CN101108348A - Nickel base crouse vent gas hydrocatalyst and manufacturing process thereof - Google Patents

Nickel base crouse vent gas hydrocatalyst and manufacturing process thereof Download PDF

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CN101108348A
CN101108348A CNA2007100527880A CN200710052788A CN101108348A CN 101108348 A CN101108348 A CN 101108348A CN A2007100527880 A CNA2007100527880 A CN A2007100527880A CN 200710052788 A CN200710052788 A CN 200710052788A CN 101108348 A CN101108348 A CN 101108348A
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oxide
active component
component
nickel
crouse
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雷家珩
钱菁
方伟
郭丽萍
童辉
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Wuhan University of Technology WUT
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Wuhan University of Technology WUT
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Abstract

The invention relates to a hydrogeneration catalyst for the tail gas of a Crouse sulphur recycle device and a preparation method for the catalyst. A nickel-based Crouse tail gas hydro catalyst, which is characterized in that the catalyst essentially comprises a main active component, a secondary active component and alumina, the mass percentage of each component is like follows: the main active component 6-20%, the secondary active component 0-5%, the alumina 80-94%, the sum of the three components is 100%; wherein, the main active component is nickel oxide, the secondary active component is one or the mixture of any two or three of chrome oxide, copper oxide and iron oxide, when the secondary active component is a mixture, the compounding ratio among the oxides is random. The invention has the advantages of the good catalyzing activity at low temperature, the low cost and the simple preparation method.

Description

A kind of nickel base crouse vent gas hydrogenation catalysts and preparation method thereof
Technical field
The present invention relates to hydrogenation catalyst of a kind of Crouse (Claus) sulfur recovery facility tail gas and preparation method thereof.
Background technology
Utilize Claus technology Recovered sulphur from the waste gas of industry such as petroleum refining, natural gas purification and coking to be widely used.The Claus reaction is subjected to the restriction of thermodynamics and process conditions, and sulfur recovery rate generally is no more than 97%, so its tail gas need could discharge through handling.One of its processing method is the SO with remnants 2Through catalytic hydrogenating reduction is H 2It is recycling to pass to the Claus device behind the S again.
At present, the Claus catalyzer for hydrogenation on tail gas is generally Co (Ni) Mo/Al 2O 3Disclose a kind of sulfur-bearing Claus tail gas hydrogenation treatment process and catalyst as Japan Patent on May 10th, 1994 (patent No. JP06127907 A2), adopted CoMo/Al in this patent 2O 3Catalyst, wherein MoO 3Content reaches 13%, and CoO is 3.5%.Disclosed Claus catalyzer for hydrogenation on tail gas is an active component with Co, Mo all among Chinese patent CN1498674, CN1621134 and the CN1936768, with the Al of SiO2 modification 2O 3Be carrier.The CoMo/Al that these patents relate to 2O 3The operating temperature of Claus catalyzer for hydrogenation on tail gas is basic identical to be 2500h in air speed -1～4000h -1, SO 2Content is under the reaction condition of 2000ppmv～9000ppmv, all will could guarantee SO in the Claus tail gas working more than 260 ℃ 2Be converted into H fully 2S.Disclose a kind of among the patent CN1230134 with SiO 2And Al 2O 3Being carrier, is active component with Mo, and Ni is the Claus catalyzer for hydrogenation on tail gas of auxiliary agent, wherein MoO 3Content reaches 13%, and NiO is 4.3%, needs and COS, CS 2Hydrolytic reagent (K/TiO 2) use simultaneously, because two kinds of catalyst activities are all lower, can only be than low-speed (1250h -1) and low SO 2Content (2667ppmv) is reaction down.In addition, Co (Ni) Mo/Al 2O 3The price of catalyst is comparatively expensive.
Summary of the invention
The object of the present invention is to provide that a kind of low-temperature catalytic activity is good, cost is low, the simple nickel base crouse vent gas hydrogenation catalysts of preparation method and preparation method thereof.
To achieve these goals, technical scheme of the present invention is: a kind of nickel base crouse vent gas hydrogenation catalysts, it is characterized in that it is made of main active component, auxiliary activity component, three kinds of components of aluminium oxide, the shared mass percent of each component is: main active component 6%～20% (preferred 10～18%), auxiliary activity component 0%～5%, 80%～94%, three kinds of component sums of aluminium oxide are 100%; Wherein, main active component is a nickel oxide, and the auxiliary activity component is any one or any one the above mixture in chromium oxide, cupric oxide, the iron oxide, during any one above mixture, is any proportioning between the oxide.
The preparation method of above-mentioned a kind of nickel base crouse vent gas hydrogenation catalysts is characterized in that it comprises the steps:
1) γ-Al 2O 3Preliminary treatment: with γ-Al 2O 3Carrier was 100 ℃～150 ℃ dryings 2～10 hours, and is standby;
2) choosing of raw material: get and γ-Al 2O 3The deionized water of the saturated water adsorptive value equal volume of carrier, standby;
According to main active component, auxiliary activity component, the shared mass percent of aluminium oxide be: main active component 6%～20% (preferred 10～18%), auxiliary activity component 0%～5%, aluminium oxide 80%～94%, wherein, main active component is a nickel oxide, the auxiliary activity component is any one or any one the above mixture in chromium oxide, cupric oxide, the iron oxide, during any one above mixture, between the oxide any proportioning; Get with the equimolar nickel nitrate of required NiO standby; Get with the equimolar aluminum nitrate of required aluminium oxide standby; Get with the equimolar corresponding nitrate of required auxiliary activity component oxide standby; The corresponding nitrate of required auxiliary activity component oxide is: chromic nitrate, copper nitrate, ferric nitrate;
3) with 2) in nickel nitrate and the pairing nitrate of auxiliary activity component be dissolved in the deionized water, be made into maceration extract; With γ-Al 2O 3Carrier is put into maceration extract, the following 60 ℃ of dippings of stirring condition 2 hours, 100 ℃～150 ℃ dryings 2～10 hours;
4), get nickel base crouse vent gas hydrogenation catalysts at last 350 ℃～550 ℃ following roastings 2～10 hours.
Nickel base crouse vent gas hydrogenation catalysts also need be handled through presulfurization before reaction, and the presulfurization condition is 10%H 2S+II 2Atmosphere, pre-curing temperature are 400 ℃, 2 hours presulfurization time.
The main active component that the Ni-based Claus tail-gas catalyst of the present invention is adopted is different from common group vib metallic element, is main active component and adopt metallic nickel, rather than plays promoting catalysis as time active component.The present invention can not mix the group vib metallic element, as molybdenum (Mo), tungsten (W) etc.Wherein the mass content of nickel oxide is 5%～20%, preferred 10%～18%.
The present invention has following beneficial effect:
(1) adopts cheap Ni, Cu, Cr, Fe element as active component, therefore have lower cost.
(2) preparation method is simple, especially utilizes equi-volume impregnating not have significant loss; Hydrogenation conversion selectivity height.
(3) resulting nickel base crouse vent gas hydrogenation catalysts is at higher reaction velocity and higher SO 2Has good low-temperature catalytic activity under the content.
The specific embodiment
In order to understand the present invention better, further illustrate content of the present invention below in conjunction with embodiment, but content of the present invention not only is confined to the following examples.
The present invention is with γ-Al 2O 3Be carrier, its physicochemical properties such as table 1:
Outward appearance Size mm Bulk density g/ml Specific area m 2/g Water absorption rate ml/g Mechanical strength newton/ Pore volume ml/g
The white spheroid Ф3-5 0.65-0.85 250-350 0.8-1.1 ≥30 ～0.90
Embodiment 1:
A kind of preparation method of nickel base crouse vent gas hydrogenation catalysts, it comprises the steps:
1) with γ-Al 2O 3Carrier was 120 ℃ of dryings 5 hours, and is standby;
2) take by weighing the Ni (NO of 2.48g 3) 26H 2O adds deionized water dissolving to 10ml in beaker, be made into maceration extract;
3) with γ-Al of 10g 2O 3Carrier is put into maceration extract, the following 60 ℃ of dippings of stirring condition 2 hours, 120 ℃ of dryings 5 hours;
4) at last 450 ℃ of following roastings 5 hours, the broken sieve of the solid that obtains is got 20～40 orders, gets nickel base crouse vent gas hydrogenation catalysts (the NiO mass content is respectively 6%).
Catalyst activity is estimated: the 2ml nickel base crouse vent gas hydrogenation catalysts is placed flat-temperature zone, reactor middle part.Presulfurization: at 400 ℃ is 10Vol.%H with content down 2S+90Vol.%H 2Mist to presulfiding of catalyst 2h.Activity rating: the catalyst that has vulcanized flows down at nitrogen and is cooled to 220 ℃, detects noresidue H in the tail gas 2Feeding flow velocity behind the S is 200ml/min, SO 2/ H 2/ N 2The SO of=0.5/5/96.5 2, H 2, N 2Reaction mixture gas (is equivalent to air speed=6000h -1, SO 2Concentration=5000ppmv).After the stable reaction, with the gas componant of gas chromatographic analysis reactor inlet and outlet.Definition makes SO 2Conversion ratio is that 100% minimum response temperature is T M, definition makes H 2The S selectivity is that 100% minimum response temperature is T NIts activity data sees Table 1.
Embodiment 2:
A kind of preparation method of nickel base crouse vent gas hydrogenation catalysts, it comprises the steps:
1) with γ-Al 2O 3Carrier was 120 ℃ of dryings 5 hours, and is standby;
2) take by weighing the Ni (NO of 4.33g 3) 26H 2O adds deionized water dissolving to 10ml in beaker, be made into maceration extract;
3) with γ-Al of 10g 2O 3Carrier is put into maceration extract, the following 60 ℃ of dippings of stirring condition 2 hours, 120 ℃ of dryings 5 hours;
4) at last 450 ℃ of following roastings 5 hours, the broken sieve of the solid that obtains is got 20～40 orders, gets nickel base crouse vent gas hydrogenation catalysts (the NiO mass content is respectively 10%).Its activity data sees Table 1.
Embodiment 3:
A kind of preparation method of nickel base crouse vent gas hydrogenation catalysts, it comprises the steps:
1) with γ-Al 2O 3Carrier was 120 ℃ of dryings 5 hours, and is standby;
2) take by weighing the Ni (NO of 6.87g 3) 26H 2O, the Cu (NO of 1.49g 3) 23H 2O adds deionized water dissolving to 10ml in beaker, be made into maceration extract;
3) with γ-Al of 10g 2O 3Carrier is put into maceration extract, the following 60 ℃ of dippings of stirring condition 2 hours, 120 ℃ of dryings 5 hours;
4) at last 450 ℃ of following roastings 5 hours, the broken sieve of the solid that obtains is got 20～40 orders, nickel base crouse vent gas hydrogenation catalysts (the NiO mass content is respectively 15%, CuO mass content be 4%).Its activity data sees Table 1.
Embodiment 4:
A kind of preparation method of nickel base crouse vent gas hydrogenation catalysts, it comprises the steps:
1) with γ-Al 2O 3Carrier was 120 ℃ of dryings 5 hours, and is standby;
2) take by weighing the Ni (NO of 9.73g 3) 26H 2O, the Cu (NO of 1.58g 3) 23H 2O adds deionized water dissolving to 10ml in beaker, be made into maceration extract;
3) with γ-Al of 10g 2O 3Carrier is put into maceration extract, the following 60 ℃ of dippings of stirring condition 2 hours, 120 ℃ of dryings 5 hours;
4) at last 450 ℃ of following roastings 5 hours, the broken sieve of the solid that obtains is got 20～40 orders, nickel base crouse vent gas hydrogenation catalysts (the NiO mass content is respectively 20%, CuO mass content be 4%).Its activity data sees Table 1.
Table 1 different activities component addition is to conversion ratio and optionally influence
Catalyst NiO content (%) CuO content (%) T M (℃) T N (℃)
Embodiment 1 embodiment 2 embodiment 3 6 10 15 0 0 4 300 280 260 320 300 280
Embodiment 4 20 4 270 290
Embodiment 5:
A kind of preparation method of nickel base crouse vent gas hydrogenation catalysts, it comprises the steps:
1) γ-Al 2O 3Preliminary treatment: with γ-Al 2O 3Carrier was 100 ℃ of dryings 2 hours, and is standby;
2) choosing of raw material:
According to main active component, the shared mass percent of aluminium oxide be: main active component 6%, aluminium oxide (γ-Al 2O 3) 94%, wherein, main active component is a nickel oxide, (according to the shared mass percent of nickel oxide (NiO)) gets with the equimolar nickel nitrate of required NiO standby; [according to aluminium oxide (γ-Al 2O 3) shared mass percent] and get with the equimolar aluminum nitrate of required aluminium oxide standby;
Get and γ-Al 2O 3The deionized water of the saturated water adsorptive value equal volume of carrier, standby;
3) with 2) in nickel nitrate be dissolved in the deionized water, be made into maceration extract; With γ-Al 2O 3Carrier is put into maceration extract, the following 60 ℃ of dippings of stirring condition 2 hours, 100 ℃ of dryings 2 hours;
4), get nickel base crouse vent gas hydrogenation catalysts at last 350 ℃ of following roastings 2 hours.
Embodiment 6:
A kind of preparation method of nickel base crouse vent gas hydrogenation catalysts, it comprises the steps:
1) γ-Al 2O 3Preliminary treatment: with γ-Al 2O 3Carrier was 130 ℃ of dryings 5 hours, and is standby;
2) choosing of raw material:
According to main active component, the shared mass percent of aluminium oxide be: main active component 10%, aluminium oxide 90%, wherein, main active component is a nickel oxide, and (according to the shared mass percent of nickel oxide (NiO)) gets with the equimolar nickel nitrate of required NiO standby; [according to aluminium oxide (γ-Al 2O 3) shared mass percent] and get with the equimolar aluminum nitrate of required aluminium oxide standby;
Get and γ-Al 2O 3The deionized water of the saturated water adsorptive value equal volume of carrier, standby;
3) with 2) in nickel nitrate be dissolved in the deionized water, be made into maceration extract; With γ-Al 2O 3Carrier is put into maceration extract, the following 60 ℃ of dippings of stirring condition 2 hours, 130 ℃ of dryings 5 hours;
4), get nickel base crouse vent gas hydrogenation catalysts at last 450 ℃ of following roastings 5 hours.
Embodiment 7:
A kind of preparation method of nickel base crouse vent gas hydrogenation catalysts, it comprises the steps:
1) γ-Al 2O 3Preliminary treatment: with γ-Al 2O 3Carrier was 150 ℃ of dryings 10 hours, and is standby;
2) choosing of raw material:
According to main active component, the shared mass percent of aluminium oxide be: main active component 20%, aluminium oxide 80%, wherein, main active component is a nickel oxide, and (according to the shared mass percent of nickel oxide (NiO)) gets with the equimolar nickel nitrate of required NiO standby; [according to aluminium oxide (γ-Al 2O 3) shared mass percent] and get with the equimolar aluminum nitrate of required aluminium oxide standby;
Get and γ-Al 2O 3The deionized water of the saturated water adsorptive value equal volume of carrier, standby;
3) with 2) in nickel nitrate be dissolved in the deionized water, be made into maceration extract; With γ-Al 2O 3Carrier is put into maceration extract, the following 60 ℃ of dippings of stirring condition 2 hours, 150 ℃ of dryings 10 hours;
4), get nickel base crouse vent gas hydrogenation catalysts at last 550 ℃ of following roastings 10 hours.
Embodiment 8:
A kind of preparation method of nickel base crouse vent gas hydrogenation catalysts, it comprises the steps:
1) γ-Al 2O 3Preliminary treatment: with γ-Al 2O 3Carrier was 120 ℃ of dryings 6 hours, and is standby;
2) choosing of raw material:
According to main active component, auxiliary activity component, the shared mass percent of aluminium oxide be: main active component 18%, auxiliary activity component 2%, aluminium oxide 80%, wherein, main active component is a nickel oxide, the auxiliary activity component is a chromium oxide; (according to the shared mass percent of nickel oxide (NiO)) gets with the equimolar nickel nitrate of required NiO standby; [according to aluminium oxide (γ-Al 2O 3) shared mass percent] and get with the equimolar aluminum nitrate of required aluminium oxide standby; (according to the shared mass percent of auxiliary activity component) gets with the equimolar corresponding nitrate of required auxiliary activity component oxide standby; The corresponding nitrate of required auxiliary activity component oxide is: chromic nitrate;
Get and γ-Al 2O 3The deionized water of the saturated water adsorptive value equal volume of carrier, standby;
3) with 2) in nickel nitrate and the pairing nitrate of auxiliary activity component be dissolved in the deionized water, be made into maceration extract; With γ-Al 2O 3Carrier is put into maceration extract, the following 60 ℃ of dippings of stirring condition 2 hours, 120 ℃ of dryings 6 hours;
4), get nickel base crouse vent gas hydrogenation catalysts at last 450 ℃ of following roastings 6 hours.
Embodiment 9:
A kind of preparation method of nickel base crouse vent gas hydrogenation catalysts, it comprises the steps:
1) γ-Al 2O 3Preliminary treatment: with γ-Al 2O 3Carrier was 130 ℃ of dryings 4 hours, and is standby;
2) choosing of raw material:
According to main active component, auxiliary activity component, the shared mass percent of aluminium oxide be: main active component 10%, auxiliary activity component 5%, aluminium oxide 85%, wherein, main active component is a nickel oxide, the auxiliary activity component is cupric oxide and iron oxide, and cupric oxide, the shared mass percent of iron oxide are 2.5%; (according to the shared mass percent of nickel oxide (NiO)) gets with the equimolar nickel nitrate of required NiO standby; [according to aluminium oxide (γ-Al 2O 3) shared mass percent] and get with the equimolar aluminum nitrate of required aluminium oxide standby; (according to the shared mass percent of auxiliary activity component) gets with the equimolar corresponding nitrate of required auxiliary activity component oxide standby; The corresponding nitrate of required auxiliary activity component oxide is: copper nitrate, ferric nitrate;
Get and γ-Al 2O 3The deionized water of the saturated water adsorptive value equal volume of carrier, standby;
3) with 2) in nickel nitrate and the pairing nitrate of auxiliary activity component be dissolved in the deionized water, be made into maceration extract; With γ-Al 2O 3Carrier is put into maceration extract, the following 60 ℃ of dippings of stirring condition 2 hours, 130 ℃ of dryings 6 hours;
4), get nickel base crouse vent gas hydrogenation catalysts at last 450 ℃ of following roastings 6 hours.
Embodiment 10:
A kind of preparation method of nickel base crouse vent gas hydrogenation catalysts, it comprises the steps:
1) γ-Al 2O 3Preliminary treatment: with γ-Al 2O 3Carrier was 120 ℃ of dryings 5 hours, and is standby;
2) choosing of raw material:
According to main active component, auxiliary activity component, the shared mass percent of aluminium oxide be: main active component 12%, auxiliary activity component 2%, aluminium oxide 86%, wherein, main active component is a nickel oxide, the auxiliary activity component is chromium oxide and iron oxide, and chromium oxide, the shared mass percent of iron oxide are 1%; (according to the shared mass percent of nickel oxide (NiO)) gets with the equimolar nickel nitrate of required NiO standby; [according to aluminium oxide (γ-Al 2O 3) shared mass percent] and get with the equimolar aluminum nitrate of required aluminium oxide standby; (according to the shared mass percent of auxiliary activity component) gets with the equimolar corresponding nitrate of required auxiliary activity component oxide standby; The corresponding nitrate of required auxiliary activity component oxide is: chromic nitrate, ferric nitrate;
Get and γ-Al 2O 3The deionized water of the saturated water adsorptive value equal volume of carrier, standby;
3) with 2) in nickel nitrate and the pairing nitrate of auxiliary activity component be dissolved in the deionized water, be made into maceration extract; With γ-Al 2O 3Carrier is put into maceration extract, the following 60 ℃ of dippings of stirring condition 2 hours, 110 ℃ of dryings 3 hours;
4), get nickel base crouse vent gas hydrogenation catalysts at last 400 ℃ of following roastings 3 hours.

Claims (3)

1. nickel base crouse vent gas hydrogenation catalysts, it is characterized in that it is made of main active component, auxiliary activity component, three kinds of components of aluminium oxide, the shared mass percent of each component is: main active component 6%～20%, auxiliary activity component 0%～5%, 80%～94%, three kinds of component sums of aluminium oxide are 100%; Wherein, main active component is a nickel oxide, and the auxiliary activity component is any one or any one the above mixture in chromium oxide, cupric oxide, the iron oxide, during any one above mixture, is any proportioning between the oxide.
2. a kind of nickel base crouse vent gas hydrogenation catalysts according to claim 1 is characterized in that: the shared mass percent of main active component: 10%～18%.
3. the preparation method of a kind of nickel base crouse vent gas hydrogenation catalysts as claimed in claim 1 is characterized in that it comprises the steps:
1) γ-Al 2O 3Preliminary treatment: with γ-Al 2O 3Carrier was 100 ℃～150 ℃ dryings 2～10 hours, and is standby;
2) choosing of raw material: get and γ-Al 2O 3The deionized water of the saturated water adsorptive value equal volume of carrier, standby;
According to main active component, auxiliary activity component, the shared mass percent of aluminium oxide be: main active component 6%～20%, auxiliary activity component 0%～5%, aluminium oxide 80%～94%, wherein, main active component is a nickel oxide, the auxiliary activity component is any one or any one the above mixture in chromium oxide, cupric oxide, the iron oxide, during any one above mixture, between the oxide any proportioning; Get with the equimolar nickel nitrate of required NiO standby; Get with the equimolar aluminum nitrate of required aluminium oxide standby; Get with the equimolar corresponding nitrate of required auxiliary activity component oxide standby;
3) with 2) in nickel nitrate and the pairing nitrate of auxiliary activity component be dissolved in the deionized water, be made into maceration extract; With γ-Al 2O 3Carrier is put into maceration extract, the following 60 ℃ of dippings of stirring condition 2 hours, 100 ℃～150 ℃ dryings 2～10 hours;
4), get nickel base crouse vent gas hydrogenation catalysts at last 350 ℃～550 ℃ following roastings 2～10 hours.
CNA2007100527880A 2007-07-19 2007-07-19 Nickel base crouse vent gas hydrocatalyst and manufacturing process thereof Pending CN101108348A (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102380311A (en) * 2010-09-01 2012-03-21 中国石油化工股份有限公司 Gasoline adsorption desulfuration regeneration smoke treatment method and tail gas hydrogenation catalyst preparation method thereof
CN101559369B (en) * 2009-05-21 2013-12-25 中国矿业大学(北京) Supported catalyst for coal pyrolysis hydrogen production and preparation method thereof
CN108970618A (en) * 2017-05-31 2018-12-11 中国石油化工股份有限公司 Catalyst for recovering sulfur and preparation method thereof

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101559369B (en) * 2009-05-21 2013-12-25 中国矿业大学(北京) Supported catalyst for coal pyrolysis hydrogen production and preparation method thereof
CN102380311A (en) * 2010-09-01 2012-03-21 中国石油化工股份有限公司 Gasoline adsorption desulfuration regeneration smoke treatment method and tail gas hydrogenation catalyst preparation method thereof
CN102380311B (en) * 2010-09-01 2013-12-25 中国石油化工股份有限公司 Gasoline adsorption desulfuration regeneration smoke treatment method and tail gas hydrogenation catalyst preparation method thereof
CN108970618A (en) * 2017-05-31 2018-12-11 中国石油化工股份有限公司 Catalyst for recovering sulfur and preparation method thereof

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