可见光水全分解材料的研究进展
杨甲，孙晓瑞*，曾婷，胡义兰
(长江师范学院 化学化工学院 重庆无机特种功能材料实验室，重庆 408100)
摘要：光催化水分解反应在光催化的研究领域具有重要地位，尤其是具有可见光水全分解性能的半导体材料最为重要。目前能够严格地按化学计量比实现可见光水全分解反应的半导体材料较少。水全分解半导体材料的匮乏是因为要实现可见光水全分解反应对半导体有两个严格的要求：1）需要半导体的禁带宽度落在1.8 ～ 3.2 eV的区间内；2）该半导体的导带和价带的电势要分别能够还原质子制氢和氧化水分子制氧。把紫外-可见光谱划分为400 nm以下，500 nm以下，600 nm以下，700 nm以下和780 nm以下5个区间，着重介绍了对可见光有响应的水全分解半导体材料的最新研究进展，最后对此类材料的发展趋势进行了展望。
关键词：光催化材料；可见光；水全分解；清洁能源
中图分类号：O643 文献标识码：A 文章编号：0258-3283（2019）
Review of the Water Splitting Photocatalyst under Visible Light YANG Jia, SUN Xiao-rui*, ZENG Ting, HU Yi-lan (Chongqing Key Laboratory of Inorganic Special Functional Materials, College of Chemistry and Chemical Engineering, Yangtze Normal University, Chongqing 408100, China), Huaxue Shiji, 2019
Abstract: The study of water decomposition is a very important reaction in the field of photocatalysis. And the photocatalyst which can overall split water is the key point in the photocatalytic research. There are two problems for the photocatalyst to meet the requirement of the water splitting. Firstly, the band gap of the semiconducting material must be between 1.8 eV and 3.2 eV; Secondly, the potential of conduction band and valence band must be enough for the reduction of H+ to H2 and the oxidation of H2O to O2, respectively. In this paper, the UV-Visible spectrum was divided into five parts, including below 400 nm, below 500 nm, below 600 nm, below 700 nm and below 780 nm. Thereafter, we attempt to provide an overview of the photocatalytic semiconducting materials which can overall water splitting under visible light irradiation. Finally, the development trend of these materials is prospected.
Key words: photocatalytic materials; visible light; water splitting; clean energy
掺Ce纳米ZnO光催化剂的结构表征及催化性能
张芳佳，王悦，张榴，张秀文，李建法*
（绍兴文理学院 化学化工学院，浙江 绍兴 312000）
摘要：为了提高ZnO微纳米材料对有机染料的光催化降解性能，以ZIF-8为中间体制备了ZnO，并对其进行稀土Ce掺杂，利用X射线粉末衍射（XRD）、傅里叶变换红外光谱（FT-IR）、扫描电镜及能谱（SEM-EDX）、透射电镜（TEM）、固体紫外光谱（UV-Vis）对光催化剂进行了系列表征，探究了掺Ce比例、光源类型对光催化降解甲基橙的影响。结果表明：掺杂适量的Ce可以提高ZnO的光催化活性；掺Ce质量为Zn质量的1%（ZnO-1%Ce）时ZnO的光催化活性最高；ZnO-1%Ce在实验所用太阳光下的光催化性能优于在紫外光下。
关键词：氧化锌；铈；合成；光催化降解；染料
中图分类号：O611.5 文献标识码：A 文章编号：0258-3283（2019）--
Catalytic Performances of Ce-doped nano-ZnO Photocatalyst ZHANG Fang-jia, WANG Yue, ZHANG Liu, ZHANG Xiu-wen, LI Jian-fa*（College of Chemistry and Chemical Engineering，Shaoxing College of Arts and Sciences，Shaoxing 312500，China）, Huaxue Shiji, 2019, 41(7 )
Abstract: In order to improve the photocatalytic degradation of organic dyes by ZnO micro/nano materials, ZnO was prepared by using ZIF-8 as an intermediate, and it was doped with rare earth Ce. The photocatalysts were characterized by XRD, FT-IR, SEM-EDX, TEM and UV-Vis spectroscopy. The effects of Ce ratio and light source on photocatalytic degradation of methyl orange were investigated. The results show that doping an appropriate amount of Ce can increase the photocatalytic activity of ZnO, and the photocatalytic activity of ZnO is best when the Ce ratio is 1% (Ce/Zn mass%). The photocatalytic performance of ZnO-1%Ce under the sunlight used in the experiment is better than that under ultraviolet light.
Key words: ZnO; Ce; synthesis; photocatalytic degradation; dye
巯基功能化介孔材料对阳离子染料的吸附应用
刘 婧1, 4，张建辉*2, 3，冷艳丽2，张榕芳1，杨 武4
（1. 甘肃农业职业技术学院 食品化工系，甘肃 兰州 730020；2. 贵州民族大学 化学工程学院，贵州 贵阳 550025； 3. 兰州资源环境职业技术学院 应用化学系，甘肃 兰州 730021； 4. 西北师范大学 化学化工学院，甘肃 兰州 730070）
摘要：以3-巯丙基-三甲氧基硅烷为有机功能试剂，采用后接枝法，合成了巯基功能化的介孔材料。修饰后的样品不仅保持了高度有序的SBA-15的二维六角结构，而且具有较高的热稳定性，较大的比表面，孔容和较窄的孔径分布。考察了HS-Zr-La-SBA-15（HS-ZLS）介孔分子筛对阳离子染料孔雀石绿和罗丹明B的吸附性能。实验结果表明，该吸附剂对两种阳离子染料均具有良好的吸附性能，吸附平衡快，吸附容量高。实验还表明该吸附剂对两种染料的吸附动力学均符合准二级动力学模型，吸附等温线符合Langmuir单分子层吸附模型。
关键词 ：介孔材料；功能化；阳离子染料；吸附
中图分类号：O69 文献标识码：A 文章编号：0258-3283（2019）--
The application of thiol-functionalized mesoporous materials in adsorption of cationic dyes LIU Jing1,3, ZHANG Jian-hui*2, LENG Yan-li2, Zhang Rong-rong, YANG Wu3 (1. Department of Food and Chemical Engineering, Gansu College of Agriculture Technology, Lanzhou 730020, China; 2. School of Chemical Engineering, Guizhou Minzu Unversity, Guiyang 550025, China; 3. Department of Applied Chemical Engineering, Lanzhou Resources & Environment Voc-Tech College, Lanzhou 730021, China; 4. College of Chemistry and Chemical Engineering, Northwest Normal University, Lanzhou 730070, China), Huaxue Shiji, 2019, 41( 7 ), ～
Abstract: Thiol-functionalized mesoporous materials HS-ZLS were respectively synthesized by a post-grafting procedure using 3-mercaptopropyl trimethoxysilane as organic modifiers. The synthesized materials still maintained inherent long-range ordered two-dimensional hexagonal channel structure of the mesoporous materials and possessed higher thermostability, bigger specific surface area and pore volume, and narrower pore size distribution. Adsorption performances of thiol-functionlized Zr-La-SBA-15(ZLS) mesoporous sieve to cationic dyes Malachite green and Rhodamine B were studied and it was found that the adsorbent possessed excellent adsorption properties including fast adsorption equilibrium and high adsorption capacities. The results also showed that the adsorption kinetics of the adsorbent to the two dyes obeyed pseudo-second-order kinetic model and the adsorption isotherms obeyed Langmuir monomolecular layer adsorption model.
Keywords: mesoporous materials ; functionalization ; cationic dyes ; adsorption
免疫分析法在克伦特罗残留检测中的应用
韦林洪1a，张军*1b，王承莉1a，董大鹏1a，王赪胤2
（1.扬州市职业大学 a.生物与化工工程学院，b. 科技产业处， 江苏 扬州 225009；2. 扬州大学 化学化工学院，江苏 扬州 225002）
摘要：克伦特罗能提高脂肪型动物的瘦肉和脂肪的比率，因此常被用做畜禽饲料添加剂。由于其化学性质稳定，残留在畜禽产品中的克伦特罗对人类健康产生了严重的危害，故检测畜禽产品中的克伦特罗残留对于保证食品安全非常重要。免疫分析法特异性强、灵敏度高、反应条件温和，广泛应用于食品安全检测。综述了免疫亲和色谱法、放射免疫分析法、酶联免疫分析法、化学发光免疫分析法、免疫层析法、时间分辨荧光免疫分析法、免疫传感器、分子印迹免疫分析法等免疫分析法在克伦特罗残留分析中的应用，并展望了这些分析方法的发展趋势。
关键词：免疫分析法；克伦特罗；分析
中图分类号：TS251.7 文献标识码：A 文章编号：0258-3283（2019）--
Application of Immunoassay in the Determination of Clenbuterol Residue WEI Lin-hong1a, ZHANG Jun *1b, WANG Cheng-li1a, DONG Da-peng1a, WANG Cheng-yin2(a. College of Biological and Chemical Engineering, b. Science and Technology Industry Department, Yangzhou Vocational University, Yangzhou 225009, China; 2. College of Chemistry and Chemical Engineering, Yangzhou University, Yangzhou 225002, China ), Huaxue Shiji, 2019, 41( 7 ), ～
Abstract: Clenbuterol can increase the ratio of lean meat and fat of fatty animals, so it is often used as feed additive for livestock. Because of its stable chemical properties, the residues in livestock products have caused serious harm to human health. Detection of clenbuterol residues in livestock products plays important role in ensuring food safety. The immunoassay, with high specificity, high sensitivity and mild reaction conditions, has been widely used in food security detection. The application of immunoassay such as immunoaffinity chromatography, radioimmunoassay, enzyme-linked immunosorbent assay, chemiluminescent immunoassay, immunochromatographic assay, time resolved fluoroimmunoassay, immunosensor and molecularly imprinted immunoassay in clenbuterol residue detection was reviewed, and development trend of these analysis methods was also prospected.
Key words：immunoassay; clenbuterol; analysis
农药及制药废水的处理技术及研究进展
刘盼1,2，扶咏梅1,2，顾效纲1，宋忠贤1,2，郭一飞*1,2
（1. 河南城建学院 市政与环境工程学院，河南 平顶山 467036；2.河南省水体污染防治与修复重点实验室，河南 平顶山 467036）
摘要：随着我国工业的发展，药物的广泛使用，致使废水中的药物日益增加，污染问题逐渐加重。首先介绍了利用电芬顿法和多孔磁性铜铁氧体对农药中的杀虫剂降解的研究，然后对制药废水的来源、危害及目前常用的处理技术进行了综述。传统的技术对制药废水的降解效果不佳，而新出现的技术包括光化学基因降解法、单色光降解法、紫外光/过氧化氢降解法、臭氧化处理法、活性炭过滤法、纳米复合材料吸附法和生物处理法的降解效果较好。对上述各方法的机理、研究进展、优缺点进行了综述，同时展望了制药废水处理技术的发展方向和趋势。
关键词：杀虫剂；制药废水；处理技术；光化学处理；臭氧处理
中图分类号：X523 文献标识码：A 文章编号：0258-3283(2019)
Research in the Treatment of Pesticide and Pharmaceutical Wastewater LIU Pan1,2，FU Yong-mei1,2，GU Xiao-gang1，SONG Zhong-xian1,2， GUO Yi-fei1,2 (1.Henan University of Urban Construction，Henan Pingdingshan 467036;2.Henan Key Laboratory of Water Pollution Cotrol and Rehabilitation, Pingdingshan 467036,China）,Huaxue Shiji,2019,41(7),
Abstract: As the development of the industry in our country and the increasing use of drugs, which enter into the water continually, the drug pollutants gradually aggravate. Firstly, the article made use of electric fenton rection and porous magnetic copper ferrite to degrade pesticides in the waste water. Then, the sources and the harmfulness of the pharmaceutical wastewater and the present commonly used treatment technology were summarized. It was found that the traditional technology is bad to degrade the pharmaceutical wastewater, so many new technology emerge at the right time. These treatment technology include photochemical gene degradation, monochromatic light degradation, ultraviolet light/hydrogen peroxide degradation, ozonation treatment, activated carbon filter method, nanocomposite adsorption method and the degradation of biological treatment. It is excellent for the effect of these new technology to degrade the pharmaceutical wastewater. At the same time, the essay prospects the development direction and the trend of treatment technology to degrade the pharmaceutical wastewater.
Key words: pesticides; pharmaceutical wastewater; treatment technology; photochemical treatment; ozonation treatment
环境监测用正丁烷气体标准样品的研制
杨静，杜健，王倩，宁红兵，李宁*
（环境保护部标准样品研究所 国家环境保护污染物计量和标准样品研究重点实验室，北京 100029）
摘要：采用称量法制备了氮气中正丁烷气体标准样品，其含量为1 μmol/mol。建立了使用气相色谱-氢火焰离子检测器（GC-FID）分析氮气中正丁烷气体标准样品的方法。此外，考察了制备方法和分析方法的可靠性，还对氮气中正丁烷气体标准样品随使用压力和时间的量值变化等性质进行了测定。最后，对气体标准样品的不确定度进行了评估。结果显示，浓度水平为1 μmol/mol的氮气中正丁烷气体标准样品的最低使用压力为1 MPa，有效期为12个月，其相对扩展不确定度为2%。
关键词：正丁烷；气体标准样品；不确定度
中图分类号：X830.5 文献标识码：A 文章编号：0258-3283（2019）
Development of N-butane Gas Standard for Environmental Monitoring YANG Jing, DU Jian, WANG Qian, NING Hong-bing, LI Ning* ( Institute for Environmental Reference Materials, State Environmental Protection Key Laboratory of Environmental Pollutant Metrology and Reference Materials, Beijing 100029, China), Huaxue Shiji, 2019
Abstract：The n-butane with concentration of 1 μmol/mol in nitrogen was prepared using a four-step weighing method. The analytical method of this gas standard was established using GC-FID and the repeatability of the preparation method and analytical method were also examined. In addition, the homogeneous and stable were performed which indicated this gas standard was homogeneous above to 1 MPa in cylinders and remained stable no less than 12 months. Finally, the expanded uncertainty of the n-butane with concentration of 1 μmol/mol in nitrogen was calculated as 2%.
Key words: n-butane; gas standard; uncertainty
水中碘离子溶液标准物质研制
刘新*，龚维，刘霞，王爱萍，姚旭霞，吕辉
（中国兵器工业集团第五三研究所，山东 济南 250031）
摘要：研制了水中碘离子溶液标准物质。采用杂质扣除法和硝酸银电位滴定法两种不同原理的方法确定原材料碘化钾的纯度。最终确定碘化钾纯度为99.80%，相对扩展不确定度为0.26%（k = 2）；采用重量-容量法配制水中碘离子溶液标准物质，并采用F检验和趋势线检验考查该标准物质的均匀性和稳定性。结果表明，研制的标称值为100 mg/L的水中碘离子溶液标准物质具有良好的均匀性和稳定性，相对扩展不确定度为1%（k = 2）。该标准物质可用来校准仪器和评价分析检测方法。
关键词：碘离子；杂质扣除法；纯度；重量-容量法；标准物质
中图分类号：150.55 文献标识码：A 文章编号：0258-3283（2019）
Preparation of the Reference Material of Iodide in Water LIU Xin*, GONG Wei, LIU Xia, WANG Ai-ping, YAO Xu-xia, LV Hui (CNGC Institute 53, Jinan 250031, China), Huaxue Shiji, 2019
Abstract: The reference material of iodide in water was prepared. The purity of potassium iodide was 99.80% and the relative expanded uncertainty was 0.26%（k = 2）,which was determined by deducting impurities and silver nitrate titration. The reference material of iodide in water was prepared by weight-volumetric method，and F test and trend line were carried out for the reference material. The results showed that the standard value of the reference material of iodide in water was 100 mg/L, and the relative expanded uncertainty was 1%（k = 2）.The reference material has good uniformity and stability. It can be used for the evaluation of iodide analysis and the calibration of the instrument.
Key words: iodide ion; impurity deduction; purity; weight-volumetric; reference material
二甲基砷溶液标准物质的研制
孙倩芸，郭波*，李锋丽，王云，邱黛君，黄清波，杨中元，朱建强
(山东省计量科学研究院，山东 济南 250014)
摘要：以高纯度的二甲基砷酸钠为原料，采用重量法制备了二甲基砷溶液标准物质。在对制备的标准物质进行定性检测的基础上，通过高效液相色谱-电感耦合等离子体质谱法对制备的标准物质进行比较法定值。同时，对标准物质的均匀性、稳定性进行考察。二甲基砷溶液标准物质的质量浓度为22.1 ug/g，扩展不确定度为U = 0.8 ug/g (k = 2)，有效期为12个月。
关键词：二甲基砷；元素形态；标准物质；不确定度
中图分类号：O655.5 文献标识码：A 文章编号：0258-3283（2019）
Preparation of Dimethylarsinic Acid Reference Material SUN Qian-yun, GUO Bo*, LI Feng-li, WANG Yun, QIU Dai-jun, HUANG Qing-bo, YANG Zhong-yuan, ZHU Jian-qiang (Shandong Institute of Metrology, Jinan 250014, China), Huaxue Shiji, 2019
Abstract: In this study, dimethylarsinic acid reference material was prepared using high purity sodium dimethylarsinate as raw materials by weighting method. On basis of quality analysis, the certified value was defined by the comparing with primary reference material by means of HPLC-ICP-MS. In addition, the checking of uniformity and stability test were systematically studied .The result revealed the certified value of the reference material was 22.1 μg/g with expanded uncertainty of U = 0.8 ug/g (k = 2) while its valid was 12 months.
Key words: dimethylarsinic; elemental speciation; reference material; uncertainty
氦中三氟化氮气体标准物质的研制
尹强，黄彦捷*，周阳，毛沅文，叶丽芳，贾相锐，陈玲
(广东省计量科学研究院，广东 广州 510405)
摘要：以高纯三氟化氮为原料气，分别使用红外光谱法及质谱法对其进行定性分析，再利用气相色谱仪及露点仪对其中的杂质进行定量检测，通过质量平衡法测定了原料气的纯度。通过重量法制备氦中三氟化氮气体标准物质，并通过均匀性实验、稳定性实验、重量法定值和不确定度评定对氦中三氟化氮气体标准物质进行了研究。结果表明，其均匀性和稳定性满足F检验和t检验要求，符合标准物质的技术规范，所制备的氦中三氟化氮标准物质具有良好的均匀性和足够的稳定性，相对扩展不确定度为2.0%（k=2）。该系列气体标准物质可望用于相关仪器的检定校准及半导体生产等相关行业的气体报警器的标定和检测。
关键词：三氟化氮；标准物质；重量法；不确定度
中图分类号： 文献标识码：A 文章编号：0258-3283（2019）
Research on a Certified Reference Material of Nitrogen Trifluoride in Helium YIN Qiang, HUANG Yan-jie, ZHOU Yang, MAO Yuan-wen, YE Li-fang, JIA Xiang-rui, CHEN Ling (Guangdong Provincial Institute of Metrology, Guangzhou 510000, China), Huaxue Shiji, 2019
Abstract：Using the high purity nitrogen trifluoride as raw gas, the qualitative analysis was carried out by IR and MS, and the impurities were quantitatively detected by gas chromatograph and dew point instrument. The purity of raw gas was determined by mass balance method. The standard materials of nitrogen trifluoride gas in helium were prepared by gravimetric method. The standard materials of nitrogen trifluoride gas in helium were studied by homogeneity test, stability test, gravimetric determination and uncertainty evaluation. The results showed that the uniformity and stability met the requirements of F-test and t-test, and met the technical specifications of the standard materials. The prepared reference materials of nitrogen trifluoride in helium had good uniformity and sufficient stability. The relative expansion uncertainty was 2.0% (k = 2). The standard material of nitrogen trifluoride in helium was analyzed and verified by the qualification unit, which ensured the accuracy and reliability of the quantity of gas reference material. At present, the gas standard material has been appled for a national second class standard material, and has been tried by many enterprises and institutions. It is expected to be used in the verification and calibration of related instruments. Furthermore, it can be used for calibration and detection of gas alarm in semiconductor production and other related industries.
Key words：nitrogen trifluoride; reference material; gravimetric analysis; uncertainty
柱内光纤发光二极管诱导荧光检测毛细管电泳测定药片中的硫胺素
邱雯曦*1，刁佩彧2，钟辉云1，周礼仕1
（1. 四川卫生康复职业学院，四川 自贡 643000；2. 成都市金堂县环保局，四川 成都 610000）
摘要：建立毛细管电泳柱内光纤发光二极管诱导荧光检测法（CE-ICFO-LED-IFD）测定维生素B1药片中硫胺素含量。以380 nm发光二极管作为激发光源，采用光纤传导激发光至检测窗口。硫胺素在电泳分析前，经铁氰化钾溶液衍生。对各种影响电泳检测硫胺素的因素进行考察，最佳电泳条件为：硼砂缓冲液浓度10 mmol/L、缓冲液pH 8.4、分离电压22 kV。硫胺素在0.05 ～ 25 μmol/L浓度范围内具有良好的线性关系（r=0.999 4），最低检出限为11 nmol/L。迁移时间和峰高相对标准偏差（RSD）分别为1.18%和3.09%。加标回收率为98.3% ～ 106.7%，相对标准偏差（RSD）为2.55% ～ 3.59%。维生素B1药片中硫胺素含量为9.88 mg/62.0 mg。该方法简便、快速、准确可靠、成本低、灵敏度高，为完善维生素B1药片质量控制提供了新的方法和依据。
关键词：毛细管电泳；发光二极管；硫胺素
中图分类号：0657.8 文献标识码：A 文章编号：0258-3283（2019）
The Application of Capillary Electrophoresis with in-column Fiber-optic Light-Emitting Diode-induced Fluorescence Detection in Determination of Thiamine QIU Wen-xi*1, DIAO Pei-yu2, ZHONG Hui-yun1, ZHOU Li-shi1（1.Department of Pharmacy, Sichuan Vocational College of Health and Rehabilitation, Zigong 643000, Sichuan, China; 2.Chengdu Jintang County Environmental Protection Bureau, Chengdu 610000, China)
Abstract: In this paper, a home-build capillary electrophoresis with in-column fiber-optic light-emitting diode-induced fluorescence detection (CE-ICFO-LED-IFD) was developed for the determination of thiamine. A UV-LED (380 nm) was used as excitation light source and an optical fiber was used to guide the excitation light into the capillary right at the detection window. Thiamine was precolumn-derivatized with potassium ferricyanide. The influence of buffer concentration, buffer pH and applied voltage was systematically investigated. Optimal separation conditions were obtained with 10 mmol/L borate buffer at pH 8.4 and an an applied voltage of 22 kV. The thiamine had a good linear relationship in the concentration ranges of 0.05~25 μmol/L (r=0.999 4) and the limit of detection (LOD) was 10 nmol/L. The relative standard deviations of migration time and peak height were 1.18% and 3.09%, respectively. The average recoveries were 98.3% ~ 106.7% with the RSDs ranging from 2.55% to 3.59%. The content of thiamine in the Vitamin B1 tablets was 9.88 mg/62.0 mg. The proposed method is simple, fast, accurate and low-cost which provides a new method and basis for improving the quality control of Vitamin B1 tablets.
Key words: capillary electrophoresis; light-emitting diodes; thiamine
高效液相色谱法同时测定尼卡巴嗪中4，4'-二硝基均苯二脲和2-羟基-4，6-二甲基嘧啶的含量
徐金雷*，赵梅仙，马佳颖，肖进，梁景乐，齐鹏，吴家鑫
（中牧实业股份有限公司，北京 100095）
摘要：建立了同时测定尼卡巴嗪中4，4'-二硝基均苯二脲(DNC)和2-羟基-4，6-二甲基嘧啶(HDP)双组分的高效液相色谱法。实验采用安捷伦Poroshell 120 Bonus-RP，(4.6×150 mm, 2.7 μm)色谱柱，水和乙腈为流动相梯度洗脱，流速为0.8 mL/min，柱温为40℃，HDP和DNC的检测波长均选择300 nm。试验结果表明HDP和DNC分别在23.3～34.9 μg/mL和56.7～85.1 μg/mL范围内线性关系良好，相关系数(r)分别为0.9998和0.9996。HDP平均回收率为100.4%，RSD为0.9%(n=9)；DNC的平均回收率为99.2%，RSD为0.8% (n=9)。建立的方法简便、准确、可靠，可更好地控制尼卡巴嗪的质量。
关键词：高效液相色谱；尼卡巴嗪；4，4'-二硝基均苯二脲(DNC)；2-羟基-4，6-二甲基嘧啶(HDP)
中图分类号：O657.72 文献标识码：A 文章编号：0258-3283（2019）
Simultaneous Determination of DNC and HDP in Nicarbazin Complex by High Performance Liquid Chromatography XU Jin-lei*, ZHAO Mei-xian, MA Jia-ying, XIAO Jin, LIANG Jing-le, QI Peng, WU Jia-xin (China Animal Husbandry Industry Co., Ltd., Beijing 100095, China), Huaxue Shiji, 2019, 41( 7)
Abstract: A high performance liquid chromatographic method was established for the simultaneous determination of 4,4’-dinitrocarbanilide (DNC) and 2-hydroxy-4, 6-dimethylpyrimidine (HDP) in nicarbazin raw material drug. Analysis was performed on a Agilent poroshell 120 Bonus-RP (4.6×150 mm, 2.7 μm) column by using water-acetonitrile as mobile phase at a flow rate of 0.8 mL/min and a column temperature of 40 ℃.The detecting wavelength of HDP and DNC were set at 300 nm. The results showed that a good linear relationship was accepted in the range of 23.3 ～ 34.9 μg/mL of HDP(r=0.9998) and 56.7 ～ 85.1 μg/mL of DNC recovery DNC (r=0.9996). The average recovery of HDP was 100.4% (n=9) with RSD of 0.9%. The average of DNC was 99.2% (n=9) with RSD of 0.8%. This method was convenient, accurate, and reliable. It was suitable to control the quality of nicarbazin raw material drug.
Key words: high performance liquid chromatography；nicarbazin；4,4’-dinitrocarbanilide(DNC)；2-hydroxy-4,6-d imethylpyrimidine(HDP)
石墨消解-盐酸保存液定容结合原子荧光法测定
土壤中总汞的研究
许娟娟，王炜*，陈欢，金扬旸
(浙江环境监测工程有限公司，浙江 杭州 310012)
摘要：采用石墨消解-盐酸保存液定容的前处理方式，结合原子荧光法测定土壤中总汞。结果表明，方法检出限为0.001 mg/kg。对不同土壤标准样品进行测定，其结果均在允许误差范围内，相对误差为 -6.7％ ～ 6.0％，相对标准偏差为1.2％ ～ 5.3％；对土壤标准样品及实际样品进行加标回收试验，回收率为94.3％ ～ 109.0％。跟踪试验结果表明，标准曲线和样品浓度在5 d内未发生明显变化。与国标法进行比对，结果表明两种方法对土壤中总汞测定结果无显著差异。
关键词：土壤中总汞；石墨消解；盐酸保存液；比对
中图分类号：X833 文献标识码：A 文章编号：0258-3283（2019）--
Graphite Digestion-Hydrochloric Acid Preservation Liquid Diluting Combined with Atomic Fluorescence Spectrometry for Determination of Total Mercury in Soil XU Juan-juan, WANG Wei*,CHEN Huan, JIN Yang-yang (Zhejiang Environmental Monitoring Engineering Co., Ltd., Hangzhou 310012, China) Huaxue Shiji, 2019, 41(5),～
Abstract: Graphite digestion-hydrochloric acid preservation liquid diluting was applied as the pretreatment method for determination of total mercury in soil by atomic fluorescence spectrometry. The result showed that the detection limit was 0.001 mg/kg. Different standard soil samples were determined, and the relative error and standard deviation were -6.7% ～ 6.0% and 1.2% ～ 5.3%, respectively. Moreover, the results were all confirmed within the allowable error. Recovery test of standard and actual soil samples were also carried out, and the recovering rate was 94.3% ～ 109%. The tracing test proved that the concentration of soil sample could be stable with 5 days. Comparison of the applied method and national standard method was presented, and there was no significant difference in the total mercury determination results.
Key words: total mercury in soil; graphite digestion; hydrochloric acid preservation liquid; comparison
不同选择性的C18检测全鹿丸中补骨脂素和异补骨脂素含量
吴小梅*1，刘征宙2，郭德勇1，卢晓伟1，陈再洁1，任兴发1，屠炳芳1
（1. 月旭科技(上海)股份有限公司，上海 201203；2. 国药集团化学试剂有限公司，上海 200002)
摘要：研究了用不同键合工艺的C18柱在药典要求的流动相条件下对全鹿丸中目标物进行分离的不同效果，通过使用不同选择性的色谱柱对全鹿丸中的补骨脂素和异补骨脂素进行含量测定，建立了高效液相色谱法中药成分测定全鹿丸中补骨脂素和异补骨脂素的方法。本方法简便、灵敏、准确、重现性好、分析时间短，满足药企对全鹿丸的质量控制要求。
关键词：高效液相色谱法；C18柱；全鹿丸；补骨脂素；异补骨脂素；中药成分测定；质量标准
中图分类号：R917 文献标识码：A 文章编号：0258-3283（2019）
Determination of psoralen and isopsoralen in alrodeer pill by C18 with different selectivity Wu Xiao-Mei*, Liu Zhengzhoub，Guo De-yonga, Lu Xiao-wei, Chen Zai-Jiea ,Ren Xing-faa, Tu Bing-fanga(a.Welch Material, Shanghai 201203 b.Sinopharm Chemical Reagent Co., LTD , Shanghai 200002)
Abstract : In this paper, the effect of C18 column with different bonding processes on the separation of target substances in alrodeer pill with the mobile phase required by Chinese Pharmacopoeia was studied. The method for the determination of psoralen and isopsoralen in alrodeer pill by high performance liquid chromatography was established by using different selective columns. And the results showed the method was simple, sensitive, accurate, reproducible, and had short analysis time. Therefore, it can meet the quality control requirement of pharmaceutical enterprises for alrodeer pill.
Key words: HPLC; C18 column; alrodeer pill; psoralen; isopsoralen; determination of Chinese Medicine
三种瓜环与多巴胺的分子包结行为研究
孟铁宏1，李春荣1，胡先运1，姜艳萍1，王恒1，肖昕*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.贵州大学 贵州省大环化学及超分子化学重点实验室，贵州 贵阳 550025)
摘要：为了开发多巴胺类药物在以瓜环为载体的超分子药物包合物方面的应用，选取了3种具有不同空腔大小的瓜环：对称四甲基六元瓜环（TMeQ[6]）、七元瓜环（Q[7]）、八元瓜环（Q[8]），利用核磁共振技术、MALDI-TOF质谱以及紫外吸收光谱等手段探究了3种瓜环与药物分子多巴胺（DA）的超分子包结行为。结果表明，DA位于TMeQ[6]的端口，与空腔较小的TMeQ[6]形成端口作用，而进入了空腔相对更大的瓜环Q[7]、Q[8]的内腔形成了主客体超分子药物包合物，为利用瓜环作为药物分子传递、缓释的载体提供了一定的理论依据。
关键词：对称四甲基六元瓜环；七元瓜环；八元瓜环；多巴胺；包结
中图分类号：O641.3 文献标识码：A 文章编号：0258-3283（2019）--
A Study of the Inclusion Behavior between Three Kind of Cucurbit[n]urils and Dopamine MENG Tie-Hong1, LI Chun-Rong1, HU Xian-Yun1, JIANG Yan-Ping1, WANG Heng1, XIAO Xin*2
(1. Public Course Teaching Department, Qiannan Medical College for Nationalities, Duyun 558000, China; 2. Key Laboratory of Macrocyclic and Supramolecular Chemistry of Guizhou Province, Guizhou University, Guiyang 550025, China), Huaxue Shiji, 2019, 41( ), ～
Abstract：In order to develop the application of dopamine (DA) in supramolecular drug inclusion complexes, three kinds of cucurbit[n]urils including TMeQ[6], Q[7] and Q[8] were employed as hosts, the supramolecular self-assembly between these cucurbit[n]urils with dopamine guest have been studied by 1HNMR spectroscopy, UV spectroscopy and mass spectrometry in details. The experimental results revealed that the DA is located the portal of the TMeQ[6], whereas the whole DA molecule are located inside the cavity of the Q[7] or Q[8] host, forming inclusion complexes. This provides a theory evidence for the use of cucurbit[n]urils as carriers for drug delivery and release.
Key words：tetramethyl-cucurbit[6]uril; cucurbit[7]uril; cucurbit[8]uril; dopamine; inclusion
基于藏红T的席夫碱合成及其对Fe(III)
的专一选择性识别研究
付晓伟，牟涛，吴晓*
（营口理工学院 化学与环境工程系，辽宁 营口 115014）
摘要：重金属污染目前已非常严重，因此识别检测重金属离子显得尤为重要。合成了基于藏红T（ST）与2-羟基-1-萘甲醛（N）的席夫碱配体ST-N，该配体在水溶液中对Hg(II)、Pb(II)、Ca(II)、Fe(II)、Fe(III)、Co(II)等18种常见金属离子中的Fe(III)有很好的专一选择性识别，其最低检测限为1 mg/L，符合《GB/T 14848-2017地下水质量标准》中铁IV类检测标准 ≤ 2.0 mg/L，且检测Fe(III)的RSD ≤ 1.17%，加标回收率在95.7% ～ 103%之间。
关键词：藏红T；重金属离子；Fe(III)；可见分光光度法
中图分类号：O641.4 文献标识码：A 文章编号：0258-3283（2019）
Synthesis of Schiff Alkali based on Saffron T and Its Specific Selective Recognition Study on Fe(III) FU Xiao-wei, MU Tao, WU Xiao* ( Chemical and Environmental Engineering, Yingkou Institute of Technology, Yingkou 115014, China), Huaxue Shiji, 2019,
Abstract: At present, heavy metal pollution is now very serious, so it is particularly important to identify and detect heavy metal ions. In this paper, the ligand ST-N was synthesized by the reaction of safranine T (ST) with 2-hydroxy-1-naphthalaldehyde (N). The ligand has a good selective recognition for Fe(III) in 18 common metal ions such as Hg(II), Pb(II), Ca(II), Fe(II), Fe(III), Co(II) in aqueous solution. The detection limit is 1 mg/L, which meets the detection standard of iron Fe(III) in Groundwater Quality Standard (GB/T 14848－2017). The detection limit is less than 2.0 mg/L. The RSD of Fe(III) was less than 1.17% and the recovery rate was between 95.7% and 103%.
Key words: safranine T; heavy metal ions; Fe(III); visible spectrophotometry
八氰钨-钴异金属配合物的合成、结构和理论研究
刘婷，姚瑶，金栋女，金杰，魏荣敏*
（德州学院 化学化工学院，山东省功能材料与配位化学高校重点实验室，山东 德州 253023）
摘要：以八氰钨为构筑单元，与过渡金属CoII离子合成了一个具有三维结构的八氰钨-钴配位聚合物CoII2(4-Mepy)8[WIV(CN)8] (4-Mepy ＝ 4-methylpyridine)。通过X-射线单晶衍射、元素分析和红外光谱对标题配合物进行了结构表征。单晶结构解析表明，标题配合物属于正交晶系，Fddd空间群，部分结晶学参数为：a ＝ 13.939(4)，b ＝ 26.397(7)，c ＝ 30.168(8) Å，V ＝ 11100(5) Å3，z ＝ 8，Dc ＝ 1.502 g/cm3，μ ＝ 2.711/mm，F(000) ＝ 5056，R ＝ 0.0468，wR ＝ 0.1062[I > 2σ(I)]。CoII离子中心均处于压缩CoN6八面体中，CoII和WIV离子通过4个CN基团与相邻异金属W彼此交替相连，形成三维网状结构。此外，基于密度泛函理论（DFT）对八氰钨-钴配位聚合物进行了量子化学计算，计算结果与实验吻合。
关键词：八氰钨；配合物；晶体结构；密度泛函理论
中图分类号：O614.8 文献标识码：A 文章编号：0258-3283（2019）--
Synthesis, Crystal Structure and Density Functional Theory Calculation on Octacyanotungstate(IV)-Bridged Cobalt Complex LIU Ting, YAO Yao, JIN Dong-Nv, JIN Jie, WEI Rong-Min*(School of Chemistry and Chemical Engineering, Dezhou University, Key Laboratory of Coordination Chemistry and Functional Materials in Universities of Shandong, Dezhou 253023) Huaxue Shiji, 2019, 41(7), ～
Abstract: The title complex with the general formula CoII2(4-Mepy)8[WIV(CN)8] (1, 4-Mepy ＝ 4-methylpyridine) has been synthesized and confirmed by single crystal X-ray diffraction, elemental analysis and infrared spectrum. Single crystal X-ray diffraction analysis reveals that it crystallizes in orthorhombic, Fddd space group with a ＝ 13.939(4), b ＝ 26.397(7), c ＝ 30.168(8)Å, V ＝ 11100(5)Å3, z ＝ 8, Dc ＝ 1.502 g/cm3, μ ＝ 2.711/mm, F(000) ＝ 5056, R ＝ 0.0468 and wR ＝ 0.1062 with I > 2σ(I). CoII ions lie in the center of the compressed [CoN6] octahedron in title complex, CoII and WIV ions are alternately bridged by cyano groups forming a three dimension bimetallic framework. The quantum calculation of the title complex has been performed by density functional theory method. The results of the calculation are consistent with the experiments.
Keywords: octacyanotungstate(IV), complex, crystal structure, DFT calculations
正交试验优选刺三加茎、叶中总多酚的提取工艺
及含量测定研究
高林晓*1, 2，郭蒙1，黄绍敏1，马考1，刘杰3，杨再波1, 2
（1. 黔南民族师范学院 化学化工学院，贵州 都匀 558000；2. 贵州省普通高校民族药用植物资源开发工程研究中心，贵州 都匀 558000；3. 山东新时代药业有限公司，山东 临沂 273400）
摘要：以刺三加茎、叶为原料，采用超声波辅助技术提取刺三加茎、叶中总多酚。通过单因素实验和正交试验优选了刺三加茎、叶中提取总多酚类物质的最佳工艺条件。结果表明，刺三加茎中总多酚的最佳提取工艺：乙醇体积分数45%、料液比1:35（g/mL）、提取时间50 min、提取温度45 ℃，总多酚平均含量为9.42 mg/g，提取率平均值为1.10%；刺三加叶中总多酚最佳提取工艺：乙醇体积分数45%、料液比1:10（g/mL）、提取时间70 min、提取温度50 ℃，总多酚平均含量为13.46 mg/g，提取率平均值为1.35%。刺三加茎、叶中加标平均回收率分别为98.13%和99.18%，相对标准偏差分别为1.35%和1.68%（n = 6）。该实验方法简便、可靠、准确，从而为进一步研究总多酚在实际生产中的应用提供了理论依据。
关键词：刺三加；超声提取；总多酚；正交试验；酒石酸亚铁比色法
中图分类号：R284.2 文献标识码：A 文章编号：0258-3283（2019）
Optimization of Extraction Technology by Orthogon Test and Determination of Total Polyphenol in Acanthopanan Trifoliatus Stems and Leaves GAO Lin-xiao*1, 2, GUO Meng1, HUANG Shao-min1, MA Kao1, LIU Jie3, YANG Zai-bo1, 2 (1. School of Chemistry and Chemical Engineering, Qiannan Normal College for Nationalities, Duyun 558000, China; 2. Engineering Research Center for Development of Ethnic Medicinal Plant Resources in Colleges and Universities of Guizhou Province, Duyun 558000, China; 3. Shandong New Time Pharmaceutical Co., Ltd, Linyi 273400, China), Huaxue Shiji, 2019,
Abstract: Using Acanthopanan trifoliatus stems and leaves as raw materials, the total polyphenols in the Acanthopanan trifoliatus stems and leaves were extracted by ultrasonic-assisted extraction. The optimum extraction conditions of total polyphenols from stems and leaves in the Acanthopanan trifoliatus were optimized by single factor experiment and orthogonal test. The results showed that the optimal extraction technology of total polyphenols in Acanthopanan trifoliatus stems was as follows: the volume fraction of ethanol was 45%, the ratio of material to liquid was 1:35(g/mL), the extraction time was 50 min, and the extraction temperature was 45 ℃. Under these conditions, the extraction rate of total polyphenol was the highest. The highest content of total polyphenols was 9.42 mg/g, and the average extraction rate of total polyphenols was 1.10%. The optimum extraction technology of total polyphenols in Acanthopanan trifoliatus leaves was as follows: the volume fraction of ethanol was 45%, the ratio of material to liquid was 1:10(g/mL), the extraction time was 70 min, and the extraction temperature was 50 ℃. The highest content of total polyphenols was 13.46 mg/g, and the average extraction rate of total polyphenols was 1.35%. The average recoveries were 98.13% and 99.18%, and the RSD (n = 6) were 1.35% and 1.68%, respectively. The method was simple, accurate and reliable. It was suitable for the determination of total polyphenols in the stems and leaves of Acanthopanan trifoliatus. Therefore, it provided a theoretical basis for further research on the application of total polyphenols in practical production.
Key words: Acanthopanan trifoliatus; ultrasonic extraction; total polyphenol; orthogonal test; ferrous tartrate colourimetry method
5-甲氧基-2,3-二甲基-1H-吲哚的合成
孙明娜1，周毅1，张培全1，王声1，孙明姣*2
（1.广州医科大学 药学院&附属第五医院，广东 广州 511436；2.杭州市肿瘤医院 肿瘤研究所，浙江 杭州 310002）
摘要：以5-甲氧基-2-甲基-1H-吲哚为原料，先后经Vilsmeier-Haack反应和还原反应制得标题化合物。5-甲氧基-2-甲基-1H-吲哚与DMF/POCl3反应生成5-甲氧基-2-甲基-1H-吲哚-3-甲醛，该中间体在氰基硼氢化钠/冰醋酸的催化下还原、脱水生成标题化合物，其结构经1H NMR、13C NMR、MS表征。该合成方法具有原料廉价易得、操作简便易控、反应条件温和、收率高等优点，标题化合物是一种重要的有机合成中间体，广泛用于医药领域。
关键词：5-甲氧基-2,3-二甲基-1H-吲哚；合成；5-甲氧基-2-甲基-1H-吲哚；氰基硼氢化钠
中图分类号：O626 文献标识码：A 文章编号：0258-3283（2019）
Synthesis of 5-Methoxy-2,3-dimethyl-1H-indole SUN Ming-na1, ZHOU Yi1, ZHANG Pei-quan1, WANG Sheng1, SUN Ming-jiao*2 (1. School of Pharmaceutical Sciences & the Fifth Affiliated Hospital, Guangzhou Medical University, Guangzhou 511436, China; 2. Institute of Cancer, Hangzhou Cancer Hospital, Hangzhou 310002, China), Huaxue Shiji, 2019, 41(7),
Abstract: 5-Methoxy-2,3-dimethyl-1H-indole is an important organic intermediate. In this work, 5-methoxy-2-methyl-1H-indole as the starting material was firstly converted to 5-methoxy-2-methyl-1H-indole-3-carbaldehyde via a Vilsmeier–Haack reaction. The latter intermediate was subjected to sodium cyanoborohydride and acetic acid in THF to synthesize the target compound, which was confirmed by 1HNMR、13CNMR and MS. This method has considerable advantages in terms of the use of easily available raw material, simple operation, mild reaction conditions and high yield.
Key words: 5-methoxy-2, 3-dimethyl-1H-indole; synthesis; 5-methoxy-2-methyl-1H-indole; sodium cyanoborohydride
磺酸功能化胆碱的制备及其在吲唑并[2,1-b]酞嗪-1,6,11-三酮合成中的应用
王英磊*，叶红勇，杜朝军，张群安
(南阳理工学院 生物与化学工程学院，河南 南阳 473004)
摘要：以氯化胆碱为主要原料，制备了一种环境友好型催化剂磺酸功能化胆碱。在磺酸功能化胆碱用量10%、反应温度80 ℃的条件下，不同取代基芳香醛与5, 5-二甲基-1,3-环己二酮（或1,3-环己二酮）和邻苯二甲酰肼在水相中顺利完成3组分“一锅煮”反应，以83% ～ 95%的产率合成了一系列目标化合物。该方法反应条件温和，底物普适性和官能团兼容性优良，后处理操作简便，催化剂重复利用6次后仍保持较高的催化活性，符合绿色化学与清洁生产的发展理念。
关键词：磺酸功能化胆碱；吲唑并[2,1-b]酞嗪-1,6,11-三酮；多组分反应；回收使用
中图分类号：TQ612.6 文献标识码：A 文章编号：0258-3283（2019）--
Preparation of Sulfonic Acid Functionalized Choline and Application on Synthesis of Indazolo[2,1-b]phthalazine-1,6,11-triones WANG Ying-lei*, YE Hong-yong, DU Chao-jun, Zhang Qun-an (School of Biological and Chemical Engineering, Nanyang Institute of Technology, Nanyang 473004, China) huaxue shiji, 2019, 41( 7), ～
Abstract： The environment-friendly catalyst of sulfonic acid functionalized choline was prepared with choline chloride as the main raw material. Under the conditions of 10 mol% of sulfonic acid functionalized choline dosage, 80℃ of reaction temperature, the one-pot three-component reaction of various aromatic aldehyde, 5,5-dimethyl-1,3 -cyclohexanedione (or 1,3-cyclohexanedione) and phthalhydrazide were completed successfully in water, for the synthesis of a series target compounds in yield of 83% ～ 95%. Several advantages such as mild reaction conditions, excellent substrate universality and functional group compatibility, simple post-treatment operation were offered and the catalyst still retains high activity after six times of recycling, which meet the development concept of green chemistry and cleaner production.
Keywords：sulfonic acid functionalized choline; indazolo[2,1-b]phthalazine-1,6,11-trione; multi-component reaction; reuse
6,7-二溴-1,4-二氢-1,4-环氧萘的合成研究
仝红娟*1, 2，贺新怀1, 2，唐文强1, 2，刘斌1, 2
(1.陕西国际商贸学院 医药学院，陕西 西安 712046；2．陕西省中药绿色制造技术协同创新中心，陕西 西安712046）
摘要：报道目标化合物的简便制备方法。以1,2,4,5-四溴苯为原料，在正丁基锂作用下形成不稳定的苯炔中间体，再与呋喃发生Diels-Alder反应得到目标化合物。产物结构经1HNMR、13CNMR和ESI-MS确证。通过对反应条件研究，确定最佳反应条件为：n （1, 2, 4, 5-四溴苯）：n（呋喃） ＝ 1：5，正丁基锂用量为1.2倍物质的量，反应溶剂为甲苯，室温反应30 min，产物收率为82.1 %。同时，该方法被用于6, 7-二甲氧基-1, 4-二氢-1, 4-环氧萘的合成，收率为77.6 %。
关键词：1,4-二氢-1,4-环氧萘；Diels-Alder反应；苯炔；合成
中图分类号：TQ463 文献标识码：A 文章编号：0258-3283（2019）--
Synthesis of 6,7-Dibromo-1,4-dihydro-1,4-epoxynaphthalene TONG Hong-juan*1,2, HE Xin-huai1,2, TANG Wen-qiang1,2, LIU Bin1,2 (1. School of Pharmacy, Shaanxi Institute of International Trade & Commerce, Xi’an 712046, China; 2. Collaborative innovation center of green manufacturing technology for traditional Chinese medicine in Shaanxi province, Xi’an 712046, China) Huaxue Shiji, 2019, 41(7)～
Abstract: The target compound was synthesized by an efficient and practical method from 1,2,4,5-tetrabromobenzene, involving benzyne forming in the presence of n-BuLi, then Diels-Alder reaction of benzyne with furan. The structure of the product was confirmed by 1HNMR, 13CNMR and ESI-MS. The optimal reaction conditions were investigated. The results showed that the target product was obtained in a yield of 82.1 % by the reaction of with n (1, 2, 4, 5-tetrabromobenzene)：n (furan) ＝ 1：5 in toluene as solvent, 1.2 times the amount of substance of n-BuLi was used at room temperature for 30 min. Also, 6, 7-dimethoxy-1, 4-dihydro-1, 4-epoxynaphthalene was obtained with this process in a yield of 77.6%.
Key words: 1,4-Dihydro-1,4-Epoxynaphthalene; Diels-Alder reaction; benzyne; synthesis
2-萘二硫醚制备新工艺研究
张瑞华，刘景辉*，乔开迪，胡国勤
（郑州大学 化工与能源学院，河南 郑州 450000）
摘要：以2-萘磺酰氯为原料，以碘化钾/亚硫酸氢钠/甲酸组成的还原体系制备标题化合物，产物的结构经1H NMR和13C NMR表征。通过单因素和正交试验，考察反应物物质的量比、反应温度、反应时间等对收率的影响，最终确定合成标题化合物的最优条件为：n（2-萘磺酰氯）:n（亚硫酸氢钠）=1:4、n(2-萘磺酰氯):n（甲酸）=1:3.5、n（2-萘磺酰氯）:n（碘化钾）= 1:2.5、水作为溶剂、反应温度为100 ℃、反应时间2.5 h，产品收率为69.7%，纯度可达96%以上。该方法原料易得、操作简单，并实现了对还原剂的部分循环利用，为工业化奠定了基础。
关键词：二硫化物；碘化钾；2-萘磺酰氯；优化
中图分类号：TQ46 文献标识码：A 文章编号：0258-3283（2019）
Synthesis of 2-Naphthalene Disulfide ZHANG Rui-hua，LIU Jing-hui*, QIAO Kai-di, HU Guo-qin （College of Chemical Engineering and Energy，Zhengzhou University，Zhengzhou 450000, China）, Huaxue Shiji, 2019, 41(7 ),
Abstract : 2-Naphthalene disulfide was prepared by 2-naphthalenesulfonyl chloride, and the raw material was reduced by the system consisting of potassium iodide, sodium hydrogen sulfite and formic acid. The structure of the product was confirmed by 1HNMR and 13CNMR. Via single factor and orthogonal experiments, the effects of the amount of raw materials, reaction temperature and reaction time on the yield were investigated. The optimal conditions for the synthesis of 2-naphthalene disulfide were as follows: n(2-naphthalenesulfonyl chloride)︰n(NaHSO3)=1︰4, n(2-naphthalenesulfonyl chloride):n(HCOOH)=1:3.5, n(2-naphthalenesulfonyl chloride): n(KI)= 1:2.5, water as a solvent, The reaction temperature is 100℃, the reaction time is 2.5 h, the product yield is 69.7%, and the purity is over 96%. The method has the advantages of easy availability of raw materials, simple operation, and partial recycling of the reducing agent, which lays a foundation for industrialization.
Key words: disulfide; potassium iodide; 2-naphthalenesulfonyl chloride; optimization
