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固定化磺基离子液体催化合成5-羟甲基糠醛研究 被引量:6
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作者 张元元 邓俊辉 +3 位作者 单玉华 周永生 王桂敏 李明时 《高校化学工程学报》 EI CAS CSCD 北大核心 2010年第5期824-829,共6页
对微球硅胶固定化离子液体(IL3)催化果糖脱水合成5-羟甲基糠醛(HMF)进行了研究。以微球硅胶为载体,通过γ-氯丙基三甲氧基硅烷将磺基功能化离子液体-N-磺丙基咪唑盐(IL2)化学键联到其上制得IL3。用液氮吸附、13C-NMR、元素分析及酸度测... 对微球硅胶固定化离子液体(IL3)催化果糖脱水合成5-羟甲基糠醛(HMF)进行了研究。以微球硅胶为载体,通过γ-氯丙基三甲氧基硅烷将磺基功能化离子液体-N-磺丙基咪唑盐(IL2)化学键联到其上制得IL3。用液氮吸附、13C-NMR、元素分析及酸度测定等方法对IL3进行分析与表征,并考察其在果糖脱水合成HMF反应过程中的催化性能。研究结果表明:IL3能有效催化果糖脱水生成HMF。IL2固载量越高,IL3的表面酸度越大、但比表面积和孔体积都下降。当IL2的固载量为45.4%时,所制得的催化剂(45.4-IL3)对果糖脱水生成HMF具有较好的催化性能。过高的反应温度和果糖浓度会使生焦反应加剧,导致HMF收率降低。在115℃、15%~25%(wt)果糖溶液中反应是较合适的,HMF收率维持在80%以上。IL3可方便地循环使用,但随循环使用次数增加,HMF生成速率和收率都呈下降趋势。尤其是催化剂循环使用四次后,HMF收率明显下降,是反应过程中生成的不溶性焦质在催化剂表面覆盖所致。 展开更多
关键词 5-羟甲基糠醛 磺基离子液体 固定化 微球硅胶 果糖
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固相萃取-GC/MS法测定地表水中3-甲基吲哚
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作者 薛祥晔 鲜啟鸣 冯建昉 《环境监测管理与技术》 CSCD 2017年第2期53-55,共3页
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... 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%。 展开更多
关键词 3-甲基吲哚 微球硅胶填料 固相萃取 气相色谱/质谱法 地表水
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硅胶微球形填料固相萃取气质联用技术测定地表水中萘、苊、菲、芘 被引量:2
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作者 薛祥晔 胡恩宇 薛光璞 《四川环境》 2013年第1期21-24,共4页
为改进水样通过固相萃取柱的能力,合成了中位数粒径为88μm硅胶微球形填料,健合C18后,装填为600 mg规格的固相萃取柱,用于提取地表水中萘、苊、菲、芘。结果表明,水样可借助滤过吸咐装置,依靠自身重力通过该固相萃取柱,滤过流量平稳为10... 为改进水样通过固相萃取柱的能力,合成了中位数粒径为88μm硅胶微球形填料,健合C18后,装填为600 mg规格的固相萃取柱,用于提取地表水中萘、苊、菲、芘。结果表明,水样可借助滤过吸咐装置,依靠自身重力通过该固相萃取柱,滤过流量平稳为10ml/min。水样固相萃取处理后,用气质联用技术测定,样品相对标准偏差小于8.4%,加标回收率为93.2%~105%。在地表水环境监测中,该固相萃取柱可用于水样萘、苊、菲、芘的固相提取。 展开更多
关键词 硅胶微球形填料 固相萃取 气相色谱 质谱 环境监测 地表水
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Study of machining indentations over the entire surface of a target ball using the force modulation approach 被引量:1
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作者 Yuzhang Wang Yanquan Geng +3 位作者 Guo Li Jiqiang Wang Zhuo Fang Yongda Yan 《International Journal of Extreme Manufacturing》 EI 2021年第3期64-72,共9页
A modified five-axis cutting system using a force control cutting strategy was to machine indentations in different annuli on the entire surface of a target ball.The relationship between the cutting depths and the app... A modified five-axis cutting system using a force control cutting strategy was to machine indentations in different annuli on the entire surface of a target ball.The relationship between the cutting depths and the applied load as well as the microsphere rotation speed were studied experimentally to reveal the micromachining mechanism.In particular,aligning the rotating center of the high precision spindle with the microsphere center is essential for guaranteeing the machining accuracy of indentations.The distance between adjacent indentations on the same annulus and the vertical distance between adjacent annuli were determined by the rotating speed of the micro-ball and the controllable movement of the high-precision stage,respectively.In order to verify the feasibility and effect of the proposed cutting strategy,indentations with constant and expected depths were conducted on the entire surface of a hollow thin-walled micro-ball with a diameter of 1 mm.The results imply that this machining methodology has the potential to provide the target ball with desired modulated defects for simulating the inertial confinement fusion implosion experiment. 展开更多
关键词 force modulation controllable indentations entire micro-ball surface microsphere center alignment
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Preparative separation of high-purity troxerutin and related substances from mother liquor of troxerutin by silica gel column chromatography and semi-preparative liquid chromatography 被引量:1
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作者 Shaojing Liu Bei Qin +3 位作者 Hongfang Han Li Li Lili Yu Xiaojing Xu 《Journal of Chinese Pharmaceutical Sciences》 CAS CSCD 2020年第7期487-493,共7页
Troxerutin(TRO)is a mixture of semi-synthetic flavonoids prepared by hydroxyethylation of rutin,and it is commonly used for the treatment of cerebrovascular diseases.The main active ingredient is trishydroxyethyl ruti... Troxerutin(TRO)is a mixture of semi-synthetic flavonoids prepared by hydroxyethylation of rutin,and it is commonly used for the treatment of cerebrovascular diseases.The main active ingredient is trishydroxyethyl rutin.The mother liquor of TRO contains a lot of TRO and other derivatives of hydroxyethylated rutin.In order to make full use of the mother liquor of TRO,an efficient method was developed for recovering high-purity TRO from mother liquor of TRO by combining silica gel column chromatography with semi-preparative liquid chromatography.In the silica gel column chromatographic separation,the ratio of silica gel to sample and eluent composition were investigated to obtain optimum separation effect.The results showed that when the ratio of silica gel to sample was 50,and acetone–ethyl acetate–water–glacial acetic acid(10:10:3:1,v/v/v/v)was used as the eluent,the separation effect of TRO and adjacent impurities was good.Moreover,150 g of TRO with a purity of 80%could be obtained from 1 kg of mother liquor of TRO by the silica gel column chromatographic separation,and the results were consistent with the quality standard of TRO raw material.Subsequently,the semi-preparative HPLC was performed,and 100 g TRO with a purity of up to 98%(w/w)was obtained.Meanwhile,tetrahydroxyethylrutin and tetrahydroxyethylquercetin with purity greater than 98%were obtained.This work proposed the separation and preparation of TRO with high-purity from the production waste of TRO for the first time,which had certain environmental benefits and economic benefits. 展开更多
关键词 Mother liquor of troxerutin TROXERUTIN silica-gel column chromatography Semi-preparative HPLC NMR
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Interaction of Plasma Proteins with Tri-quaternary Ammonium Salt Cationic Surfactant Studied by QCM-D
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作者 Man Xi Baoyan Zhang 《Chinese Journal of Chemistry》 SCIE CAS CSCD 2015年第2期253-260,共8页
A tri-quaternary ammonium salt cationic surfactant was synthesized.Its structure was confirmed by using Fourier-transform infrared spectroscopy,^(1)H nuclear magnetic resonance spectroscopy,and X-ray photoelectron spe... A tri-quaternary ammonium salt cationic surfactant was synthesized.Its structure was confirmed by using Fourier-transform infrared spectroscopy,^(1)H nuclear magnetic resonance spectroscopy,and X-ray photoelectron spectroscopy analyses.Three model surfaces,including Au-CH_(3),Au-OH and Au-COOH,were fabricated.Adsorptions of surfactant on the three model surfaces and subsequent plasma proteins adsorption were investigated by quartz crystal microbalance with dissipation(QCM-D).The mass of surfactant on the Au-COOH surface was the largest,followed by that on the Au-CH_(3)surface,and that on the Au-OH surface.These results suggested that the main driving force of surfactant immobilization was electrostatic interaction followed by hydrophobic interaction.Based on the results obtained,we concluded that the protein mass adsorbed on Au-CH_(3)-S,Au-OH-S,and Au-COOH-S surfaces depended on the protein size and orientation.The mass and thickness of S on the Au-COOH surface is the largest and the protein adsorption capacity of Au-COOH-S surface is inferior to that of Au-CH_(3)-S.The Au-COOH-S surface could inhibit lysozyme adsorption,maintain the adsorption balance of bovine serum albumin,and induce fibrinogen-binding protein adsorption. 展开更多
关键词 tri-quaternary ammonium salt cationic surfactant self-assembled monolayers quartz crystal micro-balance with dissipation(QCM-D) proteins adsorption
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