CN102549131A - 带有大量皂化产物的脂肪酸烷基酯的纯化方法 - Google Patents

带有大量皂化产物的脂肪酸烷基酯的纯化方法 Download PDF

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CN102549131A
CN102549131A CN2010800408472A CN201080040847A CN102549131A CN 102549131 A CN102549131 A CN 102549131A CN 2010800408472 A CN2010800408472 A CN 2010800408472A CN 201080040847 A CN201080040847 A CN 201080040847A CN 102549131 A CN102549131 A CN 102549131A
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鲁道夫·邦施
埃克哈德·西德尔
赫尔穆特·萨夫特
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Abstract

本发明涉及借助于含有配位剂的含水酸性甘油相从脂肪酸烷基酯相中连续萃取杂质,特别是皂化产物的方法,所述脂肪酸烷基酯相是通过植物或动物油或脂肪的酯交换获得的,该植物或动物油或脂肪具有形成皂化产物的高倾向性。

Description

带有大量皂化产物的脂肪酸烷基酯的纯化方法
技术领域
本发明涉及通过与甘油相混合从脂肪酸烷基酯相中连续萃取杂质,特别是皂化产物的方法。
背景技术
如在例如DE 10 2006 044 467A1中所描述的,根据生产生物柴油的方法,在植物或动物来源的油或脂肪的酯交换中,最初获得粗烷基酯,该粗烷基酯取决于所使用油或脂肪的种类会或多或少地带有杂质。只有通过把这些杂质从所述粗烷基酯中分离才能得到可用的生物柴油。这些杂质由源于所述油或脂肪的粘质残余物以及皂化产物组成,所述皂化产物来源于在所用的油或脂肪中所包含的游离脂肪酸(FFA)与用于所述酯交换反应的碱性催化剂的反应,所述碱性催化剂一般为NaOH。在某些油例如麻风树油的酯交换中,在该酯交换中获得的脂肪酸烷基酯也与用作催化剂的氢氧化钠溶液反应并部分皂化。
从所述脂肪酸烷基酯相中分离所述杂质的方法是已知的。
在DE 10 2006 044 467B4中,所述粗烷基酯的纯化是借助于用1至5%的盐酸洗涤来实现的。在该工艺中,所述酸中和了所述碱性催化剂并且通过将皂转化为FFA而将其分解。
这种纯化方法的缺点在于由此得到的FFA由于它们具有由其分子中的非极性烃链所导致的斥水性而仍然留在所述烷基酯相中,并且不进入到所述酸性含水洗涤相中。由于在生物柴油中FFA通常是不需要的,标准EN 14214中规定了最大值,因此这种方法仅适用于在所述粗烷基酯中皂化产物的量不是太高的时候。
本领域技术人员还知道在高含量的皂化产物的情况下同样不能进行借助于pH中性水从脂肪酸烷基酯中萃取所述皂化产物的方法。原因一方面是在这些条件下,在所述脂肪酸烷基酯和所述萃取水的必要充分混合过程中形成了非常稳定的乳状液,从该乳状液中,所述酯相只能以损失大量酯的方式被分离出来。此外,用于萃取的设备,例如洗涤塔或混合沉降器,很快被所述皂化产物污染及堵塞。
在DE 43 01 686C1中提出在所述脂肪酸烷基酯相的纯化中完全不用水相,并且代之以使用甘油来去除杂质。随后,所述酯相中的剩余碱度应通过使用吸附剂例如漂白土或硅酸处理来去除。
作为此方法的一个优点,所说明的是其不需要水相以及对其进行再加工的成本。然而,必须看到如下缺点,不含水的、碱性甘油相对极性杂质例如过量的醇或皂的吸收能力不是很强。另外,吸附剂的使用涉及到可观的成本以及产生要被处理的残余物。
因为上述用于纯化带有大量皂化产物的脂肪酸烷基酯的方法鉴于技术或经济的原因并不适用,因此希望提供用于预纯化的方法,利用这种方法可以使皂负荷被降低到可以使用一种已知的方法进行进一步纯化的程度。
发明内容
根据本发明,此目的通过这样的方式实现:为了纯化,将所述脂肪酸烷基酯相与酸性含水甘油相混合,所述酸性含水甘油相下文中被称为洗涤甘油相,其包含甘油和5至40重量%的水以及配位剂,并且其pH值为3至6,优选4至5。
本发明进一步的发展、优点以及可能的应用还可以从下面的描述中获得。所有描述的特征自身或任意组合形成了本发明主题,而不取决于它们在权利要求中所概括的内容或它们的引用关系。
包含在所述洗涤甘油相中的酸中和了所述碱性酯交换催化剂并且由此防止了所述酯的进一步皂化。配位剂,优选柠檬酸,用于结合被引入到与所述油或脂肪进行的酯交换过程中的多价碱土金属阳离子,例如Ca,Mg,Fe和Cu离子,以形成络合物并且由此防止几乎不溶于所述酯和几乎不溶于所述洗涤甘油相的碱土金属皂的形成。
归因于水含量,所述洗涤甘油相的极性增加了,且由此增加了对要从所述酯相中除去的皂以及对其它极性杂质,如过量的甲醇或乙醇的吸收能力。
使用这种方法的特别优点在于,将其集成到通过植物和动物油或脂肪的酯交换来生产生物柴油的设备中以及生产过程中回收了用于萃取的洗涤甘油相。直接地或通过贮存罐,将待纯化的脂肪酸烷基酯相通过热交换器从最后酯交换阶段的沉降罐中供应到本发明的过程中来。根据本发明使用的洗涤甘油相是通过再加工酯交换期间获得的甘油相进行工艺内回收的。借助于对皂化产物的酸水洗,其被纯化并且通过蒸馏将其从甲醇或乙醇中释放出来。在进一步的蒸馏处理中,调整本发明方法中所要使用的甘油相的水分含量。随后,将粉状的配位剂溶于所述甘油相中。为了保证连续运转,优选将并联操作的两个批处理罐或批处理系统用于该目的。从那里,所述甘油相被供应到本发明的方法中作为洗涤甘油相。
随后将通过根据本发明的方法纯化的脂肪酸烷基酯相借助于酸水洗从残留的皂化反应产物中释放出来,并通过蒸发水分进行干燥,且由此作为待用的生物柴油存在。
在所述方法的一个特别有利方面中,将所述脂肪酸烷基酯相和所述洗涤甘油相混合是借助于萃取塔实现的,其中所述脂肪酸烷基酯相在所述塔中,在所述洗涤甘油相中由底部上升到顶部。
作为使用萃取塔的替代方案,所述方法可以借助于至少二级,优选三级的混合沉降器以逆流方式进行,其中优选使用集成到管道中的机械强力混合器。
有利地,所述方法是在环境压力下进行的,容器中充满氮气,且所述脂肪酸烷基酯相是在40℃至70℃之间,特别是在55℃至65℃之间的温度下供应到本方法中的。更低的温度会增加所述酯相和所述洗涤甘油相的粘度,并且由此会降低所述相之间的充分混合从而降低所述方法的有效性。另一方面,更高的温度会造成甲醇从所述酯相中大量释放从而引发爆炸的风险。
具体实施方式
下面将通过以下实施例阐述本发明:
实施例1
为了进行借助于双级酯交换工艺从麻风树油获得的脂肪酸甲酯的纯化,使用内径为5cm且总高为1.5m的萃取塔。所述塔包括MontzM/MN,B-1型规整填料,其具有250m2/m3的比表面积,由聚丙烯制成。所述规整填料的高度为1.0m。填充所述塔的萃取剂甘油相的入口位于所述塔的顶部。除甘油外,所述甘油相还包括15重量%的水并与柠檬酸混合。通过加入柠檬酸,将pH值调整到6。甘油相进入所述塔的连续流入量为125g/小时。
萃取物、经负载的甘油相的出口位于所述塔的底部,在最低点。在所述塔的底部,在所述规整填料的下面,供应待纯化的脂肪酸甲酯相,并且将其在甘油相的内部粉碎为小液滴,上升到所述塔的顶部且在最高点从所述塔中取出。所述脂肪酸甲酯的连续流入量为2,500g/小时。由于该酯交换过程已经被碱催化了,因此所述酯相的pH值为9,含有4重量%的皂化产物,9重量%的甲醇,0.4重量%的总甘油和100ppm的水。在所述塔顶部排出的被纯化的脂肪酸甲酯流共计2168g/小时。其包含0.05重量%的皂化产物,1重量%的甲醇,0.35重量%的总甘油和0.2重量%的水并且pH值为7。萃取是在大气压力下和65℃下进行的。在所述塔中没有形成明显的皂化产物沉淀。
实施例2
代替实施例1中使用的萃取塔,本实施例中使用三级混合沉降器。在每一级中,都是借助于集成到管道中的ULTRA TURRAX UTL型强力混合器进行混合。在所述三个沉降罐中的停留时间每个都为一个小时。进入所述混合沉降器中的材料流都和实施例1中具有相同的组成和规模。将待纯化的脂肪酸甲酯流和来自第二混合沉降器级的沉降罐的甘油相流供应到第一混合沉降器级的混合器中。所述脂肪酸甲酯流的温度为65℃。将用作萃取剂的甘油相以及来自于第二混合沉降器级的沉降罐的酯相供应到第三混合沉降器级的混合器中。借助于安装在第三混合沉降器级的混合器与沉降罐之间的热交换器,所述混合物的温度降低到25℃,以降低所述脂肪酸甲酯在所述甘油相中的溶解性从而降低脂肪酸甲酯的损失。因此,被纯化的脂肪酸甲酯相以2190kg/小时的流速和与实施例1相同的组成离开第三混合沉降器级的沉降罐。

Claims (8)

1.通过与甘油相混合从脂肪酸烷基酯相中连续萃取杂质,特别是皂化产物的方法,其特征在于所混合的甘油相含有5至40重量%的水以及配位剂,且其pH值为3至6,优选为4至5。
2.根据权利要求1所述的方法的应用,其特征在于将所述方法集成到通过植物或动物油或脂肪的酯交换来生产生物柴油的设备中。
3.根据权利要求1和2所述的方法,其特征在于所述含水甘油相是工艺过程中获得的。
4.根据权利要求1所述的方法,其特征在于所述方法是借助于萃取塔进行的,其中在所述塔内,所述脂肪酸烷基酯相由底部流向顶部且在所述甘油相中流动。
5.根据权利要求1所述的方法,其特征在于借助于至少两级,优选为三级的混合沉降器以逆流方式进行所述方法,其中优选使用集成到管道中的机械强力混合器。
6.根据权利要求1所述的方法,其特征在于将所述脂肪酸烷基酯相在40℃至70℃之间,优选55℃至65℃之间的温度下供应到所述方法中。
7.根据权利要求1所述的方法,其特征在于所述方法是在环境压力下进行的,并且将罐充满氮气。
8.根据权利要求1所述的方法,其特征在于将柠檬酸用作配位剂。
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