CN101671610B - Detergent composition for removing liquid crystal and cleaning method of liquid crystal panel - Google Patents
Detergent composition for removing liquid crystal and cleaning method of liquid crystal panel Download PDFInfo
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- CN101671610B CN101671610B CN2009101690249A CN200910169024A CN101671610B CN 101671610 B CN101671610 B CN 101671610B CN 2009101690249 A CN2009101690249 A CN 2009101690249A CN 200910169024 A CN200910169024 A CN 200910169024A CN 101671610 B CN101671610 B CN 101671610B
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- liquid crystal
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- water
- cleansing composition
- crystal panel
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D7/00—Compositions of detergents based essentially on non-surface-active compounds
- C11D7/22—Organic compounds
- C11D7/26—Organic compounds containing oxygen
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
- C11D3/16—Organic compounds
- C11D3/20—Organic compounds containing oxygen
Abstract
The present invention provides a detergent composition for removing liquid crystal and a cleaning method of a liquid crystal panel, wherein the detergent composition has high cleaning power to liquid crystal and can reduce the water discharging load to environment. The detergent composition for removing the liquid crystal is characterized by comprising an aromatic compound which is represented by a general formula (1) [in the formula, R<1> represents OCH3 or CH2OCH3, R<2> represents CH3, OCH3 or CH2OCH3]. The cleaning method of the liquid crystal panel is characterized by using the detergent composition for removing liquid crystal. The detergent composition for removing liquid crystal is preferably formed by mixing the aromatic compound represented by the general formula (1) and water.
Description
Technical field
The present invention relates to remove the purging method of liquid crystal with cleansing composition and liquid crystal panel.The application based on September 8th, 2008 spy in japanese publication be willing to 2008-229785 number and on May 25th, 2009 spy in japanese publication be willing to 2009-125163 number, advocate right of priority, quote its content here.
Background technology
Usually it is bonding to be formed with a pair of glass substrate of electrode and oriented film through tackiness agent, stays a part of opening, makes liquid crystal cell; In above-mentioned liquid crystal cell, inject liquid crystal; Seal aforementioned peristome through sealing agent, then, clean; Adhere to deflecting plate respectively at above-mentioned a pair of glass baseplate surface, make liquid crystal panel.
In such manufacturing, owing to the close clearance of relative glass substrate produces space part (narrow), this is difficult to avoided the outside of the binding part between a pair of glass substrate (opposition side of liquid crystal cell side).And when injecting liquid crystal toward liquid crystal cell, liquid crystal is owing to capillary phenomenon gets into, sticks to said narrow.Place the words of liquid crystal attached to aforementioned narrow portion (below be called " liquid crystal spot ") like this; Because the residue of said liquid crystal spot plays a part releasing agent; Probably can involve the generation of following various faults: in manufacturing process thereafter, the binding defective of peeling off, drive (driver) terminal of deflecting plate, peeling off etc. of driving that the interface rippability uncomfortable, that be used for the slimming working method of substrate of underfilling (driver underfill) films.Therefore, the cleaning in the manufacturing of liquid crystal panel need be cleaned with high-cleanness, high and removed above-mentioned liquid crystal spot.
As everybody knows, above-mentioned liquid crystal spot generally is a polarized compounds, and intermolecular interaction is strong, shows high hydrophobicity, and the dispersed or solvability in water solvent is all low.To remove this liquid crystal spot in order cleaning, in the past, to propose a kind of cleansing composition, it contains the hydrocarbon system solvent, specific gathers the hydroxy alkylidene dialkyl ether compounds and by R
11-C
6H
4-C
pH
2p-O-(C
qH
2qO)
rThe aromatic series monocyclic compound that-H representes (referring to patent documentation 1).[in the formula, R
11Expression Wasserstoffatoms, the alkyl of carbonatoms 1～3 or alkenyl, the p of carbonatoms 2 or 3 represent 0 or 1～2 integer, and q representes 2～4 integer, and r representes 0 or 1～4 integer, and r CqH2qO can be identical separately, also can be different.] also propose a kind of liquid crystal panel and use the water system liquid ceanser compositions, it contains the hydrocarbon compound of carbonatoms 8～20, alkylene oxide affixture, the R of specific mid-chain branched primary alconol
12O (AO)
kR
13The alkylene oxide affixture of expression and the water (referring to patent documentation 2) of specified amount.[in the formula, R
12Alkyl, phenyl or the benzyl of expression carbonatoms 1～6, R
13The alkyl of expression Wasserstoffatoms or carbonatoms 1～6, k representes 1～5 number, AO representes the oxyalkylene of carbonatoms 2～4.]
Patent documentation 1: japanese kokai publication hei 10-114899 communique patent documentation 2: Japanese Patent Laid is opened the 2004-2691 communique
Summary of the invention
Yet, in the cleansing composition of patent documentation 1,2 record, also insufficient for the cleaning force of the liquid crystal spot of being adhered on the such close clearance (narrow) of 2～5 μ m between a pair of glass substrate of liquid crystal panel.Again, in the invention of patent documentation 1 record, disclose respectively and directly will be cleaned thing and be immersed in and use in the cleansing composition of aliphatic hydrocarbon as host, and directly will be cleaned in the stoste that thing is immersed in above-mentioned cleansing composition the method for cleaning., state in the use in the method for cleansing composition, because there are the problems such as drainage load height to environment in organic solvents such as a large amount of use aliphatic hydrocarbons.Again; In the cleansing composition of patent documentation 2 records; Though disclose the example of blending ratio below 77 quality % of water; But when the blending ratio of the composition beyond further reducing the dewatering of organic solvent etc. suppresses the drainage load to environment, require further to improve cleaning force for the liquid crystal spot.
The present invention makes in view of above-mentioned situation; Problem is to provide a kind of purging method of removing liquid crystal with cleansing composition and liquid crystal panel; It is high for the cleaning force of liquid crystal spot with cleansing composition that this removes liquid crystal, and can reduce the drainage load to environment.
In order to solve above-mentioned problem, the inventor conscientiously studies, and the result provides following means.That is, the liquid crystal of removing of the present invention is used cleansing composition, it is characterized in that, contains the aromatics of formula (1) expression.
[changing 1]
[in the formula, R
1Expression OCH
3Perhaps CH
2OCH
3, R
2Expression CH
3, OCH
3Perhaps CH
2OCH
3]
The liquid crystal of removing of the present invention it is desirable to mixed by the aromatics and the water of above-mentioned general formula (1) expression with cleansing composition.Again; The liquid crystal of removing of the present invention is used cleansing composition; It is desirable to; Except the aromatics and the water of above-mentioned general formula (1) expression, also further mix the compound, the HLB that are selected from formula (2) expression and form at least a of nonionogenic tenside more than 11 and aprotic polar organic solvent.
[changing 2]
(in the formula, R
3Be alkyl, phenyl or the benzyl of carbonatoms 1～6, n is 0～50 number)
Again, the purging method of liquid crystal panel of the present invention is characterized in that, uses the liquid crystal of removing of the invention described above to use cleansing composition.
The invention effect
The liquid crystal of removing of the present invention is used cleansing composition, and is high for the cleaning force of liquid crystal spot, and can reduce the drainage load to environment.Again, the purging method of liquid crystal panel of the present invention can be removed the liquid crystal spot in the gap (narrow) attached to liquid crystal panel fully, and can reduce the drainage load to environment.
Description of drawings
Fig. 1 shows the liquid crystal panel of the sky before the injection liquid crystal material that uses in the present embodiment, and Fig. 1 (a) is the approximate three-dimensional map that shows liquid crystal panel, and Fig. 1 (b) is from a part of side elevational view of the observed liquid crystal panel of end 1b1 of glass substrate 1b among Fig. 1 (a).Fig. 2 is the photo of the liquid crystal material Restzustand that shows that the gap (narrow) of regulation regional (X among Fig. 1) of the liquid crystal panel corresponding with the metewand of present embodiment is interior.
Embodiment
" remove liquid crystal and use cleansing composition " of the present invention, and to remove liquid crystal be the compsn of the aromatics that contains above-mentioned general formula (1) expression (below, be called (Sa1) composition) with cleansing composition.
<(Sa1) Cheng Fen>In the above-mentioned general formula (1), R
1Expression OCH
3Perhaps CH
2OCH
3R
2Expression CH
3, OCH
3Perhaps CH
2OCH
3R
2Bonding position can be ortho position, a position or contraposition any of phenyl ring, be easy to obtain to consider from cleaning force and the industry that improves better for the liquid crystal spot, it is desirable to contraposition.(Sa1) composition O-methoxy toluene, meta-methoxy toluene are for example arranged for example, to methoxy toluene, 1; 2-dimethoxy benzene, 1; 3-dimethoxy benzene, 1,4-dimethoxy benzene, O-methoxy-alpha-methoxymethyl benzene, meta-methoxy-alpha-methoxymethyl benzene, to methoxyl group-alpha-methoxymethyl benzene, α-methoxyl group o-Xylol, α-methoxyl group m-xylene, α-methoxyl group p-Xylol, O-phthalic diethylene glycol dimethyl ether, isophthalic alcohol dme, terephthaldehyde's diethylene glycol dimethyl ether.
(Sa1) composition is so long as have above-mentioned R
1With above-mentioned R
2Two substituting groups get final product; Wherein, consider that for the cleaning force of liquid crystal spot its solubleness (25 ℃) in water it is desirable to below the 1g/100g aqueous solution from further raising; Better is below the 0.5g/100g aqueous solution, further it is desirable to 0.1～0.5g/100g aqueous solution.
(Sa1) composition can a kind uses separately, also can share more than 2 kinds.The liquid crystal of removing of the present invention is with containing of (Sa1) composition in the cleansing composition of proportional it is desirable to more than 1 quality %, and better is more than 5 quality %.(Sa1) composition contain proportionally more than lower value, further improve for the cleaning force of liquid crystal spot.On the other hand, (Sa1) the proportional higher limit that contains of composition can be 100 quality %, it is desirable to below 90 quality %, and better is below 60 quality %, further it is desirable to below 50 quality %, it is desirable to especially below the 20 quality %.(Sa1) composition contain proportional it is desirable to below 90 quality %, better is below 60 quality %, further it is desirable to below the 50 quality %; Like this; Can further reduce drainage load, it is desirable to the lower concentration below 20 quality % especially, like this environment; Cleaning force can be obtained fully, and drainage load can be reduced further environment for the liquid crystal spot.
The composition liquid crystal of removing of the present invention can contain other compositions outside above-mentioned (Sa1) composition with cleansing composition arbitrarily.Other compositions as beyond (Sa1) composition have for example water, tensio-active agent, organic solvent for example.In addition, in the present invention, the compound of surface tension below 50mN/m when " tensio-active agent " is meant and is diluted to 1 quality % with pure water under 25 ℃.Surface tension is to use tensiometer to use the platinum plate to measure the value that obtains according to the Wilhelmy method.In the present invention, " pure water " is meant through physical treatment or chemical treatment and from water, removes the water behind the impurity.Pure water has for example deionized water or zero(ppm) water etc. for example.
(tensio-active agent) tensio-active agent can use for example nonionogenic tenside, AS, cats product, amphoterics.Wherein, The effect of mixed solution generation gonorrhoea high from the intermiscibility of (Sa1) composition and water, that obtain preventing that under high temperature preservation conditions such as summer (Sa1) composition and water from mixing easily; The aspects such as electrode corrosion that are difficult for taking place to cause owing to the energising to liquid crystal panel are considered, it is desirable to nonionogenic tenside.Wherein, The effect of the litura of the mixed solution that mixes from be improved especially easily (Sa1) composition and water is considered; Better is that HLB is at the nonionogenic tenside more than 11; Further it is desirable to HLB at the nonionogenic tenside more than 12, it is desirable to HLB especially at 14～20 nonionogenic tenside.Particularly, HLB is arranged for example at Voranol EP 2001 more than 11 etc.
In addition, in the present invention, the meaning of " HLB " is wetting ability and the oil loving relative intensity that the molecule of tensio-active agent has, and is meant the value of quantifying its hydrophilic-lipophilic balance.Be the value of trying to achieve through the Griffin method (referring to Jitian, advance in rattan, Da Yuan, the mountain to compile in collaboration with " new edition tensio-active agent handbook ", industrial books Co., Ltd.,, the 234th page in 1991).(Sa1) litura of the material that mixes of composition and water it is desirable to more than 30 ℃, and better is more than 40 ℃.Litura is more than lower value, and the easily preparation that becomes presents the cleansing composition of homogeneous, transparent outward appearance.In the present invention; " litura " is meant the mixing of carrying out the cleansing composition of specified amount 0～30 ℃ TR; After the solution of preparation transparent and homogeneous, above-mentioned solution is housed in the container of regulation, is immersed in the water-bath; The temperature of water-bath is risen, the temperature of the water-bath when above-mentioned solution begins white opacity (℃).The temperature of water-bath can for example be measured through the scale that reads normal thermometer.
(organic solvent) can use polar organic solvent as organic solvent, also can use nonpolarity organic solvent.Wherein, stability (homogeneity, the transparency) consideration of the solution that mixes from intermiscibility, raising (Sa1) composition and the water that improves (Sa1) composition and water it is desirable to use polar organic solvent.
Polar organic solvent can be the protic polar organic solvent, also can be the aprotic polar organic solvent.Wherein, the stability (homogeneity, the transparency) of the solution that mixes from further raising (Sa1) composition and water is considered, it is desirable to the aprotic polar organic solvent especially.
As the aprotic polar organic solvent, for example methyl-sulphoxide (DMSO), N are arranged for example, have Sauerstoffatom (=O) material in dinethylformamide (DMF), acetone, N-Methyl pyrrolidone, the 2-butanone equimolecular; Acetonitrile etc.Wherein,, consider for the cleaning force of liquid crystal spot, it is desirable to intramolecularly and have Sauerstoffatom (=O) material it is desirable to DMSO, DMF, acetone especially, it would be desirable methyl-sulphoxide (DMSO) from further raising as the aprotic polar organic solvent.
As the protic polar organic solvent, the for example monohydroxy-alcohol of carbonatomss 1～4 such as methyl alcohol, ethanol, 1-propyl alcohol, 2-propyl alcohol, 1-butanols, the trimethyl carbinol is arranged for example; The monocarboxylic acid of carbonatomss 1～4 such as acetic acid, formic acid, butyric acid; Glycol ether etc.As glycol ether, for example have for example a side terminal for aliphatic alkyl or aromatic hydrocarbyl and opposite side terminal for the terepthaloyl moietie of Wasserstoffatoms be ether; One side terminal for aliphatic alkyl or aromatic hydrocarbyl and opposite side terminal for the Ucar 35 of Wasserstoffatoms be ether; Both-side ends is the dialkyl group glycol ether of alkyl.Wherein, as the protic polar organic solvent,, it is desirable to the compound of formula (2) expression especially to the cleaning force height of liquid crystal spot, to the low consideration of drainage load of environment.
[changing 3]
(in the formula, R
3Be alkyl, phenyl or the benzyl of carbonatoms 1～6, n is 0～50 number)
In the above-mentioned general formula (2), R
3Alkyl, phenyl or benzyl for carbonatoms 1～6.During n=0, the compound of formula (2) expression is a monohydroxy-alcohol.At this moment, R
3It is desirable to the alkyl of carbonatoms 1～6, better is methyl alcohol, ethanol, 1-propyl alcohol, 2-propyl alcohol, 1-butanols, the trimethyl carbinol, further it is desirable to ethanol.N=1～50 o'clock, the compound of formula (2) expression is that terepthaloyl moietie is ether.At this moment, R
3Alkyl consider from guaranteeing stably to obtain this point easily, it is desirable to carbonatoms 4～6.In above-mentioned formula (2), the stability (homogeneity, the transparency) of the solution that mixes from further raising (Sa1) composition and water considers that n it is desirable to 1～30 number, better is 1～10 number.In addition, the compound of general formula (2) expression is the material that is not included in the tensio-active agent of above-mentioned definition.
As non-polar organic solvent, can use for example paraffin class (12 carbon alkane, tetradecane etc.), olefines chain type hydrocarbon (aliphatic hydrocarbon) such as (dodecylene, tetradecenes etc.); The alicyclic compound of cycloalkane etc. etc.
The liquid crystal of removing of the present invention is used cleansing composition, wherein, from reducing drainage load to environment, can being easy to reason such as non-dangerous goodsization, it is desirable to the material that (Sa1) composition and water mix.In this case, the above-mentioned liquid crystal of removing is with containing of water in the cleansing composition of proportional 10～95 quality % that it is desirable to, and that better is 50～95 quality %, further it is desirable to 80～95 quality %.Containing of water is proportional more than 10 quality %, can further lower the drainage load to environment, again can be with the above-mentioned liquid crystal of removing with the cleansing composition non-dangerous goodsization.And below 95 quality %, can obtain and (Sa1) combined balance system between the composition, further improve cleaning force for the liquid crystal spot.Water is had no particular limits, can use for example zero(ppm) water, ion exchanged water, city's water.
In the above-mentioned solution that (Sa1) composition and water are mixed; Use cleansing composition as the liquid crystal of removing of the present invention; Present homogeneous and the transparent excellent solution consideration of outward appearance, stability of solution (homogeneity, the transparency) from preparing; It is desirable to; Except above-mentioned (Sa1) composition and water, also further mix the material that the compound that is selected from above-mentioned general formula (2) expression, HLB form at least a (below, with above-mentioned a kind of being called " (S2) composition ") of nonionogenic tenside more than 11 and aprotic polar organic solvent.Below, sometimes with such remove liquid crystal with cleansing composition, be about to (Sa1) composition, water and (S2) material that mixes of composition be called the clear solution of water " (Sa1)-".
(Sa1) composition in the clear solution of water " (Sa1)-" contain proportional 5～70 quality % that it is desirable to, that better is 20～70 quality %.(Sa1) composition contain proportionally more than lower value, further improve for the cleaning force of liquid crystal spot.Below higher limit, can further reduce drainage load to environment.And the liquid stability (homogeneity, the transparency) of above-mentioned clear solution further improves.(Sa1) composition can a kind uses separately, also can share more than 2 kinds.
Water in the clear solution of water " (Sa1)-" contain proportional it is desirable to more than 10 quality %, that better is 10～50 quality %.Containing of water is proportional more than lower value, can be with above-mentioned clear solution non-dangerous goodsization.
(S2) composition in the clear solution of water " (Sa1)-" contain proportional 10～70 quality % that it is desirable to, that better is 30～60 quality %.(S2) composition contain proportionally more than lower value, the stability of solution of above-mentioned clear solution (homogeneity, the transparency) further improves.Below higher limit, further improve for the cleaning force of liquid crystal spot.(S2) composition can use separately a kind of, also can and with more than 2 kinds.Through using (S2) composition, (Sa1) intermiscibility of composition and water improves.And (S2) composition uses HLB at the nonionogenic tenside more than 11, and the litura of above-mentioned clear solution uprises, and further is prevented the effect that under the high temperature preservation condition, produces gonorrhoea.Again, (S2) composition uses the aprotic polar organic solvent, further improves for the cleaning force of liquid crystal spot.
About (Sa1) composition and (S2) blending ratio of composition [(Sa1)/(S2)]; (S2) composition uses HLB when the nonionogenic tenside more than 11; It is desirable to, mass ratio (Sa1)/(HLB is at the nonionogenic tenside more than 11)=0.1～10, better is 0.1～6.When (S2) composition uses the aprotic polar organic solvent, it is desirable to mass ratio and be (Sa1)/(aprotic polar organic solvent)=0.1～10, better is 0.1～9.When (S2) composition uses the compound of above-mentioned general formula (2) expression, it is desirable to mass ratio and be (Sa1)/(compound of general formula (2) expression)=0.5～10, better is 1～6.Which kind of situation no matter, all more than the lower value of (Sa1)/(S2), cleaning improves.Below the higher limit of (Sa1)/(S2), the stability of solution of cleansing composition (homogeneity, the transparency) improves.
PH to the clear solution of water " (Sa1)-" does not have special qualification, it is desirable to 25 ℃ of following pH and be about 2～10 scope.The scope of the pH of above-mentioned clear solution about 2～10, liquid crystal panel are difficult for corroding.In the present invention; Removing liquid crystal is meant with the pH of cleansing composition; With cleansing composition temperature adjustment to 25 ℃, use glass electrode formula pH meter (ProductName: HM-30G, East Asia デ イ one ケ one ケ one manufactured); With the glass electrode direct impregnation in above-mentioned cleansing composition, through the value of the pH that shown after 1 minute.
Viscosity to the clear solution of water " (Sa1)-" does not have special qualification, it is desirable to below 25 ℃ of following 15mPas.The viscosity of above-mentioned clear solution further improves for the cleaning force of liquid crystal spot below higher limit.And, can further reduce drainage load to environment.In the present invention, remove liquid crystal and be meant, use DV-I+VISCOMETER (ProductName with the viscosity of cleansing composition; The BROOKFIELD manufactured); Use rotor No.2, under 60rpm, condition determination after 60 seconds, measure the cleansing composition of temperature adjustment to 25 ℃ and the value that obtains.
Again, the liquid crystal of removing of the present invention it is desirable to be made up of the organic solvent composition that contains (Sa1) composition with cleansing composition.At this moment, in above-mentioned organic solvent composition, it is proportional more than 20 quality % to it is desirable to containing of (Sa1) composition, and better is more than 50 quality %, also can be 100 quality %, it is desirable to 100 quality % especially.Containing of above-mentioned aromatics is proportional more than lower value, further improves for the cleaning force of liquid crystal spot.As other compositions except that (Sa1) composition that can be included in the above-mentioned organic solvent composition, for example paraffin class (12 carbon alkane, n-tetradecane), olefines chain type hydrocarbon (aliphatic hydrocarbon) such as (dodecylene, tetradecenes etc.) are arranged for example; The ester ring type compound of naphthenic hydrocarbon etc.; Protic polar organic solvent, the aprotic polar organic solvent of above-mentioned monohydroxy-alcohol, monocarboxylic acid or glycol ether etc.; (Sa1) aromatics outside the composition etc.
The liquid crystal of removing of the present invention is used cleansing composition; For example; After any composition of (Sa1) composition and water etc. put into same containers; Carry out certain stirring, can prepare (Sa1) composition and be dispersed in dispersion liquid or emulsion in any composition, perhaps (Sa1) composition and the solution of composition arbitrarily (for example, above-mentioned the clear solution of water " (Sa1)-" etc.).Also can any composition of above-mentioned organic solvent composition that contains (Sa1) composition and water etc. be mixed, prepare again.
Again, of the present invention when removing liquid crystal and being used to remove the liquid crystal spot with cleansing composition, can be directly use above-mentioned cleansing composition with the state of stoste, also can mix use with other compositions.Also can use like the back above-mentioned cleansing composition of described dilute with water.
The liquid crystal of removing of the present invention according to above explanation is used cleansing composition, can obtain the high such effect of cleaning force for the liquid crystal spot.The reason that can access this effect is also uncertain, and supposition is owing to be used for the liquid crystal of removing of the present invention with the aromatics ((Sa1) composition) of above-mentioned general formula (1) expression of cleansing composition and the intermiscibility height of liquid crystal spot.Research through the inventor; Confirm: for example, be attached to the liquid crystal spot in the gap (narrow) of liquid crystal panel, with respect to the moment dissolving of (Sa1) composition; Than previously used chain type hydrocarbon (aliphatic hydrocarbon) or ester ring type compound, the liquid crystal spot is high with the intermiscibility of (Sa1) composition.We think that this is that (Sa1) composition and liquid crystal spot get the affinity raising owing between the contained aromatics of (Sa1) composition and liquid crystal spot, have an effect each other through πDian Zi.Confirm again: compared with the situation of using the aromatics outside (Sa1) composition, when using (Sa1) composition, especially mix use with water, higher for the cleaning force of liquid crystal spot.We think this be since (Sa1) composition have 2 specific substituting group (R
1, R
2), and show a little solvability for water.
The solubleness (25 ℃) of aromatics (organic solvent) in water that the embodiment that states after in table 1, showing uses.In addition; In table 1; The ※ 1 expression MSDS of manufacturers; ※ 2 expression STN REGISTRY files (physical data (calculated value) that data are to use special-purpose software to obtain), ※ 3 expression independent administrative corporation product evaluation basic technology mechanism (nite) homepages, ※ 4 expressions are respectively based on the solubleness in water of solvent handbook (talk society).
Table 1
| Aromatics | Solubleness in the water (25 ℃) (the g/100g aqueous solution) |
| The terephthalyl alcohol dimethyl ether | 0.16 ※ 1 |
| α-methoxyl group p-Xylol | 0.29 ※ 2 |
| 1, the 2-dimethoxy benzene | 0.32 ※ 2 |
| 1, the 4-dimethoxy benzene | 0.29 ※ 2 |
| P-Xylol | 0.02 ※ 3 |
| Toluene | 0.05 ※ 3 |
| Phenylmethylether | 0.19 ※ 3 |
| Phenylcarbinol | 3.8 ※ 4 |
| Benzoglycols | 2.7 ※ 1 |
From table 1; The solubleness of the aromatics that the present invention relates to (terephthaldehyde's diethylene glycol dimethyl ether, α-methoxyl group-p-Xylol, 1,2-dimethoxy benzene, 1,4-dimethoxy benzene) in water is 0.16～0.32g/100g aqueous solution; With respect to water, show a little solvability.And p-Xylol, toluene show solvability hardly with respect to water; The solubleness of phenylcarbinol (compound that the aromatic series monocyclic compound of above-mentioned patent documentation 1 record is comprised) in water surpasses the 1g/100g aqueous solution, and is than the aromatics that the present invention relates to, high with respect to the solubleness of water.Through the inventor's research, confirm: the solubleness of use in water surpasses the aromatics of the 1g/100g aqueous solution, is difficult to obtain the effect for the cleaning force raising of liquid crystal spot.We think that this is because a little less than the adsorptivity of aromatics for the liquid crystal spot.Phenylmethylether (anisole) and the solubleness of aromatics in water that the present invention relates to are same degree, but the substituting group (OCH of phenylmethylether
3) be one, different with the aromatics that the present invention relates to.
Again, the liquid crystal of removing according to the present invention is used cleansing composition, can obtain reducing to the such effect of the drainage load of environment.The reason that obtains this effect is inferred as follows.Of the present invention remove liquid crystal with cleansing composition in, (Sa1) composition is high for the cleaning force of liquid crystal spot, and the concentration of (Sa1) composition is reduced.Again, (Sa1) composition can mix use with water, and it is not meet chemical substance to discharge amount of movement report (PRTR) system, the law of labour safety and health (Lao Anfa), poisonous substance and violent in toxicity and ban in the method (hypertoxic method) arbitrary material.Therefore, we think that of the present invention to remove liquid crystal low to the drainage load of environment with cleansing composition.In addition, YLENE and toluene meet arbitrary method in PRTR, Lao Anfa, the hypertoxic method, and phenylmethylether meets Lao Anfa.Phenylcarbinol and the benzoglycols (" R of above-mentioned patent documentation 2 records
12O (AO)
kR
13" aromatics that comprised) be the material that does not meet arbitrary method in PRTR, Lao Anfa, the hypertoxic method.
Again; According to cleansing composition of the present invention; When cleaning, owing to can dilute use for water, so even (Sa1) composition in the stoste of above-mentioned cleansing composition is a high density; Also can when cleaning, make (Sa1) composition through dilution is lower concentration, reduces the drainage load to environment.Further, also can carry out easy oily water separation film in room temperature and handle (example: Asahi Chemical Industry's fiber company is made ユ one テ Star Network FS pattern TH), can further reduce drainage load environment even become the scavenging solution of lower concentration through dilution.On the other hand, contain with high density (Sa1) composition cleansing composition the stoste sorrow since can realize carrying the time number of containers of dwindling of container dimensional reduce, so trucking costs cut down, favourable at economic aspect.And; Especially; According to (Sa1) composition, water and (S2) cleansing composition that mixes of composition; Present homogeneous and transparent outward appearance, can prepare the excellent stoste of stability of solution (homogeneity, the transparency), and can obtain to realize that as stoste the liquid crystal of removing of non-dangerous goodsization uses cleansing composition.Again, the amount of the blended of cleansing composition (Sa1) composition own also can reduce, and further reduces the drainage load to environment, simultaneously, also can obtain the excellent cleaning effect for the liquid crystal spot.
The liquid crystal of removing of the present invention is the suitable cleansing composition that is used as the scavenging solution crystal panel with cleansing composition.The aromatics of above-mentioned general formula used in the present invention (1) expression is a handy material in industry.Main application as above-mentioned aromatics; The organic synthesis raw material that the midbody of resin or the midbody of pharmaceuticals etc. are arranged for example; Purposes before these are with of the present invention to remove liquid crystal different fully with such purposes, of the present inventionly remove liquid crystal provides above-mentioned aromatics with cleansing composition new purposes.
The purging method of " purging method of liquid crystal panel " liquid crystal panel of the present invention is to use the method for liquid crystal with cleansing composition of removing of the invention described above.Purging method to liquid crystal panel of the present invention does not have special qualification, for example can carry out as follows.That is, stir of the present inventionly when removing liquid crystal, liquid crystal panel is flooded specific time (matting) with cleansing composition.The above-mentioned liquid crystal of removing is used cleansing composition, and the material that for example can use in advance any composition with (Sa1) composition and water etc. to mix also can use (Sa1) composition and composition arbitrarily, remix when cleaning respectively.Also can use the organic solvent composition that contains (Sa1) composition to replace above-mentioned (Sa1) composition again.Wherein, it is desirable to the above-mentioned liquid crystal of removing of dilute with water and use with cleansing composition, better is with the water dilution of 2～20 times amount, use.At this moment, use cleansing composition, it is desirable to use above-mentioned the clear solution of water " (Sa1)-" as the above-mentioned liquid crystal of removing.As the method for above-mentioned dilution, it is desirable to use the above-mentioned water of removing liquid crystal with 2～20 times of amounts of cleansing composition, the better water that is to use 2～15 times of amounts.Dilute the above-mentioned liquid crystal of removing with cleansing composition with the above water of doubling dose, can remove the liquid crystal spot in gap (narrow) fully, and can further reduce drainage load environment attached to liquid crystal panel.With cleansing composition, can use (Sa1) composition of lower concentration to remove the liquid crystal spot fully with the above-mentioned liquid crystal of removing of the dilution of the water below 20 times of amounts.
Then, from above-mentioned cleansing composition, take out liquid crystal panel, be immersed in (flushing operation) in the water.Then, from water, take out liquid crystal panel, use drying machine etc. carries out drying (drying process).In addition, in matting or flushing operation, can carry out ultrasonication.Carry out ultrasonication, because can the short period of time and remove the liquid crystal spot in the gap (narrow) that is attached to liquid crystal panel better, thereby desirable.Again, the purging method of liquid crystal panel of the present invention also has from nozzle etc. directly the liquid crystal of removing of the present invention to be sprayed on cleansing composition that to be cleaned thing be the method on the liquid crystal panel, then wiped etc. except above-mentioned purging method for example.According to the purging method of the liquid crystal panel of the present invention of above explanation, can remove the liquid crystal spot in gap (narrow) fully, and can reduce drainage load environment attached to liquid crystal panel.
Embodiment
Below, the present invention will be described in more detail to use embodiment, but these examples be not limit of the present invention.
The organic solvent that uses in the present embodiment [source] is described below.The structure that shows them below in the lump.
Terephthaldehyde's diethylene glycol dimethyl ether [イ Ha ラ ニ Star ケ イ chemical industry (manufacturing)].α-methoxyl group p-Xylol [イ Ha ラ ニ Star ケ イ chemical industry (manufacturing)].1,2-dimethoxy benzene [Tokyo changes into industry (manufacturing)].1,4-dimethoxy benzene [Tokyo changes into industry (manufacturing)].P-Xylol [pure chemistry (manufacturing)].Toluene [Northeast chemistry (manufacturing)].Phenylmethylether [Northeast chemistry (manufacturing)].Phenylcarbinol [Northeast chemistry (manufacturing)].Benzoglycols [Japanese emulsifying agent (manufacturing)].Hexanaphthene [pure chemistry (manufacturing)].1-dodecylene [the emerging product of bright dipping (manufacturing)].Positive 12 carbon alkane [Japan energy manufacturing)].
[changing 4]
terephthaldehyde's diethylene glycol dimethyl ether α-methoxyl group p-Xylol
1; 2-dimethoxy benzene 1, the 4-dimethoxy benzene
[Of 5]
paraxylene toluene anisole
benzyl alcohol benzene glycol
[Of 6]
cyclohexane 1 - dodecene
n-dodecane
< for the evaluation (1) of the cleaning force of liquid crystal spot>is according to as follows 1)～6) order, carry out evaluation for the cleaning force of liquid crystal spot.1) makes liquid crystal panel, use syringe to inject the liquid crystal material that the TFT liquid crystal panel is used in the gap of above-mentioned liquid crystal panel (narrow).The liquid crystal panel of the preflood sky of liquid crystal material that uses at present embodiment is presented among Fig. 1.
Fig. 1 (a) is the overview stereographic map that shows liquid crystal panel, and Fig. 1 (b) is the part side elevational view of the observed liquid crystal panel of end 1b1 side of the glass substrate 1b from Fig. 1 (a).The liquid crystal panel 10 that Fig. 1 (a) shows is made as follows, and it is bonding with a pair of glass substrate 1a, 1b by binding part 2 to be situated between through sticker, leaves peristome (not shown), makes liquid crystal cell 3 (display part), seals above-mentioned peristome with sealing agent.Be formed with electrode 6 on the liquid crystal panel 10.The liquid crystal panel 10 of made, shown in Fig. 1 (b), the distance (depth of space part 4) from the end 1a1 of glass substrate 1a to binding part 2 is 300 μ m, the distance between glass substrate 1a, 1b is 3 μ m.And; The liquid crystal panel 10 (2 inches sizes) of liquid crystal material (not shown) is injected in use in narrow gap (narrow); Carry out following 2) later operation; The outside of this binding part 2 of narrow gap (narrow) between a pair of glass substrate 1a, 1b (opposition sides of liquid crystal cell 3 sides) forms through relative glass substrate 1a, 1b and binding part 2.In addition, what the scope of being surrounded by X among Fig. 1 showed is, following 6) operation in estimate the zone of liquid crystal material Restzustand.
2) will put into the 100ml beaker by mixing each routine clean-out system combination room 20g that above-mentioned each organic solvent 2g and ion exchanged water 18g form respectively; One side is with the whisking appliance continuously stirring (600rpm) of long 2cm; One side is immersed in the stoste of cleansing composition at 60 ℃ of liquid crystal panels that will in gap (narrow), be injected with liquid crystal material down, floods 5 minutes.3) take out liquid crystal panel, clean each face, 5 seconds of each face with ion exchanged water.4) in the 100ml beaker, put into ion exchanged water 50g,, flood 10 minutes (flushing operation) 60 ℃ of following steeping fluid crystal panel.5) take out liquid crystal panel, 100 ℃ drying machine inner dryings 10 minutes.6) through polarizing microscope, the Restzustand of the liquid crystal material in the gap (narrow) in the regulation of the visual observation liquid crystal panel zone (X among Fig. 1) according to following metewand (qualified: more than 4 minutes), is estimated the cleaning force for the liquid crystal spot.The result is shown in the table 2.(metewand) 5 minutes: liquid crystal material is cleaned fully and removes.4 minutes: residual had few liquid crystal material.3 minutes: residual everywhere had a liquid crystal material.2 minutes: residual had a blocky liquid crystal material.1 minute: residual had a liquid crystal material over half.Restzustand corresponding to the liquid crystal material in the gap (narrow) in the regulation zone above-mentioned metewand, liquid crystal panel (X among Fig. 1) is shown among Fig. 2.Among Fig. 2, symbol 5 expression liquid crystal materials, symbol 1a and 1b represent glass substrate, symbol 2 expression binding parts.
[table 2]
| Organic solvent | Cleaning force to the liquid crystal spot | |
| Embodiment 1 | The terephthalyl alcohol dimethyl ether | 4.5 |
| Embodiment | ||
| 2 | α-methoxyl group-p-Xylol | 4 |
| Embodiment | ||
| 3 | 1, the 2-dimethoxy benzene | 4 minutes |
| Embodiment 4 | 1, the 4- | 5 minutes |
| Comparative example 1 | P- | 3 minutes |
| Comparative example 2 | | 3 minutes |
| Comparative example 3 | | 3 minutes |
| Comparative example 4 | | 2 minutes |
| Comparative example 5 | | 2 minutes |
| Comparative example 6 | Hexanaphthene | 1 minute |
| Comparative example 7 | The 1-dodecylene | 1 minute |
| Comparative example 8 | Positive 12 carbon alkane | 1 minute |
Can know from the result of table 2, can confirm to use the cleaning force to the liquid crystal spot of cleansing composition of embodiment 1～4 of the aromatics that the present invention relates to higher than the cleansing composition of comparative example 1～8.Again; The aromatics of the cleansing composition of embodiment 1～4 (organic solvent) concentration is low; Be 10 quality %; And above-mentioned aromatics (organic solvent) all is the material that does not meet arbitrary method in PRTR, Lao Anfa, the hypertoxic method, so the cleansing composition of embodiment 1～4 is the compsn low to the drainage load of environment.
< preparation of cleansing composition>(embodiment 5～19, comparative example 9) through mixing each composition according to well-established law, prepares each routine cleansing composition according to the composition of table 3～4 expressions.The unit of the combined amount in the table is that the total mass with cleansing composition is the quality % of benchmark, representes the pure composition conversion amount of each composition.The composition that shows in the following his-and-hers watches describes.
Aromatics (Sa1) PXDM of [explanation of the composition that shows in the table] general formula (1) expression: terephthaldehyde's diethylene glycol dimethyl ether [イ Ha ラ ニ Star ケ イ chemical industry (manufacturing)].
(Sa1) [following table is shown " (Sa1 ') composition " 12 carbon alkane to the comparison composition of composition: positive 12 carbon alkane [Japan energy manufacturing)].
Water: ion exchanged water
Be selected from the compound, HLB of general formula (2) expression at least a (S2) at nonionogenic tenside more than 11 and aprotic polar organic solvent.
(compound of general formula (2) expression) C4E3: the R in the general formula (2)
3It for butyl, n 3 triethylene glycol single-butyl ether.Trade(brand)name: Block チ セ ロ one Le 30, the manufacturing of consonance fermentation chemistry.C6E8: the R in the general formula (2)
3For hexyl, n 8 eight ethylene glycol mono hexyl ether.Ph-G EO3 mole: the R in the general formula (2)
3It for phenyl, n 3 triethylene glycol list phenyl ether.Trade(brand)name: benzoglycols-30 (PhG-30), Japanese emulsifying agent manufacturing.Ethanol: the R in the general formula (2)
3It for ethyl, n 0 monohydroxy-alcohol.Northeast chemistry is made; The protic polar organic solvent.
(HLB is the non-ionic surfactant more than 11) C10E14 (HLB=15.9): the carbonatoms of alkyl be 10 and the repeat number (the average addition mole number of ethylene oxide) of ethenoxy group be polyxyethylated (branching decyl) ether of 14.Trade(brand)name: ノ イ ゲ Application XL-140, the first industrial pharmacy manufacturing.C8E20 (HLB=17.4): the carbonatoms of alkyl be 8 and the repeat number (the average addition mole number of ethylene oxide) of ethenoxy group be polyxyethylated (2-ethylhexyl) ether of 20.Trade(brand)name: ニ ユ one コ one Le 1020, Japanese emulsifying agent manufacturing.C10E5 (HLB=11.6): the carbonatoms of alkyl be 10 and the repeat number (the average addition mole number of ethylene oxide) of ethenoxy group be polyxyethylated (branching decyl) ether of 5.Trade(brand)name: ノ イ ゲ Application XL-50, the first industrial pharmacy manufacturing.
(aprotic polar organic solvent) DMSO: methyl-sulfoxide, eastern レ Off ア イ Application ケ ミ カ Le is made.DMF:N, dinethylformamide, Northeast chemistry is made.Acetone: Northeast chemistry is made.
(S2) the comparison composition of composition [following table is shown " (S2 ') composition "] C10E4 (HLB=10.5): the carbonatoms of alkyl be 10 and the repeat number (the average addition mole number of ethylene oxide) of ethenoxy group be polyxyethylated (branching decyl) ether of 4.Trade(brand)name: ノ イ ゲ Application XL-40, the first industrial pharmacy manufacturing.
The cleansing composition 10g that < evaluation of stability of solution>[evaluation of outward appearance] will just prepare according to the composition of table 3～4 expressions puts into the tight 10ml bottle of plug respectively, and under room temperature (20 ℃), the outward appearance after 1 day is left standstill in visual observation.Its outward appearance is that the note of transparent and homogeneous does zero, be that the note of gonorrhoea～two layer isolating state is done *.Its result is shown in the table 3,4.What said here " gonorrhoea " represented is that aqueous solution integral body is in the milkiness state.What " two separate " represented is to separate into oil reservoir and water layer.
[mensuration of litura] is for each routine cleansing composition; Under 15～25 ℃, carry out the mixing of cleansing composition; Behind the solution of preparation transparent and homogeneous, above-mentioned solution 20g is housed in the glass test tube of 30ml, is immersed in the water-bath; Speed with 1 ℃/minute makes warming-in-water, the temperature of the solution when measuring above-mentioned solution and begin gonorrhoea through the scale that reads normal thermometer (℃).Its result is shown in the table 3,4.
< for the evaluation (2) of the cleaning force of liquid crystal spot>is according to as follows 1)～7) order, carry out evaluation to the cleaning force of liquid crystal spot.1) the same with above-mentioned evaluation (1), make liquid crystal panel shown in Figure 1, use syringe to inject the TFT liquid crystal panel in the gap of above-mentioned liquid crystal panel (narrow) and use liquid crystal material.
2) in the 100ml beaker, put into each routine cleansing composition 20g, dilute above-mentioned cleansing composition respectively, prepare 20 quality % aqueous solution 100g with ion exchanged water 80g (water of 4 times of amounts of above-mentioned cleansing composition).And, after stopping at last stirring, the outward appearance of the 20 quality % aqueous solution of visual observation after through 10 seconds.Its result is shown in the table 3,4.In the table, what " gonorrhoea " represented is the state that aqueous solution integral body is in milkiness.What " two separate " represented is to separate into oil reservoir and water layer.
3) 20 quality % aqueous solution 20g with each example put into the 100ml beaker respectively; Use the whisking appliance of long 2cm; One side continuously stirring (600rpm), one side will be injected with liquid crystal material in gap (narrow) liquid crystal panel is immersed under 45 ℃ in the above-mentioned 20 quality % aqueous solution, floods 15 minutes.4) take out liquid crystal panel, clean each face with ion exchanged water, each face cleaned for 5 seconds.5) in the 100ml beaker, put into ion exchanged water 50g, in 45 ℃ of following steeping fluid crystal panel 10 minutes (flushing operation).6) take out liquid crystal panel, 100 ℃ drying machine inner dryings 10 minutes.7) pass through polarizing microscope; The remaining state of the liquid crystal material in the gap (narrow) in the regulation zone (X among Fig. 1) of visual observation liquid crystal panel; According to the metewand the same (qualified: more than 4 minutes), estimate cleaning force for the liquid crystal spot with above-mentioned evaluation (1).Its result is shown in the table 3,4.
[table 3]
[table 4]
Can confirm that from the result of table 3～4 any one outward appearance of the cleansing composition of embodiment 5～18 all is a transparent and homogeneous, and high for the cleaning force of liquid crystal spot.Again, can confirm also that any one litura of the cleansing composition of embodiment 5～18 is all more than 30 ℃.Can confirm, use in the cleansing composition of embodiment 19 of (S2 ') composition different, can not get for the high effect of the cleaning force of liquid crystal spot or the outward appearance of transparent and homogeneous with (S2) composition.On the other hand, can confirm also that use in the cleansing composition of comparative example 9 of the 12 carbon alkane different with (Sa1) composition, its cleaning force for the liquid crystal spot is low, can not get the outward appearance of transparent and homogeneous.Therefore, can confirm, with (Sa1) composition, water and (S2) cleansing composition that mixes of composition present homogeneous and transparent outward appearance, its solution liquid stability (homogeneity, the transparency) excellence.And, also can confirm, because can dilute with water and use (Sa1) composition with lower concentration, therefore can reduce drainage load to environment, and high for the cleaning force of liquid crystal spot.
Again, in this evaluation (2), during the scavenging solution crystal panel, 20 quality % aqueous solution gonorrhoeas of the cleansing composition of embodiment 5～19.Contact with liquid crystal panel through the aqueous solution that makes such gonorrhoea and to clean, also can confirm in cleansing composition of the present invention and purging method, can obtain excellent cleaning effect for the liquid crystal spot.In addition, also can confirm, in the flushing operation, can easily the 20 quality % aqueous solution of gonorrhoea be removed from liquid crystal panel.
Utilizability on the industry
It is high and can reduce the liquid crystal of removing of the drainage load of environment is used cleansing composition for the cleaning force of liquid crystal spot that the present invention can provide; And the purging method that a kind of liquid crystal panel is provided; This method can be removed the liquid crystal spot in the gap (narrow) attached to liquid crystal panel fully, and can reduce the drainage load to environment.
Nomenclature
Claims (4)
1. remove liquid crystal and use cleansing composition for one kind, it is characterized in that, contain terephthaldehyde's diethylene glycol dimethyl ether.
2. as claimed in claim 1ly remove liquid crystal and use cleansing composition, it is characterized in that, also contain water.
3. as claimed in claim 2ly remove liquid crystal and use cleansing composition, also be mixed with the compound, the HLB that are selected from general formula (2) expression and constitute at least a of nonionogenic tenside more than 11 and aprotic polar organic solvent,
[changing 2]
In the formula, R
3Be alkyl, phenyl or the benzyl of carbonatoms 1～6, n is 0～50 number.
4. the purging method of a liquid crystal panel is characterized in that, uses each the described liquid crystal of removing in the claim 1～3 to use cleansing composition.
Applications Claiming Priority (6)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2008229785 | 2008-09-08 | ||
| JP2008229785 | 2008-09-08 | ||
| JP2008-229785 | 2008-09-08 | ||
| JP2009125163A JP5346686B2 (en) | 2008-09-08 | 2009-05-25 | Liquid crystal removal detergent composition and liquid crystal panel cleaning method |
| JP2009-125163 | 2009-05-25 | ||
| JP2009125163 | 2009-05-25 |
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| Publication Number | Publication Date |
|---|---|
| CN101671610A CN101671610A (en) | 2010-03-17 |
| CN101671610B true CN101671610B (en) | 2012-10-31 |
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|---|---|---|---|
| CN2009101690249A Expired - Fee Related CN101671610B (en) | 2008-09-08 | 2009-09-07 | Detergent composition for removing liquid crystal and cleaning method of liquid crystal panel |
Country Status (2)
| Country | Link |
|---|---|
| KR (1) | KR20100029703A (en) |
| CN (1) | CN101671610B (en) |
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| EP2666550A4 (en) * | 2011-01-18 | 2014-10-29 | Denki Kagaku Kogyo Kk | Ultrasonic cleaning method and apparatus |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1179169A (en) * | 1995-03-24 | 1998-04-15 | 罗纳·布朗克化学公司 | Cleaning and/or stripping copostion based on dibasic acid esters and ether as main components |
| US5789359A (en) * | 1993-05-17 | 1998-08-04 | Kabushiki Kaisha Toshiba | Detergent, method of cleaning, and apparatus for cleaning |
-
2009
- 2009-09-03 KR KR1020090082958A patent/KR20100029703A/en not_active Application Discontinuation
- 2009-09-07 CN CN2009101690249A patent/CN101671610B/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5789359A (en) * | 1993-05-17 | 1998-08-04 | Kabushiki Kaisha Toshiba | Detergent, method of cleaning, and apparatus for cleaning |
| CN1179169A (en) * | 1995-03-24 | 1998-04-15 | 罗纳·布朗克化学公司 | Cleaning and/or stripping copostion based on dibasic acid esters and ether as main components |
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| Publication number | Publication date |
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| CN101671610A (en) | 2010-03-17 |
| KR20100029703A (en) | 2010-03-17 |
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