-
乙二醇乙醚乙酸酯的合成及分析_化工专业论文范文
化工专业论文范文 目 录 摘 要I AbstractII 第1章 引 言1 1.1 乙二醇乙醚乙酸酯的性质和用途2 1.1.1 乙二醇乙醚乙酸酯的性质2 1.1.2 乙二醇乙醚乙酸酯的特殊用途3 1.2 合成乙二醇乙醚乙酸酯的生产工艺3 1.2.1 以环氧乙烷、乙醇为原料的两步法3 1.2.2 以2，2-二甲基乙醇乙酸酯和乙二醇乙醚为原料的方法4 1.2.3 以1，3，6-三氧杂环辛烷为原料的方法4 1.2.4 酯交换法4 1.2.5 均相催化环氧乙烷法4 1.2.6 非均相催化环氧乙烷法4 1.2.7 醋酸与乙二醇乙醚直接酯化法4 1.2.8 以乙二醇乙醚和冰乙酸为原料，在新型高分子复合催化剂的催化下，合成乙二醇乙醚乙酸酯5 1.2.9 以乙酸和乙二醇乙醚为原料，硅酸乙酯为硅源，通过溶胶-凝胶法(Sol-Gel)负载磷钨酸为催化剂，合成乙二醇乙醚乙酸酯6 1.3 酯化合成乙二醇乙醚乙酸酯的生产工艺6 1.3.1 催化剂的改进6 1.3.2 分离回收的改进8 1.4 固体超强酸的研究进展9 1.5 国内外发展现状10 1.6 乙二醇乙醚乙酸酯的应用12 1.7 存在的问题12 1.7.1 乙二醇乙醚乙酸酯的制备还停留在硫酸作为催化剂12 1.7.2 国内需求量的大，我国目前还处于研发阶段13 1.8 本论文的工作思路13 1.8.1 利用乙二醇乙醚和冰乙酸作为主要原料，通过直接酯化的方法，合成乙二醇乙醚乙酸酯，建立自己的分析方法13 1.8.2 研发新型催化剂替代硫酸催化剂，所研究的合成工艺符合环保要求13 1.9 本文研究意义及内容13 1.10 本论文预期达到的目的13 1.11 课题研究背景14 1.12 预期成果14 第2章 实验部分15 2.1 主要仪器设备和药品试剂15 2.1.1 主要设备及仪器15 2.1.2 主要药品及试剂15 2.2 乙二醇乙醚乙酸酯的合成反应机理18 2.3 实验方法及步骤19 2.3.1 催化剂（硅胶担载硫酸铈）的制备19 2.3.2 工艺流程19 2.3.3 产品分析20 2.4 实验装置20 3.1 单因素实验21 3.1.1 醇酸比(摩尔比)对酯化率的影响21 3.1.2 催化剂担载量对酯化率的影响21 3.1.3 反应时间对酯化率的影响22 3.2 正交实验22 3.3 红外谱图表征24 3.4 工艺条件比较26 3.4.1 催化剂重复使用比较26 3.4.2 不同的带水剂对反应酯化率的影响27 参考文献29 致 谢30 摘 要 乙二醇乙醚乙酸酯是新一代万能溶剂，具有极强的溶解能力，尤其是对聚合物的溶解力极强，广泛应用于油漆、涂料、油墨等行业。目前全球醇醚乙酸酯较大的生产国是美国、德国和日本，我国还处于研发阶段，只能限于小批量的化学试剂的生产，产品主要依靠进口。因此，国内有很大潜在市场，在开发和完善乙二醇乙醚乙酸酯的生产工艺上具有十分重要的意义。 乙二醇乙醚乙酸酯的合成方法主要有：（1）直接酯化法(以乙酸和乙二醇乙醚为原料，以硫酸、磷酸等无机酸为催化剂)；（2）酯交换法(以乙酸乙酯和乙二醇乙醚为原料)；（3）一步合成法(以环氧乙烷和乙酸乙酯为原料)。 目前国内乙二醇乙醚乙酸酯的生产大多停留在以硫酸等无机酸为催化剂的落后生产工艺。 本文主要进行硅胶担载硫酸铈催化合成乙二醇乙醚乙酸酯的研究。分别采用单因素实验法和正交实验法重点考察了醇酸摩尔比、催化剂担载量和反应时间等因素对酯化率的影响，确定了其最佳工艺条件为：醇酸摩尔比1：1.0，催化剂担载量15 %，反应时间120 min。在最佳工艺条件下，酯化率为99.70 %。与未担载的硫酸铈比较。担载的硫酸铈具有催化活性高、用量少、酯化率高和寿命长等显著优点，是一种很有前途的负载型催化剂。 关键词：乙二醇乙醚乙酸酯；硫酸铈；催化剂；合成 Abstract Glycol ethyl ether acetate is a new generation of universal solvent, it has strong ability to dissolve, especially for our highly soluble polymers, and it is widely used in paints, coatings, inks and other industries. Currently the world's larger ether acetate's producers are the United States, Germany and Japan, China is still in the research and development stage, which is only limited to low-volume production of chemical reagents, its' products are mainly imported. Therefore, there is a large potential domestic market; it has great significance in the development and improvement of glycol ethyl ether acetate's production technology. Glycol ethyl ether acetate's synthesis methods are: (1) Directly esterification method (the raw material is acetic acid and ethylene glycol ether, the catalyst are sulfuric acid, phosphoric acid and other inorganic acid); (2) Trans esterification (the raw material is ethyl acetate and ethylene glycol ether); (3) Step synthesis (the raw material is ethylene oxide and ethyl acetate). At present, glycol ethyl ether acetate's production mostly remained in the inorganic acid such as sulfuric acid as the catalyst; it is a backward production technology. In this paper, the study on the catalytic synthesis of glycol ethyl ether acetate with silica loaded cerous sulfate was carried out single factor method and orthogonal experiment method were used to investigate the effects of acid/alchohol ratio, mass fraction of sulfate cerous in the loaded catalyst stand reaction time on the acetic acid conversion, respectively and the optimal technical conditions were determined to be: acid/alchohol ratio1 : 1.0, mass fraction of sulfate cerous in the loaded catalyst 15 % and reaction time 120 min, under which the conversion of acetic acid reached 99.70 %. Compared with the unloaded sulfate cerous, the silica loaded sulfate cerous has some obvious advantages, such as better catalytic activity, less use level of catalyst, higher acetic acid conversion and long life, which is a good catalyst with potential application. Keywords: glycol ethyl ether acetate; sulfate cerous; catalyst; synthesis
-
印染废水处理研究
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 二氧化氯处理印染废水的相关研究3 1.4 二氧化氯的性质4 1.5 二氧化氯的制备方法4 1.6 二氧化氯的脱色机理4 1.7 二氧化氯应用概况5 2. 实验部分6 2.1 主要原料、试剂及仪器6 2.2 实验步骤6 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 正交设计15 3.4 正交结果16 4. 总结与展望17 致谢18 参考文献19 摘要：二氧化氯具有强氧化性、不稳定性和消毒性，其氧化能力是次氯酸的9倍多，是氯的2.6倍。本文在制备二氧化氯的基础上，用分光光度法测定反应后印染废水的含量，从而计算二氧化氯对印染废水的脱色率。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：二氧化氯对印染废水的脱色率在一定条件下能达到80%以上，搅拌速率、废水起始浓度对脱色率影响不大，温度越高废水的脱色效果越好，反应时间也很快，10分钟基本上完全反应，在酸性条件下脱色率较低，但在碱性条件下pH值越大脱色率越高。二氧化氯对废水脱色的较佳条件：反应温度25℃，反应时间20min，转速100r/min，pH=10，二氧化氯与废水反应的配比为1.5。 关键词：印染废水；二氧化氯； 脱色率；分光光度法 Study on Treatment of Printing wastewater Abstract: Chlorine dioxide has strong property of oxidation, the instability and the disinfection, its oxidized ability is more than 9 times of hypochlorous, and is 2.6 times of chlorine. This article is based on the preparation of chlorine dioxide, the content of the printing wastewater was after reaction determined by spectrophotometric methods, and thus decolourization rate of printing wastewater was calculated with chlorine dioxide. Then the decolourization effect of the printing wastewater by reaction mixing speed, the amount of chlorine dioxide, pH, reaction temperature initial concentration of printing wastewater, reaction time were studied. The experimental result indicated that, the decolourization rate can achieve above 80% by chlorine dioxide under the certain condition. The mixing speed, and initial concentration of the printing wastewater are no influence to the decolourization rate. The higher temperature is, the higher decolourization rate. The reaction is very quick. The reaction would be completed within 10 minutes. Under the alkalinity condition, the larger pH is , the higher decolourization rate is. So the best condition are the followings: reaction temperature is 25℃, reaction time is 20min, rotational speed is 100r/min, pH is 10, the ratio of the printing wastewater and a chlorine dioxide response is 1.5. Keywords: Printing wastewater; Chlorine dioxide; Decolourization rate; Spectrometric
-
环氧树脂阻燃剂的合成及表征_化工专业论文范文
化工专业论文范文 目 录 摘 要I AbstractII 1 绪 论1 1.1 阻燃问题的提出1 1.2阻燃技术发展概述1 1.3磷系阻燃剂概述2 1.4磷系阻燃剂阻燃机理3 1.5磷系阻燃剂的研究4 1.6前人的工作成果5 1.7本论文的可行性研究7 1.8本论文研究的主要内容7 2 DOPO-HB的合成8 2.1 前言8 2.2 合成方法8 2.3 实验部分8 2.3.1 实验试剂8 2.3.2 实验仪器8 2.3.3 实验步骤9 2.3.4实验流程图10 2.4 DOPO-HB的表征10 2.4.1 TGA10 2.4.2 DSC11 2.4.3 熔点12 2.4.4 红外光谱12 2.5 小结13 3 DOPO-HB溶解度的测定14 3.1概述14 3.2实验部分14 3.2.1.溶解度测定实验仪器14 3.2.2实验步骤14 3.2.3.实验装置14 3.2.4.实验结果和数据处理15 3.2.5 溶解度数据与温度的关联20 3.2.6 小结25 4 DOPO-ITA的合成26 4.1 概述26 4.2 合成原理26 4.3 实验部分26 4.3.1 实验试剂26 4.3.2 实验仪器26 4.3.3 实验步骤27 4.3.4实验流程图27 4.4 DOPO-ITA的表征28 4.4.1 TGA28 4.4.2 DSC28 4.4.3 红外光谱29 4.5小结29 5 结 论30 5.1 本论文的主要研究成果30 5.2 存在的不足与研究展望30 参考文献31 致 谢34 摘 要 DOPO（9，10-2氢-9-氧-10磷杂菲-10-氧化物）和4HBA（4-羟基苯甲醛）通过加成反应合成DOPO-HB(2-6-氧-6-氢-二苯并磷氧杂-6-酮-4-羟基苯甲醇)，同时优化了DOPO-HB的合成条件。DOPO（9，10-2氢-9-氧-10磷杂菲-10-氧化物）和ITA（衣康酸）在甲苯溶剂中反应合成DOPO-ITA({（6-氧-（6H）-二苯并-（CE）（1,2）-氧磷杂己环-6-酮）甲基}-丁二酸)，并通过红外检测（FIIR）和熔点检测法确定所得到的DOPO-HB和DOPO-ITA的化学结构。通过示差扫描热量计（DSC）和热重量分析法(TGA)测得这些固化型环氧树脂的热力学特征和热降解行为。本论文还重点研究了DOPO-HB在不同溶剂中的溶解度，结果表明，DOPO-HB在苯，甲苯，二甲苯和水中的溶解度都随温度的增加呈上升趋势，且溶解度的大小顺序为：S苯＞S二甲苯＞S甲苯 ＞S水。 关键词：环氧树脂 固化剂 阻燃剂 溶解度 Synthesis and Characterization of Epoxy Resin Flame Retardant Abstract A novel phosphorus-containing hydroxyl benzoaldehyde (DOPO-HB) from 9,10-dihydro-9-oxa-10– phosphaphenanthrene -10-oxide (DOPO) and 4-hydroxyl benzoaldehyde was obtained via simple addition reactions.The synthesis conditions of DOPO-HB were also optimized A novel phosphorous -containing flame retardants 10-(2,5-dicarbonylpropyl) 9,10-dihydro-9-oxa-10-phospha- phenanthrene-10- oxide (DOPO-ITA) was synthesized using 9,10-dihydro-9-oxa-10-phospha-phenanthrene-10-oxide (DOPO) and itaconic acid(ITA) as starting materials.The chemical structure of the obtained DOPO-HB and DOPO-ITA were characterized with FTIR, 1H and 31P NMR and elemental analysis. The DOPO-HB, with multi-phenol groups in the molecular chain, was used as a poly functional curing agent for epoxies. The activity and activation energies of the DOPO-HB curing reactions with epoxies were investigated with differential scanning calorimetry (DSC). The thermal properties and thermal degradation behaviors of the DOPO-HB-cured epoxy resins were also studied with DSC and thermo gravimetric analysis(TGA). The paper also focuses on the solubility of DOPO-HB in different solvents with the temperature trend, the results show that, the solubility of DOPO-HB in benzene, toluene and xylene, and water increases with the temperature rising. Moreover, the benzene> xylene> toluene> Water Keywords: Epoxy resin Curing agent Flame retardant solubility
