Synthesis of oleyl oleate as a jojoba oil analog

Synthesis of a wax ester analog of jojoba oil was accomplished from oleic acid and oleyl alcohol with a zeolite as catalyst. A full 2³ factorial design at two levels has been used in the synthesis. The variables selected were temperature, reduced pressure and initial catalyst concentration. The most important variable within the range studied was temperature. Reduced pressure had a negative influence, and initial catalyst concentration showed a positive influence on the process. A response equation has been determined for the yield of ester. The properties of the synthesized product are similar to those of natural jojoba oil.     

Optimization of a process for the synthesis of a sperm whale oil analogue

The development and optimization of the synthesis of an analogue of sperm whale oil have been carried out. The product is an ester with characteristics similar to those of natural sperm whale oil. A central composite design was applied in the synthesis of this fine chemical. The variables selected for the present study are reaction temperature, initial concentration of catalyst and working pressure. Temperature is the most significant factor in the esterification process, and its influence is positive. Pressure influence can be neglected, and the catalyst concentration has a positive influence on the process. Depending on the temperature value, the influence of the interactions can be more important than that of the other two main effects, pressure and catalyst concentration. Response surface models have been found adequate to represent the yield of ester. The commercial quality of the synthesized product is very similar to that of natural spermaceti. Because of its low cost, this synthesis process is considered, from an economical point of view, very attractive.     

硬脂酰单宁酸酯的合成及抗氧化作用

以单宁酸和硬脂酰氯为原料合成了一种油溶性抗氧化剂硬脂酰单宁酸酯 (C18 TA)。探讨了硬脂酰氯和单宁酸的量比、催化剂对甲苯磺酸的用量、反应温度和溶剂等对合成的影响。确定了较佳的反应条件 :n(单宁酸 )∶n(硬脂酰氯 ) =1∶2 0 ,m(单宁酸 )∶m(催化剂 ) =1 0 0 :0 .0 3 ,二氧六环作溶剂 ,反应温度 10 0～ 10 2℃ ,氮气保护下反应 4h。C18 TA在菜籽色拉油中的含量为6 0 0mg/kg时 ,6 0℃强制氧化 18d ,其POV抑制率可达 6 6 0 % ,明显高于相同条件下BHT的POV抑制率 5 6 0 %     

大豆油异丙酯的合成研究

用碱催化酯交换法合成大豆油异丙酯,考察了醇油摩尔比、催化剂用量、反应温度、反应时间对酯交换反应的影响。结果表明,合成大豆油异丙酯的最佳条件如下:醇油摩尔比10∶1,反应时间60 min,反应温度80℃,碱催化剂浓度2.0%。在此条件下,大豆油异丙酯的产率达53.07%。最后对比研究了大豆油甲酯、乙酯、异丙酯的合成,得出不同结构的醇与大豆油进行酯交换反应的规律。色谱表征表明,经酯交换作用,原料油成功转化为生物柴油。     

低温费托合成蜡油加氢裂化精制技术的研究进展

低温费托合成技术因具有产品质量性好、反应耗能低、生产能力大且催化剂种类广泛等优点在煤化工领域备受关注,低温费托合成的蜡油产品可通过加氢裂化精制获取高品质清洁油品,具有巨大的应用价值。本文首先阐述了费托合成的产物特性,分析了加氢裂化过程的反应特点、双功能催化剂的碳正离子反应机理及蜡油主要反应历程。在此基础上,着重综述了蜡油加氢裂化双功能催化剂的研究进展,讨论了活性金属组分、载体以及助剂对加氢裂化过程的影响,分析表明活性金属的负载量、载体的酸量和孔道结构对催化性能有极大影响,合理优化和平衡加氢金属活性位和裂解酸性位是确保蜡油加氢裂化催化剂活性的关键。更为重要的是,基于分子筛载体的择形效应,实现载体多级孔结构和活性位的理性集成无疑会促进蜡油加氢产物的合理分布。     

Modeling of poly(ethylene terephthalate) reactors. I. A semibatch ester interchange reactor

A comprehensive model for a semibatch ester interchange reactor has been developed with a view to investigate the effect of various process and operational variables on the DMT conversion rate as well as the by-product formation. The influence of important variables such as EG-to-DMT ratio, catalyst concentration, and operational variables such as temperature and pressure has been considered. Definite conclusions concerning the choice of the desirable range of process and operational variables to maximize productivity and minimize by-product formation have been reached.     

二聚酸甲酯的合成研究

以亚麻油经醇解反应得到的亚麻油脂肪酸甲酯为原料,在催化剂存在下,用间歇常压聚合法,合成了二聚酸甲酯。用正交试验设计考察了反应温度,催化剂用量,反应时间对二聚反应产物收率的影响,找到了最佳反应条件。     

椰子油脂肪酸单乙醇酰胺的合成

在碱性催化剂作用下以椰子油脂肪酸甲酯和单乙醇胺为原料合成椰子油脂肪酸单乙醇酰胺。考察了反应温度、反应时间、投料比、体系压力等因素对反应收率的影响 ,并通过正交实验优化了工艺条件 ,得到最佳工艺条件为 :反应温度 110℃、反应时间 5h、n(甲酯 )∶n(醇胺 ) =1∶1 1、反应体系压力 2 0kPa。在最优条件下收率可达 99%。利用重结晶法对反应产物进行分离提纯 ,并用高效液相色谱进行了分析检测     

Optimization of <Emphasis Type="Italic">Brassica carinata</Emphasis> oil methanolysis for biodiesel production

Synthesis of FAME from Brassica carinata oil to produce biodiesel was accomplished using potassium hydroxide as the catalyst. A factorial design of experiments and a central composite design were used. The variables chosen were: type of Brassica carinata oil, initial catalyst concentration, and temperature; and the responses were FAME purity and yield. The type of B. carinata oil included high-erucic B. carinata (HEBC) and lowerucic B. carinata (LEBC) varieties. The results show that the type of B. carinata oil does not affect the purity and yield of FAME. However, HEBC oil is more suitable for biodiesel production because its iodine value is lower and within the European Union specifications. The initial catalyst concentration is the most important factor, having a positive influence on FAME purity but a negative effect on FAME yield. The temperature has a significant positive effect on FAME purity and a significant negative influence on FAME yield. Second-order models were obtained to predict FAME purity and yield as a function of catalyst concentration and temperature for HEBC oil methanolysis. The best conditions for this process are 25°C, and 1.2–1.5 wt% for the catalyst concentration.     

Catalytic hydroliquefaction of North Dakota lignite part I. Effects of process variables on product distribution

Finely ground North Dakota lignite slurried in anthracene oil was hydrogenated in a continuous stirred tank reactor in the presence of a cobalt-molybdenum catalyst. Effects on product distribution of process variables such as H₂ pressure, temperature, space time, lignite concentration in anthracene oil, and catalyst concentration have been investigated. Results indicate that 80% of maf lignite can be converted into gaseous and liquid products with an oil yield of about 35% on the same basis.     

Ethanolysis of Refined Soybean Oil Assisted by Sodium and Potassium Hydroxides

The ethanolysis of refined soybean oil was investigated through a 2³ experimental design that was carried out under the following levels: ethanol:oil molar ratios (MR) of 6:1 and 12:1, NaOH concentrations of 0.3 and 1.0 wt% in relation to the oil mass, and reaction temperatures of 30 and 70 °C. The ethanol:oil MR and the alkali concentration had an almost equivalent influence on the reaction yield, whereas the influence of increased reaction temperatures was very limited and higher catalyst concentrations led to greater yield losses due to the formation of soap. Ethyl ester yields of 97.2% were obtained at 70 °C, MR of 12:1 and 0.3 wt% NaOH. Replacement of 0.3 wt% NaOH by 1.0 wt% KOH under the same reaction conditions led to lower ester yields. Likewise the former, KOH provided the maximum ester yield (95.6%) at the highest molar ratio (12:1), with the reaction temperature having little influence on the catalyst performance. Ester yields beyond 98% were only achieved when a second ethanolysis stage was included in the process. In this regard, the application of 2 wt% Magnesol^® after the first ethanolysis stage eliminated the need for water washing prior to the second ethanolysis stage and helped to generate a final product with less contaminating unreacted glycerides.     

Oil from deep water fish species as a substitute for sperm whale and jojoba oils

The lipid fraction of the deep water fish species orange roughy (Hoplostetbus atlanticus), black oreo (Allocyttus sp.) and small spined oreo (Pseudocyttus maculatus) had wax esters with even carbon numbers over the range C₃₀ to C₄₆ as the major components. The component acids and alcohols of the wax ester fraction were analyzed by gas liquid chromatography and compared with those of jojoba and sperm whale oils. Orange roughy oil was refined and deodorized and its chemical, physical and mechanical properties were determined. Hydrogenation of orange roughy oil produced a range of white crystalline waxes with melting points between 34 and 66 C. The characteristics of these waxes were very similar to those of hydrogenated jojoba oil and spermaceti. Lubricant tests performed on sulfurized orange roughy oil indicated it is comparable to sulfurized jojoba and sperm whale oils as an extreme-pressure additive in lubricants. The results show a sound technical basis on which to consider an industry based on orange roughy oil and the oreo oils as replacements for sperm whale oil and as substitutes for jojoba oil. Applications for the oil could be in the cosmetic and high-grade lubricant fields, the waxes in the polish, textile, cosmetic and pharmaceutical industries and the sulfurized derivative of orange roughy oil in the lubricant industry.     

Continuous production of palm methyl esters

A system for continuous transesterification of palm oil was developed using a continuous stirred-tank reactor (CSTR) and pumps for continuous delivery of oil and catalyst and for continuous removal of product. Potassium hydroxide was used as the catalyst, the methanol-to-oil molar ratio was 6∶1, and reaction temperature was 60°C. The yield of methyl esters increased from 58.8% of theoretical yield at a residence time of 40 min to 97.3% at a residence time of 60 min. However, higher residence times decreased the production rate. During long-term continuous operation, the CSTR displayed steady state conditions in terms of product profile and methyl ester concentration. This process has good potential in the manufacture of biodiesel.     

固体超强酸SO_4~(2-)/TiO_2催化合成利巴韦林缩合物研究

以1,2,4-三氮唑-3-羧酸甲酯和1,2,3,5-四-O-乙酰基-β-D-呋喃核糖为原料,在催化剂固体超强酸SO42-/TiO2的作用下得到了1-(2,3,5-三-O-乙酰基-β-D-呋喃核糖基)-1H-1,2,4-三唑-3-羧酸甲酯,简称利巴韦林缩合物。它是广谱抗病毒药物利巴韦林的重要中间体。通过对影响反应的多种因素进行研究以及反应条件的优化,结果表明:当催化剂为固体超强酸SO42-/TiO2、催化剂用量为12%、1,2,4-三氮唑-3-羧酸甲酯和1,2,3,5-四-O-乙酰基-β-D-呋喃核糖投料摩尔比为1.05:1、反应温度控制在100℃～110℃、反应时间为2h、甲醇重结晶,所得产物收率为87.0%,纯度99.5%(HPLC)。该反应方法催化剂易制备,催化效率较高,容易循环使用,不污染环境,有一定的再生能力,易从产品中除去,操作过程简便,产品色泽好、纯度高。     

催化合成邻苯二甲酸二辛酯的固体酸制备条件优化

采用自制的固体酸SO42-/SnO2为催化剂合成邻苯二甲酸二辛酯(DOP),通过试验分别考察浸泡硫酸浓度、颗粒度、活化温度和活化时间等因素对催化剂活性的影响。试验表明:在固体酸SO42-/SnO2催化DOP的合成中,催化剂适宜制备工艺条件是:浸泡硫酸浓度3.2 mol/L、颗粒度130目、活化温度500℃和活化时间5.0 h,DOP产率可达95%以上。固体酸SO42-/SnO2催化剂具有催化活性高、可多次重复使用、产物易纯化分离和产品色泽浅等优点,有望代替传统浓硫酸作催化剂用于DOP的合成。     

Fatty acids,fatty alcohols,and wax esters fromLimnanthes douglassi (Meadowfoam) seed oil

Limanathes douglasii seed oil glycerides contain fatty acids which predominantly (97%) have 20 or more carbon atoms. Fatty acids were prepared by saponification; fatty alcohols, by sodium reduction of the glycerides; and liquid wax esters, byp-toluenesulfonic acid-catalyzed reaction of the fatty acids with the fatty alcohols. Solid waxes were prepared by hydrogenation of the glyceride oil and of the wax esters. Chemical and physical constants were determined forLimnanthes douglasii seed oil and its derivatives. The liquid wax esters had properties very similar to those of jojoba (Simmondsia chinensis) seed oil. The solid hydrogenated wax ester was identical in physical appearance and melting point to hydrogenated jojoba seed oil. A laboratory of the Northern Utilization Research and Development Division, Agricultural Research Service, USDA.     

环氧大豆油无溶剂法合成研究

介绍了一种环氧大豆油的无溶剂法合成工艺．通过正交实验方法优选了合成工艺条件；讨论了甲酸用量、双氧水用量及滴加速度、催化剂用量、反应温度、反应时问等对产物环氧值的影响。     

连续重整装置设计参数的选择

揭示了连续重整的反应温度、压力、空速、氢油比、催化剂循环速率的相互关系,以及催化剂、原料和产品辛烷值对这些参数的影响。通过对比现有连续重整装置的设计参数及实际运行状况,充分考虑连续重整工艺和催化剂的技术进步,对新建连续重整装置的设计参数进行了探讨。     

Transesterification of rapeseed oil in subcritical methanol conditions

In this study, transesterification of rapeseed oil using subcritical methanol conditions was studied. The objective of the work was characterizing the methyl esters for its use as biodiesel in compression ignition motors. The variables affecting the methyl ester yield during the transesterification reaction, such as, the catalyst type and content, reaction temperature and pressure, the presence of hexane as co-solvent, the methanol oil molar ratio and the methanol hexane molar ratio were investigated to optimize the reaction conditions. The evolution of the process was followed by gas chromatography, determining the concentration of the methyl esters at different reaction times. The biodiesel was characterized by its density, viscosity, saponification value, iodine value, acidity index and water content, according to ISO norms. High methyl ester yield and fast reaction rate could be obtained even if the reaction pressure was relatively low, which is quite favorable to the production of biodiesel in industry.     

Software development for design and simulation of terraced wall and top fired primary steam reformers

In recent years, many research activities have been carried out on effective use of natural gas. The first step for this process, however, is converting natural gas to synthesis gas (syngas). Natural gas reforming process by means of a reformer furnace is commonly used for syngas and hydrogen production.

In this paper a windows-based software, RIPI-RefSim, is introduced. By using rigorous heat, mass, kinetic and thermodynamic models as well as taking into account the effect of catalyst shape, the software has been developed in order to provide reformer furnace simulation for syngas and hydrogen production. RIPI-RefSim can be used in three different modes (rating, simulation and design) and provides a detailed understanding of furnace performance, product characteristics, temperature, reaction rates and pressure drop profiles, effect of catalyst shape, and so on.