen in catalytic cracking dry gas, it is characterized in that containing catalytic active component and carrier, wherein catalytic active component is by main catalytic active component and help catalytic active component to form, the main catalytic active component is a Metal Palladium, in catalyst weight, palladium content is 0.01～0.5%, help catalytic active component to be selected among Ag, Au, Co, the Cr one or more, content is 0.05～1.0%, carrier is selected from aluminium oxide, active carbon, silica or molecular sieve, and catalytic active component is the surface that eggshell state is distributed in carrier.This catalyst deoxidation degree of depth under high-speed can reach 0.1ppm, and it is strong to have anti-poisoning capability, and reaction bed is difficult for characteristics such as temperature runaway.
Description
Technical field
The present invention relates to gas purification technique, further say to relate to a kind of catalyst that is used for removing traces of oxygen in catalytic cracking dry gas.
Background technology
Along with the development of chemical industry, the purification of industrial gasses more and more becomes a research topic that must solve, and wherein the deoxidation of all gases is common purification techniques.
As everyone knows, catalytic cracking in China petroleum refining industry (FCC) capacity to reprocess proportion is very big, at present, China's catalytic cracking unit scale occupies the second place of the world, dry gas output is 1.2Mt/a～3.5Mt/a, the ethene that contains 12%～19% (volume fraction) in the dry gas, most refinery is burnt catalytic cracked dry gas as the combustion gas or the torch of setting fire, cause the waste of resource and the pollution of environment.Ethene quantity in the dry gas is considerable, if it can be reclaimed, can improve the competitiveness of oil refining enterprise, also will relax the disparities between supply and demand of ethene, and it is significant to extract ethene from catalytic cracked dry gas.
Because the FCC dry gas is formed with the different of feedstock property, processing scheme and process conditions difference, wherein H to some extent
2, N
2And CH
4And C
2H
4And C
2H
6Content is bigger, O
2, CO, CO
2, C
3H
6And C
3H
8Less Deng constituent content, each constituent content excursion is bigger, forms unstable.In order from the FCC dry gas, to extract ethene, just must purify, and remove wherein trace impurity catalytic cracked dry gas, especially a small amount of oxygen (oxygen content volume fraction＜3.0% generally speaking) has removed big difficulty.
The technology that removes oxygen mainly comprises physics deoxygenation and chemical deoxidization.The deoxygenation of physics method comprises: deaeration in condenser, rectifying, absorption, film separation, Deadsorbing and oxygen removing etc.; The kind of chemical method deoxygenation is more, and application is extensive, and gas purification deoxygenation at present mainly utilizes methods such as catalytic hydrogenation, chemical absorbing, no hydrogen catalysis.
A kind of high concentration carbon monoxide synthetic gas deoxidizing catalyst that discloses among the CN1220302A, the weight ratio compositing range is: Cu5～10%, Mn2～5%, Co0.2～2%, active carbon 83～92.8%, it is said can right＜1% oxygen content high-concentration carbon monoxide gas carry out degree of depth deoxidation, purify back gas remaining oxygen＜1ppm.Said catalyst has high CO+O
2→ CO
2Catalytic activity, reaction temperature is low, but is not suitable for being used in the situation that contains alkene in the mist.
" meticulous and specialty chemicals .2001, (13), P13～14 " have reported a kind of base metal molybdenum oxide dehydrogenation catalyst, and it is big that this multifunctional efficient dehydrogenation catalyst has treating capacity, and remaining oxygen is low, the characteristics of ability sulphur, phosphorus.This activity of such catalysts component is base metal, and its price only is half of noble metal catalyst.But this dehydrogenation catalyst only can be used for the situation of the mist deoxygenation of those oxygen contents very low (0.1%～0.5%).
A kind of high strength is disclosed among the CN1175478A, highly heat-resistant catalyst, adopting titanium dioxide to add aluminium oxide is carrier, and active component is palladium and/or platinum, and this catalyst is used for thick hydrogen deoxygenation, nitrogen and the reaction of inert gas deoxidization by adding hydrogen, anti-H
2S, SO
2Poisoning capability is strong, and the catalyst strength height need not activation and regeneration.
But above-mentioned dehydrogenation catalyst can not be used for the deoxidation subtractive process of high olefin content mist, also just can not be used for FCC dry gas deoxidization technique.
Summary of the invention
The purpose of this invention is to provide a kind of catalyst, this Preparation of catalysts method of the removing traces of oxygen in catalytic cracking dry gas of prior art and method of using this catalyst of being different from.
The catalyst of removing traces of oxygen in catalytic cracking dry gas provided by the invention, contain catalytic active component and carrier, it is characterized in that catalytic active component is by main catalytic active component and help catalytic active component to form, wherein the main catalytic active component is a palladium, in catalyst weight, palladium content is 0.01～0.5%, and helping catalytic active component is among Ag, Au, Co, the Cr one or more, content is 0.05～1.0%, and various catalytic active component are the surface that eggshell state is distributed in carrier.
The said catalytic active component that helps exists with oxide form when not reducing.
Said carrier is selected from a kind of in alchlor, active carbon, silica and the molecular sieve.Said alchlor carrier can be: γ-Al
2O
3, δ-Al
2O
3, θ-Al
2O
3, α-Al
2O
3Deng, wherein be preferably θ-Al
2O
3, shape can be sphere, strip gear, sheet, cloverleaf pattern, column etc., preferably adopts ball type carrier.
Can also contain alkali metal in the said catalyst, alkali metal is used for the modulation support acidity, prolongs catalyst service life, and in catalyst carrier weight, its alkali metal ion content measured is 0.1～3.0%, preferred Na of alkali metal or K.
The present invention also provides above-mentioned Preparation of catalysts method, is the aqueous solution of used additives element salt and palladium salt, adopts equal-volume graded impregnation method to make required catalyst, and step is as follows more specifically:
(1) select for use in aluminium oxide, active carbon, silica or the molecular sieve a kind of as catalyst carrier, impregnation process is 1～30 minute in the soluble-salt solution of one or more in being selected from Ag, Au, Co, Cr, handled 5～20 hours being lower than under 300 ℃ the temperature then, wherein, the concentration of said soluble-salt solution is 10～100mg/ml;
(2) according to the water absorption rate of carrier, according to the load capacity of palladium and the water absorption rate preparation palladium-impregnated salting liquid of carrier, then catalyst is poured in the palladium solution, normal temperature dipping 1-10h obtains described catalyst after drying, the roasting again.
In step (2), palladium salt can adopt palladium nitrate, acid chloride, palladium acetylacetonate or palladium bichloride, with inorganic acid the palladium salting liquid pH value of neutrality is transferred to 0.5～6.0, preferred 1.0～3.5 before the dipping; Said baking temperature is generally at 80～200 ℃, 5～20 hours time.In the dry run, preferably stir carrier so that uniform drying.Then carrier is carried out roasting,, preferably carried out 1～8 hour at 400～500 ℃ generally at 300～700 ℃.
Preparation method provided by the invention, the first step be dipping promoter metal salt earlier, and second step was flooded main activity component metal salt again, and order can not be put upside down.
Among the preparation method provided by the invention, preferably in step (1), carrier was soaked in alkali-metal hydroxide solution 1～30 minute earlier, remove surplus liquid then, standby behind 200 ℃ of dry 4h, preferred NaOH of said alkali-metal hydroxide solution or potassium hydroxide solution.
The present invention also provides a kind of reaction of removing traces of oxygen in catalytic cracking dry gas, it is characterized in that earlier with catalyst under 100～550 ℃ of temperature with pure hydrogen or hydrogen-containing gas reduction activation, the branch of hydrogen is pressed in 1～300 crust, be room temperature～200 ℃ at reaction condition then, pressure 0.1～2.5MPa, under gas space velocity 3000～30000h-1, dry gas is contacted with catalyst, said catalyst contains catalytic active component and carrier, it is characterized in that catalytic active component is by main catalytic active component and help catalytic active component to form, wherein the main catalytic active component is a Metal Palladium, in catalyst weight, palladium content is 0.01～0.5%, helping catalytic active component is Ag, Au, Co, among the Cr one or more, content is 0.05～1.0%, carrier is selected from aluminium oxide, active carbon, a kind of in silica and the molecular sieve, various catalytic active component are the surface that eggshell state is distributed in carrier.
Catalyst provided by the invention, the skim palladium is arranged helping on the metal oxide of catalytic active component, the catalyst activity component is the surface that eggshell state is distributed in carrier, the non-uniform structure of this active component causes high activity and selectivity, when being used for the catalytic cracked dry gas deoxidation process, reaction temperature in room temperature～200 ℃, reaction pressure 0.1～2.5MPa, gas space velocity 3000～30000h
-1Condition under, the deoxidizing purification degree of depth can reach 0.1ppm, and this catalyst to have anti-poisoning capability strong, reaction bed is difficult for temperature runaway, characteristics such as easy to control, good stability.
The specific embodiment
To be further described the present invention by the following examples, but content not thereby limiting the invention.
Embodiment 1
To make with rolling ball method
θ-Al
2O
3Ball 200g, the KOH solution impregnation of usefulness 300ml5% was handled 20 minutes, and 200 ℃ of following dry 4h in drying box are standby then.With 1.62g AgNO
3Be mixed with the 300ml aqueous solution, get standby θ-Al
2O
3Ball flooded 20 minutes in this solution, removed unnecessary liquid then, placed drying box under 180 ℃, was cooled to room temperature after dry 8 hours.Get 0.382g PdCl
2Use the HCl wiring solution-forming, regulator solution pH value is 2.5 again, adjusts volume to 284ml, is poured onto then for the first time on the soaked carrier, under 80 ℃ of conditions dry 12 hours after a while, 450 ℃ of following roastings 4 hours, uses H under 150 ℃
2Reductase 12 hour is cooled to room temperature, and promptly obtaining Pd content is 0.11%, and Ag content is that 0.506% active component is the dehydrogenation catalyst that eggshell type distributes, wherein auxiliary agent K on catalyst
+Content in carrier is 1.04%.
This dehydrogenation catalyst feeding is consisted of (mass percent): C
2H
415%, H
2S0.01%, H
25%, O
20.45%, surplus is N
2Unstripped gas, at P=2.0MPa, T=433K, S.V.=5000h
-1Under the condition, detect the exit gas oxygen content less than 0.1ppm, C
2H
4Content 14.6%.
Embodiment 2
To make with rolling ball method
θ-Al
2O
3Ball 100g, the KOH solution impregnation of usefulness 150ml5% was handled 10 minutes, and 180 ℃ of following dry 4h in drying box are standby then.With 2.1g Cr (NO
3)
3.9H
2O is mixed with the 150ml aqueous solution, gets standby θ-Al
2O
3Ball flooded 30 minutes in this solution, removed unnecessary liquid then, placed drying box under 100 ℃, was cooled to room temperature after dry 8 hours.Get 0.2gPdCl
2Wiring solution-forming, regulator solution pH value is 2.5, adjusts volume to 142ml, is poured onto then for the first time on the soaked carrier, under 100 ℃ of conditions dry 12 hours after a while, 450 ℃ of following roastings 4 hours, uses H under 150 ℃
2Reductase 12 hour is cooled to room temperature, and promptly obtaining Pd content is 0.109%, and Cr content is that 0.26% active component is the dehydrogenation catalyst that eggshell type distributes, wherein auxiliary agent K on catalyst
+Content in carrier is 0.52%.
This dehydrogenation catalyst feeding is consisted of (mass percent): C
2H
415%, H
2S0.01%, H
25%, O
20.45%, surplus is N
2Unstripped gas, at P=2.0MPa, T=433K, S.V.=5500h
-1Under the condition, detect the exit gas oxygen content less than 0.1ppm, C
2H
4Content 14.3%.
Embodiment 3
To make with rolling ball method
θ-Al
2O
3Ball 40g, the NaOH solution impregnation of usefulness 60ml 5% was handled 10 minutes, and 180 ℃ of following dry 4h in drying box are standby then.With 0.72g Co (NO
3)
2.6H
2O is mixed with the 60ml aqueous solution, gets standby θ-Al
2O
3Ball flooded 30 minutes in this solution, removed unnecessary liquid then, placed drying box under 120 ℃, was cooled to room temperature after dry 12 hours.Get 0.13gPdCl
2Wiring solution-forming, regulator solution pH value is 1.5, adjusts volume to 56ml, is poured onto then for the first time on the soaked carrier, under 180 ℃ of conditions dry 12 hours after a while, 450 ℃ of following roastings 6 hours, uses H under 150 ℃
2Reduced 4 hours, and be cooled to room temperature, promptly obtaining Pd content is 0.18%, and Co content is that 0.35% active component is the dehydrogenation catalyst that eggshell type distributes, wherein auxiliary agent Na on catalyst
+Content in carrier is 0.17%.
This dehydrogenation catalyst feeding is consisted of (mass percent): C
2H
415%, H
2S0.01%, H
25%, O
20.45%, surplus is N
2Unstripped gas, at P=2.0MPa, T=373K, S.V.=3000h
-1Under the condition, detect the exit gas oxygen content less than 0.2ppm, C
2H
4Content 14.8%.
Embodiment 4
With 2.1g Cr (NO
3)
3.9H
2O is mixed with the 150ml aqueous solution, takes that rolling ball method makes
θ-Al
2O
3Ball 40g flooded 20 minutes in this solution, removed unnecessary liquid then, placed drying box under 120 ℃, was cooled to room temperature after dry 24 hours.Get 0.2g PdCl
2Wiring solution-forming, regulator solution pH value is 1.5, adjusts volume to 142ml, is poured onto then for the first time on the soaked carrier, under 180 ℃ of conditions dry 12 hours after a while, 500 ℃ of following roastings 4 hours, uses H under 200 ℃
2Reduced 1 hour, and be cooled to room temperature, promptly obtaining Pd content is 0.11%, and Cr content is 0.26% dehydrogenation catalyst.
This dehydrogenation catalyst feeding is consisted of (mass percent): C
2H
415%, H
2S0.01%, H
25%, O
20.45%, surplus is N
2Unstripped gas, at P=2.0MPa, T=433K, S.V.=5000h
-1Under the condition, detect the exit gas oxygen content less than 0.1ppm, C
2H
4Content 13.3%.
Embodiment 5
Adopt the catalyst of embodiment 1 preparation, this dehydrogenation catalyst is fed consist of (mass percent): C
2H
415%, H
2S0.06%, H
25%, O
20.45%, surplus is N
2Unstripped gas, at P=2.0MPa, T=433K, S.V.=5000h
-1Under the condition, detect the exit gas oxygen content less than 0.2ppm, C
2H
4Content 14.5%.
The reaction result of comparative examples 1 as can be seen, even the H in the unstripped gas
2S increases to 0.06% by 0.01%, and activity of such catalysts and selectivity are influenced hardly, illustrates that prepared catalyst has anti-preferably poisoning performance.
Embodiment 6
Keep the Preparation of Catalyst condition among the embodiment 1 constant, only will with rolling ball method make through 500 ℃ of roastings
γ-Al
2O
3Ball replaces θ-Al
2O
3Ball consists of (mass percent): C with prepared dehydrogenation catalyst feeding
2H
415%, H
2S 0.01%, H
25%, O
20.45%, surplus is N
2Unstripped gas, at P=2.0MPa, T=433K, S.V.=5000h
-1Under the condition, detect the exit gas oxygen content less than 0.1ppm, C
2H
4Content 13.5%.The reaction result of comparative examples 1 as can be seen, by γ-Al
2O
3The activity of the dehydrogenation catalyst of ball preparation is also better, just C
2H
4Loss amount is big slightly, but still meets the demands.
Embodiment 7
To adopt the dehydrogenation catalyst 2g of embodiment 2 preparations, the internal diameter φ 6mm that packs into, in the reaction tube of long 600mm, adopting certain refinery catalytic cracking unit's dry gas is reaction gas, dry gas consists of (mass percent): H
210.60%, H
2S 0.02%N
215.10% O
22.47% CH
425.10% C
2H
415.5%, C
2H
615%, C
3H
63.97% C
3H
80.42%, at P=2.0MPa, T=423K, S.V.=3000h
-1Under the condition, turned round continuously 1500 hours, detect the exit gas oxygen content less than 0.2ppm, C
2H
4Content 15.0%, catalyst have stability preferably.
Claims (13)
1. the catalyst of a removing traces of oxygen in catalytic cracking dry gas, it is characterized in that containing catalytic active component and carrier, wherein catalytic active component is by main catalytic active component and help catalytic active component to form, the main catalytic active component is a Metal Palladium, in catalyst weight, palladium content is 0.01～0.5%, help catalytic active component to be selected among Ag, Au, Co, the Cr one or more, content is 0.05～1.0%, carrier is selected from aluminium oxide, active carbon, silica or molecular sieve, and catalytic active component is the surface that eggshell state is distributed in carrier.
2. according to the catalyst of claim 1, the wherein said catalytic active component that helps is Ag.
3. according to the catalyst of claim 1, wherein said to help the content of catalytic active component be 0.1～0.6%.
4. according to the catalyst of claim 1, wherein said carrier is θ-Al
2O
3
5. according to the catalyst of claim 1, wherein also contain Na or K as auxiliary agent, in catalyst carrier weight, content is 0.1～3.0%.
6. according to the catalyst of claim 1, it is characterized in that this catalyst is order the soluble metal salting liquid and the soluble palladium salt solution impregnated carrier of auxiliary element obtained.
7. the Preparation of catalysts method of claim 1-6 is characterized in that this method comprises following step:
(1) select for use in aluminium oxide, active carbon, silica or the molecular sieve a kind of as catalyst carrier, impregnation process is 1～30 minute in the soluble-salt solution of one or more in being selected from Ag, Au, Co, Cr, handled 5～20 hours being lower than under 300 ℃ the temperature then, wherein, the concentration of said soluble-salt solution is 10～100mg/ml;
(2) according to the water absorption rate of carrier, according to the load capacity of palladium and the water absorption rate preparation palladium-impregnated salting liquid of carrier, then catalyst is poured in the palladium solution, normal temperature dipping 1-10h obtains described catalyst after drying, the roasting again.
8. according to the preparation method of claim 7, wherein the said palladium salt of step (2) is selected from palladium nitrate, acid chloride, palladium acetylacetonate or palladium bichloride.
9. according to the preparation method of claim 7, wherein before step (2) dipping, the palladium salting liquid pH value of neutrality is transferred to 0.5～6.0 with inorganic acid.
10. according to the preparation method of claim 9, wherein said pH value is for transferring to 1.0～3.5.
11. according to the preparation method of claim 7, said drying, its temperature are 80～200 ℃, 5～20 hours time, and said roasting, its temperature is at 300～700 ℃.
12. according to the preparation method of claim 7, it is characterized in that in step (1) precedingly, said carrier is earlier with alkali-metal hydroxide solution processing.
13. the reaction of a removing traces of oxygen in catalytic cracking dry gas, it is characterized in that earlier with catalyst under 100～550 ℃ of temperature with pure hydrogen or hydrogen-containing gas reduction activation, the branch of hydrogen is pressed in 1～300 crust, is room temperature～200 ℃, pressure 0.1～2.5MPa, gas space velocity 3000～30000h at reaction condition then
-1Down, dry gas is contacted with catalyst, said catalyst contains catalytic active component and carrier, it is characterized in that catalytic active component is by main catalytic active component and help catalytic active component to form, wherein the main catalytic active component is a Metal Palladium, in catalyst weight, palladium content is 0.01～0.5%, helping catalytic active component is among Ag, Au, Co, the Cr one or more, content is 0.05～1.0%, carrier is selected from a kind of in aluminium oxide, active carbon, silica and the molecular sieve, and various catalytic active component are the surface that eggshell state is distributed in carrier.
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| CN103100384A (en) * | 2011-11-09 | 2013-05-15 | 中国石油化工股份有限公司 | Preparation method of hydrogenation catalyst |
| CN103157471A (en) * | 2011-12-16 | 2013-06-19 | 西南化工研究设计院 | Deoxidation catalyst for olefin gas, preparation method and application thereof |
| WO2016083135A1 (en) * | 2014-11-28 | 2016-06-02 | Wacker Chemie Ag | Removal of oxygen from hydrocarbon gases |
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| CN111905837A (en) * | 2020-07-30 | 2020-11-10 | 成都龙飞科技有限公司 | Sulfur-resistant deoxidation catalyst and preparation method thereof |
| CN112705200A (en) * | 2019-10-24 | 2021-04-27 | 中国石油化工股份有限公司 | Anti-carbon monoxide poisoning deoxidation catalyst and preparation method and application thereof |
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2008
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| CN103100384A (en) * | 2011-11-09 | 2013-05-15 | 中国石油化工股份有限公司 | Preparation method of hydrogenation catalyst |
| CN103100384B (en) * | 2011-11-09 | 2015-07-22 | 中国石油化工股份有限公司 | Preparation method of hydrogenation catalyst |
| CN103157471A (en) * | 2011-12-16 | 2013-06-19 | 西南化工研究设计院 | Deoxidation catalyst for olefin gas, preparation method and application thereof |
| WO2016083135A1 (en) * | 2014-11-28 | 2016-06-02 | Wacker Chemie Ag | Removal of oxygen from hydrocarbon gases |
| CN107649146A (en) * | 2017-09-18 | 2018-02-02 | 北京华福工程有限公司 | Acetylene ring trimerization benzene catalyst and its preparation method and application |
| CN107649146B (en) * | 2017-09-18 | 2019-11-29 | 北京华福工程有限公司 | Acetylene ring trimerization benzene catalyst and its preparation method and application |
| CN111068712A (en) * | 2018-10-19 | 2020-04-28 | 中国石油化工股份有限公司 | Bifunctional catalyst for simultaneously removing oxygen and nitrogen oxide, preparation method and application thereof |
| CN112705200A (en) * | 2019-10-24 | 2021-04-27 | 中国石油化工股份有限公司 | Anti-carbon monoxide poisoning deoxidation catalyst and preparation method and application thereof |
| CN111420669A (en) * | 2020-04-21 | 2020-07-17 | 上海静好化工有限公司 | Dry gas impurity removal catalyst for refinery plant |
| CN111905837A (en) * | 2020-07-30 | 2020-11-10 | 成都龙飞科技有限公司 | Sulfur-resistant deoxidation catalyst and preparation method thereof |
| CN114345369A (en) * | 2022-01-12 | 2022-04-15 | 万华化学集团股份有限公司 | Acetyl oxidation catalyst, preparation method thereof and method for preparing vinyl acetate |
| CN114345369B (en) * | 2022-01-12 | 2023-05-30 | 万华化学集团股份有限公司 | Acetyloxidation catalyst, preparation method thereof and method for preparing vinyl acetate |
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