CN102971405B - 润滑脂组合物的制备方法 - Google Patents

润滑脂组合物的制备方法 Download PDF

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CN102971405B
CN102971405B CN201180033417.2A CN201180033417A CN102971405B CN 102971405 B CN102971405 B CN 102971405B CN 201180033417 A CN201180033417 A CN 201180033417A CN 102971405 B CN102971405 B CN 102971405B
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acid
water
slurries
grease composition
complexing agent
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CN102971405A (zh
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J-L·P·A·布罗索德
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Shell Internationale Research Maatschappij BV
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Shell Internationale Research Maatschappij BV
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  • Inorganic Chemistry (AREA)
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Abstract

一种用于制备金属络合润滑脂组合物的方法，包括如下步骤：(i)制备包含基础油、水、金属碱和络合剂的浆液，其中所述浆液中水∶固体的重量比为0.15∶1-1.5∶1；(ii)以至少为1,000,000s-1的剪切频率向所述浆液施加剪切；(iii)将来自步骤(ii)的浆液加入到C10-C24饱和或不饱和脂肪酸或其衍生物中实施皂化反应，所述皂化反应在至少80℃的温度下进行；(iv)从由步骤(iii)得到的皂化产物中除去水；(v)将来自步骤(iv)的产物加热到190-230℃；和(vi)将由来自步骤(v)的产物冷却到200-150℃以形成金属络合润滑脂组合物。本发明的方法减少了将水蒸发所需的放空时间，减少了总的批次生产时间，提供了更为能量有效的制备方法，和提高了产率。

Description

润滑脂组合物的制备方法
技术领域
本发明涉及润滑脂组合物的制备方法，和根据该方法生产的润滑脂组合物。
背景技术
润滑的主要目的是使相对移动的固体表面隔离，从而将摩擦和磨损降至最低。最常用于此目的的物质是油和脂。润滑剂的选择主要由特定应用来决定。
在存在高接触压力、不希望润滑剂从轴承泄漏或者当接触表面的运动不连续因而难以在轴承中保持分隔膜的场合使用润滑脂。由于设计简单、密封需求低和只需较少维护，在对电动机、家用电器、自动轮轴承、机器工具或飞行器配件中的滚珠轴承和滚柱轴承进行润滑时，几乎总是首先考虑润滑脂。润滑脂也用于对小型传动齿轮和许多低速滑动应用的润滑。
润滑脂主要由流体润滑剂例如油和增稠剂组成，通常还包括一种或多种性能添加剂。在配混润滑脂时，基本上使用与通常选择用于油润滑的同种类的油。锂、钙、钠、铝和钡的脂肪酸皂通常用作增稠剂。脂肪酸络合皂也公知用作润滑脂增稠剂。
尽管润滑脂组合物的制备工艺大多已知，但仍不断有改进的需求，目的是使产率达到最大和成本降到最低。特别地，批次生产时间减少使产率提高和成本降低。还有对提高润滑脂制备工艺能量效率的不断需求。
在制备润滑脂例如锂润滑脂时，需要与原料一起加入一定量的水，以促进皂化反应的效率。加入的水减小了反应器中的产品粘度，有助于混合，加快了原料之间水/油界面处的反应，从而促进化学反应。为了得到正确的润滑脂性质，然后必须将水除去，该过程通常在所谓的“放空步骤”中通过蒸发进行。该放空步骤耗时耗能，特别是对于含有更多固体成分和因而需要更多水的锂络合润滑脂的情况来说更是如此。而且，锂络合润滑脂较的较高稠度使得水的除去变得愈发困难。因此，开发一种水量减少、放空时间缩短的金属络合润滑脂的制备方法将是有利的。
已经令人惊异地发现，通过减小用于制备金属络合润滑脂的固体组分例如金属碱和络合剂的粒度，实现皂化反应明显需要更少的水，从而缩短了放空时间和提高了润滑脂装置的产率。
发明内容
根据本发明，提供一种用于制备金属络合润滑脂组合物的方法，包括如下步骤：
(i)制备包含基础油、水、金属碱和络合剂的浆液，其中所述浆液中水∶固体的重量比为0.15∶1-1.5∶1；
(ii)以至少为1,000,000s-1的剪切频率向所述浆液施加剪切；
(iii)将来自步骤(ii)的浆液加入到C10-C24饱和或不饱和脂肪酸或其衍生物中实施皂化反应，所述皂化反应在至少80℃的温度下进行；
(iv)从由步骤(iii)得到的皂化产物中除去水；
(v)将来自步骤(iv)的产物加热到至少190℃；和
(vi)将由来自步骤(v)的产物冷却到200-150℃以形成金属络合润滑脂组合物。
根据本发明，进一步提供一种通过这里所述的方法制备的润滑脂组合物。
已经令人惊异地发现，本发明的方法减少了将水蒸发所需的放空时间，减少了总的批次生产时间，提供了更为能量有效的制备方法，和提高了产率。
具体实施方案
本发明方法的第一个主要步骤包括制备包含基础油、水、金属碱和络合剂的浆液。
浆液在专用浆液槽中制备。该浆液槽是一个容器，其中固体(例如氢氧化锂、硼酸、氢氧化钙、水杨酸等)和液体(水、基础油、添加剂等)一起加入以制备分散体或“悬浮体”，之后送至高压釜。
对本发明方法中使用的基础油没有特别限制，各种常规的矿物油和合成油均可以方便地使用。出于该描述的目的，术语“基础油”的含义也包括润滑脂基础油料。
优选地，以润滑组合物的总重量为基准，润滑组合物包含至少30wt％的基础油，优选至少50wt％，更优选至少70wt％。
本发明所使用的基础油组合物适宜包含一种或多种矿物油和/或一种或多种合成油的混合物。
这里所使用的基础油优选在40℃下(依据ASTM D445)的运动粘度为10-2000mm2/s。
矿物油包括液态石油油料和溶剂处理的或酸处理的矿物润滑油，所述矿物润滑油为链烷类、环烷类或链烷/环烷混合类，它们可以通过加氢精制过程和/或脱蜡进行进一步精制。
合成油包括烃油，例如烯烃低聚物(PAOs)、二元酸酯、多元醇酯、聚亚烷基二醇和脱蜡的蜡质残液。Shell Group以商品名“XHVI”(商标)出售的合成烃基础油可以方便地使用。
用于本发明润滑油组合物的合适基础油为第I组、第II组或第III组基础油、聚α-烯烃、费-托衍生的基础油和它们的混合物。
在本发明中“第I组”基础油、“第II组”基础油和“第III组”基础油指的是根据美国石油学会(API)分类I、II和III的定义的润滑油基础油。该API分类在API出版物1509，第15版，附录E，2002年4月中定义。
可以在本发明的润滑油组合物中方便地用作基础油的合适的费-托衍生基础油为例如如下文献所公开的那些：EP 0776959、EP0668342、WO 97/21788、WO 00/15736、WO 00/14188、WO 00/14187、WO 00/14183、WO 00/14179、WO 00/08115、WO 99/41332、EP1029029、WO 01/18156和WO 01/57166。
在本发明优选的实施方案中，基础油是Royal Dutch/Shell Group的公司以商品名“HVI”或“MVIN”出售的矿物源基础油。
以金属络合润滑脂组合物的重量计，金属碱的存在量优选为1-5wt％，更优选为2-4wt％。
对可用于本发明方法的金属碱的类型没有特别限制。适用这里的金属碱的例子包括氢氧化锂、氢氧化钙、氢氧化铝、氢氧化钛和它们的混合物。用在这里的优选金属碱为氢氧化锂。
在制备过程中加入络合剂，以制备金属络合皂增稠剂。合适的络合剂包括低分子量到中等分子量的酸或二元酸。用在这里的优选络合剂选自硼酸、癸二酸、壬二酸、苯甲酸、乙二酸、丙二酸、丁二酸、戊二酸、己二酸、辛二酸、庚二酸、十二烷二酸和它们的组合物。
用在这里的特别优选的络合剂是硼酸。
这里的方法的第一步骤制备的浆液包含水。浆液中水∶固体的重量比为0.15∶1-1.5∶1，优选为0.2∶1-1∶1，更优选为0.2∶1-0.6∶1。已经令人惊异地发现，本发明方法允许加入少量的水，从而相应缩短放空时间。
浆液槽优选设置有内部混合器和再循环管线。
在所述方法的第二主要步骤中，浆液承受至少为1,000,000s-1的剪切频率。优选的剪切频率为至少1,500,000s-1，更优选为至少1,800,000s-1，甚至更优选为至少2,000,000s-1。
适于提供至少为1,000,000s-1的剪切频率的任何混合器均可在这里应用。
对浆液施加至少为1,000,000s-1的剪切频率优选减小存在于浆液中的固体(例如锂碱、络合剂)的粒度，结果使得至少90％的固体颗粒具有最大50μm的粒度。优选存在于浆液中的固体的粒度降低到平均粒度为0.0001-200μm，更优选为1-75μm，甚至更优选为3-50μm。
皂化反应在水-油界面处发生。不希望被理论所限制，将粒度减小到所述范围意味着传质面积增大，和需要更少的水来进行皂化和络合反应。
这里的方法可以使用原位(即位于浆液容器自身内部)或在线(即位于浆液容器外部)高剪切混合器。原位高剪切混合器位于浆液容器自身内部，而在线高剪切混合器位于浆液容器外部，例如在再循环管线上。在一个优选的方法中，使用了在线高剪切混合器，该高剪切混合器位于浆液容器的再循环管线上。
用于这里的合适混合器为高剪切混合器，它优选包括至少一个具有方孔的筛网，被称为“方孔高剪切混合器(SQHSM)”。在一个用于这里的合适实施方案中，高剪切混合器包括两个筛网，一个内筛网和一个外筛网，其中至少一个具有方孔。优选外筛网具有方孔。在一个实施方案中，高剪切混合器包括具有方孔的外筛网和具有槽状方孔(即呈矩形)的内筛网。也可能有包括三个筛网的高剪切混合器，优选其中至少一个筛网具有方孔。
用在这里的特别优选的高剪切混合器包括两个均具有方孔的筛网(双筛网方孔高剪切混合器)。
当高剪切混合器具有内筛网和外筛网时，通常外筛网提供至少为1,000,000s-1的剪切频率。
用于这里的合适高剪切混合器的例子为在美国专利No.3897013和美国专利No.3632227中公开的那些，它们优选装有至少一个方孔筛网，更优选装有两个方孔筛网。
用于这里的合适高剪切混合器包括但不限于下列混合器：
(1)可从Silverson商购的双筛网方孔高剪切混合器，型号为312/450MS，具有4个内部转子叶片，12个外部转子叶片，驱动速度为300RPM，额定功率为7.5kW，频率为50Hz，内部转子尖端速度为12.4m/s，外部转子尖端速度为17.95m/s，内部剪切频率为435483s-1，和外部剪切频率为2143393s-1；
(2)可从Silverson商购的双筛网方孔高剪切混合器，型号为450/600MS，具有4个内部转子叶片，12个外部转子叶片，驱动速度为300RPM，额定功率为15kW，频率为50Hz，内部转子尖端速度为17.95m/s，外部转子尖端速度为23.95m/s，内部剪切频率为714464s-1，和外部剪切频率为3320558s-1。
具有不同于50Hz例如60Hz频率的高剪切混合器也适用于这里。
在本发明方法的第三步骤中，来自步骤(ii)的浆液与C10-C24饱和或不饱和脂肪酸或其衍生物接触实施皂化反应。皂化反应在至少80℃、优选至少100℃的温度下进行。这里使用的术语“皂化反应”也包括络合反应。这里使用的术语“皂化产物”也包括络合产物。
在与来自步骤(i)的浆液接触前，可以将C10-C24饱和或不饱和脂肪酸或其衍生物预熔。通常，C10-C24饱和或不饱和脂肪酸在基础油中预熔。
用于这里的合适脂肪酸组分的例子包括脂肪酸、脂肪酸酯、脂肪酸甘油酯和它们的组合。脂肪酸组分通常包含10-24个碳原子(C10-C24)，优选为15-18个碳原子(C15-C18)。脂肪酸组分可以是饱和的或不饱和的。用于这里的合适脂肪酸组分的例子包括油酸、棕榈酸、硬脂酸和其它由牛油、氢化鱼油、蓖麻油、羊毛、油脂和松香以及它们的组合衍生的羧酸。用于制备润滑脂组合物的合适脂肪酸组分的例子包括氢化蓖麻油(HCO)、氢化蓖麻润滑脂肪酸(HCOFA)和它们的组合，优选为氢化蓖麻润滑脂肪酸(HCOFA)。氢化蓖麻油(HCO)是12-羟基硬脂酸的甘油酯。12-羟基硬脂酸是用在这里的优选脂肪酸。
氢化蓖麻润滑脂肪酸(以下称为HCOFA)通常包含至少85wt％的12-羟基硬脂酸，以HCOFA总重量计。HCOFA可能包含少量的附加组分。附加组分的例子包括棕榈酸(C16)、硬脂酸(C18)、花生酸(C20)、12-酮硬脂酸和它们的组合。这里使用的术语“氢化蓖麻润滑脂肪酸”(“HCOFA”)是指包含一定量的12-羟基硬脂酸的组合物，通常包含至少85wt％的12-羟基硬脂酸，优选包含85-87wt％的12-羟基硬脂酸，以HCOFA总重量计。
在所述方法的步骤(iv)中，从由步骤(iii)得到的皂化产物中除去水。优选地，在步骤(iv)中将来自步骤(iii)的皂化产物中除去存在的全部水，即在制备浆液时加入的水、在皂化反应中生成的水和在金属碱中存在的任何水。优选在所谓“放空步骤”中通过蒸发将水除去。优选通过将由步骤(iii)得到的皂化/络合产物加热到至少100℃、更优选至少110℃的温度来将水除去。
在步骤(iv)中将水除去之后，来自步骤(iv)的产物要经过加热步骤(v)，其中所述产物被加热到至少190℃、优选为190-230℃、更优选为195-225℃、和甚至更优选为200-220℃的温度。
在加热步骤(v)之后，产物要经过冷却步骤(vi)以形成金属络合润滑脂组合物。冷却步骤(vi)在200-150℃下、优选在195-160℃下、更优选在190-165℃下进行。冷却步骤优选在润滑脂釜中进行。
在所述方法的任选步骤(vii)中，向金属络合润滑脂组合物中加入性能添加剂。优选在润滑脂釜中加入性能添加剂。可将各种常规的润滑脂添加剂以该应用领域通常的用量掺入本发明的润滑脂中，赋予润滑脂一些所需的性质，例如氧化稳定性、粘着性、极压性和抗腐蚀性。适宜的添加剂包括：一种或多种极压/耐磨剂，例如锌盐(如二烷基或二芳基二硫代磷酸锌)、硼酸盐、取代噻二唑、聚合氮/磷化合物(例如通过将二烷氧基胺与取代的有机磷酸酯、磷酸胺、硫化的天然或合成源鲸油、硫化猪油、硫化酯、硫化脂肪酸酯和类似的硫化物质进行反应而制得)、有机磷酸酯(例如式(OR)3P＝O，其中R为烷基、芳基或芳烷基)和硫代磷酸三苯酯；一种或多种高碱性含金属清净剂，如钙或镁的烷基水杨酸盐或烷基芳基磺酸盐；一种或多种无灰分散剂添加剂，如聚异丁烯丁二酸酐与胺或酯的反应产物；一种或多种抗氧化剂，如受阻酚或胺，例如苯基α-萘胺；一种或多种防锈添加剂；一种或多种摩擦调节添加剂；一种或多种粘度指数促进剂；一种或多种降倾点添加剂；和一种或多种粘性剂。也可以加入固体材料，如石墨、粉碎的二硫化钼、滑石、金属粉末、碳酸钙和各种聚合物如聚乙烯蜡，以带赋予特定的性质。
为降低摩擦程度，本领域的技术人员会寻求使用基于有机钼的制剂，和在此类润滑组合物的专利文献中有很多建议。
下面参照如下实施例对本发明进行描述。
实施例
实施例1
使用如下制备方法来制备具有如表1所示配方的润滑脂组合物。在第一步骤中，通过将基础油(占基础油总量的10wt％)、单水合LiOH和水加入浆液槽来制备浆液。水∶固体的重量比为约0.2-0.4∶1。使用具有双筛网方孔的在线高剪切混合器对浆液进行20分钟的混合。所使用的混合器是从Silverson商购的双筛网方孔高剪切混合器，型号为312/450MS，具有4个内部转子叶片，12个外部转子叶片，驱动速度为300RPM，额定功率为7.5kW，频率为50Hz，内部转子尖端速度为12.4m/s，外部转子尖端速度为17.95m/s，内部剪切频率为435483s-1，和外部剪切频率为2143393s-1。将硼酸和分散剂加入浆液，再次进行高剪切混合。将得到的浆液送至包含基础油(占基础油总量的约50wt％)和预熔的12-羟基硬脂酸的高压釜中。用基础油对浆液槽和高剪切混合器再循环管线冲洗两次，和将冲洗液送至高压釜。
在约4巴的压力下对高压釜加热，同时放空开始。将压力保持在约4巴，直到温度达到195-200℃，同时放空结束。将高压釜加热至约220℃的最高温度，和将得到的组合物送至润滑脂釜中，然后加入剩余的基础油，冷却，加入性能添加剂，和完成。
记录每个制备步骤所用的时间。
使用表2所列的标准测试方法测量成品润滑脂组合物的各种性质。
对比例1
使用基本上与实施例1相同的制备方法来制备具有如表1所示配方的锂络合润滑脂，只是使用具有低剪切速率的桨和搅拌器型常规混合器来制备浆液。另外水∶固体的重量比为约1.5∶1。
记录每个制备步骤所用的时间。使用表2所列的标准测试方法测量成品润滑脂组合物的各种性质。
表1
  组分  对比例1(wt％)  实施例1(wt％)
  矿物油  72  75
  HCOFA  9  8
  单水合氢氧化锂  3  2
  硼酸  3  2
  分散剂  3  3
  添加剂包  10  10
表2
结果
实施例1的批次生产时间比对比例1缩短47分钟。批次生产时间的差异是实施例1的放空和加热时间更短的结果，这是由于实施例1需要水量更少的结果。与对比例1相比，实施例1缩短47分钟带来了显著的产率提高。这一显著的产率提高不能归因于对比例1与实施例1在配方上的微小差别。
由于加入水量更少意味着需要蒸发的水量更少，因而由对比例1到实施例1还存在显著的能量节约。制备对比例1的润滑脂，每批次需要加入约170kg的水。制备实施例1的润滑脂仅需约30kg的水。少加入140kg的水使每批次的能量节约为约300,000kJ。
从表2可以看出，尽管使用的水量比常规锂络合润滑脂少，但实施例1显示了至少与对比例1等同的优良的润滑脂性质。对比例1与实施例1之间微小的物理性能差别处在润滑脂制备中正常的批次差别或者测试方法重复性的范围内。

Claims (12)

1.一种用于制备金属络合润滑脂组合物的方法，包括如下步骤：
(i)制备包含基础油、水、金属碱和络合剂的浆液，其中所述浆液中水:固体的重量比为0.15:1-1.5:1；
(ii)以至少为1,000,000s-1的剪切频率向所述浆液施加剪切；
(iii)将来自步骤(ii)的浆液加入到C10-C24饱和或不饱和脂肪酸或其衍生物中实施皂化反应，所述皂化反应在至少80℃的温度下进行；
(iv)从由步骤(iii)得到的皂化产物中除去水；
(v)将来自步骤(iv)的产物加热到190-230℃；和
(vi)将由来自步骤(v)的产物冷却到200-150℃以形成金属络合润滑脂组合物。
2.根据权利要求1的方法，其中所述浆液中水:固体的重量比为0.2:1-1:1。
3.根据权利要求1或2的方法，其中所述剪切频率为至少1,500,000s-1。
4.根据权利要求1或2的方法，其中步骤(ii)利用具有至少一个方孔筛网的高剪切混合器进行。
5.根据权利要求4的方法，其中所述高剪切混合器包括两个方孔筛网。
6.根据权利要求1或2的方法，其中所述方法包括附加步骤(vii)：
(vii)向所述金属络合润滑脂组合物中加入性能添加剂。
7.根据权利要求1或2的方法，其中所述金属碱选自氢氧化锂、氢氧化钙、氢氧化铝、氢氧化钛和它们的混合物。
8.根据权利要求1或2的方法，其中所述金属碱为氢氧化锂。
9.根据权利要求1或2的方法，其中所述络合剂选自低分子量到中等分子量的酸或二元酸。
10.根据权利要求1或2的方法，其中所述络合剂选自硼酸、癸二酸、壬二酸、苯甲酸、乙二酸、丙二酸、丁二酸、戊二酸、己二酸、辛二酸、庚二酸、十二烷二酸和它们的组合物。
11.根据权利要求1或2的方法，其中所述络合剂为硼酸。
12.根据权利要求1或2的方法，其中所述C10-C24饱和或不饱和脂肪酸或其衍生物为12-羟基硬脂酸。
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