KR100648186B1 - Lubricant For Compression Type Refrigeration System Using Hydrocarbon Refrigerant - Google Patents

Lubricant For Compression Type Refrigeration System Using Hydrocarbon Refrigerant Download PDF

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Publication number
KR100648186B1
KR100648186B1 KR1020007013422A KR20007013422A KR100648186B1 KR 100648186 B1 KR100648186 B1 KR 100648186B1 KR 1020007013422 A KR1020007013422 A KR 1020007013422A KR 20007013422 A KR20007013422 A KR 20007013422A KR 100648186 B1 KR100648186 B1 KR 100648186B1
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South Korea
Prior art keywords
lubricant
less
hydrocarbon
mineral oil
refrigerant
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KR1020007013422A
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Korean (ko)
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KR20010052428A (en
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가이마이다까시
다까하시히도시
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쟈판에나지 덴시자이료 가부시키가이샤
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    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M169/00—Lubricating compositions characterised by containing as components a mixture of at least two types of ingredient selected from base-materials, thickeners or additives, covered by the preceding groups, each of these compounds being essential
    • C10M169/04—Mixtures of base-materials and additives
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    • C10M101/00—Lubricating compositions characterised by the base-material being a mineral or fatty oil
    • C10M101/02—Petroleum fractions
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    • C10M129/00—Lubricating compositions characterised by the additive being an organic non-macromolecular compound containing oxygen
    • C10M129/02—Lubricating compositions characterised by the additive being an organic non-macromolecular compound containing oxygen having a carbon chain of less than 30 atoms
    • C10M129/04—Hydroxy compounds
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    • C10M129/02—Lubricating compositions characterised by the additive being an organic non-macromolecular compound containing oxygen having a carbon chain of less than 30 atoms
    • C10M129/04—Hydroxy compounds
    • C10M129/10—Hydroxy compounds having hydroxy groups bound to a carbon atom of a six-membered aromatic ring
    • C10M129/14—Hydroxy compounds having hydroxy groups bound to a carbon atom of a six-membered aromatic ring containing at least 2 hydroxy groups
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    • C10M133/02—Lubricating compositions characterised by the additive being an organic non-macromolecular compound containing nitrogen having a carbon chain of less than 30 atoms
    • C10M133/04—Amines, e.g. polyalkylene polyamines; Quaternary amines
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    • C10M2203/1006—Petroleum or coal fractions, e.g. tars, solvents, bitumen used as base material
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    • C10M2203/10—Petroleum or coal fractions, e.g. tars, solvents, bitumen
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    • C10M2203/10—Petroleum or coal fractions, e.g. tars, solvents, bitumen
    • C10M2203/108—Residual fractions, e.g. bright stocks
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    • C10N2040/34—Lubricating-sealants
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2040/00—Specified use or application for which the lubricating composition is intended
    • C10N2040/36—Release agents or mold release agents
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2040/00—Specified use or application for which the lubricating composition is intended
    • C10N2040/38—Conveyors or chain belts
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2040/00—Specified use or application for which the lubricating composition is intended
    • C10N2040/40—Generators or electric motors in oil or gas winning field
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2040/00—Specified use or application for which the lubricating composition is intended
    • C10N2040/42—Flashing oils or marking oils
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2040/00—Specified use or application for which the lubricating composition is intended
    • C10N2040/44—Super vacuum or supercritical use
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2040/00—Specified use or application for which the lubricating composition is intended
    • C10N2040/50—Medical uses

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  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Lubricants (AREA)

Abstract

본 발명은,40℃에 있어서 동점도(動粘度)가 3∼150㎟/s, 유동점이 -25℃이하, 점도지수가 50이상, n-d-M환분석에 의한 %Cp가 50%이상 및 %CA가 12이하, 질소분이 20ppm이하, 황분이 0.02∼0.3% 및 요드가가 10gI2/100g이하인 광물유(鑛物油)를 주성분으로 하는, 저급 탄화수소냉매를 사용하는 압축식 냉동기용의 윤활제, 그 윤활제와 저급 탄화수소냉매로부터 이루어지는 냉동기용의 작동유체 조성물, 및 그 작동유체 조성물이 충전되어 있는 냉동장치이다. 본 발명의 윤활제는, 탄화수소냉매와의 상용성이 우수하고, 안정성, 윤활성이 우수한 것으로부터, 오존층 파괴, 지구온난화의 우려가 없는 탄화수소냉매를 사용하는 냉동기의 윤활제로서 매우 유용하다.The present invention has a kinematic viscosity of 3 to 150 mm 2 / s at 40 ° C, a pour point of -25 ° C or less, a viscosity index of 50 or more,% C p of 50% or more and% C A by ndM ring analysis. Lubricants for compressed refrigerators using low-grade hydrocarbon refrigerants, the lubricants of which are mainly composed of mineral oils having a value of 12 or less, 20 ppm or less of nitrogen, 0.02 to 0.3% of sulfur, and 10 gI 2 / 100g of iodine. A working fluid composition for a refrigerator made of a lower hydrocarbon refrigerant, and a refrigerating device filled with the working fluid composition. The lubricant of the present invention is very useful as a lubricant for a refrigerator using a hydrocarbon refrigerant having excellent compatibility with hydrocarbon refrigerants, excellent stability and lubricity, and no ozone layer destruction and global warming.

Description

탄화수소냉매를 사용하는 압축식 냉동기용 윤활제{Lubricant For Compression Type Refrigeration System Using Hydrocarbon Refrigerant}Lubricant For Compression Type Refrigeration System Using Hydrocarbon Refrigerant}

본 발명은, 오존층을 파괴할 우려가 없고, 또한, 지구온난화능(地球溫暖化能)도 할로겐 함유 탄화수소냉매보다도 훨씬 낮은 저급탄화수소로부터 이루어지는 탄화수소냉매를 사용하는 압축식 냉동기용의 윤활제에 관한다. 또한, 본 발명은, 상기 탄화수소냉매와 상기 윤활제로부터 이루어지는 작동유체 조성물, 및 그 작동유체 조성물이 충전된 냉동장치에 관한다.The present invention relates to a lubricant for a compressed refrigerator using a hydrocarbon refrigerant composed of lower hydrocarbons, which has no fear of destroying the ozone layer and whose global warming capacity is much lower than that of the halogen-containing hydrocarbon refrigerant. The present invention also relates to a working fluid composition comprising the hydrocarbon refrigerant and the lubricant, and a refrigerating device filled with the working fluid composition.

압축식 냉동기는, 압축기, 응축기, 팽창기구(예컨데, 팽창밸브), 증발기 등으로 이루어지고, 휘발성이 높은 냉매가 증발할 때에 주위로부터 증발열을 제거하는 성질을 이용하여 냉각을 행하여, 냉장고, 냉동고, 공조(空調), 쇼우케이스, 청량음료나 아이스크림 등의 자동판매기 등에 사용되고 있다. 더욱이, 공조나 자동판매기 등에서는 응축할 때에 생기는 열을 이용하여 난방을 행하거나, 음료나 식품을 가열 보지하는 것에도 이용되고 있다.The compressor is composed of a compressor, a condenser, an expansion mechanism (e.g., an expansion valve), an evaporator, etc., and performs cooling by using a property of removing evaporation heat from the surroundings when a highly volatile refrigerant evaporates. It is used in air-conditioning, showcases, vending machines such as soft drinks and ice cream. Moreover, in air-conditioning, vending machines, etc., it is used also for heating using the heat which arises when condensing, or heating and holding a drink or food.

종래, 전기 냉매로서는 트리클로로플루오로메탄(R11), 디클로로디플루오로메탄(R12),클로로디플루오로메탄(R22) 등의 염소를 함유하는 불화탄화수소(CFC 또는 HCFC)가 사용되어 왔다. 그러나, 이것들의 CFC 및 HCFC는 오존층을 파괴하는 환경 문제를 일으키기 때문에, 국제적으로 그 생산 및 사용이 규제되고, 현재로서는, 염소를 함유하지 않는, 예컨데, 디플루오로메탄(R32), 테트라플루오로에탄(R134 또는 R134a), 디플루오로에탄(R152 또는 R152a)등의 비염소계 불화탄화수소(HFC)로 변환되어 오고 있다. 그러나, 이것들의 HFC는, 오존층을 파괴하지 않지만, 지구온난화능이 높기 때문에 지구환경보호의 장기적인 관점으로부터 문제를 안고 있다고 염려되고 있다.Conventionally, as the electric refrigerant, fluorinated hydrocarbons (CFC or HCFC) containing chlorine such as trichlorofluoromethane (R11), dichlorodifluoromethane (R12), and chlorodifluoromethane (R22) have been used. However, since these CFCs and HCFCs cause environmental problems that destroy the ozone layer, their production and use are regulated internationally and currently do not contain chlorine, for example, difluoromethane (R32), tetrafluoro Non-chlorine fluorinated hydrocarbons (HFC) such as ethane (R134 or R134a) and difluoroethane (R152 or R152a) have been converted. However, although these HFCs do not destroy the ozone layer, they are concerned that they have problems from the long-term perspective of global environmental protection because they have high global warming ability.

그래서, 탄소수 1∼5정도의 저분자량의 저급탄화수소나 암모니아 등은 오존층을 파괴하는 일 없이, 지구온난화능도 상기의 염소계 혹은 비염소계 불화탄화수소에 비교하여 매우 낮기 때문에, 환경에 부드러운 냉매로서 주목되어 오고 있다. 이것들의 화합물은, 냉매로서 종래 주류는 아니었지만 오래 전부터 사용되고 있던 실적도 있다. 또한, 상기의 탄화수소로부터 이루어지는 냉매의 윤활제로서는, 예컨대, 특개평10-130685호 공보에 의하면, 나프텐계 또는 파라핀계의 광물유, 알킬벤젠유, 에테르유, 에스테르유, 불소유 등의 합성유가 제시되고 있다. 이것들의 윤활제 중에서도, 합성유는 일반적으로 고가이기 때문에, 염가에 입수하기 쉬운 광물유가 실용적인 관점에서 기대되고 있다.Therefore, low molecular weight hydrocarbons, ammonia, and the like having 1 to 5 carbon atoms have a low global warming capacity compared with the above chlorine-based or non-chlorine-based fluorocarbons without destroying the ozone layer. Coming. Although these compounds are not mainstream as a refrigerant conventionally, there are also the results which have been used for a long time. Moreover, as a lubricant of the refrigerant | coolant which consists of said hydrocarbon, For example, according to Unexamined-Japanese-Patent No. 10-130685, synthetic oils, such as naphthenic or paraffinic mineral oil, alkylbenzene oil, ether oil, ester oil, fluorine oil, are proposed, have. Among these lubricants, synthetic oils are generally expensive, and mineral oils that are easy to obtain inexpensively are expected from a practical point of view.

그렇지만, 저분자량의 탄화수소냉매(저급 탄화수소냉매)와 광물유계 윤활제와의 조합에 의해서도, 여러 종의 문제가 있다. 특히 탄화수소냉매를 사용하는 냉동기용 윤활제로는 후술하는 이유로부터 그 자신이 우수한 윤활특성을 갖는 것이 요망되고 있다.However, there are various kinds of problems even with the combination of a low molecular weight hydrocarbon refrigerant (lower hydrocarbon refrigerant) and a mineral oil-based lubricant. In particular, as a lubricant for a refrigerator using a hydrocarbon refrigerant, it is desired to have excellent lubricating properties for the reasons described below.

냉매로서의 저분자량의 탄화수소와 윤활제로서의 광물유는 상용성은 있지만, 비중차가 크기 때문에 자연확산만으로는 양자가 섞이기 어려운 경우가 있다. 냉동기에 있어서, 이러한 섞이기 어려운 상태에 놓여지는 것이 자주 일어난다. 예컨대, 압축기에 냉매를 충전하는 경우, 먼저 장입(裝人)하여 있는 밀도가 큰 윤활제 위에 밀도가 작은 냉매가 겹쳐지는 형이 된다. 또한, 압축기의 정지 중에 냉매가 액체의 상태로 압축기 내로 돌아오는 소위 밀려들어 올 때에도 이러한 상태는 발생한다. 이와같은 상태에서 압축기를 기동하면, 원심력에 의해 윤활제가 회전의 외측에 모이고, 윤활을 필요로 하는 내부의 베어링 등의 접동부(摺動部)에 윤활제가 충분히 골고루 미치지 않는 상태로 되어, 접동부에 마모가 발생하거나, 눌어붙기 쉽게 된다는 문제를 가지고 있다. 이 때문에, 저분자량의 탄화수소냉매를 사용하는 냉동기용 윤활제로는, 우수한 윤활특성을 갖는 것이 요망되고 있다. 또한, 탄화수소냉매는, 분자 내의 염소에 의한 극압(極壓)효과를 기대할 수 있는 염소계 불화탄화수소 냉매와 다르고, 그 자신 분자량이 작기 때문에 윤활적인 성능은 전혀 기대할 수 없다. 이것도 탄화수소냉매를 사용하는 냉동기용의 윤활제에 우수한 윤활특성을 요구하는 것을 조장하고 있다.Although low molecular weight hydrocarbons as refrigerants and mineral oils as lubricants are compatible, they may be difficult to mix by natural diffusion only due to the large specific gravity difference. In a freezer, it often happens that it is placed in such a difficult state. For example, when a compressor is filled with a refrigerant, it is a type in which a small density refrigerant is superimposed on a high density lubricant charged first. This condition also occurs when the refrigerant is pushed back into the compressor in a liquid state during shutdown of the compressor. When the compressor is started in such a state, the lubricant collects on the outside of the rotation by centrifugal force, and the lubricant is not evenly spread evenly on sliding parts such as internal bearings requiring lubrication. It has a problem that the wear occurs easily or is easily pressed. For this reason, as a lubricant for refrigerators using a low molecular weight hydrocarbon refrigerant, it is desired to have excellent lubrication characteristics. In addition, the hydrocarbon refrigerant differs from the chlorine-based fluorohydrocarbon refrigerant capable of anticipating the extreme pressure effect of chlorine in the molecule, and since its molecular weight is small, no lubricating performance can be expected at all. This also encourages the demand for excellent lubrication characteristics for lubricants for refrigerators using hydrocarbon refrigerants.

또한, 냉동기용 윤활제는, 일반적으로 밀폐계로 사용된다라고 할 수 있고, 매우 고온과 저온을 반복하는 냉동사이클에 노출되기 때문에, 열화되기 어려운, 안정성이 좋은 것이 요구되고 있다.In addition, the lubricant for refrigerators is generally used in a hermetic system, and is exposed to a refrigeration cycle that repeats very high temperature and low temperature, and therefore, it is required to have good stability that is difficult to deteriorate.

·발명의 개시Initiation of invention

본 발명은 상기의 과제를 해결하기 위해서 이루어진 것이고, 본 발명의 목적 은, 저분자량의 탄화수소냉매를 사용하는 냉동기용의 윤활제에 있어서, 그 냉매와의 상용성이 우수하고, 또한 윤활성, 안정성에도 우수한 윤활제를 제공하는 것에 있다.The present invention has been made to solve the above problems, and an object of the present invention is to provide a lubricant for a refrigerator using a low molecular weight hydrocarbon refrigerant, having excellent compatibility with the refrigerant, and excellent lubricity and stability. It is to provide a lubricant.

본 발명자는, 탄화수소냉매와 성질이 잘 맞는 좋은 광물유계 윤활제를 예의 탐색, 검토하여, 특정의 물리성상 및 성분조성을 갖는 광물유를 주성분으로 하는 윤활제는, 탄화수소냉매와의 상용성이 우수하고, 탄화수소냉매의 존재하에 있어서 안정성, 윤활성이 우수한 것을 찾아내어, 본 발명을 완성하기에 이르렀다.MEANS TO SOLVE THE PROBLEM The present inventors earnestly searched and examined the good mineral oil type | system | group lubricant suitable for the nature with a hydrocarbon refrigerant, The lubricant which has a mineral oil as a main component which has a specific physical property and a component composition is excellent in compatibility with a hydrocarbon refrigerant, and a hydrocarbon refrigerant In the presence of, it was found that the stability and lubricity were excellent, and thus the present invention was completed.

즉, 본 발명은, 40℃에 있어서 동점도가 5∼150㎟/s(cSt), 유동점이 -25℃이하, 점도지수가 50이상 및 n-d-M환분석에 의한 %Cp가 50이상 및 %CA가 12이하, 질소분이 20ppm이하, 황분이 0.02∼0.3% 및 요드가가 10gI2/100g이하인 광물유를 주성분으로 하는 탄화수소냉매를 사용하는 압축식 냉동기용의 윤활제이다.That is, the present invention has a kinematic viscosity at 40 ° C. of 5 to 150 mm 2 / s (cSt), a pour point of -25 ° C. or less, a viscosity index of 50 or more and% C p of 50 or more and% C A by ndM ring analysis. It is 12 or less, and the jilsobun 20ppm or less, a sulfur minutes lubricant appointed compression refrigeration using a hydrocarbon refrigerant as the main component 0.02~0.3%, and the iodine is 10gI 2 / 100g or less mineral oil.

또한, 본 발명은, 탄소수1∼5의 탄화수소화합물로부터 이루어지는 적어도 1종의 탄화수소냉매와, 상기 윤활제로부터 이루어지는 압축식 냉동기에 사용하는 작동유체조성물이고, 게다가, 그 작동유체조성물을 충전한 냉동장치이다.The present invention is also a working fluid composition for use in at least one hydrocarbon refrigerant comprising a hydrocarbon compound having 1 to 5 carbon atoms and a compressed refrigerator comprising the lubricant, and a refrigeration apparatus filled with the working fluid composition. .

또한, 상기 윤활제로서는, 게다가 인산 에스테르로부터 이루어지는 극압제 및/또는 페놀계 또는 아민계 산화방지제를 더욱 함유하는 것이 바람직하다.Moreover, as said lubricant, it is preferable to further contain the extreme pressure agent which consists of phosphoric acid ester, and / or a phenol type or an amine antioxidant further.

이러한 광물유를 주성분으로 하는 윤활제는, 탄화수소냉매와의 상용성이 우수하고, 압축기 접동부재에 대하여 높은 내마모성을 가지며, 게다가 우수한 안정성을 나타낸다.Lubricants based on such mineral oils are excellent in compatibility with hydrocarbon refrigerants, have high wear resistance to compressor sliding members, and exhibit excellent stability.

·발명을 실시하기 위한 최량의 형태Best mode for carrying out the invention

본 발명에 사용하는 광물유는, 40℃에 있어서 동점도가 3∼150㎟/s이다. 그 동점도가 낮으면 압축기에 있어서 밀봉성 및 윤활성이 낮게 되고, 또한 높게 되면 유동점이 너무 높아지거나, 에너지 효율도 저하된다. 바람직하게는 5∼100㎟/s이다.The mineral oil used for this invention is 3-150 mm <2> / s of kinematic viscosity in 40 degreeC. When the kinematic viscosity is low, the sealability and lubricity are low in the compressor, and when the kinematic viscosity is high, the pour point is too high or the energy efficiency is also reduced. Preferably it is 5-100 mm <2> / s.

또한, 광물유는 -25℃이하의 유동점을 갖는다. 유동점이 높으면, 압축기로부터 냉매와 함께 토출된 윤활제가 팽창기구 또는 증발기 등에서 유동성이 저하되고, 냉동 설비의 저온부위에 체류하여 전열효율의 저하를 초래하거나, 압축기 내의 윤활제부족에 의한 베어링의 마모, 눌어붙음 등을 일으킬 우려가 있다.In addition, mineral oils have a pour point of -25 ° C or less. If the pour point is high, the lubricant discharged together with the refrigerant from the compressor decreases in fluidity in the expansion mechanism or the evaporator, and stays in the low temperature part of the refrigerating equipment, resulting in a decrease in heat transfer efficiency, or the wear of the bearing due to the lack of lubricant in the compressor. It may cause sticking.

또한, 광물유는, 50이상의 점도지수를 갖는다. 냉동 사이클에 있어서, 윤활제는 압축기 토출로 고온이 되고, 팽창기구의 출구에서 저온에 노출되어 비교적 넓은 온도 범위에서 사용된다. 따라서, 온도에 의한 점도변화가 적은 점도지수가 높은 윤활제, 즉 점도지수가 높은 광물유가 요망된다. 일반적으로 장쇄(長鎖)의 쇄상(鎖狀) 탄화수소가 많이 포함되는 윤활제는 점도지수가 높고, 윤활성능도 높아진다. 광물유의 점도지수는, 80이상이 보다 바람직하다.In addition, the mineral oil has a viscosity index of 50 or more. In the refrigeration cycle, the lubricant becomes hot at the compressor discharge and is exposed to low temperatures at the outlet of the expansion mechanism and used in a relatively wide temperature range. Therefore, a lubricant having a high viscosity index, ie, a mineral oil having a high viscosity index, with a low viscosity change due to temperature is desired. In general, lubricants containing a large number of long chain hydrocarbons have a high viscosity index and lubrication performance. As for the viscosity index of mineral oil, 80 or more are more preferable.

게다가, 광물유는, n-d-M환분석에 의한 %Cp가 50이상 및 %CA가 12이다. 윤활제는, 쇄상 탄화수소가 많이 포함될수록, 환언하면, %Cp의 값이 큰 광물유를 사용할수록 윤활성이 높아지기 때문에, 윤활성이 부족한 저분자량의 탄화수소냉매에 의해 희석되어도 충분한 윤활성을 보지할 수 있고, 베어링의 마모나 눌어붙음 등은 일어 나기 어렵게 된다. %Cp는 80이상이 보다 바람직하다. 또한, %CA의 값은 점도지수에 크게 영향을 주고, 이것이 커지면 점도지수가 낮아지기 때문에 바람직하지 않다. %CA는 10이하가 보다 바람직하다. 더욱이, %CP 및 %CA는, ASTM D3238로 규정되는 n-d-M환분석에 의해 구할 수 있다.In addition, the mineral oil has a% C p of 50 or more and a% C A of 12 by ndM ring analysis. Since the lubricant contains more chain hydrocarbons, in other words, the lubricity becomes higher as the mineral oil having a larger value of% C p is used, the lubricant can retain sufficient lubricity even when diluted with a low molecular weight hydrocarbon refrigerant having insufficient lubricity. Abrasion, seizure, etc., are difficult to occur. 80% or more of% Cp is more preferable. In addition, the value of% C A greatly influences the viscosity index, which is not preferable because the viscosity index becomes lower. As for% C A , 10 or less are more preferable. Moreover,% C P and% C A can be calculated | required by the ndM ring analysis prescribed | regulated by ASTMD3238.

또한, 광물유에 포함되는 질소분이나 황분은 윤활유의 특성에 영향을 미친다. 질소분은 20중량ppm을 넘으면 색상 안정성이 나빠지기 때문에, 20중량ppm이하로 한다. 또한, 황분은 0.02∼0.3중량%, 바람직하게는 0.02∼0.1%로 한다. 황분이 많으면, 부식성이 증가하고, 적으면 윤활성이 저하되기 때문에, 상기의 범위에서 황분을 함유시키는 것이 중요하다.In addition, nitrogen content and sulfur content contained in mineral oil affect the characteristics of lubricating oil. If the nitrogen content exceeds 20 ppm by weight, the color stability deteriorates, so it is 20 ppm by weight or less. The sulfur content is 0.02 to 0.3% by weight, preferably 0.02 to 0.1%. When there is much sulfur content, corrosiveness increases, and when it is few, lubricity falls, it is important to contain sulfur content in the said range.

게다가, 본 발명의 냉동기용 윤활제에 사용하는 광물유의 요드가는, 열화에 대한 안정성을 확보하기 위해서 10gI2/100g이하로 한다. 요드가가 10gI2/100g을 넘으면 안정성이 나빠진다.In addition, in order to ensure the stability of the iodine way, degradation of the mineral oil used in the lubricant Chiller the present invention will be 10gI 2 / 100g or less. If iodine exceeds 10gI 2 / 100g, the stability becomes worse.

본 발명에 사용하는 탄화수소냉매는, 탄소수 1∼5의 저분자량의 탄화수소 화합물이다. 구체적으로는, 메탄, 에탄, 프로판, n-부탄, i-부탄, n-펜탄, i-펜탄, 네오펜탄 등의 알칸화합물, 및 시클로프로판, 시클로부탄, 시클로펜탄 등의 시클로파라핀 화합물이 들어진다. 게다가, 일부의 탄소결합이 이중결합인 상기 화합물의 유도체(상기 화합물에 대응하는 올레핀)도 사용할 수 있다. 또한, 탄화수소냉매로서, 이것들의 화합물은 단독으로 사용하는 것도, 2종 이상을 적의 조합하여 사용할 수도 있다.The hydrocarbon refrigerant used in the present invention is a hydrocarbon compound having a low molecular weight of 1 to 5 carbon atoms. Specifically, alkanes such as methane, ethane, propane, n-butane, i-butane, n-pentane, i-pentane and neopentane, and cycloparaffin compounds such as cyclopropane, cyclobutane and cyclopentane are contained. . In addition, derivatives of the compounds (olefins corresponding to the compounds) in which some carbon bonds are double bonds can also be used. In addition, as a hydrocarbon refrigerant, these compounds may be used individually or may be used in combination of 2 or more types.

저분자량의 탄화수소냉매를 사용하는 압축냉동기에 상기의 물성을 갖는 광물유를 조합하여 사용하는 것에 의해, 본 발명의 효과는 발휘된다. 즉, 전기 광물유는, 탄화수소냉매의 존재하에 있어서 상기의 양호한 윤활성 및 안정성을 나타내는 것은 원래부터, 상기 광물유는 탄화수소화합물 냉매와 분자구조가 에스테르유나 에테르유보다도 훨씬 유사하기 때문에 양호한 상용성을 나타낸다. 또한, 상기 광물유는 에스테르유나 에테르유에 비교하여 염가이기 때문에 실용적인 면에서도 매우 유용하다.The effect of this invention is exhibited by using the mineral oil which has said physical property in combination in the compression refrigerator using a low molecular weight hydrocarbon refrigerant. In other words, the electric mineral oil exhibits the above good lubricity and stability in the presence of a hydrocarbon refrigerant. Since the mineral oil has a molecular structure much similar to that of the ester compound and the ether oil, the mineral oil shows good compatibility. In addition, the mineral oil is very useful in terms of practical use because it is inexpensive compared with ester oil or ether oil.

본 발명의 윤활제는, 필요에 응하여 다른 성분을 함유해도 좋다. 예컨대, 본 발명에서 사용하는 상술한 광물유 이외의 광물유(예컨대, 나프텐계 광물유), 알킬벤젠유, 에테르유, 에스테르유, 불소유 등의 합성유 등 주지의 냉동기용 윤활제 기유나, 주지의 첨가제를 적의 배합해도 좋다. 그 첨가제로서는, 2,6-디-터셔리-부틸페놀, 2,6-디-터셔리-부틸-p-크레졸, 4,4-메틸렌-비스-(2,6-디-터셔리-부틸-p-크레졸), p,p'-디-옥틸-디-페닐아민 등의 페놀계 또는 아민계의 산화방지제, 페닐글리시딜에테르, 알킬글리시딜에테르 등의 안정제, 트리크레실포스페이트, 트리페닐포스페이트 등의 극압제, 글리세린모노올레이트, 글리세린모노올레일에테르, 글리세린모노라우릴에테르 등의 유성제, 벤조트리아졸 등의 금속 불활성화제, 폴리디메틸실록산, 폴리메타크릴아크릴레이트 등의 소포제(消泡劑) 또는 제포제(制泡劑) 등이 들어진다. 그 외, 주지의 청정분산제, 점도지수향상제, 방청제, 부식방지제, 유동점 강하제 등의 첨가제도 필요에 응하여 배합할 수 있다. 이것들의 첨가제는, 통상 본 발명의 윤활제에 10중량ppm~10중량%정도 함유되도록 배합된다. 특히, 페놀계 또 는 아민계의 산화방지제는, 0.01∼0.5중량%정도 첨가하는 것에 의해, 윤활제의 안정성, 내구성을 대폭 개선한다. 또한, 트리클레질포스페이트, 트리페닐포스페이트 등의 인산 에스테르는 극압제로서 유용하고, 소량의 첨가(예컨대, 0.05∼1.0중량%)로 눌어붙기 하중, 내마모 등의 윤활 특성을 효과적으로 향상한다.The lubricant of this invention may contain another component as needed. For example, well-known refrigerating lubricant base oils and well-known additives, such as mineral oils (for example, naphthenic mineral oil), alkylbenzene oil, ether oil, ester oil, fluorine oil, etc. other than the mineral oil mentioned above used suitably You may mix | blend. As the additive, 2,6-di-tert-butylphenol, 2,6-di-tert-butyl-p-cresol, 4,4-methylene-bis- (2,6-di-tert-butyl) phenolic or amine-based antioxidants such as -p-cresol), p, p'-di-octyl-di-phenylamine, stabilizers such as phenylglycidyl ether and alkylglycidyl ether, tricresyl phosphate, Extreme pressure agents such as triphenylphosphate, oily agents such as glycerin monooleate, glycerin monooleyl ether, glycerin monolauryl ether, metal deactivators such as benzotriazole, antifoaming agents such as polydimethylsiloxane and polymethacrylate (I) or a defoamer. In addition, additives, such as a well-known clean dispersant, a viscosity index improver, a rust preventive agent, a corrosion inhibitor, a pour point depressant, can also be mix | blended as needed. These additives are mix | blended so that about 10 weight%-about 10 weight% may be contained in the lubricant of this invention normally. In particular, by adding about 0.01 to 0.5% by weight of the phenol- or amine-based antioxidant, the stability and durability of the lubricant are greatly improved. In addition, phosphate esters such as triclezyl phosphate and triphenyl phosphate are useful as extreme pressure agents, and effectively improve lubrication characteristics such as crushing load and abrasion resistance with a small amount of addition (for example, 0.05 to 1.0% by weight).

이하에, 실시예를 나타내고, 본 발명을 더욱 자세하게 설명하는데, 본 발명은 이들의 구체적인 예시에 제한되는 것은 아니다.Although an Example is shown to the following and this invention is demonstrated in more detail, this invention is not restrict | limited to these specific examples.

평가를 위해 사용한 기름[油]Oil used for evaluation

본 발명의 냉동기용 윤활제를 평가하기 위해서, 표1 및 표2에 각각 나타내는 물성 및 조성을 갖는 광물유1∼8 및 하드형 알킬벤젠(HAB)1∼2를 준비하여, 후술하는 평가시험에 사용했다. 더욱이, 이 중에서, 광물유1∼3 및 6이, 본 발명의 윤활제의 기유(基油)에 상당한다.
In order to evaluate the refrigerator lubricant of the present invention, mineral oils 1 to 8 and hard alkylbenzene (HAB) 1 to 2 having physical properties and compositions shown in Tables 1 and 2, respectively, were prepared and used for the evaluation test described later. Moreover, among these, mineral oils 1-3 and 6 correspond to the base oil of the lubricant of this invention.

Figure 112000536618205-pct00001
Figure 112000536618205-pct00001

Figure 112000536618205-pct00002
Figure 112000536618205-pct00002

성능평가시험Performance Evaluation Test

윤활제로서 광물유1∼4 및 HAB 1∼2의 기유와, 냉매로서 i-부탄(R600a)을 사용하여, 실용성능, 윤활성(Falex 눌어붙기 하중) 및 냉매와의 상용성 등의 성능평가시험을 행했다.Performance evaluation tests such as practical performance, lubricity (Falex crushing load), and compatibility with the refrigerant were carried out using base oils of mineral oils 1 to 4 and HAB 1 to 2 as lubricants, and i-butane (R600a) as refrigerants. .

윤활제의 실용성능의 성능평가시험은, 냉장고용의 압축기를 사용한 냉동 사이클에 의한 내구시험에 따라 실시했다. 즉, 상기 기유에서 이루어지는 윤활제를 200g 및 R600a냉매를 15g 압축기에 장입하고, 압축기 토출압을 12kgf/㎠, 압축기 표면온도를 80℃로 유지하고 1000시간의 운전을 실시했다. 그 내구시험 종료 후, 압축기를 개방하고, 시험 후의 윤활제, 소위 사용유(使用油)를 채취하여 색 및 전산가(全酸價)를 측정하고, 게다가 압축기를 분해하여 피스톤, 실린더, 커넥팅로드 및 베어링의 마모량을 측정했다. The performance evaluation test of the practical performance of the lubricant was carried out in accordance with the durability test by the refrigeration cycle using a compressor for refrigerators. That is, 200 g and R600a refrigerant were charged into a 15 g compressor, and the compressor discharge pressure was 12 kgf / cm 2, and the compressor surface temperature was maintained at 80 ° C. for 1000 hours of operation. After the endurance test, the compressor is opened, the lubricant and so-called oil used after the test are taken, and the color and the total value are measured. Furthermore, the compressor is disassembled to form a piston, cylinder, connecting rod and bearing. The wear amount of the was measured.                 

게다가, 윤활성으로서 Falex 눌러붙기 하중 및 냉매와의 상용성(이층분리 온도)에 대해서도 평가했다. 이것들의 측정결과를 표3에 나타낸다.In addition, as the lubricity, the Falex adhesion load and the compatibility with the refrigerant (two-layer separation temperature) were also evaluated. Table 3 shows the results of these measurements.

Figure 112000536618205-pct00003
Figure 112000536618205-pct00003

표3에 의하면, 본 발명의 윤활제(광물유1∼3)는, 색이 모두 L1.0으로 낮고, 전산가는 모두 0.01mgKOH/g과 새 기름[新油]일 때의 값과 변함이 없으며, 게다가 압축기의 부재(피스톤, 실린더, 커넥팅로드 및 베어링)의 마모량이 모두 1.0㎛이하였다. 이것에 대하여 비교예에 상당하는 광물유4 및 HAB1∼2는, 이들의 값의 대부분이 실시예의 값보다 크고, 윤활제의 열화 및 압축기부재의 마모가 인정된다.According to Table 3, the lubricants (mineral oils 1 to 3) of the present invention were all low in L1.0, and the total value of the lubricants was 0.01 mg KOH / g and fresh oil. The amount of wear of the members of the compressor (pistons, cylinders, connecting rods, and bearings) was all 1.0 m or less. On the other hand, mineral oil 4 and HAB1-2 which correspond to a comparative example have most of these values larger than the value of an Example, and deterioration of a lubricant and abrasion of a compressor member are recognized.

안정성 시험(봄베테스트)Stability Test (Bombe Test)

또한, 광물유1∼ 8에 대해서 안정성시험(봄베테스트)을 다음과 같이 하여 행 했다. 광물유1∼8의 각각에 대해서, 300㎖의 봄베에 광물유100g과 이소부탄(R600a냉매) 20g을 넣고, 게다가 촉매로서 철(Fe), 동(Cu), 알루미늄(Al)의 철사(1.6mmø×20cm)를 넣어서 밀봉하여, 175℃에서 30일간 보지했다. 방치냉각 후, 봄베로부터 광물유1∼8 및 촉매를 꺼내어, 열화 후의 광물유의 색, 슬러지 석출의 정도, 및 각 촉매표면의 변화를 눈으로 관찰했다. 촉매의 변색량은 「대」,「중」,「소」및「없음」의 4단계로 평가하고, 슬러지석출의 정도는 「다」,「중」,「소」및「없음」의 4단계로 평가했다. 그 결과를 표4에 나타낸다.In addition, the stability test (bomb test) was performed on mineral oils 1-8 as follows. For each of mineral oils 1 to 8, 100 g of mineral oil and 20 g of isobutane (R600a refrigerant) are put in a 300 ml cylinder, and as a catalyst, iron (Fe), copper (Cu), and aluminum (Al) wire (1.6 mm ø × 20 cm) was put in and sealed, and it hold | maintained for 30 days at 175 degreeC. After standing to cool, the mineral oils 1 to 8 and the catalyst were taken out of the bomb, and the color of the mineral oil after deterioration, the degree of sludge deposition, and the change in the surface of each catalyst were visually observed. The amount of discoloration of the catalyst is evaluated in four stages of "large", "medium", "small" and "none", and the degree of sludge deposition is four stages of "high", "medium", "small" and "none". Rated by The results are shown in Table 4.

Figure 112000536618205-pct00004
Figure 112000536618205-pct00004

표4에 의하면, 본 발명의 윤활제(광물유1∼3 및 6)는, 모두의 항목에 만족할 수 있는 안정성을 나타냈는데, 점도지수, %Cp, 질소분, 황분% 및 요드가에 관한 규정치의 어느 것인가 하나 또는 복수를 만족하고 있지 않은 윤활제(광물유4∼5 및 7∼8)은, 색도 L2.0이상으로 나쁘고, 촉매의 변색, 슬러지의 석출도 인정된다.According to Table 4, the lubricants (mineral oils 1 to 3 and 6) of the present invention exhibited stability that satisfies all of the items, but the viscosity values,% C p , nitrogen content, sulfur content and% of the prescribed values for the iodine value Lubricants (mineral oils 4 to 5 and 7 to 8) that do not satisfy one or more than one are poor in chromaticity of L2.0 or more, and discoloration of the catalyst and precipitation of sludge are also recognized.

첨가제 첨가효과의 평가Evaluation of additive addition effect

게다가, 첨가제의 첨가효과를 평가하기 위해서, 광물유1에 극압제로서 트리 클레질포스페이트(TCP) 및 산화방지제로서 2,6-디-터셔리-부틸-p-클레졸(DBPC)을 표5에 나타내는 비율로 첨가하여 시험유1∼3을 조제하고, 전기와 같은 안정성시험(봄베테스트)을 행하고, 게다가 Falex 눌어붙기 하중을 측정했다. 그 결과를 표5에 나타낸다.In addition, in order to evaluate the effect of the addition of additives, Triclezylphosphate (TCP) as an extreme pressure agent in mineral oil 1 and 2,6-di-tertiary-butyl-p-clesol (DBPC) as an antioxidant are shown in Table 5. The test oils 1-3 were prepared by adding in the ratio shown, the stability test (bomb test) similar to the above was done, and Falex press load was also measured. The results are shown in Table 5.

Figure 112000536618205-pct00005
Figure 112000536618205-pct00005

더욱이, 상기 기유, 사용유 및 압축기부재에 관하는 각종 측정시험방법은 다음의 방법에 따라 실시했다. 색은 JIS K 2580의 ASTM색 시험방법에, 동점도 및 점도지수는 JIS K 2283에, %Cp 및 %CA는 ASTM D3238로 규정되는 n-d-M환분석에, 유동점은 JIS K 2269에, 전산가는 JIS K 2501에, 질소분은 JIS K 2609에, 황분은 JIS K 2541에, Falex 눌어붙기 하중은 ASTM D 3233에, 및 냉매와의 상용성(이층분리온도)은 JIS K 2211(부속서3, 단, R12를 R600a로 대체하여 적용했다.)에 각각 준거하여 구했다.Moreover, various measurement test methods for the base oil, used oil and compressor member were carried out according to the following method. Color is ASTM K test method of JIS K 2580, kinematic viscosity and viscosity index are JIS K 2283,% C p and% C A are ndM ring analysis defined by ASTM D3238, pour point is JIS K 2269, and computational value is JIS K 2501, nitrogen content in JIS K 2609, sulfur content in JIS K 2541, Falex adhesion load in ASTM D 3233, and compatibility with refrigerants (two-layer separation temperature) in JIS K 2211 (Annex 3, R12). Was replaced by R600a.).

본 발명의 냉동기용 윤활제는, 특정의 물성 및 성분조성을 갖는 광물유를 주 성분으로 하는 윤활제이기 때문에, 탄화수소냉매와의 상용성이 우수하고, 탄화수소냉매의 존재하에 있어서 안정성, 윤활성이 우수하다. 따라서, 지구환경에 부드러운 탄화수소냉매를 사용하는 냉동기의 윤활제로서 매우 유용하다.Since the refrigerator lubricant of the present invention is a lubricant mainly composed of mineral oil having specific physical properties and component compositions, it is excellent in compatibility with hydrocarbon refrigerants and excellent in stability and lubricity in the presence of hydrocarbon refrigerants. Therefore, it is very useful as a lubricant of a refrigerator using a hydrocarbon refrigerant that is gentle to the global environment.

Claims (6)

탄화수소냉매를 사용하는 압축식 냉매기용의 윤활제에 있어서, 40℃에 있어서 동점도가 3∼150㎟/s, 유동점이 -25℃이하, 점도지수가 50이상, n-d-M환분석에 의한 %Cp가 50이상 및 %CA가 12이하, 질소분이 20ppm이하, 황분이 0.02∼0.3% 및 요드가가 10gI2/100g이하인 광물유를 주성분으로 하는 것을 특징으로 하는 윤활제.Lubricants for compressed refrigerants using hydrocarbon refrigerants, having a kinematic viscosity of 3 to 150 mm 2 / s, a pour point of -25 ° C. or less, a viscosity index of 50 or more, and a% C p of 50 by ndM ring analysis at 40 ° C. or higher and% C a is less than or equal to 12, the jilsobun 20ppm or less, a sulfur minutes 0.02~0.3% and iodide is a lubricant comprising as a main component 10gI 2 / 100g or less mineral oil. 청구항1에 있어서,The method according to claim 1, 인산 에스테르로부터 이루어지는 극압제를 더욱 함유하는 윤활제.A lubricant further containing an extreme pressure agent made of a phosphate ester. 탄소수 1∼5의 탄화수소 화합물로부터 이루어지는 1종의 탄화수소냉매와, 40℃에 있어서 동점도가 5∼150㎟/s, 유동점이 -25℃이하, 점도지수가 50이상 및 n-d-M환분석에 의한 %Cp가 50이상 및 %CA가 12이하, 질소분이 20ppm이하, 황분이 0.02∼0.3% 및 요드가가 10gI2/100g이하인 광물유를 주성분으로 하는 윤활제로부터 이루어지는 것을 특징으로 하는 압축식 냉동기에 사용하는 작동유체조성물.One hydrocarbon refrigerant comprising a hydrocarbon compound having 1 to 5 carbon atoms, having a kinematic viscosity of 5 to 150 mm2 / s at 40 ° C, a pour point of -25 ° C or less, a viscosity index of 50 or more and% C p by ndM ring analysis. is less than 50 and% C a is less than or equal to 12, the jilsobun 20ppm or less, a sulfur-minute operation for use in compression refrigeration, characterized in that the 0.02~0.3%, and the iodine formed from the lubricant composed mainly of 10gI 2 / 100g or less mineral oil Fluid composition. 압축기, 응축기, 건조기, 팽창기구 및 증발기로부터 구성되는 냉동장치에 있어서, 탄소수1∼5의 탄화수소 화합물로부터 이루어지는 1종의 탄화수소냉매와, 40℃에 있어서 동점도가 5∼150㎟/s, 유동점이 -25℃이하, 점도지수가 50이상 및 n-d-M환분석에 의한 %Cp가 50이상 및 %CA가 12이하, 질소분이 20ppm이하, 황분이 0.02∼0.3% 및 요드가가 10gI2/100g이하인 광물유를 주성분으로 하는 윤활제로부터 이루어지는 작동유체 조성물이 충전되는 것을 특징으로 하는 냉동장치.In a refrigerating device comprising a compressor, a condenser, a dryer, an expansion mechanism, and an evaporator, one hydrocarbon refrigerant composed of a hydrocarbon compound having 1 to 5 carbon atoms, a kinematic viscosity of 5 to 150 mm 2 / s at 40 ° C., and a pour point − Mineral oil with 25 ° C or less, viscosity index of 50 or more and% C p of 50 or% C A by 12, nitrogen content of 20ppm, sulfur content of 0.02-0.3% and iodine value of 10gI 2 / 100g A refrigerating device, characterized in that the working fluid composition consisting of a lubricant containing as a main component is filled. 청구항 1에 있어서,The method according to claim 1, 페놀계 산화방지제를 더욱 함유하는 윤활제.A lubricant further containing a phenolic antioxidant. 청구항 1에 있어서,The method according to claim 1, 아민계 산화방지제를 더욱 함유하는 윤활제.A lubricant further containing an amine antioxidant.
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