UV (ultraviolet) analysis method for nonionic surfactant in degumming mixed liquid

The content of nonionic surfactant in the glue removal mixture was detected by UV analysis, which solved the problem that the concentration range could not be accurately monitored in the prior art, and achieved the stability and capacity improvement of the COF Film production wet process.

CN119643486APending Publication Date: 2025-03-18HEFEI ESWIN MATERIALS TECH CO LTD
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Patent Information

Application Number
CN202411691228.X
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2024-11-25
Publication Date
2025-03-18

AI Technical Summary

Technical Problem

The prior art cannot accurately detect the content of nonionic surfactant in the glue removal mixture, resulting in the inability to monitor the concentration range and chemical addition in the COF Film production wet process, affecting process stability and production capacity.

Method used

UV analysis method was used to find the absorption wavelength corresponding to the absorption peaks of DA300K and PR glue through full-band scanning, establish a linear regression equation, and calculate the content of DA300K to be tested in the mixed liquid.

Benefits of technology

The accuracy of the analysis of each component of the glue removal liquid is achieved, and the replenishment and bath concentration is clearly determined, ensuring the stability of process capabilities and avoiding product defects and production capacity impacts.

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Abstract

The invention discloses a UV (ultraviolet) analysis method for a nonionic surfactant in a degumming mixed solution, which comprises the following steps: S1, carrying out full-wave-band scanning by utilizing ultraviolet light with specific wavelength which can be absorbed by organic matters, and finding out absorption wavelengths corresponding to absorption peak values of DA300K and PR glue; s2, performing ultraviolet scanning of different concentrations of DA300K under the found absorption wavelength, establishing a linear regression equation according to the concentration and the absorption value of DA300K, and analyzing a linear relation; s3, performing ultraviolet scanning of different concentrations of the PR adhesive under the absorption wavelength for full-wave band scanning and the absorption wavelength for full-wave band scanning and ultraviolet scanning, establishing a linear regression equation according to the absorption value of the PR adhesive under the absorption wavelength, and analyzing a linear relation; and step S4, obtaining an absorption value of the PR glue under the absorption wavelength by utilizing the linear relation in the step S3, and substituting the absorption value into a linear regression equation of DA300K so as to calculate the content of DA300K to be detected in the mixed solution. According to the invention, the process capability is ensured to be stable.
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Description

Technical Field

[0001] The invention relates to a UV analysis method for nonionic surfactant in a glue removal mixed liquid. Background Art

[0002] Nonionic surfactants are surfactants that contain ether groups that do not dissociate in aqueous solution as the main hydrophilic group in the molecule, and their surface activity is reflected by neutral molecules. Nonionic surfactants have high surface activity, good solubilization, washing, antistatic, calcium soap dispersion and other properties, low irritation, and excellent wetting and washing functions. In the wet process of COF Film (polyimide film) production, the glue removal process is involved. Nonionic surfactants can strip and coat the PR (photoresist) glue to reduce the defect of anti-sticking; they can also increase the penetration and emulsification ability to make the alkali solution easier to penetrate the circuit, but the content in the mixed liquid cannot be monitored, and in the process of maintaining process stability, it is impossible to monitor the required concentration range and the addition of chemicals such as bath building and adjustment, which cannot meet the production line production.

[0003] The main technical problems currently existing include: (1) It is impossible to detect the content of DA300K in the mixed liquid. Since the surface tension test is greatly affected by NaOH and PR glue, the accuracy and repeatability are low, the error is large, and the PR glue content cannot be determined. Therefore, the surface tension meter analysis production line is not applicable and cannot meet the production line production; (2) The corresponding liquid is configured according to the process requirements. First, its concentration is configured within a certain range. As the production reaction proceeds, the concentration will gradually deviate from the effective range. When it deviates from the target range, it will cause product defects and will also affect production capacity.

[0004] In the COF Film production process, for the analysis of each component in the degumming liquid, an innovative analysis method for non-ionic surfactants in the degumming mixture is introduced. Its concentration can be analyzed before, during and after production, and failure modes can be detected at the work station to avoid further processing; differential products will be controlled within an effective system to prevent these products from flowing out of the factory.

[0005] Therefore, a UV (ultraviolet light) analysis method for non-ionic surfactant in a degumming mixture is provided. Summary of the invention

[0006] The purpose of the present invention is to overcome the existing defects and provide a UV analysis method for non-ionic surfactants in a degumming mixture, clearly analyze the content of non-ionic surfactants in the degumming mixture, accurately analyze the components of the degumming solution in the wet process of COF Film production, clearly determine the amount of replenishment and the bath concentration, thereby ensuring the stability of the process capability.

[0007] The technical solution to achieve the above purpose is:

[0008] A UV analysis method for nonionic surfactants in a degumming mixture, comprising:

[0009] Step S1, using the fact that organic matter itself can absorb ultraviolet light of a specific wavelength, a full-band scan is performed to find the absorption wavelength corresponding to the absorption peak of DA300K and PR glue;

[0010] Step S2, performing UV scanning of DA300K at different concentrations at the found absorption wavelength, establishing a linear regression equation based on the concentration and absorption value of DA300K, and analyzing the linear relationship;

[0011] Step S3, performing UV scanning of PR glue of different concentrations at the absorption wavelength for full-band scanning and the absorption wavelength for full-band scanning and UV scanning, establishing a linear regression equation according to the absorption value of PR glue at the absorption wavelength, and analyzing the linear relationship;

[0012] Step S4, using the linear relationship in step S3 to obtain the absorption value of the PR glue at the absorption wavelength, and then substituting it into the linear regression equation of DA300K to calculate the content of the DA300K to be tested in the mixed solution.

[0013] Preferably, in step S1, the absorption wavelength found satisfies that DA300K has no absorption value at the absorption wavelength corresponding to the absorption peak of PR glue.

[0014] Preferably, in step S4, assuming that in step S3, the absorption wavelength for full-band scanning is A, and the absorption wavelength for ultraviolet scanning of different concentrations of DA300K under the absorption wavelength A is B, if the absorption wavelength is A, then the absorption value of DA300K in the mixed liquid is A1=A1(mixed liquid)-A1(PR glue), if the absorption wavelength is B, then the absorption value of DA300K in the mixed liquid is B1=B1(mixed liquid)-B1(PR glue).

[0015] Preferably, in step S4, the content of DA300K to be tested in the mixed solution is calculated according to the absorption value of the PR glue at the absorption wavelength, and the calculation formula is as follows:

[0016] DA300K content = ((A1-(B1+0.0154) / 0.5037)*100*specific gravity / m-0.0257) / 0.2292.

[0018] The beneficial effects of the present invention are as follows: the present invention clarifies the bath building scheme for the tank body, avoids the operators from adding the components of the liquid medicine at will, and improves the pass rate and speed of bath building; the concentration can be analyzed before, during and after production, and avoids the components of the degumming liquid exceeding the limit and specification to cause product defects; according to the concentration analysis of the process liquid medicine, the fixed-replenishment system automatically replenishes the components at a fixed time and in a fixed quantity according to the concentration of each component, which can maintain the stability of the liquid medicine at the process end and improve the fixed-replenishment stability rate. BRIEF DESCRIPTION OF THE DRAWINGS

[0019] Figure 1 It is a flow chart of a UV analysis method of a nonionic surfactant in a degumming mixed solution of the present invention;

[0020] Figure 2 The present invention uses the fact that organic matter itself can absorb ultraviolet light of a specific wavelength, and performs full-band scanning to obtain an absorption spectrum of the absorption wavelength corresponding to the absorption peak of DA300K;

[0021] Figure 3 The present invention utilizes the fact that organic matter itself can absorb ultraviolet light of a specific wavelength, and performs full-band scanning to obtain an absorption spectrum of the absorption wavelength corresponding to the absorption peak of the PR glue. DETAILED DESCRIPTION

[0022] The technical solution of the present invention will be described clearly and completely below in conjunction with the accompanying drawings. In the description of the present invention, it should be noted that the terms "center", "up", "down", "left", "right", "vertical", "horizontal", "inside", "outside" and the like indicate directions or positional relationships based on the directions or positional relationships shown in the accompanying drawings, which are only for the convenience of describing the present invention and simplifying the description, and do not indicate or imply that the device or element referred to must have a specific direction, be constructed and operated in a specific direction, and therefore cannot be understood as a limitation on the present invention. In addition, the terms "first", "second", and "third" are used for descriptive purposes only and cannot be understood as indicating or implying relative importance.

[0023] The present invention will be further described below in conjunction with the accompanying drawings.

[0024] The principle of UV-visible absorption of organic matter is related to the π electron system of the molecule. π electrons refer to the electrons involved in conjugated bonds and aromaticity in the molecule. When there are conjugated bonds or aromatic ring structures in organic matter, the π electrons in the molecule can form an extended π electron system; this extended π electron system can absorb light energy within the ultraviolet and visible light wavelength range, causing the electrons to transition from the ground state to the excited state; the more the π electron system is extended, the wavelength range of the absorbed light will also increase accordingly. Therefore, a UV analysis method for non-ionic surfactants in adhesive removal mixtures is provided.

[0025] like Figure 1 As shown, a UV analysis method for non-ionic surfactant in a degumming mixture comprises:

[0026] Step S1, using the fact that organic matter itself can absorb ultraviolet light of a specific wavelength, a full-band scan is performed to find out the absorption wavelength corresponding to the absorption peak of DA300K and PR glue.

[0027] In the embodiment, the absorption wavelength found satisfies that DA300K has no absorption value at the absorption wavelength corresponding to the absorption peak of the PR glue.

[0028] Step S2, performing UV scanning of DA300K at different concentrations at the found absorption wavelength, establishing a linear regression equation based on the concentration and absorption value of DA300K, and analyzing the linear relationship.

[0029] Step S3, performing UV scanning of PR glue of different concentrations at the absorption wavelength for full-band scanning and the absorption wavelength for full-band scanning and UV scanning, establishing a linear regression equation according to the absorption value of PR glue at the absorption wavelength, and analyzing the linear relationship.

[0030] Step S4, using the linear relationship in step S3 to obtain the absorption value of the PR glue at the absorption wavelength, and then substituting it into the linear regression equation of DA300K to calculate the content of the DA300K to be tested in the mixed solution.

[0031] In the embodiment, it is assumed that in step S3, the absorption wavelength for full-band scanning is A, and the absorption wavelength for ultraviolet scanning of different concentrations of DA300K under the absorption wavelength A is B. If the absorption wavelength is A, the absorption value of DA300K in the mixed liquid is A1=A1(mixed liquid)-A1(PR glue). If the absorption wavelength is B, the absorption value of DA300K in the mixed liquid is B1=B1(mixed liquid)-B1(PR glue).

[0032] In the embodiment, the content of DA300K to be tested in the mixed solution is calculated according to the absorption value of the PR glue at the absorption wavelength, and the calculation formula is as follows:

[0033] DA300K content = ((A1-(B1+0.0154) / 0.5037)*100*specific gravity / m-

[0034] 0.0257) / 0.2292.

[0035] In the embodiment, if the absorption wavelengths found are 279.5 nm and 341 nm, Figure 2 , 3 As shown, the linear relationship in step S3 is used to obtain the absorption value of PR glue at a wavelength of 279.5nm, and the absorption value of DA300K in the mixed solution A 279.5 =A(mixed solution 279.5nm)-A(PR glue 279.5nm); the absorption value of PR glue at 341nm wavelength, the absorption value of DA300K in the mixed solution A 341 =A(mixed solution 341nm)-A(PR glue 341nm); then the content of DA300K to be tested in the mixed solution (%) = ((A 279.5 -(A 341+0.0154) / 0.5037)*100*specific gravity / m-0.0257) / 0.2292.

[0036] The specific experimental steps are as follows:

[0037] a. Accurately weigh 10 ml of sample into a 100 ml volumetric flask, dilute to the mark with purified water, and shake well;

[0038] b. Rinse the cuvette 3 times with purified water;

[0039] c. Use a dust-free cloth to wipe the surface of the cuvette dry (smooth surface), and return to zero with purified water at 341nm;

[0040] d. Rinse the cuvette 3 times with the sample to be tested, add the sample to be tested, wipe the surface of the cuvette (smooth surface), put it into the sample chamber, click START, test, and record data;

[0041] e. Rinse the cuvette 3 times with purified water;

[0042] f. Use a dust-free cloth to wipe the surface of the cuvette dry (smooth surface), and return to zero with purified water at 279.5nm;

[0043] g. Rinse the cuvette 3 times with the sample to be tested, add the sample to be tested, wipe the surface of the cuvette (smooth surface), put it into the sample chamber, click START, test, and record data;

[0044] h. Substitute the values ​​at the two wavelengths into the formula to obtain the data.

[0045] The above embodiments are only used to illustrate the technical solutions of the present invention, rather than to limit the same. Although the present invention has been described in detail with reference to the above embodiments, those skilled in the art should understand that the technical solutions described in the above embodiments may still be modified, or some or all of the technical features may be replaced by equivalents. However, these modifications or replacements do not deviate the essence of the corresponding technical solutions from the scope of the technical solutions of the embodiments of the present invention.

Claims

1. A UV analysis method for nonionic surfactants in a degumming mixture, characterized in that: include: Step S1, using the fact that organic matter itself can absorb ultraviolet light of a specific wavelength, a full-band scan is performed to find the absorption wavelength corresponding to the absorption peak of DA300K and PR glue; Step S2, performing UV scanning of DA300K at different concentrations at the found absorption wavelength, establishing a linear regression equation based on the concentration and absorption value of DA300K, and analyzing the linear relationship; Step S3, performing UV scanning of PR glue of different concentrations at the absorption wavelength for full-band scanning and the absorption wavelength for full-band scanning and UV scanning, establishing a linear regression equation according to the absorption value of PR glue at the absorption wavelength, and analyzing the linear relationship; Step S4, using the linear relationship in step S3 to obtain the absorption value of the PR glue at the absorption wavelength, and then substituting it into the linear regression equation of DA300K to calculate the content of the DA300K to be tested in the mixed solution.

2. The UV analysis method of nonionic surfactant in a degumming mixture according to claim 1, characterized in that: In the step S1, the absorption wavelength found satisfies that DA300K has no absorption value at the absorption wavelength corresponding to the absorption peak of the PR glue.

3. The UV analysis method of nonionic surfactant in a degumming mixture according to claim 1, characterized in that: In step S4, it is assumed that in step S3, the absorption wavelength for full-band scanning is A, and the absorption wavelength for ultraviolet scanning of different concentrations of DA300K under the absorption wavelength A is B. If the absorption wavelength is A, the absorption value of DA300K in the mixed liquid is A1=A1(mixed liquid)-A1(PR glue), and if the absorption wavelength is B, the absorption value of DA300K in the mixed liquid is B1=B1(mixed liquid)-B1(PR glue).

4. The UV analysis method of nonionic surfactant in a degumming mixture according to claim 3, characterized in that: In step S4, the content of DA300K to be tested in the mixed solution is calculated according to the absorption value of the PR glue at the absorption wavelength, and the calculation formula is as follows: DA300K content = ((A1-(B1+0.0154) / 0.5037)*100*specific gravity / m- 0.0257) / 0.2292。