CN1044492A - 致冷压缩机用润滑油 - Google Patents

致冷压缩机用润滑油 Download PDF

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Publication number
CN1044492A
CN1044492A CN90100090A CN90100090A CN1044492A CN 1044492 A CN1044492 A CN 1044492A CN 90100090 A CN90100090 A CN 90100090A CN 90100090 A CN90100090 A CN 90100090A CN 1044492 A CN1044492 A CN 1044492A
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Prior art keywords
ester
lubricant compositions
polyether polyol
making
hydrofluorocarbon
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CN90100090A
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菲利浦·W·姆格罗
埃尔顿·L·沃德
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Dow Chemical Co
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Dow Chemical Co
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Publication of CN1044492A publication Critical patent/CN1044492A/zh
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    • C09K5/02—Materials undergoing a change of physical state when used
    • C09K5/04—Materials undergoing a change of physical state when used the change of state being from liquid to vapour or vice versa
    • C09K5/041—Materials undergoing a change of physical state when used the change of state being from liquid to vapour or vice versa for compression-type refrigeration systems
    • C09K5/044—Materials undergoing a change of physical state when used the change of state being from liquid to vapour or vice versa for compression-type refrigeration systems comprising halogenated compounds
    • C09K5/045—Materials undergoing a change of physical state when used the change of state being from liquid to vapour or vice versa for compression-type refrigeration systems comprising halogenated compounds containing only fluorine as halogen
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Abstract

公开了压缩致冷的润滑剂组合物，它由95～5％(重量)的数均分子量为400～5000的聚醚多醇和5～95％(重量)的由多元醇与链烷酸制成的酯或链烷二酸与链烷醇制成的酯组成。还公开了这种润滑剂组合物的制备方法和用其配制压缩致冷用的流体组合物。

Description

本发明涉及润滑热泵和空调压缩机用的二醇和酯的共混物。
致冷剂R12（二氯二氟甲烷）用于汽车空调和许多其它类型的致冷和空调用压缩机。已证实，含氯氟烃对大气中的臭氧有破坏作用。Montreal        Accords自1990年起限制R12的生产。致冷剂R134a（1，1，1，2-四氟乙烷）具有与R12很类似的蒸汽压，其优点在于不破坏大气中的臭氧。R134a可在大多数致冷系统中代替R12而不用重新设计现存设备。R134a可用于汽车空调而无须由汽车公司重新加工。
用R134a的主要问题是，常用的润滑剂（如环烷烃矿物油）在-20～80℃不溶，而且在不同的致冷应用中会面临操作温度的问题。某些聚乙二醇在25℃或以下溶于R134a，但低于60℃发生相分离。润滑剂与致冷剂相分离能使压缩机的润滑性变差，造成磨损提高和压缩机寿命下降。致冷工业都知道，致冷剂中润滑剂浓度因热力学原因限制在约10～20%的范围内。本发明的有用性在于，压缩机厂商能在多数压缩机中用R134a和其它含氢氟烃或含氢氯氟烃代替含氯氟烃（如R12），而不必对现有的压缩机进行机械改进，而且能在很宽的温度范围内操作。
H.H.kruse等人在“致冷系统和热泵的润滑原理”（第763～783页）和ASHRAE        Transactions（90卷，2B部分，1984）中提出了空调润滑原理。
美国专利4，302，343和4，751，012公开了各种空气压缩机的润滑剂。这两篇专利表明了用酯和聚醚多醇的不同共混物制成的长效润滑剂。但是，这些共混物或在38℃下净粘度低于75厘沲（75×106m2/s），或在致冷所用的高温下不能混溶。
美国专利4，755，316介绍了含一种或多种聚醚多醇的组合物，用于润滑采用R134a的致冷压缩机。但是，′316专利介绍的组合物在压缩机中显示出高温下合适的粘度，而在同样的高温下却不能混溶，反之，在低温下显示出混溶性，但粘度却太低，不宜润滑。
本发明包括润滑剂组合物，这些润滑剂组合物能在-20℃～高于65℃的温度范围内混溶于含氢氟烃和含氢氯氟烃致冷剂，同时，于38℃（100°F）净粘度高于75厘沲（75×106m2/s）。一般来说，这种组合物由（A）和（B）构成：
（A）5～95%的聚醚多醇，其结构式为
其中Z是具有1～8个活性氢的化合物基，
R1是氢，乙基，或其混合物，
n为0或一正数，
m是一正数，
m+n值能得到数均分子量约为400～5000的聚醚多醇，
R2是氢或C1～6烷基，
P是一整数，其值等于Z的活性氢数，以及
（B）95～5%的酯，该酯选自：
（1）多元醇与链烷酸制成的酯，和
（2）链烷二酸与链烷醇制成的酯。
本发明用的中性酯是公知的和/或可买到。适宜的酯的例子是具有4～18个碳原子的二元醇、三元醇和四元醇（如甘油，乙二醇，丙二醇，季戊四醇，二季戊四醇，三季戊四醇，三羟甲基丙烷，三羟甲基丁烷和三羟甲基乙烷）与具有4～18个碳原子的链烷酸的酯。这些酯的例子为二硬脂酸乙二醇酯，二壬酸丙二醇酯，三油酸甘油酯，三羟甲基丙烷三庚酸酯和季戊四醇四庚酸酯。
C4～8一元醇与C4～18链烷二酸（如琥珀酸，己二酸，辛二酸，十四烷-1，14-二酸和16烷-1，16-二酸）的酯类也是有用的。
本发明用的聚醚多醇或聚氧化烯多醇的例子是由环氧乙烷、环氧丙烷、1-2或2-3环氧丁烷得到的多醇。上述氧化物可单独聚合（即均聚合），也可混合聚合（即共聚）。氧化物也可以以无规或嵌段的形式结合。虽然上述某些化合物可具有亲水性，但优先选用疏水性化合物，例如由环氧丙烷、环氧丁烷或其混合物衍生的化合物。
合适的封端聚氧化烯二醇的例子是由环氧乙烷、环氧丙烷和环氧丁烷衍生的物质，其中烯化氧以公知方式用具有1～8个活性氢的化合物引发。端羟基可进一步与烷基卤反应生成烷基封端的聚氧化烯二醇。这些聚醚多醇及其制备方法是公知的，参见“聚氨酯”一书（Saunders和Frish著，Interscience        Publishers出版，1962年，33～39页）。
用于制备上述聚醚多醇的合适的引发剂化合物的例子是具有1～8个活性氢的化合物，如水、甲醇、乙醇、丙醇、丁醇、乙二醇、丙二醇、丁二醇、1，6-己二醇、甘油、三羟甲基丙烷、季戊四醇、多胺，山梨醇、蔗糖和它们的混合物。
其它有用的引发剂化合物包括一元酚和二元酚及其烷基化衍生物，如苯酚、邻-、间-和对间苯甲酚、邻甲氧基苯酚、水扬醇、香芹酚、百里酚、邻-和对-羟基联苯、邻苯二酚、间苯二酚、氢醌、焦棓酚和间苯三酚。
其它有用的引发剂化合物包括氢、乙二胺、氨乙基乙醇胺、N-氨乙基哌嗪、二亚乙基二胺和三亚乙基四胺。
前述聚醚多醇的数均分子量应为400～5000，最好是500～1500。
共混前述聚醚多醇，以得到分别含5～95%（重量）的酯和95～5%（重量）的多醇、最好是70～90%多醇和30～10%酯的基础润滑剂组合物。
优选的聚醚多醇以选自甘油和乙二胺的引发剂为基础，优选的酯是C7～9链烷酸混合物的季戊四醇四酯。
本发明的成品润滑剂组合物可含有有效量的无灰添加剂，如抗氧基、缓蚀剂、金属减活剂、润滑添加剂、粘度指数改进剂和特压剂（视情况加以选择）。
本发明可以使用的有效的无灰抗氧剂的例子是苯基萘胺，即α-和β-萘胺;二苯胺;亚氨基二苄;对，对-二丁基-联苯胺;对，对′-二辛基联苯胺;以及它们的混合物;其它合适的抗氧剂是受阻酚类，如6-叔丁基苯酚、2，6-二叔丁基苯酚和4-甲基-2，6-二叔丁基苯酚。
合适的无灰金属缓蚀剂的例子是市售的产品，如N-油酰肌氨酸和Ciba-Geigy出售的Irgalube（磷酸-己酯的脂肪胺盐）。其它有效的金属缓蚀剂分别是White化学公司出售的NA-SUL        DTA和NA-SUL        EDS（二亚乙基三胺二壬基萘磺酸盐和乙二胺二壬基萘磺酸盐）。
合适的无灰亚铜金属减活剂的例子是咪唑、苯并咪唑、吡唑、苯并三唑、甲苯并三唑、2-甲基苯并三唑、3，5-二甲基吡唑和亚甲基双-苯并三唑。
致冷剂组合物用的前述添加剂的有效用量一般为：抗氧剂0.1～5.0%（重量），缓蚀剂0.1～5.0%（重量），金属减活剂0.001～5%（重量）。上述重量百分比是以聚醚多醇和酯的总重量计。可以理解，根据最终组合物所用的环境，添加剂的用量可以更多或更少。
用于本发明的致冷剂的例子是含氢氯氟烃，如氯二氟甲烷，氯氟甲烷，2，2-二氯-1，1，1-三氟乙烷，1-氯-2，2，2-三氟乙烷，1，1-二氯-1-氟乙烷、2-氯-2，2-二氟乙烷、1-氯-1，2，2，2-四氟乙烷和2-氯-1，1，2，2-四氟乙烷。
用于本发明的含氢氟烃致冷剂的例子是1，1，1，2-四氟乙烷，1，1，1-三氟乙烷，2，2-二氟乙烷，三氟甲烷，二氟甲烷，一氟甲烷，二氟乙烯、五氟乙烷和1，1，2，2-四氟乙烷。
表Ⅱ给出了本发明用致冷剂R134a（1，1，1，2-四氟乙烷）的几个例子。表Ⅰ给出了用致冷剂R134a（1，1，1，2-四氟乙烷）的几个对照。表Ⅲ示出了本发明用其它致冷剂（如R1416，R22和R123）的情况。
制备对照及实例的一般工序如下。混合经选择的多醇和酯并进行真空汽提。将玻璃安瓶用丙酮洗涤并于110℃真空干燥。将空安瓶或管子称重，并将待评价的混合物注射到管中。将管子重新称重以测定润滑剂的量。将管子抽真空以除去空气，然后浸入于Dewar烧瓶中的干冰/二氯甲烷中。将R134a在8Psig（56Mpa表压）的压力下移入管子中以得到所需润滑剂浓度。然后，将填充的安瓶分离并允许在室温（25℃）下平衡。将安瓶放在可控温度浴中，温度从-20～变化到85℃，同时观察相分离情况。相分离温度称作上溶液临界温度（USCT），以0℃表示。因玻璃安瓶设备的压力所限，不研究85℃以上的温度。USCT这种温度测定限度的体系注明高于85℃。
表Ⅰ        R134a上溶液临界温度数据
实验编号        润滑剂/净粘度        润滑剂        USCT
wt%
cs 于100°F或38℃（m2/s）（于R134a中） ℃
对照A        100Mobil        p51        25        80
（C7-9链烷酸混合物的季戊
四醇四酯）
25（25×10-6）
对照B        100Mobil        p41        16        ＞83
（三羟甲基丙烷三庚酸酯）
15（15×10-6）
对照C        100Emery        2914-D        15        ＞85
（壬二酸二甲酯）
3（3×10-6）
表Ⅰ        R134a上溶液临界温度数据
实验编号        润滑剂/净粘度        润滑剂        USCT
wt%
cs 于100°F或38℃（m2/s）（于R134a中） ℃
对照D        100L-1150        16        60
（正丁醇+PO至1150分子
量）
57（57×10-6）
对照E        100P-1000        25        70
（丙二醇+PO至1000分子量）
73（73×10-6）
对照F        100P-2000        12        ＜25
（丙二醇+PO至2000分子量）
160（16×10-5）
对照G        70/30        P2000/P425        15        45
（正丁醇+PO至425分子量）
95（95×10-6）
对照H        70/30L-1150/EMery        2914D        11        ＞70
20（2×10-5）
对照I        70/30        P-2000/Mobil        p51        13        ＜35
87（87×10-6）
对照J        30/70P-2000/Mobil        P41        20        80
40（40×10-5）
表Ⅰ表明，酯和多醇本身不具有所要求的粘度或USCT。对照H，I和J表明，甚至某些多醇/酯共混物也不具有所要求的有效粘度。
表Ⅱ        R134a上溶液临界温度数据
实验编号        润滑剂/净粘度        润滑剂        USCT
wt%
cs 于100°F或38℃（m2/s）（于R134a中） ℃
实例1        90/10        cp700（甘油+PO至        9        ＞85
700分子量）
Mobil        P51
89（89×10-6）
实例2        90/10        cp700/Mobil        p51        12        ＞85
89（89×10-6）
实例3        90/10        cp700/Mobil        P51        17        80
89（89×10-6）
实例4        90/10        cp700/Mobil        P51        22        80
89（89×10-6）
实例5        75/25        EDA511（乙二胺+PO        8        ＞80
至511分子量）/MobilP41
203（203×10-6）
实例6        75/25        EDA511        Mobil        P41        19        ＞83
203（203×10-6）
实例7        75/25        EDA511        Mobil        P41        29        ＞85
203（203×10-6）
表Ⅱ        R134a上溶液临界温度数据
实验编号        润滑剂/净粘度        润滑剂        USCT
wt%
cs 100F或38℃（m2/s）（于R134a中） ℃
实例8        75/25        EDA511        Mobil        P51        9        ＞85
245（245×10-6）
实例9        75/25        EDA511        Mobil        P51        11        ＞85
245（245×10-6）
实例10        75/25        EDA511        Mobil        P51        20        ＞85
245（245×10-6）
实例11        70/30        cp        1406（甘油+po        18        65
至1406分子量）
78（78×10-6）
表Ⅲ        R134a上溶液临界温度数据
实验编号        润滑剂/净粘度        润滑剂        USCT
wt%
cs 于100°F或38℃（m2/s）（于R134a中） ℃
用R141b        75/25        EDA511/Mobil        P51        22        ＞65
的实例12 245（245×10-6）
用R22的        75/25        EDA511/Mobil        P51        18        ＞65
实例13 245（245×10-6）
用R123        75/25        EDA511/Mobil        P51        18        ＞65
的实例14 245（245×10-6）

Claims (10)

1、一种润滑剂组合物，它在-20℃～65℃以上的温度下能混溶于含氢氟烃和含氢氯氟烃致冷剂，于38℃粘度高于75厘(75×10-6m2/s)，该润滑剂组合物包括：
(A)95～5%的聚醚多醇，其分子式为
其中z是具有1～8个活性氢的化合物基，
R是氢、乙基，或它们的混合物，
n为0或-正数，
m是-正数，
m+n值能使聚醚多醇具有400～5000的数均分子量，
R是氢或C1-6烷基，
P是一整数，其值等于Z的活性氢数，和
(B)5～95%的酯，选自
(1)由多元醇与链烷酸制成的酯，和
(2)由链烷二酸与烷醇制成的酯。
2、一种润滑剂组合物，它在-20℃～65℃以上的温度下能混溶于含氢氟烃和含氢氯氟烃致冷剂，于38℃粘度高于75厘（75×10-6m2/s），该润滑剂组合物包括：
（A）95～5%聚醚多醇，其分子式为
其中
Z是具有1～8个活性氢的化合物基，
n是一个数，其平均值能使聚醚多醇具有400～5000的数均分子量，
R是氢或C1-6烷基，
p是一整数，其值等于Z的活性氢数，和
（B）5～95%的酯，选自
（1）由多元醇与链烷酸制成的酯，和
（2）由链烷二酸与链烷醇制成的酯。
3、按照权利要求2所述的润滑剂组合物，其中聚醚多醇以选自甘油和乙二胺的基团为基础且酯是C7-9链烷酸混合物的季戊四醇四酯。
4、用于压缩致冷的流体组合物，包括
（A）一种选自含氢氯氟烃和含氢氟烃的致冷剂，和
（B）一种按权利要求1或2所述的润滑剂组合物。
5、按照权利要求4所述的组合物，其中所述流体组合物含有浓度为1～30%（重量）的润滑剂组合物。
6、按照权利要求4所述的组合物，其中所述含氢氯氟烃选自氯二氟甲烷，氯氟甲烷，2，2-二氯-1，1，1-三氟乙烷，1-氯-1，2，2，2-四氟乙烷，2-氯-1，1，2，2-四氟乙烷，1-氯-2，2，2-三氟乙烷，1，1-二氯-1-氟乙烷和2-氯-2，2-二氟乙烷，所述的含氢氟烃选自1，1，1，2-四氟乙烷，1，1，2，2-四氟乙烷，1，1，1-三氟乙烷，2，2-二氟乙烷，三氟甲烷，二氟甲烷，一氟甲烷，二氟乙烷和五氟乙烷。
7、按照权利要求4所述的组合物，其中所述含氢氟烃是1，1，1，2-四氟乙烷。
8、按照权利要求4所述的组合物，其中聚醚多醇以选自甘油和乙二胺的基团为基础且酯是C7～9，链烷酸混合物的季戊四醇四酯。
9、一种制备润滑剂组合物的方法，该组合物能在-20℃-65℃以上混溶于含氢氟烃和含氢氯氟烃致冷剂，且于38℃粘度高于75厘沲（75×106m2/s），该方法包括混合（A）和（B）：
（A）95～5%的聚醚多醇，其分子式为
其中Z是具甘1～8个活性氢的化合物基，
R是氢、乙基，或它们的混合物，
n为0或一正数，
m是一正数，
m+n值能使聚醚多醇具有400～5000的数均分子量，
R是氢或C1～6烷基，
p是一整数，其值等于Z的活性氢数，和
（B）5～95%的酯，选自
（1）由多元醇与链烷酸制成的酯，和
（2）由链烷二酸与烷醇制成的酯。
10、一种制备润滑剂组合物的方法，该组合物能在-20℃～65℃以上混溶于含氢氟烃和含氢氯氟烃致冷剂，且于38℃的粘度高于75厘沲（75×106m2/s），该方法包括混合（A）和（B）：
（A）95～5%聚醚多醇，其分子式为
其中
Z是具有1～8个活性氢的化合物基，
n是一个数，其平均值能使聚醚多醇具有400～5000的数均分子量，
R是氢或C1～6烷基，
p是一整数，其值等于Z的活性氢数，和
（B）5～95%的酯，选自
（1）由多元醇与链烷酸制成的酯，和
（2）由链烷二酸与链烷醇制成的酯。
CN90100090A 1989-01-10 1990-01-09 致冷压缩机用润滑油 Pending CN1044492A (zh)

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CA2007374A1 (en) 1990-07-10
ATE109500T1 (de) 1994-08-15
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CA2007374C (en) 2000-10-10
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AU630401B2 (en) 1992-10-29
DE69011135T2 (de) 1994-12-01
MY105235A (en) 1994-08-30
DK0378176T3 (da) 1994-08-29
NO900089D0 (no) 1990-01-09
JPH02276894A (ja) 1990-11-13
ZA90175B (en) 1991-09-25
AU4782590A (en) 1990-07-19
US4851144A (en) 1989-07-25
KR0157627B1 (ko) 1999-02-18
KR900011884A (ko) 1990-08-02

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