Quantitative Method for Surfactant in Color Film Developing Solution for TFT-LCD

Abstract

The present invention discloses a method for quantitatively determining surfactants in a color film developer for TFT-LCDs, which relates to the technical field of chemical detection. The method includes the following steps: S1: Prepare a 0.5 mol / L hydrochloric acid standard solution; S2: Calculate the concentration ω of KOH KOH ; Obtain the numerical values of the required parameters through steps S3-S4, and substitute them into the formula #imgabs0# in step S5 to obtain the content of surfactants in the color film developer. Beneficial effects: The detection method of the present invention has high accuracy, meeting the requirements of an absolute error ≤ 0.1% and a sample detection repeatability RSD ≤ 1%. The detection results of additives in different batches are reproducible, the detection process is simple to operate, the equipment investment is low, and there is no waste liquid generated, enabling the accurate and rapid detection of additives in the color film developer.

Description

Technical Field

[0001] The present invention relates to the technical field of chemical detection, and particularly relates to a method for quantitatively determining a surfactant in a color film developer for TFT-LCDs. Background Art

[0002] In the color film process of TFT-LCDs, negative photoresists are generally used. The main components of the photoresist are solvents, pigments (mainly G / R / B base color materials, BM / PS, etc.), dispersants, monomers (acrylic acid, styrene, acrylate monomers, etc.), polymers, and photoinitiators. Taking the development of negative photoresists as an example, first, the photoresist is coated, pre-baked, and exposed using a mask plate. In the area irradiated by ultraviolet light, the polymer generates free radicals by the photoinitiator to open the unsaturated double bonds and carry out cross-linking reactions. The alkali-soluble part in the un-irradiated negative photoresist can react with the KOH solution in the developer to dissolve the photoresist. Surfactants can increase the solubility of the photoresist and reduce the interfacial tension at the interface between the photoresist and the developer. The accuracy of the surfactant content will directly affect the development effect (such as whether there are development burrs or residues), affect the development time, and directly affect the yield and production capacity of the production line. Therefore, the quantitative accuracy of the surfactant in the color film developer directly affects the development effect and product yield.

[0003] The surfactant used in the color film developer is a polymer containing a benzene ring group. Its quantification can be carried out by using an ultraviolet spectrophotometer. The surfactant head group contains a benzene ring structure and has absorption in the ultraviolet region. At the maximum absorption wavelength of the surfactant, color film developers containing surfactants with different concentrations are prepared, and the absorbance is curve-fitted with the concentration to detect the content of the surfactant in the color film developer. However, the surfactant used in this method is a polymer. If accurate quantification is required, the molecular composition and distribution of each batch need to be consistent to ensure the accuracy of the detection results. However, in the actual production process, it is difficult to ensure the consistency of the surfactant in each batch. This method is applicable to the quantification of mixed surfactants with non-single structures, and other detection methods cannot achieve accurate quantification of mixed surfactants.

[0004] The Chinese patent application document with the publication number CN112698552A discloses a color film developer and its preparation method, which is composed of the following components in weight percentage: 1.0%-25.0% aqueous potassium hydroxide solution, 1.05%-20.00% surfactant, and the remaining component is ultrapure water. It is mainly used in the R, G, and B processes of color filters. It can develop the photoresist on the substrate surface. The color film developer of the present invention has good permeability to the photoresist, greatly increases the development efficiency, and at the same time weakens the adverse effects of metal ion impurities. The developed image has no other residues, meeting the requirements of high resolution and high picture quality in the current liquid crystal display process. However, this patent does not involve how to accurately detect the content of the surfactant in the color film developer. Summary of the Invention

[0005] The technical problem to be solved by the present invention is how to quickly and accurately measure the content of the surfactant in the color film developer.

[0006] The present invention realizes the solution of the above technical problem through the following technical means:

[0007] A method for quantifying additives in a color film developer for TFT-LCD, comprising the following steps:

[0008] S1: Prepare a 0.5 mol / L hydrochloric acid aqueous solution, and calibrate it with the reference substance anhydrous sodium carbonate to obtain a 0.5 mol / L hydrochloric acid standard solution;

[0009] Beneficial effects: Prepare a 0.5 mol / L hydrochloric acid standard solution, and obtain an accurate hydrochloric acid concentration through calibration with anhydrous sodium carbonate. This solution is also used to test the KOH content in the color film developer system and as a solvent for pretreatment before surfactant determination. Convert the KOH in the color film developer into potassium chloride, and achieve accurate quantification of the surfactant through the subsequent drying to constant weight process.

[0010] S2: Weigh a certain mass of the color film developer to be detected, denoted as m1, add 2-3 drops of phenolphthalein indicator (0.5% phenolphthalein ethanol solution), and titrate it with the hydrochloric acid standard solution obtained in step S1. Record the consumed volume when the solution changes from red to colorless, denoted as V1, and calculate the concentration of KOH in the color film developer according to formula (1-2) , and perform parallel tests twice, and take the average of the two times to obtain the concentration of KOH ;

[0011] Formula: …………………… (1-2);

[0012] In the formula: is the KOH concentration of the color film developer to be detected, in units of %;

[0013] V1 is the consumption volume when the hydrochloric acid standard solution titrates the KOH solution, with the unit of mL when the color of the phenolphthalein indicator changes from red to colorless;

[0014] m1 is the mass of the color film developing solution to be detected, with the unit of g;

[0015] S3: Weigh the mass of the acid and alkali resistant container after drying to constant weight, denoted as , weigh a certain mass of the color film developing solution to be detected again, denoted as m3, put it into the acid and alkali resistant container, and then add a certain volume of acid solution to the acid and alkali resistant container and mix evenly;

[0016] S4: Place the acid and alkali resistant container in step S3 on the heating equipment for heating. After the solution in the acid and alkali resistant container is evaporated to dryness, then place the acid and alkali resistant container in the oven for drying, weigh it after cooling, denoted as ;

[0017] S5: Substitute the , , , obtained in the above steps into formula (1 - 3) to obtain the content of the surfactant in the color film developing solution;

[0018] ………………(1 - 3);

[0019] In the formula:

[0020] is the mass of the acid and alkali resistant container after drying to constant weight, with the unit of g;

[0021] is the mass of the acid and alkali resistant container after evaporation to dryness and cooling after the acid addition reaction, with the unit of g;

[0022] is the mass of the color film developing solution to be detected, with the unit of g;

[0023] is the content of KOH in the color film developing solution to be detected obtained in step S2, with the unit of %;

[0024] is the molecular weight of potassium chloride, with the unit of g / mol;

[0025] is the molecular weight of potassium hydroxide, with the unit of g / mol;

[0026] is the content of the surfactant in the color film developing solution to be detected, with the unit of %.

[0027] Beneficial effects:

[0028] In the above steps S1 - S5 of the present invention, a hydrochloric acid standard solution is used. A fixed volume is added in one step, and the operation is fast and simple. After the hydrochloric acid solution is added to the system and mixed, a neutralization reaction occurs to eliminate the interference of KOH. After further drying to constant weight, the surfactant content is obtained by calculation using a formula. After the above process, the absolute error of the surfactant content detection result is ≤0.1%, and the RSD of parallel tests is ≤1%. After sampling from the color film developer production line, the surfactant content can be accurately quantified quickly.

[0029] Preferably, the method for calibrating with anhydrous sodium carbonate in step S1 includes the following steps:

[0030] (1) Place the reference substance anhydrous sodium carbonate in an oven at 270 °C and dry for 4 h. After taking it out, place it in a desiccator and cool for 1 h to room temperature;

[0031] (2) Weigh m0 (0.32 - 0.40 g) of the dried and cooled anhydrous sodium carbonate in a 100 mL small beaker. Under the DET - pH mode of an automatic potentiometric titrator, titrate with 0.5 mol / L. According to the consumption volume V2 at the second inflection point, calculate the hydrochloric acid concentration according to formula (1 - 1);

[0032] Formula: ………………………………(1 - 1)

[0033] In the formula: m0 is the mass of the weighed anhydrous sodium carbonate, unit g;

[0034] V2 is the consumption volume corresponding to the second inflection point in the process of calibrating hydrochloric acid with sodium carbonate, unit mL;

[0035] (3) The hydrochloric acid calibration requires 8 groups of parallel tests, and the relative standard deviation RSD of the data within the group is ≤0.2%. The average value is used as the final result of the hydrochloric acid calibration.

[0036] Preferably, the composition system of the color film developer to be detected in step S2 and step S3 is: the KOH content is 3 - 15%, the surfactant content is 4 - 20%, and the rest is high - purity water.

[0037] Preferably, the surfactant is selected from non - ionic surfactants.

[0038] Preferably, the non - ionic surfactant is one or a combination of fatty alcohol polyoxyethylene ether and alkylphenol polyoxyethylene ether.

[0039] Preferably, the number of ethylene oxide (EO) repeating units in the alkylphenol polyoxyethylene ether is between 9 and 15.

[0040] Preferably, the acid - and alkali - resistant container in step S3 is a high - purity copper crucible, a high - purity titanium crucible, or a high - purity gold crucible.

[0041] Preferably, the bottom of the acid and alkali resistant container in step S3 is flat, with an inner diameter of 50 - 80 mm, a thickness of 1 - 1.5 mm, and a height of 60 - 90 mm.

[0042] Preferably, after the acid and alkali resistant container in step S3 is dried to constant weight, it is stored in a desiccator for 30 min.

[0043] Preferably, the acid solution in step S3 is 0.5 mol / L hydrochloric acid solution.

[0044] Preferably, the addition amount of the acid in step S3 is 3 - 15% more than the theoretical addition amount, so that KOH is completely reacted to convert into potassium chloride salt.

[0045] Preferably, the addition amount of the acid in step S3 is 3 - 10% more than the theoretical addition amount.

[0046] Preferably, the heating device in step S4 is a constant temperature electric hot plate (the temperature uniformity of the hot plate is ±0.5 °C).

[0047] Preferably, the heating temperature of the heating device in step S4 is 140 - 170 °C, and the heating time is 25 - 35 min.

[0048] Preferably, the heating temperature of the heating device in step S4 is 150 - 160 °C.

[0049] Preferably, the temperature of the oven in step S4 is set at 100 - 120 °C, the drying time is 15 - 30 min, and the cooling time is 20 - 40 min.

[0050] Advantages of the present invention:

[0051] (1) In the above steps S1 - S5, by using a hydrochloric acid standard solution and adding a fixed volume in one step, the operation is fast and simple. After the hydrochloric acid solution is added to the system and mixed, a neutralization reaction occurs to eliminate the interference of KOH. After further drying to constant weight, the surfactant content is obtained by calculation using a formula. After the above process, the absolute error of the surfactant content detection result is ≤0.1%, and the RSD of parallel tests is ≤1%. After sampling from the color film developer production line, the surfactant content can be accurately and quickly quantified.

[0052] (2) The detection results of different batches of additives have reproducibility, the detection process is simple to operate, the equipment investment is low, and there is no waste liquid generated, which can realize the accurate and rapid detection of additives in the color film developer. Description of the Drawings

[0053] Figure 1 It is a linear relationship diagram of absorbance vs. surfactant concentration in Comparative Example 1. Detailed Embodiments

[0054] To make the objectives, technical solutions, and advantages of the embodiments of the present invention clearer, the following will, in conjunction with the embodiments of the present invention, clearly and completely describe the technical solutions in the embodiments of the present invention. Obviously, the described embodiments are some, but not all, of the embodiments of the present invention. All other embodiments obtained by those of ordinary skill in the art based on the embodiments of the present invention without creative efforts belong to the scope of protection of the present invention.

[0055] Example 1:

[0056] Prepare a color film developer sample 1:

[0057] Weigh non-ionic surfactant [alkylphenol polyoxyethylene ether (EO chain length 9 - 15)] m5 (8.0646 g), add high-purity water m6 (81.7736 g), and weigh 48.8% KOH solution m7 (8.2258 g). Mix evenly to obtain color film developer sample 1.

[0058] The KOH content in the solution is calculated according to formula (1 - 4), and the surfactant content is calculated according to formula (1 - 5).

[0059] ………………………… (1 - 4)

[0060] ………………………… (1 - 5)

[0061] In the formula:

[0062] and respectively represent the theoretical percentage contents of KOH and surfactant in the prepared color film developer;

[0063] represents the mass of the weighed surfactant, in g;

[0064] represents the mass of the weighed high-purity water, in g;

[0065] represents the mass of the weighed 48.8% potassium hydroxide solution, in g.

[0066] The KOH content in the color film developer sample 1 solution is calculated to be 4.09% according to formula (1 - 4), and the surfactant content is calculated to be 8.22% according to formula (1 - 5).

[0067] A method for quantitatively analyzing additives in a color film developer for TFT-LCDs includes the following steps:

[0068] KOH content test:

[0069] S1: Prepare a 0.5 mol / L hydrochloric acid aqueous solution and standardize it with the reference substance anhydrous sodium carbonate to obtain a 0.5 mol / L hydrochloric acid standard solution;

[0070] The method of standardizing with anhydrous sodium carbonate in step S1 includes the following steps:

[0071] (1) Place the reference substance anhydrous sodium carbonate in an oven at 270 °C for 4 h, take it out and place it in a desiccator to cool for 1 h to room temperature.

[0072] (2) Weigh m0 (0.32 - 0.40 g) of the dried and cooled anhydrous sodium carbonate in a 100 mL small beaker. Under the DET-pH mode of the automatic potentiometric titrator, titrate with 0.5 mol / L for calibration. According to the volume V2 consumed at the second inflection point, calculate the concentration of the hydrochloric acid standard solution according to the formula (1 - 1);

[0073] S2: Weigh about 5 g of the color film developer to be detected, denoted as m1 = 5.4213 g. Add 2 drops of phenolphthalein indicator and titrate with the hydrochloric acid standard solution obtained in step S1. When the solution changes from red to colorless, record the consumed volume as 7.86 mL, denoted as V1 = 7.86 mL. Calculate the concentration of KOH in the first color film developer according to the formula (1 - 2); = 4.07%;

[0074] Repeat the above steps. Weigh about 5 g of the color film developer to be detected, denoted as m1 = 5.3146 g. Add 2 drops of phenolphthalein indicator and titrate with the hydrochloric acid standard solution obtained in step S1. When the solution changes from red to colorless, record the consumed volume as 7.76 mL, denoted as V1 = 7.76 mL. Calculate the concentration of KOH in the second measured color film developer according to the formula (1 - 2); = 4.10%; Take the average of the two measurements to obtain the concentration of KOH = 4.08%;

[0075] Surfactant content detection:

[0076] S3: Weigh the mass of the high-purity titanium crucible after drying to a constant weight, denoted as = 88.0739 g. Weigh about 4 g of the color film developer to be detected, denoted as m3 = 4.0063 g, put it into the high-purity titanium crucible, and then add 6.1 mL of 0.5 mol / L hydrochloric acid solution to the high-purity titanium crucible and mix evenly;

[0077] S4: Place the high-purity titanium crucible in step S3 on a thermostatic hot plate for heating. The heating temperature is 160 °C and the heating time is 30 min. Then place the high-purity titanium crucible in an oven at 110 °C for drying for 20 min. After cooling for 30 min, weigh it and record it as = 88.6187 g;

[0078] S5: Substitute the , , , into the formula (1-3) to obtain the content of the surfactant in the color film developer;

[0079] Repeat the above steps S3 - S5 four times to obtain five test results. The specific test results are shown in Table 1:

[0080] Surfactant test conditions: Weigh about 4 g of the color film developer. Dry it on a hot plate at 160 °C for 30 min, dry it in a constant temperature oven at 110 °C for 20 min, cool it in a cooler for 30 min. The drying vessel is a high-purity titanium cup (purity > 99.99%). Add 6.1 ml of 0.5 mol / L hydrochloric acid aqueous solution (about 5% in excess). The surfactant content is calculated by substituting into formula (1-3). The results are shown in Table 1:

[0081] Table 1 Detection of the surfactant content in the self-prepared color film developer sample 1

[0082]

[0083] The absolute error of the product test result ≤ 0.1%, and the relative average standard deviation RSD of the 5 groups of parallel test results ≤ 1.0%. The accuracy and repeatability can both meet the requirements for surfactant quantification.

[0084] Example 2:

[0085] Prepare color film developer sample 2:

[0086] Weigh 5.1024 g of non-ionic surfactant [alkylphenol polyoxyethylene ether (EO chain length 9 - 15)], add 88.8264 g of high-purity water, and weigh 6.1735 g of 48.8% KOH solution. Mix evenly to prepare color film developer sample 2.

[0087] According to formulas (1-4) and (1-5) in Example 1, calculate that the KOH concentration in the solution is 3.01% and the surfactant content is 5.10%.

[0088] A method for quantifying additives in a color film developer for TFT-LCD, comprising the following steps:

[0089] KOH Content Test:

[0090] S1: Prepare an aqueous solution of 0.5 mol / L hydrochloric acid and standardize it with anhydrous sodium carbonate as the reference substance to obtain a 0.5 mol / L standard hydrochloric acid solution; the method of standardizing with anhydrous sodium carbonate in step S1 is the same as that in Example 1;

[0091] S2: Weigh about 8 g of the color film developer to be detected, denoted as m1 = 8.2634 g, add 2 drops of phenolphthalein indicator, and titrate with the standard hydrochloric acid solution obtained in step S1. Record the consumed volume as 8.96 mL when the solution changes from red to colorless, denoted as V1 = 8.96 mL. Calculate the concentration of KOH in the color film developer for the first measurement according to the formula (1 - 2) = 3.04%;

[0092] Repeat the above steps. Weigh about 8 g of the color film developer to be detected, denoted as m1 = 8.4636 g, add 2 drops of phenolphthalein indicator, and titrate with the standard hydrochloric acid solution obtained in step S1. Record the consumed volume as 9.10 mL when the solution changes from red to colorless, denoted as V1 = 9.10 mL. Calculate the concentration of KOH in the color film developer for the second measurement according to the formula (1 - 2) = 3.02%; Take the average of the two measurements to obtain the concentration of KOH = 3.03%;

[0093] Surfactant Content Detection:

[0094] S3: Weigh the mass of the high-purity titanium crucible after drying to a constant weight, denoted as = 88.1084 g. Weigh about 5 g of the color film developer to be detected, denoted as m3 = 5.0061 g, put it into the high-purity titanium crucible, and then add 4.7 mL of 0.5 mol / L hydrochloric acid solution to the high-purity titanium crucible and mix evenly;

[0095] S4: Place the high-purity titanium crucible in step S3 on a constant-temperature hot plate for heating. The heating temperature is 150 °C and the heating time is 30 min. Then place the high-purity titanium crucible in an oven at 110 °C for drying for 20 min, cool for 30 min and then weigh, denoted as = 88.6187 g;

[0096] S5: Substitute the , , , obtained in the above steps into the formula (1 - 3) to obtain the content of the surfactant in the color film developer;

[0097] Repeat the above steps S3 - S5 four more times to obtain five test results. The specific test results are shown in Table 2:

[0098] Test conditions: Dry at 150 °C on a hot plate for 30 min, dry in a constant temperature oven at 110 °C for 20 min, cool in a cooler for 30 min. Use a high - purity titanium cup (purity > 99.99%) for the drying vessel, about 5 g of color film developer, add 4.7 mL of 0.5 mol / L hydrochloric acid aqueous solution (excess by about 8%); calculate the surfactant content according to formula (1 - 3), and the results are shown in Table 2:

[0099] Table 2 Detection of surfactant content in the self - prepared color film developer sample 2

[0100]

[0101] It is preferred to control the hot - plate temperature at 150 - 160 °C, with a heating time of about 25 - 35 min. The absolute error of the test result is ≤0.1%, and the RSD ≤1%. Both the accuracy and repeatability can meet the requirements for surfactant quantification.

[0102] Example 3:

[0103] The difference between this example and Example 1 is that the KOH content in the prepared color film developer sample solution is 3% and the surfactant content is 4%. Other operation steps are the same as those in Example 1.

[0104] Example 4:

[0105] The difference between this example and Example 1 is that the KOH content in the prepared color film developer sample solution is 15% and the surfactant content is 20%. Other operation steps are the same as those in Example 1.

[0106] Example 5:

[0107] The difference between this example and Example 1 is that the non - ionic surfactant selected in the prepared color film developer sample solution is fatty alcohol polyoxyethylene ether. Other operation steps are the same as those in Example 1.

[0108] Example 6:

[0109] The difference between this example and Example 1 is that the non - ionic surfactant selected in the prepared color film developer sample solution is a mixture of fatty alcohol polyoxyethylene ether and alkylphenol polyoxyethylene ether. Other operation steps are the same as those in Example 1.

[0110] Example 7:

[0111] The difference between this example and Example 1 is that "high - purity titanium crucible" is changed to "high - purity copper crucible". Other operation steps are the same as those in Example 1.

[0112] Example 8:

[0113] The difference between this example and Example 1 is that "high-purity titanium crucible" is changed to "high-purity gold crucible", and other operation steps are the same as those in Example 1.

[0114] Example 9:

[0115] The difference between this example and Example 1 is that "high-purity titanium crucible" is changed to "high-purity gold crucible", and other operation steps are the same as those in Example 1.

[0116] Example 10:

[0117] The difference between this example and Example 1 is that "heating on a constant-temperature hot plate at a heating temperature of 150 °C" is changed to "heating on a constant-temperature hot plate at a heating temperature of 155 °C", and other operation steps are the same as those in Example 1.

[0118] Example 11:

[0119] The difference between this example and Example 1 is that "placing the high-purity titanium crucible in an oven at 110 °C for drying for 20 min and cooling for 30 min" is changed to "placing the high-purity titanium crucible in an oven at 100 °C for drying for 30 min and cooling for 20 min", and other operation steps are the same as those in Example 1.

[0120] Example 12:

[0121] The difference between this example and Example 1 is that "placing the high-purity titanium crucible in an oven at 110 °C for drying for 20 min and cooling for 30 min" is changed to "placing the high-purity titanium crucible in an oven at 120 °C for drying for 15 min and cooling for 40 min", and other operation steps are the same as those in Example 1.

[0122] Comparative Example 1:

[0123] Prepare a series of solutions of the color film developer sample 3:

[0124] Select 5 batches of non-ionic surfactants [alkylphenol polyoxyethylene ether (EO chain length 9 - 15)], weigh about 15 g of the surfactant, add about 74.7 g of high-purity water, and weigh about 10.3 g of 48.8% KOH solution to prepare five solutions with a composition of 5.0% KOH content and 15.0% surfactant content. The KOH content and surfactant content in each solution are calculated according to formulas (1-4) and (1-5), as shown in Table 3 below.

[0125] Table 3: Preparation of 5 batches of surfactant color film developer simulation solutions

[0126]

[0127] The five solutions from A to E in Table 3 were respectively detected by an ultraviolet spectrophotometer and subjected to acid treatment, followed by constant-temperature heating. The differences in the detection results between the two detection methods were compared.

[0128] 3.1 Detection of the surfactant content in the five color film developing solutions from A to E above by an ultraviolet spectrophotometer

[0129] Taking batch A as the standard solution mother liquor, it was diluted 229 times, 213 times, 199 times, 187 times, and 175 times with ultrapure water respectively to obtain standard stock solution dilutions. The scanning wavelength was adjusted to 260 nm, and ultrapure water was used as the blank. The absorbance of each diluted solution was measured, and a concentration curve of the surfactant was made through the absorbance, as Figure 1 shown.

[0130] The samples in groups ABCDE were diluted 200 times respectively to measure the absorbance values. According to the absorbance values, they were substituted into Figure 1 the fitting curve, and the surfactant concentration was calculated according to the dilution factor and calculation formula (1-6) as shown in Table 4. The difference between the measured value and the theoretical value of each solution is shown in Table 4.

[0131] ……………………(1-6)

[0132] In the formula:

[0133] The surfactant content in the color film developing solution calculated by ultraviolet spectrophotometric detection, unit %;

[0134] The absorbance of the diluted solution detected, unit Abs;

[0135] Represents the sample dilution factor.

[0136] Table 4 Comparison of the detection results and theoretical values of the surfactant content in the color film developing solution tested by ultraviolet spectrophotometry

[0137]

[0138] 3.2 Testing the surfactant content in the five color film developing solutions from A to E above by the constant-temperature heating method after pretreatment with hydrochloric acid

[0139] Test conditions for the constant-temperature heating method: Heat the hot plate at 160 °C for 25 min, dry it in a constant-temperature oven at 110 °C for 20 min, cool it in a cooler for 30 min. Use a high-purity titanium cup (purity > 99.99%) as the drying vessel, about 2.5 g of color film developer, calculate the KOH content according to 5.0%, and add 4.7 mL of 0.5 mol / L hydrochloric acid aqueous solution (excess about 5%). The additive content in the five color film developers A to E calculated according to formula (1-3) and the comparison with the theoretical values are shown in Table 5.

[0140] Table 5 Comparison of the detection results of the surfactant content in the color film developer for the constant-temperature heating test and the theoretical values

[0141]

[0142] The data comparison between Table 4 and Table 5 shows that after the pre-treatment of acidification of the color film developer, the absolute error of the results is ≤0.1% when the surfactant is detected by the constant-temperature drying method for different batches, and the detection results of the additives in different batches can meet the requirements of result reproducibility. The absolute error fluctuation detected by the ultraviolet spectrophotometer is relatively large, up to 1.27% at most, which cannot meet the quantitative requirements of the surfactant in the color film development.

[0143] The above embodiments are only used to illustrate the technical solutions of the present invention, not to limit it; although the present invention has been described in detail with reference to the foregoing embodiments, those of ordinary skill in the art should understand that they can still modify the technical solutions recorded in the foregoing embodiments, or perform equivalent replacements for some of the technical features; and these modifications or replacements do not make the essence of the corresponding technical solutions deviate from the spirit and scope of the technical solutions of the embodiments of the present invention.

Claims

1. A method for quantitatively determining a surfactant in a color film developing solution for TFT-LCD, characterized in that, Including the following steps: S1: Prepare a 0.5 mol / L hydrochloric acid aqueous solution, and standardize it with the reference substance anhydrous sodium carbonate to obtain a 0.5 mol / L hydrochloric acid standard solution; S2: Weigh a certain mass of the color film developer to be detected, denoted as , add 2 - 3 drops of phenolphthalein indicator, and titrate with the hydrochloric acid standard solution obtained in step S1. Record the consumed volume when the solution changes from red to colorless, denoted as V1. According to the formula , calculate the concentration of KOH in the color film developer . Conduct parallel tests twice and take the average of the two results to obtain the concentration of KOH ; S3: Weigh the mass of the acid and alkali resistant container after drying to constant weight, denoted as , weigh a certain mass of the color film developer to be tested, denoted as , put it into the acid and alkali resistant container, then add a certain volume of acid solution to the acid and alkali resistant container, and mix evenly; S4: Place the acid- and alkali-resistant container in step S3 on a heating device for heating, then place the acid- and alkali-resistant container in an oven for drying, weigh it after cooling, and record it as ; S5: Substitute the , , , into the formula to obtain the content of the surfactant in the color film developer; In the color film developer composition system to be detected in step S2 and step S3: the content of KOH is 3-15%, the content of surfactant is 4-20%, and the rest is high-purity water; The surfactant is alkylphenol polyoxyethylene ether; the number of ethylene oxide repeating units in the alkylphenol polyoxyethylene ether is between 9 and 15.

2. The method for quantifying surfactant in the color resist developer for TFT-LCD according to claim 1, characterized in that, The acid solution in step S3 is a 0.5 mol / L hydrochloric acid solution.

3. The method for quantifying surfactant in the color resist developer for TFT-LCD according to claim 1, characterized in that, The acid and alkali resistant container in step S3 is a high-purity copper crucible, a high-purity titanium crucible or a high-purity gold crucible.

4. The method for quantifying surfactants in the color film developing solution for TFT-LCD according to claim 1, characterized in that, The addition amount of the acid in step S3 is 3-10% more than the theoretical addition amount.

5. The method for quantifying surfactants in the color resist developer for TFT-LCD according to claim 1, characterized in that, The heating device in step S4 is a constant temperature electric hot plate.

6. The method for quantifying surfactants in the color film developer for TFT-LCD according to claim 1, characterized in that, The heating temperature of the heating device in step S4 is 150-160 °C.

7. The method for quantifying the surfactant in the color film developing solution for TFT-LCD according to claim 1, wherein In step S4, the temperature of the oven is set at 100-120 °C, the drying time is 15-30 min, and the cooling time is 20-40 min.

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