CN110987714B - Method for determining boric acid content in dye system polarizing film processing tank liquid - Google Patents
Method for determining boric acid content in dye system polarizing film processing tank liquid Download PDFInfo
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Abstract
The invention discloses a method for measuring the boric acid content in dye polarizing film processing tank liquor, which comprises the following steps: s1, pretreating a sample to be detected, filtering the sample to be detected, and removing micro impurities; s2, accurately weighing the weight of the crucible and the cover by using an electronic balance, and recording as M0; s3, adding the pretreated boric acid solution sample to be detected into a crucible, covering, and weighing by using an electronic balance, wherein the mark is M1; s4, putting the weighed sample into heating equipment for heating, and raising the temperature to 600-1000 ℃ by a program; s5, after baking and sintering, cooling to room temperature, taking out the crucible, keeping constant weight, and then weighing the crucible by using an electronic balance, and recording as M2; and S6, calculating the content of the boric acid according to M0, M1 and M2. The method for measuring the boric acid content in the dye polarizing film processing tank liquid has the characteristics of simple operation, easy realization, less man-made interference, no dependence on large instruments and low cost, and is convenient to popularize and apply.
Description
Technical Field
The invention relates to the technical field of boric acid concentration detection, in particular to a method for determining boric acid content in dye-based polarizing film processing tank liquor.
Background
The polarizer is an important optical component of the LCD display device, and functions as an optical switch in the LCD display device to determine the passage and closing of the light path. In the production and manufacturing process of the polarizer, the processing and processing procedure of the polarizing film is the most important procedure in the whole production process and is also the procedure with the largest difficulty coefficient. In the processing step of the polarizing film, boric acid is used as a cross-linking agent to perform a cross-linking reaction with the polarizing film so as to enhance the dimensional stability of the polarizing film; meanwhile, the boric acid also has a color fixing effect, is beneficial to fixing the organic dye in the polarizing film, improves the weather resistance of the polarizing film, and determines the quality of the polarizer product to a certain extent, so that how to effectively monitor the boric acid content in the bath solution of the polarizing film processing procedure has very important significance for manufacturing the high-quality polarizer product.
In the actual production process, after the organic dye dyeing treatment is finished in the dyeing tank, the polarizing film enters the boric acid tank for stretching and crosslinking treatment, the organic dye on the polarizing film is more or less brought into the boric acid tank, the main organic dyes comprise azo type dichroic dyes (specifically divided into two types of bisazo and trisazo), anthraquinone type dichroic dyes, triphendioxazine and derivative type dichroic dyes, monomethine and polymethine type dichroic dyes, and the like, and the presence of the organic dyes brings about a lot of interference on the accurate detection of the boric acid content.
At present, the method for testing the boric acid content comprises an instrument method: spectrophotometry, potentiometric titration, inductively coupled plasma emission spectrometry, and chemical analysis: neutralization titration. Wherein, the instrumental analysis method usually needs to be subjected to derivatization before detection, has a plurality of interference factors for analysis, is relatively complicated in the operation of the detection and analysis process, and has high investment cost of detection equipment; while the neutralization titration method is a chemical detection method commonly used by most polarizer manufacturers at present, the man-made interference is large when the titration end point is judged by the neutralization titration method, different analysis operators have deviation in judging the indicator end point, so that the same group of samples and different analyzers have different degrees of deviation in the obtained analysis results, and the condition brings certain difficulty in monitoring the boric acid content.
The accurate test of the boric acid content in the polarizing film processing procedure, especially the effective and accurate test of the boric acid content with organic dye, has very important influence on the management and control of the polarizer product flow, and is a problem to be solved urgently in the polarizer manufacturing industry, however, at present, there are almost no documents and patent reports specially aiming at the polarizer industry about such problems in China. It is seen that improvements and enhancements in the prior art are needed.
Disclosure of Invention
In view of the defects of the prior art, the invention aims to provide a method for measuring the boric acid content in the dye-based polarizing film processing tank liquid, and aims to solve the problem that no method which is accurate, reliable and convenient to operate is available for measuring the boric acid content in the polarizing film processing tank liquid with organic dye in the prior art.
In order to achieve the purpose, the invention adopts the following technical scheme:
a method for measuring the boric acid content in dye-based polarizing film processing bath solution, wherein the method comprises the following steps:
s1, pretreating a sample to be detected, filtering the sample to be detected, and removing micro impurities;
s2, accurately weighing the weight of the crucible and the weight of the cover with the electronic balance, and recording as M0;
s3, adding the pretreated boric acid solution sample to be detected into a crucible, covering, and weighing by using an electronic balance, wherein the mark is M1;
s4, putting the weighed sample into heating equipment for heating, and raising the temperature to 600-1000 ℃ by a program;
s5, after baking and sintering, cooling to room temperature, taking out the crucible, keeping constant weight, and weighing the crucible by using an electronic balance, wherein the weight is marked as M2;
and S6, calculating the content of the boric acid according to M0, M1 and M2.
In the method for measuring the boric acid content in the dye-based polarizing film processing tank solution, the step S4 is specifically a step of raising the temperature: in the first stage, the temperature is raised to 120 ℃ at normal temperature for 1-3 min, and the temperature is kept for 1-2 min; in the second stage, the temperature is raised for 3-5 min at 120-500 ℃, and the temperature is kept for 1-2 min; and a third stage: heating for 1-3 min at 500-1000 ℃, and keeping the temperature for 1-3 min.
In the method for measuring the boric acid content in the dye-based polarizing film processing bath solution, the third stage: heating for 1min at 500-800 ℃, and preserving heat for 3 min.
In the method for measuring the boric acid content in the dye-based polarizing film processing bath solution, the step S1 specifically includes: taking liquid to be detected, standing for 10-15 min, performing suction filtration on supernatant through a suction filtration device, and collecting filtrate as a sample to be detected.
In the method for measuring the boric acid content in the dye-based polarizing film processing tank solution, the suction filtration device adopts medium-speed filter paper.
In the method for measuring the boric acid content in the dye-based polarizing film processing bath solution, in the step S3, the sampling amount of the boric acid solution sample is 2-10 g.
In the method for measuring the boric acid content in the dye-based polarizing film processing tank liquid, the number of parallel samples is not less than 3.
Has the advantages that:
the invention provides a method for measuring the boric acid content in dye-based polarizing film processing tank liquor, which is characterized in that according to the principle that boric acid is easily decomposed by heating and organic dye is easily oxidized and volatilized at high temperature, the boric acid content can be removed, and the mass percentage of the boric acid in the solution can be calculated and obtained by measuring the weight of the solution before decomposition and the weight of boron trioxide after decomposition.
Detailed Description
The present invention provides a method for measuring boric acid content in a dye-based polarizing film processing bath solution, and the present invention will be further described in detail by way of examples in order to make the objects, technical solutions and effects of the present invention clearer and clearer. It should be understood that the specific embodiments described herein are merely illustrative of the invention and do not limit the invention.
The invention provides a method for measuring the boric acid content in dye-based polarizing film processing tank liquor, which comprises the following steps:
s1, pretreating a sample to be detected, filtering the sample to be detected, and removing micro impurities;
s2, accurately weighing the clean crucible and the weight with the cover by using an electronic balance, and recording as M0;
s3, adding the pretreated boric acid solution sample to be detected into a crucible, covering the crucible, and weighing the sample by using an electronic balance, wherein the weight is recorded as M1;
s4, placing the weighed sample into heating equipment for heating, and raising the temperature to 600-1000 ℃ by a program;
s5, after baking and sintering, cooling to room temperature, taking out the crucible, keeping constant weight, and then weighing the crucible by using an electronic balance, and recording as M2;
and S6, calculating the content of the boric acid according to M0, M1 and M2.
The method for measuring the boric acid content in the dye-based polarizing film processing tank liquid mainly utilizes the chemical characteristic that boric acid is decomposed by heat, the boric acid loses water to become metaboric acid at 100-105 ℃ in the heating process, the heating is continued, and the metaboric acid is completely decomposed and converted into boron oxide when the temperature exceeds 600 ℃, and the specific reaction formula is as follows:
the decomposed boron oxide is a stable solid substance at high temperature, and the amount of the boric acid can be obtained by measuring the amount of the boron oxide, so that the content or the concentration of the boric acid in the bath solution can be obtained.
In the method for measuring the boric acid content in the dye-based polarizing film processing tank liquid, the mass percentage content of the boric acid is obtained according to the mass relation of each compound in the reaction formula by measuring the weight (M1-M0) of the boric acid solution before decomposition and the weight (M2-M0) of the boric oxide after decomposition:
boric acid% ═ 1.776 [ (M2-M0)/(M1-M0) ] 100%
Specifically, in the method for measuring the boric acid content in the dye-based polarizing film processing bath solution, since the bath solution contains fine impurity particles and small fragments of a film falling from the polarizing film in water, and some of the fine solids are difficult to decompose and gasify at high temperature and easily interfere with the weight of the final boron oxide, a sample needs to be pretreated to remove the solid impurities, specifically: taking liquid to be detected, standing for 10-15 min, layering large solid particles through standing, and performing suction filtration on supernatant through a suction filtration device to remove tiny solid particles to obtain a purer sample to be detected. Preferably, the filter paper is medium-speed filter paper, and the medium-speed filter paper can completely remove solid impurities in the liquid to be detected and has a relatively proper filtering speed.
Specifically, in the method for measuring the boric acid content in the dye-based polarizing film processing bath solution, the temperature rise in the step S4 specifically includes: in the first stage, the temperature is raised from normal temperature to 120 ℃ for 1-3 min, and the temperature is kept for 1-2 min; in the second stage, the temperature is 120-500 ℃, the temperature rise time is 3-5 min, and the temperature is kept for 1-2 min; and a third stage: heating for 1-3 min at 500-1000 ℃, and keeping the temperature for 1-3 min. The programmed heating step can remove moisture, organic dye and other easily decomposed substances step by step and completely decompose boric acid. Setting the temperature rise range of the first stage to be between normal temperature and 120 ℃, wherein the water in the sample is mainly removed in the first stage, the more thorough the water removal is, the more beneficial the dehydration and decomposition of the subsequent boric acid is, and meanwhile, the boric acid can lose one molecule of crystal water to become metaboric acid in the first stage; setting the temperature rise range of the second stage to be 120-500 ℃, mainly removing easily decomposed organic dyes in the sample at the stage, and carbonizing impurities to form volatile carbon dioxide and water through the temperature rise treatment at the second stage due to the fact that the sample contains the organic dyes and polaroid film plastic scraps or other trace organic matters, so that interference is eliminated; setting the temperature rise range of the third stage to be 500-1000 ℃, mainly aiming at decomposing the metaboric acid as completely as possible, removing moisture from the metaboric acid at a high temperature of more than 500 ℃ to generate boron oxide, and setting the final temperature to be more than the decomposition temperature of the metaboric acid, keeping the temperature for 1-3 min to completely remove moisture in the metaboric acid, so that the measured value of the boric acid content is accurate. The device adopted in the step is a muffle furnace or a high-temperature furnace capable of raising temperature by a program.
Preferably, in the method for measuring a boric acid content in a dye-based polarizing film processing bath, the third stage: heating for 1min at 500-800 ℃, and keeping the temperature for 3 min. The maximum temperature of the third stage is set to be 800 ℃, and the temperature is kept for 3min, so that the analysis time of the sample can be saved on the basis of complete decomposition of the metaboric acid, and the time for subsequent cooling can be reduced.
Specifically, in the method for measuring the boric acid content in the dye-based polarizing film processing bath solution, in the step S3, a sample of the boric acid solution is taken in an amount of 2 to 10 g. The sampling amount of the boric acid solution sample is related to whether the sample is representative or not and influences the time required by the whole content measurement, the sampling amount is representative and cannot be too small, particularly when the concentration of boric acid is low, the sampling amount is too small, large errors are easily caused, the whole detection process is fast, the capacity of a crucible is considered and cannot be too large, and when the sampling amount is 2-10 g, the sampling amount is representative and other substances can be fast removed in the temperature programming process. It should be noted that when the parallel samples have a large difference in the detection results and a low boric acid content, the samples are re-sampled and detected, and the sampling amount is adjusted to 8-10 g.
Specifically, in the method for measuring the boric acid content in the dye-based polarizing film processing bath solution, the number of parallel samples is not less than 3. The more the number of the parallel samples is, the closer the boric acid content to the true value is, but the more the number of the parallel samples is, the longer the time required for analysis and detection is, and on the basis of ensuring the effectiveness of data, the number of the parallel samples is selected to be 3, so that the time can be shortened, and the efficiency can be improved.
Example 1
A method for measuring the boric acid content in dye-based polarizing film processing tank liquor, which comprises the following steps:
s1, taking 50mL of liquid to be detected in a liquid tank, standing for 12min, then carrying out suction filtration on supernatant through medium-speed filter paper, and collecting filtrate as a sample to be detected;
and S2, accurately weighing the clean crucible with the cover by using an electronic balance, and recording the weight as M0.
And S3, adding about 5g of the pretreated boric acid solution sample to be detected into the crucible, covering the crucible, and weighing the sample by using an electronic balance, wherein the weight is recorded as M1.
S4, placing the weighed sample into heating equipment for roasting, and adopting programmed heating, wherein in the first stage, the temperature is increased from normal temperature to 120 ℃, the heating time is 2min, and the temperature is kept for 2 min; in the second stage, the temperature is raised for 4min at 120-500 ℃, and the temperature is kept for 1 min; and a third stage: heating for 2min at 500-800 ℃, and keeping the temperature for 3 min.
And S5, after roasting is finished, taking out the crucible and weighing the crucible by using an electronic balance, wherein the M2 is recorded.
And S6, calculating the content of the boric acid according to M0, M1 and M2.
In this example, the number of the parallel samples is 3, and the boric acid content is an average value of the 3 parallel samples.
Example 2
A method for measuring the boric acid content in dye-based polarizing film processing tank liquor, which comprises the following steps:
s1, taking 50mL of liquid to be detected in a liquid tank, standing for 10min, filtering supernatant through medium-speed filter paper, and collecting filtrate as a sample to be detected;
and S2, accurately weighing the weight of the clean crucible with the cover by using an electronic balance, and recording the weight as M0.
And S3, adding about 2g of the pretreated boric acid solution sample to be detected into the crucible, covering the crucible, and weighing the sample by using an electronic balance, wherein the weight is recorded as M1.
S4, placing the weighed sample into heating equipment for roasting, and adopting programmed heating, wherein in the first stage, the temperature is increased from normal temperature to 120 ℃, the heating time is 1min, and the temperature is kept for 2 min; in the second stage, the temperature is raised for 3min at 120-500 ℃, and the temperature is kept for 2 min; and a third stage: heating for 1min at 500-600 ℃, and keeping the temperature for 3 min.
And S5, after the roasting is finished, taking out the crucible, and weighing the crucible by using an electronic balance, wherein the weight is recorded as M2 when the temperature is reduced to the room temperature.
And S6, calculating the content of the boric acid according to M0, M1 and M2.
In this example, the number of the parallel samples is 5, and the boric acid content is an average value of 5 parallel samples.
Example 3
A method for measuring the boric acid content in dye-based polarizing film processing tank liquor, which comprises the following steps:
s1, taking 50mL of liquid to be detected in a liquid tank, standing for 15min, performing suction filtration on supernatant through medium-speed filter paper, and collecting filtrate as a sample to be detected;
and S2, accurately weighing the clean crucible with the cover by using an electronic balance, and recording the weight as M0.
And S3, adding about 10g of the pretreated boric acid solution sample to be detected into the crucible, covering the crucible, and weighing the sample by using an electronic balance, wherein the weight is recorded as M1.
S4, placing the weighed sample into heating equipment for roasting, and performing temperature programming, wherein in the first stage, the temperature is increased from normal temperature to 120 ℃, the temperature increasing time is 3min, and the temperature is kept for 1 min; in the second stage, the temperature is increased for 5min at 120-500 ℃, and the temperature is kept for 1 min; and a third stage: heating for 3min at 500-1000 ℃, and keeping the temperature for 1 min.
And S5, after the roasting is finished, taking out the crucible, and weighing the crucible by using an electronic balance, wherein the weight is recorded as M2 when the temperature is reduced to the room temperature.
And S6, calculating the content of the boric acid according to M0, M1 and M2.
In this example, the number of the parallel samples is 4, and the boric acid content is an average value of the 4 parallel samples.
The method described in examples 1-3 above was used to test boric acid of known concentration, and the neutralization titration method and instrumental analysis method were used to compare the results, as shown in the following table:
as can be seen from the comparison of the above table, the boric acid content obtained by the method of the embodiments 1 to 3 of the present invention is the closest to the true boric acid content value of the sample, and the deviation is the smallest, so that the detection method of the present invention can detect the boric acid content in the aqueous solution of boric acid by mass percent more accurately.
It should be understood that equivalents and modifications of the technical solution and inventive concept thereof may occur to those skilled in the art, and all such modifications and alterations should fall within the scope of the appended claims.
Claims (6)
1. A method for measuring the boric acid content in dye-based polarizing film processing tank liquor is characterized by comprising the following steps:
s1, pretreating a sample to be detected, filtering the sample to be detected, and removing micro impurities;
s2, accurately weighing the weight of the crucible and the cover by using an electronic balance, and recording as M0;
s3, adding the pretreated boric acid solution sample to be detected into a crucible, covering, and weighing by using an electronic balance, wherein the mark is M1;
s4, placing the weighed sample into heating equipment for heating, and heating to 600-1000 ℃ by a program, wherein the program comprises the following specific steps: in the first stage, the temperature is raised to 120 ℃ at normal temperature for 1-3 min, and the temperature is kept for 1-2 min; in the second stage, the temperature is 120-500 ℃, the temperature rise time is 3-5 min, and the temperature is kept for 1-2 min; and a third stage: heating for 1-3 min at 500-1000 ℃, and preserving heat for 1-3 min;
s5, after baking and sintering, cooling to room temperature, taking out the crucible, keeping constant weight, and then weighing the crucible by using an electronic balance, and recording as M2;
s6, calculating the content of boric acid according to M0, M1 and M2, wherein the calculation formula of the content of the boric acid by mass percent is as follows: boric acid% (% 1.776: (M2-M0)/(M1-M0) × 100%.
2. The method of claim 1, wherein the third stage comprises: heating for 1min at 500-800 ℃, and keeping the temperature for 3 min.
3. The method of claim 1, wherein the step S1 specifically includes: taking liquid to be detected, standing for 10-15 min, performing suction filtration on supernatant through a suction filtration device, and collecting filtrate as a sample to be detected.
4. The method for measuring the boric acid content in the dye based polarizer processing bath solution according to claim 3, wherein the suction filtration device adopts medium speed filter paper.
5. The method of claim 1, wherein in step S3, a sample of the boric acid solution is taken in an amount of 2-10 g.
6. The method of claim 1 wherein the number of parallel samples is not less than 3.
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| IT1196499B (en) * | 1986-07-16 | 1988-11-16 | Chimica Larderello Spa Soc | PROCESS PERFECTED FOR THE PREPARATION OF BORICA DIOXIDE |
| JP5606704B2 (en) * | 2009-08-27 | 2014-10-15 | 株式会社クラレ | Manufacturing method of polarizing film |
| CN103033498B (en) * | 2012-12-21 | 2015-05-13 | 深圳市谱尼测试科技有限公司 | Method for simultaneously detecting boric acid and borax |
| CN103760055B (en) * | 2013-11-30 | 2016-02-10 | 彩虹集团电子股份有限公司 | The method of testing of silver content in a kind of silver paste |
| CN206038463U (en) * | 2016-08-11 | 2017-03-22 | 青海东台吉乃尔锂资源股份有限公司 | Detect boric acid saturation device |
| CN109211712B (en) * | 2018-10-17 | 2021-03-09 | 东旭光电科技股份有限公司 | Method for measuring water content of boric anhydride |
| CN109738575A (en) * | 2018-12-14 | 2019-05-10 | 深圳市盛波光电科技有限公司 | The detection method of boric acid content in a kind of light polarizing film |
| CN109580416A (en) * | 2018-12-27 | 2019-04-05 | 中核四0四有限公司 | Residual object, total oxide measurement temperature-rising method are always steamed in a kind of high activity liquid waste |
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