CN101381604B - 液晶单体或液晶组合物的纯化方法 - Google Patents
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Abstract
本发明涉及液晶单体或液晶组合物的纯化方法，以大孔聚酰亚胺聚合物作为吸附材料，将液晶单体或液晶组合物在15～50℃下溶解在有机溶剂中，以一定的流速穿过填有大孔吸附聚酰亚胺聚合物的柱子，吸附完成后，过滤除去吸附剂及其他固体的小颗粒，随后减压蒸馏除溶剂。本发明方法使液晶中含有的极性杂质吸附到聚合物的表面，从而降低液晶极性杂质和离子的含量，提高液晶组合物的阻抗值，从而改善液晶的电荷保持率(VHR)，达到改善液晶显示器的显示效果。
Description
技术领域
本发明涉及一种液晶单体或液晶组合物的纯化方法，特别是利用大孔强极性吸附聚合物纯化液晶单体或液晶组合物的方法。
背景技术
目前较流行的薄膜晶体管(thin film transistor，TFT)阵列驱动液晶显示器(TFT LCD)用液晶材料、超扭曲向列相(STN)显示用液晶材料，必须要求液晶材料对热、化学、电、光稳定性好，电荷保持率(VHR)高。液晶材料中离子型杂质的存在会导致显示的“串扰”、影像残留、字体模糊、对比度下降等现象，在温度较高时，离子型杂质的存在，会使液晶材料更易发生热分解，从而影响液晶材料的正常显示。这就要求通过有效的方法来降低液晶材料的离子含量和强极性的有机杂质的含量。这就意味着液晶材料必须具有较高的化学纯度以较高的电阻率。
目前用于提纯液晶的方法是使用硅胶、氧化铝、离子交换树脂、螯合物树脂、分子筛、活性炭等等，通过把他们一起混合而达到吸附离子型杂质的目的。还有通过高纯水洗涤而出去离子的方法。使用最为广泛的是硅胶、氧化铝作为吸附剂，氧化铝、硅胶极性很强，能够有效吸附离子和极性杂质，但是，这种吸附剂有比较明显的缺点：针对性不强(PI吸附)；如果是混合液晶，会破坏液晶组分，改变手性剂含量，劣化显示器显示效果。
此外，已有的提纯方法不能满足薄膜晶体管(thin film transistor，TFT)阵列驱动液晶显示器(TFT LCD)用液晶材料、超扭曲向列相(STN)显示用液晶材料所要求的更高电阻率。
发明内容
本发明目的是提供一种能够将液晶单体或液晶组合物的电阻率提高到更高数量级的液晶单体或液晶组合物的纯化方法。
本发明的大孔吸附聚酰亚胺聚合物，是一种人工合成的孔性高分子聚合物吸附剂，通过以下路线制得：
稳定剂的制备：
聚酰亚胺树脂的合成：
a)其中R1选自：
或
b)其中R2选自：
大孔聚酰亚胺聚合物吸附剂，苯类、醇类、脂肪烃等均可作为致孔。应用以上方法合成的大孔聚酰亚胺聚合物吸附剂具有如下优点：
●具有良好的吸附离子、极性杂质的能力
●物理化学稳定性好，易再生
●品种种类较多样，可根据不同类型的杂质进行针对性选择不同基团的大孔聚酰亚胺吸附材料。
本发明中，在对大孔吸附聚酰亚胺聚合物的研究过程中，发现具有以下特性：
●吸附剂结构的影响：吸附剂结构包括比表面、孔径和表面基团，对吸附效果的影响非常大。不同的孔径、表面基团会选择性的对一些杂质有更好的吸附作用，在大孔吸附聚酰亚胺聚合物中，可能发生单层、多层吸附和毛细凝结。
●采用吸附聚合物吸附，其孔直径与吸附质分子直径之比以6：1较为适宜，这样更有利于吸附的发生，提高吸附效率。吸附量的的大小由比表面大小决定。
●极性吸附聚合物可以提高对极性有机物杂质、芳香化合物杂质的吸附能力
●吸附质结构的影响，直接表现在吸附质分子量大小、分子的极性和取代基的性质等方面，反应在吸附质与介质的相互作用中。
本发明改善液晶单体或液晶组合物的电阻率的方法如下：
以大孔聚酰亚胺聚合物作为吸附材料，将液晶单体或液晶组合物在15～50℃下溶解在有机溶剂中，以一定的流速穿过填有大孔吸附聚酰亚胺聚合物的柱子，吸附完成后，用过滤膜滤除吸附剂及其他固体的小颗粒，随后减压蒸馏除溶剂。
所说溶剂为芳香族碳氢化合物，优选为甲苯、苯、石油醚、正己烷、二氯甲烷或乙酸乙酯。为了能搞达到提纯的目的，所使用的溶剂必须是高纯的产品。
所说溶剂量为液晶重量的1～35倍，优选3～20倍。
所说滤膜微孔直径为0.1～1微米，优选0.1～0.3微米。
蒸馏温度一般控制60度以下较高，通过调节真空度实现对温度的控制。
具体实施方式
实施例1
10g液晶组合物(hsg24200-100)，溶解在50ml超纯甲苯中，所得溶液通过2g大孔吸附聚酰亚胺聚合物(孔径80～120埃；直径70～230目；类型为实施例1中表述)填充的柱子中，液晶组合物溶液通过柱子进行吸附操作，控制流速2克/秒。吸附完成后，进行精密过滤，滤膜为聚四氟乙烯，孔径为0.2微米。过滤完成后，蒸去甲苯，控制温度小于55度。完成后测试电阻率：5×1012；阈值电压：1.35V(标准1.34±0.02V)
对比例1
10g液晶组合物(hsg24200-100)，溶解在50ml超纯甲苯中，所得溶液通过2g活性氧化铝(孔径90埃；直径70～230目；中性)填充的柱子中，液晶组合物溶液通过柱子进行吸附操作，控制流速2克/秒。吸附完成后，进行精密过滤，滤膜为聚四氟乙烯，孔径为0.2微米。过滤完成后，蒸去甲苯，控制温度小于55度。完成后测试电阻率：4×1012；阈值电压：1.39V(标准1.34±0.02V)
从测试结果可见，实施例1经本方法纯化后的液晶组合物与对比例1经传统方法纯化后的液晶组合物相比较，前者的电阻率提高而阈值电压降低。
Claims (6)
1.液晶单体或液晶组合物的纯化方法，其特征是以大孔聚酰亚胺聚合物作为吸附材料，将液晶单体或液晶组合物在15～50℃下溶解在有机溶剂甲苯中，以2克/秒的流速穿过填有大孔聚酰亚胺聚合物的柱子，吸附完成后，通过滤膜过滤除去吸附剂及其他固体的小颗粒，随后减压蒸馏除溶剂；所述的大孔聚酰亚胺聚合物孔径80～120埃；是如下结构单体的聚合物：
其中R1选自：
其中R2选自：
2.根据权利要求1所述的液晶单体或液晶组合物的纯化方法，其特征是所述溶剂为液晶重量的1～35倍。
3.根据权利要求2所述的液晶单体或液晶组合物的纯化方法，其特征是所述溶剂为液晶重量的3～20倍。
4.根据权利要求1所述的液晶单体或液晶组合物的纯化方法，其特征是所述滤膜微孔直径为0.1～1微米。
5.根据权利要求4所述的液晶单体或液晶组合物的纯化方法，其特征是所述滤膜微孔直径为0.1～0.3微米。
6.根据权利要求1或2或3或4或5所述的液晶单体或液晶组合物的纯化方法，其特征是蒸馏温度控制60℃以下。
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| DE102013021279A1 (de) * | 2013-12-18 | 2015-06-18 | Merck Patent Gmbh | Verfahren zum Reinigen einer Flüssigkristallmischung |
| CN106110707A (zh) * | 2016-06-17 | 2016-11-16 | 阜阳欣奕华材料科技有限公司 | 一种液晶单体或者液晶组合物的纯化方法 |
| CN109852399A (zh) * | 2018-12-29 | 2019-06-07 | 阜阳欣奕华材料科技有限公司 | 一种生产混合液晶的方法 |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5422034A (en) * | 1992-12-16 | 1995-06-06 | Hitachi Chemical Company, Ltd. | Purification of liquid crystals and liquid crystal composition |
| US6056892A (en) * | 1997-03-06 | 2000-05-02 | Mitsubishi Gas Chemical Company, Inc. | Method for purifying liquid crystal |
| JP2004004012A (ja) * | 2002-04-16 | 2004-01-08 | Okamura Seiyu Kk | 構造異性体の分離方法 |
| CN1497036A (zh) * | 2002-09-26 | 2004-05-19 | 大日本油墨化学工业株式会社 | 用于再利用液晶材料的处理方法 |
| CN1775908A (zh) * | 2005-11-25 | 2006-05-24 | 清华大学 | 一种提纯液晶的方法 |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5422034A (en) * | 1992-12-16 | 1995-06-06 | Hitachi Chemical Company, Ltd. | Purification of liquid crystals and liquid crystal composition |
| US5540857A (en) * | 1992-12-16 | 1996-07-30 | Hitachi Chemical Co., Ltd. | Purification of liquid crystals and liquid crystal composition |
| US6056892A (en) * | 1997-03-06 | 2000-05-02 | Mitsubishi Gas Chemical Company, Inc. | Method for purifying liquid crystal |
| JP2004004012A (ja) * | 2002-04-16 | 2004-01-08 | Okamura Seiyu Kk | 構造異性体の分離方法 |
| CN1497036A (zh) * | 2002-09-26 | 2004-05-19 | 大日本油墨化学工业株式会社 | 用于再利用液晶材料的处理方法 |
| CN1775908A (zh) * | 2005-11-25 | 2006-05-24 | 清华大学 | 一种提纯液晶的方法 |
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Address after: 212212 east side of Yangzhong, Jiangsu, Yangtze River Bridge Patentee after: JIANGSU HECHENG DISPLAY TECHNOLOGY Co.,Ltd. Address before: 212212, Jiangsu, Yangtze River bridge, Yangzhong Province East Jiangsu Cheng chemical materials Co., Ltd. Patentee before: JIANGSU HECHENG DISPLAY TECHNOLOGY Co.,Ltd. |
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Effective date of registration: 20160325 Address after: No. 8 Fuyang 236000 Anhui province Fuyang City Yingzhou District Hefei modern industrial park of Hefei Avenue Patentee after: FUYANG SINEVA MATERIAL TECHNOLOGY Co.,Ltd. Address before: 210000 Nanjing Chemical Industrial Park, Nanjing Province, new materials Industrial Park, East Park Road, room No. 112, room 1, No. Patentee before: JIANGSU HECHENG ADVANCED MATERIALS Co.,Ltd. |
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Address after: Fuyang 236000 Anhui province Fuyang City Yingzhou District Hefei modern industrial park of Tianzhu Road No. 1 Patentee after: FUYANG SINEVA MATERIAL TECHNOLOGY Co.,Ltd. Address before: No. 8 Fuyang 236000 Anhui province Fuyang City Yingzhou District Hefei modern industrial park of Hefei Avenue Patentee before: FUYANG SINEVA MATERIAL TECHNOLOGY Co.,Ltd. |
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