TW200413519A - Heavy hydrocarbon composition with utility as a heavy lubricant base stock - Google Patents
Heavy hydrocarbon composition with utility as a heavy lubricant base stock Download PDFInfo
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- TW200413519A TW200413519A TW092127065A TW92127065A TW200413519A TW 200413519 A TW200413519 A TW 200413519A TW 092127065 A TW092127065 A TW 092127065A TW 92127065 A TW92127065 A TW 92127065A TW 200413519 A TW200413519 A TW 200413519A
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- 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
- C10G45/00—Refining of hydrocarbon oils using hydrogen or hydrogen-generating compounds
- C10G45/58—Refining of hydrocarbon oils using hydrogen or hydrogen-generating compounds to change the structural skeleton of some of the hydrocarbon content without cracking the other hydrocarbons present, e.g. lowering pour point; Selective hydrocracking of normal paraffins
- C10G45/60—Refining of hydrocarbon oils using hydrogen or hydrogen-generating compounds to change the structural skeleton of some of the hydrocarbon content without cracking the other hydrocarbons present, e.g. lowering pour point; Selective hydrocracking of normal paraffins characterised by the catalyst used
- C10G45/64—Refining of hydrocarbon oils using hydrogen or hydrogen-generating compounds to change the structural skeleton of some of the hydrocarbon content without cracking the other hydrocarbons present, e.g. lowering pour point; Selective hydrocracking of normal paraffins characterised by the catalyst used containing crystalline alumino-silicates, e.g. molecular sieves
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- 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
- C10G45/00—Refining of hydrocarbon oils using hydrogen or hydrogen-generating compounds
- C10G45/58—Refining of hydrocarbon oils using hydrogen or hydrogen-generating compounds to change the structural skeleton of some of the hydrocarbon content without cracking the other hydrocarbons present, e.g. lowering pour point; Selective hydrocracking of normal paraffins
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- C10G45/00—Refining of hydrocarbon oils using hydrogen or hydrogen-generating compounds
- C10G45/58—Refining of hydrocarbon oils using hydrogen or hydrogen-generating compounds to change the structural skeleton of some of the hydrocarbon content without cracking the other hydrocarbons present, e.g. lowering pour point; Selective hydrocracking of normal paraffins
- C10G45/60—Refining of hydrocarbon oils using hydrogen or hydrogen-generating compounds to change the structural skeleton of some of the hydrocarbon content without cracking the other hydrocarbons present, e.g. lowering pour point; Selective hydrocracking of normal paraffins characterised by the catalyst used
- C10G45/62—Refining of hydrocarbon oils using hydrogen or hydrogen-generating compounds to change the structural skeleton of some of the hydrocarbon content without cracking the other hydrocarbons present, e.g. lowering pour point; Selective hydrocracking of normal paraffins characterised by the catalyst used containing platinum group metals or compounds thereof
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- 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
- C10G65/00—Treatment of hydrocarbon oils by two or more hydrotreatment processes only
- C10G65/02—Treatment of hydrocarbon oils by two or more hydrotreatment processes only plural serial stages only
- C10G65/04—Treatment of hydrocarbon oils by two or more hydrotreatment processes only plural serial stages only including only refining steps
- C10G65/043—Treatment of hydrocarbon oils by two or more hydrotreatment processes only plural serial stages only including only refining steps at least one step being a change in the structural skeleton
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- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M101/00—Lubricating compositions characterised by the base-material being a mineral or fatty oil
- C10M101/02—Petroleum fractions
- C10M101/025—Petroleum fractions waxes
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- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M105/00—Lubricating compositions characterised by the base-material being a non-macromolecular organic compound
- C10M105/02—Well-defined hydrocarbons
- C10M105/04—Well-defined hydrocarbons aliphatic
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- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M171/00—Lubricating compositions characterised by purely physical criteria, e.g. containing as base-material, thickener or additive, ingredients which are characterised exclusively by their numerically specified physical properties, i.e. containing ingredients which are physically well-defined but for which the chemical nature is either unspecified or only very vaguely indicated
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- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M171/00—Lubricating compositions characterised by purely physical criteria, e.g. containing as base-material, thickener or additive, ingredients which are characterised exclusively by their numerically specified physical properties, i.e. containing ingredients which are physically well-defined but for which the chemical nature is either unspecified or only very vaguely indicated
- C10M171/02—Specified values of viscosity or viscosity index
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- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2203/00—Organic non-macromolecular hydrocarbon compounds and hydrocarbon fractions as ingredients in lubricant compositions
- C10M2203/10—Petroleum or coal fractions, e.g. tars, solvents, bitumen
- C10M2203/102—Aliphatic fractions
- C10M2203/1025—Aliphatic fractions used as base material
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- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2205/00—Organic macromolecular hydrocarbon compounds or fractions, whether or not modified by oxidation as ingredients in lubricant compositions
- C10M2205/17—Fisher Tropsch reaction products
- C10M2205/173—Fisher Tropsch reaction products used as base material
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- C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
- C10N2020/00—Specified physical or chemical properties or characteristics, i.e. function, of component of lubricating compositions
- C10N2020/01—Physico-chemical properties
- C10N2020/02—Viscosity; Viscosity index
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- C10N2020/00—Specified physical or chemical properties or characteristics, i.e. function, of component of lubricating compositions
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- C10N2020/065—Saturated Compounds
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- C10N2020/01—Physico-chemical properties
- C10N2020/071—Branched chain compounds
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Description
200413519 Π) 玖、發明說明 【發明所屬之技術領域】 本發明係關於重質烴組成物,其可作爲重質潤滑劑基 料’其藉將 Fischer_Tropscll蠟予以異構化而製得,係關 於重質潤滑劑基料及係關於自此基料製得的重質潤滑劑。 【先前技術】 重質潤滑劑用於高黏度應用,其中,以輕質油爲基礎 的潤滑劑無法提供移動零件(如:重質機械油、齒輪箱、 深度衝壓油和手動傳動齒輪箱)之間足夠潤滑度。重質潤 滑劑藉合倂重質潤滑劑基料(其具重油加工潤滑油品質)和 一或多種潤滑劑添加物而製得。大多數的重質潤滑劑基料 衍生自天然石油並含芳族不飽和物(包括多核芳族物)及含 硫和氮的化合物。這些化合物降低油和重質潤滑劑的黏度 和安定性。精煉此油以移除這些組份會導致產物油的產率 低。重質烷烴可經精煉至不飽和物和雜原子化合物含量低 ,但具有無法接受的高傾倒和霧點。 對於相當純淨或優良品質且至少於使用溫度爲液體且 可作爲或用於重質潤滑劑基料的重質烴組成物有需求存在 〇 美國專利案第6 5 0 9 0,9 8 9號(T 1. e w e】I a等人)揭示一種 烷烴組份的液態烴組成物,其支化指數(以甲基氫百分比 (BI)定出)和支化密集度(藉重覆的伸甲基碳百分比定出, 其爲自末端基團或支鏈移除的四或多個碳(CH2>4),使得 (2) (2)200413519 (a) BI-0.5(CH2>4)>15 ;和 (b) BI+0.85(CH2>4)<45 ; 此係針對整個液態烴組成物測定。美國專利案第 U.S. Patent 6,09 0,9 8 9號之基料特點在於傾倒點(PP)非常低 ,低於或等於· 1 8 °C,1 〇 〇 °C運動黏度範圍較佳,由約4 c S t 至約8cSt。雖然根據美國專利案第6,090,9 8 9號之組成物 作爲重質潤滑劑基料的應用性極佳,但某些應用須使用重 質潤滑劑,特定言之,要求l〇〇°C運動黏度高於8cSt。此 通常須要相當長鏈烴分子在基料中。但是,提高烴混合物 中的烴分子鏈長,通常會提高傾倒或霧點,此非所欲者。 或者,添加物(如:黏度指數改善劑及傾倒和霧點降低劑) 會損及潤滑劑的所欲性質。除使用添加物的花費以外,添 加物不利於使用。因此,本發明的目的是要提出組成物, 其具相當高黏度、良好潤滑性和氧化安定性,但傾倒和霧 點低。 此外,對於可以作爲藥用調合物、化學和藥品製造之 類中之重質白油、藥用油、載體或基礎物的烴組成物一直 有需求存在。這樣的應用通常須要純淨的化學惰性材料, 且,例如,不會引起藥物應用過敏。換言之,對於芳族物 和含雜原子的組份非常少的烴組成物有需求存在。 本發明提出重質煙組成物’其具局黏度及低傾倒和霧 (3) (3)200413519 【發明內容】 本發明係關於相當純淨之品質優良的重質烴組成物, 其可作爲或用於重質潤滑劑基料,係關於重質潤滑劑基料 ’及係關於自此重質潤滑劑基料形成的重質潤滑劑。 此重質烴組成物主要(2 9 8重量%)包含飽和烷烴分子 ’是油狀液體,其1 0 0。(:運動黏度大於8 c S t,初(5 %)沸點 至少 8 5 0 T (4 5 4 t:),終(9 5 %)沸點至少 1,〇 〇 〇 T ( 5 3 8 t:)。 此重質烴組成物包含至少9 5重量%烷烴分子,其中至少 90重量%是異烷烴。異烷烴佔根據本發明之重質烴組成物 之院烴分子的至少9 0重量%。此重質烴組成物含有具連 續碳原子數的烴分子。異烷烴分子的支化程度(以甲基氫 百分比測定,下文中稱爲支化指數(BI))和支鏈的接近度( 或支化密集度)(藉重覆的伸甲基碳百分比測得,其爲自末 端基團或支鏈移除的四或多個碳原子(C Η 2〉4 )),使得: (a) BI-0.5(CH2>4)<:1 5 ;和 (b) BI + 0.85(CH2>4)<45 ; 此係針對整個重質烴組成物測定。此重質烴組成物可 用於或作爲重質潤滑劑基料。 支化密集度(CH2>4)描述烴中的烷烴分子之正烷烴特 性。通常,爲得到良好潤滑性,希望含有某些烷烴分子的 組成物具有相當高的正烷烴特性,即,少數支鏈和/或短 鏈。但是,預期具相當高正烷烴性質的烷烴會提供所不欲 傾倒和霧點,這是因爲正烷烴於相當高溫會自烷烴混合物 結晶出來之故。 (4) (4)200413519 支化指數(以甲基氫百分比測定)是接在骨架上的支鏈 數指標。如果有許多支鏈且支鏈主要是甲基,則此支化指 數高。 例如,就特定總數的碳原子而言,有許多支鏈和長鏈 在短骨架上的烷烴分子(即,相當少正烷烴特徵)的支化密 集度(CH2>4)相當小。具相同碳原子總數但具較少支鏈和 /或支鏈彼此或與末端基團距離較大且具相當長骨架的烷 烴分子(即,具較多正烷烴特徵的烷烴分子)的支化密集度 (CH2>4)相當大。 美國專利案第6,0 90,9 8 9號係關於液態烴組成物,其 中 BI-0.5(CH2〉4)>15。現訝異地發現到,如果卜0卜 0.5 ( C Η 2 > 4 )< 1 5,可得到黏度相當高但傾倒和霧點低的重 質烴組成物。換言之,根據本發明,支化密集度(CH2>4) 比美國專利案第6,090,9 8 9號中舉例的組成物來得大。此 爲意外發現,因爲根據本發明之重質烴組成物含有的烷烴 分子具有更多正烷烴特徵(由相當高的支化密集度得知)並 具非常低的傾倒和霧點。事實上,此發現與一般認爲低傾 倒和霧點須要少量正烷烴和相當大異烷烴特性的認知相反 〇 BI以低於24爲佳,支化密集度(CH2〉4)以大於1 7爲 另一實施例中’本發明係關於重質潤滑劑,其藉由合 倂本發明之重質潤滑劑基料和一或多種潤滑劑添加物而得 。本發明之重質烴組成物可作爲重質潤滑劑基料以外,其 (5) (5)200413519 亦具其他用途,如:藥用調合物、化學和藥品製造之類中 之重質白油、藥用油、載體或基礎物。因此,本發明的另 一實施例包含下列一或多者,或至少一部分用途,或基於 本發明之重質烴組成物:藥用調合物、化學和藥品製造之 類中之重質白油、藥用油、載體或基礎物。 另一實施例中’本發明係關於基料,其包含根據本發 明之重質烴組成物。換言之,此實施例係關於重質烴組成 物於或作爲基料之使用。較佳情況中,根據本發明之基料 由重質烴組成物構成。 圖1是本發明之重質烴組成物、本案的比較例和美國 專利案第6,0 9 0,9 8 9號(如前述者,其包括其他烴組成物) 的數據中之B I和C Η2 > 4百分比(由n M R得知)之關係圖。 ί么將美國專利条弟6,0 9 0,9 8 9號中所揭示者全數列入參考 。圖上的陰影區域定義本發明之重質烴組成物的NMR參 數。僅本發明之重質烴組成物(以衍生自Fischer-Tropsch 合成蠟質烴爲佳)和P A 0基料落在此參數空間區域內。 P A 0基料的分子組成與本發明之重質烴組成物的差別在於 ⑴它們不含具連續碳原子數的烴分子,(ii)分子上的CH3 基團的氫原于百分比低於】5,而本發明之重質烴組成物 的此値以1蜀於2 0爲佳,(i i i) P a 〇基料之得自c Η基團的 氫原子百分比以高於3爲佳,而本發明之重質烴組成物以 低於2爲佳。 實施方式之詳細說明 -9- (6) (6)200413519 本發明提出重質烴組成物,其包含至少9 5重量%烷 烴分子,其中至少90重量%是異烷烴,含有具連續碳原 子數的烴分子,於1 0 爲液體,於此溫度的運動黏度( 藉ASTM D-44 5測得)高於8cSt,初和終沸點分別是至少 8 5 0和1 0 0 0 °F ( 4 5 4和5 3 8 °C ),其中,該異烷烴分子的支 化指數(BI)(以甲基氫百分比測定)和支化密集度(CH2>4)( 藉重覆的伸甲基碳百分比測得,其爲自末端基團或支鏈移 除的四或多個碳原子))使得: (a) BI-0.5(CH2>4)<15 ;和 (b) BI + 0.85(CH2>4)<45 ; 此係針對整個重質烴組成物測定。 較佳情況中,本發明之重質烴組成物製自Fischer-Tropsch鱲,主要(^98重量%)包含飽和烷烴分子,其中 至少90重量%是非環狀烴和不超過1 0重量%環狀烴。至 少90重量%(以至少95重量%爲佳,至少98重量%更佳, 至少99重量%最佳)烷烴分子是異烷烴。烷烴環狀烴存在 量(若有的話)可高至5重量%,基本上不超過1重量%。 本發明之重質烴組成物的1 0 0 °C運動黏度(根據A S 丁 Μ D-44 5測定)大於8cSt。本發明之重質烴組成物含有具連 續碳原子數的分子並以至少9 5重量% C 3 〇 +烴分子爲佳。初 沸點至少8 5 0 °F (4 5 4 t:),以9 0 0 °F (4 8 2 °C )爲佳,終沸點至 少1,000 °F ( 5 3 8 °C )。重質烴組成物於使用溫度和壓力條件 下,基本上是液體,使用溫度和壓力基本上是75 °F (24 °C ) 和〗大氣壓(1〇]1^?3),但並非全然如此。此處所謂的初和 (7) (7)200413519 終沸點値是公稱値,係使用下文所述方法,以藉氣相層析 模擬蒸離(GCD)得到的丁5和T95分餾界限(沸騰溫度)表示 〇 異院烴系烴組份的支化度(以甲基(CH3)氫百分比測定 )或支化指數(BI)(或支化密集度)(藉重覆的伸甲基碳百分 比測得’其爲自末端基團或支鏈移除的四或多個碳原子 (CH2>4)),使得: (a) BI-〇.5(CH2>4)>15 ;和 (b) BI+〇.85(CH2>4)<45 ; 此係針對整個重質烴組成物測定。此 BI以低於 24(BI<24)爲佳,支化密集度以大於i7((CH2>4)>17)爲佳 。此重質烴組成物亦以含有至少75重量%C 3 5 +煙分子爲佳 〇 本發明之重質烴組成物與衍生自石油、散蠟、PAO油 和美國專利案第6,090,98 9號揭示之潤滑劑基料者不同, 其藉由將F i s c h e r - T r 〇 p s c h繼予以異構化而得。 含有硫、氮和金屬的烴化合物中的硫、氮和金屬量低 於5 Owppm。本發明之重質烴組成物製自硫、氮和金屬含 量低於 1 W p p m 的 F i s c h e r - T r 〇 p s c h 蠛。X -射線或 A n t e k Nitrogen試驗無法測得這些物種。 本發明之重質烴組成物是多種分子量烷烴之混合物, 在氫化脫蠟之後,殘餘的正烷烴量低於5重量%,基本上 低於1重量%,至少95重量%油分子含有至少一個支鏈, 其中的至少一半是甲基支鏈。至少一半(至少75 %更佳)剩 (8) (8)200413519 餘支鏈是乙基,較佳情況中,低於支鏈總數的2 5 % (以低 於1 5 %爲佳)具3或更多個碳原子◦支鏈碳原子總數基本 上低於構成烴分子的總碳原子數之25%,以低於20%爲佳 ,不超過15%(如:10-15%)更佳。 PAO油是偶數碳直鏈α烴(典型者是1-癸烯)的低聚反 應產物。此ΡΑΟ油分子因此包含偶數碳烴原子之混合物 ,直鏈α烴起始單體之碳原子數倍增而造成各烴分子之間 的碳原子數之間的差異。即使具偶數個碳原子的直鏈α烴 單體(如:癸烯和十二烯)低聚合形成重質潤滑劑基料油, 所得烴分子中的碳原子數仍爲偶數。此與本發明之重質烴 組成物具連續碳烴分子之混合物不同,其包含具偶數和奇 數碳原子的烴分子,其間的差別在於連續碳數(如:1、2 、3、4 ' 5、6、7和更多個碳原子)。 本發明之重質烴組成物的烴分子彼此不同點在於連續 石灰原卞數’此爲織進料之 F i s c h e 1. - T r 〇 p s c h煙合成反應的 結果,其中,蠟進料被異構化形成本發明之重質烴組成物 。較佳重質烴組成物製自以無機油爲基礎以外的合成來源 ,因此可稱爲合成重質烴組成物,本發明之重質烴組成物 不限於以合成來源爲基礎者。但在較佳實施例中,重質烴 ’下且成物基於合成來源’以基於F i s c h e r - T1. 〇 p s c h產物爲佳 ο 在Fischer-Tr〇Psch烴合成反應中,碳原子來源是CO ’烴分子同時積聚在碳原子上。相對於以ΡΑΟ爲基礎的 油’之後’本發明之重質烴組成物的烴分子具有更多直鏈 -12- (9) (9)200413519 結構,包含相當長骨架及短且少的支鏈。PAO的經典教科 書描述PAO是星狀分子,特別是參(癸烷),其爲三個癸烷 分子接於中心點。理想的星形分子是理論分子,但PAO 分子比本發明之基料中的其他分子具有較少和較長支鏈。 因此,較佳情況中,本發明之重質烴組成物的其他分 子包含至少95重量異烷烴(不超過5重量%飽和環狀物)具 有相當直鏈分子結構,低於半數支鏈具有二或多個碳原子 ,低於存在於支鏈中的碳原子總數的25%。相對於本發明 ,在PAO油的組成中,超過半數支鏈含有二或多個碳原 子且超過25 %碳原子總數處於支鏈中。 如嫻於此技術者已知者,重質潤滑劑基料有時亦稱爲 潤滑或潤滑劑基料(包括重質潤滑劑基料)是在潤;滑油範圍 內沸騰的油,具潤滑品質且可用以製備各式各樣潤滑劑( 如:潤滑油和脂)。本發明中,重質烴組成物在重質潤滑 劑範圍中沸騰。完整調配的重質潤滑劑或重質潤滑油製自 ••在重質潤滑劑基料中添加有效量的至少一種添加物,或 者,更基本地,含有超過一種添加物的添加物組合。這樣 的添加物的說明但非限制例包括一或多種淸潔劑、分散劑 、抗氧化劑、耐磨添加劑、極端壓力添加劑、傾倒點降低 劑、VI改善劑、摩擦修飾劑、乳化劑、抗氧化劑、消沫 劑、腐蝕抑制劑、密封溶脹控制添加劑。 較佳情況中,本發明之重質烴組成物包含脫蠟油,其 低溫性質能夠符合標的專一性或需求且透光和明亮,於使 用溫度和壓力條件下是油狀液體。基本上,其於75 T (24 -13- (10) (10)200413519 °C )和一大氣壓(1 0 ] kP a)的室溫和壓力條件下是油狀液體 ’於此壓力和1 〇 〇 °c爲油狀液體,但並非全然如此。一些 情況中,霧點可高於75°F (24t )。根據本發明製得之本發 明之重質烴組成物的終沸點高於]2 5 0 °F ( 6 7 7 °C ),其霧點 和傾倒點是1 °C和-3 1 °C。重質潤滑劑基料和最終重質潤 滑劑的低溫性質要求可改變並視它們的用途和它們使用的 位置而定。重質烴組成物製自:形成本發明之重質潤滑劑 基料和有效量至少一種添加物(更常是前述含有一種以上 添加物的添加物組合)之混合物。用以形成混合之本發明 之重質潤滑劑基料基本上在氫化脫蠟之後,經溫和氫化處 理和/或除濁處理,以改善其顏色 '外觀和安定性。 如已知者,濁度是混濁度或缺乏澄淸度。去濁處理基 本上藉催化或吸收法移除造成混濁的這些成份而達成。氫 化處理是一種非常溫和、相對低溫的氫化處理法,其使用 觸媒、氫和溫和反應條件移除微量雜原子化合物、芳族物 和烯烴,以改善氧化安定性和顏色。氫化處理反應條件包 括溫度由 3 0 2 至 6 6 2 °F ( 1 5 0 至 3 5 0 t ),以 3 0 2 至 4 8 2 T (150至250 °C)爲佳,總壓力由400至3000psig(2859至 2 0 7 8 6kPa)、每小時空間速度由0 . 1至5 L H S V (小時·1 ),以 0.5 至 3 小時^爲佳。此氫處理時間由 2 5 5 0 至 1 0 00 0scf/B(44.5至1 7 8 0m3/m3)。此觸媒包含載體組份和 一或多種催化性金屬組份(金屬選自 VIB族(Mo、W、C〇 和/或鐵族(Ni、Co)和 VIII族貴金屬(Pt,Pd)。此處的 V I B 和 V 111 族是指 S a r g e n t - W e 1 c h P e r i 〇 d i c T a b 1 e 〇 f -14- (11) (11)200413519
Elements (Sargent-Welch Scientific company 於 1 96 8 年取 得版權)中的VIB和VIII族。以觸媒組成物計,一或多種 金屬存在量少至重量%(貴金屬)至高至30重量%(非貴 金屬)° $父佳載體材料的酸量低,包括,如:非晶狀或晶 狀金屬氧化物(如:氧化鋁、氧化矽、氧化矽氧化鋁)和超 大孔洞晶狀材料(稱爲巨孔晶狀材料,較佳載體組份是 MCM-41之製備和使用揭示於,如:美國專利 案第 5,098,684、 5,227,353 和 5,573,657 號。 繼貝進料或 Fischer-Tropsch 蠟包含 Fischer-Tropsch 烴合成反應器中製得的蠟質烴餾份,其於反應條件爲液體 。其被稱爲蠟,這是因爲其於7 5卞(2 4艽)和;[大氣壓 (1 0 1 kPa)壓力條件下爲固體之故。其必,須含有足夠的蠟質 材料於超過1 0 0 0 °F ( 5 3 8 °C )沸騰,以製造本發明之重質烴 組成物。此蠟質進料基本上於一或多個催化脫蠟步驟(其 中,進料與氫和脫蠟觸媒於脫蠟條件下接觸)脫蠟。此異-與正烷烴比藉G C - F I D (用於含有高至2 0個碳原子的分子 之組成物)和GC-F1D和I3C-NMR之組合(用以測定含有至 少2 0個碳原子之分子之組成物)測知。芳族物藉X _ R a y 螢光(XRF)測定,此如ASTM Standard D-2622中所述者。 硫藉XRF測定(ASTM Standard D-2 6 22),氮藉針筒/輸入 氧化燃燒和化學發光偵測測定(ASTM Standard D-4 62 9)。 氫化脫蠟步驟可用觸媒包含固態酸組份、氫組份和黏 合劑。用於氫化脫蠘的適當觸媒組份之說明但非限制例包 括,如:ZSM-23、ZSM-35、ZSM-48、ZSM-57、ZSM-22 (12) 200413519 或丁〇N和氧化石夕錫磷酸鹽(被稱爲SAP〇,女丨 和4 1 )、s S Z - 3 2、/9沸石、絲光沸石和經 換的鎂鈉針沸石。也可以使用氧化鋁和非晶氧 〇 在有許多其他沸石觸媒的情況中,可能希 份與基質材料(黏合劑,耐得住此處的脫蠟法 其他彳I木件)搶合。迨樣的基材包括活性和非活 成或天然生成沸石及無機材料(如:黏土、矽 屬氧化物(如··氧化鋁))。後者可以是天然生 狀沉澱物、溶膠或凝膠形式,包括矽石和金屬 Cq物。使用材料和固態酸組份(即,與其合倂$ 能夠增進此處的轉化率和/或選擇性。適合地 科作爲稀釋劑’以控制選定方法中的轉化率, 和有規則的方式得到產物,而不須使用控制速 其他方式。通常,晶狀矽酸鹽材料摻入天然占 •膨潤土和高嶺土)中。這些材料(即,黏土、 d分作爲觸媒的黏合劑。因爲在石油精煉中, 處理手法通常較爲粗糙,會使得觸媒碎成粉末 引發加工時的問題,所以希望能夠提供粉碎強 媒。 可以與固態酸組份組合之天然生成的黏土 和高嶺土族,其包括次膨潤土,一般知道的這 有 Dixie ' McNamee、喬治亞(Georgia)和 (F1 〇 r i d a)黏土或其他者,其中,主要礦質構份 3 : S AP 〇 _ 1 1 稀土離子交 化矽氧化鋁 望固態酸組 所用溫度和 性材料及合 石和/或金 成者或凝膠 氧化物之混 _,具活性) 使用惰性材 以便以經濟 率或反應的 i成黏土(如 氧化物··等) 觸媒遭遇的 狀的物質, 度良好的觸 包括蒙脫石 樣的高嶺土 佛羅里達 是敘永石、 -16- (13) (13)200413519 高嶺石、狄克石或富矽高嶺土。這樣的黏土可以原礦的原 始狀態或經鍛燒、酸處理或化學修飾的狀態使用。 除前述材料以外,固態酸組份可以與多孔基材(如: 氧化矽-氧化鋁、氧化矽-氧化鎂、氧化矽一氧化鍩、氧 化矽一氧化钍、氧化矽-氧化鈹、氧化矽一氧化鈦)和三 元組成物(如:氧化矽-氧化鋁-氧化钍、氧化矽—氧化 金呂一氧化鉻、氧化砂一氧化銘一氧化鎂和氧化砂一氧化鎂 -氧化銷)組合。此基質可以共凝膠形式。也可以使用這 些組份之混合物。細粒固態酸組份與無機氧化物凝膠基質 的相對比例變化範圍寬,晶狀矽酸鹽組份由組合劑計之約 1至約9 0重量%,更常是約2至約8 0重量%。以使用 Z S Μ - 4 8 爲佳。 氫化反應組份包含至少一個第VIII族金屬組份,且 以至少一種VIII族貴金屬組份(如·· Pt和Pd)爲佳。以觸 媒總重計(包括ZSMM8沸石組份和觸媒組成物中所用任 何黏合劑),貴金屬濃度由約0 . 1 - 5重量%金屬,更常是約 〇·2-1重量%金屬。此處所謂 VIII族金屬是指Sargent-Welch Periodic Table of Elements (Sargent -Welch S c i e n t i f i c C o m p a n y於1 9 6 8年取得版權)中的V III族。 ZSM-48(ZSM-48 沸石包括 EU-2、EU-11 和 ZBM-30, 其結構k彳寺)之製備已爲習知,並揭不於,如:美國專利 案第4,3 97,82 7、4,5 8 5,74 7和5,07 5,2 6 9號和歐洲專利案 第0 1 42 3 1 7號,茲將其中所揭示者列入參考。可用以實 施本發明的其他氫化脫蠟觸媒包括大多藉異構化反應而非 -17- (14) (14)200413519 藉裂解或氫化裂解脫蠟的任何習知觸媒。包含I 〇和1 2員 環結構的沸石可作爲脫蠟沸石,在與催化性金屬氫化組份 倂用時更是如此。用以製造烴或本發明之重質烴組成物的 氫化脫蠟反應條件包括溫度、氫分壓和空間速度範圍分別 是 450-750 °F (232-399 °C)、10-2,000psig(69-13790kPa)和 0·卜 5.0LHSV。這些條件範圍常是 500-700 T (260-371 °C) 、100-1000psig(690-6895kPa)和 0.5-3.0LHSV,壓力更常 是 200-700psig(1379-4827kPa)。 【實施方式】 實例 實例1 此貫例中’在费料F i s c h e r - T1. 〇 p s c h煙合成反應器(其 含有載有氧化鈦、經鍊促進之非移動鈷烴合成觸媒)中製 得包含4 3 0 °F +(221 °C )蠟質烴餾份的蠟進料。此蠟包含至 少9 0重量%正烷烴和2 6.6重量% 1 0 0 0 T + ( 5 3 8 t:)餾份。其 於ZSMd8氫化脫蠟觸媒存在時,以Pt貴金屬組份脫蠟 ,形成異構物。此異搆物經分餾,移除 7 0 0 °F - ( 3 7 1 °C -)烴 ,剩餘的7〇〇°F +(37 1°C +)餾份之後經分餾以移除和回收 9 5 0 °F + ( 5 1 0 °C +)重質潤滑劑異構物餾份。此重質異構餾份 之後進一步以氫於獨立反應器中以相同的ZSMM8氫化脫 蠘觸媒予以氫化脫蠟,形成本發明之重質烴組成物或重質 潤滑劑基料。在第一和第二個反應器中的氫化脫蠟條件分 別包括溫度 586 F (308 °C )和 616°F (324 °C )及低氯壓 (15) (15)200413519 2 5 0psi( 1 7 2 4 kPa)。這些組成物性質示於附表中,100°C運 動黏度是13和15cSt。 這兩個反應器中的ZSM-48氫化脫蠟觸媒包含0.6重 量%Pt作爲氫化組份位於ZSM-48沸石的氫形式和氧化鋁 黏合劑上。ZSM-48沸石的氫形式根據美國專利案第 5,0 7 5,2 6 9號製得,茲將其中所揭示者列入參考。使用已 知程序,藉浸潤、之後鍛燒和還原地添加Pt組份。 使用ASTM D- 5 3 0 7的高溫GCD法修飾,進行氣相蒸 餾(GCD)。管柱包括具薄液相(低於0.2微米)的單一毛細 管柱。使用外標準,沸點校正範圍由5至1 00個碳。使用 溫度程式化注射器,注射之前,樣品以熱水溫和地溫熱。 使用此方法定出沸騰範圍,得到T5和T9 5 G CD結果。使 用 A S T M D - 5 7 7 3 (用於 P h a s e T w ο T e c I n s t r u m e n t s ),以潤 滑劑常規方法測定霧點値。根據用於 ISL Auto Ροιη· Point測定的 ASTM D- 5 9 5 0 測定傾倒點。下面的附表1 中的霧點和傾倒點單位是°C。黏度和黏度指數係分別根據 A S 丁 M D - 4 5 5 -和 D - 2 2 7 0 測定。 實例2 此實例中,蠟進料是Paraflint C-80,一種市售品, 在固定床 Fischer-Tropsch反應器中,自轉移鐵觸媒藉 S a s ο 1製得之經氫化處理的f i s c h e r - T r 〇 p s c h蠟。此經處理 的原料蠘含有相當高量芳族和脂族不飽和物及雜原子化合 物,其經氫化處理而製得Paraflint C-80蠟。此固態蠟是 -19- (16) (16)200413519 蒸餾餾份,其100°c黏度由6-lOcSt,公稱T5沸點約850 °F (4 5 4 °C )。在有類似於前面使用之p t / z S Μ - 4 8觸媒(但未 經硫化)存在時,其於單一反應器中以氫進行氫化脫蠟。 此氫化脫蠟反應壓力是1 000psi(6 8 9 5 kPa)。此氫化脫蠟產 物經蒸餾分餾,得到本發明之重質烴組成物,其1 〇 〇 °C黏 度是1 1 c S t,其性質亦列於附表中。
比較例A 此試驗類似於實例1,但公稱7 0 0 - 9 5 0 °F (3 7 1 - 5 1 0 °C ) 異構物在獨立反應器中,於相同ZSM-48氫化脫蠟觸媒上 ,以氫進一步氫化脫蠟,形成非本發明之組成物。其100 °C黏度是4cSt。第一和第二個反應器中的氫化脫繼條件分 別是 5 8 6 °F ( 3 0 8 °C )和 5 9 7 °F (3 1 4 °C )及低氫壓 250psi( 1 724kPa)。比較用組成物示於附表中。
比較例B 此進料、觸媒和單一氫化脫蠟反應器類似於實例2。 將蒸餾所得的氫化脫蠟產物予以分餾,製得I 0 0 °C黏度6 和8 cSt的兩種組成物。這兩種組成物皆非本發明之組成 物,列於下面的附表中以便於比較。 - 20- (17) 200413519 本發明 非本發明 黏度loot: llcSt 13cSt 15cSt 8cSt 6cSt 4cSt ]HNMR* %CH3 23.0 21.8 21.5 26.6 25.9 25.4 %ch2 75.5 76.6 76.9 71.4 72.3 72.7 %CH 1.4 1.6 1.6 2.0 1.8 1.9 BI 23.0 21.8 21.5 26.6 25.9 25.4 13C NMR** %CH2>4 18.6 19.7 19.9 11.3 14.6 16.4 BI-0.5 (CH2>4) 13.74 11.98 11.59 20.93 18.6 17.2 BI+0.85 (CH2>4) 38.80 38.55 38.39 36.17 38.3 39.4 傾倒點,°C -39 -32 -32 -60 -40 -22 T5 °F 892 915 942 832 794 713 °C 478 49] 507 444 423 378 T95 °F 1201 1199 1212 1059 992 903 °C 649 648 655 571 rnn JJJ 484
* Η (質子)共振強度百分比係關於C Η 3、C Η 2和C Η氫 * *重覆的伸甲基碳百分比是自末端基團或支鏈移除的四或 多個碳原子 以C- 1 3 NMR光譜儀分析附表中之組成物的微結構。 樣品於C D C 13中製成重量/重量濃度爲2 0 - 2 5 %的溶液, 溶液中並有7.5mg/ml Cr(acac)3。化學位移以TMS設定於 O.Oppm 爲基準。在 Varian Unity Plus 500(碳的 Larmor 頻 率1 2 5 . 7 Μ Η z ’每張光g普掃描8 〇 〇 〇次)上取得光譜。所有 -21 - (18) (18)200413519 光譜以90°激發脈衝,反轉限動WALTZ-〗6去偶合於質子 上(取數據的〇·8秒鐘期間內)’循環遲滯6秒鐘。於50°C 製備樣品和取得數據。選擇數據獲取參數(摻鉻、弛豫衰 減、反轉限動去偶合)’以確保準確和定量積分關係°至 於NMR技巧、數據獲取和計算亦請參考美國專利案第 6,0 90,9 8 9 號。 樣品的質子NMR分析於5mm可切換探頭中進行’約 80mg樣品溶解於lg CDC13中。於50°C製備樣品和取得數 據,使用V a r i a n U n i t y P 1 u s 5 0 0。以6 4次自由誘發衰減 取得數據,此處使用9 0 ^激發脈衝,弛豫衰減8.4秒鐘’ 取數據時間3.2秒鐘。質子NMR中未使用弛豫劑。 這些數據顯示本發明之重質烴組成物(黏度1 1、1 3和 1 5cSt者)的分子中,支化指數(BI)和支化密集性或支化密 集度(C Η 2 > 4 )使得: (a) BI_0.5(CH2>4)<1 5 ;和 (b) BI+0.85(CH2>4)<45 ; 此係針對整個重質烴組成物測定。此外,數據顯示就 本發明之重質烴組成物而言,BI基本上低於25,支化密 集度(CH2>4)基本上大於17。 圖1是BI與% CH2>4値的關係圖,數據得自本發明 之重質烴組成物、本案的比較例之NMR光譜及美國專利 案第6,090,98 9號(其包括其他烴組成物)的數據。茲將美 國專利案第6,0 90,9 8 9號中所揭示者全數列入參考。附圖 中的陰影部分定義出本發明之重質烴組成物的NMR參數 (19) (19)200413519 空間。僅本發明之重質烴組成物(以衍生自F丨s c h e r _
Tropsch合成蠟質烴爲佳)和pA〇基料落在此參數空間範 圍內。P A 0基料的分子組成與本發明之重質烴組成物的不 同點在於:(i)它們不含具連續碳原子數的烴分子,(丨i)分 子上的CH3基團的氫原子百分比低於1 5,而本發明之組 成物的此値基本上高於20,(iii)PAO之得自CH基團的氫 原子百分比高於3,而本發明之重質烴組成物基本上低於 2 〇 【圖式簡單說明】 圖1是BI與% CH2>4値的關係圖,數據得自本發明 之重質烴組成物、本案的比較例之NMR光譜及美國專利 案第650 9 G59 8 9號(其包括其他烴組成物)的數據。 -23-
Claims (1)
- (1) (1)200413519 拾、申請專利範圍 1 · 一種重質烴組成物,其包含至少9 5重量%烷烴分子 ’其中至少9 〇重量%是異烷烴,含有具連續碳原子數的 烴分卞’於1 0 0 °C爲液體,於此溫度的運動黏度(藉A s 丁 Μ D-445測得)高於8cSt,初和終沸點分別是至少“ο和 1 00 0 °F (4 54和5 3 8 °C ),其中,該異烷烴分子的支化指數 (B I)(以甲基氫百分比測定)和支化密集度(c H 2 > 4 )(藉重覆 的伸甲基碳百分比測得,其爲自末端基團或支鏈移除的四 或多個碳原子))使得: (a) BI-0.5(CH2>4)<15 ;和 (b) BI+0.85(CH2>4)<45 ; 此係針對整個重質烴組成物測定。 2 .如申請專利範圍第1項之組成物,其中該支化指數 (B I)低於2 4,該組成物含有至少9 5重量%烴分子具至少 三十個碳原子。 3 ·如申請專利範圍第]項之組成物,其中該支化密集 度(C Η 2 > 4 )大於 1 7。 4 ·如申請專利範圍第]至3項中任一項之組成物,其 中該異烷烴分子的不到半數支鏈具二或更多個碳原子。 5 ·如申請專利範園第1至3項中任一項之組成物,其 中該異烷烴分子中之低於碳原子總數的25%存在於該支鏈 中0 6 ·如申請專利範圍第1至3項中任一項之組成物,其 中包含至少9 8重量%飽和的烷烴,其中至少9 0重量%是 -24 - (2) (2)200413519 非環狀烴且不超過5重量%環狀烴。 7 .如申請專利範圍第】至3項中任一項之組成物,其 中低於該支鏈總數的2 5 %具有三或更多個碳原子。 8 ·如申請專利範圍第1至3項中任一項之組成物,其 中低於該支鏈總數的1 5 %具有三或更多個碳原子。 9 ·如申請專利範圍第1至3項中任一項之組成物,其 終沸點高於1 0 5 0 °F ( 5 6 6 °C )。 1 〇 ·如申請專利範圍第1至3項中任一項之組成物, 其中包含至少95重量%烴具30或更多個碳原子。 1 1 ·如申請專利範圍第1至3項中任一項之組成物, 其τ 5沸點至少9 0 0 °F。 1 2 ·如申請專利範圍第1至3項中任一項之組成物, 其中該異烷烴分子中總碳原子數的2 5 %以下存在於該支鏈 中。 1 3 .如申請專利範圍第1至3項中任一項之組成物, 其經氫化處理及視情況地經去濁處理。 1 4 ·如申請專利範圍第]至3項中任一項之組成物, 其於75°F (2 4t )和一大氣壓(]〇】kPa)壓力條件下爲液體。 1 5 .如申請專利範圍第]至3項中任一項之組成物, 其於一大氣壓(1 〇 1 k P a)壓力下的霧點和傾倒點(根據A S Τ Μ D - 5 7 7 3 和 A S T M D - 5 9 5 0 測定)分別局於 7 5 °F (2 4 °c )。 1 6 .如申請專利範圍第1戔3項中任一項之組成物, 其爲合成組成物。 ]7 .如申請專利範圍第1荽3項中任一項之組成物, -25- (3)200413519 其用於或作 、藥用油、 製造法中之 ]8 •如申 其用以降低 19. 一 種 至3項中任 20· — 種 之重質潤滑 爲藥用調合物中之重質潤滑劑基料、重質白油 載體或基礎物中之一或多者及作爲化學和藥品 組份。 請專利範圍第]至3項中任一項之組成物’ 重質潤滑劑基料的傾倒點和霧點。 重質潤滑劑基料,其包含如申請專利範圍第1 一項之組成物。 重質潤滑劑,其包含如申請專利範圍第1 8項 劑基料及一或多種潤滑劑添加物。 -26-
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US6846778B2 (en) * | 2002-10-08 | 2005-01-25 | Exxonmobil Research And Engineering Company | Synthetic isoparaffinic premium heavy lubricant base stock |
US7018525B2 (en) * | 2003-10-14 | 2006-03-28 | Chevron U.S.A. Inc. | Processes for producing lubricant base oils with optimized branching |
-
2002
- 2002-10-08 US US10/266,344 patent/US6846778B2/en not_active Expired - Lifetime
-
2003
- 2003-08-29 US US10/652,389 patent/US7241375B2/en active Active
- 2003-09-30 TW TW092127065A patent/TW200413519A/zh unknown
- 2003-09-30 AR ARP030103562A patent/AR041442A1/es unknown
- 2003-10-06 MY MYPI20033803A patent/MY127782A/en unknown
- 2003-10-07 CN CNB2003801011709A patent/CN100510032C/zh not_active Expired - Fee Related
-
2005
- 2005-03-29 ZA ZA200502513A patent/ZA200502513B/en unknown
Also Published As
Publication number | Publication date |
---|---|
ZA200502513B (en) | 2006-02-22 |
CN100510032C (zh) | 2009-07-08 |
MY127782A (en) | 2006-12-29 |
CN1703499A (zh) | 2005-11-30 |
AR041442A1 (es) | 2005-05-18 |
US20050150815A1 (en) | 2005-07-14 |
US6846778B2 (en) | 2005-01-25 |
US20040067856A1 (en) | 2004-04-08 |
US7241375B2 (en) | 2007-07-10 |
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