WO2006041170A1 - Méthode de fabrication d’un matériau poreux - Google Patents

Méthode de fabrication d’un matériau poreux Download PDF

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Publication number
WO2006041170A1
WO2006041170A1 PCT/JP2005/018984 JP2005018984W WO2006041170A1 WO 2006041170 A1 WO2006041170 A1 WO 2006041170A1 JP 2005018984 W JP2005018984 W JP 2005018984W WO 2006041170 A1 WO2006041170 A1 WO 2006041170A1
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WO
WIPO (PCT)
Prior art keywords
porous structure
producing
metal
catalyst
cryogel
Prior art date
Application number
PCT/JP2005/018984
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English (en)
Japanese (ja)
Inventor
Michihiro Asai
Toshihiko Osaki
Koji Watari
Kimiyasu Sato
Original Assignee
Ngk Insulators, Ltd.
National Institute Of Advanced Industrial Science And Technology
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Ngk Insulators, Ltd., National Institute Of Advanced Industrial Science And Technology filed Critical Ngk Insulators, Ltd.
Priority to JP2006540989A priority Critical patent/JP5098333B2/ja
Publication of WO2006041170A1 publication Critical patent/WO2006041170A1/fr

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Classifications

    • 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
    • B01D53/92—Chemical or biological purification of waste gases of engine exhaust gases
    • B01D53/94—Chemical or biological purification of waste gases of engine exhaust gases by catalytic processes
    • 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
    • B01J23/40—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals of the platinum group metals
    • B01J23/42—Platinum
    • B01J35/56—
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
    • B01J37/02—Impregnation, coating or precipitation
    • B01J37/03—Precipitation; Co-precipitation
    • B01J37/036—Precipitation; Co-precipitation to form a gel or a cogel
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
    • B01J37/32—Freeze drying, i.e. lyophilisation
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B33/00—Silicon; Compounds thereof
    • C01B33/113—Silicon oxides; Hydrates thereof
    • C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
    • C01B33/14—Colloidal silica, e.g. dispersions, gels, sols
    • C01B33/157—After-treatment of gels
    • C01B33/158—Purification; Drying; Dehydrating
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
    • C01F7/00—Compounds of aluminium
    • C01F7/02—Aluminium oxide; Aluminium hydroxide; Aluminates
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00—Physical properties of inorganic compounds
    • C01P2006/12—Surface area
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00—Physical properties of inorganic compounds
    • C01P2006/14—Pore volume

Definitions

  • the present invention relates to a method for producing a porous structure.
  • Reduction type catalyst is arranged, and NO, H in exhaust gas mainly by catalytic action of noble metal
  • oxidation catalyst for example, a catalyst in which Pt having a high oxidation activity is supported on a support such as alumina or silica is known.
  • a catalyst component such as platinum is supported on a porous support of alumina or silica
  • the alumina or silica porous support is usually placed in a solution containing the catalyst component, for example, a salt solution of the catalyst component.
  • a method of dipping, drying, and firing if necessary is employed.
  • a wet gel produced by a method such as hydrolysis and gelation of alkoxide it is a wet gel having a liquid phase of a mixture of water and an alcohol such as ethanol.
  • an alcohol such as ethanol.
  • water in the liquid phase of the wet gel is replaced with alcohol, and then the organic solvent is further removed. It was essential to replace
  • the air mouth gel currently used is inferior in water resistance and breaks down in the moment when the air mouth gel is immersed in water. Therefore, the conventional metal impregnation method using an aqueous solution containing metal ions is used. Since it is impossible to carry the support, there is a problem in that the metal ion must be added at the gel synthesis stage, and the usage is greatly limited.
  • the supercritical drying method requires a high temperature and high pressure above the critical point, and thus has a problem of safety and high cost.
  • the present invention has been made in view of the above-mentioned problems of the prior art, and the object thereof is water resistance not only having high surface area, high porosity, and high heat resistance.
  • An object of the present invention is to provide a method for producing a porous structure that can obtain a porous structure that does not cause structural destruction by contact with water and that can contribute to safety and cost reduction.
  • the present invention provides the following method for producing a porous structure.
  • a method for producing a porous structure in which a gel is produced from a raw material by a gel reaction, the gelled product is freeze-dried, and then fired to obtain a porous structure.
  • the porous structure is water-resistant and does not cause structural destruction when contacted with water.
  • the method for producing a porous structure according to any one of [1] to [6].
  • [8] [8]
  • the porous structure has a three-dimensional network skeleton structure, and metal fine particles or metal oxide fine particles or both are dispersed in a base material constituting the skeleton.
  • FIG. 1 (a) is an image diagram showing a dispersion state of silica nanoparticles (sol) in the gelation process of the method for producing a porous structure of the present invention.
  • FIG. 1 (b) is an image diagram showing a state in which silica nanoparticles (sol) are bound in a network form in the gelling process of the method for producing a porous structure of the present invention.
  • FIG. 1 (c) is an image diagram showing a gel skeleton structure in the gelation process of the method for producing a porous structure of the present invention.
  • FIG. 2 is an image diagram showing an example of a cryogel catalyst obtained by the method for producing a porous structure of the present invention.
  • the main feature of the method for producing a porous structure according to the present invention is that a gelled product is produced from a raw material by a gelation reaction, and the gelled product is freeze-dried and then fired to obtain a porous structure ( Is to obtain taliogel).
  • the gelled product is preferably freeze-dried at a trap part cooling temperature of _80 ° C or lower and a vacuum degree of lOPa or lower.
  • a trap part cooling temperature exceeds 80 ° C
  • freeze-drying of the wet gel becomes incomplete and the microstructure is destroyed by drying shrinkage.
  • the degree of vacuum at the completion of drying exceeds lOPa
  • freeze-drying is not completed, and microstructural destruction occurs due to drying shrinkage. .
  • the gelled product (wet gel) is cooled to -80 ° C or lower, and after confirming that the gely product (wet gel) is frozen, the gel is evacuated.
  • the trap part cooling temperature it is preferable to hold the trap part cooling temperature at 80 ° C or lower for about! ⁇ 3 days. At this time, the holding time varies depending on the size, density and shape of the target gelled product (wet gel), but at least the holding time at which the degree of vacuum is less than lOPa is desirable.
  • a freezer may be used for the initial cooling of the gelled product (wet gel), but it is possible to reduce the freezing time and to reduce the gelled product (wet) by cooling it as quickly as possible with a refrigerant such as dry ice ethanol or liquid nitrogen.
  • a refrigerant such as dry ice ethanol or liquid nitrogen.
  • Wet gel is preferable because it can suppress structural destruction during freezing.
  • the main composition of the raw material used in the present invention is preferably composed of at least one of silica, alumina, zirconia, and titania, and more preferably composed of alumina and silica. .
  • a solution containing metal ions, metal fine particles, metal oxide fine particles, or any one metal species may be added to the raw material in advance.
  • the porous structure obtained by the present invention has a three-dimensional network skeleton structure, and a metal fine particle, a metal oxide fine particle, a metal oxide fine particle, or both are formed on a base material constituting the skeleton.
  • a dispersed porous structure (cryogel), It can be used as it is as a catalyst.
  • the catalyst fine particles exposed on the surface of the base material are highly active, so the reaction rate per active point of the catalyst fine particles is also the catalyst by the conventional impregnation method. Faster (about 2 times), excellent in catalytic ability, and metal fine particles are almost buried in the base material, so it has excellent high-temperature heat resistance compared to conventional impregnated catalysts. .
  • the metal species used in the present invention is not particularly limited, but is preferably a noble metal such as gold, silver, platinum or palladium or a transition metal such as iron or cobalt from the viewpoint of catalytic activity. Les.
  • the particle diameter of the metal fine particles is not particularly limited, but is preferably 5 nm or less because the catalytic ability can be improved.
  • a gelled product (wet gel) is freeze-dried and then fired in an air atmosphere.
  • the metal compound derived from the metal fine particles carried by the obtained porous structure (cryogel) is reduced to metal fine particles, thereby exhibiting catalytic activity.
  • a protective molecule is used.
  • the obtained porous structure (cryogel) has a three-dimensional network skeleton structure, and the metal fine particles are dispersed in the base material constituting the skeleton.
  • the degree of exposure of the metal fine particles can be appropriately adjusted by firing in an atmosphere and then firing in a hydrogen atmosphere.
  • the method for producing a porous structure of the present invention employs freeze-drying instead of supercritical drying, thereby providing high surface area, high porosity, high
  • it is water resistant and can produce a porous structure (cryogel) that does not cause structural breakdown like air gel when contacted with water.
  • the method for producing a porous structure of the present invention does not perform supercritical drying using a high temperature 'high pressure above the critical point, so that it is excellent in safety and freeze-dried at low temperature' low pressure.
  • it is more energy-saving than supercritical drying, and the water in the liquid phase of the wet gel can be dried as it is without replacing it with alcohol (freeze drying), which simplifies the process and equipment. Because it is possible, the cost can be greatly reduced.
  • the method for producing a porous structure of the present invention has a structure that is water-resistant and can be immersed in water and re-dried as long as it does not cause structural breakdown like airgel when contacted with water.
  • porous structure (cryogel) that does not break, so conventional metal ions can be obtained simply by adding metal ions at the gel synthesis stage.
  • Metal loading can also be performed by an impregnation method using an aqueous solution containing the solution.
  • a porous structure in which the main composition is composed of silica (SiO) and platinum (Pt) is dispersed.
  • the manufacturing method of the above PtZsi 0 cryogel is as follows: (1) Gelation process
  • silica nanoparticles (sol) 10 This progresses in the liquid phase and repeats the bonding to produce silica nanoparticles (sol) 10 as an intermediate process, as shown in FIG. 1 (a).
  • the silica nanoparticle (sol) 10 continues to grow in both number and size, and is bonded in a network shape to form a gel skeleton structure 20 shown in FIG. 1 (c). .
  • the gelation time tends to be faster as the amount of HO is smaller and the amount of HPCA is smaller.
  • the increase in the amount of HO and the longer gelation time increase the gel volume as the amount of HO increases.
  • the amount of HPCA is linked to pH, which is thought to be due to the effect of pH on the gelling process.
  • the prepared gel (wet gel) is frozen at _80 ° C. or lower, and after confirmation of freezing, the trap portion cooling temperature is kept at a vacuum of ⁇ 80 ° C. or lower for a predetermined time and freeze-dried.
  • the fine network formed during the gelation process is responsible for the surface tension during drying. It will be destroyed more.
  • the air mouth gel has been dried using a supercritical fluid.
  • the surface tension is canceled by using the freeze drying method, and a fine network is maintained.
  • a dry gel (cryogel) can be obtained as it is.
  • platinum acid or the like added as a platinum source is self-decomposed by heating and reduced to platinum (including oxides). Since the reduction temperature requires a temperature higher than the autolysis temperature of the platinum compound (for example, 400 to 430 ° C for hexachloroplatinic acid), it is usually treated in an atmosphere at 500 ° C for 1 hour. I do. Further, immediately after calcination, the platinum surface is partially made of platinum oxide. Therefore, Pt / SiO cryogel (catalyst) can be obtained by performing hydrogen reduction treatment and reducing to complete metal platinum. Note that the Pt / SiO2 crystal obtained in the present invention.
  • the main form of 2 2 liogel (catalyst) has a skeleton structure 30 of a three-dimensional network, and metal fine particles 1 are dispersed in a base material 2 constituting the skeleton.
  • the force hydrogen reduction treatment in which platinum as 1 is almost absorbed in silica as the base material 2, the degree of exposure of platinum as the metal fine particles 1 can be appropriately adjusted.
  • the main composition is alumina (A1
  • the solubilization process is performed using ASB (Al (sec—BuO)) or AIP (Al (iso—PrO), which is an alumina source.
  • Boehmite sol (AIOOH) is produced by holding for a while.
  • the boehmite sol (AIOOH) obtained in the solubilization process is converted to platinum acid (HCPA: hexaclonal platinum acid hexahydrate [H (PtCl)), a platinum source protected with a chelating agent
  • the HCPA / boehmite gel (AIOOH) obtained in the gelation process is frozen at 80 ° C or lower, and after freezing is confirmed, it is kept at a trap cooling temperature of 80 ° C or lower for a specified time. And freeze-dried.
  • the fine network formed in the gelation process is destroyed by the surface tension during drying.
  • the air-mouthed gel has been dried using a supercritical fluid, but in the present invention, the surface tension is canceled and a fine network is maintained by using a freeze-drying method.
  • a dried gel (cryogel) can be obtained as it is.
  • platinum acid or the like added as a platinum source is self-decomposed by heating and reduced to platinum (including oxides). Since the reduction temperature requires a temperature higher than the autolysis temperature of the platinum compound (for example, 400 to 430 ° C for hexachloroplatinic acid), it is usually treated in an atmosphere at 500 ° C for 1 hour. By performing this, a Pt / Al 2 O cryogel (catalyst) can be obtained.
  • the evaluation was performed with FID (flame ion detector) and TCD (thermal conductivity detector).
  • the CH ⁇ CO conversion efficiency was calculated from the FID results. Since TCD has low detection sensitivity, it was used to confirm the generated gas composition (CH, CO 2) and to backup the conversion efficiency calculation.
  • urea was added to 22 g of deionized water and stirred for 15 minutes to dissolve.
  • HCPA Kisakuro port chloroplatinic acid hexahydrate to
  • TMOS tetramethoxysilane
  • the obtained lyophilized gel was placed in an alumina crucible and baked in an electric furnace at 500 ° C for 1 hour in an air atmosphere. Next, the obtained PtZSiO cryogel was treated with hydrogen (H atmosphere [3
  • spherical silica powder (SP-03B manufactured by Fuso Science Co., Ltd.) having an average particle size of 300 nm was used as a support for the catalyst by the conventional impregnation method.
  • Hydrogen reduction Pt / SiO cryogel catalyst is H
  • a material prepared with O22ml / Ptfi0.075g was prepared by hydrogen reduction treatment at each temperature (500.C, 700.C, 900 ° C). The amount of metal Pt in each catalyst was constant at 0.5%.
  • the SiO cryogel catalyst In the case of the SiO cryogel catalyst, it was 16.80%. On the other hand, in the case of the catalyst by the conventional impregnation method (hydrogen reduction 500 ° C), the exposure degree of the metal Pt was 10.84%.
  • the methane oxidation rate at 700 ° C is about 68% in the case of the 500 ° C hydrogen reduction catalyst by the conventional impregnation method, whereas in the case of the 500 ° C hydrogen reduction PtZSiO cryogel catalyst About 56%, 700 ° C Hydrogen reduction About 50 for Pt / SiO cryogel catalyst. / o, 9
  • the 500 ° C hydrogen reduction Pt / SiO cryogel catalyst was obtained by the conventional impregnation method.
  • the exposure of metal Pt is less than half, but CH oxidation performance evaluation (oxidation catalytic performance evaluation) is a catalyst approaching 500 ° C hydrogen reduction catalyst by conventional impregnation method. Have the ability. This suggests that the active sites of metal Pt functioning as a catalyst are equally high.
  • the hydrogen-reduced Pt / SiO cryogel catalyst has a high density of active sites present on the metal Pt surface, that is, it may give more active sites to the slightly exposed Pt metal surface. I found out.
  • the high temperature hydrogen treatment caused damage to the surface of the cryogel substrate, and the metal Pt was sintered and deactivated due to heat. Conceivable.
  • HCPA / boehmite sol (AIOOH) was prepared.
  • platinum source add hexaclonal platinum acid hexahydrate [H (PtCl) ⁇ 6 ⁇ ] 0 ⁇ 0749g to 0 ⁇ 5 ml of hexylene glycol in a working environment of 60 ° C and hold for 20 minutes. This was produced.
  • the obtained lyophilized gel was placed in an alumina crucible and 500% in an air atmosphere in an electric furnace.
  • Pt / Al 2 O cryogel catalyst was obtained by calcination at ° C for 1 hour.
  • the 1 O air-mouth gel catalyst was immersed in water, and the state change at that time was observed.
  • cryogel catalyst PtZAl O cryogel catalyst
  • conventional catalyst catalyst by impregnation method
  • the power of reduction at 800 ° C over the reduction at 500 ° C is a force that improves the exposure of metal Pt.
  • the exposure of metal Pt The degree is decreasing. That is, although it cannot be generally stated, it was suggested that the cryogel catalyst has higher temperature and heat resistance than the conventional catalyst.
  • the method for producing a porous structure of the present invention can be suitably used, for example, for producing a catalyst for exhaust gas treatment.

Abstract

La présente invention a pour objet une méthode de fabrication d’un matériau poreux. Ladite méthode implique l'obtention d'un matériau gélatineux à partir d'un matériau brut par réaction de gélification, la lyophilisation dudit matériau gélatineux, et sa cuisson, ce qui permet d’aboutir à la formation d’un matériau poreux. Par le biais de ladite méthode, il est possible d’obtenir un matériau poreux de surface importante, de porosité élevée et de résistance à la chaleur élevée, et qui présente en outre une résistance à l'eau, dans la mesure où il ne subit aucun dégât structurel lorsqu'il entre en contact avec l'eau. Ladite méthode représente également une amélioration en termes de coûts et de sécurité. Ladite méthode peut par exemple être employée pour produire un catalyseur de traitement des gaz d'échappement.
PCT/JP2005/018984 2004-10-15 2005-10-14 Méthode de fabrication d’un matériau poreux WO2006041170A1 (fr)

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Cited By (8)

* Cited by examiner, † Cited by third party
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JP2009018225A (ja) * 2007-07-10 2009-01-29 National Institute Of Advanced Industrial & Technology 多孔質白金−アルミナ系クリオゲル触媒の製造方法及びこれにより得られた多孔質白金−アルミナ系クリオゲル触媒
JP2009090199A (ja) * 2007-10-05 2009-04-30 National Institute Of Advanced Industrial & Technology 多孔質酸化セリウム−アルミナ系クリオゲル触媒及びその製造方法
JP2010528967A (ja) * 2007-06-06 2010-08-26 コミサリア、ア、レネルジ、アトミク、エ、オ、エネルジ、アルテルナティブ 遷移金属酸化物のカーボンコーティングされたナノ粒子の製造方法
JP2012166959A (ja) * 2011-02-09 2012-09-06 National Institute Of Advanced Industrial Science & Technology 多孔質アルミナおよびこれを用いた触媒
JP2013049034A (ja) * 2011-08-31 2013-03-14 National Institute Of Advanced Industrial Science & Technology パラジウム−アルミナ触媒及びその製造方法
CN110117000A (zh) * 2019-06-14 2019-08-13 中国科学技术大学 一种大块碳纳米纤维气凝胶及其制备方法
JP2020175387A (ja) * 2020-07-03 2020-10-29 国立研究開発法人物質・材料研究機構 金属酸化物からなる発泡体、および、その用途
WO2024071431A1 (fr) * 2022-09-30 2024-04-04 日鉄ケミカル＆マテリアル株式会社 Particules d'alumine sphériques, leur méthode de production et composition composite de résine les comprenant

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Cited By (9)

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Publication number Priority date Publication date Assignee Title
JP2010528967A (ja) * 2007-06-06 2010-08-26 コミサリア、ア、レネルジ、アトミク、エ、オ、エネルジ、アルテルナティブ 遷移金属酸化物のカーボンコーティングされたナノ粒子の製造方法
JP2009018225A (ja) * 2007-07-10 2009-01-29 National Institute Of Advanced Industrial & Technology 多孔質白金−アルミナ系クリオゲル触媒の製造方法及びこれにより得られた多孔質白金−アルミナ系クリオゲル触媒
JP2009090199A (ja) * 2007-10-05 2009-04-30 National Institute Of Advanced Industrial & Technology 多孔質酸化セリウム−アルミナ系クリオゲル触媒及びその製造方法
JP2012166959A (ja) * 2011-02-09 2012-09-06 National Institute Of Advanced Industrial Science & Technology 多孔質アルミナおよびこれを用いた触媒
JP2013049034A (ja) * 2011-08-31 2013-03-14 National Institute Of Advanced Industrial Science & Technology パラジウム−アルミナ触媒及びその製造方法
CN110117000A (zh) * 2019-06-14 2019-08-13 中国科学技术大学 一种大块碳纳米纤维气凝胶及其制备方法
JP2020175387A (ja) * 2020-07-03 2020-10-29 国立研究開発法人物質・材料研究機構 金属酸化物からなる発泡体、および、その用途
JP6999140B2 (ja) 2020-07-03 2022-02-10 国立研究開発法人物質・材料研究機構 金属酸化物からなる発泡体、および、その用途
WO2024071431A1 (fr) * 2022-09-30 2024-04-04 日鉄ケミカル＆マテリアル株式会社 Particules d'alumine sphériques, leur méthode de production et composition composite de résine les comprenant

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