CN1132781A - 润滑脂组合物 - Google Patents

润滑脂组合物 Download PDF

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Publication number
CN1132781A
CN1132781A CN95121840A CN95121840A CN1132781A CN 1132781 A CN1132781 A CN 1132781A CN 95121840 A CN95121840 A CN 95121840A CN 95121840 A CN95121840 A CN 95121840A CN 1132781 A CN1132781 A CN 1132781A
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Prior art keywords
grease
composition
lubricating grease
tricalcium phosphate
thickening material
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CN95121840A
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CN1056173C (zh
Inventor
尾崎幸洋
宗像智郎
川村靖
高濑和则
土谷哲夫
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Showa Shell Sekiyu KK
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Showa Shell Sekiyu KK
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Abstract

一种润滑脂组合物包括润滑脂和作为添加剂加入该润滑脂中的(A)和(B)，该润滑脂含基础油和包括分子式为Ca3(PO4)2的磷酸三钙和脲化合物的混合物的增稠剂，(A)是上结构式(I)的硫化二烷基二硫代氨基甲酸钼，在结构式中R1和R2各自代表选自具有1-24个碳原子的烷基的基团；m为0或1-3的整数，n是1-4的整数，条件是m+n＝4，和(B)是结构式如(II)的磷硫代硫酸三苯酯。

Description

润滑脂组合物
本发明涉及一种润滑脂组合物，该组合物用于汽车等速万向节(CVJ)、球窝接头和轮轴轴承，用于需要润滑的各种部件、例如轴承和齿轮，用于钢铁工业和其它工业的机器。
随着节省劳力或使机器小型化、减轻其重量和增加速度等近代工业的趋势，就用于这些工业机器的轴承和齿轮而论、对高级润滑脂的要求不断增长，要求其具有优良的性能特征的组合，这些性能特征如象耐热性、荷载能力、耐磨性能以及长寿命。例如，经常用于前轴驱动汽车的等速万向节的润滑，由于机动车功率和速度增加而等速万向节本身的重量减轻的趋热，要求润滑脂具有优良的耐用性、抗磨性和耐热性能。
另一方面，在钢铁厂由于设备简化和现代化的结果，轧钢机逐渐变为高速轧机或有密封轴承的轧机。由于这些，这种用途的润滑脂不仅大大地为节能所需，而且也需要有优良的荷载能力、耐热和长寿命等优良性能特征组合。因此，随着机器的进步，对于用于汽车和钢铁工业等各种工业领域的润滑脂的性能特征的要求变得更加苛刻。对于机器润滑脂的主要要求业已由称之为＂通用润滑脂＂或＂多用润滑脂＂的锂皂润滑脂变为用脲润滑脂，脲润滑脂有优良遥耐热性，能够与添加剂产生协合作用，以摩擦力。
在这种情况下，例如在U.S.P.4,840,740、4,514,312和4,787,992中介绍了代表性的技术。U.S.P.4,840,740分开了包括含有有机钼化物和二硫代磷酸锌组合物的脲润滑脂的润滑脂组合物。U.S.P.4,514,312公开了包括含有芳香胺硫代磷酸酯的脲润滑脂的润滑脂组合物。U.S.P.4,787,992公开了包括用钙皂、钙配合皂或这些任一与脲化物的混合物增稠的润滑脂和含有组合的磺酸钙和磷酸三钙作添加剂的润滑脂的组合物。JP-B-4-34590(这里所用的＂JP-B＂这个术语指的是＂已审查的日本专利公告)公开了包括含有作为必要成分的硫磷化极压添加剂的脲润滑脂的组含物，该添加剂包括(A)和(B)的组合，(A)是硫化的二烷基二硫代氨基甲酸铜，(B)是选自硫化脂和油硫化烯烃、磷酸二甲苯酯、硫代磷酸三烷基酯二烷基二硫代磷酸锌中的至少一种。此外，JP-B-4-65119公开了由通过捏合分子式为Ca3(Po4)2的磷酸三钙和基(础)油混合物而得到的润滑脂组合物。
不过，这些专利组合物有如下缺点。基于脲润滑脂的这些组合物的每一种，尽管预计到润滑脂和添加剂产生协合作用会减小摩擦力，但其载荷能力和耐热性能仍然不好。另一方面，磷酸三钙润滑脂的缺点在于虽然其在载荷能力和耐热性能方面优于脲润滑脂，但在耐磨性能方面稍差。
本发明的目的是进一步改进JP-B-4-65119公开的脲润滑脂和磷酸三钙润滑脂，从而提供在载荷能力、耐磨性能和耐热性能等方面均优于这些润滑脂的润滑脂组合物。
本发明涉及含润滑脂、和加入该润滑脂中作为添加剂的(A)和(B)的一种润滑脂组合物，润滑脂包括基(础)油和含由分子式为Ca3(Po4)2的磷酸三钙和脲化物酸的混合物的增稠剂，(A)是结构式为：
Figure A9512184000061
的硫化二烷基二硫代氨基甲酸钼，结构式中R1和R2各自代表选自具有1-24个碳原子的烷基的一个基团；m为o或1-3的一个整数，n是1-4的一个整数，条件是m＋n＝4，和(B)是结构式如下的磷硫代硫酸三苯酯，
Figure A9512184000062
其中，按组合物的总重量计，增稠剂、组分(A)和组分(B)和用量分别为2-35％(wt)、0.5-10％(Wt)和0.1-10％(wt)。
组分(A)的硫化二烷基二硫代氨基甲酸钼的实例包括硫化二乙基二硫代氨基甲酸钼、硫化二丁基二硫代氨基甲酸钼、硫化二异丁基二硫代氨基甲酸钼、硫化二(2-乙基己基)二硫代氨基甲酸钼、硫化二戊基二硫代氨基甲酸钼、硫化二异戊基二硫代氨基甲酸钼、硫化二月桂基二硫代氨基甲酸钼和硫化二硬脂酰二硫代氨基甲酸钼。按组合物的总重量计，组分(A)的加入量为0.5-10％(wt)。优选0.5-5％(wt)。如果加入量低于0.5(wt)，不能有效地增进耐磨性能和减小摩擦。如果加入量超过10％(wt)，所需的效应不再增高。
组分(B)的磷硫代硫酸三苯酯的用量按组合物的总重量计为0.1-10％(wt)，优选0.1-5％(wt)。如果其用量低于0.1％(wt)，耐磨性能和减摩性能不能改善。如果其用量超过10％(wt)，润滑性能不好。
众所周知的脲化物增稠剂可以用作可用于与磷酸三钙组合作为增稠剂的脲化合物。该脲化物不特别局限于种类。其实例包括二脲、三脲和四脲。
按组合物的总量计，增稠剂的用量为2-35％(wt)。在增稠剂中，磷酸三钙和脲化物的比例优选分别为5-95％(wt)和95-5％(wt)。这种增稠剂可以与一种或多种其它增稠剂组合使用，只要磷酸三钙和脲化合物在所有增稠剂中的总含量至少为50％(wt)。
基础油是矿物油和/或合成油。可以另外将添加剂，例如抗氧化剂、防腐剂、极压添加剂和聚合物加到本发明的组合物中。
参看实施例和比较实施例将解释本发明，但是不会以任何方式将本发明局限于此。除非另外表明，所有份数、百分数、比值(ratios)等都按重量给出。
实施例1-9和比较倒1-11
按照表l-6中所列出的每个配方(所有用量数值均以％(wt)给出)，将添加剂加到基础润滑脂中。所得的每种混合物用三辊辊辗机
Figure A9512184000071
合以制得实施例和比较实施例的润滑脂。
基(础)润滑脂组合物如下所示。正如在表1-6中所示那样，用作基(础)油的精制矿物油100℃下粘度为15mm2/s，季戊四醇酯油100℃下粘度为5mm2/s。
I、磷酸三钙/四脲润滑脂(在表中这种增稠剂用Ca/4U代表)。
两摩尔二苯甲烷4，4′-二异氰酸酯与在基(础)油中的2摩尔硬脂酰胺和1摩尔乙二胺反应。然后加入磷酸三钙，使之均匀分散在其中，得到一种润滑脂。
II.磷酸三钙/二脲润滑脂(在表中这种增稠剂用Ca/2U表示)
一摩尔二苯甲烷4，4′-二异氰酸酯与在基(础)油中的二摩尔辛胺反应。然后加入磷酸三钙，使之均匀分散在其中得到一种润滑脂。
III.磷酸三钙润滑脂
将磷酸三钙均匀分散在基(础)油中的得到润滑脂。
IV四脲润滑脂
二摩尔二苯甲烷4，4′-二异氰酸酯与在基(础)油中的二摩尔硬脂酰胺和1摩尔乙二胺反应。得到的脲化合物均匀分散在基(础)，得到润滑脂。
V.二脲润滑脂
1摩尔二苯甲烷4，4′-二异氰酸酯与在基础油中的二摩尔辛胺反应。将得到的脲化物均匀分散在基(础)油中，得到润滑脂。
VI.锂皂润滑脂
12-羟基硬脂酸锂均匀溶于基础油中，得到润滑脂。
                  表1
组成            实施例
           1      2      3
基(础)油
矿物油          75     76     79.5
季戊四醇酯油    -      -       -
增稠剂
Ca/4U           20     20      17
               (80/20)(80/20)  (50/50)
Ca/2U           -      -       -
添加剂
Mo-DTC          3      3       3
TPPT            2      1       0.5
                ---    ---     ---
总计            100    100     100(注)·所用的季戊四醇酯油是EMERY2935，由Emery Industries，Inc制造的。·在＂增稠剂＂下面每个()给出的比例表明或磷酸三钙对四脲或磷酸三钙对二脲的比例。·Mo-DTC是硫化二烷基二硫代氨基甲酸钼Sakuralube 600，由Asa-hi Denka Kogyo K.K制造的。·TPPT是硫代磷酸三苯酯(triphenyl Phosphorothionate)Irha-lube TPPT，由Ciba-Geigy Ltd.制造的。
               表2
组成                  实施例
                  4     5      6
基(础)油
矿物油           77    80      79
季戊四醇酯油     -     -       -
增稠剂
Ca/4U            17    15      15
              (50/50) (20/80)(20/80)
Ca/2U             -     -       -
添加剂
Mo-DTC           5     3       5
TPPT             1     2       1
                 ---   ---     ---
总计             100   100     100
                表3
组成                   实施例
                 7      8       9
基(础)油
矿物油           -     77.5     84
季戊四醇酯油     74    -        -
增稠剂
Ca/4U            22    -        -
                      (50/50)
Ca/2U                   -       17.5       10
                                (80/20)   (20/80)
添加剂
Mo-DTC                  3        3          5
TPPT                    1        2          1
                       ---      ---        ---
总计                   100      100        100
                 表4
组成                      比较实施例
                       1     2     3     4
基础油
矿物油                 71   71    72     81
增稠剂
磷酸三钙               25   25    25     -
四脲                   -    -     -      14
二脲                   -    -     -      -
锂皂                   -    -     -      -
添加剂
Mo-DTC                 3    3     -      3
TPPT                   1    -     -      -
硫化脂或油         -         -        -        -
环烷酸铅           -         -        -        -
硫化烯烃           -         -        3        -
Mo-DTP             -         1        -        2
                 ----       ---      ---       ---
总计             100        100      100       100(注)·所用的硫化脂或油是Lubrizol 5006，由Lubrizol Corp.制造的。·所用的环烷酸铅是Dailube L-30，由Dainippon Ink&Chemic-als，Inc制造的。·所用的硫化烯烃是Lubrizol 5340，由Lubrizol corp.制造的。·Mo-DTP是二硫代磷酸钼Sakuralube 300，由Asahi Denka KogyoK.K.制造的。
                  表5
组成                   比较实施例
                  5       6      7     8
基础油
矿物油           83      83      82    88
增稠剂
磷酸三钙         -       -       -     -
四脲             14      14      14    -
二脲             -       -       -     9
锂皂            -        -       -      -
添加剂
Mo-DTC          -        -       3      3
TPPT            -        -       1      -
硫化脂或油      3        -       -      -
环烷酸铅        -        -       -      -
硫化烯烃        -        3       -      -
Mo-DTP          -        -       -      -
                ---     ---     ---    ---
总计            100     100     100    100
                表6
组成                   比较实施例
                   9      10      11
基(础)油
矿物油            86      88      88
增稠剂
磷酸三钙          -       -       -
四脲              -       -       -
二脲              -       -       -
锂皂              9       9       9
添加剂
Mo-DTC             -       -       3
TPPT               -       -       -
硫化脂或油         3       -       -
环烷酸铅           2       -       -
硫化烯烃           -       3       -
Mo-DTP             -       -       -
                   ---     ---     ---
总计               100     100     100
将表1-6中所列的润滑脂组合物进行下列试验以评价载荷能力、耐磨性能和耐热性能。所得结果列于表7-12中。
(1)载荷能力
(4-球EP试验)
按照ASTM D2596确定烧结负荷(kgf)、最大非胶住载荷(kgf)和负荷一磨损指数。
转速：1770rpm
负荷：规定的段式加载
温度：室温
时间：10秒(2)耐磨性能
(法列克司试验)(Falex test)
根据The Institute of Petroleum in the Umited Kingdom的IP241/69，在下列条件下开始试验以后15分钟确定摩擦系数。
转速：290rpm
负荷：200Ib
温度：室温
时间：15分钟
润滑脂量：每个试验片样大约1克(3)耐热性能
(薄膜蒸发损失试验)
根据JIS Z0236将润滑脂涂到湿式试验板的50×70mm部分的一面上，涂敷量为0.5克(膜厚150μm)。这块板于150℃下加热24小时以测定产生的蒸发损失(Wt％)
                   表7
                             实施例1       2      3针入度25℃             336     333    298用过的60冲程极压条件下的润滑性最大非胶住载荷         126     100    126烧结载荷               315     400    315载荷-磨损指数          59      56     57耐磨性能摩擦系数               0.080   0.092  0.085耐热性能薄膜蒸发损失           10.1    9.5    10.8
               表8
                        实施例
                       4       5      6
针入度25℃            317     289     28
用过的60冲程
极压条件下的润滑性
最大非胶住载荷        126     126     100
烧结载荷              400     315     315
载荷-磨损指数         62      60      53
耐磨性能
摩擦系数              0.082   0.083   0.077
耐热性能
薄膜蒸发损失          10.5    11.5    11.0
                表9
                        实施例
                       7       8        9
针入度25℃            317     297      307
用过的60冲程
极压条件下的润滑性
最大非胶住载荷        100     126      100
烧结载荷              315     315      315
载荷-磨损指数          53       59       53
    耐磨性能
    摩擦系数           0.094    0.097    0.086
    耐热性能
薄膜蒸发损失           14.5     10.4     11.6
                      表10
                              比较实施例
                         1      2      3       4
针入度25℃              282    311    289     296
用过的60冲程
极压条件下的润滑性
最大非胶住载荷          126    126    100     100
烧结载荷                315    315    315     250
载荷-磨损指数           60     63     60      43
耐磨性能
摩擦系数                0.112  0.119  0.125   0.099
耐热性能
薄膜蒸发损失            8.3    7.7    9.1     13.7
表11
                          比较实施例
                      5         6    7       8
针入度25℃           282      277    360    306
用过的60冲程
极压条件下的润滑性
最大非胶住载荷       63       80    80      80
烧结载荷             160      250   200     250
载荷-磨损指数        28       36    44      39
耐磨性能
摩擦系数             0.101    0.099 0.090   0.103
耐热性能
薄膜蒸发损失         14.2     16.6  13.5    13.2
                    表12
                             比较实施例
                        9       10      11
针入度25℃             265      277    270
用过的60冲程
极压条件下的润滑性
最大非胶住载荷          50      50      50
烧结载荷               315     250     250
载荷-磨损指数    41     32     37
耐磨性能
摩擦系数         0.130  0.142  0.144
耐热性能
薄膜蒸发损失    流走    流走   流走(评价)
对于所有载荷能力、耐磨性能和耐热性能，实施例1-9的润滑脂组合物都给出好的结果。
在另一方面，使用磷酸三钙做为增稠剂的比较实施例1-3的润滑脂显示出不良的耐磨性能。比较实施例4-8的脲润滑脂显示出不良的载荷能力和耐热性能。此外，比较实施例9-11的锂皂润滑脂显然在所有载荷能力、耐磨性能和耐热性能方面都是差的。
本发明的实施方案详叙如下：
(1).一种润滑脂组合物，其含有润滑脂、和加进润滑脂中作为添加剂的(A)和(B)，润滑脂包括基础油和含分子式为Ca3(Po4)2的磷酸三钙和脲化物的混合物的增稠剂，(A)是结构式为：的硫化二烷基二硫代氨基甲酸钼，在结构式中R1和R2各自为选自具有1-24个碳原子的烷基的基团；m是o或1-3的整数；n是1-4的整数，条件是m＋n＝4，(B)是结构式如下的磷硫代硫酸三苯酯，其中按组合物的总重量计，增稠剂、组分(A)和组分(B)的含量分别为2-35％(Wt)、0.5-10％(Wt)和0.1-10％(Wt)。
(2)上面(1)项中所介绍的润滑脂组合物，其中，在增稠剂中，磷酸三钙的比例是5-95％(Wt)，脲化合物的比例是95-5％(Wt)。
(3)上面(1)或(2)项中所介绍的润滑脂组合物，其有最大非胶住载荷等80kgf或80kgf以上，优选100kgf或100kgf以上，烧结负荷等250kgf或250kgf以上，负荷-磨损指数45或45以上，摩擦系数低于0.100，薄膜蒸发损失等15.0％(Wt)或15.0％(Wt)以下。
(4)上面(3)项中所介绍的润滑脂组合物，其有最大非胶住载荷等100kgf或100kgf以上，烧结负荷250kgf或250kgf以上，最好315kgf或315kgf以上，载荷-磨损指数为50或50以上，摩擦系数低于0.100，薄膜蒸发损失13.0％(Wt)或13.0％(Wt)以下。
本发明成功地提供了一种润滑脂组合物，该润滑脂组合物具有高水平的载荷能力、耐磨性能和耐热性能并且在这些性能中具有优良的平衡。
特别地，本发明的润滑脂组合物的优选的实施方案是有最大非胶住载荷为80kgf或80kgf以上，最好100kgf或100kgf以上，烧结载荷为250kgf或250kgf以上，优选315kgf或315kgf以上，载荷-靡损指数45或45以上，优选50或50以上，摩擦系数低于0.100，薄膜蒸发损失为15.0％(Wt)或15.0％以下，优选13.0％(Wt)或13.0％以下。从而，优选的实施方案表现出对于载荷能力、耐磨性能和耐热性能的高效果。
业已详细地并参考具体的实施方案介绍了本发明对于本领域的熟练技术人员来讲，可以做出各种变化和改进，而不违背本发明的精神和范围这是明显的。

Claims (4)

1.一种润滑脂组合物，它含有润滑脂、和作为添加剂加入该润滑脂中的(A)和(B)，润滑脂包括基础油和含分子式为Ca3(Po4)2的磷酸三钙和脲的混合物的增稠剂，(A)是结构式为：
Figure A9512184000021
的硫化二烷基二硫代氨基甲酸钼，结构式中R1和R2各自代表选自具有1-24个碳原子的烷基的基团；m是0或1-3的整数；n是1-4的整数，条件是m＋n＝4，(B)是结构式如下磷硫代硫酸三苯酯，
Figure A9512184000022
其中按组合物的总重量计，该增稠剂、组分(A)和组分(B)的含量分别为2-35％(Wt)、0.5-10％(Wt)和0.1-10％(Wt)。
2.根据权利要求1的润滑脂组合物，其中，在该增稠剂中，所述磷酸三钙的比例是5-95％(Wt)，所述脲化合物的比例是95-5％(Wt)。
3.根据权利要求1的润滑脂组合物，其中，按该组合物的总重量计，组分(A)的含量为0.5-5％(Wt)。
4.根据权利要求1的润滑脂组合物，其中，按该组合物的总重量计，组分(B)的含量为0.1-5％(Wt)。
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