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CN107922878B - 具有聚亚烷基二醇和不饱和酯的流体 - Google Patents

具有聚亚烷基二醇和不饱和酯的流体 Download PDF

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CN107922878B
CN107922878B CN201680048671.2A CN201680048671A CN107922878B CN 107922878 B CN107922878 B CN 107922878B CN 201680048671 A CN201680048671 A CN 201680048671A CN 107922878 B CN107922878 B CN 107922878B
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fluid
polyalkylene glycol
oil
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base oil
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CN107922878A (zh
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M·R·格里夫斯
E·A·佐格-胡泽曼斯
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Abstract

流体含有由醇引发的聚亚烷基二醇组成的基础油，其中聚亚烷基二醇组分选自1,2‑环氧丁烷的均聚物和1,2‑环氧丁烷与环氧丙烷的共聚物；不含叔碳原子和季碳原子的甘油引发的不饱和酯；和抗氧化剂。

Description

具有聚亚烷基二醇和不饱和酯的流体
技术领域
本发明涉及聚亚烷基二醇和不饱和酯混合物的流体。
背景技术
耐火工业流体，特别是那些具有热氧化稳定性的工业流体，在高温应用中是合乎需要的，如钢铁加工和发电中的润滑剂和液压流体。提高这种工业流体的耐火性和热氧化稳定性是持续的愿望和挑战。历来被用作润滑剂的烃类油由于其可燃性在这种应用中通常是不合乎需要的。水基润滑剂比烃类油具有更好的耐火性能，但往往不合适在水分蒸发的高温应用中使用。高温应用通常需要无水润滑剂。
常规的聚亚烷基二醇(PAG)被称为烃类化合物和水的润滑剂基础油替代品。常规的PAG是使用一元醇、二元醇或三元醇引发并与环氧乙烷和/或环氧丙烷反应以形成典型地具有大于500g/mol且至多50,000g/mol的分子量的聚合物的PAG。使用这种常规PAG作为基础油的润滑剂组合物作为液压流体和涡轮机油提供了有利的性能益处。然而，除非存在抗氧化剂，否则常规PAG容易遭受氧化不稳定性。因此，当常规的基于PAG的润滑剂组合物中抗氧化剂耗尽时，润滑剂的氧化稳定性受到不合乎需要的影响。常规的PAG也具有差的油溶性。因此，为了在历史上使用烃类流体的系统中使用PAG，系统必须经过昂贵彻底的冲洗以避免用烃类流体污染传统的PAG流体。
具有油溶性的工业流体是合乎需要的并且表现出比常规PAG更好的耐火性。
发明内容
本发明提供了一种油溶性的流体并且其表现出比常规PAG更好的耐火性。本发明令人惊奇地发现将不饱和酯与油溶性PAG和抗氧化剂组合的结果，可导致相对于单独PAG或与所述的抗氧化剂组合的PAG的燃点，所得流体的燃点升高。
在第一方面，本发明是一种流体，其包含：(a)由醇引发的聚亚烷基二醇组成的基础油，其中聚亚烷基二醇组分选自1,2-环氧丁烷的均聚物和1,2-环氧丁烷和环氧丙烷的共聚物；(b)不含叔碳原子和季碳原子的甘油引发的不饱和酯；和(c)抗氧化剂。
在第二方面，本发明是一种使用所述的第一方面的流体的方法，所述的方法包括将所述的第一方面的流体引入设备中，以用作选自液压流体、涡轮流体和润滑剂的组中的材料。
本发明的流体可用作润滑剂和/或液压流体，特别是用于在含水润滑剂不合乎需要的高温和高压应用中。
具体实施方式
“和/或”的意思是“和或者可替代地”。除非另有说明，所有范围均包括端点。
试验方法是指截至本文优先权日期的最新试验方法，除非试验方法编号中标明日期为带连字符的两位数字。对试验方法的引用既包含对试验协会的引用，也包含对测试方法编号的引用。试验方法组织参考以下缩写之一：ASTM是指国际ASTM(以前称为美国材料与试验协会)；EN是指欧洲标准；DIN是指德国标准化学会；ISO是指国际标准组织。
根据ASTM D7042测定运动粘度。根据ASTM D2270计算润滑剂配方的粘度指数。根据ASTM D97测定倾点。根据ASTM D4274测量羟值。根据ASTM方法D92测定燃点值。除非另有说明，“分子量”是指通过尺寸排阻色谱法测定的重均分子量
本发明是一种包含基础油、和不饱和酯和抗氧化剂的流体。所述流体作为液压流体和/或润滑剂流体是合乎需要的。由于其阻燃性，所述的流体是特别合乎需要的。
所述的基础油是醇引发的聚亚烷基二醇。醇引发的是指聚亚烷基二醇(PAG)通过在催化条件下醇盐与醇加成并使聚合物生长至目标分子量或粘度来合成。当初始醇盐与醇的羟基反应以开始聚合过程时，聚合物生长，此后醇盐从最初的醇盐生长到彼此聚合。所述基础油的主链含有与氧原子结合的碳原子并且所述的氧原子进一步与聚氧化烯链结合。与氧结合的主链的碳合乎需要地进一步仅与选自碳和氢的元素结合。醇引发剂可以在碳链上具有一个、两个或三个羟基。因此，所得到的基础油可具有带有一个、两个或三个氧原子的碳链主链，每个氧原子具有与氧结合的聚氧化烯链。合适的引发剂包括具有三个或更多个，优选四个或更多个，并且可以包含六个或更多个、八个或更多个、九个或更多个、10个或更多个、11个或更多个、甚至12个或更多个以及通常20个或更少的碳原子的醇。通过PAG主链中的碳的数目，在PAG中所述引发剂中碳的数目是明显的。所述主链是聚氧化烯基团经由氧原子延伸的碳链。合适的引发剂的实例包括丁醇、戊醇、己醇、环己醇、庚醇、辛醇、2-乙基己醇、壬醇、癸醇、十二烷醇、硬脂醇、油醇、1,4-丁二醇、新戊二醇、1,6-己二醇、甘油和三羟甲基丙烷。
醇引发的PAG的聚氧化烯组分选自1,2-环氧丁烷的均聚物和1,2-环氧丁烷和环氧丙烷的共聚物。所述环氧丙烷合乎需要地为1,2-环氧丙烷。所述流体合乎需要地是不含环氧乙烷的均聚物和/或共聚物，以使所述基础油的油溶性最大化。合乎需要地，本发明的所述流体含有少于10wt％，优选5wt％或更少，并且最合乎需要的不含聚氧乙烯和/或聚氧乙烯共聚物，其中wt％是相对于总流体重量，以使所述流体的油溶性最大化。
合乎需要的醇引发的PAG的例子包括十二烷醇引发的环氧丙烷和1,2-环氧丁烷的共聚物。合乎需要的醇引发的PAG的另一个例子包括丁醇引发的1,2-环氧丁烷的均聚物，也称为聚丁二醇单丁基醚。
所述醇引发的PAG可以是封端的或未封端的。“未封端的”PAG在分子中具有终止聚氧化烯链的羟基(-OH)基团。相反，“封端的”PAG具有-OR官能团而不是-OH官能团来终止分子的聚氧化烯链，其中在-OR中的R是指包括烷基、芳基和羰基例如基于酯或酰胺的含碳基团。
所述醇引发的PAG的所述引发剂和PAG组分的要求使其成为油溶性的。当混合25克PAG与75克具有根据ASTM D-4052在15℃下相对密度为0.84和根据ASTM D-445在40℃下运动粘度为约48厘沲(cSt)的20-50碳加氢处理的基础油(NEXBASETM3080；NEXBASE是耐思特石油公司(Nester Oil OYJ Corporation)的商标)，并在23摄氏度(℃)下搅拌15分钟，如果它们在目视检查时形成清澈均匀的溶液，PAG被视为“油溶的”。已经发现非油溶性的PAG没有表现出本发明的流体的令人惊讶的燃点增加。
当所述醇引发的PAG是环氧丙烷(PO)和1,2-环氧丁烷(BO)的共聚物时，PO与BO的比例合乎需要地以重量计在1:1至1:3的范围内。此外，或者可替代地，所述醇引发的PAG的数均分子量合乎需要地为2000克/摩尔或更小，同时合乎需要地为500克/摩尔或更多。
所述醇引发的PAG合乎需要地以按流体总重量计70重量百分数(wt％)或更大的浓度，优选地75wt％或更大且可以80wt％或更大、85wt％或更大、90wt％或更大且甚至95wt％或更大的浓度存在于所述的流体中。
所述不饱和酯是甘油引发的不饱和酯。“甘油引发的”不饱和酯特征是所述酯具有带三个相邻的碳原子的碳主链，每个碳原子都与一个氧原子结合，而氧原子又进一步与一个酸级分链结合形成一个碳主链的酯分支。所述不饱和酯可以是例如甘油三酯或合成酯。典型的酸级分是油酸、亚油酸、亚麻酸和蓖麻油酸。
所述的不饱和酯不含具有至少一个选自叔碳原子和季碳原子的碳原子组成的组的酯。如此，所述的不饱和酯被分类为非空间位阻。值得注意的是，所述的具有叔碳原子和/或季碳原子的流体中可能有小量的材料，但所述的甘油三酯不含这种碳原子。例如，叶绿素可以少量存在植物油中，但所述的植物油的甘油三酯不含叔碳原子和季碳原子。
所述的不饱和酯在其结构中含有一个或多个碳-碳双键或三键。令人惊讶的是，当在流体组合物中包含PAG，已发现不饱和酯但不是饱和酯可有效提高醇引发PAG的燃点。饱和酯不含碳-碳双键或三键。
特别合乎需要的不饱和酯的实例包括高油酸葵花籽油(HOSO)和蓖麻油。HOSO是在甘油三酯结构的酸部分中含有约85wt％的油酸的甘油三酯。
所述的不饱和酯合乎需要地以基于流体总重量5重量百分数(wt％)或更大，优选地10wt％或更大，并且可以是15wt％或更大，同时通常是30wt％或更小，优选为25wt％或更小，并且可以是20wt％或更小的浓度存在于所述的流体中。
所述的流体还包含抗氧化剂。所述的抗氧化剂合乎需要地为含氮化合物。特别合乎需要的抗氧化剂包括选自吩噻嗪、p,p'-二辛基二苯胺和辛基化/丁基化二苯胺组成的一组。抗氧化剂通常以基于流体总重量0.25wt％或更大，优选0.5wt％或更大，并且可以是1wt％或更大，甚至1.5wt％或更大，同时通常为3wt％或更小，优选2.5wt％或更小，更优选2wt％或更小的浓度存在于所述的流体中。
用于所述的流体中特别合乎需要的抗氧化剂是吩噻嗪。
所述的流体可以含有或不含任何一种或多种添加剂的组合，包括选自抗磨极压腐蚀抑制剂，黄色金属钝化剂，染料和泡沫控制添加剂。
令人惊讶地发现，如本发明流体所述的基础油、不饱和酯和抗氧化剂的组合具有出乎意料的高燃点，这使得所述的流体在阻燃性重要时特别有用。特别地，所述的流体可用作液压流体、涡轮流体和/或润滑剂。
本发明包括使用本发明所述的流体的方法，所述的方法包括将所述的流体引入设备中，以用作选自液压流体、涡轮流体和润滑剂的组中的材料。
实施例
混合程序。通过向500毫升玻璃烧杯中加入下表中指定比例的组分并在温和的热量下(50℃最高温度)下搅拌制备200克的各比较例(Comp Ex)和实施例(Ex)。
油溶性测量。将25克流体添加到75克烃类油(NEXBASETM3080)中并在室温下搅拌15分钟。清澈均匀的混合物是“可溶的”或“S”。不清晰和/或不均匀的混合物是“不可溶”或“NS”。
燃点测量。根据ASTM D92测定流体的燃点温度。
表1鉴定了实施例和比较例中使用的材料。
表1
Figure BDA0001580618280000041
Figure BDA0001580618280000051
Figure BDA0001580618280000061
比较例A-F：聚丙二醇单丁醚基础油
表2所示的制备流体并通过燃点测定和油溶性来表征。相对于流体总重量，流体组合物以每种组分的重量百分数记录。比较例A只是基础油。比较例B和C是含有抗氧化剂的基础油。比较例D-F是基础油、抗氧化剂和酯类的组合。
结果显示没有任何流体是油溶性的。结果还显示，所述抗氧化剂增加了燃点，但酯类不会进一步增加燃点。
表2
Figure BDA0001580618280000062
比较例H-S：聚丙二醇单烯丙基醚基础油
表3和表4所示的制备流体并通过燃点测定和油溶性来表征。相对于流体总重量，流体组合物以每种组分的重量百分数记录。比较例H只是基础油。比较例I-K是含有抗氧化剂的基础油。比较例L-S是基础油、抗氧化剂和酯类的组合。
结果显示没有任何流体是油溶性的。结果还显示，所述抗氧化剂增加了燃点，但包含的饱和酯不会使燃点进一步增加超过8℃。
表3
Figure BDA0001580618280000063
Figure BDA0001580618280000071
表4
Figure BDA0001580618280000072
比较例T-AA：十二烷醇引发的PO/BO无规共聚物基础油
表5所示的制备流体并通过燃点测定和油溶性来表征。相对于流体总重量，流体组合物以每种组分的重量百分数记录。比较例T只是基础油。比较例U-X是含有抗氧化剂的基础油。比较例Y-AA是基础油、抗氧化剂和饱和酯的组合。
所述流体是油溶性的。抗氧化剂增加了燃点，但饱和酯不会使燃点进一步增加超过几摄氏度。
表5
Figure BDA0001580618280000073
a两个燃点值表示制备并评估了两个样品。
实施例1-6：十二醇引发的具有抗氧化剂和不饱和酯的PO/BO无规共聚物基础油
表6所示的制备流体并通过燃点测定和油溶性来表征。相对于流体总重量，流体组合物以每种组分的重量百分数记录。实施例(Exs)1-6是基础油、抗氧化剂和不饱和酯的组合。
结果显示所述流体是油溶性的。结果还显示(相对于比较例T、U和X)所述不饱和酯与抗氧化剂组合令人惊讶地使燃点增加55-60℃，比单独的所述基础油增加更多并且比单独所述基础油和抗氧化剂增加10-24℃。
表6
Figure BDA0001580618280000081
比较例BB和CC和实施例7-9：PO/BO共聚物基础油
表7所示的制备流体并通过燃点测定和油溶性来表征。相对于流体总重量，流体组合物以每种组分的重量百分数记录。
结果显示所述流体是油溶性的。结果还显示另一种PO/BO基础油，其中与抗氧化剂组合的不饱和酯令人惊讶地增加了比单独的所述基础油和抗氧化剂高的燃点。
表7
Figure BDA0001580618280000082
比较例DD和EE和实施例10-11：BO均聚物基础油
表8所示的制备流体并通过燃点测定和油溶性来表征。相对于流体总重量，流体组合物以每种组分的重量百分数记录。
结果显示所述流体是油溶性的。结果还显示BO均聚物基础油，其中与抗氧化剂组合的不饱和酯令人惊讶地增加了比单独的所述基础油和抗氧化剂高的燃点。
表8
Figure BDA0001580618280000091

Claims (6)

1.一种流体，包括：
（a）由醇引发的聚亚烷基二醇组成的基础油，其中所述聚亚烷基二醇组分选自1,2-环氧丁烷的均聚物和1,2-环氧丁烷与环氧丙烷的共聚物，其中聚亚烷基二醇基础油以70wt%至89wt%的浓度存在；
（b）不含叔碳原子和季碳原子的甘油引发的不饱和酯，其中所述不饱和酯选自高油酸葵花籽油和蓖麻油并且以10 wt%至25 wt%的浓度存在；和
（c）抗氧化剂，其中所述抗氧化剂为选自吩噻嗪、p,p'-二辛基二苯胺和辛基化/丁基化二苯胺的含氮化合物，其以0.25wt%至1.0 wt%的浓度存在，并且其中所述流体为油溶性的并且具有根据ASTM D92的与单独的基础油相比增加至少55℃和与单独的基础油和抗氧化剂相比增加至少10℃的燃点。
2.根据权利要求1所述的流体，其中所述的流体不含包含聚合的环氧乙烷的聚亚烷基二醇。
3.根据权利要求1所述的流体，其中所述聚亚烷基二醇选自丁醇和十二烷醇引发的聚亚烷基二醇。
4.根据权利要求1所述的流体，其中所述抗氧化剂是吩噻嗪。
5.一种使用根据权利要求1-4中任一项所述的流体的方法，所述方法包括将根据权利要求1-4中任一项所述的流体引入设备中，以用作润滑剂。
6.一种使用根据权利要求1-4中任一项所述的流体的方法，所述方法包括将根据权利要求1-4中任一项所述的流体引入设备中，以用作液压流体和涡轮流体。
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