1282359 玖、發明說明： 【發明所屬之技術領域】 本發明係關於一種液晶純化方法與裝置，尤指一種適 用於提升液晶阻值之液晶純化方法與裝置。 5 【先前技術】 液晶顯示器（Liquid Crystal Device，LCD)具有輕薄、省 電、低輻射等既有的優異特性，更具備取代傳統陰極射線 貧螢幕的怨勢’而存在廣大的商業潛力。以目前液晶生產 10 製造技術而言，STN(Super Twisted Nematic)-LCD 所要求 的液晶必需具備阻值（Specific Resistance，SR)大於ίο11 Ω .cm以上；TFT-LCD所要求的液晶則必需具備阻值大於 1〇13Ωχχη。 以目前液晶面板廠製作技術而言，生產線上只有7〇% 15的液晶順利被使用後製成產品。而只要在生產或灌面板的 過程中受到離子或水份汙染，往往會使得整批液晶皆不可 使用，一般約有30%〜50%之多必須報廢。然而，由於液晶 屬於高單價特用化學品，若因此將其當成廢棄物處理，將 造成面板廠商營業成本增加及獲利之損失。液晶材料在整 20個平板顯示器的成本中雖然佔非常小的一部份，但對顯示 裔的性能卻有決定性的影響。建立液晶純化回收相關技術 將可有效地降低生產成本，對整個產業界而言將會一項重 大的突破。 由於液晶為黏稠狀，因此相關液晶回收之先前技術多 1282359 先利用一有機溶劑將液晶完全溶解後，再利用直接接觸之 吸附法，吸附液晶溶液内不純物，或以再結晶、吸附、蒸 餾、離子交換法、過濾或是通過一填充有吸附劑之管柱， 取得純化後之液晶，再接著將液晶溶液内含之有機溶劑移 5除；上述之習知技藝中，溶劑添加並攪拌之純化方法需費 時3至5小時，而所利用以純化之液晶量僅限於i〇g以下， 並不適合於工廠之量產製作用；此外，大量使用的有機溶 劑及吸附劑，不僅增加繁雜步驟，且易於純化過程中導入 污染，而降低純化效果；同時，在溶劑移除的過程中，改 10變其原本液晶混合物之組成及光電性質的機率將隨之增 加，因而造成純化後液晶規格不符合需求。 因此’亟需發展-純化液晶之方法，以有效縮短純化 時間，並可克服純化製程中高潔淨度之要求，方便於使用 及操作，更重要的是能適合於工廠之量產製作。發明人爱 υ因於此，本於積極創作之精神，亟思一種可以解決上述問 題Γ液晶純化之方法與褒置」，幾經研究實驗終至完成此 項恭惠世人之發明。 【發明内容】 本發明係提供-液晶純化方法及其裝置 度低變異之液晶，主要係利田备换行巧间、、、电 體之過濾方式來純化液晶，刹田士々 Γ ^ …垂…" 曰曰爿用本發明可使純化後液晶之 ,.# ^^ 门時也不會改變其原本液晶之組 成及先電性質，而可於純化後直接使用。 20 1282359 *盥^，明係包含有下列步驟：（a)提供一液晶、一無機鹽 類^包含一渡材之一密閉容器；⑻混合液晶與無機鹽類成 此二物’（c)將混合物移入含濾材之密閉容器中；（幻提供 s加壓惰性氣體以過濾混合物；以及（e)取得-過濾、後之液 5曰曰，其中，無機鹽類所具備之結構孔徑直徑在15nm以下； 濾材孔彳二為OU.hm ;加壓惰性氣體之壓力範圍係 1.2-15kg/cm2 ;且惰性氣體之含水率為以下。 ^發明亦含一種液晶純化裝置，包括有：一惰性氣體 供應單元，提供一壓力範圍在1.2-15kg/cm2之加壓惰性氣 ίο體，除水單元，係用以使該惰性氣體之含水率在50ppm 乂下，以及有一過濾單元，一惰性氣體入口，一物料進 口與一產物出口之密閉槽體，係用以過濾含一液晶與一無 機鹽類之-混合物；其中，該除水單元係連接並介於該惰 性乳體供應單元以及該槽體之間；該密閉槽體内之過遽單 15 元孔徑為 0·1-〇.5μιη。 本發明叙置中，用以過濾混合物之槽體的產物出口係 連接-收集單元，以收集已過滤完成之純化液晶。 由於目前使用大量的液晶於STN之製作，因此經純化 過之液晶必須至少達到阻值在1〇uQcm以上，以符合使用 20規格；於本發明中所使用到之濾材孔徑不限，但由於要過 濾掉的是液晶中的不純物，因此孔徑範圍較佳係在 0·1_0·5μιη 之間，最佳是 本發明中所使用之無機鹽類主要作用在吸附液晶中不 純物’因此種類不限’較佳係氧化銘、彿石、氧化石夕凝膠、 1282359 氧化鈦及其類似物；最佳是氧化鋁；而氧化鋁規格如下： 純度需大於99%以上，最佳為99.3% ;表面積大於88mVg， 最佳為大於89.3m2/g ;孔洞直徑小於9nm，最佳為小於 8.09nm ;孔洞容積小於〇.4mL/g，最佳為小於〇38imL/g ,· 5灰化損失量小於〇·1%，最佳為0.08%;且表觀容積為1〇_15 mL /10g，最佳為 13 mL/lOg。 使用於本發明中之惰性氣體之壓力範圍不限，較佳係 1.2kg/cm2至7kg/cm2之間；且所使用惰性氣體其含水率不 限，較佳為50PPm以下，更佳為3〇ppm以下；適用於本發明 10之惰性氣體種類不限，較佳係氬氣、氮氣或氦氣；且所使 用之惰性氣體純度較佳係大於9 9.9 9 %。 【實施方式】 本發明係提供一種高阻值及低成&變異之丨夜晶純化 15方法及其裝置，主要係針對液晶顯示器或其他使用領域所 需求的高阻值液晶化學品，以高純度無機鹽類吸附法配合 氣壓式過濾'法進行液晶純化，以達到所要求高阻值。依據 本發明高阻值液晶之純化裝置，其中包含維持純化過程除 水之裝置及低 >万染之潔淨槽體，可使大量之液晶在短時間 20内完成純化，且可減少在純化過程微污染之導入。此外， 槽體可拆卸以利於清洗，符合高潔淨度之要求。 於本實施例中所用以進行光電性質量測之儀器，以及 各光電性質之容許誤差請參考下表： 1282359 光電性質 儀器廠牌及型號 容許誤差 相轉移溫度 Tc (°〇 TA-DSC Q10 土 2 驅動電壓Vth (V) APTIII LCAS-1 ±0·09 螺距Pitch (μηι) POM Olympus BX 50 士 0·3 雙折射率An ABBA Refractomer ATAGO DR-M2 ±0.04 介電異方性Δε APTIII LCAS-1 ±1 黏度η (20 〇C，cps) CAP1000L ±1 比電阻值SR (Q.cm) KEITHLEY 6517A ±1 實施例一 本實施例中，純化液晶之過程是將液晶與吸附劑充分 混和接觸，利用吸附劑將液晶中不純物吸附住，再利用0.2 5 // m PTFE濾膜精密過濾，以達到純化後液晶與吸附劑分 離的效果。 請參考圖1之本發明液晶純化裝置圖，包括有一氬氣 鋼瓶10,可提供一壓力範圍在1.2-15kg/cm2之加壓氬氣（純 度大於99.99%); —除水單元20，内部包括有一除水之結 10 構21，此結構係用以使完成除水後之氬氣含水率控制在 30ppm以下，且含氧率在lOppm以下，以避免純化過程中 之水氧率過高；以及一有一 0.2//mPTFE濾膜41，一氩氣 入口 42，一混合物進口 43與一產物出口 44之密閉槽體 40，係用以過濾來自混合槽30之混合物。 15 其中，該除水單元20係介於氬氣鋼瓶10以及密閉槽 10 1282359 體40之間’並分別有連通管12, 24連接；連通管24與密 閉槽體40上之氬氣入口 42相接，以藉此提供一完成除水 後之氬氣進入密閉槽體40内；連通管34接合密閉槽體40 上之混合物進口 43以及混合槽3〇，以使完成混合之液晶 5與吸附劑之混合物沿著連通管34進入到密閉槽體40内； 連通管45則連接著密閉槽體4〇上之產物出口 44以及產物 收集槽5 0，以收集完成純化之液晶；本實施例中純化裝置 之各俩槽體可拆卸再組裝，以利於清洗，符合高潔淨度之 要求。 10 首先，將液晶純化裝置組合完成；將已於除水單元20 中處理過之乾燥氬氣，沿著連通管24通入密閉槽體4〇内 備用，將一欲進行過濾之液晶，與相當於液晶之丨〇wt%的 尚純度（含有99.3%以上之氧化鋁）氧化鋁混合於混合槽 中，攪拌20分鐘使均勻混合；再接著將含吸附劑之液晶混 15合物沿著連通管34進入到密閉槽體4〇内；之後，將氬氣 氣壓控制在1.2〜7Kg/cm2，使液晶混合物通過〇·2μηι之 pTFE濾膜41 ’以與吸附劑分離，即可於產物收集槽5〇中 取得純化後之液晶。 每經過一次過濾，即以定量吸管吸取純化後液晶進行 20 SR值之量測；重複過濾流程一直到SR值達合格標準後， 即可將純化後液晶收集於儲存瓶中，以方便進行後續的物 性分析。 實施例二 將阻值為3·2 X l〇8Qcm之液晶2〇g，重複進行五次實 11 1282359 液晶量（g) 水分含量 (ppm) 阻值 (Ω .cm) 液晶回收 率(％) 純化前 20 309 3.2E+08 * 純化後 9.85 171 2.25E+11 50 施例一所述之方法，檢測結果後發現，液晶阻值提昇至2.25 X 1〇ηΩ(：ιη左右，液晶水份含量由原先309 ppm降低至171 ppm，而純化後液晶回收率為50%，其結果如表一所示。 表一、液晶純化前後之;^份、阻值&回收率 5 實施例三 將阻值為5·48 X 109Ω cm之液晶58g，重複進行五次實籲 施例一所述之方法，檢測結果後發現，液晶阻值提昇至2.37 X l〇nQcm左右，液晶水份含量由原先414 ppm降低至312 10 ppm，而純化後液晶回收率為60%，其結果如表二所示。 液晶量（g) 水分含量 (ppm) 阻值 (Ω .cm) 液晶回收 率（％) 純化前 58.0 414 5.48E+09 氺 純化後 34.5 312 2.37Ε+Π 60 表二、液晶純化前後之水份、阻值及回收率 實施例四 01 將阻值為1_〇 X 101GDcm之液晶46.2g，重複進行二次 15 實施例一所述之方法，能將液晶阻值提昇至1.1 X 1〇"Ω cm 左右，液晶水份含量由原先342 ppm降低至309 ppm，而純 化後液晶回收率為80%，其結果如表三所示。 表三、液晶純化前後之水份、阻值及回收率 液晶量（g) 水分含量 (ppm) 阻值 (Ω .cm) 液晶回收率 (%) 純化前 46.2 342 1.00E+10 氺 12 1282359 ~純化後 36.96 309 1.10E+11 80 實施例五 將阻值為1·86 X 1〇1()Ω cm之液晶95g，重複進行二次實 施例一所述之方法，能將液晶阻值提昇至丨.05 X l〇12〇cm 5 左右，液晶水份含量由原先181 ppm降低至111 ppm，而純 化後液晶回收率為85%，其結果如表四所示。液晶純化前 後之光電性質，如表五所示。液晶純化前後之光電性質數 值變化皆在量測容許誤差範圍内，表示純化前後之光電性 質無太大之改變。 10 表四、液晶純化前後之水份、阻值及回收率 液晶量（g) 水分含量 (ppm) 阻值 (Ω .cm) 液晶回收 率（％) 純化前 95 181 1 · 8 6E+1〇 * 純化後 84.6 111 1.05E+12 85 表五、液晶純化前後之光電性質 光電性質 純化前 純化後 相轉移溫度 Tc (°〇 97.8 99.0 驅動電壓Vth (V) 2.11 2.11 螺距 Pitch (μηι) 7.55 7.75 雙折射率Δη 0.1388 0.1388 介電異方性Δε 12.2 11.5 黏度 η (20 °C，cps) 22 21 實施例六 15 將阻值為7·8 X 101()Ω cm之液晶95g，進行一次實施例 一所述之方法，能將液晶阻值提昇至6.1 X i〇12Qcm左右， 液晶水份含量由原先127 ppm降低至59 ppm，而純化後液 13 1282359 晶回收率為82%，其結果如表六所示；液晶純化前後之光 電性質如表七所示。液晶純化前後之光電性質數值變化皆 在量測容許誤差範圍内，表示純化前後之光電性質無太大 之改麦。其中除了介電異方性有明顯改變外，但對液晶灌 入面板中之光電性質表現影響不大。 表六、液 曰曰 液晶量（g) 水分含量 (PPm) 阻值 (Ω .cm) 液晶回收率 (%) 純化前 95 127 7.80E+10 氺 純化後 82 59 6 · 10E+12 82 表七、液晶純化前後之光電性質 10 光電性質 純化前 純化後 相轉移溫度 Tc (°〇 106.5 107.3 驅動電壓Vth (V) 2.64 2.64 螺距 Pitch (μηι) 7.6 _ 7.9 雙折射率Δη 0.1383 0.1379 介電異方性Αε 9.1 7.7 黏度 η (20 °C，cps) 21 21 等 實施例七、對照例 利用本對照例來與上述實施例做比較。使用與實施 例六相同組成成份之液晶4g，其阻值為7·55 χ 1〇i〇q cm， 加入lOmL電子級曱苯溶劑與液晶完全溶解後，進行一次 實施例一所述之方法，再利用減壓濃縮法進行2.5小時去 除甲苯溶劑後，發現液晶阻值提昇至51 χ 1〇11〇 cm左右， 液晶水份含量由原先348 ppm降低至224 ppm，而液晶純 14 15 1282359， * * 化如後之光電性質，如表八所示。 如表八數據顯示，液晶純化前後之光電性質皆有明顯 改麦，推測可能原因為溶劑去除過程中，所造成某些液晶 單體的損失而致。 5 綜合以上之結果顯示添加甲苯溶劑進行液晶純化將造 成液晶光電性質改變。 表八 液晶純化前後之光電性質1282359 发明, the invention description: [Technical Field] The present invention relates to a liquid crystal purification method and apparatus, and more particularly to a liquid crystal purification method and apparatus suitable for improving liquid crystal resistance. 5 [Prior Art] Liquid crystal devices (LCDs) have the outstanding characteristics of lightness, power saving, low radiation, etc., and have the commercial potential to replace the traditional cathode ray poor screen. In the current manufacturing technology of liquid crystal production 10, the liquid crystal required by STN (Super Twisted Nematic)-LCD must have a specific resistance (SR) greater than ίο11 Ω.cm or more; the liquid crystal required for TFT-LCD must have resistance. The value is greater than 1〇13Ωχχη. In terms of the current production technology of the LCD panel factory, only 7〇% of the liquid crystal on the production line is successfully used to make the product. As long as it is contaminated by ions or water during the process of producing or filling the panel, it will often make the whole batch of liquid crystals unusable. Generally, about 30%~50% must be scrapped. However, since liquid crystals are high-priced special-purpose chemicals, if they are treated as waste, the panel manufacturers' operating costs will increase and profit will be lost. Liquid crystal materials, while accounting for a very small portion of the cost of the entire 20 flat panel displays, have a decisive influence on the performance of the display. The establishment of liquid crystal purification and recycling related technologies will effectively reduce production costs and will be a major breakthrough for the entire industry. Since the liquid crystal is viscous, the prior art related to liquid crystal recovery is 1282359. After completely dissolving the liquid crystal by an organic solvent, the direct contact adsorption method is used to adsorb impurities in the liquid crystal solution, or to recrystallize, adsorb, distill, and ion. The exchange method, the filtration or the column of the adsorbent is used to obtain the purified liquid crystal, and then the organic solvent contained in the liquid crystal solution is removed by 5; in the above-mentioned prior art, the solvent is added and stirred. It takes 3 to 5 hours, and the amount of liquid crystal used for purification is limited to less than i〇g, which is not suitable for mass production in the factory; in addition, the organic solvent and adsorbent used in large quantities not only add complicated steps, but also are easy to use. Contamination is introduced during the purification process, and the purification effect is lowered. At the same time, in the process of solvent removal, the probability of changing the composition and photoelectric properties of the original liquid crystal mixture will increase, thereby causing the liquid crystal specification after purification to not meet the demand. Therefore, there is a need to develop a method for purifying liquid crystals to effectively shorten the purification time, overcome the high cleanliness requirements in the purification process, facilitate use and operation, and more importantly, be suitable for mass production in factories. The inventor loves this because of this, in the spirit of active creation, thinking about a method and device that can solve the above problems, liquid crystal purification, and after several research experiments to complete the invention of this kind of Christine. SUMMARY OF THE INVENTION The present invention provides a liquid crystal purification method and a liquid crystal with low variation of the device, which is mainly used for purifying liquid crystals by Litian prepared exchange, and electric energy filtering method, and is used to clean liquid crystals. The invention can be used to make the liquid crystal after purification, and the composition of the original liquid crystal and the electro-electric properties are not changed, and can be directly used after purification. 20 1282359 *盥^, Ming system contains the following steps: (a) providing a liquid crystal, an inorganic salt containing a closed container of a ferry; (8) mixing liquid crystal with inorganic salts into two (') The mixture is transferred into a closed container containing the filter material; (the phantom is supplied with a pressurized inert gas to filter the mixture; and (e) is obtained - filtered, and the liquid is 5 曰曰, wherein the inorganic salt has a pore diameter of 15 nm or less The filter material pores are OU.hm; the pressure of the pressurized inert gas is 1.2-15kg/cm2; and the moisture content of the inert gas is below. ^The invention also includes a liquid crystal purification device including: an inert gas supply unit Providing a pressurized inert gas having a pressure range of 1.2-15 kg/cm2, the water removing unit is used to make the inert gas have a water content of 50 ppm, and a filtering unit, an inert gas inlet, and a material a sealed tank for importing a product outlet for filtering a mixture comprising a liquid crystal and an inorganic salt; wherein the water removal unit is connected between the inert milk supply unit and the tank; The closed groove In the present invention, the product outlet for filtering the mixture of the mixture is a connection-collecting unit for collecting the purified liquid crystal which has been filtered. A large amount of liquid crystal is used in the production of STN. Therefore, the purified liquid crystal must have a resistance value of at least 1 〇uQcm or more in order to comply with the use of 20 specifications; the filter material used in the present invention has an aperture diameter not limited, but is filtered out. It is an impurity in the liquid crystal, so the pore diameter range is preferably between 0·1_0·5μιη, and it is preferable that the inorganic salt used in the present invention mainly acts on adsorbing impurities in the liquid crystal. Oxidation Ming, Fossil, Oxidized Stone Gel, 1282359 Titanium Oxide and its analogues; the best is alumina; and the alumina specifications are as follows: Purity needs to be greater than 99%, preferably 99.3%; surface area greater than 88mVg, most Preferably, the diameter is greater than 89.3 m 2 /g; the pore diameter is less than 9 nm, and the optimum is less than 8.09 nm; the pore volume is less than 〇.4 mL/g, and the optimum is less than 〇38 μL/g, and the ashing loss is less than 〇·1%. Best is 0.08%; and apparent The volume is 1〇_15 mL /10g, preferably 13 mL/lOg. The pressure range of the inert gas used in the present invention is not limited, preferably between 1.2 kg/cm 2 and 7 kg/cm 2 ; The gas has an unlimited water content, preferably 50 ppm or less, more preferably 3 ppm or less; the inert gas of the present invention 10 is not limited, preferably argon, nitrogen or helium; and the inert gas used Preferably, the purity is greater than 99.99%. [Embodiment] The present invention provides a high resistance value and low-increase & variability 丨 night crystal purification 15 method and device thereof, mainly for liquid crystal display or other fields of use. The high-resistance liquid crystal chemical is purified by a high-purity inorganic salt adsorption method in combination with a pneumatic filtration method to achieve a desired high resistance value. According to the present invention, a high-resistance liquid crystal purification apparatus comprising a device for maintaining water removal in a purification process and a low-temperature cleaning tank can complete a large amount of liquid crystal purification in a short time of 20, and can be reduced in the purification process. Introduction of micro-contamination. In addition, the tank is detachable for cleaning and meets high cleanliness requirements. For the instrument used for photoelectric quality measurement in this embodiment, and the allowable error of each photoelectric property, please refer to the following table: 1282359 Optoelectronic property instrument manufacturer and model tolerance phase transition temperature Tc (°〇TA-DSC Q10 soil 2 Driving voltage Vth (V) APTIII LCAS-1 ±0·09 Pitch Pitch (μηι) POM Olympus BX 50 ±0·3 Birefringence An ABBA Refractomer ATAGO DR-M2 ±0.04 Dielectric anisotropy Δε APTIII LCAS-1 ± 1 viscosity η (20 〇C, cps) CAP1000L ±1 specific resistance value SR (Q.cm) KEITHLEY 6517A ±1 Example 1 In this embodiment, the process of purifying the liquid crystal is to thoroughly mix the liquid crystal with the adsorbent and utilize adsorption. The agent adsorbs the impurities in the liquid crystal and then precisely filters with a 0.2 5 // m PTFE filter to achieve the separation effect of the liquid crystal and the adsorbent after purification. Please refer to FIG. 1 for the liquid crystal purification device of the present invention, including an argon gas cylinder. 10, a pressure argon gas having a pressure range of 1.2-15 kg/cm2 (purity greater than 99.99%) can be provided; - the water removal unit 20 includes a water removal structure 10, which is used to complete the removal Argon gas after water Controlled below 30ppm, and oxygen content below 10ppm to avoid excessive water oxygen rate during purification; and a 0.2 / / m PTFE filter 41, an argon inlet 42, a mixture inlet 43 and a product outlet a closed tank 40 for filtering the mixture from the mixing tank 30. 15 wherein the water removal unit 20 is interposed between the argon cylinder 10 and the closed tank 10 1282359 body 40 and has a communication tube 12, respectively. 24; the connecting tube 24 is connected to the argon inlet 42 on the closed tank 40 to thereby provide an argon gas after the completion of the water removal into the sealed tank 40; the communicating tube 34 joins the mixture on the closed tank 40 The inlet 43 and the mixing tank 3 are arranged such that the mixture of the liquid crystal 5 and the adsorbent which have been mixed is introduced into the sealed tank 40 along the communication tube 34; the connecting tube 45 is connected to the product outlet 44 of the closed tank 4 and The product collection tank 50 is configured to collect the purified liquid crystal; in this embodiment, the two tanks of the purification device are detachable and reassembled to facilitate cleaning, and meet the requirements of high cleanliness. 10 First, the liquid crystal purification device is assembled; Will already be The dried argon gas treated in the water unit 20 is introduced into the closed tank body 4 along the communication pipe 24 for use, and the liquid crystal to be filtered is equivalent to the liquid crystal equivalent weight % (containing 99.3%). The above alumina) alumina is mixed in the mixing tank, stirred for 20 minutes to uniformly mix; and then the liquid crystal mixed 15 containing the adsorbent is introduced into the closed tank 4〇 along the communication tube 34; after that, the argon is used. The gas pressure is controlled at 1.2 to 7 Kg/cm2, and the liquid crystal mixture is passed through a pTFE filter 41' of 〇·2μηι to separate from the adsorbent, so that the purified liquid crystal can be obtained in the product collection tank 5〇. After each filtration, the purified liquid crystal is taken up by a quantitative pipette to measure the 20 SR value; the filtration process is repeated until the SR value reaches the qualified standard, and the purified liquid crystal can be collected in the storage bottle to facilitate subsequent follow-up. Physical analysis. In the second embodiment, the liquid crystal 2〇g with a resistance value of 3·2 X l〇8Qcm is repeated five times. 11 1282359 Liquid crystal amount (g) Moisture content (ppm) Resistance (Ω.cm) Liquid crystal recovery rate (%) 20 309 before purification 3.2E+08 * After purification 9.85 171 2.25E+11 50 The method described in Example 1, after the test results, found that the liquid crystal resistance increased to 2.25 X 1〇ηΩ (: ιη, liquid crystal moisture content From the original 309 ppm to 171 ppm, and the liquid crystal recovery rate after purification is 50%, the results are shown in Table 1. Table 1, before and after liquid crystal purification; ^ part, resistance & recovery rate 5 Example 3 will block The value of the liquid crystal is 58 g of 5·48 X 109 Ω cm, and the method described in the first embodiment is repeated five times. The detection result shows that the liquid crystal resistance is raised to about 2.37 X l〇nQcm, and the liquid crystal moisture content is from the original 414. The ppm was reduced to 312 10 ppm, and the liquid crystal recovery after purification was 60%. The results are shown in Table 2. Liquid crystal amount (g) Moisture content (ppm) Resistance (Ω.cm) Liquid crystal recovery (%) Before purification 58.0 414 5.48E+09 氺 After purification 34.5 312 2.37Ε+Π 60 Table 2, water, resistance and recovery before and after liquid crystal purification Example 4 01 The liquid crystal with a resistance value of 1_〇X 101GDcm is 46.2g, and the method of the first embodiment is repeated. The liquid crystal resistance can be raised to 1.1 X 1 〇 " Ω cm or so, liquid crystal water The content of the original part was reduced from 342 ppm to 309 ppm, and the liquid crystal recovery rate after purification was 80%. The results are shown in Table 3. Table 3. Moisture, resistance and recovery before and after liquid crystal purification Liquid crystal amount (g) Moisture Content (ppm) Resistance (Ω.cm) Liquid crystal recovery (%) Before purification 46.2 342 1.00E+10 氺12 1282359 ~ After purification 36.96 309 1.10E+11 80 Example 5 The resistance is 1·86 X 1 〇1 () Ω cm of liquid crystal 95g, repeat the method described in the second embodiment, the liquid crystal resistance can be raised to about 05.05 X l〇12〇cm 5 , the liquid crystal moisture content is reduced from the original 181 ppm To 111 ppm, and the recovery of liquid crystal after purification is 85%, the results are shown in Table 4. The photoelectric properties of liquid crystal before and after purification are shown in Table 5. The numerical values of photoelectric properties before and after liquid crystal purification are within the tolerance range of measurement. Inside, it indicates that the photoelectric properties before and after purification are not changed much. 10 Table 4, before and after liquid crystal purification Moisture, resistance and recovery Liquid crystal amount (g) Moisture content (ppm) Resistance (Ω.cm) Liquid crystal recovery (%) Before purification 95 181 1 · 8 6E+1〇* After purification 84.6 111 1.05E +12 85 Table 5. Photoelectric properties before and after liquid crystal purification Photoelectric properties Phase transfer temperature after purification Tc (°〇97.8 99.0 Drive voltage Vth (V) 2.11 2.11 Pitch Pitch (μηι) 7.55 7.75 Birefringence Δη 0.1388 0.1388 Dielectric Anisotropy Δε 12.2 11.5 Viscosity η (20 °C, cps) 22 21 Example 6 15 A liquid crystal of 95 g with a resistance of 7·8 X 101 () Ω cm is subjected to the method described in the first embodiment. The liquid crystal resistance increased to about 6.1 X i〇12Qcm, the liquid crystal moisture content decreased from 127 ppm to 59 ppm, and the purified liquid 13 1282359 crystal recovery rate was 82%. The results are shown in Table 6; The photoelectric properties are shown in Table 7. The change in the photoelectric properties of the liquid crystal before and after purification is within the measurement tolerance, indicating that the photoelectric properties before and after purification are not much changed. In addition to the significant change in dielectric anisotropy, it has little effect on the photoelectric properties of liquid crystal infusion panels. Table 6. Liquid helium liquid crystal (g) Moisture content (PPm) Resistance (Ω.cm) Liquid crystal recovery (%) 95 127 before purification 7.80E+10 氺 After purification 82 59 6 · 10E+12 82 Table VII Photoelectric properties before and after liquid crystal purification 10 Photoelectric properties Purified phase transfer temperature Tc (°〇106.5 107.3 Driving voltage Vth (V) 2.64 2.64 Pitch Pitch (μηι) 7.6 _ 7.9 Birefringence Δη 0.1383 0.1379 Dielectric anisotropy Α ε 9.1 7.7 Viscosity η (20 ° C, cps) 21 21 and the like. Example 7 Comparative Example This comparative example was used to compare with the above examples. The liquid crystal 4g having the same composition as that of Example 6 was used, and its resistance was 7 · 55 χ 1〇i〇q cm, after adding lOmL of electronic grade benzene solvent and liquid crystal completely dissolved, the method described in the first embodiment was carried out, and then the solvent was removed by a vacuum concentration method for 2.5 hours to remove the toluene solvent. The value is raised to about 51 χ 1〇11〇cm, the liquid crystal moisture content is reduced from 348 ppm to 224 ppm, and the liquid crystal purity is 14 15 1282359, * * as shown in the following photoelectric properties, as shown in Table 8. The data shows that the light before and after purification of the liquid crystal The electrical properties are obviously changed. It is speculated that the possible cause is the loss of some liquid crystal monomers caused by the solvent removal process. 5 The above results show that the addition of toluene solvent for liquid crystal purification will cause changes in the liquid crystal photoelectric properties. Photoelectric properties before and after liquid crystal purification
» 10 上述實施例僅係為了方便說明而舉例Μ，|發_ 張之杻利範圍自應以申請專利 於上述實施例。 *非僅限 【圖式簡單說明】 15圖1係本發明純化裝置系統架構圖。 連通管 除水結構24連通管 【主要元件符號說明】 10 氬氣鋼瓶 12 20 除水單元 21 15 1282359The above-mentioned embodiments are merely exemplified for convenience of explanation, and the scope of the application is patented in the above embodiments. *Not limited to [Simplified description of the drawings] 15 Fig. 1 is a system architecture diagram of the purification apparatus of the present invention. Connecting pipe Water removal structure 24 connecting pipe [Main component symbol description] 10 Argon gas cylinder 12 20 Water removal unit 21 15 1282359
3 0 混合槽 34 連通管 40 密閉槽體 41 濾膜 42 氬氣入口 43 混合物進口 44 產物出口 45 連通管 50 產物收集槽 163 0 Mixing tank 34 Connecting tube 40 Sealing tank 41 Filter membrane 42 Argon inlet 43 Mixture inlet 44 Product outlet 45 Connecting tube 50 Product collection tank 16