CN113092678A - Epoxy resin pair SF under discharge condition6Research method for influence of trace products - Google Patents
Epoxy resin pair SF under discharge condition6Research method for influence of trace products Download PDFInfo
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- 239000003822 epoxy resin Substances 0.000 title claims abstract description 87
- 229920000647 polyepoxide Polymers 0.000 title claims abstract description 87
- 238000000034 method Methods 0.000 title claims abstract description 43
- 239000000463 material Substances 0.000 claims abstract description 55
- 239000000126 substance Substances 0.000 claims abstract description 37
- 238000012360 testing method Methods 0.000 claims abstract description 26
- 238000011160 research Methods 0.000 claims abstract description 22
- 238000001514 detection method Methods 0.000 claims abstract description 21
- 230000000694 effects Effects 0.000 claims abstract description 10
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 15
- 230000008859 change Effects 0.000 claims description 13
- IISBACLAFKSPIT-UHFFFAOYSA-N bisphenol A Chemical class C=1C=C(O)C=CC=1C(C)(C)C1=CC=C(O)C=C1 IISBACLAFKSPIT-UHFFFAOYSA-N 0.000 claims description 12
- 239000004841 bisphenol A epoxy resin Substances 0.000 claims description 6
- PXKLMJQFEQBVLD-UHFFFAOYSA-N bisphenol F Chemical compound C1=CC(O)=CC=C1CC1=CC=C(O)C=C1 PXKLMJQFEQBVLD-UHFFFAOYSA-N 0.000 claims description 4
- 238000006555 catalytic reaction Methods 0.000 claims description 4
- 238000004519 manufacturing process Methods 0.000 claims description 4
- OBTWBSRJZRCYQV-UHFFFAOYSA-N sulfuryl difluoride Chemical compound FS(F)(=O)=O OBTWBSRJZRCYQV-UHFFFAOYSA-N 0.000 claims description 4
- DUGWRBKBGKTKOX-UHFFFAOYSA-N tetrafluoro(oxo)-$l^{6}-sulfane Chemical compound FS(F)(F)(F)=O DUGWRBKBGKTKOX-UHFFFAOYSA-N 0.000 claims description 4
- LSJNBGSOIVSBBR-UHFFFAOYSA-N thionyl fluoride Chemical compound FS(F)=O LSJNBGSOIVSBBR-UHFFFAOYSA-N 0.000 claims description 4
- BRLQWZUYTZBJKN-UHFFFAOYSA-N Epichlorohydrin Chemical compound ClCC1CO1 BRLQWZUYTZBJKN-UHFFFAOYSA-N 0.000 claims description 3
- 238000010891 electric arc Methods 0.000 claims description 3
- 238000002290 gas chromatography-mass spectrometry Methods 0.000 claims description 3
- 239000012212 insulator Substances 0.000 claims description 3
- 238000005259 measurement Methods 0.000 claims description 3
- VPWNQTHUCYMVMZ-UHFFFAOYSA-N 4,4'-sulfonyldiphenol Chemical compound C1=CC(O)=CC=C1S(=O)(=O)C1=CC=C(O)C=C1 VPWNQTHUCYMVMZ-UHFFFAOYSA-N 0.000 claims description 2
- 238000004566 IR spectroscopy Methods 0.000 claims description 2
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 claims description 2
- 238000004817 gas chromatography Methods 0.000 claims description 2
- 238000004949 mass spectrometry Methods 0.000 claims description 2
- 229920003986 novolac Polymers 0.000 claims description 2
- 238000004867 photoacoustic spectroscopy Methods 0.000 claims description 2
- 229910052739 hydrogen Inorganic materials 0.000 abstract description 16
- 229910052760 oxygen Inorganic materials 0.000 abstract description 16
- 229910052799 carbon Inorganic materials 0.000 abstract description 15
- 238000009413 insulation Methods 0.000 abstract description 14
- 238000004458 analytical method Methods 0.000 abstract description 7
- 238000003745 diagnosis Methods 0.000 abstract description 7
- 238000011156 evaluation Methods 0.000 abstract description 6
- 238000005516 engineering process Methods 0.000 abstract description 2
- 239000000047 product Substances 0.000 description 56
- 239000007789 gas Substances 0.000 description 22
- 230000008569 process Effects 0.000 description 8
- 239000000523 sample Substances 0.000 description 7
- 239000012535 impurity Substances 0.000 description 4
- 239000011810 insulating material Substances 0.000 description 4
- 239000007787 solid Substances 0.000 description 4
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 description 3
- 230000009471 action Effects 0.000 description 3
- 230000005540 biological transmission Effects 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
- 238000000354 decomposition reaction Methods 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 229910052731 fluorine Inorganic materials 0.000 description 3
- 239000011737 fluorine Substances 0.000 description 3
- LRWZZZWJMFNZIK-UHFFFAOYSA-N 2-chloro-3-methyloxirane Chemical compound CC1OC1Cl LRWZZZWJMFNZIK-UHFFFAOYSA-N 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 239000003990 capacitor Substances 0.000 description 2
- 239000012159 carrier gas Substances 0.000 description 2
- 239000004020 conductor Substances 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 238000001948 isotopic labelling Methods 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 238000004088 simulation Methods 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 239000004593 Epoxy Substances 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 238000010835 comparative analysis Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000006837 decompression Effects 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000009977 dual effect Effects 0.000 description 1
- 125000003700 epoxy group Chemical group 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 229910000041 hydrogen chloride Inorganic materials 0.000 description 1
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 238000011835 investigation Methods 0.000 description 1
- 238000002372 labelling Methods 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 238000004445 quantitative analysis Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 238000006798 ring closing metathesis reaction Methods 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 238000000935 solvent evaporation Methods 0.000 description 1
- 238000000638 solvent extraction Methods 0.000 description 1
- 238000005979 thermal decomposition reaction Methods 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
- G01N33/0004—Gaseous mixtures, e.g. polluted air
- G01N33/0009—General constructional details of gas analysers, e.g. portable test equipment
- G01N33/0027—General constructional details of gas analysers, e.g. portable test equipment concerning the detector
- G01N33/0036—General constructional details of gas analysers, e.g. portable test equipment concerning the detector specially adapted to detect a particular component
- G01N33/0044—Sulphides, e.g. H2S
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- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Food Science & Technology (AREA)
- Combustion & Propulsion (AREA)
- Physics & Mathematics (AREA)
- Analytical Chemistry (AREA)
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- General Health & Medical Sciences (AREA)
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Abstract
The invention discloses an epoxy resin pair SF under a discharge condition6A research method for influence of trace products belongs to the technical field of electric power. The epoxy resin-based SF6A method for detecting trace products by replacing isotope-labeled epoxy resin material parts with SF6In the gas-insulated apparatus, after the discharge test is performed, SF is measured using a detection apparatus6The variety and content of isotope-containing substances in the gas trace product are changed, so that SF of the epoxy resin under the discharge condition is realized6Study of the effect of minor products. The invention solves the problem of the prior SF6The problem that the source of C, H, O element in trace product is unknown can be directly verified by utilizing an isotope tracing method for SF of the epoxy resin material6Influence rule of trace products. The research method provided by the invention can be used for analyzing SF by utilizing a component analysis technology6The research of the gas insulation equipment for fault diagnosis and electric life evaluation provides key and reliable data support.
Description
Technical Field
The invention belongs to the technical field of electric power, and relates to an epoxy resin pair SF under a discharge condition6Research method of influence of trace products.
Background
SF6The gas insulation equipment is widely applied to a power transmission and transformation system and a power distribution system of a power grid due to the advantages of small occupied area, safe and reliable operation, long maintenance period and the like, and plays a decisive role in the safe and stable operation of the power system. Partial discharge, spark discharge, arc discharge is SF6The electrical discharge phenomena common in gas-insulated equipment, which causes SF6The gas undergoes different degrees of decomposition and SF is produced5、SF4、SF2And the like. The inside of the equipment simultaneously has solid insulating material, metal conductor material and trace moisture and oxygen impurities, and under the action of discharge, SF6The low-fluorine sulfide generated by the decomposition of the gas can further react with the substances and generate SOF2、SO2、SO2F2、SOF4、CF4、C2F6、C3F8、CO2、CO、CH4、CS2、H2S、H2Multiple SF such as HF6Trace amounts of product. In one aspect, certain trace products (e.g., HF, H)2S) solid insulating materials and metal conductor materials in the equipment are further corroded, so that the integral insulation degradation of the equipment is accelerated, and sudden insulation failure of the equipment is caused; on the other hand, some characteristic trace products (e.g. CF)4、SOF2、SO2、CO、CO2) The content and the change rule of the (A) are closely related to the type and the severity of the insulation fault. Thus, can pass SF6The component analysis of the trace product detects and finds SF in time6Early latent fault in the gas insulated equipment, and the insulating state of the gas insulated equipment is scientifically evaluated, and finally SF is realized6Condition monitoring and electrical lifetime assessment of gas-insulated equipment. Thus, for SF6The research on trace products and the influence factors thereof has important significance.
The epoxy resin is a high molecular polymer containing more than two epoxy groups in the molecule, has excellent insulating property, thermal stability and corrosion resistance, and is widely used as SF6Solid insulating materials for gas-insulated apparatus, e.g. insulators in GIS, SF6An insulating pull rod in a circuit breaker. When an electric discharge is generated near the epoxy resin material, epoxy resin molecules are decomposed to different degrees under the combined action of heat and electrons and react with SF6The low-fluorine sulfide generated by the decomposition is chemically reacted, thereby causing the deterioration of the overall insulation of the epoxy resin material and the SF6The type and concentration of the trace products cause significant effects. Thus, with respect to epoxy resin material pairs SF6The study of the effects of trace products is of great interest.
In the conventional experimental research, simulation experiments are generally adopted, different discharge types are preset near the epoxy resin material in the equipment, the discharge time and the discharge amount are adjusted, and the SF is measured by the detection equipment6The variety and content change of trace products are studied by comparative analysis to SF6Minor product effects. The disadvantage of this process is SF6The source of C, H, O element in the trace product is unknown, and SF cannot be directly proved6The variety and concentration of the trace products are affected by the epoxy resin material. In fact, SF in such simulation experiments6The C, H, O element in the trace product may originate not only from the epoxy resin material, but also from traces of moisture and oxygen impurities inside the device, other solid insulating materials, and metal material oxides. The pair of epoxy resin materials is SF6Investigation of effects of trace products and use of compositional analysis techniques on SF6The study of gas-insulated equipment for fault diagnosis and electrical life assessment both pose practical difficulties.
Disclosure of Invention
In order to overcome the disadvantages of the prior art, the invention aims to provide an epoxy resin pair SF under discharge condition6The research method of the influence of trace products solves the problem of SF6The problem that the source of C, H, O element in the trace product is unknown can be directly verified, and the epoxy resin material can be directly verified to SF6The influence rule of trace products defines SF6The variety and concentration of trace product are changed, and SF is increased6The fault diagnosis and the electric life evaluation of the gas insulation equipment use the application performance.
In order to achieve the purpose, the invention adopts the following technical scheme to realize the purpose:
the invention discloses an epoxy resin pair SF under a discharge condition6Research method for influence of trace products, namely replacing isotope-labeled epoxy resin material parts with SF6In the gas-insulated apparatus, after the discharge test is performed, SF is measured using a detection apparatus6The variety and content of isotope-containing substances in the gas trace product are changed, so that SF of the epoxy resin under the discharge condition is realized6Study of the effect of minor products.
Preferably, said one kind of epoxy resin is paired with SF under discharge condition6The research method for the influence of the trace products specifically comprises the following steps: s1, marking elements in the epoxy resin material by utilizing isotopes to obtain the epoxy resin material marked by the isotopes; s2, manufacturing the isotope-labeled epoxy resin material obtained in the step S1 into a part, and replacing the part obtained to SF6In a gas-insulated apparatus; s3, carrying out a discharge test under the condition of meeting the field working condition; s4, measuring SF by using detection equipment6The variety and content of isotope-containing substances in the gas trace product are changed; s5, analyzing the generation and evolution rules of the isotope-containing substances according to the measurement results of the variety and content change of the isotope-containing substances obtained in the step S4, and determining the SF of the epoxy resin material under the discharge condition6Influence of gaseous trace products.
Further preferably, in step S1, at least one of C element, H element, and O element in the epoxy resin material is labeled with an isotope.
Further preferably, in step S1, the epoxy resin material includes: bisphenol a type epoxy resin, bisphenol F type epoxy resin, bisphenol S type epoxy resin, hydrogenated bisphenol a type epoxy resin, and phenol novolac type epoxy resin.
Wherein, preferably, the isotope-labeled bisphenol A epoxy resin material is prepared by using bisphenol A containing C element, H element and O element isotope labels and epichlorohydrin containing C element, H element and O element isotope labels under the catalysis of sodium hydroxide.
Further preferably, in step S2, the components include: insulation boardRim, insulating tie bar, SF6The gas-insulated apparatus includes: SF6Switching equipment, GIS, GIL.
Further preferably, in step S3, the discharge test conditions include: arc discharge, partial discharge, spark discharge.
Further preferably, in step S4, SF is measured6The detection method of the gas trace product comprises the following steps: gas chromatography, mass spectrometry, gas chromatography-mass spectrometry, infrared absorption spectrometry, electrochemical sensor method, and photoacoustic spectrometry.
Further preferably, in step S4, SF6Gaseous trace products include: SOF2、SO2、SO2F2、SOF4、CF4、C2F6、C3F8、CO2、CO、CH4、CS2、H2S、H2、HF、H2O、O2。
Further preferably, the operation of analyzing the generation and evolution law of the isotope-containing substance in step S5 includes: comparing the concentrations of the isotope-containing substance and the isotope-free substance, analyzing the change rule of the isotope-containing substance and the isotope-free substance along with the test times and time, and determining the SF ratio of the epoxy resin material under the discharge condition6Influence of gaseous trace products.
Compared with the prior art, the invention has the following beneficial effects:
the invention discloses an epoxy resin pair SF under a discharge condition6The research method of the influence of trace products is that the isotope is used to mark the elements in the epoxy resin material and make corresponding parts of the equipment, and the isotope tracing method is used to research the SF of the epoxy resin material6The influence of trace products solves the problem of the prior SF6The problem that C, H, O element is unknown in trace product is to replace the part with SF6Performing discharge test in gas-insulated equipment, and measuring SF with detection equipment6The variety and content change of C, H, O isotope-containing substances in the gas trace products are analyzed, the generation and evolution rules of the isotope-containing substances are analyzed, and the SF of the epoxy resin material can be directly verified6The influence rule of trace products, and the effect of the epoxy resin material on SF under the discharge condition6Influence of gaseous trace products. Thus, the methods of the invention enable the use of compositional analysis techniques on SF6The research of the gas insulation equipment for fault diagnosis and electric life evaluation provides key and reliable data support.
Furthermore, at least one of C element, H element and O element in the epoxy resin material is marked by using isotope, so that the interference of other C, H, O element-containing materials and impurities on the detection result can be effectively eliminated, and the SF of the epoxy resin material is determined6The influence rule of trace products has good technical effect.
Furthermore, the detection method provided by the invention can be suitable for various epoxy resin materials, and has popularization value for industrial application.
Furthermore, isotope labeling treatment of C element, H element and O element is carried out on two raw materials of bisphenol A and epoxy chloropropane, and then the isotope-labeled bisphenol A epoxy resin material is prepared by sodium hydroxide catalysis, so that the cost investment of the detection method can be effectively reduced, the uniform stability of isotope labeling in parts can be effectively ensured, and further the SF based on epoxy resin is improved6The accuracy of detection of trace products ensures SF6The data of the fault diagnosis and the electric service life evaluation of the gas insulation equipment are reliable.
Further, the isotope-labeled epoxy resin material is made into an insulator, an insulating pull rod and other equipment parts and is replaced to the corresponding SF6In gas-insulated equipment, can be applied to SF under various discharge conditions6The research on trace products of the gas insulation equipment has good universality and is easy to popularize.
Further, SF containing C, H, O element was detected by various detection methods6The trace product is compared with the concentration of the substance containing the isotope and the substance not containing the isotope in the test process, and the change rule of the trace product along with the test times and time is analyzed, so that the change rule of the trace product along with the test times and the change rule of the trace product along with the test time can be determined, and the epoxy resin material for different SF can be determined6The influence of trace products of gas fills up the current technical blank and is SF6The research of the gas insulation equipment for fault diagnosis and electric life evaluation provides key and reliable data support.
Drawings
FIG. 1 shows epoxy resin pairs SF under discharge conditions according to the invention6A flow chart of the implementation of the research method of the influence of the trace products;
FIG. 2 is a process flow diagram for making an isotopically labeled bisphenol A epoxy resin;
FIG. 3 is a wiring diagram of the circuit breaker breaking experiment in the invention;
FIG. 4 is a SOF2The detection result chart of (1).
Wherein: 1-a capacitor bank; 2-a reactor; 3-a main switch; 4-high voltage probe; 5-SF6A circuit breaker; 6-Rogowski coil; 7-oscilloscope.
Detailed Description
In order to make the technical solutions of the present invention better understood, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
It should be noted that the terms "first," "second," and the like in the description and claims of the present invention and in the drawings described above are used for distinguishing between similar elements and not necessarily for describing a particular sequential or chronological order. It is to be understood that the data so used is interchangeable under appropriate circumstances such that the embodiments of the invention described herein are capable of operation in sequences other than those illustrated or described herein. Furthermore, the terms "comprises," "comprising," and "having," and any variations thereof, are intended to cover a non-exclusive inclusion, such that a process, method, system, article, or apparatus that comprises a list of steps or elements is not necessarily limited to those steps or elements expressly listed, but may include other steps or elements not expressly listed or inherent to such process, method, article, or apparatus.
The invention is described in further detail below with reference to the following figures and detailed description:
referring to FIG. 1, it can be seen that the epoxy resin pair SF under discharge condition described in this example6The research method for the influence of trace products comprises the following steps:
1. and marking at least one of C, H, O elements in the epoxy resin material by using the isotope to prepare the isotope-marked epoxy resin material.
Fig. 2 is a flow chart of a process for manufacturing isotope-labeled bisphenol a epoxy resin according to this embodiment. The isotope-labeled bisphenol A epoxy resin is prepared from isotope-labeled bisphenol A and isotope-labeled epichlorohydrin under the catalysis of sodium hydroxide. Sodium hydroxide plays a dual role therein: the first is used as a catalyst for the reaction of epoxy chloropropane and bisphenol A; secondly, the reaction product is subjected to ring closure by removing hydrogen chloride. The whole manufacturing process needs multiple steps of material adding and dissolving, reaction, decompression and recovery, solvent extraction, water washing, filtration, water washing, solvent evaporation, drying and the like to prepare the isotope-labeled epoxy resin material finished product.
2. Preparing the isotope-labeled epoxy resin material into corresponding equipment parts, and replacing the parts to SF6In a gas-insulated apparatus.
In this embodiment, the epoxy resin material labeled with isotope is prepared into 40.5kV SF6An insulating pull rod in the circuit breaker 5 and replacing the insulating pull rod with a normal pull rod in the circuit breaker.
3. And carrying out a discharge test under the condition of meeting the field working condition. Fig. 3 is a wiring diagram of the circuit breaker opening test performed in this embodiment.
Specifically, in the present embodiment, referring to fig. 3, it can be known that the test current is provided by an LC tank, where the current source capacitor bank 1 is 89.68mF, the reactor 2 is 0.1130mH, and the test current frequency is 50 Hz. Through main switches 3 and SF6The circuit breaker 5 completes the breaking test by the time sequence matching, and measures the arc current and the arc voltage through the Rogowski coil 6 and the high-voltage probe 4, and the arc current and the arc voltage are displayed through the indicatorThe wave filter 7 records the waveform. The on-off current is supposed to be set to be 10kA, the on-off is carried out for 5 times, and the gas in the gas chamber is sampled and analyzed after the on-off test is finished each time.
4. Measuring SF using a detection device6The type and content of at least one of C, H, O isotope substances in the gaseous trace product are changed. In this embodiment, a gas chromatography-mass spectrometry combined method is adopted to perform detection and analysis on a gas sample, and in order to ensure successful detection and analysis of a substance containing C, H, O isotopes, the carrier gas flow, the sample inlet temperature, the sample injection amount, the column box step rise temperature, the transmission advance temperature, the ion source and quadrupole temperature, the acquisition mode, and the solvent delay of the device need to be set reasonably.
Specifically, in the present embodiment, the instrument detection parameters are as follows:
a) and (3) carrier gas control: he, 1.5 mL/min.
b) Sample inlet temperature: at 150 ℃.
c) Sample introduction amount: 250 microliter, the split ratio is 20: 1.
d) Column temperature: keeping the temperature at 50 ℃ for 5min, and increasing the temperature to 200 ℃ at 10 ℃/min for 10 min.
e) Transmission line temperature: at 250 ℃ to obtain a mixture.
f) An ion source: EI, temperature 230 ℃ and electron energy 70 eV.
g) An acquisition mode: MS, mass range 32-500 amu.
h) Solvent retardation: 3min
5. According to the measurement result of the variety and content change of the obtained isotope-containing substance, the generation and evolution rules of the isotope-containing substance are analyzed, and the SF of the epoxy resin material is determined6Influence of gaseous trace products. Wherein, the concentrations of the isotope-containing substance and the isotope-free substance in the test process need to be fully compared, the change rule of the isotope-containing substance and the isotope-free substance along with the test times and time is analyzed, and the SF of the epoxy resin material under the discharge condition is determined6Influence of gaseous trace products.
Specifically, in this example, referring to fig. 4, it can be seen that the O element-labeled product SOF2The detection result of (2) shows that SOF can be found2The total concentration of (A) shows a gradually rising trend along with the increase of the on-off times, and the 5-time on-off test is endedPost SOF2The total concentration can reach 2347.9 ppm. S can be detected simultaneously in the process of the breaking test16OF2And S18OF2Two classes of isotope substances, of which S is the end of 5 breaking tests16OF2In a concentration of 2111.8ppm, about 89.9% of the total concentration, S18OF2The concentration of (B) was only 236.1ppm, which was about 10.1% of the total concentration. Due to the fact that18Since O is almost exclusively present in the epoxy resin material of the treated insulating tie rod, S is known to be present18OF2Is produced as a result of the thermal decomposition of the epoxy resin under the action of the hot gas stream and further reaction with the low-fluorine sulfide. From this it can be clearly derived that SF in the circuit breaker6Trace product SOF2The formation of (A) is influenced by the epoxy resin material of the insulating pull rod, but the influence degree is very limited, and only about 10 percent of SOF is generated2The formation of (2) is directly related to the insulating tie bar epoxy material, about 90% SOF2Is generated independently thereof, the partial SOF2Mainly receives trace H in the equipment2O and O2The influence of impurities. SO (SO)2、SO2F2、SOF4、CF4、C2F6、C3F8、CO2、CO、CH4、CS2、H2S、H2、HF、H2O、O2At least one of the C, H, O-element labeling substances can be subjected to similar quantitative analysis. The invention solves the problem of the prior SF6The problem that the source of C, H, O element in the trace product is unknown can be directly verified, and the epoxy resin material can be directly verified to SF6Influence rule of trace products. The research method provided by the invention can be used for analyzing SF by utilizing a component analysis technology6The research of the gas insulation equipment for fault diagnosis and electric life evaluation provides key and reliable data support.
In summary, the present invention discloses an epoxy resin pair SF under discharge condition6Method for investigating the influence of trace products, in SF6Research on epoxy resin pair SF in gas insulation equipment6Gaseous trace product effects. The method utilizes the isotope to mark C, H, O element in the epoxy resin material and makes the correspondingReplacing the component with SF6Performing discharge test in gas-insulated equipment, and measuring SF with detection equipment6The variety and the content change of C, H, O isotope-containing substances in the gas trace products are analyzed, the generation and evolution rules of the isotope-containing substances are analyzed, and the SF of the epoxy resin material are determined6Influence of gaseous trace products.
The above-mentioned contents are only for illustrating the technical idea of the present invention, and the protection scope of the present invention is not limited thereby, and any modification made on the basis of the technical idea of the present invention falls within the protection scope of the claims of the present invention.
Claims (10)
1. Epoxy resin pair SF under discharge condition6The research method of the influence of the trace products is characterized in that isotope-labeled epoxy resin material parts are replaced to SF6In the gas-insulated apparatus, after the discharge test is performed, SF is measured using a detection apparatus6The variety and content of isotope-containing substances in the gas trace product are changed, so that SF of the epoxy resin under the discharge condition is realized6Study of the effect of minor products.
2. Epoxy resin pair SF according to claim 16The research method for the influence of the trace products is characterized by comprising the following steps:
s1, marking elements in the epoxy resin material by utilizing isotopes to obtain the epoxy resin material marked by the isotopes;
s2, manufacturing the isotope-labeled epoxy resin material obtained in the step S1 into a part, and replacing the part obtained to SF6In a gas-insulated apparatus;
s3, carrying out a discharge test under the condition of meeting the field working condition;
s4, measuring SF by using detection equipment6The variety and content of isotope-containing substances in the gas trace product are changed;
s5, classifying the isotope-containing substance according to the measurement result of the type and content change of the isotope-containing substance obtained in the step S4The generation and evolution rule of isotope-containing substances are analyzed, and the SF of the epoxy resin material under the discharge condition is determined6Influence of gaseous trace products.
3. Epoxy resin pair SF according to claim 26The method for investigating the influence of a trace product is characterized in that at least one of C element, H element and O element in the epoxy resin material is labeled with an isotope in step S1.
4. Epoxy resin pair SF according to claim 26The method for studying the influence of the trace product is characterized in that in step S1, the epoxy resin material includes: bisphenol a type epoxy resin, bisphenol F type epoxy resin, bisphenol S type epoxy resin, hydrogenated bisphenol a type epoxy resin, and phenol novolac type epoxy resin.
5. The epoxy resin pair SF according to claim 46The research method for the influence of trace products is characterized in that the isotope-labeled bisphenol A epoxy resin material is prepared from isotope-labeled bisphenol A containing C elements, H elements and O elements and isotope-labeled epichlorohydrin containing C elements, H elements and O elements under the catalysis of sodium hydroxide.
6. Epoxy resin pair SF according to claim 26The method for investigating the influence of a trace product, wherein in step S2, the parts include: insulator, insulating rod, SF6The gas-insulated apparatus includes: SF6Switching equipment, GIS, GIL.
7. Epoxy resin pair SF according to claim 26The method for investigating the influence of a trace product, wherein in step S3, the discharge test conditions include: arc discharge, partial discharge, spark discharge.
8. Root of herbaceous plantThe epoxy resin pair SF according to claim 26The method for investigating the influence of a trace product, characterized in that SF is measured in step S46The detection method of the gas trace product comprises the following steps: gas chromatography, mass spectrometry, gas chromatography-mass spectrometry, infrared absorption spectrometry, electrochemical sensor method, and photoacoustic spectrometry.
9. Epoxy resin pair SF according to claim 26The method for investigating the influence of a trace product, wherein SF is used in step S46Gaseous trace products include: SOF2、SO2、SO2F2、SOF4、CF4、C2F6、C3F8、CO2、CO、CH4、CS2、H2S、H2、HF、H2O、O2。
10. Epoxy resin pair SF according to claim 26The method for studying the influence of the trace product is characterized in that in step S5, the operation of analyzing the generation and evolution law of the isotope-containing substance includes: comparing the concentrations of the isotope-containing substance and the isotope-free substance, analyzing the change rule of the isotope-containing substance and the isotope-free substance along with the test times and time, and determining the SF ratio of the epoxy resin material under the discharge condition6Influence of gaseous trace products.
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