CN1297472A - 使用烃制冷剂的压缩式制冷机用润滑剂 - Google Patents

使用烃制冷剂的压缩式制冷机用润滑剂 Download PDF

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CN1297472A
CN1297472A CN00800452A CN00800452A CN1297472A CN 1297472 A CN1297472 A CN 1297472A CN 00800452 A CN00800452 A CN 00800452A CN 00800452 A CN00800452 A CN 00800452A CN 1297472 A CN1297472 A CN 1297472A
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lubricant
mineral oil
hydrocarbon coolant
hydrocarbon
refrigerator
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CN00800452A
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CN1183236C (zh
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开米贵
高桥仁
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Eneos Corp
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Japan Energy Corp
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Abstract

本发明提供一种以在40℃的运动粘度为5—150mm2/s、流点在－25℃以下、粘度指数在50以上、由n－d－M环分析法测得的%Cp和%CA分别在50以上和在12以下、氮含量在20ppm以下、硫含量为0.02—0.3 %、碘价为10gI2/100g以下的矿物油为主要成分的、用于使用低级烃制冷剂的压缩式制冷机的润滑剂、由该润滑剂和低级烃制冷剂组成的用于制冷机的工作流体组合物及充填有该工作流体组合物的制冷装置。本发明的润滑剂与烃制冷剂的相溶性优异、稳定性、润滑性均佳,因此,作为没有破坏臭氧层、地球温室效应的担忧的用于使用烃制冷剂的制冷机的润滑剂是非常有用的。

Description

使用烃制冷剂的压缩式制冷机用润滑剂
技术领域
本发明涉及使用由没有破坏臭氧层的担忧且其地球温室化能力也远低于含卤烃制冷剂的低级烃组成的制冷剂的用于压缩式制冷机的润滑剂。此外，本发明还涉及由上述烃制冷剂和润滑剂组成的工作流体组合物和充填有该工作流体组合物的制冷装置。
发明背景
压缩式制冷机由压缩机、冷凝器、膨胀机构(如膨胀阀)、蒸发器等组成，利用挥发性大的制冷剂蒸发时从周围夺取蒸发热的性质进行冷却，被用于冰箱、冷冻机、空调、商店橱窗、清凉饮料和冰淇淋等的自动售货机等。在空调、自动售货机等中，利用冷凝时产生的热，还进行制热或被用于将饮料和食品加热保温。
以往，所用的制冷剂是三氯氟甲烷(R11)、二氯二氟甲烷(R12)、氯二氟甲炕(R22)等含有氯的氟代烃(CFC或HCFC)。但由于这些CFC和HCFC会引起破坏臭氧层的环境问题，其生产和使用在国际范围内受到限制，现在，它们正被例如二氟甲烷(R32)、四氟乙烷(R134或R134a)、二氟乙烷(R152或R152a)等不含氯的非氯系氟代烃(HFC)替代。然而，这些HFC虽然不会破坏臭氧层，但其地球温室化能力大，因此，从地球环境保护的长远观点看，人们担心其仍存在问题。
为此，碳原子数为1-5个左右的低分子量的低级烃、氨等由于不会破坏臭氧层、地球温室化能力也远低于上述含氯系或非氯系氟代烃而作为对环境友善的制冷剂而受到关注。这些化合物以往虽然不属于制冷剂的主流，但也具有长期使用的历史。此外，例如日本特许公开公报1998年第130685号还公开了用环烷系或石蜡系矿物油、烷基苯油、醚油、酯油、氟化油等合成油作为由上述烃组成的制冷剂的润滑剂。在这些润滑剂中，由于合成油一般较贵，因此，从实用的观点出发，人们对价格低廉、容易购得的矿物油抱有期望。
然而，在低分子量烃制冷剂(低级烃制冷剂)和矿物油系润滑剂的组合中，也存在各种问题。尤其是由于下述原因，人们希望使用烃制冷剂的制冷机用润滑剂自身具有优异的润滑性能。
作为制冷剂的低分子量的烃与作为润滑剂的矿物油虽然相溶，但由于比重差异大，因此，仅通过自然扩散，两者有时难以彼此混合。在制冷机中，常常出现它们被置于难以彼此混合的状态。例如，在将制冷剂充填入压缩机中时，形成密度小的制冷剂层叠在先装入的密度大的润滑剂的上面的形式。此外，在压缩机停机过程中制冷剂以液体状态回流至压缩机内时(即所谓溢流时)也会出现上述状态。在上述状态时若启动压缩机，则离心力会使润滑剂聚集在旋转外侧，导致在需要润滑的内部轴承等滑动部没有足够的润滑剂。其结果是，滑动部出现磨耗或容易出现咬粘。为此，希望使用低分子量烃制冷剂的制冷机用润滑剂具有优异的润滑性能。此外，烃制冷剂与可期望由分子内的氯而产生的极压效果的氯系氟代烃制冷剂不同，其自身分子量小，因此，完全不能期望其有润滑性能。运也促使人们要求使用烃制冷剂的制冷机用润滑剂具有优异的润滑性能。
虽然说制冷机用润滑剂一般在密闭系统中使用，但由于其通常暴露于高温和低温重复进行的制冷循环中，因此，还要求其不易劣化、稳定性好。
发明的公开
本发明是为了解决上述问题而进行的。本发明的目的是提供一种用于使用低分子量烃制冷剂的制冷机的润滑剂，该润滑剂与所述制冷剂的相溶性优异且其润滑性、稳定性也优异。
本发明者为寻求与烃制冷剂的相容性良好的矿物油系润滑剂进行了深入的研究，结果发现，以具有特定物理性状和成分组成的矿物油为主要成分的润滑剂与烃制冷剂的相溶性优异、在烃制冷剂的存在下稳定性、润滑剂性异，由此完成了本发明。
即，本发明是一种以具有以下特性的矿物油为主要成分的用于使用烃制冷剂的压缩式制冷机的润滑剂：在40℃的运动粘度为5-150mm2/s(cSt)、流点在-25℃以下、粘度指数在50以上、由n-d-M环分析法测得的％Cp和％CA分别在50以上和在12以下、氮含量在20ppm以下，硫含量为0.02-0.3％，碘价为10g I2/100g以下。
此外，本发明还是一种由1-5个碳原子的烃化合物组成的至少一种烃制冷剂与上述润滑剂混合而成的用于压缩式制冷机的工作流体组合物以及充填有该工作流体组合物的制冷装置。
上述润滑剂最好还含有磷酸酯极压剂和/或酚系或胺系抗氧化剂。
以上述矿物油为主要成分的润滑剂与烃制冷剂的相溶性优异、对压缩机滑动部的耐磨耗性高且稳定性优异。
实施本发明的最佳方式
用于本发明的矿物油在40℃的运动粘度为3-150mm2/s。若该运动粘度低，则压缩机的密封性和润滑性下降，而若运动粘度高，则流点过高，能量效率也下降。因此，最好为5-100mm2/s。
此外，矿物油的流点在-25℃以下。若流点高，则与制冷剂一起被压缩机吐出的润滑剂的流动性在膨胀机构或蒸发器等中下降并在制冷设备的低温部分滞留，可能导致导热效率下降或引起由压缩机内的润滑剂不足而产生的轴承磨耗、咬粘等。
此外，矿物油的粘度指数在50以上。在制冷循环中，润滑剂在较大的温度范围内被使用，即，它被压缩机吐出时达到高温，然后在膨胀机构的出口被暴露于低温。因此，希望有一种由温度导致的粘度变化小的高粘度指数润滑剂，即，一种粘度指数高的矿物油。一般地，长链烃含量高的润滑剂的粘度指数高，润滑性能也高。矿物油的粘度指数最好在80以上。
根据n-d-M环分析法测得的矿物油的％Cp在50以上，％CA在12以下。润滑剂中的链烃的含量越高，换言之，使用％Cp值大的矿物油，则润滑剂的润滑性越大，因此，即使被润滑性差的低分子量烃制冷机稀释，也能保持充分的润滑性，轴承不易出现磨耗和咬粘等。％Cp在80％以上则更佳。此外，％CA对粘度指数的影响大，％CA增大，则粘度指数下降，因此，是不适宜的。％CA更好地在10以下。％Cp和％CA可根据ASTM D3238中定义的n-d-M环分析法求出。
矿物油中所含的氮和硫会影响润滑油的性能。由于氮含量超过20重量ppm时，色相的稳定性会变差，因此，氮含量宜在20重量ppm以下。此外，硫含量为0.02-0.3重量％，以0.02-0.1重量％为佳。若硫含量大，则腐蚀性增大，而若硫含量小，则润滑性下降，因此，将硫含量保持在上述范围内是很重要的。
用于本发明的制冷机用润滑剂的矿物油的碘价在10gI2/100g以下，以确保其对劣化的稳定性。若碘价超过10gI2/100g，则稳定性变差。
本发明中使用的烃制冷剂是1-5个碳原子的低分子量烃化合物。具体例子有甲烷、乙烷、丙烷、正丙烷、异丁烷、正戊烷、异戊烷、新戊烷等烷烃化合物和环丙烷、环丁烷、环戊烷等环烷烃化合物。还可使用一部分碳键为双键的上述化合物的衍生物(对应于上述化合物的烯烃)。此外，作为烃制冷剂，这些化合物可单独使用，也可将二种以上适当组合后使用。
在使用低分子量烃制冷剂的压缩制冷机中将具有上述物性的矿物油组合后使用，可发挥本发明的效果。即，上述矿物油在烃制冷剂的存在下具有上述良好的润滑性和稳定性，而且，由于上述矿物油与烃化合物制冷剂在分子结构上的类似性远胜于酯油或醚油，因此，它们还具有良好的相溶性。此外，上述矿物油的价格比酯油和醚油低廉，因此，在实用方面也非常有用。
本发明的润滑剂可视需要含有其他成分。例如，可适当掺入周知的制冷机用润滑剂基油(如本发明中使用的上述矿物油以外的矿物油，例如，环烷系矿物油)或合成油(如烷基苯油、醚油、酯油、氟化油等)和周知的添加剂。该添加剂的例子有2,6-二叔丁基苯酚、2,6-二叔丁基-对甲酚、4,4-亚甲基-二(2,6-二叔丁基-对甲酚)、p,p′-二辛基-二苯基胺等酚系或胺系抗氧化剂、缩水甘油苯醚、缩水甘油烷基醚等稳定剂、磷酸三甲苯酯、磷酸三苯酯等极压剂、甘油一油酸酯、甘油油基醚、甘油一月桂基醚等油性剂、苯并三唑等金属灭活剂、聚二甲硅氧烷、聚丙烯酸甲基丙烯基酯等消泡剂或制泡剂等。此外，视需要，还可掺入周知的分散剂、粘度指数改善剂、防锈剂、防腐蚀剂、降流点剂等添加剂。这些添加剂在本发明润滑剂中的掺入量通常为10重量ppm～10重量％左右。尤其是添加约0.01-0.5重量％左右的酚系或胺系抗氧化剂，可大幅改善润滑剂的稳定性和耐久性。此外，磷酸三甲苯酯、磷酸三苯酯等磷酸酯可用作极压剂，少量添加(例如0.05-1.0重量％)，可有效改善咬粘负荷、耐磨耗等润滑性能。
实施例
下面通过实施例对本发明作更详细的说明，但本发明不限于这些具体例子。用于评价的油
为评价本发明的制冷机用润滑剂，准备好具有分别由表1和表2所示的物性和组成的矿物油1-8和硬质烷基苯(HAB)1-2，用于下述评价试验。其中，矿物油1-3和6相当于本发明的润滑剂基油。
                            表1
                                     矿物油
    1     2     3     4     5     6     7     8
颜色(ASTM)   L0.5   L0.5   L0.5   L0.5   L1.0   L0.5   L0.5   L0.5
运动粘度(mm2/s)   21.95   14.83   9.89   13.69   27.15   27.1   26.5   25.5
粘度指数     1.2     96    84     33    101    101    103   102
％Cp     63     61    59     43     66    66    68    67
％CA     9     10    10     14     5.1    5.1    4.8    4.7
流点(℃)   -27.5   -27.5   -27.5   -45.0   -27.5   -27.5    -30    -30
氮含量(重量ppm)    11     8     7   ＜1     28     3    10     5
硫含量(重量％)   0.15   0.12   0.08   0.04    0.2    0.2    0.33    0.2
总酸值(mgKOH/g)   0.01   0.01   0.01   0.01    0.01    0.01    0.01    0.01
碘价(gI2/100g)   7.6    4.8    2.2   4.5     7.5     7.5    6.8    11.2
“＜XX”表示小于XX。
                            表2
             HAB
    1     2
颜色(ASTM)     L0.5     L0.5
运动粘度(mm2/s)     14.97     9.99
粘度指数     -14      5
％Cp      -       -
％CA      -       -
流点(℃)     ＜-50.0     ＜-50.0
氮含量(重量ppm)     ＜1     ＜1
硫含量(重量％)     ＜0.01     ＜0.01
总酸值(mgKOH/g)     0.01     0.01
碘价(gI2/100g)      -       -
“＜XX”表示小于XX。性能评价试验
以矿物油1-4和HAB1-2的基油为润滑剂、以异丁烷(R600a)为制冷机，进行实用性能、润滑性(Falex咬粘负荷)和与制冷剂的相溶性等性能的评价试验。
润滑剂的实用性能的性能评价试验是通过使用冰箱用压缩机的制冷循环而进行的耐久试验。即，将包含上述基油的各润滑剂200g和R600a制冷剂15g装入压缩机中，将压缩机吐出压保持在12kgf/cm2、压缩机表面温度保持在80℃进行1000小时运转。该耐久试验结束后，将压缩机打开，取出试验后的润滑剂(即，使用油)，测定颜色和总酸值，再将压缩机卸开，测定活塞、气缸、连杆和轴承的磨耗量。
还对作为润滑性的Falex咬粘负荷和与制冷剂的相溶性(二层分离温度)进行了评价。结果见表3。
                             表3
                    矿物油           HAB
    1     2     3     4     1     2
使用油的性状 颜色(ASTM)  L1.5  L1.5  L1.5  L2.0  L1.5  L1.5
总酸值mgKOH/g  0.01  0.01  0.01  0.04  0.03  0.03
压缩机部件的磨耗量(μm) 活塞(铁) ＜1.0 ＜1.0 ＜1.0  2.1  2.5  2.9
气缸(铁) ＜1.0 ＜1.0 ＜1.0 ＜1.0 ＜1.0  1.3
连杆(铝合金) ＜1.0 ＜1.0 ＜1.0  4.2  4.9  5.6
轴承(铁) ＜1.0 ＜1.0 ＜1.0  1.2  1.7  2.6
Falex咬粘负荷(Lbf) 440  430  400  300  280  250
二层分离温度℃(制冷剂R600a) ＜-40 ＜-40 ＜-40 ＜-40 ＜-40 ＜-40
“＜XX”表示小于XX。
根据表3，本发明的润滑剂(矿物油1-3)的颜色均较低，为L1.0，总酸值均为0.01mgKOH/g，与新油时的值没有变化，而且，压缩机部件(活塞、气缸、连杆和轴承)的磨耗量均在1.0μm以下。而对应于比较例的矿物油4和HAB1-2的这些值几乎都大于实施例的值，表明出现润滑剂劣化和压缩机部件磨耗。稳定性试验(高压储气瓶试验)
用下述方法进行矿物油1-8的稳定性试验(轰击试验)。分别将矿物油1-8各100g和异丁烷(R600a制冷剂)20g装入300ml的高压储气瓶中，再加入作为催化剂的铁(Fe)、铜(Cu)、铝(Al)的金属丝(1.6mmφ×20cm)，密封，在175℃保持30日。放置冷却后，从高压储气瓶中取出矿物油1-8和催化剂，用肉眼观察劣化后的矿物油颜色、油渣析出程度及各催化剂表面的变化。催化剂的变色程度用“大”、“中”、“小”和“无”4档进行评价，油渣的析出程度用“多”、“中”、“少”和“无”4档进行评价。结果见表4。
                            表4
                                    矿物油
    1     2     3     4     5     6     7     8
   颜色(ASTM)  L1.5   L1.5   L1.5   L2.0   L4.5   L1.5   L3.0   L3.0
催化剂的变色     Fe     无     无     无     小     中     无     小     小
    Cu     无     无     无     小     中     无     中     小
    Al     无     无     无     无     无     无     无     无
油渣析出     无     无     无     无     多     无     无     少
根据表4，本发明的润滑剂(矿物油1-3和6)在所有项目均显示出令人满意的稳定性，但在粘度指数、％Cp、氮含量、硫含量％和碘价方面不能满足一个或多个规定值的润滑剂(矿物油4-5和7-8)的颜色差，在L2.0以上，还出现催化剂的变色和油渣析出。添加剂添加效果的评价
为评价添加剂的添加效果，将作为极压剂的磷酸三甲苯酯(TCP)和作为抗氧化剂的2,6-二叔丁基-对甲苯(DBPC)按表5所示比例添加到矿物油1中，配制试验油1-3，进行与前述同样的稳定性试验(高压储气瓶试验)，再测定Falex咬粘负荷。结果见表5。
                            表5
             试    验    油
    1     2     3
添加剂和添加量(重量％) 抗氧化剂(DBPC)     0.5     -     0.5
极压剂(TCP)      -     0.1     0.1
高压储气瓶试验 颜色(ASTM)     L1.5     L1.5     L1.5
    催化剂的变色     Fe     无     无     无
    Cu     无     无     无
    Al     无     无     无
油渣析出     无     无     无
使用矿物油1作为基油
上述基油、使用油和压缩机部件的各种测定试验方法具体如下：颜色按JIS K2580d ASTM颜色试验方法测定，运动粘度和粘度指数按JIS K2283法测定，％CP和％CA按ASTM D3238中规定的n-d-M环分析法测定，流点按JIS K 2269法测定，总酸值按JIS K 2501法测定，氮含量按JIS K 2609法测定，硫含量按JIS K 2541法测定，Falex咬粘负荷按ASTMD 3233法测定，与制冷剂的相溶性(二层分离温度)按JIS K 2211法(附件3，但需将R12读作R600a)测定。
由于本发明的制冷机用润滑剂以具有特定物性和成分组成的矿物油为主要成分，因此，与烃制冷剂的相溶性优异，在烃制冷剂的存在下，其稳定性、润滑性优异。因此，作为对地球环境友善的使用烃制冷剂的制冷机的润滑剂是非常有用的。

Claims (4)

1．润滑剂，用于使用烃制冷剂的压缩式制冷机，其特征在于，以在40℃的运动粘度为5-150mm2/s、流点在-25℃以下、粘度指数在50以上、由n-d-M环分析法测得的％Cp和％CA分别在50以上和在12以下、氮含量在20ppm以下、硫含量为0.02-0.3％、碘价为10gI2/100g以下的矿物油为主要成分。
2．如权利要求1所述的润滑剂，它还含有由磷酸酯组成的极压剂和/或酚系或胺系抗氧化剂。
3．用于压缩式制冷机的工作流体组合物，其特征在于，由1-5个碳原子的烃化合物组成的至少一种烃制冷剂和以在40℃的运动粘度为5-150mm2/s、流点在-25℃以下、粘度指数在50以上、由n-d-M环分析法测得的％Cp和％CA分别在50以上和在12以下、氮含量在20ppm以下、硫含量为0.02-0.3％、碘价为10gI2/100g以下的矿物油为主要成分的润滑剂组成。
4．制冷装置，由压缩机、冷凝器、干燥器、膨胀机构和蒸发器构成，其特征在于，充填有由1-5个碳原子的烃化合物组成的至少一种烃制冷剂和以在40℃的运动粘度为5-150mm2/s、流点在-25℃以下、粘度指数在50以上、由n-d-M环分析法测得的％Cp和％CA分别在50以上和在12以下、氮含量在20ppm以下、硫含量为0.02-0.3％、碘价为10gI2/100g以下的矿物油为主要成分的润滑剂组成的工作流体组合物。
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