CN103420836A - 含氟低碳脂肪酸的提纯方法 - Google Patents
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- 238000000034 method Methods 0.000 title claims abstract description 24
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- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 title description 10
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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
本发明公开了一种合成二氟乙酸酯的方法。该方法在压力容器下，采用二氯乙酸酯在无水、较高温度条件下，与氟代试剂进行氟氯交换反应，产物选择性达到95％以上。
Description
技术领域
本发明涉及含氟低碳脂肪酸的一种提纯方法。
背景技术
CN97109774提供了一种有机磺酸的提纯方法，采用pH为-0.57～7酸水处理后，将水相分离。
US2011065995公开了一种合成和分离二氟乙酸的方法，该方法以二氯乙酰氯和氟化氢为原料，在铬基催化剂存在下的气相合成二氟乙酰氟和二氟乙酸，并利用分馏塔将二氟乙酸分离出来。
CN101967091公开了一种提纯有机酸的方法，母液先经过超滤或微滤形成渗透液，再经活性炭脱色，最后用阴、阳离子交换树脂除杂，提高了有机酸的纯度。
CN1131139公开了一种利用精馏的方式提纯乙酸的方法，精馏柱塔板数不低于30，回流比不低于4，真空度在40～760mmHg，得到高纯度的乙酸。
CN1944374公开了一种醋酸的提纯方法，粗品经过吸收和气提两步骤后，经过脱轻相、脱水、脱重相、脱废酸处理后得到高产率的醋酸。
上述的提纯方法都存在各种问题，其中最主要的就是都不能严格地控制产品的含水量。采用分液、离子交换的方式，得到产品的含水量都较大。采用塔分离的方式由于含氟酸和水共沸的原因对设备要求较高，工艺上也较难控制。
发明内容
本发明的目的是提供一种含氟低碳脂肪酸的提纯方法。
含氟低碳脂肪酸的提纯方法是将含氟低碳脂肪酸粗产品经过加热蒸出低沸点杂质，加热温度为30～100℃，然后趁热过滤，用0.5～3当量的无机强碱处理，生成的含氟低碳脂肪酸盐经干燥处理，使之含水量不超过1‰，再用0.5～5当量的高浓度强酸酸化。
所述的含氟低碳脂肪酸是氟乙酸、二氟乙酸、三氟乙酸、氟丙酸、二氟丙酸、三氟丙酸、氟丁酸、二氟丁酸，以及三氟丁酸。加热温度为30～100℃，优选为50～80℃。无机强碱是氢氧化锂、氢氧化钠、氢氧化钾。高浓度强酸为98％的浓硫酸。含氟低碳脂肪酸和无机强碱的摩尔比是1∶0.5～3，优选为1∶1～2。含氟低碳脂肪酸盐与高浓度强酸的摩尔比为1∶0.5～5，优选为1∶1～4。
具体实施方式
实施例1
向500ml四口烧瓶中加入100g粗品二氟乙酸，升温至80℃，常压精馏掉低沸杂质。降温至0～10℃，滴加100g40％质量分数NaOH水溶液，滴毕搅拌反应1小时。减压蒸掉大部分水，加入200ml甲苯，升温回流至分水器基本无水分出。物料降温至5℃搅拌1小时，过滤。收集白色或淡黄色晶体，真空干燥箱中70℃烘4～6小时，水份检测＜0.1％。(滤液回收套用收率可达100％)
500ml四口烧瓶中加入98％浓硫酸300g，搅拌，冰浴控温10～20℃。缓慢、分批加入无水二氟乙酸钠118g(1mol)，加毕，撤冰浴。缓慢升温，75mmHg减压精馏得无水二氟乙酸(88.3g，收率92％)。
实施例2
向500ml四口烧瓶中加入100g粗品二氟乙酸，升温至80℃，常压精馏掉低沸杂质。降温至0～10℃，滴加140g40％质量分数KOH水溶液，滴毕搅拌反应1小时。减压蒸掉大部分水，加入200ml甲苯，升温回流至分水器基本无水分出。物料降温至5℃搅拌1小时，过滤。收集白色或淡黄色晶体，真空干燥箱中70℃烘4～6小时，水份检测＜0.1％。(滤液回收套用收率可达100％)
500ml四口烧瓶中加入98％浓硫酸300g，搅拌，冰浴控温10～20℃。缓慢、分批加入无水二氟乙酸钾134g(1mol)，加毕，撤冰浴。缓慢升温，常压精馏收集132～134℃馏分(79.7g，收率83％)。
实施例3
向500ml四口烧瓶中加入58g粗品三氟乙酸，升温至40℃，常压精馏掉低沸杂质。降温至0～10℃，滴加50g40％质量分数NaOH水溶液，滴毕搅拌反应1小时。减压蒸掉大部分水，加入200ml甲苯，升温回流至分水器基本无水分出。物料降温至5℃搅拌1小时，过滤。收集白色或淡黄色晶体，真空干燥箱中70℃烘4～6小时，水份检测＜0.1％。(滤液回收套用收率可达100％)
250ml四口烧瓶中加入98％浓硫酸150g，搅拌，冰浴控温5～10℃。缓慢、分批加入无水三氟乙酸钠68g(0.5mol)，加毕，撤冰浴。缓慢升温，常压精馏，收集72～73℃馏分(53g，收率93％)。
实施例4
向500ml四口烧瓶中加入65g粗品三氟丙酸，升温至80℃，常压精馏掉低沸杂质。降温至10～20℃，滴加50g40％质量分数NaOH水溶液，滴毕搅拌反应1小时。减压蒸掉大部分水，加入200ml甲苯，升温回流至分水器基本无水分出。物料降温至5℃搅拌1小时，过滤。收集白色或淡黄色晶体，真空干燥箱中70℃烘4～6小时，水份检测＜0.1％。(滤液回收套用收率可达100％)
向250ml四口烧瓶中加入98％浓硫酸150g，搅拌，冰浴控温5～10℃。缓慢、分批加入无水三氟丙酸钠75g(0.5mol)，加毕，撤冰浴。缓慢升温，75mmHg减压精馏收集三氟丙酸(54.4g，收率85％)。
Claims (8)
1.制备式(1)所示的二氟乙酸酯的方法。
其中R表示含有1～6个碳原子的直链或支链的脂肪族烃基，或者6个碳原子以上的芳香族烃基，其特征在于该方法在压力容器内，以二氯乙酸酯与氟代试剂为原料，采用惰性气体保护的条件下，在极性溶剂中进行氟氯交换反应，反应体系含水量不超过200ppm，反应温度从0℃到350℃，二氯乙酸酯和氟代试剂的摩尔配比为1∶0.5～5.0，反应液经精馏提纯得到高纯度二氟乙酸酯。
2.根据权利要求1的方法，其特征在于所述的二氯乙酸酯为二氯乙酸甲酯、二氯乙酸乙酯、二氯乙酸正丙酯、二氯乙酸异丙酯、二氯乙酸正丁酯、二氯乙酸仲丁酯、二氯乙酸异丁酯、二氯乙酸叔丁酯、二氯乙酸正戊酯、二氯乙酸异戊酯、二氯乙酸丁酯、二氯乙酸苯酯、二氯乙酸苄酯、二氯乙酸二甲基苄基原酯、二氯乙酸二甲基苯乙基原酯、二氯乙酸二甲基苄基乙醇酯。
3.根据权利要求1的方法，其特征在于所述的氟代试剂为氟化氢、氟化钠、氟化钾、氟化铯、氟代烷基磺酰氟、烷基酰氟、吡啶-氟化氢络合液。
4.根据权利要求1的方法，其特征在于二氯乙酸酯与氟代试剂的摩尔配比为1∶0.5～5.0，优选为1∶1.0～4.0。
5.根据权利要求1的方法，其特征在于所述的极性溶剂为N，N-二甲基甲酰胺(DMF)、二甲基亚砜(DMSO)、N，N-二甲基乙酰胺(DMAC)、乙二醇、1，2-丙二醇、1，3-丙二醇、甘油、二乙二醇、N-甲基吡咯烷酮(NMP)、环丁砜(TMS)、苄基腈、吡啶基腈、六甲基磷酸三酰胺(HMPA)、1，3-二甲基-2-咪唑喹啉酮(DMI)。
6.根据权利要求1的方法，其特征在于反应体系含水量不超过200ppm，优选为不超过100ppm。
7.根据权利要求1的方法，其特征在于反应温度从0℃到350℃，优选为80℃到300℃。
8.根据权利要求1的方法，其特征在于所述的惰性气体为氮气。
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| CN101878189A (zh) * | 2007-09-28 | 2010-11-03 | 罗地亚管理公司 | 回收氟代羧酸的方法 |
| US20110065955A1 (en) * | 2008-03-19 | 2011-03-17 | Rhodia Operations | Method For Preparing Difluoroacetic Acid and Salts Thereof |
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| CN1447787A (zh) * | 2000-08-23 | 2003-10-08 | 纳幕尔杜邦公司 | 氟代烷酸的纯化方法 |
| CN1944376A (zh) * | 2006-10-10 | 2007-04-11 | 中昊晨光化工研究院 | 一种全氟辛酸的提纯方法 |
| CN101878189A (zh) * | 2007-09-28 | 2010-11-03 | 罗地亚管理公司 | 回收氟代羧酸的方法 |
| US20110065955A1 (en) * | 2008-03-19 | 2011-03-17 | Rhodia Operations | Method For Preparing Difluoroacetic Acid and Salts Thereof |
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