JPS61120896A - Preparation of naphthenic lube base oil - Google Patents
Preparation of naphthenic lube base oilInfo
- Publication number
- JPS61120896A JPS61120896A JP24228484A JP24228484A JPS61120896A JP S61120896 A JPS61120896 A JP S61120896A JP 24228484 A JP24228484 A JP 24228484A JP 24228484 A JP24228484 A JP 24228484A JP S61120896 A JPS61120896 A JP S61120896A
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- Japan
- Prior art keywords
- lubricating base
- oil
- base oil
- coal
- producing
- 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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- Production Of Liquid Hydrocarbon Mixture For Refining Petroleum (AREA)
Abstract
Description
【発明の詳細な説明】
〔産業上の利用分野〕
この発明は、コールタール、コールタールピッチ、石炭
液化油又は石川液化ピッチを原料としてナフテン系潤滑
基油を製造する方法に関する。DETAILED DESCRIPTION OF THE INVENTION [Industrial Application Field] The present invention relates to a method for producing naphthenic lubricating base oil using coal tar, coal tar pitch, coal liquefied oil or Ishikawa liquefied pitch as a raw material.
ナフテン系潤滑基油は、ワックス含有侶の少ないナフテ
ン系の特殊な原油を原料にし、これを常圧蒸溜して軽質
弁を除去し、得られた常圧蒸溜残清を減圧蒸溜して軽質
潤滑油留分、中ｖ１潤滑油留分、及び減圧蒸溜残漬（ア
スファルト）に分１Ｊ、減圧蒸溜残渣を除く各留分につ
いてＩｉａ酸処理、白土処岸を行うか、あるいは、溶剤
抽出精製を行い、さらに特別へ品質の油が要求される場
合等、用途により水素添加処理等の精製を行うことによ
り製造されている。Naphthenic lubricating base oil is made from a special naphthenic crude oil with low wax content, which is distilled at normal pressure to remove light valves, and the resulting atmospheric distillation residue is distilled under reduced pressure to provide light lubricating oil. Each fraction except the oil fraction, medium V1 lubricating oil fraction, and vacuum distillation residue (asphalt) is subjected to IIA acid treatment, white clay treatment, or solvent extraction and purification. In cases where even higher quality oil is required, it is manufactured by refining such as hydrogenation depending on the application.
これらのナフテン系潤滑基油は、パラフィン系潤滑基油
に比較して、粘度指数が低く、低温流動性に優れている
ばかりでなく、ナフテン環が多いために溶解性にとみ、
劣化析出カーボンが軟らかい等の特徴を有する。このた
め、これらのナフテン系ｒ！ｌ滑基油は、絶縁油、ケー
ブル油、冷凍機油、コンプレッサー油あるいは低湿潤滑
油等、比較的特殊な用途にその需要が多い。These naphthenic lubricating base oils not only have a lower viscosity index and better low-temperature fluidity than paraffinic lubricating base oils, but also have high solubility due to their large number of naphthene rings.
Characteristics include that the deteriorated precipitated carbon is soft. For this reason, these naphthenic r! Lubricating oils are in high demand for relatively special uses such as insulating oils, cable oils, refrigeration oils, compressor oils, and low-humidity lubricating oils.
しかしながら、ナフテン系の特殊な原油は世界的にも枯
渇する傾向にあり、桟が国においてもこのナフテン系の
特殊な原油を確保することが次第に困難になり、ナフテ
ン系潤滑基油を安定に供給し得なくなりつつある。However, as special naphthenic crude oil tends to be depleted worldwide, it is becoming increasingly difficult for countries to secure this special naphthenic crude oil, resulting in a stable supply of naphthenic lubricating base oil. It is becoming impossible to do so.
このような状況に対処すべく、ナフテン系潤滑基油の代
替品を開発する試みも種々検討されており、例えば、溶
剤精製法によるパラフィン系潤滑基油製造の際に得られ
た芳香族成分６０重１％以上を含むエキストラクトを特
殊な触媒の存在下に高温高圧で水素添加処理してナフテ
ン系潤滑基油をＷＩＪ造づる方法（特公昭５３−１０．
０８２号公報及び特公昭５３−４７．２４．３号公報）
や、パラフィン系や混合系の原油から得られた潤滑油粗
製原料を第１の抽出帯域中において芳香族成分等に対し
優先的溶解力を有する抽出溶剤で処理しすることにより
第１のラフィネート及び第１のエキストラクトを得、次
いで第２抽出帯域中で」二足第１のラフイネ−１−を芳
香族成分に対し優先的溶解力を有する抽出溶剤で処理し
て第２のラフイネ−Ｉ・及び第２のエキストラクトを得
、上記第２のエキス１〜ラク１〜を精製処理してナフテ
ン系潤滑基油を製造する方法（特公昭５４−１０２，８
２３号公報及び特公昭５５−５５，４３０号公報）が提
案されている。In order to deal with this situation, various attempts have been made to develop substitutes for naphthenic lubricating base oils. A method for producing WIJ naphthenic lubricating base oil by hydrogenating an extract containing 1% or more by weight at high temperature and pressure in the presence of a special catalyst (Japanese Patent Publication No. 53-10.
082 Publication and Special Publication No. 53-47.24.3)
The first raffinate and A first extract is obtained, and then in a second extraction zone the first Rough Ine-1 is treated with an extraction solvent having preferential solubility for aromatic components to obtain a second Rough Ine-I. A method for producing a naphthenic lubricating base oil by obtaining a second extract and refining the second extract 1 to Raku 1 (Japanese Patent Publication No. 54-102, 8
No. 23 and Japanese Patent Publication No. 55-55,430) have been proposed.
〔発明が解決しようとする問題点及び作用〕このように
、ナフテン系潤滑基油は、一部の特殊な合成潤滑油を除
いて、そのほとんどが原油を精製して製造されているが
、近年における原油価格の高騰や供給の不安定化により
、資源確保の立場から原油に代る代替原料として石炭の
利用が必須になってきている。[Problems and effects to be solved by the invention] As described above, most naphthenic lubricating base oils, with the exception of some special synthetic lubricating oils, are produced by refining crude oil. Due to the soaring price of crude oil and the instability of its supply, the use of coal as an alternative raw material to crude oil has become essential in terms of securing resources.
しかしながら、コールタール、コールタールピッチ、石
炭液化油等の石炭系原料油から潤滑基油を製造する方法
については今だ確立されておらず、しかも、石炭系原料
油は石油系原料油と比較して窒素分の含有浴が多く、そ
の構造も直鎖アルキル基が少なく、縮合多環芳香族化合
物を主成分とするものであり、石油系原料油を使用する
従来のナフテン系潤滑基油の製造法で製造した精製油は
その酸化安定性が極めて悪く潤滑油として使用し難いと
いう問題があった。However, a method for producing lubricating base oils from coal-based feedstocks such as coal tar, coal tar pitch, and coal liquefied oil has not yet been established, and coal-based feedstocks are less effective than petroleum-based feedstocks. The bath has a high nitrogen content, has a structure with few straight-chain alkyl groups, and is mainly composed of fused polycyclic aromatic compounds. The problem is that the refined oil produced by this method has extremely poor oxidation stability and is difficult to use as a lubricating oil.
〔問題点を解決するための手段及び作用〕本発明は、か
かる観点に鑑みて創案されたもので、コールタール、コ
ールタールピッチ、石炭液化油及び石炭液化ピッチから
選ばれた石炭系原料を水素化分解又は熱分解して得られ
た炭化水素油を、必要により脱硫脱窒素して硫黄分及び
窒素分をそれぞれ１，０ＯＯＩＩＩ’１ｍ以下にした後
、核水素化する酸化安定性に優れたナフテン系潤滑基油
の製造法である。[Means and effects for solving the problems] The present invention was devised in view of this point of view, and the present invention is made by converting coal-based raw materials selected from coal tar, coal tar pitch, coal liquefied oil, and coal liquefied pitch into hydrogen. Hydrocarbon oil obtained by chemical cracking or thermal decomposition is desulfurized and denitrified if necessary to reduce the sulfur content and nitrogen content to 1,000 OOIII'1 m or less, respectively, and then nuclear hydrogenated to produce naphthenes with excellent oxidation stability. This is a method for producing lubricating base oil.
−〇 −
本発明において、原料となる炭化水素油は、］−ルター
ル、コールタールピッチ、石炭液化油又は石炭液化ピッ
チ等の石炭系原料を水素化分解したり、熱分解したり、
あるいは、これら水素化分解及び熱分解をして得られる
ものであり、好ましくは環数２〜１０の縮合多環成分を
５０重叩％以上、好ましくは６０市ｍ％１メ上含み、沸
点範囲が２００〜６． Ｏ０℃又はそれ以」二のもので
ある。このような炭化水素油としては、例えば、＝１−
ルタールピッヂを水素化する際に生成する炭化水素油や
、コールタールピッチを］−クス化する際に生成する熱
分解油等がある。-〇- In the present invention, the hydrocarbon oil used as a raw material is obtained by hydrocracking or thermally decomposing a coal-based raw material such as lutal, coal tar pitch, coal liquefied oil or coal liquefied pitch,
Alternatively, it is obtained by hydrogenolysis and thermal decomposition, preferably contains 50% or more, preferably 60% of fused polycyclic components having 2 to 10 rings, and has a boiling point range. is 200-6. 0°C or higher. As such a hydrocarbon oil, for example, =1-
There are hydrocarbon oils produced when coal tar pitch is hydrogenated, and pyrolysis oils produced when coal tar pitch is converted into alcohol.
そして、この炭化水素油は、イれが石炭に由来するもの
であるため、通常、硫黄化合物を元素硫黄分に換算して
０．０２〜２重量％含有し、また、窒素化合物を元素分
窒素分に換算して０．１〜３重量％含有している。本発
明において、これら硫黄分や窒素分の含有量が多い場合
には、好ましくは水素化精製によりこれら硫黄分や窒素
分をそれぞれ１．ｏｏｏｐｐｍ以下、好ましくは硫黄分
を１００ ｐｕ＋以下、窒素分を１００１１ｊｌｌｌＪ
メ下にする。Since this hydrocarbon oil is derived from coal, it usually contains 0.02 to 2% by weight of sulfur compounds converted to elemental sulfur content, and contains nitrogen compounds of 0.02 to 2% by weight in terms of elemental sulfur content. The content is 0.1 to 3% by weight calculated as 0.1% to 3% by weight. In the present invention, when these sulfur and nitrogen contents are high, it is preferable to reduce these sulfur and nitrogen contents to 1.0% by hydrorefining, respectively. oooppm or less, preferably sulfur content is 100 pu+ or less, nitrogen content is 10011jlllJ
Put it under your eyes.
この目的で行う水素化精製は、ＨＯｌＨ、Ｎｉ、Ｃ。The hydrorefining performed for this purpose is HOLH, Ni, C.
等、周１ｌｌｌｆＩ表第６Ｍａ及び／又は第８族の金属
から選ばれた少なくとも１種の金属成分をアルミナやシ
リカ等の担体に担持させた触媒の存在下にバッチ式や液
流通式で行うことができるが、好ましくは液流通式であ
り、この場合、反応温度２５０〜５００℃、好ましくは
３５０〜４３０℃、反応圧力２０〜３００Ｋｇ／ｃｄ−
Ｇ１好ましくは５０〜２００Ｋｇ／ｃＭ−Ｇ、液空間速
度（１−ＨＳ Ｖ ） ０ 。etc., carried out in a batch method or a liquid flow method in the presence of a catalyst in which at least one metal component selected from Group 6 Ma and/or Group 8 metals is supported on a carrier such as alumina or silica. However, it is preferably a liquid flow type, in which case the reaction temperature is 250 to 500°C, preferably 350 to 430°C, and the reaction pressure is 20 to 300 Kg/cd-
G1 preferably 50 to 200 Kg/cM-G, liquid hourly space velocity (1-HS V ) 0 .
（１−ｏｉｌの条件で行うのがよい。(It is best to perform this under 1-oil conditions.
必要により脱硫脱窒素して硫黄分及び窒素分をそれぞれ
１．ＯＯＯｒｌｌ）ｍ以下にした炭化水素油は、次に核
水素化される。この核水素化は、得られた核水素化炭化
水素油中の炭素の７０〜９０％がナフテン系炭素で、０
〜２０％が芳香族系炭素で、残余がパラフィン系炭素と
なるように行うことが好ましく、より好ましくは炭化水
素油中の芳香族炭化水素が可及的にナフテン系炭化水素
になるまで行う。If necessary, desulfurization and denitrification are performed to reduce the sulfur content and nitrogen content to 1. The hydrocarbon oil reduced to below OOOrll)m is then subjected to nuclear hydrogenation. In this nuclear hydrogenation, 70 to 90% of the carbon in the obtained nuclear hydrogenated hydrocarbon oil is naphthenic carbon, and 0.
It is preferable to carry out the process so that ~20% is aromatic carbon and the remainder is paraffinic carbon, and more preferably, the process is carried out until the aromatic hydrocarbons in the hydrocarbon oil become naphthenic hydrocarbons as much as possible.
この炭化水素油の核水素化は、Ｎ１、Ｐｌ、Ｐｄなどの
周期律表第８族の金属を珪藻土、アルミナ、マグネシア
、ボリア、シリカ等に担持した触媒を使用して大過剰の
水素ガス存在下にバッチ式や液流通式で行うことができ
るが、好ましくはバッチ式であり、この場合、反応ｍ
ａ ５０〜３００℃及び反応圧力１０〜２００ＫＦｌ／
ｒ：ｄ・Ｇの範囲の条件で行うことができる。なお、反
応時間については水素の吸収が終了するまで行うことが
好ましい。This nuclear hydrogenation of hydrocarbon oil is carried out using a catalyst in which metals from group 8 of the periodic table, such as N1, Pl, and Pd, are supported on diatomaceous earth, alumina, magnesia, boria, silica, etc., and a large excess of hydrogen gas is present. Although the reaction can be carried out in a batch manner or in a liquid flow manner, a batch method is preferable; in this case, the reaction m
a 50-300℃ and reaction pressure 10-200KFl/
This can be carried out under conditions in the range of r:d.G. In addition, regarding the reaction time, it is preferable to carry out the reaction until the absorption of hydrogen is completed.
本発明においては、炭化水素中に残存する不純物を除去
する目的で、好ましくは核水素化の前又は後に硫酸洗浄
及び／又は固体吸着による精製処理を行う。この硫酸洗
浄及び／又は固体吸着は、そのいずれか一方を行っても
よく、また、その両者を行ってもよい。また、両者を行
う場合、その順序も任意であり、いずれか一方を核水素
化の前に行い、他方を核水素化の後に行ってもよい。In the present invention, in order to remove impurities remaining in the hydrocarbon, purification treatment by sulfuric acid washing and/or solid adsorption is preferably performed before or after nuclear hydrogenation. Either one or both of the sulfuric acid cleaning and/or solid adsorption may be performed. Moreover, when performing both, the order is also arbitrary, and either one may be performed before nuclear hydrogenation, and the other may be performed after nuclear hydrogenation.
上記硫酸洗浄の処理条件については、８０〜９８％硫酸
を硫Ｉｌ／油の比０．０１〜１０．０（体積比）、好ま
しくは０．１〜１．０で混合し、調度範囲常温〜８０℃
で１５〜１５０分間撹拌して行うのがよい。また、上記
固体吸着の処理条件については、活性白土、活性アルミ
ナ、シリカアルミナ等の固体吸着剤中を０〜１５０℃の
混成範囲ｒｌ−Ｈ８Ｖ０．１〜５０ｈｒ−’、好ｔ’Ｌ
＜ハｏ、５〜１Ｑｈｒ”の速度で流通させて行うのがよ
い。Regarding the processing conditions for the above-mentioned sulfuric acid cleaning, 80-98% sulfuric acid is mixed at a sulfur/oil ratio of 0.01-10.0 (volume ratio), preferably 0.1-1.0, and the preparation range is room temperature to 80℃
It is best to stir the mixture for 15 to 150 minutes. In addition, regarding the processing conditions for the solid adsorption mentioned above, in a solid adsorbent such as activated clay, activated alumina, or silica alumina, the mixture range is 0 to 150°C rl-H8V0.1 to 50hr-', and the preferable t'L
It is preferable to circulate at a rate of 5 to 1 Qhr.
このようにして核水素化され、また、硫酸洗浄及び／又
は固体吸着により処理された生成油は、減圧熱面によっ
て適当な沸点範囲の油に分離することにより、動粘麿（
４０℃）５〜６ ＱＩＣ３ｔの範囲のナフテン系潤滑基
油を得ることができる。ここで、得られたナフテン系潤
滑基油は一１０℃以下の流動点を有するものである。The resulting oil, which has been nuclear hydrogenated in this way and treated by sulfuric acid washing and/or solid adsorption, is separated into oils with appropriate boiling point ranges by a vacuum heat surface, and then converted to kinematic viscosity (
Naphthenic lubricating base oils with a QIC of 3t can be obtained. The naphthenic lubricating base oil obtained here has a pour point of -10°C or less.
以下、実施例に基づいて、本発明方法を詳細に説明する
。Hereinafter, the method of the present invention will be explained in detail based on Examples.
実施例１
コールタールを熱部して得られた軟ピツチを水素化触媒
の存在下に水素イし処理し、ｊｑられた水素化ピッチを
ディレートコ−カーで熱分解して原料の炭化水素油を製
造した。この炭化水素油は、沸点２７０〜５００℃で、
硫黄分１． 、２００ ｐ、ｐｍ及び窒素分７．６．０
Ｏｐｐｍを含有していた。Example 1 Soft pitch obtained by heating coal tar was hydrogenated in the presence of a hydrogenation catalyst, and the hydrogenated pitch was thermally decomposed in a dilate coker to produce hydrocarbon oil as a raw material. Manufactured. This hydrocarbon oil has a boiling point of 270-500℃,
Sulfur content 1. , 200 p, pm and nitrogen content 7.6.0
It contained Oppm.
この原料炭化水素油を市販のＮ ｉ ０−ＭｏＯ３／Ａ
ｐ２０３触媒を充填した流通式高圧反応器に装入し、反
応渇１σ４００°Ｃ１水素圧力１８０Ｋｇ／ｃｄ−Ｇ、
液空間速度０ 、３ ｂｒ−１及び液−ガス比４００〜
３ 、 ＯＯ，Ｏｆ−ｌ ２−（１／ （ｌ Ｏｉ
ｌの条件で水素化精製を行った。ｊｑられた水素化精製
油の回収率は９９％であり、硫黄分は０．５ｐｐｍに減
少し、また、窒素分ｔ；ｔ ３０ ｐＩ）Ｉｌｌに減少
した。This raw material hydrocarbon oil was converted into a commercially available N i 0-MoO3/A
Charged into a flow type high pressure reactor filled with p203 catalyst, reaction temperature 1σ400°C1 hydrogen pressure 180Kg/cd-G,
Liquid hourly velocity 0, 3 br-1 and liquid-gas ratio 400~
3, OO, Of-l 2-(1/ (l Oi
Hydrorefining was carried out under the conditions of 1. The recovery rate of the hydrotreated oil was 99%, the sulfur content was reduced to 0.5 ppm, and the nitrogen content was reduced to t; t 30 pI) Ill.
次いで、上記水素化精製油に１０重♀％のニッケル触媒
を添加し、オー［〜クレープ中反応渇爪２３０℃及び水
索斤力１００ＫＦＩ／ａｒｔ−Ｇの条Ｐ１で４時間反応
させ、η香族環が可及的に核水素化された核水素化炭化
水素油を得た。Next, 10% by weight of a nickel catalyst was added to the above hydrotreated oil and reacted for 4 hours in a crepe at 230° C. and a water digging force of 100 KFI/art-G in column P1. A nuclear hydrogenated hydrocarbon oil in which the group rings were hydrogenated as much as possible was obtained.
この核水素化炭化水素油に９８％ｒｌｉ！を酸を１０市
ｍ％添加し、３０分間接触させた後、核水素化炭化水素
油と硫酸とを分離し、５％Ｎ ａ Ｏ＋−１水溶液で中
和した後水洗し、さらに、１３０℃、Ｌ ｌ−Ｉ ＳＶ
１ ｈｒ−％活性白土中を流通させて固体吸着処理し
、核水素化精製油を得た。この核水素化精製油の収率は
４０％であり、硫黄分３．０ｐｐｍ及び窒素分０．５ρ
ｐｎｌであった。98% rli in this nuclear hydrogenated hydrocarbon oil! After adding 10 m% of acid and contacting for 30 minutes, the nuclear hydrogenated hydrocarbon oil and sulfuric acid were separated, neutralized with 5% NaO+-1 aqueous solution, washed with water, and further heated at 130°C. , L l-I SV
Solid adsorption treatment was carried out by passing through activated clay for 1 hr-% to obtain nuclear hydrogenated refined oil. The yield of this nuclear hydrogenated refined oil is 40%, with a sulfur content of 3.0 ppm and a nitrogen content of 0.5 ρ.
It was pnl.
−に記核水素化精製油を熱温により沸点２５０〜３５０
℃留分と３５０へ一！１００’Ｃ留分に分別し、ナフテ
ン系潤滑基油を製造した。沸点２５０〜３５０℃のナフ
テン系潤滑基油の収率は２４％で、沸点３５０〜４００
℃のナフテン系潤滑基油の収率は４％であった。- The boiling point of the hydrogenated refined oil is 250 to 350 depending on the heat temperature.
℃ distillation and 350 to 1! It was fractionated into a 100'C fraction to produce a naphthenic lubricating base oil. The yield of naphthenic lubricating base oil with a boiling point of 250-350℃ is 24%,
The yield of naphthenic lubricating base oil at 4% was obtained.
実施例２
実施例１で使用したと同じ原料炭化水素油を実施例１と
同様な方法で水素化精製し、次いで実施例１と同様な方
法で核水素化した後、硫酸洗浄処理することなく、実施
例１ど同様な方法で活性白土により固体吸着処理し、分
別蒸溜して沸点２５０〜３５０℃留分及び沸点３５０〜
４００℃留かのナフテン系潤滑基油を得た。Example 2 The same raw material hydrocarbon oil used in Example 1 was hydrorefined in the same manner as in Example 1, and then subjected to nuclear hydrogenation in the same manner as in Example 1, without being subjected to sulfuric acid washing treatment. , solid adsorption treatment with activated clay in the same manner as in Example 1, followed by fractional distillation to obtain a fraction with a boiling point of 250-350°C and a fraction with a boiling point of 350-350°C.
A naphthenic lubricating base oil distilled at 400°C was obtained.
二 １２ 一
固体吸着処理して得られた核水素化精製油の収率は７２
％であり、硫黄分０．５ｐｐｍ及び窒素分０．３ｎｒ１
ｍであった。分別蒸溜して得られた沸点２５０〜３５０
’Ｃ留分のナフテン系潤滑基油の収率は４３％で、沸点
３５０〜４００℃留分のナフテン系潤滑基油の収率は１
２％であ・〕だ。2 12 1 The yield of nuclear hydrogenated refined oil obtained by solid adsorption treatment is 72
%, sulfur content 0.5ppm and nitrogen content 0.3nr1
It was m. Boiling point 250-350 obtained by fractional distillation
The yield of naphthenic lubricating base oil in the 'C fraction is 43%, and the yield of naphthenic lubricating base oil in the boiling point 350-400°C fraction is 1.
It's 2%.
実施例３
上記実施例２の場合と同様であるが、核水素化と活性白
土による固体吸着処理の順序を逆にしてナフテン系潤滑
基油の製造を行った。１１られた核水素化精製油の収率
は７１％であり、硫黄分０゜５ ｐｐｍ及び窒素分０．
２ｒ＋ｐｍであった。分別蒸溜して得られた沸点２５０
〜３５０℃留分のナフテン系潤滑基油の収率は４７％で
、沸点３５０〜４００℃留分のナフテン系潤滑基油の収
率は８％であった。Example 3 A naphthenic lubricating base oil was produced in the same manner as in Example 2 above, except that the order of nuclear hydrogenation and solid adsorption treatment using activated clay was reversed. The yield of the nuclear hydrogenated refined oil was 71%, with a sulfur content of 0.5 ppm and a nitrogen content of 0.5 ppm.
It was 2r+pm. Boiling point 250 obtained by fractional distillation
The yield of the naphthenic lubricating base oil in the ~350°C fraction was 47%, and the yield of the naphthenic lubricating base oil in the boiling point fraction of 350~400°C was 8%.
比較例１
核水素化を省略した以外は実施例１と同様にして潤滑基
）Ｉｌｌの製造を行った。得られた精製油を分別蒸溜し
て沸点２５０〜３５０℃留分と沸点３５０〜４００℃留
分を得た。Comparative Example 1 A lubricating group) Ill was produced in the same manner as in Example 1 except that the nuclear hydrogenation was omitted. The obtained refined oil was fractionally distilled to obtain a fraction with a boiling point of 250 to 350°C and a fraction with a boiling point of 350 to 400°C.
比較例２
核水素化を省略した以外は実施例２と同様にして潤滑基
油の製造を行った。ｉｑられた精製油を分別蒸溜して沸
点２５０〜３５０℃留分ど沸点３５０〜４００℃留分を
得た。Comparative Example 2 A lubricating base oil was produced in the same manner as in Example 2 except that nuclear hydrogenation was omitted. The iq refined oil was fractionally distilled to obtain a fraction with a boiling point of 250-350°C and a fraction with a boiling point of 350-400°C.
次に、上記実施例１〜３並びに比較例７及び２で得られ
た各潤滑基油について、粘（資）、粘度指数、流動点、
全酸価、回転ボンベ式による酸化安定性ｂｉｔｓ Ｋ
２５１４，３．３） 、引火点、比重及び色相の一般的
性状を調べた。結果を第１表に示す。Next, the viscosity, viscosity index, pour point,
Total acid value, oxidation stability bits K by rotating cylinder type
2514, 3.3), the general properties of flash point, specific gravity and hue were investigated. The results are shown in Table 1.
この第１表の結果から明らかなように、各実施例で得ら
れたナフテン系潤滑基油は、比較例のものと比較して、
酸化安定性が優れているぽか、流動点も低くなっており
、性能的に優れていることが判明した。As is clear from the results in Table 1, the naphthenic lubricating base oils obtained in each example had a
It was found that Poka has excellent oxidation stability and has a low pour point, making it excellent in terms of performance.
本発明方法によれば、石油系炭化水素油に比べて芳香族
系炭素の含有率が高く、しかも、不純物として含有され
ている窒素分が多いために従来の石油系炭化水素油を原
石とするナフテン系潤滑油の製造法を適用することがで
きなかった石炭系炭化水素油を原石にして、酸化安定性
に優れたナフテン系潤滑基油を製造することができる。According to the method of the present invention, conventional petroleum-based hydrocarbon oil is used as raw material because it has a higher aromatic carbon content than petroleum-based hydrocarbon oil and also contains a large amount of nitrogen as an impurity. A naphthenic lubricating base oil with excellent oxidation stability can be produced by using coal-based hydrocarbon oil, to which the method for producing naphthenic lubricating oil cannot be applied, as raw ore.
Claims (8)
及び石炭液化ピッチから選ばれた石炭系原料を水素化分
解又は熱分解し、得られた炭化水素油を核水素化するこ
とを特徴とする酸化安定性に優れたナフテン系潤滑基油
の製造法。(1) Oxidation characterized by hydrocracking or thermal cracking of a coal-based raw material selected from coal tar, coal tar pitch, coal liquefied oil, and coal liquefied pitch, and subjecting the obtained hydrocarbon oil to nuclear hydrogenation. A method for producing naphthenic lubricating base oil with excellent stability.
黄分及び窒素分それぞれ１０００ｐｐｍ以下にした後、
核水素化する特許請求の範囲第１項記載のナフテン系潤
滑基油の製造法。(2) After hydrocarbon oil is desulfurized and denitrified by hydrorefining to reduce the sulfur content and nitrogen content to 1000 ppm or less,
A method for producing a naphthenic lubricating base oil according to claim 1, wherein the naphthenic lubricating base oil is subjected to nuclear hydrogenation.
黄分及び窒素分それぞれ１００ｐｐｍ以下にする特許請
求の範囲第２項記載のナフテン系潤滑基油の製造法。(3) A method for producing a naphthenic lubricating base oil according to claim 2, in which hydrocarbon oil is desulfurized and denitrified by hydrorefining to reduce the sulfur content and nitrogen content to 100 ppm or less.
よる精製処理を行う特許請求の範囲第１項ないし第３項
のいずれかに記載のナフテン系潤滑基油の製造法。(4) The method for producing a naphthenic lubricating base oil according to any one of claims 1 to 3, wherein after nuclear hydrogenation, purification treatment is performed by washing with sulfuric acid and/or solid adsorption.
又は固体吸着による精製処理を行い、次いで核水素化す
る特許請求の範囲第１項ないし第３項のいずれかに記載
のナフテン系潤滑基油の製造法。(5) After hydrorefining hydrocarbon oil, washing with sulfuric acid and/or
Alternatively, the method for producing a naphthenic lubricating base oil according to any one of claims 1 to 3, which comprises performing a refining treatment by solid adsorption and then nuclear hydrogenation.
重量％以上含有し、その沸点範囲が２００〜６００℃で
ある特許請求の範囲第１項ないし第５項のいずれかに記
載のナフテン系潤滑基油の製造法。(6) Hydrocarbon oil contains 50 fused polycyclic components having 2 to 10 rings.
The method for producing a naphthenic lubricating base oil according to any one of claims 1 to 5, wherein the naphthenic lubricating base oil contains at least % by weight and has a boiling point range of 200 to 600°C.
I族の金属から選ばれた少なくとも１種の金属成分を含
有する触媒の存在下に、反応温度２５０〜５００℃、反
応圧力２０〜３００Ｋｇ／ｃｍ＾２・Ｇ、液空間速度０
．０１〜１０．０ｈｒ＾−＾１、液−ガス比１００〜５
，０００Ｈ＿２−ｌ／ｌ−ｏｉｌの条件で行う特許請求
の範囲第２項ないし第６項のいずれかに記載のナフテン
系潤滑基油の製造法。(7) Hydrorefining is carried out in Group VI and/or VII of the periodic table.
In the presence of a catalyst containing at least one metal component selected from Group I metals, the reaction temperature is 250 to 500°C, the reaction pressure is 20 to 300 Kg/cm^2 G, and the liquid hourly space velocity is 0.
．． 01~10.0hr^-^1, liquid-gas ratio 100~5
, 000H_2-l/l-oil. The method for producing a naphthenic lubricating base oil according to any one of claims 2 to 6.
た少なくとも１種の金属成分を含有する触媒の存在下に
、反応湿度５０〜３００℃、反応圧力１０〜２００Ｋｇ
／ｃｍ＾２・Ｇの条件で行う特許請求の範囲第１項ない
し第７項のいずれかに記載のナフテン系潤滑基油の製造
法。(8) Nuclear hydrogenation is carried out at a reaction humidity of 50 to 300°C and a reaction pressure of 10 to 200 kg in the presence of a catalyst containing at least one metal component selected from group VIII metals of the periodic table.
A method for producing a naphthenic lubricating base oil according to any one of claims 1 to 7, which is carried out under the conditions of /cm^2·G.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP24228484A JPS61120896A (en) | 1984-11-19 | 1984-11-19 | Preparation of naphthenic lube base oil |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP24228484A JPS61120896A (en) | 1984-11-19 | 1984-11-19 | Preparation of naphthenic lube base oil |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPS61120896A true JPS61120896A (en) | 1986-06-07 |
Family
ID=17086966
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP24228484A Pending JPS61120896A (en) | 1984-11-19 | 1984-11-19 | Preparation of naphthenic lube base oil |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS61120896A (en) |
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS62101689A (en) * | 1985-10-24 | 1987-05-12 | シエブロン リサ−チ コンパニ− | Stabilization of lubricant base stock |
| EP0310346A2 (en) * | 1987-09-28 | 1989-04-05 | Nippon Steel Chemical Co., Ltd. | Composition suitable for traction drives and process for operating the same |
| CN102337144A (en) * | 2010-07-20 | 2012-02-01 | 陕西煤业化工集团神木天元化工有限公司 | Method for preparing light fuel from medium and low-temperature coal tar generated by carbonizing lump coal |
| CN103436289A (en) * | 2013-09-13 | 2013-12-11 | 王树宽 | Method for producing naphthenic base transformer oil base oil by using coal tar oil |
| CN103436290A (en) * | 2013-09-13 | 2013-12-11 | 王树宽 | Method for producing naphthenic base refrigerating machine oil base oil by using coal tar oil |
| CN103571533A (en) * | 2012-07-20 | 2014-02-12 | 中国石油化工集团公司 | Coal tar hydrogenation system and coal tar hydrogenation method |
| CN105419864A (en) * | 2015-11-13 | 2016-03-23 | 王树宽 | System and method for preparing high-octane gasoline, aviation kerosene and naphthenic base oil with total-hydrogen-type coal tar |
| CN109321273A (en) * | 2018-09-27 | 2019-02-12 | 国家能源投资集团有限责任公司 | The method and apparatus for producing naphthenic base refrigerator oil base oil |
| CN109954490A (en) * | 2017-12-22 | 2019-07-02 | 中国石油化工股份有限公司 | A kind of reduction-state diesel oil dearomatization catalyst |
-
1984
- 1984-11-19 JP JP24228484A patent/JPS61120896A/en active Pending
Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS62101689A (en) * | 1985-10-24 | 1987-05-12 | シエブロン リサ−チ コンパニ− | Stabilization of lubricant base stock |
| EP0310346A2 (en) * | 1987-09-28 | 1989-04-05 | Nippon Steel Chemical Co., Ltd. | Composition suitable for traction drives and process for operating the same |
| CN102337144A (en) * | 2010-07-20 | 2012-02-01 | 陕西煤业化工集团神木天元化工有限公司 | Method for preparing light fuel from medium and low-temperature coal tar generated by carbonizing lump coal |
| CN103571533A (en) * | 2012-07-20 | 2014-02-12 | 中国石油化工集团公司 | Coal tar hydrogenation system and coal tar hydrogenation method |
| CN103436290B (en) * | 2013-09-13 | 2015-05-27 | 王树宽 | Method for producing naphthenic base refrigerating machine oil base oil by using coal tar oil |
| CN103436290A (en) * | 2013-09-13 | 2013-12-11 | 王树宽 | Method for producing naphthenic base refrigerating machine oil base oil by using coal tar oil |
| CN103436289A (en) * | 2013-09-13 | 2013-12-11 | 王树宽 | Method for producing naphthenic base transformer oil base oil by using coal tar oil |
| CN105419864A (en) * | 2015-11-13 | 2016-03-23 | 王树宽 | System and method for preparing high-octane gasoline, aviation kerosene and naphthenic base oil with total-hydrogen-type coal tar |
| CN105419864B (en) * | 2015-11-13 | 2017-05-03 | 王树宽 | System and method for preparing high-octane gasoline, aviation kerosene and naphthenic base oil with total-hydrogen-type coal tar |
| CN109954490A (en) * | 2017-12-22 | 2019-07-02 | 中国石油化工股份有限公司 | A kind of reduction-state diesel oil dearomatization catalyst |
| CN109954490B (en) * | 2017-12-22 | 2022-09-09 | 中国石油化工股份有限公司 | Reduced diesel dearomatization catalyst |
| CN109321273A (en) * | 2018-09-27 | 2019-02-12 | 国家能源投资集团有限责任公司 | The method and apparatus for producing naphthenic base refrigerator oil base oil |
| CN109321273B (en) * | 2018-09-27 | 2020-11-13 | 国家能源投资集团有限责任公司 | Method and device for producing naphthenic base refrigerator oil base oil |
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