JP3599265B2 - Hydrorefining method of gas oil fraction - Google Patents
Hydrorefining method of gas oil fraction Download PDFInfo
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- JP3599265B2 JP3599265B2 JP21213998A JP21213998A JP3599265B2 JP 3599265 B2 JP3599265 B2 JP 3599265B2 JP 21213998 A JP21213998 A JP 21213998A JP 21213998 A JP21213998 A JP 21213998A JP 3599265 B2 JP3599265 B2 JP 3599265B2
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Description
【０００１】
【発明の属する技術分野】
本発明は、直留軽油留分、接触分解軽油、熱分解軽油などの軽油留分を硫黄分１５０ｐｐｍ以下に深度脱硫する水素化精製方法に関する。
【０００２】
【従来の技術】
従来、軽油留分の水素化精製は、アルミナ、シリカ−アルミナなどで構成される多孔性の無機担体に水素化能を有する活性金属であるモリブデン、タングステン、ニッケル、コバルトなどを担持した触媒を水素雰囲気下において軽油留分と接触させることで行われ、このような水素化精製により、軽油留分中からヘテロ元素、すなわち硫黄、窒素などが除去される。
【０００３】
最近、環境保護の観点から軽油中に含まれる硫黄分を５００ｐｐｍ以下に低減させる、いわゆる軽油深度脱硫が要請されている。または、高度な脱窒素処理が要請され、このための精製プロセスの確立が急がれれている。上記の軽油深度脱硫を行うプロセスとして、（１）２段水素添加方法、（２）後段反応塔において原料油と水素を交流接触させる方法、（３）前段反応塔の生成油中に含まれている硫化水素を一旦気液分離槽で抜出し、その後、後段反応塔へフィードする硫化水素濃度の低減方法などが考案されている。
【０００４】
【発明が解決しようとする課題】
環境保護の高まりから軽油中の硫黄分をさらに低減し、１５０ｐｐｍ以下とするような深度脱硫が望まれている。しかし、従来の軽油深度脱硫では、このような低硫黄濃度の実現には限界があり、複雑な精製装置を新たに設けることや高度な運転技術を必要とする。また、特殊な精製装置を用いるために製油所の運転上のフレキシビリティーが低下してしまうという問題があった。
【０００５】
本発明は、上記課題を解決するもので、本発明の目的は、簡単な、従来と同等の精製装置により高度な脱硫・脱窒素が可能な水素化精製方法を提供し、また、装置運転上の制限を緩和することで精製装置のフレキシビリティーを確保することが可能な軽油留分の水素化精製方法を提供することにある。
【０００６】
【課題を解決するための手段】
本発明者は、軽油留分を水素化精製する際の運転条件を詳細に検討した結果、液空間速度、水素／油比、および、水素圧力が所定の条件を満たす場合に、高度な精製処理が可能となることを見いだし、本発明を完成したものである。
【０００７】
本発明による軽油留分の水素化精製方法は、軽油留分と水素を水素化精製用触媒に接触させ、硫黄分を２５ｐｐｍ以下、窒素分を１ｐｐｍ以下、全アロマ分が２０重量％以下で、かつ、３環以上のアロマ分が０．２重量％以下に水素化精製する方法において、軽油留分の９０％留出温度が３３０〜３７０℃であり、水素化精製用触媒が多孔性の無機担体に、金属元素換算で５〜２０重量％のモリブデンと、金属元素換算で１〜１０重量％のコバルトと、りん元素換算で０．１〜８重量％のりんが担持された触媒であり、水素化精製時の液空間速度を０．５〜１．７ｈｒ−１（０．５〜１．７／時間）とし、水素／油比を２５０〜４５０Ｌ／Ｌとし、水素圧力を４５〜９０ｋｇ／ｃｍ２とし、反応温度を３００〜３８０℃とし、かつ、水素／油比を液空間速度で割った値が２５０ｈｒ（２５０時間）以上とするものである。
【０００８】
特には、軽油留分の１０％留出温度が２４０〜２８０℃、５０％留出温度が２８０〜３２０℃であり、かつ、水素／油比を液空間速度で割った値が２５０ｈｒ以上であることが好ましい。
【０００９】
【発明の実施の形態】
［軽油留分］ 本発明の原料油となる軽油留分は、直留軽油留分を用いることが好ましく、直留軽油留分単独でもよいが、軽質熱分解油軽油や軽質接触分解軽油を直留軽油留分に混合した混合軽油留分でもよい。この直留軽油留分とは、原油を常圧蒸留して得られる、おおよそ１０％留出点が２４０〜２８０℃、５０％留出点が２８０〜３２０℃、９０％留出点が３３０〜３７０℃からなっているものである。なお、沸点及び留出点は特に断らない限り、ＪＩＳ Ｋ ２２５４「燃料油蒸留試験方法」による値である。
【００１０】
熱分解油とは、重質油留分に熱を加えて、ラジカル反応を主体にした反応により得られた軽質留分油で、例えば、ディレードコーキング法、ビスブレーキング法或いはフルードコーキング法等により得られる留分をいう。これらの留分は得られる全留分を熱分解油としてもちいてもよいが、留出温度が１５０〜５２０℃の範囲内にある留分を用いることが好適である。
【００１１】
接触分解油とは、中間留分や重質留分、特には減圧蒸留留分等をゼオライト系触媒と接触分解する際に得られる留分、特に高オクタン価ガソリン製造を目的とした流動接触分解装置において副生する分解軽油留分である。この留分は、一般に、沸点が相対的に低い軽質接触分解油と沸点が相対的に高い重質接触分解油とが別々に採取されている。本発明においては、これらの留分のいずれをも用いることができるが、前者の軽質接触分解油、いわゆるライトサイクルオイル（ＬＣＯ）を用いることが好ましい。このＬＣＯは、一般に、１０％留出点が２２０〜２５０℃、５０％留出点が２６０〜２９０℃、９０％留出点が３１０〜３５５℃の範囲内にある。また、重質接触分解油、いわゆるヘビーサイクルオイル（ＨＣＯ）は、１０％留出点が２８０〜３４０℃、５０％留出点が３９０〜４２０℃、９０％留出点が４５０℃以上にある。
【００１２】
［水素化精製用触媒］本発明に用いる水素化精製用触媒としては、アルミナ担体にモリブデンを金属元素換算で約５〜２０重量％と、コバルトを金属元素換算で１〜１０重量％担持させ、更に燐をリン元素換算で０．１〜８重量％担持した触媒を用いることが好ましい。
【００１３】
反応塔への触媒の充填は、触媒層内における効率のよい気液接触を確保するため、触媒充填機を用いるとよい。この充填機の使用によって充填時の反応塔内における触媒層面はほぼ水平となり、触媒層内における流体の偏流やこのような偏流に起因すると考えられているホットスポットの発生を防止できるだけでなく、反応塔に密に触媒が充填されるために触媒活性や触媒寿命に好ましい影響を与える。触媒層内の水平方向面内の複数ヶ所で測定した温度差が１０℃以下、特には５℃以下であることが好ましい。
【００１４】
［水素化精製］ 本発明による水素化精製条件は、液空間速度を０．５〜１．７ｈｒ−１とし、水素／油比を２５０〜４５０Ｌ／Ｌとし、水素圧力を４５〜９０ｋｇ／ｃｍ２とし、かつ、水素／油比を液空間速度で割った値が２００ｈｒ以上である。さらには、水素／油比を液空間速度で割った値が２５０ｈｒ以上であることが好ましい。反応温度は、３００〜３８０℃が用いられる。
【００１５】
本発明による水素化精製条件では、原料油中に含まれる硫黄化合物の水素化脱硫反応やアロマ分への水素添加反応などの進行に伴う発熱量が大きく、この発熱によって反応器内の触媒層が急激な温度上昇にさらされる可能性が大きい。この温度上昇は、多環アロマの生成やそれに起因する生成油の色相悪化、触媒活性の低下や触媒寿命の短命化などの原因となる。そこで本発明では、水素化精製反応装置として通常水素化精製に用いられる反応器を用いることが出来るが、上記の様な温度上昇を効果的に防止するために、反応器内の触媒層を必要に応じて複数の床に分割し、かつ必要に応じて各床の間に水素を供給できることが好ましい。この時分割した各触媒床における入口と出口の温度差は５０℃以下、特には２５℃以下にすることが好ましい。
【００１６】
本発明により水素化精製された軽油留分は、硫黄分が２５ｐｐｍ以下となる。
特には、水素／油比を液空間速度で割った値が２５０ｈｒ以上の条件下では、硫黄分が５０ｐｐｍ以下であり、全アロマ分が２０重量％以下で、かつ、２環以上のアロマ分が１重量％以下とすることが可能である。また、通常窒素分は、１ｐｐｍ以下とすることができ、３環以上のアロマ分が０．２重量％以下、特には０．１重量％以下とすることができる。
【００１７】
【発明の効果】
本発明による水素化精製方法は、液空間速度、水素／油比、水素圧力が所定の条件を満たすものであり、複雑な精製装置を用いることなく、硫黄分・窒素分の十分な低減のみでなく、アロマ分、特には２環以上のアロマ分をも低減することができる。したがって、環境に配慮された自動車用軽油などの基材に用いられる軽油留分を工業的に製造することが可能となる。
【００１８】
【実施例】
本発明を実施例により詳しく説明する。
【００１９】
原料油として中東系直留軽油留分を、水素化精製触媒として市販触媒（オリエントキャタリスト製、ＨＯＰ４６３）を用い、表１の条件で反応温度、水素圧力、液空間速度、水素／油比を変えて水素化精製を行った。用いた中東系直留軽油留分の性状は、比重０．８５５８、硫黄分１．４７重量％、窒素分１３８重量ｐｐｍ、１０％留出温度２７５℃、５０％留出温度３０７℃、９０％留出温度３５５℃である。用いた水素化精製触媒は、アルミナなどからなる担体に触媒に対する重量％としてＭｏを元素として１０ｗｔ％、Ｃｏを３ｗｔ％、Ｐを２ｗｔ％担持したものである。
【００２０】
水素化精製した軽油留分について、硫黄分をＪＩＳ Ｋ ２５４１ 電流滴定酸化法により、窒素分をＪＩＳ Ｋ ２６０９ 化学発光法により、また、アロマ分を石油学会規格に準拠してそれぞれ測定し、その結果を表１に併せて示す。
【００２１】
【表１】
評価結果から、水素圧力が４５ｋｇ／ｃｍ２以上であり、水素／油比を液空間速度で割った値（［水素／油比］／［液空間速度］）が２５０ｈｒ以上である実験例１〜２において、硫黄分が２５ｐｐｍ以下で、アロマ分１９％以下となることが分かる。[0001]
TECHNICAL FIELD OF THE INVENTION
The present invention relates to a hydrorefining method for deep-desulfurizing a gas oil fraction such as a straight gas oil fraction, a catalytic cracking gas oil, and a pyrolysis gas oil to a sulfur content of 150 ppm or less.
[0002]
[Prior art]
Conventionally, hydrorefining of a gas oil fraction has been carried out by using a catalyst in which molybdenum, tungsten, nickel, cobalt, etc., which are active metals having hydrogenation ability, are supported on a porous inorganic carrier composed of alumina, silica-alumina, etc. It is carried out by bringing the gasoline into contact with a gas oil fraction under an atmosphere, and such hydrorefining removes hetero elements, that is, sulfur, nitrogen, and the like from the gas oil fraction.
[0003]
In recent years, from the viewpoint of environmental protection, there has been a demand for so-called gas oil deep desulfurization in which the sulfur content in gas oil is reduced to 500 ppm or less. Alternatively, advanced denitrification treatment is required, and the establishment of a purification process for this purpose is urgently required. As the process for performing the above-mentioned gas oil deep desulfurization, (1) a two-stage hydrogenation method, (2) a method in which a feed oil and hydrogen are brought into AC contact in a latter-stage reaction tower, and (3) a process oil contained in the oil produced in the former-stage reaction tower A method for reducing the concentration of hydrogen sulfide, which is once extracted from a gas-liquid separation tank and then fed to a subsequent reaction tower, has been devised.
[0004]
[Problems to be solved by the invention]
Due to increasing environmental protection, there is a demand for deep desulfurization in which the sulfur content in light oil is further reduced to 150 ppm or less. However, in the conventional deep oil desulfurization, there is a limit in realizing such a low sulfur concentration, and it is necessary to newly install a complicated refining device and to use advanced operation technology. In addition, there is a problem that the operational flexibility of the refinery is reduced due to the use of a special refining device.
[0005]
An object of the present invention is to solve the above-mentioned problems, and an object of the present invention is to provide a hydrorefining method capable of performing a high degree of desulfurization and denitrification by a simple and equivalent purifying apparatus. It is an object of the present invention to provide a gas oil fraction hydrorefining method capable of securing the flexibility of a refining device by relaxing the restrictions of the above.
[0006]
[Means for Solving the Problems]
The present inventor has studied the operating conditions for hydrorefining a gas oil fraction in detail, and found that, when the liquid hourly space velocity, the hydrogen / oil ratio, and the hydrogen pressure satisfy the predetermined conditions, advanced purification treatment is performed. Have been found possible, and the present invention has been completed.
[0007]
The hydrorefining method of a gas oil fraction according to the present invention comprises contacting a gas oil fraction and hydrogen with a hydrorefining catalyst, the sulfur content is 25 ppm or less, the nitrogen content is 1 ppm or less, the total aroma content is 20 wt% or less, In the method for hydrorefining the aroma content of three or more rings to 0.2% by weight or less , the 90% distillation temperature of the gas oil fraction is from 330 to 370 ° C, and the hydrorefining catalyst is a porous inorganic material. A catalyst in which 5 to 20% by weight of molybdenum in terms of a metal element, 1 to 10% by weight of cobalt in terms of a metal element, and 0.1 to 8% by weight of phosphorus in terms of a phosphorus element are supported on a carrier; The liquid hourly space velocity during hydrorefining is 0.5 to 1.7 hr -1 (0.5 to 1.7 / hour), the hydrogen / oil ratio is 250 to 450 L / L, and the hydrogen pressure is 45 to 90 kg / hour. cm 2, and the reaction temperature was 300 to 380 ° C., and a hydrogen / Value obtained by dividing the ratio in the liquid space velocity is to a 250 hr (250 hours) or more.
[0008]
In particular, the 10% distillation temperature of the gas oil fraction is 240 to 280 ° C, the 50% distillation temperature is 280 to 320 ° C, and the value obtained by dividing the hydrogen / oil ratio by the liquid hourly space velocity is 250 hours or more . Is preferred.
[0009]
BEST MODE FOR CARRYING OUT THE INVENTION
[Light Oil Fraction] As the light oil fraction to be used as the feed oil of the present invention, it is preferable to use a straight gas oil fraction, and a straight gas oil fraction may be used alone. A mixed gas oil fraction mixed with the gas oil fraction may be used. The straight-run gas oil fraction is obtained by distilling crude oil at normal pressure, and has an approximate 10% distillation point of 240 to 280 ° C, a 50% distillation point of 280 to 320 ° C, and a 90% distillation point of 330 to 330 ° C. It consists of 370 ° C. Unless otherwise specified, the boiling point and the distillation point are values according to JIS K 2254 “Test method for distillation of fuel oil”.
[0010]
Pyrolysis oil is a light distillate oil obtained by adding heat to a heavy oil fraction and reacting mainly by a radical reaction, for example, by a delayed coking method, a visbreaking method or a fluid coking method. Refers to the fraction obtained. For these fractions, the entire fraction obtained may be used as the pyrolysis oil, but it is preferable to use a fraction having a distillation temperature in the range of 150 to 520 ° C.
[0011]
Catalytic cracking oil refers to a fraction obtained when catalytically cracking an intermediate fraction or a heavy fraction, particularly a vacuum distillation fraction, etc., with a zeolite-based catalyst, particularly a fluid catalytic cracking apparatus for producing high octane gasoline. Is a cracked gas oil fraction by-produced in the above. In this fraction, generally, a light catalytic cracking oil having a relatively low boiling point and a heavy catalytic cracking oil having a relatively high boiling point are separately collected. In the present invention, any of these fractions can be used, but it is preferable to use the former light catalytic cracking oil, so-called light cycle oil (LCO). The LCO generally has a 10% distillation point in the range of 220-250 ° C, a 50% distillation point in the range of 260-290 ° C, and a 90% distillation point in the range of 310-355 ° C. Heavy catalytic cracking oil, so-called heavy cycle oil (HCO), has a 10% distillation point of 280 to 340 ° C, a 50% distillation point of 390 to 420 ° C, and a 90% distillation point of 450 ° C or more.
[0012]
[Hydrorefining Catalyst] As the hydrorefining catalyst used in the present invention, about 5 to 20% by weight of molybdenum in terms of a metal element and 1 to 10% by weight of cobalt in terms of a metal element are supported on an alumina carrier. Further, it is preferable to use a catalyst supporting 0.1 to 8% by weight of phosphorus in terms of phosphorus element.
[0013]
For filling the reaction tower with the catalyst, a catalyst filling machine may be used to ensure efficient gas-liquid contact in the catalyst layer. By using this filling machine, the surface of the catalyst layer in the reaction tower at the time of filling becomes almost horizontal, which not only prevents the drift of the fluid in the catalyst layer and the generation of hot spots thought to be caused by such drift, but also the reaction Since the catalyst is densely packed in the column, it has a favorable effect on the catalyst activity and catalyst life. The temperature difference measured at a plurality of points in the horizontal plane in the catalyst layer is preferably 10 ° C. or less, particularly preferably 5 ° C. or less.
[0014]
[Hydrorefining] The hydrorefining conditions of the present invention are as follows: liquid hourly space velocity is 0.5 to 1.7 hr -1 , hydrogen / oil ratio is 250 to 450 L / L, and hydrogen pressure is 45 to 90 kg / cm 2. And the value obtained by dividing the hydrogen / oil ratio by the liquid hourly space velocity is 200 hours or more. Further, the value obtained by dividing the hydrogen / oil ratio by the liquid hourly space velocity is preferably 250 hours or more. A reaction temperature of 300 to 380 ° C is used.
[0015]
Under the hydrorefining conditions according to the present invention, the calorific value accompanying the progress of the hydrodesulfurization reaction of the sulfur compound contained in the feedstock oil and the hydrogenation reaction to the aroma component is large, and this heat generation causes the catalyst layer in the reactor to become large. It is likely to be exposed to sudden temperature rise. This increase in temperature causes the formation of polycyclic aroma and the resulting hue deterioration of the resulting oil, a decrease in catalytic activity and a shortened life of the catalyst. Therefore, in the present invention, a reactor usually used for hydrorefining can be used as a hydrorefining reactor, but in order to effectively prevent the above-mentioned temperature rise, a catalyst layer in the reactor is required. Is preferably divided into a plurality of beds, and hydrogen can be supplied between the beds as needed. The temperature difference between the inlet and the outlet of each time-divided catalyst bed is preferably 50 ° C. or less, particularly preferably 25 ° C. or less.
[0016]
The gas oil fraction hydrorefined according to the present invention has a sulfur content of 25 ppm or less.
In particular, under the condition that the value obtained by dividing the hydrogen / oil ratio by the liquid hourly space velocity is 250 hr or more, the sulfur content is 50 ppm or less, the total aroma content is 20% by weight or less, and the aroma content of two or more rings is It can be less than 1% by weight. Further, the nitrogen content can be usually 1 ppm or less, and the aroma content of three or more rings can be 0.2% by weight or less, particularly 0.1% by weight or less.
[0017]
【The invention's effect】
In the hydrorefining method according to the present invention, the liquid hourly space velocity, the hydrogen / oil ratio, and the hydrogen pressure satisfy predetermined conditions, and only a sufficient reduction of the sulfur content and the nitrogen content without using a complicated purification device. In addition, the aroma content, particularly the aroma content of two or more rings can be reduced. Therefore, it becomes possible to industrially produce a light oil fraction used for base materials such as light oil for automobiles, which is environmentally friendly.
[0018]
【Example】
The present invention will be described in more detail with reference to examples.
[0019]
The reaction temperature, hydrogen pressure, liquid space velocity, and hydrogen / oil ratio were determined under the conditions shown in Table 1 using a Middle Eastern straight gas oil fraction as a feed oil and a commercially available catalyst (HOP463 manufactured by Orient Catalyst) as a hydrorefining catalyst. Hydrorefining was carried out in a different manner. The properties of the used Middle Eastern straight-run gas oil fraction are specific gravity 0.8558, sulfur content 1.47% by weight, nitrogen content 138 weight ppm, 10% distillation temperature 275 ° C, 50% distillation temperature 307 ° C, 90% The distillation temperature is 355 ° C. The hydrorefining catalyst used is such that 10 wt% of Mo as an element, 3 wt% of Co, and 2 wt% of P are supported on a carrier made of alumina or the like as a weight% with respect to the catalyst.
[0020]
For the hydrorefined gas oil fraction, the sulfur content was measured according to JIS K 2541 amperometric oxidation method, the nitrogen content was measured according to JIS K 2609 chemiluminescence method, and the aroma content was measured according to the Japan Petroleum Institute standard. Are also shown in Table 1.
[0021]
[Table 1]
From the evaluation results, Experimental Example 1 in which the hydrogen pressure was 45 kg / cm 2 or more, and the value obtained by dividing the hydrogen / oil ratio by the liquid hourly space velocity ([hydrogen / oil ratio] / [liquid hourly space velocity]) was 250 hr or more. 2 shows that the sulfur content is 25 ppm or less and the aroma content is 19% or less.
Claims (2)
軽油留分の９０％留出温度が３３０〜３７０℃であり、
水素化精製用触媒が多孔性の無機担体に、金属元素換算で５〜２０重量％のモリブデンと、金属元素換算で１〜１０重量％のコバルトと、りん元素換算で０．１〜８重量％のりんが担持された触媒であり、
水素化精製時の液空間速度を０．５〜１．７ｈｒ−１とし、水素／油比を２５０〜４５０Ｌ／Ｌとし、水素圧力を４５〜９０ｋｇ／ｃｍ２とし、反応温度を３００〜３８０℃とし、かつ、水素／油比を液空間速度で割った値が２５０ｈｒ以上である軽油留分の水素化精製方法。The gas oil fraction and hydrogen are brought into contact with a hydrorefining catalyst, the sulfur content is 25 ppm or less, the nitrogen content is 1 ppm or less, the total aroma content is 20% by weight or less, and the aroma content of three or more rings is 0.2% by weight. % Or less in the method of hydrorefining,
90% distillation temperature of gas oil fraction is 330-370 ° C,
The catalyst for hydrorefining is formed on a porous inorganic carrier by adding 5 to 20% by weight of molybdenum in terms of a metal element, 1 to 10% by weight of cobalt in terms of a metal element, and 0.1 to 8% by weight in terms of a phosphorus element. Phosphorus supported catalyst,
The liquid hourly space velocity during hydrorefining is 0.5 to 1.7 hr -1 , the hydrogen / oil ratio is 250 to 450 L / L, the hydrogen pressure is 45 to 90 kg / cm 2 , and the reaction temperature is 300 to 380 ° C. Wherein the value obtained by dividing the hydrogen / oil ratio by the liquid hourly space velocity is 250 hr or more.
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