原乙酸三甲酯的合成研究

研究由乙腈为原料经守基亚氨基醋酸酯盐酸盐醇解制备原乙酸三甲酯的工艺方法，对投料比、反应料比、反应温度、反应时间及中和指示剂等工艺条件进行了研究，得出较优惠的工艺条件。     

焦化蜡油脱氮工艺研究

在实验室条件下考察了水浴温度、剂油比、含水量(酸的稀释比)等工艺条件对酸性试剂络合萃取脱除焦化蜡油中碱性氮化物的影响。确定了焦化蜡油脱氮的最佳工艺条件为:水浴温度50℃,剂油比1％,含水量0．12mL／g,在此条件下脱氮率为62．5％。此脱氮工艺方法可以有效的降低焦化蜡油中的碱氮含量,而且操作条件缓和,方法简单。     

乙酸甲酯与甲醇共沸物催化精馏水解工艺

以乙酸甲酯与甲醇共沸物为原料,采用阳离子交换树脂为催化剂,研究了乙酸甲酯催化精馏水解工艺。在实验中以捆扎包作为催化剂的装填方式,系统地研究了催化精馏段和提馏段的高度、进料位置、进料中含甲醇、水酯物质的量比、回流进料比和空速等对酯分解率的影响,获得了最佳的工艺条件。分析了传统的水解分离工艺,提出了可行的新工艺。在最佳工艺条件下,新工艺系统的能耗比传统的固定床工艺降低39.99%。     

乙腈法萃取精馏丁二烯过程模拟与工艺优化Ⅱ.乙腈质量分数、腈烃比和回流比对分离效果的影响

采用Unifac基团结构法在乙腈法萃取精馏丁二烯装置中建立了乙腈-C4系统相平衡关系,利用PROⅡ化工模拟软件对第一萃取精馏塔、第二萃取精馏塔内乙腈质量分数、腈烃比、回流比等工艺条件对分离效果的影响进行了系统分析。结果表明,第一萃取精馏塔适宜的工艺条件为:乙腈质量分数93%~94%,腈烃比7·0~8·0,回流比2·5~3·0;第二萃取精馏塔适宜的工艺条件为:乙腈质量分数93%~94%,腈烃比1·5~2·0,回流比3·0。     

Aspen Hysys在油田净化商品油蒸馏装置的应用

针对让那若尔油田油气处理厂自用油需求及气候条件等特点,采用Aspen Hysys流程模拟软件对净化商品油蒸馏工艺进行模拟,考察了塔板数、侧线抽出位置、进料温度、回流比、塔操作压力、塔底汽提蒸汽用量及侧线汽提蒸汽用量等因素对蒸馏效果的影响,并得到了相应的影响规律。又通过进料温度和回流比的正交模拟试验结合现场的实际条件优化了工艺条件,确定了冬、夏两季的加工方案工艺条件。     

硬脂酸铝制备方法的研究

研究了合成硬脂酸铝的方法、工艺路线，并考察了反应过程中的投料比、温度、pH值等对合成的影响，选出了最佳工艺条件。     

影响沉淀白炭黑吸油值和比表面积的工艺因素

采用正交试验法研究了反应物浓度、温度、时间等多种工艺因素对沉淀白炭黑吸油值的影响,得到制备沉淀白炭黑的最佳工艺条件。氮吸附实验结果表明该工艺条件下制得的白炭黑具有较高的比表面积。     

荔枝核黄酮类化合物的提取工艺研究

采用回流、热浸提、微波提取等工艺提取荔枝核黄酮类化合物,采用正交实验考察了提取溶剂浓度、提取时间、微波功率、提取温度、料液比等因素对提取率的影响,优选出不同工艺的提取条件。回流提取工艺的优化条件是:50%乙醇溶液,提取温度80℃,提取时间1h,料液比1∶10,提取3次,总黄酮得率为6.76%。热浸提工艺的优化条件是:50%乙醇溶液,提取温度70℃,提取时间1.5h,料液比1∶12,提取2次,总黄酮得率达到6.37%。微波提取工艺的优化条件是:60%乙醇溶液,微波功率700W,提取时间2.5h,料液比1∶25,总黄酮得率达到6.86%。     

高品质季戊四醇合成工艺的研究

以甲醛、乙醛、烧碱为原料合成季戊四醇,通过正交试验,考察了各种工艺条件对合成单季戊四醇收率的影响。确定的优惠工艺条件为:甲醛与乙醛的分子比6.0,碱与乙醛的分子比1.20,甲醛溶液浓度12.0%,反应温度20℃,反应时间120min。在优选的工艺条件下,单季戊四醇的收率可达94.4%。     

磷酸二氢钙制备磷酸二氢钠磷收率研究

磷酸二氢钙是湿法磷酸精细加工的重要产品,开发以磷酸二氢钙为中间产物的精加工系列产品符合目前市场需求。研究了磷酸二氢钙与硫酸钠复分解反应制备磷酸二氢钠的工艺条件,并通过浓缩结晶得到磷酸二氢钠产品。对反应温度、物料配比、液固比以及反应时间诸因素对磷收率的影响进行了研究,确定了复分解过程适宜的工艺条件：反应温度为50 ℃,物料配比（硫酸钠与磷酸二氢钙物质的量比）为1.2∶1,液固比（质量比）为4∶1,反应时间为120 min。在此条件下磷收率可达79.1%。该工艺具产品纯度高、工艺流程简单、操作简便等优点。     

Variation of Brominated Indoles and Terpenoids Within Single and Different Colonies of the Marine Bryozoan Flustra foliacea

The variation of the brominated indole and diterpenoid content within single and different colonies of the bryozoan Flustra foliacea was investigated. The secondary metabolite profile and concentrations of individual components of F. foliacea samples were established using GC-MS. Samples from 17 different collecting sites were analyzed. The alkaloid and diterpene composition of F. foliacea varied greatly depending upon the site of collection. Investigation of F. foliacea samples from a single site (Helgoland, North Sea) over a period of time showed that the alkaloid and diterpenoid profile remained constant, however concentrations of individual components varied significantly. The alkaloid and diterpenoid composition of different segments of a single colony was found to be constant. Only small differences could be detected in the essential oil composition of different colonies and segments of single colonies of F. foliacea. Two of the F. foliacea alkaloids were found in the gastropods Hydrobia ulva and Gibbula cinerea, and one alkaloid in the common starfish Asteria rubens, all collected from the surface of the bryozoan.     

The Viscosity of cottonseed oil,fractionation solvents and their solutions

Cold fractionation of cottonseed oil is made difficult by the high viscosity of the oil. This study was aimed at demonstrating the effect of solvents on the viscosity of mixtures between 0°C and 25°C with a view to facilitating the fractionation of refined cottonseed oil. The solvents used were acetone, methylethylketone, methylisobutylketone, hexane and heptane. Measurements of viscosity were carried out by means of a capillary viscometer. The ratio of the viscosity of cottonseed oil to that of pure solvents is of the order of 300. The viscosities of solutions of various ratios of solvent to oil (1/3, 1/1, 3/1) are between those of cottonseed oil and the pure solvents. The effect of the solvent/oil ratio overrides that of solvent nature. The effect of solvent in reducing the viscosity of cottonseed oil is by descending order: acetone, hexane, methylethylketone, heptane, methylisobutylketone.     

木质素/热塑性塑料复合材料界面增容的研究进展

将木质素作为一种有机颗粒填料添加到热塑性塑料中,可解决造纸黑液资源化利用、石油原料日渐紧张以及环境污染加剧等严峻问题。而木质素与热塑性塑料之间相容性直接影响木质素在塑料工业中的应用与发展。首先简要概述了木质素结构与性质和木质素/热塑性塑料复合材料的性能分析,然后系统地阐述国内外研究木质素/热塑性塑料复合材料界面增容方法及其原理;增容方法按添加相容剂、改性木质素和改性塑料进行归类,并对3种增容方法进行比较分析;接着综述了木质素复合材料中增容方法的交叉复合使用;最后对未来木质素/热塑性塑料复合材料界面增容的研究方向以及思路进行了展望。     

Pd-Pb/SiO2催化高浓度乙烯基乙炔加氢合成丁二烯

研究了硅胶负载钯铅双金属催化剂催化高浓度乙烯基乙炔加氢合成丁二烯过程。结果表明,加入适量的铅可起到分隔钯纳米粒子,阻碍钯纳米粒子团聚的作用,从而提高催化剂的催化活性,最佳Pb/Pd摩尔比为0.2。继续提高Pb/Pd摩尔比时,会生成铅钯合金相,造成催化剂活性降低。X射线光电子能谱结果表明,催化剂的催化活性与Pd 3d的电子结合能呈正相关关系。制备催化剂过程中,还原温度对催化剂的结构和催化性能影响显著。在350℃下还原得到的催化剂中金属氧化物还原不彻底,催化剂活性较低;还原温度为450℃时,则会引起钯纳米粒子烧结,造成催化剂的催化活性和对丁二烯的选择性同时降低;催化剂的最佳还原温度为400℃。在40℃催化乙烯基乙炔反应40 h后,积炭造成催化剂的孔道堵塞,催化剂失活。因此,需要进一步开展改善催化剂的抗积炭能力和使用寿命方面的研究。     

Natural products phytotoxicity A bioassay suitable for small quantities of slightly water-soluble compounds

A large variety of secondary metabolites that can inhibit germination and/or seedling growth are produced by plants in low quantities. The objective of this study was to develop a bioassay capable of reliably assessing reductions in germination percentage and seedling length of small-seeded plant species caused by exposure to minute quantities of these compounds. The germination and growth of alfalfa (Medicago saliva), annual ryegrass (Lolium multiflorum), and velvetleaf (Abutilon theophrasti) were evaluated against six known phytotoxins from five chemical classes; cinmethylin (a herbicidal cineole derivative) was selected as a comparison standard. Each phytotoxin, dissolved in a suitable organic solvent, was placed on water-agar in small tissue culture wells. After the solvent evaporated, imbibed seeds were placed on the agar; after three days, germination percentages and seedling lengths were measured. Compared to a commonly used filter paper procedure, this modified agar bioassay required smaller quantities of compound per seed for comparable bioassay results. This bioassay also readily permitted the measurement of seedling length, a more sensitive indicator of phytotoxicity than germination. Seedling length decreased sigmoidally as the toxin concentration increased logarithmically. Phytotoxicity was a function of both compound and plant species. Cinmethylin, a grass herbicide, reduced the length of annual ryegrass seedlings by 90–100%, whereas that of alfalfa and velvetleaf was inhibited slightly. The agar bioassay facilitated the rapid and reliable testing of slightly water-soluble compounds, requiring only minute quantities of each compound to give reproducible results.The mention of firm names or trade products does not imply that they are endorsed or recommended by the U.S. Department of Agriculture over other firms or similar products not mentioned.     

合成气经二甲醚羰基化及乙酸甲酯加氢制无水乙醇的研究进展

合成气经二甲醚羰基化及乙酸甲酯加氢路线制无水乙醇技术因具有诸多优点而备受市场关注。本文综述了该工艺的核心反应机理和最近研究进展。主要探讨了丝光沸石8元环与12元环对羰基化反应的作用。阐明了如何通过调变丝光沸石8元环与12元环的活性位来提高羰基化催化剂的活性与稳定性。评述了铜纳米粒子的粒径、分散度以及Cu⁺与Cu⁰的分布等特点对铜基催化剂加氢催化活性的影响。提高乙醇选择性与催化剂稳定性是该研究的重点与难点。指出羰基化催化剂的优化重点是调变丝光沸石的孔道结构,加氢催化剂的发展方向是构建高分散度的铜纳米粒子,并在反应过程中保持稳定。     

Oxidation of acylglycerols and phosphoglycerides by soybean lipoxygenase

Lipoxygenase (EC 1.13.11.12) catalyzes the incorporation of oxygen into polyunsaturated fatty acids, resulting in the formation of their corresponding hydroperoxides. The ability of a commercial preparation of soybean (Glycine max L. Merr.) lipoxygenase to catalyze the oxidation of acylglycerols and phosphoglycerides was investigated. The oxidation rate of trilinolein increased nearly 100% when 5 mM deoxycholate was added to the reaction medium. With further increases in the concentration of deoxycholate, the oxidation rate decreased slightly. The pH profile of trilinolein oxidation was bell-shaped. The rate of oxidation was maximal at pH 8, and it decreased to near zero at pH 5 and pH 11. Even under optimal conditions, the rate of trilinolein oxidation was only 3% of that of linoleic acid, and analysis of time course data showed that, at most, 15% of available linoleate was oxidized. In contrast to the slow rate of trilinolein oxidation, tested phosphoglycerides and diacylglycerols were oxidized at moderate rates. The rate of phosphoglyceride oxidation depended upon the structure of the polar head group and varied between 7–28% of the rate of linoleic acid oxidation. Diacylglycerols reacted at a rate that was 40% of that of linoleic acid. Analysis of the time course of 1,3-dilinolein oxidation showed that as much as 67% of the available linoleate could be converted to the corresponding hydroperoxide. Analyses by high-performance liquid chromatography revealed that more than 20% of the 1,3-dilinolein was converted to unidentified products that are not hydroperoxides.     

Trapping the western pine beetle at and near a source of synthetic attractive pheromone Effects of trap size and position

Western pine beetles were caught on unbaited sticky traps placed near a source ofexo-brevicomin, frontalin, and myrcene. Size of trap, distance and direction from the source of attractant, and height from the ground were varied. Significant differences in trap catch were observed in relation to each of the variables. Traps close to the source of attractant caught more beetles than traps farther from the source. Traps downwind of the source of attractant caught more beetles than did upwind traps. More males than females were trapped close to the source of attractant.Based in part on a thesis submitted by the senior author to the University of California, Berkeley, California, in partial fulfillment of the requirements for the degree Master of Science in entomology, December 1976. These studies were supported by the U.S. Forest Service and in part by the Rockefeller Foundation and a joint grant (NSF GB-34718/BMS 75-04223) from the U.S. National Science Foundation and the U.S. Environmental Protection Agency to the University of California. The findings, opinions, and recommendations are not necessarily those of the University of California or the funding agencies.Trade names and commercial enterprises or products are mentioned solely for information and do not constitute endorsement by the U.S. Department of Agriculture or University of California.     

Kondensation von Dampfgemischen nicht mischbarer Flüssigkeiten

Condensation of Vapour Mixtures of Immiscible Liquids In contrast to the condensation of pure vapours and vapour mixtures of miscible liquids, the condensation of vapour mixtures forming immiscible or only partly miscible condensates is still poorly understood. Models describing heat transfer in the latter kind of condensation deviate so much from one another, not only quantitatively but also qualitatively, that reliable design of condensers is impossible. The reason lies primarily in the variety of flow patterns of two‐phase condensates, which range from pure droplet to pure film condensation. This paper surveys literature reports of the flow patterns and heat transfer occurring during condensation of vapour mixtures in the miscibility gap of their liquids. Qualitative knowledge in this condensation area is shown to be satisfactory. Several models have been proposed for heat transfer. However, the heat transfer coefficients obtained from these models differ too much from one another to allow one to choose the “best” correlation. Our own experiments with a eutectic benzene–water mixture on a vertical tube show that the calculation scheme proposed by Hoon and Burnside leads to acceptable results.     

Direct observation of freeze-thaw instability of latex coatings via high pressure freezing and cryogenic SEM

Despite its industrial importance, the subject of freeze-thaw (F/T) stability of latex coatings has not been studied extensively. There is also a lack of fundamental understanding about the process and the mechanisms through which a coating becomes destabilized. High pressure (2100 bar) freezing fixes the state of water-suspended particles of polymer binder and inorganic pigments without the growth of ice crystals during freezing that produce artifacts in direct imaging scanning electron microscopy (SEM) of fracture surfaces of frozen coatings. We show that by incorporating copolymerizable functional monomers, it is possible to achieve F/T stability in polymer latexes and in low-VOC paints, as judged by the microstructures revealed by the cryogenic SEM technique. Particle coalescence as well as pigment segregation in F/T unstable systems are visualized. In order to achieve F/T stability in paints, latex particles must not flocculate and should provide protection to inorganic pigment and extender particles. Because of the unique capabilities of the cryogenic SEM, we are able to separate the effects of freezing and thawing, and study the influence of the rate of freezing and thawing on F/T stability. Destabilization can be caused by either freezing or thawing. A slow freezing process is more detrimental to F/T stability than a fast freezing process; the latter actually preserves suspension stability during freezing. Presented at the 82nd Annual Meeting of the Federation of Societies for Coatings Technology, October 27–29, 2004 in Chicago, IL. Tied for first place in The John A. Gordon Best Paper Competition.