陕北中低温煤焦油常压重油馏分GC-MS分析

以陕北中低温煤焦油的重油为原料,在常压蒸馏装置中切取100℃,100—200℃,200—240℃,240—270℃,270—300℃,300—340℃和340—390℃七段馏分,利用GC-MS分析馏分中化合物的组成情况。结果表明:200—240℃、270—300℃、300—340℃馏分的馏出质量最大,质量分数分别为12.62%,15.59%和17.73%;馏分中含有脂肪烃、芳香烃和酚类化合物及少量杂环化合物;酚类化合物主要富集在100—200℃、200—240℃、240—270℃3段馏分中,分别占各馏分质量的63.34%,59.65%和23.81%,所含酚类化合物主要为低级酚、C3—C4烷基苯酚、茚酚、苯二酚、萘酚和烷基萘酚等。     

陕北中低温煤焦油减压馏分的GC-MS分析

以陕北中低温煤焦油轻油为原料,在减压(1 kPa)蒸馏装置中切取＜100℃,100℃～170℃,170℃～200℃,200℃～240℃,240℃～270℃,270℃～300℃和300℃～340℃7段馏分.利用气相色谱-质谱联用技术(GC-MS)鉴定了馏分中化合物的组成和结构.结果表明,蒸馏终温为340℃可得到煤焦油约95％(质量分数);在各个馏分中都分布有脂肪烃类化合物;蒽菲类化合物主要分布在170℃～240℃馏分中;低级酚主要分布在＜100℃馏分中,酚类含量约占45％,其中苯酚含量为7.46％,甲酚含量为13％;高级酚分布于100℃～170℃和170℃～200℃馏分中;270℃～300℃和300℃～340℃馏分中也有少量低级酚和烯烃被发现,可能是高温下长链脂肪烃和高级酚类化合物发生热裂解所致.     

中/低温煤焦油酚类化合物的组成研究

借助GC-MS手段分析陕北中/低温煤焦油酚类化合物组成和分布情况.通过常减压蒸馏,将陕北中低温煤焦油切割成170℃～230℃,230℃～270℃,270℃～300℃,300℃～340℃和340℃～360℃五个窄馏分并计算收率,并用酸碱抽提法提取各窄馏分中的酚油;通过GC-MS分析了酚油中酚类化合物的组成及分布情况.结果表明,五个窄馏分分别检测出23,23,15,18和10种酚类化合物,酚类化合物占其所在馏分酚油的比率分别为96.89%,60.01%,50.90%,36.51%和36.37%.焦油中所含的酚类化合物占焦油总量的12.91%,酚类化合物主要为低级酚、C3～C4烷基苯酚和萘酚.     

陕北中低温煤焦油重油减压馏分的GC-MS分析

以陕北中低温煤焦油重油为原料,在减压(1 k Pa)蒸馏装置中切取100℃,100—170℃,170—200℃,200—240℃,240—270℃,270—300℃和300—340℃7段馏分。利用气相色谱-质谱联用技术(GC-MS)鉴定了馏分中化合物的组成。结果表明:蒸馏终温为340℃馏分收率(质量分数)为88.5%;各馏分中都分布有脂肪烃类化合物;蒽菲类化合物主要分布在170—240℃馏分中;低级酚主要分布在100℃,酚类质量分数约56%,其中苯酚质量分数为17%,甲酚质量分数为22%;270—300℃和300—340℃馏分也有少量低级酚和烯烃被发现。减压蒸馏可减少煤焦油蒸馏过程中发生缩聚、分解和结焦的可能性。     

陕北中低温煤焦油中酚类化合物的抽提研究

采用酸碱法抽提陕北中低温煤焦油轻油和重油中的酚类物质.将轻油和重油蒸馏切割成170℃～240℃,240℃～270℃,270℃～300℃三个馏分,对三个馏分分别进行了总酚含量测定.通过最小碱油比的测定得出使一定量馏分油完全反应所需最小碱用量.设计了正交实验,得出每个馏分的最佳碱洗条件.在最佳碱洗条件下,酸碱洗涤得到轻油三个馏分酚油收率为29.21%,19.70%和16.95%;对应馏分油中总酚的回收率为95.05%,93.19%和90.30%;重油三个馏分酚油收率为58.40%,40.99%和41.55%;对应总酚回收率为91.19%,87.74%和85.83%.对脱酚油的GC/MS分析,验证了酸碱法对中低温煤焦油中酚类物质进行了有效抽提.     

中低温煤焦油蒸馏过程中金属元素的迁移规律

以中低温煤焦油轻油和重油为实验原料,采用常压蒸馏获得170~200℃、200~240℃、240~270℃、270~300℃、300~320℃、320~340℃、340~360℃和360~390℃煤焦油馏分油;利用配有油品加氧制冷进样系统的ICP-OES测定了21种微量元素在馏分油中的含量,考察了不同馏分油中元素的分布情况。研究表明：在原煤焦油中,未发现Ag、Mg、Mo、Na、Ni、Fe、Mn、Cr及Ti元素,含量较高的元素有Sn、P、Al、Pb、Si,其中Sn元素在轻油和重油中的含量分别为11.78μg/g和14.04μg/g;在所有馏分油中,未发现Al、Mo、Fe、Mn、Cr及Ti元素,含量比较高的元素有Si、Sn、Na、Zn、Pb,特别是Si、Na、Sn、Zn、Ni、Pb及B元素可以有效富集于馏分油中。可能的原因是Ca、Fe、Mg、Al等金属以不同的盐类形态存在,在煤焦油脱水及<170℃蒸馏过程中,这些金属盐类会被部分带出,导致其在馏分油中的含量未富集或未检出;通过关联金属元素在馏分油中的分布与其组成的关系,馏分油中元素的分布可能与酚类化合物、杂环化合物和蒸馏温度等相关。酚类化合物及杂环化合物可能与Ag、B、Cu、Mo、Sn、Na、Zn、Ca、Pb等金属形成络合物或卟啉配合物,蒸馏温度一方面可以破坏Sn、Cd、Pb、Zn、Cu、Ca、Pb等元素在馏分油中的结合力,另一方面也可以促进这些元素与馏分油中的含氧、含氮等化合物更好地发生化合反应,进而影响金属元素在馏分油中的含量分布。     

神木中低温煤焦油酚类物质的分离与利用

测定了陕西神木中低温煤焦油轻油(L-tar)和重油(H-tar)的基本性质.通过常压蒸馏将煤焦油切割为220℃,220℃~260℃,260℃~300℃和300℃四段馏分.利用酸碱法对220℃,220℃~260℃,260℃~300℃三段馏分进行酚类提取研究,测定了三段馏分的总酚含量及最小碱油比.通过正交实验确定最佳碱洗条件,在最佳条件下,轻油对应的馏分段的总酚收率分别为92.23%,89.99%和87.91%;重油对应馏分段的总酚收率分别为94.60%,91.88%和90.73%.考察了所提取的混酚替代苯酚合成酚醛树脂的性能,轻油和重油混酚树脂的黏度及固含量分别为3.18Pa·s和3.73Pa·s以及79.39%和82.15%.     

煤液化中油馏分中酚类的影响因素研究

煤液化中油(220℃～260℃)馏分中含有大量的酚类化合物,其质量分数约20%～25%,其酚类化合物主要是由苯酚、(烷基)苯酚、(烷基)萘酚、(烷基)茚满酚和联苯酚等类型组成.考察了煤液化过程中反应温度、Mo系催化剂和添加高分油三种工艺条件对煤液化中油馏分中不同酚类的影响.结果表明,升高反应温度和加入Mo系催化剂能增加煤液化油中总粗酚产率,而添加高分油方式则不太明显;另外,添加高分油方式可以促进高级酚类中间体发生裂解、脱烷基和脱羟基等二次反应向生成分子量更小、结构更简单的低级酚类进行转化,而通过Mo系催化剂的加入可以抑制部分高级酚类向低级酚类的转化.     

陕北中低温煤焦油中吲哚提取研究

以陕北中低温煤焦油为原料,常压蒸馏并切取240~270℃馏分提取吲哚。利用傅里叶红外光谱仪(FTIR)、气相色谱质谱联用仪(GC/MS)对240~270℃馏分进行测试表征分析,考察了酸液种类、浓度、过量系数、反应温度、反应时间对吲哚提取的影响。结果表明,硫酸浓度为80%,过量系数为2.0,反应时间1.0 h,反应温度为50℃最佳。     

中低温煤焦油酚油馏分中酚类化合物的组成

以中低温煤焦油为原料,首先利用实沸点蒸馏装置得到中低温煤焦油的酚油馏分,并对酚油馏分的理化性质进行分析评价,然后对酚油馏分进行酸碱抽提处理得到碱抽提油和抽余油并进行元素分析,再利用衍生化处理和气相色谱相结合的方法对碱抽提油中的酚类化合物进行定性定量分析。结果表明:中低温煤焦油中170℃～230℃的酚油馏分收率为11.58%(质量分数),酸性组分约占酚油馏分油的65.23%(质量分数),且酚油馏分酸度高达62.04mgKOH/100mL;酚油馏分中低级酚含量很高,其中苯酚质量分数为5.84%,甲酚质量分数为20.70%,乙基苯酚质量分数为7.70%,二甲基苯酚质量分数为9.17%。酚油馏分经酸碱抽提后,含氧化合物绝大部分转移到富含酸性组分的碱抽提油中,碱抽提油中氧的质量分数高达15.11%。碱抽提油中甲酚含量最高,其中间甲酚质量分数为13.41%,对甲酚质量分数为9.24%,邻甲酚质量分数为9.09%。     

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。