JP2007153928A - 環境低負荷型燃料の製造方法および環境低負荷型燃料 - Google Patents
環境低負荷型燃料の製造方法および環境低負荷型燃料 Download PDFInfo
- Publication number
- JP2007153928A JP2007153928A JP2005347135A JP2005347135A JP2007153928A JP 2007153928 A JP2007153928 A JP 2007153928A JP 2005347135 A JP2005347135 A JP 2005347135A JP 2005347135 A JP2005347135 A JP 2005347135A JP 2007153928 A JP2007153928 A JP 2007153928A
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- Prior art keywords
- oil
- low load
- hydrocracking
- mass
- producing
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- 238000004517 catalytic hydrocracking Methods 0.000 claims abstract description 54
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- 238000006243 chemical reaction Methods 0.000 claims description 59
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- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 37
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- 235000019482 Palm oil Nutrition 0.000 description 4
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 4
- XAYGUHUYDMLJJV-UHFFFAOYSA-Z decaazanium;dioxido(dioxo)tungsten;hydron;trioxotungsten Chemical compound [H+].[H+].[NH4+].[NH4+].[NH4+].[NH4+].[NH4+].[NH4+].[NH4+].[NH4+].[NH4+].[NH4+].O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.[O-][W]([O-])(=O)=O.[O-][W]([O-])(=O)=O.[O-][W]([O-])(=O)=O.[O-][W]([O-])(=O)=O.[O-][W]([O-])(=O)=O.[O-][W]([O-])(=O)=O XAYGUHUYDMLJJV-UHFFFAOYSA-Z 0.000 description 4
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- 235000019353 potassium silicate Nutrition 0.000 description 4
- 238000010791 quenching Methods 0.000 description 4
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 description 4
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- 241000196324 Embryophyta Species 0.000 description 3
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- 229910003296 Ni-Mo Inorganic materials 0.000 description 3
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 3
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- 229940024546 aluminum hydroxide gel Drugs 0.000 description 3
- SMYKVLBUSSNXMV-UHFFFAOYSA-K aluminum;trihydroxide;hydrate Chemical compound O.[OH-].[OH-].[OH-].[Al+3] SMYKVLBUSSNXMV-UHFFFAOYSA-K 0.000 description 3
- 239000006227 byproduct Substances 0.000 description 3
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- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 description 2
- 238000010306 acid treatment Methods 0.000 description 2
- 229910052782 aluminium Inorganic materials 0.000 description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 2
- DIZPMCHEQGEION-UHFFFAOYSA-H aluminium sulfate (anhydrous) Chemical compound [Al+3].[Al+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O DIZPMCHEQGEION-UHFFFAOYSA-H 0.000 description 2
- ANBBXQWFNXMHLD-UHFFFAOYSA-N aluminum;sodium;oxygen(2-) Chemical compound [O-2].[O-2].[Na+].[Al+3] ANBBXQWFNXMHLD-UHFFFAOYSA-N 0.000 description 2
- 229910052796 boron Inorganic materials 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- WQOXQRCZOLPYPM-UHFFFAOYSA-N dimethyl disulfide Chemical compound CSSC WQOXQRCZOLPYPM-UHFFFAOYSA-N 0.000 description 2
- 238000001125 extrusion Methods 0.000 description 2
- 235000019387 fatty acid methyl ester Nutrition 0.000 description 2
- 239000000295 fuel oil Substances 0.000 description 2
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- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 description 2
- 229910052753 mercury Inorganic materials 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
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- 239000012266 salt solution Substances 0.000 description 2
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- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 1
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- 238000002144 chemical decomposition reaction Methods 0.000 description 1
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- 238000002485 combustion reaction Methods 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
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- 229910000037 hydrogen sulfide Inorganic materials 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- FAHBNUUHRFUEAI-UHFFFAOYSA-M hydroxidooxidoaluminium Chemical compound O[Al]=O FAHBNUUHRFUEAI-UHFFFAOYSA-M 0.000 description 1
- 238000009434 installation Methods 0.000 description 1
- 239000001630 malic acid Substances 0.000 description 1
- 235000011090 malic acid Nutrition 0.000 description 1
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- 239000011259 mixed solution Substances 0.000 description 1
- 229910052680 mordenite Inorganic materials 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- DCKVFVYPWDKYDN-UHFFFAOYSA-L oxygen(2-);titanium(4+);sulfate Chemical compound [O-2].[Ti+4].[O-]S([O-])(=O)=O DCKVFVYPWDKYDN-UHFFFAOYSA-L 0.000 description 1
- 238000012856 packing Methods 0.000 description 1
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- 235000012239 silicon dioxide Nutrition 0.000 description 1
- 238000011105 stabilization Methods 0.000 description 1
- 230000000087 stabilizing effect Effects 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 238000005486 sulfidation Methods 0.000 description 1
- 150000003464 sulfur compounds Chemical class 0.000 description 1
- 239000003760 tallow Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 229910000348 titanium sulfate Inorganic materials 0.000 description 1
- XJDNKRIXUMDJCW-UHFFFAOYSA-J titanium tetrachloride Chemical compound Cl[Ti](Cl)(Cl)Cl XJDNKRIXUMDJCW-UHFFFAOYSA-J 0.000 description 1
- 238000005809 transesterification reaction Methods 0.000 description 1
- UFTFJSFQGQCHQW-UHFFFAOYSA-N triformin Chemical compound O=COCC(OC=O)COC=O UFTFJSFQGQCHQW-UHFFFAOYSA-N 0.000 description 1
- 238000005292 vacuum distillation Methods 0.000 description 1
- 239000003981 vehicle Substances 0.000 description 1
- 238000010792 warming Methods 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- 239000008096 xylene Substances 0.000 description 1
- 150000003738 xylenes Chemical class 0.000 description 1
- ZXAUZSQITFJWPS-UHFFFAOYSA-J zirconium(4+);disulfate Chemical compound [Zr+4].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O ZXAUZSQITFJWPS-UHFFFAOYSA-J 0.000 description 1
- NLOQZPHAWQDLQW-UHFFFAOYSA-J zirconium(4+);disulfate;tetrahydrate Chemical compound O.O.O.O.[Zr+4].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O NLOQZPHAWQDLQW-UHFFFAOYSA-J 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
- C10G3/00—Production of liquid hydrocarbon mixtures from oxygen-containing organic materials, e.g. fatty oils, fatty acids
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
- C10G3/00—Production of liquid hydrocarbon mixtures from oxygen-containing organic materials, e.g. fatty oils, fatty acids
- C10G3/42—Catalytic treatment
- C10G3/44—Catalytic treatment characterised by the catalyst used
- C10G3/45—Catalytic treatment characterised by the catalyst used containing iron group metals or compounds thereof
- C10G3/46—Catalytic treatment characterised by the catalyst used containing iron group metals or compounds thereof in combination with chromium, molybdenum, tungsten metals or compounds thereof
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
- C10G3/00—Production of liquid hydrocarbon mixtures from oxygen-containing organic materials, e.g. fatty oils, fatty acids
- C10G3/50—Production of liquid hydrocarbon mixtures from oxygen-containing organic materials, e.g. fatty oils, fatty acids in the presence of hydrogen, hydrogen donors or hydrogen generating compounds
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
- C10G47/00—Cracking of hydrocarbon oils, in the presence of hydrogen or hydrogen- generating compounds, to obtain lower boiling fractions
- C10G47/02—Cracking of hydrocarbon oils, in the presence of hydrogen or hydrogen- generating compounds, to obtain lower boiling fractions characterised by the catalyst used
- C10G47/04—Oxides
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Abstract
【解決手段】 上記課題を解決する環境低負荷型燃料の製造方法は、沸点230℃以上の留分を含む動植物油に由来する油脂成分を含有する原料油を準備する工程と、周期律表第6A族および第8族に属する金属からなる群より選択される少なくとも1種の金属と酸性質を有する無機酸化物とを含有する水素化分解触媒の存在下、原料油または必要に応じて所定の前処理工程を経た原料油を水素化分解する水素化分解工程とを備える。
【選択図】 なし
Description
本実施形態において用いる原料油は沸点230℃以上の留分を含む動植物油に由来する油脂成分を含有するものである。本発明における油脂成分とは、天然もしくは人工的に生産、製造される動植物油脂および動植物油脂成分および/またはこれらの油脂を由来して生産、製造される油脂成分並びにこれらの油脂製品の性能を維持、向上させる目的で添加される成分を示している。かかる油脂成分としては、例えば、牛脂、菜種油、大豆油、パーム油などが挙げられる。本実施形態においては、油脂成分の種類については特に限定されないが、LCA−CO2削減の観点からは植物油脂が好ましい。更に、脂肪酸アルキル鎖の炭素数およびその反応性の観点からは菜種油、大豆油及びパーム油がより好ましい。原料油に含有される油脂成分は、複数の油脂成分の混合油であってもよく、これら油脂を使用した後の廃油であってもよい。
本実施形態の水素化前処理工程では、周期律表第6A族および第8族に属する金属からなる群より選択される少なくとも1種の金属を含む水素化触媒の存在下、上記の原料油を水素化する。この処理により原料油の脱酸素が行われ、原料油の酸素分が低減される。
本実施形態の水素化分解工程では、周期律表第6A族および第8族に属する金属からなる群より選択される少なくとも1種の金属と、酸性質を有する無機酸化物と、を含有する水素化分解触媒の存在下、水素化前処理工程を経た原料油(留出油)を水素化分解する。
上述の本実施形態の環境低負荷型燃料の製造方法により、ガソリン基材、軽油基材、灯油基材、重質ナフサ基材又は液化石油ガス基材として好適な本発明に係る環境低負荷型燃料を得ることができる。以下、各基材に好適な本発明によって得られる燃料について説明する。
濃度5質量%のアルミン酸ナトリウム水溶液1kgに水ガラス3号を加え70℃に保温した容器に入れた。一方、濃度2.5%の硫酸アルミニウム水溶液1kgを70℃に保温した別の容器に入れ、これを前述のアルミン酸ナトリウム水溶液に15分間かけて滴下した。水ガラスの量は所定のシリカ含有量となるよう調整した。混合溶液のpHが6.9〜7.5になる時点を終点とし、得られたスラリー状生成物をフィルターに通して濾取し、ケーキ状のスラリーを得た。次に、ケーキ状スラリーを還流冷却器を取り付けた容器に移し、蒸留水300mlと27%アンモニア水溶液3gを加え、70℃で24時間加熱撹拌した。続いて、加熱撹拌後のスラリーを混練装置に入れ、80℃以上に加熱し水分を除去ながら混練し、粘土状の混練物を得た。次に、得られた混練物を押出し成形機によって直径1.5mmのシリンダー形状に押出し、110℃で1時間乾燥した後、550℃で焼成し、成形担体を得た。
シリカ/アルミナ比が5のY型ゼオライトを公知の超安定化処理方法により安定化した後、1N硝酸水溶液により酸処理を施し、単位格子長が24.33Å、シリカ/アルミナ比が30、水銀圧入法によって測定される細孔直径30〜100Åを有する細孔の容積がゼオライト重量に対して0.055ml/gのプロトン型の超安定化Y型ゼオライトを得た。次に、得られた超安定化Y型ゼオライト(550g)を硝酸アンモニウム水溶液(濃度2N、3リットル)に加え、室温で撹拌してアンモニウム型に変換した。
水ガラス3号をpH14でゲル化させた後、pH7で2時間熟成して得たスラリーに、硫酸ジルコニウム(四水和物)を含む水溶液を加え、さらにそのスラリーをpH7に調整してシリカ−ジルコニア複合水酸化物を生成した。これを30分熟成した後、硫酸アルミニウム(14水和物)を含む水溶液を加えてpH7に調整し、シリカ−ジルコニア−アルミナ複合水酸化物を生成した。このスラリーからシリカ−ジルコニア−アルミナ複合水酸化物をろ過し、洗浄した後、加熱濃縮によって水分を調整し、押し出し成型、乾燥、焼成を行い、触媒担体(多孔質担体)を得た。得られた成形担体300gに、蒸留水150mlにパラタングステン酸アンモニウム、硝酸ニッケル6水和物を溶解した含浸溶液をスプレーさせながら含浸させ、水素化分解触媒としての触媒Cを得た。使用するパラタングステン酸アンモニウム、硝酸ニッケル6水和物は所定の担持量となるよう調整した。製造した触媒Cの物性を表1にまとめた。
内径20mmの第一反応管に第一の触媒として触媒Aを70ml充填し、内径20mmの第二反応管に第二の触媒として触媒Bを30ml充填した。これらの第一反応管及び第二反応管を直列にして固定床流通式反応装置に取り付けた後、ジメチルジサルファイドを加えた直留軽油(硫黄分3質量%)を用いて、触媒層平均温度300℃、水素分圧6MPa、液空間速度(LHSV)1h−1、水素/油比200NL/Lの条件下で、触媒の予備硫化を4時間行った。予備硫化が終了した後、パーム油(15℃密度0.916g/ml、酸素分11.4質量%、10%留出点588℃)および中東系の減圧軽油留分(15℃密度0.919g/ml、硫黄分2.41質量%、窒素分610質量ppm、10%留出点344℃)を20:80の容量比で混合した原料油を、第一反応管及び第二反応管における反応温度400℃、圧力10.5MPa、液空間速度(LHSV)0.7h−1の条件下で通油して水素化分解を行った。なお、第一反応管と第二反応管の間で水素ガス(クエンチ水素)を導入し、かかる水素ガスの容量比率を全導入水素量の20容量%とし、導入した全水素によって求めた水素/油比を507NL/Lとした。これらの反応条件を表2にまとめた。なお、混合原料油の酸素分は2.28質量%であった。また、上記反応温度は、触媒層の平均温度を示すものである。
分解率(質量%)={100−[生成油に含まれる沸点360℃以上の留分量(質量%)}/{[原料油に含まれる沸点360℃以上の留分量(質量%)]}×100
触媒A(40ml)を充填した第一反応管(内径20mm)と、触媒C(60ml)を充填した第二反応管(内径20mm)を直列に固定床流通式反応装置に取り付けたこと、及び、原料油の通油において液空間速度(LHSV)を0.4h−1としたこと以外は実施例1と同様にして、原料油の水素化分解を行った。実施例2の反応条件を表2にまとめた。
実施例2における原料油を、パーム油(15℃密度0.916g/ml、酸素分11.4質量%、10%留出点588℃)のみとしたこと以外は実施例2と同様にして、原料油の水素化分解を行った。実施例3の反応条件を表2にまとめた。
実施例2における、第一反応管と第二反応管の間で導入する水素ガスの容量比率を全導入水素量の0容量%としたこと、すなわち、クエンチ水素を導入しなかったこと以外は実施例2と同様にして、原料油の水素化分解を行った。実施例4の反応条件を表2にまとめた。
実施例2における原料油を、中東系の減圧軽油留分(15℃密度0.919g/ml、硫黄分2.41質量%、窒素分610質量ppm、10%留出点344℃)のみとしたこと以外は実施例2と同様にして、原料油の水素化分解を行った。比較例1の反応条件を表2にまとめた。
Claims (15)
- 沸点230℃以上の留分を含む動植物油に由来する油脂成分を含有する原料油を準備する工程と、
周期律表第6A族および第8族に属する金属からなる群より選択される少なくとも1種の金属と、酸性質を有する無機酸化物と、を含有する水素化分解触媒の存在下、前記原料油または必要に応じて所定の前処理工程を経た前記原料油を水素化分解する水素化分解工程と、
を備えることを特徴とする環境低負荷型燃料の製造方法。 - 前記水素化分解工程において、水素圧力6〜20MPa、液空間速度(LHSV)0.2〜1.5h−1、及び、水素/油比200〜2000NL/Lの反応条件下で、前記原料油または必要に応じて所定の前処理工程を経た前記原料油を水素化分解することを特徴とする請求項1に記載の環境低負荷型燃料の製造方法。
- 前記水素化分解工程の前に前記原料油を前処理する前処理工程を更に備え、
前記前処理工程が、周期律表第6A族および第8族に属する金属からなる群より選択される少なくとも1種の金属を含む水素化触媒の存在下、前記原料油を水素化する水素化前処理工程であることを特徴とする請求項1又は2に記載の環境低負荷型燃料の製造方法。 - 前記水素化前処理工程において、前記原料油中の酸素分を60質量%以上減少させることを特徴とする請求項3に記載の環境低負荷型燃料の製造方法。
- 前記原料油が、前記油脂成分の全モル数を基準としてトリグリセリド構造を有する分子を80モル%以上含むことを特徴とする請求項1〜4のいずれかに記載の環境低負荷型燃料の製造方法。
- 前記原料油が、石油系炭化水素留分を更に含有することを特徴とする請求項1〜5のいずれかに記載の環境低負荷型燃料の製造方法。
- 前記水素化分解触媒が、酸性質を有する前記無機酸化物として、シリカ、アルミナ、ボリア、ジルコニア、マグネシアおよびゼオライトからなる群より選択される2種以上から構成される複合酸化物を含むことを特徴とする請求項1〜6のいずれか1項に記載の環境低負荷型燃料の製造方法。
- 前記水素化分解触媒が、ゼオライトを含むことを特徴とする請求項1〜7のいずれか1項に記載の環境低負荷型燃料の製造方法。
- 請求項1〜8のいずれか1項に記載の製造方法により得られることを特徴とする環境低負荷型燃料。
- 沸点が260〜320℃であり、軽油基材として用いられることを特徴とする請求項9に記載の環境低負荷型燃料。
- 硫黄分が10質量ppm以下であり且つ酸素分が0.5質量%以下であることを特徴とする請求項10に記載の環境低負荷型燃料。
- 沸点が180〜230℃であり、灯油基材として用いられることを特徴とする請求項9に記載の環境低負荷型燃料。
- 硫黄分が10質量ppm以下であり且つ酸素分が0.5質量%以下であることを特徴とする請求項12に記載の環境低負荷型燃料。
- 沸点が90〜110℃であり、重質ナフサ基材として用いられることを特徴とする請求項9に記載の環境低負荷型燃料。
- 炭素数4以下の炭化水素であり、液化石油ガス基材として用いられることを特徴とする請求項9に記載の環境低負荷型燃料。
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