JP7311596B2 - 触媒組成物およびその用途 - Google Patents
触媒組成物およびその用途 Download PDFInfo
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- JP7311596B2 JP7311596B2 JP2021527857A JP2021527857A JP7311596B2 JP 7311596 B2 JP7311596 B2 JP 7311596B2 JP 2021527857 A JP2021527857 A JP 2021527857A JP 2021527857 A JP2021527857 A JP 2021527857A JP 7311596 B2 JP7311596 B2 JP 7311596B2
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- JP
- Japan
- Prior art keywords
- biochar
- range
- steam
- catalyst
- loading
- 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.)
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- 239000003054 catalyst Substances 0.000 title claims description 140
- 239000000203 mixture Substances 0.000 title claims description 78
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 103
- 238000011068 loading method Methods 0.000 claims description 77
- 229910052759 nickel Inorganic materials 0.000 claims description 53
- 229910052725 zinc Inorganic materials 0.000 claims description 52
- 239000011701 zinc Substances 0.000 claims description 52
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims description 50
- 239000010949 copper Substances 0.000 claims description 50
- 229910052802 copper Inorganic materials 0.000 claims description 49
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 48
- 238000000034 method Methods 0.000 claims description 48
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 46
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 38
- 239000002041 carbon nanotube Substances 0.000 claims description 36
- 229910052751 metal Inorganic materials 0.000 claims description 35
- 239000002184 metal Substances 0.000 claims description 35
- 229910021393 carbon nanotube Inorganic materials 0.000 claims description 31
- 238000004519 manufacturing process Methods 0.000 claims description 26
- 230000008569 process Effects 0.000 claims description 19
- 239000004215 Carbon black (E152) Substances 0.000 claims description 14
- 229930195733 hydrocarbon Natural products 0.000 claims description 14
- 150000002430 hydrocarbons Chemical class 0.000 claims description 14
- 241000209094 Oryza Species 0.000 claims description 9
- 235000007164 Oryza sativa Nutrition 0.000 claims description 9
- 235000009566 rice Nutrition 0.000 claims description 9
- 238000010438 heat treatment Methods 0.000 claims description 7
- 239000011148 porous material Substances 0.000 claims description 6
- 239000002154 agricultural waste Substances 0.000 claims description 5
- 239000010902 straw Substances 0.000 claims description 5
- 241000609240 Ambelania acida Species 0.000 claims description 4
- 239000010905 bagasse Substances 0.000 claims description 4
- 239000010903 husk Substances 0.000 claims description 4
- 238000001354 calcination Methods 0.000 claims description 3
- 239000002048 multi walled nanotube Substances 0.000 claims description 3
- 238000010306 acid treatment Methods 0.000 claims description 2
- 238000001035 drying Methods 0.000 claims description 2
- 238000012545 processing Methods 0.000 claims description 2
- 238000005406 washing Methods 0.000 claims description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 28
- 229910052739 hydrogen Inorganic materials 0.000 description 25
- 239000001257 hydrogen Substances 0.000 description 25
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 8
- 150000002739 metals Chemical class 0.000 description 8
- 229910052799 carbon Inorganic materials 0.000 description 7
- 238000006243 chemical reaction Methods 0.000 description 7
- 239000000047 product Substances 0.000 description 7
- 238000001878 scanning electron micrograph Methods 0.000 description 6
- 230000015572 biosynthetic process Effects 0.000 description 4
- 229910002092 carbon dioxide Inorganic materials 0.000 description 4
- 238000012986 modification Methods 0.000 description 4
- 230000004048 modification Effects 0.000 description 4
- 238000000197 pyrolysis Methods 0.000 description 4
- 239000007787 solid Substances 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- 230000008901 benefit Effects 0.000 description 3
- 230000003197 catalytic effect Effects 0.000 description 3
- 239000007789 gas Substances 0.000 description 3
- 239000012535 impurity Substances 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 238000000746 purification Methods 0.000 description 3
- 230000009467 reduction Effects 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 239000002028 Biomass Substances 0.000 description 2
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 2
- 239000006227 byproduct Substances 0.000 description 2
- 239000001569 carbon dioxide Substances 0.000 description 2
- 238000004523 catalytic cracking Methods 0.000 description 2
- 238000000354 decomposition reaction Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000012530 fluid Substances 0.000 description 2
- 239000005431 greenhouse gas Substances 0.000 description 2
- 239000003345 natural gas Substances 0.000 description 2
- 239000002243 precursor Substances 0.000 description 2
- 230000008929 regeneration Effects 0.000 description 2
- 238000011069 regeneration method Methods 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 238000000629 steam reforming Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000002411 thermogravimetry Methods 0.000 description 2
- ZFYIQPIHXRFFCZ-QMMMGPOBSA-N (2s)-2-(cyclohexylamino)butanedioic acid Chemical compound OC(=O)C[C@@H](C(O)=O)NC1CCCCC1 ZFYIQPIHXRFFCZ-QMMMGPOBSA-N 0.000 description 1
- 241000209140 Triticum Species 0.000 description 1
- 235000021307 Triticum Nutrition 0.000 description 1
- 240000008042 Zea mays Species 0.000 description 1
- 235000005824 Zea mays ssp. parviglumis Nutrition 0.000 description 1
- 235000002017 Zea mays subsp mays Nutrition 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 239000012298 atmosphere Substances 0.000 description 1
- 229910002091 carbon monoxide Inorganic materials 0.000 description 1
- 239000008209 carbon nanofoam Substances 0.000 description 1
- 229910021400 carbon nanofoam Inorganic materials 0.000 description 1
- 229910002090 carbon oxide Inorganic materials 0.000 description 1
- 238000003421 catalytic decomposition reaction Methods 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- XTVVROIMIGLXTD-UHFFFAOYSA-N copper(II) nitrate trihydrate Substances [Cu+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O XTVVROIMIGLXTD-UHFFFAOYSA-N 0.000 description 1
- 235000005822 corn Nutrition 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 238000000921 elemental analysis Methods 0.000 description 1
- 230000008030 elimination Effects 0.000 description 1
- 238000003379 elimination reaction Methods 0.000 description 1
- 230000007717 exclusion Effects 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 238000001722 flash pyrolysis Methods 0.000 description 1
- 238000011010 flushing procedure Methods 0.000 description 1
- 239000002803 fossil fuel Substances 0.000 description 1
- 238000003306 harvesting Methods 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 238000005470 impregnation Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000003863 metallic catalyst Substances 0.000 description 1
- AOPCKOPZYFFEDA-UHFFFAOYSA-N nickel(2+);dinitrate;hexahydrate Chemical compound O.O.O.O.O.O.[Ni+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O AOPCKOPZYFFEDA-UHFFFAOYSA-N 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 239000012299 nitrogen atmosphere Substances 0.000 description 1
- 230000006911 nucleation Effects 0.000 description 1
- 238000010899 nucleation Methods 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 230000002265 prevention Effects 0.000 description 1
- 239000013014 purified material Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000010907 stover Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000004227 thermal cracking Methods 0.000 description 1
- 238000005979 thermal decomposition reaction Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- 238000005145 wavelength dispersive X-ray fluorescence spectroscopy Methods 0.000 description 1
- SFYBRCJPMDQKHA-UHFFFAOYSA-N zinc;dinitrate;tetrahydrate Chemical compound O.O.O.O.[Zn+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O SFYBRCJPMDQKHA-UHFFFAOYSA-N 0.000 description 1
Classifications
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- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/0009—Use of binding agents; Moulding; Pressing; Powdering; Granulating; Addition of materials ameliorating the mechanical properties of the product catalyst
- B01J37/0018—Addition of a binding agent or of material, later completely removed among others as result of heat treatment, leaching or washing,(e.g. forming of pores; protective layer, desintegrating by heat)
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- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/158—Carbon nanotubes
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- B01J21/00—Catalysts comprising the elements, oxides, or hydroxides of magnesium, boron, aluminium, carbon, silicon, titanium, zirconium, or hafnium
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- B01J23/06—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of zinc, cadmium or mercury
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- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
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- B01J23/76—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
- B01J23/80—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36 with zinc, cadmium or mercury
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- B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
- B01J8/18—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with fluidised particles
- B01J8/24—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with fluidised particles according to "fluidised-bed" technique
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- C—CHEMISTRY; METALLURGY
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- 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
- C01B3/22—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen by decomposition of gaseous or liquid organic compounds
- C01B3/24—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen by decomposition of gaseous or liquid organic compounds of hydrocarbons
- C01B3/26—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen by decomposition of gaseous or liquid organic compounds of hydrocarbons using catalysts
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- C—CHEMISTRY; METALLURGY
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- C01B2203/1058—Nickel catalysts
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- C01B2203/00—Integrated processes for the production of hydrogen or synthesis gas
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2203/00—Integrated processes for the production of hydrogen or synthesis gas
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
- C01P2002/88—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70 by thermal analysis data, e.g. TGA, DTA, DSC
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- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Materials Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Nanotechnology (AREA)
- Inorganic Chemistry (AREA)
- Combustion & Propulsion (AREA)
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Health & Medical Sciences (AREA)
- General Health & Medical Sciences (AREA)
- Catalysts (AREA)
- Hydrogen, Water And Hydrids (AREA)
- Carbon And Carbon Compounds (AREA)
Description
当業者であれば、本開示が、具体的に記載されたもの以外の変形および修正の対象となることを理解されたい。本開示は、全てのそのような変形および修正を含むことを理解されたい。本開示はまた、本明細書において、参照または示される、全てのそのようなステップ、特徴、組成物および化合物を、個々にまたは集合的に、ならびにそのようなステップまたは特徴のいずれかまたは複数の任意および全ての組み合わせを含む。
便宜上、本開示のさらなる説明の前に、本明細書で使用される特定の用語、および例をここに収集する。これらの定義は、本開示の残りの部分に照らして読まれ、当業者によって理解されるべきである。本明細書で使用される用語は、当業者に認識され、知られている意味を有するが、便宜上および完全性のために、特定の用語およびそれらの意味を以下に示す。
本開示の別の実施形態において、以下を含む触媒組成物が提供される:(a)少なくとも1つのスチームバイオチャー;および(b)前記少なくとも1つのスチームバイオチャー内に配置されている、少なくとも1つの三金属触媒。
本開示のさらに別の実施形態において、以下を含む触媒組成物が提供される:(a)少なくとも1つのスチームバイオチャー;および(b)金属構造が前記少なくとも1つのスチームバイオチャー上またはその内部に組み合わせて配置されている、少なくとも1つの三金属触媒。
以下の例は、本発明の例示として与えられ、本開示の範囲を限定するものと解釈されるべきではない。前述の一般的な説明および以下の詳細な説明はいずれも例示的かつ説明的なものにすぎず、請求項に係る主題のさらなる説明を提供することを意図していることを理解されたい。
生バイオチャーは、バイオマス(おがくず、稲わら、籾殻、バガス、その他の農業廃棄物)の1つの熱分解からの副産物として得られた。熱分解は、低速、高速またはフラッシュ熱分解法から選択される任意の方法から行うことができる。おがくずは、流動床反応器中、500℃、N2雰囲気下で、連続供給により熱分解した。生成物から揮発性ガスを分離した後、生バイオチャーを回収した。生バイオチャーを、流動床で、800℃で5時間、スチームを用いてさらに改質した。
この方法は、流動床反応器で実施された。炭素源として、メタンを10SPLHの流量(300~800 l/l/hの範囲内のGHSV)で供給した。17gの触媒組成物を反応器に装填した。反応器をN2でフラッシュした後、窒素下で550℃まで加熱した。さらに、H2環境下で還元を行い、触媒組成物を3時間還元した。還元後、反応器を反応温度750℃に加熱した。
CNTの形成を、図3、図4、図5、および図6に示すSEM画像により分析した。例2のプロセスで触媒1を使用した場合、表面には、ごくわずか(very few)/無視できる(negligible)CNTが観察された(図3)。例2のプロセスで触媒2を使用した場合、SEM画像から触媒上にカーボンナノフォームの核形成が認められたが、チューブ/シートの形成は認められなかった(図4)。しかし、触媒3を用いた場合には、このプロセスにより、直径40nm~100nmの範囲の多層CNTが生成された(図4)。
本開示は、水素およびカーボンナノチューブの製造方法に使用される触媒組成物を提供する。水素の製造の他に、それはまた、高品質、特に要求の厳しい産業用途に適した純度のカーボンナノチューブを得ることを可能にする。
Claims (13)
- (a)少なくとも1つのスチームバイオチャー;および
(b)ニッケル、銅、亜鉛、およびそれらの組み合わせからなる群から選択される金属を含む少なくとも1つの三金属触媒であって、前記少なくとも1つのスチームバイオチャーに対して、ニッケル担持量が20~60重量%の範囲であり、銅担持量が0.5~5.0重量%の範囲であり、亜鉛担持量が0.5~5.0重量%の範囲である、三金属触媒、
を含む、水素ガスおよびカーボンナノチューブを製造するための触媒組成物。 - 前記少なくとも1つのスチームバイオチャーに対して、ニッケル担持量が27~31重量%の範囲であり、銅担持量が2.0~2.7重量%の範囲であり、亜鉛担持量が2.0~2.7重量%の範囲である、請求項1に記載の触媒組成物。
- 前記少なくとも1つの三金属触媒が、前記少なくとも1つのスチームバイオチャーの上に、その中に、あるいは、その上またはその中に組み合わせて、配置される、請求項1に記載の触媒組成物。
- 前記少なくとも1つのスチームバイオチャーが、700~950m2/gの範囲の表面積を有し、0.60~0.70cc/gの範囲の細孔容積を有する、請求項1に記載の触媒組成物。
- 前記少なくとも1つのスチームバイオチャーが、生バイオチャーおがくず、生バイオチャー稲わら、生バイオチャー籾殻、生バイオチャーバガス、その他の農業廃棄物、およびそれらの組み合せから得られる、請求項1に記載の触媒組成物。
- (a)生バイオチャーをスチームで加熱して、少なくとも1つのスチームバイオチャーを得ること;
(b)少なくとも1つの三金属触媒を得ること;および
(c)前記少なくとも1つの三金属触媒を、前記少なくとも1つのスチームバイオチャーに含浸(impregnate)させ、続いて焼成(calcination)して、前記組成物を得ること、
を含む、請求項1に記載の触媒組成物の製造方法。 - スチームでの生バイオチャーの加熱は、700~900℃の範囲の温度で、5~6時間の範囲の期間行われる、請求項6に記載の方法。
- (a)請求項1~5のいずれか一項に記載の組成物を得ること;
(b)少なくとも1つのガス状炭化水素と、前記請求項1~5のいずれか一項に記載の組成物とを接触させて、混合物と水素ガスとを得ること;および
(c)前記混合物を処理して、カーボンナノチューブを得ること、
を含む、水素ガスおよびカーボンナノチューブの製造方法。 - 前記少なくとも1つのガス状炭化水素と前記請求項1~5のいずれか一項に記載の組成物との接触が、15分~600分の範囲の期間、600℃~800℃の範囲の温度で行われる、請求項8に記載の方法。
- 前記少なくとも1つのガス状炭化水素が、300~800 l/l/hの範囲のGHSVを有する、請求項8に記載の方法。
- 前記混合物を処理してカーボンナノチューブを得ることが、酸性処理、洗浄、乾燥、およびそれらの組み合わせから選択されるプロセスを含む、請求項8に記載の方法。
- 前記カーボンナノチューブが、ID/IG比が0.65~1.0である多層ナノチューブである、請求項8に記載の方法。
- 前記方法が、流動床反応器、移動床反応器、または回転床反応器から選択される反応器内で実施される、請求項8に記載の方法。
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