CN1207375C - 稳定的氢化处理及氢化脱蜡润滑剂组合物 - Google Patents
稳定的氢化处理及氢化脱蜡润滑剂组合物 Download PDFInfo
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- CN1207375C CN1207375C CNB001176412A CN00117641A CN1207375C CN 1207375 C CN1207375 C CN 1207375C CN B001176412 A CNB001176412 A CN B001176412A CN 00117641 A CN00117641 A CN 00117641A CN 1207375 C CN1207375 C CN 1207375C
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- Prior art keywords
- acid
- alkyl
- formula
- weight
- hydrogen
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- 239000000203 mixture Substances 0.000 title claims abstract description 138
- 230000001050 lubricating effect Effects 0.000 title description 2
- ZZUFCTLCJUWOSV-UHFFFAOYSA-N furosemide Chemical compound C1=C(Cl)C(S(=O)(=O)N)=CC(C(O)=O)=C1NCC1=CC=CO1 ZZUFCTLCJUWOSV-UHFFFAOYSA-N 0.000 title 1
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- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 12
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- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 44
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- 229910052757 nitrogen Inorganic materials 0.000 claims description 29
- NISAHDHKGPWBEM-UHFFFAOYSA-N 2-(4-nonylphenoxy)acetic acid Chemical compound CCCCCCCCCC1=CC=C(OCC(O)=O)C=C1 NISAHDHKGPWBEM-UHFFFAOYSA-N 0.000 claims description 23
- 125000002252 acyl group Chemical group 0.000 claims description 20
- 238000000034 method Methods 0.000 claims description 19
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- 125000004432 carbon atom Chemical group C* 0.000 claims description 13
- 125000001118 alkylidene group Chemical group 0.000 claims description 10
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- QRUDEWIWKLJBPS-UHFFFAOYSA-N benzotriazole Chemical compound C1=CC=C2N[N][N]C2=C1 QRUDEWIWKLJBPS-UHFFFAOYSA-N 0.000 claims description 7
- 239000012964 benzotriazole Substances 0.000 claims description 7
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- FANGQVKSFHFPBY-UHFFFAOYSA-N 2-(3,5-ditert-butyl-4-hydroxyphenyl)propanoic acid Chemical compound OC(=O)C(C)C1=CC(C(C)(C)C)=C(O)C(C(C)(C)C)=C1 FANGQVKSFHFPBY-UHFFFAOYSA-N 0.000 claims description 6
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 6
- 125000005313 fatty acid group Chemical group 0.000 claims description 5
- 125000002887 hydroxy group Chemical group [H]O* 0.000 claims description 5
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 claims description 5
- 229910052717 sulfur Inorganic materials 0.000 claims description 5
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- QTBSBXVTEAMEQO-UHFFFAOYSA-M Acetate Chemical compound CC([O-])=O QTBSBXVTEAMEQO-UHFFFAOYSA-M 0.000 claims description 4
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- NQPDZGIKBAWPEJ-UHFFFAOYSA-N pentanoic acid group Chemical group C(CCCC)(=O)O NQPDZGIKBAWPEJ-UHFFFAOYSA-N 0.000 claims description 4
- 230000003449 preventive effect Effects 0.000 claims description 4
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims description 3
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- DIOYAVUHUXAUPX-KHPPLWFESA-N Oleoyl sarcosine Chemical compound CCCCCCCC\C=C/CCCCCCCC(=O)N(C)CC(O)=O DIOYAVUHUXAUPX-KHPPLWFESA-N 0.000 claims description 3
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- CETNXHGFXDQNQK-UHFFFAOYSA-N CCCCCCCCCCCCCCCCCCC(C)(C)C1=CC=CC=[C+]1 Chemical compound CCCCCCCCCCCCCCCCCCC(C)(C)C1=CC=CC=[C+]1 CETNXHGFXDQNQK-UHFFFAOYSA-N 0.000 claims description 2
- BACYUWVYYTXETD-UHFFFAOYSA-N N-Lauroylsarcosine Chemical group CCCCCCCCCCCC(=O)N(C)CC(O)=O BACYUWVYYTXETD-UHFFFAOYSA-N 0.000 claims description 2
- UEDBHEFYEKZZBA-UHFFFAOYSA-N ac1np5zy Chemical compound C1=CC=[C+]=C[CH]1 UEDBHEFYEKZZBA-UHFFFAOYSA-N 0.000 claims description 2
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- 125000000623 heterocyclic group Chemical group 0.000 claims description 2
- GPRLSGONYQIRFK-UHFFFAOYSA-N hydron Chemical compound [H+] GPRLSGONYQIRFK-UHFFFAOYSA-N 0.000 claims description 2
- 125000000896 monocarboxylic acid group Chemical group 0.000 claims description 2
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- 108700004121 sarkosyl Proteins 0.000 claims description 2
- 230000000087 stabilizing effect Effects 0.000 abstract description 2
- LEPSDPCROOMBQG-UHFFFAOYSA-N 1h-1,2,4-triazol-5-ylmethanamine Chemical class NCC=1N=CNN=1 LEPSDPCROOMBQG-UHFFFAOYSA-N 0.000 abstract 1
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- 238000012360 testing method Methods 0.000 description 15
- FBPFZTCFMRRESA-FSIIMWSLSA-N D-Glucitol Natural products OC[C@H](O)[C@H](O)[C@@H](O)[C@H](O)CO FBPFZTCFMRRESA-FSIIMWSLSA-N 0.000 description 14
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 14
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 13
- 239000011575 calcium Substances 0.000 description 13
- 229910052791 calcium Inorganic materials 0.000 description 13
- 239000000843 powder Substances 0.000 description 13
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 12
- 125000000217 alkyl group Chemical group 0.000 description 12
- 238000012065 two one-sided test Methods 0.000 description 12
- 229920000223 polyglycerol Polymers 0.000 description 11
- RZRNAYUHWVFMIP-GDCKJWNLSA-N 3-oleoyl-sn-glycerol Chemical compound CCCCCCCC\C=C/CCCCCCCC(=O)OC[C@H](O)CO RZRNAYUHWVFMIP-GDCKJWNLSA-N 0.000 description 10
- 150000001412 amines Chemical class 0.000 description 10
- DMBHHRLKUKUOEG-UHFFFAOYSA-N diphenylamine Chemical compound C=1C=CC=CC=1NC1=CC=CC=C1 DMBHHRLKUKUOEG-UHFFFAOYSA-N 0.000 description 10
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- CAZLTUHSNPYDLT-UHFFFAOYSA-N octadecanoic acid propane-1,2,3-triol Chemical class C(CCCCCCCCCCCCCCCCC)(=O)O.C(CCCCCCCCCCCCCCCCC)(=O)O.C(CCCCCCCCCCCCCCCCC)(=O)O.C(CCCCCCCCCCCCCCCCC)(=O)O.OCC(O)CO CAZLTUHSNPYDLT-UHFFFAOYSA-N 0.000 description 1
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- KKEYFWRCBNTPAC-UHFFFAOYSA-L terephthalate(2-) Chemical compound [O-]C(=O)C1=CC=C(C([O-])=O)C=C1 KKEYFWRCBNTPAC-UHFFFAOYSA-L 0.000 description 1
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- 125000002769 thiazolinyl group Chemical group 0.000 description 1
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- CWERGRDVMFNCDR-UHFFFAOYSA-N thioglycolic acid Chemical compound OC(=O)CS CWERGRDVMFNCDR-UHFFFAOYSA-N 0.000 description 1
- 238000004448 titration Methods 0.000 description 1
- 125000002889 tridecyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
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- 235000015112 vegetable and seed oil Nutrition 0.000 description 1
- 239000008158 vegetable oil Substances 0.000 description 1
Classifications
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Abstract
本发明涉及稳定化以防止热和氧有害作用的润滑剂组合物。该组合物包括氢化处理或氢化脱蜡的油和有效抗氧化剂稳定量的酚类抗氧化剂混合物;N,N-二取代氨基甲基-1,2,4-三唑;芳胺抗氧化剂;烷基苯氧基链烷酸;及N-酰基肌氨酸衍生物。任选可向主体润滑剂组合物中加入另外的添加剂。
Description
本发明涉及稳定化的防止热和氧的有害作用的润滑剂组合物,所述组合物包括氢化处理或氢化脱蜡油和有效抗氧化稳定量的酚类抗氧化剂;N,N-二取代的氨基甲基-1,2,4-三唑;芳胺抗氧化剂;烷基苯氧基链烷酸;及N-酰基肌氨酸衍生物的混合物。
本组合物可用于工业润滑剂应用如压缩机、液压传动装置、涡轮机油等中。
已知润滑剂容易分解,因此要求加入各种稳定剂和其它添加剂以改善性能特征。润滑剂的降解主要缘于热、机械应力,特别是由剪切力引起的应力,和化学试剂特别是大气中的氧的作用。润滑剂变坏导致总酸度增加、形成胶、褪色及机械性能如粘度损失、力量损失、聚合、腐臭和/或不好的气味。在高温使用润滑油的情况下,特别要求润滑剂抗氧化,特别是将淤浆的形成和润滑油总酸度的增加以及随之发生的润滑油和润滑体系的总体润滑能力的降低降至最小。
因此,向润滑剂中加入稳定剂以延缓或消除降解,由此延长润滑剂的寿命。例如,美国专利说明书(USP)5,580,482涉及到甘油三酯油经历氧化降解时通过加入N,N-二取代氨基甲基-1,2,4-三唑或N,N-二取代氨基甲基苯并三唑;十二碳烯琥珀酸的高级烷基取代的酰胺;酚类抗氧化剂;和芳胺抗氧化剂的稳定作用。USP 4,652,385公开通过向其中加入亚磷酸盐或二亚磷酸盐和位阻酚抗氧化剂稳定氢化处理的油。
现在已经发现在氢化处理或氢化脱蜡油中引入某些金属去活化剂、金属防腐蚀剂、位阻酚抗氧化剂、芳胺抗氧化剂的组合物得到令人惊讶的优异性能特征。
根据本发明的一个目的是通过向其中引入稳定剂组合物提供满足氧化、腐蚀和热稳定性、使用稳定性和钙相容性要求的润滑剂组合物。
根据本发明的另一个目的是通过向其中引入稳定有效量的稳定剂混合物提供稳定润滑剂的方法。
本发明涉及稳定化以防止热和氧有害作用的润滑剂组合物,该组合物包括
(a)氢化处理的油或氢化脱蜡的油;
(b)(i)有效稳定量式(I)的金属去活化剂:
其中R1为氢或C1-C12烷基,并且R2和R3彼此独立地为氢、C1-C20烷基、C3-C20烯基、C5-C12环烷基、C7-C13芳烷基、C6-C10芳基、羟基,或者R2和R3和与之相连的氮形成5-、6-或7-元杂环残基或者R2和R3分别为式(II)的残基:
R4X[(亚烷基)O]n(亚烷基)- (II)
其中X为O、S或N;R4为氢或C1-C20烷基;亚烷基为C1-C12亚烷基残基;并且n为0或1-6的整数;或者R2如上定义而R3为式(III)的残基:
或者R3为如上定义式(II)的残基而R2为式(IV)的残基:
-[亚烷基]n-N(R5)-A-[N(R5)2]m (IV)
其中m为0或1,并且当m为0时,A为式(III)的残基,而当m为1时,A为亚烷基或C6-C10亚芳基;亚烷基和n具有上述含义;并且R5为式(III)的残基,如上定义;或者
(ii)有效稳定量的式(V)的金属去活化剂:
其中R2和R3定义如上;
(c)有效稳定量的位阻酚抗氧化剂;
(d)有效稳定量的芳胺抗氧化剂;
(e)有效稳定量的式(VI)的烷基苯氧基链烷酸:
其中R6,R7,R8,R9和R10彼此独立地为氢或C1-C20烷基,并且Y为二价的C1-C20烃基,饱和或不饱和的,选自:
和-CH2-CH2-CH2-;和
(f)有效稳定量的式(VII)的N-酰基肌氨酸衍生物:
其中酰基R11-C(=O)-为含有10-20个碳原子的脂肪酸残基,并且X+为氢离子、碱金属离子或铵离子。
本发明组合物是由氢化处理或氢化脱蜡的润滑油制备的。氢化处理的油是在活性沸石催化剂存在下由经历了两级高氢压氢化处理过程的真空粗柴油馏分制备的。USP 3,493,493;3,562,149;3,761,388;3,763,033;3,764,518;3,803,027;3,941,680和4,285,804的公开内容提供了这种氢化处理方法的各种细节,在此引入这些专利作为参考。在典型氢化处理过程的第一阶段,氢气压力在20MPa左右而温度保持在约390℃,使用负载在硅铝载体上的氟化处理的Ni-W催化剂;几乎完全将含氮、硫和氧的化合物从进料中除去,其它影响包括芳烃的高饱和度和多环中间体的高度开环。将第一阶段的润滑油馏分脱蜡,并在低于第一阶段的温度在催化剂如负载在硅铝载体上的Ni-W存在下经历进一步的氢化处理。芳烃和烯烃在该阶段进一步被饱和。产物油基本不含硫或氮,并且只含痕量的芳烃,基本完全由包括烷属烃和环烷属烃的饱和物组成。该组合物也可用在溶剂精制的基料中。
氢化脱蜡油是通过在多层催化剂体系存在下使基料与氢气接触由氢化裂解的溶剂脱蜡润滑油基料制备的。在第一层中,使用例如硅铝酸盐催化剂将氢化裂解溶剂脱蜡的基料催化脱蜡。在第二层中,使用例如带有矾土或硅土基体的钯氢化处理催化剂将催化脱蜡的基料加氢精制。USP 4,822,476公开了该方法的细节,在此引入该专利作为参考。
用于本发明的金属去活化剂为式(I)的N,N-二取代氨基甲基苯并三唑或N,N-二取代氨基甲基-1,2,4-三唑或其混合物。可向这些混合物或产物中加入未取代的甲苯三唑或苯并三唑。N,N-二取代氨基甲基苯并三唑可由已知方法制备,如例如USP 4,701,273所述,例如使苯并三唑与甲醛和胺、HNR2R3反应,优选R1为氢或甲基。N,N-二取代氨基甲基-1,2,4-三唑化合物可由类似方法制备,即使1,2,4-三唑与甲醛和胺、HNR35R36反应,如USP 4,734,209所述。
优选金属去活化剂为1-[二(2-乙基己基)氨基甲基-4-甲基]苯并三唑或1-[二(2-乙基己基)氨基甲基]-1,2,4-三唑,分别以产品名IRGAMET39和IRGAMET30由CIBA提供。
在整个说明书中用CIBA商标和产品名标识的产物是从瑞士巴塞尔的CIBA Ltd.或CIBA Corporation,Tarrytown,纽约获得的。
构成本发明润滑剂组合物组分(c)的位阻酚抗氧化剂是已知的并且包括,但不限于下列化合物或化合物种类:
烷基化单酚
2,6-二叔丁基-4-甲基苯酚、2,6-二叔丁基苯酚、2-叔丁基-4,6-二甲基苯酚、2,6-二叔丁基-4-乙基苯酚、2,6-二叔丁基-4-正丁基苯酚、2,6-二叔丁基-4-异丁基苯酚、2,6-二环戊基-4-甲基苯酚、2-(β-甲基环己基)-4,6-二甲基苯酚、2,6-二(十八烷基)-4-甲基苯酚、2,4,6-三环己基苯酚、2,6-二叔丁基-4-甲氧基甲基苯酚、邻叔丁基苯酚。
烷基化氢醌
2,6-二叔丁基-4-甲氧基苯酚、2,5-二叔丁基氢醌、2,5-二叔戊基氢醌、2,6-二苯基-4-十八烷氧基苯酚。
羟基化硫代二苯醚
2,2’-硫代-二(6-叔丁基-4-甲基苯酚)、2,2’-硫代-二(4-辛基苯基)、4,4’-硫代-二(6-叔丁基-3-甲基苯酚)、4,4’-硫代-二(6-叔丁基-2-甲基苯酚)。
亚烷基双酚
2,2’-亚甲基-二(6-叔丁基-4-甲基苯酚)、2,2’-亚甲基-二(6-叔丁基-4-乙基苯酚)、2,2’-亚甲基-二(4-甲基-6-(α-甲基环己基)-苯酚)、2,2’-亚甲基-二(4-甲基-6(α-甲基环己基-苯酚)、2,2’-亚甲基-二(4-甲基-6-环己基苯酚)、2,2’-亚甲基-二(6-壬基-4-甲基苯酚)、2,2’-亚甲基-二(4,6-二叔丁基苯酚)、2,2’-亚乙基-二(4,6-二叔丁基苯酚)、2,2’-亚乙基-二(6-叔丁基-4-或-5-异丁基苯酚)、2,2’-亚甲基-二(6-(α-甲基苄基)-4-壬基苯酚)、2,2’-亚甲基-二(6-(α,α-二甲基苄基)-4-壬基苯酚)、4,4’-亚甲基-二(2,6-二叔丁基苯酚)、4,4’-亚甲基-二(6-叔丁基-2-甲基苯酚)、1,1-二(5-叔丁基-4-羟基-2-甲基苯酚)丁烷、2,6-二(3-叔丁基-5-甲基-2-羟基苄基)-4-甲基苯酚、1,1,3-三(5-叔丁基-4-羟基-2-甲基苯基)-3-正十二烷基)巯基丁烷、乙二醇-二[3,3-二(3’-叔丁基-4’-羟基苯基)丁酸酯]、二(3-叔丁基-4-羟基-5-甲基苯基)-二环戊二烯、二[2-(3’-叔丁基-2’-羟基-5’-甲基苄基)-6-叔丁基-4-甲基苯基]对苯二甲酸酯。
苄基化合物
1,3,5-三(3,5-二叔丁基-4-羟基苄基)-2,4,6-三甲基苯、二(3,5-二叔丁基-4-羟基苄基)硫醚、3,5-二叔丁基-4-羟基苄基巯基乙酸异辛基酯、二(4-叔丁基-3-羟基-2,6-二甲基苄基)二硫代对苯二甲酸酯、1,3,5-三(3,5-二叔丁基-4-羟基苄基)异氰脲酸酯、1,3,5-三(4-叔丁基-3-羟基-2,6-二甲基苄基)异氰脲酸酯、3,5-二叔丁基-4-羟基苄基膦酸二(十八烷基)酯、3,5-二叔丁基-4-羟基苄基膦酸单乙酯钙盐。
酰氨基苯酚
4-羟基月桂酸苯胺、4-羟基硬脂酸苯胺、2,4-二辛基巯基-6-(3,5-二叔丁基-4-羟基酰苯胺基)-s-三嗪、N-(3,5-二叔丁基-4-羟基苯基)氨基甲酸辛酯等;
β-(3,5-二叔丁基-4-羟基苯基)丙酸与单或多羟基醇的酯,所述醇为例如甲醇、异辛醇、2-乙基己醇、二甘醇、十八碳醇、三甘醇、1,6-己二醇、季戊四醇、新戊二醇、三羟乙基异氰脲酸酯、硫代二甘醇、二羟乙基草酰二胺;
β-(5-叔丁基-4-羟基-3-甲基苯基)丙酸与单或多羟基醇的酯,所述醇为例如甲醇、异辛醇、2-乙基己醇、二甘醇、十八碳醇、三甘醇、1,6-己二醇、季戊四醇、新戊二醇、三羟乙基异氰脲酸酯、硫代二甘醇、二羟乙基草酰二胺;
β-(3,5-二叔丁基-4-羟基苯基)丙酸的酰胺,例如N,N’-二(3,5-二叔丁基-4-羟基苯基丙酰基)六亚甲基二胺、N,N’-二(3,5-二叔丁基-4-羟基苯基丙酰基)三亚甲基二胺、N,N’-二(3,5-二叔丁基-4-羟基苯基丙酰基)肼;
特别令人感兴趣的位阻酚选自2,6-二叔丁基苯酚(IRGANOXL 140,CIBA)、BHT、2,2’-亚甲基二(4,6-二叔丁基苯酚)、1,6-六亚甲基-二(3,5-二叔丁基-羟基氢化肉桂酸酯)(IRGANOXL 109,CIBA)、((3,5-二(1,1-二甲基乙基)-4-羟基苯基)甲基)硫代)乙酸、C10-C14异烷基酯(IRGANOXL 118,CIBA)、3,5-二叔丁基-4-羟基氢化肉桂酸、C7-C9烷基酯(IRGANOXL 135,CIBA)、四(3-(3,5-二叔丁基-4-羟基苯基)丙酰氧基甲基)甲烷(IRGANOXL 1010,CIBA)、硫代二亚乙基二(3,5-叔丁基-4-羟基氢化肉桂酸酯)(IRGANOXL 1035,CIBA)、十八烷基-3,5-二叔丁基-4-羟基氢化肉桂酸酯)(IRGANOXL 1076,CIBA)和2,5-二叔丁基氢醌。这些产品是已知的并且有市售。最令人感兴趣的是3,5-二叔丁基-4-羟基氢化肉桂酸-C7-C9烷基酯。
构成本发明润滑剂组合物组分(e)的芳胺抗氧化剂是已知的并且包括,但不限于下列化合物:
N,N’-二异丙基对苯二胺、N,N’-二仲丁基对苯二胺、N,N’-二(1,4-二甲基戊基)对苯二胺、N,N’-二(1-乙基-3-甲基戊基)对苯二胺、N,N’-二(1-甲基庚基)对苯二胺、N,N’-二环己基对苯二胺、N,N’-二苯基对苯二胺、N,N’-二(萘基-2-)对苯二胺、N-异丙基-N’-苯基对苯二胺、N-(1,3-二甲基丁基)-N’-苯基对苯二胺、N-(1-甲基庚基)-N’-苯基对苯二胺、N′-环己基-N’-苯基对苯二胺、4-(对甲苯磺酰氨基)二苯胺、N,N’-二甲基-N,N’-二仲丁基对苯二胺、二苯胺、N-烯丙基二苯胺、4-异丙氧基二苯胺、N-苯基-1-萘胺、N-苯基-2-萘胺、辛基化二苯胺如p,p’-二叔辛基二苯胺、4-正丁基氨基苯酚、4-丁酰氨基苯酚、4-壬酰氨基苯酚、4-十二烷酰氨基苯酚、4-十八烷酰氨基苯酚、二(4-甲氧基苯基)胺、2,6-二叔丁基-4-二甲氨基甲基苯酚、2,4’-二氨基二苯基甲烷、4,4’-二氨基二苯基甲烷、N,N,N’,N’-四甲基-4,4’-二氨基二苯基甲烷、1,2-二(苯基氨基)乙烷、1,2-二[(2-甲基苯基)氨基]乙烷、1,3-二(苯基氨基)丙烷、邻甲苯基双胍、二[4-(1’,3’-二甲基丁基)苯基]胺、叔辛基化N-苯基-1-萘胺、单和二烷基化叔丁基/叔辛基二苯胺的混合物、2,3-二氢-3,3-二甲基-4H-1,4-苯并噻嗪、吩噻嗪、N-烯丙基吩噻嗪、叔辛基化吩噻嗪、3,7-二叔辛基吩噻嗪。
润滑剂组合物的组分(d)包括式(VIII)的优选芳胺抗氧化剂基团:
其中R12和R13彼此独立地为氢或C1-C24烷基,优选R12为氢且R13为氢或C8-C13烷基。还有特别感兴趣的是式(IX)的化合物,
其中R14,R15和R16彼此独立地氢或C1-C24烷基,并且优选为氢或C4-C18烷基。最令人感兴趣的是芳胺稳定剂包括烷基化二苯胺的混合物,以使R14、R15和R16分别为氢、C4H9和C8H17。这些芳胺稳定剂是已知的,有些有市售,且在例如USP 4,824,601中有述。
润滑剂组合物的组分(e)包括式VI的烷基苯氧基链烷酸。这些化合物本身是已知的,许多都有市售。实例包括苯氧基乙酸、对甲基苯氧基乙酸、对异丙基苯氧基乙酸、对辛基苯氧基乙酸、对壬基苯氧基乙酸、对十二烷基苯氧基乙酸、对(α-甲基-甲基-十九烷基)苯氧基乙酸、对叔戊基苯氧基乙酸、2,4-二叔戊基苯氧基乙酸、2,4-二仲戊基苯氧基乙酸、2,4-二壬基苯氧基乙酸和2-甲基-6-叔丁基苯氧基乙酸。优选C5-C18烷基苯氧基链烷酸如对叔戊基苯氧基乙酸、对辛基苯氧基乙酸、对壬基苯氧基乙酸、对十二烷基苯氧基乙酸和2,4-二壬基苯氧基乙酸。最优选对壬基苯氧基乙酸。
润滑剂组合物的组分(f)包括式VII的N-酰基肌氨酸衍生物。这些化合物本身是已知的,其中许多有市售。这类化合物的代表是月桂酰肌氨酸、棕榈酰肌氨酸、油酰肌氨酸、硬脂酰肌氨酸、妥尔油酰基肌氨酸及相应的肌氨酸碱金属或铵盐。优选的肌氨酸化合物为其中酰基基团含有12-18个碳原子者。最优选其中R11为-C17H33而X为氢者。
任选的组分
除了组分a)-f),本润滑剂组合物还可包括下列任选的组分:
有效稳定量的多元醇部分酯。适宜的多元醇部分酯选自单和二甘油酯、单乙酰基化和二乙酰基化的单甘油酯、多甘油脂肪酸酯、山梨糖醇脂肪酸酯和聚氧乙烯山梨糖醇的部分脂肪酸酯。适宜的单和二甘油酯是通过用含有8-20偶数个碳原子的饱和或不饱和羧酸的一个或两个酸残基酯化一个或两个羟基基团而衍生自甘油的。
酯化多甘油基体结构的含有8-20偶数个碳原子的饱和羧酸的酸基团优选是直链的且含有12、14、16或18个碳原子,例如正十二烷酰基、正十四烷酰基、正十六烷酰基或正十八烷酰基。
酯化甘油基体结构的含有8-20偶数个碳原子的不饱和羧酸的酸基团优选是直链的且含有12、14、16或18个碳原子和一个双键,例如9-顺-十二烯酰基、9-顺-十四烯酰基、9-顺-十六烯酰基或9-顺-十八烯酰基。
下列名称对所提及的酸基团也是常用的:9-顺-十二烯酰基(月桂烯酰基)、9-顺-十四烯酰基(肉豆蔻脑酰基)、9-顺-十六烯酰基(棕榈油酰基)、6-顺-十八烯酰基(岩芹酰基)、6-反-十八烯酰基(petroselaidoyl)、9-顺-十八烯酰基(油酰基)、9-反-十八烯酰基(反油酰基)、11-顺-十八烯酰基(11-十八烯酰基)、9-顺-二十烯酰基(gadoleoyl)、正-十二烷酰基(月桂酰基)、正-十四烷酰基(肉豆蔻酰基)、正-十六烷酰基(棕榈酰基)、正-十八烷酰基(硬脂酰基)、正-二十烷酰基(花生酰基)。
特别适宜的单和二甘油酯以商品名LoxiolG 10和G 16(Henkel)、Nutrisoft100(Grunau)、Kessco GMO(Akzo)和Ede-norGMO,GDO(Henkel)、Emerest 2421(Henkel)有售。
适宜的单乙酰化或二乙酰化单甘油酯为除酰基或脂肪酸外优选带有一个或两个乙酰基的单甘油酯。酰基优选衍生自上述带有大于十的偶数个碳原子的不饱和脂肪酸之一。使用常规分离方法如分馏由单乙酰化或二乙酰化单甘油酯的混合物获得的单甘油酯是优选的。
以商品名MYVACET(Eastman)所售的乙酰化单甘油酯是特别优选的。工业上使用MYVACET系列乙酰化甘油酯作为润滑剂、增塑剂、非离子型乳化剂和增溶剂。特别优选以商品名MYVACET 5-07,7-00,7-07,9-08,9-40和9-45K所售的产品。
适宜的多甘油脂肪酸酯由基本上纯的多甘油脂肪酸酯或不同多甘油脂肪酸酯的混合物组成,其中多甘油基体结构包括优选最多且包括10个甘油单元,它们被1-10个上述带有8-20偶数个碳原子的饱和或不饱和羧酸的酸基团酯化。
具有均一规定结构的适宜多甘油脂肪酸酯为例如二甘油单癸酸酯、二甘油单月桂酸酯、二甘油二异硬脂酸酯、二甘油单硬脂酸酯、二甘油四硬脂酸酯(2-四硬脂酸多甘油酯)、三甘油单油酸酯(3-单油酸多甘油酯)、三甘油单月桂酸酯、三甘油单硬脂酸酯(3-硬脂酸多甘油酯)、三甘油单异硬脂酸酯、六甘油二油酸酯(6-二油酸多甘油酯)、六甘油二硬脂酸酯(6-二硬脂酸多甘油酯)、十甘油二油酸酯(10-二油酸多甘油酯)、十甘油四油酸酯(10-四油酸多甘油酯)、十甘油十油酸酯(10-十油酸多甘油酯)、十甘油二硬脂酸酯(10-二硬脂酸多甘油酯)。括号中给出的是CTFA命名法。这些产品以商品名Caprol(Karlshamns USA Inc.,Columbus Ohio的商标)有售。特定的产品名称为:CAPROL 2G4S,3GO,3GS,6G20,6G2S,10G20,10G40,10G100,10G10S。另外的产品是以商品名DGLC-MC,DGLC-ML,DGLC-DISOS,DGLC-MISOS,TGLC-ML和TGLC-MISOS从Solvay Alkali GmbH,D-3002 Hannover获得的。
不同多甘油脂肪酸酯的混合物是由诸如十甘油单和二油酸酯、混合脂肪酸的多甘油酯、脂肪酸的多甘油酯和多甘油癸酸酯、可可酸酯(cocoate)、月桂酸酯、羊毛脂酸酯(lanolinate)、异硬脂酸酯和蓖麻油酸酯(ricinolate)名称确定的并且以下列商标出售:Triodan和Homodan(Grindsted Products,Grindsted Denmark的商标),特定产品名称为TRIODAN 20,55,R90和HOMODAN MO;Radiamuls(Petrofina(FINA),Brussels,Belgium的商标),特定产品名称为RADIAMULS poly 2253;和名称CAPROL PGE860或ET;或商标Plurol(Gattefosse Etablissements,Saint-Priest,France的商标),特定产品名称为PLUROL Stearique WL 1009或PLUROLOleique WL 1173。另外的产品是以商品名PGLC-C1010s,PGLC-C0810,PGLC-C1010/S,PGLC-LT2010,PGLC-LAN0510/S,PGLC-CT2010/90,PGLC-ISOSTUE,PGLC-RUE和PGLC-ISOS0410从Solvay Alkali GmbH,D-3002 Hannover获得的。
适宜的山梨糖醇脂肪酸酯优选由基本纯的山梨糖醇脂肪酸酯或不同山梨糖醇脂肪酸酯的混合物组成,其中山梨糖醇基体结构被一个上述带有8-20偶数个碳原子的饱和或不饱和直链羧酸的1-3个酸基团酯化。
适宜的山梨糖醇脂肪酸酯特别为山梨糖醇单月桂酸酯、单棕榈酸酯、单硬脂酸酯、三硬脂酸酯、单油酸酯、被半油酸酯和三油酸酯。这些产品以下列商标出售:Span(Atlas,Wilmington USA的商标),特定的产品名称为SPAN 20,40,60,65,80和85;Arlacel(Atlas的商标),特定产品名称为ARLACEL 20,40,60,80,83,85和C;Crill(Croda Chemicals Ltd.,Cowick Hall,Snaith Goole GB的商标),特定产品名称为CRILL 1,3和4;Dehymuls(Henkel,Dusseldorf DE的商标),特定产品名称为DEHYMULS SML,SMO,SMS,SSO;Famodan(Grindsted Products,Grindsted Denmark的商标),特定产品名称为FAMODAN MS和TS;Capmul(Karlshamns USA Inc.,Columbus,Ohil的商标),特定产品名称为CAPMUL S和O;和Radiasurf(Petrofina(FINA),Brussels,Belgium的商标),特定产品名称为RADIASURF 7125,7135,7145和7155。
所述聚氧乙烯山梨糖醇的部分脂肪酸酯优选由基本纯的山梨糖醇酯或不同山梨糖醇酯的混合物组成,其中脂肪酸基团的结构和聚氧乙烯链的长度可变化。山梨糖醇优选被3个聚氧乙烯链醚化并被1个脂肪酸基团酯化。但是取而代之,山梨糖醇可只被1个或2个聚氧乙烯链醚化并因此被2个或3个脂肪酸基团酯化。
总之,山梨糖醇基体结构被最少2个及最多4个亲水基团取代,聚氧乙烯链和脂肪酸基团均包括在术语“亲水基团”中。
聚氧乙烯链为直链并且优选含有4-10,特别是4-8个氧化乙烯单元。山梨糖醇基体结构上的酯基团衍生自带有8-20偶数个碳原子的饱和或不饱和直链羧酸。衍生自这种羧酸的酯基团优选为直链的并含有12,14,16或18个碳原子,例如正十二烷酰基、正十四烷酰基、正十六烷酰基或正十八烷酰基。衍生自带有8-20偶数个碳原子的不饱和羧酸的酯基团优选为直链的并含有12,14,16或18个碳原子,例如油酰基。
适宜的聚氧乙烯山梨糖醇的部分脂肪酸酯以ICI的商标Tween出售并且以化学名称聚氧乙烯(20或4)-山梨糖醇单月桂酸酯(TWEEN 20和21)、聚氧乙烯-(20)-山梨糖醇单棕榈酸酯或单硬脂酸酯(TWEEN 40和60)、聚氧乙烯-(4或20)-山梨糖醇单硬脂酸酯或三硬脂酸酯(TWEEN61和65)、聚氧乙烯-(20或5)-山梨糖醇单油酸酯(TWEEN 80或81)和聚氧乙烯-(20)-山梨糖醇三油酸酯(TWEEN 85)而闻名。
向本发明组合物中加入另外的抗氧化剂是有利的,特别是硫代二丙酸或硫代二乙酸的酯和/或醚,这些化合物在起始氢化阶段取代一些硫损失。这些化合物作为过氧化物分解剂。虽然发现硫醚化合物(C13H27OCCH2CH2)2S用于此目的很好,但其它硫醚和硫代酯也是同样有利的。这些另外的抗氧化剂是已知的并且以有效稳定量引入,例如基于稳定剂混合物总重量(即不包括润滑剂的重量)的5-30重量%,更特别为10-25重量%。
现在已令人惊讶地发现在润滑剂中使用本发明的特定添加剂组合,特别是氢化处理或氢化脱蜡的油会得到卓越的性能特征。值得注意的是由该技术制备所得的组合物不仅延缓了氧化过程,而且在使用时根据本发明的组合物比其它添加剂组合物在很大程度上更稳固,并且是钙相容的。特别发现组分(e)和(f)的组合在提供防止I,II和III组基油的钙相容稳固防锈性方面是非常有用的。还发现当存在单油酸甘油酯时它在提供防止基油的钙相容稳固防锈性方面是有用的。另外,任何基油,不只限于氢化处理或氢化脱蜡的油,均可如此处所说明的被稳定。
本发明另一个高度优选的实施方案涉及如上所定义的润滑剂组合物,该组合物另外包括有效稳定量的上述多元醇部分酯、硫醚或硫代酯或这些另外组分的组合物。
本发明氢化处理或氢化脱蜡的油组合物也可任选包括除此处所规定的稳定剂混合物之外的各种其它添加剂,以进一步改进其基本性能。这些另外的添加剂包括其它抗氧化剂、金属减活剂和防锈剂以及粘度指数改进剂、分散剂、洗涤剂、耐特压和抗磨损添加剂、倾点下降剂等。
这些另外添加剂的说明性而非限制性实例如下:
其它抗氧化剂实例
脂族或芳族亚磷酸盐、硫代二丙酸或硫代二乙酸酯、或者二硫代氨基甲酸或二硫代磷酸的盐。
其它金属减活剂实例
三唑和其它苯并三唑及其衍生物、甲苯三唑、2-巯基苯并三唑、5,5’-亚甲基二苯并三唑、4,5,6,7-四氢苯并三唑、亚水杨基丙二胺和水杨酰氨基胍及其盐。
其它防锈剂实例
其它的有机酸、其酯、金属盐和酐,例如山梨糖醇单油酸酯、环烷酸铅,烯基琥珀酸及酐,例如十二碳烯基琥珀酸酐、琥珀酸部分酯和胺;
含氮化合物,例如
I.脂族或脂环族伯、仲或叔胺和胺-有机酸和无机酸盐,例如油溶性烷基-羧酸铵;
II.杂环化合物,例如取代的咪唑啉和噁唑啉。
含磷化合物,例如膦酸的胺盐或磷酸部分酯、二烷基二硫代磷酸锌;
含硫化合物,例如二壬基萘-n-磺酸钡、石油磺酸钙;
日本特许公报15783/1973描述的γ-烷氧基丙基胺衍生物;
具有式Y-NH3-R17CO2-的盐,该式中Y为R18Q1CH2CH(OH)CH2基团,其中R17和R18独立地为例如烷基而Q1为O、CO2、NH、N(烷基)、N(烯基)或S,这些盐是通过将胺Y-NH2与酸R17CO2H混合而制备的,如DE-OS3 437 876(已出版的德国专利申请)所述;
具有式R19-Q2-CH2-CH(OH)-CH2NR20R21的化合物,该式中Q2为-O-,-S-,-SO2-,-C(O)-O-或N(Rd),其中R19为H或C1-C12烷基,R20为未取代的C1-C4烷基或被1-3个羟基取代的C2-C5烷基,R21为氢、未取代的C1-C4烷基或被1-3个羟基取代的C2-C5烷基,只要R20和R21中的至少一个是羟基取代的,而R19为C2-C20烷基-CH2-CH(OH)-CH2-NR20R21或R19为C2-C18烯基、C2-C3炔基或C3-C12环烷基,只要当Q2为-O-或-C(O)-O-时,R19为支化的C4-C20烷基。这些化合物在英国专利说明书2172 288A中有述;
具有下式的化合物:
其中R22、R23和R24独立地为氢、C1-C15烷基、C5-C12环烷基、C6-C15芳基或C7-C12芳烷基并且R25和R26独立地为氢、2-羟基乙基或2-羟基丙基,只要R25和R26不同时为氢并且当R25和R26分别为-CH2CH2OH时,R22和R23不同时为氢而R24不为戊基。这些化合物描述于已出版的欧洲专利说明书252 007中。
粘度指数改进剂的实例
聚丙烯酸酯、聚甲基丙烯酸酯、乙烯基吡咯烷酮/甲基丙烯酸酯共聚物、聚乙烯基吡咯烷酮、聚丁烷、烯烃共聚物、苯乙烯/丙烯酸酯共聚物、聚醚。
倾点下降剂的实例
聚甲基丙烯酸酯、烷基化萘衍生物。
分散剂/洗涤剂的实例
聚丁烯琥珀酸-酰胺或酰亚胺、聚丁烯膦酸衍生物、碱性磺酸和苯甲酸镁、钙和钡。
抗磨损添加剂和耐特压添加剂的实例
含硫和/或磷和/或卤素的化合物,例如硫化的蔬菜油、二烷基二硫代磷酸锌、三甲苯基磷酸酯、氯代石蜡、烷基和芳基二和三硫醚、三苯基硫代磷酸酯和磷酸胺。
所有上述任选的添加剂在配制润滑油领域是已知的,而且本领域的技术人员知道怎样选择适于特殊润滑产品最终用途的热稳定添加剂。
另外根据最终用途向本发明的润滑剂组合物中加入抗磨添加剂将是特别有益的。USP 4,584,021;5,798,321;5,750,478;5,801,130;4,191,666;4,720,288;4,025,288;4,025,583和WO 095/20592描述了可用于本发明的抗磨添加剂。在此引入这些文献作为参考。胺的其它实例为多亚烷基胺如乙二胺、二亚乙基三胺、三亚乙基四胺、四亚乙基五胺、五亚乙基六胺、九亚乙基十胺和芳胺,如USP 4,267,063所述,在此引入该专利作为参考。已经发现包括特殊胺的胺磷酸盐和混合的单及二酸磷酸酯是有利的。单及二酸磷酸酯胺具有下列结构式:
其中R27为氢、未取代或被一个或多个C1-C6烷氧基基团取代的C1-C25线性或支链烷基、饱和无环或脂环族基团、或芳基;R28为未取代或被一个或多个C1-C6烷氧基基团取代的C1-C25线性或支链烷基、饱和无环或脂环族基团、或芳基;R29为氢、C1-C25线性或支链烷基、饱和或不饱和无环或脂环族基团、或芳基;并且为氢、或者C1-C12线性或支链烷基;R30和R31彼此独立地为C1-C25线性或支链烷基、饱和或不饱和无环或脂环族基团、或芳基。优选R27和R28为线性或支链C1-C12烷基;而R29、R30和R31为线性或支链C1-C18烷基。
已经发现IRGALUBE 349(CIBA)是非常有用的,特别是提高了基油的磨损性能使之满足苛刻的军用性能标准。IRGALUBE 349具有下式:
其中R33为由正己基组成的烷基链,R34为C11-C14支链烷基,并且当x=1时y=2;当x=2时y=1。
优选的实施方案涉及润滑剂组合物,其中
(b)为1-[二(2-乙基己基)氨基甲基-4-甲基]苯并三唑;
(c)为3,5-二叔丁基-4-羟基氢化肉桂酸C7-C9烷基酯;
(d)为下式的苯基萘胺:
其中R12代表氢或C8-C13烷基;或者下式的二苯胺:
其中R12为氢并且R13为氢或C8-C13烷基;或者
(e)为壬基苯氧基乙酸;并且
(f)为式C17H33-C(O)-N(CH3)-CH2COOH的N-酰基肌氨酸。
本发明还涉及由上面所定义的组分(b)-(f)及任选组分组成的稳定剂混合物。一般稳定剂混合物由约5-30重量%,更特别约10-25重量%组分(b);15-45重量%,更特别20-40重量%组分(c);25-60重量%,更特别35-50重量%组分(d);1-15重量%,更特别2-10重量%组分(e);0.1-10重量%,更特别0.5-5重量%组分(f)组成是有利的。在本发明的优选实施方案中,存在选自以稳定剂混合物总重量为基础的0.1-10重量%,更特别0.5-5重量%的上述多元醇部分酯和15-30重量%,更特别20-25重量%的硫醚衍生物的任选组分。如果必要,可使用5-20重量%,更特别10-15重量%适当的溶剂作为稳定剂混合物中的稀释剂。
将混合物以占稳定组合物总重量约0.01-约3.0重量%的比例引入到氢化处理或氢化脱蜡的基料中。有利的范围为0.03-2.0%,且特别是约0.15-约1.05%。具体用量依赖于最终润滑油产品的目标性能。
本发明进一步涉及提高润滑油性能,特别是延缓氧化降解并由此延长其寿命的方法。因此,该方法要求专利保护稳定氢化处理或氢化脱蜡油防止热和氧的有害影响的方法,该方法包括向所述油中加入有效稳定量的上述组合物的步骤。
涉及稳定氢化处理或氢化脱蜡油的优选实施方案也适用于本发明的所有方面。
可将本发明组合物的组分(b)-(f)和任选组分的化合物与氢化处理或氢化脱蜡的润滑油以本身已知的方法混合。例如这些化合物是易溶于油的。也可以制备一种母料,其可根据使用量用适当的油稀释到适当的浓度。在这种情况下,比所述高得多的浓度是可以的。
将上述抗磨添加剂以占稳定润滑剂组合物总重量约0.01-约0.20重量%,特别是约0.025-约0.18重量%的有效稳定量引入到润滑剂组合物中。
下列实施例仅出于说明的目的而不是要以任何方式限制本发明的性质和范围。除非另外指明,份和百分比均为重量的。
实施例1-9
表I显示了根据本发明的代表性组合物1-9的组成及试验结果。这些组合物是通过将所述添加剂在60℃搅拌1小时溶解在氢化处理和/或氢化脱蜡或溶剂精制的油中而制备的。
根据ASTM D-665B对组合物1-15(表I和II)进行生锈性能评价,这是在合成海水存在下进行的。测试结果一般在24小时测定,为了满足诸如MIL-17331H标准的要求,也在48小时测定。
表1
1 | 2 | 3 | 4 | 5 | 6 | 7 | 8 | 9 | |
油(1) | 99.90 | - | - | 99.85 | 99.80 | 99.75 | 99.70 | 99.65 | 99.50 |
油(2) | - | - | - | - | - | - | - | - | - |
油(3) | - | 99.90 | - | - | - | - | - | - | - |
油(4) | - | - | 99.90 | - | - | - | - | - | - |
烷基化二苯胺(5) | 0.013 | 0.013 | 0.013 | 0.020 | 0.025 | 0.032 | 0.038 | 0.044 | 0.063 |
苯基-α-萘胺(6) | 0.005 | 0.005 | 0.005 | 0.007 | 0.010 | 0.012 | 0.015 | 0.017 | 0.025 |
二(十三烷基)硫代二丙酸酯(7) | 0.025 | 0.025 | 0.025 | 0.037 | 0.050 | 0.062 | 0.074 | 0.087 | 0.124 |
3,5-二叔丁基-4-羟基氢化肉桂酸C7-C9烷基酯(8) | 0.024 | 0.024 | 0.024 | 0.036 | 0.048 | 0.060 | 0.072 | 0.084 | 0.120 |
取代的甲苯三唑(9) | 0.024 | 0.024 | 0.024 | 0.036 | 0.048 | 0.060 | 0.072 | 0.084 | 0.120 |
壬基苯氧基乙酸(10) | 0.008 | 0.008 | 0.008 | 0.012 | 0.016 | 0.021 | 0.025 | 0.029 | 0.041 |
N-酰基肌氨酸(11) | 0.002 | 0.002 | 0.002 | 0.002 | 0.003 | 0.004 | 0.005 | 0.006 | 0.008 |
D665锈化试验结果24小时(12)48小时(12) | 通过失败 | 通过---- | 通过---- | 通过通过 | 通过通过 | 通过通过 | 通过通过 | 通过通过 | 通过通过 |
表I中的注释具有下列含义:
组分a)
(1)氢化裂解、等脱蜡(isodewaxed)、氢化处理基油(商品名:RLOP240N;Chevron)
(2)ISO 32氢化处理基油(P1810;Petro Canada)
(3)ISO 32氢化处理精制基油(HPO170;Sun Oil)
(4)ISO 46氢化处理精制基油(HPO300;Sun Oil)
添加剂组合物
(5)IRGANOX L57(CIBA)
(6)PANA(Fanwood Chemicals)
(7)Evanstab 13(Hampshire Chemical Corp.)
(8)IRGANOX L135(CIBA)
(9)IRGAMET 39(CIBA)
(10)IRGACOR NPA(CIBA)
(11)Sarkosyl O(CIBA)
组合物1-15显示相对含有其它添加剂组合物的样品,根据本发明优选实施方案稳定的油样品(即组合物1-9的壬基苯氧基乙酸和N-酰基肌氨酸的特殊组合)显示了显著改进的防锈性。根据本发明稳定的油在添加剂浓度约为0.1重量%时通过锈化试验,而用对比添加剂组合物稳定的油直到添加剂浓度达到约0.5重量%时才开始通过试验。
表II显示根据本发明稳定的氢化处理或氢化脱蜡油满足了军用标准MIL-17672D的性能要求以及市场上所用的多数R&O油的性能目标。组合物2和3与上述表I所指相同。
表II
组合物2 | 组合物3 | 17672D标准限 | |
RPVOT(min.) | 295/310 | 385/400 | |
TOST寿命(hr.) | 3589 | 3285 | 1,000(最小) |
TOST淤浆(mg.) | 3.0酸值=0.4 | 9.0酸值=0.3 | 100(最大) |
锈化试验 | 通过 | 通过 | 通过 |
泡沫(ml.)序列1序列2序列3 | 0/0(1)0/0(1)0/0(1) | 0/0(1)0/0(1)0/0(1) | 65/065/065/0 |
反乳化·油层(ml)·水层(ml)·乳液层(ml)·分离时间(min.) | 42(浑浊)38(模糊)05 | 43(浑浊)37(模糊)05 | 40(最大)40(最大)3(最大)30 |
液体酸值(mg KOH/g) | 0.1 | 0.1 | 0.2(最大) |
基料酸值(mg KOH/g) | 0.1 | 0.1 | - |
注(1):向组合物中加入消泡剂
以分钟为单位的RPVOT(旋转压力容器氧化试验)是根据ASTM D-2272测定的。较长的氧化寿命表明较好的抗氧性。
TOST寿命(抗氧化矿物油的氧化特性)是根据ASTM D943测定的。测定了酸值增长2.0的时间(以小时为单位)。较长的寿命表明特定润滑剂组合物较好的抗氧性。酸值是根据ASTM D-664通过滴定测定的。
TOST淤浆(决定抗氧化矿物油的淤浆化和腐蚀倾向)是根据ASTMD4310测定的。试验结束时产生的淤浆量越少,特定润滑剂组合物的抗氧化性越好。
润滑油的发泡特性是根据ASTM D-892测定的。低到不发泡是所希望的。第一个数表示向油中吹空气5分钟后产生的泡沫体积。第二个数表示不向油中吹空气10分钟后存在的泡沫体积。
反乳化率(石油和合成液体的水分离性)是根据ASTM D 1410测定的。润滑剂与水之间的高度分离是所希望的。结果是以在将两种液体的混合物不搅动放置一定时间后产生的油体积、水体积和乳液体积报告的。17672D军用标准要求液体在30分钟内明显分层,允许的最大乳液水平为3ml,油为40ml,水为40m1。军用标准17331H要求液体在30分钟内明显分层,允许的最大乳液水平为0ml,油为40ml,水为40ml。
实施例10-15
表III显示了对比组合物及组合物10-15的试验结果:
表III
10 | 11 | 12 | 13 | 14 | 15 | |
油(2) | 99.55 | 99.50 | - | - | - | - |
油(3) | - | - | 99.50 | - | 99.45 | - |
油(4) | - | - | - | 99.50 | - | 99.45 |
烷基化二苯胺(5) | 0.057 | 0.063 | 0.063 | 0.063 | 0.069 | 0.069 |
苯基-α-萘胺(6) | 0.022 | 0.025 | 0.025 | 0.025 | 0.027 | 0.027 |
二(十三烷基)硫代二丙酸酯(7) | 0.112 | 0.124 | 0.124 | 0.124 | 0.136 | 0.136 |
3,5-二叔丁基-4-羟基氢化内桂酸C7-C9烷基酯(8) | 0.108 | 0.120 | 0.120 | 0.120 | 0.132 | 0.132 |
取代的甲苯三唑(9) | 0.108 | 0.120 | 0.120 | 0.120 | 0.132 | 0.132 |
十二碳烯基琥珀酸的脂肪酰胺(12) | 0.044 | 0.050 | 0.050 | 0.050 | 0.054 | 0.054 |
D665锈化试验结果·24小时·48小时 | 失败失败 | 通过---- | 失败失败 | 失败失败 | 通过---- | 通过---- |
表III中注释具有下列含义:
(2)-(9)如表I所定义
(12)Hitec 536(乙基)
实施例16-31
表IV和V显示了对比组合物16-31及试验结果。这些组合物是以与组合物1-9同样的方法制备的。组合物16-31是根据ASTM D 665A和B部分评价的。该过程的A部分是在蒸馏水存在下进行的。如果在该过程完成时在钢试验样品上未观察到一个锈点则认为样品通过试验。反乳化率(石油和合成液体的水分离性)是根据ASTM D 1401测定的。润滑剂与水之间的高度分离是所希望的。结果是以在将两种液体的混合物不搅动放置一定时间后产生的油、水和乳液的体积报告的。在本研究中所用的防腐蚀剂没有一个对油的水分离特性产生不利影响。
表IV
16 | 17 | 18 | 19 | 20 | 21 | 22 | 23 | 24 | 25 | |
N-酰基肌氨酸(1) | ---- | ---- | ---- | 0.03 | ---- | ---- | ---- | 0.015 | 0.03 | 0.015 |
壬基苯氧基乙酸(2) | ---- | 0.03 | ---- | ---- | 0.015 | 0.015 | 0.03 | ---- | ---- | ---- |
甘油单油酸酯(3) | ---- | ---- | 0.03 | ---- | 0.015 | 0.025 | 0.015 | 0.025 | 0.015 | 0.015 |
基体组合物(4) | 0.29 | 0.29 | 0.29 | 0.29 | 0.29 | 0.29 | 0.29 | 0.29 | 0.29 | 0.29 |
基油(5) | 平衡 | 平衡 | 平衡 | 平衡 | 平衡 | 平衡 | 平衡 | 平衡 | 平衡 | 平衡 |
D665A锈化试验结果·24小时 | 失败 | 失败 | 失败 | 通过 | 失败 | 失败 | 通过 | 通过 | 通过 | 通过 |
D665B锈化试验结果24小时 | 失败 | 失败 | 失败 | 失败 | 失败 | 失败 | 失败 | 通过 | 通过 | 通过 |
反乳化D1401(82℃)油/水/乳液共用时间(min) | 42/38/03 | 43/37/06 | 44/36/04 | 43/37/05 | 43/37/03 | 43/37/05 | 43/37/06 | 41/39/03 | 41/39/03.5 | 41/39/03 |
表IV中的注释具有下列含义:
(1)和(2)如表I所定义
(3)KesscoGMO(Akzo)
(4)基体组合物:1500ppm IRGANOX L135(3,5-二叔丁基-4-羟基氢化肉桂酸C7-C9烷基酯;CIBA);300ppm IRGANOX L 57(烷基化二苯胺;CIBA);400ppm IRGAMET 39(取代的甲苯三唑;CIBA)
(5)基油:ISO溶剂精制基油(商品名:Esso Solvent Neutral 600;Exxon):40℃粘度:113mm2/s;粘度指数:93;硫含量:0.5%;芳烃含量:8.8%。
表V
26 | 27 | 28 | 29 | 30 | 31 | |
N-酰基肌氨酸(1) | - | 0.005 | 0.0225 | 0.005 | 0.005 | 0.005 |
壬基苯氧基乙酸(2) | - | 0.0225 | 0.0485 | 0.0225 | 0.0225 | 0.024 |
甘油单油酸酯(3) | - | - | - | 0.005 | 0.01 | 0.0032 |
基体组合物(4) | 0.243 | 0.243 | 0.243 | 0.243 | 0.243 | 0.268 |
基油(5) | 平衡 | 平衡 | 平衡 | 平衡 | 平衡 | 平衡 |
D665A锈化试验结果24小时 | - | 失败 | - | - | - | - |
D665B锈化试验结果24小时 | 失败 | 失败 | 失败 | 通过 | 通过 | 通过 |
表V中的注释具有下列含义:
(1)和2)如表I所定义
(3)如表IV所定义
(4)基体组合物:810ppm BHT(NaugardBHT;UniroyalChemicals);810ppm IRGANOX L 135;540ppm IRGANOX L57TM;135ppm IRGAMET 30TM(CIBA);135ppm IRGAMET 39TM(CIBA)
(5)基油:ISO 220氢化处理油(商品名:Wintershall VG 220,Exxon):40℃粘度:224cSt
组合物16-31显示根据本发明另一个优选实施方案稳定的某些基油(即组合物29-31的壬基苯氧基乙酸、N-酰基肌氨酸和甘油单油酸酯的特定组合或者组合物23-25的N-酰基肌氨酸和甘油单油酸酯的特定组合)与不包含该防锈添加剂组合的组合物相比显著改进了防锈性。这些根据本发明稳定的基油在添加剂浓度为约0.03wt.%时通过锈化试验。当不用甘油单油酸酯稳定时这些基油不能通过锈化试验。
实施例32-37
表VI和VII显示了根据本发明制备的组合物32-42的组成和试验结果。这些组合物按实施例1制备。测定了一些组合物的D 665 B,RPVOT,TOST寿命和TOST淤浆。结果列于表VI和VII。
表VI
32 | 33 | 34 | 35 | 36 | 37 | |
基油(1,13) | 99.52 | 99.52 | 99.39 | 99.37 | 99.40 | 99.58 |
烷基化二苯胺(2) | 0.10 | 0.10 | 0.08 | 0.08 | 0.13 | 0.15 |
苯基-α-萘胺(3) | 0.08 | 0.08 | 0.10 | 0.10 | 0.17 | 0.060 |
二(十三烷基)硫代二丙酸酯 | 0.04 | 0.04 | 0.05 | 0.05 | ---- | ---- |
3,5-二叔丁基-4-羟基氢化肉桂酸C7-C9烷基酯(5) | ---- | 0.18 | 0.25 | 0.25 | 0.14 | 0.15 |
2,6-二叔丁基苯酚(6) | 0.18 | ---- | ---- | ---- | ---- | ---- |
取代的甲苯三唑 (7) | 0.05 | 0.05 | 0.10 | 0.10 | 0.045 | 0.035 |
壬基苯氧基乙酸(8) | 0.025 | 0.025 | 0.025 | 0.042 | 0.028 | 0.01 |
N-酰基肌氨酸(9) | 0.005 | 0.005 | 0.005 | 0.008 | 0.004 | 0.01 |
甘油单油酸酯(10) | ---- | ---- | ---- | ---- | 0.007 | ---- |
TEGDME(11) | ---- | ---- | ---- | ---- | 0.084 | ---- |
甲基三唑(12) | ---- | ---- | ---- | ---- | ---- | 0.005 |
D665B锈化试验结果·24小时 | 通过 | 通过 | 通过 | 通过 | 通过 | 通过 |
RPVOT,D 2272(min) | 956 | 744 | 946 | 878 | 1573 | 790 |
表VI中的注释具有下列含义:
(1)氢化裂解、等脱蜡(isodewaxed)、氢化处理基油(商品名:RLOP240N;由Chevron生产)
(6)IRGANOX L 140(CIBA)
(11)四甘醇二甲醚(Tetraglyme,Ferro Corp.)
(12)甲苯三唑(CIBA)
(13)配方37所得结果,是在ISO 46氢化处理基油(Mobil Jurong;由Exxon Mobil生产)中产生的
注释2、3、4、5、和7-19如表I所定义。注释10如表IV所定义。
表VII
38 | 39 | 40 | 41 | 42 | |
油(1) | 99.85 | 99.40 | 99.29 | 98.95 | 99.19 |
烷基化二苯胺(5) | 0.020 | 0.076 | 0.089 | 0.13 | 0.089 |
苯基-α-萘胺(6) | 0.007 | 0.030 | 0.035 | 0.052 | 0.10 |
二(十三烷基)硫代二丙酸酯(7) | 0.037 | 0.15 | 0.18 | 0.26 | 0.18 |
3,5-二叔丁基-4-羟基氢化肉桂酸C7-C9烷基酯(8) | 0.036 | 0.14 | 0.17 | 0.25 | 0.17 |
取代的甲苯三唑(9) | 0.036 | 0.14 | 0.17 | 0.25 | 0.20 |
壬基苯氧基乙酸(10) | 0.012 | 0.050 | 0.059 | 0.087 | 0.059 |
N-酰基肌氨酸(11) | 0.002 | 0.010 | 0.012 | 0.017 | 0.012 |
RPVOT(min.) | 302 | ---- | 838 | 878 | 1073 |
TOST寿命(hr.) | 3589 | 4875 | 6753 | 8738 | 9992 |
TOST淤浆(mg.) | 3.0 | 63 | 41 | 67 | 27 |
注释1和5-11已在表I中定义。
实施例43-44
将IRGALUBE 349(胺、C11-C14支化烷基、含有磷酸二己酯和磷酸单己酯的化合物)包含(0.16重量%)在组合物2和3的润滑剂组合物中以分别形成组合物43和44。然后让组合物43和44经历MIL-17331H的性能测试。结果列于表VIII。
表VIII
43 | 44 | MIL-17331H标准限 | |
RPVOT(min.) | 90 | 115 | |
TOST寿命(hr.) | 3769 | 3403 | 1000(最小) |
TOST淤浆(mg.) | 23酸值=0.3 | 14酸值=0.2 | 100(最大) |
锈化试验 | 通过 | 通过 | 48小时后通过 |
泡沫(ml.)序列1序列2序列3 | 0/00/00/0 | 0/00/00/0 | 65/065/065/0 |
反乳化(ml.)·油层(ml)·水层(ml)·乳液层(ml)·分离时间(min.) | 43(浑浊)37(透明)015 | 43(浑浊)37(透明)010 | 4040030 |
液体酸值(mg KOH/g) | 0.2 | 0.3 | 0.3(最大) |
注:1向组合物中加入消泡剂
如上述测定RPVOT、TOST寿命、TOST淤浆、发泡和反乳化率。根据联邦标准791方法6503测定磨损性(四球磨损试验)。试验结束时所产生的伤痕直径越小表明特定润滑剂组合物提供的耐磨损性越好。
实施例45-49
将根据本发明制备的组合物的钙相容性与对比组合物进行比较。组合物45和46是根据本发明以与上述组合物1-9类似的方法制备的。组合物47包括Hitec 575,是来自Ethyl Corporation的防锈抗氧化组合物。组合物48包含与组合物45和46等量的相同组分,但使用琥珀酸半酯(IRGACOR L12)代替本发明的防腐蚀剂。组合物49包含与组合物45和46等量的相同组分,但使用烷基化酸/酯(Lubrizol 859)代替本发明的防腐蚀剂。钙相容性研究的结果列于表IX:
表IX
组合物 | 45 | 46 | 47 | 48 | 49 |
浓度(重量%) | 0.5 | 1.05 | 0.5 | 0.5 | 0.5 |
过滤指数 | 1.1 | 1.0 | >2 | >>2 | >>>2 |
钙相容性是根据下列步骤进行的:将300ml含有0.1体积%去离子水和30ppm钙污染物的样品密封并于70℃保存96小时。随后将该样品在黑暗中保存48小时。记录每100ml过滤液体的时间。过滤指数(FI)是通过下式决定的:FI=[T300-T200]/[2(T100-T50)],其中TN代表油通过过滤器一定体积(即50ml,100ml,200ml或300ml)的时间。过滤指数<2是所希望的并定为“通过”。过滤指数≥2是不希望的并定为“失败”。
如这些结果所示,根据本发明制备的组合物是钙相容的并能通过钙相容性试验而对比组合物是钙不相容的且在试验中失败。
Claims (10)
1.润滑剂组合物,该组合物包括
(a)氢化处理油或氢化脱蜡油;和一种稳定剂混合物,其中所述混合物包括
(b)(i)基于稳定剂混合物总重量的5-30重量%式(I)的金属去活化剂:
其中R1为氢或C1-C12烷基,并且
R2和R3彼此独立地为氢、C1-C20烷基、C3-C20烯基、C5-C12环烷基、C7-C13芳烷基、C6-C10芳基、羟基,或者
R2和R3和与之相连的氮形成5-、6-或7-元杂环残基,或者
R2和R3分别为式(II)的残基:
R4X[(亚烷基)O]n(亚烷基)- (II)
其中X为O、S或N;
R4为氢或C1-C20烷基;
亚烷基为C1-C12亚烷基残基;和
n为0或1-6的整数;或者
R2如上定义而R3为式(III)的残基:
或者R3为如上定义的式(II)的残基而R2为式(IV)的残基:
-[亚烷基]n-N(R5)-A-[N(R5)2]m (IV)
其中m为0或1,并且,
当m为0时,A为式(III)的残基,和
当m为1时,A为亚烷基或C6-C10亚芳基;和
亚烷基和n具有上述含义;并且
R5为式(III)的残基,如上定义;或者
(ii)基于稳定剂混合物总重量的5-30重量%的式(V)的金属去活化剂:
其中R2和R3定义如上;
(c)基于稳定剂混合物总重量的15-45重量%的位阻酚抗氧化剂;
(d)基于稳定剂混合物总重量的25-60重量%的芳胺抗氧化剂;
(e)基于稳定剂混合物总重量的1-15重量%的式(VI)的烷基苯氧基链烷酸:
其中R6,R7,R8,R9和R10彼此独立地为氢或C1-C20烷基,并且Y为二价的C1-C20烃基,选自
(f)基于稳定剂混合物总重量的0.1-10重量%的式(VII)的N-酰基肌氨酸衍生物:
其中酰基R11-C(=O)-为含有10-20个碳原子的脂肪酸残基,并且X+为氢离子、碱金属离子或铵离子。
2.根据权利要求1的润滑剂组合物,该组合物另外包括基于稳定剂混合物总重量的0.1-10重量%的多元醇部分酯、基于稳定剂混合物总重量的15-30重量%的硫醚或硫代酯或这些另外组分的组合物。
3.根据权利要求1的润滑剂组合物,进一步包括(C13H27OCCH2CH2)2S。
4.根据权利要求1的润滑剂组合物,其中式I的金属去活化剂为1-[二(2-乙基己基)氨基甲基-4-甲基]苯并三唑。
5.根据权利要求1的润滑剂组合物,其中式I的金属去活化剂为1-[二(2-乙基己基)氨基甲基]-1,2,4-三唑。
6.根据权利要求1的润滑剂组合物,其中烷基苯氧基链烷酸组分(e)选自苯氧基乙酸、对甲基苯氧基乙酸、对异丙基苯氧基乙酸、对辛基苯氧基乙酸、对壬基苯氧基乙酸、对十二烷基苯氧基乙酸、对(α-甲基-甲基-十九烷基)苯氧基乙酸、2,4-二叔戊基苯氧基乙酸、2,4-二仲戊基苯氧基乙酸、2,4-二壬基苯氧基乙酸和2-甲基-6-叔丁基苯氧基乙酸。
7.根据权利要求1的润滑剂组合物,其中N-酰基肌氨酸衍生物选自月桂酰肌氨酸、棕榈酰肌氨酸、油酰肌氨酸、硬脂酰肌氨酸、和妥尔油酰基肌氨酸或相应的肌氨酸碱金属或铵盐。
9.根据权利要求1的润滑剂组合物,进一步包括选自另外的抗氧化剂、金属减活剂、防锈剂、粘度指数改进剂、分散剂、洗涤剂、耐特压和抗磨添加剂及倾点下降剂的添加剂或者其混合物。
10.用于稳定氢化处理油或氢化脱蜡油以防止热和/或氧的有害作用的方法,该方法包括向所述油中添加根据权利要求1的稳定剂混合物的步骤。
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CNB001176412A Expired - Fee Related CN1207375C (zh) | 1999-05-19 | 2000-05-18 | 稳定的氢化处理及氢化脱蜡润滑剂组合物 |
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Country | Link |
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US (1) | US6410490B1 (zh) |
EP (1) | EP1054052B1 (zh) |
JP (1) | JP4614025B2 (zh) |
CN (1) | CN1207375C (zh) |
DE (1) | DE60029049T2 (zh) |
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-
2000
- 2000-05-10 EP EP00810399A patent/EP1054052B1/en not_active Expired - Lifetime
- 2000-05-10 DE DE60029049T patent/DE60029049T2/de not_active Expired - Lifetime
- 2000-05-18 US US09/573,402 patent/US6410490B1/en not_active Expired - Fee Related
- 2000-05-18 JP JP2000146450A patent/JP4614025B2/ja not_active Expired - Fee Related
- 2000-05-18 CN CNB001176412A patent/CN1207375C/zh not_active Expired - Fee Related
Also Published As
Publication number | Publication date |
---|---|
EP1054052B1 (en) | 2006-06-28 |
EP1054052A2 (en) | 2000-11-22 |
DE60029049D1 (de) | 2006-08-10 |
CN1274743A (zh) | 2000-11-29 |
DE60029049T2 (de) | 2007-06-21 |
JP4614025B2 (ja) | 2011-01-19 |
US6410490B1 (en) | 2002-06-25 |
JP2000351984A (ja) | 2000-12-19 |
EP1054052A3 (en) | 2001-02-07 |
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