三甲基戊二醇制取催化剂的研究

论文编号:CL085  论文字数:11404,页数:32

摘 要：2,2,4—三甲基—1,3—戊二醇(以下简称TMPD)，是一种重要的精细化工中间体。作为重要的精细化工原料，TMPD广泛应用于香料合成、表面活性剂、多酯增塑剂及医药中间体的合成等方面。
 由于国内对TMPD的合成工艺、产品深加工及应用开发不够，很难寻到国产TMPD的商品。因此我们需优化TMPD生产工艺，使国内生产出优质的TMPD。
 本文主要以异丁醛为原料，用NaOH水溶液作为催化剂合成了TMPD。重点在于优化反应条件，找出最佳的生产工艺，提纯产物并对其进行红外等各种表征，研究产物的品质。优化后的反应条件为：以NaOH水溶液为催化剂，第一、第二阶段的最佳浓度分别为20%,50%；第一、第二阶段的催化剂用量分别为15ml，40ml；第一阶段反应温度为30~50℃，时间2h；第二阶段氧化还原反应时间为8h，升温过程为90℃反应3h，120℃反应3h，140℃反应2h；催化剂2的加入方式为分两次各20ml的补加方式。实验中，产率最高达50.22%。实验结果较满意。
关键词：异丁醛；氢氧化钠；羟醛反应；2,2,4—三甲基—3—羟基戊醛;TMPD

Abstract: 2,2,4-trimethyl-1,3-pentanediol(TMPD) is one of important intermediante.As a raw material in fine chemical industry,TMPD is widely used in manufacturing spices, surfactants, plasticizers,medical intermediants and so on.
It is hard to obtain TMPD with good quality since domestic TMPD synthesis technology, product and application development is not enough.Hence,it is high time for us to optimize  production technology in order to manufactured TMPD in domestic market.
This article is mainly describe that the synthesis of TMPD through condensation of isobutyraldehyde and cross cannizzaro reaction by NaOH solution .The goal is to find optimization of reaction conditions, best production technology. After purification,product was characterized by infrared spectroscopy to ensure its quality. The optimal conditions for reaction are listed as below: NaOH solution as the catalyst, the best concentration are 20%, 50% respectively;the best amount of catalyst are 15ml and 40ml; the first stage of the reaction temperature is 30 to 50℃ with 2h;the second stage of redox reaction time is 8h ,the specific procedure ,90℃ 3h, 120℃ 3h,140℃ 2h; Catalyst 2 was added for two times which was 20ml each time. The best experimental yield was 50.22%.
Keywords：Isobutyraldehyde; sodium hydroxide solution; aldolcondensation; isobutyraldol;2,2,4—trimethyl—1,3—pentanediol

目  录
中文摘要 I
英文摘要 II
目录 III
1. 绪论 1
 1.1  背景及意义 1
 1.1.1 TMPD的用途 1
 1.2  合成方法 2
 1.2.1 加氢合成 2
      1.2.2 其他合成方法 4
      1.2.3 提纯方法 4
2. 实验部分 6
 2.1 实验原料及试剂 6
 2.2 实验仪器设备 6
 2.3 实验方法 6
 2.4 实验原理 7
 2.5 实验步骤 8
 2.5.1 蒸馏原料异丁醛 8
 2.5.2 TMPD的合成 9
 2.5.3 产物提纯 10
 2.5.4 产品检测方法 10
 2.5.5 计算方法 11
 2.6 单因素实验 12
     2.6.1 氧化还原反应温度的研究 12
     2.6.2 氧化还原反应时间的研究 12
 2.6.3 催化剂加入量的研究 12
 2.6.4 催化剂浓度条件的研究 13
 2.6.5 催化剂2加入方式的研究 14
3. 结果与讨论 15
 3.1  TMPD的物理性质  15
 3.2 单因素实验结果分析  15
 3.2.1 反应温度对产率的影响  15
     3.2.2 反应时间对产率的影响 16
     3.2.3 催化剂用量对产率的影响 17
     3.2.4 催化剂浓度对产率的影响 19
     3.2.5 催化剂2的加入方式对产率的影响 21
 3.3  红外波谱图分析与表征 22
     3.3.1 异丁醛红外光谱图分析 22
     3.3.2 TMPD红外光谱图分析 23
     3.3.3 反应物与产物对比分析 24
4．总结与展望 25
致谢 26
参考文献 27