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CN1302855A - 含有未转化羟基的多元醇酯组合物 - Google Patents

含有未转化羟基的多元醇酯组合物 Download PDF

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Publication number
CN1302855A
CN1302855A CN00108763A CN00108763A CN1302855A CN 1302855 A CN1302855 A CN 1302855A CN 00108763 A CN00108763 A CN 00108763A CN 00108763 A CN00108763 A CN 00108763A CN 1302855 A CN1302855 A CN 1302855A
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Prior art keywords
acid
branched
lubricant
synthetic ester
lubricant according
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CN1109736C (zh
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R·H·施洛斯伯格
H·S·奥德里齐
L·D·舍伍德-威廉姆斯
J·S·索伯塔
M·A·克里瓦里斯
D·P·利塔
D·G·L·霍尔特
F·H·戈登
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ExxonMobil Chemical Patents Inc
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Exxon Chemical Patents Inc
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Abstract

一种合成酯组合物,它有热和氧化稳定性、较低的摩擦系数和较低的磨损,其中酯组合物为通式R(OH)n的支链醇或直链醇和至少一种有约C5至C13范围碳数的支链一元羧酸的反应产物,其中R为有约2至20个碳原子的脂族或环脂族基团,n至少为2;其中按支链醇或直链醇中羟基的总量计,合成酯组合物有约5至35%未转化羟基。

Description

含有未转化羟基的多元醇酯组合物
本发明是1995年3月14日提交的美国专利申请书08/403366的部分接续申请书。
本发明一般涉及多元醇酯组合物，与传统的合成酯类相比，它们有更高的热/氧化稳定性、更低的摩擦系数和更低的磨损。更具体地说，本发明独特的多元醇酯在多元醇与支链酸的反应产物中有未转化的羟基，因此可使未转化的羟基用于此完全酯化的多元酯类大大推迟开始氧化降解作用。在一定数量的多元酯的基础上，本发明还使保持合格的热/氧化稳定性所需的抗氧化剂的用量减少或完全不用。
目前商业使用的润滑剂由各种天然的和合成的基础原料视其用途而定与各种添加剂配方和溶剂混合来制备。基础原料通常包括矿物油、深度精制矿物油、聚α烯烃(PAO)、聚亚烷基二醇(PAG)、磷酸酯、硅油、二酯和多元醇酯。
根据热和氧化规格要求，最需要的润滑剂应用场合是航空燃气轮机油。多元醇酯类常用在航空燃气轮机油中作基础原料。尽管与其他的基础原料(如矿物油、聚α烯烃等)相比，多元醇酯具有特有的热/氧化稳定剂，但是甚至这些合成酯润滑剂都要发生氧化降解；并且在未经进一步改性的条件下，不能长期用于氧化条件下。已知这种降解作用与酯类基础原料的氧化和水解有关。
传统的合成多元醇酯航空燃气轮机油配方需要添加抗氧化剂(也称氧化抑制剂)。抗氧化剂使酯类基础原料在使用中质量变差的倾向减小，这一质量变差可由生成氧化产物如淤渣和在金属表面上的似漆膜沉积物以及由粘度和酸度的增加得到证据。这样的抗氧化剂包括芳基胺(如二辛基苯基胺和苯基α萘基胺)等。
经常需要更换航空燃气轮机油或者为抑制氧化加入抗氧化剂，这样就使维护航空燃气轮机的总费用增加。最希望有这样一种酯类基础原 料，与传统的合成酯基础原料相比，它有高得多的热/氧化稳定性，其中酯类基础原料不需因分解(即氧化降解)而经常更换。在经济上，也希望不用或减少通常加到这样的润滑剂基础原料中的抗氧化剂的数量。
由于热氧化作用，弱的碳氢键断裂，在酯上生成不稳定的碳自由基。传统抗氧化剂的作用是将氢原子转移到不稳定的碳自由基上，并进行自由基“愈合”(healing)。以下反应方程式说明抗氧化剂(AH)的作用：
抗氧化剂分子转化成自由基，但这一自由基(A·)比含酯体系的自由基要稳定得多。因此，酯的有效寿命延长了。当加入的抗氧化剂消耗掉时，酯自由基不愈合，从而出现多元酯组合物的氧化降解。在本专业中大家熟悉的相对热/氧化稳定性的一种测量方法是使用高差压扫描量热法(HPDSC)。
HPDSC已用于评价调配汽车润滑油(见J．A.Walker,W.Tsang,SAE 801383)、合成润滑油(见M.Wakakura,T.Sato,Journal ofJapanese Petroleum Institute,24(6),pp.383-392(1981))和多元醇酯生产的润滑油(见A.Zeeman,Thermochim,Acta,80(1984)1)的热/氧化稳定性。在这些评价中，测量了主体油氧化的时间，它称为诱导时间。诱导时间越长表明相应油有更高的抗氧化剂浓度或有更有效的抗氧化剂，或者在固定的抗氧化剂含量下，表明相应油有固有地更稳定的基础原料。对汽车润滑剂来说，更高的诱导时间与减粘点时间有关。
如上所述，HPDSC的使用提供了一种通过氧化诱导时间测量稳定性的方法。多元醇酯可与固定数量的抗氧化剂二辛基二苯基胺调合。这一固定数量的抗氧化剂对多元醇酯基础原料提供了固定程度的保护，使它不受整体氧化。因此，以这一方式有更长诱导时间的试验油料有更大的固有抗氧化性。对于不加抗氧化剂的高羟基含量的酯类来说，诱导时间越长说明基础原料本身的稳定性越高，也说明由于游离羟基的存在，酯类固有的抗氧化性。
本发明人已开发了一种独特的多元醇酯组合物；当与传统的合成多元醇酯组合物相比，它有高的热/氧化稳定性。这可通过由多元醇与支链 酸或支链/直链酸的混合物以这样的方式合成多元醇酯组合物来实现，以致多元醇酯组合物有大量未转化的羟基。高度分支的多元醇酯主链骨架使这种高羟基含量的酯起类似抗氧化剂的作用，也就是使新型多元醇酯组合物的热/氧化稳定性显著提高，正如用高差压扫描量热法(HPDSC)测量的。也就是说，这一新型多元醇酯组合物提供一种分子内机理，它能清除烷氧化物自由基和烷基过氧化物自由基，从而显著降低氧化降解的速率。
本发明的新型多元醇酯组合物的热和氧化稳定性可不用或减少必需加到特定润滑剂中的抗氧化剂的含量，从而为润滑剂制造商大大节省了费用。
本发明人还发现，这些独特的高羟基含量的多元醇酯在曲轴箱发动机润滑剂应用场合中有良好摩擦和磨损效果。最后，本发明的新型高羟基含量的多元醇酯与没有酯添加剂或与完全酯化的合成酯相比可明显节约燃料。
本发明还提供许多另外的优点，正如以下描述的，这些优点将变得很明显。
一种有热和氧化稳定性的合成酯组合物，它含有以下组分的反应产物：有通式R(OH)n的支链醇或直链醇，其中R为有2-20个碳原子的脂族或环脂族基团和n至少为2；至少一种约C5至C13范围碳数的支链一元羧酸，其中按支链醇或直链醇中的羟基总量计，合成酯组合物有约5至35％未转化的羟基。
优选的是，对于所用的支链酸或支链/直链混合酸的数量来说，支链醇或直链醇过量10-35％(当量)。在支链醇或直链醇与酸酯化时，支链醇或直链醇约60至90％的羟基转化。生成的本发明的合成酯组合物在220℃、3.445兆帕空气和0.5％(重量)Vanlube81抗氧化剂(即二辛基二苯基胺)下用HPDSC测量的热/氧化稳定性大于50分钟、优选大于100分钟。
多元醇酯组合物含有至少一种以下的化合物：R(OOCR′)n、R(OOCR′)n-1OH、R(OOCR′)n-2(OH)2和R(OOCR′)n-i(OH)i，其中n为一个至少2的整数、R为含有约2至20或更多碳原子的脂族或 环脂族烃基，R′为任何一个有约C4至C12范围碳原数的支链脂族烃基，以及(ⅰ)为一个约0至n的整数。除非预先除去R(OH)n，多元醇酯组合物还可含有过量的R(OH)n。
任选的是，反应产物可含有至少一种直链酸；按支链一元羧酸的总量计，直链酸的数量为约1至80％(重量)。直链酸为任何一种约C2至C12范围碳数的饱和烷基羧酸。
这一新型的合成多元醇酯组合物与也由相同的支链醇或直链醇与支链一元羧酸生成的完全酯化的组合物相比，有约高20至200％或更高的热/氧化稳定性，如用HPDSC法测量的；按支链醇或直链醇中羟基的总量计，后者有小于10％未转化的羟基。本发明的完全酯化的合成多元醇酯组合物的羟基数通常有小于5。
任选的是，按合成多元醇酯组合物计，抗氧化剂的数量为约0至5％(质量)、更优选约0.01至2.5％(质量)。
本发明还包括这样一种润滑剂，它由至少一种有如上所述有未转化羟基的合成多元醇酯组合物和润滑剂添加剂配方制成。此外，也可将溶剂加到润滑剂中，其中润滑剂含有约60至99％(重量)合成多元醇酯组合物、约1至20％(重量)添加剂配方和约0至20％(重量)溶剂。
润滑剂优选选自曲轴箱发动机油、二冲程发动机油、弹射器油、液压液、钻井液、燃气轮机油、润滑脂、压缩机油和功能液。
添加剂配方含有至少一种选自以下的添加剂：粘度指数改进剂、腐蚀抑制剂、氧化抑制剂、分散剂、润滑油流动改进剂、清洁剂和防锈剂、倾点下降剂、消泡剂、耐磨剂、密封膨胀剂(seal swellant)、摩擦改进剂、极压添加剂、颜色稳定剂、破乳剂、润湿剂、漏水改进剂、杀菌剂、钻头润滑剂、稠化剂或胶凝剂、抗乳化剂、金属钝化剂和添加剂增溶剂。
根据本发明，可用这一独特的合成多元醇酯组合物和至少一种另外的基础原料调合制成，后者选自矿物油、深度精制的矿物油、聚α烯烃、聚亚烷基二醇、磷酸酯、硅油、二酯和多元醇酯。合成多元醇酯组合物与按调合的基础原料总量计约1至50％(重量)的另一基础原料调合、优选1-25％、最优选1-15％(重量)。
本发明还涉及一种制备合成酯组合物的方法，该法包括支链醇或直链醇与至少一种支链酸在有或没有酯化催化剂下，在约140至250℃、约30至760毫米汞柱(3.999-101.308千帕)下反应约0.1至12小时、优选2至8小时的步骤，其中按支链醇或直链醇中的羟基总量计，合成酯组合物有约5至35％未转化的羟基。任选的是，支链酸可用支链酸和直链酸的混合物代替。然后在接触步骤中，通产物与一种固体如氧化铝、沸石、活性炭、白土等接触来处理产物。
图1为各种有未转化羟基键联在上的多元醇酯的HPDSC结果与羟基数的关系图；
图2为HPDSC结果与聚α烯烃(PAO)调合的各种酯的百分数的关系图；
图3a和b为3,5,5-三甲基己酸制得的各种酯与摩擦系数的关系图；
图4为3,5,5-三甲基己酸制得的各种酯与磨损量的关系图；
图5为燃料节省百分数与各种酯的关系图；由程序Ⅵ筛选发动机的燃料效率试验得到；
图6为在加钼或不加钼的条件下，磨损量和末期摩擦系数与合成润滑剂调合的各种基础原料的关系图。
本发明的多元醇酯组合物优选通过多羟基化合物与至少一种支链酸反应来制备。在多元醇酯组合物中，对于所用的酸用量来说，多元醇优选过量约10至35％(当量)。调节进料多元醇的组成，以便得到所需的产物酯组成。
根据本发明，生成的高羟基含量的酯在使用或不使用传统的抗氧化剂如V-81的条件下通常都抗高温氧化。
酸优选为高度支链的酸，以致键联到生成的酯组合物上的未转化羟基起类似抗氧化剂的作用，它将氢原子转移到酯分子在热作用下生成的不稳定碳自由基上，从而使自由基“愈合”(即将碳自由基转化成稳定的醇和氧)。这些起内抗氧化剂作用的未转化羟基可显著减少，或在某些情况下不需将昂贵的抗氧化剂加入到多元醇酯组合物中。而且，与调合有类似数量抗氧化剂的酯相比，键联有未转化羟基的酯表明有高得多 的热/氧化稳定性。
有未转化羟基的多元醇酯与类似的完全酯化的多元醇酯相比，有更低的末期摩擦系数和磨损量，这一事实表明这些多元醇酯还可用作抗磨剂或摩擦改进剂。
另一方面，直链酸可按1∶99至80∶20的比例与支链酸混合，随后与支链醇或直链醇反应，如上所述的。但是，在所有支链酸的情况下使用的相同摩尔过量醇在混合酸的情况下也是需要的，以致按醇中羟基的总量计，通过醇与混合酸反应生成的合成酯组合物仍有约5至35％未转化的羟基。
酯化反应优选在以下条件下进行约0.1至12小时、优选2-8小时：使用或不使用催化剂、约140至250℃、约30至760毫米汞柱(3.999至101.308千帕)。反应器中的化学计量是随真空汽提过量酸的能力变化的，以便得到优选的最终组合物。
如果酯化反应在催化条件下进行，那么优选的酯化催化剂是钛、锆和锡催化剂，如钛、锆和锡的醇化物、羧酸盐和螯合物。有选择的酸催化剂也可用于这一酯化过程。参见US5324853(Jones等)，它于1994年6月28日颁发；以及US3056818(Werber)，它于1962年10月2日颁发，在这里它们作为参考并入。
作为例子，可与支链酸或支链酸与直链酸的混合物反应的醇是以下通式表示的多元醇(即多羟基化合物)：
R(OH)n式中，R为任何脂族或环脂族烃基(优选烷基)，n至少为2。烃基可含有约2至约20或更多的碳原子；烃基还可含有各种取代基，如氯、氮和/或氧原子。多羟基化合物通常可含有一个或多个氧亚烷基；因此，多羟基化合物包括如聚醚多醇这样的化合物。用于制备羧酸酯的多羟基化合物中所含的碳原子数(即碳数，其中在整个申请书中使用的术语“碳数”指在酸或醇中碳原子的总数，视情况而定)和羟基数可在很宽范围内变化。
以下的醇特别适用作多元醇：新戊二醇、2,2-二羟甲基丁烷、三羟甲基乙烷、三羟甲基丙烷、三羟甲基丁烷、单季戊四醇、工业级季 戊四醇、二-季戊四醇、三季戊四醇、乙二醇、丙二醇和聚亚烷基二醇(如聚乙二醇、聚丙二醇)、1,4-丁二醇、山梨醇等、2-甲基丙二醇、聚丁二醇等；及其掺合物，如乙二醇和丙二醇的聚合混合物。最优选的醇是工业级季戊四醇(如约88％单季戊四醇、10％二季戊四醇和1-2％三季戊四醇)、单季戊四醇、二季戊四醇、新戊二醇和二羟甲基丙烷。
支链酸优选为一元羧酸，其碳数在约C5至C13范围内、优选约C7至C10，其中甲基或乙基支链是优选的。一元羧酸优选为至少一种选自如下的酸：2,2-二甲基丙酸(新戊酸)、新庚酸、新辛酸、新壬酸、异己酸、新癸酸、2-乙基己酸(2EH)、3,5,5-三甲基己酸(TMH)、异庚酸、异辛酸、异壬酸和异癸酸。一种特别优选的支链酸是3,5,5-三甲基己酸。这里使用的术语“新”指三烷基乙酸，即在α碳位被烷基三取代的酸。这些烷基等于或大于甲基，如以下结构式所示：
Figure A0010876300121
式中，R1、R2和R3等于或大于甲基，但不为氢。3,5,5-三甲基己酸有以下结构式：
优选的一元和/或二元直链羧酸是任何一种直链饱和烷基羧酸，其碳数在约C2至C18范围内、优选C2-C10。
直链酸的一些例子包括乙酸、丙酸、戊酸、庚酸、辛酸、壬酸和癸酸。所选的多元酸包括任何一种C2-C12多元酸，如己二酸、壬二酸、癸二酸和十二碳二酸。
根据本发明，合成有大量未转化羟基的多元醇酯组合物的方法通常按以下反应方程式进行： ；    (Eq.1) 式中，n为至少2的整数，R为任何脂族或环脂族烃基，含有约2至约20个碳原子，并任选有取代基如氯、氮和/或氧，R′为任何有约C4至C12范围碳数的支链脂族烃基、更优选约C6至C9，其中甲基或乙基支链是优选的，(ⅰ)为约0至n的整数。
上述反应方程式1的反应产物其本身可用作润滑剂基础原料，或与其他基础原料混合作为润滑剂基础原料，其他基础原料如矿物油、深度精制矿物油、聚α烯烃(PAO)、聚亚烷基二醇(PAG)、磷酸酯、硅油、二酯和多元醇酯。当与其他基础原料混合时，本发明的部分酯组合物按调合基础原料总量计，其用量优选为约1至50％(重量)、更优选约1至约25％(重量)、最优选约1至15％(重量)。
本发明还涉及有高热/氧化稳定性的高羟基含量的复杂酯。复杂酸酯通过多元醇、一元羧酸和多元羧酸(如已二酸)反应制得。与典型的多元醇酯(即多元醇和一元羧酸)相比，由于生成二聚物、三聚物和其他低聚物，复杂酸酯有更高的粘度。正如多元醇酯的情况一样，复杂酸酯通常在多元醇部分有高转化率的方法中制备。用羟基数给出这一转化的量度。作为例子，在航空燃气轮机油中使用的多元醇酯通常的羟基数为约5毫克KOH/克或更低，表明有很高的转化率。本发明人现已发现，复杂酸酯的不完全或部分转化实际上可得到比有低羟基数的复杂酸酯有更高的热/氧化稳定性，正如用HPDSC法测量的。
复杂醇酯通过多元醇、C6-C13醇和一元羧酸或多元酸反应来制备。与典型的多元醇酯(即多元醇和一元羧酸)相比，复杂醇酯类似复杂酸酯，有更高的粘度。本发明人已发现，复杂醇酯的不完全或部分转化可得到比有低羟基数的复杂酸酯有更高的热/氧化稳定性，如用HPDSC法测量的。
本发明的多元醇酯组合物可用于各种润滑剂的配方，如曲轴箱发动机油(即客车发动机油、重载柴油发动机油和客车柴油发动机油)、二冲程发动机油、弹射器油、液压液、钻井液、航空和其他燃气轮机油、润滑脂、压缩机油、功能液和其他工业和发动机润滑应用场合。与本发明的多元醇酯组合物一起使用的润滑油包括有润滑粘度的矿物烃油和合 成烃油，以及与其他合成油的混合物。合成烃油包括长链烷烃，如十六烷；以及烯烃聚合物，如己烯、辛烯、癸烯和十二碳烯等的低聚物。其他合成油包括(1)没有游离羟基的完全酯化的酯油，如有2-20个碳原子的一元羧酸的季戊四醇酯、有2-20个碳原子的一元羧酸的三羟甲基丙烷酯；(2)聚缩醛；以及(3)硅氧烷液。其中特别适用的合成酯是由多元羧酸扣一元醇制得的。更优选的是由季戊四醇或其与二季戊四醇和三季戊四醇的混合物与含有1-20个碳原子的脂族一元羧酸或其混合物完全酯化制得的酯液。
在上述的某些润滑剂配方中，溶剂的使用与具体的应用有关。可使用的溶剂包括烃类溶剂，如甲苯、苯、二甲苯等。
本发明的配方润滑剂优选含有约60-99％(重量)至少一种本发明的多元醇酯组合物、约1至20％(重量)润滑剂添加剂配方和约0至20％(重量)溶剂。另外，基础原料可含有1-50％(重量)至少一种选自如下的另外的基础原料：矿物油、深度精制的矿物油、烷基化的矿物油、聚α烯烃、聚亚烷基二醇、磷酸酯、硅油、二酯和多元醇酯。
曲轴箱润滑油
多元醇酯组合物可用于点燃式发动机和压燃式发动机用曲轴箱润滑油配方(即客车发动机油、重载柴油发动机油和客车柴油)。下面所列添加剂通常按这样的数量使用，以便提供添加剂产生的正常功能。单个组分的典型用量也列入下表。所列的所有数值都为有效成分的质量百分数。
添加剂 ％(质量)(宽范围) ％(质量)(优选范围)
无灰分散剂 0.1-20 1-8
金属清净剂 0.1-15  0.2-9
腐蚀抑制剂 0-5 0-1.5
二烷基二硫代磷酸金属盐 0.1-6 0.1-4
补充抗氧化剂 0-5 0.01-1.5
倾点下降剂 0.01-5 0.01-1.5
抗泡剂 0-5 0.001-0.15
补充抗磨剂 0-0.5  0-0.2
摩擦改进剂 0-5 0-1.5
粘度改进剂 0.01-6 0-4
合成油基础原料和/或矿物油基础原料 其余部分 其余部分
单个添加剂可以任何适合的方法加到基础原料中。例如，可通过按所需的浓度将每一组分分散或溶解在基础原料中的方法将每一组分直接加到基础原料中。这样的调合步骤可在常温下或升温下进行。
优选的是，除粘度改进剂和倾点下降剂外，所有添加剂都可调合到在这里称为添加剂配方的浓缩的添加剂配方中，也就是随后调合到基础原料中，以制得成品润滑剂。这样的浓缩物的使用是方便的。浓缩物通常被配制成含有适当数量的各种添加剂，以便在当浓缩物与预定数量的基础原料混合时，最终的配方中有所需的浓度。
浓缩物优选按US4938880中公开的方法制备。该专利公开了在至少约100℃下预调合的无灰分散剂和金属清净剂制得预混合物。此后，将预混合物冷却到至少85℃，并加入其他组分。
最终的曲轴箱润滑油配方可使用2-20％(质量)、优选5-10％(质量)、更优选约7至8％(质量)浓缩物或添加剂配方，其余为基础原料。
无灰分散剂含油溶性聚合烃类主链，带有能与要分散的颗粒结合的官能基。通常，分散剂含有胺、醇、酰胺或酯极性部分，它们常通过桥联基连接到聚合物主链上。例如，无灰分散剂可选自长链烃取代的一元羧酸和二元羧酸或其酸酐的盐、酯、氨基酯、酰胺、亚胺和恶唑啉；长 链烃的硫代羧酸酯衍生物；有多胺直接连接在上的长链脂族烃；以及由长链取代的酚与甲醛缩合制得的曼尼期缩合产物和聚亚烷基多胺。
粘度改进剂(VM)起到使润滑油有高温和低温操作性的作用。所用的VM可有单功能作用，或可为多功能的。
还起分散剂作用的多官能粘度改进剂也是已知的。适用的粘度改进剂是聚异丁烯，乙烯、丙烯和更高碳α烯烃的共聚物，聚甲基丙烯酸酯，聚甲基丙烯酸烷基酯，甲基丙烯酸共聚物，不饱和二元羧酸和乙烯基化合物的共聚物苯乙烯和丙烯酸酯的共聚物，苯乙烯/异戊二烯、苯乙烯/丁二烯和异戊二烯/丁二烯的部分氢化共聚物，以及丁二烯和异戊二烯和异戊二烯/二乙烯基苯的部分氢化均聚物。
含金属的或成灰的清净剂起减少或除去沉积物的清净剂作用以及起酸中和剂或防锈剂作用，从而减少了磨损和腐蚀，延长了发动机的寿命。清净剂通常含有极性的头，带有长的疏水尾，极性头为酸性有机化合物的金属盐。盐可含有基本上化学计量的金属，通常称为正常盐或中性盐，通常其总碱数(TBN)为0-80，如ASTM D-2896测量的。可能含有由过量金属化合物如氧化物或氢氧化物与酸性气体如二氧化碳反应得到的大量金属盐。生成的高碱性清净剂含中和的清净剂作为金属碱(如碳酸盐)胶束的外层。这样的高碱性清净剂的TBN可为150或更大，通常为250-450或更大。
可使用的清净剂包括油溶性的中性和高碱性磺酸盐、酚盐、硫化的酚盐、硫代膦酸盐、水杨酸盐、环烷酸盐以及其他油溶性的金属羧酸盐，特别是碱金属或碱土金属盐，如钠、钾、锂、钙和镁盐。最常用的金属是钙和镁，它们可单独存在于用于润滑剂的清净剂中，或钙和/或镁与钠的混合物存在于用于润滑剂的清净剂中。特别适合的金属清净剂是TBN为20-450的中性和高碱性磺酸钙；TBN为50-450的中性和高碱性酚钙和硫化的酚钙。
二烃基二硫代磷酸金属盐常用作抗磨剂和抗氧化剂。金属可为碱金属或碱土金属，或铝、铅、锡、钼、锰、镍或铜。锌盐是最常用于润滑油的；按润滑油组合物的总重计，其用量为0.1-10、优选0.2-2％(重量)。它们可用已知的技术、按以下步骤制备：首先通过一种或多 种醇或酚与P2S5反应制成二烃基二硫代磷酸(DDPA)，然后用锌化合物中和制成DDPA。例如，二硫代磷酸可通过伯醇和仲醇的混合物反应制得。此外，可制备多重二硫代磷酸，其中一些烃基有完全仲烃基特性，而另一些烃基有完全伯烃基特性。为了制备锌盐，任何一种碱性或中性锌化合物都可使用，但通常最好使用氧化物、氢氧化物和碳酸盐。由于在中和反应中使用过量的碱性锌化合物，商业添加剂常常含有过量的锌。
氧化抑制剂或抗氧化剂降低基础原料在使用中质量变差的倾向，这一质量变差可由氧化产物如淤渣和在金属表面上的似漆膜的沉积物以及由粘度增加得到证据。这样的氧化抑制剂包括受阻酚类、优选有C5-C12烷基侧链的烷基酚硫代酯的碱土金属盐、壬基酚钙硫化物、无灰油溶性酚盐和硫化的酚盐、硫磷化的或硫化的烃类、磷酯、硫代氨基甲酸金属盐、油溶性铜化合物，如US4867890中公开的，以及含钼的化合物。
可含有摩擦改进剂，以提高燃料的经济性。油溶性烷氧基化的一胺和二胺是大家熟悉的，它们增加边界层的润滑性。胺类可原样使用或以与硼化合物(如氧化硼、卤化硼、偏硼酸盐、硼酸硼酸一烷基酯、二烷基酯或三烷基酯)的加成物或反应产物的形式使用。
其他摩擦改进剂也是已知的。其中有由羧酸和酸酐与烷醇反应制成的酯。其他传统的摩擦改进剂通常有共价键联到亲油的烃链上的极性端基(如羧基或羟基)。羧酸和酸酐与烷醇的酯在US4702850中公开。其他传统的摩擦改进剂的例子由M.BelZer在“Journal of Tribology”(1992),vol.114,pp.675-682和M.Belzer和S.Jahanmir在“Lubrication Science”(1988),vol.1,pp,3-26中描述。一个这样的例子是有机金属钼。
可使用选自非离子型聚氧亚烷基多元醇及其酯、聚氧亚烷基酚和阴离子型烷基磺酸的防锈剂。
可使用含铜和铅的腐蚀抑制剂，但通常本发明配方不需要它们。通常，这样的化合物是含有5-50个碳原子的硫杂二唑多硫化物、它们的衍生物及其聚合物。如US2719125、2719126和3087932中公开的1,3,4-硫杂二唑的衍生物是代表性的。其他类似的材料在US 3821236、 3904537、4097387、4107059、4136043、4188299和4193882中公开。另外的添加剂是硫杂二唑的硫代和多硫代次磺酰胺，如英国专利说明书No.1560830中公开的。苯并三唑衍生物也在这类添加剂的范围内。当这些化合物含在润滑组合物中时，它们的数量优选不超过0.2％(重量)活性成分。
可使用少量破乳组分。优选的破乳组分在EP330522中公开。它通过氧化烯与双环氧化物与多元醇反应的加成物反应来制得。破乳剂的用量不应超过0.1％(质量)活性成分。宜为0.001-0.05％(质量)活性成分。
倾点下降剂，也称润滑油流动改进剂使流体流动或倾倒的最低温度下降。这样的添加剂是大家熟悉的。改进流体低温流动性的这些添加剂中代表性的是富马酸C8-C18二烷基酯/乙酸乙烯酯共聚物、聚甲基丙烯酸烷基酯等。
许多化合物可用来控制起泡，包括聚硅氧烷类型的消泡剂，如硅油或聚二甲基硅氧烷。
上述添加剂中有一些可有多重效果，例如一种添加剂可作为分散剂-氧化抑制剂。这方面是大家熟悉的，不需进一步详述。
二冲程发动机油
多元醇酯组合物可与所选的润滑剂添加剂一起用于二冲程发动机油的配方。优选的二冲程发动机油通常用本发明制得的多元醇酯组合物与任何传统的二冲程发动机油添加剂配方一起配制。下列添加剂通常以这样的数量使用，以致提供添加剂产生的正常功能。添加剂配方可包括但不限于粘度指数改进剂、腐蚀抑制剂、氧化抑制剂、偶合剂、分散剂、极压添加剂、颜色稳定剂、表面活性剂、稀释剂、清净剂和防锈剂、倾点下降剂、抗泡剂和抗磨剂。
本发明的二冲程发动机油通常可使用约75至85％基础原料、约1至5％溶剂，其余为添加剂配方。
用于润滑剂的上述添加剂的例子在以下文献中描述，在这里它们作为参考并入：US4663063(Davis),1987年5月5日颁发；US5330667(Tiffany,Ⅲ等)，1994年7月19日颁发；US4740321(Davis等)， 1988年4月26日颁发；US5321172(Alexander等)，1994年6月14日颁发；US5049291(Miyaji等)，1991年9月17日颁发。
弹射器油
弹射器是用于在海上将飞机乘客弹射出飞机的装置。多元醇酯组合物可与所选的润滑剂添加剂一起用于弹射器油配方。优选的弹射器油通常用本发明制得的多元醇酯组合物与任何传统的弹射器油添加剂配方一起来配制。下列添加剂通常按这样的数量使用，以致提供添加剂产生的正常功能。添加剂配方可包括但不限于粘度指数改进剂、腐蚀抑制剂、氧化抑制剂、极压添加剂、颜色稳定剂、清净剂和防锈剂、抗泡剂、抗磨剂和摩擦改进剂。这些添加剂在以下文献中描述：Klamann，“润滑剂及相关产品”，Verlag Chemie,Deerfield Beach,FL,1984，在这里作为参考并入。
本发明的弹射器油通常可使用约90至99％基础原料，其余为添加剂配方。
液压液
多元醇酯组合物可与所选的添加剂配方一起用于液压液配方。优选的液压液通常用本发明制得的多元醇酯组合物与任何传统的液压液添加剂配方一起来配制。下列添加剂通常按这样的数量使用，以致提供添加剂产生的正常功能。添加剂配方可包括但不限于粘度指数改进剂、腐蚀抑制剂、边界润滑剂、破乳剂、倾点下降剂和抗泡剂。
本发明的液压液通常可使用约90至99％基础原料，其余为添加剂配方。
其他添加剂在1988年11月8日颁发给Jokinen等的US4783274中公开，在这里作为参考并入。
钻井液
多元醇酯组合物可与所选的润滑剂添加剂一起用于钻井液配方。优选的钻井液通常用本发明制得的多元醇酯组合物与任何传统的钻井液添加剂配方一起来配制。下列添加剂通常按这样的数量使用，以致提供添加剂产生的正常功能。添加剂配方可包括但不限于粘度指数改进剂、腐蚀抑制剂、润湿剂、漏水改进剂、杀菌剂和钻头润滑剂。
本发明的钻井液通常可使用约60至90％基础原料和约5至25％溶剂，其余为添加剂配方。参见1983年5月3日颁发给Walker等的US4382002，在这里作为参考并入。
适合的烃类溶剂包括：矿物油、特别是那里沸程为200-400℃、有良好氧化稳定性的石蜡基油，如Exxon Chemical Americas,Houston,Texas销售的Mentor 28；柴油和瓦斯油；以及芳族重石脑油。
燃气轮机油
多元醇酯组合物可与所选的润滑剂添加剂一起用于燃气轮机油的配方。优选的燃气轮机油通常用本发明制得的多元醇酯组合物与任何传统的燃气轮机油添加剂配方一起来配制。下列的添加剂通常按这样的数量使用，以致提供添加剂产生的正常功能。添加剂配方可包括但不限于粘度指数改进剂、腐蚀抑制剂、氧化抑制剂、稠化剂、分散剂、破乳剂、颜色稳定剂、清净剂和防锈剂和倾点下降剂。
本发明的燃气轮机油通常使用约65至75％基础原料和约5至30％溶剂，其余为添加剂配方；按组合物的总重计，通常为约0.01至约5.0％(重量)。
润滑脂
多元醇酯组合物可与所选的润滑剂添加剂一起用于润滑脂配方。润滑脂中的主要成分是稠化剂或胶凝剂，润滑脂配方中的差别常常涉及这一成分。除稠化剂或胶凝剂外，特定的润滑基础原料和可使用的各种添加剂也可影响润滑脂的其他性质和特性。
优选的润滑脂通常用本发明制得的多元醇酯组合物与任何传统的润滑脂添加剂配方一起来配制。下列添加剂通常按这样的数量使用，以致提供添加剂产生的正常功能。添加剂配方可包括但不限于粘度的指数改进剂、氧化抑制剂、极压添加剂、清净剂和防锈剂、倾点下降剂、金属钝化剂、抗磨剂和稠化剂或胶凝剂。
本发明的润滑脂通常可使用约80至95％基础原料和约5至20％稠化剂或胶凝剂，其余为添加剂配方。
用于润滑脂配方的典型稠化剂包括碱金属皂类、白土、聚合物、石棉、炭黑、硅胶、聚脲和铝络合物。皂稠化的润滑脂是最通用的，锂皂 和钙皂是最常用的。简单皂润滑脂由长链脂肪酸的碱金属盐与12-羟基硬脂酸锂制得，主要的由12-羟基硬脂酸、氢氧化锂-水化物和矿物油制得。复杂皂润滑脂也常使用，含有有机酸混合物的金属盐。目前正在使用的一种典型的复杂皂润滑脂是由12-羟基硬脂酸、氢氧化锂-水化物、壬二酸和矿物油制得的复杂锂皂润滑脂。锂皂在许多专利中公开和举例，其中包括US3758407(Harting),1973年9月11日颁发；US3791973(Gilani),1974年2月12日颁发；和US3929651(Murray),1975年12月30日颁发；所有的专利与1983年7月12日颁发给Alexander的US4392967一起在这里作为参考并入。
用于润滑脂的添加剂的说明可在以下文献中找到：Boner，“现代润滑脂”，1976年，第5章，它以及在其他产品中上面所列的添加剂在这里作为参考并入。
压缩机油
多元醇酯组合物可与所选的润滑剂添加剂一起用于压缩机油的配方。优选的压缩机油通常用本发明制得的多元醇酯组合物与任何传统的压缩机油添加剂配方一起来配制。下列的添加剂通常按这样的数量使用，以致提供添加剂产生的正常功能。添加剂配方可包括但不限于氧化抑制剂、添加剂增溶剂、防锈剂/金属钝化剂、破乳剂和抗磨剂。
本发明的压缩机油通常可使用约80至99％基础原料和约1至15％溶剂，其余为添加剂配方。
压缩机油添加剂也在US5156759(Culpon,Jr.)中公开，它于1992年10月20日颁发，在这里作为参考并入。
在许多润滑剂应用场合中，如在航空燃气轮机油中，得到热/氧化稳定的润滑剂产品是极重要的。测量润滑剂相对热/氧化稳定性的一种方法是高差压扫描量热法(HPDSC)。在这一试验中，将样品加热到一固定的温度，并保持在空气(或氧气)压力下，测量分解开始的时间。分解时间越长，样品越稳定。在下文所述的所有情况下，除非具体说明，条件如下：220℃、3.445兆帕(500磅/寸2)空气(即0.689兆帕(100磅/寸2)氧和2.756兆帕(400磅/寸2)氮)，加入0.5％(重量)二辛基二苯基胺(Vanlube-81)作为抗氧化剂。
本发明的有未转化羟基的独特多元醇酯还表明有高极性，本发明人发现，在曲轴箱发动机中这一点在减少摩擦和磨损中是很重要的。
本发明有未转化羟基的新型多元醇酯与没有酯添加剂或有完全酯化的合成酯相比，还有显著的燃料节省。对于5W40油来说，节省燃料百分数通常为约2至2.5％，如用程序Ⅵ筛选机试验测定的。节省燃料百分数随试验油的粘度变化。
实施例1
为了比较，下表1说明在碳链上没有未转化羟基的多元醇酯组合物比传统的非多元醇酯有高的热/氧化性能。
表1
    样品号     酯     HPDSC分解时间，分
    12345678     TMP/C7/C9/TMHTMP/C7/C810己二酸二异庚酯己二酸二异辛酯己二酸二异癸酯己二酸二(十三烷基)酯邻苯二甲酸二异辛酯邻苯二甲酸二(十三烷基)酯     23.923.411.69.76.03.98.010.2
TMP为三羟甲基丙烷。
C7为直链C7酸。
C9为直链C9酸。
TMH为3,5,5-三甲基己酸
C810为3-5％(摩尔)n-C6酸、48-58％(摩尔)n-C8酸、36-42％(摩尔)n-C10酸和0.5-1.0％(摩尔)n-C12酸的混合物。
下表2中所列数据表明，多元醇酯的热/氧化性能存在相当大的改进余地，如HPDSC试验测量的。特别是，应当指出，3,5,5-三甲基己酸和2,2-二甲基丙酸(即新戊酸(neoC5))的酯在HPDSC试验中是特别稳定的。
表2
  样品号     酯 HPDSC分解时间，分
    910111213141516     TMP/n-C9Tech PE/n-C9TMP/TMHTech PE/TMHMPE/TMHTMP/n-C550％TMP/TMH和50％TMP/n-C5MPE/TMH/neo-C5     14.214.711914814351.965.7168
n-C9为直链C9酸
Tech PE为工业级季戊四醇(即88％单季戊四醇、10％二季戊四醇和1-2％三季戊四醇)。
MPE为单季戊四醇。
n-C5为直链C5酸。
TMH为3,5,5-三甲基己酸。
neo-C5为2,2-二甲基丙酸。
酯上有未转化羟基的多元醇酯用工业级季戊四醇和3,5,5-三甲基己酸(样品18)通过每摩尔工业级季戊四醇与约225％(摩尔当量)3,5,5-三甲基己酸混合来制备。在下表3中与用过量的3,5,5-三甲基己酸由工业级季戊四醇与3,5,5-三甲基己酸制得的传统多元醇酯(样品17)进行了比较。
表3
  样品号     酯 HPDSC分解时间，分
    1718     Tech PE/TMHTech PE/TMH重/25％未转化羟基     148468
Tech PE为工业级季戊四醇(即88％单季戊四醇、10％二季戊四醇和1-2％三季戊四醇)。
TMH为3,5,5-三甲基己酸。
上表1-3中所列数据支持本发明人的发现：含有至少5％(摩尔) 未转化羟基的多元醇酯的组合物与传统的多元醇酯和非多元醇酯相比，有令人吃惊地高热/氧化稳定性，如用HPDSC测量的。
实施例2
当与三羟甲基丙烷和直链酸(7810)制得的多元醇酯相比时，某些含有至少5％(摩尔)未转化羟基的多元醇酯在HPDSC试验中，其热/氧化性质有显著地提高。这些酯含有特定类型分支，对于三羟甲基丙烷(TMP)和季戊四醇(单季戊四醇级和工业级)酯都观测到提高。下表4汇集了本发明人得到的结果。
    表4
  样品号     酯   羟基数   HPDSC分解时间，分
    123456789101112131415   TMP/2EHTMP/2EHTMP/2EHMPE/2EHMPE/2EHTechPE/2EHTechPE/TMHTechPE/TMHTechPE/TMHTechPE/TMHTMP/7810TMP/7810TMP/7810TMP/7810TMP/7810     2064.075.012.163.83.6＜108668.5＞500.225.726.843.573.8     30.1225.3125.324.4183.517.514826836446826.121.322.921.326.5
羟基数用传统的近红外技术以毫克KOH/克样品为单位测量。
2EH为2-乙基己酸。
TechPE为工业级季戊四醇(即88％单季戊四醇、10％二季戊四醇和1-2％三季戊四醇)。
MPE为单季戊四醇。
TMH为3,5,5-三甲基己酸。
TMP为三羟甲基丙烷。
7810为37％(摩尔)n-C7酸与63％(摩尔)下列酸的混合物：3-5％(摩尔)n-C9酸、48-58％(摩尔)n-C8酸、36-42％(摩尔)n-C10酸和0.5-1.0％(摩尔)n-C12酸。
上表4所列结果和图1说明，当最初加入的所有抗氧化剂(Vanlube-81)被消耗掉时，酯自由基不愈合，迅速出现分解，如在含有少量未转化羟基的样品1、4和6中表明的以及在直链酸制成的多元醇酯中表明的，不管未转化羟基存在的数量如何(见样品号11-15)。就某些支链酯如样品号2、3和6-10来说，未转化羟基(即与完全酯仅分子变化)能将其氢转移到首先形成的自由基上，以致得到更稳定的自由基，从而成为另一抗氧化剂。就上述样品号11-15所列的直链酸酯来说，未转化羟基的氢转移形成内自由基比最初形成的自由基稳定不了多少，从而使分解时间没有明显变化。上表4的结果图示于附图1。
实施例3
下表5中所列的结果说明，根据本发明，由多元醇和支链酸制得的含未转化羟基的多元醇酯组合物有内在抗氧化剂性能。
           表5
  样品号     酯   羟基数 HPDSC分解时间，分
    12345     TechPE/TMHTechPE/TMHTechPE/L9TechPE/TMHTechPE/TMH     大于50大于50小于5小于5小于5  468，含有0.5％V-8158.3，不含有no V-8116.9，含有0.5％V-81148，含有0.5％V-813.14，不含有V-81
V-81为二辛基二苯基胺
TechPE为工业级季戊四醇(即88％单季戊四醇、10％二季戊四醇和1-2％三季戊四醇)。
TMH为3,5,5-三甲基己酸。
L9为62-70％(摩尔)直链C9酸和30-38％(摩尔)支链C9 酸的混合物。
上表5的结果说明，含有未转化羟基的多元醇酯(即样品号1和2)与没有任何显著数量游离的或未转化的羟基的传统多元醇酯相比，大大延长润滑剂配方的氧化诱导时间。而且，这些独特的多元醇酯与抗氧化剂如V-81组合可显著延长分解所需的时间(见样品号1)。虽然当这一多元醇酯不含任何另加的抗氧化剂时分解时间有所缩短，但与有抗氧化剂的传统C9酸多元醇酯相比，分解所需的时间仍长约3.5倍(即58.3分(样品号2)与16.9分(样品3))。此外，样品4和5说明，与羟基数大于50由相同酸和多元醇得到的多元醇酯组合物相比(如样品1和2)，不管是否有抗氧化剂与相应的多元醇酯组合物混合，羟基数小于5的多元醇酯组合物的分解出现都早得多。这一点清楚地说明，合成碳链上有未转化羟基的多元醇酯组合物使生成的产物有高的热/氧化稳定性，如用HPDSC测量的。最后，样品2和5的比较(其中不使用抗氧化剂)清楚地确定由工业级季戊四醇和3,5,5-三甲基己酸制备的有大量未转化羟基键联在上的多元醇酯(HPDSC为58.3分)与有很少或没有未转化羟基的相同多元醇酯(HPDSC为3.14分)相比有抗氧化剂性能。
实施例4
下表6的数据说明，本发明由多元醇和支链酸制得的含有未转化羟基的多元醇酯当与其他烃类基础原料如聚α烯烃(PAO)调合时，也能提高热/氧化稳定性。
表6
样品号     基础原料组成 羟基数* HPDSC分解时间，分钟**
    123456789101112  PAO695％PAO6和5％TMP/781090％PAO6和10％TMP/781075％PAO6和25％TMP/781095％PAO6和5％TechPE/TMH90％PAO6和10％TechPE/TMH75％PAO6和25％TechPE/TMH95％PAO6和5％MPE/2EH90％PAO6和10％MPE/2EH95％PAO6和5％MPE/TMH90％PAO6和10％MPE/TMH75％PAO6和25％MPE/TMH ＜5＜5＜5＜5＜5＜563.863.868.568.568.5     10.6512.9913.4918.3012.8913.5217.0318.1928.7522.5753.68108.86
PAO6为1-癸烯低聚物。
*羟基数以毫克KOH/克样品为单位测量，为调合油含酯部分的羟基数。
**表示HPDSC测量在190℃和3.445兆帕下、在0.5％Vanlube-81添加剂(即二辛基二苯基胺)存在下进行。
2EH为2-乙基己酸。
TechPE为工业级季戊四醇(即88％单季戊四醇、10％二季戊四醇和1-2％三季戊四醇)。
MPE为单季戊四醇。
TMH为3,5,5-三甲基己酸。
TMP为三羟甲基丙烷。
7810为37％(摩尔)n-C7酸和63％(摩尔)下列混合物的混合物：3-5％(摩尔)n-C6酸、48-58％(摩尔)n-C8酸、36-42％(摩尔)n-C10酸和0.5-1.0％(摩尔)n-C12酸。
上表6中所列结果和图2说明，含有至少10％未转化羟基的多元醇酯组合物(即样品数8-12)当与烃类基础原料如聚α烯烃调合时，使热/氧化稳定性提高，如用HPDSC法测量的。
实施例5
下表7所列的数据说明，本发明由多元醇和支链酸制得的含有未转化羟基的多元醇酯与0.5％Vanlube81(一种抗氧化剂)混合能推迟热/氧化降解开始的时间，如HPDSC法测量的。以下样品在3.445兆帕(500磅/寸2)空气(即0.689兆帕(100磅/寸2)氧和2.756兆帕(400磅/寸2)氮)测量。
表7
样品   烃类     酯 比值 温度(℃) 羟基数 HPDSC(分)
    123456  SN150SN150SN150SN150SN150SN150  MPE/2EHMPE/2EHMPE/2EHMPE/TMHMPE/TMHMPE/TMH  95/590/1075/2595/590/1075/25     190190190190190190   63.563.563.568.568.568.5     14.5322.4131.9416.9817.5857.18
SN150为有14-34个碳原子的低硫、中性、饱和、直链烃。
TMH为3,5,5-三甲基己酸
2EH为2-乙基己酸。
MPE为单季戊四醇。
实施例6
都由3,5,5-三甲基己酸(Cekanoic 9酸)制得的以下酯有高的性能。例如，与其他完全酯化的合成酯相比，有大量未转化羟基的单羟基季戊四醇有最低的摩擦(即0.115)和磨损量(即1.35)。各配方在100℃、220磅负荷、速度420转/分(0.77米/秒)下，在法列克司环块摩擦试验机中试验2小时。摩擦系数为试验末期值。试验末期值有大约1.5％的相对标准偏差(1σ)。试验后，用多重扫描表面光度仪测定磨损量。对于Superflo QC样，相对标准偏差(1σ)约为12％。结果列入下表8和附图3a和3b。
表8
酯 末期摩擦   磨损量
二酯磷酸酯偏苯三酸酯工业级季戊四醇酯三羟甲基丙烷酯工业级季戊四醇酯W/未转化羟基   0.12450.11950.11750.11800.11800.1150     2.352.002.652.102.751.35
实施例7
几种不同的高羟基数的酯和非酯在基本上为缩短的程序Ⅵ筛选机试验的程序Ⅵ筛选机试验中，在完全配方中10％含量下被试验，与含非酯的配方和与类似的低羟基数酯配方相比，表明有优良的燃料经济性能。
         表9
酯 燃料节省率，％
无＊TMP/CK9C12/二酯TMP/C810KJ-106TMP/CK9(OH)**TMP/C810(OH)**     0.801.041.151.211.232.312.42
TMP表示三羟甲基丙烷
CK9为三-3,5,5-三甲基己酸。
C810为3-5％(摩尔)n-C6酸、48-58％(摩尔)n-C8酸、36-42％(摩尔)n-C10酸和0.5-1.0％(摩尔)n-C12酸的混合物。
KJ-106为Ketjenlube 106，为由1-癸烯、顺酐和丁醇制得的低聚物。
*表示聚α烯烃。
**表示由TMP和CK9制得的部分酯，其中25％羟基未转化。
***表示由TMP和C810制得的部分酯，其中25％羟基未转化。
正如上表9说明的，本发明有未转化羟基的合成酯比许多传统的完全酯化的酯基础原料和聚α烯烃有意想不到地大得多的燃料节省。
实施例8
在法列克司环块摩擦试验机中，加入10％(重量)本发明的高羟基含量的酯，即有约25％未转化的羟基的三羟甲基丙烷和C810的酯，与含非酯的配方或与加入其他低羟基含量的酯(即5或更少)相比，在摩擦性能和磨损性能方面有很大的好处。
少数油用Ultron DI(清净抑制剂)添加剂配方以及8％Shellvis 251配方在S150N(即有14-34个碳原子的一种低硫、中性、饱和、直链烃)中。配方用不同“极性”的酯得到：己二酸二异十三烷基酯、辛酸/癸酸三羟甲基丙烷酯和TMP8/10 (OH)(即一种含有三羟甲基丙烷和C810酸的高羟基含量的酯，每一分子TMP8/10留约1个未转化羟基)，含有或不含100ppm钼(如MV82，一种商业MoDTC)。此外，10％“top-treats”S150N和TMP8/10(OH)高羟基含量的酯在1995 10W-30 SuperFlo中试验。下表10示出以下各表使用的配方：
表10
样品 配方
 S150N-Euro包装 S150N+8％Shellvis 251+Ultron DI
 Euro+己二酸二(异十三烷基)酯 S150N+8％Shellvis 251+ULTRONDI+10％己二酸二(异三十烷基)酯
 Euro+辛酸/癸酸三羟甲基丙烷酯 S150N+8％Shellvis 251+ULTRONDI+10％辛酸/癸酸三羟甲基丙烷酯
 Euro+TMP8/10(OH) S150N+8％Shellvis 251+ULTRONDI+10％TMP8/10(OH)
 S150N-Ultron(M) S150N+8％Shellvis 251+ULTRONDI(M)
 Euro+己二酯二(异十三烷基)酯(M) S150N+8％Shellvis 251+ULTRONDI(M)+己二酯二(异十三烷基)酯
 Euro+辛酯/癸酸三羟甲基丙烷酯(M) S150N+8％Shellvis 251+ULTRONDI(M)+10％辛酯/癸酸三羟甲基丙烷基
 Euro+TMP8/10(OH)(M) S150N+8％Shellvis 251+ULTRONDI(M)+10％TMP8/10(OH)
 SF(95) 商业1995 10W30 SuperFlo
 SF+S150N  SF10W30(95)+10％S150N
 SF+TMP8/10(OH) SF10W30+10％TMP8/10(OH)
(M)表示100ppm钼以MoDTC(二硫代氨基甲酸钼)存在。
上述配方在100℃、220磅(99.8公斤)负荷、420转/分(0.77米/秒)下，在法列克司环块摩擦试验机中试验2小时。摩擦系数为试验末期值。试验末期值表示约1.5％的相对标准偏差(1σ)。试验后，用多重扫描表面光度仪测定磨损量。对于SuperFlo QC样品来说，相对标准偏差(1σ)为约12％。结果列入下表11和附图6。
表11
样品号 磨损量 末期摩擦系数
S150N-Euro包装Euro+己二酸二(异十三烷基)酯Euro+辛酸/癸酸三羟甲基丙烷酯Euro+TMP8/10(OH)S150N-Ultron(M)Euro+己二酸二(异十三烷基)酯(M)Euro+辛酸/癸酸三羟甲基丙烷酯(M)Euro+TMP8/10(OH)(M)SF(95)SF+S150NSF+TMP8/10(OH) 4.413.392.570.812.681.931.831.173.533.512.42 0.1270.1230.1150.1030.0980.0900.1020.1040.1330.1180.118
S150N为有14-34个碳原子的低硫、中性、饱和、直链烃。
C810为3-5％(摩尔)n-C6酸、48-58％(摩尔)n-C8酸、36-42％(摩尔)n-C10酸和0.5-1.0％(摩尔)n-C12酸的混合物。
TMP8/10表示由三羟甲基丙烷和C810酸制得的酯，其中生成的酯有25％未转化羟基。
上述Euro-TMP8/10(OH)样与没有10％本发明高羟基含量的酯组分的其他润滑剂配方相比，在磨损量和末期摩擦系数方面有明显的好处。甚至在钼存在下，与有钼的基础原料相比，高羟基含量的酯有明显的抗磨好处。
实施例9
为了测定1％浓度的高羟基数的酯加到配制的矿物油中是否有好处，在法列克司环块摩擦试验机中试验了两种油。基准方案油称为SETI(即小发动机试验设备)标准油，是一种全配方的矿物基础油，有大约0.06％的磷含量(如ZDDP)。将1％(重量)本发明的TMP/C810(OH)。涡流距离传感器用于测量每一油在12个条件的磨损速率，同时也测定了摩擦系数。下表12所列的结果说明仅加入1％高羟基数的酯可在磨损性能和摩擦性能方面有改进。磨损测量的准确性为±0.2微米/ 小时，在某些很慢的磨损的情况下可能出现负磨损速率。
表12
    条件     SETI标准油   SETI标准油+1％C8/C10 TMP-OH
  油温℃   速度(转/分)   负荷(磅) 磨损速率(微米/小时)   摩擦系数   磨损速率(微米/小时)   摩擦系数
    60   105     110     0.03   0.122     -0.18    0.122
    60   105     220     0.15   0.140     -0.12   0.130
    60   420     110     0.14   0.097     0.11   0.095
    60   420     220     1.86   0.137     0.32   0.120
    100   105     110     0.08   0.138     -0.14   0.120
    100   105     220     0.41   0.141     -0.01    0.123
    100   420     110     0.62   0.132     0.09   0.107
    100   420     220     2.01   0.136     0.20   0.116
    140   105     110     0.33   0.137     0.02   0.115
    140     105     220     0.38   0.137     -0.15   0.115
    140   420     110     1.33   0.131     0.18   0.113
    140   420     220     2.54   0.132     0.68   0.111
实施例10
制备以下复杂酸酯，其中将羟基数调节到完全酯和部分酯之间。由下表13所列的数据可以看出，较低的转化率，即羟基数大于10毫克KOH/克得到更高的热/氧化稳定性，如用HPDSC法测定的。
表13
复杂酸酯 羟基数(毫克KOH/克)   HPDSC(分)
TMP+己二酸+Ck9TMP+己二酸+Ck9TMP+己二酸+Ck9TPE+己二酸+Ck9TPE+己二酸+Ck9TPE+己二酸+Ck9     4.7743.5065.206.5827.2861.52     29.3061.0775.5335.9679.49105.97
TMP为三羟甲基丙烷。
TPE为工业级季戊四醇。
Ck9为3,5,5-三甲基己酸。
虽然我们已说明和公开了本发明几个实施方案，但应清楚地理解，对熟悉本专业的技术人员是明显的许多变化同样是敏感的。所以，我们不希望限制到所说明和公开的细节中，而希望在附后的权利要求书的范围内说明所有的变化和改进。

Claims (30)

1．一种由以下组分制备的润滑剂：
至少一种有热和氧化稳定性的合成酯组合物和一种润滑剂添加剂配方，前者含有通式R(OH)n的支链醇或直链醇和至少一种有约C5至C13范围碳数的支链一元羧酸的反应产物，其中R为有约2至20个碳原子的脂族或环脂族基团，n至少为2，其中按所述的支链醇或直链醇中的羟基总量计，所述的合成酯组合物有约5至35％未转化的羟基。
2．根据权利要求1的合成酯组合物，其中当所述的支链醇或直链醇与所述的支链一元羧酸酯化时，所述支链醇或直链醇中约50至90％羟基被转化。
3．根据权利要求1的润滑剂，其中所述的酯组合物含有至少一种以下化合物：R(OOCR’)n、R(OOCR’)n-1(OH)、R(OOCR’)n-2(OH)2、R(OOCR’)n-i(OH)i；其中n为至少2的整数，R为含有约2至约20或更多碳原子的任何脂族或环脂族烃基，R’为有约C4至C12范围碳数的任何支链脂族烃基，(ⅰ)为约0至n的一个整数。
4．根据权利要求3的润滑剂，其中所述的反应产物还含有至少一种直链酸，按所述的支链一元羧酸的总量计，所述的直链酸的数量为约1至80％(重量)。
5．根据权利要求4的润滑剂，其中所述的直链酸为有约C2至C12范围碳数的任何直链饱和烷基羧酸。
6．根据权利要求1的润滑剂，其中与按所述的支链醇或直链醇中羟基总量计，由所述的支链醇或直链醇与所述的支链一元羧酸制得的，含有小于10％未转化羟基的完全酯化的组合物相比，所述的合成酯组合物有高20至200％的热/氧化稳定性，如用高差压扫描量热法测量的。
7．根据权利要求1的润滑剂，其中所述的合成酯组合物的羟基数为至少20。
8．根据权利要求1的润滑剂，其中按所述的合成酯组合物计，还含有约0至5％(质量)抗氧化剂。
9．根据权利要求8的润滑剂，其中按所述的合成酯组合物计，所述的抗氧化剂的数量为约0.01至2.5％(质量)。
10．根据权利要求9的润滑剂，其中所述的抗氧化剂为芳基胺。
11．根据权利要求10的润滑剂，其中所述的芳基胺选自二辛基苯基胺、苯基α萘基胺和更重的低聚芳基胺。
12．根据权利要求1的润滑剂，其中所述的支链酸为有约C5至C10范围碳数的任何一元羧酸。
13．根据权利要求5的润滑剂，其中所述的直链酸为有约C2至C7范围碳数的任何直链饱和烷基羧酸。
14．根据权利要求1的润滑剂，其中所述的支链醇或直链醇选自：新戊二醇、2,2-二羟甲基丁烷、三羟甲基乙烷、三羟甲基丙烷、三羟甲基丁烷、单季戊四醇、工业级季戊四醇、二季戊四醇、三季戊四醇、乙二醇、丙二醇、聚亚烷基二醇、1,4-丁二醇、山梨醇、甘油和2-甲基丙二醇。
15．根据权利要求1的润滑剂，其中所述的支链酸为至少一种选自以下的酸：2,2-二甲基丙酸、新庚酸、新辛酸、新壬酸、异己酸、新癸酸、2-乙基己酸、3,5,5-三甲基己酸、异庚酸、异辛酸、异壬酸和异癸酸。
16．根据权利要求5的润滑剂，其中所述的直链酸为至少一种选自以下的酸：乙酸、丙酸、戊酸、庚酸、辛酸、壬酸和癸酸。
17．根据权利要求5的润滑剂，其中所述的直链酸为至少一种选自以下的酸：己二酸、壬二酸、癸二酸和十二碳二酸。
18．根据权利要求1的润滑剂，其中所述的润滑剂为所述的合成酯组合物和至少一种另外的选自以下的基础原料的调合物、矿物油、深度精制的矿物油、烷基化的矿物油、聚α烯烃、聚亚烷基二醇、磷酸酯、硅油、二酯和多元醇酯。
19．根据权利要求18的润滑剂，其中所述的合成酯组合物按调合基础原料的总量计，与约1至50％(重量)的所述的另外的基础原料 调合。
20．根据权利要求1的润滑剂，其中所述的添加剂配方含有至少一种选自以下的添加剂：粘度指数改进剂、腐蚀抑制剂、氧化抑制剂、分散剂、润滑油流动改进剂、清净剂和防锈剂、倾点下降剂、抗泡剂、抗磨剂、密封膨胀剂、摩擦改进剂、极压添加剂、颜色稳定剂、破乳剂、润湿剂、漏水改进剂、杀菌剂、钻头润滑剂、稠化剂或胶凝剂、抗乳化剂、金属钝化剂、偶联剂、表面活性剂和添加剂增溶剂。
21．根据权利要求1的润滑剂，其中还含有溶剂。
22．根据权利要求21的润滑剂，其中所述的润滑剂含有约60至99％(重量)所述的合成酯组合物、约1至20％(重量)所述的添加剂配方和约0至20％(重量)所述的溶剂。
23．根据权利要求1的润滑剂，其中所述的合成酯与矿物油或另外的合成酯调合。
24．根据权利要求1的润滑剂，其中所述的合成酯组合物还含有多元酸，从而生成复杂酸酯。
25．根据权利要求1的润滑剂，其中所述的合成酯组合物还含有第二醇，从而生成复杂醇酯。
26．根据权利要求1的润滑剂，其中所述的润滑剂选自二冲程发动机油配方、弹射器油配方、液压液配方、钻井液配方、燃气轮机油配方、润滑脂配方和压缩机油配方。
27．一种曲轴箱润滑油配方，它由至少一种有热和氧化稳定性的合成酯组合物和润滑剂添加剂配方制成，合成酯组合物含有通式R(OH)n的支链醇或直链醇和至少一种有约C5至C13范围碳数的支链一元羧酸的反应产物，其中R为有约2至20个碳原子的脂族或环脂族基团，n至少为2，其中按所述的支链醇或直链醇中羟基总量计，所述的合成酯组合物有约5至35％未转化羟基。
28．根据权利要求27的配方，其中所述的添加剂配方含有至少一种选自以下的添加剂：无灰分散剂、金属清净剂、腐蚀抑制剂、二烷基二硫代磷酸金属盐、抗氧化剂、倾点下降剂、抗泡剂、抗磨剂、摩 擦改进剂和粘度改进剂。
29．根据权利要求1的润滑剂，其中所述的合成酯与至少一种另外的基础原料调合，以致与不含所述合成酯的润滑剂相比，燃料相对节省约2％。
30．根据权利要求29的润滑剂，其中所述的合成酯以约5至25％(重量)的数量加到润滑剂中。
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