CN1337991A - 冷冻润剂组合物 - Google Patents

冷冻润剂组合物 Download PDF

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Publication number
CN1337991A
CN1337991A CN00803148A CN00803148A CN1337991A CN 1337991 A CN1337991 A CN 1337991A CN 00803148 A CN00803148 A CN 00803148A CN 00803148 A CN00803148 A CN 00803148A CN 1337991 A CN1337991 A CN 1337991A
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China
Prior art keywords
lubricant
composition
refrigerant
alkyl
ester
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CN00803148A
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S·科尔
P·T·吉布
S·J·兰德勒斯
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Imperial Chemical Industries Ltd
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Imperial Chemical Industries Ltd
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Publication of CN1337991A publication Critical patent/CN1337991A/zh
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Abstract

本发明公开了一种含抗沉积组分的具有抗沉积作用的润滑剂组合物,其特别适用于冷冻压缩机的润滑并减少或消除在冷冻系统中收缩区域中不想要的沉积物。

Description

冷冻润滑剂组合物
本发明涉及一种润滑剂组合物，更具体地说，本发明涉及一种具有抗沉积作用的润滑剂组合物，其特别适用于对冷冻压缩机进行润滑。本发明还涉及一种冷冻系统，其包含一种冷冻剂和一种润滑组合物，并涉及润滑剂组合物的用途及抑制或除去不想要残余物的方法。
常规冷冻系统一般具有压缩机、冷凝器、膨胀装置和蒸发器，它们联接在一起形成一个回路，其中，冷冻剂循环并连续进行冷凝和蒸发，从而提供冷冻效果。在冷冻系统中可采用各种类型的压缩机，包括往复式压缩机、滚动式压缩机、旋转式压缩机和螺杆式压缩机，可根据具体应用进行选择。压缩机包含在使用过程中被润滑的移动部件。在冷冻系统中的膨胀装置通常包含冷凝剂压缩流动区域，例如可为毛细管或膨胀阀。
不同的材料可用于构造冷冻系统的组件，包括金属和塑料材料。其它材料如油可用于此类系统硬件的装配，冷冻剂加工流体的组分，特别是添加剂有可能进行热分解或水解。在使用过程中及磨损过程中，这些材料可能会存在于冷冻回路中，并通过冷冻剂的流动在系统中以不想要的残余物运送。其它的不想要的残余物也可经对冷冻系统的维护或修理而引入，或者，在使用后，后填加新的冷冻剂或润滑剂至系统中。就特定的塑料材料而言，在冷冻回路中可发现作为不想要的残余物的石蜡材料、聚α烯烃、硅油，特别是高分子量的含碳物质，及非极性材料。这些材料可能会沉积于冷冻系统中，特别是沉积于狭窄区域中，从而引起阻塞及捕集添加剂材料，例如颗粒性材料。由于这些阻塞，可能造成操作性能变差，在极端情形下，会引起系统失效。
通常，有两种类型的冷冻系统。第一种系统中，润滑剂和冷冻剂以混合物存在，并在冷冻系统中循环，例如在自动冷冻系统中循环，第二种系统中，冷冻剂在系统中循环，而润滑剂存在于压缩机的机油箱中，例如开闭式密封压缩机和所谓的工业和商业冷冻机。在第二种情形下，应设计系统避免或至少减少润滑剂从压缩机机油箱中携带进入冷冻回路，虽然在实际使用时，由于润滑剂被夹带进入冷冻剂气体中，这种情形在一定程度上通常还是会发生。一旦润滑剂被带入冷冻回路中，其必然会在系统中转送，并沉积回机油箱中，从而由于可能使机油箱中润滑油水平降低，导致冷冻效率降低。
多年来，碳氯氟化合物如二氯二氟甲烷(R-12)用作冷冻剂，但是，其涉及对臭氧层的破坏。自从1987年蒙特利尔协议以来，这种材料已被逐步淘汰，暂时代之以氢氯氟碳化合物，也被氢氟碳化合物所代替。具体而言，已发现，1，1，1，2-四氟乙烷(R-134a)广泛用作R-12的代用品冷冻剂。HFC和HCFC冷冻剂均包含氢，它们通常比氯氟碳化合物冷冻剂更具有极性。这会进一步加剧由于在冷冻系统中存在不想要的残余物而引起的问题，特别是，当采用HFC冷冻剂时，与CFC冷冻剂相比，这种材料通常在极性冷冻剂中的溶解性更低。
由于在循环冷冻剂中存在外来物质而造成的阻塞问题目前是通过改进膨胀装置的机械设计来解决的，例如，在装置的较冷的部分的毛细管具有较大的直径，从而减少了外来物质沉积的可能。人们还试图减少在生产过程中引入系统中的外来物质的含量。具有全密封压缩机的冷冻系统特别证实了这些由于外来物质存在于压缩机电动机中而引起的问题。这些研究存在当新的制造材料需要采用时需评价和测试冷冻系统的缺陷，因而仅取决了有限的成功。
业已发现，在冷冻系统中加入一种具有抗沉积作用的组分，与不想要残余物存在相关的问题如毛细管阻塞问题可以减少或避免。进而，还发现，具有两亲性质的组分可提供适宜的抗沉积作用。
按照本发明的第一个方面，提供了一种冷冻润滑剂组合物，其包含一种润滑剂和一种两亲性抗沉积组分。
按照本发明的第二个方面，本发明包含一种用于具有含氢冷冻剂的冷冻系统中的冷冻润滑剂组合物，其包含一种合成润滑剂和一种两亲性抗沉积组分。
业已发现，本发明的组合物可增强不想要残余物的传送特性，从而减少沉积和/或有助于除去沉积物，例如，通过将残余物溶解或分散于在冷冻系统中的冷冻剂物流中。
冷冻剂适宜为一种氢氟碳化合物(HCFC)冷冻剂，氢氟碳化合物(HFC)冷冻剂，或至少包含HFC、HCFC之一或两者的冷冻剂。但是，本发明适用于包含其它冷冻剂的冷冻系统，包括二氧化碳和氨气，选择性地与一种或多种冷冻剂组合。适宜地，冷冻剂不含氯原子，因此，冷冻剂优选基本上仅由HFC冷冻剂组成。HCFC’s和HFC’s至少包含一个碳原子和一个氟原子，仅在HCFC’s情形下，包含一个或多个氯原子。
HCFC’s的实例包括氯二氟甲烷(R22)和二氯三氟乙烷(R123)。
HFC’s的实例包括1，1，1，2-四氟乙烷(R134a)，1，1，1，2，2-五氟乙烷(R125)，二氟甲烷(R-32)，1，1，1-三氟乙烷(R143a)和1，1-二氟乙烷(R-152a)。在冷冻剂掺混物中也可包括通常存在的其它组分，包括烃，特别是具有1-6个碳原子的烃，例如，丙烷、异丁烷、丁烷和戊烷，氟代烃和其它冷冻剂，如二氧化碳。
当冷冻剂包含HFC时，特别是当冷冻剂基本上由HFC组成时，可能会加剧在冷冻系统中，特别是在膨胀装置中阻塞引起的问题。
当冷冻剂包括HFC，例如，1，1，1，2-四氟乙烷(R134a)或HFC’s的掺混物如R407C、R410A和R404A时，本发明是特别有益的。
各种用于冷冻系统中的合成润滑剂是公知的，例如，聚亚烷基二醇(PAGs)和多元醇酯。这些润滑剂通常与HFC冷凝剂一起使用，并具有相对较高的极性。由于使用这些润滑剂也可能会加剧不想要的残余物沉积的问题。
不想要的残余物通常为非极性或高分子量的，而包含HFC’s的冷冻剂通常具有相对较高的极性，结果，不想要的残余物难于溶解或分散于冷冻剂和润滑剂的物流中。
本发明的另一个方面提供了一种用于带有冷冻剂的冷冻系统中的冷冻润滑剂组合物，所述冷冻剂包含氢氟碳化合物，所述冷冻润滑剂组合物包含一种合成的润滑剂和一种两亲性抗沉积组分，合成润滑剂包含多元醇酯和/或聚氧化亚烷基二醇。
本发明还涉及一种冷冻系统，其包含压缩机、冷凝器、膨胀装置和蒸发器，它们联接在一起形成一个回路，其中，冷冻剂循环并连续进行冷凝和蒸发，从而提供冷冻效果，冷冻剂包含氢氟碳和/或氢氯氟碳冷冻剂，系统进一步包含一种合成的润滑剂，其包含多元醇酯和/或聚氧化亚烷基二醇和一种两亲性抗沉积组分。
本发明还提供了包含润滑剂和两亲性抗沉积组分的冷冻润滑剂在用于抑制对冷冻系统的性能有不利影响的沉积物沉积的冷冻系统中的用途。
另一方面，本发明提供了一种抑制冷冻系统中不想要的残余物沉积或除去残余物的方法，该方法包括在充入一种含氢冷冻剂和一种包含润滑剂和两亲性抗沉积组分的冷冻剂组合物时运行冷冻系统。
本发明的另一个方面，将抗沉积剂加至已用冷冻剂和润滑剂改变的冷冻系统中。组分可以自身加入或以浓缩物加入用于该系统的润滑剂中。因此，已运行的系统可接受组分或浓缩物而无需进行后充填过程，或者在通过加入组分或浓缩物而关闭之前清洁的由清洁作用带来的效益。
因此，冷冻系统的优选操作方法包括以下步骤：运行含冷冻剂和润滑剂的冷冻系统，向系统中加入抗沉积组分，进一步运行系统从而抑制不想要的残余物的沉积或除去沉积物。
两亲组分必须在所采用的剂量下具有最佳的两亲平衡性和在循环的冷冻剂/润滑剂混合物中的溶解性，从而提供抗沉积作用，以充分减少或在冷冻系统中的阻塞形成。组分两亲性的测量可通过在随后定义的标准实验中观察组分的作用来获得。
在该实验中，为方便起见称之为“分散性实验”，将3GS矿物油(商购自Suniso)、新戊基多元醇酯和两亲性组分分散于1，1，1，2-四氟乙烷(R134a)中，记录混合物从R134a中完全相分离的时间。将50wt％的3GS矿物油与50wt％的季戊四醇酯(以商品名EMKARATE RL(32H级)商购自ICI)混合，形成实验用油混合物(TOM)。向该TOM中加入为油混合物重量1wt％的两亲组分以形成均匀的混合物。然后，在大约20℃下，将TOM与两亲组分及液体R134a混合，其重量比为100份TOM∶100份R134a∶1份抗沉积组分，剧烈搅拌以形成R134a与TOM的分散体。然后，目视测量从搅拌停止到形成2个明显不同液相所需的时间。所述时间提供了添加剂在提供抗沉积作用中有效性的度量，相对于不含组分的样品来说，形成明显不同相的时间越长则表明效力越强。在本发明中，优选相分离形成两个明显不同的澄清液相仅在至少10秒后，更优选30秒，首选在至少1分钟后。特别优选的是，这些组分延迟组分的相分离至少3分钟，最好是至少5分钟。作为参考，TOM与R134a的混合物(无抗沉积组分)几乎立即分离，在任何情形下均低于5秒。本发明的基本要求是，在实验中所采用的浓度下，在实验过程中的任何时候，组分不能从实验混合物中沉淀出来。
抗沉积组分可为任一种能够满足分散性实验标准的物质。该组分通常在其分子内具有几个部分，至少一个部分为亲油的，并且，至少一个部分对R134a的亲合力要大于对亲油部分的亲合力，并且其可被称之为极性部分。
抗沉积组分可为阳离子、两性、非离子或阴离子的。特别优选组分为阴离子的，并在分子内包含非极性部分。
优选组分包含作为极性部分的可离子化部分，其最好是离子化的形式，特别为阴离子部分，或包含氟碳基团的部分，或者是既为可离子化的部分又为包含氟碳基团的部分。适宜的阴离子部分包括硫酸根、磺酸根、磷酸根和羧酸根以及具有活性氢的部分，例如，阴离子氟表面活性剂，包括以商品名ZONYL从Aldrich商购的化合物。阴离子的硫酸盐和羧酸盐因其稳定性和性能方面的原因相对是不优选的。氟碳基团可为任一种包含碳原子和氟原子的基团，例如，包括烃基，其中，至少一个氢原子被氟原子取代，和选择性地所有的氢原子被氟原子取代，也就是说，一个基团完全包含碳和氟原子，例如，三氟甲基、五氟乙基、七氟丙基。优选地，氟碳基团具有1-8个碳原子，更优选1-6个碳原子，特别是1-3个碳原子。氟碳基团可为直链或支链基团。特别优选的物质包括烷基琥珀酸盐，例如，二辛基磺基琥珀酸盐和芳族磺酸和石油磺酸盐。离子部分可以盐或优选以酸形式使用。
适宜的非离子组分包括由亚烷基氧化物和得自于具有活性氢原子部分和亲油部分得到的烷基烷氧基化物，例如长链醇。优选的亲油部分包括具有脂族烃基的部分，例如具有6-22个碳原子的烃基，芳族烃基和其混合物。适宜的具有活性氢原子的部分包括醇基团、胺基团、羧酸基团，而不论其来自酸、酯或酸酐。
其它适宜的非离子组分包括聚亚烷基二醇的酯和氟化聚醚。
特别优选的抗沉积组分的实例包括下表1中列出且属于此类的那些化合物。特别优选的实例包括二烷基磺基琥珀酸酯和其盐、氟代脂族聚合醚、烷基芳族磺酸和其盐和甲基丙烯酸甲酯、甲基丙烯酸和甲氧基聚环氧乙烷甲基丙烯酸酯的梳状接枝共聚物以及丙烯酸接枝共聚物的溶液。
抗沉积组分在组合物中的适宜含量为0.001-5wt％，优选0.001-3wt％，更优选0.01-3wt％，首选0.05-1wt％，例如0.5wt％，以润滑剂重量计。组分适宜与润滑剂在加至冷冻系统之前进行混合。理想地可采用单一一种抗沉积组分或这种组分的混合物，如一种阴离子组分和一种非离子组分的混合物。
要求抗沉积组分的用量应使其在冷冻系统中于冷冻剂/润滑剂混合物中保持溶解。如果组分在所采用的剂量下不能保持溶解状态，则可能会引起系统中不希望发生的阻塞。
组分在冷冻剂和润滑剂混合物中的溶解度将取决于具体采用的物质以及测定溶解度时的条件。在冷冻系统中，冷冻剂在出口至膨胀装置的蒸发可能会呈现出最苛刻的情况，在此情形下，由于低温，组分必须保持可溶状态，通常在冷冻剂的沸点附近。
适宜地，应选择抗沉积组分的含量和类型以使组分在润滑剂占冷冻剂/润滑剂混合物10wt％下溶解于在冷冻剂与润滑剂混合物中，在冷冻剂的沸点下使用。
可用于本发明的适宜的合成润滑剂包含下述中的一种或其组合：多元醇酯，特别是新戊基多元醇酯、聚亚烷基二醇、聚乙烯基醚和烷基苯。特别适宜的润滑剂为多元醇酯和/或聚亚烷基二醇，选择性地与烷基苯进行组合。
优选用于本发明工作流体组合物中的合成润滑剂选自被称之为多元醇酯的那些，特别是新戊基多元醇酯，其特别具有相对较高的热稳定性。适宜的新戊基多元醇酯包括季戊四醇、多季戊四醇如二和三季戊四醇、三羟甲基烷烃如三羟甲基丙烷和新戊二醇的酯。这种酯可与直链和/或支链的脂族羧酸形成，如直链和/或支链链烷酸，或其可酯化的衍生物，例如酸酐。为增加酯润滑剂的粘度，在合成酯润滑剂时，也可采用少量的脂族多元羧酸，如脂族二元羧酸或其可酯化衍生物。但是，当在合成过程中采用这种脂族多元酸(或其可酯化的衍生物)时，优选其用量应不超过羧酸总量的50 mol％，更优选不超过30 mol％，特别是不超过10 mol％。为方便起见，除非清楚地排除了这种定义，本文中所用术语“羧酸”包括了所述酸的可酯化衍生物。通常，在合成中羧酸的用量应足以酯化包含于多元醇中的所有羟基，但在某些时候，残余羟基官能团是可以接受的。
一种优选的新戊二醇酯润滑剂为一种包含通式II的一种或多种化合物之一：
R(OC(O)R1)n                 II其中，
R为由季戊四醇、二季戊四醇、三季戊四醇、三羟甲基乙烷、三羟甲基丙烷或新戊二醇除去羟基后得到的烃基，或者为由季戊四醇、二季戊四醇、三季戊四醇、三羟甲基乙烷、三羟甲基丙烷或新戊二醇除去一定比例的羟基后得到的含羟基的烃基；
每一个R1独立地为H、直链脂族烃基、支链脂族烃基、含羧酸或羧酸酯取代基的脂族烃基(直链或支链)，只要至少一个R1基团为直链脂族烃基或支链脂族烃基；
n为整数。
上面所述的对于R1的脂族烃基可被取代，例如被氯、氟和溴取代，和/或可包含杂原子如氧和氮，其可悬垂于碳链上或成为烃基的碳链的一部分。但是，优选烃基包含氢、碳和选择性的氧，例如，其中，R1为含羧酸酯取代基的羧酸的脂族烃基。特别优选烃基仅包含碳和氢原子。
式II的酯润滑剂可通过使适宜的多元醇或多元醇的混合物与适宜的羧酸或酸混合物进行反应制得。羧酸的可酯化衍生物也可用于合成，如其酰卤、酸酐和低级烷基酯。适宜的酰卤为酰氯，适宜的低级烷基酯为甲基酯。脂族多元羧酸或其可酯化的衍生物也可用于合成酯润滑剂。当脂族多元羧酸用于合成酯润滑剂时，形成的润滑剂将包含一种或多种式II的化合物，其中，至少R1基团之一为含羧酸或羧酸酯取代基的脂族烃基(直链或支链)。多元羧酸与两种或多种醇分子进行反应的能力提供了增加所形成酯分子量的手段，从而提供了增加润滑剂粘度的手段。这种多元羧酸的实例包括马来酸、己二酸和琥珀酸，特别是己二酸。但是，通常仅采用一元羧酸用来合成酯润滑剂，而多元羧酸使用时是与一种或多种一元羧酸一起使用，仅成为用于合成中的羧酸总量的一小部分。当脂族多元羧酸用于合成时，优选其用量不超过用于合成的羧酸总量的50mol％，更优选不超过30mol％，特别是不超过10mol％，一种或多种一元羧酸构成其余所用酸。
适宜用于合成中的羧酸(或其可酯化的衍生物)的用量应足以将包含于多元醇中的所有羟基酯化，在此情形下，形成的润滑剂将包含式II的一种或多种化合物，其中，R为由季戊四醇、二季戊四醇、三季戊四醇、三羟甲基乙烷、三羟甲基丙烷或新戊二醇除去羟基后得到的烃基。但是，在某些情形下，包含残余羟基官能团的酯润滑剂也可接受。这种润滑剂包含一种或多种式II的化合物，其中，R为由季戊四醇、二季戊四醇、三季戊四醇、三羟甲基乙烷、三羟甲基丙烷或新戊二醇除去一定比例的羟基后得到的含羟基的烃基。包含残余(未反应)羟基官能团的酯通常称之为部分酯，包含它们的润滑剂可采用一定量的羧酸或未充分酯化所有包含于多元醇中的羟基的酸制备。
新戊二醇酯润滑剂可包含单一一种式II的化合物，即单一一种多元醇与单一一种一元羧酸形成的反应产物。但是，酯润滑剂也可包含一种混合酯组合物，其包含两种或多种式II的单一化合物。这种混合酯组合物可通过制备两种或多种单一酯，然后将这些酯掺混于一起制得。在合成酯中采用两种或多种羧酸将产生一种在单一化合物内具有两个或多个酸的酯。这些物质也适用于单独使用或与其它单一酯或混合酯混合使用。因此，也可掺混不同的混合酯组合物，这些酯的每一种通过在其合成过程中采用两种或多种多元醇和/或两种或多种羧酸制得。
优选的新戊烯基多元醇酯润滑剂包含一种或多种式II的化合物，其中，R为由季戊四醇、二季戊四醇、三羟甲基丙烷或新戊二醇除去羟基后得到的烃基。
优选地，每一个式II中的R1独立地为直链脂族烃基或支链脂族烃基。
优选用于R1的直链脂族烃基为直链烷基，特别是C3-12直链烷基，更优选C5-10直链烷基，首选C5-8直链烷基。适宜的直链烷基包括正戊基、正己基、正庚基、正辛基、正壬基和正癸基。包含该烷基的酯可在酯的合成过程中采用直链链烷酸(或其可酯化的衍生物)制备。
优选用于R1的支链脂族烃基为支链烷基，特别是C4-14支链烷基，更优选C6-12支链烷基，首选C8-10支链烷基。适宜的支链烷基的实例包括异戊基、异己基、异庚基、异辛基、异壬基、异癸基、2-乙基丁基、2-甲基己基、2-乙基己基、3，3，5-三甲基己基、新戊基、新庚基和新癸基。包含该烷基的酯可在酯的合成过程中采用支链链烷酸(或其可酯化的衍生物)制备。
在本发明特别优选的实施方案中，酯润滑剂包含一种或多种通式III的酯 R 2 ( O - C - R 3 O ) p - - - - III 其中
R2为由戊季四醇、二季戊四醇或三羟甲基丙烷除去羟基后获得的烃基；
每一个R3独立地为直链烷基或支链烷基。
p为整数3、4或6。
其中，一种或多种所述的多元醇、一种或多种直链链烷酸或其可酯化的衍生物以及选择性的一种或多种支链链烷酸或其可酯化的衍生物用来合成酯润滑剂。
优选地，在合成酯时采用两种或多种链烷酸，特别是两种链烷酸的混合物或其可酯化的衍生物。更优选地，一种或多种直链烷酸或其可酯化的衍生物与一种或多种支链的链烷酸或其可酯化的衍生物的混合物用于合成过程。因此，本发明特别优选的酯润滑剂为混合酯组合物，其包含多种式III的化合物。
当直链和支链链烷酸混合物用于合成酯时，优选地，直链链烷酸优选卤所采用的羧酸总量的至少25mol％，例如25-50mol％。这样，包含于多元醇或多元醇混合物中的至少25mol％，例如25-75mol％的羟基可与所述直链链烷酸反应。
包含一种或多种式III化合物的酯基润滑剂提供了一种在所需润滑剂性质间的良好平衡，特别是在所需润滑剂性质间良好的平衡，特别是显示出优良的热稳定性，优良的水解稳定性和可接受的溶解性及与冷冻剂的掺混性。特别理想的是，用于工作流体组合物中的润滑剂显示出优良的热稳定性，所述组合物被设计来代替基于R-22和R-502的现有组合物。
优选地，R2为季戊四醇或二季戊四醇除去羟基后获得的烃基。
优选用于R3的直链和支链烷基为如上对R1所述的那些，并且采用相应的链烷酸或其可酯化的衍生物获得。
特别优选的酯基润滑剂包含基于季戊四醇或其低聚物或新戊二醇与具有5-10个碳原子的直链和/或支链酸的酯基润滑剂。适宜的润滑剂的实例包括冷冻润滑剂EMKARATE RL，其商购自ICI，具体等级为22H，32H和68H。酸的可酯化衍生物也可用于合成酯。
适宜的聚氧化亚烷基二醇润滑剂包括羟基引发的聚氧化亚烷基二醇，例如，用一元醇如甲醇和丁醇或多元醇如季戊四醇和甘油引发的环氧乙烷和/或环氧丙烷低聚物。这种聚氧化亚烷基二醇也可采用适宜的的末端基团进行端封，包括烷基，如甲基。
优选的聚氧化亚烷基二醇润滑剂的平均分子量为约150-3000，其包含通式I的一种或多种化合物：
A[-O-(CH2CH(CH3)O)1(CH2CH2O)m-Q]x         I其中
A为由含羟基的有机化合物在除去羟基后获得的残基；
Q表示氢、取代或未取代的烷基、酰基、芳烷基或芳基；
l和m独立地为0或整数，只要l或m之一为整数，x为整数。
聚氧化亚烷基二醇润滑剂可采用本领域技术人员公知的常规技术制备。因此，在一种方法中，含羟基的有机化合物与环氧乙烷和/或环氧丙烷反应形成含末端羟基的环氧乙烷和/或环氧丙烷低聚物/聚合物。选择性地，再将这种物质醚化产生式I的聚氧化亚烷基二醇。最终形成的聚氧化亚烷基二醇可包含一种该类化合物的混合物，所述化合物的聚合度不同，即氧化亚乙基和/或氧化亚丙基残基数不同。进而，醇和/或酚的混合物可用作形成聚氧化亚烷基二醇润滑剂中的引发剂，也可采用提供不同Q基团的醚化剂的混合物。包含通式I化合物的混合物的聚氧化亚烷基二醇润滑剂的分子量将表示所有存在的化合物的平均分子量，从而给出的润滑剂可包含特定的聚氧化亚烷基二醇，其分子量可超出上述范围，只要所有化合物的平均分子量在该范围内。
在通式I的聚氧化亚烷基二醇中的部分A为由含羟基的有机化合物除去羟基后获得的残基。可以理解，这决非意味着部分A需要通过除去羟基来生产。这种化合物包含一元醇和多元醇和酚。当用作形成聚氧化亚烷基二醇的引发剂的含羟基的化合物为一元醇或酚时，A优选为烃基，更优选烷基、芳基、烷芳基或芳烷基，特别是烷基。适宜的用于A的烷基可选自直链、支链或环状烷基。优选地，A为C1-15烷基，更优选C1-12，特别是C1-10，首选C1-6烷基。烷基可为直链或支链的，特别优选直链C1-6烷基。烷基的具体实例包括甲基、乙基、正丙基、异丙基、正丁基、异丁基、仲丁基、叔丁基、各种戊基、各种己基、环戊基、环己基等。特别优选的用于A的烷基为甲基或正丁基。
其它用于A的适宜的烃基为那些由苄基醇和酚如苯酚、甲酚、壬基酚、间苯二酚和双酚A除去羟基后得到的基团。
当多元醇用于形成聚氧化亚烷基二醇时，A优选为烃基。适宜的用于A的烃基为那些由多元醇除去羟基后获得的基团，所述多元醇例如为乙二醇、丙二醇、1，4-丁二醇、1，6-己二醇、二甘醇、一缩二丙二醇、新戊二醇、环己烷二甲醇、甘油、1，2，6-己三醇、三羟甲基丙烷、季戊四醇、二季戊四醇和山梨醇。特别优选的用于A的烃基为由甘油除去羟基后获得的基团。
在通式I的聚氧化亚烷基二醇中的部分Q为H、取代或未取代的烷基、芳烷基或芳基。优选用于Q的取代或未取代的芳烷基为取代或未取代的苄基。优选用于Q的取代或未取代的芳基包括苯基和烷基取代的苯基。优选地，Q为取代或未取代，例如卤代的烷基，特别是取代或未取代的C1-12烷基，更优选取代或未取代C1-4烷基。适宜用于Q的烷基可选自直链、支链或环状烷基，特别是直链烷基。虽然用于Q的烷基可为取代或未取代的，但优选未取代的。因此，特别优选用于Q的烷基选自甲基、乙基、丙基、异丙基和各种丁基。特别优选用于Q的烷基为甲基。
通式I的聚氧化亚烷基二醇可为聚氧化亚乙基二醇、聚氧化亚丙基二醇或聚(氧化亚乙基/氧化亚丙基)二醇。在后一种情形下，氧化亚乙基和氧化亚丙基残基在聚合物链中可随机地设置或以嵌段设置。优选的聚氧化亚烷基二醇为聚氧化亚丙基二醇和聚(氧化亚乙基/氧化亚丙基)二醇。
润滑剂组合物也可包含一种或多种在冷冻润滑剂领域中常规采用的添加剂。具体可提及的是抗氧化剂和热稳定改善剂，腐蚀抑制剂，金属减活化剂，粘度指数改善剂，抗磨剂和耐极压添加剂。这些添加剂是本领域技术人员公知的。当润滑剂成为包含一种或多种添加剂的润滑剂组合物的一部分时，这些添加剂的用量为现有技术中的常规用量。优选地，所有添加剂的总量应不超过润滑剂组合物总重量的8％，如5％。
适宜的抗氧化剂和热稳定改善剂可选自：二苯基-、二萘基-和苯基萘基-胺，苯基和萘基可被取代。具体实例包括：N，N’-二苯基亚苯基二胺、对辛基二苯基胺、对，对-二辛基二苯基胺、N-苯基-1-萘基胺、N-苯基-2-萘基胺、N-(对十二烷基)-苯基-2-萘基胺、二-1-萘基(对十二烷基)-苯基-2-萘基胺、-二-1-萘基胺和二-2-萘基胺。其它适宜的抗氧化和热稳定改善剂可选自吩噻嗪如N-烷基吩噻嗪和受阻酚，如6-(叔丁基)苯酚、2，6-二-(叔丁基)苯酚、4-甲基-2，6-二-(叔丁基)苯酚和4，4’-亚甲基二(-2，6-二-[叔丁基]苯酚)。
适宜的亚铜金属减活化剂可选自：咪唑、苯并咪唑、2-巯基苯并噻唑、2，5-二巯基噻二唑、亚水杨基丙二胺、吡唑、苯并三唑、甲苯并三唑、2-甲基苯并咪唑、3，5-二甲基吡唑和亚甲基二-苯并三唑。更一般的减活化剂和/或腐蚀抑制剂的实例包括有机酸和其酯、其金属盐和酸酐，如N-油酰基-肌氨酸、脱水山梨醇单油酸酯、环烷酸铅、十二碳烯基-琥珀酸和其部分酯和酰胺，4-壬基苯氧基乙酸；伯、仲和叔脂族和脂环族胺和有机酸和无机酸的胺盐，如油溶性烷基羧酸铵；杂环含氮化合物，如噻二唑、取代的咪唑啉和恶唑啉；醌和蒽醌；链烯基琥珀酸酐或酸的酯和酰胺衍生物，二硫代碳酸盐(二thiocarbarnates)，二硫代磷酸盐；和烷基酸磷酸酯的胺盐和其衍生物。
适宜的粘度指数改善剂包括聚甲基丙烯酸酯聚合物、吡咯烷酮与甲基丙烯酸酯的共聚物、聚丁烯聚合物和苯乙烯与丙烯酸酯的共聚物。
适宜的抗磨损剂和耐极压剂的实例包括硫化的脂肪酸和脂肪酸酯，如硫化的脂肪酸辛酯；硫化的萜烯；硫化的烯烃；有机多硫化物；有机亚磷衍生物，包括胺磷酸酯、烷基酸式磷酸酯、三烷基和三芳基偶磷硫羰酸酯，三烷基和三芳基膦和二烷基亚磷酸酯，如磷酸和单己基酯的胺盐，二壬基胺萘磺酸的胺盐，三苯基磷酸酯，三萘基(tripaphthyl)磷酸酯，二苯基甲苯基和二甲苯基苯基磷酸酯，三甲苯基磷酸酯，萘基二苯基磷酸酯，三苯基偶磷硫羰酸酯；二硫代碳酸，如二烷基二硫代氨基甲酸锑；氯代和/或氟代烃和黄原酸盐酯。
通过下述非限定性实例说明本发明。
实施例1
按照下述过程制备多种实验混合物：将如下表1所示的10g的EMKARATERL(由ICI供给)级32H与10g的3GS矿物油(购自Suniso)和0.2g的抗沉积组分混合。然后，将混合物加至20g的R134a中，随后进行如上提出的分散性实验。然后，测量分离物质的时间，结果如表1所示。
表1
抗沉积组分 供应商 分离时间
SPAN 85 ICI 15秒
SPAN 80 ICI 25秒
FC430 3M 90秒
FC431 3M 10秒
ZONYL FSJ Aldrich 30秒
ZONYL FSP Aldrich 10秒
ZONYL FSA Aldrich 10秒
TRITON X-100 BDH 20秒
TWEEN 20 ICI 10秒
TWEEN 60 ICI 25秒
SURFYNOL SE Lancaster 15秒
二辛基磺基琥珀酸酯 Lancaster ＞5分钟
HYPERMER CG6 ICI 10秒
TWEEN 80 ICI 20秒
SPAN 80 ICI 10秒
SYNPERIONIC 91/6 ICI 10秒
ATLAS G1284 ICI 30秒
SYNPERONIC A7 ICI 10秒
ZONYL FSE Aldrich 15秒
十二烷基苯磺酸 Aldrich ＞5分钟
十二烷基硫酸盐 Aldrich 25秒
丙烯酸月桂酯 Lancaster 15秒
硬脂酸烯丙酯 Lancaster 20s 20秒
2-羟基棕榈酸 Lancaster 35秒
实施例2-5和比较例A和B
在下述“实验方法”中，于毛细管实验装置中对各种抗沉积组分的作用进行实验。
建立实验装置。该装置具有L’Unite Hermetique压缩机(AZ1330Y型)，其经管线与毛细管相连，通过密闭的偶合换热器。来自毛细管的回管通过偶合换热器并返回压缩机，完成循环冷冻组合物的回路。平均抽吸和排放压力分别为15和200 psig。毛细管的内径为0.65mm，管长2.2m。环境温度大约为20℃。在毛细管进行流量测量之前和之后均设置三路阀。
在压力为150 psig下使氮气通过毛细管，将压力逐渐增大，测量使5升氮气通过毛细管所需的时间以进行平静，由其记录每分钟的平均流速(升)。然后，用R-134a净化系统，然后充入R-134a至冷冻剂的蒸气压。将来自ICI的润滑剂300 ml的EMKARATE RL 22H多元醇酯油加至压缩机中。对于比较例B和实施例2-5来说，在充入润滑剂之前，计量加入基于润滑剂重量500ppm的石蜡。加入石蜡起到阻塞材料作用。测定石蜡的加入量以使在5天内由限制流速引起的阻塞至多为50％，在另5天时，流速大约为50％。
抗沉积组分形成实施例2-5中的油成分，在充入之前的量大约为1wt％。
将系统运行大约20天。物质通过毛细管的流动每天测量一次，直至限制保持基本恒定，或者管子阻塞，从而流动降低至低于原始值的约50％。在两次实验之前，将装置和压缩机清洗以用于以后的实验。
为进行比较(比较例A和B)，仅采用冷冻剂和润滑剂(比较例A)对实验装置运行20天，然后，如前所述附加采用蜡(比较例B)。在这些参考操作中，无抗沉积组分存在。
然后，在实验装置中连续对在表2列出的抗沉积组分进行实验，通过毛细管的流速在约20天内进行测量。
这些实验的结果如表3所示，参考运行过程标记为比较例A和B，其它实验被称为实施例2-5。
实验的抗沉积组分如下：
表2
 实施例         组分                   化学   供应商
    2        FC430                  氟碳酯     3M
    3     SURFYNOL SE     2，4，7，9-四甲基-5-癸炔-4，7-二醇 Lancaster
    4   阴离子表面活性剂             二辛基磺基琥珀酸酯 Lancaster
    5     Hypermer CG6        丙酮接枝共聚物的水/丙二醇溶液    ICI
表3时间          A          B            2           3           4          50             100.0      100.0        100.0       100.0       100.0      100.00.5                                               96.71                        84.7         93.9        86.2        95.2       95.41.5           101.12                        82.2         87.4        88.83                        63.3                     83.14             87.8                                84.3        93.4       88.25                                     89.0                    92.7       88.96             85.5       60.4         93.2                               88.57             85.2       60.7         86.6        80.0        92.4       89.68             84.6       60.1         83.5        80.0        91.99                        60.2         77.2        81.710                       58.311            84.8                                76.9        91.712            84.6                    89.0                    91.1       82.313            85.9                    88.8                    92.3       80.614            84.8                    86.1         74.0       92.4       78.915            85.6                    86.6         74.3       93.3       75.116            85.8                    75.117                                    74.9                    94.1       80.818            86.3                    73.9                               81.919            85.4       84.120                       83.621                                     87.222                                     83.223                                     74.124                                     85.0
表3所示结果表明，各种抗沉积组分减少了由石蜡引起的系统中的阻塞程度，从而保持了高的流速。具体而言，可以看出，二辛基磺基琥珀酸酯和FC430减少了石蜡的阻塞程度，类似的结果仅在润滑剂自身进行实验时才能获得(比较例A)。进而，抗沉积组分显示出减少毛细管的阻塞率，以及由于石蜡造成的总阻塞。
本发明的优选实施方案中，当按照如前所示实验方法进行实验时，使用抗沉积组分使得原始流速的至少65％，特别是至少75％在20天后得以保持。最理想地，优选组分提供清洁作用，这使系统中的流速，即在润滑剂和冷冻剂中加入500 ppm石蜡时的流速与仅采用相同的润滑剂和相同的冷冻剂循环时系统的流速相当，流速按照如前所述方法测量。

Claims (18)

1.一种冷冻润滑剂组合物，其包含一种润滑剂和一种两亲抗沉积组分。
2.一种用于具有含氢冷冻剂的冷冻系统中的权利要求1的润滑剂组合物，它包含合成润滑剂和两亲抗沉积组分。
3.一种用于具有冷冻剂的冷冻系统中的权利要求1或2任一项的润滑剂组合物，所述冷冻剂包含氢氟碳和/或氢氯氟碳化合物，所述组合物包含一种合成润滑剂，和一种两亲抗沉积组分，合成润滑剂包含多元醇酯和/或聚亚烷基二醇。
4.根据前述任一项权利要求的组合物，其中，两亲抗沉积组分应在本文所述的分散性实验中，在至少10秒后R134a与总油混合物的相分离。
5.根据前述任一项权利要求的组合物，其中，抗沉积组分为阴离子性的，并在其分子中包含非极性部分。
6.根据权利要求5的组合物，其中，分子中的非极性部分包含氟碳基团。
7.根据权利要求1-4任一项的组合物，其中，组分为阴离子性的，并包含磺酸根或磷酸根部分。
8.根据权利要求1-4任一项的组合物，其中，抗沉积组分选自烷基磺基琥珀酸盐、芳族磺酸和石油磺酸盐，氟脂族的聚合酯和丙烯酸接枝共聚物的溶液。
9.根据前述任一项权利要求的组合物，其中，抗沉积组分的含量为0.001-5wt％，以润滑剂重量计。
10.根据前述任一项权利要求的组合物，其中，润滑剂包含通式II的化合物：
R  (OC(O)R1)n               II其中，R为由季戊四醇、二季戊四醇、三季戊四醇、三羟甲基乙烷、三羟甲基丙烷或新戊二醇除去羟基后得到的烃基，或者为由季戊四醇、二季戊四醇、三季戊四醇、三羟甲基乙烷、三羟甲基丙烷或新戊二醇除去一定比例的羟基后得到的含羟基的烃基；每一个R1独立地为H、直链脂族烃基、支链脂族烃基、含羧酸或羧酸酯取代基的脂族烃基(直链或支链)，只要至少一个R1基团为直链脂族烃基或支链脂族烃基；n为整数。
11.根据权利要求10的组合物，其中，酯包含季戊四醇、二季戊四醇和/或三季戊四醇的酯，每一个R1基团选自直链脂族烃基和支链脂族烃基。
12.根据前述任一项权利要求的组合物，其中，润滑剂包含聚亚烷基二醇。
13.根据前述任一项权利要求的组合物，其中，冷冻剂包含1，1，1，2-四氟乙烷。
14.根据前述任一项权利要求的组合物，其中，冷冻剂包含两种或多种氢氟碳冷冻剂的掺混物。
15.一种冷冻系统，其包含压缩机、冷凝器、膨胀装置和和蒸发器，它们联接在一起形成一个回路，其中，冷冻剂循环并连续进行冷凝和蒸发，从而提供冷冻效果，冷冻剂包含氢氟碳和/或氢氯氟碳冷冻剂，系统进一步包含一种如前述权利要求任一项所述的冷冻润滑剂组合物。
16.权利要求1-14任一项的冷冻润滑剂在用于抑制对冷冻系统的性能有不利影响的残余物沉积或除去残余物的冷冻系统中的用途。
17.一种抑制冷冻系统中残余物沉积或除去残余物的方法，该方法包括在充入含氢冷冻剂和权利要求1-14任一项所述的冷冻润滑剂组合物时运行冷冻系统。
18.根据权利要求17的方法，包括下述步骤：运行含冷冻剂和润滑剂的冷冻系统，向系统中加入抗沉积组分，进一步运行系统从而抑制不想要的残余物的沉积或除去沉积物。
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ID29793A (id) 2001-10-11
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AU776207B2 (en) 2004-09-02
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WO2000044860A1 (en) 2000-08-03
BR0007691A (pt) 2001-11-06
US20020013233A1 (en) 2002-01-31
AU2117900A (en) 2000-08-18
US6849583B2 (en) 2005-02-01
SK10492001A3 (sk) 2002-01-07

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