CN110922980A - 一种端基为氟代烷氧基的液晶材料的提纯方法 - Google Patents
一种端基为氟代烷氧基的液晶材料的提纯方法 Download PDFInfo
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- 125000004428 fluoroalkoxy group Chemical group 0.000 title claims abstract description 13
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- 229910021536 Zeolite Inorganic materials 0.000 claims description 2
- 238000005341 cation exchange Methods 0.000 claims description 2
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 claims description 2
- 150000004706 metal oxides Chemical class 0.000 claims description 2
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- 239000010457 zeolite Substances 0.000 claims description 2
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- 238000004128 high performance liquid chromatography Methods 0.000 description 5
- 239000000203 mixture Substances 0.000 description 5
- 239000012535 impurity Substances 0.000 description 3
- 150000001875 compounds Chemical class 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 238000001179 sorption measurement Methods 0.000 description 2
- 150000001336 alkenes Chemical group 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
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- 239000002994 raw material Substances 0.000 description 1
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- C09K19/30—Non-steroidal liquid crystal compounds containing at least two non-condensed rings containing saturated or unsaturated non-aromatic rings, e.g. cyclohexane rings
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- C09K19/10—Non-steroidal liquid crystal compounds containing at least two non-condensed rings containing at least two benzene rings
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- C09K19/30—Non-steroidal liquid crystal compounds containing at least two non-condensed rings containing saturated or unsaturated non-aromatic rings, e.g. cyclohexane rings
- C09K19/3001—Cyclohexane rings
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Abstract
本发明提供了一种端基为氟代烷氧基的液晶材料的提纯方法，包括如下步骤：(1)向待提纯的液晶材料中添加吸附剂，混合均匀；(2)将混有吸附剂的液晶材料投入离子膜提纯器中，施加外加电场，吸附0.5～3h，收集提纯后的液晶材料。所述电场强度1kV/cm～10kV/cm，电极间距20mm～50mm。本发明的端基为氟代烷氧基的液晶材料的提纯方法，提纯精度高，操作方便，无需使用其他溶剂即可进行提纯，节约了成本，更加安全环保。
Description
技术领域
本发明涉及一种提纯方法，尤其是一种高沸点端烯类液晶材料的提纯方法。
背景技术
随着显示面板对液晶材料纯度的要求越来越高，现有的提纯工艺已无法满足液晶材料超高纯度的要求。由于液晶材料的高技术壁垒，导致高纯度的中高端液晶材料市场多年来一直处于垄断状态。开发出高品质液晶单体的提纯方式势在必行。
液晶材料粗品除含有主要产品外，还含有微量无机杂质和大量极性有机杂质，而这些杂质主要是在液晶化合物合成过程中从原材料或仪器设备或生产环境引入，或由反应产生的副产物以及未反应的物料造成。目前有关液晶化合物的提纯方法主要有吸附法、分子蒸馏或精馏法、外加电场法、柱层析法等，这些方法虽能获得高精度的液晶产品，但是过程繁琐，提纯过程中使用的有机溶剂多数带有毒性且易燃易爆，有害健康且不利于环保，提纯后还会产生废液处理等问题，给企业带来了新的压力。
发明内容
本发明提供了一种端基为氟代烷氧基的液晶材料的提纯方法。
本发明的技术方案如下：
一种端基为氟代烷氧基的液晶材料的提纯方法，包括如下步骤：
(1)向待提纯的液晶材料中添加吸附剂，混合均匀；
(2)将混有吸附剂的液晶材料投入离子膜提纯器中，施加外加电场，吸附0.5～3h，收集提纯后的液晶材料；
所述吸附剂选自活性氧化铝、活性炭、硅胶、沸石中的一种或多种。
所述外加电场是交流电场。
所述吸附剂的孔径为1～10nm，吸附剂的比表面积为500～1000m2/g。
所述吸附剂与液晶材料的质量比1:5～1:20。
所述液晶材料在外加电场下的吸附时间为1～1.5h。
所述离子膜提纯器选自单一离子膜提纯器、双槽离子膜提纯器、三槽离子膜提纯器中的一种。
所述提纯器的离子膜为均相阴、阳离子交换膜，电极为网式贵金属氧化物涂层电极。
所述电场强度为1kV/cm～10kV/cm，电极间距为20～50mm。
有益效果：本发明的端基为氟代烷氧基的液晶材料的提纯方法，提纯精度高，操作方便，无需使用其他溶剂即可进行，节约成本，更加安全环保。
具体实施方式
实施例1
1.取3g含有
的待提纯液晶材料，0.6g孔径和比表面积分别为4nm和600m2/g的硅胶，混合均匀；
2.将混有硅胶的液晶材料投入到离子膜提纯器中，采用氧化物薄膜电极，极间距为20mm，电场强度为3kV/cm，保持60min，收集提纯后的液晶材料。经HPLC分析纯度为99.8％。
实施例2
1.取3g含有
的待提纯液晶材料，0.6g孔径和比表面积分别为4nm和600m2/g的硅胶，混合均匀；
2.将混有硅胶的液晶材料投入到离子膜提纯器中，采用氧化物薄膜电极，极间距为20mm，电场强度为3kV/cm，保持60min，收集提纯后的液晶材料。经HPLC分析纯度为99.5％。
实施例3
1.取3g含有
的待提纯液晶材料，0.6g孔径和比表面积分别为4nm和600m2/g的活性氧化铝，混合均匀；
2.将混有活性氧化铝的液晶材料投入到离子膜提纯器中，采用氧化物薄膜电极，极间距为20mm，电场强度为3kV/cm，保持60min，收集提纯后的液晶材料。经HPLC分析纯度为99.9％。
实施例4
1.取3g含有
的待提纯液晶材料，0.3g孔径和比表面积分别为4nm和600m2/g的活性氧化铝，混合均匀；
2.将混有活性氧化铝的液晶材料投入到离子膜提纯器中，采用氧化物薄膜电极，极间距为35mm，电场强度为5kV/cm，保持75min，收集提纯后的液晶材料。经HPLC分析纯度为99.7％。
实施例5
1.取3g含有
的待提纯液晶材料，0.3g孔径和比表面积分别为4nm和600m2/g的硅胶，混合均匀；
2.将混有硅胶的液晶材料投入到离子膜提纯器中，采用氧化物薄膜电极，极间距为35mm，电场强度为5kV/cm，保持75min，收集提纯后的液晶材料。经HPLC分析纯度为99.6％。
Claims (8)
1.一种端基为氟代烷氧基的液晶材料的提纯方法，其特征在于，包括以下步骤：
(1)向待提纯的液晶材料中添加吸附剂，混合均匀；
(2)将混有吸附剂的液晶材料投入离子膜提纯器中，施加外加电场，吸附0.5～3h，收集提纯后的液晶材料；
所述吸附剂选自活性氧化铝、活性炭、硅胶、沸石中的一种或多种。
2.根据权利要求1所述的端基为氟代烷氧基的液晶材料的提纯方法，其特征在于，所述外加电场是交流电场。
3.根据权利要求1所述的端基为氟代烷氧基的液晶材料的提纯方法，其特征在于，所述吸附剂的孔径为1～10nm，吸附剂的比表面积为500～1000m2/g。
4.根据权利要求1所述的端基为氟代烷氧基的液晶材料的提纯方法，其特征在于，所述的吸附剂与液晶材料的质量比1:5～1:20。
5.根据权利要求1所述的端基为氟代烷氧基的液晶材料的提纯方法，其特征在于，所述液晶材料在外加电场下的吸附时间为1～1.5h。
6.根据权利要求2所述的端基为氟代烷氧基的液晶材料的提纯方法，其特征在于，所述提纯器选自单一离子膜提纯器、双槽离子膜提纯器、三槽离子膜提纯器中的一种。
7.根据权利要求2所述的端基为氟代烷氧基的液晶材料的提纯方法，其特征在于，所述提纯器的离子膜为均相阴、阳离子交换膜，电极为网式贵金属氧化物涂层电极。
8.根据权利要求1或2所述的端基为氟代烷氧基的液晶材料的提纯方法，其特征在于，所述电场强度为1kV/cm～10kV/cm，电极间距为20～50mm。
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| PCT/CN2018/108921 WO2020056795A1 (zh) | 2018-09-20 | 2018-09-30 | 一种端基为氟代烷氧基的液晶材料的提纯方法 |
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| CN112251239A (zh) * | 2020-09-02 | 2021-01-22 | 阜阳欣奕华材料科技有限公司 | 液晶材料的纯化方法 |
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| CN101173172A (zh) * | 2006-10-30 | 2008-05-07 | 比亚迪股份有限公司 | 一种液晶的提纯方法 |
| CN101210183A (zh) * | 2006-12-27 | 2008-07-02 | 比亚迪股份有限公司 | 一种提纯液晶材料的方法 |
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| CN101760204A (zh) * | 2009-12-08 | 2010-06-30 | 武汉工业学院 | 一种电场吸附提纯液晶的方法 |
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| DE10125708A1 (de) * | 2000-06-21 | 2002-03-28 | Merck Kgaa | Hochohmige nematische flüssigkristalline Mischungen und Reinigngsverfahren dafür |
| JP2003064364A (ja) * | 2001-08-29 | 2003-03-05 | Dainippon Ink & Chem Inc | 液晶材料精製装置及び液晶材料精製方法 |
| JP2003166091A (ja) * | 2001-11-28 | 2003-06-13 | Dainippon Ink & Chem Inc | 液晶材料精製装置及び液晶材料精製方法 |
| JP2003335711A (ja) * | 2002-03-11 | 2003-11-28 | Dainippon Ink & Chem Inc | 液晶化合物の精製方法 |
| DE102013020400A1 (de) * | 2013-12-10 | 2015-06-11 | Merck Patent Gmbh | Reinigungsvorrichtung |
| DE102013021279A1 (de) * | 2013-12-18 | 2015-06-18 | Merck Patent Gmbh | Verfahren zum Reinigen einer Flüssigkristallmischung |
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| CN101173172A (zh) * | 2006-10-30 | 2008-05-07 | 比亚迪股份有限公司 | 一种液晶的提纯方法 |
| CN101210183A (zh) * | 2006-12-27 | 2008-07-02 | 比亚迪股份有限公司 | 一种提纯液晶材料的方法 |
| CN101760203A (zh) * | 2009-12-08 | 2010-06-30 | 武汉工业学院 | 一种提纯液晶材料的方法 |
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| CN112251239A (zh) * | 2020-09-02 | 2021-01-22 | 阜阳欣奕华材料科技有限公司 | 液晶材料的纯化方法 |
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