Synthesis of Ultrafine SiC Powders from Carbon-Silica Hybridized Precursors with Carbothermic Reduction

Inorganic-organic hybrid gels were prepared by simultaneous condensation of the liquid mixture of ethyl silicate, ethyl borate and water soluble phenol resin with low molecular weight. The liquid mixtures were changed into lightly colored transparent gels after a catalyst addition and stirring. The obtained gels were crushed, dried and fired in controlled conditions to yield the inorganic precursors. Since the tailored inorganic precursors mainly consisted of SiO2 and carbon, silicon carbide was formed with the heat treatments in an Ar atmosphere beyond 1773 K with carbothermic reduction. The properties and morphology of the formed silicon carbide powders in terms of the starting precursor compositions and the conditions of the carbothermic reduction were investigated with SEM, XRD and TG-DTA analysis.     

Mechanistic study of thermal behavior and combustion performance of epoxy resins: I homopolymerized TGDDM

Tetraglycidyl 4,4′-diaminodiphenylmethane (TGDDM) undergoes homopolymerization on heating. Intramolecular reactions which compete with crosslinking favor the formation of cyclic structures with increasing thermal and fire resistance of the resin, whereas physical mechanical properties tend to decrease. The mechanism of thermal decomposition of TGDDM is studied by thermogravimetry, differential scanning calorimetry and thermal volatilization analysis with characterization of volatiles evolved and residue left. Thermal degradation of poly-(TGDDM) starts at 260°C with elimination of water from secondary alcoholic groups which is a typical pathway for epoxy resin degradation. Resulting unsaturations weaken bonds in the β-position and provoke the first chain breaking at allyl–amine and allyl–either bonds. With increasing temperature, saturated alkyl–ether bonds and alkyl carbon–carbon bonds are broken first, followed by the most stable alkyl–aryl bonds at T>365°C. The combustion performance of TGDDM is discussed on the basis of the thermal degradation behavior.     

A straightforward preparation of a polystyrene thiol resin

A mild and efficient two-step synthesis of a polystyrene thiol resin is reported. Firstly, a polystyrene resin was reacted with an activated sulfoxide to afford the resin bound bis-(2-methoxy-carbonylethyl)-sulfonium trifluoromethanesulfonate. Smooth β-elimination based dealkylations afforded the polystyrene thiol resin with good and controlled loading. Its reactivity was assessed through a derivatisation step.     

电迁移微离子色谱及其应用

本文提出一种新型的离子色谱方法,采用恒电流电场代替机械泵输送离子,研制出体积小、重量轻、成本低、易操作的电迁移微离子色谱仪,并检测了几种常见的阴离子,Cl~-、Br~-、NO_2~-的检测极限为10~(-11)～10~(-12)mol,峰高和保留时间重现性相对标准偏差均<3％,进样量与峰高的线性关系良好。     

配糖蛋白B—阳离子丙烯酸树脂微胶囊的性能研究

本文研究了配糖蛋白B-阳离子丙烯酸树脂微胶囊的形态、粒径及粒径分布,并在模拟胃液的酸性缓冲液中进行了微胶囊的溶解释放试验。结果表明该微胶囊能溶于人体的胃液中,可配制适合儿童口服的混悬剂。     

Functionalization of chitosan with 3-nitro-4-amino benzoic acid moiety and its application to the collection/concentration of molybdenum in environmental water samples

A chitosan resin functionalized with 3-nitro-4-amino benzoic acid moiety (CCTS-NABA resin) was newly synthesized for the collection/concentration of trace molybdenum by using cross-linked chitosan (CCTS) as base material. The carboxyl group of the moiety was chemically attached to amino group of cross-linked chitosan through amide bond formation. The adsorption behavior of molybdenum as well as other 60 elements on the resin was examined by passing the sample solutions through a mini-column packed with the resin. After the elution of the elements collected on the resin with 1 M HNO₃, the eluates were analyzed by inductively coupled plasma-mass spectrometry (ICP-MS) and atomic emission spectrometry (ICP-AES).

The CCTS-NABA resin can adsorb several metal ions, such as vanadium, gallium, arsenic, selenium, silver, bismuth, thorium, tungsten, tin, tellurium, copper, and molybdenum at appropriate pHs. Among these metal ions, only molybdenum could be adsorbed almost completely on the resin at acidic regions. An excellent selectivity toward molybdenum could be obtained at pH 3–4. The adsorption capacity of CCTS-NABA resin for Mo(VI) was 380 mg g⁻¹ resin. Through the column pretreatment, alkali and alkaline earth metals in river water and seawater samples were successfully removed.

The CCTS-NABA resin was applied to the adsorption/collection of molybdenum in river water and seawater samples. The concentrations of molybdenum in river water samples were found in the range of 0.84 and 0.95 ppb (ng g⁻¹), whereas molybdenum in seawater was about 9 ppb. The validation of the proposed method was carried out by determining molybdenum in the certified reference materials of SLRS-4, CASS-4, and NASS-5 after passing through the CCTS-NABA resin; the results showed good agreement with the certified values.     

纤维素基磁性聚偕胺肟树脂的研究——锌副族金属离子在树脂上的吸附

研究了Ｚｎ２＋、Ｃｄ２＋、和Ｈｇ２＋离子在碱式纤维素基磁性聚偕胺肟树脂（ＢＭＡＯ）上的吸附动力学。结果表明，吸附速度受粒内扩散所控制。测得粒内扩散系数分别是１．２２×１０－４、２．４２×１０－４和３．９０×１０－４ｃｍ２·ｓ－１；Ｈｇ２＋离子在树脂上的吸附行为符合Ｆｒｅｕｎｄｌｉｃｈ和Ｌａｎｇｍｕｉｒ等温吸附方程；浓集因数随Ｈｇ２＋离子浓度降低而上升，有利于从稀溶液中除去Ｈｇ２＋离子。将树脂加至Ｚｎ２＋、Ｃｄ２＋或Ｈｇ２＋离子浓度为５０ｐｐｍ的溶液中，离子去除率分别是９６．１、９９．９和９９．３％。     

弱酸树脂D113对S-腺苷-L-蛋氨酸的交换行为及分离应用研究

考察了S-腺苷-L-蛋氨酸 (S-adenosyl-L-methionine, SAM) 在弱酸树脂争光D113上的静态吸附及分离行为,利用Langmuir等温式对平衡等温线进行了拟合,实验表明,随着pH的提高,平衡交换量增加,提高温度和SAM的初始浓度在一定程度上能促进内扩散过程,利用D113树脂在f 1.7×30.0cm小型柱上从酵母提取液中分离SAM的得率为90%以上,纯度达87%以上。     

PAN-S浸渍树脂富集方波溶出法测定痕量的铅、镉、铜和锌

用1-(2-吡啶偶氮)-2-萘酚-6-磺酸(PAN-S)水溶液处理201×7强碱性阴离子交换树脂,制备了具有PAN-S功能团的浸渍树脂。经过最佳条件选择,在同一水样中,可以同时富集Pb2 、Cu2 、Zn2 、Cd2 。实验结果表明,PAN-S树脂用于痕量元素的分离富集具有交换速度快、易于洗脱、富集倍数大、选择性好等优点。建立了PAN-S树脂富集-分离铅、镉、铜和锌离子的方波溶出法的测定方法,并可用于海水中的测定,结果令人满意。     

树脂吸附法处理3,6-二氯水杨酸生产废水

研究了树脂吸附法处理3,6-二氯水杨酸生产废水的工艺过程。结果表明,NDA-77吸附树脂对该废水具有良好的吸附-脱附效果。经树脂吸附处理,废水中主要有机污染物2,5-二氯苯酚和3,6-二氯水杨酸均得到去除,总有机碳(TOC)由210mg/L降为20mg/L以下,吸附饱和的树脂可采用稀碱液实现完全再生。经吸附处理去除有机物后,废水中含有20%的KCl,可进入工厂现有的KCl隔膜电解装置,用于KOH的生产。