CN104741123A - Novel nano ferrite adsorption desulfurization catalyst and preparation method thereof - Google Patents
Novel nano ferrite adsorption desulfurization catalyst and preparation method thereof Download PDFInfo
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Abstract
The invention belongs to the technical field of fuel processing and petroleum chemical engineering, and relates to a novel nano ferrite adsorption desulfurization catalyst MeFe2O4, wherein Me comprises but not the same with Mg, Zn, Ni, Co and Cu. The preparation method comprises the following steps: dissolving transition metal nitrate, Fe-containing nitrate and fuels in water, heating the obtained solution in a microwave furnace rapidly, decomposing so as to generate a great quantity of combustible gases and emit a great amount of heat, and combusting reactants reaching the spontaneous ignition point; and reacting so as to obtain a solid material, namely the novel nano ferrite adsorption desulfurization catalyst. The novel nano ferrite adsorption desulfurization catalyst is relatively high in desulfurization selectivity, can prevent the loss of octane value and cetane value due to olefins hydrogenation while deeply removing sulfocompound in fuel oil, and has relatively good industrial application prospect.
Description
Technical field
The invention belongs to fuel processing and technical field of petrochemical industry, relate in distillate ultra-deep absorption desulfurization a kind of novel ferrite catalyst used.Concretely, adopt the precursors such as the transition metal salt solution of the certain stoichiometric proportion of microwave induced combustion synthesis method process, solution containing iron salts and reducing agent, namely form stable spinel structure nanometer ferrite catalyst (MeFe
2o
4) and the ultra-deep absorption desulfurization catalytic applications of prepared material.
Background technology
Along with the shortage of petroleum resources and countries in the world are to the restriction of sulfur content in oil products, the low sulfuration of the fuel such as gasoline, diesel oil, to clean be trend of the times.At present, the hydro desulfurization gram generally adopted effectively removes inorganic sulfur and simple organic sulfur compound, but it is more difficult to removing of condensed ring thiophene class sulfur-containing compound and derivative thereof, and require HTHP and hydrogen environment, and employing noble metal catalyst, this makes the financial cost of desulfurization increase, and can be octane number and the Cetane number decline of fuel oil in hydrogenation process, therefore, need to find a kind of newly, economically viable petrol and diesel oil process for deep desulphurization.Adsorption desulfurize technology is compared and hydrodesulfurization technology, simply, easily and fast and effectively reduces costs and operating cost, can not reduce the octane number of gasoline and the Cetane number of diesel oil in processing procedure, is the desulfur technology being expected to realize zero sulphur target.
At present, adsorption desulfurize technology mainly adopts the adsorbents such as molecular sieve, active carbon, oxide to remove sulfur-containing compound.Wherein molecular sieve and acticarbon are mainly through physical absorption desulfurization, although sulfide can be removed at normal temperatures and pressures, adsorbent regenerating easily, but due to physical adsorption process poor selectivity, sulfur capacity is lower, and very easily reaches balance, be difficult to sulfur content is dropped to very low, therefore, be difficult to be promoted in application aspect.And adopt metal oxide sorbents to be the strong interaction utilized between adsorbent and sulphur atom, realized by reactive adsorption desulfurization, there is selective good, the feature such as desulfurization depth is high, catalyst life is long, can sulfur-containing compound in deep removal fuel oil, and alkene hydrogenation hardly, thus hydrogen consumption is lower.
US Patent No. 6346190 discloses the S-Zorb technique developed by ConocoPhilips (COP) company, adopts ZnO, NiO and Al
2o
3and SiO
2for adsorbent, combined fluidized bed reactor and cyclic regeneration technology, show good desulfurization performance and stability in the desulfurization of catalytic gasoline.But this technique is very brightless for the treatment of the commercial introduction prospect of diesel oil: first, in order to ensure fully to contact with absorbent particles, diesel oil distillate need be gasified totally, this will negate temperature >380 DEG C (end point of distillation), consequent energy consumption, coking problem, will offset otherwise advantage greatly.
Chinese patent CN201410254990.1 discloses a kind of fuel oil deep absorption desulfurization catalyst and method for making and application, there is provided a kind of specific area high, reaction temperature and, intensity is high, hydrogen consumes little fuel oil deep absorption desulfurization catalyst, but the preparation technology of this catalyst is loaded down with trivial details, and sulfur capacity is less, and application is subject to certain restrictions.
Chinese patent CN101940908 also discloses a kind of ultra-deep absorption desulfurization agent, and this adsorbent, mainly based on zinc oxide, can only be used for the desulfurization of light-end products, not obvious to the desulfurized effect of heavy oil product.
For the deficiencies in the prior art, the present invention intends the nanometer ferrite adsorbent developing a kind of novel cheapness, and is applied to the ultra-deep absorption desulfurization of fuel oil.Nanometer ferrite adsorbent prepared by the present invention, not only preparation method is simple, mild condition, synthesis cost is low, environmental friendliness, and the deep absorption desulfurization of prepared material to fuel oil has higher desulfuration selectivity, can while the sulfur-containing compound in deep removal fuel oil, the octane number avoiding olefins hydrogenation to cause and the loss of Cetane number.
Summary of the invention
The invention provides a kind of novel nano ferrite absorbing desulfurization catalyst, the sulfur-containing compound in petroleum distillate has very high desulfuration selectivity, thus high-efficiency and economic achieve deep desulfuration.
Nanometer ferrite absorbing desulfurization catalyst of the present invention is MeFe
2o
4; Wherein Me comprises Mg, Zn, Ni, Co, Cu etc. and not identical, and ferrite absorbing desulfurization catalyst is nickel ferrite based magnetic loaded NiFe
2o
4, cobalt ferrite CoFe
2o
4, magnesium ferrite MgFe
2o
4, zinc ferrite ZnFe
2o
4, coppe ferrite CuFe
2o
4, coppe ferrite zinc ZnCuFe
2o
4.
The minor amount of water solution necessarily measuring the metal nitrate of ratio, iron content nitrate solution and fuel heats to adopt microwave induced combustion synthesis method by above-mentioned nanometer ferrite absorbing desulfurization catalyst preparation method in microwave environment, it is made to reach reaction temperature fast, initiation reaction.Concrete steps are as follows:
By the transition metal nitrate of certain stoichiometric proportion, iron content nitrate and the dissolving of fuel in minor amount of water, solution decomposes a large amount of combustibility gas of generation in micro-wave oven after heated fast, release a large amount of heat, reactant is self-burning after reaching self-ignition point simultaneously.In whole course of reaction, nitrate plays oxidant, and fuel and catabolite thereof play reducing agent, and microwave plays induced oxidation reduction.After having reacted, gained solid material is nanometer ferrite absorbing desulfurization catalyst.
In above-mentioned nanometer ferrite absorbing desulfurization catalyst preparation adopt transition metal nitrate to be ferric nitrate, with one or both nitrate in magnesium nitrate, zinc nitrate, copper nitrate, nickel nitrate, cobalt nitrate.Fuel is the one in urea, polyethylene glycol, sorbierite and glycine.
The above-mentioned microwave reaction time is 1-30min, and Best Times is 5-15min, microwave power is 400-1200W.
In above-mentioned nanometer ferrite absorbing desulfurization catalyst preparation, the mol ratio of transition metal nitrate and fuel is 0.1-2.Different proportion can obtain the nanometer ferrite absorbing desulfurization catalyst of different-grain diameter and pattern.
Above-mentioned novel nano ferrite absorbing desulfurization catalyst is used for the desulfurization process of the sulfur-containing compound in petroleum distillate, this novel nano ferrite absorbing desulfurization catalyst is after deep absorption desulfurization, under an oxygen-containing atmosphere through 400-700 DEG C of process 1-3h, realize the regeneration of novel nano ferrite absorbing desulfurization catalyst.
Nanometer ferrite absorbing desulfurization catalyst of the present invention, shows higher activity and selective, improves catalytic process efficiency, effectively realize the deep desulfuration of petroleum distillate, produce clean fuel, be with a wide range of applications in deep absorption desulfurization reaction.Utilize microwave induced combustion synthesis method to prepare nanometer ferrite adsorbent fast in a mild condition, preparation is simple, without the need to calcining, products therefrom particle diameter is little, distribution is relatively more even, mild condition, synthesis cost is low, environmental friendliness.This catalyst is higher desulfuration selectivity in deep absorption desulfurization reaction and display, is significantly stripped of the sulfur-containing compound in petroleum distillate, thus efficiently, economical achieves deep desulfuration, generating clean fuel.
Accompanying drawing explanation
Fig. 1 is the X-ray diffractogram of different nanometer ferrite absorbing desulfurization catalyst.
Fig. 2 is the adsorption desulfurize data of different nanometer ferrite absorbing desulfurization catalyst catalysis thiophene.
Detailed description of the invention
The specific embodiment of the present invention is described in detail below in conjunction with accompanying drawing and technical scheme.
Embodiment 1: nanometer zinc ferrite (ZnFe
2o
4) preparation of absorbing desulfurization catalyst
Be dissolved in 1665mmol minor amount of water by 33mmol zinc nitric acid, 67mmol iron nitric acid and 200mmol urea, wherein the mol ratio of urea, metal nitrate, water is 2:1:16.65.Solution is decompose 15min after heated fast in the micro-wave oven of 800W at power.Produce a large amount of combustibility gas in course of reaction, release a large amount of heat simultaneously, make reactant self-burning after reaching self-ignition point.After having reacted, gained solid material is nanometer zinc ferrite (ZnFe
2o
4) absorbing desulfurization catalyst.One in fuel polyethylene glycol, sorbierite and glycine is replaced urea, the nanometer zinc ferrite (ZnFe of different-grain diameter can be prepared equally
2o
4) absorbing desulfurization catalyst.
Embodiment 2: nano nickel ferrite (NiFe
2o
4) preparation of absorbing desulfurization catalyst
Be dissolved in 1665mmol minor amount of water by 33mmol nickel nitric acid, 67mmol iron nitric acid and 50mmol glycine, wherein the mol ratio of glycine, metal nitrate, water is 0.5:1:16.65.Solution is decompose 30min after heated fast in the micro-wave oven of 1200W at power.Produce a large amount of combustibility gas in course of reaction, release a large amount of heat simultaneously, make reactant self-burning after reaching self-ignition point.After having reacted, gained solid material is nano nickel ferrite absorbing desulfurization catalyst.
Embodiment 3: nano magnesium ferrite (MgFe
2o
4) preparation of absorbing desulfurization catalyst
Be dissolved in 1665mmol minor amount of water by 33mmol magnesium nitric acid, 67mmol iron nitric acid and 170mmol polyethylene glycol, wherein the mol ratio of polyethylene glycol, metal nitrate, water is 1.7:1:16.65.Solution is decompose 10min after heated fast in the micro-wave oven of 400W at power.Produce a large amount of combustibility gas in course of reaction, release a large amount of heat simultaneously, make reactant self-burning after reaching self-ignition point.After having reacted, gained solid material is nano magnesium ferrite (MgFe
2o
4) absorbing desulfurization catalyst.
Embodiment 4: nano ferrous acid copper zinc (CuZnFe
2o
4) preparation of absorbing desulfurization catalyst
Be dissolved in 1665mmol minor amount of water by 25mmol copper nitric acid, 25mmol zinc nitric acid, 50mmol iron nitric acid and 200mmol urea, wherein the mol ratio of urea, metal nitrate, water is 2:1:16.65.Solution is decompose 30min after heated fast in the micro-wave oven of 800W at power.Produce a large amount of combustibility gas in course of reaction, release a large amount of heat simultaneously, make reactant self-burning after reaching self-ignition point.After having reacted, gained solid material is nano ferrous acid copper zinc (CuZnFe
2o
4) absorbing desulfurization catalyst.
Embodiment 5: the performance study of nanometer zinc ferrite catalyst in deep absorption desulfurization reaction
With the thiophene solution of total sulfur content 3000mg/L for model compound, wherein normal heptane is solvent, investigate nanometer zinc ferrite adsorption desulfurize reaction in desulphurizing activated.Reaction is carried out in fixed bed reactors.
Reaction condition is: catalyst nano zinc ferrite: 0.3g, temperature, 500 DEG C, pressure: 1.0MPa, and volume space velocity is: 2h
-1, hydrogen-oil ratio is: 600.Product analysis adopts gas-chromatography, hydrogen flame detector.Before reaction, nanometer zinc ferrite catalyst, at 100sccm hydrogen flow rate, activates 2h at 500 DEG C.Reaction result is shown in accompanying drawing 2.Along with the reaction time is to 38h, sulfur removal rate is down to 50% by 100%.Meanwhile, to reacted catalyst roasting 2h under 500 DEG C of air atmospheres, find the regeneration that can realize nanometer zinc ferrite through XRD analysis.
Embodiment 6: the performance study of nano magnesium ferrite catalyst in deep absorption desulfurization reaction
With the thiophene solution of total sulfur content 3000mg/L for model compound, wherein normal heptane is solvent, investigate nano magnesium ferrite adsorption desulfurize reaction in desulphurizing activated.Reaction is carried out in fixed bed reactors.
Reaction condition is: catalyst nano magnesium ferrite: 0.3g, temperature, 400 DEG C, pressure: 1.0MPa, and volume space velocity is: 2h
-1, hydrogen-oil ratio is: 600.Product analysis adopts gas-chromatography, hydrogen flame detector.Before reaction, nano magnesium ferrite catalyst, at 100sccm hydrogen flow rate, activates 2h at 500 DEG C.Reaction result is shown in accompanying drawing 2.Along with the reaction time is to 38h, sulfur removal rate is down to 75% by 100%.Meanwhile, to reacted catalyst roasting 2h under 500 DEG C of air atmospheres, find the regeneration that can realize nano magnesium ferrite through XRD analysis.
Embodiment 7: the performance study of nano nickel ferrite catalyst in deep absorption desulfurization reaction
With the thiophene solution of total sulfur content 3000mg/L for model compound, wherein normal heptane is solvent, investigate nano nickel ferrite adsorption desulfurize reaction in desulphurizing activated.Reaction is carried out in fixed bed reactors.
Reaction condition is: catalyst nano nickel ferrite based magnetic loaded: 0.3g, temperature, 500 DEG C, pressure: 1.0MPa, and volume space velocity is: 2h
-1, hydrogen-oil ratio is: 600.Product analysis adopts gas-chromatography, hydrogen flame detector.Before reaction, nano nickel ferrite catalyst, at 100sccm hydrogen flow rate, activates 2h at 500 DEG C.Reaction result is shown in accompanying drawing 2.Along with the reaction time is to 38h, sulfur removal rate is down to 65% by 80%.Meanwhile, to reacted catalyst roasting 2h under 500 DEG C of air atmospheres, find the regeneration that can realize nano nickel ferrite through XRD analysis.
Embodiment 8: nano ferrous acid copper zinc (CuZnFe
2o
4) performance study of catalyst in deep absorption desulfurization reaction
With the thiophene solution of total sulfur content 3000mg/L for model compound, wherein normal heptane is solvent, investigates desulphurizing activated in adsorption desulfurize reaction of nano ferrous acid copper zinc.Reaction is carried out in fixed bed reactors.
Reaction condition is: catalyst nano coppe ferrite zinc: 0.3g, temperature, 500 DEG C, and pressure: 1.0MPa, volume space velocity is: 2h
-1, hydrogen-oil ratio is: 600.Product analysis adopts gas-chromatography, hydrogen flame detector.Before reaction, nano ferrous acid copper zinc catalyst, at 100sccm hydrogen flow rate, activates 2h at 500 DEG C.Reaction result is shown in accompanying drawing 2.Along with the reaction time is to 38h, sulfur removal rate is down to 58% by 90%.Meanwhile, to reacted catalyst roasting 2h under 500 DEG C of air atmospheres, find the regeneration that can realize nano ferrous acid copper zinc through XRD analysis.
Claims (4)
1. a novel nano ferrite absorbing desulfurization catalyst, is characterized in that, this nanometer ferrite absorbing desulfurization catalyst is MeFe
2o
4, wherein Me comprises Mg, Zn, Ni, Co, Cu, and not identical; Be specially nickel ferrite based magnetic loaded NiFe
2o
4, cobalt ferrite CoFe
2o
4, magnesium ferrite MgFe
2o
4, zinc ferrite ZnFe
2o
4, coppe ferrite CuFe
2o
4, coppe ferrite zinc ZnCuFe
2o
4.
2. the preparation method of novel nano ferrite absorbing desulfurization catalyst according to claim 1, it is characterized in that, step is as follows: transition metal nitrate, iron content nitrate and fuel are dissolved in water, the solution obtained heated fast in micro-wave oven, decompose and produce a large amount of combustibility gas, release large calorimetric, reactant is self-burning after reaching self-ignition point simultaneously; The solid material having reacted gained is novel nano ferrite absorbing desulfurization catalyst; Described transition metal nitrate is ferric nitrate, mixes with one or more nitrate in magnesium nitrate, zinc nitrate, copper nitrate, nickel nitrate, cobalt nitrate; Described fuel is urea, polyethylene glycol, sorbierite or glycine; Described transition metal nitrate and the mol ratio of fuel are 0.1-2, and the microwave reaction time is 1-30min, and microwave power is 400-1200W.
3. preparation method according to claim 2, is characterized in that, the described microwave reaction time is 5-15min.
4. novel nano ferrite absorbing desulfurization catalyst according to claim 1 is used for the desulfurization process of the sulfur-containing compound in petroleum distillate, it is characterized in that, this novel nano ferrite absorbing desulfurization catalyst is after deep absorption desulfurization, under an oxygen-containing atmosphere through 400-700 DEG C of process 1-3h, realize the regeneration of novel nano ferrite absorbing desulfurization catalyst.
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| CN108269980A (en) * | 2018-01-03 | 2018-07-10 | 桂林理工大学 | A kind of method for preparing high-performance di-iron trioxide/zinc ferrite combination electrode material |
| CN108690039A (en) * | 2018-06-26 | 2018-10-23 | 大连理工大学 | A kind of method that sorb dehydration of alcohols prepares isobide |
| CN110116001A (en) * | 2019-05-24 | 2019-08-13 | 攀枝花学院 | Ferrous acid bronzing-Fenton catalysis magnetic composite and preparation method thereof |
| CN110479283A (en) * | 2019-08-27 | 2019-11-22 | 华中科技大学 | The catalyst and its preparation and application of a kind of nickel load on coppe ferrite spinelle surface |
| CN110747004A (en) * | 2019-11-15 | 2020-02-04 | 河南科技大学 | Application of spinel ferrite magnetic nano catalyst in oil product desulfurization |
| CN112266024A (en) * | 2020-10-15 | 2021-01-26 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation method of cactus-shaped magnesium ferrate nano material, product and application |
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| CN110479283A (en) * | 2019-08-27 | 2019-11-22 | 华中科技大学 | The catalyst and its preparation and application of a kind of nickel load on coppe ferrite spinelle surface |
| CN110747004A (en) * | 2019-11-15 | 2020-02-04 | 河南科技大学 | Application of spinel ferrite magnetic nano catalyst in oil product desulfurization |
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| CN114950448A (en) * | 2022-06-28 | 2022-08-30 | 南京信息工程大学 | ZnFe 2 O 4 Process for preparing base catalyst and its application |
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