JP4197407B2 - Lubricating oil composition for bearings - Google Patents
Lubricating oil composition for bearings Download PDFInfo
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- JP4197407B2 JP4197407B2 JP2002182553A JP2002182553A JP4197407B2 JP 4197407 B2 JP4197407 B2 JP 4197407B2 JP 2002182553 A JP2002182553 A JP 2002182553A JP 2002182553 A JP2002182553 A JP 2002182553A JP 4197407 B2 JP4197407 B2 JP 4197407B2
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Description
【0001】
【発明の属する技術分野】
本発明は軸受用潤滑油組成物に係り、特には工作機械主軸等のジェット潤滑方式に適した低粘度の軸受用潤滑油組成物に関する。
【0002】
【従来の技術】
工作機械は、近年、高効率化のため、主軸スピンドルの高速化や、さらには航空機用部品や電子部品に使用されるアルミニウム系合金等での高精度加工が望まれている。主軸スピンドルの潤滑方式には、グリース潤滑、オイルエアー潤滑、オイルミスト潤滑、及びジェット潤滑があるが、このうち、多量の潤滑油を軸受に噴射して軸受を潤滑、冷却するジェット潤滑方式が主軸の高速化に最適とされている。高速化にともなう主軸の熱変形を抑えて加工物の加工精度を向上させるためには、潤滑油の撹拌抵抗をできるだけ少なくする必要があるのでジェット潤滑で使用される軸受潤滑油は、40℃の動粘度が1〜22mm2/sという低粘度のものが用いられる。しかし、低粘度の潤滑油は油膜が形成されにくく、高い耐摩耗性と耐荷重性を付与するためには添加剤の配合は不可欠である。なかでもジアルキルジチオリン酸亜鉛(ZnDTP)は、低コスト、優れた耐摩耗性、耐荷重性を示すため、広く用いられている。
【0003】
ところで、工作機械においては被加工物の加工方式や材質に応じた切削油が使用されているが、近年、主軸の高速化にともない、潤滑システム内に切削油が混入しやすい環境となってきている。一方、最近では、水溶性切削油が広く用いられ、これと軸受油との適合性が重要となっており、特に、アルカリ性の高い水溶性切削油に起因した軸受油中の添加剤の劣化消耗により、軸受油の初期性能が十分に維持できず、またスラッジの発生や腐食の問題が生じてきた。
【0004】
【発明が解決しようとする課題】
本発明は上記課題を解決するもので、本発明の目的は超低粘度基油を用いても高い耐摩耗性と耐荷重性を有するとともに、水溶性切削油が混入しても添加剤の劣化、スラッジの発生や腐食の問題が生じない低粘度軸受用潤滑油組成物を提供することである。
【0005】
【課題を解決するための手段】
すなわち、本発明は40℃における動粘度が1〜25mm2/sの基油に、潤滑油全量基準で、下記一般式(1)
【0006】
【化1】
[(R1O−)mP(OH)n(=O)][NH(−R2)2]n (1)
【0007】
(上記式中、R1及びR2は、炭素数3〜25の直鎖あるいは分岐鎖アルキル基、アルケニル基又はアルキル置換あるいは非置換芳香族基を示し、m及びnは整数で、m+n=3、nは1又は2である。)で示した酸性リン酸エステルアミン塩を0.1〜5質量%含有する軸受用潤滑油組成物、より好ましくは、これにさらに、潤滑油全量基準で、チオリン酸エステルを0.05〜2質量%及び/又はチアジアゾール化合物を0.05〜2質量%含有する軸受用潤滑油組成物に関するものである。
【0008】
【発明の実施の形態】
本発明の基油としては、40℃における動粘度(JIS K 2283に規定される方法による)が1〜25mm2/s、特に好ましくは1〜5mm2/sのもので、鉱油系又は合成系のいずれか、あるいは両者を混合したものを用いることができる。
【0009】
鉱油系基油は、原油を蒸留して得られた潤滑留分、特には潤滑軽質留分を、水素化精製、溶剤脱れき、溶剤抽出、溶剤脱ろう、水添脱ろう、接触脱ろう、水素化分解、アルカリ蒸留、硫酸洗浄、白土処理等、いずれか1又は2以上組み合わせて精製を行うことにより、好適な潤滑基油を得ることができる。さらには、炭素数11〜15のノルマルパラフィンやイソパラフィン等も好適に用いることができる。本発明においては、上記所定の動粘度になるような沸点範囲を有する潤滑油留分を精製して得られた鉱油系基油を単独で用いても良いが、複数の精製された潤滑油留分を混合して、所定の動粘度になるように調製しても良い。
【0010】
合成系基油としては、ポリ-α-オレフィン、脂肪酸エステル、リン酸エステル、ポリアルキレングリコール等が好適である。これらの合成系基油は、単独で用いても、複数を組み合わせて用いても良い。
【0011】
上記一般式(1)に示す酸性リン酸エステルアミン塩は、式中のR1が炭素数3〜25の直鎖あるいは分岐鎖アルキル基、アルケニル基又はアルキル置換あるいは非置換芳香族基であるが、炭素数5〜20のものがより好ましく、なかでもヘキシル基、オクチル基、オレイル基やトリル基を有するものの入手が容易で、特に好ましい。
また、上記式中のR2は炭素数1〜25の直鎖あるいは分岐鎖アルキル基であるが、特には炭素数5〜20のものが好ましい。
【0012】
なお、本発明においては、上記一般式(1)の酸性リン酸エステルアミン塩を添加するのに代えて、上記一般式(1)の左側の酸性リン酸エステル部分に相当するエステルとこれと当量もしくはそれ以下の上記一般式(1)の右側のアミン部に相当するアミンとをそれぞれ別々に添加し、潤滑油中で、一般式(1)の酸性リン酸エステルアミン塩を形成するようにしても良い。
これらの酸性リン酸エステルアミン塩は、潤滑油全量基準で、0.1〜5質量%、好ましくは0.2〜1質量%含有するようにすると良い。
【0013】
本発明の軸受用潤滑油組成物には、チオリン酸エステルを配合することもできる。このチオリン酸エステルとしては、一般に潤滑油の極圧剤として使用されているものを用いることができるが、特には下記一般式(2)で示される化合物を用いることが、耐腐食性の点から好ましい。
【0014】
【化2】
(R3−O−)3P=S (2)
【0015】
上記式中、R3は置換又は非置換芳香族を表す。このR3は、特には、フェニル基やt-ブチルフェニル基のものが好ましい。
これらのチオリン酸エステルは、潤滑油全量基準で、0.05〜2質量%、好ましくは0.1〜1質量%含有するようにすると良い。
【0016】
本発明に用いるチアジアゾール化合物とは、チアジアゾール骨格を有する化合物であれば特に支障なく使用できるが、特には、チアジアゾール骨格中の炭素に、スルフィド基又はポリスルフィド基が置換した化合物、例えば、1,3,4−チアジアゾール骨格を有する化合物では、下記一般式(3)で表される化合物が好ましい。
【化3】
【0017】
上記式中のR4及びR5はそれぞれ独立して炭素数5〜30の炭化水素基、m及びnがそれぞれ独立して1〜4の整数を示す。
また、この骨格部分が1,3,4−体以外の、1,2,3−体、1,2,4−体等のものでも同様に用いることができ、また、チアジアゾール化合物の2種以上が混合したものであっても、本発明の目的上何ら支障がない。なお、上記一般式(3)中のR4及びR5の炭化水素基は、直鎖及び/又は分枝、飽和及び/又は不飽和のいずれでも良く、特に、炭素数5〜15のアルキル基が好ましい。
本発明で用いるチアジアゾール化合物は、潤滑油全量基準で、0.01〜2質量%、好ましくは0.03〜1質量%含有するようにすると良い。
【0018】
本発明の軸受用潤滑油組成物には、他の一般に用いられている潤滑油添加剤、例えば、酸化防止剤、防錆剤、粘度指数向上剤、流動点降下剤、消泡剤、金属不活性化剤等を適宜、添加することができる。
酸化防止剤としては、ジ−t−ブチルパラクレゾールなどのフェノール系化合物、アルキル化ジフェニルアミンやαナフチルアミンなどのアミン系化合物、亜リン酸エステルなどのリン系化合物が挙げられる。
防錆剤としては、アルケニルコハク酸エステル、アルケニルコハク酸部分エステル、ソルビタンエステル、スルフォン酸金属塩などが挙げられる。
粘度指数向上剤、流動点降下剤としては、ポリメタアクリレートポリマーやオレフィンコポリマーなどを挙げることができる。
消泡剤としては、シリコーンポリマー、ポリメタアクリレートポリマーなどを挙げることができる。
また金属不活性化剤には、ベンゾトリアゾール、及びベンゾトリアゾール誘導体などを挙げることができる。
【0019】
【実施例】
以下、実施例より本発明の軸受用潤滑油組成物をより詳細に説明するが、本発明はそれらにより何ら制限されるものではない。
実施例及び比較例の軸受潤滑油組成物を調製するに当たり、以下の基材を用いた。下記の基油と添加剤とを60℃で1時間撹拌加熱し、添加剤の溶解を確認の上、試験に供した。
【0020】
(1)潤滑油基油
炭素数12と13のノルマルパラフィンを質量比で60対40の割合に混合したものを基油とした。40℃での動粘度は1.5mm2/sである。
【0021】
(2)添加剤
(a)摩耗防止剤
摩耗防止剤としては、以下の酸性リン酸エステルアミン塩、チオリン酸エステル、チアジアゾールを用いた。また比較としてZnDTP(ジアルキルジチオリン酸亜鉛)も用いた。
a−1:酸性リン酸エステルアミン塩
[式(1)のR1:n−ヘキシル、R2:C11〜C14のアルキル基]
a−2:酸性リン酸エステルアミン塩
[式(1)のR1:オレイル、R2:C8のアルキル基]
a−3:チオリン酸エステル
[式(2)のR3:t−ブチルフェニル]
a−4:チアジアゾール
[式(3)のR4+R5:アルキル基であって合計炭素数22、m,n:3]
a−5:ZnDTP
[Sec.C6アルキル基タイプ]
(b)酸化防止剤
b−1:フェノール系酸化防止剤
[ジ−t−ブチルパラクレゾール]
b−2:アミン系酸化防止剤
[ジオクチルジフェニルアミン]
【0022】
(3)潤滑性の評価
供試油の耐摩耗性及び耐荷重能をそれぞれ評価した。耐摩耗性は、シェル4球耐摩耗性試験方法(ASTM D2260準拠、1400 rpm、15 kgf/cm2、30 min、室温)による摩耗痕(mm)を計測した。耐荷重能は、曽田式4球法耐荷重能試験方法(JIS K 2519,Shock法)による焼付荷重(MPa)を測定した。
【0023】
(4)水溶性切削油との混合安定性評価
供試油と水溶性切削油との混合による銅の腐食性、スラッジ析出性を以下の方法により評価した。供試油200mlに、水溶性切削油[A1種(エマルション系)、又はA2種(ソリュブル系)]を精製水で20倍希釈したもの20mlを加え、銅板触媒の存在下に、回転数1500rpm、温度60℃で、168時間撹拌した(JIS K 2510の装置を使用)。撹拌後の供試油について、銅板触媒の変色(JIS K 2513の規定により評点)を観察し、汚染度(JIS B 9931)を測定した。
実施例及び比較例の以上の結果を表1にまとめて示す。
【0024】
【表1】
【0025】
摩耗防止剤として酸性リン酸エステルを配合した実施例1〜5は、水溶性切削油A1種、A2種ともに銅の変色は1bレベルで良好であった。また、汚染度は11mg/100ml以下であり、後に示す比較例に比べ大幅に小さい。潤滑性は、酸性リン酸エステルアミン塩にチオリン酸エステル、及び/又はチアジアゾールを所定量配合することにより、耐摩耗性を維持しつつ、耐荷重能も比較例レベルを示した。これより、水溶性切削油との混合安定性に優れ、かつ優れた耐摩耗性とするためには、酸性リン酸エステルアミン塩の配合が効果的であり、さらに耐荷重能を付与するためには、チオリン酸エステル、及び/又はチアジアゾールを所定量配合することが有望であることが確認された。
摩耗防止剤としてZnDTPを配合した比較例1は、優れた耐摩耗性と耐荷重能を示した。しかし、水溶性切削油A1種との混合試験においては、汚染度が高く、A2種では銅の変色が大きかった。
【0026】
【発明の効果】
本発明の軸受用潤滑油組成物は、高い耐摩耗性と耐荷重性を有するとともに、水溶性切削油が混入してもスラッジの発生や腐食の問題がほとんど生じないという格別の効果を奏する。[0001]
BACKGROUND OF THE INVENTION
The present invention relates to a lubricating oil composition for bearings, and more particularly to a low-viscosity lubricating oil composition for bearings suitable for jet lubrication systems such as machine tool main shafts.
[0002]
[Prior art]
In recent years, machine tools have been demanded to increase the spindle spindle speed and to perform high-precision machining with aluminum alloys used for aircraft parts and electronic parts in order to increase efficiency. Grease lubrication, oil-air lubrication, oil mist lubrication, and jet lubrication are the main spindle spindle lubrication methods. Of these, the jet lubrication method in which a large amount of lubricating oil is injected onto the bearing to lubricate and cool the bearing is the main spindle. It is said to be optimal for speeding up. In order to suppress the thermal deformation of the main shaft accompanying the increase in speed and improve the machining accuracy of the workpiece, it is necessary to reduce the stirring resistance of the lubricating oil as much as possible. Therefore, the bearing lubricating oil used in jet lubrication is 40 ° C. A kinematic viscosity having a low viscosity of 1 to 22 mm 2 / s is used. However, low viscosity lubricating oil is difficult to form an oil film, and the addition of additives is indispensable for imparting high wear resistance and load resistance. Among these, zinc dialkyldithiophosphate (ZnDTP) is widely used because it exhibits low cost, excellent wear resistance, and load resistance.
[0003]
By the way, cutting oils according to the processing method and material of the workpiece are used in machine tools, but in recent years, as the speed of the spindle has increased, it has become an environment where cutting oil is likely to be mixed in the lubrication system. Yes. On the other hand, recently, water-soluble cutting oil has been widely used, and compatibility with the bearing oil has become important. In particular, deterioration and consumption of additives in bearing oil due to water-soluble cutting oil with high alkalinity are important. As a result, the initial performance of the bearing oil cannot be sufficiently maintained, and sludge generation and corrosion problems have arisen.
[0004]
[Problems to be solved by the invention]
The present invention solves the above problems, and the object of the present invention is to have high wear resistance and load resistance even when an ultra-low viscosity base oil is used, and to deteriorate additives even if water-soluble cutting oil is mixed. Another object of the present invention is to provide a lubricating oil composition for low viscosity bearings which does not cause sludge generation and corrosion problems.
[0005]
[Means for Solving the Problems]
That is, according to the present invention, a base oil having a kinematic viscosity at 40 ° C. of 1 to 25 mm 2 / s is represented by the following general formula (1) based on the total amount of lubricating oil.
[0006]
[Chemical 1]
[(R 1 O—) m P (OH) n (═O)] [NH (—R 2 ) 2 ] n (1)
[0007]
(In the above formula, R 1 and R 2 represent a linear or branched alkyl group having 3 to 25 carbon atoms, an alkenyl group, or an alkyl-substituted or unsubstituted aromatic group, m and n are integers, and m + n = 3 , N is 1 or 2.) A lubricating oil composition for bearings containing 0.1 to 5% by mass of the acidic phosphate ester amine salt shown in (2), more preferably, based on the total amount of lubricating oil, The present invention relates to a bearing lubricating oil composition containing 0.05 to 2% by mass of a thiophosphate and / or 0.05 to 2% by mass of a thiadiazole compound.
[0008]
DETAILED DESCRIPTION OF THE INVENTION
The base oil of the present invention has a kinematic viscosity at 40 ° C. (according to the method defined in JIS K 2283) of 1 to 25 mm 2 / s, particularly preferably 1 to 5 mm 2 / s. Either of these or a mixture of both can be used.
[0009]
Mineral oil base oils are obtained by hydrorefining, solvent removal, solvent extraction, solvent dewaxing, hydrodewaxing, catalytic dewaxing of lubricating fractions obtained by distilling crude oil, especially lubricating light fractions, A suitable lubricating base oil can be obtained by performing purification by combining any one or more of hydrocracking, alkali distillation, sulfuric acid washing, clay treatment, and the like. Further, normal paraffins and isoparaffins having 11 to 15 carbon atoms can be suitably used. In the present invention, a mineral oil base oil obtained by refining a lubricating oil fraction having a boiling range such that the predetermined kinematic viscosity is obtained may be used alone, but a plurality of refined lubricating oil fractions may be used. The components may be mixed to prepare a predetermined kinematic viscosity.
[0010]
As the synthetic base oil, poly-α-olefin, fatty acid ester, phosphate ester, polyalkylene glycol and the like are suitable. These synthetic base oils may be used alone or in combination.
[0011]
In the acidic phosphate ester salt represented by the general formula (1), R 1 is a linear or branched alkyl group having 3 to 25 carbon atoms, an alkenyl group, or an alkyl-substituted or unsubstituted aromatic group. Among them, those having 5 to 20 carbon atoms are more preferable, and those having a hexyl group, an octyl group, an oleyl group, and a tolyl group are particularly preferable because they are easily available.
Further, R 2 in the above formula is a linear or branched alkyl group having 1 to 25 carbon atoms, and particularly preferably one having 5 to 20 carbon atoms.
[0012]
In the present invention, instead of adding the acidic phosphate amine salt of the general formula (1), an ester corresponding to the acidic phosphate ester portion on the left side of the general formula (1) and the equivalent thereof Alternatively, the amine corresponding to the right amine part of the general formula (1) below is added separately to form an acidic phosphate amine salt of the general formula (1) in the lubricating oil. Also good.
These acidic phosphate ester amine salts may be contained in an amount of 0.1 to 5% by mass, preferably 0.2 to 1% by mass, based on the total amount of the lubricating oil.
[0013]
A thiophosphate ester can also be blended in the bearing lubricating oil composition of the present invention. As this thiophosphate ester, those generally used as extreme pressure agents for lubricating oils can be used. In particular, the use of a compound represented by the following general formula (2) is preferable from the viewpoint of corrosion resistance. preferable.
[0014]
[Chemical 2]
(R 3 —O—) 3 P = S (2)
[0015]
In the above formula, R 3 represents a substituted or unsubstituted aromatic. R 3 is particularly preferably a phenyl group or a t-butylphenyl group.
These thiophosphates may be contained in an amount of 0.05 to 2% by mass, preferably 0.1 to 1% by mass, based on the total amount of the lubricating oil.
[0016]
The thiadiazole compound used in the present invention can be used without any problem as long as it has a thiadiazole skeleton, and in particular, a compound in which a sulfide group or a polysulfide group is substituted on the carbon in the thiadiazole skeleton, for example, 1, 3, In the compound having a 4-thiadiazole skeleton, a compound represented by the following general formula (3) is preferable.
[Chemical 3]
[0017]
R 4 and R 5 in the above formula are each independently a hydrocarbon group having 5 to 30 carbon atoms, and m and n are each independently an integer of 1 to 4.
In addition, this skeleton portion can be used in the same manner as the 1,2,3-isomer, 1,2,4-isomer other than the 1,3,4-isomer, and two or more kinds of thiadiazole compounds. Even if they are mixed, there is no problem for the purpose of the present invention. The hydrocarbon group of R 4 and R 5 in the general formula (3) may be linear and / or branched, saturated and / or unsaturated, particularly an alkyl group having 5 to 15 carbon atoms. Is preferred.
The thiadiazole compound used in the present invention may be contained in an amount of 0.01-2% by mass, preferably 0.03-1% by mass, based on the total amount of the lubricating oil.
[0018]
The bearing lubricating oil composition of the present invention contains other commonly used lubricating oil additives such as antioxidants, rust inhibitors, viscosity index improvers, pour point depressants, antifoaming agents, metal An activator or the like can be appropriately added.
Examples of the antioxidant include phenol compounds such as di-t-butylparacresol, amine compounds such as alkylated diphenylamine and α-naphthylamine, and phosphorus compounds such as phosphite.
Examples of the rust inhibitor include alkenyl succinic acid esters, alkenyl succinic acid partial esters, sorbitan esters, and sulfonic acid metal salts.
Examples of the viscosity index improver and the pour point depressant include polymethacrylate polymers and olefin copolymers.
Examples of antifoaming agents include silicone polymers and polymethacrylate polymers.
Examples of the metal deactivator include benzotriazole and benzotriazole derivatives.
[0019]
【Example】
Hereinafter, although the lubricating oil composition for bearings of the present invention will be described in more detail with reference to Examples, the present invention is not limited thereto.
In preparing the bearing lubricating oil compositions of Examples and Comparative Examples, the following base materials were used. The following base oil and additive were stirred and heated at 60 ° C. for 1 hour, and the dissolution of the additive was confirmed and subjected to the test.
[0020]
(1) Lubricating base oil A mixture of normal paraffins having 12 and 13 carbon atoms in a mass ratio of 60:40 was used as the base oil. The kinematic viscosity at 40 ° C. is 1.5 mm 2 / s.
[0021]
(2) Additive (a) Antiwear Agent As the antiwear agent, the following acidic phosphate amine salts, thiophosphate esters, and thiadiazoles were used. For comparison, ZnDTP (zinc dialkyldithiophosphate) was also used.
a-1: Acid phosphate ester amine salt [R 1 in formula (1): n-hexyl, R 2 : C11-C14 alkyl group]
a-2: Acid phosphate ester amine salt [R 1 in formula (1): oleyl, R 2 : alkyl group of C8]
a-3: thiophosphate [R 3 in formula (2): t-butylphenyl]
a-4: thiadiazole [R 4 + R 5 in formula (3): alkyl group, total carbon number 22, m, n: 3]
a-5: ZnDTP
[Sec. C6 alkyl group type]
(B) Antioxidant b-1: Phenolic antioxidant [di-t-butylparacresol]
b-2: Amine-based antioxidant [dioctyldiphenylamine]
[0022]
(3) Evaluation of lubricity The wear resistance and load bearing capacity of the test oil were evaluated. The abrasion resistance was measured by a wear mark (mm) according to a shell 4-ball abrasion resistance test method (according to ASTM D2260, 1400 rpm, 15 kgf / cm 2 , 30 min, room temperature). The load bearing capacity was measured by the seizure load (MPa) according to the Kamata type 4-ball method load bearing capacity test method (JIS K 2519, Shock method).
[0023]
(4) Evaluation of mixing stability with water-soluble cutting oil Copper corrosivity and sludge precipitation due to mixing of the test oil and water-soluble cutting oil were evaluated by the following methods. To 200 ml of the test oil, 20 ml of 20-fold diluted water-soluble cutting oil [A1 type (emulsion type) or A2 type (soluble type)] with purified water is added, and in the presence of a copper plate catalyst, the number of revolutions is 1500 rpm, The mixture was stirred at a temperature of 60 ° C. for 168 hours (using a device of JIS K 2510). For the sample oil after stirring, the discoloration of the copper plate catalyst (score according to the provisions of JIS K 2513) was observed, and the degree of contamination (JIS B 9931) was measured.
The above results of Examples and Comparative Examples are summarized in Table 1.
[0024]
[Table 1]
[0025]
In Examples 1 to 5 in which acidic phosphate ester was blended as an antiwear agent, the discoloration of copper was good at the 1b level in both the water-soluble cutting oils A1 and A2. Further, the degree of contamination is 11 mg / 100 ml or less, which is significantly smaller than the comparative example shown later. Lubricating property showed the comparative example level, while maintaining abrasion resistance by mix | blending a predetermined amount of thiophosphate ester and / or thiadiazole with acidic phosphate ester amine salt. From this, in order to have excellent mixing stability with water-soluble cutting oil and excellent wear resistance, the compounding of acidic phosphate amine salt is effective, and further to impart load bearing capacity It has been confirmed that it is promising to mix a predetermined amount of thiophosphate and / or thiadiazole.
The comparative example 1 which mix | blended ZnDTP as an antiwear agent showed the outstanding abrasion resistance and load bearing capacity. However, in the mixing test with the water-soluble cutting oil A1 type, the degree of contamination was high, and with the A2 type, the discoloration of copper was large.
[0026]
【The invention's effect】
The bearing lubricating oil composition of the present invention has high wear resistance and load resistance, and exhibits a special effect that sludge generation and corrosion problems hardly occur even when a water-soluble cutting oil is mixed.
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JP6666691B2 (en) * | 2015-11-04 | 2020-03-18 | シェルルブリカンツジャパン株式会社 | Lubricating oil composition |
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