ES2563407T3 - Composición de grasa lubricante - Google Patents

Composición de grasa lubricante Download PDF

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Publication number
ES2563407T3
ES2563407T3 ES08758645.9T ES08758645T ES2563407T3 ES 2563407 T3 ES2563407 T3 ES 2563407T3 ES 08758645 T ES08758645 T ES 08758645T ES 2563407 T3 ES2563407 T3 ES 2563407T3
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Prior art keywords
fat
members
mixture
group
agents
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Inventor
Günther BODESHEIM
Martin Schmidt-Amelunxen
Dieter Sohn
Stefan Grundei
Andrea HÖPKE
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Klueber Lubrication Muenchen GmbH and Co KG
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Klueber Lubrication Muenchen SE and Co KG
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    • C10M133/00Lubricating compositions characterised by the additive being an organic non-macromolecular compound containing nitrogen
    • C10M133/02Lubricating compositions characterised by the additive being an organic non-macromolecular compound containing nitrogen having a carbon chain of less than 30 atoms
    • C10M133/38Heterocyclic nitrogen compounds
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    • C10M135/08Lubricating compositions characterised by the additive being an organic non-macromolecular compound containing sulfur, selenium or tellurium containing a sulfur-to-oxygen bond
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    • C10M2201/066Molybdenum sulfide
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    • C10M2217/044Polyamides
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    • C10M2229/025Unspecified siloxanes; Silicones used as base material
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Abstract

Composición de grasa lubricante que consta de una mezcla de (a) un 5 a un 95% en peso de aceite base hecho a base de aceites con viscosidad habitual para lubricantes industriales, que consta de un éster de un ácido di-, tri- o tetracarboxílico aromático o alifático con un alcohol de C7 a C22 o con alcoholes de C7 a C22 en forma de mezcla, de un polifeniléter o difeniléter alquilado, de un éster de trimetilolpropano, pentaeritrito o dipentaeritrito con ácidos carboxílicos alifáticos de C7 a C22, de ésteres de ácidos dímeros de C18 con alcoholes de C7 a C22, y de ésteres complejos, como componentes únicos o en cualquier mezcla, o se selecciona de entre los miembros del grupo que consta de poli-α-olefinas, naftalinas alquiladas, benzoles alquilados, poliglicoles, aceites de silicona y perfluoropoliéteres, (b) un 1 a un 30% en peso de líquido iónico o de una mezcla de varios líquidos iónicos seleccionados de entre los miembros del grupo que consta de trihexil(tetradecil)fosfonio-bis(trifluorometilsulfonil)imida, N-etil-3-metilpiridinio-nona-fluorobutanosulfonato, butilmetilpirrolidinio-bis(trifluorometilsulfonil)imida, 1-etil-3-metilimidazolio-(bis)trifluorometilsufonilimida, 1-etil-3-metilimidazoliometilsulfato, (c) un 3 a un 50% en peso de espesante seleccionado de entre los miembros del grupo que consta de un producto de reacción de un diisocianato, 2,4-diisocianatotoluol, 2,6-diisocianatotoluol, 4,4'- diisocianatodifenilmetano, 2,4'-diisocianatodifenilmetano, 4,4'-diisocianatodifenilo, 4,4'-diisocianato-3,3'- dimetildifenilo, 4,4'-diisocianato-3,3'-dimetilfenil-metano, que pueden usarse en solitario o bien en combinación, con una amina de fórmula general R'2N-R, o una diamina de fórmula general R'2N-R-N-R'2, en donde R es un resto arilo, alquilo o alquileno con 2 a 22 átomos de carbono y R' es idéntico o distinto y es hidrógeno o un resto alquilo, alquileno o arilo, o con una mezcla de aminas de diaminas o bien jabones metálicos, sulfonatos metálicos, jabones complejos metálicos, bentonita, polvo de silicato, politetrafluoroetileno (PTFE), poliamida y poliimida, y (d) un 0,1 a un 10% en peso de aditivos habituales en solitario o bien en combinación, seleccionados de entre los miembros del grupo que consta de agentes protectores contra la corrosión, agentes protectores contra la oxidación, agentes protectores contra el desgaste, agentes para la reducción del rozamiento, agentes para la protección contra las influencias metálicas, estabilizadores UV y lubricantes sólidos inorgánicos u orgánicos, seleccionados de entre los miembros del grupo que consta de poliimida, politetrafluoroetileno (PTFE), grafito, óxidos metálicos, nitruro de boro, disulfuro de molibdeno y fosfato.

Description

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EP 2164935
Tabla 3
Muestra
Formulación estándar con un 5% de MBPimida con un 2% de MBPimida con un 1% de MBPimida
Penetración en reposo en mm-1 DIN ISO 2137
278 264 264 274
Penetración de batanado 60 DT en mm-1 DIN ISO 2137
286 274 268 274
Separación de aceite 30 h 150ºC FTMS 791 C 321
10,1% 4,4% 4,6% 4,9%
Pérdida por evaporación 24 h 150ºC DIN 58397 Parte 1
3,98% 4,7% 4% 3,5%
[0049] También al usar de un 1 a un 5% en peso de líquido iónico se pone asimismo de manifiesto una reducida separación de aceite, incluso cuando el tiempo de ensayo se prolonga hasta 30 horas.
Ejemplo 3
[0050] En este ejemplo, a base de una grasa para rodamientos que consta de un hidrocarburo sintético, un éster sintético, un diisocianato aromático y monoaminas alifáticas se fabrica una grasa estándar a la que se le añade un 10% de MBPimida, y esta grasa se somete a ensayo en una máquina de pruebas de rodamientos ROF. Con esta prueba se determina la duración de la composición de grasa lubricante sometida a ensayo y se determinan las temperaturas superiores de uso de grasas lubricantes en rodamientos a altos números de revoluciones y bajas cargas axiales y radiales normalizadas. Como rodamiento de ensayo se usó un rodamiento ranurado de bolas 6204-2Z-C3/VM104 que estaba sometido a una carga de 100 N para la carga axial y 200 N para la carga radial, a un número de revoluciones de 18000 rpm y a una temperatura de 160ºC y que estaba cargado con una cantidad de llenado de 1,5 cm3. Se demostró que la composición de grasa lubricante sin IL tenía un valor L50 de 186 horas y la composición de grasa lubricante tenía un valor L50 de 717 horas. Esto demuestra el claro mejoramiento de la duración de una composición de grasa lubricante con líquido iónico.
Ejemplo 4
[0051] En este ejemplo se determina la fuerza de soldadura VKA según DIN 51350. Para ello se usó una grasa para rodamientos que constaba de éster sintético, perfluoropoliéter (PFPE), diisocionato aromático y una mezcla de aminas alifáticas y aromáticas. Fueron sometidas a la prueba de la fuerza de soldadura VKA las siguientes composiciones de grasa lubricante.
[0052] En cuanto a las composiciones de grasa lubricante, se trata de grasas de la clase NLGI 2-3: Grasa 1: Estándar con perfluoropoliéter Grasa 2: Estándar sin perfluoropoliéter con un 2,5% de EMIMimida Grasa 3: Estándar sin perfluoropoliéter con un 5% de EMIMimida Grasa 4: Estándar sin perfluoropoliéter con un 7,5% de EMIMimida Grasa 5: Estándar sin perfluoropoliéter con un 10% de EMIMimida
Tabla 4
Grasa lubricante
VKA Fuerza tolerada/fuerza de soldadura/diámetro cazoleta
Grasa 1
1600 N / 1800 N / 2,6 mm
Grasa 2
1500 N / 1600 N / 2,5 mm
Grasa 3
2400 N / 2600 N / 3,2 mm
Grasa 4
3600 N / 3800 / 3,5 mm
Grasa 5
4400 N / 4600 N / 4,0 mm
[0053] La comparación de los valores VKA demuestra que con una adición de más de un 2,5% de líquido iónico se logra un mejor valor VKA.
Tabla 5
Grasa lubricante
Bequiet + VKA Fuerza tolerada/fuerza de soldadura/diámetro cazoleta
Grasa 1
GN4 1600 N / 1800 N / 2,6 mm
Grasa 5
GN4 4400 N / 4600 N / 4,0 mm
[0054] Además, con una adición de un 10% de líquido iónico se pone asimismo de manifiesto un mejor valor VKA para valores de ruido igual de buenos.
[0055] Las grasas fueron también sometidas a una prueba de grasas para rodamientos FE 9 en la que se determina la duración de las grasas sometidas a ensayo y se determina la temperatura superior de uso de grasas lubricantes en rodamientos a números de revoluciones medianos y cargas axiales medianas. Se usó como rodamiento un rodamiento
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especial FAG 529689 H 109 (que corresponde a un rodamiento de bolas de contacto angular 7206 B con jaula de acero), con una jaula JP2 a un número de revoluciones de 6000 rpm, una carga axial de 1500 N, una temperatura de 200ºC y una cantidad de llenado de 2 cm3. Las grasas lubricantes sometidas a ensayo y los resultados de los valores L10 y L50 están indicados en la Tabla 6.
Tabla 6
Grasa lubricante
Concepción de la grasa FE 9 200ºC
Grasa 1
Estándar con perfluoropoliéter L10: 10 h L50: 13 h
Grasa 3
Estándar sin PFPE + 5% de EMIMimida perfluoropoliéter L10: 8 h L50: 25 h
Grasa 5
Estándar sin PFPE + 10% de EMIMimida L10: 63 h L50: 80 h
Grasa 6
Estándar sin PFPE + 10% de MBPimida L10: 45 h L50: 55 h
Grasa 7
Estándar sin PFPE + 10% de EMMIMimida L10: 16 h L50: 72 h
[0056] La tabla demuestra que mediante la adición de líquidos iónicos las grasas tienen unos más largos tiempos de funcionamiento, como se desprende de la comparación con los valores determinados para la Grasa 1 con perfluoropoliéter sin líquidos iónicos.
[0057] Otra composición de grasa lubricante fue sometida a una prueba FAG FE 9, y a esta grasa sin PFPE le fue añadido un 10% de HDPimida (Grasa 8). Fueron obtenidos los siguientes tiempos de funcionamiento: L10: 66 h, L50: 101
h. Estos resultados demuestran que las composiciones de grasa lubricante según la invención satisfacen las exigencias para grasas para rodamientos según las normas DIN para una temperatura de uso de hasta 200ºC.
Ejemplo 5
[0058] En este ejemplo se determina la fuerza de soldadura VKA según DIN 51350. Para ello se usó una grasa para rodamientos que constaba de éster sintético, diisocianato aromático y aminas alifáticas como composición estándar. Las composiciones de grasa lubricante que se indican a continuación fueron entonces sometidas a la prueba de la fuerza de soldadura VKA.
[0059] En cuanto a las composiciones de grasa lubricante, se trata de grasas de la clase NLGI 2-3: Grasa 1: Estándar sin IL Grasa 2: Estándar con adición de un 5% de EMIMimida (sustituto del aceite) Grasa 3: Estándar con adición de un 10% de EMIMimida (sustituto del aceite)
Tabla 7
Grasa lubricante
VKA Fuerza tolerada/fuerza de soldadura/diámetro cazoleta
Grasa 1
< 1200 N
Grasa 2
1400 N / 1600 N / 2,5 mm
Grasa 3
3800 N / 4000 N / 3,5 mm
[0060] La Tabla 7 demuestra que la fuerza de soldadura mejora y se obtienen mejores valores VKA con el uso de IL en la grasa.
Tabla 8
Grasa lubricante
Bequiet + VKA Fuerza tolerada/fuerza de soldadura/diámetro cazoleta
Grasa 1
GN4 < 1200 N
Grasa 3
GN4 3800 N / 4000 N / 3,5 mm
[0061] Mejor valor VKA para un valor de ruido igual de bueno (uso de un 10% de IL): Además se estudió si mediante la adición de líquidos iónicos puede evitarse el endurecimiento de las grasas por acción de la temperatura.
[0062] Con exposición a una temperatura de 160ºC se usó una así llamada “prueba de la pequeña cápsula de aluminio”. Para ello se mide en primer lugar la viscosidad de la grasa aún no sometida a las condiciones de ensayo. En una pequeña cápsula de aluminio de un diámetro de aprox. 50 mm y una altura de aprox. 15 mm se aplica una capa lo más lisa y homogénea posible de la grasa a someter a ensayo hasta un % de la altura de la pequeña cápsula. A continuación la pequeña cápsula se cierra con la tapa adecuada. La pequeña cápsula cerrada se pone a continuación sobre una chapa de horno y se somete a elevada temperatura en un horno. Con un ritmo semanal se mide la viscosidad de la grasa.
8 EP 2164935
[0063] La viscosidad dinámica aparente se mide a 300 seg.-1 y a 25ºC.
[0064] Fueron sometidas a esta prueba las siguientes composiciones de grasa lubricante. Grasa 1: Formulación estándar sin IL Grasa 5: Adición de un 1% de EMIM etilsulfato Grasa 6: Adición de un 3% de EMIM etilsulfato Grasa 7: Adición de un 5% de EMIM etilsulfato
Tabla 9
Sin usar
1 semana 2 semanas 3 semanas
Grasa 1
2794 5545 4548 4650
Grasa 5
3312 2000 1842 1425
Grasa 6
3320 No mensurable -- ---
Grasa 7
3348 No mensurable -- --
10 [0065] Los valores de la viscosidad dinámica aparente están indicados en mPas.
[0066] Con una adición de un 1% de EMIM etilsulfato la grasa es más blanda, con un 3% la grasa es muy inhomogénea (no mensurable) y con un 5% queda totalmente “descompuesta” (no mensurable).
15 [0067] Puede apreciarse claramente que mediante la adición de un 1% de EMIM etilsulfato el material se mantiene más blando al verse sometido a alta temperatura.
Ejemplo 6
20 [0068] En este ejemplo se estudia el mejoramiento de las grasas para cojinetes de ruedas con la adición de líquidos iónicos. En particular las grasas para los rodamientos de las ruedas de los camiones están sujetas a estrictas exigencias tanto desde el punto de vista térmico como también con respecto a la carga. Una particularmente elevada solicitación térmica se da cuando los vehículos tienen que ser continuamente frenados al recorrer por ejemplo puertos de montaña. Para la simulación de esta solicitación se realizan ensayos de rodamientos FE 8 que están caracterizados por un
25 periódico cambio de temperatura.
[0069] Como grasa lubricante de base para estos ensayos se usa una composición hecha a base de una poli-α-olefina, un diisocianato aromático, una mezcla de aminas alifáticas y aromáticas y un jabón complejo de litio (estándar).
30 [0070] Se usaron las siguientes composiciones de grasa lubricante: Grasa 1: formulación estándar Grasa 2: estándar más un 5% de HDPimida
[0071] Estas composiciones de grasa lubricante fueron sometidas a los ensayos que se indican a continuación en la 35 Tabla 10.
Tabla 10
Grasa lubricante
Penetración en reposo en mm-1 Penetración de batanado 60 DT en mm-1 Resistencia al agua Fluopresión en mbares
Grasa 1
223 226 0 1125
Grasa 2
223 223 0 1075
Grasa lubricante
Separación de aceite 7 d 40ºC Separación de aceite 30 h 150ºC
Grasa 1
0,54% 2,85%
Grasa 2
0,57% 5,42%
40 [0072] La grasa a la que se añadió un 5% de HDPimida presentó una mayor separación de aceite.
[0073] Para estudiar el endurecimiento se realizó la prueba de la pequeña cápsula de aluminio con tapa que se ha descrito anteriormente.
45 [0074] Las mediciones de viscosidad se realizaron a 160ºC, y los valores están indicados en mPas. Tabla 11
sin usar
5 días 12 días 19 días 25 días 34 días
Grasa 1
9956 8014 8619 8771 10276 12243
Grasa 2
9395 7522 5492 5717 8817 8508
9
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US20100105586A1 (en) 2010-04-29
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MX2009013879A (es) 2010-01-27
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