CN105223217A - The method that in detecting insulating oil, active sulfur compound exists in situation is there is based on oxygen - Google Patents
The method that in detecting insulating oil, active sulfur compound exists in situation is there is based on oxygen Download PDFInfo
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- CN105223217A CN105223217A CN201510577997.1A CN201510577997A CN105223217A CN 105223217 A CN105223217 A CN 105223217A CN 201510577997 A CN201510577997 A CN 201510577997A CN 105223217 A CN105223217 A CN 105223217A
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Abstract
The method that in detecting insulating oil, active sulfur compound exists in situation is there is based on oxygen, comprise the following steps 1. to be utilized by the copper conductor wrapped with insulating paper Linear cut to cut equipment to be slit into the uniform sample of some shapes and to be placed in vacuum tank, under certain condition, keep 12-48 hour; 2. in insulating oil, add DBDS, after seal under environment that is airtight, that be full of nitrogen; 3. by above-mentioned sealed copper winding sample as in vacuum ageing oven, thermal aging time is 72-1000 hour, copper winding is divested insulating paper, detects after Linear cut; The present invention has following beneficial effect: the method for inspection of the present invention is considered in power equipment has a small amount of oxygen to there is situation, by regulating ageing environment vacuum degree control oxygen concentration, carries out acceleration heat ageing to copper conductor.By utilizing scanning electron microscope to generate situation to copper conductor surface microscopic topographic (etch pit distribution and the degree of depth) and corrosion product, in detecting insulating oil, whether active sulfur compound exists, and detects power equipment running status thus.
Description
Technical field
The invention belongs to electrical engineering and material science and intersect category, specifically, being a kind of based under oxygen existence, by utilizing STUDY ON Scanning Electron Microscope copper conductor microscopic appearance and corrosion product to generate situation, judging the method for inspection that whether there is active sulfur compound in insulating oil component.
Background technology
Paper oil insulation is the primary insulation form of the composition of important power transmission and transforming equipment in the electrical networks such as oil-immersed power transformer, sleeve pipe, reactor and capacitor, the performance degradation that paper oil insulation occurs under the effects such as heat, electric field and oxygen, acid, water grading factors and electrical specification decline are one of key factors causing oil immersed type power transmission and transforming equipment fault.Major part achievement in research generally believes, the agine mechaism of paper oil insulation material is under above-mentioned each factor effect, the fiber molecule long-chain forming oilpaper material and the hydrocarbon compound forming insulating oil decompose, strand is caused to shorten, generate furan compound, moisture, sour isopolarity small-molecule substance be dissolved in oil, thus cause the machinery of paper oil insulation, electric property declines.But in recent years, a kind ofly causing the new phenomenon of paper oil insulation hydraulic performance decline---" oily sulfur corrosion causes insulating property to fail " phenomenon obtains understanding and the concern of people gradually.This phenomenon is mainly because the active sulfur compound in insulating oil and copper conductor react, generating a kind of semiconductor cuprous sulfide is deposited on insulating paper, and shift between insulating paper layer, reduce the conductivity of paper oil insulation, increase dielectric loss, and finally cause breakdown accident.The international bulk power grid CIGRE council has set up WGA2-32 and A2-40 working group in succession in 2005 and 2009, has carried out monographic study to the problem such as " cuprous sulfide in transformer " and " the long-term suppression of cuprous sulfide and hazard evaluation ".Research report is pointed out, although the source of strict control mineral oil and sulfur content can reduce the probability of happening of this phenomenon to a certain extent, but in fact also cannot stop the harm caused by this phenomenon completely, as long as because the content of active sulfur reaches 1ppm in transformer insulation oil, the copper product in transformer will be corroded.CIGRE points out in research report " also having a lot of problem to need to be familiar with further, to study and to solve about the oily sulfur corrosion phenomenon in transformer ".
Over nearly 5 years, the hazard mechanism of oily sulfur corrosion problem to the equipment such as transformer, reactor obtains Preliminary study.The harm, source, coherent detection standard, braking measure etc. of active sulfur in mineral insulating oil are all studied.Most of imported oils that transformer (containing reactor) insulating oil uses, concentrate on several large insulating oil production supplier: Mitsubishi, Sweden Ni Nasi, shell, state's produce oil is generally Karamay, Xinjiang and Lanzhou oil, show from findings of the survey, state's produce oil and Mitsubishi's oil, shell are oily general not containing active sulfur, and Ni Nasi oil all exists active sulfur problem substantially.The suggestion that Ni Nasi oil manufacturing company provides is: in operating transformer oil, add passivator.And comparatively generally acknowledge in the world at present method be also add passivator in transformer oil, passivator is benzotriazole (BTA) and derivant thereof.The heteroatomss such as N, O, S in BTA and derivative molecular thereof contain lone pair electrons; be easy to combine with the d track of metal form coordination bond; or metal carrying supplied for electronic forms back coordination key to heteroatoms; thus form diaphragm in metal surface, stop the oxidation of Transformer Winding coil and the contact with active sulfur in oil.But passivator can not make established copper sulfide occur backward reaction and can only suppress to corrode further generation, and passivator can constantly consume in time.But do not contain in the insulating oil of active sulfur at state's produce oil and Mitsubishi's oil, oily these of shell and still there is inactive sulfur, such as: in domestic In Karamay Oil, sulfur content is about 890ppm.When local overheating or shelf depreciation, inactive sulfur can change to active sulphur.Simultaneously in power equipment, the existence of trace oxygen also can the carrying out of accelerated corrosion.What this illustrated passivator adds the generation can taking precautions against active sulfur problem to a certain extent, but the problem of copper sulfur corrosion still exists.Select suitable method, especially consider detection transformer being carried out under the existence of trace oxygen to active sulfur, and effective risk assessment is carried out to transformer and running status assessment is significant.
Summary of the invention
Technical matters: technical matters to be solved by this invention is: provide a kind of based under oxygen existence, by utilizing STUDY ON Scanning Electron Microscope copper conductor microscopic appearance and corrosion product to generate situation, judge the method for inspection that whether there is active sulfur compound in insulating oil component.
Technical scheme: for solving the problems of the technologies described above, the technical solution used in the present invention is:
There is based on oxygen the method that in detecting insulating oil, active sulfur compound exists in situation, it is characterized in that, this measuring method comprises the following steps:
The copper conductor wrapped with insulating paper utilizes Linear cut to cut equipment and is slit into the uniform sample of some shapes and is placed in vacuum tank by step 1., dry 12-72 hour at 80-100 DEG C, after be cooled to 20-40 DEG C, immerse the degassed new transformer oil (not containing active sulfur compound, total sulfur content≤1000ppm) that dewaters and keep 12-48 hour;
Step 2. adds DBDS in insulating oil, and concentration is 0-1000ppm, and by oil (quality g): (surface area cm
2) ratio scope be 2-50, insulating oil is added in conical flask, copper conductor sample after immersion oil is loaded in conical flask simultaneously, copper winding is kept vertically to hang immersion insulating oil, after conical flask is placed in vacuum nitrogen case, vacuumize and under vacuum state, fill nitrogen to one standard atmospheric pressure, after seal under environment that is airtight, that be full of nitrogen;
Step 3. is by above-mentioned sealed copper winding sample as in vacuum ageing oven, and control temperature 80-200 DEG C, vacuum tightness 0.01-1MPa carry out thermal aging test, and thermal aging time is 72-1000 hour, copper winding is divested insulating paper, detects after Linear cut;
Step 4. directly observes copper conductor surface condition, utilizes scanning electron microscope/power spectrum to detect copper conductor surface microscopic topographic and element kind and content further, observes etch pit size, the degree of depth and corrosion product and generates situation.(as there is etch pit on copper conductor surface, and in etch pit, occurring that shape is cubical corrosion product)
Beneficial effect of the present invention: there is no under considering that oxygen exists situation at present, by observing copper conductor microscopic appearance and corrosion product situation, the method that in detecting insulating oil, whether active sulfur compound exists.The present invention has following beneficial effect:
The method of inspection of the present invention is considered in power equipment has a small amount of oxygen to there is situation, by regulating ageing environment vacuum degree control oxygen concentration, carries out acceleration heat ageing to copper conductor.By utilizing scanning electron microscope to generate situation to copper conductor surface microscopic topographic (etch pit distribution and the degree of depth) and corrosion product, in detecting insulating oil, whether active sulfur compound exists, and detects power equipment running status thus.
Accompanying drawing explanation
Fig. 1, Fig. 2 are the microscopic appearance of aging rear copper conductor sample surfaces in insulating oil in example 1 step 4 of the present invention;
Fig. 3, Fig. 4, Fig. 5 are microscopic appearance and the corrosion product generation situation of aging rear copper conductor sample surfaces in 200ppmDBDS insulating oil in example 2 step 4 of the present invention;
Fig. 6, Fig. 7, Fig. 8 are microscopic appearance and the corrosion product generation situation of aging rear copper conductor sample surfaces in 500ppmDBDS insulating oil in example 3 step 4 of the present invention.
Embodiment
Below in conjunction with accompanying drawing and embodiment, technical scheme of the present invention is described in detail.
Embodiment 1:
Of the present inventionly a kind ofly consider that oxygen exists the method that in detecting insulating oil, active sulfur compound exists in situation, comprise the following steps:
The copper conductor wrapped with insulating paper utilizes Linear cut to cut equipment and is slit into the uniform sample of some shapes and is placed in vacuum tank by step 1., at 90 DEG C dry 48 hours, after be cooled to 40 DEG C, immerse the degassed new transformer oil that dewaters and keep 12 hours.
Step 2. presses 1g oil: 0.5cm
2the ratio of copper adds insulating oil in conical flask, copper conductor sample after immersion oil is loaded in conical flask simultaneously, copper bar is kept vertically to hang immersion insulating oil, after conical flask is placed in vacuum nitrogen case, vacuumize and under vacuum state, fill nitrogen to one standard atmospheric pressure, after seal under environment that is airtight, that be full of nitrogen.
Step 3. is by above-mentioned copper conductor sample respectively as in 150 DEG C of vacuum ageing ovens, and control vacuum 0.9MPa and carry out thermal aging test, thermal aging time is 72 hours, and sampling is measured.
Step 4. utilizes scanning electron microscope/power spectrum to detect copper conductor surface microscopic topographic and element kind and content, observes etch pit size and corrosion product generates situation.Fig. 1, Fig. 2 are the microscopic appearance of aging rear copper conductor sample surfaces in insulating oil in case step 4 of the present invention, corrosion-free phenomenon.
Embodiment 2:
Of the present inventionly a kind ofly consider that oxygen exists the method that in detecting insulating oil, active sulfur compound exists in situation, comprise the following steps:
The copper conductor wrapped with insulating paper utilizes Linear cut to cut equipment and is slit into the uniform sample of some shapes and is placed in vacuum tank by step 1., at 90 DEG C dry 48 hours, after be cooled to 40 DEG C, immerse the degassed new transformer oil that dewaters and keep 12 hours.
Step 2. adds DBDS in insulating oil, and concentration is 200ppm, by 1g oil: 0.5cm
2the ratio of copper adds insulating oil in conical flask, copper conductor sample after immersion oil is loaded in conical flask simultaneously, copper bar is kept vertically to hang immersion insulating oil, after conical flask is placed in vacuum nitrogen case, vacuumize and under vacuum state, fill nitrogen to one standard atmospheric pressure, after seal under environment that is airtight, that be full of nitrogen.
Step 3. by above-mentioned copper conductor sample respectively as in 145 DEG C of vacuum ageing ovens, control vacuum 0.5MPa and carry out thermal aging test, thermal aging time is 96 hours, and sampling is measured, macroscopically see that copper conductor surface color slightly changes, change to brown by light is yellow.
Step 4. utilizes scanning electron microscope/power spectrum to detect copper conductor surface microscopic topographic and element kind and content, observes etch pit size and corrosion product generates situation.Fig. 3, Fig. 4, Fig. 5 are microscopic appearance and the corrosion product generation situation of aging rear copper conductor sample surfaces in 200ppmDBDS insulating oil in case step 4 of the present invention, obvious etch pit has been there is from figure copper conductor surface, and occur that obvious shape is cubical corrosion product in hole, through power spectrum test mainly containing elements such as Cu, S, C.
Embodiment 3:
Of the present inventionly a kind ofly consider that oxygen exists the method that in detecting insulating oil, active sulfur compound exists in situation, comprise the following steps:
The copper conductor wrapped with insulating paper utilizes Linear cut to cut equipment and is slit into the uniform sample of some shapes and is placed in vacuum tank by step 1., at 90 DEG C dry 48 hours, after be cooled to 40 DEG C, immerse the degassed new transformer oil that dewaters and keep 12 hours.
Step 2. adds DBDS in insulating oil, and concentration is 500ppm, by 1g oil: 0.5cm
2the ratio of copper adds insulating oil in conical flask, copper conductor sample after immersion oil is loaded in conical flask simultaneously, copper bar is kept vertically to hang immersion insulating oil, after conical flask is placed in vacuum nitrogen case, vacuumize and under vacuum state, fill nitrogen to one standard atmospheric pressure, after seal under environment that is airtight, that be full of nitrogen.
Step 3. is by above-mentioned copper conductor sample respectively as in 130 DEG C of vacuum ageing ovens, and control vacuum 0.01MPa and carry out thermal aging test, thermal aging time 240 hours, sampling is measured.
Step 4. utilizes scanning electron microscope/power spectrum to detect copper conductor surface microscopic topographic and element kind and content, observes etch pit size and corrosion product generates situation.Fig. 6, Fig. 7, Fig. 8 is microscopic appearance and the corrosion product generation situation of aging rear copper conductor sample surfaces in 500ppmDBDS insulating oil in case step 4 of the present invention, obvious etch pit has been there is from figure copper conductor surface, but the number of etch pit, diameter and the degree of depth are all obviously greater than aging rear copper conductor sample surfaces situation in 200ppmDBDS insulating oil, and in hole, occur that obvious shape is that cubical corrosion product quantity is obviously more than the amount of product in rear copper conductor sample etches hole aging in 200ppmDBDS insulating oil, through power spectrum test still mainly containing Cu, S, the elements such as C.
Claims (1)
1. there is based on oxygen the method that in detecting insulating oil, active sulfur compound exists in situation, it is characterized in that, this measuring method comprises the following steps:
The copper conductor wrapped with insulating paper utilizes Linear cut to cut equipment and is slit into the uniform sample of some shapes and is placed in vacuum tank by step 1., dry 12-72 hour at 80-100 DEG C, after be cooled to 20-40 DEG C, immerse the degassed new transformer oil dewatered, oil is not containing active sulfur compound, total sulfur content≤1000ppm, and keep 12-48 hour;
Step 2. adds DBDS in insulating oil, and concentration is 0-1000ppm, and by oil quality g: surface area cm
2ratio scope be 2-50, insulating oil is added in conical flask, copper conductor sample after immersion oil is loaded in conical flask simultaneously, copper winding is kept vertically to hang immersion insulating oil, after conical flask is placed in vacuum nitrogen case, vacuumize and under vacuum state, fill nitrogen to one standard atmospheric pressure, after seal under environment that is airtight, that be full of nitrogen;
Step 3. is by above-mentioned sealed copper winding sample as in vacuum ageing oven, and control temperature 80-200 DEG C, vacuum tightness 0.01-1MPa carry out thermal aging test, and thermal aging time is 72-1000 hour, copper winding is divested insulating paper, detects after Linear cut;
Step 4. directly observes copper conductor surface condition, utilizes scanning electron microscope to detect copper conductor surface microscopic topographic further, observes etch pit size, the degree of depth and corrosion product and generates situation.
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Cited By (4)
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| CN105699417A (en) * | 2016-01-25 | 2016-06-22 | 云南电网有限责任公司电力科学研究院 | Characterization method for corrosive sulfur of transformer insulating oil |
| CN106198588A (en) * | 2016-08-17 | 2016-12-07 | 云南电网有限责任公司电力科学研究院 | The detection method of objectionable impurities in a kind of transformator copper conductor |
| CN107390258A (en) * | 2017-09-12 | 2017-11-24 | 广东电网有限责任公司电力科学研究院 | The confirmation method of point of discharge on a kind of insulating paper |
| CN108802341A (en) * | 2017-05-03 | 2018-11-13 | 北京至感传感器技术研究院有限公司 | The on-line monitoring system of active sulfur in liquid oil |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105699417A (en) * | 2016-01-25 | 2016-06-22 | 云南电网有限责任公司电力科学研究院 | Characterization method for corrosive sulfur of transformer insulating oil |
| CN106198588A (en) * | 2016-08-17 | 2016-12-07 | 云南电网有限责任公司电力科学研究院 | The detection method of objectionable impurities in a kind of transformator copper conductor |
| CN108802341A (en) * | 2017-05-03 | 2018-11-13 | 北京至感传感器技术研究院有限公司 | The on-line monitoring system of active sulfur in liquid oil |
| CN107390258A (en) * | 2017-09-12 | 2017-11-24 | 广东电网有限责任公司电力科学研究院 | The confirmation method of point of discharge on a kind of insulating paper |
| CN107390258B (en) * | 2017-09-12 | 2019-03-22 | 广东电网有限责任公司电力科学研究院 | The confirmation method of point of discharge on a kind of insulating paper |
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Application publication date: 20160106 |