JP4246496B2 - ワックス状ラフィネートの製造方法 - Google Patents
ワックス状ラフィネートの製造方法 Download PDFInfo
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Description
(a)フィッシャー・トロプシュ生成物中の炭素原子数60以上の化合物と炭素原子数30以上の化合物との重量比が少なくとも0.2であり、かつフィッシャー・トロプシュ誘導原料中の化合物の少なくとも30重量%が炭素原子数30以上の化合物であるフィッシャー・トロプシュ誘導原料を水素化分解/水素化異性化する工程、
(b)工程(a)の生成物から、沸点範囲200〜450℃のT10 重量%と沸点範囲400〜650℃のT90 重量%とを有するワックス状ラフィネート生成物を単離する工程、
によるワックス状ラフィネート生成物の製造方法に向けたものである。
工程(a)で使用される比較的重質のフィッシャー・トロプシュ誘導原料は、炭素原子数が30以上の化合物を少なくとも30重量%、好ましくは少なくとも50重量%、更に好ましくは少なくとも55重量%含有する。更に、フィッシャー・トロプシュ誘導原料中の、炭素原子数60以上の化合物と炭素原子数30以上の化合物との重量比は少なくとも0.2、好ましくは少なくとも0.4、更に好ましくは少なくとも0.55である。好ましくはフィッシャー・トロプシュ誘導原料は、ASF−アルファ値(Anderson−Schulz−Flory連鎖生長ファクター)が少なくとも0.925、好ましくは少なくとも0.935、更に好ましくは少なくとも0.945、なお更に好ましくは少なくとも0.955のC20 + フラクションを含有するフィッシャー・トロプシュ生成物から誘導される。
工程(b)では工程(a)の生成物は、1つ以上のガス油フラクション、沸点範囲が200〜450℃のT10重量%、沸点範囲が400〜650℃のT90重量%及び更に好ましくは沸点が550℃未満のT90重量%を有するワックス状ラフィネート生成物に分離される。また工程(a)での転化率及び工程(a)への原料全体の特性に依存して、工程(b)で高沸点フラクションを得ることができる。
工程(b)の真空蒸留は、所望のワックス状ラフィネート生成物が前記特定範囲の沸点を有すると共に、100℃での動粘度が好ましくは3〜10cStで得られるように操作することが好ましい。
流動点低下処理により、処理毎に基油の流動点が10℃を越え、好ましくは20℃を越え、更に好ましくは25℃を越えて低下することが判る。
接触脱蝋法は、触媒及び水素の存在下でワックス状ラフィネート生成物の流動点が上記特定したように低下するいかなる方法でも実施できる。好適な脱蝋触媒は、モレキュラーシーブ及び任意に第VIII族金属のような水素化機能を有する金属との組合せを有する不均質触媒である。モレキュラーシーブ、更に好適には中間細孔サイズのゼオライトは、接触脱蝋条件下でワックス状ラフィネート生成物の流動点を低下させる良好な触媒能力を示した。好ましい中間細孔サイズのゼオライトは、0.35〜0.8nmの細孔直径を有する。好適な中間細孔サイズのゼオライトは、ZSM−5、ZSM−12、ZSM−22、ZSM−23、SSZ−32、ZSM−35及びZSM−48である。他の好ましいモレキュラーシーブ群は、シリカ−アルミナホスフェート(SAPO)材料である。これら材料のうち、SAPO−11は、例えばUS−A−4859311に記載されるように、最も好ましい。ZSM−5は、いかなる第VIII族金属も存在しない場合、そのHSMZ−5の形態で任意に使用できる。その他のモレキュラーシーブは、添加した第VIII族金属と組合せて使用することが好ましい。好適な第VIII族金属は、ニッケル、コバルト、白金及びパラジウムである。可能な組合せの例は、Pt/ZSM−35、Ni/ZSM−5、Pt/ZSM−23、Pd/ZSM−23、Pt/ZSM−48及びPt/SAPO−11である。好適なモレキュラーシーブ及び脱蝋条件の更なる詳細及び例は、WO−A−9718278、US−A−4343692、US−A−5053373、US−A−5252527及びUS−A−4574043に記載される。
この基油自体は、例えば自動変速機流体(ATF)、自動車(ガソリン又はディーゼル)エンジンオイル、タービンオイル、油圧オイル、電気用オイル又はトランスオイル及び冷却機オイル、の一部として利用できる。
WO−A−9934917の実施例IIIの触媒を水素化分解工程(工程(a))に用いて同刊行物の実施例VIIで得られたフィッシャー・トロプシュ生成物のC5 〜C750 ℃+ フラクションを連続的に供給することにより、ワックス状ラフィネート生成物を得た。この原料はC30+生成物を約60重量%含有していた。C60+/C30+比は約0.55であった。このフラクションは、水素化分解工程においてEP−A−532118の実施例1の触媒と接触させた。
工程(a)の流出物を連続的に蒸留して軽質分、燃料及び沸点370℃以上の残留物“R”を得た。水素化分解工程に供給する新鮮な原料に対する(on)ガス油フラクションの収率は、43重量%であった。残留物“R”の大部分は、工程(a)に再循環し、残部は、真空蒸留により第1表に示すような特性を有するワックス状ラフィネート生成物と、沸点が510℃を越えるフラクションとに分離した。
水素化分解工程(a)の条件は、新鮮な原料の重量の1時間当り空間速度(WHSV) 0.8kg/l.h、再循環原料のWHSV 0.2kg/l.h、水素ガス速度=1000 Nl/kg、全圧=40バール、及び反応器温度 335℃である。
┌─────────────┬──────────┐
│70℃での密度(kg/m3)│ 779.2 │
├─────────────┼──────────┤
│vK@100(cSt) │ 3.818 │
├─────────────┼──────────┤
│流動点(℃) │ +18 │
├─────────────┼──────────┤
│回収(重量%)時の沸点デー│ 5% 355℃ │
│タ │ 10% 370℃ │
│ │ 50% 419℃ │
│ │ 90% 492℃ │
│ │ 95% 504℃ │
└─────────────┴──────────┘
実施例1のワックス状ラフィネート生成物を、WO−A−0029511の実施例9に記載の、0.7重量%Pt及び30重量%ZSM−5を含有する脱アルミ化シリカ結合ZSM−5触媒と接触させることにより脱蝋して、基油を製造した。脱蝋条件は、水素 40バール、WHSV=1kg/l.h及び温度 340℃である。
脱蝋油を蒸留して3つの基油フラクション:沸点378〜424℃のフラクション(脱蝋工程の原料に対する収率は14.2重量%)、沸点418〜455℃のフラクション(脱蝋工程の原料に対する収率は16.3重量%)及び沸点が455℃を越えるフラクション(脱蝋工程の原料に対する収率は21.6重量%)を得た。更なる詳細は第2表に示す。
┌───────────────┬─────┬─────┬─────┐
│ │軽質 │中質 │重質 │
│ │グレード │グレード │グレード │
├───────────────┼─────┼─────┼─────┤
│20℃での密度 │805.8│814.6│822.4│
├───────────────┼─────┼─────┼─────┤
│流動点(℃) │<−63 │<−51 │−45 │
├───────────────┼─────┼─────┼─────┤
│40℃での動粘度(cSt) │ │19.06│35.0 │
├───────────────┼─────┼─────┼─────┤
│100℃での動粘度(cSt) │3.16 │4.144│6.347│
├───────────────┼─────┼─────┼─────┤
│VI │適用不能 │121 │134 │
├───────────────┼─────┼─────┼─────┤
│Noack揮発度(重量%) │適用不能 │10.8 │2.24 │
├───────────────┼─────┼─────┼─────┤
│硫黄含有量(ppm) │<1ppm│<1ppm│<5ppm│
├───────────────┼─────┼─────┼─────┤
│飽和物(重量%) │適用不能 │99.9 │適用不能 │
├───────────────┼─────┼─────┼─────┤
│シクロパラフィン含有量 │適用不能 │18.5 │適用不能 │
│(重量%)(*) │ │ │ │
├───────────────┼─────┼─────┼─────┤
│CCSで測定した−40℃での │適用不能 │3900 │適用不能 │
│動力学粘度 │ │cP │ │
└───────────────┴─────┴─────┴─────┘
(*)前記基油の飽和物フラクションについて、フィールド脱着/フィールドイオン化インターフェースを備えたFinnigan MAT90質量分析計で測定。
脱蝋油を蒸留して3つの異なる基油生成物に分離した他は実施例2を繰り返した。それらの特性を第3表に示す。
┌───────────────┬─────┬─────┬─────┐
│ │軽質 │中質 │重質 │
│ │グレード │グレード │グレード │
├───────────────┼─────┼─────┼─────┤
│20℃での密度 │809.1│817.2│825.1│
├───────────────┼─────┼─────┼─────┤
│流動点(℃) │<−63 │<−51 │−39 │
├───────────────┼─────┼─────┼─────┤
│40℃での動粘度(cSt) │ │23.32│43.01│
├───────────────┼─────┼─────┼─────┤
│100℃での動粘度(cSt) │3.181│4.778│7.349│
├───────────────┼─────┼─────┼─────┤
│VI │適用不能 │128 │135 │
├───────────────┼─────┼─────┼─────┤
│Noack揮発度(重量%) │適用不能 │7.7 │適用不能 │
├───────────────┼─────┼─────┼─────┤
│硫黄含有量(ppm) │<5ppm│<5ppm│<5ppm│
├───────────────┼─────┼─────┼─────┤
│飽和物(重量%) │ │99.0 │ │
├───────────────┼─────┼─────┼─────┤
│CCSで測定した−40℃での │ │5500 │ │
│動力学粘度 │ │cP │ │
├───────────────┼─────┼─────┼─────┤
│接触脱蝋工程の原料に対する収率│15.3 │27.4 │8.9 │
│(重量%) │ │ │ │
└───────────────┴─────┴─────┴─────┘
脱蝋油を蒸留して3つの異なる基油生成物と1つの中間ラフィネートとに分離した他は実施例2を繰り返した。それらの特性を第4表に示す。
┌─────────────┬────┬────┬────┬────┐
│ │軽質 │中間ラフ│中質 │重質 │
│ │グレード│ィネート│グレード│グレード│
├─────────────┼────┼────┼────┼────┤
│20℃での密度 │806 │811.3│817.5│824.5│
├─────────────┼────┼────┼────┼────┤
│流動点(℃) │<−63│−57 │<−51│−39 │
├─────────────┼────┼────┼────┼────┤
│40℃での動粘度(cSt) │10.4 │ │23.51│42.23│
├─────────────┼────┼────┼────┼────┤
│100℃での動粘度(cSt) │2.746│3.501│4.79 │7.24 │
├─────────────┼────┼────┼────┼────┤
│VI │103 │ │127 │135 │
├─────────────┼────┼────┼────┼────┤
│Noack揮発度 │適用不能│ │6.8 │1.14 │
├─────────────┼────┼────┼────┼────┤
│硫黄含有量(ppm) │<5 ppm│ │<5 ppm│<5 ppm│
├─────────────┼────┼────┼────┼────┤
│飽和物(重量%) │測定せず│ │99.5 │ │
├─────────────┼────┼────┼────┼────┤
│CCSで測定した−40℃ │ │ │5500│ │
│での動力学粘度 │ │ │ cP│ │
├─────────────┼────┼────┼────┼────┤
│接触脱蝋工程の原料に対する│22.6 │8.9 │22.6 │11.1 │
│収率 │ │ │ │ │
└─────────────┴────┴────┴────┴────┘
Claims (8)
- (a)フィッシャー・トロプシュ生成物中の炭素原子数60以上の化合物と炭素原子数30以上の化合物との重量比が少なくとも0.4であり、かつフィッシャー・トロプシュ誘導原料中の化合物の少なくとも50重量%が炭素原子数30以上の化合物であるフィッシャー・トロプシュ誘導原料を25〜70重量%の転化率で水素化分解/水素化異性化する工程、
(b)工程(a)の生成物から、沸点範囲200〜450℃のT10 重量%と沸点範囲400〜650℃のT90 重量%とを有するワックス状ラフィネート生成物を単離する工程、
によるワックス状ラフィネート生成物の製造方法。 - 前記フィッシャー・トロプシュ誘導原料が、ASF−アルファ値(アンダーソン−シュルツ−フローリー連鎖生長ファクター)が少なくとも0.925のC 20 + フラクションを含有するフィッシャー・トロプシュ生成物から誘導される請求項1に記載の方法。
- 前記ワックス状ラフィネート生成物のT90重量%沸点が、550℃未満である請求項1又は2に記載の方法。
- 前記ワックス状ラフィネート生成物の100℃での動粘度が、3〜10cStである請求項1〜3のいずれか1項に記載の方法。
- 請求項1〜4のいずれか1項に記載の方法で得られたワックス状ラフィネート生成物の潤滑基油製造への使用。
- 前記基油が、前記ワックス状ラフィネート生成物の接触脱蝋により製造される請求項5に記載の使用。
- 前記潤滑基油の飽和物フラクション中のシクロパラフィン含有量が、12〜20重量%である請求項6に記載の使用。
- 前記ワックス状ラフィネート生成物の流動点が0℃を越え、かつ該ワックス状ラフィネートが固体状態で窒素の覆い下に基油の製造地域に輸送されたものである請求項5〜7のいずれか1項に記載の使用。
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