CN111610249A - Method for evaluating aging state of high-temperature vulcanized silicone rubber - Google Patents

Method for evaluating aging state of high-temperature vulcanized silicone rubber Download PDF

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CN111610249A
CN111610249A CN202010485651.XA CN202010485651A CN111610249A CN 111610249 A CN111610249 A CN 111610249A CN 202010485651 A CN202010485651 A CN 202010485651A CN 111610249 A CN111610249 A CN 111610249A
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silicone rubber
temperature vulcanized
vulcanized silicone
aging
evaluating
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CN111610249B (en
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万涛
查方林
巢亚峰
李文波
刘凯
徐松
王峰
黄福勇
黄颖
胡胜
吴晓文
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State Grid Corp of China SGCC
Electric Power Research Institute of State Grid Hunan Electric Power Co Ltd
State Grid Hunan Electric Power Co Ltd
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State Grid Corp of China SGCC
Electric Power Research Institute of State Grid Hunan Electric Power Co Ltd
State Grid Hunan Electric Power Co Ltd
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    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
    • G01N27/62—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating the ionisation of gases, e.g. aerosols; by investigating electric discharges, e.g. emission of cathode

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Abstract

The invention discloses a method for evaluating the aging state of high-temperature vulcanized silicone rubber, which is based on SiCH3 +With SiC3H9 +The mass spectrum peak height ratio value is used as an aging judgment basis to evaluate the aging state. The invention carries out the detection and quantitative analysis of the flight time secondary ion mass spectrum aiming at the characteristic products in the silicone rubber aging process, thereby accurately judging the service life state of the material. The power grid company can judge whether the composite insulator needs to be replaced by adopting the diagnosis method, so that the safe and stable operation of the power grid is guaranteed.

Description

Method for evaluating aging state of high-temperature vulcanized silicone rubber
Technical Field
The invention relates to a method for evaluating the aging state of a composite insulator, in particular to a method for evaluating the aging state of a high-temperature vulcanized silicone rubber composite insulator.
Background
The insulator used in the early electric power industry is made of ceramic or glass, and in the last 80 th century, China starts to develop the composite insulator, and the composite insulator is widely used in most seriously polluted areas and many newly-built power transmission lines at present due to the excellent pollution flashover resistance. According to statistics, the usage amount of the composite insulators operated in China on line is accumulated to be more than 700 thousands (110kV and above voltage level by 2014), the composite insulators account for a large proportion of the number of the composite insulators operated in the world on line (the number of the composite insulators operated in 50kV and above voltage level is more than 2000 thousands by 2013), and the composite insulators are the countries which use the most composite insulators all over the world at present. The composite insulator mainly comprises three parts, namely high-temperature vulcanized silicone rubber, an epoxy resin glass fiber reinforced plastic core rod and a hardware fitting. The reinforced high-temperature vulcanized silicone rubber (HTV-SR) filled with various additives has better stain resistance, strong hydrophobicity, hydrophobic migration, recoverability, convenient maintenance and the like, is more superior to other organic insulating materials in performance, has already been tested for decades of actual operation abroad, and gradually becomes a preferred material of an external insulating umbrella cover.
The composite insulator is subjected to the comprehensive action of various factors in the operation process, including electrical, mechanical and environmental factors, and along with the increase of the operation time, the silicon rubber composite insulator has the phenomena of hydrophobicity reduction, umbrella skirt color change, hardening, embrittlement, pulverization, cracking, electric leakage tracking or electric corrosion damage, end sealing failure, flashover with unknown reasons and the like, so that a circuit is tripped, and the safe and stable operation of a power grid is influenced. Generally, the service life of the composite insulator is considered to be 8-12 years, if the composite insulator is not replaced in time, a power grid safety accident can be caused, and if the composite insulator is replaced in advance, a large amount of economic loss can be caused, so that the composite insulator service life state can be accurately evaluated.
CN201610485019, CN201610149966, CN201510958923, CN201510958583 and CN201510570741 establish methods of judgment, prediction, classification and experimental evaluation of the aging state of the composite insulator based on the trapped charge amount, the thermal stimulation current characteristics and the hygroscopicity and dielectric characteristics. CN201310495248 adopts slow positron beam measurement to obtain Doppler spread spectrum distributed along with positron incident energy, and judges umbrella skirt aging state. The methods are based on the change of electrical and physical characteristics of the aged silicon rubber material, and the performance characteristics of the aged silicon rubber material are measured to obtain the aging condition information, and the methods are not essentially different from performance testing methods such as hydrophobicity, surface roughness and the like. CN201610604578 uses infrared spectroscopy to detect main chain and side chain groups of silicone rubber, and the method further introduces the detection object into the microstructure of substance, which is a very meaningful exploration, but is limited to the characteristics of infrared spectroscopy, and can only roughly judge the change of groups, and cannot understand the change of substance content in the aging process, and has certain limitation in quantitative analysis.
Disclosure of Invention
The invention aims to solve the technical problem of providing a method for evaluating the aging state of high-temperature vulcanized silicone rubber, which can detect and quantitatively analyze characteristic products in the aging process of the silicone rubber so as to accurately judge the service life state of a material.
A method for evaluating the ageing state of high-temperature vulcanized silicone rubber directly adopts mass spectrometry to analyze solid high-temperature vulcanized silicone rubber to be tested and evaluates the ageing state of the solid high-temperature vulcanized silicone rubber.
The invention innovatively adopts a mass spectrum mode to evaluate the aging degree of the solid high-temperature vulcanized silicone rubber.
In the invention, the mass spectrum is preferably a time-of-flight secondary ion mass spectrum.
Preferably, the high-temperature vulcanized silicone rubber is at least one of methyl silicone rubber, methyl vinyl silicone rubber and methyl phenyl vinyl silicone rubber.
Preferably, the high-temperature vulcanized silicone rubber to be detected is a high-temperature vulcanized silicone rubber composite insulator.
Preferably, the mass spectrometric measurement is carried out and is based on SiCH3 +With SiC3H9 +The mass spectrum peak height ratio is used as an aging judgment basis to evaluate the aging state.
In the invention, the high-temperature vulcanized silicone rubber is innovatively measured by adopting mass spectrum, preferably time-of-flight secondary ion mass spectrum, and is innovatively measured according to SiCH3 +With SiC3H9 +The mass spectrum peak height ratio is used as an aging judgment basis to evaluate the aging state.
In the invention, the aging degree is evaluated based on the mass spectrum peak height ratio, and the larger the mass spectrum peak height ratio is, the more serious the aging is represented.
A preferred method of the invention comprises the steps of:
(1) and shearing a sample to be detected from the high-temperature vulcanized silicone rubber composite insulator. The size of the sample to be detected is preferably 1cm2～2cm2。
(2) Soaking the sample to be tested in methanol or ethanol. The soaking time is preferably 6-12 h.
(3) And drying the soaked sample to be detected. The drying can be carried out by the existing means.
(4) Detecting the surface of a sample to be detected by using a time-of-flight secondary ion mass spectrometer;
(5) analyzing the positive ion spectrum, and taking SiCH with m/z of 433 +SiC with m/z 733H9 +The peak height ratio of (A) is used as an aging judgment basis, and the larger the value is, the more serious the aging is.
The more preferable steps of the invention are as follows:
(1) shearing 1cm from composite insulator2～2cm2Left and right samples;
(2) soaking the sample in methanol or ethanol for 6 hours or 12 hours, and removing polar impurities on the surface of the composite insulator;
(3) naturally drying or drying below 60 ℃;
(4) detecting the surface of the sample by using a time-of-flight secondary ion mass spectrometer;
analyzing the positive ion spectrum, and taking SiCH with m/z of 433 +SiC with m/z 733H9 +The peak height ratio of (A) is used as the aging judgment basis, and the larger the value is, the more serious the aging is.
The invention also provides a method for replacing the high-temperature vulcanized silicone rubber composite insulator, which is used for evaluating the aging degree of the running high-temperature vulcanized silicone rubber composite insulator when SiCH is used3 +With SiC3H9 +When the mass spectrum peak height ratio of the insulator is more than or equal to 1, the insulator is replaced by a new high-temperature vulcanized silicon rubber composite insulator.
Advantageous effects
The invention discloses a method for evaluating the aging state of a high-temperature vulcanized silicone rubber composite insulator, which is used for carrying out flight time secondary ion mass spectrometry detection and quantitative analysis on a characteristic product in the silicone rubber aging process so as to accurately judge the service life state of a material. The power grid company can judge whether the composite insulator needs to be replaced by adopting the diagnosis method, so that the safe and stable operation of the power grid is guaranteed.
Drawings
FIG. 1 shows the result of the secondary flight time ion mass spectrometry detection of the composite insulator subjected to ultraviolet aging for 300 hours in example 1;
FIG. 2 shows the results of ion mass spectrometry for the secondary flight time of the unaged composite insulator in example 1.
Detailed Description
Example 1:
the method for evaluating the aging state of the high-temperature vulcanized silicone rubber composite insulator (110kV alternating-current rod type suspension composite insulator) comprises the following steps:
(1) respectively shearing 1cm from unaged and ultraviolet aged composite insulator for 300 hours2Left and right samples;
(2) soaking the sample in ethanol for 6 hours, and removing polar impurities on the surface of the composite insulator;
(3) naturally drying;
(4) detecting the surface of the sample by using a time-of-flight secondary ion mass spectrometer;
(5) analyzing the positive ion spectrogram, and calculating SiCH with m/z of 433 +SiC with m/z 733H9 +The ratio of the peak heights of (a), the ratio of the unaged sample is 0.17, and the ratio of the sample aged by ultraviolet for 300 hours is 0.25.

Claims (9)

1. The method for evaluating the aging state of the high-temperature vulcanized silicone rubber is characterized in that the aging state of the solid high-temperature vulcanized silicone rubber to be tested is evaluated by directly adopting mass spectrometry.
2. The method for evaluating the aging state of high-temperature vulcanized silicone rubber according to claim 1, wherein the mass spectrum is a time-of-flight secondary ion mass spectrum.
3. The method for evaluating the aging state of high-temperature vulcanized silicone rubber according to claim 1, wherein the high-temperature vulcanized silicone rubber is methyl silicone rubber, methyl vinyl silicone rubber, methyl phenyl vinyl silicone rubber.
4. The method for evaluating the aging state of high-temperature vulcanized silicone rubber according to claim 1, wherein the high-temperature vulcanized silicone rubber to be tested is a high-temperature vulcanized silicone rubber composite insulator.
5. As claimed in claim 1The method for evaluating the aging state of the high-temperature vulcanized silicone rubber is characterized by comprising the following steps of3 +With SiC3H9 +The mass spectrum peak height ratio is used as an aging judgment basis to evaluate the aging state.
6. The method for evaluating the aging state of high-temperature vulcanized silicone rubber according to claim 5, wherein the larger the mass spectrum peak height ratio, the more severe the aging is represented.
7. The method for evaluating the aging state of a high-temperature vulcanized silicone rubber according to claim 1, comprising the steps of:
(1) shearing a sample to be detected from the high-temperature vulcanized silicone rubber;
(2) soaking a sample to be detected in methanol or ethanol;
(3) drying the soaked sample to be detected;
(4) detecting the surface of a sample to be detected by using a time-of-flight secondary ion mass spectrometer;
(5) analyzing the positive ion spectrum, and taking SiCH with m/z of 433 +SiC with m/z 733H9 +The peak height ratio of (A) is used as an aging judgment basis, and the larger the value is, the more serious the aging is.
8. The method for evaluating the aging state of high-temperature vulcanized silicone rubber according to claim 7, wherein the sample to be tested has a size of 1cm2～2cm2；
The soaking time is 6-12 h.
9. A method for replacing a high-temperature vulcanized silicone rubber composite insulator, characterized in that the method of any one of claims 1 to 8 is used for evaluating the aging degree of an operating high-temperature vulcanized silicone rubber composite insulator when SiCH is used3 +With SiC3H9 +When the mass spectrum peak height ratio of the insulator is more than or equal to 1, the insulator is replaced by a new high-temperature vulcanized silicon rubber composite insulator.
CN202010485651.XA 2020-06-01 2020-06-01 Method for evaluating aging state of high-temperature vulcanized silicone rubber Active CN111610249B (en)

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Cited By (3)

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Publication number Priority date Publication date Assignee Title
CN112147475A (en) * 2020-11-03 2020-12-29 国网四川省电力公司电力科学研究院 Method for identifying state of room temperature vulcanized silicone rubber material
CN112432969A (en) * 2020-11-06 2021-03-02 电子科技大学 Composite insulator aging degree improvement detection method based on modulation photothermal radiation
CN113325026A (en) * 2021-04-29 2021-08-31 中国电力科学研究院有限公司 Method for determining aging criterion of silicon rubber insulating material

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112147475A (en) * 2020-11-03 2020-12-29 国网四川省电力公司电力科学研究院 Method for identifying state of room temperature vulcanized silicone rubber material
CN112432969A (en) * 2020-11-06 2021-03-02 电子科技大学 Composite insulator aging degree improvement detection method based on modulation photothermal radiation
CN113325026A (en) * 2021-04-29 2021-08-31 中国电力科学研究院有限公司 Method for determining aging criterion of silicon rubber insulating material

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