CN113275013A - Iron oxide/aluminum oxide compound and preparation method and application thereof - Google Patents

Iron oxide/aluminum oxide compound and preparation method and application thereof Download PDF

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CN113275013A
CN113275013A CN202110528392.9A CN202110528392A CN113275013A CN 113275013 A CN113275013 A CN 113275013A CN 202110528392 A CN202110528392 A CN 202110528392A CN 113275013 A CN113275013 A CN 113275013A
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gel
iron oxide
aluminum
oxide
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吴配月
马兆菲
颜学敏
杨欢
李颢
程仲富
邓飞
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Yangtze University
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
    • B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
    • B01J23/74—Iron group metals
    • B01J23/745—Iron
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
    • B01J23/002—Mixed oxides other than spinels, e.g. perovskite
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
    • B01J37/02—Impregnation, coating or precipitation
    • B01J37/03—Precipitation; Co-precipitation
    • B01J37/036—Precipitation; Co-precipitation to form a gel or a cogel
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
    • B01J37/08—Heat treatment
    • B01J37/082—Decomposition and pyrolysis
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
    • C10G45/00—Refining of hydrocarbon oils using hydrogen or hydrogen-generating compounds
    • C10G45/02—Refining of hydrocarbon oils using hydrogen or hydrogen-generating compounds to eliminate hetero atoms without changing the skeleton of the hydrocarbon involved and without cracking into lower boiling hydrocarbons; Hydrofinishing
    • C10G45/04—Refining of hydrocarbon oils using hydrogen or hydrogen-generating compounds to eliminate hetero atoms without changing the skeleton of the hydrocarbon involved and without cracking into lower boiling hydrocarbons; Hydrofinishing characterised by the catalyst used
    • C10G45/06—Refining of hydrocarbon oils using hydrogen or hydrogen-generating compounds to eliminate hetero atoms without changing the skeleton of the hydrocarbon involved and without cracking into lower boiling hydrocarbons; Hydrofinishing characterised by the catalyst used containing nickel or cobalt metal, or compounds thereof

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  • Materials Engineering (AREA)
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  • Oil, Petroleum & Natural Gas (AREA)
  • Physics & Mathematics (AREA)
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  • Compounds Of Iron (AREA)

Abstract

The invention discloses an iron oxide/aluminum oxide compound and a preparation method and application thereof, and belongs to the technical field of thickened oil viscosity reduction. The preparation method comprises the following steps: s1, mixing Fe2O3Dispersing the nano particles in an ethanol solution, and then sequentially adding a phase separation agent, an aluminum salt and a gel inducer to obtain a mixed sol solution; s2, carrying out sol-gel conversion on the mixed sol solution at 40-50 ℃ to obtain wet gel, and then drying the wet gel at 40-60 ℃ to obtain dry gel; s3, roasting the xerogel at 800-900 ℃ to obtain the iron oxide/aluminum oxide compound. The invention also discloses the iron oxide/aluminum oxide compound prepared by the preparation method. In addition, the present invention also includes the above-mentioned oxygenThe application of the ferric oxide/aluminum oxide compound in the degradation of thick oil. The viscosity reducing rate of the compound to thickened oil can reach 75.2%, the proportion of heavy components cracked into light components after viscosity reduction can reach 38.7%, and the compound has good thermal stability.

Description

Iron oxide/aluminum oxide compound and preparation method and application thereof
Technical Field
The invention relates to the technical field of thickened oil viscosity reduction, and particularly relates to an iron oxide/aluminum oxide compound and a preparation method and application thereof.
Background
Increasingly, thickened oil is favored as an unconventional energy source with great potential. The catalytic viscosity reduction by the hydrothermal cracking is one of the common technologies for exploiting the thick oil, high-temperature steam is injected into an oil layer, a catalytic viscosity reducer by the hydrothermal cracking is added at the same time, the oil layer is regarded as a natural reactor, the catalytic cracking of the thick oil is realized under the hydrothermal condition by utilizing the heat provided by the steam under the action of the catalytic viscosity reducer, and the macromolecular part in the thick oil is cracked into micromolecules, so that the viscosity of the thick oil is irreversibly reduced, and the aim of easily exploiting the thick oil is fulfilled. The key of the technology lies in the effective hydrothermal cracking catalytic viscosity reducer.
In the process of developing the thickened oil catalytic viscosity reducer, researchers usually select transition metals such as copper and iron as catalytic activity centers of the catalytic viscosity reducer, and use hydrogen donor ligands (tetrahydronaphthalene, toluene, formic acid) and the like) in combination to catalyze the hydrogenation and fracture of C-R (O, N, S) bonds, promote the hydrogenation and impurity removal of thickened oil, and effectively improve the quality of the thickened oil. However, the viscosity reducing catalyst and the viscosity reducing agent used in the conventional thickened oil production still have the problems of low catalytic viscosity reducing efficiency, poor thermal stability and high heavy component content in the thickened oil after viscosity reduction.
Therefore, the problem to be solved in the art is to provide a material which can effectively carry out the hydrothermal cracking catalytic viscosity reduction on the thick oil.
Disclosure of Invention
The invention aims to overcome the technical defects, provides an iron oxide/aluminum oxide compound and a preparation method and application thereof, and solves the technical problems that in the prior art, the catalytic viscosity reduction of the thickened oil through the thermal cracking of water is low in efficiency and poor in thermal stability, and the content of heavy components in the viscosity reduced thickened oil is high.
In order to achieve the technical purpose, the technical scheme of the invention provides an iron oxide/aluminum oxide compound and a preparation method and application thereof.
The invention provides a preparation method of an iron oxide/aluminum oxide compound, which comprises the following steps:
s1, mixing Fe2O3Dispersing the nano particles in an ethanol solution, and then sequentially adding a phase separation agent, an aluminum salt and a gel inducer to obtain a mixed sol solution;
s2, carrying out sol-gel conversion on the mixed sol solution at 40-50 ℃ to obtain wet gel, and drying the wet gel at 40-60 ℃ to obtain dry gel;
s3, roasting the xerogel at 800-900 ℃ to obtain the iron oxide/aluminum oxide compound.
Further, in step S1, the Fe2O3The mass of the nano particles is 1-10% of the mass of the aluminum salt.
Further, in step S1, the mass ratio of the phase separation agent, the aluminum salt, and the gel induction agent is (0.06 to 0.12): (4.26-4.38): (3.05-3.17).
Further, in step S2, the sol-gel conversion is performed for 18 to 36 hours.
Further, in step S2, the drying is performed at 40 to 60 ℃ for 3 to 7 days.
Further, in step S3, the baking time is 4 to 6 hours.
Further, in step S1, the aluminum salt is added into the ice bath environment and stirred for 20-40min until the aluminum salt is dissolved, and then the gel inducer is added and stirred for 5-10 min to obtain the mixed sol solution.
Further, in step S1, the phase separation agent is polyethylene oxide; and/or, the gel inducer is propylene oxide; and/or the aluminum salt is aluminum chloride.
The invention also provides the iron oxide/aluminum oxide compound prepared by the preparation method.
Furthermore, the invention also provides an iron oxide/aluminum oxide compound prepared by the preparation method or an application of the iron oxide/aluminum oxide compound in the degradation of thick oil.
Compared with the prior art, the invention has the beneficial effects that: in the preparation method provided by the invention, the supported Fe2O3The nano particles are uniformly dispersed in the sol phase and the gel phase, the agglomeration of the nano particles is effectively avoided, the prepared iron oxide/aluminum oxide composite has a three-dimensional through and crosslinked multi-stage pore canal, the contact between a catalyst and macromolecules in an oil phase is facilitated, the obtained multi-stage pore canal composite material can absorb a macromolecule association structure of a heavy component of the heavy oil, and fully contacts with the heteroatoms in the heavy component to take effect so as to promote the removal of part of the heteroatoms, the catalytic activity of the catalyst is better exerted, the iron oxide and the aluminum oxide in the composite have a catalytic synergistic effect, the viscosity reduction rate of the heavy oil can reach 85.2 percent, the proportion of the heavy component cracked into a light component after the viscosity reduction can reach 38.7 percent, the high-temperature 240 ℃ also has better degradation performance, and the thermal stability is good.
Drawings
FIG. 1 is a Scanning Electron Microscope (SEM) image of an iron oxide/alumina composite prepared in example 1 of the present invention.
FIG. 2 is an XRD pattern of an iron oxide/alumina composite prepared in example 1 of the present invention.
Detailed Description
The specific embodiment provides a preparation method of an iron oxide/aluminum oxide compound, which comprises the following steps:
s1, mixing Fe2O3Dispersing nano particles in an ethanol solution, carrying out ultrasonic treatment for 10-30min, then sequentially adding a phase separation agent until the nano particles are completely dissolved, then adding aluminum salt in an ice bath environment, stirring for 20-40min until the nano particles are completely dissolved, and then adding a gel inducer under the conditions of normal temperature and normal pressure, and violently stirring for 5-10 min to obtain a mixed sol solution; said Fe2O3The mass of the nano particles is 1-10% of the mass of the aluminum salt(ii) a The mass ratio of the phase separating agent to the aluminum salt to the gel inducer is (0.06-0.12): (4.26-4.38): (3.05-3.17); the phase separating agent is polyethylene oxide, and the relative molecular mass is preferably 1 x 106Polyethylene oxide of (a); the aluminum salt is aluminum chloride, and further the aluminum chloride is crystalline aluminum chloride AlCl3·6H2O; the gel inducer is propylene oxide; the volume concentration of ethanol in the ethanol solution is 40-55%;
s2, putting the mixed sol solution into a sealed test tube, carrying out sol-gel conversion in a constant-temperature water bath box at 40-50 ℃ for 18-36h to obtain wet gel, and then transferring the wet gel to a constant-temperature drying box to dry at 40-60 ℃ for 3-7 days to obtain dry gel;
s3, transferring the dried gel to a muffle furnace, and roasting at 800-900 ℃ for 4-6 h to obtain the iron oxide/aluminum oxide compound.
The specific embodiment also comprises the iron oxide/aluminum oxide compound prepared by the preparation method.
The specific embodiment also provides an iron oxide/aluminum oxide compound prepared by the preparation method or an application of the iron oxide/aluminum oxide compound in the degradation of thick oil.
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is described in further detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
Example 1
This example proposes an iron oxide/alumina composite prepared by the following steps:
s1, mixing Fe2O3Dispersing the nanoparticles in ethanol solution, performing ultrasonic treatment for 30min, and sequentially adding phase-separating agent polyethylene oxide (relative molecular weight of 1 × 10)6) Adding crystalline aluminum chloride in an ice bath environment, stirring for 20min until the crystalline aluminum chloride is completely dissolved, adding a gel inducer propylene oxide under the conditions of normal temperature and normal pressure, and violently stirring for 5min to obtain a mixed sol solution; what is needed isFe2O3The mass of the nanoparticles is 5% of the mass of the aluminium salt; the mass ratio of the polyethylene oxide, the crystalline aluminum chloride and the propylene oxide is 0.12: 4.38: 3.17; the volume concentration of ethanol in the ethanol solution is 50 percent;
s2, putting the mixed sol solution into a sealed test tube, carrying out sol-gel conversion in a constant-temperature water bath box at 50 ℃ for 30h to obtain wet gel, and then transferring the wet gel to a constant-temperature drying box to dry at 40 ℃ for 7 days to obtain dry gel;
s3, transferring the xerogel to a muffle furnace, and roasting for 4h at 900 ℃ to obtain the iron oxide/aluminum oxide compound.
As can be seen from FIG. 1, the iron oxide/aluminum oxide composite particles prepared by the present example are large, stacked and porous; in FIG. 2, with γ -Al2O3Characteristic diffraction peak of (JCPDS No.10-0425), and alpha-Fe2O3The characteristic diffraction peak (JCPDS No.33-0664) of this example further demonstrates the success of the iron oxide/aluminum oxide composite.
Example 2
This example proposes an iron oxide/alumina composite prepared by the following steps:
s1, mixing Fe2O3Dispersing the nanoparticles in ethanol solution, performing ultrasonic treatment for 20min, and sequentially adding phase-separating agent polyethylene oxide (relative molecular weight of 1 × 10)6) Until the solution is completely dissolved, adding crystalline aluminum chloride in an ice bath environment, stirring for 40min until the solution is completely dissolved, then adding a gel inducer, namely propylene oxide, under the conditions of normal temperature and normal pressure, and violently stirring for 10min to obtain a mixed sol solution; said Fe2O3The mass of the nanoparticles is 8% of the mass of the aluminium salt; the mass ratio of the polyethylene oxide, the crystalline aluminum chloride and the propylene oxide is 0.06: 4.26: 3.05; the volume concentration of ethanol in the ethanol solution is 40%;
s2, putting the mixed sol solution into a sealed test tube, carrying out sol-gel conversion for 36h in a constant-temperature water bath box at 45 ℃ to obtain wet gel, and then transferring the wet gel to a constant-temperature drying box to dry for 3 days at 60 ℃ to obtain dry gel;
s3, transferring the xerogel to a muffle furnace, and roasting for 6h at 900 ℃ to obtain the iron oxide/aluminum oxide compound.
Example 3
This example proposes an iron oxide/alumina composite prepared by the following steps:
s1, mixing Fe2O3Dispersing the nanoparticles in ethanol solution, performing ultrasonic treatment for 10min, and sequentially adding phase-separating agent polyethylene oxide (relative molecular weight of 1 × 10)6) Until the solution is completely dissolved, adding crystalline aluminum chloride in an ice bath environment, stirring for 30min until the solution is completely dissolved, then adding a gel inducer, namely propylene oxide, under the conditions of normal temperature and normal pressure, and violently stirring for 10min to obtain a mixed sol solution; said Fe2O3The mass of the nanoparticles is 1% of the mass of the aluminium salt; the mass ratio of the polyethylene oxide, the crystalline aluminum chloride and the propylene oxide is 0.1: 4.3: 3.12; the volume concentration of ethanol in the ethanol solution is 40%;
s2, putting the mixed sol solution into a sealed test tube, carrying out sol-gel conversion in a constant-temperature water bath box at 50 ℃ for 18h to obtain wet gel, and then transferring the wet gel to a constant-temperature drying box to dry at 50 ℃ for 5 days to obtain dry gel;
s3, transferring the dried gel to a muffle furnace, and roasting at 800 ℃ for 5h to obtain the iron oxide/aluminum oxide compound.
Example 4
This example proposes an iron oxide/alumina composite prepared by the following steps:
s1, mixing Fe2O3Dispersing the nanoparticles in ethanol solution, performing ultrasonic treatment for 10min, and sequentially adding phase-separating agent polyethylene oxide (relative molecular weight of 1 × 10)6) Until the solution is completely dissolved, adding crystalline aluminum chloride in an ice bath environment, stirring for 30min until the solution is completely dissolved, then adding a gel inducer, namely propylene oxide, under the conditions of normal temperature and normal pressure, and violently stirring for 8min to obtain a mixed sol solution; said Fe2O3The mass of the nanoparticles is 10% of the mass of the aluminium salt; the polyethylene oxide and the knotThe mass ratio of the crystalline aluminum chloride to the propylene oxide is 0.12: 4.26: 3.17; the volume concentration of ethanol in the ethanol solution is 50 percent;
s2, putting the mixed sol solution into a sealed test tube, carrying out sol-gel conversion in a constant-temperature water bath box at 40 ℃ for 28h to obtain wet gel, and then transferring the wet gel to a constant-temperature drying box to be dried at 40 ℃ for 7 days to obtain dry gel;
s3, transferring the dried gel to a muffle furnace, and roasting at 850 ℃ for 5.5h to obtain the iron oxide/aluminum oxide composite.
Comparative example 1
This comparative example differs from example 1 only in that: in step S3, the xerogel is roasted at 700 ℃ to obtain an iron oxide/alumina composite; the other steps are the same.
Comparative example 2
This comparative example used the same amount of Fe as the content ratio of the iron oxide/alumina composite obtained in example 12O3The nano particles and the alumina are physically mixed to obtain a mixture of the nano particles and the alumina.
Application example 1
The Touha thick oil is used as a reactant (the initial viscosity is 36650 mPas at 50 ℃), the iron oxide/alumina composites prepared in examples 1-4 and the samples prepared in comparative example 1 and comparative example 2 are respectively used as catalytic viscosity reducers, the reaction temperature is 120 ℃, the reaction time is 6h, the addition amount of the catalyst is 0.2% of the mass of the thick oil, and the addition amount of water is 10% of the mass of the thick oil. And measuring the viscosity value of the reactant and evaluating the catalytic performance of the catalyst. The viscosity reduction ratio was calculated as Δ η (%) ((. eta.0- η)/. eta.0) × 100%, and η 0 (unit mPa · s) and η (unit mPa · s) respectively represent the viscosity of the oil sample before and after the reaction, and the viscosity reduction ratio and the proportion of the heavy component cracked into the light component were measured after the viscosity reduction, and the results are shown in table 1.
TABLE 1 results of degradation of thickened oils for samples of examples 1 to 4 and comparative examples 1 to 2
Figure BDA0003067195300000071
It can be seen from table 1 that the compounds prepared in examples 1-4 all have good viscosity-reducing effect on thick oil, the viscosity-reducing rate is as high as 75.2%, and the heavy component can be efficiently cracked into light component, and the occupation ratio of the heavy component into the light component is as high as 38.7%. In the comparative example 1, the roasting temperature is low, so that the performance of catalytic degradation of the thick oil of the prepared compound is influenced, the viscosity reduction rate is low, the capability of cracking a heavy component into a light component is also weak, and in addition, the viscosity reduction effect of the compound-free iron oxide and aluminum oxide in the comparative example 2 is obviously poorer, which shows that the compound prepared by the preparation method provided by the application has a certain viscosity reduction effect. Comparative example 2 the reason for the poor viscosity reduction effect may be that the iron oxide nanoparticles are directly mixed with alumina to cause the blockage of the pore channel, which is not favorable for the full contact of the catalyst and the thick oil and influences the catalytic effect.
In addition, the thickened oil after visbreaking in the examples 1 to 4 is detected to have greatly reduced colloid content and greatly increased aromatic hydrocarbon content, and the oxidation reaction is mainly carried out on the colloid in the non-hydrocarbon part.
The iron oxide/aluminum oxide compound provided by the invention can be used for the hydrothermal cracking catalytic viscosity reduction exploitation of the thick oil, can obtain higher thick oil catalytic viscosity reduction efficiency in the thick oil exploitation, is simple in preparation process, provides a new idea for the hydrothermal viscosity reduction of the thick oil, and has good practicability and wide market prospect.
The above-described embodiments of the present invention should not be construed as limiting the scope of the present invention. Any other corresponding changes and modifications made according to the technical idea of the present invention should be included in the protection scope of the claims of the present invention.

Claims (10)

1. A method for preparing an iron oxide/aluminum oxide composite, which is characterized by comprising the following steps:
s1, mixing Fe2O3Dispersing the nano particles in an ethanol solution, and then sequentially adding a phase separation agent, an aluminum salt and a gel inducer to obtain a mixed sol solution;
s2, carrying out sol-gel conversion on the mixed sol solution at 40-50 ℃ to obtain wet gel, and drying the wet gel at 40-60 ℃ to obtain dry gel;
s3, roasting the xerogel at 800-900 ℃ to obtain the iron oxide/aluminum oxide compound.
2. The method according to claim 1, wherein in step S1, the Fe2O3The mass of the nano particles is 1-10% of the mass of the aluminum salt.
3. The production method according to claim 1, wherein in step S1, the mass ratio of the phase separation agent, the aluminum salt, and the gel induction agent is (0.06 to 0.12): (4.26-4.38): (3.05-3.17).
4. The method according to claim 1, wherein the sol-gel conversion is performed for 18 to 36 hours in step S2.
5. The method according to claim 1, wherein the drying is performed at 40 to 60 ℃ for 3 to 7 days in step S2.
6. The method of claim 1, wherein in step S3, the baking time is 4-6 h.
7. The method according to claim 1, wherein in step S1, the aluminum salt is added in an ice bath environment and stirred for 20-40min until the aluminum salt is dissolved, and then the gel inducer is added and stirred for 5-10 min to obtain the mixed sol solution.
8. The production method according to claim 1, characterized in that, in step S1, the phase separation agent is polyethylene oxide; and/or, the gel inducer is propylene oxide; and/or the aluminum salt is aluminum chloride.
9. An iron oxide/alumina composite prepared by the preparation method according to any one of claims 1 to 8.
10. An iron oxide/alumina composite prepared by the preparation method of claims 1-8 or an application of the iron oxide/alumina composite of claim 9 in the degradation of heavy oil.
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