脂肪醇聚氧乙烯醚磷酸酯三乙醇胺盐的研制及其应用

以脂肪醇和环氧乙烷为原料,五氧化二磷为酯化剂,三乙醇胺为中和剂,合成了脂肪醇聚氧乙烯醚磷酸酯三乙醇胺盐,对其合成工艺及其复配油剂在腈纶上的应用进行了研究。结果表明,最佳合成工艺条件为:环氧乙烷与脂肪醇的摩尔比为2．0,脂肪醇聚氧乙烯醚与五氧化二磷的摩尔比为3．8,五氧化二磷投料时间1．5 h,酯化温度70℃,酯化反应时间3．0 h,三乙醇胺的加入量是脂肪醇聚氧乙烯醚磷酸酯的0．73-0．76 倍。用酯肪醇聚氧乙烯醚磷酸酯三乙醇胺盐为单体复配的油剂,其在腈纶中的应用情况与进口日本油剂相当。     

Bio-based flexible polyurethane foam synthesized from palm oil and natural rubber

As environment friendly polymers are required to reduce the green-house gas emissions and global warming, bio-based polyurethane foam (PUF) is attracting interest from the industrial sector and researchers. Bio-based polyols for PUF have been synthesized from various renewable resources, mostly plant oils. The present study explored a novel bio-based PUF produced from a mixture of bio-based polyols synthesized from palm oil and natural rubber. Palm oil-based polyol (POP) was synthesized via an epoxidation reaction of double bonds of palm oil followed by complete oxirane ring-opening. Hydroxy telechelic natural rubber (HTNR) was synthesized by oxidative degradation using periodic acid and sodium borohydride. For comparison, two diisocyanates were used: toluene-2,4-diisocyanate and polymeric methylene diphenyl diisocyanate. POP and HTNR were miscible and all PUFs showed polyhedral semi-closed cells and hardness was in the flexible foam range. One possible application of the novel PUF could be thermal insulation.     

Synthesis and characterization of palm‐based resin for UV coating

The production of UV curable acrylated polyol ester prepolymer from palm oil and its downstream products offer potential and promising materials for applications such as polymeric film preparation and coatings. In this study, palm olein polyol was reacted with acrylic acid in the presence of a catalyst and inhibitors via condensation esterification process. The reaction temperature of 80°C and the stirring rate of 400 rpm produce a homogeneous product. Based on iodine value result, the suitable amount of p‐toluene sulfonic acid monohydrate used as catalyst was 3.0% (w/w) of palm olein polyol. Different UV curable formulations have been investigated using the synthesized prepolymers with monomers and a small amount of photoinitiator. Monomers used were 1,6‐hexanediol diacrylate (HDDA) and trimethylolpropane triacrylate (TMPTA) while photoinitiator used was 1‐hydroxy cyclohexyl phenylketone (Irgacure 184). The mixtures were cured to make thin polymeric films under UV radiation with doses between 2 and 14 passes (energy per pass is 0.6 J/cm²). Coating and curing was carried out on glass for pendulum hardness and FTIR analysis. Pendulum hardness of the film prepared using monomer HDDA and the prepolymer previously synthesized using 3.0% catalyst was 24.5%. The radiation dose needed was 14 passes. The highest pendulum hardness of 49.4% was achieved using monomer TMPTA and the prepolymer synthesized using 2.0% catalyst. The radiation dose needed was 10 passes. © 2008 Wiley Periodicals, Inc. J Appl Polym Sci, 2009     

Enzymatic synthesis of palm olein-based fatty thiohydroxamic acids

Fatty thiohydroxamic acids (FTAs) have been successfully synthesized from palm olein and thiohydroxamic acid by a one-step lipase catalyzed reaction. The use of immobilized lipase (Lipozyme RMIM) as the catalyst for the preparation reaction provides an easy isolation of the enzyme from the products and other components in the reaction mixture. The FTAs were characterized using Fourier transform infrared (FTIR) spectroscopy, proton nuclear magnetic resonance ((1)H NMR) technique and elemental analysis. The highest conversion percentage (95 %) was obtained when the process was carried out for 30 hours using urea to palm oil ratio of 6.0: 1.0 at 40 °C. The method employed offers several advantages such as renewable and abundant of the raw material, simple reaction procedure, environmentally friendly process and high yield of the product.     

Green Synthesis of Gold Nanoparticles in Pomegranate Seed Oil Stabilized Using Laser Ablation

In this paper, gold nanoparticles were synthesized in pomegranate seed oil using a laser ablation. The nano fluids were characterized using UV–Vis spectroscopy, transmission electron microscopy and Fourier transform infrared spectroscopy. The nanoparticles were formed inside the pomegranate seed oil in spherical form, and the particle size ranged from 12 to 4 nm, and the gold nanoparticles were capped with COO^? of carboxylic acid groups of fatty acid in pomegranate seed oil.     

Production of fatty acid methyl esters over a limestone-derived heterogeneous catalyst in a fixed-bed reactor

Production of fatty acid methyl esters (FAME) via the transesterification of different vegetable oils and methanol with a limestone-derived heterogeneous catalyst was investigated in a fixed-bed reactor at 65 °C and ambient pressure. This heterogeneous catalyst, as a 1 or 2 mm cross-sectional diameter extrudate, was prepared via a wet mixing of thermally treated limestone with Mg and Al compounds as binders and with or without hydroxyethyl cellulose (HEC) as a plasticizer, followed by calcination at 800 °C. The physicochemical properties of the prepared catalysts were characterized by various techniques. Palm kernel oil, palm oil, palm olein oil and waste cooking oil could be used as the feedstocks but the FFA and water content must be limited. The extrudate catalyst prepared with the HEC addition exhibited an enhanced formation of FAME due to an increased porosity and basicity of the catalyst. The FAME yield was increased with the methanol/oil molar ratio. The effect of addition of methyl esters as co-solvents on the FAME production was investigated. The structural and compositional change of the catalysts spent in different reaction conditions indicated that deactivation was mainly due to a deposition of glycerol and FFA (if present). The FAME yield of 94.1 wt.% was stably achieved over 1500 min by using the present fixed-bed system.     

纳米TiO_2催化臭氧化降解水中草酸

本实验以钛酸四丁酯为前驱物,乙醇和正己烷作为晶形导向剂,通过水热法合成不同晶形的TiO2催化剂。催化剂的结构特性采用X射线衍射(XRD)来表征。催化剂的催化活性通过对水中草酸晶形催化臭氧化降解来进行评估;通过研究叔丁醇对催化剂臭氧化反应的影响,证明反应遵循羟基自由基(HO·)反应机理。     

In-situ synthesis of MCM-41 on ceramic membranes and its application in transesterification as catalyst support for p-toluenesulfonic acid

In this study, a new kind of solid acid catalyst p-toluenesulfonic acid/MCM-41/ceramic membrane was synthesized by in situ synthesis and impregnation method, which has shown its favorable catalytic activity, as verified in the transesterification and catalyst characterization. The catalyst was characterized by powder X-ray diffraction, scanning electron microscopy, transmission electron microscopy and Fourier-transform infrared spectroscopy. The transesterification of palm oil and methanol results showed that p-toluenesulfonic acid/MCM-41/ceramic membrane had the highest catalytic activity with immersing p-toluenesulfonic acid solution concentration of 0.15 mol/L. Different operation parameters of the transesterification of palm oil with methanol, such as catalyst amount, catalytic mass ratio, reaction time, reaction temperature and methanol/palm oil molar ratio were investigated. Under the optimum conditions of 4 % of fresh catalyst (catalytic mass ratio is 4.37 %), 80 min of reaction time, reaction temperature of 120 °C and methanol to palm oil molar ratio of 12:1, a relatively high fatty acid methyl ester yield of 95.6 % was obtained.     

New polyester acrylate resins from palm oil for wood coating application

The aim of this study is to investigate the potential use of palm oil and to prepare new UV (ultraviolet) radiation‐curable acrylated polyester prepolymers, which could be used in the wood coating industry. Thus, palm oil‐based acrylated polyester resins PEPP‐1 (from refined, bleached, and deodorized palm oil) and PEPP‐2 (from crude palm oil) were synthesized at the Advanced Oleochemical Technology Centre (AOTC) laboratory of Palm Oil Research Institute of Malaysia (PORIM). The performances of these resins with respect to their curing rate and physical‐mechanical properties of cured products under UV radiation were studied. It can be concluded that newly synthesized UV radiation‐curable polyester acrylated prepolymers (palm oil based), namely PEPP‐1 and PEPP‐2, can be used as radiation curable coating materials for wood coating applications. © 2001 John Wiley & Sons, Inc. J Appl Polym Sci 79: 2156–2163, 2001     

Composites as cracking catalysts in the production of biofuel from palm oil: Deactivation studies

Composite catalysts HZSM-5/alumina (CZA) and Al-MCM-41/alumina (CMA) were synthesized and tested for their catalytic cracking activity in the production of biofuel from palm oil. Both composite catalysts were characterized for their structure, acidity and surface morphology. The addition of alumina in the composite catalysts improved their hydrothermal stability due to the changes in the surface morphology. The deactivation of the catalysts was studied by obtaining time on stream data by varying the palm oil to catalyst ratio of 8–16. The deactivation data were analyzed using different activity models and the deactivation parameters were determined.     

Synthesis and characterization of size controlled nano copper oxide structures for antioxidant study and as eco-friendly lubricant additive for bio-oils

This research work aims at the synthesis of Copper oxide (CuO) nanostructures with the application as additives for biolubricant oils, particularly Pongamia oil. The CuO particles were synthesized by a simple co-precipitation methodology. The nanostructures were characterized via analytical and microscopic techniques. The p-XRD analysis reveals the formation of size-controlled CuO formation, and the particle size was affirmed using both scherrer and William son Hall methods with particle size less than 14 nm. The surface morphology studies were substantiated by microscopic techniques. Elemental analysis reveal the purity of the prepared nanostructures. The monodispersed nanostructures are obtained with polydispersity index (PDI) of a value of 0.0550. The antioxidant property of CuO NPs was analyzed and is found in dose dependent manner, with efficiency of 71.9% at 50 μg/mL The influence of CuO nanoparticles on the viscosity of the lubricant is studied using the rheometer. The effect of these nanostructures on the friction characteristic is studied using a Ring-On-Block lubricity tester. The particles varied from 0.5 to 1 % wt. The CuO nanoparticles reduces the viscosity of the pongamia oil bio lubricants by 5.52% in comparision with the pongamia oil blended neem oil. The coefficient of Friction (COF) was found to be superlative for 0.75 % wt CuO added to Pongamia oil. The experimental result shows that CuO nanostructures is more effective than the blending of Neem oil with Pongamia oil and cane be used as an additives in the bio lubricants as the viscosity and friction modifier.     

微波辐射硫酸铁催化合成丙二酸二乙酯的研究

研究了利用微波辐射技术,在硫酸铁的催化下以丙二酸和无水乙醇为原料合成丙二酸二乙酯的反应,探讨了原料配比、反应时间、催化剂用量、带水剂、反应温度等对酯化率的影响。通过实验确定了最佳反应条件：n（乙醇）∶n（丙二酸）为3∶1,催化剂硫酸铁用量为1.0g,带水剂环己烷用量为20mL,微波辐射时间为10min,结果表明：该反应条件温和,方法简便,酯化率可达72.1%。利用折光率、红外光谱分析等对产品进行了物性、组成和结构表征。     

相转移催化法合成19,19,26,26-四十四烷基四羧酸四乙酯

研究了以丙二酸二乙酯、l,6-二溴己烷为原料,以十六烷基三甲基溴化铵(CTMBA)和聚乙二醇(PEG-1000)为协同相转移催化剂,在一定条件下首先合成了非离子Gemini表面活性剂中间体1,1,8,8-辛基四羧酸四乙酯,进而通过加原料溴代十八烷于1,1,8,8-辛基四羧酸四乙酯中,在相同催化剂条件下合成了标题化合物....     

Characterization of stabilized porous magnetite core–shell nanogel composites based on crosslinked acrylamide/sodium acrylate copolymers

Stabilized and dispersed superparamagnetic porous nanogels based on sodium acrylate (AA‐Na) and acrylamide (AM) in a surfactant‐free aqueous system were synthesized via solution polymerization at room temperature. The formation of magnetite nanoparticles was confirmed and their properties characterized using Fourier transform infrared spectroscopy. Extensive characterization of the magnetic polymer particles using transmission electron microscopy (TEM), dynamic light scattering and zeta potential measurements revealed that Fe₃O₄ nanoparticles were incorporated into the shells of poly(AM/AA‐Na). The average particle size was 5–8 nm as determined from TEM. AM/AA‐Na nanoparticles with a diameter of about 11 nm were effectively assembled onto the negatively charged surface of the as‐synthesized Fe₃O₄ nanoparticles via electrostatic interaction. Crosslinked magnetite nanocomposites were prepared by in situ development of surface‐modified magnetite nanoparticles in an AM/AA‐Na hydrogel. Scanning electron microscopy was used to study the surface morphology of the prepared composites. The morphology, phase composition and crystallinity of the prepared nanocomposites were characterized. Atomic force microscopy and argon adsorption–desorption measurements of Fe₃O₄.AM/AA indicated that the architecture of the polymer network can be a hollow porous sphere or a solid phase, depending on the AA‐Na content. © 2013 Society of Chemical Industry     

Enzymatic synthesis of fatty hydrazides from palm oils

Fatty hydrazides (FH) have been successfully synthesized from palm oils by a one-step lipase catalyzed reaction. The synthesis was carried out by treating the oils with hydrazine hydrate at neutral pH using an immobilized lipase, Lipozyme as the catalyst. The percentages of conversion of RBD (refined, bleached and deodorized) palm oil (PO), RBD palm olein (POn), RBD palm stearin (PS) and RBD palm kernel olein (PKOn) into their fatty hydrazides are 95, 97, 97 and 99, respectively.     

Long term activity of modified ZnO nanoparticles for transesterification

Biodiesel can be produced by the transesterification of natural oils with methanol using modified ZnO nanoparticles as catalyst. Crude algae oil, corn oil from DDGs, crude palm oil, crude soybean oil, crude coconut oil, waste cooking oil, food-grade soybean oil and food-grade soybean oil with 3% water and 5% FFA addition were converted into FAME within 3 h using this new catalyst. The ZnO nanoparticles were reused 17 times without any activity loss in a batch stirred reactor and the average yield of FAME was around 93.7%. ZnO nanoparticles were used continuously for 70 days in a fix bed continuous reactor and the average yield of FAME was around 92.3%. XRD, ICP, TEM and HRTEM were used to characterize the long term used catalyst structure. Results show that this catalyst is a mixture of wurtzite ZnO nanoparticles and some amorphous materials and that the used catalysts have similar crystal structure to fresh catalyst. ICP results show that this catalyst does not dissolve in biodiesel, methanol, oil and glycerine-methanol solutions. It has a stable crystal structure under the reaction conditions. The high catalytic activity, long catalyst life and low leaching properties demonstrate these modified ZnO nanoparticles have potential in a commercial biodiesel production process.     

Fatty acid esters of glycidol in refined fats and oils

Discrepancies in the analysis of 3‐chloropropane‐1,2‐diol (3‐MCPD) esters can be explained by the hypothesis that in some refined oils significant amounts of fatty acid esters of glycidol (glycidyl esters) are present in addition to 3‐MCPD esters. Glycidyl esters were separated from triacylglycerols by gel permeation chromatography (GPC) and detected by gas chromatography‐mass spectrometry (GC‐MS). Six samples of palm oil and palm oil‐based fats were analyzed by GPC and GC‐MS. In chromatograms of all samples, significant peaks, retention time and mass spectra in conformity with self‐synthesized glycidyl palmitate and glycidyl oleate were detectable. Quantification of individual glycidyl esters was not possible because of a lack of pure standards. Concentration of ester‐bound glycidol in different samples of fats and oils was estimated using an indirect difference method. Glycidyl esters could be detected only in refined, but not in crude or native, fats and oils. The highest concentrations were detected in palm oil and palm oil‐based fats. In a palm oil sample, glycidyl ester concentration varied according to different deodorization parameters, temperature, and time, while 3‐MCPD ester concentration was relatively constant, indicating that mitigation of glycidyl esters possibly may be achieved by optimizing refining parameters.     

Vegetable oil aided hydrothermal synthesis of cerium oxide nanocrystals

Hydrothermal synthesis of cerium oxide nanocrystals was performed with in-situ surface modification using soybean oil and palm oil as capping agents. The synthesized nanocrystals were examined by X-ray diffraction (XRD), transmission electron microscopy (TEM), Fourier transform infrared spectroscopy (FT-IR) and thermogravimetric analysis (TGA). TEM results showed single crystalline nature with stable dispersion. FT-IR spectra and TGA plots further confirmed the adsorption of fatty acid molecules onto cerium oxide surface. Our findings have the advantages of reduced materials costs compared to using single component surfactants and the production of valuable by-product glycerol.     

Preparation and Characterization of Poly L-Lactide/Triclosan Nanoparticles for Specific Antibacterial and Medical Applications

This work aims at preparation of poly-L-lactide (PLLA)/triclosan nanoparticles as antibacterial products used in some specific medical applications. PLLA was synthesized by the reaction extrusion via the ring opening polymerization of L-lactide using a continuous single-stage process, which is a fast and easy method. The PLLA triclosan nanoparticles were prepared by the emulsification–diffusion process with few modifications. Chloroform was used for the surface reaction of triclosan without any chemical shifts. The resulting nanoparticles with various triclosan quantities were fully characterized. The release as well as its kinetics was studied using the UV-visible spectroscopy. All the results confirmed the high stability and process efficiency of molecular dispersion and attachment of triclosan to PLLA. The sample containing 30% triclosan showed the best form among the others with the highest encapsulation efficiency. The synthesized nanoparticles with the controlled antibacterial activity could be considered as an appropriate alternative for application as antibacterial agent in the implantable surgical products as well as the drug delivery and wound-dressing applications.     

Polyester Polyol-Based Polyurethane Adhesive; Effect of Treatment on Rubber Surface

Polyester polyols were synthesized using vegetable oil fatty acids having different characteristics (mainly in terms of hydroxyl functionality) and epoxy resin, using triethylamine as a catalyst. Polyols were characterized by the FTIR spectroscopy. Polyurethane adhesives were synthesized from it and used in bonding rubber. Treatment of sulphuric acid on the non-polar styrene butadiene rubber (SBR) surface was studied for the bond strength improvement via an increase in wettability of the rubber surface. Wettability was found by measuring the contact angle using Goniometer. Bond strength was evaluated by a 180° T-peel test. The surface modification and mode of bond failure were studied by Scanning Electron Microscopy (SEM). The synthesized polyurethane adhesives were compared with the commercial adhesive.