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A Study of Poly (3-Hydroxybutyrate- Co-3-Hydroxyvalerate)

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A Study of Poly (3-Hydroxybutyrate- Co-3-Hydroxyvalerate) JOURNAL OF COMPOSITE Article MATERIALS Journal of Composite Materials 2018, Vol. 52(23) 3199–3207 ! The Author(s) 2018 A study of poly (3-hydroxybutyrate- Article reuse guidelines: sagepub.com/journals-permissions co-3-hydroxyvalerate) biofilms’ DOI: 10.1177/0021998318763246 journals.sagepub.com/home/jcm thermal and biodegradable properties reinforced with halloysite nanotubes SM Kamrul Hasan1, S Zainuddin1, J Tanthongsack1, MV Hosur1 and L Allen2 Abstract The aim of this study is to investigate and optimize the performance of a promising biopolymer, poly (3-hydroxybutyrate- co-3-hydroxyvalerate) which can potentially replace non-biodegradable synthetic polymers derived from toxic petroleum products. Poly (3-hydroxybutyrate-co-3-hydroxyvalerate) biofilms were prepared using solvent casting method, and its thermal properties were determined using thermogravimetric and differential scanning calorimetry techniques. Also, the durability and biodegradability of these films were studied by keeping the samples in water and Alabama soil conditions for various lengths of time. Our results showed that the thermal and moisture resistance of poly (3-hydroxybutyrate- co-3-hydroxyvalerate) biopolymer can be enhanced significantly with the addition of low halloysite nanotubes concen- trations. Also, the biodegradation process of the poly (3-hydroxybutyrate-co-3-hydroxyvalerate) films was faster with the addition of halloysite nanotubes attributed to the accelerated microbial microorganism reaction in the soil. This study led to cognize that the PHBV biopolymers added with halloysite nanotubes can be successfully used for various bio- medical, industrial and structural applications, and then decompose at a desired faster rate afterward. Keywords Biopolymer, halloysite nanotubes, thermal properties, durability, biodegradation Introduction durability and biodegradability information has limited their use in many potential possible applications in large Environmental concern, waste disposal by incineration, volume.4,5 depletion of nonrenewable resources, and scarcity of pet- In recent years, natural nanoparticles such as mont- roleum sources and energy requirements have raised morillonite nanoclay and halloysite nanotubes (HNTs) alarming environmental concerns worldwide for the con- have enhanced mechanical and thermal properties of tinuous applications of synthetic plastic-/polymer-based biopolymers, while maintaining the composites bio- products. In contrast, the growing interest in biomater- nature.4,6,7 Nanoparticles provide a large surface area ials extracted from natural resources provided an for rapid phase interaction as well as more matrix inter- excellent alternative to synthetic materials because of facial adhesion. Conventional plastic engineering also its environmentally friendly and 100% biodegradable elucidated the attractive properties of nanofiller-infused nature.1 One such biomaterial from a polyhydroxy polymeric composites such as flame retardancy, surface alkonites (PHAs) family is poly(3-hydroxybutyrate- co-3-hydroxyvalerate) (PHBV) which is currently used 1Department of Materials Science and Engineering, Tuskegee University, or considered for film packaging, water filtration, and USA biomedical applications.2,3 The mechanical properties of 2Department of Chemistry, Talladega College, USA PHBV polymer are almost similar to some polyolefins Corresponding author: like polypropylene, which makes it an excellent alterna- Shaik Zainuddin, Department of Materials Science and Engineering, tive to many synthetic-based polymers. However, poor Tuskegee University, Alabama 36088, USA. thermal stability, low crystallization rate, and lack of Email: [email protected] 3200 Journal of Composite Materials 52(23) advantage, material transparency, heat resistance, gas melt processible thermoplastic polymer (pallet form) permeability reduction as well as barrier properties.8,9 made from the biological fermentation of renewable Among these nanoparticles, HNTs, a member of carbohydrate feedstocks. An unmodified tubular- Kaolin group has a high potential to be used as shaped HNTs were obtained by Natural Nano, reinforcement materials. HNTs have tubelike structure Pittsford NY, USA, and chloroform (99.5%) was similar to carbon nanotubes (CNTs) with a diameter purchased from Sigma Aldrich, Saint Louis, USA. typically smaller than 100 nm and length in between 10 500 nm to 1.2 microns. The external surface of Processing of thin films HNTs is mainly composed of the siloxane (Si–O–Si) groups, whereas the internal surface consists of a gibbs- Neat films. At first, 10 gm of PHBV was dissolved in ite like an array of aluminol (Al-OH) groups.7 HNTs 120 ml chloroform using a continuous magnetic stirring contain two types of hydroxyl groups, which are situ- for 24 h. The resulting solution was then vacuum mixed ated on the surface of the nanotubes and in between the using 100 kPa pressure for 15 min at a speed rate of layers which are called inner and outer hydroxyl 1500 r/min to remove the entrapped air bubbles. groups, respectively. The presence of hydroxyl groups Finally, the films were prepared by spreading the mixture that form hydrogen bonding with the polymer matrix on a glass plate and curing at room temperature for 24 h. favors good dispersion.11,12 Furthermore, high aspect The films were cured at room temperature for longer to ratio and large surface area of HNTs ensure the good ensure the complete evaporation of chloroform. interaction between nanofiller and the polymer matrix, respectively.6,8 Several researchers have incorporated PHBV/HNTs films. At first, 3–15 wt.% HNTs was dis- HNTs as a filler in various polymer matrices and persed in chloroform using ultrasonication process for reported significant enhancement in the tensile strength 1 h at an amplitude of 45% with 5/5 s on/off pulse rate. and stiffness, thermal stability, fire retardancy and Ten grams of PHBV polymer was then dissolved into the moisture resistance.7,13,14 A few researchers have HNT/chloroform solution and the films were prepared also investigated the durability and biodegradability following the exact procedure used for the neat films. of various polymer/clay nanocomposites such as poly (3-caprolactone)/clay, polylactide/clay, polyvinyl alco- hol/clay, and poly (3-hydroxybutyrate)/clay compos- Experimental procedure 15,16 ites. In addition to enhancement in durability, the Differential scanning calorimetry researchers also found that nanoclay promulgates the biodegradation of polymeric composites.16 However, to Differential scanning calorimetry (DSC) was used to the best of our knowledge, no study on the durability analyze the melting temperature and crystallization and biodegradation behavior of PHBV/HNTs films, behavior of the nanocomposites. Measurements were specifically when exposed to water and soil condition- carried out on Q1000 analyzer in a nitrogen atmos- ing, has been reported to date. Also, efforts have not phere. Ten to twelve milligrams of samples were encap- been made to optimize the concentration of HNTs and sulated into the aluminum pan and heated from À20C investigate its impact on the overall morphological and to 250C at a ramp rate of 10C/min. From DSC endo- thermal performance of these composites, including the therms, the melting temperature (Tm) and enthalpy of durability and biodegradability properties. fusion (VHm) were determined. The degree of crystal- In this study, we have processed neat and PHBV/ linity was determined using equation (1) HNTs composites by adding 0–15 wt.% HNTs and VH investigated the thermal performance using differential X ¼ m  100% ð1Þ c V 0 scanning calorimetry (DSC) and thermogravimetric fp Hm analysis (TGA). In addition, the moisture absorption À1 and biodegradable behavior of these composites were where VHm (Jg ) indicates the melting enthalpy of also studied by placing the composite films in water for polymer matrix, fp represents the polymer weight frac- 0 À1 17 315 h, and in Alabama soil for 12 weeks, respectively. tion in the sample, and VHm (146 Jg ) stands for the melting enthalpy of pure crystalline polymer matrix. Materials and processing Thermogravimetric analysis Materials Thermogravimetric analysis (TGA) was conducted by TA PHBV, a bacterial grade 100% biopolymer containing Q500 analyzer to determine the thermal decomposition of 12 mol% of valerite was purchased from Goodfellow neat and PHBV/HNTs films. Ten to twelve milligrams Corporation, Coraopolis, USA. PHBV is an easily of samples were used and the TGA, derivative Hasan et al. 3201 thermogravimetric (DTG) and residual weight percentages 4  4 cm were placed in a pit dig in Tuskegee, Alabama were recorded in a nitrogen atmosphere from 30 to 550C. soil under completely natural conditions for 2, 3, 5, 8, and 12 weeks, respectively. The samples were then Water absorption behavior taken out after each interval and washed with distilled water to remove the dirt. Finally, the samples were Water absorption behavior (WAB) of films was inves- dried at 50C for 8 h and weighed. The degree of soil tigated by submerging the 2  2 cm samples in water for degradation was calculated using equation (4) a time interval of 2–315 h. The films were taken out of the water after each interval, dried with a paper towel, W À W Percentage soil degradation ¼ 2 1  100% and the percentage of water absorption was calculated W1 using equation (2) ð4Þ Wf À Wi where W and W are the weights of the PHBV films Percentage water absorption ¼  100% ð2Þ 1 2 Wi before and after the soil degradation. where
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