JP6120121B2 - Container for storage or transport of liquid crystal - Google Patents

Container for storage or transport of liquid crystal Download PDF

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JP6120121B2
JP6120121B2 JP2016553066A JP2016553066A JP6120121B2 JP 6120121 B2 JP6120121 B2 JP 6120121B2 JP 2016553066 A JP2016553066 A JP 2016553066A JP 2016553066 A JP2016553066 A JP 2016553066A JP 6120121 B2 JP6120121 B2 JP 6120121B2
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liquid crystal
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crystal material
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alkyl group
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JPWO2016056454A1 (en
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平田 真一
真一 平田
孝福 車
孝福 車
小川 真治
真治 小川
原 智章
智章 原
梅津 安男
安男 梅津
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DIC Corp
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B65CONVEYING; PACKING; STORING; HANDLING THIN OR FILAMENTARY MATERIAL
    • B65DCONTAINERS FOR STORAGE OR TRANSPORT OF ARTICLES OR MATERIALS, e.g. BAGS, BARRELS, BOTTLES, BOXES, CANS, CARTONS, CRATES, DRUMS, JARS, TANKS, HOPPERS, FORWARDING CONTAINERS; ACCESSORIES, CLOSURES, OR FITTINGS THEREFOR; PACKAGING ELEMENTS; PACKAGES
    • B65D81/00Containers, packaging elements, or packages, for contents presenting particular transport or storage problems, or adapted to be used for non-packaging purposes after removal of contents
    • B65D81/18Containers, packaging elements, or packages, for contents presenting particular transport or storage problems, or adapted to be used for non-packaging purposes after removal of contents providing specific environment for contents, e.g. temperature above or below ambient
    • B65D81/20Containers, packaging elements, or packages, for contents presenting particular transport or storage problems, or adapted to be used for non-packaging purposes after removal of contents providing specific environment for contents, e.g. temperature above or below ambient under vacuum or superatmospheric pressure, or in a special atmosphere, e.g. of inert gas
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B65CONVEYING; PACKING; STORING; HANDLING THIN OR FILAMENTARY MATERIAL
    • B65DCONTAINERS FOR STORAGE OR TRANSPORT OF ARTICLES OR MATERIALS, e.g. BAGS, BARRELS, BOTTLES, BOXES, CANS, CARTONS, CRATES, DRUMS, JARS, TANKS, HOPPERS, FORWARDING CONTAINERS; ACCESSORIES, CLOSURES, OR FITTINGS THEREFOR; PACKAGING ELEMENTS; PACKAGES
    • B65D81/00Containers, packaging elements, or packages, for contents presenting particular transport or storage problems, or adapted to be used for non-packaging purposes after removal of contents
    • B65D81/24Adaptations for preventing deterioration or decay of contents; Applications to the container or packaging material of food preservatives, fungicides, pesticides or animal repellants
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B65CONVEYING; PACKING; STORING; HANDLING THIN OR FILAMENTARY MATERIAL
    • B65DCONTAINERS FOR STORAGE OR TRANSPORT OF ARTICLES OR MATERIALS, e.g. BAGS, BARRELS, BOTTLES, BOXES, CANS, CARTONS, CRATES, DRUMS, JARS, TANKS, HOPPERS, FORWARDING CONTAINERS; ACCESSORIES, CLOSURES, OR FITTINGS THEREFOR; PACKAGING ELEMENTS; PACKAGES
    • B65D85/00Containers, packaging elements or packages, specially adapted for particular articles or materials
    • GPHYSICS
    • G02OPTICS
    • G02FOPTICAL DEVICES OR ARRANGEMENTS FOR THE CONTROL OF LIGHT BY MODIFICATION OF THE OPTICAL PROPERTIES OF THE MEDIA OF THE ELEMENTS INVOLVED THEREIN; NON-LINEAR OPTICS; FREQUENCY-CHANGING OF LIGHT; OPTICAL LOGIC ELEMENTS; OPTICAL ANALOGUE/DIGITAL CONVERTERS
    • G02F1/00Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics
    • G02F1/01Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour 
    • G02F1/13Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour  based on liquid crystals, e.g. single liquid crystal display cells

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  • Engineering & Computer Science (AREA)
  • Physics & Mathematics (AREA)
  • Mechanical Engineering (AREA)
  • Nonlinear Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • General Physics & Mathematics (AREA)
  • Optics & Photonics (AREA)
  • Food Science & Technology (AREA)
  • Packages (AREA)
  • Packaging Frangible Articles (AREA)
  • Liquid Crystal (AREA)

Description

本発明は、安定した品質維持が求められる有機材料である液晶材料に使用する容器及びその容器を使った貯蔵又は輸送の方法に関する。   The present invention relates to a container used for a liquid crystal material which is an organic material for which stable quality maintenance is required, and a storage or transport method using the container.

液晶表示素子は、時計、電卓をはじめとして、各種測定機器、自動車用パネル、ワードプロセッサー、電子手帳、プリンター、コンピューター、テレビ、時計、広告表示板等に用いられるようになっている。液晶表示方式としては、その代表的なものにTN(ツイステッド・ネマチック)型、STN(スーパー・ツイステッド・ネマチック)型、TFT(薄膜トランジスタ)を用いた垂直配向型やIPS(イン・プレーン・スイッチング)型等がある。これらの液晶表示素子に用いられる液晶材料は、一般的には数種類から数十種類の化合物から構成される液状の組成物であって、それぞれの使用される用途や表示方式によって、最適な物性値や性能を求められる。更に、液晶表示素子の信頼性や寿命等の観点から水分、空気、熱、光などの外的要因に対して安定であることも求められる。また、液晶材料は、イオン性不純物等が混入すると液晶表示素子の電気的性能が悪化するため、その保管においても十分な管理が求められる。   Liquid crystal display elements are used in various measuring instruments, automobile panels, word processors, electronic notebooks, printers, computers, televisions, watches, advertisement display boards, as well as watches and calculators. Typical liquid crystal display methods include TN (twisted nematic) type, STN (super twisted nematic) type, vertical alignment type using TFT (thin film transistor), and IPS (in-plane switching) type. Etc. The liquid crystal material used in these liquid crystal display elements is generally a liquid composition composed of several to several tens of compounds, and has the optimum physical properties depending on the intended use and display method. And performance is required. Furthermore, the liquid crystal display element is required to be stable against external factors such as moisture, air, heat, and light from the viewpoint of reliability and lifetime. Moreover, since liquid crystal material deteriorates the electrical performance of the liquid crystal display element when ionic impurities or the like are mixed in, the liquid crystal material is required to be sufficiently managed in its storage.

液晶材料の保管には、100mLから1L程度のガラス瓶が使用されることが一般的であるが、液晶表示素子の大型化が進み、使用される液晶材料が増えることに伴って、液晶材料を保管する容器も大容量であることが必要となってきている。   For storage of liquid crystal materials, glass bottles of about 100 mL to 1 L are generally used. However, liquid crystal materials are stored as the liquid crystal display elements increase in size and use more liquid crystal materials. The container to be used is also required to have a large capacity.

しかし、大容量のガラス瓶はコストがかかり、また、運搬時にガラス瓶を破損してしまう危険性もある。また、液晶表示素子を製造するために液晶材料を液晶パネルに封入する方法として、液晶材料の保管容器に液晶材料を注入する装置へ導入する管を直接繋ぎ、ポンプ等で送り込む方式が提案されている。しかしながら、液晶表示素子の大型化に伴い、液晶材料を送り込むための圧力が大きくなり、そのために液晶材料の保管容器の耐圧も十分に強いものが求められるようになっている。   However, large-capacity glass bottles are costly and there is a risk of breaking the glass bottles during transportation. In addition, as a method of sealing a liquid crystal material in a liquid crystal panel in order to manufacture a liquid crystal display element, a method of directly connecting a pipe introduced into a device for injecting the liquid crystal material into a liquid crystal material storage container and feeding it with a pump or the like has been proposed. Yes. However, as the size of the liquid crystal display element increases, the pressure for feeding the liquid crystal material increases, and for this reason, a liquid container with a sufficiently high pressure resistance is required.

このような中、ステンレス製の液晶材料の貯蔵容器と液晶材料を注入するユニットが一体化した液晶表示素子の製造装置が提案されている。(特許文献1)
また、耐腐食性鋼鉄製の容器を用い。破損防止、液晶材料の汚染防止およびリユースによる環境的調和の改善を目的とした輸送および貯蔵の方法が提案されている。(特許文献2)
しかしながら、貯蔵や輸送の際にこれまで以上に高いレベルでの液晶材料の長期的な品質維持が求められていた。
Under such circumstances, a liquid crystal display element manufacturing apparatus in which a stainless steel liquid crystal material storage container and a unit for injecting liquid crystal material are integrated has been proposed. (Patent Document 1)
Also, use a container made of corrosion resistant steel. Transportation and storage methods have been proposed for the purpose of preventing damage, preventing contamination of liquid crystal materials, and improving environmental harmony through reuse. (Patent Document 2)
However, long-term quality maintenance of liquid crystal materials at a higher level than before has been required during storage and transportation.

特開2001−154210号公報JP 2001-154210 A 特開2005−157361号公報JP 2005-157361 A

本発明が解決しようする課題は、衝撃に対する破損等の問題が無く液晶材料をガス等の圧力により直接製造装置に移し替える作業にも耐えうることと、大型であっても軽量であることを両立する容器であって、更に液晶材料の品質の長期安定性を維持することができる容器を提供することである。また、これを用いた貯蔵又は輸送の方法を提供することである。   The problem to be solved by the present invention is that there is no problem such as breakage due to impact and that it can withstand the work of transferring the liquid crystal material directly to the manufacturing apparatus by the pressure of gas etc. and that it is lightweight even if it is large It is another object of the present invention to provide a container that can maintain the long-term stability of the quality of the liquid crystal material. Moreover, it is providing the method of the storage or transport using this.

本発明は、上記課題を解決するために鋭意検討した結果、気密性を有し、丈夫で軽く、更に特定の素材で構成される容器とすることで、長期的に品質安定性を与えることのできる貯蔵および輸送のための容器が得られることを見出し本発明の完成に至った。   As a result of diligent studies to solve the above-mentioned problems, the present invention provides long-term quality stability by providing a container that is airtight, strong and light, and made of a specific material. The inventors have found that a container for storage and transportation that can be obtained is obtained, and the present invention has been completed.

すなわち、気密性を有しフッ素系樹脂またはポリエステル樹脂を主成分とする素材から成ることを特徴とする有機材料の貯蔵又は運搬のための容器を提供する。   That is, the present invention provides a container for storing or transporting an organic material, which is airtight and made of a material mainly composed of a fluorine-based resin or a polyester resin.

本発明の容器は、耐衝撃性、耐圧性、軽量性を有することに加え、液晶材料の比抵抗値や電圧保持率を高い状態で貯蔵および輸送することができ、更に長期間において、その状態を維持することができることから、液晶材料の長期の品質安定性を与える。また、1Lもしくは1kgを超える大ロットの容量の貯蔵及び運搬に適用することができ、作業性が向上する。本発明の容器は、TN表示モード、IPS表示モード、VA表示モード、PSVA表示モード等のTFT駆動液晶表示素子を作製するために用いられる液晶材料の貯蔵および輸送に有用である。   In addition to having impact resistance, pressure resistance, and light weight, the container of the present invention can be stored and transported in a state where the specific resistance value and voltage holding ratio of the liquid crystal material are high, and the state is maintained for a long period of time. Can maintain the long-term quality stability of the liquid crystal material. Moreover, it can be applied to storage and transportation of large lots exceeding 1 L or 1 kg, and workability is improved. The container of the present invention is useful for storing and transporting a liquid crystal material used for manufacturing a TFT-driven liquid crystal display element such as a TN display mode, an IPS display mode, a VA display mode, and a PSVA display mode.

本発明の容器は、品質の安定性を求められる有機材料、特に液晶材料の貯蔵や輸送に用いられる。   The container of the present invention is used for storage and transportation of organic materials, particularly liquid crystal materials, for which quality stability is required.

本発明の容器は、正圧や負圧に対して気密性を有し、衝撃に耐えうる剛直性を有するが、圧力容器としての機能を有することが好ましい。正圧にする場合、容器内に圧縮空気や窒素ガスやアルゴンガス等の不活性ガスを封入するための分配器や圧力計を取り付けられるようになっていることが好ましく、負圧にする場合、真空ポンプによる減圧化を行うため配管を取り付けられるようになっていることが好ましい。   The container of the present invention has airtightness against positive pressure and negative pressure and has rigidity capable of withstanding an impact, but preferably has a function as a pressure container. When making a positive pressure, it is preferable to be able to attach a distributor or pressure gauge for sealing an inert gas such as compressed air, nitrogen gas or argon gas in the container. It is preferable that a pipe can be attached to reduce the pressure by a vacuum pump.

また、本発明の容器は、内容物の品質の安定性の観点から水や空気に対する気密性を有することが好ましい。   Moreover, it is preferable that the container of this invention has airtightness with respect to water or air from a viewpoint of stability of the quality of the content.

本発明の容器は、有機材料に接する面がフッ素系樹脂またはポリエステル樹脂を主成分とする素材より成る。本発明の容器全体がフッ素系樹脂またはポリエステル樹脂を主成分とするものでも良いし、金属製やプラスチック製の容器の中にフッ素系樹脂またはポリエステル樹脂を主成分とする袋を入れ、この袋を容器として使用しても良い。この場合には、フッ素系樹脂またはポリエステル樹脂を主成分とする袋を使用した後には新しい袋を使用する使い方をすることができる。また、その他の容器の構成として、金属製容器やプラスチック製容器の内面にフッ素系樹脂またはポリエステル樹脂をコーティングしても良い。   In the container of the present invention, the surface in contact with the organic material is made of a material mainly composed of a fluororesin or a polyester resin. The whole container of the present invention may be mainly composed of a fluororesin or a polyester resin, or a bag mainly composed of a fluororesin or a polyester resin is placed in a metal or plastic container. It may be used as a container. In this case, a new bag can be used after using a bag mainly composed of a fluororesin or a polyester resin. As another container configuration, a fluorine resin or a polyester resin may be coated on the inner surface of a metal container or a plastic container.

本発明の容器の素材の主成分であるフッ素系樹脂またはポリエステル樹脂は、具体的には、フッ素樹脂としてはポリテトラフルオロエチレン(PTFE)、ポリクロロトリフルオロエチレン(PCTFEまたはCTFE)、ポリフッ化ビニリデン(PVDF)、ポリフッ化ビニル(PVF)、ペルフルオロアルコキシフッ素樹脂(PFA)、四フッ化エチレン・六フッ化プロピレン共重合体(FEP)、エチレン・四フッ化エチレン共重合体(ETFE)又はエチレン・クロロトリフルオロエチレン共重合体(ECTFE)が好ましく、PTFE、PVF、PFAまたはETFE、が好ましく、PTFE、ETFE又はPFAが好ましい。ポリエステル樹脂としては、ポリエチレンテレフタラート(PET)、ポリトリメチレンテレフタレート(PTT)、ポリブチレンテレフタレート(PBT)、ポリエチレンナフタレート(PEN)又はポリブチレンナフタレート(PBN)が好ましく、PENまたはPBNが好ましい。   Specifically, the fluororesin or polyester resin that is the main component of the material of the container of the present invention includes polytetrafluoroethylene (PTFE), polychlorotrifluoroethylene (PCTFE or CTFE), and polyvinylidene fluoride as the fluororesin. (PVDF), polyvinyl fluoride (PVF), perfluoroalkoxy fluororesin (PFA), tetrafluoroethylene / hexafluoropropylene copolymer (FEP), ethylene / tetrafluoroethylene copolymer (ETFE) or ethylene / Chlorotrifluoroethylene copolymer (ECTFE) is preferred, PTFE, PVF, PFA or ETFE is preferred, and PTFE, ETFE or PFA is preferred. As the polyester resin, polyethylene terephthalate (PET), polytrimethylene terephthalate (PTT), polybutylene terephthalate (PBT), polyethylene naphthalate (PEN) or polybutylene naphthalate (PBN) is preferable, and PEN or PBN is preferable.

本発明の容器の内表面は、特定の処理等がなされていても良い。   The inner surface of the container of the present invention may be subjected to a specific treatment.

本発明の容器の容量は、1L以上であることが好ましく、5L以上であることが更に好ましい。軽量性を有し、耐圧性、衝撃性に耐えうるので、100L以上であることもできる。   The capacity of the container of the present invention is preferably 1 L or more, and more preferably 5 L or more. Since it is lightweight and can withstand pressure resistance and impact resistance, it can also be 100 L or more.

本発明の容器は、比抵抗等の電気的性能の長期的安定性が求められる電子デバイス製造用有機材料に使用されることが好ましく、液晶表示素子用の液晶材料に使用されることが更に好ましく、TFT駆動液晶表示素子用の液晶材料に使用されることが特に好ましい。   The container of the present invention is preferably used for an organic material for manufacturing an electronic device that requires long-term stability of electrical performance such as specific resistance, and more preferably used for a liquid crystal material for a liquid crystal display element. It is particularly preferable to be used as a liquid crystal material for TFT-driven liquid crystal display elements.

本発明の容器に使用される液晶材料として、例えば、フッ素基が導入された液晶化合物を含有する液晶組成物が挙げられる。   Examples of the liquid crystal material used in the container of the present invention include a liquid crystal composition containing a liquid crystal compound into which a fluorine group is introduced.

フッ素基が導入された液晶化合物として、具体的には以下のようなものが挙げられる。   Specific examples of the liquid crystal compound into which a fluorine group is introduced include the following.

Figure 0006120121
Figure 0006120121

(式中、R11は炭素数1〜15のアルキル基を表し、該アルキル基中の1つ又は2つ以上の−CH−は、酸素原子が直接隣接しないように、−O−、−CH=CH−、−CO−、−OCO−、−COO−、−CFO−又は−OCF−で置換されてよく、該アルキル基中の1つ又は2つ以上の水素原子は任意にハロゲンで置換されていてもよく、A11、A12はそれぞれ独立して下記の何れかの構造(In the formula, R 11 represents an alkyl group having 1 to 15 carbon atoms, and one or two or more —CH 2 — in the alkyl group is —O—, — CH = CH—, —CO—, —OCO—, —COO—, —CF 2 O— or —OCF 2 — may be substituted, and one or more hydrogen atoms in the alkyl group may be optionally substituted It may be substituted with halogen, and A 11 and A 12 are each independently any one of the following structures

Figure 0006120121
Figure 0006120121

(該構造中シクロヘキサン環の1つ又は2つ以上の−CH−は酸素原子が直接隣接しないように、−O−で置換されていてもよく、X61及びX62はそれぞれ独立して−H、−Cl、−F、−CF又は−OCFを表す。)を表し、Xは−H、−Cl又は−Fを表し、Yは−F、−OCHF、−CF又は−OCFを表し、Z11及びZ12はそれぞれ独立して単結合、−CH=CH−、−CHO−、−OCH−、−CHCH−、−(CH−、−OCF−又は−CFO−を表し、mは0〜4を表し、A12及び/又はZ12が複数存在する場合、それらは同一であっても、異なっていてもよい。)
また、その他のフッ素基が導入された液晶化合物として、具体的には以下のようなものが挙げられる。
(In the structure, one or more —CH 2 — of the cyclohexane ring may be substituted with —O— so that the oxygen atom is not directly adjacent to each other, and X 61 and X 62 are each independently — H represents —H, —Cl, —F, —CF 3 or —OCF 3 ), X represents —H, —Cl or —F, and Y represents —F, —OCHF 2 , —CF 3 or —OCF. 3 and Z 11 and Z 12 are each independently a single bond, —CH═CH—, —CH 2 O—, —OCH 2 —, —CH 2 CH 2 —, — (CH 2 ) 4 —, — OCF 2 - or -CF 2 O-a represents, m 1 represents 0 to 4, when a 12 and / or Z 12 is plurally present, they may be the same or different. )
Specific examples of the liquid crystal compound into which other fluorine groups are introduced include the following.

Figure 0006120121
Figure 0006120121

(式中、R21及びR22はそれぞれ独立して炭素数1〜15のアルキル基を表し、該アルキル基中の1つ又は2つ以上の−CH−は、酸素原子が直接隣接しないように、−O−、−CH=CH−、−CO−、−OCO−、−COO−、−CFO−又は−OCF−で置換されてよく、該アルキル基中の1つ又は2つ以上の水素原子は任意にハロゲンで置換されていてもよく、A21、A22はそれぞれ独立して下記の何れかの構造(In the formula, R 21 and R 22 each independently represent an alkyl group having 1 to 15 carbon atoms, and one or two or more —CH 2 — in the alkyl group is not directly adjacent to an oxygen atom. May be substituted with —O—, —CH═CH—, —CO—, —OCO—, —COO—, —CF 2 O— or —OCF 2 —, one or two of the alkyl groups. The above hydrogen atoms may be optionally substituted with halogen, and A 21 and A 22 are each independently one of the following structures:

Figure 0006120121
Figure 0006120121

を表し、Z21及びZ22はそれぞれ独立して単結合、−CH=CH−、−CHO−、−OCH−、−CHCH−、−(CH−、−OCF−又は−CFO−を表し、m及びmは0〜3を表すが、m+mは1〜3を表し、A21、A22、Z21及び/又はZ22が複数存在する場合、それらは同一であっても、異なっていてもよい。)
上記の液晶化合物は、誘電率異方性が負の液晶材料を調製する際に主要に使用されるものであるが、誘電率異方性が負の液晶材料は、液晶材料の中でもより高い品質や品質の経時安定性を求められるため、本発明の容器を誘電率異方性が負の液晶材料に使用することは特に好ましい。
Z 21 and Z 22 are each independently a single bond, —CH═CH—, —CH 2 O—, —OCH 2 —, —CH 2 CH 2 —, — (CH 2 ) 4 —, —OCF. 2 -, or -CF 2 O-, although m 2 and m 3 represent 0 to 3, m 2 + m 3 represents 1~3, a 21, a 22, Z 21 and / or Z 22 is more If present, they may be the same or different. )
The above liquid crystal compounds are mainly used when preparing liquid crystal materials with negative dielectric anisotropy, but liquid crystal materials with negative dielectric anisotropy are of higher quality than liquid crystal materials. It is particularly preferable to use the container of the present invention for a liquid crystal material having a negative dielectric anisotropy, because stability over time and quality are required.

本発明の容器に使用される液晶材料には、フッ素基が導入された液晶化合物以外の液晶化合物も含有することができる。具体的には以下のような一般式(III−A)〜一般式(III−J)で表される化合物が挙げられる。   The liquid crystal material used in the container of the present invention can also contain a liquid crystal compound other than a liquid crystal compound into which a fluorine group has been introduced. Specific examples include compounds represented by the following general formula (III-A) to general formula (III-J).

Figure 0006120121
Figure 0006120121

(式中、R及びRはそれぞれ独立して炭素数1〜15のアルキル基を表し、該アルキル基中の1つ又は2つ以上の−CH−は、酸素原子が直接隣接しないように、−O−、−CH=CH−、−CO−、−OCO−、−COO−、−CFO−又は−OCF−で置換されてよく、該アルキル基中の1つ又は2つ以上の水素原子は任意にハロゲンで置換されていてもよい。)
これらの液晶化合物は単独で用いても、複数を混合して用いても良い。
(In the formula, R 5 and R 6 each independently represents an alkyl group having 1 to 15 carbon atoms, and one or two or more —CH 2 — in the alkyl group is not directly adjacent to an oxygen atom. May be substituted with —O—, —CH═CH—, —CO—, —OCO—, —COO—, —CF 2 O— or —OCF 2 —, one or two of the alkyl groups. (The above hydrogen atoms may be optionally substituted with halogen.)
These liquid crystal compounds may be used alone or in combination.

TFT駆動用液晶表示素子に用いられる液晶材料は、高比抵抗値あるいは高電圧保持率を有し、更にその経時安定性を強く求められることから、本発明の容器は好適である。特に、比抵抗値1.0×1012Ω・cm以上の液晶材料に適用することが好ましく、1.0×1013Ω・cm以上の液晶材料に適用することがより好ましく、1.0×1014Ω・cm以上の液晶材料に適用することが更に好ましい。The container of the present invention is suitable because the liquid crystal material used for the TFT driving liquid crystal display element has a high specific resistance value or a high voltage holding ratio, and its stability over time is strongly required. In particular, it is preferably applied to a liquid crystal material having a specific resistance value of 1.0 × 10 12 Ω · cm or more, more preferably applied to a liquid crystal material having a specific resistance value of 1.0 × 10 13 Ω · cm or more. More preferably, it is applied to a liquid crystal material of 10 14 Ω · cm or more.

本発明の容器は、フッ素系樹脂を主成分とする素材とすることで液晶材料の比抵抗や電圧保持率等の電気的性能を劣化させることなく、長期間に渡って、変化が極めて小さく、特性の維持をすることができるため、貯蔵および輸送に使用することが好ましい。また、液晶材料を貯蔵あるいは輸送に使用している本発明の容器を配管等で、そのまま液晶表示素子の製造装置に連結することもできる。   The container of the present invention has a very small change over a long period of time without deteriorating the electrical performance such as the specific resistance and voltage holding ratio of the liquid crystal material by using a fluorine resin as a main component. It is preferable to use it for storage and transportation because the characteristics can be maintained. Further, the container of the present invention in which the liquid crystal material is used for storage or transportation can be directly connected to a liquid crystal display element manufacturing apparatus by piping or the like.

本発明の容器は、輸送の際の移動を容易するために容器の底に底車等を取り付けることもできる。   In the container of the present invention, a bottom wheel or the like can be attached to the bottom of the container in order to facilitate movement during transportation.

本発明の容器は、容器内を正圧や負圧の状態にすることができるように、気密性を有し、耐圧性のバルブ等を取り付けた構造とすることができる。   The container of the present invention can be structured to have airtightness and a pressure-resistant valve so that the inside of the container can be in a positive pressure or negative pressure state.

本発明の容器は、剛直で気密性を持たせることで、貯蔵や輸送の際に、容器内を真空状態したり、不活性ガス雰囲気状態することができる。これにより、容器内の有機材料が水や酸素により影響を受けないようにすることできる。   Since the container of the present invention is rigid and airtight, the inside of the container can be evacuated or in an inert gas atmosphere during storage and transportation. Thereby, it is possible to prevent the organic material in the container from being affected by water or oxygen.

以下に実施例を挙げて本発明を更に詳述するが、本発明はこれらの実施例に限定されるものではない。また、以下の実施例及び比較例の組成物における「%」は『質量%』を意味する。
実施例において化合物の記載について以下の略号を用いる。なお、nは自然数を表す。
(側鎖)
-n -CnH2n+1 炭素原子数nの直鎖状のアルキル基
n- CnH2n+1- 炭素原子数nの直鎖状のアルキル基
-On -OCnH2n+1 炭素原子数nの直鎖状のアルコキシル基
nO- CnH2n+1O- 炭素原子数nの直鎖状のアルコキシル基
-V -CH=CH2
V- CH2=CH-
-V1 -CH=CH-CH3
1V- CH3-CH=CH-
-2V -CH2-CH2-CH=CH3
V2- CH3=CH-CH2-CH2-
-2V1 -CH2-CH2-CH=CH-CH3
1V2- CH3-CH=CH-CH2-CH2
(連結基)
-n- -CnH2n-
-nO- -CnH2n-O-
-On- -O-CnH2n-
-COO- -C(=O)-O-
-OCO- -O-C(=O)-
-CF2O- -CF2-O-
-OCF2- -O-CF2-
(環構造)
EXAMPLES The present invention will be described in further detail with reference to examples below, but the present invention is not limited to these examples. Further, “%” in the compositions of the following Examples and Comparative Examples means “% by mass”.
The following abbreviations are used for the description of compounds in the examples. Note that n represents a natural number.
(Side chain)
-n -C n H 2n + 1 linear alkyl group with n carbon atoms
n-C n H 2n + 1- linear alkyl group having n carbon atoms
-On -OC n H 2n + 1 linear alkoxyl group with n carbon atoms
nO- C n H 2n + 1 O- Linear alkoxyl group with n carbon atoms
-V -CH = CH 2
V- CH 2 = CH-
-V1 -CH = CH-CH 3
1V- CH 3 -CH = CH-
-2V -CH 2 -CH 2 -CH = CH 3
V2- CH 3 = CH-CH 2 -CH 2-
-2V1 -CH 2 -CH 2 -CH = CH-CH 3
1V2- CH 3 -CH = CH-CH 2 -CH 2
(Linking group)
-n- -C n H 2n-
-nO- -C n H 2n -O-
-On- -OC n H 2n -
-COO- -C (= O) -O-
-OCO- -OC (= O)-
-CF2O- -CF 2 -O-
-OCF2- -O-CF 2-
(Ring structure)

Figure 0006120121
Figure 0006120121

実施例中、測定した特性は以下の通りである。   In the examples, the measured characteristics are as follows.

ni :ネマチック相−等方性液体相転移温度(℃)
cn :固体相−ネマチック相転移温度(℃)
Δn :20℃における屈折率異方性
Δε :20℃における誘電率異方性
η :20℃における粘度(mPa・s)
γ :20℃における回転粘度(mPa・s)
33 :20℃における弾性定数K33(pN)
比抵抗値 :25℃における比抵抗値(Ω・cm)
電圧保持率:60Hz、1V印加条件での60℃における電圧保持率(%)
イオン密度:0.05Hz、20V印加条件での60℃におけるイオン密度(pC/cm−3
また、重合性化合物含有液晶組成物に使用した重合性化合物の代表例として式(Ib−3)の化合物を用いたが、本発明は該重合性化合物に限定されるものではない。
T ni : Nematic phase-isotropic liquid phase transition temperature (° C.)
T cn : Solid phase-nematic phase transition temperature (° C.)
Δn: Refractive index anisotropy at 20 ° C. Δε: Dielectric anisotropy at 20 ° C. η: Viscosity at 20 ° C. (mPa · s)
γ 1 : rotational viscosity at 20 ° C. (mPa · s)
K 33 : Elastic constant at 20 ° C. K 33 (pN)
Specific resistance value: Specific resistance value at 25 ° C. (Ω · cm)
Voltage holding ratio: 60 Hz, 1 V voltage holding ratio at 60 ° C. (%)
Ion density: 0.05 Hz, ion density at 60 ° C. under 20 V application condition (pC / cm −3 )
Moreover, although the compound of Formula (Ib-3) was used as a representative example of the polymerizable compound used in the polymerizable compound-containing liquid crystal composition, the present invention is not limited to the polymerizable compound.

Figure 0006120121
Figure 0006120121

以下に実施例を挙げて本発明を更に詳述するが、本発明はこれらの実施例に限定されるものではない。
(実施例1、実施例2および比較例1)
代表的な液晶組成物としてLC−Aを調製した。液晶組成物の構成とその物性値は表1のとおりであった。
EXAMPLES The present invention will be described in further detail with reference to examples below, but the present invention is not limited to these examples.
(Example 1, Example 2 and Comparative Example 1)
LC-A was prepared as a typical liquid crystal composition. The composition of the liquid crystal composition and its physical property values are shown in Table 1.

Figure 0006120121
Figure 0006120121

LC−A 99.5%に式(Ib−3)の重合性化合物0.5%添加した重合性化合物含有液晶組成物MLC−1を調製した。   A polymerizable compound-containing liquid crystal composition MLC-1 in which 0.5% of the polymerizable compound of the formula (Ib-3) was added to 99.5% of LC-A was prepared.

鋼鉄(SUS304)製の容量10Lの耐圧構造を有する容器を2基製造し、内表面に物理研磨および電界研磨を施したのちに中性洗剤、アルコール系洗浄剤および/又は超純水により充分な洗浄を実施した。また、ポリエチレンナフタレート(PEN)からなる容量10Lの耐圧構造を有する容器を製造し、充分に洗浄を行った。MLC−1を上記容量10Lの鋼鉄(SUS304)製容器(比較例1)、ポリテトラフルオロエチレン(PTFE)からなる内袋を有する容量10Lの鋼鉄(SUS304)製容器(実施例1)及びPENからなる内袋を有する容量10Lの容器(実施例2)に充填・密閉した。上記PTFEからなる内袋は中性洗剤、アルコール系洗浄剤および/又は超純水で洗浄し、充分に乾燥させたものを用いた。室温でMLC−1を充填した各容器を保管し、1ヶ月後に開封し品質評価を行った。評価結果を表2に示す。   Two containers with a pressure-resistant structure made of steel (SUS304) having a capacity of 10 L are manufactured, and after the inner surface is physically polished and electropolished, it is sufficient to use neutral detergent, alcohol-based detergent and / or ultrapure water. Washing was performed. Further, a container having a pressure-resistant structure having a capacity of 10 L made of polyethylene naphthalate (PEN) was manufactured and sufficiently washed. MLC-1 from a 10 L steel (SUS304) container (Comparative Example 1), a 10 L steel (SUS304) container (Example 1) having an inner bag made of polytetrafluoroethylene (PTFE), and PEN A 10 L container (Example 2) having an inner bag was filled and sealed. The inner bag made of PTFE was washed with a neutral detergent, an alcohol-based detergent and / or ultrapure water and sufficiently dried. Each container filled with MLC-1 was stored at room temperature, opened one month later, and evaluated for quality. The evaluation results are shown in Table 2.

Figure 0006120121
Figure 0006120121

比較例1である鋼鉄製容器に充填したMLC−1は1ヵ月後と比抵抗値および電圧保持率の下落、ならびにイオン密度の増加が見られた。一方、実施例1であるPTFEからなる内袋を有する鋼鉄製容器及び実施例2であるPENからなる容量10Lの容器に充填したMLC−1は比抵抗値、電圧保持率およびイオン密度に大きな変化は見られなかった。
以上のことから、本発明の容器は液晶材料の品質と強い相関のある比抵抗値、電圧保持率およびイオン密度などの指標を変化させない優れた容器であることが確認された。
MLC-1 filled in a steel container as Comparative Example 1 showed a decrease in resistivity and voltage holding ratio and an increase in ion density after one month. On the other hand, MLC-1 filled in a steel container having an inner bag made of PTFE as Example 1 and a 10 L container made of PEN as Example 2 has a large change in specific resistance value, voltage holding ratio and ion density. Was not seen.
From the above, it was confirmed that the container of the present invention is an excellent container that does not change indicators such as specific resistance, voltage holding ratio, and ion density, which have a strong correlation with the quality of the liquid crystal material.

Claims (7)

液晶材料との接触面がポリエステル樹脂を主成分とする素材であり、前記液晶材料が、一般式(III−A)〜一般式(III−J)
Figure 0006120121
(式中、R 及びR はそれぞれ独立して炭素数1〜15のアルキル基を表し、該アルキル基中の1つ又は2つ以上の−CH −は、酸素原子が直接隣接しないように、−O−、−CH=CH−、−CO−、−OCO−、−COO−、−CF O−又は−OCF −で置換されてよく、該アルキル基中の1つ又は2つ以上の水素原子は任意にハロゲンで置換されていてもよい。)で表される化合物の群から選ばれる化合物を含有し、水及び酸素に対する気密性を有する液晶材料貯蔵又は運搬容器。
The contact surface with the liquid crystal material is a material mainly composed of a polyester resin, and the liquid crystal material is represented by the general formula (III-A) to the general formula (III-J).
Figure 0006120121
(In the formula, R 5 and R 6 each independently represents an alkyl group having 1 to 15 carbon atoms, and one or two or more —CH 2 in the alkyl group is not directly adjacent to an oxygen atom. May be substituted with —O—, —CH═CH—, —CO—, —OCO—, —COO—, —CF 2 O— or —OCF 2 —, one or two of the alkyl groups. The above hydrogen atom may be optionally substituted with halogen.) A liquid crystal material storage or transportation container containing a compound selected from the group of compounds represented by:
金属製又はプラスチック製の容器の中に、前記素材の袋に口を取り付けた容器を入れた請求項1記載の容器。 The container according to claim 1, wherein a container having a mouth attached to a bag of the material is placed in a metal or plastic container. ポリエステル樹脂がポリブチレンテレフタレート(PBT)、ポリエチレンナフタレート(PEN)又はポリブチレンナフタレート(PBN)が主成分である請求項1又は2のいずれか1項に記載の容器。 The container according to any one of claims 1 and 2, wherein the polyester resin is mainly composed of polybutylene terephthalate (PBT), polyethylene naphthalate (PEN), or polybutylene naphthalate (PBN). 前記有機材料が、誘電率異方性が負の液晶材料である請求項1〜3のいずれか1項に記載の容器。 The container according to claim 1, wherein the organic material is a liquid crystal material having a negative dielectric anisotropy. 前記誘電率異方性が負の液晶材料が、以下の一般式
Figure 0006120121
(式中、R 21 及びR 22 はそれぞれ独立して炭素数1〜15のアルキル基を表し、該アルキル基中の1つ又は2つ以上の−CH −は、酸素原子が直接隣接しないように、−O−、−CH=CH−、−CO−、−OCO−、−COO−、−CF O−又は−OCF −で置換されてよく、該アルキル基中の1つ又は2つ以上の水素原子は任意にハロゲンで置換されていてもよく、A 21 、A 22 はそれぞれ独立して下記の何れかの構造
Figure 0006120121
を表し、Z 21 及びZ 22 はそれぞれ独立して単結合、−CH=CH−、−CH O−、−OCH −、−CH CH −、−(CH −、−OCF −又は−CF O−を表し、m 及びm は0〜3を表すが、m +m は1〜3を表し、A 21 、A 22 、Z 21 及び/又はZ 22 が複数存在する場合、それらは同一であっても、異なっていてもよい。)で表される化合物を含有する請求項4に記載の容器。
The liquid crystal material having a negative dielectric anisotropy is represented by the following general formula:
Figure 0006120121
(In the formula, R 21 and R 22 each independently represent an alkyl group having 1 to 15 carbon atoms, and one or two or more —CH 2 in the alkyl group is not directly adjacent to an oxygen atom. May be substituted with —O—, —CH═CH—, —CO—, —OCO—, —COO—, —CF 2 O— or —OCF 2 —, one or two of the alkyl groups. The above hydrogen atoms may be optionally substituted with halogen, and A 21 and A 22 are each independently one of the following structures:
Figure 0006120121
Z 21 and Z 22 are each independently a single bond, —CH═CH—, —CH 2 O—, —OCH 2 —, —CH 2 CH 2 —, — (CH 2 ) 4 —, —OCF. 2 -, or -CF 2 O-, although m 2 and m 3 represent 0 to 3, m 2 + m 3 represents 1~3, a 21, a 22, Z 21 and / or Z 22 is more If present, they may be the same or different. The container of Claim 4 containing the compound represented by this .
請求項1〜5のいずれか一項に記載の容器を用いた貯蔵又は運搬の方法。 The method of storage or conveyance using the container as described in any one of Claims 1-5. 不活性ガス雰囲気下で行う請求項6記載の貯蔵又は運搬の方法。 The method for storage or transportation according to claim 6, which is carried out in an inert gas atmosphere.
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