JP5527311B2 - 液晶組成物の製造方法 - Google Patents
液晶組成物の製造方法 Download PDFInfo
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- JP5527311B2 JP5527311B2 JP2011253872A JP2011253872A JP5527311B2 JP 5527311 B2 JP5527311 B2 JP 5527311B2 JP 2011253872 A JP2011253872 A JP 2011253872A JP 2011253872 A JP2011253872 A JP 2011253872A JP 5527311 B2 JP5527311 B2 JP 5527311B2
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- liquid crystal
- crystal composition
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- hydrocarbon solvent
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- 239000004973 liquid crystal related substance Substances 0.000 title claims description 64
- 239000000203 mixture Substances 0.000 title claims description 58
- 238000004519 manufacturing process Methods 0.000 title claims description 16
- 239000002904 solvent Substances 0.000 claims description 23
- 150000001875 compounds Chemical class 0.000 claims description 15
- 238000000034 method Methods 0.000 claims description 15
- 239000004215 Carbon black (E152) Substances 0.000 claims description 8
- 239000003463 adsorbent Substances 0.000 claims description 8
- 238000001914 filtration Methods 0.000 claims description 8
- 229930195733 hydrocarbon Natural products 0.000 claims description 8
- 150000002430 hydrocarbons Chemical class 0.000 claims description 8
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 6
- 239000000741 silica gel Substances 0.000 claims description 5
- 229910002027 silica gel Inorganic materials 0.000 claims description 5
- 230000007704 transition Effects 0.000 claims description 5
- 239000007788 liquid Substances 0.000 claims description 4
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 3
- 239000011148 porous material Substances 0.000 claims description 3
- 150000001338 aliphatic hydrocarbons Chemical group 0.000 claims description 2
- 238000011049 filling Methods 0.000 claims description 2
- 239000012535 impurity Substances 0.000 claims description 2
- 238000000967 suction filtration Methods 0.000 claims description 2
- 238000009835 boiling Methods 0.000 claims 1
- IMNFDUFMRHMDMM-UHFFFAOYSA-N N-Heptane Chemical compound CCCCCCC IMNFDUFMRHMDMM-UHFFFAOYSA-N 0.000 description 16
- 238000010438 heat treatment Methods 0.000 description 8
- 210000002858 crystal cell Anatomy 0.000 description 7
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 7
- 239000004810 polytetrafluoroethylene Substances 0.000 description 7
- 238000005259 measurement Methods 0.000 description 6
- 101000585157 Homo sapiens CST complex subunit STN1 Proteins 0.000 description 5
- 101000820457 Homo sapiens Stonin-2 Proteins 0.000 description 5
- 102100021683 Stonin-1 Human genes 0.000 description 5
- 102100021684 Stonin-2 Human genes 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 5
- 239000011159 matrix material Substances 0.000 description 5
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- 229910001873 dinitrogen Inorganic materials 0.000 description 4
- 238000002156 mixing Methods 0.000 description 4
- 239000000523 sample Substances 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- 235000002597 Solanum melongena Nutrition 0.000 description 3
- 244000061458 Solanum melongena Species 0.000 description 3
- 210000004027 cell Anatomy 0.000 description 3
- 239000003960 organic solvent Substances 0.000 description 3
- 238000000746 purification Methods 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 description 2
- 239000002033 PVDF binder Substances 0.000 description 2
- OFBQJSOFQDEBGM-UHFFFAOYSA-N Pentane Chemical compound CCCCC OFBQJSOFQDEBGM-UHFFFAOYSA-N 0.000 description 2
- 239000001913 cellulose Substances 0.000 description 2
- 229920002678 cellulose Polymers 0.000 description 2
- DIOQZVSQGTUSAI-UHFFFAOYSA-N decane Chemical compound CCCCCCCCCC DIOQZVSQGTUSAI-UHFFFAOYSA-N 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 238000002296 dynamic light scattering Methods 0.000 description 2
- 239000005262 ferroelectric liquid crystals (FLCs) Substances 0.000 description 2
- 239000000706 filtrate Substances 0.000 description 2
- 239000012299 nitrogen atmosphere Substances 0.000 description 2
- BKIMMITUMNQMOS-UHFFFAOYSA-N nonane Chemical compound CCCCCCCCC BKIMMITUMNQMOS-UHFFFAOYSA-N 0.000 description 2
- 230000000704 physical effect Effects 0.000 description 2
- 239000003495 polar organic solvent Substances 0.000 description 2
- -1 polypropylene Polymers 0.000 description 2
- 229920002981 polyvinylidene fluoride Polymers 0.000 description 2
- 239000012488 sample solution Substances 0.000 description 2
- XDTMQSROBMDMFD-UHFFFAOYSA-N Cyclohexane Chemical compound C1CCCCC1 XDTMQSROBMDMFD-UHFFFAOYSA-N 0.000 description 1
- 239000005909 Kieselgur Substances 0.000 description 1
- 239000000020 Nitrocellulose Substances 0.000 description 1
- 239000004677 Nylon Substances 0.000 description 1
- 229920012266 Poly(ether sulfone) PES Polymers 0.000 description 1
- 239000004743 Polypropylene Substances 0.000 description 1
- 229910021536 Zeolite Inorganic materials 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 229920002301 cellulose acetate Polymers 0.000 description 1
- 125000004122 cyclic group Chemical group 0.000 description 1
- 230000001627 detrimental effect Effects 0.000 description 1
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- 239000002019 doping agent Substances 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 239000004744 fabric Substances 0.000 description 1
- 239000003365 glass fiber Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000000155 melt Substances 0.000 description 1
- 229920001220 nitrocellulos Polymers 0.000 description 1
- 239000004745 nonwoven fabric Substances 0.000 description 1
- 229920001778 nylon Polymers 0.000 description 1
- TVMXDCGIABBOFY-UHFFFAOYSA-N octane Chemical compound CCCCCCCC TVMXDCGIABBOFY-UHFFFAOYSA-N 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000000123 paper Substances 0.000 description 1
- 229920001155 polypropylene Polymers 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 230000003068 static effect Effects 0.000 description 1
- FKHIFSZMMVMEQY-UHFFFAOYSA-N talc Chemical compound [Mg+2].[O-][Si]([O-])=O FKHIFSZMMVMEQY-UHFFFAOYSA-N 0.000 description 1
- 239000010457 zeolite Substances 0.000 description 1
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- Liquid Crystal Substances (AREA)
Description
比抵抗を高めるためには、組成物を構成する個々の液晶化合物のそれぞれについて高い比抵抗が達成されている必要がある。しかしながら、比抵抗の高い液晶化合物を使用しても、それらの混合物である液晶組成物を製造するときに品質を劣化させてしまうことがある。液晶組成物の製造方法としては、アセトン、クロロホルム、メタノール等の有機溶媒に溶解させて混合した後有機溶媒を除去する方法が提案されている(特許文献1及び2参照)。しかしながら、提案されている極性の有機溶剤に溶解させる方法では、有機溶剤の不純物やドーパントにより液晶組成物の比抵抗が著しく低下する問題がある。さらに極性の有機溶剤が除去しきれず残留することが多く、液晶組成物の比抵抗を低下させる原因になる。
比抵抗(Ω・cm)の測定は川口電気(株)製エレクトロメーターMMAII-17Aにて、セルギャップ1mmの液体電極LP-05型を用いて1VDCを印加して行った。
(パネル中での信頼性評価)
液晶組成物をTN用液晶セル(セルギャップ8.3μm)に真空注入し、UV硬化性樹脂(スリーボンド社製、Three Bond 3026)で封止し、液晶セルを作製した。
(参考例1)
転移温度94.7℃のSTN用液晶組成物STN1の作製について記載する。STN用液晶組成物STN1の組成を下記に示す。
参考例1に記載した組成と同様のSTN用液晶組成物STN1を特開2002-194356号公報に記載している方法に従い作製した。
(実施例1)
転移温度94.0℃のSTN用液晶組成物STN2を20g作製した。STN用液晶組成物STN2の組成を下記に示す。
実施例1に記載した組成と同様のSTN用液晶組成物STN2を特開2002-194356号公報に記載している方法に従い作製した。
Claims (5)
- 2種以上の液晶化合物を炭化水素系溶媒に溶解し、孔径10μmから0.001μmのフィルターを備えた濾過塔に、製造する液晶組成物の5質量%から0.1質量%のシリカゲル又はアルミナである吸着剤を充填して濾過した後、50KPa〜100Paの減圧下で溶媒を留去することを特徴とする液晶組成物の製造方法。
- 炭化水素系溶剤が脂肪族炭化水素系溶剤である請求項1記載の製造方法。
- 炭化水素系溶剤の高沸点不純物が5ppm以下である請求項1、又は2記載の製造方法。
- 溶媒の留去を、液晶組成物のネマチック相−等方性液体転移温度以下で行う請求項1〜3のいずれか一項に記載の製造方法。
- 減圧下に吸引濾過する請求項請求項1〜4のいずれか一項に記載の製造方法。
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JP2011253872A JP5527311B2 (ja) | 2011-11-21 | 2011-11-21 | 液晶組成物の製造方法 |
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JP2005088456A Division JP2006265453A (ja) | 2005-03-25 | 2005-03-25 | 液晶組成物の製造方法 |
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JP2012077308A JP2012077308A (ja) | 2012-04-19 |
JP5527311B2 true JP5527311B2 (ja) | 2014-06-18 |
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Family Cites Families (8)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPS57204512A (en) * | 1981-06-11 | 1982-12-15 | Sharp Corp | Manufacture of liquid crystal display element |
JPS6487685A (en) * | 1987-09-29 | 1989-03-31 | Seimi Chem Kk | Production of liquid crystal composition of high resistivity |
JPH0762347A (ja) * | 1993-08-25 | 1995-03-07 | Hitachi Chem Co Ltd | 精製された液晶の製造方法、液晶セル及び液晶表示装置 |
JPH08277391A (ja) * | 1995-02-10 | 1996-10-22 | Shin Etsu Chem Co Ltd | 液晶化合物の精製方法 |
JPH1046149A (ja) * | 1996-07-31 | 1998-02-17 | Canon Inc | 液晶組成物の調製方法 |
JPH11131063A (ja) * | 1997-03-06 | 1999-05-18 | Mitsubishi Gas Chem Co Inc | 精製された液晶の製造法 |
JP2003342576A (ja) * | 2001-07-31 | 2003-12-03 | Dainippon Ink & Chem Inc | 液晶化合物の精製方法 |
JP4228578B2 (ja) * | 2002-02-14 | 2009-02-25 | Dic株式会社 | 液晶表示素子用原材料の精製方法 |
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