MCM-41介孔分子筛的合成及其对铜离子的吸附性能简

以微硅粉为硅源,CTAB和PEG-6000为模板剂,合成MCM-41介孔分子筛。采用XRD、N₂吸附-脱附曲线、FTIR以及TEM表征了其结构、比表面积、孔径分布及晶体形貌,并且以该样品为吸附剂,对含Cu²⁺的溶液进行了静态吸附实验。结果表明,以微硅粉为硅源成功合成了具有典型六方排列孔道结构的MCM-41,其比表面积为869.5 m²/g,孔容为0.97 cm³/g,平均孔径为3.3 nm;溶液pH为5~6时,MCM-41对Cu²⁺的去除效果最好;MCM-41对Cu²⁺的最大吸附吸附容量36.3 mg/g;MCM-41对Cu²⁺的吸附性能符合Langmuir吸附方程的特征。动力学研究表明,该过程符合准二级动力学模型。     

磷酸微波活化多孔生物质炭对亚甲基蓝的吸附特性

以甘蔗渣为原料,采用微波辅助H3PO4活化法制备富含含氧酸官能团的中孔生物质炭。通过扫描电子显微镜SEM、傅立叶变换红外光谱FT-IR等技术对生物质炭物理化学性质进行表征,并通过静态实验法,探讨炭样对亚甲基蓝的吸附行为及热力学性质。结果表明,H3PO4活化制备蔗渣生物质炭的适宜条件为浸渍比1：1,烘干时间10h,活化功率900W,活化时间22min,在此条件下制得的生物质炭得率为39．2％,碘值为817mg／g,亚甲基蓝值为229mg／g,为国家一级品标准的1．7倍。红外光谱分析表明,炭样表面以羟基、羰基、羧基等酸性官能团为主。静态吸附实验表明,Freundlich方程与Redlich—Peterson方程能较好地描述等温吸附行为,表现为优惠吸附。热力学研究表明,吸附吉布斯自由能（△G0）〈0,说明吸附反应是自发过程,而吸附标准焓变（△H0）〉70KJ／mol,表明亚甲基蓝在制备炭样上的吸附是吸热反应,升温有利于吸附,且化学反应在吸附过程中发挥了重要作用。     

Hydrothermal liquefaction phase behavior of microalgae & model compounds in fused silica capillary reactor

A fused silica capillary reactor combined with a heating/cooling stage, a microscope and a digital camera were used to investigate phase behavior during the hydrothermal liquefaction of microalgae (Dunaliella tertiolecta) and model compounds, including soya protein and glycine, starch, glucose and xylose, stearic acid and palmitic acid. Bubbles were generated at 246°C and disappeared at 360°C upon heating when Dunaliella tertiolecta used as feedstocks. Moreover, liquid products were generated at 300°C upon heating and oily liquid products began to separate out at 250°C upon cooling. The phase behavior of soya protein was similar to that of the Dunaliella tertiolecta. Meanwhile, there only observed the bubbles generation during hydrothermal liquefaction of glycine. Heating the starch, glucose and xylose above 350°C generated black solids from carbonization. Stearic acid and palmitic acid only had the process of melting, dissolution, dispersion and precipitation.     

二乙烯三胺改性聚多巴胺包覆硅胶吸附日落黄

采用二乙烯三胺(DETA)改性聚多巴胺(PDA)包覆硅胶(SG)得到吸附剂SG@DETA/PDA。通过FTIR、SEM和氮气吸附-脱附等技术对SG@DETA/PDA进行了形貌和结构表征,并考察了其对阴离子染料日落黄的吸附性能。表征结果显示,SG@DETA/PDA表面有PDA微球团聚形成的较为致密的包覆层,其比表面积和孔体积均比吸附剂SG@PDA有小幅提高。实验结果表明:SG@DETA/PDA吸附日落黄的最佳工艺条件为溶液p H 2.0、吸附时间2.0 h、初始染料质量浓度150 mg/L,在上述最佳工艺条件及298 K温度条件下SG@DETA/PDA对日落黄的吸附容量为175.56 mg/g。SG@DETA/PDA吸附日落黄的过程可以分别用准二级动力学方程和Langmuir等温吸附方程很好地拟合,该吸附过程主要是通过静电作用的单分子层吸附,是一个吸热自发的熵增过程。     

An impingement plate method to detect deposits of pyrethroid insecticides

Abstract

A silica gel impingement plate for monitoring pyrethroid deposits in environmentally sensitive areas is described. The plate is simple, commercially available, and inexpensive. A residue analysis method is given for deltamethrin deposits with 83.3% mean recovery and a minimum quantifiable limit of 0.005 μg/plate. Pyrethroid deposits are strongly adsorbed to the silica gel, which prevents wash‐off by rainfall and slows photodegradation. In two field experiments, deltamethrin was readily detected 3 weeks after direct spray applications at 6 and 10 g ai/ha. Deltamethrin dissipation on the plates was first‐order with a half‐life of 2.9 ‐ 3.7 d. Photoisomers of deltamethrin were also detected on the plates and the ratio of photoisomers to deltamethrin increased over time. This ratio will indicate the age of deposits in monitoring situations.     

植物根瘤内痕量Frankia DNA的提取及鉴定

建立了一种简捷、快速植物根瘤内痕量Frankia DNA的提取方法,即采集自然态下根瘤,剥离瘤瓣,取瘤瓣尖经液氮研主民粉末,以20g/L CTAB（十六烷基三甲基溴化铵）消化胞壁,然后以d=5-10μm的石英粉吸附DNA,再以无菌去离子蒸馏水释放DNA,所获DNA产率及纯度较酚／氯仿法好。经对辽宁沙棘、色赤杨根瘤的瘤内痕量Frankia DNA及体外培养的9种Frankia菌株DNA分纯,并用于酶切及PCR,获满意结果。图3参12     

固相萃取-GC/MS法测定地表水中3-甲基吲哚

采用微球硅胶键合C_(18)固相萃取柱萃取水样中的3-甲基吲哚,并用气质联用法测定,方法在0 mg/L~10.0 mg/L范围内线性良好,方法检出限为0.2μg/L。空白水样3个质量浓度水平的加标回收率为89%~94%,7次测定结果的RSD为2.3%~6.9%。用该方法测定7个实际地表水样品,其中4个地表水样品检出3-甲基吲哚,地表水样的加标回收率为81.5%~97.0%。     

红外光谱法测定粉尘中游离二氧化硅综述

全面地回顾了国内外红外光谱法测定粉尘中游离二氧化硅的研究成果。系统而重点地介绍了溴化钾压片法、粉尘滤膜样品重沉积和采样滤膜直接测定技术,分析了样品粒度、标准石英物质和矿物干扰物对测定结果的影响及干扰消除方法;还介绍了国外对红外光谱法与Ｘ－射线衍射法进行比较性研究的结果和动态,并得出结论。文章所列参考文献对本领域研究人员和基层检测人员具有很高的参考价值。     

Adsorptive removal of resorcinol on a novel ordered mesoporous carbon (OMC) employing COK-19 silica scaffold: Kinetics and equilibrium study

Phenolic compounds and their derivatives have been found in industrial wastewater, which pose threats to the natural environment. Ordered mesoporous carbon(OMC) has been identified as an ideal adsorbent possessing high specific surface area and large pore volume to alleviate these pollutants. A novel ordered mesoporous carbon was prepared using COK-19 template with the cubic Fm3 m structure for the first time. Ordered mesoporous silica COK-19 was synthesized and reported in 2015. Sucrose as the carbon precursor was impregnated into the mesopores of silica and converted to carbon through carbonization process using sulfuric acid as a catalyst. Ordered mesoporous carbon was obtained after the removal of silica framework using hydrofluoric acid. Boric acid was employed for the preparation of OMCs with tunable pore sizes in the range of 6.9–16.6 nm. Several characterization techniques such as nitrogen adsorption–desorption isotherms, transmission electron microscope(TEM), Fourier transform infrared spectroscopy, Boehm titration and elemental analysis were employed to characterize the OMCs. The pore size analysis and TEM images confirmed that OMC has replicated the mesostructure of the COK-19. Results obtained from adsorption kinetics and isotherms suggest that the Pseudo-second-order model and Langmuir isotherm well described the experimental data.     

氯化钠/纳米疏水二氧化硅超细干粉制备及灭火性能研究

选用氯化钠为基体制备金属火灾超细干粉灭火剂。应用反溶剂法对其改性,使纳米疏水二氧化硅吸附在氯化钠晶体表面,其中分散剂为PEG-1000。结果表明,纳米疏水二氧化硅的添加有利于细化氯化钠颗粒,但过量的添加会起反作用,最佳用量为3 wt%左右,平均粒径为2.18μm。镁片灭火实验证明超细复合干粉的灭火性能明显好于传统氯化钠灭火剂(商用D类灭火剂),纳米疏水二氧化硅最佳添加量为3 wt%,此时灭火时间仅需传统灭火剂的一半。最后利用FDS5.0模拟干粉颗粒与燃烧火焰作用过程,模拟结果表明干粉覆盖对火焰具有一定的抑制效果,并分析了复合干粉灭火机理。