CN102641740A - Diene selective hydrogenation catalyst and preparation method - Google Patents
Diene selective hydrogenation catalyst and preparation method Download PDFInfo
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Abstract
The invention discloses a diene selective hydrogenation catalyst, wherein alumina or modified alumina serves as a carrier, nickel serves as an active component, and alkali metals or alkaline earth metals, VIB metals, X metals and rare earth metals serve as auxiliaries; and when the total weight of the catalyst is metered by 100% in weight percentage, the catalyst contains 10% to 20% of nickel oxide, 0.5% to 5% of the alkali metals and/or the alkaline earth metals, 1% to 7% of oxide of VIB elements, 0.5%to 5% of oxide of auxiliary X metal elements and 2% to 5% of oxide of rare earth elements, wherein the X metals is one or more out of cadmium, zinc, copper and silver. The catalyst has very high hydrogenation activity and selectively under a relatively low temperature, is good in stability, and is mainly applicable to diene selective hydrogenation reaction of pyrolysis gasoline and FCC gasoline.
Description
Technical field
The present invention relates to a kind of diene selective hydrogenation nickel-base catalyst and preparation method, this catalyst mainly is applicable to diolefin selective hydrogenation reaction in the oil product, is particularly useful for the selective hydrogenation of diolefin in drippolene and the FCC gasoline fraction.
Background technology
Contain a large amount of height unsaturated hydrocarbons in drippolene and the FCC gasoline, as: diolefin, styrene etc., these materials are polymerization reaction take place very easily at high temperature; Form oligomer and colloid, influence the stability of oil product, and also can in last handling process, on the surfaces externally and internally of catalyst, assemble owing to the polymerization rubber; The duct of blocking catalyst; The activated centre of covering catalyst, thus the rapid deactivation of catalyst caused, catalyst is shortened service life.Therefore before carrying out following process, need carry out the cryogenic selective hydrogenation to drippolene and FCC gasoline, making diolefin saturated is corresponding monoolefine.
Industry is at present gone up the selective hydrocatalyst of using and mainly contained two kinds: a kind of is noble metal catalyst, is active component with Pd mainly, and catalyst hydrogenation activity is higher; Serviceability temperature is low; But price is comparatively expensive, and impurity abilities such as anti-arsenic, anticol matter are relatively poor, and water repelling property is also bad.Another kind is a non-precious metal catalyst; It mainly is active component with Ni; Catalyst hydrogenation activity is relatively low, and serviceability temperature is higher, but price is comparatively cheap; And because the influence of factors such as architectural difference and tenor height, catalyst has certain appearance arsenic, anticol mass-energy power and water-resistant capacity.Receive that domestic gasoline stocks is changeable, the influence of device and mode of production difference; Impurity content is rising trend gradually in the raw material; Make noble metal catalyst show inadaptability, the phenomenon that the cycle of operation shortens occurs, so the market of nickel-base catalyst enlarges rapidly raw material.
CN101302439A has reported a kind of catalyst, and at 3～10nm, specific area is 300～400m with the aperture
2The aluminium oxide of/g is a carrier, load nickel oxide, molybdenum oxide and the third metal oxide.Wherein nickel oxide content is 1.2～11.2wt% of carrier, and molybdenum oxide content is 1.1～15.4wt% of carrier, and the third metal oxide content is 1.1～7.8wt% of carrier, can be cupric oxide, cobalt oxide, silver oxide, iron oxide or bismuth oxide.This catalyst has stronger surface acidity, mainly is applicable to hydrocracking reaction.
CN1035240C discloses a kind of methyl iso-butyl ketone (MIBK)/DIBK synthetic catalyst, is carrier with the aluminium oxide, is active component with cupric oxide or zinc oxide, nickel oxide, magnesia.Catalyst reaction temperatures is higher, has good activity and selectivity for synthesize methyl-isobutyl ketone and DIBK.
US6750374 has reported a kind of prepared from benzene and hydrogen cyclohexane catalyst; This catalyst is a carrier with aluminium oxide or silica; Load Ni, Cu and the third component (comprising among Cr, Mg, Fe, Co, Zn, Mo, the Sn at least a); Wherein Ni content is 15～35% of catalyst, and Cu content is that the 1～15%, the 3rd constituent content of catalyst is 0～5% of a catalyst.This catalyst is full hydrogenation catalyst, and light-off temperature high (feeding temperature is greater than 100 ℃) is mainly gas-solid phase reaction.
At present, Ni-based selective hydrocatalyst also exists reaction temperature higher, the problem that activity, selectivity and stability have much room for improvement.
Summary of the invention
The object of the invention is intended to develop a kind of diene selective hydrogenation catalyst and preparation method; Particularly a kind of Ni-based diolefin selective hydrogenation catalyst; This catalyst is applicable to the reactions such as selective hydrogenation of diolefin in drippolene, the FCC gasoline fraction, can realize the selective hydrogenation of diolefin at a lower temperature.
Catalyst provided by the invention is a carrier with aluminium oxide or modified aluminas, is 100wt% in the catalyst weight; Contain nickel oxide 10～20wt%, preferred 12～18wt%, VIB element oxide 1～7wt%; Preferred 2～4wt%, rare earth oxide 2～5wt%, auxiliary agent X metallic element oxide 0.5～5.0wt%; Preferred 1～3wt%, X metal are one or more in cadmium, zinc, copper, the silver; Alkali metal and/or alkaline-earth metal 0.5～5wt%, preferred 1～4wt%.Specific surface area of catalyst is 70～150m
2/ g, pore volume are 0.30～0.65ml/g, mainly are applicable to the selective hydrogenation of diolefin in drippolene, the FCC gasoline fraction.
Said vib metal element can be one or more in chromium, molybdenum, the tungsten, preferably chromium and/or molybdenum.The adding of chromium, molybdenum and/or tungsten can suppress the generation of nickel aluminate, improves active component and carrier interactions, improves the active component utilization rate.
The preferred La of said rare earth element, Ce can be wherein one or more.The adding of rare earth element can weaken active component nickel to the absorption affinity of monoolefine and benzene, and has eliminated the tendency that forms nickel aluminate, has improved the quantity at catalyst hydrogenation activity center, helps the raising of catalyst selectivity.
Said X metallic element can be one or more in cadmium, zinc, copper, the silver, and the adding of this component can improve pore canal structure of catalyst, improves catalyst activity.
Described alkali metal and/or alkaline-earth metal preferably are selected from Li, K, Mg.Must contain alkali metal and/or alkaline-earth metal in the catalyst of the present invention, like among Li, K, the Mg one or more.The adding of this component can be regulated the carrier hole structure, improves the decentralization of active component nickel.Alkali metal and/or alkaline-earth metal can prepare in the process at alumina support and add, and also can in the activity component impregnation process, introduce.
Each constituent content must be controlled at proper range in the catalyst of the present invention.Wherein, the content of nickel oxide is low excessively, and the active sites that catalyst can provide is very few, and too high levels then makes the nickel crystallite gathering grow up easily, and is all unfavorable to the raising of catalyst activity.The adding of VIB element oxide can suppress the generation of nickel aluminate; Improve active component and carrier interactions, improve the active component utilization rate, if can occupy the carrier duct but its addition is too high; Reduce specific surface area of catalyst, unfavorable to catalyst activity.
The present invention is the preparation method of limiting catalyst not, can be immersion process for preparing, preferred equi-volume impregnating; Said alkali metal compound and alkaline earth metal compound can be its halide, nitrate, preferred its nitrate, and the adding of alkali metal or alkaline-earth metal can be in the preparing carriers process, to add, and in maceration extract, adds in the time of also can being Preparation of Catalyst.Modified aluminas can be the modified aluminas that often uses in the prior art, normally metal or nonmetal is added to reshaping roasting in the boehmite.
The present invention also provides a kind of this Preparation of catalysts method; It is characterized in that the compound of active component nickel, VIB element, rare earth element, alkali metal, alkaline-earth metal and X metallic element is added in the entry, fully after the dissolving, maceration extract pH value is adjusted to 3～5; Alumina support impregnated in the maceration extract; Each component is carried on the alumina support, after 100～120 ℃ of dryings, makes at 300～450 ℃ of following roasting 4～6h.
The preparation process of this alumina support can for: with the boehmite extruded moulding, 100～120 ℃ of oven dry, 800～1000 ℃ of roasting 3～6h.
The present invention also provides another kind of this Preparation of catalysts method; It is characterized in that the compound of active component nickel, VIB element, rare earth element and X metallic element is added in the entry, fully after the dissolving, maceration extract pH value is adjusted to 3～5; Modified aluminium oxide supports impregnated in the maceration extract; Each component is carried on the modified aluminium oxide supports, after 100～120 ℃ of dryings, makes at 300～450 ℃ of following roasting 4～6h.This modified aluminium oxide supports is meant in boehmite extruded moulding process and adds alkali metal and/or alkaline earth metal compound carries out modification to alumina precursor, 100～120 ℃ of oven dry then, 800～1000 ℃ of carriers that roasting 3～6h makes.
The nickel that adds in the catalyst preparation process, rare earth element, X element compound can be sulfate, nitrate, halide, acetate of its solubility etc., preferably its nitrate.
Said VIB element is its water-soluble compound, and preferred its ammonium salt is like ammonium dichromate, metamolybdic acid ammonium, ammonium molybdate, ammonium tungstate etc.
Catalyst provided by the invention preferably adds ability water-soluble big molecular organic complexing agent or organic sequestering agent when the preparation maceration extract; The adding of organic complexing agent can improve the decentralization of active component on carrier and the stability of maceration extract; Improve activity of such catalysts and stability; Preferred complexing agent and/or chelating agent have polybasic carboxylic acid class such as citric acid; Polyalcohols such as triethylene-glycol, ethylene glycol, polynary amine such as EDTA, ethylenediamine etc., the mol ratio of organic complexing agent and/or chelating agent and active component nickel is 1: 5～1: 10.
The catalyst that makes through said method also need reduce and Passivation Treatment before use, further improves diolefin hydrogenation activity, selectivity and the long period stability of catalyst of the present invention.
Nickel-base catalyst of the present invention all can use in fixed bed reactors, can be applied to drippolene, the reaction of FCC gasoline selective hydrogenation of diolefin as.
Catalyst of the present invention has good low temperature active, and the raw material applicability is strong, for drippolene C
5～C
9Diene in cut and the FCC gasoline fraction all has higher hydrogenation activity and hydrogenation selectivity.
Enumerate specific embodiment below and further set forth the characteristics and the catalytic performance of catalyst of the present invention, embodiment does not constitute any qualification to practical range of the present invention just for the present invention is described.
The specific embodiment
Analytical method and standard:
Oil distillation: adopt oil product test method SYB-2110-60 to measure;
Iodine value: adopt the ICl method to measure, show with gram iodine/100 gram oil meters;
Diene: adopt apple acid anhydrides method to measure, show with gram iodine/100 gram oil meters;
Arsenic content: adopt the DV-4300 Atomic Emission Spectrometer AES to measure;
Sulfur content: adopt the WK-2B Microcoulomb instrument to measure;
Colloid: adopt oil product test method SYB-2103-60 to measure;
Specific surface and pore-size distribution: adopt the Tristar-3000 instrument, measure with static state low temperature nitrogen adsorption capacity method.
The tenor of catalyst is measured: adopt Varian AA240FS atomic absorption spectrometry.
Embodiment 1
With boehmite, lithium nitrate solution, nitric acid and water mixer kneader, behind the extruded moulding, in 120 ℃ of dry 6h, 900 ℃ of roasting 5h make catalyst carrier Z
AThe mixed impregnant liquor of preparation nickel nitrate, zinc nitrate, ammonium molybdate, lanthanum nitrate, EDTA, triethylene-glycol, wherein the mol ratio of EDTA, triethylene-glycol and active component nickel is 1: 5, regulates maceration extract pH value to 4 then, impregnated in 100gZ
AOn the carrier, ageing 12h, 120 ℃ of oven dry, 400 ℃ of roasting 4h make the finished catalyst C1 that contains nickel oxide 12wt%, lithia 1.0wt%, zinc oxide 3.0wt%, molybdenum oxide 3.0wt%, lanthana 3.0wt%.
Embodiment 2
With boehmite, nitric acid and water mixer kneader, behind the extruded moulding, in 120 ℃ of dry 6h, 950 ℃ of roasting 5h make catalyst carrier Z
BThe mixed impregnant liquor of preparation nickel nitrate, potassium nitrate, cadmium nitrate, ammonium molybdate, cerous nitrate, triethylene-glycol, wherein the mol ratio of triethylene-glycol and active component nickel is 1: 7, regulates maceration extract pH value to 3, impregnated in 100gZ
BOn the carrier, ageing 12h, 120 ℃ of oven dry, 450 ℃ of roasting 4h make the finished catalyst C2 that contains nickel oxide 13wt%, potassium oxide 1.6wt%, cadmium oxide 3.0wt%, molybdenum oxide 2.5wt%, cerium oxide 3.0wt%.
Embodiment 3
The preparing carriers method is with embodiment 2.The mixed impregnant liquor of preparation nickel nitrate, lithium nitrate, potassium nitrate, copper nitrate, ammonium metatungstate, lanthanum nitrate, citric acid, wherein the mol ratio of citric acid and active component nickel is 1: 8, regulates maceration extract pH value to 4, impregnated in 100gZ
BOn the carrier, ageing 12h, 120 ℃ of oven dry, 400 ℃ of roasting 4h make the finished catalyst C3 that contains nickel oxide 14.5wt%, lithia 1.0wt%, potassium oxide 1.5wt%, cupric oxide 2.5wt%, tungsten oxide 3.5wt%, lanthana 3.5wt%.
Embodiment 4
Carrier Z
BThe preparation method is with embodiment 2.The mixed impregnant liquor of preparation nickel nitrate, potassium nitrate, silver nitrate, ammonium molybdate, lanthanum nitrate, cerous nitrate, ethylene glycol, wherein the mol ratio of ethylene glycol and active component nickel is 1: 7, regulates maceration extract pH value to 5, impregnated in 100gZ
BOn the carrier, ageing 12h, 120 ℃ of oven dry, 350 ℃ of roasting 4h make the finished catalyst C4 that contains nickel oxide 13.5wt%, potassium oxide 2.0wt%, silver oxide 2.5wt%, molybdenum oxide 4.0wt%, lanthana 2.0wt%, cerium oxide 1.5wt%.
Embodiment 5
Carrier Z
BThe preparation method is with embodiment 2.The mixed impregnant liquor of preparation nickel nitrate, magnesium nitrate, zinc nitrate, ammonium dichromate, cerous nitrate, EDTA, wherein the mol ratio of EDTA and active component nickel is 1: 6, regulates maceration extract pH value to 4.5, impregnated in 100gZ
BOn the carrier, ageing 12h, 120 ℃ of oven dry, 430 ℃ of roasting 5h make the finished catalyst C5 that contains nickel oxide 15wt%, magnesia 1.5wt%, zinc oxide 1.5wt%, chromium oxide 2.0wt%, cerium oxide 4.0wt%.
Embodiment 6
Carrier Z
BThe preparation method is with embodiment 2.The mixed impregnant liquor of preparation nickel nitrate, potassium nitrate, magnesium nitrate, zinc nitrate, silver nitrate, ammonium molybdate, lanthanum nitrate, triethylene-glycol, wherein the mol ratio of triethylene-glycol and active component nickel is 1: 9, regulates maceration extract pH value to 4, impregnated in 100gZ
BOn the carrier; Ageing 12h; 120 ℃ of oven dry, 400 ℃ of roasting 4h make the finished catalyst C6 that contains nickel oxide 16wt%, potassium oxide 1.5wt%, magnesia 2.5wt%, zinc oxide 2.0wt%, silver oxide 1.0wt%, molybdenum oxide 2.0wt%, lanthana 3.5wt%.
Embodiment 7
Carrier Z
AThe preparation method is with embodiment 1.Prepare the mixed impregnant liquor of nickel nitrate, lithium nitrate, zinc nitrate, ammonium molybdate, ammonium metatungstate, lanthanum nitrate, EDTA then, wherein the mol ratio of EDTA and active component nickel is 1: 5.5, regulates maceration extract pH value to 4.8, impregnated in 100gZ
AOn the carrier, ageing 12h, 120 ℃ of oven dry, 450 ℃ of roasting 4h make the finished catalyst C7 that contains nickel oxide 14wt%, lithia 2.0wt%, zinc oxide 2.5wt%, molybdenum oxide 2.0wt%, tungsten oxide 1.5wt%, lanthana 4.0wt%.
Comparative Examples 1
Carrier Z
AThe preparation method is with embodiment 1.Prepare the mixed impregnant liquor of nickel nitrate, ammonium molybdate, lanthanum nitrate, EDTA, triethylene-glycol then, wherein the mol ratio of EDTA, triethylene-glycol and active component nickel is 1: 5, regulates maceration extract pH value to 4, impregnated in 100gZ
AOn the carrier, ageing 12h, 120 ℃ of oven dry, 400 ℃ of roasting 4h make the finished catalyst D1 that contains nickel oxide 12wt%, lithia 1.0wt%, molybdenum oxide 3.0wt%, lanthana 3.0wt%.
Comparative Examples 2
Carrier Z
BThe preparation method is with embodiment 2.The mixed impregnant liquor of preparation nickel nitrate, potassium nitrate, cadmium nitrate, metamolybdic acid ammonium, triethylene-glycol, the mol ratio of triethylene-glycol and active component nickel is 1: 7, regulates maceration extract pH value to 3, impregnated in 100gZ
BOn the carrier, ageing 12h, 120 ℃ of oven dry, 450 ℃ of roasting 4h make the finished catalyst D2 that contains nickel oxide 13wt%, potassium oxide 1.6wt%, cadmium oxide 3.0wt%, molybdenum oxide 2.5wt%.
Comparative Examples 3
Carrier Z
BThe preparation method is with embodiment 2.Prepare the mixed impregnant liquor of nickel nitrate, potassium nitrate, cadmium nitrate, cerous nitrate, triethylene-glycol then, the mol ratio of triethylene-glycol and active component nickel is 1: 7, regulates maceration extract pH value to 3, impregnated in 100gZ
BOn the carrier, ageing 12h, 120 ℃ of oven dry, 450 ℃ of roasting 4h make the finished catalyst D3 that contains nickel oxide 13wt%, potassium oxide 1.6wt%, cadmium oxide 3.0wt%, cerium oxide 3.0wt%.
Comparative Examples 4
The preparing carriers method is with embodiment 2.The mixed impregnant liquor of preparation nickel nitrate, potassium nitrate, silver nitrate, metamolybdic acid ammonium, lanthanum nitrate, cerous nitrate, ethylene glycol, wherein the mol ratio of ethylene glycol and active component nickel is 1: 7, regulates maceration extract pH value to 5, impregnated in 100gZ
BOn the carrier, ageing 12h, 120 ℃ of oven dry, 350 ℃ of roasting 4h make the finished catalyst D4 that contains nickel oxide 9.0wt%, potassium oxide 2.0wt%, silver oxide 2.5wt%, molybdenum oxide 4.0wt%, lanthana 2.0wt%, cerium oxide 1.5wt%.
Comparative Examples 5
The preparing carriers method is with embodiment 2.The mixed impregnant liquor of preparation nickel nitrate, zinc nitrate, ammonium dichromate, cerous nitrate, EDTA, wherein the mol ratio of EDTA and active component nickel is 1: 6, regulates maceration extract pH value to 4.5, impregnated in 100gZ
BOn the carrier, ageing 12h, 120 ℃ of oven dry, 430 ℃ of roasting 5h make the finished catalyst D5 that contains nickel oxide 15wt%, zinc oxide 1.5wt%, chromium oxide 2.0wt%, cerium oxide 4.0wt%.
Table 1 is each components contents of catalyst in embodiment and the Comparative Examples.
Each constituent content of catalyst in table 1 embodiment and the Comparative Examples
Evaluating catalyst: adopt C
5～C
9Drippolene is a raw material; Feedstock property is seen table 2; Catalyst sample in embodiment 1～7, the Comparative Examples 1～5 is estimated; Evaluating catalyst carries out on 100mL adiabatic reactor hydrogenation reaction device, and catalyst cools the temperature to 60 ℃ then and carries out presulfurization carrying out will in 400 ℃ hydrogen atmosphere, reducing before the hydrogenation reaction 17h.The presulfurization condition is: with the straight-run naphtha of the sulfur content 70 μ g/g 3h that turns round.Passivation pressure 0.5MPa, hydrogen to oil volume ratio 200, liquid air speed 6h
-1
Sulfuration begins to carry out hydrogenation reaction after finishing, and appreciation condition is: reaction pressure 2.8MPa, 60 ℃ of reaction inlet temperatures, fresh feed oil air speed 3.0h
-1, hydrogen to oil volume ratio 200: 1.Each evaluating catalyst time is 200h, and iodine value, diene are once analyzed in the 12h sampling, and the average data of 200h evaluation result is as shown in table 3.
Table 2 feedstock oil (C
5～C
9) index
Table 3 catalyst activity evaluation result
Can find out that from experimental data catalyst of the present invention just has good hydrogenation activity and selectivity at a lower temperature, and better to the adaptability of raw material, to C
5～C
9Full feedstock has good hydrogenation effect.
Claims (10)
1. a diene selective hydrogenation catalyst is characterized in that catalyst is a carrier with aluminium oxide or modified aluminas, is active component with nickel, is auxiliary agent with alkali metal or alkaline-earth metal, vib metal, X metal, rare earth metal; In the total catalyst weight is 100wt%; Catalyst contains nickel oxide 10～20wt%, alkali metal and/or alkaline earth oxide 0.5～5wt%, VIB element oxide 1～7wt%; Auxiliary agent X metallic element oxide 0.5～5wt%, the X metal is one or more in cadmium, zinc, copper, the silver; Rare earth oxide 2～5wt%.
2. catalyst according to claim 1; It is characterized in that containing in the catalyst nickel oxide 12～18wt%, alkali metal and/or alkaline earth oxide 1～4wt%, VIB element oxide 2～4wt%; Auxiliary agent X metallic element oxide 1～3wt%, rare earth oxide 2～5wt%.
3. catalyst according to claim 1 is characterized in that alkali metal and/or alkaline-earth metal are one or more in lithium, potassium, the magnesium.
4. catalyst according to claim 1 is characterized in that the VIB element is one or more in chromium, molybdenum, the tungsten.
5. catalyst according to claim 4 is characterized in that the VIB element is chromium and/or molybdenum.
6. catalyst according to claim 1 is characterized in that rare earth element is lanthanum and/or cerium.
7. described Preparation of catalysts method of claim 1; It is characterized in that the compound of active component nickel, VIB element, rare earth element, alkali metal, alkaline-earth metal and X metallic element is added in the entry, fully after the dissolving, maceration extract pH value is adjusted to 3～5; Alumina support impregnated in the maceration extract; Each component is carried on the alumina support, after 100～120 ℃ of dryings, makes at 300～450 ℃ of following roasting 4～6h.
8. preparation method according to claim 7 is characterized in that the preparation process of alumina support is: with the boehmite extruded moulding, and 100～120 ℃ of oven dry, 800～1000 ℃ of roasting 3～6h.
9. described Preparation of catalysts method of claim 1; It is characterized in that the compound of active component nickel, VIB element, rare earth element and X metallic element is added in the entry, fully after the dissolving, maceration extract pH value is adjusted to 3～5; Modified aluminium oxide supports impregnated in the maceration extract; Each component is carried on the modified aluminium oxide supports, after 100～120 ℃ of dryings, makes at 300～450 ℃ of following roasting 4～6h; This modified aluminas is meant in boehmite extruded moulding process and adds alkali metal and/or alkaline earth metal compound carries out modification to alumina precursor, 100～120 ℃ of oven dry then, 800～1000 ℃ of carriers that roasting 3～6h makes.
10. according to claim 7 or 9 described preparation methods; It is characterized in that adding in the maceration extract organic complexing agent and/or chelating agent; Be in citric acid, triethylene-glycol, ethylene glycol, EDTA, the ethylenediamine one or more, the mol ratio of organic complexing agent and/or chelating agent and active component nickel is 1: 5～1: 10.
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