Cu-SSZ-13分子筛氮氧化物SCR催化机理的研究进展
刘春红*1, 2，郑渭建1, 2，孙士恩1, 2，杜凯敏1, 2，胡晨晖1, 2，卓佐西1, 2，林贻超*3
(1. 浙江省火力发电高效节能与污染物控制技术研究重点实验室，浙江 杭州 311121；
2. 浙江浙能技术研究院有限公司，浙江 杭州 311121；
3. 中国科学院 宁波材料技术与工程研究所，浙江 宁波 315201)
摘要：Cu-SSZ-13分子筛对于氮氧化物（NOx）具有优异的选择性催化还原（SCR）活性，其使用温度窗口宽（200～500 oC），高N2选择性和水热稳定性，可应用于移动源或者固定源的尾气脱硝。然而Cu-SSZ-13分子筛的SCR催化反应机理非常复杂，相关研究进展缓慢，例如对于Cu催化位点的认识还不够全面且有争议。鉴于此，本文系统阐述并讨论了Cu-SSZ-13分子筛氮氧化物SCR催化机理的研究进展，着重介绍了Cu-SSZ-13分子筛中Cu位点的种类和在结构中的分布以及各自在SCR条件下所参与的化学反应，并对目前一些争议的实验结论进行归纳分析，以期为此类催化剂的设计提供参考。
关键词：Cu-SSZ-13分子筛；SCR；机理；氮氧化物；催化
中图分类号：TQ424.25 文献标志码：A 文章编号：0258-3283（2020）--
Progress in Mechanism of Selective Catalytic Reduction of NOx Over Cu-SSZ-13 Zeolite
LIU Chun-hong*1, 2, ZHEN Wei-jian1, 2, SUN Shi-en1, 2, DU Kai-min1, 2, HU Chen-hui1, 2, ZHUO Zuo-xi1, 2, LIN Yi-chao3（1. Zhejiang Provincial Key Laboratory of Energy Conservation & Pollutant Control Technology for Thermal Power, Hangzhou 311121, China; 2. Zhejiang Energy Group R&D Institute Co., Ltd., Hangzhou 311121, China; 3. Ningbo Institute of Materials Technology and Engineering, Chinese Academy of Sciences, Ningbo 315201, China) Huaxue Shiji, 2020, 42(12), ～
Abstract:Cu-SSZ-13 zeolite possesses excellent selective catalytic reduction (SCR) of NOx performance under a wide operating temperature range from 200 oC to 500 oC, high N2 selectivity and high hydrothermal stability, can be applied to reducing NOx in the exhaust of mobile and stationary sources. However, the SCR mechanism of Cu-SSZ-13 zeolite is very complicated and the research progress is slow. For example, the active Cu sites in Cu-SSZ-13 are not fully understood.Therefore，in this review, the SCR mechanism of Cu-SSZ-13 zeolite are summarized and discussed，and the Cu species in Cu-SSZ-13 structure, the their related reactions under SCR are emphasized，and the research debates are summarized and discussed, in the hope ofproviding a reference for the design of these catalysts.
Key words: Cu-SSZ-13 zeolite; SCR; Mechanism; NOx; catalysis
Cr2S3/CdS光催化剂制备及其产氢性能研究
郑炜山，何岸，余铮，赵增迎*
（中国地质大学（北京） 数理学院，北京 100083）
摘要：现代社会能源和环境问题促使以太阳能利用为目标的新能源研究成为热点。为了进一步提高光解水产氢催化剂CdS的性能，首先采用水热法制备了六方相CdS纳米晶体，然后将Cr2S3负载于CdS，制备了Cr2S3/CdS复合光催化剂。利用X射线衍射、扫描电镜、透射电镜、紫外可见吸收光谱、荧光光谱以及表面光电压谱等对样品的组成结构、微观形貌、光电性能，以及光解水产氢性能进行了测试表征。实验结果表明：当Cr/Cd物质的量比为0.8时，Cr2S3/CdS复合催化剂产氢效率达到533.7 μmol/h，是未复合CdS样品性能的1.8倍，性能改善的原因来自Cr2S3/CdS光吸收性能及光生电荷分离传输效率的提高。
关键词：Cr2S3；CdS；光解水产氢；水热法；复合光催化剂
中图分类号：TN104.3 文献标识码：A 文章编号：0258-3283（2020）
Preparation of Cr2S3/CdS Composite Photocatalyst and Its Hydrogen Production Performance
ZHENG Wei-shan, HE An, YU Zheng, ZHAO Zeng-ying* (School of Science, China University of Geosciences, Beijing 100083, China), Huaxue Shiji, 42(12)
Abstract：Energy and environmental problems in modern society have made the research of using solar energy become a hot spot. In order to further improve the hydrogen production efficiency of typical photocatalyst CdS, the CdS photocatalyst crystal was first prepared by hydrothermal method, and then the Cr2S3/CdS composite photocatalyst was prepared by hydrothermal reaction with chromic salt. The structure, morphology, optoelectronic properties and hydrogen production catalytic properties of the samples were characterized and tested by using X-ray diffractometer, scanning electron microscope, transmission electron microscope, UV-vis absorption spectrum fluorescence spectrometer, and surface photovoltage spectra, etc. The experimental results showed that when the Cr/Cd ratio was 0.8, the hydrogen production efficiency of the Cr2S3/CdS composite photocatalyst reached 533.7 μmol/h, which was 1.8 times that of the uncomposited CdS. The performance improvement is due to the improved light absorption performance of Cr2S3/CdS and the photogenerated charge separation transport efficiency.
Key words: chromium sulfide; cadmium sulfide; photocatalytic hydrogen production; hydrothermal method; composite photocatalyst
离子液体微乳液法合成Co-MOFs及其在甲苯催化氧化中应用
苏小燕，黄诚*，凡长坡，刘媛媛
（东南大学成贤学院 制药与化学工程学院，江苏 南京 210088）
摘要：室温条件下，在四元W/O型离子液体微乳液体系中制备了3种Co-MOFs纳米晶体，并表征了它们的结构和组成。为提高有机配体在水中的溶解度，选择DMF作为添加剂，从而保证Co-MOFs晶体在极性核中生长。通过调节离子液体与表面活性剂（TX-100）的质量比，有效地控制了样品的形貌和尺寸，并利用分子动力学模拟验证了该微乳体系对晶体形貌和尺寸控制的机理。同时，评价了该材料在甲苯选择性氧化反应中的催化性能。当离子液体与TX-100的质量比为1.5时，获得了由平均尺寸约为140 nm的纳米片聚集而成的晶体。该样品在甲苯氧化中表现出最佳的催化性能，其中甲苯转化率为14.5%，苯甲醛选择性为94.9%。
关键词：金属有机框架；控制合成；离子液体；微乳液法；催化氧化
中图分类号：O69 文献标识码：A 文章编号：0258-3283（2020）
Preparation of Co-MOFs by Ionic Liquid Microemulsion and Their Application in Catalytic Oxidation of Toluene
SU Xiao-yan, HUANG Cheng*, FAN Chang-po, LIU Yuan-yuan (Department of Chemical and Pharmaceutical Engineering, Southeast University Chengxian College, Nanjing 210088, China), Huaxue Shiji, 2020, 42(12)
Abstract: Three Co-MOF nanocrystals were prepared in a quaternary W/O microemulsion system at room temperature and characterized in detail. DMF was selected as additive to improve the dissolution of organic linker in water droplets and ensure the formation of Co-MOF crystals in polar core. The morphology and size of Co-MOFs were successfully controlled by adjusting the mass ratio of ionic liquid and TX-100. The mechanism of crystal growth in the microemulsion system was confirmed by molecular dynamic simulation. Meanwhile, the catalytic performance of these samples was studied in selective oxidation reaction of toluene. When the mass ratio of ionic liquid and TX-100 was 1.5, the aggregated crystal was obtained which cumulated by nanoplate with an average size of approximately 140 nm. This sample exhibited the best catalytic performance in toluene oxidation with 14.5% toluene conversion and 94.9% benzaldehyde selectivity.
Key words: metal-organic frameworks; controlled synthesis; ionic liquid; catalytic oxidation
烯酰吗啉·福美双超低容量喷雾剂的制备与应用
刘琴1，王晓宇1，韦昆1，李兴忠2，罗会*2
（1. 贵州大学 精细化工研究开发中心，贵州 贵阳 550025；2. 贵州省农业科学院果树科学研究所，贵州 贵阳 550006）
摘要：将烯酰吗啉、福美双原药溶解，依次加入磺酸盐类助剂和聚醚与嵌段聚醚类助剂，再加入油性溶剂与填料，搅拌均匀后，制备为透明均相稳定的烯酰吗啉·福美双超低容量喷雾油剂，该药剂符合超低容量喷雾油剂的质量要求。通过室内活性试验以及田间生物活性试验，评价了烯酰吗啉·福美双超低容量喷雾油剂对荔枝霜疫霉病的防治效果。室内生物活性试验结果表明，1%烯酰吗啉·福美双超低容量喷雾油剂对荔枝霜疫霉病菌具有显著的抑制作用，在浓度为100 μg/mL时，抑制率可达97.5%。此外，田间药效试验表明，1%烯酰吗啉·福美双超低容量喷雾油剂对荔枝霜疫霉病具有良好的防治效果，7 d防治效果为92.6%，是防治荔枝霜疫霉病的理想药剂。
关键词：烯酰吗啉；福美双；超低容量喷雾；荔枝霜疫霉病；田间药效试验
中图分类号：S436.67 文献标识码：A 文章编号：0258-3283（2020）
Preparation and Application of Dimethomorph Thiram Ultra-low Volume Spray
LIU Qin1, WANG Xiao-yu1, WEI Kun1, LI Xing-zhong2, LUO Hui*2 (1. Center for R&D of Fine Chemicals, Guizhou University, Guiyang 550025, China; 2.Guizhou Fruit Institute, Guizhou Academy of Agricultural Sciences, Guiyang 550006, China), Huaxue Shiji, 2020, 42(12)
Abstract: Add organic solvents to dimethomorph and thiram to completely dissolve them. Subsequently, sulfonate auxiliaries and polyether and block polyether additives are added to them, then the oily solvent and filler are added successively. The mixture is evenly mixed to prepare transparent, homogeneous and stable dimethomorph thiram ultra-low volume (ULV) spray oil agent. The agent meets the quality requirements of the ULV spray oil agent. Meanwhile, the effects of dimethomorph thiram ULV spray oil agent on Phytophthora lychee were evaluated by laboratory bioactivity tests and field efficacy trials. The results of laboratory bioactivity tests showed that 1% dimethomorph thiram ULV spray oil agent had a significant inhibition rate against Phytophthora lychee, and the inhibition rate was 97.5% when the concentration was 100 μg/mL. The field efficacy trials showed that dimethomorph thiram ULV spray oil agent had a od control effect on Phytophthora lychee, which reached 92.6% in 7 days.
Key words: dimethomorph; thiram; ultra-low volume spray; Phytophthora lychee; field efficacy trials
磺胺类药物金属配合物的研究进展
杜秀红*1，崔节虎2，刘隽1，行书丽1，石科1
（1. 河南医学高等专科学校 检验系，河南 郑州 451191；2. 郑州航空工业管理学院 环境功能材料重点实验室，河南 郑州 450015）
摘要：磺胺类药物配体因具有特殊的芳香环结构、丰富的配位原子以及良好的抗菌、抗癌药物活性等优势，成为新型金属配合物抗菌/抗癌药物研究的热点。重点综述磺胺类药物金属配合物的合成方法、配位模式、抗菌性能和抗癌性能的研究进展，探讨合适的合成方法、有效的配位模式、抗菌/抗癌作用规律等。通过对已报道磺胺类药物金属配合物的系统研究，为设计开发高效、低毒、抗耐药性的新型抗菌/抗癌药物奠定基础。
关键词：磺胺类药物；磺胺类药物金属配合物；抗菌；抗癌
中图分类号：O641.4 文献标识码：A 文章编号：0258-3283（2020）
Progress of Sulfonamides Metal Complexes
DU Xiu-hong*1, CUI Jie-hu2, LIU Jun1, XING Shu-li1, SHI Ke1 (1. Department of Laboratory Medicine, Henan Medical College, Zhengzhou 451191, China; 2. Key Laboratory of Environment Functional Materials, Zhengzhou University of Aeronautics, Zhengzhou 450015, China), Huaxue Shiji, 2020, 42(12)
Abstract：Sulfonamides ligands have the advantages of special aromatic ring structure, abundant coordination atoms, od antibacterial and anticancer biological properties, which make sulfonamides metal complexes become the research hotspot of new metal complexes in antibacterial/anticancer drugs. Synthesis methods, coordination patterns, antibacterial and anticancer properties of metal complexes of sulfonamides are reviewed. The suitable synthesis methods, effective coordination modes and antibacterial/anticancer action rule are explored. Through systematic study of the reported metal complexes of sulfonamides, the foundation is laid for the design and exploitation of new antibacterial/anticancer drugs with high efficiency, low toxicity and no drug resistance.
Key words: sulfonamides; sulfonamides metal complexes; antibacterial; anticancer
QuEChERS在动物源食品药物残留前处理方法的进展
刘权辉1,2，王彤彤1, 2，王敏*1,2，周剑1,2，杨梦瑞1,2
(1. 中国农业科学院农业质量标准与检测技术研究所，北京 100081；
2. 农业农村部农产品质量安全重点实验室，北京 100081)
摘要：近年来，随着食品安全问题逐渐成为大众关注的焦点，相关检测技术得到快速发展，在食品安全监管体系中处于越来越重要的地位。围绕QuEChERS方法在动物源食品的药物残留检测过程中的研究进展和应用现状进行综述，针对不同基质的特点以及采用的方法进行详细的讨论，并且对动物源食品的药物残留检测方法的未来发展状况进行了展望。能够推动QuEChERS方法在药物残留的研究中广泛的方法研究和应用，为后期检测人员开展实验提供宝贵的方法借鉴，并被逐渐扩展到其他领域的研究和检测中。
关键词: QuEChERS；动物源食品；药物残留；前处理方法；应用进展
中图分类号：S-1 文献识别码：A 文章编号：0258-3283（2020）
Progress of QuEChERS for Drug Residues in Animal-derived Foods
LIU Quan-hui1,2, WANG Tong-tong1,2, WANG Min*1,2, ZHOU Jian1,2, YANG Meng-rui1,2 (1. Institute of Quality Standard and Testing Technology for Agro-Products of Chinese Academy of Agricultural Sciences (CAAS), Beijing 100081, China; 2. Key Laboratory of Agri-food Safety and Quality, Ministry of Agriculture and Rural Affairs, Beijing 100081, China), Huaxue Shiji, 2020, 42(12)
Abstract: In recent years, with the food-safety occurrences continuously attracting public attentions, the related detection technologies have been developed rapidly. These technologies play a vital role in the vernment-supervision system. In this paper, we reviewed the progress and applications of QuEChERS methods for detection of drug residues in animal-derived foods, discussed the characteristics of different matrices and methods in detail, and prospected the development of detection methods for drug residues. This paper can promote the development and applications of QuEChERS methods in the determination of drug residues, provide valuable comparisons for laboratory technicians to carry out experiments, and gradually expand to other detection and research fields.
Key words: QuEChERS; animal derived-foods; pretreatment; application progress
氮氧自由基类化合物的生物活性研究进展
梁晶1,2，李晓丽2，秦向阳2，姚团利1，王玉琨*2
（1. 陕西科技大学 化学与化工学院，陕西 西安 710021；2. 空军军医大学 药学系，陕西 西安 710032）
摘要：综述氮氧自由基类化合物在生物活性研究方面的研究进展，为本领域研究者提供重要的借鉴和参考资料。以氮氧自由基（Nitroxide Radical）和Tempol为关键词在美国化学文摘（CA）数据库或者知网进行检索，查阅相关文献进行归类总结。稳定的有机氮氧自由基具有生物相容性和生物降解性好等优点。在生命科学研究中，氮氧自由基最初被用作阐明细胞膜结构和功能的自旋示踪剂。近年来，研究证明一些氮氧自由基分子具有广泛的生物活性，包括自由基清除、抗缺氧损伤、防辐射、抗肿瘤、抗缺血再灌注损伤、心肌保护、神经保护、抗炎镇痛等。
关键词：氮氧自由基；生物活性；抗肿瘤；抗辐射；抗缺血再灌注损伤
中图分类号：R914.4 文献标识码：A 文章编号：0258-3283（2020）
Research Progress of Biological Activities of Nitroxide Radical Compounds
LIANG Jing1,2, LI Xiao-li2, QIN Xiang-yang2, YAO Tuan-li1, WANG Yu-kun*2 (1. School of Chemistry and Chemical Engineering, Shaanxi University of Science and Technology, Xi'an 710021, China; 2. Department of Pharmacy, Air Force Medical University, Xi'an 710032, China), Huaxue Shiji, 2020, 42(12)
Abstract: The research progress of nitroxide radicals in the biological activity research was reviewed, and provided important reference and reference materials for researchers in the field. Using nitroxide radical and tempol as keywords was to search the American Chemical Abstracts (CA) database or CNKI, and referd to relevant documents for classification and summary. The stable organic nitroxide radicals have the advantages of biocompatibility and od biodegradability. In life science research, nitroxide radicals were originally used as spin tracers to clarify the structure and function of cell membranes. In recent years, studies have shown that some nitroxide free radical molecules have a wide range of biological activities, including free radical scavenging, anti-anoxic damage, radiation protection, anti-tumour, anti-ischemia-reperfusion injury, myocardial protection, neuroprotection, anti-inflammatory and analgesic and so on.
Key words：nitroxyl radicals; biological activity; anti-tumour; anti-radiation; anti-ischemia-reperfusion injury
广西不同产地兰香草总黄酮含量测定及抗氧化活性研究
陈美安*，林春花，郭庆，李宗泽，黄星海，梁雪，林群峰
（广西中医药大学 药学院，广西 南宁 530001）
摘要：以兰香草为研究对象，选择提取方式、提取溶剂、料液比和提取时间进行单因素实验，在单因素实验基础上，采用Box-Behnken 响应面法优化其总黄酮提取工艺，并测定广西不同产地兰香草总黄酮含量及评价其体外抗氧化活性。结果表明，最佳回流提取工艺为：乙醇浓度65%，料液比1:43 g/mL，提取时间89 min，1号兰香草总黄酮含量平均值为66.69 mg/g（RSD =0.02%, n=3）。10个不同产地兰香草总黄酮含量有所差异，其中，总黄酮含量最高的是宜州区，含量最低是武鸣县。不同产地兰香草总黄酮具有一定的总抗氧化能力，能够有效地清除DPPH自由基，效果弱于同浓度条件下VC。总黄酮含量与总抗氧化能力、清除DPPH自由基能力均无显著相关性(P>0.05)。
关键词：兰香草；总黄酮；含量；响应面法；抗氧化活性
中图分类号：R284 文献标识码：A 文章编号：0258-3283（2020）
Study on the Total Flavonoids Content Determination and Antioxidant Activity of Caryopteris incana (Thunb. ) Miq. from Different Areas in Guangxi
CHEN Mei-an*, LIN Chun-hua, GUO Qing, LI Zong-ze, HUANG Xing-hai, LIANG Xue, LIN Qun-feng (College of Pharmacy, Guangxi University of Chinese Medicine, Nanning 530001, China), Huaxue Shiji, 2020, 42(12)
Abstract: Single factor experiments were carried out by choosing extraction mode, extraction solvent, solid-liquid ratio and extraction time from Caryopteris incana (Thunb. ) Miq.. Based on the results of single factor experiment, the Box-Behnken response surface methodology was used to optimize the extraction process of total flavonoids, and the contents of total flavonoids in Caryopteris incana (Thunb. ) Miq. from different areas of Guangxi province was determined and their antioxidant activities in vitro were compared and evaluated. The results showed that the optimal reflux extraction process were as followed : ethanol concentration 65%, solid-liquid ratio 1:43 g/mL and extraction time 89 min. Under these conditions, the the average content of total flavonoids of Caryopteris incana (Thunb.) Miq. No.1 were 66.69 mg/g (RSD = 0.02%, n = 3). The content of total flavonoids of Caryopteris incana (Thunb.) Miq. from ten different areas were varied. Among them, the highest content of total flavonoids was from Yizhou, the lowest content was from Wuming. The total flavonoids of Caryopteris incana (Thunb.) Miq. from different areas had a certain total antioxidant capacity, and they could scavengeg DPPH radical effectively, which were all weaker than the same concentration of vitamin C. There was no significant correlation between total flavonoids content and the total antioxidant capacity and the scavenging activity on DPPH radical (P > 0.05).
Key words: Caryopteris incana (Thunb. ) Miq.; total flavonoids; content; response surface methodology; antioxidant activity
谷风*a,b，翦英红a,b，刘虹a
（吉林化工学院 a. 资源与环境工程学院，b. 水处理吉林省重点工程研究中心，吉林 吉林 132022）
摘要:以盐酸酸化凹凸棒土为脱色剂，对废食用油进行脱色。通过单因素试验找到最佳脱色条件，并在此基础上，以凹凸棒土盐酸酸化浓度、酸化凹凸棒土使用量、脱色温度、脱色时间为考察因素，以废食用油脱色率为响应参数，使用响应面方法进行优化设计。结果表明，在最优化状态下的脱色条件为：脱色剂（酸化凹凸棒土）酸化浓度3.0 mol/L、脱色剂（酸化凹凸棒土）使用量15.6%、脱色温度111.0 ℃、脱色时间23.0 min，在此条件下测得废食用油脱色率最高可达87.63%，脱色后的废食用油接近无色。该方法耗费低廉、简便高效，脱色剂容易再生利用、对环境友好，可用于废弃油脂资源化利用的前期处理。
关键词：废食用油; 酸化凹凸棒土; 脱色; 脱色率; 响应面优化
中图分类号：TS224.2 文献标识码：A 文章编号：0258-3283（2020）
Optimization of Decolorization Process of Waste Edible Oil by Response Surface Methodology
GU Feng*a,b, JIAN Ying-hong a,b, LIU Honga (a. School of Resources and Environmental Engineering, b. Jilin Key Engineering Research Center of Water Treatment, Jilin Institute of Chemical Technology, Jilin 132022, China), Huaxue Shiji, 2020, 42(12)
Abstract: Using attapulgite as decolorizing agent, the waste edible oil was decolorized. The optimum decolorization conditions were found by single factor test, and on this basis, the response surface method was used to optimize the design of attapulgite acidizing concentration, acidizing attapulgite usage, decolorization temperature and decolorization time. The results showed that the decolorization conditions were as follows: decolorizer (acidizing attapulgite) acidizing concentration 3.0 mol/L, decolorizer (acidizing attapulgite) use 15.6%, decolorization temperature 111.0 ℃, decolorization time 23.0 min. Under this condition, the decolorization rate of waste edible oil can reach 87.63%, and the waste edible oil after decolorization is close to colorless. The method is cheap, simple and efficient, easy to reuse and environment-friendly, and can be used in the early treatment of waste oil resource utilization.
Key words: waste edible oil; acidified attapulgite; tarnish; decolorization rate; response surface optimization
多维色谱技术快速检测电子气中痕量气体杂质的方法研究
魏王慧，董翊，于瑞祥，陈鹰，姜阳，任逸尘，高艳秋*
（上海市计量测试技术研究院，上海 201203）
摘要：采用多维气相色谱，通过不同色谱柱的组合变换、配合反吹、中心切割等操作技术，分别对六氟化硫、四氟化碳、氢气3种电子气中的6～7种杂质检测进行了方法开发。使用气体稀释法做出了5个浓度下氢气中各组分的响应校准曲线，线性良好，最低浓度点0.05×10-6 mol/mol时的RSD均小于10%。系统地描述了3种电子气检测方法的开发过程和经验技巧，计算了检出限，均远好于市场检测需求，其中六氟化硫各组分检出限在20×10-9～30×10-9 mol/mol，四氟化碳各组分检出限在16×10-9～26×10-9 mol/mol，氢气各组分检出限在8×10-9～16×10-9 mol/mol，方法重复性好、检测效率高，可作为标准操作规范向社会开放共享。
关键词：多维色谱；电子气；杂质；反吹；中心切割
中图分类号: O657.71 文献标识码: A 文章编号：0258-3283（2020）
Research on the Method of Rapid Detection of Trace Gas Impurities in Electronic Degrade Gas by Multidimensional Chromatography
WEI Wang-hui, DONG Yi, YU Rui-xiang, CHEN Ying, JIANG Yang, REN Yi-chen, GAO Yan-qiu* (Shanghai Institute of Measurement and Testing Technology, Shanghai 201203, China), Huaxue Shiji, 2020, 42(12)
Abstract：In this essay, the multi-dimensional gas chromatography was used, as long as the back-flush and center cut technology, to developing the analyzing method of 6～7 impurities in three electronic grade gases: sulfur hexafluoride, carbon tetrafluoride and hydrogen with the combination of different chromatographic columns. The gas dilution method was used to make a response calibration curve for each component in hydrogen at 5 concentrations. The linearity was od, and the RSD at the lowest concentration point of 0.05×10-6 mol/mol was less than 10%. The development process and experience skills of three electronic grade gas analysis methods were systematically described. The limits of detection were calculated, which are far better than the market detection requirements. The detection limits of each component were 20×10-9～30×10-9 mol/mol, 16×10-9～26×10-9 mol/mol and 8×10-9～16×10-9 mol/mol for sulfur hexafluoride, carbon tetrafluoride and hydrogen, respectively. The methods had od repeatability and high detection efficiency, and could be shared with the society as a standard operating specification.
Key words: multi-dimensional chromatography; electronic grade gas; impurity; back-flush; center-cut
基于PET原理的FAM标记核酸适配体的汞离子检测研究
张华伟，赵晗，于丽佳*
（国家卫生健康委职业安全卫生研究中心，北京 102308）
摘要：汞作为毒性最大的重金属之一，在环境中难以降解。利用光致诱导电子转移（PET）原理设计单端荧光标记核酸适配体的用于汞离子检测研究。采用分子荧光光谱进行表征，激发波长490 nm,发射光谱范围为516～650 nm。在适配体5’末端修饰鸟嘌呤(G)碱基作为荧光萃灭基团，在3'末端修饰荧光素（FAM）基团。加入汞离子后，无规则卷曲单链形成茎环结构双链，G碱基与FAM接近产生PET效应荧光萃灭。在此体系中，线性范围为3～9 nmol/L，检测限为0.15 nmol/L，可在自来水中检测Hg2+，回收率82.5%～98%。具有较高的灵敏度和特异性，操作方法简单。
关键词：汞离子；适配体探针；光致诱导电子转移；茎环结构；荧光策略
中图分类号: O657.31 文献标识码: A 文章编号：0258-3283（2020）--
Study on Mercury Ion Detection of FAM Labeled Aptamers Based on PET Principle
ZHANG Hua-wei, ZHAO Hao, YU Li-jia* (National Center for Occupational Safety and Health, NHC, Beijing 102308, China), Huaxue Shiji, 2020, 42(12), ～
Abstract: Mercury as one of heavy metals is high toxic to human health, which is difficult to degrade in the environment. Based on photoinduced electron transfer principle, a mercury detection probe consisting of a fluorescent labeled nucleic acid aptamer (HgAP) was designed. The fluorescence spectra was adopted with excitation wavelength 490 nm and emission wavelength range from 516 nm to 650 nm. Guanine (G) base was modified at the 5'-end of HgAP as fluorescence extraction group, and at the 3'-terminus as the FAM. After the addition of mercury ion, the irregular coil single chain formed the stem ring structure double chain, and the G base was close to FAM, resulting in PET fluorescence extraction. The linear range was 3-9 nmol/L and the detection limit was 0.15 nmol/L. This method could test Hg2+ in tap water with recovery rate rang from 82.5-98%. It has high sensitivity and specificity, and the operation method is simple.
Key words: mercury; aptamer probe; photoinduced electron transfer; stem-loop structure; fluorescence strategy
电子级掺杂锑扩散源锑含量的测定
孟宪冬，孟蓉，王连旺*
（北京化学试剂研究所有限责任公司，北京 102607）
摘要：建立了微波消解-溴酸钾法测定电子级掺杂锑扩散源锑含量的测试方法。在样品中加入盐酸（无硝酸根），经过微波消解，用盐酸（无硝酸根）控制酸度，滴定时温度为70 ～ 90℃，以甲基橙为指示剂，用溴酸钾标准滴定溶液直接滴定锑扩散源中锑含量。试验表明，该方法回收率为99.20% ～ 100.24%，相对标准偏差(RSD，n = 6)为0.073% ～ 0.10%，分析结果稳定、准确度高，适用于高分子材料有机锑扩散源常量滴定分析，能够满足电子级掺杂锑扩散源的分析检测要求。方法快速准确，具有良好的经济效益和社会效益。
关键词：微波消解；溴酸钾法；氧化还原；有机锑；常量分析
中图分类号：O652.1 文献标识码：A 文章编号： 0258-3283（2020）
Determination of Antimony Content in Electronic Grade Antimony Spin-on Dopant
MENG Xian-dong, MENG Rong, WANG Lian-wang* (Lnstitute of Chemical Reagents Co. Ltd., Beijing 102607, China), Huaxue Shiji, 2020, 42(12)
Abstract: A method for the determination of antimony content in electronic grade antimony spin-on dopant by microwave digestion-potassium bromate method was established. Hydrochloric acid (nitrate free) was added to the sample, after microwave digestion, the acidity was controlled by hydrochloric acid(nitrate free), and the temperature during titration was 70~90°C, methyl orange as indicator, the antimony content in electronic grade antimony spin-on dopant was directly titrated with standard titration solution of potassium bromate. Test results showed that the recovery rate of the method was 99.20%~100.24%, the relative standard deviation was (RSD，n = 6) 0.073%~0.10%, the analysis result was stable and the accuracy was high. The method is suitable for the constant titration analysis of organic antimony spin-on dopant polymer materials, it can meet the analysis and detection requirements of electronic grade antimony spin-on dopant. The method is rapid and accurate, and has od economic and social benefits.
Key words: microwave digestion; potassium bromate method; oxidation reduction; organic antimony; constant analysis
甲基肼和偏二甲肼水含量标准物质的研制及不确定度评定
赵坦*1，钟秋1，徐林楠1，侯倩倩2，李俊1，方涛1
（1. 北京航天试验技术研究所, 北京 100074；
2. 中国兵器工业集团第五三研究所，山东 济南 250031)
摘要：建立了甲基肼（MMH）和偏二甲肼（UDMH）水含量标准物质制备方法及不确定度评定模型。采用预先测定的低水含量MMH和UDMH为原料，并通过向其中加入纯水的方式，制备出符合拟研制标准物质技术指标要求的标物样品。改进了现有气相色谱法，采用液体水分标准物质校正法作为定值方法，解决了配制标准物质的溯源性问题。均匀性和稳定性考察结果表明，所制备的标准物质均匀性良好，有效期12个月。联合八家实验室开展标物赋值，结合定值、均匀性和稳定性考察结果进行不确定度评估，扩展不确定度均不超过0.04%。该标准物质可用于MMH和UDMH水含量的准确快速定值及专用测试设备的性能检验。
关键词：甲基肼；偏二甲肼；水含量；标准物质；不确定度
中图分类号：O657.7 文献标识码：A 文章编号：0258-3283(2020)--
Preparation of Reference Material of Water Content in Methylhydrazine and Unsymmetrical Dimethylhydrazine and Evaluation for Uncertainty
ZHAO Tan*1, ZHONG Qiu1, XU Lin-nan1, HOU Qian-qian2, LI Jun1, FANG Tao1 (1. Beijing Institute of Aerospace Testing Technology, Beijing 100074, China; 2. Institute 53 of China Ordnance Industry Group, Jinan 250031, China), Huaxue Shiji, 2020, 42(12), ～
Abstract: The preparation method of reference material of water content in methylhydrazine (MMH)and unsymmetrical dimethylhydrazine(UDMH)and uncertainty evaluation model of was established. Using the pre-determined low water content MMH and UDMH as raw materials, and by adding pure water to it, prepare a standard sample that meets the technical requirements of the proposed standard substance. The existing gas chromatography method is improved, and the liquid moisture standard substance correction method is used as the setting method to solve the traceability problem of the prepared standard substance. The inspection results of uniformity and stability show that the prepared standard material has od uniformity and is valid for 12 months. Combined with eight laboratories to carry out standard assignment, combined with the evaluation results of fixed value, uniformity and stability to evaluate the uncertainty, the expanded uncertainty does not exceed 0.04%. The standard material can be used for accurate and rapid determination of the water content of MMH and UDMH and the performance test of special test equipment.
Key words: MMH; UDMH; water content; reference material; uncertainty
酰胺醇类混合标准溶液的稳定性研究
黄鸾玉*，吴祥庆，韦信贤，杨姝丽，吴明媛，罗旭
（广西水产科学研究院，广西 南宁 530021）
摘要：建立甲醇中酰胺醇类混合标准溶液的稳定性评定方法，使用液相色谱串联质谱法精确测定混合标准溶液中各标准物质浓度随储存条件及储存时间的变化。结果表明，制备的混合标准溶液均匀性良好，各标准物质F值均小于95%的置信水平下的理论临界值；酰胺醇类混合标准溶液热稳定性不好，在40 ℃存储条件下降解较明显，浓度越低降解率越高；配置浓度高的混合标准溶液，在运输过程中避光并采取冰袋或其他控温措施，更易于保持其稳定性；该混合标准溶液在4 ℃避光储存6个月，其浓度值基本保持稳定，6个月以后浓度值呈现下降趋势。该混合标准溶液可用于食品和环境的残留检测及相关分析方法的确认与评价，有效期为6个月。
关键词：酰胺醇类；混合标准溶液；标准物质；液相色谱-串联质谱法；稳定性
中图分类号：O657.7 文献标志码：A 文章编号：0258-3283(2020)--
Stability Study of Amphenicols in Methanol as Certified Reference Materials
HUANG Luan-yu*, WU Xiang-qing, WEI Xin-xian, YANG Shu-li, WU Ming-yuan, LUO Xu (Guangxi Academy of Fishery Sciences, Guangxi Nanning 530021, China), Huaxue Shiji, 42(12), ～
Abstract: A method for the stability evaluation of amphenicols mixed standard solution in methanol was established.Each standard substance in the mixed standard solution was accurately determined by liquid chromatography tandem mass spectrometry(LC/MS/MS)in different storage conditions and different storage time. The results showed that the mixed standard solution had od uniformity and the F value of each standard substance was less than the theoretical critical value under the 95% confidence level. The heat stability of the mixed standard solution was bad, it was more obvious at 40℃. The lower concentration had the higher degradation rate. Mixed standard solution with high concentration, avoid light and take ice packs in transit or other measures for temperature controlling can easier to maintain its stability. The mixed standard solution was well stable in 6 months after being stored in dark at 4℃. After more than 6 months, with the extension of storage time, the concentration showed a downward trend.The mixed standard solution can be used for food and environmental residue detection, identification and evaluation of the correlation analysis method,and the validity is 6 months.
Key words: amphenicols; mixed standard solution; reference material; liquid chromatography-tandem mass spectrometry; stability
烤甘薯浸膏提取工艺优化及香味成分分析
郑美玲1，杨金初2，朱远洋1，许克静2，张文洁1，张峻松*1
（1. 郑州轻工业大学 食品与生物工程学院，河南 郑州 450001；2. 河南中烟工业有限责任公司 技术中心，河南 郑州 450000）
摘要：为提升烤甘薯浸膏香气品质和作用特征，利用气相色谱-质谱法(GC-MS)确定了烤甘薯浸膏香味成分，并以其含量为考察指标，通过单因素试验和正交试验优化得到烤甘薯浸膏的最佳提取工艺，并对烤甘薯浸膏香气进行感官评价。结果表明：烤甘薯的最佳提取工艺条件为乙醇体积分数90%，料液比1:8，超声功率200 W，超声温度35 ℃，超声时间30 min；该工艺条件下得到的烤甘薯浸膏香味成分主要包括呋喃类（51.24%）、呋喃酮类（9.42%）、吡喃酮类（14.43%），总含量为23.77 mg/g；该提取方式下得到的烤甘薯浸膏能够保留直接烘烤的特征香韵物质，烤甜香浓郁。
关键词：烤甘薯浸膏；超声辅助萃取；正交试验；香味成分
中图分类号：TS41 文献标识码：A 文章编号：0258-3283（2020）--
Optimization of Extraction Process and Analysis of Aroma Components of Roasted Sweet Potato Extract
ZHENG Mei-ling1, YANG Jin-chu2, ZHU Yuan-yang1, XU Ke-jing2, ZHANG Wen-jie1, ZHANG Jun-song*1 (1. College of Food and Bioengineering, Zhengzhou University of Light Industry, Zhengzhou 450001, China; 2. Technology Center, China Tobacco Henan Industrial Co., Ltd., Zhengzhou 450000, China), Huaxue Shiji, 2020, 42(12)
Abstract: In order to improve the aroma quality and functional characteristics of roasted sweet potato extract, the aroma components of roasted sweet potato extract were determined by gas chromatography-mass spectrometry (GC-MS), and the optimal extraction process of roasted sweet potato extract was obtained by single factor test and orthonal test, and the aroma of roasted sweet potato extract was evaluated by sensory evaluation. The results showed that: (1) the optimum extraction conditions were as follows: ethanol volume fraction 90%, solid-liquid ratio 1:8, ultrasonic power 200 W, ultrasonic temperature 35 ℃ and ultrasonic time 30 min; (2) the main aroma components of roasted sweet potato extract were furans (51.24%), furanone (9.42%), pyranones (14.43%), and the total content was 23.77% mg·g-1; (3) the roasted sweet potato extract obtained by this extraction method can retain the characteristic aroma substances of direct baking, and the roasted sweet flavor is rich.
Key words: roasted sweet potato extract; ultrasonic-assisted extraction; orthonal test; aroma components
对称四芳基乙烯衍生物的合成与性质研究
王静*1，余欢2，王银柳1，王倩1
(1. 商丘师范学院 化学化工学院，河南 商丘 476000；2. 商丘市第二高级中学，河南 商丘 476000)
摘要：以二苯甲酮衍生物为原料，经McMurry偶联反应合成得到对称的四芳基乙烯衍生物，其结构经1HNMR、13CNMR、MS及元素分析表征。新分子的聚集诱导发光性能均优于四苯乙烯。在聚集态，荧光寿命都超过3 ns，其中TPE-4OBz达到5.93 ns。新分子都具有较高的固体荧光量子产率，其中TPE-4Me可达45.54%。以上研究说明取代基的引入提高了分子的聚集诱导发光性能，为进一步的应用研究提供可能。单晶结构显示，TPE-4Me具有螺旋桨构型，为发光机理研究提供模型。
关键词：四芳基乙烯；聚集诱导发光；Mcmurry偶联反应；合成；光学性质
中图分类号：O625.1 文献标识码：A 文章编号：0258-3283（2020）--
Synthesis and Characterization of Symmetrical Tetra-aryl Ethene Derivatives
WANG Jing*1, YU Huan2, WANG Yin-Liu1, WANG Qian1 (1. Department of Chemistry Chemical Engineering, Shangqiu Normal University, Shangqiu 476000, China; 2. Shangqiu Second Senior High School, Shangqiu 476000, China), Huaxue Shiji, 2020, 42(12)
Abstract：New symmetrical tetra-aryl ethene derivatives were designed and synthesized by McMurry coupling reaction from benzophenone derivatives. The structure and purity of all the new compounds were confirmed by 1H、13C NMR spectra and MS associated with elemental analysis. All the new compounds showed aggregation-induced emission property which were better than tetraphenylethene. The PL lifetime of all aggregated samples were lengthened to more than 3 ns, indicating that the nonradiative pathway may be blocked in aggregate states. The PL lifetime of TPE-4OBz can reach to 5.93 ns. The solid fluorescence quantum yields were improved, which was 45.54% of TPE-4Me. These results indicated that the different substitutions improved the aggregation-induced emission property, which provided the possibility of application. Single crystals of TPE-4Me is propeller configuration, which provides a model for the research of aggregation-induced emission mechanism.
Key words：tetra-aryl ethene; aggregation-induced emission; McMurry coupling reaction; synthesis; optical property
3-碘-6-氯咪唑并[1, 2-b]哒嗪的合成研究
程伟1，张向龙2，陈启绪1，袁文鹏*1
（1. 齐鲁工业大学（山东省科学院） 山东省科学院菏泽分院 山东省生物工程技术创新中心，山东 菏泽 274000；2. 山东友帮生化科技有限公司 山东省小分子杂环化合物工程实验室，山东 菏泽 274000）
摘要：标题化合物是一种重要的药物中间体，广泛应用于抗癌药物、抗病毒药物和抗感染药物的生产。为了优化其合成路线，以水合肼和马来酸酐为起始原料，在酸催化下发生缩合反应，再用三氯氧磷进行氯化，与氨水发生氨解反应，再与氯乙醛进行关环缩合，最后与NIS发生碘代共5步反应合成，总产率为58.7%。产物结构经1H NMR、13CNMR确证。与已有的文献方法相比，报道的合成路线具有化学选择性好、操作简便、产率高、避免柱层析分离、利于放大生产的特点。
关键词：水合肼；马来酸酐；3-碘-6-氯咪唑并[1, 2-b]哒嗪；合成
中图分类号：R914.5 文献标识码：A 文章编号：0258-3283（2020）
Synthesis of 3-Iodo-6-chloroimidazo[1, 2-b]pyridazine
CHENG Wei1, ZHANG Xiang-long2, CHEN Qi-xu1, YUAN Wen-peng*1 (1. Biological Engineering Technology Innovation Center of Shandong Province, Heze Branch, Qilu University of Technology (Shandong Academy of Sciences), Heze 274000, China; 2. Shandong Engineering Laboratory of Small Molecule Heterocyclic Compounds, Shandong Youbang Biochemical Technology Co., Ltd., Heze 274000, China), Huaxue Shiji, 2020, 42(12)
Abstract: The title compound is an important intermediate of drugs, which can be widely used in the production of anti-virus drugs, anti-cancer drugs and anti-infective drugs. In order to optimize its synthetic route, taking hydrazine hydrate and maleic anhydride as the raw materials, the synthesis gradually went through the following five-step reaction processes with the total yield of 58.7%: condensation reaction catalyzed by acid, chlorination with phosphorus oxychloride, ammonolysis with ammonia water, ring-closing condensation with chloroacetaldehyde, and iodization with NIS. The structure was confirmed by 1H NMR and 13CNMR. Compared with the reported synthetic routes, the protocol takes the advantages of od chemical selectivity, easy operation, high yield, avoiding column chromatography separation and suited for scale-up production.
Key words: hydrazine hydrate; maleic anhydride; 3-iodo-6-chloroimidazo [1,2-b] pyridazine; synthesis
7-卤代-1-茚酮类化合物的合成研究
马俊钥，牟芃兴，曹国锐*
（青岛科技大学 化工学院，山东 青岛 266042）
摘要：研究了标题化合物的新合成方法，以茚酮为原料，经硝化、硝基还原、卤代以及重氮化反应合成标题化合物。探讨了硝化反应中硫酸和硝化剂的用量对产率的影响，当n (硫酸)∶n (6-硝基-茚酮) = 37.5∶1.0、n (硝酸钾)∶n (6-硝基-茚酮) = 1.2∶1.0时，硝化反应产率最高，达到66.0%。优化了重氮化反应中亚硝酸钠、盐酸和次磷酸用量，当n (亚硝酸钠)∶n (6-氨基-7-卤代-茚酮) = 1.3∶1.0、n (盐酸)∶n (6-氨基-7-卤代-茚酮) = 3∶1、n (次磷酸)∶n (6-氨基-7-卤代-茚酮) = 13∶1时，重氮化反应产率最高，可达到84.8%。此方法反应路线短、操作简便、反应条件温和、适用范围广。
关键词：7-卤代-1-茚酮；6-硝基-茚酮；6-氨基-7-卤代-茚酮；硝化反应；重氮化反应
中图分类号：O625.29 文献标识码：A 文章编号：0258-3283（2020）
Study on the Synthesis of 7-Halo-1-indanones
MA Jun-yue, MU Peng-xing, CAO Guo-rui* (College of Chemistry Engineering, Qingdao University of Science and Technology, Qingdao 266042, China), Huaxue Shiji, 2020, 42(12)
Abstract：A new synthetic method of the title compounds was studied. The target product was synthesized from indone by nitration, reduction reaction, halogenation and diazotization reaction. The effects of the amount of sulfuric acid and nitrating agent on the reaction yield were discussed. When n (sulfuric acid) : n (6-nitro -indanone) = 37.5 : 1.0, n (potassium nitrate) : n (6-nitro-indanone) = 1.2 : 1.0, the yield of the nitrification reaction was the highest, which could reach 66.0%. The amount of sodium nitrite, acid and hypophosphorous acid in the diazotization reaction was optimized. When n (sodium nitrite) : n (6-amino-7-halo-indanone) = 1.3 : 1.0, n (hydrochloric acid) : n (6-amino-7-halo-indanone) = 3 : 1, n (hypophosphorous acid) : n (6-amino-7-halo-indanone) = 13 : 1, the diazotization yield is the highest, which can reach 84.8%. This method has a short reaction route, mild conditions, and a wide range of applications.
Key words：7-halo-1-indanones; nitrification; diazotization reaction
2-取代7-(N, N-二乙胺基)-4-羟甲基香豆素的合成方法改进
孙立梅a，马星光a，许永娣a，董原辰b，孙亚伟*a
（a. 中国石油大学 化学工程学院，山东 青岛 266580；b. 中国科学院化学研究所，北京 100190）
摘要：以7-(N, N-二乙氨基)-4-(羟甲基)香豆素为原料，经醚化、硫代、缩合和脱保护等4步反应，以较高产率得到一系列2-位修饰的7-(N, N-二乙氨基)-4-(羟甲基)香豆素，该类化合物可用于制备一系列可见光波段响应的光保护试剂。在该类化合物的合成改进中，采用丁基醚来保护香豆素4位上的羟甲基，避免了硫代过程中副反应的发生，并且以有机碱替代硝酸银和氧化铅等重金属盐，以高效、简洁的操作实现了目标分子的制备，为大规模生产该类化合物提供了新的方法。
关键词：香豆素；封端化合物；可见光
中图分类号：O629.74 文献标识码：A 文章编号：0258-3283（2020）
Improved Synthesis of 2-Substituted 7-(N, N-Diethylamino)-4-(hydroxymethyl) Coumarin
SUN Li-meia, MA Xing-guanga, XU Yong-dia, DONG Yuan-chenb, SUN Ya-weia* (a. College of Chemical Engineering, China University of Petroleum, Qingdao 266580, China; b. Institute of Chemistry Chinese Academy of Science, Beijing 100190, China), Huaxue Shiji, 2020, 42(12)
Abstract：A new method of 3’, 5’-diaminedeoxynucleoside’s synthesis was reported by using the combination of Mitsunobu reaction and Staudinger reduction, the hydroxy group on 2’-deoxynucleoside was transfer to amino group with the ribose’s configuration maintained. Non-explosive diphenylphosphoryl azide was utilized as azide source to replace toxic sodium azide, and triphenylphosphine was chosen as in situ reductant in azide to amine’s conversion. The whole process is easy to handle and no hazard reagents was used, provids us new choice in 3’, 5’ –diaminedeoxynucleosides’ synthesis.
Key words: coumarin; caged compounds; visible light
双氧水/钨酸钠高效催化氧化制备邻二硝基甲苯
张敏，刘红利，刘影，葛忠学，丁可伟，翟连杰，朱勇*
（西安近代化学研究所，陕西 西安 710065）
摘要：为提供一种高收率、高纯度的2,3-二硝基甲苯及3,4-二硝基甲苯的合成方法，以双氧水/浓硫酸为氧化体系，钨酸钠为催化剂，2-甲基-6-硝基苯胺、4-甲基-2-硝基苯胺分别为原料，通过催化氧化探索了两种邻二硝基甲苯的合成方法，收率分别为93.5%和92.3%，纯度为98.8%和99.2%。利用红外光谱、核磁共振谱及元素分析对其结构进行了表征，分别考察了不同的氧化体系、反应温度、反应时间、氧化剂用量和催化剂用量等因素对收率和纯度的影响，获得了合成2,3-二硝基甲苯和3,4-二硝基甲苯的最佳工艺条件。并对催化氧化反应机理进行了推测。利用DSC对化合物的热稳定性进行了分析，结果表明：2,3-二硝基甲苯及3,4-二硝基甲苯的熔点分别为63.66、65.16 ℃，气化起始温度分别为169.5、148.16 ℃。
关键词：钨酸钠；过氧化氢；二硝基甲苯；催化氧化；氧化体系
中图分类号：TJ55 文献标识码：A 文章编号：0258-3283（2020）
Synthesis of Dinitrotoluene by Highly Efficient Catalytic Oxidation in H2O2 /Na2WO4 System
ZHANG Min, LIU Hong-li, LIU Ying, GE Zhong-xue, DING Ke-wei, ZHAI Lian-jie, ZHU Yong* (Xi’an Modern Chemistry Research Institute, Xi’an 710065, China), Huaxue Shiji, 2020, 42(12)
Abstract: Synthesis of 2, 3-dinitrotoluene and 3, 4-dinitrotoluene with high yield and purity were researched by catalytic oxidation in H2O2/H2SO4 /Na2WO4 system from 2-methyl-6-nitroaniline and 4-methyl-2-nitroaniline, respectively. The yield of 2, 3-dinitrotoluene was 93.5% with the purity of 98.8%, and the yield of 3, 4-dinitrotoluene was 92.3% with the purity of 99.2%. Their structures were characterized by means of FT-IR, 1H NMR, 13C NMR and elemental analysis. The effects of oxidant system, reaction temperature, reaction time, oxidant dosage and catalyst dosage on the oxidation reaction to prepare dinitrotoluene were investigated, and the optimized synthesis conditions were obtained. The mechanism of catalytic oxidation was speculated. The thermal stabilities of dinitrotoluene were studied by differential scanning calorimetry (DSC). The results show that the melting point of 2,3-Dinitrotoluene and 3,4-dinitrotoluene were 63.66 ℃ and 65.16 ℃, respectively. And the gasification starting temperatures were 169.5℃ and 148.16℃, respectively.
Key words: sodium tungstate; hydrogen peroxide; dinitrotoluene; catalytic oxidation
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