论文总字数：27073字

摘 要

随着戊二胺在工业、农业上的广泛应用，且由于石油化工加工制备戊二胺存在能耗大、环境污染等问题，使微生物发酵法制备戊二胺成为新的趋势。但仍存在从上游发酵液中提纯戊二胺的问题。本文利用色谱法从戊二胺盐溶液中分离戊二胺，本文对不同类别的树脂进行了筛选，选定了1213大孔吸附树脂，该树脂对戊二胺和硫酸盐的选择性系数达到1.93，对戊二胺的吸附量达到75mg/g,能较好的将戊二胺与硫酸盐溶液分离。同时，基于1213树脂测定了戊二胺和硫酸根单组分在不同温度下的等温吸附曲线，并进行了戊二胺单组分的吸附动力学实验和在不同条件下，如进样量、柱高径比、流速对戊二胺硫酸盐溶液色谱峰的影响。本实验结果表明温度升高，1213树脂对戊二胺和硫酸根离子的吸附能力减弱，吸附是放热过称，且在10min内树脂能对戊二胺达到吸附平衡，且流速、进样量增加戊二胺的分离度降低，柱高径比增加分离度增大。

关键词 戊二胺 硫酸盐 色谱分离 大孔吸附树脂

Separation of 1,5-diaminopentane conversion solution

ABSTRACT

With the wide application of diaminopentane in industry and agriculture, and the problem of high energy consumption and environmental pollution caused by petrochemical processing of diaminopentane, the preparation of diaminopentane by microbial fermentation has become a new trend. However, there is still a problem of purifying diaminopentane from the upstream fermentation broth. In this paper, the separation of diaminopentane from the diaminopentane salt solution was carried out by chromatography. The different types of resins were screened and 1213 macroporous adsorption resin was selected. The selectivity coefficient of the resin to diaminopentane and sulfate reached 1.93. The adsorption amount of diaminopentane reaches 75 mg/g,which can better separate the diaminopentane from the sulfate solution. At the same time, the isothermal adsorption curves of diaminopentane and sulfate single component at different temperatures were determined based on 1213 resin, and the adsorption kinetics of diaminopentane monocomponent was investigated and the effects of different injection rates, column height-to-diameter ratio and flow rate on the chromatographic peak of diaminopentane sulfate solution were investigated. The results of this experiment show that the temperature is increased, the adsorption capacity of 1213 resin to diaminopentane and sulfate ion is weakened, the adsorption is exothermic, the resin can reach the adsorption equilibrium of diaminopentane within 10 min, reduced separation of diaminopentane with increasing flow rate and injection volume and increased separation as the height-to-diameter ratio of the column increases.

Key Words: 1,5-diaminopentane;Sulfate;Chromatographic separation;Macroporous resin

目录

摘要 I

ABSTRACT II

第一章 引言 1

1.1 前言 1

1.2 戊二胺概述 1

1.2.1 戊二胺的理化性质 1

1.2.2 戊二胺的应用 2

1.2.3 生物基戊二胺的市场现状 2

1.3 戊二胺生产方法 3

1.3.1 化学合成 3

1.3.2 微生物发酵法 3

1.3.3 全细胞催化法 4

1.4戊二胺分离方法 4

1.4.1 萃取法 4

1.4.2 离子交换层析法 6

1.5戊二胺的检测方法 6

1.5.1 高效液相色谱法 7

1.5.2 气相色谱法 8

1.5.4 离子色谱法 9

第二章 实验器材和方法 10

2.1 实验材料与设备 10

2.1.1 实验仪器 10

2.1.2 实验试剂 10

2.1.3 树脂 10

2.2 实验方法 11

2.2.1 绘制标准曲线 11

2.2.2 树脂的筛选 11

2.2.3 洗脱液的选择 12

2.2.4 绘制吸附等温线 12

2.2.5 吸附动力学实验 13

2.2.6 单柱分离实验 13

2.2.7 分离度和回收率测定 13

2.2.8 实验条件控制 14

2.2.9 吸附热力学模型 14

2.3分析方法 15

2.4 本章小结 15

第三章 结果与讨论 16

3.1 标准曲线 16

3.2 树脂初筛结果 17

3.3 初筛树脂上柱分离结果 19

3.4 吸附等温线 21

3.5 吸附动力学 22

3.6 色谱峰实验 22

3.6.1 不同流速对色谱峰的影响 23

3.6.2 不同进样量对色谱峰的影响 23

3.6.3 不同柱高径比对色谱峰的影响 24

第四章 结论与展望 26

4.1 主要结论 26

4.2 展望 26

参考文献 28

致谢 31

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