CN111103366A - Method for detecting cross-linking agent in EVA photovoltaic film - Google Patents
Method for detecting cross-linking agent in EVA photovoltaic film Download PDFInfo
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Abstract
The invention discloses a method for detecting a cross-linking agent in an EVA photovoltaic film, which comprises the following steps: the method comprises the following steps: obtaining a characterization test chart of a cross-linking agent standard sample; step two: dissolving an EVA photovoltaic film sample by using a solvent to obtain a solution to be detected; step three: and (4) performing instrument analysis on the solution to be tested obtained in the step two, comparing the characterization test chart of the cross-linking agent standard sample obtained in the step one, and performing qualitative and quantitative analysis on the cross-linking agent in the EVA photovoltaic film. The detection method of the cross-linking agent in the EVA photovoltaic film can be used for carrying out qualitative analysis and highly accurate quantitative analysis on the triallyl isocyanurate in the EVA photovoltaic film. Meanwhile, the detection method of the cross-linking agent in the EVA photovoltaic film has higher anti-interference performance, and can eliminate the interference of other cross-linking agents on the testing result of triallyl isocyanurate; the method has extremely high reproducibility and excellent practical application and popularization values.
Description
Technical Field
The invention relates to the field of a detection method of a cross-linking agent, in particular to a detection method of a cross-linking agent in an EVA photovoltaic film.
Background
With the wide application of the EVA photovoltaic film material, the types of the cross-linking agents used in the system are more and more. Triallyl isocyanurate is a high molecular weight monomer of multifunctional olefin containing aromatic heterocycle, which has wide application, and is mainly used as a cross-linking agent and an auxiliary cross-linking agent of various thermoplastic materials, ion exchange resin and special rubber. The determination of the content is also of great significance.
At present, a common method for determining the content of triallyl isocyanurate is a gas chromatography or gas chromatography-mass spectrometry combined method, and because the boiling point of triallyl isocyanurate is high, the prior art usually uses a high column temperature to achieve the detection purpose, but the self-polymerization of triallyl isocyanurate is caused, the accuracy of the analysis result is not high, and the reproducibility is poor. Meanwhile, in the prior art, solvents such as toluene, chloroform and the like are generally adopted to dissolve, precipitate or extract the EVA photovoltaic membrane material, so that the used auxiliary agents are left in soluble substances, but because the crosslinking agent in the EVA photovoltaic membrane material often contains components such as triallyl isocyanurate, a peroxide crosslinking agent and the like, the triallyl isocyanurate is easy to self-polymerize, the peroxide is active in nature, is greatly influenced by temperature, is unstable and easy to decompose, and can also have certain influence on the quantitative and qualitative result of the triallyl isocyanurate. Therefore, a method for detecting the cross-linking agent in the EVA photovoltaic film with high accuracy, strong anti-interference performance and high reproducibility is needed.
Disclosure of Invention
In order to solve the technical problem, the invention provides a method for detecting a cross-linking agent in an EVA photovoltaic film, which comprises the following steps:
the method comprises the following steps: obtaining a characterization test chart of a cross-linking agent standard sample;
step two: dissolving an EVA photovoltaic film sample by using a solvent to obtain a solution to be detected;
step three: and (4) performing instrument analysis on the solution to be tested obtained in the step two, comparing the characterization test chart of the cross-linking agent standard sample obtained in the step one, and performing qualitative and quantitative analysis on the cross-linking agent in the EVA photovoltaic film.
As a preferred technical scheme, the solvent of the second step is acetone and/or triethanolamine.
As a preferred technical solution, the weight ratio of acetone to triethanolamine is 1: (0.3-0.4).
As a preferred technical scheme, the instrumental analysis in the third step is HS-GCMS and/or GCMS.
As a preferable technical scheme, the temperature rising program of the GCMS or the HS-GCMS is as follows: keeping the initial temperature at 60-80 ℃ for 1-3 min, raising the temperature to 90-110 ℃ at 4-6 ℃/min, raising the temperature to 110-130 ℃ at 3-5 ℃/min, keeping the temperature for 4-6 min, raising the temperature to 140-160 ℃ at 4-6 ℃/min, and keeping the temperature for 1-3 min.
As a preferred technical scheme, the mass spectrum conditions of GCMS or HS-GCMS are as follows: the ion source E1 has ionization energy of 70eV, ion source temperature of 160-200 ℃, quadrupole rod temperature of 140-160 ℃ and scanning mass range of 40-1000 amu.
As a preferred technical scheme, the headspace condition of the HS-GCMS is as follows: the equilibrium temperature is 90-110 ℃, and the equilibrium time is 20-40 min.
As a preferable technical scheme, the testing sequence of the instrument analysis is that HS-GCMS is firstly used for qualitative analysis, and then GCMS is used for quantitative analysis.
As a preferred technical solution, the crosslinking agent in the EVA photovoltaic film includes triallyl isocyanurate.
As a preferable technical scheme, the crosslinking agent in the EVA photovoltaic film also comprises one or more of 1, 1-di-tert-butylperoxy-3, 3, 5-trimethylcyclohexane, 2, 5-dimethyl-2, 5-di- (tert-butylperoxy) hexane and tert-butylperoxy-2-ethylhexyl carbonate.
Has the advantages that: the detection method of the cross-linking agent in the EVA photovoltaic film can perform qualitative analysis and highly accurate quantitative analysis on the triallyl isocyanurate in the EVA photovoltaic film, and can also perform accurate qualitative analysis on other cross-linking agents in the EVA photovoltaic film, such as 1, 1-di-tert-butylperoxy-3, 3, 5-trimethylcyclohexane, 2, 5-dimethyl-2, 5-di- (tert-butylperoxy) hexane and tert-butylperoxy carbonic acid-2-ethylhexyl ester. Meanwhile, the detection method of the cross-linking agent in the EVA photovoltaic film has higher anti-interference performance, and can eliminate the interference of other cross-linking agents on the testing result of triallyl isocyanurate; the method has extremely high reproducibility and excellent practical application and popularization values.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, and it is obvious that the drawings in the following description are some embodiments of the present invention, and other drawings can be obtained by those skilled in the art without creative efforts.
FIG. 1: an HS-GCMS spectrogram of an EVA photovoltaic film sample used in example 1 of the invention;
FIG. 2: GCMS spectrum of the EVA photovoltaic film sample used in example 1 of the present invention.
Detailed Description
The technical features of the technical solutions provided by the present invention are further clearly and completely described below with reference to the specific embodiments, and the scope of protection is not limited thereto.
The words "preferred", "more preferred", and the like, in the present invention refer to embodiments of the invention that may provide certain benefits, under certain circumstances. However, other embodiments may be preferred, under the same or other circumstances. Furthermore, the recitation of one or more preferred embodiments does not imply that other embodiments are not useful, nor is it intended to exclude other embodiments from the scope of the invention.
In order to solve the technical problem, the invention provides a method for detecting a cross-linking agent in an EVA photovoltaic film, which comprises the following steps:
the method comprises the following steps: obtaining a characterization test chart of a cross-linking agent standard sample;
step two: dissolving an EVA photovoltaic film sample by using a solvent to obtain a solution to be detected;
step three: and (4) performing instrument analysis on the solution to be tested obtained in the step two, comparing the characterization test chart of the cross-linking agent standard sample obtained in the step one, and performing qualitative and quantitative analysis on the cross-linking agent in the EVA photovoltaic film.
< step one >
In a preferred embodiment, the first step is: and obtaining a characterization test chart of the cross-linking agent standard sample.
The cross-linking agent standard sample, namely the standard test sample, can be obtained by commercial purchase; in the invention, the solvent used for obtaining the characterization test pattern of the cross-linking agent standard sample in the step one is the same as the solvent used for dissolving the sample in the step two.
In a more preferred embodiment, the crosslinker standard comprises a triallyl isocyanurate standard.
In a further preferred embodiment, the crosslinker standard further comprises one standard of 1, 1-bis-tert-butylperoxy-3, 3, 5-trimethylcyclohexane, 2, 5-dimethyl-2, 5-bis- (tert-butylperoxy) hexane, 2-ethylhexyl tert-butylperoxycarbonate.
The triallyl isocyanurate, also known as triallyl isocyanurate, has CAS number 1025-15-6, TAIC for short, and is purchased from Shanghai Yan Biotech Co., Ltd.
The 1, 1-di-tert-butylperoxy-3, 3, 5-trimethylcyclohexane has a CAS number of 6731-36-8 and is purchased from Shanghai Yan Biotech Co., Ltd.
The 2, 5-dimethyl-2, 5-bis- (t-butylperoxy) hexane, commonly known as bis-di-penta, CAS number 78-63-7, was purchased from Baishun Biotech, Inc., Shanghai.
The tert-butyl peroxy carbonic acid-2-ethylhexyl ester is TBEC for short, has CAS number of 34443-12-4, and is purchased from Tai Fuji chemical Co.
In a preferred embodiment, the test method for the characterization test pattern of the cross-linker standard sample is GCMS and/or HS-GCMS.
In a more preferred embodiment, the test methods for characterizing test patterns of the crosslinker standard sample are GCMS and HS-GCMS.
The GCMS, Gas chromatography mass spectrometry (Gas chromatography).
The HS-GCMS is a headspace-gas chromatography-mass spectrometer.
GCMS/HS-GCMS
In a preferred embodiment, the GCMS or HS-GCMS column is a siloxane column.
In a preferred embodiment, the siloxane chromatography column is selected from one or more of a dimethylpolysiloxane column, a diphenylvinyl dimethylpolysiloxane column, and a diphenyldimethylpolysiloxane column.
In a more preferred embodiment, the siloxane chromatography column is a diphenyldimethylpolysiloxane column.
The diphenyldimethylpolysiloxane column was an AC-5 capillary column (30 m. times.0.32 mm. times.0.25 μm) from SGE Analytical Science, Australia.
In a preferred embodiment, the GC conditions of GCMS or HS-GCMS are: column flow rate: 1.0 mL/min; sample introduction amount: 1.0 μ L; the temperature of a sample inlet is 200 ℃; the carrier gas is He, and the concentration is 1.0 mL/min; the split ratio is 30: 1.
in a preferred embodiment, the temperature raising program of the GCMS or the HS-GCMS is as follows: keeping the initial temperature at 60-80 ℃ for 1-3 min, raising the temperature to 90-110 ℃ at 4-6 ℃/min, raising the temperature to 110-130 ℃ at 3-5 ℃/min, keeping the temperature for 4-6 min, raising the temperature to 140-160 ℃ at 4-6 ℃/min, and keeping the temperature for 1-3 min.
In a more preferred embodiment, the temperature increase procedure of the GCMS or HS-GCMS is: the initial temperature is maintained at 70 deg.C for 2min, then the temperature is raised to 100 deg.C at 5 deg.C/min, then raised to 120 deg.C at 4 deg.C/min, and after 5min, the temperature is raised to 150 deg.C at 5 deg.C/min, and then maintained for 2 min.
In a preferred embodiment, the mass spectrometric conditions of GCMS or HS-GCMS are: the ion source E1 has ionization energy of 70eV, ion source temperature of 160-200 ℃, quadrupole rod temperature of 140-160 ℃ and scanning mass range of 40-1000 amu.
In a more preferred embodiment, the mass spectrometric conditions of GCMS or HS-GCMS are: and (3) an ion source E1, wherein the ionization energy is 70eV, the ion source temperature is 180 ℃, the quadrupole rod temperature is 150 ℃, and the scanning mass range is 40-1000 amu.
In a preferred embodiment, the headspace conditions in the HS-GCMS are: the equilibrium temperature is 90-110 ℃, and the equilibrium time is 20-40 min.
In a more preferred embodiment, the headspace conditions in the HS-GCMS are: the equilibrium temperature is 100 ℃ and the equilibrium time is 30 min.
< step two >
In a preferred embodiment, the second step is: and dissolving the EVA photovoltaic film sample by using a solvent to obtain a solution to be detected.
In a preferred embodiment, the solvent of step two is acetone and/or triethanolamine.
In a more preferred embodiment, the solvent of step two is a mixture of acetone and triethanolamine.
In a preferred embodiment, the weight ratio of acetone to triethanolamine is 1: (0.3-0.4).
In a more preferred embodiment, the weight ratio of acetone to triethanolamine is 1: 0.35.
in the prior art, solvents such as toluene, chloroform and the like are generally adopted to dissolve, precipitate or extract the EVA photovoltaic membrane material, so that the used auxiliary agents are left in soluble substances, but because the crosslinking agent in the EVA photovoltaic membrane material often comprises components such as triallyl isocyanurate, a peroxide crosslinking agent and the like, the triallyl isocyanurate is easy to self-polymerize, and the peroxide is active in nature, is greatly influenced by temperature, is unstable and is easy to decompose, and can influence the quantitative and qualitative result of the triallyl isocyanurate to a certain extent.
The inventor finds that in the development process, when the solvent used by the EVA photovoltaic film sample is a mixture of acetone and triethanolamine, and the weight ratio of the acetone to the triethanolamine is 1: (0.3-0.4), the accuracy of the final test result is improved to a certain extent. The inventor conjectures that when acetone and triethanolamine are added in a certain proportion, the triethanolamine can improve the capability of acetone penetrating into the EVA photovoltaic film to a certain extent, and a solution to be detected with a certain concentration of the cross-linking agent can be obtained without dissolving, precipitating or extracting; meanwhile, a certain amount of triethanolamine is added, so that the dissolution of EVA components in the EVA photovoltaic film can be reduced to a certain extent, and the test error is reduced. When the amount of acetone is too much, the mixture of acetone and triethanolamine is easy to generate a layering phenomenon, which is not beneficial to the dissolution of the cross-linking agent; when the amount of triethanolamine is excessive, excessive tertiary amine groups are introduced into the donor system, so that the amount of other components in the liquid to be tested is obviously increased, and the accuracy of the test result is influenced.
< step three >
In a preferred embodiment, the third step is: and (4) performing instrument analysis on the solution to be tested obtained in the step two, comparing the characterization test chart of the cross-linking agent standard sample obtained in the step one, and performing qualitative and quantitative analysis on the cross-linking agent in the EVA photovoltaic film.
In a more preferred embodiment, the crosslinker in the EVA photovoltaic film comprises triallyl isocyanurate.
In a further preferred embodiment, the crosslinking agent in the EVA photovoltaic film further comprises one or more of 1, 1-di-tert-butylperoxy-3, 3, 5-trimethylcyclohexane, 2, 5-dimethyl-2, 5-bis- (tert-butylperoxy) hexane, and 2-ethylhexyl tert-butylperoxycarbonate in combination.
(Instrument analysis)
In a preferred embodiment, the instrumental analysis in step three is HS-GCMS and/or GCMS.
The HS-GCMS and/or GCMS test method in the third step adopts the same limitation as the first step.
The inventor finds that through a great deal of failed experimental exploration, continuous summarization and improvement, when a siloxane chromatographic column, particularly a diphenyl dimethylpolysiloxane column, is adopted as a chromatographic column of GCMS or HS-GCMS, and specific GC conditions, a temperature rise program, mass spectrum conditions and headspace conditions are adopted, the accuracy of a final test result is further improved, and the anti-interference performance is improved. The inventors speculate that the possible reason is that the residual EVA component in the liquid to be tested can be adsorbed to a certain extent by using the siloxane chromatographic column and specific test conditions, so that the purity of the cross-linking agent component in the test result is increased; meanwhile, specific test conditions are favorable for vaporization and separation of different cross-linking agent components in the liquid to be tested and different interactions with the siloxane chromatographic column, so that different cross-linking agent components are subjected to peak emergence more accurately, and the anti-interference performance of the test is improved.
In a more preferred embodiment, the instrumental analysis in step three is HS-GCMS and GCMS.
In a further preferred embodiment, the instrumental analysis is performed in a test sequence using qualitative analysis using HS-GCMS followed by quantitative analysis using GCMS.
The invention finds out in the development process that the weight ratio of the raw materials is 1: (0.3-0.4) dissolving the EVA photovoltaic film sample by using a mixture of acetone and triethanolamine as a solvent, simultaneously performing HS-GCMS and GCMS linkage analysis, and adopting a siloxane chromatographic column and specific GC conditions, a heating program, mass spectrum conditions and headspace conditions, so that the accuracy of a test result is improved, the anti-interference performance is further improved, and the repeatability is also remarkably improved. The inventor believes that after the EVA photovoltaic film sample is dissolved by acetone and triethanolamine in a specific proportion, the dissolution of impurities in the sample is reduced, and the concentration of a cross-linking agent in a liquid to be detected is improved; the siloxane chromatographic column, the specific GC condition, the temperature-raising program, the mass spectrum condition and the headspace condition are adopted, so that different cross-linking agent components in the liquid to be tested are vaporized and separated, and the purity of the cross-linking agent components is increased, so that the peaks of the different cross-linking agent components are more accurate, and the anti-interference performance of the test is improved; meanwhile, HS-GCMS and GCMS linkage analysis methods are adopted, after HS-GCMS testing is carried out, partial fragment information or complete molecular structure information of all cross-linking agent components can be obtained relatively accurately, so that the cross-linking agent can be analyzed qualitatively and accurately, and all cross-linking agent components in a sample to be tested can be judged as accurately as possible; and GCMS tests performed on the basis can eliminate the interference of other components, and the triallyl isocyanurate is accurately and quantitatively analyzed by an instrument external standard method. When only GCMS test is carried out, the interference component in the cross-linking agent can not be measured, so that the triallyl isocyanurate in the cross-linking agent can not be accurately and quantitatively analyzed; when only HS-GCMS is carried out, only part of the cross-linking agent components can be quantitatively analyzed, and the structural information of the complete triallyl isocyanurate molecules cannot be obtained and can be accurately and qualitatively analyzed.
The present invention will now be described in detail by way of examples, and the starting materials used are commercially available unless otherwise specified.
Examples
Example 1
the method comprises the following steps: obtaining GCMS and HS-GCMS characterization test charts of a crosslinking agent triallyl isocyanurate standard sample and a 1, 1-di-tert-butylperoxy-3, 3, 5-trimethylcyclohexane standard sample;
step two: the weight ratio of acetone to triethanolamine used for an EVA photovoltaic film sample is 1: dissolving the mixture of 0.35 to obtain a solution to be detected;
step three: and qualitatively analyzing the solution to be detected obtained in the second step by using HS-GCMS compared with the characterization test chart of the cross-linking agent standard sample obtained in the first step, and then quantitatively analyzing the solution to be detected by using GCMS through an external standard method of an instrument.
Wherein the column of GCMS or HS-GCMS in step one and step three is a diphenyldimethylpolysiloxane column, an AC-5 capillary column (30 m. times.0.32 mm. times.0.25 μm) from SGE Analytical Science, Australia. The GC conditions of the GCMS or the HS-GCMS in the first step and the third step are as follows: column flow rate: 1.0 mL/min; sample introduction amount: 1.0 μ L; the temperature of a sample inlet is 200 ℃; the carrier gas is He, and the concentration is 1.0 mL/min; the split ratio is 30: 1. the temperature rise program of the GCMS or the HS-GCMS is as follows: the initial temperature is maintained at 70 deg.C for 2min, then the temperature is raised to 100 deg.C at 5 deg.C/min, then raised to 120 deg.C at 4 deg.C/min, and after 5min, the temperature is raised to 150 deg.C at 5 deg.C/min, and then maintained for 2 min. The mass spectrum conditions of the GCMS or the HS-GCMS in the first step and the third step are as follows: and (3) an ion source E1, wherein the ionization energy is 70eV, the ion source temperature is 180 ℃, the quadrupole rod temperature is 150 ℃, and the scanning mass range is 40-1000 amu. The headspace conditions in the HS-GCMS in the first step and the third step are as follows: the equilibrium temperature is 100 ℃ and the equilibrium time is 30 min.
The preparation raw materials of the EVA photovoltaic film sample used in this example are: 99.4 wt% of ethylene-vinyl acetate copolymer, 0.1 wt% of triallyl isocyanurate and 0.5 wt% of 1, 1-di-tert-butylperoxy-3, 3, 5-trimethylcyclohexane. The preparation method comprises the following steps: adding the preparation raw materials into methanol at 70 ℃, uniformly mixing, continuously stirring for 4h, filtering, drying and discharging to obtain the EVA photovoltaic film sample.
The ethylene-vinyl acetate copolymer used in this example, EVA resin, CAS number 24937-78-8, is 3155 from DuPont, USA. The triallyl isocyanurate, CAS number 1025-15-6, was purchased from Shanghai, screening Biotech, Inc. The 1, 1-di-tert-butylperoxy-3, 3, 5-trimethylcyclohexane has a CAS number of 6731-36-8 and is purchased from Shanghai Yan Biotech Co., Ltd.
Example 2
Embodiment 2 of the present invention provides a method for detecting a crosslinking agent in an EVA photovoltaic film, including the following steps:
the method comprises the following steps: obtaining GCMS and HS-GCMS characterization test charts of a crosslinking agent triallyl isocyanurate standard sample and a 1, 1-di-tert-butylperoxy-3, 3, 5-trimethylcyclohexane standard sample;
step two: the weight ratio of acetone to triethanolamine used for an EVA photovoltaic film sample is 1: dissolving the mixture of 0.3 to obtain a solution to be detected;
step three: and qualitatively analyzing the solution to be detected obtained in the second step by using HS-GCMS compared with the characterization test chart of the cross-linking agent standard sample obtained in the first step, and then quantitatively analyzing the solution to be detected by using GCMS through an external standard method of an instrument.
Wherein the column of GCMS or HS-GCMS in step one and step three is a diphenyldimethylpolysiloxane column, an AC-5 capillary column (30 m. times.0.32 mm. times.0.25 μm) from SGE Analytical Science, Australia. The GC conditions of the GCMS or the HS-GCMS in the first step and the third step are as follows: column flow rate: 1.0 mL/min; sample introduction amount: 1.0 μ L; the temperature of a sample inlet is 200 ℃; the carrier gas is He, and the concentration is 1.0 mL/min; the split ratio is 30: 1. the temperature rise program of the GCMS or the HS-GCMS is as follows: the initial temperature is maintained at 60 ℃ for 1min, then the temperature is increased to 90 ℃ at 4 ℃/min, then the temperature is increased to 110 ℃ at 3 ℃/min, the temperature is increased to 140 ℃ at 4 ℃/min after the temperature is maintained for 4min, and the temperature is maintained for 1 min. The mass spectrum conditions of the GCMS or the HS-GCMS in the first step and the third step are as follows: ion source E1, ionization energy 70eV, ion source temperature 160 ℃, quadrupole temperature 140 ℃, scanning mass range 40 amu. The headspace conditions in the HS-GCMS in the first step and the third step are as follows: the equilibration temperature is 90 ℃ and the equilibration time is 20 min.
The EVA photovoltaic film sample used in this example was the same as the example sample.
The ethylene-vinyl acetate copolymer used in this example, EVA resin, CAS number 24937-78-8, is 3155 from DuPont, USA. The triallyl isocyanurate, CAS number 1025-15-6, was purchased from Shanghai, screening Biotech, Inc. The 1, 1-di-tert-butylperoxy-3, 3, 5-trimethylcyclohexane has a CAS number of 6731-36-8 and is purchased from Shanghai Yan Biotech Co., Ltd.
Example 3
Embodiment 3 of the present invention provides a method for detecting a crosslinking agent in an EVA photovoltaic film, including the following steps:
the method comprises the following steps: obtaining GCMS and HS-GCMS characterization test charts of a crosslinking agent triallyl isocyanurate standard sample and a 1, 1-di-tert-butylperoxy-3, 3, 5-trimethylcyclohexane standard sample;
step two: the weight ratio of acetone to triethanolamine used for an EVA photovoltaic film sample is 1: dissolving the mixture of 0.4 to obtain a solution to be detected;
step three: and qualitatively analyzing the solution to be detected obtained in the second step by using HS-GCMS compared with the characterization test chart of the cross-linking agent standard sample obtained in the first step, and then quantitatively analyzing the solution to be detected by using GCMS through an external standard method of an instrument.
Wherein the column of GCMS or HS-GCMS in step one and step three is a diphenyldimethylpolysiloxane column, an AC-5 capillary column (30 m. times.0.32 mm. times.0.25 μm) from SGE Analytical Science, Australia. The GC conditions of the GCMS or the HS-GCMS in the first step and the third step are as follows: column flow rate: 1.0 mL/min; sample introduction amount: 1.0 μ L; the temperature of a sample inlet is 200 ℃; the carrier gas is He, and the concentration is 1.0 mL/min; the split ratio is 30: 1. the temperature rise program of the GCMS or the HS-GCMS is as follows: the initial temperature is kept at 80 ℃ for 3min, then the temperature is increased to 110 ℃ at 6 ℃/min, then the temperature is increased to 130 ℃ at 5 ℃/min, after the temperature is kept for 6min, the temperature is increased to 160 ℃ at 6 ℃/min, and the temperature is kept for 3 min. The mass spectrum conditions of the GCMS or the HS-GCMS in the first step and the third step are as follows: ion source E1, ionization energy 70eV, ion source temperature 200 ℃, quadrupole temperature 160 ℃, scanning mass range 1000 amu. The headspace conditions in the HS-GCMS in the first step and the third step are as follows: the equilibration temperature is 110 ℃ and the equilibration time is 40 min.
The EVA photovoltaic film sample used in this example was the same as the example sample.
The ethylene-vinyl acetate copolymer used in this example, EVA resin, CAS number 24937-78-8, is 3155 from DuPont, USA. The triallyl isocyanurate, CAS number 1025-15-6, was purchased from Shanghai, screening Biotech, Inc. The 1, 1-di-tert-butylperoxy-3, 3, 5-trimethylcyclohexane has a CAS number of 6731-36-8 and is purchased from Shanghai Yan Biotech Co., Ltd.
Example 4
Embodiment 4 of the present invention provides a method for detecting a crosslinking agent in an EVA photovoltaic film, which is implemented in a similar manner to embodiment 1, except that the weight ratio of acetone to triethanolamine in the step two is changed from 1: 0.35 is replaced by 1: 0.25.
example 5
Embodiment 5 of the present invention provides a method for detecting a crosslinking agent in an EVA photovoltaic film, which is implemented in a similar manner to embodiment 1, except that the weight ratio of acetone to triethanolamine in step two is changed from 1: 0.35 is replaced by 1: 0.45.
example 6
Example 6 of the present invention provides a method of detecting a crosslinker in an EVA photovoltaic film, the specific embodiment of which is similar to example 1, except that the GCMS or HS-GCMS column in step one and step three is replaced with a diphenylphenyldimethylpolysiloxane column, an AC-10 capillary column (30m × 0.32mm × 0.25 μm) from SGE Analytical Science, australia.
Example 7
Embodiment 7 of the present invention provides a method for detecting a crosslinking agent in an EVA photovoltaic film, which is implemented in a similar manner to embodiment 1, except that the temperature rise procedure of GCMS or HS-GCMS is as follows: the initial temperature is maintained at 55 deg.C for 2min, then raised to 100 deg.C at 5 deg.C/min, then raised to 120 deg.C at 4 deg.C/min, maintained for 5min, then raised to 150 deg.C at 5 deg.C/min, and maintained for 2 min.
Example 8
Embodiment 8 of the present invention provides a method for detecting a crosslinking agent in an EVA photovoltaic film, which is implemented in a similar manner to embodiment 1, except that the temperature raising procedure of GCMS or HS-GCMS is as follows: the initial temperature is kept at 85 ℃ for 2min, then the temperature is increased to 100 ℃ at 5 ℃/min, then the temperature is increased to 120 ℃ at 4 ℃/min, the temperature is increased to 150 ℃ at 5 ℃/min after the temperature is kept for 5min, and the temperature is kept for 2 min.
Example 9
Embodiment 9 of the present invention provides a method for detecting a crosslinking agent in an EVA photovoltaic film, which is implemented in a similar manner to embodiment 1, except that the temperature raising procedure of GCMS or HS-GCMS is as follows: the initial temperature is maintained at 70 ℃ for 2min, then the temperature is increased to 85 ℃ at 5 ℃/min, then the temperature is increased to 120 ℃ at 4 ℃/min, the temperature is increased to 150 ℃ at 5 ℃/min after the temperature is maintained for 5min, and the temperature is maintained for 2 min.
Example 10
Embodiment 10 of the present invention provides a method for detecting a crosslinking agent in an EVA photovoltaic film, which is implemented in a similar manner to embodiment 1, except that the temperature raising procedure of GCMS or HS-GCMS is as follows: the initial temperature is maintained at 70 deg.C for 2min, then raised to 115 deg.C at 5 deg.C/min, then raised to 120 deg.C at 4 deg.C/min, maintained for 5min, then raised to 150 deg.C at 5 deg.C/min, and maintained for 2 min.
Example 11
Embodiment 11 of the present invention provides a method for detecting a crosslinking agent in an EVA photovoltaic film, which is implemented in a similar manner to embodiment 1, except that the temperature raising procedure of GCMS or HS-GCMS is as follows: the initial temperature is maintained at 70 deg.C for 2min, then the temperature is raised to 100 deg.C at 5 deg.C/min, then raised to 105 deg.C at 4 deg.C/min, and after 5min, the temperature is raised to 150 deg.C at 5 deg.C/min, and then maintained for 2 min.
Example 12
Embodiment 12 of the present invention provides a method for detecting a crosslinking agent in an EVA photovoltaic film, which is implemented in a similar manner to embodiment 1, except that the temperature raising procedure of GCMS or HS-GCMS is as follows: the initial temperature is maintained at 70 deg.C for 2min, then raised to 100 deg.C at 5 deg.C/min, then raised to 165 deg.C at 4 deg.C/min, maintained for 5min, then raised to 150 deg.C at 5 deg.C/min, and maintained for 2 min.
Example 13
Embodiment 13 of the present invention provides a method for detecting a crosslinking agent in an EVA photovoltaic film, which is implemented in a similar manner to embodiment 1, except that the temperature raising procedure of GCMS or HS-GCMS is as follows: after the initial temperature of 70 ℃ is kept for 2min, the temperature is raised to 150 ℃ at the speed of 5 ℃/min and kept for 2 min.
Example 14
Embodiment 14 of the present invention provides a method for detecting a crosslinking agent in an EVA photovoltaic film, which is implemented in a similar manner to embodiment 1, except that the temperature raising procedure of GCMS or HS-GCMS is as follows: the initial temperature is maintained at 70 deg.C for 2min, then raised to 100 deg.C at 5 deg.C/min, and then raised to 150 deg.C at 4 deg.C/min, and maintained for 2 min.
Example 15
Embodiment 15 of the present invention provides a method for detecting a cross-linking agent in an EVA photovoltaic film, which is implemented in a similar manner to embodiment 1, except that the mass spectrometry conditions of GCMS or HS-GCMS are as follows: and (3) an ion source E1, wherein the ionization energy is 70eV, the ion source temperature is 150 ℃, the quadrupole rod temperature is 150 ℃, and the scanning mass range is 40-1000 amu.
Example 16
Embodiment 16 of the present invention provides a method for detecting a cross-linking agent in an EVA photovoltaic film, which is implemented in a similar manner to embodiment 1, except that the mass spectrometry conditions of GCMS or HS-GCMS are as follows: and (3) an ion source E1, wherein the ionization energy is 70eV, the ion source temperature is 210 ℃, the quadrupole rod temperature is 150 ℃, and the scanning mass range is 40-1000 amu.
Example 17
Embodiment 17 of the present invention provides a method for detecting a crosslinking agent in an EVA photovoltaic film, which is implemented in a similar manner to embodiment 1, except that the mass spectrometry conditions of GCMS or HS-GCMS are as follows: and (3) an ion source E1, wherein the ionization energy is 70eV, the ion source temperature is 180 ℃, the quadrupole rod temperature is 130 ℃, and the scanning mass range is 40-1000 amu.
Example 18
Embodiment 18 of the present invention provides a method for detecting a cross-linking agent in an EVA photovoltaic film, which is implemented in a similar manner to embodiment 1, except that the mass spectrometry conditions of GCMS or HS-GCMS are as follows: and (3) an ion source E1, wherein the ionization energy is 70eV, the ion source temperature is 180 ℃, the quadrupole rod temperature is 170 ℃, and the scanning mass range is 40-1000 amu.
Example 19
Embodiment 19 of the present invention provides a method for detecting a crosslinking agent in an EVA photovoltaic film, which is implemented in a similar manner to embodiment 1, except that the headspace conditions in HS-GCMS are as follows: the equilibration temperature is 80 ℃ and the equilibration time is 30 min.
Example 20
Embodiment 20 of the present invention provides a method for detecting a crosslinking agent in an EVA photovoltaic film, which is implemented in a similar manner to embodiment 1, except that the headspace conditions in HS-GCMS are as follows: the equilibration temperature is 120 ℃, and the equilibration time is 30 min.
Example 21
Example 21 of the present invention provides a method for detecting a cross-linking agent in an EVA photovoltaic film, which is implemented in a similar manner as example 1, except that only GCMS test is performed in step one and step three.
Example 22
Example 22 of the present invention provides a method for detecting a crosslinker in an EVA photovoltaic film, the specific implementation of which is similar to example 1, except that only HS-GCMS test is performed in step one and step three.
Example 23
Embodiment 23 of the present invention provides a method for detecting a crosslinking agent in an EVA photovoltaic film, which is implemented in a similar manner to embodiment 1, except that the EVA photovoltaic film used in this embodiment is prepared from the following raw materials: 99.4 wt% of ethylene-vinyl acetate copolymer and 0.6 wt% of triallyl isocyanurate were prepared in the same manner as in example 1.
The ethylene-vinyl acetate copolymer used in this example, EVA resin, CAS number 24937-78-8, is 3155 from DuPont, USA. The triallyl isocyanurate, CAS number 1025-15-6, was purchased from Shanghai, screening Biotech, Inc.
Example 24
Embodiment 24 of the present invention provides a method for detecting a crosslinking agent in an EVA photovoltaic film, which is implemented in a similar manner to embodiment 1, except that the EVA photovoltaic film used in this embodiment is prepared from the following raw materials: 99.4 wt% of ethylene-vinyl acetate copolymer, 0.1 wt% of triallyl isocyanurate, 0.25 wt% of 1, 1-bis-tert-butylperoxy-3, 3, 5-trimethylcyclohexane, and 0.25 wt% of 2, 5-dimethyl-2, 5-bis- (tert-butylperoxy) hexane were prepared in the same manner as in example 1.
The ethylene-vinyl acetate copolymer used in this example, EVA resin, CAS number 24937-78-8, is 3155 from DuPont, USA. The triallyl isocyanurate, CAS number 1025-15-6, was purchased from Shanghai, screening Biotech, Inc. The 1, 1-di-tert-butylperoxy-3, 3, 5-trimethylcyclohexane has a CAS number of 6731-36-8 and is purchased from Shanghai Yan Biotech Co., Ltd. The 2, 5-dimethyl-2, 5-bis- (tert-butylperoxy) hexane, CAS number 78-63-7, was purchased from Baishun, Inc., Shanghai.
Example 25
Embodiment 25 of the present invention provides a method for detecting a crosslinking agent in an EVA photovoltaic film, which is implemented in a similar manner to embodiment 1, except that the EVA photovoltaic film used in this embodiment is prepared from the following raw materials: 99.4 wt% of ethylene-vinyl acetate copolymer, 0.1 wt% of triallyl isocyanurate, 0.2 wt% of 1, 1-bis-tert-butylperoxy-3, 3, 5-trimethylcyclohexane, 0.15 wt% of 2, 5-dimethyl-2, 5-bis- (tert-butylperoxy) hexane, and 0.15 wt% of tert-butylperoxy carbonate-2-ethylhexyl ester were prepared in the same manner as in example 1.
The ethylene-vinyl acetate copolymer used in this example, EVA resin, CAS number 24937-78-8, is 3155 from DuPont, USA. The triallyl isocyanurate, CAS number 1025-15-6, was purchased from Shanghai, screening Biotech, Inc. The 1, 1-di-tert-butylperoxy-3, 3, 5-trimethylcyclohexane has a CAS number of 6731-36-8 and is purchased from Shanghai Yan Biotech Co., Ltd. The 2, 5-dimethyl-2, 5-bis- (tert-butylperoxy) hexane, CAS number 78-63-7, was purchased from Baishun, Inc., Shanghai. The tert-butyl peroxycarbonic acid-2-ethylhexyl ester has a CAS number of 34443-12-4 and is purchased from Tai Fuji chemical Co.
Example 26
Embodiment 26 of the present invention provides a method for detecting a crosslinking agent in an EVA photovoltaic film, which is implemented in a similar manner to embodiment 1, except that the EVA photovoltaic film used in this embodiment is prepared from the following raw materials: ethylene-vinyl acetate copolymer 99.4 wt%, triallyl isocyanurate 0.1 wt%, and 2, 5-dimethyl-2, 5-bis- (t-butylperoxy) hexane 0.5 wt%, which was prepared in the same manner as in example 1.
The ethylene-vinyl acetate copolymer used in this example, EVA resin, CAS number 24937-78-8, is 3155 from DuPont, USA. The triallyl isocyanurate, CAS number 1025-15-6, was purchased from Shanghai, screening Biotech, Inc. The 2, 5-dimethyl-2, 5-bis- (tert-butylperoxy) hexane, CAS number 78-63-7, was purchased from Baishun, Inc., Shanghai.
Example 27
Embodiment 27 of the present invention provides a method for detecting a crosslinking agent in an EVA photovoltaic film, which is implemented in a similar manner to embodiment 1, except that the EVA photovoltaic film used in this embodiment is prepared from the following raw materials: 99.4 wt% of ethylene-vinyl acetate copolymer, 0.1 wt% of triallyl isocyanurate, 0.25 wt% of 2, 5-dimethyl-2, 5-bis- (t-butylperoxy) hexane, and 0.25 wt% of t-butylperoxy carbonate-2-ethylhexyl ester were prepared in the same manner as in example 1.
The ethylene-vinyl acetate copolymer used in this example, EVA resin, CAS number 24937-78-8, is 3155 from DuPont, USA. The triallyl isocyanurate, CAS number 1025-15-6, was purchased from Shanghai, screening Biotech, Inc. The 2, 5-dimethyl-2, 5-bis- (tert-butylperoxy) hexane, CAS number 78-63-7, was purchased from Baishun, Inc., Shanghai. The tert-butyl peroxycarbonic acid-2-ethylhexyl ester has a CAS number of 34443-12-4 and is purchased from Tai Fuji chemical Co.
Example 28
Embodiment 28 of the present invention provides a method for detecting a crosslinking agent in an EVA photovoltaic film, which is implemented in a similar manner to embodiment 1, except that the EVA photovoltaic film used in this embodiment is prepared from the following raw materials: 99.4 wt% of ethylene-vinyl acetate copolymer, 0.1 wt% of triallyl isocyanurate, and 0.5 wt% of 2-ethylhexyl t-butylperoxycarbonate were prepared in the same manner as in example 1.
The ethylene-vinyl acetate copolymer used in this example, EVA resin, CAS number 24937-78-8, is 3155 from DuPont, USA. The triallyl isocyanurate, CAS number 1025-15-6, was purchased from Shanghai, screening Biotech, Inc. The tert-butyl peroxycarbonic acid-2-ethylhexyl ester has a CAS number of 34443-12-4 and is purchased from Tai Fuji chemical Co.
Example 29
Embodiment 29 of the present invention provides a method for detecting a crosslinking agent in an EVA photovoltaic film, which is implemented in a similar manner to embodiment 1, except that the EVA photovoltaic film used in this embodiment is prepared from the following raw materials: 98.7 wt% of ethylene-vinyl acetate copolymer, 0.3 wt% of triallyl isocyanurate, and 1.0 wt% of 1, 1-di-tert-butylperoxy-3, 3, 5-trimethylcyclohexane were prepared in the same manner as in example 1.
The ethylene-vinyl acetate copolymer used in this example, EVA resin, CAS number 24937-78-8, is 3155 from DuPont, USA. The triallyl isocyanurate, CAS number 1025-15-6, was purchased from Shanghai, screening Biotech, Inc. The 1, 1-di-tert-butylperoxy-3, 3, 5-trimethylcyclohexane has a CAS number of 6731-36-8 and is purchased from Shanghai Yan Biotech Co., Ltd.
The method mainly limits the main steps in the detection method of the cross-linking agent in the EVA photovoltaic film correspondingly, and can adopt a general method which is well known by the technicians in the field for other steps which are not limited.
Performance testing
1. The accuracy is as follows: the test data of the crosslinking agent in the EVA photovoltaic film measured in examples 1 to 29 are compared with the kind of the crosslinking agent in the real sample, and the measured crosslinking agent is √ when the actual crosslinking agent is present, the undetected crosslinking agent is ×, and the cross-linking agent not actually included is — ". For the quantitative analysis of the crosslinker triallyl isocyanurate, the deviation is calculated, which is (actual crosslinker content-measured crosslinker content)/actual crosslinker content. The results are shown in Table 1.
TABLE 1 accuracy test results
2. Anti-interference performance: the dispersion ratio of the content of the crosslinking agent triallyl isocyanurate in comparative example 1 and examples 23 to 29 can be obtained.
And (3) testing results: by comparison, even when the crosslinking agent in the EVA photovoltaic film comprises triallyl isocyanurate and other crosslinking agents, such as 1, 1-di-tert-butylperoxy-3, 3, 5-trimethylcyclohexane, 2, 5-dimethyl-2, 5-di- (tert-butylperoxy) hexane and tert-butyl peroxycarbonate-2-ethylhexyl ester, the deviation rate of the measured triallyl isocyanurate content is only 0.01 percent, and the interference component can be accurately and qualitatively analyzed.
3. Reproducibility: the EVA photovoltaic film samples used in example 1 were tested 10 times in the same manner as in example 1, and the deviation ratios of the test data of the crosslinker in the EVA photovoltaic films were recorded, and the results are shown in Table 2, wherein the samples were designated as examples 1-10.
TABLE 2 reproducibility test results
The combination of the above experimental results shows that: the detection method of the cross-linking agent in the EVA photovoltaic film can be used for carrying out qualitative analysis and highly accurate quantitative analysis on the triallyl isocyanurate in the EVA photovoltaic film, and the deviation rate is only 0.01%; accurate qualitative analysis can also be carried out on other cross-linking agents in the EVA photovoltaic film, such as 1, 1-di-tert-butylperoxy-3, 3, 5-trimethylcyclohexane, 2, 5-dimethyl-2, 5-di- (tert-butylperoxy) hexane and tert-butylperoxy-2-ethylhexyl carbonate, for example, the HS-GCMS spectrum of the EVA photovoltaic film sample used in the example 1 of the invention is shown in figure 1, and the GCMS spectrum of the EVA photovoltaic film sample used in the example 1 of the invention is shown in figure 2. Meanwhile, the detection method of the cross-linking agent in the EVA photovoltaic film has higher anti-interference performance, and can eliminate the interference of other cross-linking agents on the testing result of triallyl isocyanurate; the method has extremely high reproducibility and excellent practical application and popularization values.
The foregoing examples are merely illustrative and serve to explain some of the features of the method of the present invention. The appended claims are intended to claim as broad a scope as is contemplated, and the examples presented herein are merely illustrative of selected implementations in accordance with all possible combinations of examples. Accordingly, it is applicants' intention that the appended claims are not to be limited by the choice of examples illustrating features of the invention. The invention is not limited to the embodiments described above, but rather, many modifications and variations may be made by one skilled in the art without departing from the scope of the invention.
Claims (10)
- The detection method of the cross-linking agent in the EVA photovoltaic film is characterized by comprising the following steps:the method comprises the following steps: obtaining a characterization test chart of a cross-linking agent standard sample;step two: dissolving an EVA photovoltaic film sample by using a solvent to obtain a solution to be detected;step three: and (4) performing instrument analysis on the solution to be tested obtained in the step two, comparing the characterization test chart of the cross-linking agent standard sample obtained in the step one, and performing qualitative and quantitative analysis on the cross-linking agent in the EVA photovoltaic film.
- 2. The method for detecting the cross-linking agent in the EVA photovoltaic film according to claim 1, wherein the solvent in the second step is acetone and/or triethanolamine.
- 3. The method for detecting the cross-linking agent in the EVA photovoltaic film according to claim 2, wherein the weight ratio of the acetone to the triethanolamine is 1: (0.3-0.4).
- 4. The method for detecting the cross-linking agent in the EVA photovoltaic film of claim 1, wherein the instrumental analysis in the third step is HS-GCMS and/or GCMS.
- 5. The method for detecting the cross-linking agent in the EVA photovoltaic film according to claim 4, wherein the temperature rise program of GCMS or HS-GCMS is as follows: keeping the initial temperature at 60-80 ℃ for 1-3 min, raising the temperature to 90-110 ℃ at 4-6 ℃/min, raising the temperature to 110-130 ℃ at 3-5 ℃/min, keeping the temperature for 4-6 min, raising the temperature to 140-160 ℃ at 4-6 ℃/min, and keeping the temperature for 1-3 min.
- 6. The method for detecting the cross-linking agent in the EVA photovoltaic film according to claim 4 or 5, wherein the mass spectrum condition of GCMS or HS-GCMS is as follows: the ion source E1 has ionization energy of 70eV, ion source temperature of 160-200 ℃, quadrupole rod temperature of 140-160 ℃ and scanning mass range of 40-1000 amu.
- 7. The method for detecting the cross-linking agent in the EVA photovoltaic film according to claim 6, wherein the headspace condition of HS-GCMS is as follows: the equilibrium temperature is 90-110 ℃, and the equilibrium time is 20-40 min.
- 8. The method for detecting the cross-linking agent in the EVA photovoltaic film according to claim 4, wherein the test sequence of the instrumental analysis is qualitative analysis by using HS-GCMS and then quantitative analysis by using GCMS.
- 9. The method for detecting the crosslinking agent in the EVA photovoltaic film according to claim 1, wherein the crosslinking agent in the EVA photovoltaic film comprises triallyl isocyanurate.
- 10. The method for detecting the cross-linking agent in the EVA photovoltaic film of claim 9, wherein the cross-linking agent in the EVA photovoltaic film further comprises one or more of 1, 1-di-tert-butylperoxy-3, 3, 5-trimethylcyclohexane, 2, 5-dimethyl-2, 5-bis- (tert-butylperoxy) hexane, and tert-butylperoxy-2-ethylhexyl carbonate.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105651898A (en) * | 2016-03-29 | 2016-06-08 | 阿特斯(中国)投资有限公司 | Method for testing cross-linking agent content in EVA (ethylene vinyl acetate copolymer) film |
| US20190369079A1 (en) * | 2017-01-10 | 2019-12-05 | Sumitomo Electric Industries, Ltd. | Method for detecting residual crosslinking aid |
-
2019
- 2019-12-13 CN CN201911280073.XA patent/CN111103366A/en not_active Withdrawn
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105651898A (en) * | 2016-03-29 | 2016-06-08 | 阿特斯(中国)投资有限公司 | Method for testing cross-linking agent content in EVA (ethylene vinyl acetate copolymer) film |
| US20190369079A1 (en) * | 2017-01-10 | 2019-12-05 | Sumitomo Electric Industries, Ltd. | Method for detecting residual crosslinking aid |
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| Title |
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| SUNG-SEEN CHOI ET AL.: "Considering factors for analysis of crosslink density of poly(ethylene-co-vinyl acetate) compounds", 《POLYMER TESTING》 * |
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