高分子材料导热性能影响因素研究进展

介绍了高分子材料导热性能影响因素研究进展，重点阐释了聚合物基体的结构特性（链结构、分子间相互作用、取向、结晶度等）、导热填料（种类、含量、形态、尺寸等）以及制备方法等对高分子材料导热性能的影响。     

Preparation of faceted TaN grains by heating Ta-containing oxides in BN crucible with Na

Single-crystal grains of TaN were synthesized by heating Ta₂O₅, FeTa₂O₆, or FeTaO₄ in a BN crucible together with Na metal in an Ar atmosphere at 1100 °C. The BN crucible acted a solid source of nitrogen. Aggregates of columnar ε-TaN single crystals 10–150 μm in size were formed on the inner wall of the BN crucible when either Ta₂O₅ or FeTa₂O₆ was used. On the other hand, platelet-like single crystals of θ-TaN 1–50 μm in size were obtained from FeTaO₄. The results of wavelength-dispersive X-ray spectrometry indicated that the compositions of the ε-TaN and θ-TaN crystals were close to the stoichiometric ideal.     

The effects of washing a collagen sample prior to TEM examination

Transmission electron microscopy (TEM) is an important analysis technique to visualize (bio)macromolecules and their assemblies, including collagen fibers. Many protocols for TEM sample preparation of collagen involve one or more washing steps to remove excess salts from the dispersion that could hamper analysis when dried on a TEM grid. Such protocols are not standardized and washing times as well as washing solvents vary from procedure to procedure, with each research group typically having their own protocol. Here, we investigate the influence of washing with water, ethanol, but also methanol and 2-propanol, for both mineralized and unmineralized collagen samples via a protocol based on centrifugation. Washing with water maintains the hydrated collagen structure and the characteristic banding pattern can be clearly observed. Conversely, washing with ethanol results in dehydration of the fibrils, often leading to aggregation of the fibers and a less obvious banding pattern, already within 1 min of ethanol exposure. As we show, this process is fully reversible. Similar observations were made for methanol and propanol. Based on these results, a standardized washing protocol for collagenous samples is proposed.     

Laser-assisted preparation of monolithic acidic catalysts for biomass conversion

5-(Hydroxymethyl)furfural (5-HMF) is a vital platform molecule from which a variety of high-value-added fine chemicals and polymerizable monomers can be prepared. The use of solid acids to catalyze the conversion of biomass into 5-HMF is environmentally friendly and economical. However, exploiting the high yield of 5-HMF in a highly concentrated reactant system is challenging. Herein, we present a laser-assisted method for preparing highly acidic monolithic acidic catalysts. A monolithic acidic catalyst based on metal Zr sheets was synthesized and used to catalytically convert 30 wt% fructose into 5-HMF (conversion rate: 96%; yield: 95%). The catalyst was immediately separated from the reaction solution by direct removal at the end of the reaction. Catalytic efficiency was largely unaffected after 10 cycles of use, and the same catalytic efficiency was observed after laser-regeneration, highlighting the potential industrial applicability of the developed catalyst.     

海洋非成岩天然气水合物原位快速制备实验及评价

我国的海洋天然气水合物（以下简称水合物）资源主要分布在沿海大陆架水深介于300～3 000 m的深水区，具有弱胶结、非成岩的特征，为了测试和研究该类型水合物必须原位、大量、快速制备样品，而目前常用的搅拌法、喷淋法、鼓泡法等制备技术却存在着生成速度慢、储气密度低等问题。为此，自主设计、研制了1 062 L非成岩水合物快速制备釜，针对我国南海非成岩水合物的物性特征，开展了搅拌法、鼓泡法、喷淋法单一制备方法及“三合一”法（上述3种方法相结合）水合物制备实验，测试了实验过程中温度、压力、电阻率及反应时间等数据，分析比较了几种不同制备方法的水合物生成情况与制备效率。实验结果表明：①搅拌法、鼓泡法、喷淋法制备水合物过程中，生成的水合物均缓慢增加并逐渐铺满整个液面；②搅拌法制备过程中可以观测到明显的诱导期，而喷淋法、鼓泡法及“三合一”法却无明显的诱导期；③单一制备方法及“三合一”法制备水合物过程中，电阻率均随反应时间的增加而增加，其变化趋势亦与水合物制备速率基本一致；④“三合一”法的制备周期明显短于单一制备方法（搅拌法、喷淋法、鼓泡法单一方法的制备时间分别约为“三合一”法的5.14倍、3.59倍、3.16倍）。结论认为，所研制的1 062 L水合物快速制备釜能够实现海洋非成岩水合物样品的原位、快速制备；较之于单一制备方法，“三合一”法大大提高了水合物的制备效率。     

五味子泡腾片的制备工艺及质量评价

研究五味子泡腾片的制备工艺,并对其进行质量评价。以崩解时限、产气量、pH值为评价指标,采用单因素和正交试验优化泡腾崩解剂配比、泡腾崩解剂质量分数、聚乙二醇(polyethylene glycol,PEG)6000的用量,并通过片剂重量差异、崩解时限、pH值、产气量、硬度及脆碎度和五味子醇甲的含量对产品进行质量控制。结果表明,柠檬酸∶碳酸氢钠最佳配比为1∶0.7(质量比),泡腾崩解剂的最佳质量分数为55%,五味子水提物浸膏质量分数26%,PEG 6000的最佳质量分数为5%,甜菊糖苷2%,氯化钠2%,乳糖10%。最优工艺条件下制备的泡腾片,外表呈浅粉色,片剂表面光滑,可迅速溶于水中,产生丰富气泡,汤色呈浅粉色,并伴有五味子特有香气,口味酸甜适中,口感良好,每片泡腾片中五味子醇甲的含量为(9.79±0.18)mg,平均片重(500±20)mg,崩解时限为(87.42±1.91)s,pH值平均值为4.63±0.071,崩解时限、pH值均符合药典规定。     

花状与颗粒状NiMn2O4纳米材料的制备及其超级电容性能

分别以尿素和氨水为沉淀剂，采用热溶剂法制备了多孔的花状NiMn₂O₄和颗粒状NiMn₂O₄纳米电极材料，采用 X射线衍射仪、扫描电镜、透射电镜和N₂ 吸附-脱附等手段对NiMn₂O₄材料的物相、形貌结构和孔径分布进行了表征，并通过循环伏安、恒电流充放电、交流阻抗等方法测试了所制备材料的电化学性能。研究了沉淀剂对NiMn₂O₄材料形貌、微观结构及电化学性能的影响。结果表明：以尿素为沉淀剂的NiMn₂O₄是由纳米片组成的花状结构，纳米片厚度为50～60nm，比表面积为104m²/g。在 1A/g 电流密度下比电容为1614F/g，在5A/g电流密度下，尿素为沉淀剂的花状NiMn₂O₄材料经1000次恒电流充放电后其比电容可达初始值的89%。以氨水为沉淀剂的多孔NiMn₂O₄为直径约30nm的纳米颗粒结构，颗粒间团聚严重，比表面积为91m²/g。在1A/g电流密度下比电容为1147F/g，在5A/g电流密度下，氨水为沉淀剂的颗粒状NiMn₂O₄材料经1000次恒电流充放电后其比电容可达初始值的80%。尿素为沉淀剂的花状NiMn₂O₄具有优越的超级电容性能。     

提高新疆准东露天煤成浆性的实验研究

为提高准东露天煤的成浆性能,利用宽沟煤、乌东煤、北山煤、黑山煤、红沙泉煤5种煤与准东露天煤进行了混合制浆实验,考察了各单种煤的成浆性能以及单种煤最高成浆浓度条件下混合制浆的煤浆性能。单一准东露天煤浆的成浆性研究表明:准东露天煤单独制浆时,在添加剂添加率3‰下,煤浆最高质量分数为47%,黏度650 mPa·s,但煤浆流动性和稳定性一般。与不同种煤混合制浆研究表明:准东露天煤与宽沟煤、黑山煤容易混合成浆,煤浆的浓度、流动性、稳定性均有明显提高;在准东露天煤与宽沟煤、黑山煤质量比5∶5时,煤浆质量分数可达57%,可满足水煤浆气化炉生产对煤浆的要求。     

不同粒度纳米碳酸钙的可控制备

不同粒度的纳米碳酸钙具有不同的特性和应用范围,目前不同粒度纳米碳酸钙的可控制备方法还未见报道。以氯化钙、碳酸铵为原料,以乙醇、柠檬酸和焦磷酸钠为分散剂,采用复分解法研究了不同制备条件对纳米碳酸钙粒径的影响规律,在此基础上制备出平均粒径为17~71 nm的碳酸钙,并对其进行了表征。实验结果表明,所制备的纳米碳酸钙均为球霰石型,纯度很高,而且形貌近似球形。制备条件对纳米碳酸钙的粒径有显著的影响：随着反应温度升高,纳米碳酸钙的粒径减小;随着氯化钙滴加时间的增加,纳米碳酸钙的粒径增大;随着反应物浓度的提高,纳米碳酸钙的粒径先减小后增大;当分散剂为柠檬酸和焦磷酸钠的混合溶液时所得纳米碳酸钙的粒径最小,当分散剂为乙醇和焦磷酸钠的混合溶液时所得纳米碳酸钙的粒径最大。利用这些影响规律通过控制制备条件可以实现所需粒径纳米碳酸钙的可控制备。