CN111337442A - Method for measuring PVA optical film dissolution amount - Google Patents
Method for measuring PVA optical film dissolution amount Download PDFInfo
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- CN111337442A CN111337442A CN202010212168.4A CN202010212168A CN111337442A CN 111337442 A CN111337442 A CN 111337442A CN 202010212168 A CN202010212168 A CN 202010212168A CN 111337442 A CN111337442 A CN 111337442A
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- 239000012788 optical film Substances 0.000 title claims abstract description 31
- 238000000034 method Methods 0.000 title claims abstract description 21
- 238000004090 dissolution Methods 0.000 title claims abstract description 18
- 239000000243 solution Substances 0.000 claims abstract description 72
- 238000002835 absorbance Methods 0.000 claims abstract description 27
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 claims abstract description 19
- 239000004327 boric acid Substances 0.000 claims abstract description 19
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 13
- 238000001514 detection method Methods 0.000 claims abstract description 5
- 229940077844 iodine / potassium iodide Drugs 0.000 claims abstract description 5
- 239000011259 mixed solution Substances 0.000 claims abstract description 3
- NLKNQRATVPKPDG-UHFFFAOYSA-M potassium iodide Chemical compound [K+].[I-] NLKNQRATVPKPDG-UHFFFAOYSA-M 0.000 claims description 15
- DKNPRRRKHAEUMW-UHFFFAOYSA-N Iodine aqueous Chemical compound [K+].I[I-]I DKNPRRRKHAEUMW-UHFFFAOYSA-N 0.000 claims description 13
- 239000012086 standard solution Substances 0.000 claims description 7
- ZCYVEMRRCGMTRW-UHFFFAOYSA-N 7553-56-2 Chemical compound [I] ZCYVEMRRCGMTRW-UHFFFAOYSA-N 0.000 claims description 6
- 239000011630 iodine Substances 0.000 claims description 6
- 229910052740 iodine Inorganic materials 0.000 claims description 6
- 239000012153 distilled water Substances 0.000 claims description 4
- 238000002791 soaking Methods 0.000 claims description 2
- 239000004372 Polyvinyl alcohol Substances 0.000 description 53
- 229920002451 polyvinyl alcohol Polymers 0.000 description 53
- 239000010408 film Substances 0.000 description 11
- 239000003153 chemical reaction reagent Substances 0.000 description 3
- 229920001621 AMOLED Polymers 0.000 description 2
- RLTYKOCELUYEKF-UHFFFAOYSA-N [I].OB(O)O Chemical compound [I].OB(O)O RLTYKOCELUYEKF-UHFFFAOYSA-N 0.000 description 2
- 238000004043 dyeing Methods 0.000 description 2
- 238000010828 elution Methods 0.000 description 2
- 239000004973 liquid crystal related substance Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 150000003384 small molecules Chemical class 0.000 description 2
- 229920002284 Cellulose triacetate Polymers 0.000 description 1
- NNLVGZFZQQXQNW-ADJNRHBOSA-N [(2r,3r,4s,5r,6s)-4,5-diacetyloxy-3-[(2s,3r,4s,5r,6r)-3,4,5-triacetyloxy-6-(acetyloxymethyl)oxan-2-yl]oxy-6-[(2r,3r,4s,5r,6s)-4,5,6-triacetyloxy-2-(acetyloxymethyl)oxan-3-yl]oxyoxan-2-yl]methyl acetate Chemical compound O([C@@H]1O[C@@H]([C@H]([C@H](OC(C)=O)[C@H]1OC(C)=O)O[C@H]1[C@@H]([C@@H](OC(C)=O)[C@H](OC(C)=O)[C@@H](COC(C)=O)O1)OC(C)=O)COC(=O)C)[C@@H]1[C@@H](COC(C)=O)O[C@@H](OC(C)=O)[C@H](OC(C)=O)[C@H]1OC(C)=O NNLVGZFZQQXQNW-ADJNRHBOSA-N 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000008358 core component Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000010413 mother solution Substances 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000008961 swelling Effects 0.000 description 1
- 238000011144 upstream manufacturing Methods 0.000 description 1
Classifications
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/30—Staining; Impregnating ; Fixation; Dehydration; Multistep processes for preparing samples of tissue, cell or nucleic acid material and the like for analysis
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- Physics & Mathematics (AREA)
- Life Sciences & Earth Sciences (AREA)
- Health & Medical Sciences (AREA)
- Pathology (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Spectroscopy & Molecular Physics (AREA)
- Molecular Biology (AREA)
- Biomedical Technology (AREA)
- Engineering & Computer Science (AREA)
- Investigating Or Analysing Materials By Optical Means (AREA)
- Investigating Or Analysing Materials By The Use Of Chemical Reactions (AREA)
Abstract
The invention discloses a method for measuring the dissolution amount of a PVA optical film, which is to soak the PVA optical film to be measured in water to prepare an extracting solution to be measured; and taking a mixed solution of a boric acid solution and an iodine/potassium iodide solution as a developing solution, adding the developing solution into the extracting solution to be detected, then measuring the absorbance, and obtaining the concentration of PVA in the extracting solution to be detected according to a standard relation curve of the absorbance and the concentration of PVA, thereby calculating the dissolution amount of the PVA optical film. The method can simply and efficiently realize trace detection of PVA in the solution, can quickly detect the dissolution amount of the PVA optical film, and has guiding significance for evaluating the quality of the PVA optical film product.
Description
Technical Field
The invention belongs to the field of polaroids, and particularly relates to a method for measuring the dissolution amount of a PVA optical film.
Background
The polarizer is a core component for producing the liquid crystal display panel, and the polyvinyl alcohol (PVA) optical film is a key material for producing the polarizer. Nowadays, the demand for large-sized liquid crystal is getting larger and more, and more new products are developed, as the mainstream of the next generation display: an Active Matrix Organic Light Emitting Diode (AMOLED) display has the characteristics of flexibility and ultrathin, so that the requirements on raw materials of various links are very strict, and particularly the PVA optical film at the upstream of an industrial chain.
The existing method for producing the polarizer is to form a polarizing film after pre-swelling, iodine dyeing, uniaxial extension and boric acid curing of a formed PVA film, and then respectively attach cellulose triacetate films (TAC) to two sides. However, during the manufacturing process of the polarizing film, the PVA film may have dissolved substances, such as additives and small molecules in the PVA film, which may contaminate the downstream dyeing tank for producing the polarizer. Furthermore, since too many small molecules are dissolved in the PVA film, the PVA film is not uniformly dyed, and thus the amount of PVA dissolved in the PVA film needs to be measured.
However, no effective method for measuring the amount of elution of the PVA optical film is available at present.
Disclosure of Invention
Based on the defects of the prior art, the invention provides a method for measuring the dissolution amount of a PVA optical film, so that the accurate and efficient determination of the dissolution amount of the PVA optical film can be realized.
In order to realize the purpose of the invention, the following technical scheme is adopted:
the invention discloses a method for measuring the dissolution amount of a PVA optical film, which is characterized by comprising the following steps: soaking the PVA optical film to be detected in water to prepare an extracting solution to be detected; and taking a mixed solution of a boric acid solution and an iodine/potassium iodide solution as a developing solution, adding the developing solution into the extracting solution to be detected, then measuring the absorbance, and obtaining the concentration of PVA in the extracting solution to be detected according to a standard relation curve of the absorbance and the concentration of PVA, thereby calculating the dissolution amount of the PVA optical film. The method specifically comprises the following steps:
step 1, adding boric acid into water, and shaking up to obtain a boric acid solution; adding iodine and potassium iodide into water, and shaking uniformly to obtain an iodine-potassium iodide solution; mixing a boric acid solution and an iodine-potassium iodide solution to obtain a color developing solution;
step 2, cutting the PVA optical film to be tested to X m in area2The n pieces of (1) are used as samples to be detected; putting n samples to be detected into distilled water with the temperature of 10-40 ℃ and the volume of Y mL, and standing for 2-6h to obtain an extracting solution to be detected;
step 3, taking M mL of the color development solution obtained in the step 1, using the to-be-detected extracting solution to fix the volume to N mL, standing for 10-60min, and then using a spectrophotometer to determine absorbance A; obtaining the concentration C mg/L of PVA in the extracting solution to be detected according to a standard relation curve of the absorbance and the concentration of PVA, and then calculating according to a formula (1) to obtain the dissolution amount Z mg/m of the PVA optical film to be detected2：
Z＝C×Y×N/((N-M)×1000×X×n) (1)。
Further, the standard relationship curve of the absorbance and the concentration of PVA is obtained as follows: preparing a series of PVA standard solutions with the concentration ranging from 10mg/L to 150 mg/L; respectively adding PVA standard solutions with various concentrations into the M mL of developing solution, fixing the volume to N mL, standing for 10-60min, and measuring the absorbance by using a spectrophotometer; and (3) drawing a standard relation curve of the absorbance and the PVA concentration by taking the PVA solution concentration C as an abscissa and the absorbance value A as an ordinate: a ═ KC + B, where a is absorbance value, C (mg/L) is PVA solution concentration, and K, B is constant.
In the step 1: the concentration of the boric acid solution is preferably 20-50g/L, more preferably 30-35 g/L; the concentration of iodine in the iodine-potassium iodide solution is preferably 5-20g/L, the concentration of potassium iodide is preferably 20-40g/L, more preferably 10-15g/L and the concentration of potassium iodide is preferably 25-30 g/L; the volume ratio of the boric acid solution to the iodine-potassium iodide solution is preferably 2 to 5:1, more preferably 3: 1.
Preferably, in step 2, the PVA optical film to be measured is cut into a circle or a square, and the area of the PVA optical film is not more than 0.01m2，n≥10。
Preferably, the detection wavelength of the spectrophotometer is 600-750 nm.
The invention has the beneficial effects that:
1. the method can simply and efficiently realize trace detection of PVA in the solution, can quickly detect the dissolution amount of the PVA optical film, and has guiding significance for evaluating the quality of the PVA optical film product.
2. The invention adopts boric acid solution and iodine-potassium iodide solution to be mixed as color developing solution. The iodine solution and PVA can form a blue complex, but when the concentration of the PVA solution is too low, no obvious color reaction exists, the measured absorbance value is very small, and the error is very large; after the boric acid solution is added, even the PVA with low concentration can present obvious blue-green color, and the measured absorbance value can accurately reflect the real condition of the PVA content in the solution.
Detailed Description
The following examples are given for the detailed implementation and specific operation of the present invention, but the scope of the present invention is not limited to the following examples.
The following examples are not specifically described, and the raw materials and reagents used are commercially available conventional materials and are not subjected to any special treatment.
Example 1
Step 1, preparing a PVA standard solution: 20mg of PVA was weighed out and put into a 100mL volumetric flask, 100mL of volume was fixed with distilled water to prepare 200mg/L PVA solution, which was used as a mother solution to prepare a series of PVA standard solutions (150mg/L, 120mg/L, 100mg/L, 80mg/L, 60mg/L, 50mg/L, 40mg/L, 30mg/L, 20mg/L, 10mg/L) having a concentration in the range of 10mg/L to 150 mg/L.
Step 2, adding 30.0g of boric acid into 1000mL of water, and shaking up to obtain 30.0g/L of boric acid solution; adding 10.0g of iodine and 25.0g of potassium iodide into 1000mL of water, and shaking uniformly to obtain an iodine-potassium iodide solution, wherein the iodine concentration is 10.0g/L, and the potassium iodide concentration is 25.0 g/L; mixing and shaking the boric acid solution and the iodine-potassium iodide solution according to the volume ratio of 3:1 to obtain a color development solution;
step 3, drawing a standard relation curve of the absorbance and the PVA concentration: taking 50mL of boric acid-iodine/potassium iodide color developing reagent, using the PVA standard solution with each concentration prepared in the step 1 to perform constant volume to 200mL, shaking up, standing for 15min, and then using a spectrophotometer to determine the absorbance A of each solution at 680 nm. The absorbance a was plotted as the ordinate and the PVA concentration as the abscissa, and a standard curve was plotted: a is 0.1048C-0.0298.
Step 4, measuring the dissolution amount of the sample to be measured, namely taking 25 pieces of 10cm × 2cm PVA optical film samples produced by three different processes, respectively putting the samples into distilled water with the temperature of 30 ℃ and the volume of 1000mL, and standing for 3 hours to obtain the extracting solution to be measured of each sample;
taking 50mL of boric acid-iodine/potassium iodide color developing reagent, fixing the volume to 200mL by using the extract to be measured of each sample, shaking up, standing for 15min, measuring the absorbance of each solution at 680nm by using a spectrophotometer, measuring each sample for three times, wherein the relative standard deviation is less than or equal to 0.5 percent, meeting the requirement, and taking an average value.
Obtaining the concentration C mg/L of PVA in each extracting solution to be detected according to a standard relation curve of the absorbance and the concentration of PVA, and then calculating to obtain the dissolution amount of PVA optical film samples produced by three different processes: z (mg/m)2) C × 1000 × 200/(150 × 1000 × 0.002 × 25) the results are shown in table 1.
TABLE 1
| Sample (I) | 1 | 2 | 3 |
| Absorbance of the solution | 1.747 | 2.142 | 1.278 |
| Amount of elution (mg/m)2) | 452.2 | 552.7 | 332.8 |
Experimental data show that the PVA film dissolution amount produced by different processes has obvious difference, so that the method can well reflect the PVA film dissolution amount and provide an index for the quality detection of the PVA optical film.
The above description is only exemplary of the present invention and should not be taken as limiting the invention, and any modifications, equivalents, improvements, etc. made within the spirit and principle of the present invention should be included in the scope of the present invention.
Claims (6)
1. A method for measuring the amount of PVA optical film released is characterized in that: soaking the PVA optical film to be detected in water to prepare an extracting solution to be detected; and taking a mixed solution of a boric acid solution and an iodine/potassium iodide solution as a developing solution, adding the developing solution into the extracting solution to be detected, then measuring the absorbance, and obtaining the concentration of PVA in the extracting solution to be detected according to a standard relation curve of the absorbance and the concentration of PVA, thereby calculating the dissolution amount of the PVA optical film.
2. The method of claim 1, comprising the steps of:
step 1, adding boric acid into water, and shaking up to obtain a boric acid solution; adding iodine and potassium iodide into water, and shaking uniformly to obtain an iodine-potassium iodide solution; mixing a boric acid solution and an iodine-potassium iodide solution to obtain a color developing solution;
step 2, cutting the PVA optical film to be tested to X m in area2The n pieces of (1) are used as samples to be detected; putting n samples to be detected into distilled water with the temperature of 10-40 ℃ and the volume of Y mL, and standing for 2-6h to obtain an extracting solution to be detected;
step 3, taking M mL of the color development solution obtained in the step 1, using the to-be-detected extracting solution to fix the volume to N mL, standing for 10-60min, and then using a spectrophotometer to determine absorbance A; obtaining the concentration C mg/L of PVA in the extracting solution to be detected according to a standard relation curve of the absorbance and the concentration of PVA, and then calculating according to a formula (1) to obtain the dissolution amount Z mg/m of the PVA optical film to be detected2：
Z＝C×Y×N/((N-M)×1000×X×n) (1)。
3. The method of claim 2, wherein: the standard relation curve of the absorbance and the PVA concentration is obtained according to the following method: preparing a series of PVA standard solutions with the concentration ranging from 10mg/L to 150 mg/L; respectively adding PVA standard solutions with various concentrations into the M mL of developing solution, fixing the volume to N mL, standing for 10-60min, and measuring the absorbance by using a spectrophotometer; and drawing a standard relation curve of the absorbance and the PVA concentration by taking the PVA solution concentration as an abscissa and the absorbance value as an ordinate.
4. The method of claim 2, wherein: in the step 1, the concentration of the boric acid solution is 20-50g/L, the concentration of iodine in the iodine-potassium iodide solution is 5-20g/L, the concentration of potassium iodide is 20-40g/L, and the volume ratio of the boric acid solution to the iodine-potassium iodide solution is 2-5: 1.
5. The method of claim 2, wherein: in step 2, the PVA optical film to be measured is cut to be round or square, and the area is not more than 0.01m2，n≥10。
6. A method according to claim 2 or 3, characterized in that: the detection wavelength of the spectrophotometer is 600-750 nm.
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| CN202010212168.4A CN111337442A (en) | 2020-03-24 | 2020-03-24 | Method for measuring PVA optical film dissolution amount |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112858084A (en) * | 2021-01-18 | 2021-05-28 | 安徽皖维高新材料股份有限公司 | Method for evaluating quality of PVA optical film |
| CN113884456A (en) * | 2021-10-14 | 2022-01-04 | 山东诚创蓝海医药科技有限公司 | Polyvinyl alcohol content determination and analysis method |
| CN114047181A (en) * | 2021-10-09 | 2022-02-15 | 万华化学集团股份有限公司 | Method for detecting PVA coating on surface of composite reverse osmosis membrane |
| CN115266966A (en) * | 2022-07-07 | 2022-11-01 | 重庆光谱新材料科技有限公司 | Method for detecting content of dissolved matter of polyvinyl alcohol film |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112858084A (en) * | 2021-01-18 | 2021-05-28 | 安徽皖维高新材料股份有限公司 | Method for evaluating quality of PVA optical film |
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| CN114047181A (en) * | 2021-10-09 | 2022-02-15 | 万华化学集团股份有限公司 | Method for detecting PVA coating on surface of composite reverse osmosis membrane |
| CN114047181B (en) * | 2021-10-09 | 2024-06-25 | 万华化学集团股份有限公司 | Method for detecting PVA coating on surface of composite reverse osmosis membrane |
| CN113884456A (en) * | 2021-10-14 | 2022-01-04 | 山东诚创蓝海医药科技有限公司 | Polyvinyl alcohol content determination and analysis method |
| CN115266966A (en) * | 2022-07-07 | 2022-11-01 | 重庆光谱新材料科技有限公司 | Method for detecting content of dissolved matter of polyvinyl alcohol film |
| CN115266966B (en) * | 2022-07-07 | 2024-05-07 | 重庆光谱新材料科技有限公司 | Method for detecting content of dissolved matter of polyvinyl alcohol film |
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