JOINT MECHANICAL ACTIVATION OF POLYAMIDE PA-6 AND KAOLINITE. Branch of RAS, Kutateladze str., 18, Novosibirsk (Russia)

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1 JOINT MECHANICAL ACTIVATION OF POLYAMIDE PA-6 AND KAOLINITE I.A. Vorsina 1, T.F. Grigorieva 1, T.A. Udalova 1, E.V. Ovchinnikov 2, V.A. Struk 2, N.Z. Lyakhov 1 1 Institute of Solid State Chemistry and Mechanochemistry, Siberian Branch of RAS, Kutateladze str., 18, Novosibirsk (Russia) 2 Yanka Kupala Grodno State University, Grodno (Belarus) grig@solid.nsk.ru Polyamide PA-6 is one of the leaders among construction materials, it has high heat endurance, high level of mechanical characteristics, good antifriction properties. Because of good antifriction properties, PA-6 is introduced as an additive into lubricants, most frequently in the form of the polymer composite incorporating also modifying agents. These composites based on simple and complex oxides possess high wear resistance. The formation of a polymeric composite, independently of the method used, involves adhesion of the polymer to the particles of the modifying agent; this process is accompanied by the formation of physical (adsorption) and chemical bonds between the inorganic filler and the polymer. The working characteristics of a polymeric composite depend not only on the nature of the polymer and modifying agent, on their mass ratio in the composite but also on the character of bonding between them. Because of this, investigation of the formation of the polymeric composite and the character of bonds between its components is urgent and necessary. The goal of the present work was to study the character of bonding between the components in polymeric composites PA-6 + kaolinite, prepared using the mechanochemical method with different mass ratios (m.r.). Polyamide PA-6, with the structural formula (NH-[CH 2 ] 5 -CO-)- n and layered silicate kaolinite Al 2 (Si 2 O 5 )(OH) 4 were used int he work. Mechanical activation (MA) was carried out in a ball mill of the planetary type AGO-2 with water cooling. The IR absorption spectra (IRS) were recorded with Specord-75 IR and IFS-66 instruments. The samples were prepared for recording using the standard procedure. X- 191

2 ray phase analysis (XPA) was carried out using DRON-3М and URD-63 diffractometers (Cu K α - radiation). Previously [1] we established that the MA of kaolinite in a highenergy mill causes within the first 20 s the rupture of hydrogen bonds holding the layers in packs. As a result, bonding in the tetra- and octahedral frameworks of the layer are distorted. After the activation of kaolinite for τ a >1 min, almost complete destruction of kaolinite structure is observed. The macromolecules of polyamide PA-6 are bound with each other through hydrogen bonds. The degree of crystallinity of the polymer is 40-70%. Hydrogen of the amide group is able to get substituted by alkyl and other radicals. The IRS of PA-6 (Fig. 1) contains characteristic bands of stretching and bending vibrations of the amide group and СН 2 groups [2] (Table). Fig. 1. PA-6: curve 1 before, curve 2- after MA 30c 192

3 Table Frequencies of the characteristic bands of polyamide PA - 6 δ СН2 [2],, cm -1 δ NH ν C=O CH 2 νas νs δ NH ν NH Initial PA PA-6 + Kaolinite 1410 a = 4 min Note: δ bending vibration; ν stretching vibration; - overtone The diffraction patterns of the polymer (Fig. 2) contain two clear reflections: d 1 = 4,44 (I/I s = 100) and d 2 = 3,71(I/I s = 100). The IRS and diffraction patterns of PA-6 before and after MA for τ a <1 min are almost identical (Fig 1, 2). Fig. 2. XPA PA-6: - curve 1 before, 2- after MA 30c It is known [3] that acid active centres and a smaller amount of basic ones are formed on kaolinite surface during its MA. 193

4 It was also established in [4] that the basic centres of silicate interact with acid centres on the surface of acids during the joint mechanical activation. A solid-phase mechanochemical reaction occurs; it is neutralization of hydroxo groups of kaolinite by the protons of the acid. As a result, a strong chemical bond between kaolinite and the anions of organic acid is formed. The IRS of reaction product corresponds to the IRS of the salt of organic acid. Water is also formed during the mechanochemical neutralization reaction; the characteristic bands of water are observed in the IRS of the product [4]. Taking into account these considerations, as well as the ability of hydrogen atoms in the amide groups of the polymer to get substituted by various radicals, we may assume the possibility of the mechanochemical neutralization during the joint MA of PA-6 with kaolinite. Indeed, similarly to the case of pure kaolinite [1], the IRS of the mixture polyamide + kaolinite (m.r. = 3 : 7) after MA for МА τ a =4 min (Fig 3, curve 2) exhibits a decrease in the intensity of stretching and bending vibrations of bonds: ν, δ (Al)-OH; ν, δ Si-O-(Al), Si-O-Al corresponding to the regions cm -1, cm -1, cm -1 and with the maximum at 545 cm -1. Fig. 3. IRS (3.0g PA g kaolinite): curve 1 before, curve 2 - after MA 4 min; (9.0g PA g kaolinite): curve 3 before, curve 4- after MA 4 min 194

5 The bands of antisymmetric ν as and symmetric ν s Si-O-Si stretching vibrations of the tetrahedrons of the silicon-oxygen framework, in the region cm -1 and with the maximum at 685 cm -1 disappear almost completely. Similarly to the case of MA of pure kaolinite, we observe changes of the parameters of vibrational bands ν, δ Si-O - bonds, cm -1 and with the maximal at 465 and 425 cm -1 [5] (Fig. 3, curve 2, 4). At the same time, the intensity of ν and δ (NH) bands decreases, their maxima shift. No substantial changes of the parameters of ν (C=O), ν as (CH 2 ) and ν s (CH 2 ) band are observed (Table). We suppose that the obtained results provide evidence of disordering of kaolinite structure as a result of MA of kaolinite in mixture with polyamide, due to the rupture of (Al)-OH bonds and consequent disturbance of bonds in octa- and tetrahedral frameworks of the layer. The surface active centres are formed, too. The active centres of the basic character interact with the protons of amide groups of PA-6. As a result, water and the polymeric composite are formed. The polymer and kaolinite are chemical bound with each other in this composite. So, MA of kaolinite with polyamide involves the mechanochemical neutralization similar tot he reaction of kaolinite with organic acid. The formation of water in the course of neutralization is confirmed by increased absorption within the range cm -1 ; as a consequence, the ν(-nh-) band of the amide group becomes asymmetric. The δ ОН (Н 2 О) band is in the region of δ (-NH-), cm -1 (Fig. 3). The major reflections of kaolinite are conserved in the diffraction patterns of the polymeric composite; only their intensity decreases: d 1 = 7,17 (I/I s = 100), d 2 = 3.57 (I/I s = 80) and d 3 = 3.37 (I/I s = 35). The reflections of polyamide is superimposed on the series of kaolinite reflections in the region d = , so one cannot consider any changes of the parameters of polyamide reflections. The XPA data allow us to suppose that the structure of initial kaolinite is conserved in the polymeric composite. It should be noted that the distortion of kaolinite structure during its MA in mixture with polyamide is observed in the IRS for τ a > 1 min. In the case of the activation of pure kaolinite this occurs for τ a =10 s, that is, the polymer slows down the destruction of silicate structure. With an increase in the content of polyamide in the mixture, for example for m.r. = 1 : 1, the changes of the bands related to the mixture components in the IRS and the changes of reflections in the diffraction 195

6 patterns after МА, with τ a =4 min, are similar to the changes for the mixture with m.r. = 3 : 7. However, with further increase in the polymer content in the mixture, for example for m.r. = 9 : 1, the changes of the bands related to kaolinite and polyamide in the IRS after MA with τ a =4 min becomes quite different. As one can see in Fig. 3, curve 4, the bands that do not disappear after activation are those corresponding to ν as and ν s vibrations of Si-O-Si bonds of the tetrahedrons of the silicon-oxygen framework, the region cm -1 and the band with the maximum at 685 cm -1. Only a decrease in the intensities and broadening of all the kaolinite bands occur. Neither shift of polymer bands nor the appearance of new bands are observed. In this case, that is, for the m.r. polyamide : kaolinite 4 : 1, gradual amorphization of kaolinite is likely to take place. However, in the presence of the polymer, the destruction of silicate structure proceeds not so actively. The IRS of kaolinite in mixture with PA-6 with m.r. = 4 : 1 after MA for 4 min practically corresponds to the IRS of pure kaolinite mechanically activated for 30 s < τ a < 1 min. The diffraction patterns of such a sample (Fig. 4) contain very weak but Fig. 4. XPA (3.0g PA g kaolinite): curve 1 - before, curve 2 - after MA 4 min; (9.0g PA g kaolinite): curve 3 - before, curve 4 - after MA 4 min 196

7 clear reflections from the basal planes of kaolinite (001), d 1 = 7.17 и (002) d 2 = The reflections of polyamide broaden and run into one reflection with two maxima d 1 = 4.4 and d 2 = 3.7, which is the evidence of definite distortions of the polymer structure. So, the performed studies of MA of polyamide PA-6 kaolinite mixtures with different mass ratios of the components showed that the character of bonding between them in the composites formed during the joint MA depends on their mass ratio. For m.r. polyamide : kaolinite 1 : 1, similarly to the case of MA of kaolinite with organic acids, mechanochemical interaction occurs between the components of the mixture; during the interaction, the basic centres of kaolinite interact with acidic centres of the polymer. This means that the solid-phase neutralization proceeds with the formation of a chemical bond between between kaolinite and polymer. For m.r. polyamide : kaolinite > 1: 1, we suppose that amorphization of kaolinite occurs but no so actively than amorphization of pure kaolinite. The polymer somewhat slows down this process. Without the polymer, activation of kaolinite for τ a >1 min leads to the formation of practically amorphous product. The IRS of kaolinite in mixture with PA-6 after MA for 4 min practicallyl completely corresponds to the IRS of pure kaolinite activated mechanically for 30 s < τ a < 1 min. In the case of mixtures with the m.r. polyamide : kaolinite > 1 : 1, we suppose that the number of basic centres formed during MA is insufficient for mechanochemical neutralization to proceed. Acknowledgment The work is carried out under the Integration Project of SB RAS No. 19 and BRFFI No.X12CO-009. References 1. Grigorieva T.F., Vorsina I.A., Barinova A.P., Lyakhov N.Z. Initial stages of the mechanochemical activation of kaolinite and talc. // Zh. Neorg. Khim., V. 32, No. 1, p Socrates G. Infrared Characteristic Group Frequences. New York, 1980., 226p. 3. Ikekawa A., Hayakawa S. Mechanochemistry of organic optical isomers // Siberian chemical journal P

8 4. Grigorieva T.F., Vorsina I.A., Barinova A.P., Boldyrev V.V. Mechanochemical synthesis of dispersed layered composites based on kaolinite and a number of organic and inorganic acids. Investigation by means of IR spectroscopy // Neorg. Materialy, 1996, V. 32, No. 2, p Plyusnina I.I. Infrared spectra of minerals. Moscow, Publishing House of MSU, 1977, - 175p. 198

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