论文总字数：17538字

摘 要

环氧大豆油是用大豆油经过氧化处理后制得的一种化工产品，是一种使用广泛的聚氯乙烯无毒增塑剂兼稳定剂。同时，其环氧基团经开环后得到多元醇，可进一步用于润滑油或聚氨酯材料的制备。由于反应原料中有双氧水，常规间歇釜式反应存在安全隐患，且产品品质一般。微流场技术是一项基于过程强化的技术革新。与传统间歇式反应相比，微流场技术具有操作成本低、过程易于控制、易于工业放大、过程安全等优势。得益于极高的比表面积，可实现高效传质传热；作为连续流反应，其返混较小，可有效提升反应选择性。

论文针对环氧大豆油现有合成工艺弊端及性能不足，以大豆油为原料，结合现有微通道中环氧大豆油的合成工艺参数，采用中式管道反应器，通过优化参数，实现环氧大豆油的千吨级连续化合成。

本研究基于团队已有植物油环氧化相关工艺参数，通过微调，逐步放大。采用康宁微反应器进行大豆油环氧化时，过氧化氢与甲酸等摩尔、与双键摩尔比为1:1，催化剂硫酸与稳定剂EDTA-2Na均占大豆油质量的3%，反应温度75℃，停留时间3min，可合成环氧值6.3%的环氧大豆油。采用自行开发的大通量管式反应器进行环氧大豆油的放大生产，过氧化氢与甲酸等摩尔、与双键摩尔比为1:1，催化剂硫酸占大豆油质量的3%，稳定剂EDTA-2Na占大豆油质量的5%，反应温度75℃，停留时间4min，可合成环氧值6.0%的环氧大豆油，达到市售高品质环氧大豆油的水平，实现环氧大豆油1000t/a规模化生产。

关键词：微流场技术 环氧化 工艺

Abstract

The epoxy soybean oil is a kind of chemical product which is produced by the oxidation of soybean oil. It is a kind of widely used polyvinyl chloride, non-toxic plasticizer and stabilizer. At the same time, the epoxy groups are obtained by the open loop, and can be further used for the preparation of lubricating oil or polyurethane materials. Because of the hydrogen peroxide in the reaction raw material, the conventional batch reactor has the safety hidden trouble, and the product quality is general. Micro flow field technology is a process based on the strengthening of the technological innovation. Compared with the traditional batch reactor, the micro flow field has the advantages of low operation cost, easy control, easy to process and safety. Due to the extremely high specific surface area, high heat and mass transfer can be realized. Moreover, as a continuous flow reaction, micro flow field’s returning to smaller mixing can effectively improve the selectivity of the reaction.

In order to solve the problem of the shortcomings of the existing synthesis process and properties of epoxy soybean oil, we used soybean oil as raw material, combined with the existing micro channel epoxy soybean oil in the synthesis process parameters, then we used Chinese pipe reactor to epoxidize soybean oil kiloton continuous production by optimizing the parameters.

Pilot scale test of epoxidation of vegetable oil. Referring to the relevant parameters about epoxidation of vegetable oil in lab scale, the production scale was gradually enlarged by fine-tuning. When the Corning reactor was employed, the conditions were as follows: molar ratio of hydrogen peroxide to formic acid, double bond was set as 1:1:1, the catalyst sulphuric acid and stabilizer EDTA-2Na account for 3 wt% of the soybean oil mass, the temperature was set as 75 °C, and the residence time was set as 3 min. Under the mentioned conditions, an epoxidized soybean oil with an epoxy content of 6.3% was obtained. When the self-designed high flux tubular reactor was employed, the conditions were as follows: molar ratio of hydrogen peroxide to formic acid, double bond was set as 1:1:1, the catalyst sulphuric

acid and stabilizer EDTA-2Na accounts for 3 and 5 wt% of the soybean oil mass, respectively, the temperature was set as 75 °C, and the residence time was set as 4 min. Under the mentioned conditions, an epoxidized soybean oil with an epoxy content of 6.0% was obtained, reaching the level of commercially available high-quality epoxidized soybean oil. Thus, a production line of 1000 t/a for epoxidized soybean oi was successfully established.

Key words: Microflow system;Epoxidation; Technology.

目 录

摘 要 I

Abstract II

第一章 绪论 1

1.1 环氧大豆油概况 1

1.1.1 环氧大豆油简介 1

1.1.2 环氧大豆油合成方法 1

1.2 微流场技术概况 3

1.2.1 微流场技术的特点 3

1.2.2 微流场技术的应用 4

1.3 课题研究目的及研究内容 6

1.3.1 研究目的 5

1.3.2 研究内容 6

第二章 大豆油环氧化中试 7

2.1 前言 7

2.2 实验部分 7

2.2.1 实验原料 7

2.2.2 中试装置 8

2.2.3 环氧大豆油的中试合成 10

2.2.4 测试与表征 12

2.3 结果与讨论 13

2.3.1 康宁微反应器中合成环氧大豆油 13

2.3.2 管式反应器中合成环氧大豆油 14

第三章 结论与展望 16

3.1 结论 16

3.2 展望 16

参考文献 17

致 谢 20

第一章 绪论

1.1 环氧大豆油概况

1.1.1 环氧大豆油简介

请支付后下载全文，论文总字数：17538字