CN107987918B - 内燃机润滑油组合物及提高内燃机润滑油清净性的方法 - Google Patents
内燃机润滑油组合物及提高内燃机润滑油清净性的方法 Download PDFInfo
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- CN107987918B CN107987918B CN201610985317.4A CN201610985317A CN107987918B CN 107987918 B CN107987918 B CN 107987918B CN 201610985317 A CN201610985317 A CN 201610985317A CN 107987918 B CN107987918 B CN 107987918B
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- alkyl
- acid
- lubricating oil
- internal combustion
- combustion engine
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- 239000000203 mixture Substances 0.000 title claims abstract description 43
- 239000010687 lubricating oil Substances 0.000 title claims abstract description 39
- 238000002485 combustion reaction Methods 0.000 title claims abstract description 26
- 238000000034 method Methods 0.000 title claims abstract description 13
- -1 alkyl salicylate Chemical compound 0.000 claims abstract description 73
- 239000003599 detergent Substances 0.000 claims abstract description 30
- 229960001860 salicylate Drugs 0.000 claims abstract description 30
- 230000003078 antioxidant effect Effects 0.000 claims abstract description 24
- 239000003963 antioxidant agent Substances 0.000 claims abstract description 23
- BDHFUVZGWQCTTF-UHFFFAOYSA-M sulfonate Chemical compound [O-]S(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-M 0.000 claims abstract description 21
- 239000002270 dispersing agent Substances 0.000 claims abstract description 20
- 239000002199 base oil Substances 0.000 claims abstract description 16
- 229910052751 metal Inorganic materials 0.000 claims abstract description 15
- 239000002184 metal Substances 0.000 claims abstract description 15
- 230000001050 lubricating effect Effects 0.000 claims abstract description 10
- 239000003921 oil Substances 0.000 claims description 43
- YGSDEFSMJLZEOE-UHFFFAOYSA-N Salicylic acid Natural products OC(=O)C1=CC=CC=C1O YGSDEFSMJLZEOE-UHFFFAOYSA-N 0.000 claims description 32
- 239000002585 base Substances 0.000 claims description 29
- FJKROLUGYXJWQN-UHFFFAOYSA-N papa-hydroxy-benzoic acid Natural products OC(=O)C1=CC=C(O)C=C1 FJKROLUGYXJWQN-UHFFFAOYSA-N 0.000 claims description 22
- 229960004889 salicylic acid Drugs 0.000 claims description 22
- 238000006243 chemical reaction Methods 0.000 claims description 16
- KZNICNPSHKQLFF-UHFFFAOYSA-N succinimide Chemical compound O=C1CCC(=O)N1 KZNICNPSHKQLFF-UHFFFAOYSA-N 0.000 claims description 16
- 239000003054 catalyst Substances 0.000 claims description 15
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims description 14
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- 239000004711 α-olefin Substances 0.000 claims description 13
- RAXXELZNTBOGNW-UHFFFAOYSA-N imidazole Natural products C1=CNC=N1 RAXXELZNTBOGNW-UHFFFAOYSA-N 0.000 claims description 12
- YGSDEFSMJLZEOE-UHFFFAOYSA-M salicylate Chemical compound OC1=CC=CC=C1C([O-])=O YGSDEFSMJLZEOE-UHFFFAOYSA-M 0.000 claims description 12
- 229920002367 Polyisobutene Polymers 0.000 claims description 11
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- 238000002360 preparation method Methods 0.000 claims description 11
- 229960002317 succinimide Drugs 0.000 claims description 11
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims description 10
- 229920000137 polyphosphoric acid Polymers 0.000 claims description 10
- 239000011701 zinc Substances 0.000 claims description 10
- 229910052725 zinc Inorganic materials 0.000 claims description 10
- 238000005804 alkylation reaction Methods 0.000 claims description 9
- 150000003839 salts Chemical class 0.000 claims description 9
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- LSNNMFCWUKXFEE-UHFFFAOYSA-M Bisulfite Chemical compound OS([O-])=O LSNNMFCWUKXFEE-UHFFFAOYSA-M 0.000 claims description 7
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- 150000001342 alkaline earth metals Chemical class 0.000 claims description 7
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- 230000007935 neutral effect Effects 0.000 claims description 6
- 150000004996 alkyl benzenes Chemical class 0.000 claims description 5
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- 238000006386 neutralization reaction Methods 0.000 claims description 5
- 230000035484 reaction time Effects 0.000 claims description 5
- JOXIMZWYDAKGHI-UHFFFAOYSA-N toluene-4-sulfonic acid Chemical compound CC1=CC=C(S(O)(=O)=O)C=C1 JOXIMZWYDAKGHI-UHFFFAOYSA-N 0.000 claims description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 4
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 4
- JUJWROOIHBZHMG-UHFFFAOYSA-N pyridine Substances C1=CC=NC=C1 JUJWROOIHBZHMG-UHFFFAOYSA-N 0.000 claims description 4
- UMJSCPRVCHMLSP-UHFFFAOYSA-N pyridine Natural products COC1=CC=CN=C1 UMJSCPRVCHMLSP-UHFFFAOYSA-N 0.000 claims description 4
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 3
- AFVFQIVMOAPDHO-UHFFFAOYSA-N Methanesulfonic acid Chemical compound CS(O)(=O)=O AFVFQIVMOAPDHO-UHFFFAOYSA-N 0.000 claims description 3
- 229910002651 NO3 Inorganic materials 0.000 claims description 3
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 claims description 3
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims description 3
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 3
- VLTRZXGMWDSKGL-UHFFFAOYSA-M perchlorate Inorganic materials [O-]Cl(=O)(=O)=O VLTRZXGMWDSKGL-UHFFFAOYSA-M 0.000 claims description 3
- VLTRZXGMWDSKGL-UHFFFAOYSA-N perchloric acid Chemical compound OCl(=O)(=O)=O VLTRZXGMWDSKGL-UHFFFAOYSA-N 0.000 claims description 3
- ITMCEJHCFYSIIV-UHFFFAOYSA-N triflic acid Chemical compound OS(=O)(=O)C(F)(F)F ITMCEJHCFYSIIV-UHFFFAOYSA-N 0.000 claims description 3
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 claims description 2
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- 230000009471 action Effects 0.000 claims description 2
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- 150000001450 anions Chemical class 0.000 claims description 2
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- 150000001768 cations Chemical class 0.000 claims description 2
- XPPKVPWEQAFLFU-UHFFFAOYSA-N diphosphoric acid Chemical compound OP(O)(=O)OP(O)(O)=O XPPKVPWEQAFLFU-UHFFFAOYSA-N 0.000 claims description 2
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- 150000003139 primary aliphatic amines Chemical class 0.000 claims description 2
- 229940005657 pyrophosphoric acid Drugs 0.000 claims description 2
- UNXRWKVEANCORM-UHFFFAOYSA-N triphosphoric acid Chemical compound OP(O)(=O)OP(O)(=O)OP(O)(O)=O UNXRWKVEANCORM-UHFFFAOYSA-N 0.000 claims description 2
- 125000004169 (C1-C6) alkyl group Chemical group 0.000 claims 2
- JXLHNMVSKXFWAO-UHFFFAOYSA-N azane;7-fluoro-2,1,3-benzoxadiazole-4-sulfonic acid Chemical compound N.OS(=O)(=O)C1=CC=C(F)C2=NON=C12 JXLHNMVSKXFWAO-UHFFFAOYSA-N 0.000 claims 2
- 150000003902 salicylic acid esters Chemical class 0.000 claims 1
- 239000011574 phosphorus Substances 0.000 abstract description 14
- 229910052698 phosphorus Inorganic materials 0.000 abstract description 14
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 abstract description 13
- 239000004071 soot Substances 0.000 abstract description 8
- 238000005299 abrasion Methods 0.000 abstract description 6
- 239000008186 active pharmaceutical agent Substances 0.000 abstract description 6
- 230000003647 oxidation Effects 0.000 abstract description 6
- 238000007254 oxidation reaction Methods 0.000 abstract description 6
- 239000010705 motor oil Substances 0.000 abstract description 5
- 239000006185 dispersion Substances 0.000 abstract description 3
- 239000000047 product Substances 0.000 description 21
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 14
- 229910052791 calcium Inorganic materials 0.000 description 14
- 239000011575 calcium Substances 0.000 description 14
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 13
- 239000011593 sulfur Substances 0.000 description 10
- 229910052717 sulfur Inorganic materials 0.000 description 10
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 description 9
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 9
- 239000010710 diesel engine oil Substances 0.000 description 9
- 239000012071 phase Substances 0.000 description 9
- 239000000463 material Substances 0.000 description 7
- 238000003756 stirring Methods 0.000 description 7
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 description 6
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 6
- 230000015572 biosynthetic process Effects 0.000 description 6
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- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 5
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- OZAIFHULBGXAKX-UHFFFAOYSA-N 2-(2-cyanopropan-2-yldiazenyl)-2-methylpropanenitrile Chemical compound N#CC(C)(C)N=NC(C)(C)C#N OZAIFHULBGXAKX-UHFFFAOYSA-N 0.000 description 4
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- 239000002253 acid Substances 0.000 description 4
- 125000000217 alkyl group Chemical group 0.000 description 4
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 description 4
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- GTBGXKPAKVYEKJ-UHFFFAOYSA-N decyl 2-methylprop-2-enoate Chemical compound CCCCCCCCCCOC(=O)C(C)=C GTBGXKPAKVYEKJ-UHFFFAOYSA-N 0.000 description 3
- 238000004821 distillation Methods 0.000 description 3
- GMSCBRSQMRDRCD-UHFFFAOYSA-N dodecyl 2-methylprop-2-enoate Chemical compound CCCCCCCCCCCCOC(=O)C(C)=C GMSCBRSQMRDRCD-UHFFFAOYSA-N 0.000 description 3
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- 229940080264 sodium dodecylbenzenesulfonate Drugs 0.000 description 3
- ATZHWSYYKQKSSY-UHFFFAOYSA-N tetradecyl 2-methylprop-2-enoate Chemical compound CCCCCCCCCCCCCCOC(=O)C(C)=C ATZHWSYYKQKSSY-UHFFFAOYSA-N 0.000 description 3
- 238000005406 washing Methods 0.000 description 3
- KYCQOKLOSUBEJK-UHFFFAOYSA-M 1-butyl-3-methylimidazol-3-ium;bromide Chemical compound [Br-].CCCCN1C=C[N+](C)=C1 KYCQOKLOSUBEJK-UHFFFAOYSA-M 0.000 description 2
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 description 2
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Abstract
本发明提供了一种内燃机润滑油组合物及提高内燃机润滑油清净性的方法。本发明的内燃机润滑油组合物，包括0.5％‑6％的烷基水杨酸盐清净剂，1％‑8％的高碱值磺酸盐清净剂，1％‑8％的低碱值磺酸盐清净剂，1％‑8％的无灰分散剂，0.05％‑3％的抗氧化剂，1％‑15％的粘度指数改进剂和余量的润滑基础油。本发明的内燃机油组合物具有较低的磷含量，较低的金属腐蚀性，优异的高温清净性、烟炱分散性能，较好的抗氧化性及抗磨性，可以满足API CH‑4的性能要求。
Description
技术领域
本发明涉及一种内燃机润滑油组合物，尤其涉及一种适用于柴油机发动机的润滑油组合物。
背景技术
目前，随着柴油机向小尺寸、大功率方向发展，使得柴油发动机的工作温度更高、负荷更大，对于油品的要求更高。例如在柴油发动机内部，活塞顶岸工作温度最高达到300℃以上，这个温度会加剧油品氧化，产生大量的结焦前驱物、有机酸、无机酸等极性物质。同时，油品在这个温度和负荷下工作，会产生大量的烟炱，导致机油变稠和发动机磨损。因此，普通油品的清净、分散、抗氧化、抗磨的能力，已经不能满足以上要求。
另外，现代汽车工业更加注重环保，柴油机油向着低硫、磷含量的方向发展。其中油品低磷更加重要，油品低磷可以保证尾气排放系统催化剂的正常工作。目前，欧洲的重负荷柴油机油规格ACEA 6-04提出硫、磷限制，规定硫含量不大于0.3％，磷含量不大于0.08％，ACEA-04轿车C类油也对硫、磷含量做提出限制，C1不大于0.2％，C2、C3不大于0.3％；磷含量C1不大于0.05％，C2、C3为0.07％～0.09％。
总之，现代柴油机油开发中面临三个主要的问题，即如何进一步提高油品的高温清净性、分散烟炱能力及降低油品的磷含量。
一般说来，要分散油品中结焦前驱物、中和有机酸和无机酸，需要开发性能更优的金属清净剂，要解决油品中烟炱带来的油品变稠、抗磨性变差问题，则要靠性能更好的无灰分散剂和抗磨剂。
目前，在解决高温清净性问题时，常常使用各种清净剂的复配，例如用高碱值磺酸盐和高碱值硫化烷基酚盐复配。要解决烟炱分散性问题，需要采用分散性更好的无灰分散剂。而目前采用的金属清净剂的高温清净性不能完全满足要求，需要增加剂量，这样就造成组合物成本的提高，如果减少其它添加剂加入量，也会使得油品对分散、抗磨性的要求变高。
CN 1523090A介绍了一种发动机润滑油组合物，尤其是一种用于重负荷柴油发动机的润滑油组合物，其中含有适量的高碱值水杨酸盐、低碱值水杨酸盐、硫化烷基酚盐、硼化双丁二酰亚胺无灰分散剂、高分子无灰分散剂、二烷基二硫代磷酸锌及酚型、胺型辅助抗氧剂。该润滑油组合物可满足SAE J 300和API CF-4柴油机油的规格要求。该组合物配方简单，成本低，调制方便。
CN 101935574A介绍了一种发动机润滑油组合物，尤其是一种用于重负荷柴油发动机的润滑油组合物，该组合物含有适量的烷基水杨酸盐、硫化烷基酚盐、磺酸盐、高分子无灰分散剂、聚异丁烯双丁二酰亚胺无灰分散剂、二烷基二硫代磷酸锌、酚型抗氧剂、胺型抗氧剂以及含硫型抗氧抗磨剂，可满足GB11122-2006规定的CF-4柴油机油的规格要求。
CN 1782049A涉及一种润滑油组合物，以组合物总重为基准，包括下列组分；A)至少一种数均分子量为1500～4000的高分子量聚异丁烯丁二酰亚胺无灰分散剂，含量为25～50w％；B)至少一种硼含量为0.05～4.0w％的硼化聚异丁烯丁二酰亚胺分散剂，含量为3～18w％；C)至少一种与酚偶联的聚异丁烯丁二酰亚胺分散剂，含量为2～18w％；D)至少一种金属清净剂，含量为25～45w％；E)至少一种抗氧抗腐剂，含量为3～18w％。该组合物具有优异的烟炱分散性能，同时赋予油品良好的抗氧化、抗腐蚀性能，加入到高粘度指数的I类、II类基础油或合成基础油中，可以调配出CF-4或以上级别的高档柴油机油。
US 5719107使用硼化的高分子量聚异丁烯丁二酰亚胺调配重负荷柴油机油，油品能够达到API CF-4、CG-4的要求。
CN 1746280A公开了一种低硫、低磷和低灰分的润滑油组合物，其中硫含量小于0.3wt％，磷含量小于0.08wt％，灰分小于0.8wt％，该组合物中使用了含硼的添加剂和总碱值为200～400mgKOH/g的烷基水杨酸盐，其中无灰分散剂中的氮与硼的质量比为3～5：1，该组合物具有降低润滑油粘度和提高活塞清净性的作用。
US 6569818公开了一种润滑油组合物，其中的金属清净剂选自碱值为10～350mgKOH/g的非硫化的碱金属或碱土金属的烷基水杨酸盐、或非硫化的具有曼尼奇(Mannich)碱结构的烷基酚衍生物的碱金属或碱土金属盐。
通过以上专利看出，为了满足柴油机油苛刻的高温清净性要求，润滑油组合物中不同结构的清净剂复配时容易产生沉淀。同时，现有的烷基水杨酸盐合成时采用的工艺一般为柯尔贝－施密特(Kolbe-Schmidt)反应得到，产品中残留的烷基酚较多，使得产品的清净性、分散性等不能满足高质量柴油机油的要求。因此，现有的技术中仍然需要改进。
发明内容
本发明提供了一种内燃机润滑油组合物及提高内燃机润滑油清净性的方法。
本发明的内燃机润滑油组合物，包括0.5％-6％的烷基水杨酸盐清净剂，1％-8％的高碱值磺酸盐清净剂，1％-8％的低碱值磺酸盐清净剂，1％-8％的无灰分散剂，0.05％-3％的抗氧化剂，1％-15％的粘度指数改进剂和余量的润滑基础油。
本发明所述的烷基水杨酸盐的制备方法包括：将烷基水杨酸、溶剂、促进剂、中性油、碱金属和/或碱土金属的氧化物、水、助促进剂A进行中和反应，然后加入助促进剂B、通入二氧化碳进行碳酸化反应，收集产物。
所述烷基水杨酸的制备方法是：将α-烯烃、水杨酸和/或水杨酸酯在催化剂作用下进行烷基化反应，收集产物；所述催化剂是将离子液体、多聚磷酸和有机酸盐在30～100℃混合1～12h而得。
所述的α-烯烃为C10-C30的α-烯烃，优选C12-C24的α-烯烃，最优选C14-C20的α-烯烃。
所述的水杨酸酯是C1-C4的水杨酸酯，优选C1-C2的水杨酸酯，最优选水杨酸甲酯。
所述的水杨酸和/或水杨酸酯与α-烯烃的摩尔比为1～2：1，优选1～1.6：1，最优选1.1～1.3：1。
所述离子液体的阳离子为烷基咪唑或烷基吡啶，所述离子液体的阴离子为四氟硼酸根、三氟甲基磺酸根、六氟磷酸根、对甲苯磺酸根、硝酸根、高氯酸根、甲磺酸根、草酸根和硫氢酸根中的一种。
所述烷基咪唑的结构为：
其中的R1、R2分别独立地选自C1-C6的烷基，优选C1-C4的烷基。
所述烷基吡啶的结构为：
其中的R为C1-C6的烷基，优选C1-C4的烷基。
所述四氟硼酸根、三氟甲基磺酸根、六氟磷酸根、对甲苯磺酸根、硝酸根、高氯酸根、甲磺酸根、草酸根和硫氢酸根的结构依次为：
所述离子液体可以选用烷基咪唑四氟硼酸盐、烷基咪唑三氟甲基磺酸盐、烷基咪唑六氟磷酸、烷基咪唑硫氢酸盐、烷基吡啶四氟硼酸盐、烷基吡啶三氟甲基磺酸盐、烷基吡啶六氟磷酸和烷基吡啶六氢酸盐中的一种或多种。
所述多聚磷酸的结构为：Hn+2PnO3n+1，其中n为大于等于1的正整数，优选1-3的正整数。
所述多聚磷酸可以选用磷酸(H3PO4)、焦磷酸(H4P2O7)和三聚磷酸(H5P3O10)中的一种或多种。
所述有机酸盐优选有机羧酸的金属盐和/或有机磺酸的金属盐。所述的有机羧酸优选C2-C18的脂肪酸，最优选C3-C15的脂肪酸。所述的有机磺酸优选C6-C18的磺酸或带有C6-C18烷基的苯磺酸，最优选带有C8-C15烷基的苯磺酸。所述的金属是碱金属和/或碱土金属，例如锂、钠、钾、钙、镁和钡中的一种或多种，优选钠和/或钙。
所述催化剂是将离子液体、多聚磷酸和有机酸盐在30-100℃混合1-12h而得，其中所述离子液体、多聚磷酸和有机酸盐之间的质量比为100：5～30：5～20，优选100：10～25：5～15。
所述催化剂的加入量是α-烯烃、水杨酸和/或水杨酸酯的总质量的1％-100％，优选2％-50％，最优选3％-10％。
所述烷基化反应的温度为50～250℃，优选80～200℃，最优选100～160℃。
所述烷基化反应的时间为1～16小时，优选2～12小时，最优选3～8小时。
本发明所述碱金属和/或碱土金属的氧化物可以选用氧化钠、氧化锂、氧化钙、氧化镁和氧化钡中的一种或多种，优选氧化钠、氧化锂、氧化钙和氧化镁中的一种或多种，最优选氧化钙。
本发明所述溶剂可以是烷烃，也可以是芳香烃，优选馏程在60～180℃的直馏汽油、正辛烷、苯、甲苯和二甲苯中的一种或多种。
本发明所述中性油优选100℃运动粘度为2～6mm2/S的润滑基础油，例如可以选用100SN、150SN润滑油老三套工艺处理油和100N、150N加氢精制油中的一种或多种。
本发明所述的促进剂为C1～C4醇，优选为甲醇、乙醇、丙醇、丁醇和乙二醇中的一种或多种。所述促进剂可以作为无机相和有机相的载体，使得反应混合物中气、液、固三相之间的传质速率更快，油相和水相混合均匀，使反应易于进行。
本发明所述的助促进剂A为C4-C10的脂肪族伯胺、氨水和氯化钙中的一种或多种。
本发明所述的助促进剂B为聚甲基丙烯酸酯和/或聚丙烯酸酯，优选甲基丙烯酸C1～C25烷基酯的共聚物和/或丙烯酸C1～C25烷基酯的共聚物。
在本发明的烷基水杨酸盐的制备方法中，烷基水杨酸的用量为100份；促进剂的用量为20～200份，优选为40～100份；溶剂的用量为200～800份，优选为100～300份；中性油的用量为50～300份，优选为80～150份；碱金属和/或碱土金属的氧化物的用量为15～150份，优选为15～100份；水的用量为10～50份，优选为20～40份；助促进剂A的用量为2～50份，优选为5～50份；助促进剂B的用量为1～50份，优选为1～30份。
在本发明的烷基水杨酸盐的制备方法中，所述中和反应的温度为40～60℃，优选为45～55℃，反应时间优选20～60min。
在本发明的烷基水杨酸盐的制备方法中，所述二氧化碳的通入量为理论值的60％～140％，所述二氧化碳通入量的理论值是：与烷基水杨酸反应后剩余的碱金属和/或碱土金属的氧化物再与二氧化碳发生完全反应的量；所述碳酸化反应的温度是40～60℃，优选为45～55℃，反应时间优选30～100min。
合成所述烷基水杨酸盐清净剂中的烷基水杨酸是由水杨酸和/或水杨酸酯与长链烯烃经烷基化反应得到，烷基化反应采用的催化剂是前述的离子液体、多聚磷酸、有机酸盐复合催化剂，环保、高效。合成的烷基水杨酸中游离的烷基酚含量低，使得烷基水杨酸盐产品中副产物少，清净剂得到改善。
本发明中使用的高碱值磺酸盐为碱值大于等于300mgKOH/g的磺酸盐清净剂，优选碱值为300-400mgKOH/g的烷基苯磺酸钙清净剂和/或烷基苯磺酸镁清净剂。
本发明中使用的低碱值磺酸盐为碱值在20-50mgKOH/g之间的磺酸盐清净剂，优选碱值在20-35mgKOH/g之间的烷基苯磺酸钙清净剂和/或烷基苯磺酸镁清净剂。
本发明所述的无灰分散剂优选聚异丁烯丁二酰亚胺无灰分散剂，更优选聚异丁烯单丁二酰亚胺和聚异丁烯双丁二酰亚胺的混合物，二者比例在1:1-1:6。
本发明所述的抗氧化剂为二烷基二硫代磷酸锌和无灰抗氧化剂的混合物，二者之间的质量比为1：2-1：10。所述二烷基二硫代磷酸锌优选二(C4-C8)烷基二硫代磷酸锌。所述无灰抗氧化剂是烷基芳胺型和/或屏蔽酚型抗氧剂，常用的烷基芳胺型抗氧剂是二烷基二苯胺，常用的屏蔽酚型抗氧剂是2,6二叔丁基对甲酚或者是β-(3,5-二叔丁基-4-羟基苯基)丙酸辛酯。
本发明所述的粘度指数改进剂优选数均分子量为50000～100000的乙丙共聚物，优选的乙丙共聚物中乙烯含量为40～60质量％，丙烯含量为60～40质量％。使用粘度指数改进剂可以调制内燃机润滑油的粘度，提高内燃机的工作效率，节约燃料。
本发明组合物中所用的润滑基础油优选烃类润滑基础油，例如可以选用API Ⅰ类油、Ⅱ类油、Ⅲ类油和Ⅳ类油中的一种或多种，更优选100℃粘度为3～20mm2/s的润滑基础油。
本发明的提高内燃机润滑油清净性的方法是将前面所述的烷基水杨酸盐加入到内燃机润滑油中。
本发明的内燃机油组合物具有较低的磷含量，较低的金属腐蚀性，优异的高温清净性、烟炱分散性能，较好的抗氧化性及抗磨性，可以满足API CH-4的性能要求。
具体实施方式
内燃机润滑油组合物的性能评价方法如下：
高温清净性：
在L-1型板式成焦器上进行成漆和成焦板实验。成焦：板温/油温＝320℃/100℃，时间2小时，停/开时间＝45秒/15秒。成漆：板温/油温＝300℃/150℃，时间2小时，连续。
在L-A型清净性试验仪上进行试验，以考察其高温清净性。板温/油温＝300℃/100℃，时间1小时，停/开时间＝40秒/20秒。油滴速度1.0ml/min。
抗氧化安定性：
用PDSC压力差示扫描量热方法考察油品的热氧化安定性。
分散性试验：
将2.5％的碳黑分散于油中，高速搅拌后，50℃恒温18h，滴油，计算扩散圈和油圈比值。
油膜破裂负荷：GB/T3142-82润滑剂的减摩抗磨性能评价方法。
磨斑直径：SH/T 0189润滑油抗磨损性能测定法(四球机法)。
ASTM D5968(CBT)金属腐蚀性评定方法。
实施例1催化剂制备
1-甲基-3-丁基咪唑四氟化硼盐-偏磷酸-十二烷基苯磺酸钠催化剂IL-1的合成
在三口烧瓶中加入1mol N-甲基咪唑、1.05mol 1-溴代正丁烷，通入N2吹扫20mim后，开启搅拌并加热至85℃维持30～36h。反应结束后静置冷却至室温，溶液下层为淡黄色，上层为未反应的原料。倾去上层液体，将3倍体积的乙酸乙酯加入到下层液体中清洗，然后分离出乙酸乙酯，以除去未反应的原料。洗完后，在70℃干燥24h，得到淡黄色粘稠的1-甲基-3-丁基咪唑溴盐。
将得到的1-甲基-3-丁基咪唑溴盐溶解于二氯甲烷中，在其中加入NaBF4含量为1mol的水溶液，常温下搅拌反应24h。反应完毕，将二氯甲烷相用水少量多次洗涤，然后利用旋转蒸发仪除去二氯甲烷，真空干燥，得到离子液体1-甲基-3-丁基咪唑四氟化硼盐。
取上述合成的1-甲基-3-丁基咪唑四氟化硼盐100克，加入到三口烧瓶中，加入10克偏磷酸，7克十二烷基苯磺酸钠，升温到75℃，搅拌3小时，形成黄色粘稠液体，即为1-甲基-3-丁基咪唑四氟化硼盐-偏磷酸-十二烷基苯磺酸钠催化剂，记为IL-1。
实施例2 IL-1催化的水杨酸烷基化反应
在500mL三口烧瓶中加入20克催化剂IL-1、100克C16α-烯烃(Mn＝224.4，0.446摩尔)、70.78克水杨酸(Mn＝138.12，0.512摩尔)，通入氮气，开启搅拌，加热，控制温度在140℃-142℃之间，反应5小时。
反应结束后，将三口烧瓶降温，当物料降温至40℃以下时，停止搅拌，加入150克120号溶剂汽油。将三口烧瓶中的物料取出，置于分液漏斗中分层，收集上层的油相，下层的离子液体可以重复使用。在油相中加入300克蒸馏水洗涤三次，脱除油相中未反应的水杨酸，并用无水硫酸镁干燥油相，最后得到深褐色的烷基水杨酸A。
用气相色谱外标法分析油相中的剩余α-烯烃的含量，计算后发现，烷基水杨酸A的转化率为90.2％，产物烷基水杨酸A的酸值为63.2mgKOH/g(SH/T0092石油酸检验法)。
实施例3聚甲基丙烯酸酯PMA1的合成
在三口烧瓶中，加入40克基础油150SN(中国石化燕山石化生产，100℃运动粘度为5.7mm2/s)，15克甲基丙烯酸癸酯，5克甲基丙烯酸甲酯，30克甲基丙烯酸十四醇酯，10克甲基丙烯酸十二醇酯，加入0.08克偶氮二异丁腈，引入氮气保护反应物，打开搅拌并升温至75℃，此时观察反应物有明显的放热，控制反应温度为90℃，预聚反应2小时，物料明显变粘稠，再加入0.05克偶氮二异丁腈，逐渐升温至105℃进行共聚反应5小时，得到浅黄色的粘稠液体。在氮气保护下，将反应后物料降至25℃，得到甲基丙烯酸甲酯、甲基丙烯酸癸酯、甲基丙烯酸十二醇酯、甲基丙烯酸十四醇酯的四元共聚物，为本发明所述的润滑油粘度指数改进剂PMA1。在所得的共聚物中，各聚合单体含量分别为：甲基丙烯酸甲酯8.3质量％、甲基丙烯酸癸酯25质量％、甲基丙烯酸十二醇酯16.7质量％、甲基丙烯酸十四醇酯50质量％，其Mn为25280。
实施例4高碱值烷基水杨酸钙的合成
在带有电动机搅拌器及冷凝管的500毫升三口烧瓶中加入烷基水杨酸A100克，120号溶剂汽油250毫升，甲醇25克，蒸馏水6克，150SN中性油50克(中国石化燕山石化公司生产)，氢氧化铵6克，氧化钙30克，聚甲基丙烯酸酯(PMA1)5克，控制反应温度在45～50℃，中和反应30min后，通入二氧化碳，通气速率在0.062L/min之间，通入量达到理论值(10.74L)的90％时，停止通气，然后升温到120℃脱醇、水。得到的物料中加入100毫升汽油，然后放入医用离心机中，以转速4000rpm离心，将离心后的闪蒸物放入带有减压设施的蒸馏瓶中，首先升温到120℃常压蒸馏，然后给系统进行减压蒸馏，最后得到棕褐色的粘稠的175克添加剂。产品的碱值为298mgKOH/g，浊度为72JTU，产品粘度为62.3mm2/s。
内燃机油组合物的实施例5～8和对比例1-4
将150SN、500SN、150BS按70：25：5的质量比调制成基础油，其性能可以满足15W/40基础油的要求。
将高、低碱值磺酸盐清净剂、高碱值烷基水杨酸钙、抗氧化剂、无灰分散剂、粘度指数改进剂加入调制好的基础油中制成内燃机油组合物的实施例5～8和对比例1-4，使用的添加剂名称和指标如下：
清净剂：
高碱值磺酸钙：碱值311mgKOH/g，钙含量10.2质量％，硫含量1.8质量％；
低碱值磺酸钙：碱值28mgKOH/g，钙含量1.5质量％，硫含量2质量％；
高碱值烷基水杨酸钙A(实施例4合成)，碱值为298mgKOH/g，钙含量10.9质量％；
高碱值烷基水杨酸钙B，296mgKOH/g(采用传统的KB反应得到烷基水杨酸，再钙化得到高碱值产品)，钙含量10.9质量％。
无灰分散剂：
单聚异丁烯丁二酰亚胺(T151)，氮含量2.1质量％，碱值为50mgKOH/g；
双聚异丁烯丁二酰亚胺(T152)，氮含量1.25质量％，碱值为55mgKOH/g。
抗氧化剂：
二烷基二硫代磷酸锌(T203)，锌含量10.2质量％，硫含量14.0质量％，磷含量7.7质量％；
二烷基二苯胺(T534)，氮含量4.634质量％，碱值为179mgKOH/g；
T512酚酯型抗氧剂，闪点(开口)224℃，密度(20℃)0.9628g/cm3；
二烷基二硫代氨基甲酸酯，闪点大于170℃，无锡南方添加剂公司生产。
粘度指数改进剂(T613)：乙丙共聚物，分子量Mn为85000，乙烯含量51质量％，丙烯含量49质量％。
各个内燃机润滑油组合物的配方组成见表1，组合物的磷含量、清净性、抗氧化性、分散性、抗磨性和金属腐蚀性价结果见表2。
表1内燃机润滑油组合物的实施例和对比例
表2性能评定
由表2数据可以看出，本发明的内燃机油组合物具有优异的高温清净性、烟炱分散性、抗氧化性、低温性能、抗磨性，可以满足API 15W/40CH-4的技术要求。
Claims (7)
1.一种内燃机润滑油组合物，包括0.5%-6%的烷基水杨酸盐清净剂，1%-8%的高碱值磺酸盐清净剂，1%-8%的低碱值磺酸盐清净剂，1%-8%的无灰分散剂，0.05%-3%的抗氧化剂，1%-15%的粘度指数改进剂和余量的润滑基础油； 所述烷基水杨酸盐清净剂的制备方法包括：将烷基水杨酸、溶剂、促进剂、中性油、碱金属和/或碱土金属的氧化物、水、助促进剂A进行中和反应，然后加入助促进剂B、通入二氧化碳进行碳酸化反应，收集产物；所述的促进剂为C1～C4醇；所述的助促进剂A为C4-C10的脂肪族伯胺、氨水和氯化钙中的一种或多种；所述的助促进剂B为聚甲基丙烯酸酯和/或聚丙烯酸酯；在所述烷基水杨酸盐清净剂的制备方法中，烷基水杨酸的用量为100份；溶剂的用量为200～800份；促进剂的用量为20～200份；中性油的用量为50～300份；碱金属和/或碱土金属的氧化物的用量为15～150份；水的用量为10～50份；助促进剂A的用量为2～50份；助促进剂B的用量为1～50份； 所述烷基水杨酸的制备方法是：将α-烯烃、水杨酸和/或水杨酸酯在催化剂作用下进行烷基化反应，收集产物；所述催化剂是将离子液体、多聚磷酸和有机酸盐在30～100℃混合1～12h而得；所述催化剂的加入量是α-烯烃、水杨酸和/或水杨酸酯的总质量的1%-100%； 所述离子液体的阳离子为烷基咪唑或烷基吡啶，所述离子液体的阴离子为四氟硼酸根、三氟甲基磺酸根、六氟磷酸根、对甲苯磺酸根、硝酸根、高氯酸根、甲磺酸根、草酸根和硫氢酸根中的一种；
所述烷基咪唑的结构为：
其中的R1、R2分别独立地选自C1-C6的烷基；
所述烷基吡啶的结构为：
其中的R为C1-C6的烷基；
所述多聚磷酸的结构为：Hn+2PnO3n+1，其中n为大于等于1的正整数；
所述有机酸盐选自有机羧酸的金属盐和/或有机磺酸的金属盐； 所述离子液体、多聚磷酸和有机酸盐之间的质量比为 100：5～30：5～20。
2.按照权利要求1所述的润滑油组合物，其特征在于，所述的α-烯烃为C10-C30的α-烯烃，所述的水杨酸酯是C1-C4的水杨酸酯，所述的水杨酸和/或水杨酸酯与α-烯烃的摩尔比为1～2：1。
3.按照权利要求1所述的润滑油组合物，其特征在于，所述离子液体选自烷基咪唑四氟硼酸盐、烷基咪唑三氟甲基磺酸盐、烷基咪唑六氟磷酸、烷基咪唑硫氢酸盐、烷基吡啶四氟硼酸盐、烷基吡啶三氟甲基磺酸盐、烷基吡啶六氟磷酸和烷基吡啶六氢酸盐中的一种或多种；所述多聚磷酸选自磷酸、焦磷酸和三聚磷酸中的一种或多种；所述有机酸盐选自有机羧酸的金属盐和/或有机磺酸的金属盐，所述的有机羧酸选自C2-C18的脂肪酸，所述的有机磺酸选自C6-C18的磺酸或带有C6-C18烷基的苯磺酸，所述的金属是碱金属和/或碱土金属。
4.按照权利要求1所述的润滑油组合物，其特征在于，所述烷基化反应的温度为50～250℃，所述烷基化反应的时间为1～16小时。
5.按照权利要求1所述的润滑油组合物，其特征在于，在所述烷基水杨酸盐的制备方法中，所述中和反应的温度为40～60℃，反应时间为20～60min；所述二氧化碳的通入量为理论值的60％～140％；所述碳酸化反应的温度为40～60℃，反应时间为30～100min。
6.按照权利要求1所述的润滑油组合物，其特征在于，所述高碱值磺酸盐为碱值大于等于300 mgKOH/g的磺酸盐清净剂；所述低碱值磺酸盐为碱值在20-50 mgKOH/g之间的磺酸盐清净剂；所述的无灰分散剂选自聚异丁烯丁二酰亚胺无灰分散剂；所述的抗氧化剂为二烷基二硫代磷酸锌和无灰抗氧化剂的混合物，二者之间的质量比为1：2 - 1：10；所述的粘度指数改进剂选自数均分子量为50000～100000的乙丙共聚物；所用的润滑基础油选自烃类润滑基础油。
7.一种提高内燃机润滑油清净性的方法，其特征在于，将权利要求1-6之一中所述的烷基水杨酸盐加入到内燃机润滑油中。
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