环氧亚麻油的制备工艺研究

通过单因素实验方法催化合成了环氧亚麻油,以产品环氧值为考察指标,研究了催化剂种类、反应时间、催化剂用量、甲酸用量、双氧水用量、反应温度对反应的影响.结果表明,以硫酸为催化剂,反应时间8 h,反应温度为65℃,反应物料质量比m(亚麻油):m(甲酸):m(硫酸):m(双氧水)=1:0.06:0.0015:0.65,硫酸0....     

亚麻油催化异构化改性研究(Ⅰ)

以负载型镍催化剂对亚麻油的双键异构化进行了研究,获得了催化剂最佳配方及制备条件。确定了亚麻油异构化的最佳工艺参数。在此条件下,异构化亚麻油的共轭三烯键可达百分之十二。异构化亚麻油涂膜的干性,耐水、耐化学试剂性能均优于“双漂”亚麻油。     

亚麻油催化异构化改性研究（I）

以负载型镍催化剂以亚麻油的双键异构化进行了研究，获得了催化剂最佳配方及制备条件。确定了亚麻油异构化的最佳工艺参数，在此条件下，异构化亚麻油的共轭三烯键可达百分之十二，异构化亚麻油涂膜的干性，耐水，耐化学试剂性能均优于“双漂”亚麻油。     

二环戊二烯双酚型环氧树脂及环氧酯漆的合成研究

本文用二环戊二烯和苯酚合成二环戊二烯双酚,再用它与环氧氯丙烷合成二环戊二烯双酚型环氧树脂,并用这种环氧树脂与亚麻油酸合成气干型环氧酯漆,测试了漆膜的性能。实验证明,适当的酚超量和较低的滴加二环戊二烯的反应温度可控制二环戊二烯的自聚反应。     

硫酸氢铵盐离子液体催化亚麻油制备生物柴油的研究

以浓硫酸和三乙胺为原料制备了酸性离子液体硫酸氢铵盐[Et3NH][HSO4],作为催化剂用于亚麻油与甲醇酯交换反应制备生物柴油。考察了催化剂添加量、醇油摩尔比、反应温度和反应时间等因素对酯交换产品收率的影响。试验结果表明:硫酸氢铵盐离子液体对酯交换反应有很高的催化活性,在甲醇与亚麻油摩尔比为8∶1、催化剂占原料油质量分数6%、反应温度120℃和反应时间5 h的优化条件下,酯交换产品收率可达90%以上。产物中含有十五酸甲酯、软脂酸甲酯等长链酯类物质,与生物柴油的化学组成分相似,说明离子液体硫酸氢铵盐能够催化制备生物柴油。     

过氧化氢一步法制备环氧亚麻油工艺

报道了亚麻油在以石油醚为溶剂、磷酸为催化剂的条件下,经甲酸、双氧水环氧化,一步合成增塑剂———环氧亚麻油的一种新方法。该法反应条件温和,操作方法简单,反应时间较短,而且产物各项指标均可达到增塑剂标准:环氧值>7.8,碘值<10,酸值<0.5。     

过氧化氢一步法制备环氧亚麻油工艺

报道了亚麻油在以石油醚为溶剂、磷酸为催化剂的条件下,经甲酸、双氧水环氧化,一步合成增塑剂——环氧亚麻油的一种新方法。该法反应条件温和,操作方法简单,反应时间较短,而且产物各项指标均可达到增塑剂标准：环氧值＞7.8,碘值＜10,酸值＜0.5。     

亚麻油酸开环环氧树脂的研究

本文以N,N-二甲基苄胺为催化剂,通过亚麻油酸对环氧树脂E51进行开环反应制备了一种多元醇,并通过傅里叶红外光谱及1HNMR对其结构进行表征。研究了反应温度和反应时间对反应进程的影响,结果表明反应条件在100℃下反应4h时最佳。     

β-二酮镍催化丙烯的二聚反应

丙烯二聚是生产板重要的Co烯烃的重要方法。用β—二酮镍络合物催化丙烯二聚是一个十分活跃的研究领域。作者结合自己的实验工作,对各种β—二酮镍络合物催化丙烯二聚的催化剂性能,助催化剂的影响,反应条件,反应转化率,产物的线性率以及反应的机理等进行了归纳和总结。     

二聚亚麻油酰氯的合成与表征

以二聚亚麻油酸和三氯化磷为原料,经过酰氯化反应有效合成了标题化合物.通过正交实验研究了物料物质的量比、反应温度、反应时间对合成工艺的影响,确定最优工艺条件:n(二聚亚麻油酸):n(三氯化磷)=1:2.8,反应温度为70℃.反应时间6h,所得产品纯度达90%,总收率85%以上.采用IR、1HNMR和13CNMR对目标化合...     

Mizellare Zweiphasen-Hydroformylierung von ungesättigten Fettstoffen mit wasserlöslichen Rhodiumcarbonyl/tert. Phosphan-Komplexkatalysatorsystemen

Micellar Two Phase-Hydroformylation of Multiple Unsaturated Fatty Substances with Water Soluble Rhodiumdicarbonyl/tert. Phosphine Catalyst Systems Low- and medium-molecular ω-unsaturated carboxylic acid methyl esters inclusive of the ω-decenoic acid ester can be hydrofomylated successfully according to the two phase method in an aqueous-organic medium using the water soluble rhodium carbonyl/tris(sodium-m-sulfonatophenyl)phosphine complex as catalyst system. Highermolecular unsaturated fatty acid esters, e.g. the triple unsaturated linolenic acid methyl ester or fatty oils like linseed oil can be hydroformylated only according to the micellar two phase technique in course of which surfactant micelles cause a solubilisation of the water insoluble unsaturated fatty substances in the aqueous catalyst phase. The different efficiences of the various types of surfactants for the micellar two phase hydroformylation was investigated and interpreted. Best suitable for the micellar two-phase hydroformylation are cationic surfactants. By means of these surfactants linolenic acid methyl ester could be hydroformylated to the triformyl derivative with a selectivity of 55%. The recovery of the catalyst solution free from losses of rhodium succeeded by simple phase separation in a technically satisfying manner.     

Fatty acid esters of furfuryl alcohol

Summary Furfuryl esters were prepared from linseed oil and methyl palmitate by alcoholysis using metallic sodium as the catalyst. They were also prepared from linseed oil and from methyl oleate by partial saponification in furfuryl alcohol. These esters, although containing conjugated double bonds, did not possess any increased drying power. Iodine numbers were determined by several methods, and, except with the Woburn reagent, the furfuryl group was found to exhibit a higher iodine number when combined as an ester than when present as the free alcohol. Furfuryl esters were found to polymerize to products of greatly decreased iodine number and increased acidity, showing that polymerization involved both deacylation and reaction at the double bonds of the furan ring. Paper No. 53, Journal Series, Chemical Research Department, General Mills, Inc.     

制备脂肪酸甲酯的新工艺研究

采用新型固体碱催化剂LDH/LDO进行菜油酯交换反应制备脂肪酸甲酯 ,产率达 98.5%以上。该工艺操作简单 ,可直接获得脂肪酸甲酯和副产物甘油 ,催化剂可回收再生 ,整个过程无三废污染。     

C_(22)-三元酸三酯的合成

C22-三元酸三酯的合成以棉籽油甲酯为原料,将非共轭的亚油酸甲酯在催化剂作用下转化成共轭亚油酸甲酯,同时与富马酸二酯发生D iels-A lder反应,生成C22-三元酸三酯。采用正交实验设计探讨了C22-三元酸的甲基二异戊酯的投料比、温度、催化剂用量、反应时间对合成反应的影响。富马酸二酯加入量按照富马酸二酯∶亚油酸甲酯(摩尔比)=1.1∶1投料,反应温度选择在200~210℃,催化剂碘的用量在0.6%,反应控制在2 h,最佳转化率相对于亚油酸甲酯可达96%。     

C22-二元酸单甲酯的合成

以棉籽油甲酯为原料,将非共轭的亚油酸甲酯在催化剂作用下转化共轭亚油酸甲酯,同时与富马酸发生Diels-Alder反应,生成C22-二元酸单甲酯,并采用正交实验设计探讨了投料比、温度、催化剂用量、反应时间对合成反应的影响。富马酸加入量按照n(富马酸)∶n(亚油酸甲酯)=1.1∶1投料,反应温度选择在200～210°C,催化剂碘的用量在0.3%(质量分数),反应控制在2h,转化率相对于亚油酸甲酯为98%。此工艺易于实现产业化。     

Fatty acid methyl ester as reactive diluent in thermally cured solvent-borne coil-coatings—The effect of fatty acid pattern on the curing performance and final properties

Four different fatty acid methyl esters (FAMEs): rape seed methyl ester (RME), tall oil methyl ester (TOME), and two types of linseed oil methyl ester (Linutin) have been studied as reactive diluents in thermally cured solvent-borne coil-coatings. The purpose was to evaluate the effect of fatty acid methyl ester structure on the curing performance and final properties of the coating. The permanent incorporation of the reactive diluent via transesterification reaction has been followed with ¹H NMR analysis of model systems. Dynamic mechanical analysis (DMA) measurements, of free-standing films, show that the glass transition temperature (T_g) decreases upon addition of the reactive diluent. Both the amount of incorporated reactive diluent and the final film properties are affected by the number and placement of alkene-bonds in the FAME.     

Optimization of the reaction parameters for fast pseudo single-phase transesterification of sunflower oil

Transesterification of sunflower oil with methanol was carried out using potassium hydroxide and methoxide as catalysts and MTBE as cosolvent. The aim of this work was to study and optimize the reaction parameters. Chosen parameters were reaction time, catalyst amount and methanol amount (expressed as catalyst-to-oil and methanol-to-oil molar ratios, respectively). The response variables were methyl ester content (ME) and acid value (AV) due to their relationship with the completion and yield reaction, respectively. A factorial plus composite design was developed to carry out the optimization. From this design, several quadratic models have been used to fit the experimental data. All the factors studied had a positive influence on methyl ester content and acid value, except the methanol amount on acid value. For methoxide catalyst, optimum values were 0.235 catalyst to oil molar ratio, 12 methanol to oil molar ratio and 5 min reaching 99 wt.% ME and 0.20 mg KOH/g of AV.     

Process optimization for methyl ester production from waste cooking oil using activated carbon supported potassium fluoride

This paper presents the transesterification of waste cooking palm oil (WCO) using activated carbon supported potassium fluoride catalyst. A central composite rotatable design was used to optimize the effect of molar ratio of methanol to oil, reaction period, catalyst loading and reaction temperature on the transesterification process. The reactor was pressurized up to 10 bar using nitrogen gas. All the variables were found to affect significantly the methyl ester yield where the most effective factors being the amount of catalyst and reaction temperature, followed by methanol to oil ratio. A quadratic polynomial equation was obtained for methyl ester yield by multiple regression analysis using response surface methodology (RSM). The optimum condition for transesterification of WCO to methyl ester was obtained at 3 wt.% amount of catalyst, 175 °C temperature, 8.85 methanol to oil molar ratio and 1 h reaction time. At the optimum condition, the predicted methyl ester yield was 83.00 wt.%. The experimental value was well within the estimated value of the model. The catalyst showed good performance with a high yield of methyl ester and the separation of the catalyst from the liquid mixture is easy.     

The optimization of the ultrasound-assisted base-catalyzed sunflower oil methanolysis by a full factorial design

The ultrasound-assisted sunflower oil methanolysis using KOH as a catalyst was studied at different reaction conditions. A full factorial experiment 3³ with replication was performed. The effects of three reaction variables, methanol-to-oil molar ratio, catalyst loading and the reaction temperature on fatty acid methyl ester yield were evaluated by the analysis of variance and the multiple regression. At the 95% confidence level all three factors and the interaction of the reaction temperature and methanol-to-oil molar ratio were effective on fatty acid methyl ester formation, the most important factor being the catalyst loading. The relationship between the factors and their interactions was modeled by the second-order polynomial equation.     

Transesterification of karanja (Pongamia pinnata) oil by solid basic catalysts

The transesterification of karanja oil with methanol was carried out using solid basic catalysts. Alkali metal‐impregnated calcium oxide catalysts, due to their strong basicity, catalyze the transesterification of triacylglycerols. The alkali metal (Li, Na, K)‐doped calcium oxide catalysts were prepared and used for the transesterification of karanja oil containing 0.48–5.75% of free fatty acids (FFA). The reaction conditions, such as catalyst concentration, reaction temperature and molar ratio of methanol/oil, were optimized with the solid basic Li/CaO catalyst. This catalyst, at a concentration of 2 wt‐%, resulted in 94.9 wt‐% of methyl esters in 8 h at a reaction temperature of 65 °C and a 12 : 1 molar ratio of methanol to oil, during methanolysis of karanja oil having 1.45% FFA. The yield of methyl esters decreased from 94.9 to 90.3 wt‐% when the FFA content of karanja oil was increased from 0.48 to 5.75%. The performance of this catalyst was not significantly affected in the presence of a high FFA content up to 5.75%. The catalytic activities of Na/CaO and K/CaO were also studied at the optimized reaction conditions. In these two cases, the reaction initially proceeds slowly, however, leading to similar yields as in the case of Li/CaO after 8 h of reaction time. The purified karanja methyl esters have an acid value of 0.36 mg KOH/g and an ester content of 98.6 wt‐%, which satisfy the American as well as the European specifications for biodiesel in terms of acid value and ester content.