双-[γ-(三乙氧基硅)丙基]-四硫化物水相合成方法的研究

以γ-氯丙基三乙氧基硅烷为原料,在水相中通过相转移催化合成了双-[γ-(三乙氧基硅)丙基]-四硫化物(Si-69).讨论了反应温度、γ-氯丙基三乙氧基硅烷与多硫化钠的量之比、相转移催化荆的用量等对合成反应的影响.水相中合成Si-69的较佳工艺为:γ-氯丙基三乙氧基硅烷与多硫化钠的量之比为2.1:1,相转移催化剂的用量为γ-氯丙基三乙氧基硅烷质量的2%,反应温度80℃,可制得硫含量高于22.8%,纯度高达95%以上的Si-69.     

一锅法制备含硫硅烷偶联剂TESPT

利用歧化和缩合反应原理,采用相转移催化一锅法将原料氢氧化钠、硫磺和γ-氯丙基三乙氧基硅烷制备成双-3-(三乙氧基硅烷)丙基四硫化物,考察了原料配比、氢氧化钠浓度、滴加方式及催化剂等对产品质量及收率的影响。结果表明,优化工艺条件为:氢氧化钠∶硫磺∶γ-氯丙基三乙氧基硅烷质量比为1.00∶1.33∶4.06,氢氧化钠浓度为25%,以2%四丁基氯化铵复配季铵盐作催化剂,歧化反应温度70℃,反应时间50 min,缩合反应温度85℃,滴加γ-氯丙基三乙氧基硅烷1 h,在此条件下,产率95.6%,硫含量为22.7%。     

一锅法制备含硫硅烷偶联剂TESPT

利用歧化和缩合反应原理,采用相转移催化一锅法将原料氢氧化钠、硫磺和γ-氯丙基三乙氧基硅烷制备成双-3-(三乙氧基硅烷)丙基四硫化物,考察了原料配比、氢氧化钠浓度、滴加方式及催化剂等对产品质量及收率的影响。结果表明,优化工艺条件为:氢氧化钠∶硫磺∶γ-氯丙基三乙氧基硅烷质量比为1.00∶1.33∶4.06,氢氧化钠浓度为25%,以2%四丁基氯化铵复配季铵盐作催化剂,歧化反应温度70℃,反应时间50 min,缩合反应温度85℃,滴加γ-氯丙基三乙氧基硅烷1 h,在此条件下,产率95.6%,硫含量为22.7%。     

新型硅烷偶联剂硫氰基丙基三乙氧基硅烷合成

由硫氰化钾与γ-氯丙基三乙氧基硅烷合成硫氰基丙基三乙氧基硅烷，在温度120—130℃回流反应3h，收率82％左右。该硅烷偶联剂应用于多种天然及合成橡胶的补强，偶联效果好。     

双-（γ-三乙氧基硅丙基）四硫化物

中南大学的陈雷等人以九水硫化钠、硫粉、γ-氯丙基三乙氧基硅烷为原料,甲苯为溶剂,得到双-（γ-三乙氧基硅丙基）四硫化物。较佳工艺条件为：硫与九水硫化钠的量之比为3：1,甲苯与九水硫化纳的量之比为36：1,γ-氯丙基三乙氧基硅烷与多硫化钠的量之比为2．1：1,无水乙醇与多硫化钠的量之比为8：1,反应温度80℃,合成时间3．5h。制得的产品外观淡黄色,     

硫氰基丙基三乙氧基硅烷的合成

以硫氰酸盐、γ-氯丙基三乙氧基硅烷[γ-Cl(CH2)3Si(C2H5O)3]为原料，合成了硅烷偶联剂硫氰基丙基三乙氧基硅烷。讨论了硫氰酸盐和溶剂的种类、反应温度，以及硫氰酸盐、γ-氯丙基三乙氧基硅烷、溶剂的配比对反应的影响。结果表明，以硫氰化钾(KSCN)为原料、二甲基甲酰胺(DMF)为溶剂，且KSCN与γ-Cl(CH2)3Si(C2H5O)3、DMF的质量比为1：2．36：2．4--2．5时，在120--130℃回流反应3h，硫氰基丙基三乙氧基硅烷的收率可达82％左右；其应用性能与德国Degussa公司的Si-264相当。     

新型橡塑硫化助剂的合成

以九水硫化钠、硫粉、γ-氯丙基三乙氧基硅烷为原料,甲苯、乙醇作溶剂,合成了双-(γ-三乙氧基硅丙基)二硫化物。讨论了反应物比例、溶剂用量、反应温度和时间等因素对产率的影响。结果表明,最佳工艺条件:硫与九水硫化钠的物质的量比为1.05:1,甲苯与九水硫化钠的物质的量比为36:1,γ-氯丙基三乙氧基硅烷与过硫化钠的物质的量比为2.1:1,无水乙醇与过硫化钠的物质的量比为5.0:1,反应温度为80℃,反应时间为4 h。最终制得的产品外观为淡黄色,类乙醇香味,产率为95.63%,含硫量达13.8%,产品贮存时间长。     

含异氰酸酯基丙基三乙氧基硅烷的合成

研究了氯丙基三乙氧基硅烷与氰酸钾反应制备异氰酸酯基丙基三乙氧硅烷的方法,考察了反应温度,反应物的配比优化,溶剂种类以及保护试剂的种类对合成产率的影响,确立了最佳的合成条件：反应物氯丙基三乙氧基硅烷与氰酸钾的摩尔比为1：1．15,DMF为溶剂,己内酰胺为保护试剂,反应温度为125℃,收率可达92％,并采用波谱分析确证了目标物质的结构。     

双组份相转移催化法合成双-[3-(三乙氧基硅烷)丙基]-四硫化物的研究

以γ-氯丙基三乙氧基硅烷、硫化钠和硫磺为原料,采用相转移催化法合成双-[3-(三乙氧基硅烷)丙基]-四硫化物。通过正交实验探讨了Na_2S_4溶液制备的最佳工艺条件:硫磺:硫化钠质量比为1:0.85、反应温度50℃、真空度为0.05 MPa、反应时间40 min;利用单因素实验分析确定Si-69合成反应条件为:γ-氯丙基三乙氧基硅烷:硫磺:硫化钠质量比5.6:1:0.85、反应温度80℃左右、反应时间2.0h左右;并讨论了相转移催化剂、复合有机胺、水解抑制剂对产品质量和收率的影响。采用该方法能提高产物收率、缩短反应时间、降低反应温度,所得产品的外观呈淡黄色透明液体,含硫量达22.5%,纯度达到98.5%,收率达95%以上。     

硅胶固载γ－氯丙基三甲氧基硅烷制备水不溶性杀菌剂中间体

北京石油化工学院的李凤艳等采用硅胶作为水不溶性杀菌剂的载体，以γ－氯丙基三甲氧基硅烷作为连接硅胶和杀菌活性官能团的偶联剂；在硅胶上键合γ－氯丙基三甲氧基硅烷的最佳反应条件为：二甲苯作溶剂，80 ℃反应6 h以上，硅胶最好经丙酮处理，γ－氯丙基三甲氧基硅烷与硅胶的质量比为1∶1。使用该中间体制备的水不溶性杀菌剂2 mg／mL时，杀菌率达到98%。     

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.     

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.     

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。     

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.     

Inorganic/organic nanocomposite coatings: The next step in coating performance

Inorganic/organic hybrid materials have considerable promise and are beginning to become a major area of research for many coating usages, including abrasion and corrosion resistance. Our primary approach is to prepare the inorganic phase in situ within the film formation process of the organic phase. The inorganic phase is introduced via sol-gel chemistry into a thermosetting organic phase. By this method, the size, periodicity, spatial positioning, and density of the inorganic phase can be controlled. An important aspect of the inorganic/organic hybrid materials is the coupling agent. The initial task of the coupling agent is to provide uniform mixing of the oligomeric organic phase with the sol-gel precursors, which are otherwise immiscible. UV-curable inorganic/organic hybrid systems have the advantages of a rapid cure and the ability to be used on heat sensitive substrates such as molded plastics. Also, it is possible to have better control of the growth of the inorganic phase using UV curing. It is our ultimate goal to completely separate the curing of inorganic and organic phases to gain complete control over the morphology, and hence optimization of “all” the coating properties. Thus far, it has been found that concomitant UV curing of the inorganic and organic phases using titanium sol-gel precursors afforded nanocomposite coatings which completely block the substrate from UV light while maintaining a transparent to visible light. Also, it has been found that the morphology of the inorganic phase is highly dependent on the concentration and reactivity of the coupling agent. Presented at the 82nd Annual Meeting of the Federation of Societies for Coatings Technology, October 27–29, 2004, in Chicago, IL.     

Ethanol and (−)-α-Pinene: Attractant Kairomones for Some Large Wood-Boring Beetles in Southeastern USA

Ethanol and α-pinene were tested as attractants for large wood-boring pine beetles in Alabama, Florida, Georgia, North Carolina, and South Carolina in 2002–2004. Multiple-funnel traps baited with (−)-α-pinene (released at about 2 g/d at 25–28°C) were attractive to the following Cerambycidae: Acanthocinus nodosus, A. obsoletus, Arhopalus rusticus nubilus, Asemum striatum, Monochamus titillator, Prionus pocularis, Xylotrechus integer, and X. sagittatus sagittatus. Buprestis lineata (Buprestidae), Alaus myops (Elateridae), and Hylobius pales and Pachylobius picivorus (Curculionidae) were also attracted to traps baited with (−)-α-pinene. In many locations, ethanol synergized attraction of the cerambycids Acanthocinus nodosus, A. obsoletus, Arhopalus r. nubilus, Monochamus titillator, and Xylotrechus s. sagittatus (but not Asemum striatum, Prionus pocularis, or Xylotrechus integer) to traps baited with (−)-α-pinene. Similarly, attraction of Alaus myops, Hylobius pales, and Pachylobius picivorus (but not Buprestis lineata) to traps baited with (−)-α-pinene was synergized by ethanol. These results provide support for the use of traps baited with ethanol and (−)-α-pinene to detect and monitor common large wood-boring beetles from the southeastern region of the USA at ports-of-entry in other countries, as well as forested areas in the USA.