Desarrollo de un material compuesto de polietileno de alta densidad reciclado reforzado con fibras de cisco de café - caracterización dinámico mecánica

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(31) 9')(.!0./!7*()C6.74!<.!9*.)0.!.7!/'<!8'/*@)'8*47.<!E!03)'7(.!./!//.7'04!0./!('7l3.!0.! @'D'!9).<*C7$!. ! !"#$%&'()*+,-C.,/3&4)4'$,43,+)%&*K3+5,3+,3",%'+;#3,43,7'H',:&3$)*+,. A/!=404!.7!./!l3.!<.!i*8*.)47!/'<!9)*=.)'<!9)3.@'<!2'//*0'<!23.!./!0.!=3/(*c2).83.78*'<! 847! 37'! )'=9'! 0.! (.=9.)'(3)'! .7().! r%#PzK! E! %P"zK! 847! 37! (*.=94! 0.! ).94<4! '! r %#PzK!0.!P!=*73(4<!E!37!*78).=.7(4!0.!#zKs=*7$j!37'!2).83.78*'!f7*8'!0.!%!R+!E!37'! 0.24)='8*C7!0./!"$%e$! A/!=47('D.!0.!/'<!9)4@.('<!<.!i*+4!*7*8*'/=.7(.!.7!./!8/'=9!0.!8F&''$(5+-8$1'-.!/3.64! <.!84))*6*C!93.<!/4<!).<3/('04<!4@(.7*04<!).9).<.7('@'7!<4/4!)3*04$!A<(4!<.!0.@.!'!l3.! ./!='(.)*'/!74!.<!<32*8*.7(.=.7(.!9.<'04!E!<.!=3.h.!0.7()4!0.!/'!9)4@.('!94)!l3.!74! .<(k! 2*D4! .7! /4<! .B().=4<$! I'=@*H7! <.! 84))*6*.)47! /4<! 9')k=.()4<! 0.! (.=9.)'(3)'! E! 2).83.78*'! @'<'04<! .7! N%:O ya que el rango era muy amplio y dados los niveles de nitrógeno disponibles se prefirió hacer un mayor numero de pruebas. Los parámetros para las pruebas subsiguientes fueron entonces, manteniendo el modo de !. -S!.

(32) multi-frecuencias, temperaturas entre -120˚C y 100˚C con tiempo de reposo en -120˚C de dos minutos e incremento de temperatura de 3˚C/min., frecuencia única de 5 Hz y una deformación del 0.1%. En las normas de la ASTM utilizan un aumento de temperatura de 2˚C/min., sin embargo en la literatura recomiendan el aumento mencionado anteriormente ya que mantiene la resolución de los datos y acorta el tiempo de cada prueba. El montaje de las probetas, se hizo esta vez en el clamp de dual cantilever para asegurar que la probeta esté fija en los extremos y en el medio logrando de esta forma mejores resultados. Cada prueba dura aproximadamente dos horas si se cuenta el tiempo de enfriado de la máquina, por esta razón la programación de los experimentos es de gran importancia. Se llevaron a cabo doce pruebas de las trece propuestas dada una restricción del nitrógeno líquido . Se escogieron aquellas que serían más probables de obtener un desempeño óptimo del material y se desechó aquella que se pensó seria la formulación menos óptima.. ! !"#$%&'()*+,--.,8"'9:,#%)")R'45,:'&',:&#37'$. !. -,!.

(33) E8%R',V$!"&),$ Para los resultados se decidió mostrar gráficas de cada formulación de matriz/refuerzo con todas las variaciones en cantidad de agente de acople presentes. De esta manera se puede explorar de forma más concisa cómo influye el agente de acople. Así mismo se generaron gráficas donde se aprecia que la concentración del agente de acople se mantiene constante y se observa cómo afecta las propiedades, la cantidad de refuerzo dentro de la matriz afecta. Luego se generaron gráficas que conjugan los mejores y peores resultados dadas las condiciones anteriores. Los resultados obtenidos reflejan las predicciones hechas a partir de las especulaciones basadas en la bibliografía revisada. Hay ciertas discrepancias que se explicarán luego al ver los gráficos.. E8;%FA0:/3%01%"/G-214-G61453% Las graficas del módulo de almacenamiento, como se discutió anteriormente, representan la energía que el material retiene durante los ciclos de carga. Esta es mayor cuando el material está cerca de su zona mas elástica y va decreciendo a medida que el material se vuelve más viscoso. El módulo de almacenamiento también esta relacionado directamente con la capacidad del material para soportar carga. Es evidente en las gráficas siguientes que, al agregar cisco de café a la matriz, tiene un efecto claro en el módulo incrementándolo casi un 50% en el mejor de los casos. Se presentarán las gráficas mas representativas a continuación, el resto se encuentran en los anexos.. !. #"!.

(34) ! T&'=)(',-.,D*4#"5,43,1"9'(3+'9)3+%5,',CU,'K3+%3,43,'(5:"3. Se puede notar en la Gráfica 1, cómo se distancian las formulaciones del material virgen. Se nota claramente que la mejor combinación en todos los casos, sin tener en cuenta el agente de acople, es la de 60% PEAD y 40% fibra. La caída en el valor de E’, primero lentamente y luego más aceleradamente se da a medida que el material pierde su comportamiento elástico, al hacerse mas acelerada la caída el refuerzo la compensa y atenúa. Esto se debe a que las fibras obstaculizan el movimiento de los meros, y por tanto la disipación de energía, lo que demuestra también una mayor estabilidad térmica de la matriz gracias a la fibra.. !. #%!.

(35) ! T&'=)(',?.,D*4#"5,43,'"9'(3+'9)3+%5,',IU,'K3+%3,43,'(5:"3. Al analizar los valores de las dos gráficas también notamos que, contra nuestras predicciones, no son aquellas formulaciones que tienen el agente de acople las que mejor desempeño tienen. Esto se puede apreciar mejor en la gráfica siguiente. Al analizar el problema se llegó a la conclusión que la forma de preparar las fibras con el anhídrido maleico no es la mas adecuada. Esto se debe a dos razones, la primera, que las fibras deben sumergirse en un líquido y al secarse en el horno se pegan unas a otras; aunque el proceso de premezcla intentó separarlas, la dispersión de éstas en la matriz no fue la mejor. La segunda, el porcentaje de agente de acople realmente presente en la mezcla no es tan fácil de controlar y por ende no produce resultados totalmente claros de la situación. El mejor desempeño se obtiene con las fibras sin anhídrido maleico porque éstas se comportan como fibras de menor tamaño, cualidad que se ha encontrado mejora de manera sustancial el comportamiento del material en este sentido.. !. #-!.

(36) ! T&'=)(',@.,D*4#"5,43,1"9'(3+'9)3+%5,(5+,JCU,/012,E,GCU,=)7&'. A continuación se presenta una gráfica en la cual se pueden apreciar las formulaciones con el mejor y peor desempeño, junto con el comportamiento del material virgen. Esto con el propósito de acentuar la diferencia entre los dos y para demostrar que aun la peor formulación ofrece una mejoría en comparación con el material virgen.. ! T&'=)(',G.,D*4#"5,43,'"9'(3+'9)3+%5,93H5&,E,:35&,&3$#"%'45. !. ##!.

(37) E8<%FA0:/3%01%HJ>060-% Como se dijo anteriormente las gráficas del módulo de pérdida representan la energía que ‘pierde’ o disipa el material durante los ciclos de carga. En las gráficas podemos ver dos picos claros de relajación, el " y el #. El pico " es el que aparece totalmente a la izquierda y que no está completo; este corresponde a la temperatura de transición vítrea (Tg) del material. En estudios similares se había notado que este pico se movía levemente a una temperatura mayor, pero en el estudio actual esto ocurrió muy poco. Al llevar a cabo otras pruebas con intervalos de temperatura más cortos, para tener una mejor imagen de lo que sucede, se sugiere para estudios futuros llevar el material a temperaturas más bajas y para ver que sucede antes del pico ". El segundo pico, #, se asocia al movimiento de segmentos de cadena en las fases cristalinas relacionados a la reorganización de defectos en los cristales [14].. ! T&'=)(',I.,D54#"5,43,:3&4)4',(5+,GCU,/012,E,JCU,=)7&'. En la gráfica siguiente se aprecia mejor que en la anterior cómo el pico de relajación #. !. #:!.

(38) incrementa su valor a casi el triple del valor de la matriz virgen. El incremento se debe probablemente a la presencia de fibras de cisco de café que reducen la flexibilidad de la matriz introduciendo restricciones en el movimiento de meros en las temperaturas de relajación [14]. No es muy claramente evidenciable la función del agente de acople en las gráficas por la misma razón ya mencionada anteriormente sobre el uso del mismo.. ! T&'=)(',J.,D*4#"5,43,:3&4)4',(5+,JCU,/012,E,GCU,=)7&'. El efecto de la adición de fibras en diferentes porcentajes, bajo el mismo porcentaje de AM, se refleja en la gráfica siguiente en donde se puede apreciar que, en el caso del módulo de pérdida, a diferencia del módulo de almacenamiento, la mejor combinación es la de 50% fibra y 50% PEAD. Se podría decir que hay suficiente matriz para contener a la fibra y suficiente fibra para retirarle carga a la matriz.. !. #P!.

(39) ! T&'=)(',O.,D*4#"5,43,:3&4)4',',IU,'K3+%3,43,'(5:"3. Como se mostró con E’, a continuación se presenta una gráfica comparativa del mejor desempeño, el peor desempeño y el material virgen para ilustrar mejor el beneficio que obtenido.. ! T&'=)(',B.,D*4#"5,43,:3&4)4',93H5&,E,:35&,&3$#"%'45,. ! !. #>!.

(40) !. E8@%!-4P1451%01%01/5-% Las gráficas de tangente de delta muestran cuánta respuesta tiene el material, en términos de deformación, ante un esfuerzo dado. Como se dijo anteriormente, delta es el ángulo de desfase entre la señal de entrada y la de salida, entre más se acerque a cero la tangente, mejor se comporta el material elásticamente. Teniendo esto en mente podemos apreciar cómo ocurre esto al adicionar fibras a la matriz. Como se evidencia en las gráficas, el valor inicial de tan ! decrece, mantiene un comportamiento similar al de la matriz en la zona media y, cuando ya comienza a fluir el material, se mantiene de nuevo por debajo.. ! T&'=)(',S.,6'+K3+%3,43,43"%',GCU,/012,E,JCU,=)7&'. La cantidad de fibra agregada a la matriz es, de nuevo, un factor determinante como se puede notar en la gráfica anterior, 60% de fibra, y en la gráfica siguiente, 40% de fibra. La reducción visible en los picos sucede porque son las fibras las que soportan el esfuerzo y no permiten en gran parte que se deforme la matriz. En este caso, la mayor cantidad de fibra. !. #G!.

(41) no logra que el comportamiento sea mejor durante todo el ciclo de carga, pero podemos ver como actúa en el primer pico de relajación teniendo mucho menor desfase. En el área media, y cuando el material ya es altamente viscoso, la segunda combinación se comporta mucho mejor como lo podemos comprobar en la gráfica siguiente. Se puede apreciar también que no existe mucha diferencia entre aquellas fibras que fueron tratadas con anhídrido maleico y aquellas que no lo fueron. Esto, como se comentó anteriormente, se debe a los malos resultados que se tuvieron al mezclar el agente de acople a la fibra y no a la matriz. De todas maneras se puede evidenciar cierta acción de la interfase.. ! T&'=)(',-C.,6'+K3+%3,43,43"%',JCU,/012,GCU,=)7&'. En este caso nos concentramos en analizar cuál formulación de fibra es óptima para el caso de la tangente de delta y encontramos que, a diferencia del módulo de pérdida, la combinación optima es la de 40% fibra y 60% PEAD como lo fue para el módulo de almacenamiento. Esta comprobación reitera lo comentado antes sobre el módulo de almacenamiento y la manera en la cual esa combinación parece ser la más propicia en !. #S!.

(42) términos de otorgarle rigidez al material.. ! T&'=)(',--.,6'+K3+%3,43,43"%',9'%3&)'",'",IU,43,'K3+%3,43,'(5:"3. A continuación se muestra la gráfica del mejor y el peor desempeño para ilustrar mejor las diferencias entre una y otra y ofrecer una comparación fiable con la matriz.. % T&'=)(',-?.,6'+K3+%3,43,43"%',93H5&,E,:35&,&3$#"%'45,. !. #,!.

(43) I8%"*a$+,+,%b%&+,(V,+X*% K4=4! <.! 93.0.! h.)! 8/')'=.7(.! .7! /4<! ).<3/('04<! /'<! 9)49*.0'0.<! 0./! ='(.)*'/! 84=93.<(4! <47! =.D4).<j! .7! (H)=*74<! =.8k7*84<j! l3.! /'<! 0./! ='(.)*'/! h*)6.7$! M*7! .=@')64!9')'!(.7.)!37'!=.D4)!h*<*C7!0.!.<(4<!8'=@*4<!.<!7.8.<')*4!84=9')')/4<!847! 4()4<!84=93.<(4<!<*=*/').<!8).'04<!'!7*h./!*7(.)7'8*47'/$!! T7! .<(30*4! <.=.D'7(.! .7! 0470.! <.! =*0*.)47! /'<! 9)49*.0'0.<! 0./! 84=93.<(4! .7().! RF;As2*@)'! 0.! E3(.! N%:O! .7847()C! l3.! /'<! 9)49*.0'0.<! =.8k7*8'<! 0./! ='(.)*'/! =.D4)'@'7! '/! '0*8*47')! '6.7(.! 0.! '849/.$! A<(4! <.! h.! ).2/.D'04! .7! ./! '3=.7(4! .7! ./! =403/4! 0.! '/='8.7'=*.7(4$! R'E! 37'! '7'/46Q'! .7! .<(.! <.7(*04! .7().! ./! 84=93.<(4! ()'('04! .7! .<(.! 9)4E.8(4! E! 'l3./! i.8i4! 847! E3(.$! A7! /4<! <*63*.7(.<! 04<! 6)k2*84<! <.! 93.0.! h.)! l3.! /4<! 4)0.7.<! 0.! ='67*(30j! ('7(4! 84=4! 0./! ='(.)*'/! h*)6.7! 84=4! 0./! ='(.)*'/!84=93.<(4j!<47!'7k/464<$!A7!/'!I'@/'!<3@<*63*.7(.!<.!847<*67')47!h'/4).<!'! 0*2.).7(.<!(.=9.)'(3)'<!9')'!h.)!.<('<!<*=*/*(30.<!='<!8/')'=.7(.$!. ! T&'=)(',-@.,D*4#"5,43,'"9'(3+'9)3+%5,:'&',(59:#3$%5,/012VE#%3N,14':%'4',43,W-GX,. !. :"!.

(44) ! T&F=)(',-G.,D*4#"5,43,'"9'(3+'9)3+%5,(5+,JCU,/012,E,GCU,=)7&'N,. R'E!l3.!(.7.)!.7!=.7(.!l3.!'37l3.!/4<!C)0.7.<!0.!='67*(30!<.!='7(*.7.7!0.7()4!0.! /4<! =*<=4! /Q=*(.<! i'E! 8'=@*4<! .7! /4<! h'/4).<$! A<(4! <.! 0.@.! 94<*@/.=.7(.! '! 04<! 2'8(4).<j!./!9)*=.)4j!.7!./!84=93.<(4!;A5FsE3(.!3(*/*+')47!37'!8')6'!0.!2*@)'!0./!#"e! =*.7()'<!l3.!/'!=.D4)!.7847()'0'!9')'!;A5Fs8*<84!0.!8'2H!23.!0.!:"e$!A<(4!84=4!<.! .B93<4!'7(.)*4)=.7(.!(*.7.!37!.2.8(4!0*).8(4!<4@).!/'<!9)49*.0'0.<!94)l3.!/'!2*@)'!/.! 4(4)6'!)*6*0.+!'!/'!='()*+$!A/!<.63704!2'8(4)!23.!/'!*784)).8('!3(*/*+'8*C7!0./!'6.7(.!0.! '849/.!.7!.<(.!()'@'D4j!.2.8(4!l3.!<.!93.0.!'9).8*')!.7!/'!0*2.).78*'!.B*<(.7(.!.7().!/4<! ).<3/('04<! 0./! ')(Q83/4! 0470.! /'<! 9)49*.0'0.<! <*63.7! =.D4)'704! '/! '6).6')! ./! '7iQ0)*04!='/.*84!E!.7!/4<!).<3/('04<!0./!9).<.7(.!()'@'D4!0.!*7h.<(*6'8*C7j!.7!./!83'/! ./!=.D4)!).70*=*.7(4!<.!4@(3h4!847!./!84=93.<(4!<*7!'6.7(.!0.!'849/.$!V4!4@<('7(.j!<.! '9).8*'!8C=4!/'!'0*8*C7!0.!8*.)('!8'7(*0'0!0.!'7iQ0)*04!='/.*84j!.7!.<(.!8'<4!8.)8'!'/! Pej! 9)4038.! @3.74<! ).<3/('04<$! A<! *=94)('7(.! '74(')! l3.! .7! '=@'<! =.0*8*47.<! /4<!. !. :%!.

(45) h'/4).<! 0./! ;A5F! h*)6.7! <47! 9)k8(*8'=.7(.! /4<! =*<=4<j! 0.! .<'! ='7.)'! 940.=4<! 8472*)=')!l3.!/4<!).<3/('04<!<47!8472*'@/.<$! Temperatura (˚C) -120. 0. 100. PEAD virgen. 2.50E+03 1.30E+03 3.00E+02. PEAD/Yute (70/30)[14]. 3.50E+03 1.90E+03 5.00E+02. Módulo de PEAD/Yute+PEMA[14] 3.70E+03 2.50E+03 9.00E+02 Almacenamiento (Mpa) PEAD/Cisco de café (60/40) 6.00E+03 3.00E+03 8.00E+02 PEAD/Cisco de café +AM. 5.00E+03 2.70E+03 8.00E+02. 6'7"',G.,859:'&'()*+,9*4#"5,43,'"9'(3+'9)3+%5,/012VE#%3,E,/012V()$(5,43,('=>,. 5!=3E!@'D'<!(.=9.)'(3)'<!940.=4<!4@<.)h')!l3.!./!84=93.<(4!847!8*<84!0.!8'2H!(*.7.! 37! 84=94)('=*.7(4! 8.)8'! 0.! >"e! =.D4)! l3.! ./! 0.! E3(.j! (.7*.704! .7! 83.7('! /4! .<('@/.8*04! <4@).! /'! 8')6'! 0.! 2*@)'! .7! 8'0'! 374$! M*7! .=@')64j! '/! '3=.7(')! /'! (.=9.)'(3)'! <.! '9).8*'! 8C=4! /'<! 9)49*.0'0.<! <.! .l3*9')'7! E! ./! 84=94)('=*.7(4j! '/! '3=.7(')!/'!h*<84<*0'0j!.<!8'<*!./!=*<=4$!!M.!93.0.!.<('@/.8.)!37'!'7'/46Q'!9').8*0'! .7! ./! 8'<4! 0.! /4<! 4()4<! 04<! 2'8(4).<! l3.! 23.)47! .<(30*'04<j! .7847()'704! <*=*/').<! ).<3/('04<!0.!'l3.//4<!0./!')(*83/4!847<3/('04$! K4=4!<.!i.!9).<.7('04!'!()'hH<!0./!9).<.7(.!()'@'D4!E!.7!/'<!).2.).78*'<!847<3/('0'<j! /4<!2'8(4).<!l3.!23.)47!8'=@*'04<!<47!0.!'/('!*=94)('78*'!.7!./!84=94)('=*.7(4!0./! 84=93.<(4j!94)!.<('!)'+C7!<.!6.7.)C!37!6)'2*84!.7!./!83'/!<.!84=9')'7!8'0'!37'!0.!/'<! 24)=3/'8*47.<!'!37'!(.=9.)'(3)'!0'0'j!9')'!'<Q!4@<.)h')!<*!.B*<(.!37'!(.70.78*'!.7!/'! h')*'8*C7!0.!/4<!2'8(4).<$!. !. :-!.

(46) ;')'! i'8.)! /'! 84=9')'8*C7! <.! 6.7.)')47! ().<! 6)k2*8'<! '! (.=9.)'(3)'<! l3.! <.! 847<*0.)')47! *=94)('7(.<! .7! 8'0'! 374! 0.! /4<! 8'<4<$! A7! ./! 8'<4! 0./! =C03/4! 0.! '/='8.7'=*.7(4!<.!.<846*C!37'!(.=9.)'(3)'!=.0*'j!847!/'!83'/!./!84=94)('=*.7(4!0./! ='(.)*'/!.<!847<('7(.j!.<('!(.=9.)'(3)'!23.!0.!"zK$!A7!./!8'<4!0./!=C03/4!0.!9H)0*0'! <.!./*6*C!/'!(.=9.)'(3)'!=k<!8.)8'7'!'/!9*84!'/2'!94)l3.!.<(.!.<!./!=4=.7(4!.7!./!83'/! ./!='(.)*'/!84=*.7+'!'!84=94)(')<.!847!=k<!h*<84<*0'0j!/'!(.=9.)'(3)'!.<846*0'!23.! 0.!P"!zK$!;4)!f/(*=4j!9')'!./!8'<4!0.!/'!('76.7(.!0.!0./('!<.!3(*/*+C!/'!(.=9.)'(3)'!=k<! 8.)8'7'!'!/'!(.=9.)'(3)'!0.!()'7<*8*C7!hQ().'j!93.<!.7!.<(.!937(4!.<!74(4)*4!./!8'=@*4! '/!h')*')!/4<!2'8(4).<!E'!.B93.<(4<j!/'!(.=9.)'(3)'!.<846*0'!23.!r%-"zK$!. ! T&F=)(',-I.,D*4#"5,43,'"9'(3+'9)3+%5,3+,=#+()*+,43,('+%)4'4,43,=)7&',E,:5&(3+%'H3,43,'K3+%3,43,'(5:"3N,. M.!4@<.)h'!37'!(.70.78*'!8/')'!.7!/'!=.D4)Q'!0./!=C03/4!0.!'/='8.7'=*.7(4!0470.!.<! =.D4)! ./! ).70*=*.7(4! =*.7()'<! /'! 8'7(*0'0! 0.! 2*@)'! (*.70.! '/! :"! e! 0.! 8')6'! E! ./!. !. :#!.

(47) 94)8.7('D.!0./!'6.7(.!0.!'849/.!(*.70.!'!8.)4$!A/!9.4)!).70*=*.7(4!/4!.7847()'=4<!847! /'!84=@*7'8*C7!0.!P"!e!0.!2*@)'!E!%"e!'6.7(.!0.!'849/.$!. ! T&F=)(',-J.,D*4#"5,43,:>&4)4',3+,=#+()*+,43,('+%)4'4,43,=)7&',E,:5&(3+%'H3,43,'K3+%3,43,'(5:"3N,. A7! ./! 8'<4! 0./! =C03/4! 0.! 9H)0*0'! <.! 4@<.)h'! /'! =*<='! (.70.78*'! l3.! .7! ./! '7(.)*4)! 8472*)='704! 0.! .<('! ='7.)'! /'<! <394<*8*47.<! <4@).! ./! 3<4! 0.! 8'0'! 37'! 0.! /'<! h')*'@/.<$! A7! .<(.! 8'<4! /'! f7*8'! 0*2.).78*'! l3.! <.! 4@<.)h'! 847<*<(.! .7! l3.! ./! =.D4)! 0.<.=9.g4!<.!.783.7()'!.7!/'!84=@*7'8*C7!0.!P"e!2*@)'!E!"e!'6.7(.!0.!'849/.$!M*7! .=@')64! <.! 4@<.)h'! ('=@*H7! l3.! /'! (.70.78*'! 0./! 6)k2*84! i'8*'! /4<! =*<=4<! h'/4).<! l3.! .7! ./! 8'<4! '7(.)*4)! .<! 8/')'$! A<! )'+47'@/.! 9.7<')! l3.! 37'! 8')6'! 0.! '7iQ0)*04! ='/.*84!0./!%Pe!<.!'8.)8'!'!/4<!).<3/('04<!C9(*=4<j!9.)4!0'0'!/'!(.70.78*'!0./!).<(4! 0.!/'!6)k2*8'!.<!hk/*04!0.8*)!l3.!/4<!=.D4).<!).<3/('04<!<.!.783.7()'7!.7!/'<!=.74).<! 8478.7()'8*47.<!0./!'6.7(.!0.!'849/.$!!. !. ::!.

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Referencias