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WO2002032573A1 - Preparation d'un catalyseur permettant de decomposer l'hydrazine et ses applications - Google Patents

Preparation d'un catalyseur permettant de decomposer l'hydrazine et ses applications Download PDF

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Publication number
WO2002032573A1
WO2002032573A1 PCT/CN2000/000409 CN0000409W WO0232573A1 WO 2002032573 A1 WO2002032573 A1 WO 2002032573A1 CN 0000409 W CN0000409 W CN 0000409W WO 0232573 A1 WO0232573 A1 WO 0232573A1
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WO
WIPO (PCT)
Prior art keywords
catalyst
type
hours
metal
fluorite
Prior art date
Legal status (The legal status 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 status listed.)
Ceased
Application number
PCT/CN2000/000409
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English (en)
Chinese (zh)
Inventor
Yuyang Zhuang
Yihuang Zhang
Hui Dong
Binglun Tian
Shuwen Wang
Ruijie Wang
Jinzhou Yan
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
SHENYANG DONGYU GROUP CO Ltd
Original Assignee
SHENYANG DONGYU GROUP CO Ltd
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 SHENYANG DONGYU GROUP CO Ltd filed Critical SHENYANG DONGYU GROUP CO Ltd
Priority to AU2001212663A priority Critical patent/AU2001212663A1/en
Publication of WO2002032573A1 publication Critical patent/WO2002032573A1/fr
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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Classifications

    • C—CHEMISTRY; METALLURGY
    • C06—EXPLOSIVES; MATCHES
    • C06D—MEANS FOR GENERATING SMOKE OR MIST; GAS-ATTACK COMPOSITIONS; GENERATION OF GAS FOR BLASTING OR PROPULSION (CHEMICAL PART)
    • C06D5/00—Generation of pressure gas, e.g. for blasting cartridges, starting cartridges, rockets
    • C06D5/04—Generation of pressure gas, e.g. for blasting cartridges, starting cartridges, rockets by auto-decomposition of single substances
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
    • B01J23/002—Mixed oxides other than spinels, e.g. perovskite
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • 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
    • B01J23/8933—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 also combined with metals, or metal oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J35/00—Catalysts, in general, characterised by their form or physical properties
    • B01J35/19—Catalysts containing parts with different compositions
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B21/00—Nitrogen; Compounds thereof
    • C01B21/02—Preparation of nitrogen
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B3/00—Hydrogen; Gaseous mixtures containing hydrogen; Separation of hydrogen from mixtures containing it; Purification of hydrogen
    • C01B3/02—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen
    • C01B3/04—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen by decomposition of inorganic compounds, e.g. ammonia
    • 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
    • B01J21/00—Catalysts comprising the elements, oxides, or hydroxides of magnesium, boron, aluminium, carbon, silicon, titanium, zirconium, or hafnium
    • B01J21/18—Carbon
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/30—Hydrogen technology
    • Y02E60/36—Hydrogen production from non-carbon containing sources, e.g. by water electrolysis

Definitions

  • the present invention relates to the preparation and application of a catalyst, in particular to a catalyst capable of decomposing hydrazine into N 2 and 3 ⁇ 4 at normal temperature.
  • BACKGROUND Hydrazine is a widely used chemical material containing hydrogen.
  • There are several main ways of hydrazine decomposition: 3N 2 3 ⁇ 4 ⁇ N 2 + 4 Li 3 ; ⁇ -1 STkJ.mor 1
  • thermodynamic data It is not difficult to see from the above thermodynamic data that hydrazine is easily decomposed, and the products are mainly NH 3 and N 2 .
  • researchers have done a lot of research on the decomposition of hydrazine on the surface of metal single crystals, metals and metal-supported catalysts, and believe that there are two ways to break the intramolecular bond of hydrazine: one is the break of NH bond; two It is the break of the NN key.
  • the NH bond energy is ⁇ 1
  • the NN bond energy is ⁇ . ⁇ 1
  • the NN bond is more easily broken in thermodynamics.
  • An object of the present invention is to provide a novel catalyst which can effectively solve the above problems, which can decompose hydrazine into hydrogen and nitrogen with high selectivity at room temperature.
  • the composition formula of the catalyst can be expressed as: XYC, where X is Fe, Co, Ni, Cu, Zn, Ru, Rl, Pd, In, Os, Ir, Pt, Au metal element, Y is a perovskite-type or fluorite-type or goethite-type composite oxide, C is a nano-carbon black, X may be one or more metals, and europium is one of three types of oxides Species, C can be added or not added.
  • the above catalysts can be divided into two types: supported type and mixed type:
  • the general formula of the supported type is expressed as ⁇ / ⁇ , where X is Fe, Co, Ni, Cu, Zn, Ru, Rh, Pd, In, Os , Ir, Pt, Au metal elements, Y is a perovskite-type or fluorite-type or goethite-type composite oxide, X may be one or more metals, and Y is one of three types of oxides , The loading of X on Y is 0.5 ⁇ 20%; the composition formula of the mixed type is expressed as (X / C) a + Y b , where X is Fe, Co, Ni, Cu, Zn, Ru, Rh, Pd, In, (Ir, Pt, Au metal elements, C is nano carbon black, Y is perovskite or fluorite or goethite type composite oxide, X may be one or more metals, Y It is one of three types of oxides, and the loading
  • the preferred component for the first type of catalyst is between 1 and 10%
  • the preferred component for the second type of catalyst is between 10 and 25%, l> a: b> 0.1.
  • the (X / C) a + Y b type catalyst preparation method can be divided into two steps: The first step is the preparation of X / C, including metal salt solution impregnation-roasting-reduction method; impregnation-reduction dry method, gold carbonyl Chemical decomposition of chemical compounds Product method, grinding-calcination-reduction method. The second step is the mixing of X / C and Y, including mechanical mixing method, grinding method, grinding-ultrasonic vibration method.
  • Preparation method of supported catalyst First, the sol-gel method (using EDTA and citric acid as co-complexing agents, using soluble metal salts as starting materials, and hexanediol and glycerol as dispersants is used. Stir at 70-90 ° C to form a transparent colloid.
  • the colloid is cured at 100-150 ° C, pre-baked at 250-350 ° C for 1-10 hours, and finally calcined at 1000-1400 ° C for 1-100 hours.
  • solid grinding method using metal nitrate as raw material, first mixing and grinding thoroughly, then firing at 1000-1400 ° C, taking out every 1-5 hours, then grinding and firing, repeated 5-10 times) to prepare calcium titanium Mineral or fluorite or goethite type composite oxide, then add ethanol or water, formaldehyde, KOH, and the soluble metal salt or acid solution to be supported, and stir at 20 ⁇ 60 ° C for 1 ⁇ 4 hours , Filter or stand and pour the upper solution, rinse with water to make the pH reach 7, and then dry at 8 (150 ° C).
  • Preparation method of mixed catalyst Disperse nano carbon black with ethanol, then add formaldehyde, KOH and required metal soluble salt, stir at 20 60 Q C for 14 hours, filter or leave to pour the upper solution, rinse with water The PH value reaches 7, and it is dried at 80 ⁇ 150 ° C to obtain X / C.
  • X / C and perovskite-type or fluorite-type or goethite-type composite oxides obtained during the preparation of a supported catalyst are mixed and ground, and then the mixed solid is immersed in a distilled aqueous solution for 0.1 to 3 hours under ultrasonic vibration. 80 ⁇ 150 ° C.
  • the gas produced by the catalyst of the present invention after decomposing pure hydrazine or hydrazine hydrate at normal temperature can be used as a hydrogen source for a proton exchange membrane fuel cell.
  • Air breathing at normal temperature can achieve a single cell voltage of 0.8V and a current density of 1.50mA / cm 2 .
  • the above-mentioned hydrogen can be used as a hydrogen source in metal processing.
  • the catalyst provided by the present invention can decompose hydrazine or hydrazine hydrate with high selectivity to generate hydrogen gas at normal temperature.
  • the selectivity of hydrogen is represented by S, S-2 [H 2 ] X100 / 2 [H 2 ] +3 [NH 3 ] o
  • Figure 1 shows Bao. 5 Sr (). 5 Co. . 6 Fe. . 4 Ow powder diffraction XRD pattern.
  • FIG. 2 is a schematic diagram of an application example (a fuel cell using hydrogen produced by decomposition of hydrazine) as a raw material.
  • Fig. 3 is a polarization curve of a proton membrane fuel cell test unit using hydrogen produced by the decomposition of hydrazine as a hydrogen source on an evaluation device. (Operating conditions: the pressure of 3 ⁇ 4 is 0.1 MPa, the flow rate is 50 ml / min, the pressure of air is 0.1 MPa, and the battery temperature is 90 ° C.)
  • the pressure of 3 ⁇ 4 is 0.1 MPa
  • the flow rate is 50 ml / min
  • the pressure of air is 0.1 MPa
  • the battery temperature is 90 ° C.
  • the supported catalyst has the general formula (X / C) a + Y b , where X is Fe, Co, Ni, Cu, Zn, Ru, Rh, Pd, In, Os, Ir, Pt, Au, C is nano carbon black, Y is one of three types of oxide rhenium, and the loading of X on C is 0.540%.
  • the catalyst composition of this embodiment is: (lOroPt / Q ⁇ CBao.sSro.sCoo.eFeo ⁇ Os.s). Its preparation method is as follows:
  • the perovskite-type Ba a5 Sr was prepared by complex method. . 5 Co. . 6 Fe. . 4 0 3 _ s oxide. Weigh 70 g of EDTA acid and dissolve it in 200 liters of concentrated ammonia water under heating, add 0.1mol Ba (O 3 ) 2 crystals, heat to dissolve, and then add 0.1 mol Sr (N0 3 ) 2 , 0.12mol Co (N0 3 ) 2 , 0.08 A mixed solution of mol Fe (N0 3 ) 3 is heated and stirred at 80 ° C. As the water evaporates, a transparent hot-melt fuchsia colloid is obtained. The colloid is cured at 120 ° C for several hours, and then 300 ° C.
  • XRD powder diffraction measurement showed that a pure phase perovskite structure was formed, as shown in Figure 1.
  • the BET specific surface area measurement showed that the specific surface area of the powder was 50 m2 / g.
  • the XR diffraction peak half-width method calculates the grain size of the powder to be 15-40 nm.
  • the general formula of the mixed catalyst is: X / Y, where X is Fe, Co, Ni, Cu, Zn, Ru, Rh 3 Pd ; In, Os, Ir, Pt, Au metal elements, Y is perovskite or For fluorite-type or goethite-type composite oxides, X may be one or more metals, Y is one of three types of oxides, and the loading amount of X on Y is 0.5 to 20%.
  • the catalyst composition of this embodiment is: 10% Pt / La 2 Ba. , 8 Co 3 Fe. . 7 O s . Its preparation method is as follows:
  • the perovskite-type La 2 Ba Q. 8 Co 3 Fe 7 O s was prepared by the complex method, 70 g of EDTA acid was weighed and dissolved in 200 ml of concentrated ammonia water, and 0,04 mol La (N0 3 ) 3 was 0.16 mol. Ba (NO 3 ) 2 , 0.06 mol Co (NO 3 ) 2 , Fe (NO 3 ) 3 were added to the solution, stirred at 80 ° C as the water evaporated to obtain a colloid, and the colloid was cured at 120 ° C. For thousands of hours, then pre-baking at 300 ° C for 2 hours, and finally baking in a muffle furnace at 1050 ° C for 10 hours Get powder. Add 0.9g La 2 Ba. .
  • a hydrazine catalyst hydrogen is produced in a reactor as shown in FIG. 2 and supplied to a fuel cell.
  • 1 is a fuel cell
  • 2 is an air pipe
  • 3 is a catalytic reaction tank
  • 4 is hydrazine hydrate
  • 5 is a catalyst.
  • the reaction was carried out at normal temperature, and 0.03 g of Lao. 2 Sr 0. 8 Co 0. 2 Fe 0. 8 O s + Pt / C catalyst was added, La 0. 2 Sr 0. S Co a2 Fe 0 , 8 Os and Pt /
  • the mass ratio of the two substances C is 1: 1.
  • the 13 ⁇ 4 produced by the decomposition of hydrazine enters the fuel cell, and the measured single cell voltage is 0.8V and the current density is 150mA / cm 2 .
  • the performance curve of the battery is shown in Figure 3. After 1 week of catalytic reaction, no significant change in battery performance was found.

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Combustion & Propulsion (AREA)
  • Inorganic Chemistry (AREA)
  • Health & Medical Sciences (AREA)
  • General Health & Medical Sciences (AREA)
  • Catalysts (AREA)

Abstract

L'invention concerne un catalyseur destiné à décomposer dans des conditions de température ambiante une hydrazine pure ou une hydrazine mélangée à de l'eau afin d'obtenir N2 et H2 ainsi que son procédé de préparation. Le catalyseur faisant l'objet de cette invention se compose des éléments suivants: XYC, X pouvant désigner Fe, Co, Ni, Cu, Zn, Ru, Rh, Pd, In, Os, Ir, Pt, Au, Y désignant des oxydes complexes de type perofskite ou de type fluorite ou encore de type millérite, C désignant un noir de carbone nanométrique, X pouvant désigner un ou plusieurs fers, Y désignant un type parmi les trois types d'oxyde, C pouvant être ajouté ou pas. Ledit catalyseur permet d'obtenir un hydrogène par décomposition fortement sélective de l'hydrazine pure ou de l'hydrate d'hydrazine. L'hydrogène obtenu peut servir de source d'hydrogène à une pile à combustible ou tenir lieu de source d'hydrogène lors du traitement des métaux.
PCT/CN2000/000409 2000-10-17 2000-10-30 Preparation d'un catalyseur permettant de decomposer l'hydrazine et ses applications Ceased WO2002032573A1 (fr)

Priority Applications (1)

Application Number Priority Date Filing Date Title
AU2001212663A AU2001212663A1 (en) 2000-10-17 2000-10-30 The preparation of a hydrazine decomposition catalyst and its use

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
CN00123085A CN1348835A (zh) 2000-10-17 2000-10-17 一种用于肼分解催化剂制备及应用
CN00123085.9 2000-10-17

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WO2002032573A1 true WO2002032573A1 (fr) 2002-04-25

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CN (1) CN1348835A (fr)
AU (1) AU2001212663A1 (fr)
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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111871420A (zh) * 2020-08-03 2020-11-03 重庆工业职业技术学院 一种钛基二氧化锡载萤石形氧化镍电催化剂的制备方法及其应用
JP2023511592A (ja) * 2020-01-22 2023-03-20 シーアン クリステン マテリアルズ テクノロジー コーポレーション リミテッド 化合物、その調製方法及びエネルギー物質としての使用
CN116212844A (zh) * 2022-12-14 2023-06-06 中国科学院大连化学物理研究所 一种单原子分散锆硅改性氧化铝载体及其制备方法和应用

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CN102161003B (zh) * 2011-02-14 2012-09-19 东南大学 一种用于肼降解催化剂的制备和应用方法
CN102558244B (zh) * 2012-01-10 2014-06-25 大连理工大学 邻苯二硫酚基和二氮烯架桥的双核铁配合物、其制备方法及应用
CN102603808B (zh) * 2012-02-03 2014-08-27 大连理工大学 邻苯二硫酚基和氨/胺架桥的双核铁配合物、其制备方法及应用
CN105777458B (zh) * 2014-12-26 2018-05-29 比亚迪股份有限公司 一种用于汽车安全气囊气体发生器的自动点火药及其制备方法
CN105561775B (zh) * 2015-12-23 2018-02-27 中国科学院兰州化学物理研究所 一种偏二甲肼废气的催化氧化处理方法
CN113026051A (zh) * 2021-03-12 2021-06-25 中国科学技术大学 钌锰氧化物固溶体、其制备方法及作为酸性氧析出反应电催化剂的应用

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4122671A (en) * 1962-10-26 1978-10-31 Shell Oil Company Hydrazine decomposition and other reactions
US4324819A (en) * 1970-10-20 1982-04-13 United Aircraft Corporation Catalyst for hydrazine decomposition and the method of producing the catalyst
US4348303A (en) * 1970-10-20 1982-09-07 United Technologies Corporation Catalyst for hydrazine decomposition
JPS59199022A (ja) * 1983-04-26 1984-11-12 Matsushita Electric Ind Co Ltd ＮＯｘ低減化方法
EP0499264A1 (fr) * 1991-02-15 1992-08-19 Nissan Motor Company Limited Méthode de production d'un catalyseur pour la décomposition de l'hydrazine

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4122671A (en) * 1962-10-26 1978-10-31 Shell Oil Company Hydrazine decomposition and other reactions
US4324819A (en) * 1970-10-20 1982-04-13 United Aircraft Corporation Catalyst for hydrazine decomposition and the method of producing the catalyst
US4348303A (en) * 1970-10-20 1982-09-07 United Technologies Corporation Catalyst for hydrazine decomposition
JPS59199022A (ja) * 1983-04-26 1984-11-12 Matsushita Electric Ind Co Ltd ＮＯｘ低減化方法
EP0499264A1 (fr) * 1991-02-15 1992-08-19 Nissan Motor Company Limited Méthode de production d'un catalyseur pour la décomposition de l'hydrazine

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2023511592A (ja) * 2020-01-22 2023-03-20 シーアン クリステン マテリアルズ テクノロジー コーポレーション リミテッド 化合物、その調製方法及びエネルギー物質としての使用
JP7444493B2 (ja) 2020-01-22 2024-03-06 シーアン クリステン マテリアルズ テクノロジー コーポレーション リミテッド 化合物、その調製方法及びエネルギー物質としての使用
CN111871420A (zh) * 2020-08-03 2020-11-03 重庆工业职业技术学院 一种钛基二氧化锡载萤石形氧化镍电催化剂的制备方法及其应用
CN111871420B (zh) * 2020-08-03 2023-07-18 重庆工业职业技术学院 一种钛基二氧化锡载萤石形氧化镍电催化剂的制备方法及其应用
CN116212844A (zh) * 2022-12-14 2023-06-06 中国科学院大连化学物理研究所 一种单原子分散锆硅改性氧化铝载体及其制备方法和应用

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CN1348835A (zh) 2002-05-15

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