CN113390818A - Method for measuring epoxy group and carboxyl group contents of VPI (vacuum pressure impregnation) resin - Google Patents
Method for measuring epoxy group and carboxyl group contents of VPI (vacuum pressure impregnation) resin Download PDFInfo
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- CN113390818A CN113390818A CN202110652576.6A CN202110652576A CN113390818A CN 113390818 A CN113390818 A CN 113390818A CN 202110652576 A CN202110652576 A CN 202110652576A CN 113390818 A CN113390818 A CN 113390818A
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- vpi
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- resin
- epoxy
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- 238000000034 method Methods 0.000 title claims abstract description 27
- 229920005989 resin Polymers 0.000 title claims abstract description 24
- 239000011347 resin Substances 0.000 title claims abstract description 24
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 title claims abstract description 23
- 125000003700 epoxy group Chemical group 0.000 title claims abstract description 19
- 238000005470 impregnation Methods 0.000 title claims description 6
- 238000006243 chemical reaction Methods 0.000 claims abstract description 15
- 238000005259 measurement Methods 0.000 claims abstract description 11
- 238000010521 absorption reaction Methods 0.000 claims description 9
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 claims description 8
- 238000012360 testing method Methods 0.000 claims description 7
- 230000008859 change Effects 0.000 claims description 6
- 239000004593 Epoxy Substances 0.000 claims description 4
- 238000005033 Fourier transform infrared spectroscopy Methods 0.000 claims description 3
- 230000008569 process Effects 0.000 abstract description 12
- 238000011160 research Methods 0.000 abstract description 9
- 238000004519 manufacturing process Methods 0.000 abstract description 8
- 239000003822 epoxy resin Substances 0.000 abstract description 6
- 239000000463 material Substances 0.000 abstract description 6
- 229920000647 polyepoxide Polymers 0.000 abstract description 6
- 238000009413 insulation Methods 0.000 abstract description 3
- 229910000976 Electrical steel Inorganic materials 0.000 abstract description 2
- 239000003973 paint Substances 0.000 abstract description 2
- 238000004080 punching Methods 0.000 abstract description 2
- 150000001875 compounds Chemical class 0.000 abstract 1
- 238000005516 engineering process Methods 0.000 description 4
- 238000007689 inspection Methods 0.000 description 4
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000003618 dip coating Methods 0.000 description 2
- 238000007598 dipping method Methods 0.000 description 2
- 239000003292 glue Substances 0.000 description 2
- 238000002329 infrared spectrum Methods 0.000 description 2
- 238000012797 qualification Methods 0.000 description 2
- 238000004566 IR spectroscopy Methods 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000027455 binding Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 239000010445 mica Substances 0.000 description 1
- 229910052618 mica group Inorganic materials 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
Images
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N21/35—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light
- G01N21/3577—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light for analysing liquids, e.g. polluted water
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N21/35—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light
- G01N2021/3595—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light using FTIR
Abstract
The invention discloses a method for measuring epoxy group and carboxyl content of VPI impregnating resin, which can be used for measuring the content of groups in the impregnating resin used for manufacturing main insulation of a VPI stator coil, representing the curing process of epoxy resin, has the advantages of quick measurement, high precision, good repeatability, simple and convenient operation, contribution to more scientific production guidance, good application prospect and popularization and application in the reaction process measurement and research of materials such as silicon steel sheet paint for stator punching sheets of large-scale motors, epoxy resin compounds for end fixing and the like.
Description
Technical Field
The invention relates to the field of large-scale generator stator coils, in particular to a method for measuring epoxy and carboxyl contents of VPI impregnating resin.
Background
Two main insulation manufacturing processes of large-scale generator stator coils are used in the world nowadays, wherein a VPI dip coating process is favored by various foreign motor manufacturers, and a low-glue dipping process is a manufacturing process of wrapping a low-glue mica tape outside a conducting wire, dipping low-viscosity VPI resin in a vacuum dip coating tank, and then curing and molding. Wherein the VPI impregnating resin assumes a binding action, which dominates the transformation of the material morphology during the curing process. At present, the research of VPI impregnating resin in domestic motor manufacturers still stays in the control of macroscopic indexes such as viscosity, acid value and the like, along with the development of science and technology, the conventional means are gradually difficult to meet the requirements of scientific research and production, and a more scientific and advanced microscopic research method needs to be introduced urgently to break the bottleneck of progress. The infrared spectroscopy technology is a technical means capable of researching the molecular structure of the epoxy resin, can examine the curing process of the epoxy resin from the molecular angle, more scientifically guides the process application, and guides the research of the impregnating resin to step into the microscopic era.
Disclosure of Invention
Therefore, the invention aims to provide a method for measuring the epoxy content and the carboxyl content of VPI impregnating resin, which can be used for carrying out molecular structure research on the VPI impregnating resin for a low-gel vacuum pressure impregnation process, and can be used for representing the change of reactant concentration in the resin curing process by measuring the relative content of two reactive groups, namely epoxy groups and carboxyl groups relative to an unreacted group, so as to represent the resin curing process and scientifically guide production.
The technical scheme adopted by the invention is as follows:
1) starting a Fourier transform infrared spectrometer equipped with a reflection measurement module, removing background noise, and adding VPI (vacuum pressure impregnation) resin to be tested into a test window to completely cover the test window;
2) setting the scanning times to 16 times, setting the scanning wave number range to 40-4000, and starting scanning;
3) after scanning, carrying out peak marking treatment on the spectrogram, and marking an absorption peak at 915 wave number, an absorption peak at 1750 wave number and an absorption peak at 1500 wave number;
4) measuring the peak height of each marked characteristic peak, and respectively recording as h915、h1750、h1500；
5) Calculated as the relative contents of epoxy group and carboxyl group, h915Divided by h1500Is the content of epoxy groups relative to the benzene ring, h1750Divided by h1500Is the content of carboxyl groups relative to benzene rings;
6) and (3) taking VPI impregnating resin in different reaction stages, measuring according to the method, calculating the relative content of the epoxy group and the carboxyl group according to the method in the step 5, and drawing a change curve of the content of the epoxy group along with the reaction and a change curve of the content of the carboxyl group along with the reaction.
Compared with the prior art, the invention has the beneficial effects that:
1) the content of the active groups is determined, and the reaction process is accurately researched. The content of the epoxy group and the carboxyl group relative to the benzene ring is measured, so that the content of the epoxy group and the carboxyl group is measured, a content change curve of the two groups along with the reaction is drawn, the most core field of the reaction is deepened, the resin curing process is represented more accurately, and the technological process can be guided more scientifically.
2) The measurement is accurate, and the repeatability is good. The infrared spectrum is a mature testing method in the field of chemical analysis, has extremely high precision, good repeatability and more accurate data measurement, and is beneficial to scientific research and inspection.
3) The dosage is less, the operation is simple and convenient, and the measurement is rapid. The method has the advantages of less sample demand, simple and convenient operation and quick measurement, and can be widely applied to the fields of scientific research, inspection and the like.
Drawings
FIG. 1 is a flow chart of the operation of the present invention.
Detailed Description
The invention is further described with reference to the following figures and detailed description.
As shown in fig. 1:
1) starting a Fourier transform infrared spectrometer equipped with a reflection measurement module, removing background noise, and adding VPI (vacuum pressure impregnation) resin to be tested into a test window to completely cover the test window;
2) the wave number scanning range of the infrared spectrometer is 400-4000, and the scanning times are 16;
3) after scanning, carrying out peak marking treatment on a spectrogram, wherein an absorption peak near 915 wave number is an epoxy characteristic peak, an absorption peak near 1750 wave number is a carboxyl characteristic peak, a resin curing main reaction is a reaction between an epoxy group and a carboxyl group, and the absorption peak near 1500 wave number is selected as a benzene ring reference peak;
4) measuring the peak height of each marked characteristic peak, and respectively recording as h915、h1750、h1500；
5) H915/h1500 is the content of the epoxy group relative to the benzene ring, h is calculated according to the relative content of the epoxy group and the carboxyl group1750/h1500Is the content of carboxyl groups relative to benzene rings;
6) the VPI impregnating resin in different reaction stages is taken, the measurement is carried out according to the method, the relative content of the epoxy group and the carboxyl group is calculated, and a variation curve of the content of the epoxy group along with the reaction and a variation curve of the content of the carboxyl group along with the reaction can be drawn.
The method can also be used as a material inspection means, an infrared spectrogram of the evaluated material is measured to serve as an inspection basis, a spectrogram of a sample is compared with the evaluation spectrogram when the subsequent material needs to be inspected, and the similarity value can serve as a criterion for qualification or non-qualification.
In conclusion, the VPI impregnating resin performance research method based on the infrared spectrum technology can be used for measuring the group content of the impregnating resin used in the VPI stator coil main insulation manufacturing technology which is popular in the world at present, represents the epoxy resin curing process, guides production more scientifically, has high measurement precision, good repeatability, is simple and convenient to operate, is quick to measure, has good application prospect, and can be popularized and applied to the aspect of measuring the group content of materials such as silicon steel sheet paint of stator punching sheets of large-scale motors, epoxy resin for end fixing and the like.
The present invention is illustrative only and not intended to limit the scope thereof, and those skilled in the art can make modifications to the present invention without departing from the spirit and scope thereof.
Claims (1)
1. A method for measuring the epoxy and carboxyl content of VPI impregnating resin is characterized by comprising the following steps:
1) starting a Fourier transform infrared spectrometer equipped with a reflection measurement module, removing background noise, and adding VPI (vacuum pressure impregnation) resin to be tested into a test window to completely cover the test window;
2) setting the scanning times to 16 times, setting the scanning wave number range to 40-4000, and starting scanning;
3) after scanning, carrying out peak marking treatment on the spectrogram, and marking an absorption peak at 915 wave number, an absorption peak at 1750 wave number and an absorption peak at 1500 wave number;
4) measuring the peak height of each marked characteristic peak, and respectively recording as h915、h1750、h1500；
5) Calculated as the relative contents of epoxy group and carboxyl group, h915Divided by h1500Is the content of epoxy groups relative to the benzene ring, h1750Divided by h1500Is the content of carboxyl groups relative to benzene rings;
6) and (3) taking VPI impregnating resin in different reaction stages, measuring according to the method, calculating the relative content of the epoxy group and the carboxyl group according to the method in the step 5, and drawing a change curve of the content of the epoxy group along with the reaction and a change curve of the content of the carboxyl group along with the reaction.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110652576.6A CN113390818A (en) | 2021-06-11 | 2021-06-11 | Method for measuring epoxy group and carboxyl group contents of VPI (vacuum pressure impregnation) resin |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110652576.6A CN113390818A (en) | 2021-06-11 | 2021-06-11 | Method for measuring epoxy group and carboxyl group contents of VPI (vacuum pressure impregnation) resin |
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| Publication Number | Publication Date |
|---|---|
| CN113390818A true CN113390818A (en) | 2021-09-14 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202110652576.6A Pending CN113390818A (en) | 2021-06-11 | 2021-06-11 | Method for measuring epoxy group and carboxyl group contents of VPI (vacuum pressure impregnation) resin |
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| CN (1) | CN113390818A (en) |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5142151A (en) * | 1989-11-17 | 1992-08-25 | Allied-Signal Inc. | Method for measuring degree of cure of resin in a composite material and process for making the same |
| CN101435772A (en) * | 2008-12-12 | 2009-05-20 | 三星高新电机（天津）有限公司 | Epoxide-resin glue curing degree and hardness detecting and analyzing method |
| CN103542892A (en) * | 2013-10-28 | 2014-01-29 | 哈尔滨电机厂有限责任公司 | Evaluation method of vacuum pressure impregnating resin |
| CN112552485A (en) * | 2019-09-25 | 2021-03-26 | 日清纺化学株式会社 | Method for curing epoxy resin composition |
| JP2021050287A (en) * | 2019-09-25 | 2021-04-01 | 日清紡ケミカル株式会社 | Curing agent for epoxy resin, epoxy resin composition and cured product thereof |
-
2021
- 2021-06-11 CN CN202110652576.6A patent/CN113390818A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5142151A (en) * | 1989-11-17 | 1992-08-25 | Allied-Signal Inc. | Method for measuring degree of cure of resin in a composite material and process for making the same |
| CN101435772A (en) * | 2008-12-12 | 2009-05-20 | 三星高新电机（天津）有限公司 | Epoxide-resin glue curing degree and hardness detecting and analyzing method |
| CN103542892A (en) * | 2013-10-28 | 2014-01-29 | 哈尔滨电机厂有限责任公司 | Evaluation method of vacuum pressure impregnating resin |
| CN112552485A (en) * | 2019-09-25 | 2021-03-26 | 日清纺化学株式会社 | Method for curing epoxy resin composition |
| JP2021050287A (en) * | 2019-09-25 | 2021-04-01 | 日清紡ケミカル株式会社 | Curing agent for epoxy resin, epoxy resin composition and cured product thereof |
Non-Patent Citations (1)
| Title |
|---|
| 郑芸 等: "反应性硅氧烷改性VPI环氧树脂的研究", 《绝缘材料》 * |
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