Preparation And Characterization Of Polylactic Acid/ Polycaprolactone/ Modified Clay Composites

In this study, synthesis and characterisation of fatty hydroxamic acid (FHA) from palm olein with hydroxylamine using reflux method. FTIR spectrum, 1H NMR and elemental analysis tests conducted on FHA reveal that FHA was successfully produced from palm olein,. The conversion percentage of palm olein to FHA increases (81%) when the optimum reaction time to be 10 hours and a molar ratio of (hydroxylamine to palm olein) 7:1. FHA was used as one of the organic compounds to modify natural clay (Na-MMT). The clay modification was carried out by stirring the clay particles in an aqueous solution of the FHA or octadecylammonium (ODA) by which the clay layer distance increases from 12.2 Å to 31.02 Å and 29.49 Å, respectively. The modified clays were then used in the preparation of polylactic acid/polycaprolactone (PLA/PCL) composites. The optimum clay contents that yielded maximum tensile strength were 2% and 3% for PLA/PCL-ODA-MMT and PLA/PCL-FHA-MMT, respectively. The intercalation of the modifier in the clay layer was characterized by X-ray diffraction (XRD), thermogravimetric analysis (TGA) and Fourier Transform Infrared (FTIR). Elemental analysis (CHN) was used to estimate the amount of FHAs and ODA in the clay. In the first part of the preparation, the composites were synthesized by melt blending of the modified clay and PLA/PCL by a two-roll-mill internal mixer blending at a temperature setting of 185°C, rotor speed of 50 rpm and the mixing time of 12 minutes. Mechanical properties of the produced composites were then characterized by an lnstron universal testing machine. The composites were also synthesized by using solution casting in the second part of the study. In this process, Chloroform was chosen to dissolve PLA and PCL under magnetic stirrer for 1 h. The required amount of the modified clay was added to the mixture, the composites were poured into Petri dish and left to dry. The results indicate that the presence of the modified clay has dramatically improved the properties. Both of PLA/PCL-ODA-MMT and PLA/PCL-FHA-MMT composites prepared by melt blending have high tensile strength 38.91 MPa and 39.31 MPa compared to those of solution casting 31.43 MPa and 32.84 MPa for PLA/PCL-ODA-MMT and PLA/PCL-FHA-MMT, respectively. These composites were further characterized by XRD, FTIR, TGA and scanning electron microscopy (SEM).It was found that similar results of FTIR and TGA were obtained when solution casting and melt blending processes were used to produce PLA/PCL, PLA/PCLODA- MMT and PLA/PCL-FHA-MMT. Thermal stability of these composites was improved to 349.26 °C and 354.62 °C for PLA/PCL-ODA-MMT and PLA/PCLFHA- MMT, respectively, compared with the blend of polymers 342.15 °C. While the values of basal spacing in melt blending were higher 34.61 Å and 36.15 Å compare with those of solution casting 31.15 Å and 33.18 Å for PLA/PCL-ODA-MMT and PLA/PCL-FHA-MMT, respectively

Modification of Montmorillonite by new surfactants.

The sodium Montmorillonite is not susceptible to polymer due to its organophobic character and has low basal spacing. This study reports on the effect of three new organic cations including Triethyl Amine (TEA), Tripropyl Amine (TPA) and Trioctyl Amine (TOA) on the basal spacing of the clay as indictors to the sociability of the clay to the incorporation of polymers. The Fourier Transform Infrared spectroscopy (FTIR) was used to evaluate the incorporation of the three organic cations in the clay. The X-ray diffraction technique was utilized to indicate the basal spacing of the treated clay as a measure of the susceptibility of new organoclays. The FTIR, XRD and CHNS elemental analysis results shown that the three new organic cations acrylonitrile/montmorillonite were successfully incorporated in the Montmorollite clay. X-ray diffraction indicates that the basal spacings in acrylonitrile/montmorillonite of the treated clay with TEA, TPA and TOA individually increased by 14.2, 15.1 and 19.5Å, respectively. FTIR spectra illustrate that amine compounds were successfully intercalated into the clay layers

Chemical synthesis and characterization of N-hydroxy-N-methyl fattyamide from palm oil.

In this study, N-hydroxy-N-methyl fattyamide (HMFA) has been synthesized by refluxing of palm oil and N, methyl hydroxylamine. The products were characterized using the complex formation test of hydroxamic acid group with copper(Π), various technique methods including nuclear magnetic resonance ('H NMR) spectroscopy, Fourier transform infrared (FTIR) spectroscopy and elemental analysis. Parameters that may affect the conversion of palm oil to HMFA including the effect of reaction time, effect of organic solvent and effect of, M, methyl hydroxylamine /oil molar ratio were also investigated in this study. Results of characterization indicate that HMFA was successfully produced from palm oil. The conversion percentage of palm oil into N-hydroxy-N-methyl Fattyamide was around 79. Results also showed that hexane is the best organic solvent to produce the HMFA. The optimum reaction time to achieve the maximum conversion percentage of the palm oil into HMFA was found to be 16 hours, and the optimum molar ration of M, methyl hydroxylamine/oil was found to be 6.5:1.0

Synthesis and characterization of fatty hydroxamic acids from triacylglycerides

In this study, fatty haydroxamic acids (FHAs), which have biological activities as antibiotics and antifungal, have been synthesized via refluxing of triacylglycrides, palm olein, palm stearin or corn oil with hydroxylamine hydrochloride. The products were characterized using the complex formation test of hydroxamic acid group with zinc(I), copper(II) and iron(III), various technique methods including nuclear magnetic resonance ((1)H NMR) spectroscopy, Fourier transform infrared (FTIR) spectroscopy and elemental analysis. Parameters that may affect the conversion of oils to FHAs including the effect of reaction time, effect of organic solvent and effect of hydro/oil molar issue were also investigated in this study. Results of characterization indicate that FHAs were successfully produced from triacylglycrides. The conversion percentages of palm stearin, palm olein and corn oil into their fatty hydroxamic acids are 82, 81 and 78, respectively. Results also showed that hexane is the best organic solvent to produce the FHAs from the three oils used in this study. The optimum reaction time to achieve the maximum conversion percentage of the oils to FHAs was found to be 10 hours for all the three oils, while the optimum molar ration of hydro/to oil was found to be 7:1 for all the different three oils

Modification of montmorillonite by Difattyacyl thiourea using cation exchange process.

Cation exchange process was used to modify for montmorillonite (Na-MMT) by difatty acyl thiourea (DFAT). Basal spacing functional groups identification and thermal stability of this organomontmorillonite (OMMT) were characterized using X-ray Diffraction (XRD), Fourier transform infrared (FTIR) spectroscopy arid thermogravimetric analysis (TGA) respectively. Elemental analysis was also used to know the composition of OMMT.The (XRD) results showed that the basal spacing of the treated clay with DFAT increased from 1.23 nm to 3.05 nm. The highest d-spacing was observed at 2.00 CEC. FTIR spectra illustrate that DFAT compound was successfully intercalated into the clay layers. Thermogravimetric analysis shows that the thermal decomposition of organoclay occurs with higher temperature than pure DFAT

Preparation and characterization of polylactic acid/polycaprolactone clay nanocomposites

Biopolymer nanocomposites, which have attracted much attention due to their biodegradability and biocompatibility, have been prepared by melt blending polylactic acid (PLA)/polycaprolactone (PCL) and two types of organoclay (OMMT) include octadecylamine-montmorillonite (ODA-MMT) and fatty hydroxamic acid- montmorillonite (FHA-MMT). Materials were characterized using X-ray Diffraction (XRD), Fourier transform infrared (FTIR) spectroscopy, thermogravimetric analysis (TGA), elemental analysis and scanning electron microscopy (SEM). Mechanical properties were also investigated for these nanocomposites. The nanocomposites showed increasing mechanical properties and thermal stability. XRD results indicated that the materials formed intercalated nanocomposites. SEM morphology showed that increasing content of OMMT reduces the domain size of phase separated particles. Additionally, a solution casting process has been used to prepare these nanocomposites and characterized to compare these results with above process. These nanocomposites offer potential for diversification and application of biopolymer due to their good properties such as improved thermal and mechanical properties

Chemical synthesis and characterization of palm oil-based difatty acyl thiourea

Difatty acyl thiourea (DFAT), which has biological activities as antibiotics and antifungal, has been synthesized from palm oil and thiourea using sodium ethoxide as catalyst. Ethyl fatty ester (EFE) and glycerol were produced as by-products. The synthesis was carried out by reflux palm oil with thiourea in ethanol. In this process, palm oil converted to about 81% pure DFAT after 11 hour and molar ratio of thiourea to palm oil was 6.0: 1 at 78 degrees C. Elemental analysis, Fourier transform iInfrared (FTIR) spectroscopy and (1)H nuclear magnetic resonance (NMR) technique were used to characterize both DFAT and EFE

Synthesis of palm oil-based fatty methylhydrazide

Fatty methylydrazides (FMHs) have been successfully synthesized from palm oil. Glycerol was produced as a by-product. The synthesis was carried out by reflux palm oil with methylhydrazine in hexane. FMHs have been characterized using elemental analysis, Fourier transform infrared spectroscopy and 1H nuclear magnetic resonance technique. The results showed that a 6:1 molar ratio of palm oil to methylhydrazine, a round 78 % maximum conversion of palm oil into FMHs and a 10 h reaction time are the optimum reaction conditions

Spectrophotometric Determination of Cobalt(II) and Lead(II) Using (1,5-Dimethyl-2-Phenyl-4-((2,3,4-Trihydroxy Phenyl) Diazenyl)-1H-Pyrazol-3(2H)-One) as Organic Reagent: Using It as Antimicrobial and Antioxidants

The azo organic reagent (1,5-dimethyl-2-phenyl-4-((2,3,4-trihydroxy phenyl) diazenyl)-1H-pyrazol-3(2H)-one) (DPTPD) was prepared and used for the spectrophotometric determination of cobalt(Ⅱ) and Lead(Ⅱ), by the selective and surfactant-sensitized method based on the ternary complexes formation of Co(Ⅱ) and Pb(Ⅱ). The reagent had absorption maximum at 381 nm, and reacted with Co2+ to form a purple reddish complex with λmax = 430 nm at pH = 7.5, while it formed a red complex with Pb2+ of λmax = 417 nm at pH= 6. Beer's law for the determination over the range of 1 - 25 ppm and 1 - 33 ppm for Co(Ⅱ) and Pb(Ⅱ), respectively. The molar absorptivity (Є) and Sandell's sensitivity values of Co(Ⅱ) and Pb(Ⅱ) complexes were found to be 1.02 × 104, 3.3 ×104 mol-1 cm-1, and 0.0725, 0.0269 μg cm-2 at 430, 417 nm, respectively. The stability constant was found to be 1.1 × 108 L mol-1 and 2.3 × 108 L mol-1 for Co(Ⅱ) and Pb(Ⅱ), respectively. Detection limit relative standard deviation, relative error and recovery were predestined for 15 ppm standard solution of Co(Ⅱ) and Pb(Ⅱ) complexes, respectively. The important interferences with most ions like Cr+3, Mn2+, Fe3+, Zn2+, Hg2+, Mo+2, Pt2+ and Cd+2 were studied using the appropriate masking agents. The method was applied for the determination of Co(Ⅱ) in filling sample; the result obtained was incompatible with that by the flame atomic absorption spectrometry method. The organic reagent (DPTPD) was diagnosed as an anti-bacterial and an antioxidant