WO2000016898A1 - Catalyseur de decomposition des composes organiques chlores - Google Patents

Catalyseur de decomposition des composes organiques chlores Download PDF

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Publication number
WO2000016898A1
WO2000016898A1 PCT/JP1999/005099 JP9905099W WO0016898A1 WO 2000016898 A1 WO2000016898 A1 WO 2000016898A1 JP 9905099 W JP9905099 W JP 9905099W WO 0016898 A1 WO0016898 A1 WO 0016898A1
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WIPO (PCT)
Prior art keywords
catalyst
carrier
chlorinated organic
catalyst component
gold
Prior art date
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PCT/JP1999/005099
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English (en)
Japanese (ja)
Inventor
Osamu Kajikawa
Shosei Oh
Noboru Kawase
Takeshi Maeda
Tominori Sato
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Osaka Gas Co., Ltd.
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Filing date
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Application filed by Osaka Gas Co., Ltd. filed Critical Osaka Gas Co., Ltd.
Publication of WO2000016898A1 publication Critical patent/WO2000016898A1/fr

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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
    • B01J23/38—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals
    • B01J23/48—Silver or gold
    • B01J23/52—Gold
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
    • B01D53/34—Chemical or biological purification of waste gases
    • B01D53/74—General processes for purification of waste gases; Apparatus or devices specially adapted therefor
    • B01D53/86—Catalytic processes
    • B01D53/8659—Removing halogens or halogen compounds
    • B01D53/8662—Organic halogen compounds
    • 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
    • B01J23/38—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals
    • B01J23/54—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
    • B01J23/66—Silver or gold
    • 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
    • B01J23/89—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with noble metals

Definitions

  • the present invention relates to a catalyst for cracking, particularly to a catalyst for cracking chlorinated organic compounds.
  • PCB polychlorobiphenyl
  • dioxins are a general term for polychlorinated dibenzo-para-dioxins (PCDs) and polychlorinated dibenzofurans (PCDFs).
  • PCDs polychlorinated dibenzo-para-dioxins
  • PCDFs polychlorinated dibenzofurans
  • dioxins are extremely toxic environmental pollutants.
  • tetrachloride Jibenzodai Okishin T 4 CDD s
  • T 4 CDD s tetrachloride Jibenzodai Okishin
  • chlorinated organic compounds such as polychlorobiphenyl, black phenol and black benzene are less toxic than dioxins, but under certain conditions, for example, various elements in fly ash in incinerators Has been found to be easily converted to dioxins in the exhaust gas temperature range using the catalyst as a catalyst, and is therefore recognized as an environmental pollutant, like dioxins. For this reason, from the viewpoint of environmental protection, the need to remove various chlorinated organic compounds from exhaust gas as described above is rapidly increasing.
  • a denitration catalyst composed of vanadium pentoxide, tantalum oxide, and titania, or a catalyst in which platinum is supported on the denitration catalyst
  • silica 'boria' alumina composite oxide and zeolite having a molar ratio of silica to alumina of 30 or more are used.
  • a catalyst in which 0.1 to 10 g of at least one element selected from the group consisting of platinum, palladium and iridium or an oxide thereof is supported per liter of at least one of them Japanese Patent Laid-Open No.
  • a mixed oxide catalyst comprising a vanadate product and an oxide of at least one element selected from the group consisting of yttrium, boron and lead is known.
  • the catalysts can decompose chlorinated organic compounds to some extent, their ability is small and it is often difficult to say that they are truly effective decomposition catalysts for chlorinated organic compounds.
  • the exhaust gas contains particulate and gaseous chlorinated organic compounds, which are difficult to be decomposed by the above-mentioned catalyst.
  • An object of the present invention is to realize a catalyst having high decomposition activity for chlorinated organic compounds. Disclosure of the invention
  • the catalyst for decomposing chlorinated organic compounds according to the present invention comprises a carrier, a first catalyst component comprising a gold element supported on the carrier, and magnesium, aluminum, silicon, Consists of at least one element selected from the group consisting of titanium, manganese, iron, cobanolate, nickel, copper, zinc, yttrium, zirconium, niobium, molybdenum, indium, tin, lanthanum, and cerium.
  • the second catalyst component is included.
  • the carrier used here is, for example, one having oxidation resistance.
  • This carrier is, for example, at least one selected from the group consisting of silica, alumina, zeolite and activated clay.
  • the support has, for example, a specific surface area of at least 100 m 2 Zg and an average pore diameter of at least 10 ⁇ .
  • the carrier is, for example, in at least one form of a fiber state and a particle state.
  • the first catalyst component is 0.05 to 5 g per 100 g of carrier
  • the second catalyst component is per 100 g of carrier:! To 25 g, respectively, and the molar ratio of the first catalyst component to the second catalyst component is set to 0.05 to 0.2.
  • the method for producing a catalyst for decomposing chlorinated organic compounds according to the present invention comprises the steps of: providing a carrier with a gold compound that can be converted to a gold element; magnesium, aluminum, silicon, titanium, manganese, iron, covanolate, nickel, and copper.
  • the gold compound and the precursor are, for example, gold hydroxide and a hydroxide of at least one element selected from the first element group, respectively.
  • the step of converting the gold compound and the precursor to the gold element and the oxide may include, for example, the step of supporting the carrier supporting the gold compound and the precursor at 250 to 700 ° C. a step of heat treatment in one atmosphere selected from among inert gas atmosphere and in air temperature range, the heat-treated carrier 2 0 0 ⁇ 6 0 0 D temperature range of the reducing gas atmosphere of C And further performing a heat treatment.
  • the carrier is subjected to, for example, a pretreatment step in which the carrier is boiled in a 3% to saturated aqueous solution of an inorganic acid in a temperature range from room temperature to a boiling temperature, then washed with water and dried, and per 100 g thereof.
  • a pretreatment step in which the carrier is boiled in a 3% to saturated aqueous solution of an inorganic acid in a temperature range from room temperature to a boiling temperature, then washed with water and dried, and per 100 g thereof.
  • the pretreatment is performed in advance by at least one of the pretreatment steps of the catalyst etching treatment in a reducing gas atmosphere of C.
  • the inorganic acid used at this time is, for example, at least one selected from the group consisting of nitric acid, hydrochloric acid, hydrofluoric acid, sulfuric acid, and phosphoric acid.
  • a gold element and an oxide of a predetermined element are supported on a carrier, so that it has high resolving power and decomposition activity for various chlorinated organic compounds including particles.
  • a chlorinated organic compound decomposition catalyst that can be exhibited can be produced.
  • the catalyst for decomposing chlorinated organic compounds of the present invention is for decomposing various chlorinated organic compounds, and includes a carrier, and a first catalyst component and a second catalyst component supported on the carrier. I have.
  • each of the first catalyst component and the second catalyst component is usually carried on a carrier in a state of being randomly dispersed.
  • the carrier used in the present invention is a known various carrier generally used for supporting various catalyst components, and the shape and form are not particularly limited. For example, even if the carrier is in a fiber state, Or in the form of particles. Further, a mixture of a fiber state and a particle state may be used. Further, it may be in a fibrous state, a particle state or a mixture thereof, into a desired shape (for example, a honeycomb shape). It is preferable that the fibrous carrier is molded into a desired shape and used, since the pressure loss of the gas to be treated is large. However, the carrier in the particulate state is molded because the pressure loss of the gas to be treated is small. It can be used without any modification.
  • the catalyst for decomposing chlorinated organic compounds of the present invention uses a particulate carrier, for example, it is possible to secure prompt circulation of exhaust gas simply by directly filling it into an exhaust gas decomposition treatment tower of an incineration facility. At the same time, it is possible to effectively decompose various chlorinated organic compounds in the form of gas and particles contained in exhaust gas.
  • examples of the fibrous carrier include carbon fibers and activated carbon fibers.
  • the carbon fibers usable here are obtained by spinning various known carbon precursors and infusing or carbonizing them.
  • Activated carbon fibers are obtained by spinning various known carbon precursors, making them infusible or carbonized, and activating them.
  • preferred as carbon fibers and activated carbon fibers are: It is at least one member selected from the group consisting of polyacrylonitrile, rayon, pitch, and lignin-poval, that is, one member selected from the group or a mixture of two or more members.
  • an activated carbon fiber When such an activated carbon fiber is used, its specific surface area and average pore diameter are likely to be set in the preferable ranges described later, and both chlorinated organic compounds in gaseous form and in particulate form can be effectively removed. Can be disassembled.
  • examples of the carrier in the form of particles include silica, alumina, granular charcoal, granular activated carbon, zeolite, and activated clay. Two or more kinds of such particulate carriers may be used as a mixture.
  • granular activated carbon particularly granular activated carbon obtained by chemical activation, has a large specific surface area and is characterized in that the catalyst component is easily dispersed on the surface.
  • the granular activated carbon mentioned here is a concept including powdered activated carbon having a small particle diameter.
  • the average particle size of the carrier in a particulate state is not particularly limited, but is usually preferably 0.1 to 20 mm, more preferably 3 to 1 Omm, in consideration of the pressure loss of the gas to be treated.
  • silica in a particle state used as a carrier in the present invention examples include “Silica Gel A”, “Silica Gel B”, and “Silica Gel RD” (trade names) of Fuji Davison Corporation.
  • the particulate alumina examples include, for example, “Neobead C”, “Neobead D” and “Ne obead SA” (trade names) of Mizusawa Chemical Co., Ltd.
  • Examples of the granular activated carbon include, for example, trade names “C arb T ech—A”, “C arb T ech—B”, “WH 2 C—20 / 48”, and “WH2C—8 32 ",” WH2C-28Z7 OSS ",” G2X-4 / 6_1 "and” G2C-4 / 8 ".
  • powdered activated carbon for example, trade names “M-24”, “M-30” and “M_3” of Osaka Gas Co., Ltd. 8 "and the trade names of Nimura Chemical Co., Ltd.” chemical activated carbon "and” steam activated carbon ".
  • Preferred as the carrier used in the catalyst of the present invention are those having oxidation resistance, for example, silica, alumina, zeolite, activated clay or a mixture of any combination thereof.
  • a carbon-based carrier such as activated carbon fiber coated with polysilane or siloxane and heat-treated can also exhibit oxidation resistance.
  • such carriers themselves are not easily oxidized and are stable, so that it is possible to realize a long-life catalyst for decomposing chlorinated organic compounds exhibiting stable decomposition activity over a long period of time. it can.
  • such a carrier having oxidation resistance usually has a phase transition point in a temperature range of 150 ° C. or more when subjected to thermal analysis (TG analysis), or 250 ° C. Even if left for one month in an oxidizing atmosphere, the weight loss rate is 0.3% or less.
  • a preferable carrier used in the catalyst of the present invention has a specific surface area of at least 100 m 2 / g (ie, at least 100 n ⁇ Z g) and an average pore diameter of at least 10 ⁇ . (That is, 10 ⁇ or more). If the specific surface area of the carrier is less than 100 m 2 / g and the average pore diameter is less than 100 ⁇ , the amount of gas that can be processed per unit weight of the carrier will be small, and the chlorinated organic compound will be included. It may be difficult to efficiently and effectively treat the gas to be treated such as exhaust gas. In addition, the particulate chlorinated organic compound may not be easily adsorbed, and it may be difficult to effectively decompose such a chlorinated organic compound.
  • a specific surface area of the carrier is at least 3 0 O m 2 / g, the at least 5 0 0 m 2 / g and more preferably les.
  • the average pore diameter is more preferably at least 14 angstroms, and even more preferably at least 18 angstroms.
  • the specific surface area mentioned above is The BET specific surface area determined according to the deposition method.
  • the average pore diameter is a value calculated from the BET specific surface area measured by the nitrogen adsorption method and the value of the pore volume.
  • a porous carrier as described above When a porous carrier as described above is used, its pore volume can be determined by the specific surface area and the average pore diameter described above, but is usually at least 0.15 cc / g (ie, 0.15 cc / g). cc / g or more), and more preferably at least 0.50 cc / g.
  • the pore volume referred to here is the total pore volume that can be determined according to the nitrogen adsorption method.
  • the above-mentioned carrier used in the present invention may be appropriately surface-treated for the purpose of increasing the carrying amount of the first catalyst component and the second catalyst component. Examples of the surface treatment include a boiling treatment with an aqueous solution of an acid and a catalyst etching treatment as described below.
  • the first catalyst component supported on the carrier as described above is made of fine particles of gold, particularly gold.
  • the amount of the first catalyst component supported on the carrier is usually set to 0.05 to 5 g, preferably 0.1 to 3 g, more preferably 0.5 to 2 g per 100 g of the carrier. If the supported amount is less than 0.05 g, the catalyst of the present invention may hardly exhibit catalytic activity, that is, almost no activity for decomposing chlorinated organic compounds. Conversely, if it exceeds 5 g, the size of the gold particles increases, and the catalytic activity of the catalyst of the present invention may be extremely reduced.
  • the first catalyst component is usually supported on a carrier in the form of fine particles having an average particle diameter of 20 nm or less.
  • the second catalyst component supported on the carrier is magnesium, aluminum, silicon, titanium, manganese, iron, covanolate, nickel, copper, zinc, yttrium, zirconium, niobium, molybdenum, indium, tin, lanthanum, and cerium.
  • Group of elements consisting of Pt (1st group of elements) Power An oxide of the selected element.
  • the second catalyst component may be a mixture of two or more oxides of an element selected from the element group.
  • Acid I dry matter described above is not particularly limited to a variety of oxides of elements included in the element group described above, for example, magnesium oxide (MgO), aluminum oxide Niumu (A 1 2 0 3) oxide Kei element (S i 0, S i 0 2), titanium oxide (T i 0, T i 2 ⁇ 3, T i O 2), manganese oxide (MnO, Mn 3 0 4, Mn 2 0 3, Mn 0 2, Mn0 3, Mn 2 0 7), Sani ⁇ (F E_ ⁇ , F e 3 ⁇ 4, F e 2 0 3) , Sani ⁇ Kono Noreto (CoO, Co 2 0 3, Co 3 ⁇ 4, CO0 2), nickel oxide (N i ⁇ , N i 3 0 4, N I_ ⁇ 2), copper oxide (Cu0 2, CuO), zinc oxide (ZnO), Sani ⁇ yttrium (Y 2 ⁇ 3) acid I arsenide zirconium (Z R_ ⁇ 2), niobium oxide (NbO,
  • the amount of the second catalyst component supported on the carrier is usually set to 1 to 25 g, preferably 5 to 25 g, more preferably 12 to 20 g per 100 g of the carrier. If the supported amount is less than 1 g, the catalyst of the present invention may hardly show any catalytic activity. Conversely, if it exceeds 25 g, the second catalyst component may be separated from the carrier.
  • the ratio between the first catalyst component and the second catalyst component supported on the carrier is usually
  • the molar ratio of the first catalyst component to the two catalyst components is set to be 0.005 to 0.2, preferably 0.01 to 0.2, and more preferably 0.03 to 0.15. If this molar ratio is less than 0.005, the catalyst of the present invention may hardly exhibit catalytic activity. Conversely, if it exceeds 0.2, the size of the fine gold particles as the first catalyst component becomes large, and the catalytic activity of the catalyst of the present invention may be extremely reduced.
  • the catalyst for decomposing chlorinated organic compounds of the present invention can be basically produced by supporting a first catalyst component and a second catalyst component on a carrier. For this purpose, it is preferable to previously modify the surface chemical state.
  • the catalyst etching treatment is a treatment in which a predetermined catalyst is dispersed in a carrier, and the existing pores of the carrier are enlarged or new pores are formed in the carrier by the action of the catalyst.
  • the carrier subjected to such a surface modification treatment has improved adhesion of the first catalyst component and the second catalyst component, and can increase the amount of these catalyst components carried.
  • the specific surface area, pore volume, and average pore diameter of the carrier can be increased, so that the adsorptivity of the particulate chlorinated organic compound is increased, and the decomposition characteristics are improved. Can be enhanced.
  • gold as first catalyst component, also a mixture of iron oxide as a second catalyst component (Fe 2 0 3) and lanthanum oxide (La 2 ⁇ 3), it
  • the total amount of the supported catalyst is pitch-based. It is only 2.5% by weight per 100 g of activated carbon fiber.
  • the carrier was used as the carrier.
  • gold is used as the first catalyst component
  • magnesium oxide (MgO) is supported as the second catalyst component by the coprecipitation method using an aqueous sodium carbonate solution as a precipitant
  • pitch-based activated carbon is used. If the fiber is not subjected to a catalyst etching treatment, the total amount of the supported catalyst is only 3.1% by weight per 100 g of the pitch-based activated carbon fiber.
  • the aqueous acid solution used when the carrier is boiled in an aqueous acid solution to modify its surface chemical state is an aqueous inorganic acid solution.
  • the inorganic acid that can be used here include nitric acid, hydrochloric acid, hydrofluoric acid, sulfuric acid, and phosphoric acid.
  • Such an aqueous solution of an inorganic acid may be prepared by mixing two or more inorganic acids.
  • the concentration of the inorganic acid is usually preferably set to 3% to a saturated concentration, but a higher acid concentration usually gives a better surface modification effect.
  • the boiling temperature of the carrier with the aqueous solution of an acid described above can be set in a range from room temperature to the boiling temperature of the aqueous solution of the acid, and the boiling time is usually 1 minute or more. Is set. The higher the boiling temperature and the longer the boiling time, the better the surface modification effect.
  • the treated carrier is washed with water.
  • the decomposition activity of the catalyst for decomposing chlorinated organic compounds of the present invention may be reduced.
  • the etching catalyst is dispersed in the carrier.
  • the etching catalyst used herein is, for example, at least one metal element selected from the group consisting of iron, nickel, ruthenium, rhodium, palladium, and platinum (second element group).
  • the dispersion amount of such an etching catalyst is usually 0.01 to 5 g, preferably 0.05 to 2.0 g, more preferably 0.1 to 1.0 g per 100 g of the carrier. Set to 0 g. If the amount of dispersion is less than 0.01 g, the surface of the carrier may not be sufficiently modified. Conversely, if it exceeds 5 g, the entire surface of the carrier may be catalytically etched, and fine surface irregularities may not be formed.
  • the above-mentioned etching catalyst may be dispersed in a carrier as a compound of the above-mentioned metal element.
  • the above dispersion amount is a value in terms of a metal element.
  • the compound of the metal element for example, acetate, nitrate, sulfate and the like can be used.
  • a method of dispersing the etching catalyst in the carrier various known methods, for example, a known metal dispersion method such as an impregnation method, a precipitation method, a coprecipitation method, and a vapor deposition method can be adopted. These dispersion methods can be appropriately selected according to the type of the above-mentioned metal element or its compound.
  • the support is heat-treated in a temperature range of 300 to 700 ° C (preferably 350 to 550 ° C).
  • a sufficient etching effect may not be provided to the carrier.
  • the temperature exceeds 700 ° C., fine particles of the etching catalyst dispersed in the carrier grow and sinter, so that a sufficient etching effect may not be obtained.
  • the treatment time is preferably set to 5 minutes or more, but the longer the treatment time, the higher the surface treatment effect.
  • the oxygen-containing functional group on the surface of the carrier and the carbon-carbon bond having a weak binding force are formed under the action of the above-mentioned etching catalyst exhibiting hydrogenation activity.
  • the carrier subjected to the catalytic etching treatment has an increased specific surface area, pore volume, and average pore diameter.
  • the surface of the support after the catalyst etching treatment changes in the surface chemical state, such as the distribution of functional groups and the concentration of the functional groups, as compared with before the treatment, and the metal or metal compound, that is, the first catalyst component and the second catalyst The adhesion of the components increases.
  • the above-mentioned boiling treatment and catalyst etching treatment for the carrier may be performed either or both, or both.
  • the order of the treatment is not particularly limited, and the boiling treatment may be performed before the catalyst etching treatment, or the boiling treatment may be performed after the catalyst etching treatment.
  • a porous carrier having a specific surface area and an average pore diameter set as described above is used as the carrier, the specific surface area and the average pore diameter of the carrier are determined before the boiling treatment and the catalyst etching treatment as described above.
  • the above range may be set before the processing, or the above range may be set by the above preprocessing. In other words, this type of support should have its specific surface area and average pore diameter set within the above ranges before the catalyst component supporting step described below.
  • the first catalyst component and the second catalyst component are supported on the carrier treated as described above.
  • various known methods for example, a chemical method such as an impregnation method, a precipitation and precipitation supporting method, a coprecipitation method, and a precipitation method with magnesium citrate, and A known method of dispersing and supporting a metal or a metal compound, such as a physical method such as an evaporation method or a kneading method, can be employed.
  • a gold compound that can be converted into a first catalyst component that is, gold
  • a second catalyst component that is, an oxide of an element as described above
  • a gold hydroxide can be used as the gold compound, and a hydroxide of the above-mentioned element constituting the second catalyst component can be used as the precursor.
  • a hydroxide of the above-mentioned element constituting the second catalyst component can be used as the precursor.
  • Such various hydroxides can be provided to a carrier by employing, for example, the above-mentioned coprecipitation method.
  • the gold hydroxide and the hydroxides of the above elements applied to the carrier are usually heat-treated in an inert gas atmosphere, and then, if necessary, in a reducing gas atmosphere. By performing the above, it is possible to convert them into the desired gold and oxides of the above-described elements, respectively.
  • the carrier is silica or aluminum, which has oxidation resistance.
  • the heat treatment step in an inert gas atmosphere may be performed in air.
  • the heat treatment in an inert gas atmosphere converts the hydroxide of the above-mentioned element supported on the carrier into a target oxide to form the second catalyst component. It is a process of.
  • the heat treatment temperature here is usually from 250 to 700 ° C., preferably from 300 to 45 ° C. (Set to TC. If this treatment temperature is lower than 250 ° C., If the temperature exceeds 700 ° C., the produced metal oxide is sintered, and the activity of the catalyst of the present invention is reduced.
  • the heat treatment time is usually preferably set to 5 minutes or more, and when the heat treatment time is less than 5 minutes, the hydroxide of the above-mentioned element is converted into the target oxide. Unfortunately, there are cases.
  • the gold oxide generated simultaneously by the heat treatment in the above-mentioned inert gas atmosphere (or in the air) is reduced and converted into a gold element itself.
  • This is a step for forming a first catalyst component.
  • the heat treatment temperature here is usually set at 200 to 600 ° C, preferably at 250 to 400 ° C. If the treatment temperature is lower than 200 ° C., it may be difficult to convert the gold oxide into the gold element. Conversely, when the treatment temperature exceeds 600 ° C., other oxides (ie, the second catalyst component) generated by the heat treatment in the above-described inert gas atmosphere (or in the air) may contain metallic elements.
  • the heat treatment time is usually preferably set to 5 minutes or more in order to easily convert the gold oxide to a gold element.
  • the above-mentioned inert gas atmosphere Alternatively, other oxides formed by the heat treatment in the air
  • the treatment temperature and treatment time need to be adjusted appropriately so that only the gold oxide is reduced and converted to elemental gold. Since the catalyst for decomposing chlorinated organic compounds of the present invention has the first catalyst component and the second catalyst component supported on the above-described carrier, it can be converted into dioxins and dioxins.
  • PCB polychlorobiphenyl
  • trichloroethylene trichloroethane
  • dichloromethane chlorophenol
  • chlorobenzene and other halogenated hydrocarbon compounds. It can be broken down and converted to non-toxic low molecular weight compounds.
  • the catalyst for decomposing chlorinated organic compounds of the present invention can, of course, effectively oxidatively decompose gaseous chlorinated organic compounds, but has a very high decomposition activity, so that it can be treated with conventional catalysts.
  • the difficult chlorinated organic compound in particulate form can be effectively oxidatively decomposed at the same time.
  • the particulate chlorinated organic compound may be used in the present invention because of the unique porous structure of the carrier.
  • the catalyst is easily trapped (adsorbed) by the catalyst, and can be effectively oxidatively decomposed in the trapped state.
  • chlorinated organic compounds such as dioxins contained in the exhaust gas are used. 95% or more of the compounds are oxidatively decomposed at a space velocity of 5,000 hr- 1 or more within a temperature range of 150-300 ° C for more than 50,000 hr, and are easily converted to non-toxic low-molecular compounds. As a result, it is easy to reduce the concentration of dioxins and the like in the exhaust gas released into the atmosphere to several ng ZNm 3 or less in terms of international equivalent toxicity.
  • the catalyst of the present invention uses the above-mentioned catalyst having oxidation resistance as a carrier, the activity of the catalyst is hardly reduced even when used continuously in a high-temperature atmosphere.
  • stable decomposition activity for chlorinated organic compounds can be maintained for a long period of time.
  • the activated carbon fibers supporting the above-mentioned hydroxyl compound are filled in a ceramic tubular electric furnace, fired in a nitrogen atmosphere at 450 ° C for 2 hours, and then fired in a hydrogen atmosphere at 350 ° C. Further reduction treatment was performed for one hour.
  • the gold as a first catalyst component, iron oxide (Fe 2 ⁇ 3) and lanthanum oxide (La 2 0 3) and chlorinated organic compound decomposing supported on activated carbon fiber as the second catalyst component Catalyst was obtained.
  • This catalyst has a weight ratio of the first catalyst component to the second catalyst component (first catalyst component / second catalyst component) of 7.5 / 100, and iron oxide and lanthanum oxide constituting the second catalyst component.
  • the weight ratio with tan (lanthanum oxide / iron oxide) was 30Z70, and the weight ratio between the total of all catalyst components and the activated carbon fiber (total catalyst component / activated carbon fiber) was 13.0 / 10.
  • the catalyst for decomposing the chlorinated organic compound obtained in this manner is The activity of degrading phenol by phenol was evaluated.
  • the obtained catalyst for decomposing chlorinated organic compounds was filled in a flow reactor using a stainless steel reaction tube (inner diameter 19 mm x length 40 Omm) with an internal volume of 113 ml. OO Oh r- ', temperature 220.
  • air containing 3,500 ppm of o-chlorophenol was flowed as a sample.
  • the o-chlorophenol concentration in the sample before and after passing through the reactor was analyzed using a gas chromatograph equipped with an FID detector, and the analysis value was used to determine the o-chlorophenol content according to the following formula.
  • the solution rate was determined. The result was 95.6%.
  • Example 1 100 g of the same coal tar pitch-based activated carbon fiber as used in Example 1 was boiled under the same conditions as in Example 1.
  • An aqueous solution in which 95.44 g was dissolved and 1,000 g were placed in a beaker equipped with a digital pH meter. Then, while stirring the solution in the beaker, a 5% by weight aqueous solution of sodium carbonate was slowly dropped, and the pH of the solution was set to 10.2. Thereafter, the activated carbon fiber was taken out of the beaker, washed with water, and dried at 120 ° C. for 8 hours. As a result, active raw carbon fibers supporting the respective hydroxides of gold and magnesium were obtained.
  • the obtained activated carbon fiber was heat-treated in a nitrogen atmosphere and a hydrogen atmosphere under the same conditions as in Example 1 to obtain gold as the first catalyst component and magnesium oxide as the second catalyst component.
  • MgO magnesium oxide
  • This catalyst is composed of the first catalyst component and the second catalyst component.
  • Weight ratio (1st catalyst component / 2nd catalyst component) was 6.3X100, and the weight ratio of the total of all catalyst components to the activated carbon fiber (all catalyst components Z activated carbon fiber) was 13.5 / 100.
  • the resulting chlorinated organic compound decomposition catalyst was evaluated for its acid-decomposition activity against o-chlorophenol in the same manner as in Example 1, and the result was 84.3%.
  • Example 1 100 g of the same coal tar pitch-based activated carbon fiber as used in Example 1 was boiled under the same conditions as in Example 1.
  • the obtained activated carbon fiber was heat-treated in a nitrogen atmosphere and a hydrogen atmosphere under the same conditions as in Example 1 to obtain gold as the first catalyst component and iron oxide as the second catalyst component.
  • (Fe 2 ⁇ 3) and Sani ⁇ cerium (CeO 2) was obtained chlorinated organic I ⁇ decomposition catalyst supported on activated carbon fibers.
  • the weight ratio of the first catalyst component to the second catalyst component was 6.5 / 100, and cerium oxide and iron oxide constituting the second catalyst component were used.
  • the weight ratio (cerium oxide / iron oxide) was 30 Z70, and the weight ratio (total catalyst component / activated carbon fiber) of the sum of all catalyst components and activated carbon fiber was 13.7Z100.
  • the chlorinated organic compound decomposition catalyst obtained was evaluated for its oxidative decomposition activity against o-chlorophenol in the same manner as in Example 1, and the result was 93.3%.
  • the activated carbon fibers in which nickel acetate was dispersed were filled into a ceramic tubular electric furnace, and were subjected to an etching treatment in a 100% hydrogen atmosphere set at 500 ° C. for 4 hours. And the total amount of the thus etched treated active carbon fiber, salt gold tetrahydrate (HAuC 1 4 ⁇ 4H 2 0 ) 3. 24 g, iron nitrate (F e (N0 3) 3 '6H 2 0) 53. 13 g and lanthanum nitrate (L a (N0 3) 3 ⁇ 6H 2 0) 11. solution 1 obtained by dissolving 96 g, was placed in a 000 g in a beaker fitted with a digital pH meter.
  • the obtained activated carbon fiber was placed in a nitrogen atmosphere under the same conditions as in Example 1. And heat-treated in a hydrogen atmosphere, and gold as the first catalyst component, iron oxide as a second catalyst component (F e 2 0 3) and lanthanum oxide (La 2 0 3) and active carbon fiber ⁇ Thus, a catalyst for decomposing chlorinated organic compounds supported on was obtained.
  • the weight ratio of the first catalyst component to the second catalyst component was 8.0 / 100, and lanthanum oxide and iron oxide constituting the second catalyst component were used.
  • the weight ratio (San-i-lantern Z iron oxide) was 30/70, and the weight ratio of the total of all the catalyst components to the activated carbon fibers (all the activated carbon fibers) was 14.2Z100.
  • the chlorinated organic compound decomposition catalyst obtained was evaluated for acid decomposition activity against o-chlorophenol in the same manner as in Example 1, and the result was 97.
  • Example 4 The same operation as in Example 4 was carried out except that activated carbon fibers which were boiled in the same manner as in Example 1 were used, and gold as the first catalyst component and iron oxide as the second catalyst component were used. (F e 2 O 3) and to obtain a lanthanum oxide (La 2 0 3) and is supported on the active carbon fiber chlorinated organic I arsenide compound cracking catalyst.
  • the weight ratio of the first catalyst component to the second catalyst component was 9.8 / 100, and lanthanum oxide and iron oxide constituting the second catalyst component were used.
  • the weight ratio (lanthanum oxide / iron oxide) was 30,770, and the weight ratio (total catalyst component / activated carbon fiber) of the total of all catalyst components to activated carbon fiber was 14.9Z100.
  • the obtained chlorinated organic compound decomposition catalyst was evaluated for o-chlorophenol enzymatic decomposition activity in the same manner as in Example 1, and the result was 99.5%.
  • solution 1 obtained by dissolving 96 g, and 000 g in a beaker fitted with a digital p H meter . Then, while stirring the solution in the beaker, a 5% by weight aqueous solution of sodium carbonate was slowly dropped, and the pH of the solution was set to 8.0. Thereafter, the silica gel was taken out of the beaker, washed with water, and dried at 120 ° C. for 8 hours. As a result, a silica gel carrying the respective hydroxy compounds of gold, iron and lanthanum was obtained.
  • the silica gel used here had a phase transition point in the temperature range of 150 ° C. or higher when subjected to thermal analysis, and had oxidation resistance.
  • the above-mentioned hydroxide-supported silica gel was charged into a ceramic tubular electric furnace, fired in an air atmosphere at 450 ° C for 2 hours, and then further heated in a hydrogen atmosphere at 350 ° C for 1 hour. Reduction treatment was performed.
  • the gold as a first catalyst component
  • the second iron oxide as a catalyst component (F e 2 0 3) and lanthanum oxide (La 2 ⁇ 3) and chlorinated organic Ihigo supported on silica gel
  • This catalyst had a weight ratio of the first catalyst component to the second catalyst component (the first catalyst component Z and the second hornworm medium component) of 7.5 / 100.
  • the weight ratio with lanthanum (lanthanum oxide / iron oxide) was 30/70, and the weight ratio with the total of all catalyst components and silica gel as the support (all catalyst components Z silica gel) was 8.5 / 100.
  • the above-mentioned alumina gel supporting the hydroxyl compound was filled in a ceramic tubular electric furnace, fired in an air atmosphere of 450 ° C for 2 hours, and further heated in a hydrogen atmosphere of 350 ° C. Reduction treatment was performed for 1 hour.
  • the gold as a first catalyst component for iron oxide (Fe 2 0 3) and lanthanum oxide (La 2 ⁇ 3) and chlorinated organic compounds supported on alumina gel degradation as the second catalyst component A catalyst was obtained.
  • This catalyst has a weight ratio of the first catalyst component to the second catalyst component (first catalyst component Z second catalyst component) of 7.5 / 100, and iron oxide and lanthanum oxide constituting the second catalyst component.
  • the weight ratio with tan (lanthanum oxide / iron oxide) was 30/70, and the weight ratio between the total of all catalyst components and the alumina gel as the carrier (all catalyst components Z alumina gel) was 9.9 / 100.
  • the resulting chlorinated organic compound decomposition catalyst was evaluated for its acid-decomposition activity against o-chloromouth phenol in the same manner as in Example 1, and the result was 76.
  • solution 1 obtained by dissolving 96 g, and 000 g in a beaker fitted with a digital p H meter. Then, while stirring the solution in the beaker, a 5% by weight aqueous solution of sodium carbonate was slowly dropped, and the pH of the solution was set to 8.0. Thereafter, the granular activated carbon was taken out of the beaker, washed with water, and dried at 120 ° C for 8 hours. As a result, a granular activated carbon carrying the respective hydroxides of gold, iron and lanthanum was obtained.
  • the above-mentioned granular activated carbon supporting the hydroxide is filled in a ceramic tubular electric furnace, and calcined in a nitrogen atmosphere at 450 ° C for 2 hours, and then further heated in a hydrogen atmosphere at 350 ° C. Time reduction treatment was performed.
  • the gold as a first catalyst component iron oxide (F e 2 0 3) and lanthanum oxide (La 2 0 3) and chlorinated organic compound decomposing supported on granular activated carbon as the second catalyst component Catalyst was obtained.
  • the weight ratio of the first catalyst component to the second catalyst component was 7.5 / 100, and iron oxide and lanthanum oxide constituting the second catalyst component were used.
  • Weight ratio (lanthanum oxide Z iron oxide) was 30770, and the weight ratio of the total of all the catalyst components to the granular activated carbon as the carrier (all the catalytic components were granular activated carbon) was 11.2Z100.
  • the powdered activated carbon supporting the above-mentioned hydroxide was filled in a ceramic tubular electric furnace, fired in a nitrogen atmosphere at 450 ° C for 2 hours, and then fired in a hydrogen atmosphere at 350 ° C. For another 1 hour.
  • the gold as a first catalyst component iron oxide (F e 2 ⁇ 3) and lanthanum oxide (L a 2 0 3) and is supported on a powdered activated carbon chlorinated organic as the second catalyst component
  • a catalyst for compound decomposition was obtained.
  • This catalyst had a weight ratio of the first catalyst component to the second catalyst component (first catalyst component Z, second catalyst component) of 7.5Z100, and iron oxide and lanthanum oxide constituting the second catalyst component.
  • the weight ratio (lanthanum oxide / iron oxide) is 30/70, and the weight ratio of the total of all catalyst components to the powdered activated carbon as a carrier (all catalyst components powdered activated carbon) is 16.5 / 100 Met.
  • the resulting chlorinated organic compound decomposition catalyst was evaluated for its oxidative decomposition activity against o-chlorophenol in the same manner as in Example 1, and the result was 10
  • the activated clay used here had a phase transition point in a temperature range of 150 ° C. or higher when subjected to thermal analysis, and had oxidation resistance.
  • the activated clay supporting the above-mentioned hydroxide was filled in a ceramic tubular electric furnace, and calcined in an air atmosphere at 450 ° C for 2 hours, and then reduced for 35 hours in a hydrogen atmosphere of TC (1 hour). treated.
  • the gold as a first catalyst component, a chlorinated organic to the iron oxide as a second catalyst component (Fe 2 0 3) and lanthanum oxide (La 2 0 3) is supported on the activated clay
  • a catalyst for decomposing a compound was obtained having a weight ratio of the first catalyst component to the second catalyst component (first catalyst component Z second catalyst component) of 7.5 / 100.
  • the weight ratio of iron oxide and lanthanum oxide (lanthanum oxide / iron oxide) constituting the second catalyst component is 30770, and the weight ratio of the sum of all catalyst components and activated clay as a carrier (total catalyst component / activated clay) was 9.3Z100.
  • the obtained catalyst for decomposing chlorinated organic compounds was evaluated for oxidative decomposition activity against o-chloromouth phenol in the same manner as in Example 1, and the result was 92.
  • a garbage incinerator equipped with an exhaust gas decomposition tower as shown in Fig. 1 was constructed.
  • the refuse incinerator 1 mainly includes an incinerator 2, an exhaust gas decomposition treatment tower 3, and an exhaust gas flow path 4 for connecting the incinerator 2 and the exhaust gas decomposition treatment tower 3.
  • the incinerator 2 includes a primary incinerator 5 and a secondary incinerator 6 disposed above the primary incinerator 5.
  • the primary incinerator 5 has a combustion chamber 7 for incinerating garbage 20, and an exhaust passage 8 is connected to the combustion chamber 7 toward the secondary incinerator 6.
  • the secondary incinerator 6 is configured in a tower shape with one end connected to an exhaust passage 8, and in order from the exhaust passage 8 side, a reburn burner 9, a ceramic checker 10, a secondary combustion chamber 11, and an ejector 1 blower 1 It has two.
  • the exhaust gas decomposition treatment tower 3 includes a catalyst chamber 13 for charging a catalyst, and an exhaust gas inflow path 14 and an exhaust gas inflow path 15 are connected to the catalyst chamber 13. Further, the inlet 14 and the outlet 15 are provided with sampling ports 16 and 17 for sampling exhaust gas, respectively.
  • the exhaust gas passage 4 has one end connected to the secondary incinerator 6 of the incinerator 2 and the other end connected to the inflow path 14 of the exhaust gas decomposition tower 3, and the water spray cooling tower 18. Yes.
  • the exhaust gas generated when the refuse 20 is incinerated in the combustion chamber 7 is guided through the exhaust path 8 into the secondary incinerator 6, where the reburner 9 Then, it flows into the exhaust gas passage 4 after being further burned.
  • the exhaust gas introduced into the exhaust gas passage 4 is cooled by the water spray cooling tower 18 and then guided into the exhaust gas decomposition treatment tower 3, where the exhaust gas is decomposed in the catalyst chamber 13 and the exhaust gas 1 Released from 5 to the outside.
  • the catalyst obtained in the fifth embodiment is provided in the catalyst chamber 13 of the above-described refuse incinerator 1.
  • the garbage was actually incinerated by charging the chlorinated organic compound decomposition catalyst, and the state of oxidative decomposition of dioxins in exhaust gas under the conditions shown in Table 1 was examined.
  • the exhaust gas serving as a sample was collected from the sampling port 16 before the treatment in the catalyst chamber 13 and from the sampling port 17 after the treatment.
  • the method of sample collection and analysis were in accordance with the “Guideline for Standard Measurement and Analysis of Dioxins in Waste Disposal” specified by the Ministry of Health and Welfare of Japan described in the Sanitation No. 38, February 26, 1997.
  • the measurement of the oxygen concentration in the exhaust gas, the exhaust gas temperature, and the exhaust gas flow rate are based on the zirconure method and the JISZ method of the “Oxygen in the exhaust gas method” specified in Japanese Industrial Standards JIS KO 301-1989, respectively. 880 8-1995 K-type thermocouple method in "Measurement method of dust concentration in exhaust gas", and "Measurement method of dust concentration in exhaust gas” specified in JISZ 8808-1995 Pitot tube method.
  • Table 2 (Table 2-1 and Table 2) show the measurement results of the concentration of gaseous and particulate dioxins contained in the exhaust gas collected at the inlet and outlet sides of the catalyst chamber 13, respectively. — See 2).
  • Exhaust gas density (kg / m 3 ) 0.74 2 0.854 Static exhaust gas pressure (kPa) 0.14 0.000 Exhaust gas flow rate (mZ s) 5.0 4.3
  • T 4 CDD dibenzodioxin tetrachloride
  • T 4 CDD s dibenzodioxins tetrachloride
  • PCDD s Polychlorinated dibenzo 'para-dioxins
  • PCDF s Polychlorinated dibenzofurans
  • OCDD s octachloride dibenzodioxins
  • Example 6 Using the catalyst for decomposing chlorinated organic compounds obtained in Example 6 in place of the catalyst for decomposing chlorinated organic compounds obtained in Example 5, and using the exhaust gas in the same manner as in Example 11 The state of oxidative degradation of dioxins was investigated. The results are shown in Table 3 (Tables 3-1 and 3-2). In Table 3, abbreviations and "TEF" indicating chlorinated organic compounds are the same as those in Table 2.
  • PCDD s 3400 1 2 0 8 1 6 1 05 76.0 1 2.4
  • Example 8 Using the catalyst for decomposing chlorinated organic compounds obtained in Example 8 in place of the catalyst for decomposing chlorinated organic compounds obtained in Example 5, dioxin in the exhaust gas in the same manner as in Example 11 The state of oxidative decomposition of the species was investigated. The results are shown in Table 5 (Table 5-1 and Table 5-2). In Table 5, abbreviations and "TEF" indicating chlorinated organic compounds are the same as those in Table 2.
  • Example 9 Using the catalyst for decomposing chlorinated organic compound obtained in Example 9 instead of the catalyst for decomposing chlorinated organic compound obtained in Example 5, in the same manner as in Example 11 The state of oxidative decomposition of dioxins in exhaust gas was investigated. The results are shown in Table 6 (Table 6-1 and Table 6-2). In Table 6, the abbreviations and "TEF" indicating the chlorinated organic compound are the same as those in Table 2.
  • Example 10 The catalyst for decomposing chlorinated organic compounds obtained in Example 10 was used in place of the catalyst for decomposing chlorinated organic compounds obtained in Example 5, and the same method as in Example 11 was carried out. The state of oxidative degradation of dioxins was examined. The results are shown in Table 7 (Table 7-1 and Table 7-2). In Table 7, the abbreviations and "TEF" indicating the chlorinated organic compound are the same as those in Table 2.

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Abstract

Cette invention se rapporte à un catalyseur de décomposition des composés organiques chlorés, qui comprend un support et, placés tous les deux sur ce support, un premier constituant catalytique contenant un élément or et un second constituant catalytique contenant un oxyde d'au moins un élément choisi dans le groupe constitué par le magnésium, l'aluminium, le silicium, le titane, le manganèse, le fer, le cobalt, le nickel, le cuivre, le zinc, l'ytttrium, le zirconium, le niobium, le molybdène, l'indium, l'étain, le lanthane et le cérium. Ce support possède une surface spécifique d'au moins 100 m2/g et un diamètre moyen des pores d'au moins 10 angströms, et il est de préférence résistant à la chaleur. Ce catalyseur se caractérise par une forte action de décomposition sur divers composés organiques chlorés, y compris ceux sous forme particulaire et à l'état gazeux.
PCT/JP1999/005099 1998-09-22 1999-09-17 Catalyseur de decomposition des composes organiques chlores WO2000016898A1 (fr)

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* Cited by examiner, † Cited by third party
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JP2008280184A (ja) * 2007-05-08 2008-11-20 National Institute Of Advanced Industrial & Technology セリウムを含有するメソポーラスシリカと貴金属の超微粒子の複合体、その複合体の製造方法、並びにその複合体を触媒に用いた微量一酸化炭素の酸化的除去方法及びアルコール類の酸化的脱水素反応によるケトン類の合成方法
JP2013504683A (ja) * 2009-09-15 2013-02-07 エイビーエス マテリアルズ インコーポレイテッド 膨潤性材料および使用方法
RU2488441C1 (ru) * 2012-07-18 2013-07-27 ФЕДЕРАЛЬНОЕ ГОСУДАРСТВЕННОЕ БЮДЖЕТНОЕ УЧРЕЖДЕНИЕ НАУКИ ИНСТИТУТ ОРГАНИЧЕСКОЙ ХИМИИ им. Н.Д. ЗЕЛИНСКОГО РОССИЙСКОЙ АКАДЕМИИ НАУК (ИОХ РАН) Катализатор для окислительного разложения хлорорганических соединений в газах и способ его получения
US9144784B2 (en) 2005-09-30 2015-09-29 Abs Materials Sorbent material and method for using the same
CN112427032A (zh) * 2019-08-26 2021-03-02 万华化学集团股份有限公司 一种催化焚烧氯乙烯聚合含湿尾气的催化剂及其制备方法

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US9144784B2 (en) 2005-09-30 2015-09-29 Abs Materials Sorbent material and method for using the same
JP2008280184A (ja) * 2007-05-08 2008-11-20 National Institute Of Advanced Industrial & Technology セリウムを含有するメソポーラスシリカと貴金属の超微粒子の複合体、その複合体の製造方法、並びにその複合体を触媒に用いた微量一酸化炭素の酸化的除去方法及びアルコール類の酸化的脱水素反応によるケトン類の合成方法
JP2013504683A (ja) * 2009-09-15 2013-02-07 エイビーエス マテリアルズ インコーポレイテッド 膨潤性材料および使用方法
RU2488441C1 (ru) * 2012-07-18 2013-07-27 ФЕДЕРАЛЬНОЕ ГОСУДАРСТВЕННОЕ БЮДЖЕТНОЕ УЧРЕЖДЕНИЕ НАУКИ ИНСТИТУТ ОРГАНИЧЕСКОЙ ХИМИИ им. Н.Д. ЗЕЛИНСКОГО РОССИЙСКОЙ АКАДЕМИИ НАУК (ИОХ РАН) Катализатор для окислительного разложения хлорорганических соединений в газах и способ его получения
CN112427032A (zh) * 2019-08-26 2021-03-02 万华化学集团股份有限公司 一种催化焚烧氯乙烯聚合含湿尾气的催化剂及其制备方法

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