论文总字数：17825字

摘 要

随着丁三醇在医药、军事方面的广泛应用，它的需求量急剧增长。由于化学法生产丁三醇对环境和能源产生的压力，低成本的非粮食底物生物发酵法生产丁三醇已日益成为新的研究方法。而目前主要面临的问题为发酵法生产丁三醇浓度较低和较高的分离提纯成本。本研究致力于通过色谱法从发酵液中分离出高纯度丁三醇，使丁三醇能够得到有效的分离，且成本较低。基于目前已有的发酵产物收率情况，发酵液中除了含丁三醇，还含有大量的发酵中间产物木糖酸，木糖酸与丁三醇比例为12:5。综合分析了丁三醇和木糖酸的分子结构与物性差异，丁三醇分子由于含有四个C，长链C具有非极性效应，所以首先对非极性树脂进行了初步筛选。用丁三醇与木糖按比例混合而成的溶液进行分析，发现HD-1、HD-4、HD-6、AX-1对两者的选择性系数分别为2.66、1.85、1.68、2.85，吸附量分别为7.31 mg/l、10.06 mg/l、9.26 mg/l、7.38 mg/l，但丁三醇在树脂柱上的色谱峰表现为拖尾峰，不利于两者的分离。为了得到更加理想的分离效果，继而对极性树脂AX-7、AX-10、MR-5和氢型树脂SA-1进行了静态吸附试验，发现氢型树脂的选择性系数达到了1.45，且用水就能实现两者的完全分离，收率达到95%以上，所以选定氢型树脂SA-1为纯化丁三醇所用的分离介质。同时，基于SA-1树脂，测定了丁三醇和木糖单组份和双组份在不同温度下的吸附等温线，并计算得到了吸附热力学函数∆H、∆G和∆S的值。本实验研究结果表明，丁三醇和木糖在树脂上的吸附呈现线性趋势，且相对于木糖，丁三醇是强吸附组分，温度对丁三醇和木糖的吸附影响较弱，吸附是放热自发的过程。氢型树脂SA-1能实现丁三醇和木糖的有效分离。

关键词:丁三醇 木糖 色谱分离 氢型树脂 水解吸

ABSTRACT

As the use of 1,2,4-butanetriol has increased, the demand has increased dramatically. Because of the pressure on the environment and energy produced by the chemical process,the low cost non-food substrate biological methods production of 1,2,4-butanetriol is the new research direction. At present, the main problems are the lower concentrations of 1,2,4-butanetriol and higher separation and purification costs. The aim of this study is to separate high-purity 1,2,4-butanetriol from the fermentation broth by chromatography, so that the 1,2,4-butanetriol can be effectively separated and the cost become low. Based on the current yield of fermented products, the fermentation broth not only contains 1,2,4-butanediol, also contains a large number of xylonic acid, The ratio of xylonic acid to 1,2,4-butanetriol is 12:5。By compare the differences between 1,2,4-butanetriol and xylonic about the molecular structure and physical properties,1,2,4-butanetriol molecules contains four C, and long chain C has a non-polar effect. Therefore, the non-polar resin is the first choice.With 1,2,4-butanetriol and xylonic acid in proportion to the mixture of the solution for analysis,the partition coefficient are 2.66、1.85、1.68、2.85，and the Adsorption capacity are 7.31 mg/l、10.06 mg/l、9.26 mg/l、7.38 mg/l。The chromatographic peaks of 1,2,4-butanetriol on the resin column showed trailing peaks, which were detrimental to the separation of the two.In order to obtain a more ideal separation effect, the static adsorption test of the polar resins AX-7, AX-10, MR-5 and the hydrogen-based resin SA-1 was carried out, and the selectivity coefficient of the hydrogen-type resin was found up to 1.45 . The separation of the two can be achieved by just use the water as eluent , the yield reached 95% or more. So the selected hydrogen-based resin SA-1 is the separation medium used for the purification of 1,2,4-butanetriol. At the same time, the adsorption isotherms of 1,2,4-butanetriol and xylonic mono-components and two-component at different temperatures were determined based on SA-1 resin, and the values of adsorption thermodynamic functions ΔH、ΔG and ΔS were calculated. The results showed that the adsorption of 1,2,4-butanetriol and xylonic on the resin showed a linear trend, and 1,2,4-butanetriol was a strongly adsorbed component. The temperature had little effect on the adsorption of 1,2,4-butanetriol and xylonic, and the adsorption was spontaneous process. SA-1 resin can achieve the effective separation of 1,2,4-butanetriol and xylonic.

KEYWORDS : Chromatography ; 1,2,4-butanetriol ;Hydrogen type cation exchange resin ; Water elution

目 录

摘要 I

ABSTRACT II

第一章 文献综述 1

1.1前言 1

1.2丁三醇简 1

1.2.1丁三醇的性质 1

1.2.2丁三醇的应用 2

1.2.3丁三醇的历史 2

1.2.4 本研究的主要方法 4

第二章 实验器材和方法 6

2.1 实验仪器及试剂 6

2.1.1 实验主要仪器 6

2.1.2 实验主要试剂 6

2.2 实验方法 7

2.2.1绘制标准曲线 7

2.2.2树脂的筛选 8

2.2.3绘制吸附等温线 8

2.2.4平衡吸附容量与分离度测定 9

2.2.5 洗脱液的选择 9

2.3分析方法 9

2.4 本章小结 10

第三章 结果与讨论 11

3.1树脂筛选结果 11

3.2 对初步筛选树脂进行分离度测试 12

3.3 吸附等温线 14

3.3.1吸附等温线 14

3.3.2 热力学计算 16

3.4 分离度和回收率测定结果 19

第四章 结论与展望 22

4.1 主要结论 22

4.2展望 22

参考文献 24

致谢 26

第一章 文献综述

1.1前言

由于环境压力空前，人们在生产过程中都倾向于使用低污染、少浪费、能够循环利用的方法，保证对环境的友好；由于能源急剧紧张，生产过程中要求尽可能实现在节约能源、废物利用、降低成本的同时还可以保护环境，以实现可持续发展。应势而生的生物法相比化学方法在这方面展现了不可估量的前景。相比化学生产方法的高耗能、高污染，生物法具有对废物循环利用，无污染，低耗能，低成本，反应条件要求低等诸多优点。

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