JP2004323626A - Fuel oil compatible with environment and its manufacturing method - Google Patents
Fuel oil compatible with environment and its manufacturing method Download PDFInfo
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Abstract
Description
【０００１】
【発明の属する技術分野】
本発明は、環境への影響を低減した灯油、ジェット燃料油などの環境対応燃料油およびその製造方法に関し、詳しくは硫黄分、芳香族分を低減することで環境問題に配慮しつつかつ十分な低温特性を確保した環境対応燃料油およびその製造方法に関する。
【０００２】
【従来の技術】
近年、環境問題の高まりから灯油、ジェット燃料油などの燃料油中の硫黄分、芳香族分の低減が求められている。例えば、ストーブやボイラー等の外燃用に供される灯油についても、住宅の気密性向上により燃焼ガスのクリーン化が求められている。また、灯油留分はジェット燃料用にも供されることから、実用上低温性能についても維持する必要がある。
【０００３】
一方、フィッシャー・トロプシュ（Ｆｉｓｃｈｅｒ−Ｔｒｏｐｓｃｈ）法によれば天然ガスの改質で得られる合成ガス（水素と一酸化炭素よりなる）からノルマルパラフィンを主成分とし、硫黄と芳香族をほとんど含まない炭化水素を合成することができる。この合成された炭化水素を原料として合成燃料油を製造することが近年注目されている（例えば、特許文献１〜７参照。）。しかし、このような合成燃料油は、硫黄分、芳香族分が十分に低いものではあるが、石油系の灯油と比較すると、低温性能が十分でない。
【０００４】
【特許文献１】
特表平１１−５１３７２９号公報
【特許文献２】
特表平１１−５１３７３０号公報
【特許文献３】
特表２００１−５１１２０７号公報
【特許文献４】
特表２００１−５２２３８２号公報
【特許文献５】
特表２００２−５０７６３５号公報
【特許文献６】
特表２００２−５２６６３６号公報
【特許文献７】
特表２００２−５２６６３７号公報
【０００５】
【発明が解決しようとする課題】
本発明は、このような課題を解決するもので、硫黄分、芳香族分が十分に低く、かつ、実用上十分な低温性能を確保し、さらに、ジェット燃料へ混合する基材として十分な性能を確保した環境対応燃料油およびその製造方法を提供することを課題とするものである。
【０００６】
【課題を解決するための手段】
本発明者らは、ノルマルパラフィンを原料にして水素化分解および異性化を行って得られた生成油の重質ノルマルパラフィン含有量に着目し、その特定の留分を燃料油として用いることにより、このような課題を解決することができることを見出し、本発明を完成した。
【０００７】
本発明による環境対応燃料油の製造方法は、ノルマルパラフィン原料を、担体に水素化活性金属が担持された触媒と接触させることで水素化分解および異性化を行い、生成油を得る工程と、この生成油を分留して９５％留出温度が２６０℃以下の留分を得る工程を含むものであり、特には、前記ノルマルパラフィン原料がＦｉｓｃｈｅｒ−Ｔｒｏｐｓｃｈ法により合成されたものであることが好ましい。
【０００８】
また、本発明による環境対応燃料油は、密度が０．７４ｇ／ｃｍ３〜０．７８ｇ／ｃｍ３、硫黄分が１０質量ｐｐｍ以下、析出点が−５０℃以下、炭素数１４以上のノルマルパラフィン含有量が４．０質量％以下、炭素数１１以下のノルマルパラフィン含有量が０．５〜１５．０質量％、２２０℃以下の留分が５０〜９５容量％、かつ、芳香族分が５質量％以下である。この環境対応燃料油は、外燃用、ジェット燃料用の燃料として好ましく用いられる。
【０００９】
【発明の実施の形態】
〔ノルマルパラフィン原料〕
本発明の製造方法で用いるノルマルパラフィン原料は、軽質ノルマルパラフィンは水素化分解および異性化の反応性が低いので、必要に応じてあらかじめ蒸留等により原料油の軽質留分をカットしたものが好ましく、具体的には初留点としては３００℃以上、特には３１０℃以上、１０％留出温度としては３５０℃以上、特には３６０℃以上の原料を使用することが好ましい。また、このノルマルパラフィン原料の重質分は、分解により灯軽油留分のノルマルパラフィンに転換されるので、同じく蒸留などにより重質過ぎる留分をカットすることが好ましく、終点としては６００℃以下、特には５９０℃以下とすること、９０％留出温度としては５６０℃以下、特には５５０℃以下とすることが好ましい。これらにより水素化分解および異性化の反応率、灯軽油収率を高くすることができる。
【００１０】
ノルマルパラフィン原料中のノルマルパラフィン含有量は８５質量％以上、特には９５質量％以上が好ましい。不純物含有量としては、硫黄分５００ｐｐｍ以下、特には５０ｐｐｍ以下、また、窒素分１００ｐｐｍ以下、特には１０ｐｐｍ以下が好ましい。
【００１１】
ノルマルパラフィン原料は、上記の性状を有するものが好ましく使用することができる。特にその種類を限定するものではないが、石油精製工程、例えば潤滑油製造工程の１つである溶剤脱ろう工程から得られるスラックワックスや、Ｆｉｓｃｈｅｒ−Ｔｒｏｐｓｃｈ法により合成された合成ワックスなどを用いることができる。これらのワックスには様々な種類のものがあるが、単独で用いても、または２種以上混合して用いても良く、スラックワックスと合成ワックスとを混合して用いも良い。特にはＦｉｓｃｈｅｒ−Ｔｒｏｐｓｃｈ法による合成ワックスを単独で用いることが好ましい。なお、Ｆｉｓｃｈｅｒ−Ｔｒｏｐｓｃｈ法とは、一酸化炭素と水素を、触媒を用いて反応させ、主にノルマルパラフィン、また少量ではあるがオレフィンやアルコール等を合成する方法である。
【００１２】
〔触媒〕
本発明の燃料油の製造方法で用いる触媒は、担体に水素化活性金属を担持したものである。例えば、特表２００２−５２３２３１号公報あるいは特許第２９０１０４７号公報に開示されている触媒が、好ましく用いられる。本発明の製造方法において、好ましく用いることができる担体は、シリカアルミナを含む無機多孔質酸化物からなる担体である。シリカアルミナを、アルミナをバインダーとして担体に成形させたものが好ましい。結晶質のシリカアルミナとしてはモルデナイトが好ましい。シリカアルミナは非晶質または結晶質のものを用いることができるが、非晶質を用いることが好ましい。非晶質シリカアルミナのシリカ／アルミナモル比の範囲は３〜８が好ましい。担体にはアルミニウム、ケイ素の酸化物以外は含まれていない方が好ましいが、マグネシア、ジルコニア、ボリア、カルシア等を含ませることもできる。
【００１３】
担持される水素化活性金属に特に制限はないが、周期律表の第６族、第９族、および第１０族から選ばれる１種または２種以上の金属成分を含むことが好ましい。第６族、第９族、第１０族から選ばれる金属としては、モリブデン、タングステン、コバルト、ロジウム、イリジウム、ニッケル、白金、パラジウムが挙げられ、特にモリブデン、タングステン、コバルト、ニッケルなどの非貴金属が水素化活性成分として好ましく用いられる。水素化活性金属の担持量は、金属元素の合計量が０．０５〜３５質量％、特には０．１〜３０質量％となるように添加、担持することが好ましい。
【００１４】
〔水素化分解および異性化〕
本発明の製造方法で用いる水素化分解および異性化は、反応温度が３００〜４００℃、特には３２０〜３５０℃、水素圧力が１〜２０ＭＰａ、特には３〜９ＭＰａ、水素／オイル比が１００〜２０００ＮＬ／Ｌ、特には３００〜１５００ＮＬ／Ｌ、液空間速度（ＬＨＳＶ）が０．５〜５ｈｒ−１の反応条件で行うことが好ましい。
【００１５】
ノルマルパラフィン原料中の３６０℃以上の成分うち、３６０℃未満の成分となった割合を分解率として定義すると、灯油留分の異性化率と収率を上げるためには、分解率は５０〜８５質量％が好ましい。８５質量％を超える分解率では、灯油留分が二次分解を起こしてしまう。
【００１６】
〔灯油留分〕
本発明の製造方法では、水素化分解および異性化工程による生成油から、１０％留出温度が１６０℃以上好ましくは１７０℃以上、９５％留出温度が２６０℃以下好ましくは２５０℃以下の留分（以下、灯油留分とも言う）を分留する。
【００１７】
〔配合〕
本発明の製造方法では、上述の灯油留分をそのまま灯油として、あるいは他の基材と混合してジェット燃料や、ストーブやボイラーなどの外燃用燃料として、また、それらの燃料の基材として用いることができる。他の基材としては、例えば、原油を精製して生産される灯油あるいはそれらの半製品、中間製品などの配合用基材が挙げられる。燃料への添加剤としては、低温流動性向上剤、酸化防止剤、金属不活性化剤、腐食防止剤等の公知の燃料添加剤を添加してもよい。通常、燃料油が灯油として取引される場合には、軽油識別剤が添加される。
【００１８】
〔環境対応燃料油〕
本発明による環境対応燃料油は、密度が０．７４ｇ／ｃｍ３〜０．７８ｇ／ｃｍ３、硫黄分が１０質量ｐｐｍ以下、析出点が−５０℃以下、炭素数１４以上のノルマルパラフィン含有量が４．０質量％以下、炭素数１１以下のノルマルパラフィン含有量が０．５〜１５．０質量％、２２０℃以下の留分が５０〜９５容量％、かつ、芳香族分が５質量％以下である。
【００１９】
硫黄分は５質量ｐｐｍ以下、特には１質量ｐｐｍ以下が好ましい。析出点は−５５℃以下、特には−６５℃以下が好ましい。芳香族分は３質量％以下、特には１質量％以下が好ましい。
【００２０】
本発明による環境対応燃料油の蒸留性状として、１０％留出温度は１６０℃以上特には１７５℃以上が好ましく、９５％留出温度は２２０℃〜２６０℃、特には２２０℃〜２５０℃が好ましい。２２０℃以下の留分は６０〜９０容量％が好ましい。
【００２１】
【実施例】
以下、実施例に基づき本発明を詳細に説明するが、この実施例により、本発明が限定して解釈されるものではない。
【００２２】
〔触媒Ａの調製〕
シリカアルミナ粉体および擬ベーマイト粉体を混合、混練して、シリンダー状に成形した後、乾燥し、６００℃で焼成することで担体を調製した。この担体は、乾燥担体基準で、シリカアルミナ８０質量％およびアルミナ２０質量％からなり、直径約１．６ｍｍのシリンダー形状であった。シリカアルミナ粉体としては、シリカ／アルミナモル比４．４、凝集粒径１〜１０μｍのもの９４．４質量％、強熱減量１６．９質量％の粉体を用いた。
【００２３】
この担体に、メタタングステン酸アンモニウムを含有する水溶液、および硝酸ニッケルを含有する水溶液を含浸し、乾燥後、５００℃で焼成して、触媒中にタングステンを１１．０質量％およびニッケルを１．０質量％含む触媒Ａを調製した。
【００２４】
〔触媒Ｂの調製〕
モルデナイト粉体および擬ベーマイト粉体を混合、混練して、シリンダー状に成形した後、乾燥し、６００℃で焼成することで担体を調製した。この担体は、乾燥担体基準で、モルデナイト７質量％およびアルミナ９３質量％からなり、直径１．４ｍｍのシリンダー形状であった。モルデナイト粉体としては、シリカ／アルミナモル比２１０、ゼオライト細孔長径７．０オングストロームの粉体を用いた。
この担体に、モリブデン酸アンモニウムを含有する水溶液、硝酸ニッケルを含有する水溶液、燐酸を含有する水溶液を含浸し、乾燥後、５００℃で焼成して、触媒中にモリブデンを１２質量％、ニッケルを４質量％およびリンを２．５質量％含む触媒Ｂを調製した。
【００２５】
〔水素化分解・異性化〕
触媒充填量１００ｍＬの固定床流通式反応装置に触媒Ａを充填し、予備硫化した後、後述のノルマルパラフィン原料を用い、圧力４ＭＰａ、水素／原料油供給比６６０ＮＬ／Ｌ、ＬＨＳＶ＝１．０ｈｒ−１、反応温度３３０℃、分解率８１質量％の反応条件で水素化分解・異性化反応を行い、得られた生成油から灯油留分を分留して、本発明の灯油Ａ（実施例１）を得た。
【００２６】
触媒Ａの代わりに触媒Ｂを用い、反応温度３６２℃、分解率４４質量％とする以外は、触媒Ａの場合と同様にして、灯油Ｂ（実施例２）を得た。
【００２７】
ノルマルパラフィン原料としては、ＳＭＤＳ（Ｓｈｅｌｌ Ｍｉｄｄｌｅ Ｄｉｓｔｉｌｌａｔｅ Ｓｙｎｔｈｅｓｉｓ）製ＳＸ−５０を用いた。これは、１５℃換算での密度０．８１ｇ／ｍＬ、初留点３１６℃、１０％留出温度３７９℃、９０％留出温度４５７℃、終点４８９℃であり、Ｆｉｓｃｈｅｒ−Ｔｒｏｐｓｃｈ法により合成されたものである。
【００２８】
得られた灯油Ａ、Ｂと比較例として示す市販灯油の性状を表１に示す。なお、性状測定について、密度はＪＩＳ Ｋ ２２４９、硫黄分はＪＩＳ Ｋ ２５４１、引火点はＪＩＳ Ｋ ２２６５、煙点はＪＩＳ Ｋ ２５３７、析出点はＪＩＳ Ｋ ２２７６、そして、蒸留性状はＪＩＳ Ｋ ２２５４によりそれぞれ測定した。芳香族分およびノルマルパラフィン含有量は、ガスクロマトグラフィにより分析した。
【００２９】
【表１】
上記表１から、灯油Ａ、Ｂは、硫黄分が１ｐｐｍ以下および芳香族分が１質量％以下と市販灯油より極めて低く、さらに、市販灯油と比べて、析出点が低く、低温特性に特に優れていることがわかる。
【００３１】
【発明の効果】
本発明による環境対応燃料油は、特定の性状を有し、特定の蒸留特性を有し、かつ、特定のノルマルパラフィン含有量分布を有するものであるから、特に硫黄分、芳香族分が極めて低く、と同時に、十分な低温性能を有するものであるから、本発明により、実用性能に優れ、かつ環境保全に優れた環境対応燃料油を提供することが可能となる。[0001]
TECHNICAL FIELD OF THE INVENTION
The present invention relates to an environment-friendly fuel oil such as kerosene and jet fuel oil with reduced impact on the environment, and a method for producing the same. The present invention relates to an environment-friendly fuel oil having low-temperature characteristics and a method for producing the same.
[0002]
[Prior art]
2. Description of the Related Art In recent years, there has been a demand for a reduction in sulfur content and aromatic content in fuel oils such as kerosene and jet fuel oils due to increasing environmental problems. For example, kerosene used for external combustion in stoves, boilers, and the like is also required to have a cleaner combustion gas by improving the airtightness of houses. Further, since the kerosene fraction is also used for jet fuel, it is necessary to maintain low-temperature performance for practical use.
[0003]
On the other hand, according to the Fischer-Tropsch method, a synthesis gas (composed of hydrogen and carbon monoxide) obtained by reforming natural gas contains carbon as a main component containing normal paraffins and containing almost no sulfur and aromatics. Hydrogen can be synthesized. The production of synthetic fuel oil using the synthesized hydrocarbon as a raw material has recently attracted attention (for example, see Patent Documents 1 to 7). However, although such a synthetic fuel oil has a sufficiently low sulfur content and aromatic content, its low-temperature performance is not sufficient as compared with petroleum-based kerosene.
[0004]
[Patent Document 1]
Japanese Patent Publication No. 11-513729 (Patent Document 2)
Japanese Unexamined Patent Publication No. Hei 11-513730 [Patent Document 3]
Japanese Patent Publication No. 2001-511207 [Patent Document 4]
Japanese Patent Publication No. 2001-522382 [Patent Document 5]
JP 2002-507635 A [Patent Document 6]
Japanese Patent Application Publication No. 2002-526636 [Patent Document 7]
JP-T-2002-526637 [0005]
[Problems to be solved by the invention]
The present invention solves such a problem, and has a sufficiently low sulfur content and aromatic content, and ensures a sufficiently low temperature performance for practical use, and has a sufficient performance as a base material to be mixed with jet fuel. It is an object of the present invention to provide an environmentally friendly fuel oil and a method for producing the same, which ensure the above.
[0006]
[Means for Solving the Problems]
The present inventors have paid attention to the heavy normal paraffin content of the product oil obtained by performing hydrocracking and isomerization using normal paraffin as a raw material, and by using a specific fraction thereof as a fuel oil, The inventors have found that such a problem can be solved, and have completed the present invention.
[0007]
The method for producing an environment-friendly fuel oil according to the present invention comprises the steps of: subjecting a normal paraffin raw material to a catalyst having a hydrogenation active metal supported on a carrier to perform hydrocracking and isomerization to obtain a product oil; and The method includes a step of fractionating the produced oil to obtain a fraction having a 95% distillation temperature of 260 ° C. or lower, and particularly preferably the normal paraffin raw material synthesized by the Fischer-Tropsch method. .
[0008]
The environment-friendly fuel oil according to the present invention has a density of 0.74 g / cm 3 to 0.78 g / cm 3 , a sulfur content of 10 mass ppm or less, a precipitation point of -50 ° C. or less, and normal paraffin having 14 or more carbon atoms. The content is 4.0% by mass or less, the content of normal paraffin having 11 or less carbon atoms is 0.5 to 15.0% by mass, the fraction at 220 ° C. or less is 50 to 95% by volume, and the aromatic content is 5%. % By mass or less. This environmentally friendly fuel oil is preferably used as a fuel for external combustion and jet fuel.
[0009]
BEST MODE FOR CARRYING OUT THE INVENTION
[Normal paraffin raw material]
The normal paraffin raw material used in the production method of the present invention is preferably one in which the light fraction of the raw oil is cut in advance by distillation or the like as necessary, since light normal paraffin has low reactivity of hydrocracking and isomerization, Specifically, it is preferable to use a raw material having an initial boiling point of 300 ° C. or higher, particularly 310 ° C. or higher, and a 10% distillation temperature of 350 ° C. or higher, particularly 360 ° C. or higher. In addition, since the heavy fraction of this normal paraffin raw material is converted into normal paraffin of the kerosene oil fraction by decomposition, it is preferable to cut a too heavy fraction by distillation or the like. In particular, the temperature is preferably 590 ° C or lower, and the 90% distillation temperature is preferably 560 ° C or lower, particularly preferably 550 ° C or lower. With these, the reaction rates of hydrocracking and isomerization and the yield of kerosene gas oil can be increased.
[0010]
The normal paraffin content in the normal paraffin raw material is preferably 85% by mass or more, particularly preferably 95% by mass or more. The impurity content is preferably 500 ppm or less, more preferably 50 ppm or less, and preferably 100 ppm or less, particularly 10 ppm or less of nitrogen.
[0011]
As the normal paraffin raw material, those having the above properties can be preferably used. Although there is no particular limitation on the type thereof, use of a slack wax obtained from a petroleum refining process, for example, a solvent dewaxing process, which is one of lubricating oil manufacturing processes, or a synthetic wax synthesized by the Fischer-Tropsch method is used. Can be. Although there are various kinds of these waxes, they may be used alone or as a mixture of two or more kinds, or a mixture of slack wax and synthetic wax may be used. In particular, it is preferable to use a synthetic wax by the Fischer-Tropsch method alone. The Fischer-Tropsch method is a method in which carbon monoxide and hydrogen are reacted using a catalyst to synthesize mainly normal paraffin and, to a lesser extent, olefins and alcohols.
[0012]
〔catalyst〕
The catalyst used in the method for producing a fuel oil of the present invention is one in which a hydrogenation active metal is supported on a carrier. For example, a catalyst disclosed in JP-T-2002-523231 or JP-A-290147 is preferably used. In the production method of the present invention, a carrier that can be preferably used is a carrier composed of an inorganic porous oxide containing silica alumina. It is preferable that silica alumina is formed into a carrier using alumina as a binder. Mordenite is preferred as the crystalline silica alumina. Amorphous or crystalline silica alumina can be used, but amorphous is preferable. The range of the silica / alumina molar ratio of the amorphous silica alumina is preferably 3 to 8. It is preferable that the carrier does not contain any other than oxides of aluminum and silicon, but magnesia, zirconia, boria, calcia, and the like can also be contained.
[0013]
The supported hydrogenation active metal is not particularly limited, but preferably contains one or more metal components selected from Group 6, Group 9, and Group 10 of the periodic table. Examples of the metal selected from Group 6, Group 9, and Group 10 include molybdenum, tungsten, cobalt, rhodium, iridium, nickel, platinum, and palladium, and in particular, non-noble metals such as molybdenum, tungsten, cobalt, and nickel. It is preferably used as a hydrogenation active component. It is preferable to add and carry the hydrogenation-active metal such that the total amount of the metal elements is 0.05 to 35% by mass, particularly 0.1 to 30% by mass.
[0014]
(Hydrolysis and isomerization)
In the hydrocracking and isomerization used in the production method of the present invention, the reaction temperature is 300 to 400 ° C., particularly 320 to 350 ° C., the hydrogen pressure is 1 to 20 MPa, particularly 3 to 9 MPa, and the hydrogen / oil ratio is 100 to 100. The reaction is preferably performed under the reaction conditions of 2000 NL / L, particularly 300 to 1500 NL / L, and a liquid hourly space velocity (LHSV) of 0.5 to 5 hr -1 .
[0015]
When the ratio of components having a temperature of 360 ° C. or more in the normal paraffin raw material to components having a temperature of less than 360 ° C. is defined as the decomposition rate, in order to increase the isomerization rate and the yield of the kerosene fraction, the decomposition rate is 50 to 85. % By mass is preferred. If the decomposition rate exceeds 85% by mass, the kerosene fraction will undergo secondary decomposition.
[0016]
(Kerosene fraction)
In the production method of the present invention, a 10% distillation temperature of 160 ° C. or more, preferably 170 ° C. or more, and a 95% distillation temperature of 260 ° C. or less, preferably 250 ° C. or less, from the oil produced by the hydrocracking and isomerization steps. Fraction (hereinafter also referred to as kerosene fraction).
[0017]
[Formulation]
In the production method of the present invention, the above kerosene fraction as it is as kerosene, or as a jet fuel by mixing with another base material, as a fuel for external combustion such as a stove or a boiler, and as a base material for those fuels Can be used. Examples of other base materials include base materials for blending kerosene produced by refining crude oil, semi-finished products, and intermediate products thereof. As an additive to the fuel, a known fuel additive such as a low-temperature fluidity improver, an antioxidant, a metal deactivator, and a corrosion inhibitor may be added. Usually, when fuel oil is traded as kerosene, a light oil discriminating agent is added.
[0018]
[Environment-friendly fuel oil]
The environment-friendly fuel oil according to the present invention has a density of 0.74 g / cm 3 to 0.78 g / cm 3 , a sulfur content of 10 mass ppm or less, a precipitation point of -50 ° C. or less, and a normal paraffin content of 14 or more carbon atoms. Is 4.0% by mass or less, the content of normal paraffins having 11 or less carbon atoms is 0.5 to 15.0% by mass, the fraction at 220 ° C. or less is 50 to 95% by volume, and the aromatic component is 5% by mass. It is as follows.
[0019]
The sulfur content is preferably 5 mass ppm or less, particularly preferably 1 mass ppm or less. The precipitation point is preferably -55 ° C or less, particularly preferably -65 ° C or less. The aromatic content is preferably 3% by mass or less, particularly preferably 1% by mass or less.
[0020]
As the distillation properties of the environment-friendly fuel oil according to the present invention, the 10% distillation temperature is preferably 160 ° C. or higher, particularly 175 ° C. or higher, and the 95% distilling temperature is 220 ° C. to 260 ° C., particularly preferably 220 ° C. to 250 ° C. . The fraction at 220 ° C. or lower is preferably 60 to 90% by volume.
[0021]
【Example】
Hereinafter, the present invention will be described in detail with reference to examples. However, the present invention is not construed as being limited by these examples.
[0022]
[Preparation of Catalyst A]
The silica-alumina powder and the pseudo-boehmite powder were mixed and kneaded, formed into a cylinder, dried, and fired at 600 ° C. to prepare a carrier. This carrier was composed of 80% by mass of silica alumina and 20% by mass of alumina on a dry carrier basis, and had a cylindrical shape with a diameter of about 1.6 mm. As the silica-alumina powder, a powder having a silica / alumina molar ratio of 4.4, an aggregate particle diameter of 1 to 10 μm, 94.4% by mass, and a loss on ignition of 16.9% by mass was used.
[0023]
The carrier is impregnated with an aqueous solution containing ammonium metatungstate and an aqueous solution containing nickel nitrate, dried, and calcined at 500 ° C. to make the catalyst contain 11.0% by mass of tungsten and 1.0% by mass of nickel. A catalyst A containing the catalyst was prepared.
[0024]
[Preparation of catalyst B]
The carrier was prepared by mixing and kneading the mordenite powder and the pseudo-boehmite powder, forming the mixture into a cylinder, drying, and firing at 600 ° C. This carrier was composed of 7% by mass of mordenite and 93% by mass of alumina on a dry carrier basis, and had a cylindrical shape with a diameter of 1.4 mm. As the mordenite powder, a powder having a silica / alumina molar ratio of 210 and a zeolite pore major axis of 7.0 angstroms was used.
The carrier is impregnated with an aqueous solution containing ammonium molybdate, an aqueous solution containing nickel nitrate, and an aqueous solution containing phosphoric acid, dried and calcined at 500 ° C., so that the catalyst contains 12% by mass of molybdenum and 4% of nickel in the catalyst. Catalyst B containing 2.5% by weight of phosphorus and 2.5% by weight of phosphorus was prepared.
[0025]
(Hydrolysis / isomerization)
After the catalyst A was charged into a fixed-bed flow-type reactor having a catalyst loading of 100 mL and preliminarily sulfurized, the pressure was 4 MPa, a hydrogen / feed oil supply ratio was 660 NL / L, LHSV = 1.0 hr − 1 , a hydrocracking / isomerization reaction was carried out under the reaction conditions of a reaction temperature of 330 ° C. and a decomposition rate of 81% by mass, and a kerosene fraction was fractionated from the obtained product oil to obtain kerosene A of the present invention (Example 1). ) Got.
[0026]
Kerosene B (Example 2) was obtained in the same manner as in the case of the catalyst A, except that the catalyst B was used instead of the catalyst A, and the reaction temperature was 362 ° C. and the decomposition rate was 44% by mass.
[0027]
As a normal paraffin raw material, SX-50 manufactured by Shell Middle Distillate Synthesis (SMDS) was used. This has a density of 0.81 g / mL in terms of 15 ° C., an initial distillation point of 316 ° C., a 10% distillation temperature of 379 ° C., a 90% distillation temperature of 457 ° C., and an end point of 489 ° C., and is synthesized by the Fischer-Tropsch method. It is something.
[0028]
Table 1 shows the properties of the obtained kerosene A and B and commercial kerosene shown as a comparative example. Regarding the property measurement, the density was JIS K 2249, the sulfur content was JIS K 2541, the flash point was JIS K 2265, the smoke point was JIS K 2537, the precipitation point was JIS K 2276, and the distillation property was JIS K 2254. It was measured. The aromatic content and normal paraffin content were analyzed by gas chromatography.
[0029]
[Table 1]
From Table 1 above, kerosene A and B have a sulfur content of 1 ppm or less and an aromatic content of 1 mass% or less, which is extremely lower than that of commercial kerosene, and have a lower precipitation point and are particularly excellent in low-temperature properties as compared with commercial kerosene. You can see that it is.
[0031]
【The invention's effect】
The environment-friendly fuel oil according to the present invention has specific properties, has specific distillation characteristics, and has a specific normal paraffin content distribution, so that the sulfur content and the aromatic content are particularly low. At the same time, since the fuel oil has a sufficient low-temperature performance, the present invention makes it possible to provide an environment-friendly fuel oil having excellent practical performance and excellent environmental protection.
Claims (5)
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