偏高岭土微波加热合成NaX分子筛及其机理探讨

本文以偏高岭土为主要原料,采用微波加热法合成了静态饱和吸水量超过32.0％的NaY分子筛.进行了单因素实验,考察了晶化时间、胶化时间、n(Na2 O/Al2O3)对合成分子筛的影响.通过静态水吸附测定、XRD、IR和SEM等测试手段考察反应条件对合成NaX分子筛的影响,并对NaY分子筛晶体生长规律进行了探讨研究.实验得...     

NaY型分子筛膜的合成及表征

采用二次生长法,在管状莫来石支撑体外表面水热合成了NaY型分子筛膜。讨论了多种因素,如凝胶老化时间、合成温度、合成时间等对膜合成的影响。采用X射线衍射(XRD)和扫描电子显微镜(SEM)对膜进行了表征。XRD谱图证明在支撑体外表面形成了NaY型分子筛,根据SEM照片,膜层厚度在10~20μm。该膜表现出了对水的很高选择性,表明所制备的膜缺陷较少。     

NaY分子筛合成工艺

报道了以具有独特组成的硅铝凝胶为导向剂制备NaY分子筛的方法。所合成的NaY分子筛用SEM、XRD和BET等进行了表征,结果表明,该NaY分子筛粒径2μm左右,硅铝比n(SiO2)/n(Al2O3)为3.28,结晶度90%,比表面积703 m2/g。除晶化过程外,该合成NaY分子筛的工艺过程均在室温下进行,具有反应条件温和,易于调控的特点。     

ZSM-5/NaY型复合分子筛膜的制备及其渗透汽化性能研究

采用水热合成法在n(SiO_2)∶n(Al_2O_3)∶n(Na_2O)∶n(H_2O)为25∶1∶22∶600的合成液体系中合成高性能的ZSM-5/NaY型复合分子筛膜,考察了陈化时间、合成液中水的摩尔分数、合成时间以及合成温度对膜的渗透汽化分离性能的影响,同时,考察了ZSM-5/NaY型复合分子筛膜的稳定性。利用SEM和XRD对膜的形态结构进行表征。结果表明,在合成液陈化18 h后,在105℃下晶化6 h,可成功制备出连续致密的ZSM-5/NaY型复合分子筛膜;在75℃下分离90%的异丙醇/水体系,渗透侧水质量分数可以达到99.15%以上,渗透通量保持在2.12 kg/(m~2·h)以上,并且具有良好的重复性。     

油页岩渣制备洗涤助剂4A分子筛的工艺条件和性能研究

以油页岩渣为原料,采用水热合成法制得4A分子筛.重点考察了n(Na2O)/n(SiO2)比、n(H2O)/n(Na2O)比、晶化时间、晶化温度对分子筛Ca2+交换量的影响.适宜的合成条件为:n(Na2O)/n(SiO2)=2.5,n(H2O)/n(Na2O) =50,晶化时间18 h,晶化温度90℃.并用XRD、SEM测试手段对合成的分子筛的晶体结构、表面形貌等进行了表征,结果表明,制备的样品为4A型分子筛结构,属于立方形晶型.     

低Na_2O/Al_2O_3比凝胶一步晶化法合成高硅小晶粒NaY分子筛

NaY晶体的n(Na_2O)∶n(Al_2O_3)=1.0,但现有NaY合成工艺的起始凝胶的n(Na_2O)/n(Al_2O_3)均较高,导致大量原料中的Na_2O及相应量其他组分没有转化为产品,而是进入晶化母液被滤除,因此NaY生产企业期望采用更低n(Na_2O)∶n(Al_2O_3)的凝胶来提高NaY合成收率。对起始凝胶Na_2O与Al_2O_3物质的量比为3.84~4.64的水热合成NaY分子筛做了研究。结果表明,在100℃以下晶化时,n(Na_2O)∶n(Al_2O_3)=3.84的低碱度凝胶不能晶化出NaY分子筛;在100℃以上晶化时,n(Na_2O)∶n(Al_2O_3)=3.84的低碱度凝胶能够晶化出结晶度、硅铝比(Si O2与Al_2O_3物质的量比,下同)均较高且无杂晶的NaY。其最佳的晶化条件:晶化温度为110℃、晶化时间为30 h。并可重复制备出平均结晶度为95%、平均骨架硅铝比为5.93、典型粒径约为1μm的小晶粒NaY分子筛,原料平均转化率达68.2%。     

不同添加剂对合成NaY分子筛的影响

本文以工业水玻璃为原料,对合成超细NaY分子筛进行了研究.考察了添加吐温-20、乙酸及二者混合物对合成NaY分子筛的影响,采用XRD、SEM、TEM等技术对所合成的分子筛进行了表征.结果表明,加入吐温20、乙酸及二者混合物均能降低分子筛的粒径,且添加二者混合物对于降低分子筛的晶粒尺寸和提高分散度均具有明显的促进作用,当二者混合物组成为吐温20含量为合成体系Al2O3含量的0.1％,乙酸含量是合成体系Al2 O3含量的150％时,可以得到粒径分布较窄、晶粒大小为180 nm左右及分散度较好的NaY分子筛.     

L沸石合成及其影响因素的研究

采用水热合成法成功合成出高结晶度的L沸石.合成初始凝胶(物质的量)组成为5.4K2O:5.7Na2O:1Al2O3:30SiO2:500H2O,反应温度为175℃,反应时间为24 h.采用X射线衍射(XRD)、扫描电镜(SEM)对合成的沸石分子筛进行了表征.XRD检测结果表明:制备的沸石具有L沸石典型特征峰,结晶度较高.SEM检测结果表明:合成的L沸石分子筛呈圆柱状,粒径约为1 μm,大小均匀.由于L沸石晶化区间相对狭窄,合成过程中须严格控制反应条件,所以又全面考察了水热合成条件对L沸石晶化的影响,结果表明:nSiO2/nAl2O3、Nh2o/n(Na2O+K2O)、nNa2O/n(Na2O+K2O)对结晶过程影响很大;陈化可以较好地减小晶粒尺寸,增加晶粒均匀度.     

气化灰渣合成13X分子筛及其表征

以气化灰渣为原料,通过水热反应合成13X分子筛,研究n(SiO2):n(Al2 O3),n(Na2O):n(SiO2)和结晶温度对气化灰渣合成13X分子筛的影响,并利用XRD,SEM,FTIR,TG-DTG和BET等方法对合成产物的化学组成、微观形貌、表面基团、热稳定性、吸附性能和孔隙结构进行表征.结果表明:预处理后的...     

晶化条件对合成亚微米NaA分子筛的影响

以硅溶胶为硅源、偏铝酸钠为铝源,通过水热合成法制备亚微米NaA分子筛,探究晶化条件对合成NaA分子筛的影响。采用X射线衍射(XRD)、扫描电镜(SEM)分析手段表征合成样品的物相、结晶度、形貌和粒径大小。结果表明:在碱度为n(H_2O)/n(Na_2O)=30,30℃陈化24h条件下,最佳的晶化温度为100℃,晶化时间为1h,在最佳条件下合成的A型分子筛晶型完整、粒度分布均匀、粒径为300~500nm。     

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.     

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.     

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.     

Many Drugs of Abuse May Be Acutely Transformed to Dopamine,Norepinephrine and Epinephrine In Vivo

It is well established that a wide range of drugs of abuse acutely boost the signaling of the sympathetic nervous system and the hypothalamic–pituitary–adrenal (HPA) axis, where norepinephrine and epinephrine are major output molecules. This stimulatory effect is accompanied by such symptoms as elevated heart rate and blood pressure, more rapid breathing, increased body temperature and sweating, and pupillary dilation, as well as the intoxicating or euphoric subjective properties of the drug. While many drugs of abuse are thought to achieve their intoxicating effects by modulating the monoaminergic neurotransmitter systems (i.e., serotonin, norepinephrine, dopamine) by binding to these receptors or otherwise affecting their synaptic signaling, this paper puts forth the hypothesis that many of these drugs are actually acutely converted to catecholamines (dopamine, norepinephrine, epinephrine) in vivo, in addition to transformation to their known metabolites. In this manner, a range of stimulants, opioids, and psychedelics (as well as alcohol) may partially achieve their intoxicating properties, as well as side effects, due to this putative transformation to catecholamines. If this hypothesis is correct, it would alter our understanding of the basic biosynthetic pathways for generating these important signaling molecules, while also modifying our view of the neural substrates underlying substance abuse and dependence, including psychological stress-induced relapse. Importantly, there is a direct way to test the overarching hypothesis: administer (either centrally or peripherally) stable isotope versions of these drugs to model organisms such as rodents (or even to humans) and then use liquid chromatography-mass spectrometry to determine if the labeled drug is converted to labeled catecholamines in brain, blood plasma, or urine samples.     

Novel polyurethane coating technology through glycidyl carbamate chemistry

Glycidyl carbamate chemistry combines the excellent properties of polyurethanes with the crosslinking chemistry of epoxy resins. Glycidyl carbamate functional oligomers were synthesized by the reaction of polyfunctional isocyanate oligomers and glycidol. The oligomers were formulated into coatings with several amine functional crosslinkers at varying stoichiometric ratios and cured at different temperatures. Properties such as solvent resistance, hardness, and impact resistance were dependent on the composition and cure conditions. Most coatings had an excellent combination of properties. Studies were carried out to determine the kinetics of the curing reaction of the glycidyl carbamate functional oligomers with multifunctional and model amines. Detailed kinetic analysis of the curing reactions was also undertaken. The results indicated that the glycidyl carbamate functional group is more reactive than a glycidyl ether group. Presented at the 82nd Annual Meeting of the Federation of Societies for Coatings Technology, on October 27–29, 2004, in Chicago, IL.