KR101785408B1 - Fabrication method of monolith catalyst for steam reforming of hydrocarbons - Google Patents
Fabrication method of monolith catalyst for steam reforming of hydrocarbons Download PDFInfo
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- KR101785408B1 KR101785408B1 KR1020150086413A KR20150086413A KR101785408B1 KR 101785408 B1 KR101785408 B1 KR 101785408B1 KR 1020150086413 A KR1020150086413 A KR 1020150086413A KR 20150086413 A KR20150086413 A KR 20150086413A KR 101785408 B1 KR101785408 B1 KR 101785408B1
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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
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/02—Solids
- B01J35/04—Foraminous structures, sieves, grids, honeycombs
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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
- B01J23/06—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of zinc, cadmium or mercury
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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
- B01J23/16—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
- B01J23/24—Chromium, molybdenum or tungsten
- B01J23/26—Chromium
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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
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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
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/0009—Use of binding agents; Moulding; Pressing; Powdering; Granulating; Addition of materials ameliorating the mechanical properties of the product catalyst
- B01J37/0018—Addition of a binding agent or of material, later completely removed among others as result of heat treatment, leaching or washing,(e.g. forming of pores; protective layer, desintegrating by heat)
Abstract
The present invention relates to a catalyst for steam reforming of hydrocarbons, and more particularly to a monolith catalyst for steam reforming of hydrocarbons coated with a honeycomb support by preparing a wash coat by dispersing a transition metal on a carbon-based metal support. The monolith catalyst for steam reforming of hydrocarbon according to the present invention can increase catalytic activity by increasing the contact area with reactants by coating the honeycomb type support with a washcoat in which the transition metal is dispersed in the form of washcoat, Can be produced. In addition, functional groups can be introduced through chemical pretreatment of the support, so that various transition metals can be supported. Therefore, it is possible to use the support and the metal according to the reaction conditions as a catalyst for reforming aliphatic and aromatic hydrocarbons.
Description
The present invention relates to a catalyst for steam reforming of hydrocarbons, and more particularly to a monolith catalyst for steam reforming of hydrocarbons in which a transition metal is dispersed in a carbon-based metal support to prepare wash coats and the honeycomb support is coated.
In the atmosphere in accordance with the use of fossil fuels, the greenhouse gas carbon dioxide (CO 2), methane (CH 4), hydrogen sulfide (H 2 S), carbonyl sulfide (COS) and so on by acid gas concentration is increasing, global warming resulting problem . To solve this problem, electricity generation using fuel cells is a representative technology for reducing greenhouse gas emissions by increasing conversion efficiency, and uses hydrogen and syngas produced by reforming hydrocarbons.
The production of hydrogen and synthesis gas through reforming of hydrocarbons, including fossil fuels, biomass tar, DME, alcohol, Volatile Organic Compounds (VOCs), etc., do. The catalyst used here is mainly prepared by dispersing metal ions on activated alumina, silica, or metal oxide support having a large surface area. However, existing catalysts have a problem that they are easily inactivated by coking of carbon during the reaction.
Of the fixed bed reactors most commonly used for gasification of solid fuels, upflow gasifiers have advantages of low initial investment, availability of fuel with high moisture content and simple process, / Nm < 3 > of hydrocarbons are generated, which may cause adverse effects on the downstream equipment. Therefore, in order to utilize the syngas, purification and removal processes are required. For this purpose, a steam reforming process using a transition metal, particularly nickel (Ni), which is a catalyst of a hydrocarbon decomposition process, is mainly used, and a catalyst metal support capable of evenly dispersing the catalyst in order to increase the efficiency of the catalyst is needed. Also, since the gaseous catalytic reaction occurs on the surface of the solid catalyst, the wider the surface area, the more the reaction by the active substance spreading on the surface increases. That is, when the surface area of the catalyst is increased to maximize the active site, the catalytic activity is increased. At this time, the catalyst support does not exhibit catalytic activity, but serves to maintain and improve the stability and durability of the prepared catalyst.
When a low-grade coal with ion-exchange ability is used as a metal carrier and the transition metal ions are dispersed in a low-grade coal through ion exchange, the catalyst can be dispersed in a very small and even distribution , The related expression is as follows.
2 (-COOH) + Ni 2+ - (COO) 2 Ni + H 2
As such, the use of low grade coal can disperse small and even metal ions more efficiently than with a conventional metal carrier. However, at high temperatures, low grade coal is involved in the steam reforming reaction and losses occur. Therefore, high-grade coal with lower reactivity than low-grade coal can be used at high temperatures.
Japanese Patent Application Laid-Open No. 2006-328268 discloses a biomass gasification method and system using a metal support carrier, and a method and system for recovering metal particles from the metal carrier. In other words, tar was dispersed in low-grade coal by using transition metal as a catalyst for steam reforming with beneficial gas (H 2 + CO) in biodegradation and gasification process. However, when low grade coal is used as a metal support, low grade coal is consumed in the steam reforming reaction at a certain temperature or higher in the steam reforming process.
Korean Patent No. 0542911 relates to a low-pressure catalyst for gasoline reforming used in a fuel cell vehicle, wherein the surface of the ceramic honeycomb carrier is wash-coated with submicron alumina or a precursor thereof to sufficiently enlarge the effective surface area and amount of the catalyst Pressure catalyst for gasoline reforming of a fuel cell vehicle produced by supporting a transition metal catalyst powder. However, this is a catalyst using alumina, which is easily inactivated by coking of carbon during the reaction.
Therefore, it is necessary to develop a catalyst for reforming hydrocarbon steam having high activity and high stability.
SUMMARY OF THE INVENTION The present invention has been made in view of the above problems, and it is an object of the present invention to provide a monolith catalyst for steam reforming of hydrocarbons coated with a honeycomb support by preparing a wash coat by dispersing a transition metal on a carbon-based metal support.
In order to solve the above problem, the present inventors prepared a washcoat composition by dispersing metal ions on a carbon-based metal support through an ion exchange method and wash-coating the honeycomb support with a washcoat composition to prepare a monolith catalyst for steam reforming of hydrocarbons The catalytic activity can be increased by increasing the contact area with the reactant, and the durability is excellent. Thus, the present invention has been completed.
The present invention relates to a honeycomb type support having a gas flow channel formed therein; And a wash coat layer formed on the honeycomb-shaped support, wherein the wash coat layer has a particle diameter of the constituent particles of 1 占 퐉 to 50 占 퐉; And a transition metal ion or a transition metal compound ion dispersed in the metal support. The present invention also provides a monolith catalyst for steam reforming of a hydrocarbon.
The present invention also provides a monolith catalyst for steam reforming of hydrocarbons, wherein the honeycomb-shaped support comprises ceramic or metal and has a gas flow channel of 10 to 1,000 cpsi.
The present invention is further characterized in that the carbon-based metal carrier is at least one selected from the group consisting of peat, argon, lignite, bituminous coal, bituminous coal, anthracite, graphite, active carbon, , Thereby providing a monolith catalyst for steam reforming of hydrocarbons.
The transition metal may be at least one selected from the group consisting of nickel (Ni), iron (Fe), copper (Cu), chromium (Cr) and zinc (Zn) K is a mixture of at least one selected from the group consisting of sodium (Na), calcium (Ca) and magnesium (Mg) and the transition metal.
The present invention also provides a monolith catalyst for steam reforming of hydrocarbons wherein the transition metal or transition metal mixture comprises 3 to 30 weight% of the carbon-based metal support.
The present invention also relates to a method for producing a monolith catalyst for steam reforming of hydrocarbons, the method comprising the steps of supporting a transition metal ion or a transition metal ion mixture on a carbon-based metal support having a particle size of 1 to 50 탆, Lt; / RTI > Mixing the composition with water to produce a washcoat slurry; Forming a washcoat layer on the honeycomb-shaped support inner and outer walls of the slurry; Drying the honeycomb-shaped support having the washcoat layer formed thereon at a temperature ranging from room temperature to 100 ° C, followed by reduction-sintering at 300 ° C to 650 ° C.
The transition metal may be at least one selected from the group consisting of nickel (Ni), iron (Fe), copper (Cu), chromium (Cr) and zinc (Zn) K is a mixture of at least one selected from the group consisting of sodium (Na), calcium (Ca) and magnesium (Mg) and the transition metal, and provides a method for producing a monolith catalyst for steam reforming of hydrocarbons.
The present invention also provides a process for producing a monolith catalyst for steam reforming of hydrocarbons wherein the transition metal or transition metal mixture comprises 3 to 30 weight% of the carbon-based metal support.
The present invention is further characterized in that the carbon-based metal carrier is at least one selected from the group consisting of peat, argon, lignite, bituminous coal, bituminous coal, anthracite, graphite, active carbon, , And a method for producing a monolith catalyst for steam reforming of hydrocarbons.
The present invention also provides a method for producing a monolith catalyst for steam reforming of hydrocarbons, wherein the honeycomb-shaped support is made of ceramic or metal and has a gas flow channel of 10 to 1,000 cpsi.
The present invention further provides a method for producing a monolith catalyst for steam reforming of hydrocarbon, which further comprises the step of acid-treating the carbon-based metal support before carrying the transition metal or transition metal mixture on the carbon-based metal support .
The monolith catalyst for steam reforming of hydrocarbon according to the present invention can increase the catalytic activity by increasing the contact area with reactants as a result of coating the carbon carrier on which the transition metal is dispersed on the honeycomb support in the form of wash coat, A high monolith catalyst can be produced. Also, functional groups can be introduced through the chemical pretreatment of the support, so that various transition metals can be supported. Therefore, it is possible to select necessary support materials and metals according to reaction conditions and use them as aliphatic and aromatic hydrocarbon reforming catalysts .
1 is a schematic view of a honeycomb type support according to an embodiment of the present invention.
Figure 2 is a schematic view of the inside of a monolith catalyst coated with a honeycomb support according to one embodiment of the present invention.
3 is a TEM (transmission electron microscopy) photograph of a washcoat composition according to one embodiment of the present invention.
Prior to the detailed description of the present invention, terms and words used in the present specification and claims should not be construed as limited to ordinary or dictionary terms. Therefore, the embodiments described in this specification and the configurations shown in the drawings are merely the most preferred embodiments of the present invention and do not represent all the technical ideas of the present invention. Therefore, It is to be understood that equivalents and modifications are possible.
In one aspect, the present invention provides a honeycomb-shaped support having a gas flow channel formed therein; And a wash coat layer formed on the honeycomb-shaped support, wherein the wash coat layer has a particle diameter of the constituent particles of 1 占 퐉 to 50 占 퐉; And a transition metal ion or a transition metal mixture ion dispersed in the metal support. The present invention also relates to a monolith catalyst for steam reforming of hydrocarbons.
Hydrocarbon steam reforming is a method of synthesizing hydrogen, carbon monoxide or synthesis gas by reacting hydrocarbons and water vapor at a high temperature in the presence of a catalyst. Generally, carbon monoxide, carbon dioxide and hydrogen are produced by the reaction represented by the following formula (1). The present invention relates to a monolith catalyst for reforming hydrocarbon steam, wherein the monolith catalyst comprises a honeycomb type support having a gas flow channel formed therein and a wash coat layer formed on the honeycomb type support.
The honeycomb-shaped substrate of the present invention has a plurality of parallel longitudinal gas flow channels having a honeycomb structure. FIG. 1 is a schematic illustration of a honeycomb-shaped support of the present invention, wherein the honeycomb-shaped support has gas flow channels of 10 to 1,000 cpsi (cells per square inch), and preferably 200 to 500 cpsi . FIG. 2 shows the inside of the monolith catalyst of the present invention schematically. The
The washcoat layer of the present invention is coated on the honeycomb-shaped support in the form of a thin film, and is composed of a catalyst composition for reforming hydrocarbon steam. The composition includes a carbon-based metal support having particle diameters of 1 to 50 占 퐉, and transition metal ions or transition metal compound ions dispersed in the metal support. Wherein the carbon-based metal support is a low grade coal comprising peat, argon or lignite; High grade coal, including bituminous coal, bituminous coal or anthracite; But are not limited to, one or more selected from the group of advanced carbon sources including graphite, active carbon, and carbon black.
The hydrocarbon steam reforming reaction of the present invention is carried out at 300 to 800 캜. In the case where a conventional low grade coal is used as a catalyst support and a catalyst is produced, the catalyst is operated at a temperature of 400 ° C. to 600 ° C. since it is consumed in the steam reforming process in many cases at a temperature of 400 ° C. or more in the steam reforming reaction (See Takayuki Takarada, Yasukastu Tamei and Akira Tomota, Reactivities of 34 coal under steam gasification, Fuel, 1985, 64, 1438, etc.). Therefore, the hydrocarbon reforming performed at 400 ° C to 600 ° C using the catalyst of the present invention can use low grade coal as the carbon-based metal support. On the other hand, a monolith catalyst using high grade coal, graphite, active carbon, carbon black or the like, which is an advanced carbon source of the present invention, as a metal support is preferable at a high temperature of 600 ° C or higher. When the above-described advanced carbon source is used as the metal support, the hydrocarbon steam reforming reaction can be carried out at a high temperature, so that the reforming reaction of methane, ethane, propane, butane and other aliphatic and aromatic hydrocarbons Lt; / RTI >
The wash coat comprising the carbon-based metal support of the present invention, particularly the wash coat using coal, is advantageous for the dispersion of the metal ion or metal mixture, which is a catalytically active substance, through micropores, and exhibits catalytic activity by itself. In addition, the spent catalyst can be energized, the recovery of the metal ion or the metal mixture after use of the catalyst is easy, and the catalyst deactivation due to carbon deposition during the hydrocarbon reforming can be prevented. In addition, by coating the honeycomb-shaped support in the form of a wash coat, the contact area with the reactant can be maximized to increase the catalytic activity efficiency of the hydrocarbon steam reforming reaction. In the monolith catalyst of the present invention, the carbon-based metal support is required to be atomized to increase the mechanical strength of the washcoat. In one embodiment of the present invention, the average particle diameter of the above-mentioned atomized and ground carbon-based metal support particles is not particularly limited, but is 1 탆 to 50 탆. When the average particle size of the atomized carbon-based metal support is 1 탆 or less or 50 탆 or more, the adhesion to the honeycomb type support or the mechanical strength of the coated wash coat is reduced. Further, the amount of the catalyst that can be coated on the honeycomb type support of the present invention is limited by the coating thickness. If the coating is thick, the channel will be constrained and the pressure loss will be higher when used. Thick coatings can also cause catalyst adhesion problems.
In the case of low-grade coal, especially in the above-mentioned atomized pulverized carbon-based metal carrier, it is possible to disperse the metal without pretreatment because of the existence of an ion exchange functional group in the coal, and other high grade coal such as high grade coal, graphite, it is effective to perform ion exchange by generating a functional group capable of ion exchange through chemical pretreatment for active carbon or carbon black. FIG. 3 is a graph showing the results of a metal-coal washcoat composition prepared by acid treatment of bituminous coal as a high grade coal at 2O < 0 > HNO3 solution for 3 hours at 60 & TEM photograph. It can be seen from the TEM photograph that the metal is evenly dispersed in the bituminous coal. In one embodiment of the present invention, the process for the chemical pretreatment is an acid treatment, wherein the acid treatment includes but is not limited to HCl, H 2 SO 4 , HNO 3 , H 3 PO 4, and H 2 CO 3 , And the amount of ion-exchangeable functional groups is changed depending on acid treatment conditions. The conditions may vary depending on the type or amount of the metal to be ion-exchanged and may be, for example, 1 to 20 hours in an aqueous HNO 3 solution of 1 M to 3 M at a temperature of 60 ° C, but are not limited thereto. A transition metal or a transition metal mixture is dispersed in the acid-treated carbon-based metal support through an ion exchange reaction to prepare a washcoat composition. In one embodiment of the present invention, the transition metal is at least one selected from the group consisting of nickel (Ni), iron (Fe), copper (Cu), chromium (Cr) and zinc (Zn) Is a mixture of at least one selected from the group consisting of potassium (K), sodium (Na), calcium (Ca) and magnesium (Mg) The transition metal or transition metal mixture is contained in an amount of 3 to 30 weight% with respect to the carbon-based metal support.
In another aspect, the present invention is directed to a method for preparing a monolith catalyst for steam reforming of hydrocarbons. The method comprises the steps of forming a washcoat composition by supporting a transition metal ion or a transition metal ion mixture on a carbon-based metal support having a particle size of 1 m to 50 m by preparing a monolith catalyst for steam reforming of hydrocarbons ; Mixing the composition with water to produce a washcoat slurry; Forming a washcoat layer on the honeycomb-shaped support inner and outer walls of the slurry; Drying the honeycomb-shaped support on which the wash-coat layer is formed at a temperature of from room temperature to 100 ° C, and then reducing and sintering the coating at 300 ° C to 650 ° C.
In the case of washcoat, transition metal ions or transition metal compound ions are supported on the atomized and acid treated carbon-based metal support by an ion exchange method to prepare carrier particles carrying the transition metal, and the adhesion of the washcoat and the honeycomb- Such as alumina (Al 2 O 3 ), silica (SiO 2 ), magnesia (MgO), ceria (CeO 2 ), zirconia (ZrO 2 ), and the like, in combination with suitable excipients such as washcoat compositions in water, (Y 2 O 3 ) or perovskite (ABO 3 , A = La, Sr, Ca, Ba, Mg, Y and B = Fe, Cr, Ti, Co, Cu, Mn, Ni, , Sn, Si) and the like to prepare a slurry. In one embodiment, the slurry is prepared by a milling method, and the solids capacity of the slurry is 20 wt% to 60 wt%. The carrier is immersed in the slurry at least once so that a honeycomb type support may be immersed in the prepared slurry and a predetermined lower weight, for example, 30 g / L to about 300 g / L may be adhered to the slurry, By attaching it to the carrier wall, it becomes a monolith type catalyst. The honeycomb type support coated with washcoat is dried at a temperature of from room temperature to 100 ° C for 1 to 10 hours under air injection conditions and then sintered in a reducing atmosphere of N 2 at 300 ° C to 650 ° C.
Hereinafter, embodiments are provided to facilitate understanding of the present invention. However, the following examples are provided only for the purpose of easier understanding of the present invention, and the present invention is not limited to the following examples.
Example
Example 1
The bitterness treated with 2 M HNO 3 for 3 hours was immersed in a Ni ion solution and mixed at room temperature. 5 to 10 weight% of gamma-alumina was added thereto, followed by ball-milling to adjust the particle size to 1 m to 15 m. The viscosity was adjusted appropriately to the coating, followed by a 120 g / L wash coating on a 300 cpsi cordierite honeycomb support in a vacuum suction system. The coated honeycomb type support was dried at 100 ° C., and then calcined in a nitrogen atmosphere at 650 ° C. to prepare a final monolith catalyst.
Example 2
The lignite was immersed in an aqueous mixture of Ni and Cu ions and mixed at room temperature. 5% by weight of ceria (CeO 2 ) and 5% by weight of silica were added thereto, followed by ball milling to adjust the particle size to 1 탆 to 15 탆. The viscosity was adjusted appropriately for the coating and wash coated at 100 g / L on a 300 cpsi cordierite honeycomb support in a vacuum suction system. The coated honeycomb type support was dried at 100 ° C., and then calcined in a nitrogen atmosphere at 650 ° C. to prepare a final monolith catalyst.
While the present invention has been described in connection with what is presently considered to be the preferred embodiments, it is to be understood that the invention is not limited to the disclosed embodiments, but, on the contrary, .
All technical terms used in the present invention are used in the sense that they are generally understood by those of ordinary skill in the relevant field of the present invention unless otherwise defined. The contents of all publications referred to herein are incorporated herein by reference.
1. Monolith catalyst
10. Honeycomb type support
20. Wash coat
21. Carbon-based metal support
22. Transition metal or transition metal mixture
Claims (11)
The method comprises the steps of: preparing a washcoat composition having a particle diameter of 1 탆 to 50 탆 and carrying a transition metal ion or a transition metal composite ion on the carbon-based metal support;
Mixing said composition with water and adding an excipient to prepare a washcoat slurry to a solids content of 20 wt% to 60 wt%;
Forming a washcoat layer on the honeycomb-shaped support inner and outer walls of the slurry;
Drying the honeycomb-shaped support having the washcoat layer at a temperature ranging from room temperature to 100 ° C, followed by reduction-sintering at 300 ° C to 650 ° C,
The transition metal or transition metal mixture is contained in an amount of 3 to 30 wt% based on the carbon-based metal support,
The transition metal is at least one selected from the group consisting of nickel (Ni), iron (Fe), copper (Cu), chromium (Cr) and zinc (Zn)
Wherein the transition metal mixture is a mixture of at least one selected from the group consisting of potassium (K), sodium (Na), calcium (Ca), and magnesium (Mg)
Wherein the excipient is at least one selected from the group consisting of alumina (Al2O3), silica (SiO2), magnesia (MgO), ceria (CeO2), zirconia (ZrO2), yttria (Y2O3)
A method for producing a monolith catalyst for steam reforming of hydrocarbons.
Wherein the carbon-based metal carrier is at least one selected from the group consisting of peat, argon, lignite, bituminous coal, bituminous coal, anthracite, graphite, active carbon,
A method for producing a monolith catalyst for steam reforming of hydrocarbons.
The honeycomb type support body is made of ceramic or metal,
Having gas flow channels of 10 to 1,000 cpsi,
A method for producing a monolith catalyst for steam reforming of hydrocarbons.
Further comprising the step of acid-treating the carbon-based metal support before the transition metal or transition metal mixture is supported on the carbon-based metal support.
A method for producing a monolith catalyst for steam reforming of hydrocarbons.
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