磷石膏制备硫酸钙晶须的初步研究

以磷石膏为原料,直接采用水热法制备硫酸钙晶须,为磷石膏制备硫酸钙晶须的工业化生产提供重要理论依据。实验考察反应温度、料浆初始pH、反应时间、料浆浓度及磷石膏粒度对生成硫酸钙晶须的影响,用扫描电镜观察硫酸钙晶须的形貌,并通过偏光显微镜和图像分析软件分析不同反应条件下制备的硫酸钙晶须的直径和长度。结果表明:反应温度为130~140℃,料浆初始pH为4.0,反应时间为4 h,料浆质量分数为5%,原料粒度为50~75μm是生成硫酸钙晶须的最佳反应条件,在此条件下可制备出平均直径为2μm,长径比为42的硫酸钙晶须产品。     

高纯天然石膏水热法制备硫酸钙晶须研究

以高纯天然石膏为原料，加压水热法制备高品质硫酸钙晶须。采用常规分析方法、XRD和扫描电镜等手段分析和表征石膏原料和硫酸钙晶须产品。结果表明，制备硫酸钙晶须的最优条件为：料浆质量分数为6.0%，转晶剂氯化镁加入量为石膏质量的0.05%，硫酸加入量为水体积的1.0%，反应时间为4.0 h，快速过滤干燥即得硫酸钙晶须产品。分析结果表明：硫酸钙晶须长度最大为280.4 μm，最小为19.59 μm，平均长度为80 μm；硫酸钙晶须直径最大为5.86 μm，最小为0.20 μm，平均直径为2.67 μm；通过统计分析可知，长径比范围为10～80。     

磷石膏水热合成法制备硫酸钙晶须工艺研究

研究了以磷石膏为原料水热合成法制备硫酸钙晶须的工艺条件。结果表明,最佳工艺条件为磷石膏占总物料的质量分数为3.0%、反应体系p H 4.0、反应温度135℃、反应时间3.0 h;该条件下,硫酸钙晶须外观形貌规整,分散均匀,平均白度为96.99%,平均直径为0.15μm,平均长径比为63.89;用所得硫酸钙晶须制得的晶须纸性能优异。     

脱硫石膏制备硫酸钙晶须的试验研究

以脱硫石膏为原料通过水热合成法制备硫酸钙晶须,借助X射线衍射仪、扫描电子显微镜、能谱仪、热重分析仪等测试手段进行分析,研究了酸化预处理、料浆浓度以及反应温度对制备硫酸钙晶须的影响。结果表明:酸化预处理可以有效去除原料中的CaCO₃杂质;随着料浆浓度和反应温度的增加,晶须长径比均呈现先增大后减小的趋势;当料浆浓度为3%(质量分数),pH值为6.5,反应温度为120 ℃,反应时间为2 h时,取得的硫酸钙晶须最佳平均长度为161.2 μm,最佳平均长径比为46.06。     

不同固液比和原料粒度对脱硫石膏制备硫酸钙晶须的影响

以脱硫石膏为原料。采用水热法工艺制备硫酸钙晶须。并借助XRD、高分辨显微镜等分析方法,深入探讨了不同固液比和原料粒度对硫酸钙晶须生长行为的影响。结果表明：随着固液比的不断减小,硫酸钙晶须的长径比呈先升高后降低的趋势;当固液比为1：10时,长径比达到最大,其值为68．65;随着原料粒度的减小．硫酸钙晶须的直径不断减小,硫酸钙晶须的长径比不断增加,当原料粒度为1．60μm时,长径比达到68.65。     

磷石膏制备硫酸钙晶须的条件研究

磷石膏是湿法制备磷酸过程中产生的固体废渣,既会对环境产生污染,又会造成资源浪费。为提高废料磷石膏的综合利用价值,研究了以磷石膏原料制备硫酸钙晶须,考察了原料预处理、料浆浓度、晶型助长剂和pH对硫酸钙晶须产率和形貌的影响。用扫描电镜（SEM）、图像颗粒分析显微镜和X射线衍射（XRD）对产品进行观察和检测。结果表明, 通过原料的预处理,可得到最佳反应条件：料浆质量分数为2%、采用硫酸镁为晶型助长剂、pH为3。在此条件下,晶须产率可达36.4%,平均长径比可达60,产品为半水硫酸钙晶须。     

磷石膏制备硫酸钙晶须的研究

随着我国磷复肥的发展,磷石膏的产量逐年增多,综合利用面临严重挑战。以磷石膏为原料,采用酸结晶提取法制备硫酸钙晶须,考察反应温度、盐酸浓度、反应时间、液固质量比等因素对生成硫酸钙晶须的影响,用扫描电镜观察硫酸钙晶须的形貌,并分析了硫酸钙晶须的物理及化学特性。结果表明,生成硫酸钙晶须的最佳反应条件为反应温度80℃、盐酸w(H~+)0.20%~0.22%、液固质量比20、反应时间30 min,在此条件下可制备出平均直径为1~4μm,长径比为40~120的硫酸钙晶须产品,满足造纸及填料用要求。     

制盐废石膏制备硫酸钙晶须

以制盐废石膏为原料采用水热法制备硫酸钙晶须,研究了料浆浓度、反应温度、反应时间、晶型助长剂氯化镁用量以及pH值对硫酸钙晶须收率和形态的影响。结果表明,较佳反应条件为：料浆浓度为15．0％,140℃下反应8h,反应体系的pH值=3。在此条件下,收率可达54．2％,平均长径比为55。     

杂质对硝基磷石膏制备硫酸钙晶须形貌的影响

以硝基磷石膏为原料,通过加压水热法制备硫酸钙晶须,探讨磷、氟、氮等杂质对硫酸钙晶须生长过程的影响,分析杂质对晶须微观形貌及长径比的影响,并通过X射线衍射分析杂质对晶须生长过程的影响。结果表明:可溶性氟化钠、不溶性氟化钙对硫酸钙晶须的生长均具有明显的抑制作用,随着药剂用量的增加,长径比明显变小,且团聚严重;磷酸三钠对硫酸钙晶须的生长具有明显细化作用,当磷酸三钠用量为2%时,磷酸钙晶须平均直径为1.8μm;硝酸钠对硫酸钙晶须的生长影响不大。     

页岩提钒中和渣制备硫酸钙晶须填料的研究

以页岩提钒中和渣为原料,采用水热法制备硫酸钙晶须,并进行稳定-改性处理,最终制备用于填充塑料的硫酸钙晶须填料。研究了反应温度、反应时间、料浆浓度及助晶剂用量对硫酸钙晶须长径比的影响以及改性剂用量、初始料浆浓度、改性温度及改性时间对硫酸钙晶须改性效果的影响。结果表明,在反应温度为130℃、反应时间为6 h、料浆质量分数为3%、助晶剂六水氯化镁用量为10%的条件下,制备出的硫酸钙晶须长径比达90,但晶须在空气中易水化变粗,长径比降至20以下。在硬脂酸用量为4%、初始料浆质量分数为8%、改性温度为90℃、改性时间为20 min的条件下,制备的硫酸钙晶须填料活性指数达0.72,吸油值为0.278 8 g/g,制得的硫酸钙晶须填料呈棒状或纤维状,表面光滑,结晶度较好,长径比稳定在40~50。结合XRD、SEM、FT-IR分析可知,硬脂酸能有效抑制晶须水化过程,保持晶须晶型及形貌稳定,硬脂酸通过与晶须表面发生化学键链接封闭其亲水活性点而抑制晶须水化。     

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.     

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.     

Highly moisture-proof polysilsesquioxane coating prepared via facile sol-gel process

A highly moisture-proof polysilsesquioxane coating was obtained from a new bis-silylated precursor, which was synthesized from 3-aminopropyltriethoxysilane (APTES) and m-xylylene diisocyanate (m-XDI) in tetrahydrofuran (THF) and verified by ¹H MAS NMR. For direct comparison purposes, an SiO₂ coating was also prepared by the Stöber method using tetraethoxysilane (TEOS) as the reactant. Interestingly, the coating obtained from the polysilsesquioxane sol exhibited a much higher moisture resistance capability than its counterpart, which was attributed to its more compact feature between nanoparticles as characterized by N₂ absorption experiment and transmission electron microscopy (TEM). Furthermore, its high transparency of about 92% showed potential for application in the protection of optical crystals.