CN105906592B - 一种2-呋喃甲酸异戊酯纯化的方法 - Google Patents
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Abstract
本发明提供了提供一种2‑呋喃甲酸异戊酯纯化的方法，工业级2‑呋喃甲酸异戊酯经过装有本专利技术制得的吸附剂的层析柱中进行吸附，温度50～100℃，流速1‑5BV/h，可得到2‑呋喃甲酸异戊酯纯化产品。
Description
技术领域
本发明涉及一种提纯的方法，特别是一种2-呋喃甲酸异戊酯纯化的方法。
背景技术
我国是糠醛生产大国，产品主要供应国际市场，受国际贸易影响严重，一旦出口减少，糠醛生产厂家会很被动，因此研究开发糠醛资源深加工和综合利用具有重要意义。糠酸异戊酯又名呋喃甲酸异戊酯，是糠醛深加工产品呋喃环香料中糠酸酯类的一种，具有可可和巧克力味，糠醛为原料制备2-呋喃甲酸异戊酯，产物含有微量的含有2-呋喃甲酸-2-甲基丁酯，需要进一步提纯。
CN103391930A公开了作为增塑剂的呋喃二甲酸的C11-C13二烷基酯。采用真空条件下，使用氮气气提进行纯化，再经冷却过滤，得到纯度99.5％的酯含量
CN103380120A公开了作为增塑剂的呋喃二甲酸戊酯。在沸石的存在下将过量的醇在减压下去除，并通过蒸馏纯化粗产物，得到产品。
CN102666521A公开了一种2，5-呋喃二甲酸的二烷基酯的制备方法，该方法包括以下步骤：在高于140℃的温度下，使包括选自5-羟甲基糠醛(HMF)、5-羟甲基糠醛的酯、5-甲基糠醛、5(氯甲基)糠醛、5-甲基糠酸、5-(氯甲基)糠酸、2，5-二甲基呋喃和两种以上这些化合物的混合物的化合物的进料在氧化催化剂存在的情况下与氧化剂接触。
目前文献中所报道的提纯2-呋喃甲酸异戊酯的方法，主要采用蒸馏的方法，仍含有一些杂质不能去除，需要新的纯化方法。
发明内容
本发明目的在于解决现有技术中存在的上述技术问题，提供一种2-呋喃甲酸异戊酯纯化的方法。
本发明所述的一种2-呋喃甲酸异戊酯纯化的方法，通过以下步骤制备：
步骤1.吸附剂的制备：
在反应釜中按重量份计加入100份氯甲基化聚苯乙烯树脂、500-1000份二氯乙烷，50-100份质量百分比浓度20-50的三乙胺水溶液，1-5份N-(1，3-二甲基丁酯)-N’-苯基对苯二胺，1-10份1，3-二甲基丁胺盐酸盐，在20-60℃反应15-50h，过滤，烘干后得到吸附剂；
步骤2.吸附提纯2-呋喃甲酸异戊酯：
按重量份计，100份工业级2-呋喃甲酸异戊酯经过装有吸附剂的层析柱中进行吸附，温度50～100℃，流速1-5BV/h，可得到2-呋喃甲酸异戊酯纯化产品。
所述的氯甲基化聚苯乙烯树脂为市售产品，如上海紫一试剂厂生产的产品；N-(1，3-二甲基丁酯)-N’-苯基对苯二胺为市售产品，如山东金盛新材料科技有限公司生产的产品；
所述的工业级2-呋喃甲酸异戊酯为市售产品；1，3-二甲基丁胺盐酸盐为市售产品。
与现有技术相比，本发明的催化剂及其制备方法，具有以下有益效果：
胺基树脂骨架上带有二甲基丁酯，二甲基丁胺官能团，提高了对2-呋喃甲酸异戊酯中2-呋喃甲酸-2-甲基丁酯等杂质的吸附能力，可得到质量百分含量最高99.9％的2-呋喃甲酸异戊酯产品。
具体实施方式
以下实例仅仅是进一步说明本发明，并不是限制本发明保护的范围。
实施例中工业级2-呋喃甲酸异戊酯，质量百分含量99.11，其中含有2-呋喃甲酸-2-甲基丁酯杂质。
实施例1：
步骤1.吸附剂的制备：在2000L反应釜中加入100Kg氯甲基化聚苯乙烯树脂、800Kg二氯乙烷，80Kg质量百分比浓度40的三乙胺水溶液，3KgN-(1，3-二甲基丁酯)-N’-苯基对苯二胺，5Kg1，3-二甲基丁胺盐酸盐，在40℃反应30h，过滤，烘干后得到吸附剂；
步骤2.吸附提纯2-呋喃甲酸异戊酯：
将1000Kg工业级2-呋喃甲酸异戊酯经过装有吸附剂的层析柱中进行吸附，温度70℃，流速2BV/h，可得到2-呋喃甲酸异戊酯纯化产品。2，5-呋喃二甲酸异戊酯质量百分含量见表1，编号为M-1。
实施例2：
步骤1.吸附剂的制备：在2000L反应釜中加入100Kg氯甲基化聚苯乙烯树脂、500Kg二氯乙烷，50Kg质量百分比浓度40的三乙胺水溶液，1KgN-(1，3-二甲基丁酯)-N’-苯基对苯二胺，1Kg1，3-二甲基丁胺盐酸盐，在20℃反应15h，过滤，烘干后得到吸附剂；
步骤2.吸附提纯2-呋喃甲酸异戊酯：
将100Kg工业级2-呋喃甲酸异戊酯经过装有吸附剂的层析柱中进行吸附，温度50℃，流速1BV/h，可得到2-呋喃甲酸异戊酯纯化产品。2，5-呋喃二甲酸异戊酯质量百分含量见表1，编号为M-2。
实施例3
步骤1.吸附剂的制备：在2000L反应釜中加入100Kg氯甲基化聚苯乙烯树脂、1000Kg二氯乙烷，100Kg质量百分比浓度40的三乙胺水溶液，5KgN-(1，3-二甲基丁酯)-N’-苯基对苯二胺，10Kg1，3-二甲基丁胺盐酸盐，在60℃反应50h，过滤，烘干后得到吸附剂；
步骤2.吸附提纯2-呋喃甲酸异戊酯：
将100Kg工业级2-呋喃甲酸异戊酯经过装有吸附剂的层析柱中进行吸附，温度100℃，流速5BV/h，可得到2-呋喃甲酸异戊酯纯化产品。2，5-呋喃二甲酸异戊酯质量百分含量见表1，编号为M-3。
对比例1
不加入N-(1，3-二甲基丁酯)-N’-苯基对苯二胺，其它同实施例1。2，5-呋喃二甲酸异戊酯质量百分含量见表1，编号为M-4。
对比例2
不加入1，3-二甲基丁胺盐酸盐，其它同实施例1。2，5-呋喃二甲酸异戊酯质量百分含量见表1，编号为M-5。
对比例3
不加入1，3-二甲基丁胺盐酸盐，N-(1，3-二甲基丁酯)-N’-苯基对苯二胺，其它同实施例1。2，5-呋喃二甲酸异戊酯质量百分含量见表1，编号为M-6。
经过气相色谱检测，实施例1-3以及对比例1-3提纯后2，5-呋喃二甲酸异戊酯质量百分含量的比较见表1：
表1：不同工艺做出的试验样品吸附后，2，5-呋喃二甲酸异戊酯质量百分含量的比较
| 编号 | 2，5-呋喃二甲酸异戊酯质量百分含量％ |
| M-1 | 99.95 |
| M-2 | 99.96 |
| M-3 | 99.98 |
| M-4 | 99.86 |
| M-5 | 99.73 |
| M-6 | 99.41 |
以上仅为本发明的具体实施例，但本发明的技术特征并不局限于此。任何以本发明为基础，为解决基本相同的技术问题，实现基本相同的技术效果，所作出的简单变化、等同替换或者修饰等，皆涵盖于本发明的保护范围之中。
Claims (1)
1.一种2-呋喃甲酸异戊酯纯化的方法，其特征在于包括以下步骤：
步骤1.吸附剂的制备：
在反应釜中按重量份计加入100份氯甲基化聚苯乙烯树脂、500-800份二氯乙烷，50-80份质量百分比浓度20-40的三乙胺水溶液，1-5份N-(1，3-二甲基丁酯)-N’-苯基对苯二胺，1-5份1，3-二甲基丁胺盐酸盐，在20-40℃反应15-30h， 过滤，烘干后得到吸附剂；
步骤2.吸附提纯2-呋喃甲酸异戊酯：
按重量份计，100份工业级2-呋喃甲酸异戊酯经过装有吸附剂的层析柱中进行吸附，温度50～70℃，流速1-2BV/h，可得到2-呋喃甲酸异戊酯纯化产品。
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| 硫酸氢钠催化合成糠酸异戊酯的工艺研究;孟祥福;《食品科技》;20080531;第5卷;第138-140页 * |
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