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CN1047525A - 用于制冷的组合物和方法 - Google Patents

用于制冷的组合物和方法 Download PDF

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Publication number
CN1047525A
CN1047525A CN90103760A CN90103760A CN1047525A CN 1047525 A CN1047525 A CN 1047525A CN 90103760 A CN90103760 A CN 90103760A CN 90103760 A CN90103760 A CN 90103760A CN 1047525 A CN1047525 A CN 1047525A
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Prior art keywords
composition
oil
hfc
fluorine
viscosity
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托马斯·迈克尔·迪斯
乔治·基思·亨利
希瑟·李·伯格曼
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EIDP Inc
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EI Du Pont de Nemours and Co
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Publication of CN1047525A publication Critical patent/CN1047525A/zh
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Abstract

公开了一种用于压缩制冷的混合物，该混合物由制冷剂和至少一种氟化烃构成，氟化烃中氟/碳重量比约为0.5至5，其100的SUS粘度至少为50，倾点低于约-20℃。

Description

本发明涉及与制冷剂一起用于压缩制冷和空调系统的润滑剂。更具体地说，本发明涉及与有1-4个碳原子的饱和烃一起使用的润滑剂，饱和烃被至少一个氯或氟原子部分或全部取代，其标准沸点为-80℃至+50℃。本发明具体涉及与四氟乙烷（例如1，1，1，2-四氟乙烷（HFC-134a）和1，1，2，2-四氟乙烷（HFC-134）等）、其次与五氟乙烷（HFC-125）一起使用的润滑剂。这些化合物被当作二氯二氟甲烷（CFC-12）的替换品，尤其是在汽车空调系统中。本发明的润滑剂不仅在汽车空调系统的整个运行温度范围内都与HFC-134a等完全混溶，而且在此温度范围内也与CFC-12完全混溶。因此，在从CFC-12向HFC-134a过渡期间，它们可以与CFC-12一起在同一系统内使用。
用CFC-12作制冷剂的制冷系统通常用矿物油来润滑压缩机（例如见1980        ASHRAE系统手册第32章中的讨论）。在制冷系统的整个温度范围，即-45℃至65℃，CFC-12与上述矿物油完全混溶。在汽车空调中，与CFC-12一起使用的常常是100°F的粘度约为500        SUS（赛波特通用秒数）的石蜡油和环烃油。这些油的“倾点”低于-20℃，210°F的粘度约为55        SUS，并且在-10℃至100℃的温度范围内与CFC-12制冷剂完全混溶。因此，溶在制冷剂中的油流过空调系统中的制冷回路并与制冷剂一起返回到压缩机。虽然由于制冷剂的蒸发造成的低温可能使油聚集，但在冷凝期间它并不分离。与此同时，润滑压缩机的这种油会含有一些制冷剂，这可能会影响其润滑性质。
当在这些制冷系统中用HFC-134a或HFC-134代替CFC-12时，最好是能使用与CFC-12一起用的同一种油。这样就不需要设备有重大的变动，系统所使用的条件也无需大的改变。如果在系统运行期间润滑剂与制冷剂分离，可能会产生严重问题，即，压缩机可能润滑不足。这在汽车空调系统中可能最为严重，因为压缩机不是分开润滑，制冷剂与润滑剂的混合物在整个系统内循环。但是遗憾的是，矿物油与四氟乙烷基本上不混溶。
ASHRAE的两份最近的出版物讨论了与润滑剂和制冷剂分离有关的问题。它们是kruse和Schroeder的“制冷系统和热泵中润滑的基础”，登载在ASHRAE        Transactions第90卷，Part2B，763-782页（1984年）;和Spauschus的“制冷和空调压缩机用润滑剂的评价”，刊登在上述刊物同一期的784-798页。
总之，在混合物组成和操作温度的整个范围内与油不完全混溶的制冷剂，随着温度从室温升高或降低，可能会变得混溶或不混溶。不混溶区域可能呈现各种形状，即抛物线形或非抛物线形。作为抛物线，混溶温度对混合物中油百分含量的曲线可能将其开口或凹下部分朝向低温或高温。抛物线的闭口或凸出部分则分别代表最高或最低温度，高于或低于该温度时制冷剂与润滑油完全混溶。这些温度称作最高或最低“会溶温度”。除抛物线外，这些曲线可能呈歪斜的抛物线形，或是斜率变化的曲线，在曲线之上或之下发生不混溶现象。
本发明的目的之一是提供一种润滑油与四氟乙烷等制冷剂（例如HFC-134a）的组合，使混溶区包括在压缩制冷中遇到的整个温度和组成范围，即，在-45℃到至少20℃、最好是到HFC-134 a的临界温度100℃，所有组合物都完全混溶。另一目的则是提供在压缩制冷中使用上述组合物的方法。
授与日本油脂公司等的美国专利4，248，726（1981年2月5日颁布）和美国专利4，267，064（1981年5月12日）提到用聚二元醇油，例如粘度指数至少为150的聚丙二醇（或其烷基醚）和缩水甘油醚型环氧化合物作为供含卤制冷剂用的高粘冷冻油组合物。所公开的这些聚二醇/缩水甘油醚组合物可与氟利昂11、12、13、22、113、114、500和502一起使用;与氟利昂12或22一起用“特别有效”。杜邦公司标题为“冷冻油”的《研究公开》17486号公开了将聚（亚烷基）二醇，例如联合碳化物公司出售的Ucon        LB-165和Ucon        LB-525，与HFC-134a一起使用。这些二醇是聚丙二醇，它们是单官能的，由氧化丙烯用正丁醇引发制备。该文指出，这些油与制冷剂的组合物在至少低至-50℃的温度在所有的比例下都相混溶，并且在175℃在钢、铜和铝存在下大约六天内都是热稳定的。美国专利4，755，316（1988年7月5日颁发给Allied-Signal公司）也提到使用聚（亚烷基）二醇。但是这些二醇就羟基而言至少是双官能的，总量中至少有80%的氧化丙烯单元，剩下的20%可以是由氧化乙烯、氧化丁烯或能与氧化丙烯聚合的酯、烯烃等衍生得到。应该注意，该专利中只举例说明了双官能聚（亚烷基）二醇含100%氧化丙烯单元的情形。
本发明是基于以下的发现：使用数量上足以润滑（用于汽车时通常为10-20%（体积），在某些情形可高达50%（体积））的至少一种氟化烃（饱和的或不饱和的），在从-40℃到至少20℃，最好是到100℃（HFC-134a的临界温度）的温度范围内，可以和四氟乙烷与五氟乙烷完全混溶，通常是80-90%（体积）的四氟乙烷（HFC-134与HFC-134a）、五氟乙烷（HFC-125）及其它的1-4碳原子的饱和烃或其混合物，该饱和烃被至少一个氯或氟原子部分或全部取代，其标准沸点为-80℃至+50℃。作为润滑剂的氟化烃，其氟碳重量比是约0.5至5，100°F的SUS粘度至少为50，倾点小于约-20℃，此后称其为“HFC油”。
优选的HFC油包括Rf（CH2）nCH＝CH2的聚合物以及Rf（CH2）nCH＝CH2与各种乙烯基化合物（例如丁基乙烯基醚、丙烯腈等）的共聚物，其中“Rf”可以是从CF3-至C10F21-或者更高的任一基团，最好是C6F13-、C8F17-、C10F21-和更高级的基团;n＝0-2，但最好是n＝1。属于这一类的一种特别有用的HFC油是“Rf”中60%为C6F13-、30%为C8F17-、剩下的为C10F21-和更高级的碳氟基，而且n＝1。还发现这些优选的HFC油在CFC、特别是在CFC-12中完全混溶。
本发明中另一类可与四氟乙烷一起使用的HFC油是六氟丙烯或类似的全氟化碳在长链脂族烃（C8或更高）上的接枝产物。在以H·Cripps的名义提交的美国专利申请CH-1686中提到了这些化合物。
制冷剂与润滑剂（HFC油）的重量比可以从99/1至1/99，最好是从99/1至70/30之间的任一数值。这些油的100°F下的粘度可以从50至3000        SUS，但对于大多数商业用途是从100至1200SUS。
已知使用适量的“特压（EP）添加剂”能改善油的润滑性能和载荷特性，从而提高制冷剂-润滑剂组合物的质量。可用于本发明的EP添加剂包括在美国专利4，755，316的表D中公开的添加剂中。较好的是一种有机磷酸酯SYN-O-AD8478，它是三（2，4，6-三叔丁基苯基）磷酸酯/磷酸三苯酯的70%/30%混合物，由Stauffer化学公司生产。
EP添加剂也可以与美国专利4，755，316的表D中公开的某些抗磨添加剂、氧化及热稳定性改进剂、腐蚀抑制剂、粘度指数改进剂、洗涤剂和消泡剂一起使用。这些添加剂也可以部分或全部氟化。
最佳实施例的描述
如前所述，四氟乙烷（例如HFC-134a、HFC-134）和五氟乙烷（HFC-125），特别是HFC-134a，其物理特性使得它们可以替代CFC-12，而压缩制冷设备只需作微小变动。它们可以彼此混合，也可与其它制冷剂混合，其它制冷剂包括CFC-12（CCl2F2）、HCFC-22（CHClF2）、HFC-152a（CH3CHF2）、HCFC-124（CHClFCF3）、HCFC-124a（CHF2CClF2）、HCFC-142b（CH3CClF2）、HFC-32（CH2F2）、HFC-143a（CH3CF3）、HFC-143（CHF2CH2F）、和FC-218（CF3CF2CF3）;对于本发明来说，不排除这些混合物。但是，在四氟乙烷或五氟乙烷与其它制冷剂的混合物中，只包括那些在-40℃至约+20℃的范围内与本发明的润滑剂相混溶的混合物。
HFC-134a是优选的四氟乙烷制冷剂，可用先有技术中公开的任何方法制备，例如见美国专利2，745，886;2，887，427;4，129，603;4，158，675;4，311，863;4，792，643和英国专利1，578，933和2，030，981。
优选的HFC油是Rf（CH2）nCH＝CH2的聚合产物，其中Rf基的碳原子数为2至20，最好是6至10，n为0或1。这一类化合物中最好的是其中的Rf＝C6F13（60%）、C8F17（30%）、剩下的为C10F21和更高级的碳氟基，n＝0或1。
这些化合物可以用美国专利4，606，832、4，668，749和4，673，712中公开的任何一种方法制备。一种采用过氧化物引发剂的聚合方法较好，其反应温度在50℃至200℃之间。
这些HFC油的粘度范围可以从100°F下的50至3000        SUS变化。另外，其单体可以和多种乙烯基化合物共聚以改善其润滑性质，这些乙烯基化合物包括但不局限于乙烯基醚、丙烯酸酯、甲基丙烯酸酯、丙烯腈、乙烯基乙氧基化物或卤化的单体。HFC油可以和其它润滑剂（例如全氟化碳）混合，以调节粘度和/或润滑性质。
具体地说，在本发明组合物和在为压缩制冷和空调设备提供润滑的本发明方法中使用的润滑剂具有以下特点：
100°F下的粘度
50至3000        SUS，最好是100至1200        SUS，具体对于汽车空调为约500        SUS。
倾点
＜-20℃，对于100        SUS和500        SUS油，最好分别是从-20℃至约-50℃和-20℃至-30℃。
溶解度或混溶范围
从100℃至下述温度100%混溶：（a）对于1-99%（重量）HFC-134a与100°F粘度为50        SUS至2500        SUS的HFC润滑剂的混合物，低于-40℃;（b）对于优选的二乙烯基醚共聚物，低于-30℃;（c）对于优选的520        SUS混合物，低于-35℃。
四球磨损试验
用一组特定的钢球。磨痕和摩擦系数等于或略高于目前在汽车空调系统中与CFC-12一起使用的油，即，当用CFC-12在大气压下饱和时磨痕为0.37毫米，摩擦系数为0.07。
“法列克斯”（破坏负荷试验）
用特定类型的钢制作三角滑块和针。破坏负荷等于或大于CFC/冷冻油组合物的值，即，当用CFC-12在大气压下饱和时为1300磅。
1.制冷剂在润滑剂中的溶解度
在溶解度试验中用6毫升制冷剂和润滑剂的混合物。混合物通常含30、60、和90%（重量）的制冷剂。将这些无空气的混合物装在封口Pyrex玻璃管（内径7/16英寸，长5.5英寸，容量约12.5毫升）中。测定制冷剂/润滑剂溶解度时将试管完全浸在各试验温度的浴中至少15分钟，并搅动以促进混合和平衡。确定制冷剂/润滑剂混合物变成混溶或不混溶时的温度，测量精度约为±2℃。当混合物出现并保持“条纹”线、形成絮块、或形成两液体层时，称其为不混溶。这些溶解度试验在93℃至-50℃范围进行。因安全原因不在93℃以上作试验。假定HFC-134a/油的混合物若在93℃时溶解，则在HFC-134a的临界温度100.5℃也仍然溶解。
2.制冷剂和润滑剂的稳定性
将3毫升制冷剂和0.3毫升润滑剂与试件（钢1010/铜/铝1100，2 3/8 英寸×1/4英寸×1/16英寸，120号粒度表面光洁度）在无氧条件下装入Pyrex试管（内径7/16英寸，高5.5英寸，体积约12.5毫升）中并封口。试样的顶端用铜丝捆在一起，金属之间用铜丝环在顶端分开。将试管在268℃垂直贮存11.8天。然后检查管内物品的外观变化。再将制冷剂转移到气体取样球管中，用气相色谱法分析制冷剂的分解产物，即HFC-143（HFC-134a的分解产物）或HCFC-22（CFC-12的分解产物）。然后将这些结果按照所产生的HF和HCl换算为各自的当量。
3.润滑性
a.四球磨损试验
在ASTM        D4172中详细叙述了试验步骤。将该方法作如下修改：将20千克的负荷于1200转/分下施加在52100号钢球上，钢球浸在10毫升润滑剂中。将制冷剂（HFC-134a或CFC-12）经过一根聚四氟乙烯毛细管以0.75标准立方英尺/小时的速度通入润滑剂中，以便在润滑剂上提供一个大气压的制冷剂气体，产生气体饱和的润滑剂。
b.法列克斯针/三角滑块负荷破坏试验
在ASTM        D3233中详细叙述了试验步骤。三角滑块由AISIC-1137号钢制成（洛氏硬度C-20至24，表面光洁度5至10微英寸）。试验针由AISI        3135号钢制成（洛氏硬度B-87至91，表面光洁度5至10微英寸）。象在“四球磨损试验”中一样，将制冷剂气体通入油中进行试验。
4.粘度和粘度变化率
a.粘度是决定流体对剪切力的阻力的一种性质。根据测量的方法，粘度可以用绝对粘度、运动粘度或赛波特秒数通用粘度（SSU）来表示。根据ASTM        D-445中的表，可以容易地将SSU转换为平方毫米/秒（厘沲），但要将运动粘度转换为绝对粘度则必须知道密度。冷冻油是按粘度等级销售的，ASTM已提出一个供工业使用的标准化粘度等级体系（D-2422）。
粘度随温度升高而减小，随温度降低而增加。温度与运动粘度之间的关系用下式表示：
loglog（V+0.7）＝A+BlogT（公式1）
其中V＝运动粘度（平方毫米/秒，厘沲）
T＝热力学温度（开尔文）
A、B＝各个油的常数
此关系式是ASTM发表的粘度温度图的基础，它可在很宽的温度范围内得到粘度的直线图。在油是均相液体的温度范围内可应用此图。
b.粘度变化率是温度变化造成的油的粘度改变量的量度。此比值为上述式1中的“B”，不同的油通常有不同的粘度变化率。
5.倾点
任何打算在低温下使用的油应该在可能遇到的最低温度下仍能流动。测定倾点的步骤见ASTM        D-97。
参照以下实例和对照例将会更清楚地了解本发明。
实例1HFC油
本实例代表了用于制备优选的HFC油，即Rf-（CH2）CH＝CH2的聚合产物，以及在压缩制冷中它与HFC-134a一起使用的已知最佳方式。具体地说，制备这种HFC油时将100克Rf（CH2）CH＝CH2加到反应容器中，将容器加热至110℃并用氮气喷洗1小时。取下喷洗装置，换上氮气头。将12.5克碳酸叔丁基过氧异丙基酯（在一种沸程为150-200℃的溶剂油中的75%溶液）一次加到反应器中的溶液里。溶液随后在110℃加热约18小时。用1HNMR监测反应，直到σ5和6ppm之间的烯烃峰消失。将容器冷却，真空蒸馏，在釜温60℃和10托的压力下除去挥发物。所得的90-100克黄色液体经分析为前述的Rf（CH2）CH＝CH2聚合产物：
Figure 901037605_IMG1
其中Rf＝（CF2）yF，Y＝6（60%）、8（30%）、10及更高（10%）。
产物的1H-NMR光谱分析表明原料的化学位移消失，而形成产物的宽多重峰。原料有以下谱线：6.0-5.7（m，1H）;5.6-5.3（m，2H）;3.05（三重峰中的双峰，2H，J＝20HZ，J＝6.6HZ）。产物在3.0至0.9ppm之间给出宽多重峰。红外分析表明在3050-2850cm-1（CH＝CH2，和CH2的伸张振动）和1400-1000cm-1（CF2伸张振动）有吸收。13C-NMR显示出产物在123至19ppm的范围内的几个峰，但是明显地没有与原料单体对应的在126（三重峰）和123ppm的峰。用气相渗透计法测得平均分子量为3200。
产物的100°F粘度及倾点分别为1000SUS和低于-20℃。改变工艺变量使100°F粘度为440至2540        SUS。因为后一种油在210°F的粘度为99.6        SUS，所以粘度变化率（公式1）为-4.14。这优于在汽车空调中与CFC-12共用的环烷油的变化率-4.23。这种油的倾点为-23℃，40℃和100℃的粘度分别为525        SUS和55SUS。
这些低粘度至高粘度的HFC油，从至少-40℃到溶解度试验中采用的最高温度93℃，均与HFC-134a完全混溶。在高粘度油中加入1.3%（重量）SYN-O-AD        8478        EP添加剂将最低混溶温度从-40℃升至-35℃。SYN-O-AD是Stauffer化学公司的产品。另外，因为CFC-12在从-40℃至93℃也完全混溶，所以HFC油可以互换地用于压缩制冷系统。
在表Ⅰ和Ⅱ对照例中提到的其它商品油或试验性油，缺乏作 为合格的汽车空调系统润滑剂所要求的溶解性（从-10℃至100℃完全混溶）。表Ⅱ包括目前在汽车空调中与CFC-12一起使用的Suniso        5GS环烷油和BVM-100N石蜡油。
表Ⅲ和Ⅳ列出了用“四球磨损试验”、“法列克斯”针/三角滑块试验、负荷破坏试验对本实例的HFC油及其它油的润滑性测定结果。HFC油远比目前与CFC-12一起用于汽车空调的环烷油和石蜡油优越。
HFC-134a或CFC-12与HFC油和金属在一起的稳定性也优于环烷油或石蜡油（表Ⅴ）。表中的目测效果等级是：0-无变化，1-极其轻微的、可接受的变化，2-很轻微的、不明确的变化，3-轻微但不合格的变化，4-中等不合格的变化，5-显著变化。
实例2-HFC油单体/丁基乙烯基醚（BVE）共聚物
本实例涉及共聚物HFC油，即Rf-CH＝CH2与nC4H9OCH＝CH2的共聚产物的制备和它与HFC-134a一起在压缩制冷系统中的使用。
具体地说，制备共聚物HFC油的方法是，在反应容器中加入70-95克Rf-CH＝CH2和30-5克丁基乙烯基醚，然后重复实例1的步骤。
产物的1H-NMR光谱分析表明，与烯属质子相应的化学位移（6.5-5.0ppm）消失，谱图中在3.0-1.0ppm之间出现宽峰。13C NMR在123和19ppm之间显示出产物的峰。另外，相应于RfCH＝CH2的原料烯烃峰，即127（三重峰）和126（三重峰）ppm的峰消失。红外光谱在3000-2850cm-1（CH2伸张）与1400-1000cm-1（CF2伸张）显示有吸收。
表Ⅵ列出了油的粘度范围和这些油在HFC-134a中的溶解度。丁基乙烯基醚在共聚物中可接受的组成范围是约1至30%（重量），最好是约1至10%（重量）。
不同粘度的HFC油可以混合，以调节成种种居中的粘度值。也可以将HFC油与其它油相混合以得到特定的粘度，尤其是如果第二种油也在HFC-134a中完全溶解时。第二种油的具体实例是1，1，1，2，2，3，3，4，4，5，5，6，6-十三氟-7-十六碳烯（TDFH），它的100°F粘度为34        SUS，倾点为-17℃，从93至-17℃在HFC-134a中完全混溶。实例1的100°F粘度为1800        SUS的HFC油与TDFH油的混合物（其中TDFH占9.1%重量），在100°F和210°F的粘度分别为520        SUS和55        SUS。这样得出的粘度变化率为-4.21，优于在汽车空调中与CFC-12一起使用的环烷油（变化率-4.23）。它的溶解度特性列在表Ⅶ，表明它从93℃到至少-35℃是混溶的。
配制一个HFC油/TDFH为89.3/10.7（重量）的混合物，其100°F的粘度为525        SUS，试验其润滑性能。表Ⅷ表明，当用制冷剂在大气压下饱和时，此混合物在四球磨损试验中不比对照油优越，但在法列克斯试验中则优于对照样品。加入特压添加剂能提高头一种试验的结果。
可以与HFC油混合的其它油类是部分或完全氟化的烃类。
表1
HFC-134a与商品氟化油的溶解度
（试验范围93℃至-50℃）
实验        对于所示HFC-134a浓度（重量%）的混溶范围（℃）
编号        润滑剂        30%        60%        90%
对照A        Halocarbon        700/95的        93至8        93至7        93至-4
6.7/93.3（重量）混合物
（a），500        SUS
对照B        Krytox        GPL混合物（b，        93至0        93至10        93至20
c），150        SUS
对照C        Krytox        GPL混合物（b，        93至10        93至20        93至20
c），480        SUS
对照D        Fomblin        Y25/5（b，d），        93至5        93至15        93至15
417        SUS
对照E        Fomblin        Z-15（b，d），        93至5        93至28        75至28
417        SUS
对照F        Demnum        S-65（b，d），        93至15        93至22        93至22
300        SUS
a-聚氯三氟乙烯油，Halocarbon        Products公司产品。
b-全氟化聚烷基醚油
c-杜邦公司的产品
d-Montedison集团Montefuos分公司的产品
e-Daikin工业公司的产品
表Ⅱ
HFC-134a与现有的各种冷冻机油的溶解度
对于所示的HFC-134a在润滑剂中的浓度（重量%）的混溶范围（℃）
实验编号        脂肪酸的双戊赤藓醇酯（c）        30%        60%        90%
对照G        240SUS        -50+        -4+        40+
对照H        290        SUS        -44+        -17+        70+
脂肪酸聚乙二醇酯（d）
对照I        144        SUS        -21+        54（a）        54（a）
对照J        620        SUS        -4+        4+        70+
对照K        830        SUS        -6+        70+        70+
环烷油（e）
对照L        Suniso        5GS（500        SUS，38%        54（a）        54（a）        54（a）
芳族）
对照M        Witco        500（500        SUS）        54（a）        54（a）        54（a）
对照N        实验油（520        SUS，47%        54（a）        54（a）        54（a）
芳族）
对照O        实验油（529        SUS，75%        54（a）        54（a）        54（a）
芳族）
石蜡油（f）
对照P        BVM-100N（500        SUS）        54（a）        54（a）        54（a）
烷基苯
对照Q        Zerol        300（300        SUS）（g）        54（a）        54（a）        54（a）
对照R        DN600（125        SUS）（h）        54（a）        54（a）        54（a）
对照S        Almos        HAB        15F（78SUS）（i）        55+        在（b）内        在（b）内
硅油
对照T，u，V        L-45油（163，231和462        SUS）（j）
+-在所示温度和高于所示温度下溶解
a-可能在高于所示温度的某个温度下溶解
b-从93至-50℃完全不溶
c-Hercules公司产品
d-CPI        Engineering公司产品
e-Witco化学公司产品
f-BVM        Associates产品
g-Shrieve化学公司产品
h-Conoco公司产品
i-日本油脂公司产品
j-联合碳化物公司产品。
表Ⅲ
225°F在一个大气压的制冷剂气体压力下润滑剂在四球
磨损试验中的润滑性能
100°F粘度 球的磨痕※摩擦
实验编号 制冷剂 润滑剂 （SUS） （毫米）（a） 系数※（b）
1 HFC-134a HFC油※※1000 0.221 0.058
2 CFC-12 HFC油※※0.221 0.051
3 无 HFC油※※0.409 0.072
对照X        CFC-12        环烷油        525        0.373        0.072
对照Y        无        环烷油        0.618        0.050
对照Z        CFC-12        石蜡油        500        0.368        0.071
对照A′        无        石蜡油        0.505        0.056
对照B′        CFC-134a        Krytox        143AC        1247        0.511        0.080
对照C′        无        Krytox        143AC        0.336        0.076
a-±0.028标准误差
b-±0.006标准误差
＊-越小越好
＊＊-实例1中制备的HFC油
表Ⅳ
在一个大气压的制冷剂气体压力下，润滑剂
在法列克斯针/三角滑块试验中的负荷能力
100°F粘度        破坏负荷        破坏时的转矩
实验编号        气体        润滑剂（SUS）        （磅）＊        （英寸.磅）＊
4        HFC-134a        HFC油＊＊        1000        2250        34
5        CFC-12        HFC油＊＊        1000        2250        43
6        无        HFC油＊＊        1000        2250        50
对照D′        CFC-12        环烷油        525        1250        24
对照E′        无        环烷油        525        750        13
对照F′        CFC-12        石蜡油        500        1300        26
＊越大越好
＊＊实例1中制备的HFC油
表Ⅴ
HFC-134a在与润滑剂及栓联的钢-1010/铜/
铝-1100在268°F接触11.8天后的稳定性
（近似等于在汽车中用10年）
产生的Cl-或F-＊ 目测的效果等级
实验编号        制冷剂        润滑剂        （ppm）        液体        钢        Cu        Al
7        HFC-134a        HFC油＊＊        ＜0.2＊        0        0        0        0
8        CFC-12        HFC油＊＊        8        0        1（a）        0        1（b）
对照G        CFC-12        环烷油        423        4（c）        3（d）        2（f）        2（g）
对照H        CFC-12        石蜡油        -        0        3（e）0        0
a-极其轻微的变暗-30%液相
b-痕量蚀斑-＜1%表面
c-褐色加中等黑色沉淀
d-褐色沉积物/灰色膜-25%/75%表面加上在液气界面（LGI）处固体的中等沉积物
e-轻微镀铜加灰膜-100%表面
f-深度变暗-25%加上在液气界面处中等沉积物
g-很轻微的腐蚀加上液气界面处中等沉积物
＊        无HFC-134a分解
＊＊        实例1中制备的HFC油
Figure 901037605_IMG2
表Ⅶ
HFC-134a与HFC油/TDFH油（89.3/10.7，重量）的
混合油的溶解度
试验范围：93至-50℃
HFC-134a在        温度范围
试验编号        HFC-134a/油中的重量%        （℃）        情况
13        30        93至-45        轻微发浑
60        93至10        透明溶液
10至-40        轻微发浑
90        93至-38        透明溶液
表Ⅷ
HFC油/TDFH（89.3/10.7，重量）混合物在一大气压的制冷剂气体压力下的润滑性
环烷油
HFC/TDFH油（520        SUS）（a）        （525        SUS）（b）
四球磨损试验        实验编号14        对照I′
磨痕（毫米）（c）        0.510        0.373
摩擦系数（d）        0.075        0.072
法列克斯试验
破坏负荷＊（磅）        1780        1250
破坏时的转矩＊（英寸.磅）        40        24
a-在HFC-134a下
b-在CFC-12下
c-±0.028标准误差
d-±0.006标准误差
＊数字越大越好

Claims (13)

1、一种用于压缩制冷的组合物，它含有：
(a)一种具有1-4个碳原子的饱和烃，它被至少一个氯原子或氟原子部分或全部取代，其标准沸点在-80℃至+50℃的范围；
(b)数量足以起润滑作用的至少一种氟化烃，该烃的氟/碳重量比约为0.5至5，100°F的SUS粘度至少为50。
2、权利要求1的组合物，其中的组分（a）是由1，1，1，2-四氟乙烷、1，1，2，2-四氟乙烷、五氟乙烷、二氯二氟甲烷和三氯三氟乙烷中选择的至少一种化合物。
3、权利要求1的组合物，其中的组分（b）是Rf（CH2）nCH＝CH2的聚合物，其中Rf是CF3-至C20F41-，n＝0-2。
4、权利要求3的组合物，其中的Rf含有约60%的C6F13-，30%的C8F17-，10%的C10F21-和更高级的碳氟基;n＝1。
5、权利要求3的组合物，其中所述的聚合物是Rf（CH2）nCH＝CH2与1-30%（重量）的至少一种共聚单体的共聚物，该单体选自乙烯基醚、丙烯酸酯、甲基丙烯酸酯、丙烯腈及乙烯基乙氧化物。
6、权利要求5的组合物，其中所述共聚单体是丁基乙烯基醚。
7、权利要求3的组合物，其中所述聚合物是Rf（CH2）nCH＝CH2和1-10%（重量）的丁基乙烯基醚的共聚物。
8、权利要求3的组合物，其中的组分（a）是1，1，1，2-四氟乙烷。
9、权利要求7的组合物，其中的组分（a）是1，1，1，2-四氟乙烷。
10、权利要求1的组合物，其中的组分（b）与至少一种氟化烃相混合，该氟化烃的氟/碳重量比约为0.5至5，100°F的SUS粘度至少为50。
11、权利要求3的组合物，其中的组分（b）还含有最高达20%（重量）的1，1，1，2，2，3，3，4，4，5，5，6，6-十三氟-7-十六碳烯。
12、一种适合与饱和烃制冷剂一起用于压缩制冷的润滑剂，所述饱和烃制冷剂含1至4个碳原子，它被至少一个氯或氟原子部分或全部取代，其标准沸点在-80℃至+50℃范围内;所述润滑剂主要由至少一种氟化烃组成，其中的氟/碳比约为0.5至5，其100°F的SUS粘度至少为50，倾点低于-20℃。
13、一种润滑压缩制冷设备的方法，该设备用具有1至4个碳原子的饱和烃作为作为制冷剂，饱和烃被至少一个氯原子或氟原子部分或全部取代，其标准沸点在-80℃至+50℃范围内，所述方法主要包括使用至少一种氟化烃与上述制冷剂的组合物，氟化烃在组合物中占10%-50%（体积），它的氟/碳重量比约为0.5至5，其100°F的SUS粘度为100至1200，倾点低于-20℃。
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ATE99353T1 (de) 1994-01-15
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AU640652B2 (en) 1993-09-02
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US4944890A (en) 1990-07-31
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