WO2020230815A1 - 潤滑油組成物の検査方法およびその潤滑油組成物の製造方法 - Google Patents
潤滑油組成物の検査方法およびその潤滑油組成物の製造方法 Download PDFInfo
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- WO2020230815A1 WO2020230815A1 PCT/JP2020/019104 JP2020019104W WO2020230815A1 WO 2020230815 A1 WO2020230815 A1 WO 2020230815A1 JP 2020019104 W JP2020019104 W JP 2020019104W WO 2020230815 A1 WO2020230815 A1 WO 2020230815A1
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- lubricating oil
- oil composition
- particle size
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- average particle
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
- G01N23/20—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by using diffraction of the radiation by the materials, e.g. for investigating crystal structure; by using scattering of the radiation by the materials, e.g. for investigating non-crystalline materials; by using reflection of the radiation by the materials
- G01N23/201—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by using diffraction of the radiation by the materials, e.g. for investigating crystal structure; by using scattering of the radiation by the materials, e.g. for investigating non-crystalline materials; by using reflection of the radiation by the materials by measuring small-angle scattering
Definitions
- the present invention relates to a method for inspecting a lubricating oil composition and a method for producing the lubricating oil composition.
- the present application claims priority based on Japanese Patent Application No. 2019-092842 filed in Japan on May 16, 2019, the contents of which are incorporated herein by reference.
- a lubricating oil composition that simultaneously improves multiple performances such as low friction, torque increase, and fuel efficiency is required.
- a lubricating oil composition is for an engine lubricating oil in which nanocarbon particles fullerene, an organic solvent, a viscosity index improver, an abrasion adjusting agent, and a cleaning dispersant are mixed with a lubricating base oil such as mineral oil or ester oil.
- Additive compositions are known (see, for example, Patent Document 1).
- fullerenes may be added to the lubricating oil composition used in the refrigerant compressor (see, for example, Patent Document 2).
- an important property of a lubricating oil composition is a wear coefficient, etc., but it takes time and effort to measure. Therefore, in the manufacturing process of the lubricating oil composition, the properties of the lubricating oil composition are specified by using the density, kinematic viscosity, viscosity index, pour point, total acid value, etc., which are easy to measure, as indexes (for example). See Non-Patent Document 1).
- the present invention has been made in view of the above circumstances, and even a lubricating oil composition containing fullerene can stably reproduce wear resistance characteristics by using a method that is relatively easy to measure. It is an object of the present invention to provide a method for inspecting a lubricating oil composition and a method for producing a lubricating oil composition.
- the present invention provides the following means for solving the above problems.
- the particle size (r) of the particles present in the lubricating oil composition containing the base oil and fullerene is measured, and the measured value of the particle size (r) and the wear coefficient of the lubricating oil composition are measured.
- a method for inspecting a lubricating oil composition which comprises selecting a lubricating oil composition based on a predetermined range of particle diameter (r) set by correlation with a value.
- SAXS small-angle X-ray scattering method
- [6] A method of calculating the average particle size (R) of the particles from the value of the scattering vector at which the scattering intensity ratio of the lubricating oil composition and the base oil is the maximum value with respect to the scattering vector (hereinafter, method S).
- [7] A method for producing a lubricating oil composition, which comprises a step of sorting by the inspection method for the lubricating oil composition according to any one of the above [1] to [6].
- a method for inspecting a lubricating oil composition capable of stably reproducing wear resistance characteristics by using a method that is relatively easy to measure even for a lubricating oil composition containing fullerene, and a method thereof.
- a method for producing a lubricating oil composition can be provided.
- the method for inspecting the lubricating oil composition according to the present embodiment may refer to the particle size (r) of the particles present in the lubricating oil composition containing the base oil and fullerene (hereinafter, simply referred to as the particle size (r)). ), And the lubricating oil composition is selected based on a predetermined range set by the correlation between the measured value of the particle size (r) and the measured value of the wear coefficient of the lubricating oil composition. .. That is, the method for inspecting the lubricating oil composition according to the present embodiment includes the following three steps.
- Second step A predetermined range of particle size (r) is set.
- the lubricating oil composition inspected by the method for inspecting the lubricating oil composition according to the present embodiment contains a base oil and a fullerene.
- the base oil contained in the lubricating oil composition in the present embodiment is not particularly limited, and usually, mineral oil and synthetic oil widely used as the base oil of the lubricating oil are preferably used.
- Mineral oil used as a lubricating oil is generally a carbon-carbon double bond contained inside saturated by hydrogenation and converted into saturated hydrocarbon.
- mineral oils include paraffin-based base oils and naphthenic base oils.
- synthetic oils include synthetic hydrocarbon oils, ether oils, ester oils, and the like.
- synthetic oils are poly ⁇ -olefin, diester, polyalkylene glycol, polyalphaolefin, polyalkylvinyl ether, polybutene, isoparaffin, olefin copolymer, alkylbenzene, alkylnaphthalene, diisodecyl adipate, monoester, dibasic acid ester, and tri.
- Basic acid ester polyol ester (trimethylolpropane caprilate, trimethylolpropane pelargonate, pentaerythritol 2-ethylhexanoate, pentaerythritol pelargonate, etc.), dialkyldiphenyl ether, alkyldiphenyl sulfide, polyphenyl ether, silicone lubricating oil ( Dimethyl silicone, etc.), perfluoropolyether, etc. are included.
- poly ⁇ -olefins, diesters, polyol esters, polyalkylene glycols, and polyalkyl vinyl ethers are preferable.
- mineral oils and synthetic oils one type may be used alone, or two or more types selected from these may be mixed and used at an arbitrary ratio.
- the fullerene contained in the lubricating oil composition in the present embodiment is not particularly limited in structure and production method, and various fullerenes can be used.
- fullerenes include C 60 and C 70 , which are relatively easily available, higher-order fullerenes, and mixtures thereof.
- C 60 and C 70 are preferable from the viewpoint of high solubility in lubricating oil, and C 60 is more preferable from the viewpoint of less coloring in lubricating oil.
- C 60 is contained in an amount of 50% by mass or more.
- the fullerene may be chemically modified for the purpose of further enhancing the solubility in the base oil.
- the chemically modified fullerene include phenyl C61 butyric acid methyl ester ([60] PCBM), diphenyl C62 dibutyric acid methyl ester (Bis [60] PCBM), phenyl C71 butyric acid methyl ester ([70] PCBM), and phenyl C85.
- Examples thereof include butyric acid methyl ester ([85] PCBM), phenyl C61 butyric acid butyl ester ([60] PCBB), phenyl C61 butyric acid octyl ester ([60] PCBO), an inden adduct of fullerene, and a pyrrolidine derivative of fullerene.
- the lubricating oil composition in the present embodiment may contain additives as long as the effects of the present embodiment are not impaired.
- the additives to be blended in the lubricating oil composition in the present embodiment are not particularly limited.
- the additive include a commercially available antioxidant, a viscosity index improver, an extreme pressure additive, a cleaning dispersant, a pour point lowering agent, a corrosion inhibitor, a solid lubricant, an oiliness improver, a rust preventive additive, and an anti.
- examples thereof include emulsifiers, antifoaming agents and hydrolysis inhibitors.
- One of these additives may be used alone, or two or more of these additives may be used in combination.
- antioxidants examples include dibutylhydroxytoluene (BHT), butylhydroxyanisole (BHA), 2,6-di-tert-butyl-p-cresol (DBPC), and 3-arylbenzofuran-2-one (hydroxycarboxylic acid). (Intramolecular cyclic ester of acid), phenyl- ⁇ -naphthylamine, dialkyldiphenylamine, benzotriazole and the like.
- viscosity index improver examples include polyalkylstyrene and hydride additives of styrene-diene copolymer.
- Examples of the extreme pressure additive include dibenzyldisulfide, allyl phosphate, allyl phosphite, amine salt of allyl phosphate, allyl thiophosphate, amine salt of allyl thiophosphate, and naphthenic acid.
- Examples of the cleaning dispersant include benzylamine succinic acid derivatives, alkylphenol amines and the like.
- Examples of the pour point lowering agent include chlorinated paraffin-naphthalene condensate, chlorinated paraffin-phenol condensate, polyalkyl styrene type and the like.
- Examples of the anti-emulsifier include alkylbenzene sulfonate and the like.
- Examples of the corrosion inhibitor include dialkylnaphthalene sulfonate and the like.
- the lubricating oil composition in the present embodiment is plastic processing such as industrial gear oil; hydraulic hydraulic oil; compressor oil; refrigerating machine oil; cutting oil; rolling oil, pressing oil, forging oil, drawing oil, drawing oil, punching oil and the like. It can be used for various purposes such as oil; metal processing oil such as heat treatment oil and discharge processing oil; slip guide surface oil; bearing oil; rust preventive oil; heat transfer oil.
- Examples of the particles in the lubricating oil composition according to the present embodiment include particles derived from fullerenes such as aggregates of fullerenes and aggregates of fullerenes and base oil molecules.
- the method for measuring the particle size (r) of the particles may be any method that can measure the particle size in the nanometer region. Specific examples thereof include a dynamic light scattering method, a laser diffraction method, and a small-angle X-ray scattering method.
- the small-angle X-ray scattering method (hereinafter, may be referred to as the SAXS method) is used. It is preferable to use it.
- SAXS method small-angle X-ray scattering method
- the measured particle size (r) is the average particle size (R)
- R the average particle size
- the particle size and distribution of the particles in the lubricating oil composition can be obtained by analyzing the intensity of the scattered X-rays from the particles in the lubricating oil composition.
- the region where the scattered X-rays are generated is, for example, in the case of X-rays having a wavelength of 1.54 ⁇ using a Cu target, the measurement angle 2 ⁇ is about 0.1 to 10 degrees.
- the basic principles of the small-angle X-ray scattering method can be referred to in the book "Glatter & Kratky eds (1982) Small Angle X-ray Scattering, Academic Press, London (1982), Pages 17-51.” ..
- the X-ray scattering intensity profile of the particles in the lubricating oil composition is obtained by the SAXS method.
- the vertical axis of the X-ray scattering intensity profile of the particle is the X-ray scattering intensity ISAXS (Q), and the horizontal axis is the scattering vector Q (nm -1 ) depending on the measurement angle 2 ⁇ and the wavelength ⁇ .
- the magnitude of the scattering vector Q is defined by the following equation (1).
- the average particle size (R) of the particles in the lubricating oil composition is calculated using the following G method or S method.
- ISAXS (Q) is the scattering intensity of the particles
- ⁇ is the electron density difference of the particles with respect to the base oil
- V p is the volume of the particles.
- the X-ray scattering intensity profile of the particles in the lubricating oil composition measured by the SAXS method and the X-ray scattering intensity profile of the base oil are obtained.
- the following equation (3) is used by obtaining the ratio of the X-ray scattering intensity of the particles to the X-ray scattering intensity of the base oil with respect to the scattering vector Q and using the scattering vector Q max that maximizes the X-ray scattering intensity ratio. ),
- the average particle size (R) of the particles can be calculated.
- the average particle size (R) of the particles is calculated from the X-ray scattering intensity profile by the above-mentioned SAXS method.
- the accuracy of sorting can be further improved by sorting the lubricating oil composition in which the calculated value from the SAXS method is within the set predetermined range. As a result, the wear resistance characteristics of the lubricating oil composition can be predicted more stably.
- the average particle size (R) of the particles may be calculated by using the G method alone, the S method alone, or the G method and the S method at the same time.
- the selection criterion can be that the average particle diameter (R) calculated by the two methods is within a predetermined range. In that case, the accuracy of selecting the lubricating oil composition can be improved.
- the method for producing a lubricating oil composition of the present embodiment includes a step of selecting a lubricating oil composition obtained by mixing base oil and fullerene by the inspection method of the lubricating oil composition of the present embodiment.
- the method for producing the lubricating oil composition of the present embodiment preferably includes the following steps in detail.
- a step of mixing a base oil and a fullerene, dissolving a dissolved component of the fullerene in the base oil, and if necessary, performing filtration, heat treatment, etc. to obtain a lubricating oil composition containing the base oil and the fullerene ( Hereinafter referred to as "dissolving step”).
- the average particle size (R) of the lubricating oil composition is calculated from the X-ray scattering intensity profile by the SAXS method, and the lubricant composition whose value is within the set range is passed and is out of the set range.
- a step of selecting a lubricating oil composition by rejecting the lubricating oil composition of (hereinafter referred to as "inspection step”).
- the method for producing the lubricating oil composition of the present embodiment may further include the following steps, if necessary. (3) A step of mixing lubricating oil compositions produced in a plurality of different batches to obtain a new lubricating oil composition so that they can be selected as acceptable in the "inspection step” (hereinafter referred to as “readjustment step”). .).
- readjustment step a method for producing the lubricating oil composition of the present embodiment will be described in detail.
- the raw material fullerene is put into the base oil, and the dispersion treatment is carried out for 1 to 48 hours using a dispersion means such as a stirrer while heating at around room temperature or as necessary.
- a dispersion means for dispersing fullerene in the base oil include a stirrer, an ultrasonic disperser, a homogenizer, a ball mill, and a bead mill. In this way, a liquid in which fullerene is dissolved or dispersed in the base oil (sometimes referred to as "fullerene solution”) is obtained.
- the amount of fullerene added may be any amount as long as the fullerene concentration in the fullerene solution is a desired concentration. Further, when a step of removing the insoluble component described later is provided during the dissolution step, it is advisable to add a large amount of fullerene in consideration of the amount of fullerene removed by this step. Although it depends on the solvent, in general, the fullerene concentration in the fullerene solution in which fullerene is difficult to precipitate as an insoluble component is preferably in the range of 1 mass ppm to 1 mass%.
- a fullerene solution having a desired concentration may be obtained by obtaining a fullerene solution having a higher concentration than desired and diluting with a base oil.
- the fullerene solution obtained as described above may be used as it is as a lubricating oil composition. Further, it is preferable that a step of removing the insoluble component is provided during the dissolution step, and the fullerene solution from which the insoluble component is removed is used as a lubricating oil composition.
- the step of removing the insoluble component is preferably provided after the dispersion treatment of dispersing the fullerene in the base oil in the dissolution step. Examples of the step of removing the insoluble component include (1) a removal step using a membrane filter, (2) a removal step using a centrifuge, and (3) a removal step using a combination of a membrane filter and a centrifuge. Can be mentioned.
- a removal step using a membrane filter is preferable when a small amount of lubricating oil composition is obtained, and (2) centrifugation is used when a large amount of lubricating oil composition is obtained.
- a removal step using a separator is preferred.
- the dissolution step especially when the fullerene solution is heated, it is preferable to carry out in a non-oxidizing atmosphere.
- a non-oxidizing atmosphere for example, by substituting the inside of the container containing the fullerene solution with an inert gas such as nitrogen gas or argon gas, or by bubbling the fullerene solution in the container with an inert gas, the fullerene solution becomes an inert gas. It is preferable to achieve an equilibrium state.
- the inspection step is a step of calculating the average particle size (R) of the particles in the lubricating oil composition and selecting the lubricating oil composition.
- the average particle size (R) of the particles in the lubricating oil composition is calculated from the X-ray scattering intensity profile of the lubricating oil composition obtained in the dissolution step by the SAXS method.
- Lubricating oil compositions whose average particle size (R) is within a predetermined range are selected as acceptable, and lubricating oil compositions outside the predetermined range are selected as rejected.
- the predetermined range of the average particle size (R) is the average particle size (R) in which the wear coefficient becomes a desired range from the correlation between the wear coefficient of the lubricating oil composition and the average particle size (R). Can be set by finding.
- the average particle size (R) is measured for each of the lubricating oil compositions produced in a plurality of different batches. Thereby, the predetermined range of the average particle size (R) can be determined in consideration of the wear resistance characteristics, and the lubricating oil composition can be classified into a pass product and a reject product.
- the readjustment step is a step of obtaining a passing lubricating oil composition by mixing an appropriate amount of the rejected lubricating oil composition with the passing lubricating oil composition. Specifically, the newly prepared lubricating oil composition is measured again in the above inspection step for the average particle size (R) of the particles, and an appropriate amount is mixed so that the measured value falls within a predetermined range. Obtain a lubricating oil composition. The amount of the rejected lubricating oil composition to be mixed with the accepted product may be determined by measuring the average particle size (R) of the particles in the mixed lubricating oil composition. By classifying the lubricating oil composition, the following effects can be obtained.
- the method for producing a lubricating oil composition of the present embodiment even if the lubricating oil composition contains fullerenes, wear resistance can be predicted by using a method that is relatively easy to measure. It becomes possible to accurately sort the lubricating oil composition into a pass product and a reject product.
- the above method is a method for measuring the average particle size (R) of particles in a lubricating oil composition by the SAXS method.
- fullerene are added to the mineral oil to prepare three types of fullerene solutions having a fullerene concentration of 2.5 mass ppm, 25.0 mass ppm, and 250.0 mass ppm. did.
- the fullerene concentration of the solution was calculated from the amount of fullerene charged. Further, 100 ml of the obtained fullerene solution was taken out and transferred to a 250 ml stainless steel pressure-resistant container. Next, the inside was replaced with nitrogen gas and then sealed, and this was not heat-treated. Alternatively, the heat treatment was performed by immersing the product in an oil bath at 150 ° C. for 2 hours or 15 hours.
- Nine kinds of lubricating oil compositions shown in Table 1 were obtained. Three points of each type of lubricating oil composition were prepared, that is, a total of 27 samples were prepared.
- the wear resistance characteristics of the obtained lubricating oil composition were evaluated using a friction and wear tester (manufactured by Antonio Par, product name "ball-on-disc tribometer").
- the material of the substrate and balls constituting the friction and wear tester was SUJ2, which is a high carbon chrome bearing steel material.
- the ball had a diameter of 6 mm and the substrate used was a 15 mm square.
- the lubricating oil composition was applied to one main surface of the substrate.
- the balls were slid on one main surface of the substrate through the lubricating oil composition so that the balls would draw concentric orbits.
- the velocity of the ball on one main surface of the substrate was 20 mm / sec, and the load of the ball on one main surface of the substrate was 25 N.
- the maximum diameter of the circle was D ( ⁇ m).
- the maximum diameter D is defined as the wear coefficient. That is, the smaller the number of the maximum diameter D, the more the wear is suppressed, which is a preferable state as the lubricating property of the lubricating oil composition. It usually wears out in a circular shape, but may be oval. In that case, the portion having the maximum diameter is defined as the maximum diameter D. This measurement was performed in an environment of 25 ⁇ 2 ° C.
- Example 1 Small-angle X-ray scattering measurements were performed on 27 samples of the lubricating oil composition and the base oil (mineral oil A) to obtain a scattering intensity profile of particles.
- the average particle size ( RG ) was calculated by the above-mentioned G method using the scattering intensity profile of the obtained particles. Then, the wear coefficient of 27 samples of the lubricating oil composition was measured, and the relationship between the average particle size ( RG ) and the wear coefficient is shown in FIG. Table 2 shows the values of the average particle size ( RG ) and the wear coefficient.
- the correlation coefficient between the average particle size ( RG ) and the wear coefficient was ⁇ 0.80, and a correlation was observed between the average particle size ( RG ) and the wear coefficient.
- the correlation coefficient was determined by the method of least squares. When the absolute value of the correlation coefficient is 0.70 or more, it is judged that the correlation exists.
- a lubricating oil composition having an average particle size ( RG ) within a specific range is selected, thereby selecting a lubricating oil composition having a wear coefficient within a desired range. Can be done.
- the lubricating oil composition having the wear coefficient exceeding the value B can be selected as a rejected product. Further, in FIG. 1, if a small amount even reject lubricating oil composition in the region C 1, the following method, the wear coefficient is adjusted in the lubricating oil composition of the following acceptable product value B be able to. To reject the lubricating oil composition, by adding the lubricating oil composition of accepted products in the region D 1, it is possible to average particle diameter (R G) is set to a value A 1 or more.
- Example 2 Using scattering intensity profile of the scattered intensity profile and mineral oil A of particles, wherein except for calculating the average particle diameter of the particles (R S) in Method S, in the same manner as in Example 1, the average particle diameter of the particles (R S ) And the wear coefficient were evaluated.
- the correlation coefficient between the average particle size ( RS ) and the wear coefficient is ⁇ 0.89, and the absolute value is 0.70 or more, so that the average particle size ( RS ) is used.
- a correlation was found in the wear coefficient. Therefore, also in Example 2, by selecting a lubricating oil composition having an average particle diameter ( RS ) within a specific range, it is possible to select a lubricating oil composition having a wear coefficient within a desired range. I found out.
- the lubricating oil composition having the wear coefficient exceeding the value B can be selected as a rejected product. Further, in FIG. 2, if the amount of the rejected lubricating oil composition in region C 2 is small, the lubricating oil composition of the accepted product having a wear coefficient of B or less is adjusted by the following method. Can be done.
- the addition of accepted products in the lubricating oil composition to reject the lubricating oil composition is in the region D 2, it is possible to average particle diameter (R S) is a value A 2 or more.
- the correlation coefficient between the kinematic viscosity and the wear coefficient was 0.11, and the absolute value was less than 0.70. Therefore, no correlation was observed between the kinematic viscosity and the wear coefficient. Therefore, it was found that the wear coefficient of the lubricating oil composition cannot be estimated from the kinematic viscosity of the lubricating oil composition to select the lubricating oil composition.
- wear resistance can be predicted by measuring the average particle size (R) of particles present in the lubricating oil composition, and lubrication can be predicted.
- the oil composition can be sorted into acceptable and unacceptable products with high accuracy. Therefore, the acceptable lubricating oil composition selected in the present invention is effective for suppressing scratches and wear of metal parts in sliding parts of automobiles, home appliances, industrial machines and the like.
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Abstract
Description
本願は、2019年5月16日に、日本に出願された特願2019-092842号に基づき優先権を主張し、その内容をここに援用する。
また、潤滑油組成物の製品の潤滑特性を測定することで、潤滑特性が許容範囲にある製品を選別することができるが、そのためには、製品ロット毎にボールオンディスク等の摩耗試験を行う必要がある。この場合、手間と時間がかかり、また試験基板等の費用が嵩むため、摩耗試験は製造ロット毎に実施するには適さない。
[1] 基油とフラーレンとを含む潤滑油組成物の中に存在する粒子の粒径(r)を測定し、前記粒径(r)の測定値と前記潤滑油組成物の摩耗係数の測定値との相関によって設定された粒径(r)の所定範囲に基づいて潤滑油組成物を選別することを特徴とする潤滑油組成物の検査方法。
[2] 前記粒子の粒径(r)を、動的光散乱法、レーザー回折法、または、X線小角散乱法(SAXS)法によって測定する[1]に記載の潤滑油組成物の検査方法。
[3] 前記粒径(r)が、前記潤滑油組成物の中に存在する粒子の平均粒径(R)である[1]または[2]に記載の潤滑油組成物の検査方法。
[4] 前記粒子の平均粒径(R)を、X線小角散乱法(SAXS法)によって測定する上記[3]に記載の潤滑油組成物の検査方法。
[5] 前記粒子の平均粒径(R)を、Guinierプロットの傾きから算出する方法(以下、G法ということがある)により、求める上記[4]に記載の潤滑油組成物の検査方法。
[6]前記粒子の平均粒径(R)を、散乱ベクトルに対して前記潤滑油組成物と前記基油の散乱強度比が最大値となる散乱ベクトルの値から算出する方法(以下、S法ということがある)により、求める上記[4]に記載の潤滑油組成物の検査方法。
[7]上記[1]~[6]のいずれかに記載の潤滑油組成物の検査方法により選別する工程を含む、潤滑油組成物の製造方法。
本実施形態に係る潤滑油組成物の検査方法は、基油とフラーレンとを含む潤滑油組成物の中に存在する粒子の粒径(r)(以下単なる粒径(r)と称する場合がある)を測定し、前記粒径(r)の測定値と前記潤滑油組成物の摩耗係数の測定値との相関によって設定された所定範囲に基づいて潤滑油組成物を選別することを特徴とする。すなわち、本実施形態に係る潤滑油組成物の検査方法は、以下の3つのステップを含む。
第一ステップ:複数の潤滑油組成物中に存在する粒子の粒径(r)と潤滑油組成物の摩耗係数を測定し、粒径(r)と摩耗係数の相関関係(例えば、摩耗係数(B)―粒径(r)の近似直線:B=kR+c)を算出する。
第二ステップ:粒径(r)の所定範囲を設定する。
第三ステップ:検査対象となる潤滑油組成物に存在する粒子の粒径(r)を測定し、粒径(r)が所定の範囲内であれば、合格品とし、粒径(r)が所定範囲外であれば、不合格品とする。
前記粒径(r)が前記潤滑油組成物の中に存在する粒子の平均粒径(R)(以下単なる平均粒径(R)と称する場合がある)であることが好ましい。
本実施形態に係る潤滑油組成物の検査方法で検査される潤滑油組成物は、基油とフラーレンとを含む。
本実施形態における潤滑油組成物に含まれる基油は、特に限定されるものではなく、通常、潤滑油の基油として広く使用されている鉱油および合成油が好適に用いられる。
本実施形態における潤滑油組成物に含まれるフラーレンは、構造や製造法が特に限定されず、種々のものを用いることができる。フラーレンとしては、例えば、比較的入手しやすいC60やC70、さらに高次のフラーレン、あるいはそれらの混合物が挙げられる。フラーレンの中でも、潤滑油への溶解性の高さの点から、C60およびC70が好ましく、潤滑油への着色が少ない点から、C60がより好ましい。C60を含む混合物の場合は、C60が50質量%以上含まれることが好ましい。
本実施形態における潤滑油組成物は、基油とフラーレン以外にも、本実施形態の効果を損なわない範囲で、添加剤を含有することができる。
本実施形態における潤滑油組成物に配合する添加剤は、特に限定されない。添加剤としては、例えば、市販の酸化防止剤、粘度指数向上剤、極圧添加剤、清浄分散剤、流動点降下剤、腐食防止剤、固体潤滑剤、油性向上剤、錆び止め添加剤、抗乳化剤、消泡剤、加水分解抑制剤等が挙げられる。これらの添加剤は、1種を単独で用いてもよく、2種以上を併用してもよい。
粘度指数向上剤としては、例えば、ポリアルキルスチレン、スチレン-ジエンコポリマーの水素化物添加剤等が挙げられる。
極圧添加剤としては、ジベンジルジサルファイド、アリルリン酸エステル、アリル亜リン酸エステル、アリルリン酸エステルのアミン塩、アリルチオリン酸エステル、アリルチオリン酸エステルのアミン塩、ナフテン酸等が挙げられる。
清浄分散剤としては、ベンジルアミンコハク酸誘導体、アルキルフェノールアミン類等が挙げられる。
流動点降下剤としては、塩素化パラフィン-ナフタレン縮合物、塩素化パラフィン-フェノール縮合物、ポリアルキルスチレン系等が挙げられる。
抗乳化剤としては、アルキルベンゼンスルホン酸塩等が挙げられる。
腐食防止剤としては、ジアルキルナフタレンスルホン酸塩等が挙げられる。
本実施形態に係る潤滑油組成物中の粒子は、例えば、フラーレンの凝集体、フラーレンと基油分子の会合体等、フラーレン由来の粒子が挙げられる。上記粒子の粒径(r)の測定方法は、ナノメートル領域の粒径を測定することができる方法であればよい。具体的には、例えば、動的光散乱法、レーザー回折法、X線小角散乱法等が挙げられる。なお、本実施形態の潤滑油組成物中に存在する粒子は、粒子径が1nm~100nm領域のものが多いと推定されるため、X線小角散乱法(以下、SAXS法ということがある)を用いることが好ましい。
前記各測定法において、測定される粒径(r)が平均粒径(R)であると、粒径(r)と摩耗係数との強い相関関係を得やすく好ましい。
潤滑油組成物において、基油に対する粒子の電子密度差が一定であるとし、粒子の形状を球状、かつ粒径(r)が均一であると仮定すると、Q<1/rの小角領域では、Guinier近似を用いることができる。Guinier近似により、粒子の散乱強度ISAXS(Q)は下記の式(2)で表すことができる。
Guinier近似において、粒子の形状などの仮定を設けることがあるが、これらの仮定が要らない観点から、より簡便なS法を用いて、粒子の平均粒径を解析することが好ましい。
本実施形態の潤滑油組成物の製造方法は、基油とフラーレンとを混合して得た潤滑油組成物を、本実施形態の潤滑油組成物の検査方法により選別する工程を含む。
(1)基油とフラーレンとを混合し、フラーレンの溶解成分を基油中に溶解し、必要に応じてろ過、加熱処理等を経て、基油とフラーレンを含む潤滑油組成物を得る工程(以下、「溶解工程」という。)。
(2)SAXS法により、X線散乱強度プロファイルから潤滑油組成物の平均粒径(R)を算出し、その値が設定された範囲内にある潤滑剤組成物を合格、設定された範囲外の潤滑油組成物を不合格として、潤滑油組成物を選別する工程(以下、「検査工程」という。)。
本実施形態の潤滑油組成物の製造方法は、さらに必要に応じて、以下の工程を含んでいてもよい。
(3)「検査工程」で合格として選別され得るように、複数の異なるバッチで製造した潤滑油組成物を混合して、新たな潤滑油組成物を得る工程(以下、「再調整工程」という。)。
以下、本実施形態の潤滑油組成物の製造方法を詳細に説明する。
原料のフラーレンを基油に投入して攪拌機等の分散手段を用いて、室温付近または必要に応じて加温しながら1時間~48時間の分散処理を施す。
基油にフラーレンを分散させるための分散手段としては、例えば、撹拌機、超音波分散装置、ホモジナイザー、ボールミル、ビーズミル等が挙げられる。
このようにして基油中にフラーレンが溶解または分散した液(「フラーレン溶液」ということがある。)を得る。
さらに、不溶成分を除去する工程を、溶解工程中に設け、不溶成分を除去したフラーレン溶液を潤滑油組成物とすることが好ましい。不溶成分を除去する工程は、溶解工程において、基油にフラーレンを分散させる分散処理後に設けることが好ましい。不溶成分を除去する工程としては、例えば、(1)メンブランフィルターを用いた除去工程、(2)遠心分離器を用いた除去工程、(3)メンブランフィルターと遠心分離器を組み合わせて用いる除去工程等が挙げられる。これらの除去工程の中でも、濾過時間の点から、少量の潤滑油組成物を得る場合は(1)メンブランフィルターを用いた除去工程が好ましく、大量の潤滑油組成物を得る場合は(2)遠心分離器を用いた除去工程が好ましい。
検査工程は、潤滑油組成物中の粒子の平均粒径(R)を算出し、潤滑油組成物を選別する工程である。溶解工程で得られた潤滑油組成物についてSAXS法により、X線散乱強度プロファイルから潤滑油組成物中の粒子の平均粒径(R)を算出する。その平均粒径(R)の値が所定範囲内にある潤滑油組成物を合格、所定範囲外の潤滑油組成物を不合格として選別する。この平均粒径(R)の所定範囲は、上述したように潤滑油組成物の摩耗係数と、平均粒径(R)との相関から、摩耗係数が所望の範囲になる平均粒径(R)を求めることにより設定することができる。複数の異なるバッチで製造した潤滑油組成物毎に、平均粒径(R)の測定を行う。これにより、耐摩耗特性を考慮して平均粒径(R)の所定範囲を決定し、潤滑油組成物を合格品と不合格品等に分類することができる。
再調整工程は、不合格になった潤滑油組成物を合格品の潤滑油組成物へ適量混合することにより、合格品の潤滑油組成物を得る工程である。具体的には、新たに調整された潤滑油組成物を再度上記検査工程にて粒子の平均粒径(R)の測定をし、測定値が所定範囲に入るように適量混合し、合格品の潤滑油組成物を得る。合格品に混合する不合格品の潤滑油組成物の量は、混合後の潤滑油組成物中の粒子の平均粒径(R)を測定して判断すると良い。
潤滑油組成物を分類することにより、次のような効果が得られる。(1)粒子の平均粒径(R)が不合格となる潤滑油組成物を排除することができる。(2)粒子の平均粒径(R)が不合格の範囲に含まれる潤滑油組成物を合格品の潤滑油組成物に混合することにより、新たに合格となり得る潤滑油組成物を得ることができる。
鉱油A(製品名:ダイアナフレシアP-46、出光興産社製)2Lと、フラーレン(フロンティアカーボン社製、nanomTM purple SUT、C60)を下記所定量混合し、室温にて、スターラーを用いて6時間で撹拌した。攪拌終了後、0.1μmのメンブランフィルターを通して濾過することで、フラーレン溶液を得た。ここで鉱油に対してフラーレンを0.5mg、5.0mg、50.0mg加えて、フラーレン濃度が2.5質量ppm、25.0質量ppm、250.0質量ppmの3種類のフラーレン溶液を調製した。なお、溶液のフラーレン濃度がフラーレンの仕込み量より算出した。
さらに、得られたフラーレン溶液を100ml取り出し、これを250mlのステンレス製の耐圧容器に移した。次に内部を窒素ガスで置換した後に密栓し、これを熱処理しなかった。または、150℃のオイルバスに2時間あるいは15時間浸漬させて熱処理を行なった。表1に示す潤滑油組成物1~9の9種類の潤滑油組成物を得た。各種類の潤滑油組成物をそれぞれ3点調製し、すなわち、合計27サンプルを調製した。
(X線小角散乱測定)
潤滑油組成物に対して、X線小角散乱測定を実施した。詳細は以下となる。
測定システム:SAXSpace(AntonPaar製)
X線:波長(λ):0.1524nm
検出器:Mythen(1次元計数型検出器)
適正な露光条件(アッテネーター及び露光時間)を選定の上、潤滑油組成物と基油(バックグラウンド)の二次元散乱パターンを記録した。画像処理ソフトFit2d(Europeansynchrotron research facility)を用い、それぞれ、横軸が散乱ベクトル、縦軸が散乱強度の散乱強度プロファイルを得た。潤滑油組成物の散乱強度から、基油の散乱強度を引くことにより、粒子の散乱強度プロファイルを得ることができた。
得られた潤滑油組成物について、摩擦摩耗試験機(Anton Paar社製、製品名「ボールオンディスクトライボメーター」)を用いて、耐摩耗特性を評価した。
摩擦摩耗試験機を構成する基板およびボールの材質を、高炭素クロム軸受鋼鋼材であるSUJ2とした。なお、ボールは直径が6mm、基板は15mm角を用いた。
まず、基板の一主面に潤滑油組成物を塗布した。次に、潤滑油組成物を介して、基板の一主面上にて、ボールが同心円状の軌道を描くように、ボールを摺動させた。基板の一主面上におけるボールの速度を20mm/秒、ボールによる基板の一主面に対する荷重を25Nとした。基板の一主面上におけるボールの摺動距離が積算15mに到達した時点で、ボールを装置より取り出し、ボールの基板との接触面を、光学顕微鏡で観察し、表面のすり減りを、すり減り面の円の最大直径をD(μm)とした。ここで最大直径Dを摩耗係数と定義した。つまり、最大直径Dの数字が小さいほど、摩耗が抑制されており、潤滑油組成物の潤滑特性として好ましい状態である。通常、円形にすり減るが、楕円を帯びる場合がある。その場合は、最大径になる部分を最大直径Dとした。なお、この測定は25±2℃の環境下で行った。
約50mLの潤滑油組成物をガラス製ビーカーに取り出し、これを40℃の水浴に30分間浸漬した。
次に、日本工業規格 JIS Z8803:2011に規定されている液体の粘度測定方法細管粘度計による粘度測定方法に準ずる方法により、潤滑油組成物の動粘度を測定した。
前記潤滑油組成物の27サンプルと基油(鉱油A)について、X線小角散乱測定を行い、粒子の散乱強度プロファイルを得た。得た粒子の散乱強度プロファイルを用いて、前記G法で、平均粒径(RG)を算出した。そして、潤滑油組成物27サンプルの摩耗係数測定を行い、平均粒径(RG)と摩耗係数の関係を図1に示す。平均粒径(RG)と摩耗係数の値を表2に示す。
粒子の散乱強度プロファイルと鉱油Aの散乱強度プロファイルを用い、前記S法で粒子の平均粒径(RS)を算出したこと以外は、実施例1と同様に、粒子の平均粒径(RS)と摩耗係数の関係を評価した。
平均粒径(RS)と摩耗係数の値を表3に、平均粒径(RS)と摩耗係数の関係を図2に示す。
前記潤滑油組成物の27サンプルについて、動粘度(mm2/s)および摩耗係数を測定し、動粘度と摩耗係数の関係を評価した。動粘度と摩耗係数の測定結果を表4に、動粘度と摩耗係数の関係を図3に示す。
Claims (7)
- 基油とフラーレンとを含む潤滑油組成物の中に存在する粒子の粒径(r)を測定し、前記粒径(r)の測定値と前記潤滑油組成物の摩耗係数の測定値との相関によって設定された粒径(r)の所定範囲に基づいて潤滑油組成物を選別することを特徴とする潤滑油組成物の検査方法。
- 前記粒子の粒径(r)を、動的光散乱法、レーザー回折法、または、X線小角散乱法(SAXS)法によって測定する請求項1に記載の潤滑油組成物の検査方法。
- 前記粒径(r)が、前記潤滑油組成物の中に存在する粒子の平均粒径(R)である請求項1または2に記載の潤滑油組成物の検査方法。
- 前記粒子の平均粒径(R)を、X線小角散乱法(SAXS)法によって測定する請求項3に記載の潤滑油組成物の検査方法。
- 前記粒子の平均粒径(R)を、Guinierプロットの傾きから算出する請求項4に記載の潤滑油組成物の検査方法。
- 前記粒子の平均粒径(R)を、散乱ベクトルに対して前記潤滑油組成物と前記基油の散乱強度比が最大値となる散乱ベクトルの値から算出する請求項4に記載の潤滑油組成物の検査方法。
- 請求項1~請求項6のいずれか1項に記載の潤滑油組成物の検査方法により選別する工程を含む、潤滑油組成物の製造方法。
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Citations (8)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP2003139680A (ja) * | 2001-11-05 | 2003-05-14 | Denki Kagaku Kogyo Kk | 粒度分布測定方法 |
JP2006113042A (ja) * | 2004-09-17 | 2006-04-27 | Dainippon Ink & Chem Inc | 有機顔料の平均一次粒子径、粒径分布、及び凝集粒子径の測定方法 |
JP2008164294A (ja) * | 2006-12-26 | 2008-07-17 | Toribotex Co Ltd | 潤滑状態評価装置、潤滑状態評価方法、プログラム及び記録媒体 |
JP2008266501A (ja) | 2007-04-24 | 2008-11-06 | Sumikou Junkatsuzai Kk | エンジンオイル用添加剤組成物 |
JP2011145162A (ja) * | 2010-01-14 | 2011-07-28 | Japan Atomic Energy Agency | 流体中微粒子のx線検出法 |
WO2017141825A1 (ja) | 2016-02-19 | 2017-08-24 | パナソニックIpマネジメント株式会社 | 冷媒圧縮機およびそれを用いた冷凍装置 |
JP2019045390A (ja) * | 2017-09-05 | 2019-03-22 | 昭和電工株式会社 | 針状物質の物性の測定方法 |
JP2019092842A (ja) | 2017-11-22 | 2019-06-20 | テルモ株式会社 | 医療器具の留置方法、医療器具、及び医療器具の留置装置 |
Family Cites Families (9)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP4730714B2 (ja) * | 2008-08-28 | 2011-07-20 | 日産自動車株式会社 | グリース組成物 |
JP5747230B2 (ja) * | 2011-06-17 | 2015-07-08 | Nokクリューバー株式会社 | 導電性グリース組成物 |
JP2013234869A (ja) * | 2012-05-07 | 2013-11-21 | Ihi Corp | 油中不溶解物検出装置 |
CN103820193A (zh) * | 2014-02-24 | 2014-05-28 | 广东美芝制冷设备有限公司 | 润滑油组合物及其应用 |
CN104560307A (zh) * | 2014-12-30 | 2015-04-29 | 中国人民解放军空军勤务学院 | 含纳米二硫化钨的抗磨减摩润滑油添加剂 |
WO2016125859A1 (ja) * | 2015-02-05 | 2016-08-11 | 出光興産株式会社 | グリースおよびグリースの製造方法 |
JP2018168356A (ja) * | 2017-03-29 | 2018-11-01 | 昭和電工株式会社 | 潤滑油組成物及びその製造方法 |
WO2019082883A1 (ja) * | 2017-10-25 | 2019-05-02 | 昭和電工株式会社 | フラーレン含有潤滑油組成物及びその製造方法 |
US11220652B2 (en) * | 2017-12-06 | 2022-01-11 | Showa Denko K.K. | Method for inspecting lubricating oil composition and method for producing lubricating oil composition |
-
2020
- 2020-05-13 JP JP2021519457A patent/JP7027676B2/ja active Active
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Patent Citations (8)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP2003139680A (ja) * | 2001-11-05 | 2003-05-14 | Denki Kagaku Kogyo Kk | 粒度分布測定方法 |
JP2006113042A (ja) * | 2004-09-17 | 2006-04-27 | Dainippon Ink & Chem Inc | 有機顔料の平均一次粒子径、粒径分布、及び凝集粒子径の測定方法 |
JP2008164294A (ja) * | 2006-12-26 | 2008-07-17 | Toribotex Co Ltd | 潤滑状態評価装置、潤滑状態評価方法、プログラム及び記録媒体 |
JP2008266501A (ja) | 2007-04-24 | 2008-11-06 | Sumikou Junkatsuzai Kk | エンジンオイル用添加剤組成物 |
JP2011145162A (ja) * | 2010-01-14 | 2011-07-28 | Japan Atomic Energy Agency | 流体中微粒子のx線検出法 |
WO2017141825A1 (ja) | 2016-02-19 | 2017-08-24 | パナソニックIpマネジメント株式会社 | 冷媒圧縮機およびそれを用いた冷凍装置 |
JP2019045390A (ja) * | 2017-09-05 | 2019-03-22 | 昭和電工株式会社 | 針状物質の物性の測定方法 |
JP2019092842A (ja) | 2017-11-22 | 2019-06-20 | テルモ株式会社 | 医療器具の留置方法、医療器具、及び医療器具の留置装置 |
Non-Patent Citations (2)
Title |
---|
"Small-Angle X-Ray Scattering", 1982, ACADEMIC PRESS, pages: 17 - 51 |
See also references of EP3971268A4 |
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JPWO2020230815A1 (ja) | 2020-11-19 |
US20220074840A1 (en) | 2022-03-10 |
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