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Composite materials based on wastes of flat glass processingA.V. Gorokhovskya,*, J.I. Escalante-Garciaa, G.Yu. Gashnikovab,L.P. Nikulinab, S.E. ArtemenkobaDepartment of Engineering Ceramics, CINVESTAV Unidad Saltillo, Carr. Saltillo-Monterrey km13, AP 663, Saltillo, CP25000 Coahuila, MexicobDepartment of Chemical Technology, Technological Institute of Saratov State Technical University, Pl. Svobody 17, Engels 413100,Russian FederationAccepted 3 November 2004Available online 25 December 2004AbstractGlass mirrors scrap and poly (vinyl) butiral waste (PVB) obtained from flat glass processing plants were investigated as raw mate-rials to produce composites. The emphasis was on studying the influence of milled glass mirror waste contents on properties of com-posites produced with PVB. The characterization involved: elongation under rupture, water absorption, tensile strength and elasticmodulus tests. The results showed that the composite containing 10 wt% of filler powder had the best properties among the com-positions studied. The influence of the time of exposure in humid atmosphere on the composite properties was investigated. It wasfound that the admixture of PVB iso-propanol solution to the scrap of glass mirrors during milling provided stabilization of theproperties of the composites produced.? 2004 Elsevier Ltd. All rights reserved.1. IntroductionThe use of industrial wastes to produce compositematerials is one of the current problems of industry; thisprovides a means to decrease environmental contamina-tion. Flat glass processing involves the generation ofwastes, like scrap of glass mirrors as well as strips ofpoly (vinyl) butiral film (PVB), from the manufactureof automobile windscreens (Garner, 1996) and safetyarchitectural glass (Lievens, 1995). Clean PVB wastecan be recycled on the basis of well-known technologicalprocesses; however, about 520% of this waste containscontamination, which precludes its recycling. Moreover,in developing countries there is little efforts or possibilityfor the recycling of this type of waste. Additionally,waste from glass mirror production (scrap or mirrorsnot meeting standards) has to be disposed because ofthe lack of technological processes oriented towards itsutilization (Foss, 1997). The amounts of such wastecan reach 1015% of commercial production in differentplants.Taking into account that the plants oriented to flatglass processing, usually produce both types of theaforementioned wastes or are located close by, it wasof interest to investigate the possibility of producingglass-polymer composites based on the complex utiliza-tion of such wastes that are inapplicable for recycling.The production of composites based on PVB wastes isespecially attractive in developing countries, where theircollection as well as transportation into the plants spe-cialized in PVB recycling is economically unprofitable.The high adhesion properties of the PBV to the soda-lime-silicate glass surface (Garner, 1996; Gopal et al.,1997) make the composite, based on PVB waste andmilled glass, a promising material useful for differentapplications. The best scheme is that for plants produc-ing both wastes, for example in the manufacturing ofdifferent profiled rods, characterized with high mechan-ical properties stable in conditions of humid atmosphereand temperature changes. However, the presence of0956-053X/$ - see front matter ? 2004 Elsevier Ltd. All rights reserved.doi:10.1016/j.wasman.2004.11.007*Corresponding author. Tel.: +52 844 438 9600; fax: +52 844 4389610.E-mail address: alexandesaltillo.cinvestav.mx (A.V. Gorokhovsky)./locate/wasmanWaste Management 25 (2005) 733736metal particles on the glass surface of milled glass mirrorscrap as well as the use of PVB waste could negativelyinfluence the exploitation properties and thus must beinvestigated.2. MethodologyWastes of Saratovsteklo Inc. (Russia) were used forthe experiments. The glass used to produce mirrorshad the following chemical composition (wt%): 73.1SiO2; 1.1 Al2O3; 8.6 CaO; 3.6 MgO; 13.6 Na2O. Themirror coating was formed by vacuum sputtering ofstainless steel. PVB waste was obtained from the poly-mer film B-17 produced by Monsanto.In Series 1 of the experiments, the filler was producedby dry ball milling of glass mirror scrap, in jars of alu-mina with balls of alumina, to reach a surface area of4000 100 cm2/g (controlled by LHM-8MD Russianequipment). The ground glass was then added to PVBwaste molten at 115 ?C, the latter was previously ad-mixed with 0.5 wt% of poly (ethyl) silane (PES-5, Volzh-skii, Russia) to promote the blending of componentsand increase homogeneity of composition. The ratio ofglass powder and molten PVB was varied in the rangeof 130 wt%. The mixtures obtained were used to pro-duce films by quenching, as well as rods by extrusion.It is well known that water vapor adsorption onto thesurface of soda-lime-silicate glasses influences theiradhesion to polymers (Kawaguchi and Pearson, 2003;Gu et al., 2000; Radhakrishnan and Unde, 1999). Ithas been shown (Soshko et al., 1989) that the admixturesof some organic polymers into the glass scrap duringmilling promoted the modification of the glass surfaceby the products of their thermo-mechanical destruction(Dhaliwal and Hay, 2000). For this reason, an addi-tional batch of Series 2 was prepared using compositesmade from the resulting material obtained after jointball milling of glass mirrors scrap admixed with PVBwaste dissolved at room temperature in iso-propanol(15% solution); the weight ratio of glass scrap andPVBalcohol solution was 0.05. It was expected thatthe glass powder thus obtained would have enhancedhydrophobic properties and improved adhesion toPVB. To characterize such surface modification, the ob-tained fillers were investigated by TGA/DTGA (PerkinElmer/Seiko Instruments, Japan) for the following typesof glass powder: (a) fresh dry milled, (b) dry milledand exposed to a humid atmosphere for a month, (c)milled with PVB alcohol solution and exposed to a hu-mid atmosphere for a month.The average tensile mechanical strength of the com-posite articles was measured by testing 18 specimens ofeach system using the ER-5046-5 Russian equipment.The Young modulus was measured following theE1875-00e1 ASTM standard using UZIS equipment(LETI, Russia).Taking into account the influence of environmentalfactors on the properties of materials produced, speci-mens of the two composites, prepared with the fillersof Series 1 and 2, were exposed for three months at 25?C in air (40% humidity); and the same mechanical tests,as previously described, were repeated to determine therange of variation in the main characteristics duringexploitation.3. Results and discussionThe main characteristics of composites with differentcontents of glass powder for Series 1, measured immedi-ately after their production, are presented in Table 1.The introduction of 110 wt% of glass powder into thematrix of PVB waste increased the mechanical strengthof the composite (by 1.6 times) and decreased its relativeelongation under the rupture (by 1.3 times). Further in-crease of glass powder contents decreased the exploita-tion properties.The influence of exposure to a humid atmosphere onthe exploitation properties of the composite, made fromSeries 1 with 10 wt% of glass powder (highest mechani-cal properties), is presented in Figs. 1 and 2. All thetested properties decreased only during the first twomonths of exposure and then stabilized. The same effectwas displayed by the results presented in Table 2, show-ing the properties of composites obtained with thefresh and old (exposed in air for a month) glasspowder. Such reduction in the exploitation propertiesobserved, in agreement with published results (Kellerand Mortelmans, 1999), can be attributed to the pro-cesses taking place on the surface of glass filler beforethe production of composites: adsorption (condensa-tion) of water vapor from the atmosphere, leaching ofsodium ions, and crystallization of Na2CO3and NaH-Table 1The properties of composites obtained by extrusion of samples made of separate dry milling of glassPropertiesContents of glass powder (wt%)01351015202530Young module (MPa)Tensile strength (MPa)7.97.05.4Relative elongation under rupture (%)318345288271237328295286142734A.V. Gorokhovsky et al. / Waste Management 25 (2005) 733736CO3as a result of the sodium ions interaction with dis-solved CO2. The presence of these crystals and adsorbedwater onto the surface of glass filler decreased adhesionwith PVB. At the same time, modification of the glasspowder surface during the milling of glass mirrors scrapwith PVB alcohol solution (Series 2) can increase thehydrophobic properties of the glass powder and stabilizethe structure of the composite. A comparison of proper-ties for composites from Series 1 and 2 is shown in Figs.1 and 2; an improvement and increased stability of prop-erties of the composite produced in Series 2 can benoted.The obtained data of DTGA (Fig. 3) indicates thatthe old glass filler, in comparison with the fresh fil-ler obtained by dry ball milling, is characterized by theadditional intensive peak at 350420 ?C, related to thedesorption of chemically adsorbed water (Hench, 1978;Gorokhovsky, 1988). At the same time, this peak is ab-sent for the filler milled jointly with the PVB solution iniso-propanol; moreover, the quantity of condensedwater is much less. The additional peaks in the thermo-gram of this filler are related to the melting and thermaldecomposition of PVB (Dhaliwal and Hay, 2000). Thus,it is possible to propose that the effect of stabilization ofthe mechanical properties, obtained for the compositeproduced on the base of glass powder with modified sur-face (Series 2), was achieved due to a decreased adsorp-tion of water vapor.The composite rods of different profiles, produced byextrusion of the batch based on the PVB wastes andglassy filler (10 wt%), obtained by joint ball milling ofglass mirrors scrap with PVB waste, dissolved at roomtemperature in iso-propanol (15% solution), were ap-plied in Salavatsteklo Co. (Salavat, Russia) to manufac-ture the double glazing blocks, as well as bases for thestorage and transportation of glass sheets of high thick-ness (weight).4. ConclusionsCompositematerialswith attractive exploitationproperties can be produced on the basis of typical wastesof flat glass processing: poly (vinyl) butiral ribbons andglass mirror scrap. The contents about of 10 wt% ofglass powder results in composites with high and stablemechanical properties. The introduction of PVB alco-hol solution resulted in the stabilization of propertiesof the composites in the case of exposure to humidatmospheres.Table 2Properties of composites, made from Series 1 and with 10 wt% of glasspowder, produced immediately after the milling and after one monthof glass powder storage in airPropertyType of glass powder appliedOne monthafter millingFresh powderYoung modulus (MPa)3.84.3Tensile strength (MPa)8.211.2Relative elongation beforethe rupture (%)281237010203040506050100150200250300350400450500Temperature,CDTG, microg/min123456112ABCFig. 3. DTGA data obtained for different types of filler: A freshdry milled, B old dry milled, C old milled with PVB alcoholsolution. 1, 2 desorption of condensed water, 3 desorption ofchemically adsorbed water, 4 melting of PVB; 5, 6 thermaldecomposition of PVB and its derivatives formed by milling.3530Characteristics25Relative elongation under a rupture 2015Tensile strength105Youngmodulus0050100150Exposure, daysFig. 1. Influence of exposure to humid atmosphere on properties ofcomposites produced with powder obtained from Series 1 (continuouslines) and Series 2 (dashed lines): relative elongation under a rupture(%10?1), tensile strength (MPa), Young modulus (MPa).32.5Sweling, wt.%21.510.50050100150Exposure, daysFig. 2. Influence of exposure in humid atmosphere (dashed lines) andwater (continuous lines) on weight of composite rods produced fromSeries 1 (d) and Series 2 (s).A.V. Gorokhovsky et al. / Waste Management 25 (2005) 733736735ReferencesDhaliwal, A.K., Hay, J.N., 2000. The characterization of polyvinylbutyral by thermal analysis. Thermochimica Acta 391 (12), 245255.Foss, R.V., 1997. Recycling of architectural and automotive glass inEurope. With emphasis on Germany. In: Proc. of 6th InternationalConference on Architectural and Automotive Glass, Tampere, pp.4448.Garner, J., 1996. Automotive glass windscreen design and shaping.Glass Technology 37 (5), 151152.Gopal, S., Ramchandran, R., Agnihotry, R.S.A., 1997. Polyvinylbutyral based solid polymeric electrolytes: preliminary studies.Solar Energy Materials