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Development of Synergistic Heat Stabilizers for Pvc from Zinc Borate-Zinc Phosphate

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Development of Synergistic Heat Stabilizers for Pvc from Zinc Borate-Zinc Phosphate View metadata, citation and similar papers at core.ac.uk brought to you by CORE provided by DSpace@IZTECH Institutional Repository Chemical Engineering Communications ISSN: 0098-6445 (Print) 1563-5201 (Online) Journal homepage: http://www.tandfonline.com/loi/gcec20 DEVELOPMENT OF SYNERGISTIC HEAT STABILIZERS FOR PVC FROM ZINC BORATE-ZINC PHOSPHATE Cem Aykut Erdoğdu , Sevdiye Atakul , Devrim Balköse & Semra Ülkü To cite this article: Cem Aykut Erdoğdu , Sevdiye Atakul , Devrim Balköse & Semra Ülkü (2008) DEVELOPMENT OF SYNERGISTIC HEAT STABILIZERS FOR PVC FROM ZINC BORATE- ZINC PHOSPHATE, Chemical Engineering Communications, 196:1-2, 148-160, DOI: 10.1080/00986440802293148 To link to this article: http://dx.doi.org/10.1080/00986440802293148 Published online: 20 Oct 2008. Submit your article to this journal Article views: 537 View related articles Citing articles: 4 View citing articles Full Terms & Conditions of access and use can be found at http://www.tandfonline.com/action/journalInformation?journalCode=gcec20 Download by: [Izmir Yuksek Teknologi Enstitusu] Date: 20 November 2016, At: 23:05 Chem. Eng. Comm., 196:148–160, 2009 Copyright # Taylor & Francis Group, LLC ISSN: 0098-6445 print/1563-5201 online DOI: 10.1080/00986440802293148 Development of Synergistic Heat Stabilizers for PVC from Zinc Borate-Zinc Phosphate CEM AYKUT ERDOG˘ DU,1 SEVDIYE ATAKUL,2 DEVRIM BALKO¨ SE,2 AND SEMRA U¨ LKU¨ 2 1Pigment Sanayi A. S¸., I˙zmir, Turkey 2Department of Chemical Engineering, I˙zmir Institute of Technology, I˙zmir, Turkey The importance of flame-retardant and smoke-suppressed poly(vinyl chloride) (PVC) compositions is increasing gradually in the polymer industry since PVC releases smoke and toxic gases (hydrogen chloride, HCl) during heating at tempera- tures above 140C with the result of dehydrochlorination reaction. In this study, the synergistic effects of zinc borate (ZB)-zinc phosphate (ZP) on the thermal stability of PVC were investigated using thermal techniques. The induction and stability time values of PVC plastigels were obtained at 140 and 160C. The results revealed that PVC plastigels having only ZP and ZB retarded dehydrochlorination of PVC com- pared with the unstabilized sample. However, the plastigels with both ZB and ZP had a superior synergistic effect on char formation of PVC. Since the induction per- iods of the samples having both ZB and ZP were higher than those of the unstabi- lized samples having only ZB or only ZP, the synergistic effect was observed. Keywords Heat stabilizer; PVC; Thermal degradation; Zinc borate; Zinc phosphate Introduction It is well known that poly(vinyl chloride) (PVC) has high chlorine content, so it is an incombustible material. The construction of buildings often requires the use of fire- or flame-retardant jacketing, facing materials for heating, duct insulation, electrical insulation applications, cables, and domestic uses such as in gutters, doors, profiles, house siding, and similar applications involving plies of combustible sheet material or plies of such sheet materials laminated to various substrates such as aluminum foil and fiberglass batting. Because of its lower cost and versatility, PVC is often used to prepare such sheet materials by being blended with various additives that are designed to impart the required flame-retardant characteristics. PVC has good flame retardancy because of its high chlorine content, but it is not a safe material in fires because it releases high levels of smoke and toxic gases leading to a color change from brown and even black in the end (Pi et al., 2002; Ning and Guo, 2000; Baltaciog˘lu and Balko¨se, 1999). Additives such as compounds containing metals like antimony, zinc, copper, Address correspondence to Sevdiye Atakul, Department of Chemical Engineering, I˙zmir Institute of Technology, Gu¨lbahc¸e Ko¨yu¨, 35430 Urla, I˙zmir, Turkey. E-mail: sevdiyeatakul@ iyte.edu.tr 148 Heat Stabilizers for PVC 149 Figure 1. A representative curve for PVC Thermomat results. iron, aluminum, magnesium, and molybdenum are widely used in reducing flammability and in smoke suppression, and the most important commercial smoke suppressants are zinc and aluminum compounds (Pi et al., 2002; Ning and Guo, 2000). One of the most used flame retardants is zinc borate (XZnO Á YB2O3 Á ZH2O). Boron can be used as a flame retardant in both the condensed and vapor phases. Under flaming conditions boron and halogens form the corresponding trihalide. Since boron trihalides are effective Lewis acids, they promote cross-linking, minimiz- ing decomposition of the polymer into volatile flammable gases (Schubert, 1995, 1994). Recent studies indicated the synergistic effect of zinc borate and aluminum trihydrate on the flame retardancy and smoke suppression of PVC (Pi et al., 2002; Ning and Guo, 2000). Zinc phosphate is an anticorrosive white pigment usually produced from zinc oxide and phosphorous acid or zinc salts and phosphates. Smoke densities of smoke-retardant PVC compositions of nickel and zinc salts were evaluated accord- ing to their smoke formation during burning in a National Bureau of Standards (NBS) smoke chamber. It has been clearly stated that the compositions with NiO and ZP have reduced smoke generation (Dickens, 1976). The effects of synergistic fire-retardant additives consisting essentially of boric acid and zinc oxide or zinc phosphate were investigated by determining the limiting oxygen index (LOI) of plasticized PVC samples. In this study, LOI values were obtained in the samples where boric acid and zinc oxide or zinc phosphate were com- bined. According to the results, the LOI of the control sample was 23.7 and the high- est LOI index (29.8), which means more flame and fire retardation, was observed for the plasticized PVC having 30 pbw boric acid and 30 pbw zinc oxide (Ismat, 1977). Thermal stabilization of PVC can be determined by PVC Thermomat equip- ment. When PVC plastigels are heated in a PVC Thermomat in the presence of nitro- gen gas, the conductivity of water, through which nitrogen gas is passed, changes with respect to time. The period when the conductivity starts to increase is called the induction time, and the period when the conductivity value reaches 50 mS=cm is called the stability time. This value is the maximum acceptable level of degra- dation. Rate of dehydrochlorination can be determined by the conductivity of the solution where the evolved HCl gas is transferred (Atakul et al., 2005). A represen- tative curve for PVC Thermomat results is shown in Figure 1. 150 C. A. Erdog˘du et al. Table I. Plastisol compositions used in the experiments (values in phr) Sample no. PVC DOP Viscobyk 5025 ZB ZP 1 100 80 5 — — 2 100 80 5 — 2.5 3 100 80 5 0.5 2.0 4 100 80 5 1.0 1.5 5 100 80 5 1.25 1.25 6 100 80 5 1.5 1.0 7 100 80 5 2.0 0.5 8 100 80 5 2.5 — This study aims to investigate the synergistic effect of the combination of zinc borate (ZB) and zinc phosphate (ZP) on flame retardancy. Optimum synergistic composition of ZB and ZP in thermal stabilization of plasticized PVC is determined as well. Experimental Section Materials PVC, dioctyl phthalate (DOP), Viscobyk 5025 (BYK Chemicals, Wallingford, USA), different amounts of zinc borate (ZB) (2ZnO Á 3B2O3 Á 3.5H2O), and zinc phosphate (ZP) (Zn3 (PO4)2) were used to produce PVC plastigels. The amounts of additives used in the experiments are given in Table I. A typical emulsion-type commercial PVC resin (Petvinil P.38=74) was used for plastisol preparation. DOP was used as a plasticizer (Merck, Darmstadt, Germany), and its density is 0.98 g=mL and molecular weight is 390.54 g=mol. Viscobyk 5025 was used as a wetting agent having a density (at 20C) of 0.88 g=mL and refractive index of 1.45. ZB and ZP were supplied from Heron Chemicals and Pigment Sanayi A.S¸., respectively. Preparation of PVC Plastisol and PVC Plastigel The PVC plastisol was prepared by mixing PVC (resin), dioctyl phthalate (DOP) (plas- ticizer), and Viscobyk 5025 (suspension aid). They were stirred by a mechanical mixer (IKA Labortecnik). Thereafter different amounts of ZB and ZP were added to PVC plastisol samples and they were stirred by a glass rod. All mixtures contained 100 parts PVC,80partsDOP,5partsViscobyk5025,and2.5partsZB,ZP,ortheirmixtures.The plastisol compositions are listed in Table I. Subsequent to the mixing, the obtained PVC plastisols were poured onto gloss cardboard papers that were then passed through a film applicator at 300 mm from Sheen Instruments (Sheen 113 N), which is capable of sheet- ing them into forms of thin, self-supporting films. All plastisol films were gelled for 15 min in an air-circulating oven (EV 018) at 140 Æ 3C. Since the plasticizer diffused into the particles of PVC resin, the films were gelled and plastigel films were obtained. Morphology of Zinc Borate, Zinc Phosphate, and PVC Plastigels Zinc borate, zinc phosphate powders, and the PVC plastigel films, gelled at 140C for 15 min and heated at 160C for 90 min, were studied by scanning electron microscopy Heat Stabilizers for PVC 151 (Philips, XL-30SFG). In order to determine the morphologies of PVC plastigel films, they were cut by sharp scissors to obtain their cross-sectional area. The films were mounted vertically to observe their cross section. Color Measurement The yellowness index value, which gives an idea of the physical deterioration of the heated films when compared with the unheated ones, was measured by a fiber optic spectrophotometer (Spectrocam, Avantes) for unstabilized film and heated plastigels at 140 and 160C. Thermal Stability Test The thermal stability tests were carried out using a 763 PVC Thermomat. It is equipped with two heating blocks, each with four measuring positions. Two sets of four samples can be heated and measured at two different temperatures at each block individually or eight samples can be measured at the same temperature.
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