β3-SiW11Ni/石墨烯复合材料的制备及对亚甲基蓝的吸附性能
马荣华*，韩泽群
（齐齐哈尔大学 化学与化学工程学院，黑龙江 齐齐哈尔 161006）
摘要：合成了杂多酸/氧化石墨烯复合材料β3-SiW11Ni/GO。用红外光谱、紫外光谱和X-射线粉末衍射仪对样品进行了表征，并对催化剂投入量、染料的初始浓度、溶液的 pH:等条件进行探究，确定了其反应最佳条件。结果表明，亚甲基蓝被β3-SiW11Ni/GO吸附的最佳条件为pH 8、催化剂用量为80 mg/L、染料浓度为15mg/L，最大吸附率达89.80%，最大吸附量可达111.3 mg/g。
关键词：杂多酸；氧化石墨烯；亚甲基蓝；吸附
中图分类号：O641.4 文献标识码：A 文章编号：
Synthesis and Adsorption Properties of β3-SiW11Ni/GO for Methylene Blue Wastewater MA Rong-hua*, HAN Ze-qun（College of Chemistry and Chemical Enginering，Qiqihaer University，Qiqihaer 161006, China）, Huaxue Shiji, 2018, 40(3)
Abstract: The β3-SiW11Ni/GO composite was synthesized and confirmed using IR, UV and XRD. Absorption parameters including the amount of catalyst, the initial concentration of dye, and the pH of solution were investigated, and the best absorption conditions were determined. Results showed that pH value of 8, catalyst dosage of 80 mg/L, and dye concentration of 15 mg/L was optimized as the best condition for methylene blue absorption using the β3-SiW11Ni/GO composite catalyst. The removal efficiency of methylene blue could reach up to 89.8%, the maximum adsorption capacity of up to 111.3mg/g.
Key word：heteropoly acid；grapheme oxide；methylene blue；adsorption
新型硅钨酸有机盐的合成及催化油酸酯化
栾庆洁，李思佳，刘丽君，龚树文*
（聊城大学 化学化工学院 功能有机分子与材料实验室，山东 聊城 252059）
摘要：利用喹啉-2-甲酸修饰硅钨酸，制备了一种新型的硅钨酸有机盐催化剂（QA-HSiW）。采用X-射线粉末衍射（XRD）、红外光谱（FT-IR）、热重分析（TG）以及电位滴定等方法对催化剂进行分析，并以油酸和甲醇的酯化反应为探针反应，评价催化剂在酯化反应中的催化性能。结果表明，QA-HSiW不仅保留了硅钨酸的Keggin结构，且具有较高的酸度和良好的热稳定性。QA-HSiW表现出优良的酯化催化反应活性，在较优条件下油酸酯化转化率可达99.8%，而且催化剂具有良好的稳定性，经过简单过滤可重复使用，5次以后催化剂仍具有较好的催化活性，反应过程中催化剂的物相及Keggin结构保持不变。
关键词：硅钨酸盐；固体酸催化剂；Keggin结构；酯化
中图分类号：O643.3 文献标识码：A 文章编号：0258-3283（2018）
Preparation and Catalytic Esterification Activity of Novel Organic-silicotungstate LUAN Qing-jie, LI Si-jia, LIU Li-jun, GONG Shu-wen*（Institution of Functional Organic Molecules and Materials, School of Chemistry and Chemical Engineering, Liaocheng University, Liaocheng 252059, China），Huaxue Shiji, 2018, 40(3)
Abstract：A novel organic-silicotungstate catalyst (QA-HSiW) was prepared by the modifying of H4SiW12O40 with quinaldic acid. The QA-HSiW was characterized by powder X-ray diffraction (XRD), infrared spectroscopy (FTIR), thermogravimetric analysis (TG) and potentiometric titration. Then the catalyst was employed for esterification of oleic acid to evaluate its acid-catalytic activity. The results indicated that QA-HSiW was not only maintained the typical Keggin structure of HSiW, but also presented strong acid strength and good thermal stability. QA-HSiW exhibited excellent catalytic activity in esterification and the conversion of oleic acid could reach up to 99.8% under optimal conditions. QA-HSiW had good reusability and there was no obvious change for the phase and the Keggin structureof catalyst after the reaction.
Key words：silicotungstate; solid acid catalyst; Keggin structure; esterification
羟基磷灰石纳米晶体的制备、表征及补钙效能研究
尹美林，赵善科，郑岩，史淑丹，孙玉琦*
（锦州医科大学 药学院，辽宁 锦州 121001）
摘要: 以氯化钙和磷酸氢二钠为先驱体、聚丙烯酸为稳定剂，采用化学沉淀法制备羟基磷灰石纳米晶体。采用傅里叶红外光谱仪（FT-IR）、X-射线衍射仪（XRD）、扫描电子显微镜（SEM）、动态激光散射仪（DLS）等对该晶体的结构、晶型、粒径、形态、Zeta电位进行表征。通过大鼠口服羟基磷灰石纳米晶体后，对骨源性碱性磷酸酶（BALP）水平和股骨密度（BMD）进行评价。结果表明，所制得的羟基磷灰石为针状晶体，粒径分布均匀，平均粒径为（144.7 ± 5.3）nm，Zeta电位为（-23.2 ± 0.59）mV，BALP水平较低，BMD值较高。所制备的羟基磷灰石纳米晶体具有较好稳定性和一定的补钙作用。
关键词：羟基磷灰石纳米晶体；制备；表征；化学沉淀法；补钙效能
中图分类号：R944.9 文献标识码：A 文章编号：0258-3283(2018)
Preparation and Calcium Supplement Efficiency of Hydroxyapatite Nanocrystals YIN Mei-lin，ZHAO Shan-ke，ZHENG Yan，SHI Shu-dan，SUN Yu-qi*( , Jinzhou Medical University，Jinzhou 121001, China), Huaxue Shiji, 2018, 40(3)
Abstract: The hydroxyapatite nanocrystals were prepared by chemical precipitation method using calcium chloride and disodium hydrogen phosphate as precursors and polyacrylic acid as stabilizers. The structure, crystal form, particle size, morphology and Zeta potential of the crystal were characterized by Fourier infrared spectrometer, X-ray diffraction (XRD), scanning electron microscopy (SEM) and dynamic laser scattering (DLS). Bone alkaline phosphatase (BALP) and bone mineral density (BMD) were evaluated after oral administration of hydroxyapatite nanocrystals. The results showed that the prepared hydroxyapatite was needle-like crystals with uniform particle size distribution, average particle size was (144.7 ± 5.3) nm, Zeta potential was (-23.2 ± 0.59) mV, BALP level was lower and femoral density was higher. Therefore, the prepared hydroxyapatite nanocrystals have good stability and certain calcium-supplementing effect.
Key words: hydroxyapatite nanocrystals；preparation；characterization；chemical precipitation method；calcium supplement efficiency
新型螺环化合物的合成、表征与除草活性研究
曾伍兰*a，江津河b，刘慧莲b
（潍坊学院 a.化学化工与环境工程学院 微尺度研究所，b. 生物与农业工程学院，山东 潍坊 261061）
摘要：以6，10-二氧杂螺[4.5]7，9-十烷二酮为先导化合物，合成了两种新型螺环化合物C15H14N2O6和C15H14ClNO4，并通过红外光谱(IR)，元素分析(EA)和X-射线单晶衍射分析对其结构进行了表征。结果表明，C15H14N2O6属于单斜晶系，晶胞群为P21/c，晶胞参数为：a = 11.251(2) Å，b = 11.001(2) Å，c = 12.750(3) Å，β = 114.20(3)º，V = 1439.5(5) Å3，Z = 4；C15H14ClNO4也属于单斜晶体，晶胞群为P21/c，晶胞参数为：a = 13.159(3) Å，b = 6.2197(12) Å，c = 17.750(4) Å，β = 96.46(3)º，V = 1443.5(5) Å3，Z = 4。C—H···O 和 N—H···O分子间作用力对晶体C15H14N2O6的稳定性起到重要作用，而C—H···O、C—H···p 分子间作用力和p···p 堆积作用所形成的三维网状结构加强了C15H14ClNO4的结构稳定性。还对两种化合物的除草活性进行了研究，发现它们对双子叶植物的生长具有较好的抑制作用。
关键词：合成；晶体结构；6，10-二氧杂螺[4.5]7，9-十烷二酮；除草活性
中图分类号：TK730 文献标识码：A 文章编号：0258-3283（2018）
Synthesis, Characterization and Herbicidal Activity of New Spiro Compounds ZENG Wu-lan*a, JIANG Jin-heb, LIU Hui-lianb(a. Microscale Science Institute, Department of Chemistry and Chemical Engineering; b. College of Biological and Agricultural Engineering, Weifang University, Weifang 261061, China)
Abstract:Two new spiro compounds derived from 6,10-dioxaspiro[4.5]decane-7,9-dione group, C15H14N2O6 and C15H14ClNO4, have been synthesized and confirmed by IR, elemental analysis and single-crystal X-ray diffraction. C15H14N2O6 crystallizes in monoclinic, space group P21/c with a = 11.251(2) Å, b = 11.001(2) Å, c = 12.750(3) Å, β = 114.20(3)º, V = 1439.5(5) Å3, Z = 4. C15H14ClNO4 is also of monoclinic system, space group P21/c with a = 13.159(3) Å, b = 6.2197(12))Å, c = 17.750(4) Å, β = 96.46(3)º, V = 1443.5(5) Å3, Z = 4. It is very interesting that C–H···O and N–H···Ointermolecular interactions play a significant role in stabilizing the crystal structures in C15H14N2O6. While, C–H···O hydrogen bonding together with C–H···p supramolecular interactions and p···p stacking interactions may strengthen the stability of the three dimensional framework in C15H14ClNO4. The herbicidal activity of two target compounds has been investigated. The result shows that they both possess good herbicidal activity against dicotyledon.
Key words: synthesis; crystal structure; 6,10-dioxaspiro[4.5]decane-7,9-dione; herbicidal activity
基于八元瓜环对抗肿瘤药盐酸厄洛替尼溶解度的影响研究
李春荣*1，孟铁宏1，郑相勇2
（1. 黔南民族医学高等专科学校 公共课教学部，贵州 都匀 558000；2. 山东博迈康药物研究有限公司，山东 济南 250101）
摘要：为提高抗肿瘤药盐酸厄洛替尼的生物利用度，以盐酸厄洛替尼（ELTN）为客体、八元瓜环Q[8]为主体，利用紫外-可见吸收光谱法研究了Q[8]对盐酸厄洛替尼的超分子相互作用。考察了溶液pH对作用体系的影响，同时研究了Q[8]对盐酸厄洛替尼的增溶性和溶出度。实验结果表明，在pH＜7条件下，Q[8]与盐酸厄洛替尼能够形成包结比为2︰1的稳定包结物，包结物的稳定常数为3.9×1012 L2/mol2。Q[8]的加入能明显改善盐酸厄洛替尼的溶解度并提高盐酸厄洛替尼的溶出度，且溶液酸性越强，效果越显著。在人工模拟胃液(pH 1.2)中，包结物Q[8]-ELTN的累积溶出度提高了近14倍，说明Q[8]不仅能提高盐酸厄洛替尼的溶解性，还具有潜在的药物运输载体的特性。
关键词：瓜环；盐酸厄洛替尼；紫外-可见吸收光谱；溶解度
中图分类号：O625.6 文献标识码：A 文章编号：0258-3283(2018)
Effect on Solubility on Antineoplastic Drug Erlotinib Hydrochloride Based on Cucurbit[8]uril LI Chun-rong*1, MENG Tie-hong1, ZHENG Xiang-yong2(1. Public Course Teaching Department, Qiannan Medical College for Nationalities, Duyun 558000, China; 2. Shandong Bomaikang Yaowu Yanjiu Co., Ltd, Jinan 250101, China), Huaxue Shiji, 2018, 40(3)
Abstract: To improve the bioavailability of antineoplastic drug erlotinib hydrochloride(ELTN), with antineoplastic drug erlotinib hydrochloride as guest and cucurbit[8]uril as host in this work, the supramolecular interaction of cucurbit[8]uril with erlotinib hydrochloride was investigated by UV-Vis spectroscopy. The effects on supramolecular interaction of the solution pH and the solubility and dissolution rate of cucurbit[8]uril to erlotinib hydrochloride were also investigated. The results showed that under the condition of solution pH<7, a 2 : 1 ratio complex was formed, and the formation constant was 3.9×1012 L2/mol2. The solubility and dissolution of erlotinib hydrochloride had a marked improvement with the added of cucurbit[8]uril, the lower the pH of the acid solution is, the more significant the solubility and dissolution rate of cucurbit[8]uril to erlotinib hydrochloride will be. Cumulative release rate of complex Q[8]-ELTN was increased about 14 times in artificial gastric juice(pH 1.2). Solubility and dissolution rate of erlotinib hydrochloride can be enhanced by cucurbit[8]uril, and cucurbit[8]uril may be preeminently potential drug carrier properties.
Key words: cucurbit[n]urils; erlotinib hydrochloride; UV-Vis spectroscopy; solubility
白杨素结构修饰及其衍生物的活性研究进展
王京，王杨，杨杰，张磊*
(遵义医学院 药学院，贵州 遵义 563003)
摘要：白杨素是一种分离自紫葳科植物木蝴蝶的黄酮类天然产物，具有广泛的生物活性，如抗肿瘤、降糖、抗菌、杀虫、抗炎和抗氧化等。白杨素的重要药理活性引起了国内外研究人员的广泛关注，但其存在水溶性差、生物利用度低以及体内容易被糖基化代谢失活等不足。主要综述近年来白杨素结构修饰及其衍生物的活性研究进展，包括抗肿瘤、降糖、抗菌以及其他生物活性，以期有益于白杨素的进一步研究。
关键词：白杨素；结构修饰；衍生物；生物活性
中图分类号：R284 文献标识码：A 文章编号：0258-3283（2018）
Progress in Structure Modifications and Biological Activities of Chrysin Derivatives WANG Jing, WANG Yang, YANG Jie, ZHANG Lei*(School of Pharmacy, Zunyi Medical College, Zunyi 563003, China), Huaxue Shiji, 2018, 40(3)
Abstract: Chrysin is a flavonoid extracted from Oroxylumindicum (L.)Vent, and it showed extensive biological activities, such as antitumor, hypoglycemic, antibacterial, insecticidal, anti-inflammatory and antioxidant, etc. So those important pharmacological activities caused the attention of researchers. However, some works also indicate that there are several disadvantages for chrysin, including poor soluble, poor bioavailability and glycosylation metabolic. Therefore, in order to improve the solubility of chrysin and enhance metabolic stability, a lot of the structure modification works have been made. Many derivatives of chrysin with various biological activities have been obtained in recent years. This work will review the advance in the progress of structure modification of chrysin and biological activities of chrysin derivatives, mainly including anti-tumor, hypoglycemic, antibacterial and other biological activities for the further study of chrysin.
Key words：chrysin; structure modification; derivative; biological activity
HPLC法同时测定叶面肥中4种植物生长调节剂的研究
李珍1, 2，郑义1，段路路*2，杨一2，武娟2
（1. 上海应用技术大学 化学与环境工程学院，上海 201418；2. 上海化工研究院，上海 200062）
摘要：采用高效液相色谱法对叶面肥中4种植物生长调节剂（脱落酸、烯效唑、氯吡脲和萘乙酸）进行检测。优选的色谱条件为：色谱柱：Symmetry Shield RP18柱（250 mm×4.6 mm）；流动相：V（乙腈）︰V（水）（磷酸调至pH 3.0）= 70 : 30，等度洗脱；柱温：40 ℃；进样量：10 μL；流速：1.0 mL/min；PDA检测器；检测波长为203 nm。测定4种植物生长调节剂的含量在2 ~ 100 mg/L范围的线性相关系数在0.999以上，回收率为95.7% ~ 103.5%，RSD≤2%（n = 8）。本实验所建立的方法能够在同一色谱条件下检测出4种植物生长调节剂的含量，且方法方便快捷、灵敏度高，可满足对化肥中植物生长调节剂的实际需求。
关键词：高效液相色谱法；植物生长调节剂；乙腈；叶面肥
中图分类号：O657.7 文献标识码：A 文章编号：0258-3283（2018）
Simultaneous Determination for 4 Kinds of Plant Growth Regulators in Foliar Fertilizer via HPLC LI Zhen1, 2, ZHENG Yi1, DUAN Lu-lu*2, YANG Yi2, WU Juan2 (1. School of Chemical and Environmental Engineering, Shanghai Institute of Technology, Shanghai 201418, China; 2. Shanghai Research Institute of Chemical Industry, Shanghai 200062, China）, Huaxue Shiji, 2018, 40(3)
Abstract: Four kinds of plant growth regulators (abscisic acid, uniconazole, forchlorfenuron and naphthaleneacetic acid)in foliar fertilizer were measured using HPLC. Optimization of chromatographic conditions: chromatographic column: symmetry shield RP18(250 mm×4.6 mm); mobilephase: acetonitrile-water(pH 3.0), such as degree of elution; column temperature: 40 ℃; sample quantity: 10 μL; flow velocity:1.0 mL/min; PDA detector; detection wavelength: 203 nm. In the content of four kinds of plant growth regulators in 2 ~ 100 mg/L range of linear correlation coefficient over 0.999. The detection limit was 0.1 mg/L, recovery was 95.7% ~ 95.7%, RSD≤2%(n=8). This method can detect the content of four plant growth regulators under the same chromatographic conditions, and it is convenient and quick and sensitive, which can meet the actual demand.
Key words: high performance liquid chromatography; plant growth regulator; acetonitrile; foliar fertilizer
GO-CMWNTs-CS-GCE电极电化学检测青菜中亚硝酸盐的含量
张军丽*，闫永康，徐启杰，张佳欣
(黄淮学院 化学与制药工程学院，河南 驻马店 463000)
摘要：采用氧化石墨烯(GO)、羧基化碳纳米管(CMWNTs)/壳聚糖(CS)复合膜滴涂玻碳电极(GCE)得到修饰电极(GO-CMWNTs-CS-GCE)，并用于检测NO2-。采用循环伏安法考察亚硝酸根的电化学行为，探究了亚硝酸根的检测条件。结果表明，在扫速0.1 V/s，pH 4.7（PBS缓冲溶液）的条件下，修饰电极对NO2-的氧化有显著的电催化活性，线性范围为1.0×10-7 ～ 0.40 mol/L；信噪比为S/N=3时，检出限为1.1×10-8 mol/L。修饰电极呈现良好的稳定性、重现性和抗干扰性，可用于腐败青菜中亚硝酸盐的测定。
关键词：氧化石墨烯；壳聚糖；GO-CMWNTs-CS-GCE电极；亚硝酸盐
中图分类号: O657.1 文献标识码:A 文章编号：0258-3283（2017）
Electrochemical Detection of Nitrite Content in Lettuce by GO-CMWNTs-CS-GCE Electrode ZHANG Jun-li*, YAN Yong-kang, XU Qi-jie, ZHANG Jia-xin (College of chemical and pharmaceutical engineering，Huanghuai University，Zhumadian 463000，China), Huaxue Shiji, 2018, 40(1)
Abstract：The electrode was modified by cast-coating grapheneoxide and carboxylic multi-walled carbon nanotube/chitosan composite on GCE, which could be applied for the detection of nitrite. Elecstrochemical behavior of nitrite was investigated by cyclic voltammetry, and the detection conditions of nitrite was explored. The results showed that the amperometric response of the sensor for nitrite reached the maximum value on the conditions of pH 4.7 (PBS) and scanning rate of 0.1 V/s. The sensor could detect nitrite in a wide linear range from 1.0×10-7 ～ 0.40 mol/L with a detection limit of 1.1×10-8mol/L (signal-to-noise S/N=3). As a result, modified GCE electrode has very good cycling stability, data reproducibility and anti-interference capability. The method may be applied to detect NO2- in cured vegetables.
Key words: Graphene oxide; chitosan; GO-CMWNTs-CS-GCE electrode; nitrite
汽油中硅含量的单波长色散X-射线荧光光谱法与电感耦合等离子体发射光谱法比对
吴志鹏*，关雎，肖伟
（广州能源检测研究院，广东 广州 511447）
摘要：建立了单波长色散X-射线荧光光谱法（MWDXRF）测定汽油中硅含量的方法，并与国标ICP-OES方法进行了对比，考察了MWDXRF方法的准确性、重复性和加标回收率以及不同标准溶液对MWDXRF方法结果的影响。结果表明，在硅含量很低的情况下，采用MWDXRF方法得出的结果会比ICP-OES方法得出的结果偏大，随着硅浓度的不断增大，两种方法之间的结果差异也越来越小，且采用不同类型的标准溶液进行MWDXRF方法分析得出的结果并无明显差异。MWDXRF方法的相对标准偏差＜5.0%，加标回收率在97.8% ~ 118.2%之间，结果准确可靠，适用于硅含量浓度为0 ~ 250.0 mg/kg范围内的汽油样品。
关键词：汽油；硅；单波长色散X-射线荧光光谱法；电感耦合等离子发射光谱法
中图分类号：O657.34 文献标识码：A 文章编号：0258-3283（2018 ）
Comparison of Determination of Silicon Content in Gasoline by Single Wavelength Dispersive X-ray Fluorescence Spectrometry and Inductively Coupled Plasma Optical Emission Spectrometry WU Zhi-peng，GUAN Ju，XIAO Wei（Guangzhou institute of energy testing，Guangzhou 511447，China）, Huaxue Shiji, 2018, 40(3)
Abstract：Methods for the determination of silicon content in gasoline by monochromatic wavelength dispersive X-ray fluorescence spectrometry （MWDXRF）was established with comparing with national standard ICP-OES. The accuracy, reproducibility and recovery rate of MWDXRF and the effect of different standard solutions on the results of MWDXRF were investigated. The results show that under the condition of low silicon content, the results obtained by MWDXRF are larger than those obtained by ICP-OES, with the increasing of silicon concentration, the difference between the two methods was getting smaller and smaller, and the results of MWDXRF were not different by different standard solutions. The recovery rate of MWDXRF was respectively 97.8% ～ 118.2% with relative standard deviation was less than 5.0%. The method was accurate, reliable and suitable for the determination of silicon content in gasoline samples with a concentration of 0 ～ 250.0 mg/kg.
Key words：gasoline；silicon；MWDXRF；ICP-OES
微波辅助甲酯化-微型液液萃取-气相色谱法测定
卷烟中的非挥发有机酸和脂肪酸
沈艳飞，赵常山，赵立恒，陈建华，耿永勤，杨叶昆，孔维松，张承明，李雪梅，李晶*
(云南中烟工业有限责任公司 技术中心，云南 昆明 650231)
摘要：建立了微波辅助甲酯化-微型液液萃取-气相色谱分离分析卷烟中非挥发性有机酸（乳酸、丙二酸、乙酰丙酸、草酸、苹果酸、柠檬酸）和脂肪酸（棕榈酸、硬脂酸、亚油酸）的方法。实验采用优化前处理条件：10%硫酸-甲醇(V/V)为甲酯化衍生溶液，微波罐压力为200 kPa，温度为150℃，在600 W 功率下保持10 min；利用自主开发设计的微型液-液萃取装置，以二氯甲烷为萃取溶液进行反应后甲酯溶液的萃取；利用优化的气相色谱条件，可以实现对11种有机酸的分离检测，在1.0～420 mg/mL范围内具有较好的线性，各待测物的线性相关系数均大于0.999，检出限在0.20 ～ 0.36 mg/mL之间；对样品进行不同水平的添加考察实验回收率，平均回收率在92 ～ 108%之间，方法相对标准偏差(RSD)为2.65% ～ 3.48%。所建立的方法操作简易，溶剂消耗量小，线性相关性好，重复性佳，可以满足对于卷烟样品中有机酸的检测要求。
关键词：非挥发有机酸；脂肪酸；微波辅助甲酯化；微型液-液萃取；气相色谱
中图分类号：TS412 文献标识码：A 文章编号：
Determination of Nonvolatile Organic Acids and Fatty Acids in Cigarette by Microtype Solvent Extraction and Gas Chromatography SHEN Yan-fei, ZHAO Chang-shan, ZHAO Li-heng, CHEN Jian-hua, GENG Yong-qin, YANG Ye-kun, KONG Wei-song, ZHANG Cheng-ming, LI Xue-mei, LI Jing* (R&D Center, China Tobacco Yunnan Industrial Co.,Ltd, Kunming 650231,China)
Abstract：A new method coupling microwave-assisted derivatization with microtype liquid-liquid extraction (LLE) and gas chromatography (GC) was established for determination of nonvolatile organic acids (lactic acid, malonic acid, laevulinic acid, oxalic acid, malic acid, citric acid) and fatty acids (hexadecanoic acid, stearic acid, linoleic acid) in cigarette samples. The optimized pretreatments were using 10% sulfuric acid-methanol as the esterification reagent while the power of microwave was fixed at 600 W reacting for 10 min under the pressure of 200 kPa and the temperature of 150 ℃. With the self-designed device for microtype LLE, the dichloromethane (CH2Cl2) was chosen as the extraction solvent. With the optimal separation conditions, regression equations revealed acceptable linearity (R > 0.999) across the working-standard range (1.0 ～ 420 µg/mL) for the 11 target analysts. The spiked recoveries of real samples were in the range of 92% ～ 108% with the relative standard deviations （RSD）of 2.65% ～ 3.48%. With the advantages of accessibility, less solvent consumption, acceptable linearity and good reproducibility, this simple method can be used to determine nonvolatile organic acids (lactic acid, malonic acid, laevulinic acid, oxalic acid, malic acid, citric acid) and fatty acids in cigarette samples simultaneously.
Key words: nonvolatile organic acids; fatty acids; microwave-assisted derivatization; microtype liquid-liquid extraction (LLE);Gas chromatography (GC)
硫化钼样品预处理对测定总铁含量的影响研究
程伟琴1, 2，赵增兵1, 2，张谦华1, 2，王毅楠1, 2，霍二福1, 2, 3，成兰兴＊1, 2
（1. 河南省化工研究所有限责任公司，河南 郑州 450052；2．河南省精细化工中间体工程技术研究中心，河南 郑州 450052；3．河南省科学院质量检验与分析测试研究中心，河南 郑州 450008）
摘要：通过优化硫化钼样品预处理的工艺参数，提高铁的浸出率，从而更加准确地测定硫化钼中铁的含量。首先，选择硝酸氯酸钾-盐酸湿法消解体系，加入过量氨水调节溶液pH。利用紫外分光光度法测定硫化钼中的总铁含量，其中测量结果标准偏差为0.0004062，平均加样回收率为99.89%。该方法测定结果准确度高、易操作，能够满足科研和产品检验的要求，为生产过程控制和质量控制提供一定的分析依据。
关键词：铁；硫化钼；磺基水杨酸；预处理
中图分类号：O655.24 文献标识码：A 文章编号：0258-3283（2017）
Effect on the Determination of Iron Content in Molybdenum Disulfide by Pretreatment CHENG Wei-qin1, 2,ZHAO Zeng-bing1, 2, ZHANG Qian-hua1, 2, WANG Yi-nan1, 2, Huo Er-fu1, 2, 3, CHENG Lan-xing＊1, 2(1. Henan Chemical Industry Research Institute Co., Ltd., Zhengzhou 450052, China; 2. Fine Chemical Intermediate Engineering Technology Research Center of Henan Province, Zhengzhou 450052, China; 3. Quality Inspection and Analytical Test Research Center, Henan Academy of Sciences, Zhengzhou 450008, China)
Abstract: By optimizing the process parameters of the pretreatment of sulfide molybdenum samples, the leaching rate of iron was improved, and the iron content of molybdenum sulfide was determined more accurately.Firstly, the nitrate potassium chlorate-hydrochloric acid wet digestion system was chosen, and solution pH was adjustment by add the excess ammonia.Thetotaliron content inmolybdenum disulfide wasdeterminedby ultraviolet (UV) spectrophotometry, and the standard deviation of the measurement result is 0.0004062, the average recovery is 99.89%. The method is more accurate, easy to operate and can meet the requirements of scientific research and product inspection, and provides an important analysis basis for the production process control and quality control.
Key words: iron; molybdenum disulfide; 5-sulfosalicylic acid;pretreatment
塑胶跑道上空空气中挥发性有机化合物的成分特征研究
刘干，郑伟涛*，谢衍
（武汉体育学院 体育工程与信息技术学院 运动干预与健康促进湖北省协同创新中心 国家体育总局体育工程重点实验室，湖北 武汉 430079）
摘要：采用气相色谱-质谱联用（GC-MS）技术对SUMMA罐收集的塑胶跑道上空空气进行挥发性有机化合物（VOCs）定性定量检测，检出其空气中的VOCs覆盖了烷烃、烯烃、炔烃、芳香烃、卤代烃、含氧类有机物和含氮类有机物等七大类，共92种，且高碳烷烃（C6 ～ C12）、卤代烷烃和苯系物的有机物单体数量较多，含氧类有机物的检出质量浓度最高。VOCs单体的检出率集中在76.47%以上，平均检出质量浓度主要集中在小于1.00 μg/m³，且丙酮的平均检出质量浓度最大。
关键词：塑胶跑道；挥发性有机化合物；SUMMA罐采集；气相色谱-质谱联用
中图分类号：O659 文献标识码：A 文章编号：0258-3283（2018）
Volatile Organic CompoundsCharacteristics in the Air above Plastic Runway LIU Gan, ZHENG Wei-tao*, XIE Yan（1. Key Lab of Sports Engineering of General Administration of Sport of China, Hubei Provincial Collaborative Innovation Center for Exercise and Health Promotion, School of Sports Engineering and Information Tech., Wuhan Sports University, Wuhan 430079, China）, Huaxue Shiji, 2018, 40(1)
Abstract：This work collected the air over plastic runway by SUMMA canister and detected by gas chromatography-mass spectrometry. 92 Kinds of VOCs were detected included alkane, alkene, alkyne, aromatic hydrocarbon, halogenated hydrocarbon, oxy-organics and nitrogenous organic compounds. High carbon alkanes (C6 ～ C12), halogenated alkanes and benzene have more organic monomers, and oxy-organics have the highest quality concentrations. The detection rate of each organic monomer was concentrated over 76.47%, the average quality concentration mainly under 1.00 μg/m³ and acetone was the highest in average quality concentration.
Key words：plastic runway; volatile organic compounds (VOCs); SUMMA canister; gas chromatography-mass spectrometry(GC-MS)
LC-ICP-MS联用测定稻米中的无机汞和甲基汞
龚燕1, 2，尚晓虹2，赵馨*2
(1. 无锡市疾病预防控制中心，江苏 无锡 214023；2. 国家食品安全风险评估中心，北京 100021)
摘要：建立稻米中无机汞（Hg（Ⅱ））和甲基汞（MeHg）的液相色谱-电感耦合等离子体质谱检测方法。样品中的Hg（Ⅱ）和MeHg经提取液（0.1% L-半胱氨酸+5%甲醇）超声提取、0.22 μm水系滤膜过滤净化， 以0.1% L-半胱氨酸+0.06 mol/乙酸铵+5%甲醇为流动相，用VenusilR MP C18色谱柱分离，以电感耦合等离子体质谱进行测定。结果显示，Hg（Ⅱ）和MeHg能有效分离，且在0.10 ～ 5.00 μg/L范围内线性关系良好。当称样量为0.5 g时，方法的检出限（LOD）为0.001 mg/kg，定量限(LOQ)为0.003 mg/kg，Hg（Ⅱ）的加标回收率为94.5% ～ 96.3%，MeHg的加标回收率为99.1% ～ 106.7%。本方法准确、快速、便捷，可应用于稻米中Hg（Ⅱ）、MeHg的同时测定。
关键词：LC-ICP-MS；稻米；汞；甲基汞
中图分类号：R155.5 文献标识码： A 文章编号：0258-3283(2017)
Determination of Mercury and Methylmercury in Rice by HPLC-ICP-MS GONG Yan*1,2, SHANG Xiao-hong2, ZHAO Xin2（1. Wuxi Center for Disease Control and Prevention,Jiangsu Wuxi 214023,China; 2.China National Center for Food Safety Risk Assessment，Beijing 100021,China）
Abstract：To establish a method for the determination of mercury and methylmercury in rice by high performance liquid chromatography coupled with inductively coupled plasma mass spectrometry (LC-ICP-MS). Mercury and methylmercury in sample were ultrasonic extracted by 0.1% L- cysteine +5% methanol, purified by 0.22 μm water filtration, separated by Venusil, R, MP C18 column ,with 0.1%L- cysteine +5% methanol +0.06 mol/L ammonium acetate as the mobile phase, and determinated by inductively coupled plasma mass spectrometry. Hg (II) and MeHg could be well separated, and it showed good linearity in the range of 0.10 ～ 5.00 μg/L. When the sample size is 0.5 g, the limit of detection was 0.001 mg/kg, the limit of quantification was 0.003 mg/kg ,and the average recoveries of Hg (II) and MeHg were 94.5% ～ 96.3% and 99.1% ～ 106.7%. The method was accurate, rapid, simple, and can be used for simultaneous determination of mercury (II) and methylmercury in rice.
Key word：LC-ICP-MS; rice; mercury; methyl mercury
醋酸氢化可的松纯度标准物质的定值及不确定度分析
陈怡，张辉*，邓超
（浙江省计量科学研究院，浙江 杭州 310013）
摘要：建立了醋酸氢化可的松纯度标准物质的定值和不确定度评定方法。通过旋光法、紫外-可见光谱法和傅里叶变换红外光谱法进行了定性分析。再利用质量平衡法原理，采用高效液相色谱（HPLC）多家实验室联合法对醋酸氢化可的松的有机主成分进行了测定，同时采用热重分析法、卡尔·费休库伦法和顶空进样-气相色谱法对灰分、水分和溶剂残留含量进行了测定。然后，运用HPLC法对醋酸氢化可的松的分装样品进行均匀性和稳定性检验。最后，根据测量模型评定不确定度，定值结果为98.75%，相对扩展不确定度为0.85%（k = 2）。
关键词：标准物质；醋酸氢化可的松；质量平衡法；高效液相色谱；不确定度
中图分类号：O625 文献标识码：A 文章编号：0258-3283（2017）
Purity Determination and Uncertainty Evaluation of Hydrocortisone AcetateReference Material CHEN Yi，ZHANG Hui*，DENG Chao(Zhejiang Provincial Institute of Metrology，Hangzhou 310013 China)
Abstract：The approach for purity determination and uncertainty evaluation of hydrocortisone acetate reference material was established. The qualitative analysis was performed via polarimetry method, ultraviolet-visible spectroscopy (UV) and fourier transform infrared spectroscopy (FT-IR). The qualitative analysis, on the other hand, was made on the principle of mass balance method. In order to enhance the accuracy of the purity determination, the content determination of the main component was carried out by the joint efforts from by several laboratories performing experiments under the same condition of high performance liquid chromatography (HPLC), and the content of other impurities i.e. ash, moisture and residual solvent were also determined by thermogravimetry analysis, Karl Fischer coulometric method and headspace sampling-gas chromatography, respectively. The uniformity and stability of phenol reference material was investigated by HPLC. Finally, the determination of uncertainty were accomplished by establishment of the measurement models. The purity determined in this way was 98.75% with the relative standard uncertainty of 0.85% (k = 2).
Key words：reference material；hydrocortisone acetate；mass balance method；high performance liquid chromatography；uncertainty
α-Fe2O3纳米微球的合成及气敏性能研究
付双*，刘得水，李红梅，许凤，夏春辉，李爽，孙革
（齐齐哈尔医学院 药学院，黑龙江 齐齐哈尔 161006）
摘要：采用溶剂热法制备了球状结构的氧化铁前驱体，再经400 ℃热处理后得到α-Fe2O3纳米微球。通过TG、IR、XRD和SEM等手段对产物结构和形貌进行了表征。结果表明，合成的α-Fe2O3纳米微球直径约为500 nm。此外，我们将α-Fe2O3纳米微球制备成厚膜型气敏元件并进行了气敏性能测试，在工作温度为150 ℃时，α-Fe2O3纳米微球对苯胺(AN)有良好的选择性和较高的灵敏度，最低检出限可达到1.9 mg/m3，对38 mg/m3苯胺的响应值为10.4。测试结果表明，α-Fe2O3纳米微球可用于制备苯胺气体传感器。
关键词：溶剂热法；纳米微球；α-Fe2O3；苯胺气敏性
中图分类号：O614 文献标识码：A 文章编号：0258-3283（2018）
Synthesis and Gas-sensing Properties of Fe2O3 nanospheres FU Shuang*, LIU De-shui, LI Hong-mei, XU Feng, XIA Chun-hui, LI Shuang, SUN Ge (College of Pharmacy, Qiqihar Medical University, Qiqihar 161006, China), Huaxue Shiji, 2018, 40(3)
Abstract: Spherical iron oxide precursor was prepared using solvothermal method, and thermally treated at 400℃ to obtain α-Fe2O3 nanoparticle. The structures and morphologies of the as-obtained products were confirmed by TG, IR, XRD, and SEM. The results showed that the diameter of α-Fe2O3 nanoparticle is about 500 nm. In addition, the thick film of α-Fe2O3 nanoparticle was fabricated as gas sensor and performed the gas sensing test. When the working temperature was set at 150 ℃, α-Fe2O3 nanoparticle has very good selectivity and high sensitivity to aniline (AN). The minimum detection limit can reach down to 1.9 mg/m3, and response value for 38 mg/m3 aniline analyte can be 10.4. These results show that the α-Fe2O3 nanoparticle can be used to prepare practical gas sensors for aniline.
Key words: solvothermal method; nanoparticle; α-Fe2O3; aniline gas sensing
光谱探针在测定食品中痕量铅中的应用
郭明鑫1，张召凤2，李考学2，郭蒙*2
（1．山东省昌乐二中，山东 昌乐 262400；2．潍坊学院 化学化工与环境工程学院，山东 潍坊 261061）
摘要: 建立了一种以芹菜素为光谱探针测定食品中铅的方法。在pH 8.10、9.0 × 10-3 mol/L三（羟甲基）氨基甲烷-HCl缓冲溶液、2.99 × 10-5 mol/L芹菜素溶液中，Pb2+浓度在2.4 × 10-7 ～ 4.8 × 10-6 mol/L范围内与吸光度降低值呈良好的线性关系，线性方程为：DA =1.8×10-2c +9.76×10-3(10-6 mol/L)(R=0.994)，检出限达到2.3×10-7 mol/L，并将该法成功应用于黑乌龙茶中铅的测定。经过研究发现铅与芹菜素形成配合比为1︰2的配合物。
关键词: 芹菜素；铅；紫外光谱法；配合比
中图分类号：O657.3 文献标识码：A 文章编号：0258-8283（2018）
Application of Spectral Probe on Determination of Trace Lead in Food GUO Ming-xin1, ZHANG Zhao-feng2, LI Kao-xue2, GUO Meng*2(1. Shandong Changle No.2 High School, Changle 262400, China；2. College of Chemistry & Chemical and Environmental Engineering, Weifang University, Weifang 261061, China), Huaxue Shiji, 2018, 40(3)
Abstract: Using apigenin as a spectral probe, a method for the determination of lead in food was established. In the range of 2.4 × 10-7 ~ 4.8 × 10-6 mol/L, there was a good linear relationship between the reduction of absorbance with the concentration of lead ions under the pH 8.10，9.0 × 10-3 mol/L Tris-HCl buffer solution, 2.99 × 10-5mol/L apigenin solution. The linear equation was DA =1.8×10-2c +9.76×10-3(10-6 mol/L)(R=0.994). The detection limit of this method was 2.3×10-7 mol/L. And the lead in black oolong tea was successfully determined. In addition, the results showed that the complexation ratio of lead with apigenin was 1 : 2.
Key words: apigenin; lead; ultraviolet spectroscopy; complexation ratio
超声波辅助合成反式二苯乙烯
鞠萍，杜丽，王庆源，窦生艳，杨华，张玉琦，王记江，张恩生*
（延安大学 化学与化工学院 陕西省化学反应工程重点实验室，陕西 延安 716000）
摘要：报道了一种在超声波辅助条件下，基于McMurry 反应合成反式二苯乙烯的新方法。采用单因素实验，研究了超声波辅助条件下TiCl4/锌粉用量、反应温度、反应时间及超声功率对反应收率的影响，筛选得到了优化的合成条件。在优化合成条件下完成了21种反式二苯乙烯类化合物的超声波辅助合成，采用FT-IR、EI-MS、1HNMR、13CNMR等表征手段对产物进行了结构确证。研究表明，该方法可有效减少TiCl4/锌粉及溶剂用量、缩短反应时间、提高反应收率并且具有较广的底物适用性。
关键词：超声波辅助合成；McMurry反应；反式二苯乙烯
中图分类号：O621 文献标识码：A 文章编号：0258-3283(2018)
Ultrasonic-Assisted Synthesis of Trans-stilbenes JU Ping, DU Li, WANG Qing-yuan, DOU Sheng-yan, YANG Hua, ZHANG Yu-qi, WANG Ji-jiang, ZHANG En-sheng*(College of Chemistry and Chemical Engineering, Shaanxi Key Laboratory of Chemical Reaction Engineering, Yan′an University, Yan′an 716000, China)，Huaxue Shiji, 2018, 40(3)
Abstract: An ultrasonic-assisted McMurry reaction for the facile synthesis of trans-stilbenes was developed. The optimized reaction conditions were obtained after screening various reaction conditions such as the amount of TiCl4/Zn, reaction temperature, reaction time as well as the ultrasonic power. The scope of this method was explored under the optimized reaction conditions and 21 desired trans-stilbenes were prepared. The structure of the products were confirmed by FT-IR, EI-MS, 1HNMR and 13CNMR. It is note worthy that this method offers several advantages including short reaction times, less solvent and TiCl4/Zn consumption and wide substrate scope.
Key words: ultrasonic-assisted synthesis; McMurry reaction; trans-stilbenes
(S)-2-氨基-3-乙酰氨基丙酸甲酯的合成
王凯a，周文a，江帅b，刘博[1]a
(广州中医药大学 a. 第二临床医学院，b. 中药学院，广东 广州 510006)
摘要：以价廉易得的L-天冬酰胺为起始原料，经Cbz保护、Hofmann重排、酯化、乙酰化、Cbz脱保护5步反应得到重要中间体即目标化合物，总收率达37.5%，其结构经ESI-HRMS、1HNMR和IR确证。
关键词：L-天冬酰胺；(S)-2-氨基-3-乙酰氨基丙酸甲酯；合成
中图分类号： TQ253 文献标识码：A 文章编号：0258-3283（2018）
Synthesis of Methyl-(S)-3-acetamido-2-aminopropanoate WANG Kaia, ZHOU Wena, JIANG Shuaib, LIU Bo*a (a. The Second Clinical College, b. School of Chinese Materia Medica, Guangzhou University of Chinese Medicine, Guangzhou 510006, China), Huaxue Shiji, 2018, 40(3)
Abstract：Methyl-(S)-3-acetamido-2-aminopropanoate was synthesized from L-asparagine as the starting material, via a five-step reaction of N-Cbz protection, Hofmann rearrangement, esterification, acetylation, and Cbz-deprotection. The overall yield of this important target compound was 37.5%. Its structure was confirmed by ESI-HRMS, 1HNMR and IR.
Key words：L-asparagine; methyl-(S)-3-acetamido-2-aminopropanoate; synthesis
4-色满酮肟酯衍生物的合成与结构表征
吴利欢*，徐洪伍，覃超国，张晓强
(肇庆学院 环境与化学工程学院，广东 肇庆 526060)
摘要：以取代和未取代4-色满酮为原料，与盐酸羟胺发生缩合反应得到中间体4-色满酮肟，然后在弱碱条件下与酸酐或酰氯反应合成一系列新型的4-色满酮肟酯衍生物。探讨了反应原料配比、催化剂的用量对合成中间体的影响，得出最佳配比为n(色满酮)︰n(盐酸羟胺)︰n(无水乙酸钠) = 1︰5︰2。所合成的化合物结构通过IR、1HNMR、13CNMR和HRMS进行了鉴定和表征。
关键词：4-色满酮肟酯；合成；表征
中图分类号：O623 文献标识码：A 文章编号：0258-3283（2018）
Synthesis and Characterization of 4-Chromanone Oxime Esters Derivatives WU Li-huan*, XU Hong-wu, QIN Chao-guo, ZHANG Xiao-qiang (School of Environmental and Chemical Engineering, Zhaoqing University, Zhaoqing 526060, China), Huaxue Shiji, 2018, 40(3)
Abstract: Under weak base condition, a series of 4-chromanone oxime esters derivatives were synthesized by the reaction of anhydride or acyl chloride with 4-chromanone oxime, which were prepared by condensation of substituted and unsubstituted 4-chromanone with hydroxylamine hydrochloride. The effects of catalyst amount, the ratio of material on the yield of the intermediate were discussed and the best molar ratio was obtained, which is n(chromanone) : n(hydroxylamine hydrochloride) : n (sodium acetate anhydrous) = 1 : 5 : 2. The structures of compounds were confirmed by IR, 1HNMR, 13CNMR and HR-MS.
Key words: 4-chromanone oxime ester; synthesis; characterization
磺酸功能化壳聚糖催化合成氧杂蒽二酮衍生物
王英磊*，刘学国，杜朝军，张莉
(南阳理工学院 生物与化学工程学院，河南 南阳 473004)
摘要：以生物质壳聚糖作为原料，制备了磺酸功能化壳聚糖固体酸性催化剂，在无溶剂条件下催化芳香醛和5, 5-二甲基-1, 3-环己二酮（或1, 3-环己二酮）反应合成了一系列氧杂蒽二酮衍生物，产率达84% ~ 96%。该方法对环境友好、操作简单，且催化剂易于分离和回收使用，符合绿色化学的要求。
关键词：磺酸功能化壳聚糖；氧杂蒽二酮；无溶剂；重复使用
中图分类号：O626.41 文献标识码：A 文章编号：0258-3283（2018）
Synthesis of 1, 8-Dioxo-octahydroxanthene Derivatives Catalyzed by Sulfonic Acid Functionalized Chitosa WANG Ying-lei*, LIU Xue-guo, DU Chao-jun, ZHANG Li(School of Biological and Chemical Engineering, Nanyang Institute of Technology, Nanyang 473004, China), Huaxue Shiji, 2018, 40(3)
Abstract：The solid acid of sulfonic acid functionalized chitosan was prepared by using biomass chitosan as raw material, which was applied as an efficient catalyst for the synthesis of a series of 1, 8-dioxo-octahydroxanthene derivatives via the condensation of aromatic aldehyde and 5, 5-dimethyl-1, 3-cyclohexanedione (or 1, 3-cyclohexanedione) under solvent-free conditions in yields of 84% ~ 96%. This method is friendly to environment, simple manipulation, and the catalyst is easy to separate and reuse, which meets the requirement of green chemistry.
Key words：sulfonic acid functionalized chitosan; 1, 8-dioxo-octahydroxanthene; solvent-free; recycle
2-溴-3, 5, 6-三氯吡嗪的合成
杨烁1, 2，吴明圆1, 2，周志旭1, 2，赵春深*1, 2, 3
(1. 贵州大学 药学院，贵州 贵阳 550025；2. 贵州药物合成工程实验室，贵州 贵阳 550003；
3. 贵州发酵工程与生物制药重点实验室，贵州 贵阳 550003)
摘要：标题化合物是一种重要的医药化工中间体。以2, 6-二氯吡嗪为起始原料，经氨化、亲电取代以及桑德迈尔3步反应制备了目标化合物，其结构经IR、MS、1HNMR和13CNMR确证。该合成方法未见文献报道，原料廉价易得、操作方便且收率较高，反应总收率为65.7%。
关键词：2-溴-3, 5, 6-三氯吡嗪；2, 6-二氯吡嗪；合成
中图分类号：O626.1 文献标识码：A 文章编号：0258-3283(2018)
Synthesis of 2-Bromo-3, 5, 6-trichloro-pyrazine YANG Shuo1, 2, WU Ming-yuan1, 2, ZHOU Zhi-xu1, 2, ZHAO Chun-shen*1, 2, 3 (1. School of Pharmaceutical Sciences, Guizhou University, Guiyang 550025, China; 2. Guizhou Engineering Laboratory for Synthetic Drugs, Guiyang 550025, China; 3. Key Laboratory of Guizhou for Fermentation Engineering and Biomedicine, Guiyang 550025, China), Huaxue Shiji, 2018, 40(3)
Abstract: 2-Bromo-3, 5, 6-trichloro-pyrazine is an important pharmaceutical chemical intermediates. In this paper, the target compound was synthesized by ammonification reaction, electrophilic substitution reaction and Sandmeyer reaction with 2, 6-dichloro-pyrazine as the starting material. The structure was confirmed by IR, MS, 1HNMR and 13CNMR. The synthesis process has never been reported before in the literatures. The raw materials are cheap and easy to get in this method with high yield. The total yield was 65.7%.
Key words: 2-bromo-3, 5, 6-trichloro-pyrazine; 2, 6-dichloro-pyrazine; synthesis
蒸馏结晶耦合工艺制备高纯对溴甲苯
郭建国*1, 2，吴孝兰1, 2，陈浩云1, 2，宋忠哲3，顾金凤1, 2
（1. 上海化学试剂工程技术研究中心，上海 200002；2. 国药集团化学试剂有限公司，上海 200002；3.上海沃凯生物技术有限公司，上海 金山 201507）
摘要：以甲苯、氢溴酸和次氯酸钠为原料，氢溴酸和次氯酸钠反应生成的氯化溴为高活性溴化剂，避免了有毒有害、易挥发的液溴为溴化剂的传统操作；在室温下高选择性、温和地合成了低邻溴甲苯含量的对溴甲苯。然后利用蒸馏-结晶耦合技术，蒸馏后采用无溶剂、分步本体熔融结晶，去除甲苯、2-溴甲苯等微量杂质，制备了高纯对溴甲苯；蒸馏-结晶耦合技术操作可控、连续。整个工艺绿色环保、高效低能耗、原料易得、条件温和、易操作，适合规模化制造。
关键词：蒸馏结晶耦合工艺；高纯；对溴甲苯；高选择性；甲苯；氢溴酸；次氯酸钠；分步结晶
中图分类号：TQ031.8 文献标识码：A 文章编号：0258-3283(2018)
Preparation of High Purity p-Bromotoluene by Distallation-crystallization Coupling Process GUO Jian-guo*1, 2, WU Xiao-lan1, 2, CHEN Hao-yun1, 2, SONG Zhong-zhe3, GU Jin-feng1, 2
Abstract: Using toluene, HBr and sodium hypochlorite as raw materials to synthesis p-bromotoluene with high chemoseletivity. Then, high purity p-bromotoluene was prepared via distallation-crystallization coupling process. The process was run continually by using step operation at crystallization part. The raw materials are industrial and the process is easy to control and scale-up.
Key words: distallation-crystallization coupling process；high purity; p-bromotoluene; high chemoseletivity; toluene; hydrobromic acid; sodium hypochlorite；step crystallization
