CN106478581A - 一种维生素e醋酸酯的制备方法 - Google Patents
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Abstract
本发明公开一种维生素E醋酸酯的制备方法，包括以下步骤：2,3,5‑三甲基氢醌与异植物醇在由浓硫酸、硫酸铜、氯化锡组成的催化剂催化下反应生成维生素E，所得维生素E再与醋酐发生酯化反应，得到维生素E醋酸酯。本发明以浓硫酸、硫酸铜、氯化锡为催化剂，各组分有很好的协同催化功能，减少了催化剂的使用量，降低了反应温度，有效减少了反应副产物，提高了反应收率；本发明操作简便，生产难度小，制造成本低，环境友好，适合大规模工业化生产。
Description
技术领域
本发明属于维生素制备领域，具体是一种维生素E醋酸酯的制备方法。
背景技术
维生素E具有抗衰老，提高免疫力的作用，对心脑血管疾病有辅助治疗作用，在制药行业、保健品行业、食品行业、化妆品行业得到了广泛的应用。维生素E最主要的商品化形式是维生素E醋酸酯(一般指α-生育酚乙酸酯)，工业上维生素E醋酸酯一般先通过三甲基氢醌和异植物醇、植醇或其衍生物的缩合得到生育酚，然后生育酚再与乙酸酐进行酯化反应得到维生素E醋酸酯。
中国专利CN01104390《制备α-生育酚乙酸酯的方法》公开了一种在循环法中制备α-生育酚乙酸酯的方法，其公开了制备方法：最初得到的α-生育酚和α-生育酚乙酸酯的混合物用醋酸酐酯化，形成醋酸；通过萃取后得到的催化剂醋酸溶液被再生，含醋酸的再生溶液被返回到反应中，以及合并的在前面步骤中得到的含活性催化剂组分卤化锌和氢卤酸的催化剂醋酸溶液被浓缩，并以液体形式被返回到反应中。该方法催化剂可循环套用，减轻了环保的压力。但是醋酸和水分离过程中存在分离效率低、能耗高的问题；浓缩含活性催化剂组分卤化锌和氢卤酸的催化剂醋酸溶液能耗高，循环用的催化剂体系水分不好控制导致催化剂在随后的循环套用中α-生育酚的五元环异构体逐渐升高，甚至不合格，所以该方法实际上并不适用于工业化生产。
中国专利CN102336732A公开一种一锅法制备维生素E乙酸酯的生产方法，该方法分为三步：制备三甲基氢醌；制备DL-α-生育酚；制备维生素E乙酸酯，虽然是一锅制备，但步骤繁琐，导致维生素E乙酸酯的收率低。
发明内容
本发明的目的在于提供一种维生素E醋酸酯的制备方法。
本发明的目的可以通过以下技术方案实现：
一种维生素E醋酸酯的制备方法，其特征在于，包括以下步骤：
(1)向反应溶剂中加入2,3,5-三甲基氢醌和由浓硫酸、硫酸铜、氯化锡组成的催化剂，搅拌至物料溶解，在N2保护下，温度控制30-33℃，在3-3.5h内滴加异植物醇，滴加完毕，升温至62-66℃，保温反应2.5h，反应结束，分液，减压蒸馏回收溶剂，反应液洗涤，萃取维生素E，去离子水洗涤直至溶液pH为7，其中，异植物醇与2,3,5-三甲基氢醌的质量比为2-2.5:1，硫酸铜与2,3,5-三甲基氢醌的质量比为0.045-0.05:1，氯化锡与2,3,5-三甲基氢醌的质量比为0.006-0.012:1，浓硫酸与与2,3,5-三甲基氢醌的质量比为0.2-0.4:1；
(2)向步骤(2)洗涤后的维生素E层中加入醋酸酐与硼氢化钠，N2保护下，升温至126-130℃酯化反应3.5h，反应结束，减压精馏回收醋酸酐，用水及70-80％甲醇交叉洗涤至洗出液pH为7，洗涤两次，50-60℃减压浓缩，回收石油醚，浓缩毕，得维生素E醋酸酯，其中，醋酸酐与2,3,5-三甲基氢醌的重量比为2.3-2.7:1，硼氢化钠的加入量为醋酸酐质量的0.1-0.16％。
进一步方案，所述步骤(1)升温速率为0.1-0.2℃/min。
进一步方案，所述步骤(1)反应溶剂为直链烃、芳香烃中的至少一种。
进一步方案，所述步骤(1)中异植物醇与2,3,5-三甲基氢醌的质量比为2.2:1，硫酸铜与2,3,5-三甲基氢醌的质量比为0.048:1，氯化锡与2,3,5-三甲基氢醌的质量比为0.009:1，浓硫酸与与2,3,5-三甲基氢醌的质量比为0.3:1。
本发明的有益效果：本发明以浓硫酸、硫酸铜、氯化锡为催化剂，各组分有很好的协同催化功能，减少了催化剂的使用量，降低了反应温度，有效减少了反应副产物，提高了反应收率；本发明操作简便，生产难度小，制造成本低，环境友好，适合大规模工业化生产。
具体实施方式
下面结合具体实施例对本发明作进一步详细描述。
实施例1
向反应溶剂中加入2,3,5-三甲基氢醌1000g和由200g浓硫酸、45g硫酸铜、6g氯化锡组成的催化剂，搅拌至物料溶解，在N2保护下，温度控制30℃，在3h内滴加异植物醇2000g，滴加完毕，以0.1℃/min的速率升温至62℃，保温反应2.5h，反应结束，分液，减压蒸馏回收溶剂，反应液洗涤，萃取维生素E，去离子水洗涤直至溶液pH为7；
向洗涤后的维生素E层中加入醋酸酐2300g与硼氢化钠2.3g，N2保护下，升温至126℃酯化反应3.5h，反应结束，减压精馏回收醋酸酐，用水及70-80％甲醇交叉洗涤至洗出液pH为7，洗涤两次，50℃减压浓缩，回收石油醚，浓缩毕，得维生素E醋酸酯。
实施例2
向反应溶剂中加入2,3,5-三甲基氢醌1000g和由300g浓硫酸、48g硫酸铜、9g氯化锡组成的催化剂，搅拌至物料溶解，在N2保护下，温度控制33℃，在3.2h内滴加异植物醇2200g，滴加完毕，以0.2℃/min的速率升温至64℃，保温反应2.5h，反应结束，分液，减压蒸馏回收溶剂，反应液洗涤，萃取维生素E，去离子水洗涤直至溶液pH为7；
向洗涤后的维生素E层中加入醋酸酐2500g与4g硼氢化钠，N2保护下，升温至130℃酯化反应3.5h，反应结束，减压精馏回收醋酸酐，用水及70-80％甲醇交叉洗涤至洗出液pH为7，洗涤两次，55℃减压浓缩，回收石油醚，浓缩毕，得维生素E醋酸酯。
实施例3
向反应溶剂中加入2,3,5-三甲基氢醌1000g和由400g浓硫酸、50g硫酸铜、12g氯化锡组成的催化剂，搅拌至物料溶解，在N2保护下，温度控制33℃，在3.5h内滴加异植物醇2500g，滴加完毕，以0.15℃/min的速率升温至66℃，保温反应2.5h，反应结束，分液，减压蒸馏回收溶剂，反应液洗涤，萃取维生素E，去离子水洗涤直至溶液pH为7；
向洗涤后的维生素E层中加入醋酸酐2700g与3.24g硼氢化钠，N2保护下，升温至128℃酯化反应3.5h，反应结束，减压精馏回收醋酸酐，用水及70-80％甲醇交叉洗涤至洗出液pH为7，洗涤两次，55℃减压浓缩，回收石油醚，浓缩毕，得维生素E醋酸酯。
上述的对实施例的描述是为便于该技术领域的普通技术人员能理解和应用本发明。熟悉本领域技术的人员显然可以容易地对实施案例做出各种修改，并把在此说明的一般原理应用到其他实施例中而不必经过创造性的劳动。因此，本发明不限于这里的实施案例，本领域技术人员根据本发明的揭示，不脱离本发明范畴所做出的改进和修改都应该在本发明的保护范围之内。
Claims (4)
1.一种维生素E醋酸酯的制备方法，其特征在于，包括以下步骤：
(1)向反应溶剂中加入2,3,5-三甲基氢醌和由浓硫酸、硫酸铜、氯化锡组成的催化剂，搅拌至物料溶解，在N2保护下，温度控制30-33℃，在3-3.5h内滴加异植物醇，滴加完毕，升温至62-66℃，保温反应2.5h，反应结束，分液，减压蒸馏回收溶剂，反应液洗涤，萃取维生素E，去离子水洗涤直至溶液pH为7，其中，异植物醇与2,3,5-三甲基氢醌的质量比为2-2.5:1，硫酸铜与2,3,5-三甲基氢醌的质量比为0.045-0.05:1，氯化锡与2,3,5-三甲基氢醌的质量比为0.006-0.012:1，浓硫酸与与2,3,5-三甲基氢醌的质量比为0.2-0.4:1；
(2)向步骤(2)洗涤后的维生素E层中加入醋酸酐与硼氢化钠，N2保护下，升温至126-130℃酯化反应3.5h，反应结束，减压精馏回收醋酸酐，用水及70-80％甲醇交叉洗涤至洗出液pH为7，洗涤两次，50-60℃减压浓缩，回收石油醚，浓缩毕，得维生素E醋酸酯，其中，醋酸酐与2,3,5-三甲基氢醌的重量比为2.3-2.7:1，硼氢化钠的加入量为醋酸酐质量的0.1-0.16％。
2.根据权利要求1所述的一种维生素E醋酸酯的制备方法，其特征在于，所述步骤(1)升温速率为0.1-0.2℃/min。
3.根据权利要求1所述的一种维生素E醋酸酯的制备方法，其特征在于，所述步骤(1)反应溶剂为直链烃、芳香烃中的至少一种。
4.根据权利要求1所述的一种维生素E醋酸酯的制备方法，其特征在于，所述步骤(1)中异植物醇与2,3,5-三甲基氢醌的质量比为2.2:1，硫酸铜与2,3,5-三甲基氢醌的质量比为0.048:1，氯化锡与2,3,5-三甲基氢醌的质量比为0.009:1，浓硫酸与与2,3,5-三甲基氢醌的质量比为0.3:1。
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