CN100370287C - Method for instant monitoring dyeing solution composition change for polarized light plate process - Google Patents
Method for instant monitoring dyeing solution composition change for polarized light plate process Download PDFInfo
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- CN100370287C CN100370287C CNB2005100059805A CN200510005980A CN100370287C CN 100370287 C CN100370287 C CN 100370287C CN B2005100059805 A CNB2005100059805 A CN B2005100059805A CN 200510005980 A CN200510005980 A CN 200510005980A CN 100370287 C CN100370287 C CN 100370287C
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Abstract
The present invention provides a method for instantly monitoring the change of the composition of dyeing solution in the production process of a polarization plate, wherein the change of a reduction reaction of the dyeing solution is detected and the composition of the dyeing solution is analyzed by an ion chromatograph, and the concentration of the dyeing solution is measured by an ion concentration analyzer. The present invention can be used for instantly controlling the consumption of iodine ions in the production process and the time to replacing the dyeing solution, and controlling the content of the iodine ions in the polarization plate.
Description
Technical field
The method of monitoring program parameter when the present invention makes relevant for a kind of Polarizer, but the method that particularly changes relevant for staining solution constituent in a kind of immediately monitoring Polarizer processing procedure.
Background technology
Polarizer (Polarizing Sheet) or be called light polarizing film (Polarizing Film), generally have and be transformed into the function of polar biased light with not having a natural light of deflection polarity, the light that Polarizer can produce polarization depends primarily on the polarisation material that dyes on Polarizer.Generally speaking, the iodine light polarizing film that adopt in the application of LCD more, when LCD does not add Polarizer, light can free in and out liquid crystal groove, be not subjected to the influence of extra electric field, but after the levels of liquid crystal groove respectively adds Polarizer, seeing through of light controlled with regard to available extra electric field, the feasible variation that visually can experience light and shade, hence one can see that, the function of Polarizer is promptly transferring non-polarization light to polar biased light, and LCD is exactly to utilize this polar biased light to add that the liquid crystal torque characteristic reaches whether passing through of control light, and causes the effect of display light and shade.
Light polarizing film roughly can be divided into absorption and reflective two kinds of forms, and wherein absorption light polarizing film can be divided into O type, E type, metal gate type, iodine and dyestuff light polarizing film again.And dyestuff (DyeType Polarizing Film) and iodine light polarizing film (Iodine Type Polarizing Film) are utilized iodide ion (I
3 -And I
5 -) or dye molecule diffusion infiltrate in the macromolecule membrane layer, polyvinyl alcohol (PVA) (Polyvinyl Alcohol for example, PVA) thin layer, in this macromolecule membrane layer, do the arrangement of systematicness by iodide ion or dye molecule, therefore, can absorb the light component that is parallel to its orientation, and only allow the light component of vertical direction pass through, and produce one and have the light polarizing film of polar biased light characteristic.The light polarizing film that general Thin Film Transistor-LCD (TFT-LCD) uses is promptly used dyestuff or iodine light polarizing film; extending into tens of millimeter (millimeter; mm) upper and lower sides of thick polyvinyl alcohol film layer pastes a protective seam respectively again; triacetate fiber (triacetyl-cellulose for example; TAC) thin layer; therefore, polyvinyl alcohol (PVA) and triacetate fiber thin layer can constitute the light polarizing film structure of a similar sandwich structure.
Generally speaking in Polarizer, the iodide ion in iodine and the potassium iodide can form the wrong ion (I of brown triiodo
2+ I
-→ I
3 -), and the wrong ion of iodine can be used reductive agent, for example sodium thiosulfate (SodiumThiosuflate, Na
2S
2O
3) or Vitamin C produce reduction reaction and be reduced into colourless iodide ion.Because Polarizer is a main material with iodine and potassium iodide mainly, yet in the process of Polarizer dyeing, the content and the concentration of the wrong ion of iodine are occupied epochmaking role, therefore, the content of the wrong ion of the iodine after carrying out reduction and concentration thereof can influence the effect of Polarizer dyeing.In view of the above, demand urgently providing a kind of can at-once monitor Polarizer processing procedure in the method for the wrong ion concentration of iodine and content, to help the more effectively processing procedure of management and control Polarizer and the use of saving soup.
Summary of the invention
According to aforesaid demand, a purpose of the present invention is for providing a kind of method that the staining solution constituent changes in the Polarizer processing procedure of monitoring, it utilizes the redox reaction of ion chromatograph test iodide ion, with the consumption of instant control iodide ion on processing procedure and the time of replacing soup.
Another object of the present invention is for providing a kind of method that staining solution constituent in the Polarizer processing procedure changes of monitoring, and it utilizes an ion chromatograph to analyze the content of the impurity in the former material of chemicals, with the content of iodide ion in the further control Polarizer.
Another purpose of the present invention is for providing a kind of method that the staining solution constituent changes in the Polarizer processing procedure of monitoring, and it utilizes the concentration of iodide ion in the ion concentration analyser test Polarizer, with the use of available energy ground management and control soup.
According to above-described purpose, the invention provides a kind of method that the staining solution constituent changes in the Polarizer of monitoring, comprise and use ion chromatograph and ion concentration analyser that the step of this method comprises:
One staining solution through dilution is provided, and this staining solution comprises iodide ion and the wrong ion of iodine, and the staining solution of this dilution is to use the deionized water dilution, and the multiple of dilution is 1000-500,000 times;
Add a reductive agent in this staining solution, make and carry out a reduction reaction in this staining solution;
Carry out a qualitative analysis, use described ion chromatograph to determine the variation of this reduction reaction in this staining solution; And
Carry out a certain amount of analysis, use described ion concentration analyser to measure the concentration of the wrong ion of this iodine in this staining solution.
Embodiment
Next be detailed description of the present invention, in the following explanation description of processing procedure and structure do not comprised the entire flow of making.The existing skill that the present invention continued to use is only done quoting of emphasis formula at this, to help elaboration of the present invention.
The present invention discloses the method that the staining solution constituent changes in a kind of immediately monitoring Polarizer processing procedure, provide an ion chromatograph to carry out qualitative analysis, to determine the constituent in the staining solution, and execution quantitative test, with concentration and the content that determines iodide ion in the soup, wherein the electrical conductivity that imposes a condition of ion chromatograph is 21.02 microseconds (μ s), and pressure is 1496 working pressures (psi), and flow velocity is 1.20 ml/min.The ion chromatography principle is the negative ion to be measured that utilizes in the sample solution, with sodium carbonate and sodium bicarbonate flowing lotion flow through one row the ion-exchange chromatography pipe time, because of its with the strong basicity exchange resin of low capacity between affinity different and separated, negative ion to be measured after the separation, when flowing through the restraining device of Zeo-karb of a high power capacity again, be converted into the form of the high electrical conductivity acid of tool, flowing lotion then converts the carbonic acid of low electrical conductivity to, when the negative ion to be measured after conversion is flowed through the conductivity detector again, can give qualitative reaching quantitatively according to its hold-up time and crest area.Therefore, ion chromatograph utilizes the difference of ion-exchange capacity, the ion in the solution can be separated when the tubing string of filling through ion exchange resin, and then after changing through flowing lotion, give qualitative according to its hold-up time and crest area.
Flowing lotion used in the present invention adds sodium carbonate and sodium bicarbonate in 2000 milliliters the deionized water, and its purity, weight and electrical conductivity are as shown in Table 1.
The condition of table one flowing lotion used in the present invention
| Nomenclature of drug | Sodium carbonate (Na 2CO 3) | Sodium bicarbonate (NaHCO 3) |
| Purity | ＞99％ | ＞99％ |
| Sampling | 0.7462 gram | 0.1686 gram |
| Electrical conductivity | The 16-25 microsecond | (asking updates) |
In the method that the staining solution constituent changes in monitoring Polarizer processing procedure provided by the present invention, utilize the difference of Ohm law (Ohm ' s Law) and various zwitterion activity and produce different electrical conductivities, quantitatively reach the iodide ion in the qualitative analysis soup, the asynchronism(-nization) that the mode of its separation utilizes different ions to occur is distinguished.
Iodide ion solution used in the present invention adds iodine in the liquor kalii iodide, need to add deionized water (DI Water) dilution, and the multiple of dilution can be 2-1, and 000,000 times, the preferably is 10-500,000 times.Because the awkward water-soluble material of iodine, its solubleness is approximately 3 grams per liters, so the mode of shaking with ultrasonic is dissolved in iodine in the deionized water.In addition, reductive agent used in the present invention is a Vitamin C, wherein, 1 gram Vitamin C is dissolved in the water, and after being diluted to 100 milliliters, the reductive agent that at every turn adds 0.2 milliliter is in iodide ion solution.
Process from the above mentioned, in one preferred embodiment of the method that the staining solution constituent changes in the immediately monitoring Polarizer processing procedure of the present invention, iodine and liquor kalii iodide are added deionized water to be finished the dilution back and is injected in the ion chromatograph, then, this iodide ion solution is added to be injected in this ion chromatograph after Vitamin C reduces again and analyze, the result of its analysis can learn in showing as shown in Table 2, the optimum value that adds in deionized water dilution iodine and the liquor kalii iodide is 50,000 times.
The reduction of table two iodide ion changes
| Extension rate | The crest time of occurrence | The area size | |
| Iodine stoste | 10 | 12.78-18.43 | 281552534.68 |
| Iodine stoste reduction back (adding Vitamin C) | 10 | ---- | ---- |
| Iodine stoste | 100 | 18.99-26.51 | 26013962.81 |
| Iodine stoste reduction back (adding Vitamin C) | 100 | 17.45-24.88 | 477446052.00 |
| Iodine stoste | 1000 | 21.05-24.93 | 2592849.20 |
| Iodine stoste reduction back (adding Vitamin C) | 1000 | 20.65-24.70 | 3759461.20 |
| Iodine stoste | 50000 | 20.08-22.20 | 367433.00 |
| Iodine stoste reduction back (adding Vitamin C) | 50000 | 19.7-22.28 | 723464.68 |
| Iodine stoste | 500000 | 20.99-21.83 | 15318.2 |
| Iodine stoste reduction back (adding Vitamin C) | 500000 | 20.22-22.15 | 134612.8 |
Owing to be primary raw material with iodine and potassium iodide in the processing procedure of Polarizer, therefore, the instant variation of understanding iodide ion is an important research to the processing procedure of Polarizer.Observe the result of table two, can find that the reduction that utilizes ion chromatograph can clearly observe iodide ion changes, wherein, its reduction variation all appears at identical time zone, for example, iodine stoste is diluted 50 with deionized water, in the time of 000 times, the time point that iodide ion solution crest occurs is identical with the time point that other extension rate occurs, similarly, after the iodide ion solution of this identical extension rate added the Vitamin C reduction, it still had identical time zone (hold-up time) with the iodide ion solution of the reduction of other extension rate, so in view of the above can be qualitative go out wrong ion of iodine and the preceding iodide ion of reduction after the reduction.
In addition, the iodide ion solution of different extension rates, (I before its reduction
3 -) and reduction back (I
-) all have quite significantly area change, because the present invention utilizes Vitamin C that the wrong ion of iodine is reduced into iodide ion, therefore, the redox that the area before the reduction of the deduction of the area after the reduction is iodine changes, and in view of the above, can reach quantitative purpose.So the present invention can by ion chromatograph simply and the redox that detects iodide ion apace immediately change.
After qualitatively analyze goes out wrong ion of iodine and iodide ion, the method of iodide ion concentration and content also can utilize ion concentration analyser collocation iodide ion selection electrode to calculate and determine the concentration of the wrong ion of iodine in each solution tank in processing procedure (comprising staining trough, extension slot and revisal groove etc.) in the monitoring Polarizer of the present invention, simultaneously, the present invention is inserted in nernst equation with standard addition method with the current potential of measured iodide ion, and converses the concentration of the wrong ion of iodine.
Using the ion concentration analyser to calculate and measure in the method for the wrong ion of iodine, the iodide ion solution that will comprise wrong ion of iodine and iodide ion dilutes with deionized water, its extension rate is 100 times, afterwards, select the concentration of the above-mentioned iodide ion solution of electrode analysis with iodide ion, then, get the tens of milliliters of iodide ion solution, and add tens of milliliters of Vitamin Cs the wrong ion of iodine is reduced into iodide ion, therefore, the wrong ion of iodine can be reduced into iodide ion in the iodine solution originally, then, select the concentration of the iodide ion solution after electrode analysis reduces again with iodide ion, afterwards, the numerical value after the measured reduction is deducted the concentration that the preceding numerical value of reduction is the wrong ion of iodine.Utilize iodide ion to select result that electrode measures the iodide ion solution in each solution tank as shown in Table 3.
Table three is analyzed the preceding concentration that reaches after reducing of iodide ion reduction with the ion concentration analyser
| Before the reduction (1,000,000/, ppm) | The reduction back (1,000,000/, ppm) | (before one reduction of reduction back)/reduction back (1,000,000/, ppm) | |
| Staining trough | |||
| 7.92 | 10.23 | 0.226 | |
| 8.19 | 10.49 | 0.219 | |
| 9.20 | 11.41 | 0.194 | |
| 8.97 | 11.06 | 0.189 | |
| 9.56 | 12.42 | 0.230 | |
| 9.75 | 11.95 | 0.184 | |
| 9.86 | 12.00 | 0.178 | |
| 9.95 | 12.31 | 0.192 | |
| 10.72 | 12.38 | 0.134 | |
| 10.10 | 12.29 | 0.178 | |
| 10.27 | 12.38 | 0.170 | |
| 10.39 | 12.70 | 0.182 | |
| 11.23 | 12.75 | 0.119 | |
| Extension slot | |||
| 191.00 | 196.00 | 0.026 | |
| 191.00 | 196.00 | 0.026 | |
| 191.00 | 196.00 | 0.026 | |
| 193.00 | 200.00 | 0.035 | |
| 193.00 | 200.00 | 0.035 | |
| 193.00 | 199.00 | 0.030 | |
| 193.00 | 200.00 | 0.035 | |
| 193.00 | 200.00 | 0.035 | |
| 193.00 | 200.00 | 0.035 | |
| 194.00 | 200.00 | 0.030 | |
| 192.00 | 200.00 | 0.040 | |
| 193.00 | 201.00 | 0.040 | |
| 189.00 | 197.00 | 0.041 | |
| The revisal groove | |||
| 276.00 | 277.00 | 0.004 | |
| 269.00 | 272.00 | 0.011 | |
| 269.00 | 271.00 | 0.007 | |
| 265.00 | 267.00 | 0.007 |
| 270.00 | 272.00 | 0.007 | |
| 270.00 | 271.00 | 0.004 | |
| 267.00 | 271.00 | 0.015 | |
| 271.00 | 273.00 | 0.007 | |
| 268.00 | 270.00 | 0.007 | |
| 262.00 | 266.00 | 0.015 | |
| 263.00 | 267.00 | 0.015 | |
| 263.00 | 265.00 | 0.008 | |
| 258.00 | 261.00 | 0.011 |
Be noted that by table three and can learn that the ratio of the wrong ion of its iodine in staining trough is for the highest, therefore, can confirm that staining reaction mainly occurs in staining trough.
Since on the processing procedure of Polarizer with the wrong ion (I of iodine
3 -) infiltrate through in the polyvinyl alcohol film, therefore, the content of the wrong ion of iodine occupies important role in the Polarizer processing procedure, so utilize variation that ion concentration analyser and ion chromatograph monitor iodide ion in the Polarizer processing procedure as can be known, only need the concentration of immediately monitoring or adjustment staining trough can determine the effect that Polarizer dyes, and the time of soup is changed in decision in view of the above, and need not extra extension slot and revisal groove to be carried out the soup adjustment, so the use of management and control and saving soup effectively.
The above is preferred embodiment of the present invention only, is not in order to limit the right of applying for a patent of the present invention; Simultaneously above description should be understood and be implemented for the special personage who knows the present technique field, so other does not break away from the equivalence of being finished under the disclosed spirit of the present invention and change or modification, all should be included in the described claim scope.
Claims (7)
1. the method that the staining solution constituent changes in the immediately monitoring Polarizer processing procedure comprises and uses ion chromatograph and ion concentration analyser, and the step of this method comprises:
One staining solution through dilution is provided, and this staining solution comprises iodide ion and the wrong ion of iodine, and the staining solution of this dilution is to use the deionized water dilution, and the multiple of dilution is 1000-500,000 times;
Add a reductive agent in this staining solution, make and carry out a reduction reaction in this staining solution;
Carry out a qualitative analysis, use described ion chromatograph, determine the variation of this reduction reaction in this staining solution; And
Carry out a certain amount of analysis, use described ion concentration analyser, measure the concentration of the wrong ion of this iodine in this staining solution.
2. the method that the staining solution constituent changes in the immediately monitoring Polarizer processing procedure as claimed in claim 1, described reductive agent is a Vitamin C, 1 gram Vitamin C is dissolved in the water, and after being diluted to 100 milliliters, the reductive agent that at every turn adds 0.2 milliliter is in iodide ion solution.
3. the method that the staining solution constituent changes in the immediately monitoring Polarizer processing procedure as claimed in claim 1, it is characterized in that, this reduction reaction is that this reductive agent is added in the staining solution of this dilution, so that the wrong ion of this iodine in the staining solution of this dilution is reduced to iodide ion.
4. the method that the staining solution constituent changes in the immediately monitoring Polarizer processing procedure as claimed in claim 1 is characterized in that comprising an extension rate when diluting the staining solution of this dilution with this deionized water is 50,000 times.
5. the method that the staining solution constituent changes in the immediately monitoring Polarizer processing procedure as claimed in claim 1 is characterized in that, more comprises to utilize an iodide ion to select electrode to analyze the staining solution of this dilution.
6. the method that the staining solution constituent changes in the immediately monitoring Polarizer processing procedure as claimed in claim 1, it is characterized in that, this quantitative test comprise utilize this ion concentration analyser measure before this reduction reaction respectively and this reduction reaction after the concentration of staining solution of this dilution.
7. the method that the staining solution constituent changes in the immediately monitoring Polarizer processing procedure as claimed in claim 6, it is characterized in that the concentration of the wrong ion of this iodine that described ion concentration analyser is measured is the numerical value before the numerical value after the iodide ion reduction reaction is deducted this iodide ion reduction reaction.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2005100059805A CN100370287C (en) | 2005-02-02 | 2005-02-02 | Method for instant monitoring dyeing solution composition change for polarized light plate process |
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|---|---|---|---|
| CNB2005100059805A CN100370287C (en) | 2005-02-02 | 2005-02-02 | Method for instant monitoring dyeing solution composition change for polarized light plate process |
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|---|---|
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| CN100370287C true CN100370287C (en) | 2008-02-20 |
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| TWI640555B (en) * | 2017-08-16 | 2018-11-11 | 住友化學股份有限公司 | Method and system for manufacturing a polarizer film |
Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3920397A (en) * | 1973-08-06 | 1975-11-18 | Dow Chemical Co | Apparatus and method for quantitative analysis of ionic species by liquid column chromatography |
| JPS5885405A (en) * | 1981-11-17 | 1983-05-21 | Nitto Electric Ind Co Ltd | Manufacture of polarizing film |
| JPH06118230A (en) * | 1992-10-02 | 1994-04-28 | Seiko Epson Corp | Polarizer |
| JPH0829617A (en) * | 1994-07-18 | 1996-02-02 | Sumitomo Chem Co Ltd | Polarizing plate |
| US6197258B1 (en) * | 1996-10-25 | 2001-03-06 | University Of Maryland, Baltimore | Photoluminescent sensors of chemical analytes |
| US6398961B1 (en) * | 2000-07-20 | 2002-06-04 | Ecolab Inc. | Device and method for sensing low level iodine in aqueous solution |
| US20030189275A1 (en) * | 2002-04-06 | 2003-10-09 | Cael John J. | Enhanced intrinsic polarizer |
| US20030188390A1 (en) * | 2002-04-08 | 2003-10-09 | Kao Corporation | Hair dye composition |
-
2005
- 2005-02-02 CN CNB2005100059805A patent/CN100370287C/en not_active Expired - Fee Related
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3920397A (en) * | 1973-08-06 | 1975-11-18 | Dow Chemical Co | Apparatus and method for quantitative analysis of ionic species by liquid column chromatography |
| JPS5885405A (en) * | 1981-11-17 | 1983-05-21 | Nitto Electric Ind Co Ltd | Manufacture of polarizing film |
| JPH06118230A (en) * | 1992-10-02 | 1994-04-28 | Seiko Epson Corp | Polarizer |
| JPH0829617A (en) * | 1994-07-18 | 1996-02-02 | Sumitomo Chem Co Ltd | Polarizing plate |
| US6197258B1 (en) * | 1996-10-25 | 2001-03-06 | University Of Maryland, Baltimore | Photoluminescent sensors of chemical analytes |
| US6398961B1 (en) * | 2000-07-20 | 2002-06-04 | Ecolab Inc. | Device and method for sensing low level iodine in aqueous solution |
| US20030189275A1 (en) * | 2002-04-06 | 2003-10-09 | Cael John J. | Enhanced intrinsic polarizer |
| US20030188390A1 (en) * | 2002-04-08 | 2003-10-09 | Kao Corporation | Hair dye composition |
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