CN101210183B - Method for purifying liquid crystal material - Google Patents
Method for purifying liquid crystal material Download PDFInfo
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- CN101210183B CN101210183B CN2006101673305A CN200610167330A CN101210183B CN 101210183 B CN101210183 B CN 101210183B CN 2006101673305 A CN2006101673305 A CN 2006101673305A CN 200610167330 A CN200610167330 A CN 200610167330A CN 101210183 B CN101210183 B CN 101210183B
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Abstract
A method for purifying liquid crystal material comprises the steps of settling a liquid crystal material loaded in a semi-sealed conductive box in an electric field environment, and extracting the liquid crystal material in the electric field environment. By adopting electric field action, the method for purifying the liquid crystal material can improve the resistivity of liquid crystal material to above 6*10<13> omega*cm; on the other hand, no solvent is needed so no pollution is caused to environment. Additionally, the electric field environment is typically achieved in the semi-sealed conductive glass box, thus achieving less influence by the environment and the operation, no secondary contamination on the liquid crystal, good reproducibility, and stable production of high-resistivity liquid crystal material. Additionally, the invention also has the advantages of high yield and low liquid crystal loss.
Description
Technical field
The invention relates to a kind of method of purifying liquid crystal material.
Background technology
Liquid crystal display device has been widely used in the various display terminals at present because of having advantages such as volume is little, in light weight, low in energy consumption, driving voltage is low.Critical material liquid crystal in the liquid crystal display device has a significant impact the various aspects of performance of indicating meter.Liquid crystal not only will have very high purity, and needs very high resistivity, generally must reach 10
11More than the ohmcm, especially, higher to the requirement of resistivity for display types such as high-grade STN, TFT, generally need reach 10
13More than the ohmcm.
The factor that influences liquid crystal purity is a lot, the solvent that comprises in monomer liquid crystal or the mixed liquid crystal, unreacted material, various byproduct of reaction, moisture, various zwitterions etc. completely for example, these all can impact the performance of liquid crystal, therefore want the good liquid crystal of obtained performance must remove these impurity.Remove desolvate, material, side reaction thing, moisture etc. can make liquid crystal monomer reach required purity to unreacted with the chemical process of routine completely.And zwitterion wherein is difficult to remove after reaching certain purity again, thereby makes the raising of liquid crystal resistivity comparatively difficult.And the zwitterion in the liquid crystal is one of key factor that influences liquid crystal resistivity, and ion content is high more, and the resistivity of liquid crystal is low more.Thereby, want to improve the resistivity of liquid crystal, must remove the content of the zwitterion in the liquid crystal as far as possible.
At present, absorption method is because of it is direct, easy, effect is better relatively, and is therefore many to the research of absorption method, also is the method that zwitterion the most generally uses of removing, and sorbent material commonly used has aluminum oxide, silica gel, gac, molecular sieve, polyimide particles etc.For example, it is that the polyimide that 0.1-5000 micron, specific surface are not less than 1 meters squared per gram is done the sorbent material liquid crystal purifying that US 6056892 discloses with median size, can make the resistivity of the ZLI-4792 liquid crystal that Merck Japan Ltd. produces bring up to 1.2 * 10
12Ohmcm.
US 5540857 discloses a kind of method of purification of anti-ferroelectric liquid crystals, this method comprises the anti-ferroelectric liquid crystals solution of preparation, gained solution is contacted, filters the gained liquid crystal solution with at least a sorbent material in zeolite, aluminum oxide and the silica gel and remove solvent in the liquid crystal solution, obtains resistivity and is at least 5 * 10
12The liquid crystal of ohmcm.
CN 1775908A discloses a kind of method of liquid crystal purifying, this method comprises the mixture of activated carbon fiber or activated carbon fiber and activated alumina added in the liquid crystal material and forms mixing material, mixing material is mixed in organic solvent, stirs, after removing solid impurity and solvent, obtain the liquid crystal material of high purity and high resistivity.Using this method, can be 6.0 * 10 with initial electrical resistivity
12The resistivity of the monomer liquid crystal of ohmcm brings up to 3 * 10
13More than the ohmcm, be 5.0 * 10 with initial electrical resistivity
12The resistivity of the mixed liquid crystal of ohmcm brings up to 3 * 10
13More than the ohmcm.
Though aforesaid method can improve the resistivity of liquid crystal to a certain extent, but above-mentioned absorption method all needs to use a large amount of organic solvents, this can cause environmental pollution on the one hand, also can increase cost on the other hand, extend manufacture cycle, the most important thing is, purity requirement to solvent itself is very high, in actually operating, be easy to the impurity of solvent itself is incorporated in the liquid crystal, so often occur purifying the phenomenon that purity and/or resistivity are low more on the contrary more in field of liquid crystals.Thereby aforesaid method can't be stablized the resistivity that improves liquid crystal material effectively.
Summary of the invention
The objective of the invention is to stablize the shortcoming of the resistivity that improves liquid crystal material effectively, a kind of method that can stablize the purifying liquid crystal material of the resistivity that improves liquid crystal material effectively is provided for the method that overcomes existing purifying liquid crystal material.
The method of purifying liquid crystal material provided by the invention comprises that the liquid crystal material that will be contained in the conductive glass box of semitight stops, and takes out liquid crystal material then in electric field environment in electric field environment.
The method of purifying liquid crystal material provided by the invention is by in electric field environment, improves the resistivity of liquid crystal material with electric field action, can make the resistivity of liquid crystal reach 6 * 10 on the one hand
13More than the ohmcm,, thereby can not cause pollution problem to environment on the other hand because need not to use solvent; In addition, because electric field environment is normally by realizing in the conductive glass box of semitight, thereby is subjected to the influence of environment and operation little, do not have the secondary pollution problem to liquid crystal, reproducibility is good, can stably produce the high resistivity liquid crystal material.In addition, this method also has yield height, the low advantage of liquid crystal loss.
Description of drawings
Fig. 1 is the structural representation of the used conductive box of the present invention.
Embodiment
According to method provided by the invention, wherein said electric field environment is preferably the electric field environment that voltage is not less than 50 volts, for example is the electric field environment of 50-900 volt for voltage, and more preferably voltage is the electric field environment of 150-350 volt.Voltage is big more, and the effect that liquid crystal material resistivity is improved is good more, but also high more to the requirement of equipment.Can apply voltage by two ends and realize electric field environment in conductive box.Described conductive box can be the various containers of being made by various electro-conductive materials, as the conductive glass box.Because glass has transparent, easy to clean, stable performance, non-metal ion, do not adsorb the advantage of liquid crystal material substantially, so the preferred conductive container of the present invention is the conductive glass box, as the indium tin oxide-coated glass box.Described conductive glass box can directly be commercially available, be generally hexahedron structure, as shown in Figure 1, two wherein relative surfaces 1 are conductive surface, the conductive glass that tin indium oxide (ITO) can be arranged for surface-coated, described surperficial 1 is preferably two bigger surfaces of area, and remaining surface is a Surface Insulation.The equal metal clad electrode 2 of an end separately in the one side that is coated with tin indium oxide on two surfaces 1, be electrically connected with the positive and negative electrode of power supply by this metal electrode 2, realize the conductive surface of conductive box and being electrically connected of power supply, to obtain the electric field environment of purifying liquid crystal material of the present invention.The liquid crystal material inlet 3 and the liquid crystal material outlet 3 ' of the brilliant material turnover of feed flow are arranged respectively on the conductive glass box, described liquid crystal material inlet 3 and liquid crystal material outlet 3 ' preferably lay respectively on the different surfaces of conductive glass box, can avoid like this without the pollution of the liquid crystal of purifying the back liquid crystal of purifying, outlet lays respectively on two relative Surface Insulations of conductive glass box, to improve the time of liquid crystal material in electric field environment as far as possible more preferably described liquid crystal material inlet with liquid crystal material.
There is no particular limitation to the size of conductive glass box, can be any size, and for example the surface-area of conductive box can be 1-2 square metre.The thickness of described conductive box can be the 50-1000 micron, is preferably the 100-300 micron, that is to say, the thickness of liquid crystal material can be the 50-1000 micron, is preferably the 100-300 micron.
The time that liquid crystal material stops in electric field environment can be 1-10 hour, is preferably 4-7 hour.
Method provided by the invention can be injected above-mentioned conductive glass box by liquid crystal material, applies voltage then on the conductive glass box, and liquid crystal material is in the electric field environment.Resistivity through the liquid crystal material after the above-mentioned processing can reach 6 * 10
13More than the ohmcm.
This method can be injected liquid crystal material by the liquid crystal material import from the conductive glass box, export through the liquid crystal material after the electric field environment effect from the liquid crystal material exit then, thereby the intermittent type of realization liquid crystal material or continous way is purified.Liquid crystal material can inject the conductive glass box by vacuum suck method or pressurization, and the concrete operations of vacuum suck method or pressurization have been conventionally known to one of skill in the art.The speed of injecting stops liquid crystal material under electric field environment time is 1-10 hour, preferred 4-7 hour, specifically decide, for example on the size of conductive glass box, for volume is the conductive glass box that 0.1-1 rises, and the injection speed of liquid crystal material can be 0.5-1 liter/6 hour.
Liquid crystal material purification principle of the present invention is, by in electric field environment, staying for some time, making the ion in the liquid crystal material also is the edge of conductive surface by positive terminal or the negative pole end that electric field is adsorbed onto electric field, and liquid crystal material does not rearrange under electric field action, like this, in electric field environment, realized separating of ion and liquid crystal material, take out liquid crystal material after, ion is still stayed in the conductive box.Through after a while or after absorption goes up a certain amount of ion, can change conductive box or clean conductive box.
Method provided by the invention both had been applicable to the purification of monomer liquid crystal, also was applicable to the purification of mixed liquid crystal.
The following examples will the present invention is further illustrated.
This embodiment is used to illustrate the method for purifying liquid crystal material provided by the invention.
Using vacuum pump is 3.0 * 10 by pressurization with initial electrical resistivity
112 liters of 4-of ohmcm (trans-4 '-propyl group cyclohexyl) benzene cyanogen monomer liquid crystal inject length be 1.5 meters, wide be that 0.5 meter, height are 1000 microns indium tin oxide-coated glass box (production of Nan Bo company), on two conductive glass of this conductive glass box, apply 200 volts volts DS, the injection speed of control monomer liquid crystal is 1 liter/6 hours, exit at this conductive glass box receives the liquid crystal material of purifying, and obtaining 1.99 liters of resistivity is 6.3 * 10
13The liquid crystal material of ohmcm.
Embodiment 2
This embodiment is used to illustrate the method for purifying liquid crystal material provided by the invention.
Using vacuum pump is 4.0 * 10 by pressurization with initial electrical resistivity
122 liters of 4-of ohmcm (trans-4 '-propyl group cyclohexyl) benzene cyanogen monomer liquid crystal inject length be 1.5 meters, wide be that 0.5 meter, height are 1000 microns indium tin oxide-coated glass box (production of Nan Bo company), on two conductive glass of this conductive glass box, apply 280 volts volts DS, the injection speed of control monomer liquid crystal is 0.5 liter/6 hours, exit at this conductive glass box receives the liquid crystal material of purifying, and obtaining 1.99 liters of resistivity is 6.8 * 10
13The liquid crystal material of ohmcm.
This embodiment is used to illustrate the method for purifying liquid crystal material provided by the invention.
Using vacuum pump is 4.0 * 10 by pressurization with initial electrical resistivity
122 liters of 4-of ohmcm (trans-4 '-propyl group cyclohexyl) benzene cyanogen monomer liquid crystal inject length be 1.5 meters, wide be that 0.5 meter, height are 1000 microns indium tin oxide-coated glass box (production of Nan Bo company), on two conductive glass of this conductive glass box, apply 180 volts volts DS, the injection speed of control monomer liquid crystal is 0.8 liter/6 hours, exit at this conductive glass box receives the liquid crystal material of purifying, and obtaining 1.99 liters of resistivity is 6.4 * 10
13The liquid crystal material of ohmcm.
Embodiment 4
This embodiment is used to illustrate the method for purifying liquid crystal material provided by the invention.
Using vacuum pump is 4.0 * 10 by pressurization with initial electrical resistivity
122 liters of mixed liquid crystals of ohmcm inject length be 1.5 meters, wide be that 0.5 meter, height are 1000 microns indium tin oxide-coated glass box (production of Nan Bo company), on two conductive glass of this conductive glass box, apply 200 volts volts DS, the injection speed of control monomer liquid crystal is 0.8 liter/6 hours, exit at this conductive glass box receives the liquid crystal material of purifying, and obtaining 1.99 liters of resistivity is 6.9 * 10
13The liquid crystal material of ohmcm.
Claims (7)
1. the method for a purifying liquid crystal material, it is characterized in that, this method comprises that the liquid crystal material that will be contained in the conductive box of semitight stops in electric field environment, in electric field environment, take out liquid crystal material then, described liquid crystal material is monomer liquid crystal or mixed liquid crystal, described electric field environment is that voltage is the electric field environment of 50-900 volt, and the described residence time is 1-10 hour.
2. method according to claim 1, wherein, described electric field environment is that voltage is the electric field environment of 150-350 volt.
3. method according to claim 1, wherein, the described residence time is 4-7 hour.
4. method according to claim 1, wherein, the thickness of described liquid crystal material is the 50-1000 micron.
5. method according to claim 4, wherein, the thickness of described liquid crystal material is the 100-300 micron.
6. method according to claim 1, wherein, the conductive box of described semitight is the regular hexahedron conductive glass box that comprises liquid crystal material inlet and liquid crystal material outlet, two relative surfaces that area is bigger are conductive surface, other four surfaces are by Surface Insulation, and outlet lays respectively on two relative Surface Insulations the liquid crystal material inlet with liquid crystal material.
7. method according to claim 1, wherein, electric field environment is electrically connected with two conductive surfaces of conductive box respectively by the positive and negative electrode with power supply and obtains.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2006101673305A CN101210183B (en) | 2006-12-27 | 2006-12-27 | Method for purifying liquid crystal material |
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| CN2006101673305A CN101210183B (en) | 2006-12-27 | 2006-12-27 | Method for purifying liquid crystal material |
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| CN101210183A CN101210183A (en) | 2008-07-02 |
| CN101210183B true CN101210183B (en) | 2011-01-26 |
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| CN110922980A (en) * | 2018-09-20 | 2020-03-27 | 江苏和成新材料有限公司 | Purification method of liquid crystal material with fluoroalkoxy as end group |
| CN109438701B (en) * | 2018-09-21 | 2021-06-29 | 深圳市大分子科技有限公司 | Conductive container applied to polyimide purification and electronic grade polyimide product |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2003064364A (en) * | 2001-08-29 | 2003-03-05 | Dainippon Ink & Chem Inc | Liquid crystal material-purifying device and liquid crystal material-purifying method |
| JP2003104947A (en) * | 2001-09-28 | 2003-04-09 | Dainippon Ink & Chem Inc | Method for purifying liquid crystal compound by magnetic field application |
| JP2003166091A (en) * | 2001-11-28 | 2003-06-13 | Dainippon Ink & Chem Inc | Apparatus and method for refining liquid crystal material |
| TW200426204A (en) * | 2003-05-22 | 2004-12-01 | Ind Tech Res Inst | Purification process and device for liquid crystal |
| JP4086812B2 (en) * | 2004-05-31 | 2008-05-14 | Ｔｄｋ株式会社 | Multilayer capacitor |
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2003064364A (en) * | 2001-08-29 | 2003-03-05 | Dainippon Ink & Chem Inc | Liquid crystal material-purifying device and liquid crystal material-purifying method |
| JP2003104947A (en) * | 2001-09-28 | 2003-04-09 | Dainippon Ink & Chem Inc | Method for purifying liquid crystal compound by magnetic field application |
| JP2003166091A (en) * | 2001-11-28 | 2003-06-13 | Dainippon Ink & Chem Inc | Apparatus and method for refining liquid crystal material |
| TW200426204A (en) * | 2003-05-22 | 2004-12-01 | Ind Tech Res Inst | Purification process and device for liquid crystal |
| JP4086812B2 (en) * | 2004-05-31 | 2008-05-14 | Ｔｄｋ株式会社 | Multilayer capacitor |
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