水热沉淀法制备TiO2纳米粉体的研究

以Ti(SO4)2水溶液为前驱物,尿素为沉淀剂,采用水热沉淀法制备TiO2纳米粉体.利用XRD、TEM、DTA等分析测试手段对所得TiO2粉体的晶相组成、晶体形貌等性质进行了研究,讨论了晶粒尺寸与前驱物摩尔比、反应温度、保温时间之间的关系.结果表明,前驱物摩尔比为1∶2～1∶4,在140～200℃保温2～6h的水热条件下,可制得粒径为十几纳米的锐钛矿型TiO2晶体.实验得出,随着前驱物摩尔比减少、反应温度升高、保温时间延长,晶体粒径增大.     

纳米羟基磷灰石的超声波辅助水热合成及其表征

以CaCO3和Ca(H2PO4)2.H2O[钙磷比n(Ca)/n(P)=1.67]的混合物为前驱体,在超声波辅助下,水热法制备了纳米羟基磷灰石(n-HAP)。利用X射线衍射仪、透射电子显微镜、傅里叶红外吸收光谱仪对其进行了表征。分析了pH值、反应温度、水热合成时间以及超声波频率等对羟基磷灰石纳米晶体结构和形貌的影响。结果表明,随着水热合成温度的提高、时间的延长,有利于n-HAP晶体发育完整;提高前驱物pH值可以显著促使产物粒径变小,当水热合成温度为200°C,反应时间8 h,pH=11时,n-HAP为横向尺寸在40~50 nm的六方柱状晶体。红外谱图分析表明,有少量的CO32-进入n-HAP晶体,此种方法制备的羟基磷灰石在结晶形态、组成、结构上更与人骨接近,更适合作为生物医学材料。     

开放水热法制备莫来石复相纳米晶体的影响因素

以天然高岭土为原料,经精细化处理煅烧制备莫来石.用常压、开放水热技术制备出莫来石复相纳米晶体材料.实验表明:常压、开放水热条件下制备莫来石复相纳米晶粉体的水热反应中,采用质量比为m(Na2O)/m(SiO2)=2.8,m(H2O)/m(Na2O)=35～30,0～80℃控温升温1 h,在80℃保温2 h,可制备出尺寸为80～100 nm莫来石复相纳米晶体.所制备的莫来石纳米晶体的水热溶液相变驱动力△μ为(3.609～4.672)×10-20 J/mol;水热体系溶解度控制在3.891×10-6 mol/L;熔解热△E为18.846 kJ/mol;晶体生长速率常数选择0.85～0.92,有利于快速成核和晶体生长,并且可以很好地控制晶体尺寸和分散度.     

加压水溶液法制备工艺对α型高强石膏性能的影响

采用加压水溶液法以脱硫石膏为原料制备高强石膏,其工艺参数是决定高强石膏制备品质的关键。通过研究水热温度、水热时间、搅拌转速及料浆浓度四种工艺参数对α型高强石膏性能的影响规律,对不同工艺参数下制备样品的晶体形貌和石膏相组成进行定性及定量分析,并优化出加压水溶液法制备α型高强石膏的最佳工艺。结果表明,水热温度对生成晶体的尺寸及长径比的影响较大,水热时间主要影响晶体的尺寸,对长径比的影响不大,而水热温度和水热时间是影响α型高强石膏相组成的重要因素。搅拌转速和料浆浓度主要影响高强石膏尺寸及长径比,对石膏相组成影响不大。在最佳工艺条件下:水热温度130 ℃、水热时间4 h、搅拌转速250 r/min及料浆浓度30%(质量分数),制备的α型高强石膏2 h抗折强度为5.4 MPa,烘干抗压强度为41.9 MPa。     

水热碱蚀与碱溶滤联合处理制备介孔丝光沸石

以硅酸钠溶胶和铝酸钠为硅、铝源,采用水热合成和离子交换法制备了质子型丝光沸石(H-MOR)。研究水热碱蚀与碱溶滤联合处理对H-MOR改性样品的介孔结构、晶体形貌、组成及酸性质的影响。结果表明:用初始浸渍液对H-MOR进行水热碱蚀,H-MOR骨架脱硅选择性高,晶体含有均一的筛状介孔;水热碱蚀与一次碱溶滤处理的样品具有尺度分布较窄的槽形介孔,沸石骨架硅铝比降低而介孔率增加;再度进行碱溶滤处理,沸石的最可几介孔尺寸和累计介孔体积进一步增大,而残留抽出物(无定形SiO2–Al2O3)的硅铝比为生成介孔丝光沸石晶相的5倍以上。联合碱处理的丝光沸石样品具有骨架脱硅选择性和介孔率高、介孔分布(4.4~5.7nm)可控的特性,其结晶度、固有微孔结构和酸性质退化程度较低。     

水热法改性工业级Mg（OH）2晶体形貌研究

以工业级Mg（OH）2为原料,应用水热技术对Mg（OH）2晶体形貌和颗粒尺寸进行改性。考察了水、乙醇和尿素3种水热溶剂对Mg（OH）2晶体的影响。通过扫描电镜（SEM）表征可知,3种水热溶剂在一定程度上都可以改善工业级薄片状Mg（OH）2晶体的形貌和团聚状态。尤其是尿素对Mg（OH）2改性效果最为明显,在250℃下改性可以得到尺寸在10μm．形貌非常规整的立方体晶体。     

高碱度水热条件下方沸石的合成机理及动力学

以偏铝酸钠为铝源、硅酸钠为硅源、氢氧化钠为矿化剂、四乙基氢氧化铵为模板剂,在高碱度水热条件下合成了方沸石晶体。采用X射线衍射仪(XRD)和扫描电子显微镜(SEM)对合成产物的物相组成和微观形貌进行了表征,并对方沸石晶体的合成机制进行了探讨。利用等温相变动力学原理研究了方沸石晶体生长动力学。结果表明,在180℃下随着反应时间的增加,水热产物的结晶度逐渐增强;水热合成方沸石晶体的Avrami指数n=1.59,说明晶体的形成反应主要以溶解沉淀机制进行。     

以多孔炭为模板合成中空介孔丝光沸石

以多孔炭为模板,水热条件下首次合成了具有中空结构的介孔丝光沸石.采用X-射线衍射(XRD)、扫描电镜(SEM)、透射电镜(TEM)、N2物理吸附/脱附等测试手段对合成的样品进行了表征.结果表明,制备的新型材料为具有规则六棱柱外貌的中空介孔丝光沸石,晶体的内腔尺寸约为8 μm,晶体的壁厚约为1 μm,且晶体壁中存在大量尺寸约为9.0 nm的介孔.     

TlBr粉末的水热重结晶提纯和TlBr晶体生长(英文)

采用水热重结晶法提纯TlBr,用等离子耦合质谱仪检测痕量杂质。结果表明:水热重结晶法是一种有效的TlBr提纯方法,经一次水热重结晶提纯后,杂质Ca,Fe,Mg,K,Zn,Cu,Na和Si的总浓度从139.6×10–6(质量分数,下同)下降为9.3×10–6;随着溶液冷却速率的下降,杂质含量下降幅度明显增大。对比真空蒸馏提纯法,水热重结晶法具有更高的提纯效率。以水热重结晶制备的TlBr粉为原料,采用垂直Bridgman法生长了尺寸为φ8mm×55mm的TlBr晶体。TlBr晶体的禁带能为(2.83±0.005)eV,电阻率为2.26×1011(Ω·cm)。     

KTP晶体的水热法生长与形貌研究

以K2HPO4、KH2PO4、H2O2的混合水溶液为矿化剂,以熔盐法生长的KTP为培养料,采用水热法,生长出了尺寸为24mm×14mm×60mm(a×b×c)磷酸钛氧钾(KTP)晶体.分析了水热条件下KTP晶体的形貌和结晶习性,并对(100)面上出现高指数面的原因进行了研究.     

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.     

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.