煤焦油中蒽、菲、咔唑的精制技术

主要介绍了煤焦油中蒽、菲和咔唑的精制方法,系统地总结了溶剂洗涤法、精馏-溶剂法、结晶-精馏法、乳化液膜法、区域熔融法、溶剂萃取-恒沸蒸馏-升华法和化学分离法、新型分离法等精制蒽、菲及咔唑的工艺原理,对各种方法所具有的优势及不足之处进行了评述。     

溶剂结晶法用于蒽渣精制高纯咔唑研究

利用物性估算的方法估算了蒽、咔唑、二甲苯及氯苯间的范德华引力能,并测定了相应的溶解度.利用气质联用(GC-MS)对原料蒽渣中各个组分进行定性分析,以气相色谱内标标准曲线法对工艺过程中每一步所得产品中蒽、菲、咔唑和芴的含量进行了定量分析.结果表明,氯苯与蒽和咔唑间的引力能均大于二甲苯,与溶解度相一致.采用二甲苯两步溶解结晶后,菲和芴的去除率分别为96%和91%.以氯苯为溶剂精制咔唑,可得到含量为98.68%的高纯咔唑,咔唑的单程回收率在45%以上.     

N-乙烯基咔唑的合成及表征

以咔唑和甲基丁炔醇为原料,反应生成N-乙烯基咔唑,反应液经过进一步处理得到纯品N-乙烯基咔唑。考察了反应用溶剂、反应温度及反应时间对N-乙烯基咔唑收率的影响。结果表明：合成产物的最佳溶剂是DMSO,最佳反应温度为140℃,最佳反应时间为12h。产物经FTIR、1HNMR、13CNMR进行结构表征。N-乙烯基咔唑的液相色谱纯度>99.5%,气相色谱纯度>99.5%,熔点64℃,总产率85%,合成产物可作为电子级化学品使用。     

稠杂环芳烃醛树脂的研究取得初步成果

丹东市化工研究所采用工业菲为原料,试制稠杂环芳烃醛树脂与塑料,已完成了小试验研究。制得的树脂性能,一般达到和超过酚醛树脂性能,经推广在石棉摩擦制动制品(即刹车片)方面应用,效果较好。一、采用的原料如下: 1.工业菲:纯度60～75％(石家庄桥西焦化厂产品)。该所实测成份: 原菲:菲62.22％,咔唑3.36％,蒽16.52％。新菲1:菲58.79％,咔唑3.15％,蒽18.57％。新菲2:菲63.79％,咔唑2.77％,蒽14.53％。     

用结晶—蒸馏法制取精蒽—精咔唑

用精蒽氧化制取的蒽酮是酸性染料、还原染料和分散染料的中间体。咔唑主要用于生产染料中间体,也可用于生产医药、杀虫剂和特种聚合物。从煤焦油制得的粗蒽中含蒽量25％～40％,含咔唑10％～18％。 过去,一般采用溶剂法制取精蒽,但此法只能从粗蒽中回收蒽,咔唑等则随残油排出,还存在产品收率低和环境污染严重等问题。即使对于目前国内广泛使用的溶剂-洗涤法,虽能从     

从粗蒽中提取精蒽和精咔唑的研究

介绍了以粗蒽为原料,轻苯作溶剂,经溶剂萃取、恒沸蒸馏制取94%的精蒽,再以蒸馏残渣为原料,经升华提取91%的咔唑的试验情况,同时优选出了最佳的工艺参数。     

焦油中精蒽／咔唑提取工艺的评述

介绍了近年来从焦油中提取精蒽和咔唑产品工艺的现状,并对两种常用工艺从工艺方案合理性、技术先进性及经济技术三方面做了较详尽的比较分析和综合评述。提出结晶－蒸馏法是目前提取精蒽／咔唑技术先进、工艺合理、有发展前途的工艺。同时提出了对现有溶剂洗涤法制取精蒽和咔唑工艺状况的改进设想。     

直接缩聚法合成聚乳酸的研究

研究了以乳酸为单体,用直接缩聚法合成聚乳酸的反应过程。利用联苯醚作为溶剂,与体系的水分进行共沸回流,达到充分脱水的目的。探讨了反应历程中包括温度、反应时间、溶剂用量、催化剂用量等参数对聚合产物的分子量的影响。     

重结晶法提纯碳酸亚乙烯酯的研究

采用重结晶法对碳酸亚乙烯酯(VC)粗品进行提纯,考察了重结晶溶剂、溶剂用量、重结晶温度、恒温时间、重结晶次数对提纯效果的影响,并确定了最佳条件。研究结果表明:重结晶法提纯后VC纯度明显提高,且收率高。     

萃取法生产咔唑的研究

蒽、菲、咔唑是我国染料、塑料、农药、油漆、造纸和国防等工业的重要原料,外贸出口需要量也较大。若将粗蒽中的咔唑分离出来,既可满足国内外市场的需要,而且又为工业菲的分离利用创造了条件。采用萃取法新工艺制备咔唑,改变了传统工艺中糠醛聚合树脂对生产的影响。制备的咔唑产品纯度≥95%,收率30%以上。1实验原料粗蒽质量见表1。二甲基甲酰胺(DMF)由衡阳化工厂生产,含量99%。重质苯由鞍钢化工总厂生产,经常压蒸馏处理,切取140～200℃的馏分。2实验装置常压蒸馏装置由1000mL三口烧瓶、800mm冷凝器、2kW电炉、调压器(0～250V)及温度计等…     

Insect antifeedant properties of anthranoids from the genusVismia

Vismiones and ferruginins, representatives of a new class of lypophilic anthranoids from the genusVismia were found to inhibit feeding in larvae of species ofSpodoptera, Heliothis, and inLocusta migratoria.     

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.     

Ethanol and (−)-α-Pinene: Attractant Kairomones for Bark and Ambrosia Beetles in the Southeastern US

In 2002–2004, we examined the flight responses of 49 species of native and exotic bark and ambrosia beetles (Coleoptera: Scolytidae and Platypodidae) to traps baited with ethanol and/or (−)-α-pinene in the southeastern US. Eight field trials were conducted in mature pine stands in Alabama, Florida, Georgia, North Carolina, and South Carolina. Funnel traps baited with ethanol lures (release rate, about 0.6 g/day at 25–28°C) were attractive to ten species of ambrosia beetles (Ambrosiodmus tachygraphus, Anisandrus sayi, Dryoxylon onoharaensum, Monarthrum mali, Xyleborinus saxesenii, Xyleborus affinis, Xyleborus ferrugineus, Xylosandrus compactus, Xylosandrus crassiusculus, and Xylosandrus germanus) and two species of bark beetles (Cryptocarenus heveae and Hypothenemus sp.). Traps baited with (−)-α-pinene lures (release rate, 2–6 g/day at 25–28°C) were attractive to five bark beetle species (Dendroctonus terebrans, Hylastes porculus, Hylastes salebrosus, Hylastes tenuis, and Ips grandicollis) and one platypodid ambrosia beetle species (Myoplatypus flavicornis). Ethanol enhanced responses of some species (Xyleborus pubescens, H. porculus, H. salebrosus, H. tenuis, and Pityophthorus cariniceps) to traps baited with (−)-α-pinene in some locations. (−)-α-Pinene interrupted the response of some ambrosia beetle species to traps baited with ethanol, but only the response of D. onoharaensum was interrupted consistently at most locations. Of 23 species of ambrosia beetles captured in our field trials, nine were exotic and accounted for 70–97% of total catches of ambrosia beetles. Our results provide support for the continued use of separate traps baited with ethanol alone and ethanol with (−)-α-pinene to detect and monitor common bark and ambrosia beetles from the southeastern region of the US.     

Methyl 2,4,6-decatrienoates Attract Stink Bugs and Tachinid Parasitoids

Halyomorpha halys (Stål) (Pentatomidae), called the brown marmorated stink bug (BMSB), is a newly invasive species in the eastern USA that is rapidly spreading from the original point of establishment in Allentown, PA. In its native range, the BMSB is reportedly attracted to methyl (E,E,Z)-2,4,6-decatrienoate, the male-produced pheromone of another pentatomid common in eastern Asia, Plautia stali Scott. In North America, Thyanta spp. are the only pentatomids known to produce methyl 2,4,6-decatrienoate [the (E,Z,Z)-isomer] as part of their pheromones. Methyl 2,4,6-decatrienoates were field-tested in Maryland to monitor the spread of the BMSB and to explore the possibility that Thyanta spp. are an alternate host for parasitic tachinid flies that use stink bug pheromones as host-finding kairomones. Here we report the first captures of adult and nymph BMSBs in traps baited with methyl (E,E,Z)-2,4,6-decatrienoate in central Maryland and present data verifying that the tachinid, Euclytia flava (Townsend), exploits methyl (E,Z,Z)-2,4,6-decatrienoate as a kairomone. We also report the unexpected finding that various isomers of methyl 2,4,6-decatrienoate attract Acrosternum hilare (Say), although this bug apparently does not produce methyl decatrienoates. Other stink bugs and tachinids native to North America were also attracted to methyl 2,4,6-decatrienoates. These data indicate there are Heteroptera in North America in addition to Thyanta spp. that probably use methyl 2,4,6-decatrienoates as pheromones. The evidence that some pentatomids exploit the pheromones of other true bugs as kairomones to find food or to congregate as a passive defense against tachinid parasitism is discussed.     

2007～2008年世界塑料工业进展

收集了2007年7月～2008年6月世界塑料工业的相关资料,介绍了2007～2008年国外塑料工业的发展情况,提供了世界塑料产量、消费量及全球各类树脂的需求量及产能情况.按通用热塑性树脂(聚乙烯、聚丙烯、聚苯乙烯、聚氯乙烯、ABS树脂)、工程塑料(尼龙、聚碳酸酯、聚甲醛、热塑性聚酯、聚苯醚)、特种工程塑料(聚苯·硫醚、液晶聚合物、聚醚醚酮)、通用热固性树脂(酚醛、聚氨酯、不饱和聚酯树脂、环氧树脂)不同品种的顺序,对树脂的产量、消费量、供需状况及合成工艺、产品应用开发、树脂品种的延伸及应用的进一步扩展等技术作了详细介绍.     

2005～2006年国外塑料工业进展

收集了2005年7月～2006年6月国外塑料工业的相关资料,介绍了2005—2006年国外塑料工业的发展情况。提供了世界塑料产量、消费量及全球各类树脂生产量以及各国塑料制品的进出口情况。作为对比,介绍了中国塑料的生产情况。按通用热塑性树脂（聚乙烯、聚丙烯、聚苯乙烯、聚氯乙烯、ABS树脂）、工程塑料（聚酰胺、聚碳酸酯、聚甲醛、热塑性聚酯、聚苯醚）、通用热固性树脂（酚醛、聚氨酯、不饱和树脂、环氧树脂）、特种工程塑料（聚苯硫醚、液晶聚合物、聚醚醚酮）的品种顺序,对树脂的产量、消费量、供需状况及合成工艺、产品开发、树脂品种的延伸及应用的扩展作了详细的介绍。