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含N配体的金属有机配合物的合成与表征
摘 要 本文采用水热合成法合成4-4`联吡啶与金属的配合物。并借助拉曼光谱、XRD、红外光谱等手段对4-4`联吡啶与金属所合成的配合物进行了光谱分析。在进行光谱测试时，操作条件、样品制备等条件均能影响测试结果，通过XRD确定4-4`联吡啶与金属在高温下可以配位成金属有机配合物。通过拉曼光谱、红外光谱分析，可以确定配合物中几种分子振动，如C-H键的伸缩振动，环呼吸震动等。 关键词: 4-4`联吡啶 拉曼光谱 XRD N with the metal complex organic synthesis and characterization Abstract In the paper, hydrothermal synthesis of 4-4 `bipyridine and metal complexes. And with Raman spectroscopy, XRD, infrared spectroscopy, and other means to 4-4 `bipyridine and the synthesis of metal complexes were spectrometry. During spectrum tests, operating conditions, sample preparation, and other conditions can affect the test results, identified by XRD 4-4 `bipyridine and metal at a high temperature can be coordinated into a metal organic complexes. By Raman spectroscopy, infrared spectrometry, can be identified in several complex molecular vibration, such as the C-H stretching vibration, Central breathing vibration. Keywords: 4,4-Bipyridine Raman spectrum XRD 目 录 摘 要I AbstractII 第一章 文献综述1 1.1超分子化学的简述及研究进展1 1.1.1超分子的定义1 1.1.2超分子的结构特征2 1.2 金属配位化合物2 1.2.1 配合物简述2 1.2.2 配合物结构2 1.2.3 金属配位化合物合成方法3 1.2.3.1常温法3 1.2.3.2水热合成法3 1.2.3.3高温法3 1.2.4 配合物的应用3 1.2.5配位化合物的命名4 1.3 分子光谱的研究4 1.3.1 分子光谱的基础研究4 1.3.2 分子光谱的最新研究进展4 1.4 拉曼光谱的简述及研究应用5 1.4.1 拉曼光谱的简述5 1.4.2 拉曼光谱的应用5 1.4.3拉曼光谱分析类别6 1.5 红外光谱的研究应用6 1.6 XRD简述7 1.6.1XRD的原理7 1.6.2XRD在化学中的应用7 1.7本文研究的目的8 第二章 实验部分9 2.1 实验所用原料及反应条件9 2.2 实验试剂的纯度及来源9 2.3 实验所用设备9 2.4 化合物的制备 含氮配体的金属配合物的合成9 第三章 结果与讨论13 3.1 拉曼光谱测试13 3.1.1 样品制备13 3.1.2 测试条件及仪器13 3.1.3 测试步骤14 3.1.4 表征结果分析14 3.2 X射线衍射测试（XRD）19 3.2.1 测试原理19 3.2.2 样品制备19 3.2.3 测试条件及仪器19 3.2.4 测试步骤19 3.2.5 表征结果分析20 3.3 红外光谱测试23 3.3.1 样品制备23 3.3.2 测试条件及仪器23 3.3.3 测试步骤23 3.3.4 表征结果分析23 第四章 结论27 致 谢28 参考文献29
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微胶囊的性能研究
目 录 中文摘要3 英文摘要4 目 录5 1 绪论1 1.1 微胶囊技术1 1.2 喷雾干燥法3 1.3 冷冻干燥法5 1.4 鼓风干燥法5 1.5 微胶囊芯材释放研究的现状5 2 实验部分7 2.1 试剂与仪器7 2.2 辅酶Q10微胶囊的制备8 2.3 辅酶Q10微胶囊化效果的评定及其品质分析9 2.3.1 傅立叶变换红外光谱图的制作9 2.4 微胶囊化效果的评定10 2.5 微胶囊品质评定11 3 实验结果与讨论14 3.1 辅酶Q10的傅立叶变换红外光谱图分析14 3.2 辅酶Q10在乙醇溶液中的标准曲线15 3.3 不同干燥方法包埋率的比较16 3.4 辅酶Q10产品流动性测定18 3.5 DHA微胶囊缓释性的研究18 4 结论与展望25 4.1 结论25 4.2 展望25 致 谢26 参考文献27 摘 要：本文建立了紫外分光光度法定量测定辅酶Q10的分析方法，其定量检测波长为275nm，在2.018～16.144μg/ml浓度范围内线性良好，其线性回归方程为： y = 0.0334x + 0.0127，相关系数R2=0.9999。用建立的方法定量分析了所制备的辅酶Q10微胶囊样品的包埋率；用测量休止角的方法来测定微胶囊产品的流动性。实验结果表明，所制备的微胶囊产品流动性良好，其中以冷冻干燥法制得的产品流动性最好，以喷雾干燥法制得的产品包埋率相对最高。本文还研究了DHA微胶囊的在不同pH值环境下的缓释情况，绘制出不同pH条件下的动力学曲线，探究DHA微胶囊的释放动力学机理，得出本实验所用DHA微胶囊的释放符合零级释放动力学机理。 关键词：微胶囊；包埋率；流动性；缓释性；动力学曲线 Research on Properties of Microcapsules Abstract: In this paper, quantitative analysis of coenzyme Q10 is carried out by UV spectrophotometry analysis, the wavelength of quantitative detection is 275nm, good linearity in the concentration range of 2.018 ~ 16.144μg/ml, the linear regression equation is: y = 0.0334x + 0.0127, the correlation coefficient R2 = 0.9999. We use the established method to quantitative analysis the embedded sample rate of the prepared coenzyme Q10 microcapsules; the liquidity of the prepared microcapsules is detected by measuring the angle, and the result showed that the liquidity of the prepared microcapsules is good., in which the product prepared by freeze-dring method has the best liquidity , and the one prepared by spray-drying has relatively highest embedding rate. This experiment also measured the control-release status of microencapsulated DHA under different pH values, so as to draw the kinetics curve under different pH values. Research into the mechanism of control-release kinetics of DHA microcapsules,the results showed that: In this experiment,the control-release of the DHA microencapsules is in line with the zero-level mechanism of release kinetics. Keywords：Microcapsules;Embedding rate;Liquidity;Control release;Kinetics curve
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化工生产中异常数据处理
目 录 中文摘要I 英文摘要II 目 录III 1 绪论1 1.1 课题背景1 1.2 课题研究的目的和意义1 1.3数据挖掘研究现状2 2 异常数据处理方法5 2.1 数据挖掘5 2.2 数据挖掘的方法和技术6 2.3 聚类方法8 2.4离群点的识别方法16 3 PCA和神经网络的应用19 3.1 主成分分析(PCA)介绍19 3.2 延迟焦化模型21 3.3 数据处理23 3.4结果与讨论28 4 总结与展望29 致 谢30 参考文献31 摘 要：本论文面向实际化工生产过程的软测量技术，融合了大量的现场观测数据，其中的任一异常数据（野值）的出现都可能导致模型的预测效果下降，甚至完全失败，因此对测量数据进行预处理非常重要。以延迟焦化过程焦炭产率软测量模型为例，考虑以多变量的聚类分析为异常样本数据的识别方法，进行识别异常样本数据并解释这些异常样本对后继建模结果的影响。 本文首先总结、探讨关于数据挖掘、离群点分析、聚类算法方面取得的已有主要研究成果。并详细介绍了基于密度的聚类算法和神经网络，并结合延迟焦化过程焦炭产率软测量模型，对原数据做成分分析和神经网络，再对处理过的数据进行成分分析和神经网络分析，并对它们进行比较。 关键词：聚类分析；离群点；异常数据； Abnormal data processing in chemical production Abstract:This thesis for actual chemical production process of soft measurement technology,including a large field of observation data, any abnormal data (wild) may cause the model prediction,even completely failed,so for measuring data pretreatment is very important.With delayed coking process coke yield soft measurement model,for example,consider multivariable clustering analysis for abnormal data of identification method,identification and interpretation of these abnormal data for subsequent modeling results abnormal samples. This paper summarizes and discusses about the data mining, the outliers,clustering algorithm of existing research results.And introduces in detail the clustering algorithm based on density and neural network,and delayed coking process coke production rate of the soft measurement model,the original data component analysis and neural network, and then processed data of composition analysis and neural network analysis.Finally comparing with them. Keywords：Clustering analysis;outliers；Abnormal data；
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水产品营养成分传统分析方法与仪器检测方法比较研究
1绪 论1 1.1传统水分、蛋白质及脂肪的测定方法2 1.1.1水分含量测定方法2 1.1.2蛋白质含量的测定方法3 1.1.3脂肪含量的测定方法5 1.2快速的水分、蛋白质及脂肪含量测定方法6 1.3实验背景及创新点8 2 实验部分10 2.1材料与试剂10 2.2 设备10 2.3实验方法11 3 结果和讨论14 3.1不同的蛋白质测定方法所得结果14 3.2不同的脂肪测定方法所得结果16 3.3 不同的水测定方法所得结果19 3.4 讨论21 4 总结与展望23 致 谢24 参考文献25 摘要：开展水产品营养成分传统分析方法和现代仪器分析方法的比较研究，建立二者之间的误差修正关系。分别以养殖大黄鱼、虾、贻贝的干货和鲜货做为实验材料。用传统分析方法和仪器检测方法做相同营养成分的测定并研究其差异。有关蛋白质含量、水分含量积脂肪含量的测定，传统的定量方法分别采用凯氏定氮法、常压干燥法及索氏提取法,而实验中对于蛋白质、水分及脂肪含量的测定分别采用自动凯氏定氮仪、卤素水分仪及脂肪测定仪。实验表明：仪器分析方法完全可以替代传统分析方法。两者之间存在微小差异。一般仪器方法测定的结果其相对平均偏差较小。 关键词：凯氏定氮；脂肪测定；水分测定；蛋白质测定； Aquatic nutrients along with the traditional analysis methods and comparative study of detection methods Abstract: Aquatic nutrients to carry out the traditional analysis methods and modern methods of instrumental analysis of the comparative study between the establishment of the relationship between error correction. Were cultured large yellow croaker, shrimp, mussels of the dry goods and fresh produce as experimental materials. Using traditional analytical methods and equipment to do the same detection method of the determination of nutrients and to study their differences. Related to protein content, fat content, moisture content determination of the plot, the traditional quantitative methods were used Kjeldahl method, atmospheric pressure drying method and the Soxhlet extraction method, and the experiment for protein, moisture and fat content were measured using automatic Kay Miriam's fixed nitrogen, halogen moisture and fat analyzer instrument. Experiments show that: instrumental analysis can replace the traditional methods of analysis. There is little difference between the two. General Instrument measured the results of its relatively smaller average deviation. Key words: Kjeldahl; Fat measurement; Determination of Water; Protein Determination
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污泥制备活性炭
目录 中文摘要………………………………………………………………………………Ⅰ 英文摘要………………………………………………………………………………Ⅱ 目录……………………………………………………………………………………Ⅲ 1 绪论1 1.1 污泥的分类及性质1 1.2 污泥的处理4 1.3 污泥的再利用5 1.4 污泥制取活性炭国内外研究现状6 1.5污泥活性炭的国内外应用现状6 2 实验部分10 2.1 实验仪器与试剂10 2.2 污泥活性碳制备11 2.3 产品性能检测11 3 结果与讨论15 3.1 实验结果15 3.2 实验结果讨论17 4 总结与展望19 致 谢20 参考文献21 摘要：本论文主要介绍了污泥的分类、性质、处理方法及再利用和污泥活性炭吸附剂的制备方法及其应用现状。我们在此基础上进行了污泥活性炭的制备以及其性能检测。虽然最后没有测出碘值，但是我们进行了一系列的分析并进行了总结，主要是由于未对污泥进行特性分析，操作不规范等各方面的原因造成的。 关键词：污泥;活性炭;碘值 Activated Carbon Produced from Sludge Abstract ：This paper mainly introduced the classification of sludge, nature, treatment and sludge reuse and preparation methods of activated carbon adsorbent and its application status，On this basis we carried out the preparation of activated sludge and their performance testing. Although the iodine value was not measured, we carried out a series of analysis and took a summary, Mainly it is caused by lack of analysis of sludge characteristics, operation and other non-standard. Keywords：Sludge;Activated carbon;The iodine value
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洋甘菊精油超临界二氧化碳提取工艺研究
目录 中文摘要I 英文摘要II 目录III 1 绪论1 1.1 概述1 1.2 洋甘菊精油的应用1 1.3 洋甘菊精油的提取国内外现状1 1.4 研究内容概述5 2 实验部分6 2.1 实验材料与试剂7 2.2 实验方法7 3 结果与讨论11 3.1 洋甘菊的超临界CO2流体萃取工艺研究11 3.2 超临界CO2分子蒸馏耦合分离20 4 总结与展望22 4.1 总结22 4.2 展望22 致谢24 参考文献25 摘 要：采用超临界CO2流体萃取技术对洋甘菊中精油的萃取工艺进行了研究，考察了萃取压力、萃取温度、萃取时间以及分离器条件等工艺参数对浸膏得率和萃取产物品质的影响。经过试验，确定了洋甘菊浸膏萃取的工艺条件为：萃取压力20MPa，萃取温度50℃，萃取时间2.0 h，浸膏得率为3.74%。在此萃取条件下，初步研究了采用了三步分离的方法初步优化分离精油和杂质组分，得到的洋甘菊精油得率为0.16%。对得到的精油产品进行气相色谱分析，并与传统的水蒸气蒸馏和溶剂提取进行了比较，结果显示采用超临界CO2流体萃取洋甘菊精油具有较明显的优势。同时对洋甘菊超临界CO2流体萃取得到的浸膏进行了分子蒸馏的初步研究，初步得到了洋甘菊浸膏的分离工艺参数为蒸馏温度120℃、真空度3.0Pa、转速350r /min、出油率为7.26%。 关键词：洋甘菊；精油 ；超临界CO2萃取；分子蒸馏 The Research on Supercritical CO2 Extraction of Essential Oil from the Flower of Chamomile Abstract: The essential oil from the flower of chamomile was extracted with supercritical CO2. Influences of extraction pressure, temperature, extraction time and separation conditions on the yield and the quality of extractive were investigated. The yield of extractive was 3.74 % at appropriate conditions of pressure 20MPa , temperature 50 ℃and extraction time 2.0 h .At this extraction conditions, the yield of essential oil was 0.16% while the three step separation was used to optimize the separation of essential oil from unwanted components. The results of supercritical CO2 extraction experiments were compared with those obtained with steam distillation and maceration. The obtained essential oil were analysed by GC. It can be concluded, that SFE offers considerable advantages over the conventional method of steam distillation and maceration for separation of essential oil compounds from chamomile. The technology of molecular distillation of concretes from chamomile were also studied.. The results showed that the appropriate refining conditions were determined as distillation temperature 120℃,pressure 3. 0 Pa and scratch speed 350 r/ min. Yield of refined chamomile essential oil reached 7.26 %. Keywords：Chamomile; essential oil; supercritical CO2 extraction; molecular distillation
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制革浸灰助剂及其应用工艺研究
摘 要：传统的硫化碱脱毛法会产生大量高污染废液及废气，严重影响了生态环境。本论文研究了偏硅酸钠以及胰酶在皮革脱毛工序中的应用，通过单因素试验，考察了处理时间、胰酶浓度、浸液PH值和偏硅酸钠浓度对实验结果的影响，通过四因素三水平正交试验，得到最佳处理工艺条件：处理时间为7h、胰酶浓度为0.4%、混合液的pH值为7.9、偏硅酸钠浓度为0.1%。 关键词：皮革；脱毛；偏硅酸钠；胰酶 目 录 中文摘要I 英文摘要II 目 录III 1 绪论1 1.1 制革业概述1 1.2 脱毛工序概述1 1.3 脱毛技术现状2 2 实验部分4 2.1 实验材料与设备仪器4 2.2 工艺流程4 2.3 分析测试4 3 结果与讨论6 3.1 处理时间对处理结果的影响6 3.2 胰酶浓度对处理结果的影响7 3.3 浸液pH值对处理结果的影响10 3.4 偏硅酸钠浓度对处理结果的影响12 3.5 四因素三水平正交实验15 3.6 正交实验结果分析19 4 总结与展望21 致 谢22 参考文献23 Study on the Application of Leather Auxiliaries in the Leather Industry Abstract：The traditional dehairing process which used sodium sulfide produced lots of high pollution waste and emission .In this paper, the application of sodium metasilicate and pancreatin during dehairing process is researched. Through single factor tests, different results for the variation of the time for soaking, concentration of the pancreatin, PH of the tanning liquor and the concentration of the sodium metasilicate are discovered. Through four factors and three levels orthogonal, the best experimental conditions have been found: time for soaking is 7h; concentration of the pancreatin is 0.4%; PH of the tanning liquor is 7.9; concentration of the sodium metasilicate is 0.1%. Keywords：Leather; Dehairing; Sodium metasilicate; Pancreatin
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汽油中含氧化合物的检测与研究
目 录 中文摘要I 英文摘要II 目录III 1 绪论1 研究背景1 1.2 目前提高辛烷值的方法1 1.3 含氧添加剂现状2 1.4汽油中含氧物质的测定3 1.4.1 传统方法3 1.4.2 二维气相色谱中心切割技术4 2实验部分5 2.1Deans Switch 工作原理5 2.2仪器、试剂及分析条件7 3 结果与讨论9 3.1建立电磁阀切割时间表9 3.2校正曲线的测绘14 3.3精密度17 3.4ASTM D4815专用标准混标的测定18 3.5汽油样品的测定和加标回收率19 4总结与展望21 4.1总结21 4.2展望21 致 谢23 附录26 摘 要：采用二维气相色谱方法分析汽油中氧化物添加剂；采用配有微板流路控制阀(Deans switch)的Agilest 7890N 气相色谱系统，进行动态中心切割，将汽油基体切入到第二根色谱柱，并可快速简便地设定切割时间。这一技术增强了色谱分离度，使得氧化物与烃类基质完全分开；提高了极性低含量添加剂分析结果的可信度；多种常用的氧化物添加剂的测定证实了系统卓越的校正和定量性能；用该方法分析汽油中0%～10%的含氧添加剂，各物质校正曲线的线性相关性良好，相关系数均大于0.999；标准样品5次重复测定的相对标准偏差均小于1.29%；车用汽油实际样品中含氧添加剂的加标回收率在90%～110%之间；采用反吹技术可以大大的减少分析时间，提高了分析效率。该方法是车用汽油中含氧添加剂测定的一种快捷，准确可靠的分析方法。 关键词：二维气相色谱；微板流路控制技术；含氧添加剂；汽油 Abstract: A two-dimensional GC method for the analysis of oxygenated additives in gasline is described .This method employ an Agilent 7890N GC system equipped with a Deans swith device to dynamically heart-cut the analytes from the gasline matrix to a second GC column . The unique design of the heat-cut device allows fast easy method setup when determining cut times .The Agilent 7890N GC electronic pneumatices control (EPC) used for this system provides better retention time precision that allows narrower cut times for better resolution an quantitative precision . Excellent calibration an quantitative performance of this system is demonstrated for several commonly used oxygenated additives .The linearity test showed that the correlation coefficient r2 values for oxygenated additives were all higher than 0.999.The results showed that the relative standard (RSDs) of standard samples in five continued were within 1.29%and the recoveries of added standards tests were from 90%～110%.The EPC of the Agilent 7890N GC is shown to enable greater productivity by decreasing analysis times with a backflushing technique .The method is quick ,sinple an useful for the determination of oxygenated in gasline . Keywords：two-dimensional gas chromatography ;capillary flow technique (Deans Switch );oxygenated ;gasline
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ClO2染料脱色研究
摘 要：二氧化氯具有强氧化性、不稳定性和消毒性。本文在制备二氧化氯的基础上，用分光光度法测定反应后酸性红染料废水的含量，从而计算二氧化氯对酸性红染料废水的脱色率。研究搅拌速度、二氧化氯用量、pH值、反应温度、反应时间、废水初始浓度等对废水的脱色效果。实验结果表明：搅拌速率、废水起始浓度以及反应温度对脱色率影响不大，反应速度很快，10分钟基本上完全反应。在碱性条件下脱色率较低，但在酸碱度达到一定值后对脱色率影响很小。二氧化氯对废水脱色的较佳条件：反应温度30℃，反应时间10min，转速250r/min，pH=6，酸性红染料与二氧化氯反应的摩尔比为1:3.17。通过对实验数据的处理得到二氧化氯与酸性红的反应为一级反应，并得到以下的阿伦尼乌斯方程:k=0.12e-231.11/RT以及动力学方程: r=kcA0.5cB0.5。 关键词：酸性红染料废水；二氧化氯； 脱色率；动力学 目 录 中文摘要Ⅰ 英文摘要Ⅱ 目录Ⅲ 1． 绪论．1 1.1 印染废水的特点1 1.2 印染废水的处理方法1 1.3 ClO2在印染废水中的应用．3 1.4 ClO2的性质．4 1.5 ClO2的制备方法．5 1.6 ClO2的脱色机理．5 1.7 应用概况5 2. 实验试剂与玻璃仪器．7 2.1 主要原料和试剂7 2.2 主要仪器7 2.3 实验步骤7 3. 实验结果与讨论．9 3.1 标准曲线的绘制9 3.2 单因素考察．10 3.3 染料与二氧化氯反应的摩尔比推算．16 3.4 动力学计算．16 4. 结论．18 致谢19 参考文献20 Study on Dye’s Decolorization by ClO2 Abstract: Chlorine dioxide has strong property of oxidation, the instability and the disinfection. This article is based on the preparation of chlorine dioxide, the content of the acid red dye wastewater was after reaction determined by spectrophotometric methods, and thus decolourization rate of acid red dye wastewater was calculated with chlorine dioxide. Then the decolourization effect of the dye wastewater by reaction mixing speed, the amount of chlorine dioxide, pH, reaction temperature, initial concentration of dye wastewater, reaction time were studied. The experimental result indicated that, the mixing speed, initial concentration of the dye wastewater and reaction temperature are little influence to the decolourization rate. The reaction is very quick,The reaction would be completed within 10 minutes. Under the alkalinity condition, the larger pH is , the lower decolourization rate is,and the pH is out of scope is little influence to the decolourization rate. So the best condition are the followings: reaction temperature is 30℃, reaction time is 10min, rotational speed is 250r/min, pH is 6, the ratio of the acid red dye wastewater and a chlorine dioxide response is 3.17.To deal with the data of the experiment we get the result: the reaction is first order, and Arrhenius Equation is k=0.12e-231.11/RT, dynamic equation is r=kcA0.5cB0.5. Keywords: Acid red dye wastewater; Chlorine dioxide; Decolourization rate; Kinetics
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吡啶联吡唑类化合物合成及性质研究
目 录 中文摘要I 英文摘要II 目录III 1. 绪论1 1.1 吡啶类农药的研究进展1 1.2 吡唑类农药的研究进展1 1.3 酰胺类农药的研究进展1 1.4 含吡唑基吡啶类化合物2 1.5 含吡唑基、吡啶基酰胺类化合物3 1.6 合成路线4 2. 实验部分7 2.1 仪器与试剂7 2.2 试验操作7 3. 结果与讨论10 3.1 试验结果10 3.2 讨论22 3.3 生测结果24 4．总结与展望25 致谢26 参考文献27 摘 要：本论文以3-氨基-2氯吡啶为原料，经过重氮化，还原成肼基，再环和得到吡唑取代基酯类，最后水解等四步反应得到中间体5-甲基-1-（2-氯吡啶-3基） -4-吡唑羧酸,再以它为母体，经过酰氯化，再与不同取代基的苯胺反应得到系列1酰胺类目标产物。另外，以1-（吡啶-3-基）-5-三氟甲基-1H-4-吡唑羧酸为中间体，经过酰氯化，再与不同取代基的苯胺反应得到系列2酰胺类目标产物。 得到的29个产物经核磁、质谱和熔点测定进行结构表征。并对其进行生物活性研究。 关键词：吡啶，吡唑，吡啶联吡唑，酰胺，生物活性 Abstract: A synthetic method of pyridine-compound pyrazole was design. An intermediate 5-methyl-(2-chloro-pyridine-3-)-pyrazole-4-carboxylic acid was explored.It was performed by using 3-amino-2-chloro pyridine as the starting materials in three steps including diazotization,reduction and cyclize to form the attempted product. Using it to acyl chloride,then reacted with different substituted aniline to obtain attempted 1st series acylamide,; At the same time, using 1 - (pyridine-3) -5 - trifluoromethyl -pyrazole-4-carboxylic acid as an intermediates, according to acyl chloride,then reacted with different substituted aniline to obtain attempted 2sec series acylamide. The structural characterization of the getted 29 product was study by H-NMR,MS and M.p apparatus.Then study their biological active. Keywords：pyridine; pyrazole; acyl chloride; synthesis,biological active;
