CN111050811A - Method for oxidizing carbon monoxide, carbon monoxide oxidizing apparatus, air cleaner, and gas mask - Google Patents
Method for oxidizing carbon monoxide, carbon monoxide oxidizing apparatus, air cleaner, and gas mask Download PDFInfo
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Abstract
本发明提供一氧化碳的氧化方法，包括在催化剂的存在下以100℃以下的温度将含有一氧化碳气体和氧气的混合气体中的一氧化碳气体利用该混合气体中的氧气进行氧化的工序，混合气体的氯化氢浓度小于1体积％，催化剂包含含有金红石晶型氧化钛的载体和担载于该载体的含钌元素的物质，含钌元素的物质为选自金属钌和钌化合物中的至少1种。The present invention provides a method for oxidizing carbon monoxide, which includes a step of oxidizing carbon monoxide gas in a mixed gas containing carbon monoxide gas and oxygen at a temperature of 100° C. or lower with oxygen in the mixed gas in the presence of a catalyst. The hydrogen chloride concentration of the mixed gas Less than 1% by volume, the catalyst includes a carrier containing rutile crystal titanium oxide and a ruthenium element-containing substance supported on the carrier, and the ruthenium element-containing substance is at least one selected from metal ruthenium and ruthenium compounds.
Description
Technical Field
The present invention relates to a method for oxidizing carbon monoxide, a carbon monoxide oxidation apparatus, an air cleaner and a gas mask.
Background
Conventionally, a method of reducing carbon monoxide by oxidizing carbon monoxide contained in exhaust gas of an automobile and air to form carbon dioxide has been known. As a catalyst for oxidizing carbon monoxide, a catalyst composed of platinum and alumina is known, and for example, japanese patent application laid-open No. 04-215845 (patent document 1) describes that 50% of carbon monoxide contained in an exhaust gas is oxidized at 230 ℃ to carbon dioxide by an oxidation reaction using a catalyst composed of platinum and alumina.
Documents of the prior art
Patent document
Patent document 1: japanese laid-open patent publication No. H04-215845
Disclosure of Invention
In recent years, there has been a demand for a method of oxidizing carbon monoxide at a lower temperature.
The purpose of the present invention is to provide a method capable of oxidizing carbon monoxide even at a temperature of 100 ℃ or lower.
Another object of the present invention is to provide a device, an air cleaner and a gas mask capable of oxidizing carbon monoxide even at a temperature of 100 ℃.
The present invention provides the following.
[1] A method for oxidizing carbon monoxide, comprising a step of oxidizing carbon monoxide gas in a mixed gas containing carbon monoxide gas and oxygen gas at a temperature of 100 ℃ or lower in the presence of a catalyst by oxygen in the mixed gas,
the hydrogen chloride concentration of the mixed gas is less than 1 volume percent,
the catalyst comprises a carrier containing rutile type titanium oxide and a substance containing ruthenium element loaded on the carrier,
the ruthenium element-containing substance is at least 1 selected from the group consisting of metallic ruthenium and ruthenium compounds.
[2] The method for oxidizing carbon monoxide according to item [1], wherein the mixed gas has a relative humidity of 90% RH or less.
[3] The method for oxidizing carbon monoxide according to [1] or [2], wherein the mixed gas contains air.
[4] A carbon monoxide oxidation device is a carbon monoxide oxidation device containing a carbon monoxide oxidation catalyst,
the carbon monoxide oxidation catalyst comprises a support containing rutile type titanium oxide and a ruthenium element-containing substance supported on the support,
the ruthenium element-containing substance is at least 1 selected from the group consisting of metallic ruthenium and ruthenium compounds.
[5] The carbon monoxide oxidation apparatus according to [4], which is an air purifier.
[6] A gas mask is a gas mask containing a carbon monoxide oxidation catalyst,
the carbon monoxide oxidation catalyst comprises a support containing rutile type titanium oxide and a ruthenium element-containing substance supported on the support,
the ruthenium element-containing substance is at least 1 selected from the group consisting of metallic ruthenium and ruthenium compounds.
According to the present invention, a method capable of oxidizing carbon monoxide even at a temperature of 100 ℃ or lower can be provided.
According to the present invention, it is possible to provide a device, an air cleaner, and a gas mask capable of oxidizing carbon monoxide even at a temperature of 100 ℃.
Detailed Description
< carbon monoxide oxidation catalyst >
A method for oxidizing carbon monoxide and a carbon monoxide oxidation catalyst (hereinafter, also referred to as "carbon monoxide oxidation catalyst") used in a carbon monoxide oxidation apparatus according to the present invention will be described.
The carbon monoxide oxidation catalyst comprises a support containing rutile crystalline titanium oxide and a ruthenium element-containing substance supported on the support.
Examples of the ruthenium element-containing substance include at least 1 selected from the group consisting of metallic ruthenium and ruthenium compounds.
The carbon monoxide oxidation catalyst may contain 2 or more species of ruthenium element-containing substances.
The carbon monoxide oxidation catalyst may contain both metallic ruthenium and a ruthenium compound.
(1) Ruthenium compound
The ruthenium compound is a compound containing ruthenium element.
Examples of the ruthenium compound include ruthenium oxide, ruthenium chloride, chlororuthenate hydrate, ruthenate salt, ruthenium oxychloride salt, ruthenium amine complex chloride, ruthenium bromide, ruthenium carbonyl complex, ruthenium organic acid salt, ruthenium nitrosyl complex, and ruthenium phosphine complex.
Examples of ruthenium oxide include RuO2、RuO4。
Examples of ruthenium chloride include RuCl3、RuCl3Hydrates, and the like.
As the chlororuthenate, K is mentioned3RuCl6、〔RuCl6〕3-、K2RuCl6And the like.
As the chlororuthenate hydrate, there may be mentioned [ RuCl ]5(H2O)4〕2-、〔RuCl2(H2O)4〕+And the like.
As the salt of ruthenic acid, K is mentioned2RuO4And the like.
The ruthenium oxychloride may include Ru2OCl4、Ru2OCl5、Ru2OCl6And the like.
The salt of ruthenium oxychloride may include K2Ru2OCl10、Cs2Ru2OCl4And the like.
As ruthenium amine complexesExamples of the compound include [ Ru (NH)3)6〕2+、〔Ru(NH3)6〕3+、〔Ru(NH3)5H2O〕2+And the like.
Examples of the chloride of the ruthenium amine complex include [ Ru (NH)3)5Cl〕2+、〔Ru(NH3)6〕Cl2、〔Ru(NH3)6〕Cl3、〔Ru(NH3)6〕Br3And the like.
Examples of ruthenium bromide include RuBr3、RuBr3Hydrates, and the like.
Examples of the ruthenium carbonyl complex include Ru (CO)5、Ru3(CO)12And the like.
The organic acid salt of ruthenium may be [ Ru3O(OCOCH3)6(H2O)3]OCOCH3Hydrate, Ru2(RCOO)4Cl (R represents an alkyl group having 1 to 3 carbon atoms), and the like.
The nitrosylruthenium complex may include K2〔RuCl5NO)〕、〔Ru(NH3)5(NO)〕Cl3、〔Ru(OH)(NH3)4(NO)〕(NO3)2、Ru(NO)(NO3)3And the like.
From the viewpoint of catalytic activity and acquisition easiness, the ruthenium compound is preferably ruthenium oxide, ruthenium chloride, ruthenium bromide, a salt of ruthenic acid, or a ruthenium nitrosyl complex.
The carbon monoxide oxidation catalyst may contain 2 or more kinds of ruthenium compounds.
From the viewpoint of catalytic activity, the content of the ruthenium element-containing substance in the carbon monoxide oxidation catalyst is preferably 0.1 to 20 wt%, more preferably 0.5 to 10 wt%, and still more preferably 1.0 to 5 wt%, based on the metal ruthenium.
From the viewpoint of catalytic activity, the content of the ruthenium element-containing substance is preferably 0.1 to 20% by weight, more preferably 0.5 to 10% by weight, and still more preferably 1.0 to 5% by weight, based on the metal ruthenium, when the total amount of the ruthenium element-containing substance and the support is 100% by weight.
(2) Support containing rutile crystal form titanium oxide
The carrier contained in the carbon monoxide oxidation catalyst contains titanium oxide (titanium (IV) oxide) in the rutile crystal form. The carrier may contain titanium oxide of anatase crystal form (titanium (IV) oxide) in addition to titanium oxide of rutile crystal form.
From the viewpoint of catalytic activity, the content of rutile type titanium oxide in the titanium oxide contained in the carrier is preferably 20% by weight or more, more preferably 30% by weight or more, further preferably 50% by weight or more, further preferably 80% by weight or more, and particularly preferably 90% by weight or more, with the total amount of titanium oxide contained in the carrier taken as 100% by weight.
The carrier may contain a substance other than titanium oxide. Examples of the substance other than titanium oxide include metal oxides other than titanium oxide.
The carrier may contain a composite oxide of titanium oxide and other metal oxides in addition to the rutile type titanium oxide.
The support may be a mixture of titanium oxide and other metal oxides.
Examples of the metal oxide other than titanium oxide include alumina, silica, and zirconia.
When the carrier contains a substance other than titanium oxide (for example, a metal oxide other than titanium oxide), the content of titanium oxide in the carrier is usually 10% by weight or more, preferably 30% by weight or more, more preferably 40% by weight or more, and further preferably 50% by weight or more.
As a method for producing rutile type titanium oxide, a known method can be used, and for example, the following methods can be mentioned.
A method in which titanium tetrachloride is dropped into ice-cooled water and dissolved, then neutralized with an aqueous ammonia solution at a temperature of 20 ℃ or higher to produce titanium hydroxide (orthotitanic acid), and the precipitate thus produced is washed with water to remove chloride ions, and then fired at a temperature of 600 ℃ or higher (catalytic preparation chemistry, 1989, p 211, lecture).
A method of introducing an oxygen-nitrogen mixed gas into a titanium tetrachloride evaporator to prepare a reaction gas, and introducing the reaction gas into a reactor to perform an oxidation reaction of the reaction gas at 900 ℃ or higher (catalyst preparation chemistry, 1989, page 89, lecture).
A method of hydrolyzing titanium tetrachloride in the presence of ammonium sulfate and then firing the hydrolyzed titanium tetrachloride (for example, the catalyst technical note 10 is a general overview of catalysts by element classification, 1978, page 254, Koshikamiu).
[ d ] method of firing titanium oxide in anatase form (for example, metal oxide and composite oxide, 1980, page 107, lecture).
A method of hydrolyzing an aqueous titanium chloride solution by heating.
A method of mixing an aqueous solution of a titanium compound such as titanium sulfate or titanium chloride with rutile type titanium oxide powder, followed by thermal hydrolysis and alkaline hydrolysis, and then firing at a temperature of about 500 ℃.
The rutile titanium oxide crystal may be a commercially available titanium oxide crystal.
The support may be obtained by shaping the rutile titanium oxide crystal form into a desired shape. In the case where the support contains a metal oxide other than the rutile type titanium oxide, it can be obtained by molding a mixture of the rutile type titanium oxide and the metal oxide other than the rutile type titanium oxide into a desired shape. The obtained molded product may be subjected to operations such as crushing, pulverizing, and classifying.
The support containing rutile type titanium oxide can be confirmed by X-ray diffraction analysis, and the X-ray source is not particularly limited, and for example, K α ray of copper can be mentioned.
When K α radiation of copper was used as an X-ray source, it was confirmed that the carrier contained rutile type titanium oxide by the presence or absence of a diffraction peak at 27.5 degrees 2 θ of the (110) plane, and when the carrier contained anatase type titanium oxide, a diffraction peak at 25.3 degrees 2 θ of the (101) plane was observed.
Therefore, when a copper K α ray is used as the X-ray source, the content ratio (weight ratio) of the rutile crystal to the anatase crystal can be determined from the intensity of the diffraction peak at 27.5 degrees 2 θ of the (110) plane and the intensity of the diffraction peak at 25.3 degrees 2 θ of the (101) plane.
In the X-ray diffraction analysis using K α rays of copper, the carrier may have at least a diffraction peak derived from rutile crystal, or may have a diffraction peak derived from rutile crystal and a diffraction peak derived from anatase crystal.
The rutile titanium oxide or the carrier constituting the carrier may be subjected to surface treatment for the purpose of preventing the catalyst from being degraded in performance due to adsorption of a substance, which causes catalyst poisoning, on the surface of the catalyst.
The substance used for the surface treatment may be either an inorganic substance or an organic substance.
Examples of the inorganic substance used for the surface treatment include metal oxides and metal hydroxides. Examples of the metal constituting the metal oxide and the metal hydroxide include aluminum, silicon, zinc, titanium, zirconium, iron, cerium, tin, and the like.
The inorganic substances used for the surface treatment may be used alone in 1 kind, or 2 or more kinds may be used in combination.
The method for preparing the metal oxide and the metal hydroxide is not particularly limited and may be prepared from the corresponding metal salt. The kind of the metal salt is not particularly limited and is appropriately selected depending on the production method.
Examples of the organic material used for the surface treatment include fatty acids and silylating agents.
Examples of the fatty acid include stearic acid, oleic acid, isostearic acid, and myristic acid.
Examples of the silylating agent include organosilanes, organosilylamines, organosilylamides and derivatives thereof, and organosilazanes.
Examples of the organosilane include trimethylchlorosilane, dichlorodimethylsilane, chlorobromodimethylsilane, nitrotrimethylsilane, triethylchlorosilane, dimethylbutyliodosilane, dimethylphenylchlorosilane, dimethylchlorosilane, dimethyl-n-propylchlorosilane, dimethylisopropylchlorosilane, tert-butyldimethylchlorosilane, tripropylchlorosilane, dimethyloctylchlorosilane, tributylchlorosilane, trihexylchlorosilane, dimethylethylchlorosilane, dimethyloctadecylchlorosilane, n-butyldimethylchlorosilane, bromomethyldimethylchlorosilane, chloromethyldimethylchlorosilane, 3-chloropropyldimethylchlorosilane, dimethoxymethylchlorosilane, methylphenylchlorosilane, triethoxychlorosilane, dimethylphenylchlorosilane, methylphenvinylchlorosilane, benzyldimethylchlorosilane, diphenylchlorosilane, and, Diphenylmethylchlorosilane, diphenylvinylchlorosilane, tribenzylchlorosilane, 3-cyanopropyldimethylchlorosilane, etc.
Examples of the organosilylamines include N-trimethylsilylimidazole, N-t-butyldimethylsilylimidazole, N-dimethylethylsilylimidazole, N-dimethyl-N-propylsilylimidazole, N-dimethylisopropylsilylimidazole, N-trimethylsilyldimethylamine, N-trimethylsilyldiethylamine, N-trimethylsilylpyrrole, N-trimethylsilylpyrrolidine, N-trimethylsilylpiperidine, 1-cyanoethyl (diethylamino) dimethylsilane, pentafluorophenyldimethylsilylamine and the like.
Examples of the organosilylamide and the derivative include N, O-bis (trimethylsilyl) acetamide, N, O-bis (trimethylsilyl) trifluoroacetamide, N-trimethylsilylacetamide, N-methyl-N-trimethylsilyltrifluoroacetamide, N-methyl-N-trimethylsilylheptafluorobutyramide, N- (t-butyldimethylsilyl) -N-trifluoroacetamide, N, O-bis (diethylhydrosilyl) trifluoroacetamide, and the like.
Examples of the organosilazane include hexamethyldisilazane, heptamethyldisilazane, 1,3, 3-tetramethyldisilazane, 1, 3-bis (chloromethyl) tetramethyldisilazane, 1, 3-divinyl-1, 1,3, 3-tetramethyldisilazane, and 1, 3-diphenyltetramethyldisilazane.
Examples of the other silylating agents include N-methoxy-N, O-bis (trimethylsilyl) trifluoroacetamide, N-methoxy-N, O-bis (trimethylsilyl) carbamate, N, O-bis (trimethylsilyl) sulfamate, trimethylsilyl trifluoromethanesulfonate, and N, N' -bis (trimethylsilyl) urea.
The organic materials used for the surface treatment may be used alone in 1 kind, or 2 or more kinds may be used in combination.
From the viewpoint of easily achieving the above object, the silylating agent is preferably an organic silazane, more preferably hexamethyldisilazane.
(3) Other constituents which may be contained in the carbon monoxide oxidation catalyst
The carrier of the carbon monoxide oxidation catalyst may carry a metal element other than ruthenium.
Examples of the metal element other than ruthenium include transition metals such as silver and copper, and typical metals such as zinc and tin.
The metal element other than ruthenium may be supported in a state of being reduced to metal (in the form of a metal simple substance), may be supported in the form of a metal oxide, or may be supported in the form of a composite oxide containing a plurality of metal elements.
Further, the metal element other than ruthenium may be alloyed with ruthenium supported on the carrier, or may be formed into a composite oxide containing ruthenium.
When a carbon monoxide oxidation catalyst is used, the carbon monoxide oxidation catalyst may be diluted with an inactive substance.
(4) Preparation method of carbon monoxide oxidation catalyst
The carbon monoxide oxidation catalyst can be prepared by supporting a ruthenium element-containing substance on a carrier by a method such as an impregnation method, an ion exchange method, or a coprecipitation method. The solvent used in the impregnation method is not particularly limited, and water, ethanol, or the like can be used.
Examples of the shape of the catalyst include spherical particles, cylindrical pellets, rings, honeycombs, monoliths (モノリス), corrugations, and particles of an appropriate size obtained by molding a carrier and then pulverizing and classifying the molded carrier.
In the case of spherical particles, cylindrical pellets or rings, the catalyst diameter is preferably 10mm or less from the viewpoint of catalytic activity. The catalyst diameter referred to herein means the diameter of a sphere when it is spherical, the diameter of a cross section when it is cylindrical and granular, and the maximum diameter of a cross section when it is other shapes.
In the case of a honeycomb shape, a monolith shape, or a corrugated shape, the opening diameter is preferably 20mm or less.
The carbon monoxide oxidation catalyst may be obtained by heat treatment after preparation and before use. This may improve the catalytic activity or prolong the catalyst life.
The heat treatment temperature is not particularly limited, and is usually 100 to 500 ℃.
The heat treatment may be performed in an inert gas such as nitrogen, argon, or helium, in air, or in a gas containing carbon monoxide, hydrogen, or the like.
< method for oxidizing carbon monoxide >
The method for oxidizing carbon monoxide according to the present invention is a method using the above-described catalyst for oxidizing carbon monoxide, and includes a step of oxidizing carbon monoxide gas in a mixed gas containing carbon monoxide gas and oxygen gas at a temperature of 100 ℃ or lower in the presence of the catalyst by oxygen in the mixed gas.
According to the method for oxidizing carbon monoxide of the present invention, since the above-mentioned carbon monoxide oxidation catalyst is used, carbon monoxide can be oxidized by a catalytic reaction even at a reaction temperature of 100 ℃. Carbon dioxide is generated by oxidation of carbon monoxide.
The step of oxidizing may be performed by supplying the mixed gas containing a carbon monoxide gas and an oxygen gas to a housing portion housing the carbon monoxide oxidizing catalyst, for example. At this time, the carbon monoxide gas in the mixed gas is oxidized by the oxygen gas in the mixed gas.
The housing portion may be a part of a device, an appliance, or the like.
A step of preparing a mixed gas containing carbon monoxide gas and oxygen gas by mixing, chemical reaction, or the like of gases may be provided before the step of oxidizing.
The mixed gas may be, for example, a gas containing air, or may be composed of air.
The oxygen contained in the mixed gas can be obtained by a common industrial method such as a pressure swing adsorption method of air, cryogenic separation, or the like.
The hydrogen chloride concentration of the mixed gas is less than 1 vol%, preferably 0.5 vol% or less, more preferably 0.1 vol% or less, and further preferably 0 or substantially 0 vol% (less than the detection limit).
If the hydrogen chloride concentration is less than 1% by volume, the carbon monoxide gas in the mixed gas can be oxidized using the above-mentioned carbon monoxide oxidation catalyst even at a temperature of 100 ℃ or lower. If the hydrogen chloride concentration is 1 vol% or more, the oxidation reaction tends to proceed insufficiently, and the catalyst life tends to be reduced easily.
The concentration of the carbon monoxide gas in the mixed gas may depend on the application of the carbon monoxide oxidation catalyst, and is, for example, 0.0001 to 10 vol%, preferably 0.0005 to 5 vol%, and more preferably 0.001 to 3 vol%.
The concentration of oxygen in the mixed gas is a concentration at which the amount of oxygen contained becomes equal to or more than the theoretical amount required for oxidizing carbon monoxide, and may be, for example, 0.1 to 30 vol%, or 0.1 to 21 vol%. When the mixed gas is air containing carbon monoxide, the oxygen concentration in the mixed gas is usually 21 vol% or less.
The mixed gas may contain other components than carbon monoxide gas and oxygen gas.
Examples of the other components include water vapor, nitrogen, carbon dioxide, helium, aldehydes, fatty acids, sulfur compounds, nitrogen compounds, and the like. The mixed gas may contain only 1 kind of other components, or may contain 2 or more kinds.
When the mixed gas supplied to the carbon monoxide oxidation catalyst contains other components, the other components may be oxidized together in the oxidation step.
The mixed gas may contain water vapor as described above. However, the relative humidity of the mixed gas is preferably 90% RH or less, more preferably 60% RH or less, further preferably 30% RH or less, further preferably 10% RH or less, particularly preferably 5% RH or less, and most preferably 0% RH.
The smaller the moisture content of the mixed gas supplied to the carbon monoxide oxidation catalyst, the higher the catalytic activity, and the higher the conversion rate of carbon monoxide to carbon dioxide tends to increase.
In order to reduce the amount of water in the mixed gas supplied to the carbon monoxide oxidation catalyst, a means for dehydrating the mixed gas may be combined with a device containing the carbon monoxide oxidation catalyst, or the like. Examples of the dehydration treatment include dehydration treatment using a molecular sieve, zeolite, silica gel, or the like.
Examples of the aldehyde include formaldehyde, acetaldehyde, and propionaldehyde.
Examples of the fatty acid include formic acid, acetic acid, and propionic acid.
Examples of the sulfur compound include methyl mercaptan, sulfur dioxide, hydrogen sulfide, carbon disulfide, carbonyl sulfide, and the like.
Examples of the nitrogen compound include trimethylamine, triethylamine, ethylamine, and ammonia.
The step of oxidizing may be performed by bringing the carbon monoxide gas and the oxygen gas in the mixed gas into contact with a carbon monoxide oxidation catalyst to oxidize the carbon monoxide gas in the mixed gas with the oxygen gas in the mixed gas. The contact may be performed by introducing the mixed gas into a housing portion for housing the carbon monoxide oxidation catalyst. The mixed gas may be introduced into a housing portion for housing the carbon monoxide oxidation catalyst by applying pressure, or may be introduced into the housing portion by sucking air.
In one embodiment, the oxidation reaction in the oxidation step is performed by a fixed bed vapor phase flow reaction system, a fluidized bed vapor phase flow reaction system, a rotor-type moving bed reaction system, or the like.
In another embodiment, the oxidation reaction in the oxidation step is performed by leaving the carbon monoxide oxidation catalyst in the mixed gas to be in contact with the mixed gas.
The reaction temperature in the oxidation step is usually 100 ℃ or lower. From the viewpoint of catalytic activity, the reaction temperature is preferably 0 ℃ or higher, more preferably 10 ℃ or higher, and still more preferably 20 ℃ or higher. The reaction temperature is preferably 80 ℃ or lower, more preferably 60 ℃ or lower, still more preferably 50 ℃ or lower, still more preferably 40 ℃ or lower, and particularly preferably 30 ℃ or lower, from the viewpoint of durability of the catalyst.
In the method and apparatus for oxidizing carbon monoxide according to the present invention, the amount of the carbon monoxide oxidation catalyst used is usually 10 to 500000 hours per 1L of the mixed gas supply rate (GHSV) of the carbon monoxide oxidation catalyst in a standard state (0 ℃, 0.1MPa)-1The amount of (c).
In the method for oxidizing carbon monoxide and the carbon monoxide oxidizing apparatus according to the present invention, the gas linear velocity of the mixed gas at the dead tower reference is usually 1m/s to 40 m/s. The superficial gas linear velocity is a ratio of a total amount of supply velocities in a standard state (0 ℃, 0.1MPa) of all gas components supplied to the storage unit to a cross-sectional area of the storage unit such as a reactor. The reaction pressure is usually 0.1MPa to 5 MPa.
< carbon monoxide oxidation device and respirator >
The carbon monoxide oxidation device according to the present invention includes the carbon monoxide oxidation catalyst according to the present invention.
Examples of the carbon monoxide oxidation apparatus include plants in a plant such as a chemical plant or a carbon monoxide oxidation plant constituting a part thereof; machines or machines having a function of oxidizing carbon monoxide.
According to the carbon monoxide oxidation apparatus of the present invention, a gas having a reduced carbon monoxide concentration or containing no carbon monoxide can be obtained. Alternatively, according to the carbon monoxide oxidation apparatus of the present invention, the carbon monoxide concentration in the environment can be reduced, or an environment containing no carbon monoxide can be obtained.
For example, in a carbon monoxide oxidation apparatus installed in a plant, the oxidation reaction in the oxidation step is preferably performed by a fixed-bed vapor phase flow reaction method, a fluidized-bed vapor phase flow reaction method, a rotor-type moving bed reaction method, or the like.
In the carbon monoxide oxidation apparatus installed in a plant, the storage unit for storing the carbon monoxide oxidation catalyst may be a reactor, a reaction tower (catalytic tower), or the like.
In the carbon monoxide oxidation apparatus installed in a plant, the mixed gas introduced into the storage unit may be a gas generated in the plant or the like.
In order to reduce the amount of water in the mixed gas supplied to the housing section for housing the carbon monoxide oxidation catalyst, a device for dehydrating the mixed gas may be provided upstream of the housing section.
Another example of a carbon monoxide oxidation device is an air purifier.
In the air cleaner, the gas supplied to the housing portion housing the carbon monoxide oxidation catalyst is usually a mixed gas composed of air, but is not limited thereto.
In the air cleaner, the concentration of the carbon monoxide gas in the mixed gas supplied to the housing portion housing the carbon monoxide oxidation catalyst may be, for example, 0.001 vol% to 0.1 vol%. The oxygen concentration of the mixed gas is preferably 21 vol% or more.
In order to reduce the amount of water in the mixed gas supplied to the housing section for housing the carbon monoxide oxidation catalyst, a device section for performing dehydration treatment on the mixed gas may be provided upstream of the housing section.
Another example of the carbon monoxide oxidation apparatus is a carbon dioxide laser enclosed gas regeneration apparatus.
In the carbon dioxide laser sealed gas regeneration device, the mixed gas supplied to the housing section housing the carbon monoxide oxidation catalyst is a carbon dioxide laser sealed gas. The oxygen concentration of the enclosed gas is preferably 0.1 to 1.0 vol%, and the carbon monoxide concentration is preferably 0.1 to 2 vol%. The enclosed gas usually contains carbon dioxide. The concentration of carbon dioxide in the enclosed gas is preferably 5 to 20 vol%.
In order to reduce the amount of water in the mixed gas supplied to the housing section for housing the carbon monoxide oxidation catalyst, a device section for performing dehydration treatment on the mixed gas may be provided upstream of the housing section.
The respirator according to the present invention contains the above-described carbon monoxide oxidation catalyst.
By wearing the respirator, carbon monoxide inhalation can be prevented.
The carbon monoxide oxidation catalyst can be applied to devices other than the above-exemplified devices, and appliances and supplies other than gas masks.
Examples
Various measurements were made as follows for the following examples and comparative examples.
(a) supporting ratio of ruthenium-containing substance
The supporting ratio of the ruthenium element-containing substance means a content ratio (wt%) of the ruthenium element-containing substance contained in 100 wt% of the catalyst.
The supporting ratio of the ruthenium element-containing substance was calculated from the following formula.
The supporting ratio (wt%) of the ruthenium element-containing substance was 100 × { (weight of catalyst) - (weight of carrier) }/(weight of catalyst)
Ruthenium content in [ b ] catalyst
The ruthenium content in the catalyst was calculated from the following formula.
The ruthenium content (weight%) in the catalyst was (supporting rate obtained in [ a ] above) × (atomic weight of ruthenium 101.07)/(molar mass of ruthenium oxide 133.07)
The content of rutile type titanium oxide (IV) and the content of anatase type titanium oxide (IV) in the carrier
The support containing titanium oxide was subjected to X-ray diffraction analysis under the following conditions.
(conditions for X-ray diffraction analysis)
The device comprises the following steps: rotor Flex RU200B manufactured by Rigaku corporation "
X-ray source copper K α ray
X-ray output: 40kV-40mA
Divergent slit: 1 degree
Scattering slit: 1 degree
Receiving a slit: 0.15mm
Scanning speed: 1 degree/min
Scanning range: 5.0 to 75.0 DEG
The weight ratio of rutile crystals to anatase crystals in the titanium oxide contained in the carrier is determined by the following formula.
The intensity of the diffraction peak at 27.5 degrees 2 θ of the (110) plane/(the intensity of the diffraction peak at 25.3 degrees 2 θ of the (101) plane) in the weight ratio of the rutile crystal to the anatase crystal
In any of the catalysts prepared in the examples described below, the titanium oxide contained in the carrier was composed of both rutile crystals and anatase crystals. Therefore, the content of rutile crystals in the titanium oxide contained in the carrier is determined by the following formula, assuming that the whole titanium oxide contained in the carrier is 100 wt%.
The content (wt%) of rutile crystals in titanium oxide contained in the carrier is 100 × { (110) plane intensity of diffraction peak 27.5 degrees 2 θ }/{ (110) plane intensity of diffraction peak 27.5 degrees 2 θ + (101) plane intensity of diffraction peak 25.3 degrees 2 θ }
The content of anatase crystals in the titanium oxide contained in the carrier is determined by the following formula, assuming that the whole titanium oxide contained in the carrier is 100 wt%.
The content (wt%) of anatase crystals in titanium oxide contained in the carrier is 100 × { (101) plane intensity of diffraction peak 25.3 degrees 2 θ }/{ (110) plane intensity of diffraction peak 27.5 degrees 2 θ + (101) plane intensity of diffraction peak 25.3 degrees 2 θ }
< example 1 >
(1) Preparation of the catalyst
Rutile titanium oxide (STR-60R made by Sakai chemical industry Co., Ltd., "rutile crystal content: 100 wt.%) 50 parts by weight and α -alumina (AES-12 made by Sumitomo chemical Co., Ltd.)" 50 parts by weight were mixed, and then 12.8 parts by weight of a diluted titanium oxide sol (CSB made by Sakai chemical industry Co., Ltd., "titanium oxide content: 39 wt.% in the titanium oxide sol, and" anatase crystal content: 100 wt.%) was added to 100 parts by weight of the mixture and kneaded.
The obtained kneaded material is extruded into a cylindrical shape having a diameter of 1.5mm phi, dried, and then pulverized into a length of about 2 to 4 mm.
The obtained molded body was fired in air at 650 to 680 ℃ for 3 hours to obtain a carrier composed of a mixture of titania and α -alumina (titania content in the carrier: 55 wt%).
The carrier was impregnated with commercially available ruthenium chloride hydrate (RuCl)3Hydrate) was added, followed by drying. Thereafter, the catalyst (1) was obtained by firing at 250 ℃ for 2 hours in the air. Catalyst (1) containing ruthenium oxide (RuO)2) As a ruthenium element-containing substance supported on the carrier. In the catalyst (1), the supporting ratio of the ruthenium element-containing substance was 4% by weight.
In the above manner, the ruthenium content (Ru content) in the catalyst (1), the rutile crystal content and the anatase crystal content in the titanium oxide contained in the carrier of the catalyst (1) were determined. The results are shown in Table 1.
(2) Oxidation reaction of carbon monoxide
6.0g of the obtained catalyst (1) was charged in a glass tubular reactor having an inner diameter of 16 mm. A mixed gas (composition: carbon monoxide 600ppm, molecular oxygen (oxygen) 21 vol%, nitrogen balance, relative humidity 0% RH, hydrogen chloride concentration 0 vol%) prepared by mixing carbon monoxide, oxygen and nitrogen was supplied at a rate of 1600h-1The reaction mixture was fed into a reactor and reacted at 25 ℃.
The outlet Gas (Gas after reaction) was sampled at 1 hour from the start of the reaction, and the carbon monoxide concentration and the carbon dioxide concentration were analyzed by a Gas probe tube (Gas Tech co., ltd.). The conversion (%) of carbon monoxide was determined based on the following formula. The results are shown in Table 1.
Conversion (%) ═ 100 × (carbon dioxide concentration in outlet gas)/(carbon monoxide concentration in mixed gas)
< example 2 >
(1) Preparation of the catalyst
Rutile Titanium oxide ("F1-R" manufactured by Showa Titanium corporation), rutile content: 93 wt% ]100parts by weight and 29 parts by weight of pure water were used to dilute a titanium oxide sol ("CSB" made by sakai chemical industry co., ltd., titanium oxide content in the titanium oxide sol: 39% by weight, content of anatase form of titanium oxide: 100 wt% ], 12.8 parts by weight, and kneading.
The obtained kneaded material is extruded into a cylindrical shape having a diameter of 3.0mm phi, dried, and then pulverized into a length of about 3 to 5 mm.
The molded body thus obtained was fired in air at 600 ℃ for 3 hours to obtain a carrier composed of titanium oxide (content of titanium oxide in the carrier: 100% by weight).
The carrier was impregnated with commercially available ruthenium chloride hydrate (RuCl)3Hydrate) was added, followed by drying. Thereafter, the catalyst (2) was obtained by firing at 250 ℃ for 2 hours in the air. Catalyst (2) containing ruthenium oxide (RuO)2) As a ruthenium element-containing substance supported on the carrier. In the catalyst (2), the supporting ratio of the ruthenium element-containing substance was 4% by weight.
The ruthenium content (Ru content) in the catalyst (2), the rutile crystal content and the anatase crystal content in the titanium oxide contained in the carrier of the catalyst (2) were determined in the above manner. The results are shown in Table 1.
(2) Oxidation reaction of carbon monoxide
The oxidation reaction of carbon monoxide was carried out in the same manner as in (2) of example 1 except that the supported ruthenium oxide (2) was packed in the reactor, and the conversion (%) of carbon monoxide was determined. The results are shown in Table 1.
< example 3 >
(1) Preparation of the catalyst
The catalyst (1) was obtained in accordance with (1) in example 1.
(2) Oxidation reaction of carbon monoxide
6.0g of the catalyst (1) was charged in a glass tubular reactor having an inner diameter of 16 mm. A raw material gas (composition: carbon monoxide 600ppm, molecular oxygen (oxygen) 21 vol%, nitrogen balance, relative humidity 30% RH, hydrogen chloride concentration 0 vol%) prepared by mixing carbon monoxide, oxygen, nitrogen and water was supplied at a rate of 1600h-1The reaction mixture was fed into a reactor and reacted at 25 ℃.
The outlet Gas (Gas after the reaction) was sampled after 1 hour from the start of the reaction, and the carbon monoxide concentration and the carbon dioxide concentration were analyzed by a Gas probe tube (manufactured by Gas Tech), and the conversion (%) of carbon monoxide was determined in the same manner as in (2) of example 1. The results are shown in Table 1.
< example 4 >
(1) Preparation of the catalyst
The catalyst (1) was obtained in accordance with (1) in example 1.
(2) Oxidation reaction of carbon monoxide
6.0g of the catalyst (1) was charged in a glass tubular reactor having an inner diameter of 16 mm. A raw material gas (composition: carbon monoxide 600ppm, molecular oxygen (oxygen) 21 vol%, nitrogen balance, relative humidity 60% RH, hydrogen chloride concentration 0 vol%) prepared by mixing carbon monoxide, oxygen, nitrogen and water was supplied at a rate of 1600h-1The reaction mixture was fed into a reactor and reacted at 25 ℃.
The outlet Gas (Gas after reaction) at 1 hour from the start of the reaction was sampled, and the concentrations of carbon monoxide and carbon dioxide were analyzed by a Gas probe tube (Gas Tech co., ltd.) to determine the conversion (%) of carbon monoxide in the same manner as in (2) of example 1. The results are shown in Table 1.
< comparative example 1 >
(1) Preparation of the catalyst
Gamma-alumina (made by Strem Chemicals, inc.) was impregnated with a commercially available aqueous solution of chloroplatinic acid hydrate, and then dried. Then, the resultant was fired at 250 ℃ for 2 hours in air to obtain a platinum alumina in which platinum was supported on the γ -alumina carrier at a supporting rate of 3 wt%. The platinum content in the catalyst was 3 wt%.
(2) Oxidation reaction of carbon monoxide
The oxidation reaction of carbon monoxide was carried out in the same manner as in (2) of example 1 except that the obtained platinum alumina was charged into the reactor, and the conversion (%) of carbon monoxide was determined. The results are shown in Table 1.
[ Table 1]
Claims (6)
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| PCT/JP2018/031186 WO2019054151A1 (en) | 2017-09-14 | 2018-08-23 | Method for oxidizing carbon monoxide, device for oxidizing carbon monoxide, air purifier, and gas mask |
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| CN102489295A (en) * | 2011-12-07 | 2012-06-13 | 中国科学院福建物质结构研究所 | Metal-loaded titanium-based catalyst and preparation method thereof |
| JP2014144408A (en) * | 2013-01-28 | 2014-08-14 | Nippon Steel & Sumitomo Metal | Catalyst for oxidation of carbon monoxide, method for manufacturing the same, and method for removing carbon monoxide in gas |
| CN108212149A (en) * | 2017-04-22 | 2018-06-29 | 天津大学 | High dispersive type ruthenium oxide catalysts and its preparation method and application |
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| JP3251009B2 (en) | 1990-10-19 | 2002-01-28 | 株式会社豊田中央研究所 | Exhaust gas purification catalyst |
| JPH05201702A (en) * | 1991-06-03 | 1993-08-10 | General Motors Corp <Gm> | Selective removing method of carbon monoxide and its device |
| JP2869525B2 (en) * | 1996-08-29 | 1999-03-10 | 社団法人日本造船研究協会 | Method and apparatus for removing carbon monoxide in reformed gas |
| JP3404739B2 (en) * | 2000-10-16 | 2003-05-12 | 株式会社豊田中央研究所 | Filter, and air cleaner and air conditioner using the same |
| JP2002226205A (en) * | 2001-01-29 | 2002-08-14 | Sumitomo Chem Co Ltd | How to oxidize carbon monoxide |
| JP4336121B2 (en) * | 2002-03-01 | 2009-09-30 | 石原産業株式会社 | Catalyst and method for producing the same |
| JP4119974B2 (en) * | 2002-12-06 | 2008-07-16 | 独立行政法人産業技術総合研究所 | Catalyst composite for removing carbon monoxide and carbon monoxide removing method using the same |
| JP4857137B2 (en) * | 2007-02-13 | 2012-01-18 | 出光興産株式会社 | Method for producing carbon monoxide removal catalyst |
| US9352300B2 (en) * | 2011-09-19 | 2016-05-31 | University Of The Witwatersrand, Johannesburg | Thermally stable nano-catalyst |
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2018
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- 2018-08-23 JP JP2019541969A patent/JPWO2019054151A1/en active Pending
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102489295A (en) * | 2011-12-07 | 2012-06-13 | 中国科学院福建物质结构研究所 | Metal-loaded titanium-based catalyst and preparation method thereof |
| JP2014144408A (en) * | 2013-01-28 | 2014-08-14 | Nippon Steel & Sumitomo Metal | Catalyst for oxidation of carbon monoxide, method for manufacturing the same, and method for removing carbon monoxide in gas |
| CN108212149A (en) * | 2017-04-22 | 2018-06-29 | 天津大学 | High dispersive type ruthenium oxide catalysts and its preparation method and application |
Non-Patent Citations (1)
| Title |
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| FAN YANG等: "Determining the Behavior of RuOx Nanoparticles in Mixed-Metal Oxides: Structural and Catalytic Properties of RuO2/TiO2(110) Surfaces", 《ANGEW.CHEM.INT.ED.》 * |
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