CN101890351A - Eggshell type nickel-based catalyst - Google Patents
Eggshell type nickel-based catalyst Download PDFInfo
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- CN101890351A CN101890351A CN2009100845488A CN200910084548A CN101890351A CN 101890351 A CN101890351 A CN 101890351A CN 2009100845488 A CN2009100845488 A CN 2009100845488A CN 200910084548 A CN200910084548 A CN 200910084548A CN 101890351 A CN101890351 A CN 101890351A
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Abstract
The invention discloses an eggshell type nickel-based catalyst and a preparation method and application thereof, belonging to the technical field of nickel-based catalysts and aiming at developing the eggshell type nickel-based catalyst for meeting the demand. The research shows that the eggshell type nickel-based catalyst can be prepared by dissolving nickel salt into ammonia water solution, loading the mixed solution on a catalyst carrier by adopting a spraying or immersing mode, drying, roasting and reducing. The active component of nickel is mostly centralized in an area from the surface of the carrier to the part of 0.7mm below the surface and can remarkably improve the conversion rate and the selectivity of the catalyst. The invention can be applied to the technical fields of hydrogen addition and trace amount of carbon monoxide removal from hydrogen and the like.
Description
Technical field
The present invention relates to a kind of nickel-base catalyst, specifically, relate to a kind of nickel component and be distributed in eggshell type nickel-based catalyst in the catalyst perimeter.
Background technology
In petrochemical industry, hydrogenation reaction is used noble metal carrier catalyst and non-noble metal supported catalyst usually, the noble metal catalyst of working load palladium in C-2-fraction and C 3 fraction selective hydrogenation for example, the non-precious metal catalyst of working load nickel usually in gasoline hydrogenation and the benzene hydrogenation.In order to make full use of expensive noble metal and to improve activity of such catalysts and selectivity, generally noble metal carrier catalyst is prepared into egg-shell catalyst, and along with the continuous development of catalyst preparation technology, people do the eggshell of carried noble metal more and more thinner.
For example, US 5648576 discloses the method that a kind of carbon two or carbon three alkynes gas phases are selectively hydrogenated into corresponding alkene.This method is in the presence of hydrogen, and gas phase treatment contains the material of acetylene or propine allene on the catalyst of sphere or bar shaped.Catalyst system therefor contains palladium and at least a periodic table of elements IB family metal (preferred silver) and aluminium oxide, and wherein the weight ratio of IB family metal and palladium is that 0.05～0.4, at least 80% palladium and at least 80% IB family Metal Distribution are being r by radius
1(mean radius that is equivalent to the catalyst of sphere or extrusion molding) and radius are r
2(r
2At least equal 0.8r
1) sphere or catalyst volume that the face of cylinder limited within.Active component palladium and IB family metal are to adopt infusion process to load on the carrier.
Yet the active component of also not seeing at present about non-precious metal catalyst especially nickel-base catalyst is the report that eggshell type distributes.About the research of nickel-base catalyst, pay close attention to more be active component nickel be nanoparticle be distributed on the carrier and the reduction act of nickel to the influence of catalyst performance.For example, waited comparative analysis quietly suddenly nano nickel catalyst and traditional Raney's nickel catalyst, and summarized the multiple preparation method of nano nickel catalyst emphatically and looked forward to application prospect (present Research of catalyzer for hydrogenization of nano nickel and the prospect of nano nickel catalyst, powder metallurgy industry, 2006, the 16th the 1st phase of volume, the 45th～48 page).The performance of catalyst is not only relevant, also relevant with the distribution of nickel in the carrier duct with the effect power of the particle size of active component nickel and nickel and carrier.For example, if reactant molecule is difficult to enter depths, catalyst duct, the utilization rate that is distributed in the nickel at hole depth place so may be lower.The product molecule that generates in the reaction of depths, catalyst duct further reacts as can not in time spreading out, and influences selection of catalysts on the one hand, will influence life of catalyst on the other hand.Especially internally be diffused as the reaction of control step, wish that reaction occurs in the position that is beneficial to reactant and product diffusion, general hope occurs in catalyst coating, and the palladium as the eggshell type palladium catalyst is distributed in the eggshell type nickel-based catalyst in the extremely thin top layer.In addition, in the cost of nickel-base catalyst, the large percentage that the cost of active component nickel is shared if the nickel component that is distributed in the depths, duct that utilization rate is not high moves in the zone near catalyst coating, can significantly improve activity of such catalysts and selectivity undoubtedly.Thereby, develop a kind of eggshell type nickel-based catalyst at present and have very large learning value and remarkable economic efficiency.
Summary of the invention
The present invention is in order to satisfy at present to developing the demand of eggshell type nickel-based catalyst, carried out intensive research, through discovering, by regulating active component nickel distribution situation on catalyst carrier, make the active component nickel major part concentrate on carrier surface in the zone of half degree of depth of central shaft, can significantly improve the conversion ratio and the selectivity of catalyst.
The present invention realizes that the technical scheme of above-mentioned purpose is:
Eggshell type nickel-based catalyst of the present invention is made up of carrier and the active component nickel that loads on the carrier, weight and weight percent meter with catalyst, the nickel content of described catalyst is that the nickel more than 5%～60%, 90% is distributed in carrier surface to the caltalyst of degree of depth 0.7mm.
Preferably, the nickel more than 95% is distributed in carrier surface to the caltalyst of degree of depth 0.7mm.
Preferably, with the weight and the weight percent meter of catalyst, described catalyst contains 10%～40% nickel.
Preferably, described method for preparing catalyst is: with the soluble salts of active components dissolving, solvent is the mixture of ammoniacal liquor and water, and the weight ratio of ammoniacal liquor and water is 1: 0～0.5, with the spray solution or the impregnated carrier of gained, and drying, decomposition and reduction then.
Preferably, described carrier is a two or more mixture in aluminium oxide, silica, active carbon, titanium dioxide or molecular sieve or these carriers.
The invention provides a kind of method for preparing eggshell type nickel-based catalyst, this method is simple to operation, and preparation process is few, and repeatability is reliable, and the field that prepared Ni-based loaded catalyst is used for many hydrogenation has higher activity and selectivity.
Specific solution is, with the soluble salts of active components dissolving, solvent is the mixture of ammoniacal liquor and water, and the weight ratio of ammoniacal liquor and water is 1: 0～0.5, and with the spray solution or the impregnated carrier of gained, dry then, decomposition is also reduced.Described ammoniacal liquor is commercially available concentrated ammonia liquor, and the mass percent concentration of ammoniacal liquor is generally 25%～28%, with NH
3Meter.When the ratio of water was 0, solvent was independent ammoniacal liquor, not dilute with water.
Preferably, load there is the catalyst carrier of nickel salt in 100 ℃～150 ℃ oven dry.
Preferably, the reduction temperature of described catalyst is 200 ℃～500 ℃, and the time is 3～8h.
The nickel salt that catalyst of the present invention uses can be any soluble nickel salt, comprises nickel nitrate, nickelous carbonate, basic nickel carbonate, nickel acetate, citric acid nickel, nickelous sulfate etc. for example.
Catalyst of the present invention also can comprise other active component and/or auxiliary agent.For example introduce Acidity of Aikalinity and nickel and the carrier interactions of alkaline components, improve catalyst activity and optionally effect thereby play to improve catalyst.For example introduce molybdenum and/or tungsten component,, make the nickel particle thinner and more even to disperse the nickel component better.
The invention provides the multiple application of eggshell type nickel-based catalyst.
Catalyst of the present invention also can be used for various hydrogenation reactions.Eggshell type nickel-based catalyst for example of the present invention can be used for pyrolysis gasoline hydrogenation, can be used for the prepared from benzene and hydrogen cyclohexane, and it is C 5 hydrogenated etc. to can be used for carbon four.In various hydrogenation processes, can select suitable hydrogenation technique condition according to the technical conditions and the experience of this area.Catalyst of the present invention does not have specific (special) requirements.
Catalyst of the present invention can be used for removing the carbon monoxide in the hydrogen.Contain carbon monoxide in the hydrogen, can use the catalyst poisoning of this hydrogen usually or reduce activity, thereby the carbon monoxide in the hydrogen need be changed into the methane that usually catalyst is not had influence.For example, the reactor of the hydrogen that will contain micro CO by catalyst of the present invention is housed is being methane with co hydrogenation wherein.
The nickel component of existing nickel-base catalyst is distributed on the whole carrier, and in catalyst of the present invention, most of nickel component is distributed in the housing of carrier, and the centronucleus part does not have the nickel component substantially, and this distribution mode helps various catalytic reactions undoubtedly.Reactant arrives active sites easily, and especially internally diffusion reaction is more favourable, and the product that reaction generates can leave active sites quickly, thereby helps improving activity of such catalysts, also helps improving selection of catalysts.Studies show that catalyst of the present invention has higher conversion ratio and selectivity to synthetic fatty amine.Method for preparing catalyst of the present invention is simple to operation, and repeatability is high.
The specific embodiment
Further explain Catalysts and its preparation method of the present invention in the mode of embodiment below, but the present invention is not limited to this.
Embodiment 1
Six water nickel nitrates are dissolved in make maceration extract in the ammoniacal liquor, used ammoniacal liquor is mixed with weight ratio by commercially available 25%～28% ammoniacal liquor and water at 1: 0.5, adopt equivalent impregnation method dipping spherical alumina carrier, alumina support is produced by the Beijing Chemical Research Institute, and specific area is 250m
2/ g, pore volume are 0.44ml/g, and drying is 4 hours under 120 ℃, 420 ℃ of following roastings 4 hours, reduce 8 hours down at 350 ℃ with hydrogen then, make catalyst A, in the weight of catalyst, contain the nickel of 10 weight %.The catalyst spheres particle is cut in half, can be clear that, the nickel component is distributed in carrier surface to the caltalyst of degree of depth 0.7mm, can't see the nickel component substantially in the spherical nucleus of the degree of depth greater than 0.7mm.
Embodiment 2
Six water nickel nitrates are dissolved in make maceration extract in the ammoniacal liquor, used ammoniacal liquor is mixed with weight ratio by commercially available 25%～28% ammoniacal liquor and water at 1: 0.3, adopt equivalent impregnation method dipping spherical alumina carrier, alumina support is produced by the Beijing Chemical Research Institute, and specific area is 274m
2/ g, pore volume is 0.45ml/g, earlier 60 ℃ dry 4 hours down, then 120 ℃ dry 4 hours down, again 420 ℃ of following roastings 4 hours, and then flood drying, roasting equally one time, reduced 8 hours down at 375 ℃ with hydrogen, make catalyst B,, contain the nickel of 20 weight % in the weight of catalyst.The catalyst spheres particle is cut in half, can be clear that, the nickel component is distributed in carrier surface to the caltalyst of degree of depth 0.7mm, can't see the nickel component substantially in the spherical nucleus of the degree of depth greater than 0.7mm.
Embodiment 3
Six water nickel nitrates are dissolved in make maceration extract in the ammoniacal liquor, used ammoniacal liquor is mixed with weight ratio by commercially available 25%～28% ammoniacal liquor and water at 1: 0.1, adopt spray method to spray the spherical alumina carrier, alumina support is produced by the Beijing Chemical Research Institute, and specific area is 264m
2/ g, pore volume are 0.45ml/g, earlier 60 ℃ dry 4 hours down, then 120 ℃ dry 4 hours down, 420 ℃ of following roastings 4 hours, repeat said process then again, reduced 8 hours down at 375 ℃ with hydrogen at last, make catalyst C,, contain the nickel of 22 weight % in the weight of catalyst.The catalyst spheres particle is cut in half, can be clear that, the nickel component is distributed in carrier surface to the caltalyst of degree of depth 0.7mm, can't see the nickel component in the spherical nucleus of the degree of depth greater than 0.7mm.
Embodiment 4
Six water nickel nitrates are dissolved in make maceration extract in the ammoniacal liquor, used ammoniacal liquor is mixed with weight ratio by commercially available 25%～28% ammoniacal liquor and water at 1: 0.2, adopt spray method to spray the spherical alumina carrier, alumina support is produced by the Beijing Chemical Research Institute, and specific area is 264m
2/ g, pore volume are 0.45ml/g, and drying is 4 hours under 120 ℃, again 420 ℃ of following roastings 4 hours, reduce 8 hours down at 375 ℃ with hydrogen, make catalyst D, in the weight of catalyst, contain the nickel of 12 weight %.The catalyst spheres particle is cut in half, can be clear that, the nickel component is distributed in carrier surface to the caltalyst of degree of depth 0.7mm, can't see the nickel component in the spherical nucleus of the degree of depth greater than 0.7mm.
Embodiment 5
Six water nickel nitrates are dissolved in make maceration extract in the ammoniacal liquor, used ammoniacal liquor is commercially available 25%～28% ammoniacal liquor, adopts equivalent impregnation method dipping spherical alumina carrier, and alumina support is produced by the Beijing Chemical Research Institute, and specific area is 158m
2/ g, pore volume is 0.8ml/g, first following dry 4 hours at 60 ℃, then 120 ℃ dry 4 hours down, again 420 ℃ of following roastings 4 hours, repeat above-mentioned dipping, drying and roasting process three times then, reduced 8 hours down at 390 ℃ with hydrogen, make catalyst E,, contain the nickel of 38 weight % in the weight of catalyst.The catalyst spheres particle is cut in half, can be clear that, the nickel component is distributed in carrier surface to the caltalyst of degree of depth 0.7mm, can't see the nickel component substantially in the spherical nucleus of the degree of depth greater than 0.7mm.
Comparative example 1
Six water nickel nitrates are dissolved in make the aqueous solution in the water, adopt equivalent impregnation method dipping spherical alumina carrier, alumina support is produced by the Beijing Chemical Research Institute, and specific area is 250m
2/ g, pore volume are 0.44ml/g, and drying is 4 hours under 120 ℃, again 420 ℃ of following roastings 4 hours, reduce 8 hours down at 350 ℃ with hydrogen, make catalyst F, in the weight of catalyst, contain the nickel of 10 weight %.The catalyst spheres particle is cut in half, can be clear that, the nickel component is evenly distributed in the catalyst whole particle substantially.
Comparative example 2
Method according to US2008118642A1 prepares catalyst G.Six water nickel nitrates are dissolved in make the aqueous solution in the water, adopt spray method dipping spherical alumina carrier, alumina support is produced by the Beijing Chemical Research Institute, and specific area is 250m
2/ g, pore volume are 0.44ml/g, and drying is 4 hours under 120 ℃, again 420 ℃ of following roastings 4 hours, reduce 8 hours down at 350 ℃ with hydrogen, make catalyst G, in the weight of catalyst, contain the nickel of 10 weight %.The catalyst spheres particle is cut in half, can see that the nickel component is distributed in carrier surface substantially to the caltalyst of degree of depth 0.7mm.
Embodiment 6
Present embodiment is hydrogenated to example fully with cracking c_5 and explains the application of catalyst of the present invention in field of hydrogenation, but application of the present invention is not limited to this.
Employed cracking c_5 material is provided by Yanshan Petrochemical company, and its composition is listed in table 1.
Catalyst B being packed in the fixed bed reactors, the cracking c_5 material is mixed the back with hydrogen and stream enters bed from the bed lower end, is that 60 ℃, hydrogen to oil volume ratio are 60, the volume hourly space velocity is 2h in inlet temperature
-1Catalytic performance with evaluate catalysts under the 3MPa.Composition with material behind gas chromatographic analysis raw material and the hydrogenation.Result of the test shows that behind the hydrogenation, monoolefine content is 0.3 weight % in carbon five materials, does not detect diolefin, thereby catalyst B of the present invention can be hydrogenated into alkane fully with the cracking c_5 raw material.
Table 1
Embodiment 7
Present embodiment is explained catalyst of the present invention application in the micro CO in removing hydrogen.
Respectively with catalyst A, F and the G fixed-bed tube reactor of packing into of preparation, under 400 ℃ of temperature and pressure 3.0MPa, with hydrogen reducing 6 hours, the hydrogen volume air speed was 2500h
-1, be cooled to 170 ℃ of reaction temperatures, feed unstripped gas, this unstripped gas contains 95% H
2, 0.4% carbon monoxide and the methane of surplus, the feed gas volume air speed is 10000h
-1, carrying out evaluation test, the content of carbon monoxide is listed in table 2 with evaluation result in the assay products.
Table 2
| Catalyst | Outlet CO content, ppm |
| A | ?＜1ppm |
| F | ?85ppm |
| G | ?38ppm |
From the result of the test of table 2 as can be seen, under identical process conditions, although the nickel content of catalyst is identical,, catalyst A of the present invention has advantages of high catalytic activity.Different and the crystal grain differences that produce that difference only is that the distribution mode of nickel component is different and the preparation process parameter is regulated, so catalyst activity and optionally distinguish and derive from own character of catalyst and preparation method thereof.
Claims (5)
1. eggshell type nickel-based catalyst, it is characterized in that, described catalyst is made up of carrier and the active component nickel that loads on the carrier, weight and weight percent meter with catalyst, the nickel content of described catalyst is that the nickel more than 5%～60%, 90% is distributed in carrier surface to the caltalyst of degree of depth 0.7mm.
2. nickel-base catalyst as claimed in claim 1 is characterized in that, the nickel more than 95% is distributed in carrier surface to the caltalyst of degree of depth 0.7mm.
3. nickel-base catalyst as claimed in claim 1 is characterized in that, with the weight and the weight percent meter of catalyst, described catalyst contains 10%～40% nickel.
4. as the described nickel-base catalyst of one of claim 1-3, it is characterized in that, described method for preparing catalyst is: soluble salts of active components is dissolved, solvent is the mixture of ammoniacal liquor and water, the weight ratio of ammoniacal liquor and water is 1: 0～0.5, with the spray solution or the impregnated carrier of gained, drying, decomposition and reduction then.
5. nickel-base catalyst as claimed in claim 1 is characterized in that, described carrier is a two or more mixture in aluminium oxide, silica, active carbon, titanium dioxide or molecular sieve or these carriers.
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| CN115672333A (en) * | 2022-10-12 | 2023-02-03 | 中国石油大学(华东) | Ni-series eggshell-type catalyst, preparation method and method for selective hydrogenation and olefin removal of reformed oil |
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