CN102175502A - Method for oscillated extraction of furfural components from insulated oil - Google Patents
Method for oscillated extraction of furfural components from insulated oil Download PDFInfo
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- CN102175502A CN102175502A CN 201110020618 CN201110020618A CN102175502A CN 102175502 A CN102175502 A CN 102175502A CN 201110020618 CN201110020618 CN 201110020618 CN 201110020618 A CN201110020618 A CN 201110020618A CN 102175502 A CN102175502 A CN 102175502A
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- extraction
- furfural
- medical glass
- needle tubing
- oil
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Abstract
The invention relates to the technical field of power transmission and transformation, in particular to a method for oscillated extraction of furfural components from insulated oil of a power transformer. The method comprises the following steps of: 1) extracting about 50mL oil samples from a 100mL medical glass needle tube and adjusting the volume of the oil samples to 40mL; 2) adjusting a 100mL medical glass needle tube to maintain a 10mL space, adding 5.0mL alcohol, performing oscillation extraction, and detecting furfural, wherein time for the balance of the oscillation extraction is more than or equal to three minutes, and temperature for the extraction is less than or equal to 30 DEG C. Based on the oscillation theory, the method is simple and fast in operation and stable in extraction rate and accords with the requirement of quantitative analysis, and lays a solid foundation for subsequent instrument analysis and evaluation on paper insulation aging and insulation service life of a transformer.
Description
Technical field
The present invention relates to the power transmission and transformation technical field, specifically relate to furfural component oscillation extraction method in a kind of electric power transformer insulated oil.
Background technology
Power transformer paper insulation is in operation and is subjected to the acting in conjunction of acid compound in heat, moisture content, oxygen and the oil, cellulose meeting cracking, degraded, produce some Oxygenic heterocyclic compounds, furfural is exactly a kind of main oxygen helerocyclics that cellulose macromolecule degraded back forms.The most reliable method of judging the papery insulation ag(e)ing is to survey its degree of polymerization, but this method sampling difficulty only just can be carried out when cover is hung in the transformer overhaul.Adopted a kind of comparatively practical transformer Aging of Oil-paper Insulation in Oil method of discrimination-high performance liquid chromatography (HPLC) furfural content analytic approach abroad, this method can estimate the degree of polymerization of insulating paper by furfural content in the test oil.Because transformer insulation oil is in long-time running, oxidized inevitably, deterioration, its deterioration product and impurity composition complexity, oil sample directly should not be injected the liquid chromatography separating column, to avoid of the pollution of deterioration oil product to chromatographic column, therefore selecting the methyl alcohol of strong polarity for use is extractant, and the furfural extraction in the transformer oil is come out to seem very necessary.
The present domestic methyl alcohol that uses carries out furfural extraction as extractant, usually use the method for Centrifugical extraction, by with a certain amount of transformer insulation oil with after a certain amount of methyl alcohol mixes, put into centrifugal separator and carry out extract and separate, the methyl alcohol mixed liquor after the taking-up extraction is analyzed furfural content wherein then.Because this method need be purchased centrifugal separator, extraction process is loaded down with trivial details, therefore utilizes existing transformer oil analytical equipment, and the innovation of carrying out the furfural extraction method just seems necessary.
Summary of the invention
The technical problem to be solved in the present invention is the deficiency that exists at prior art, and furfural component oscillation extraction method in a kind of insulating oil is provided.
Furfural component oscillation extraction method is achieved by following technical proposals in a kind of insulating oil of the present invention: furfural component oscillation extraction method in a kind of insulating oil, it is characterized in that: described method comprises the steps:
1) in 100mL medical glass needle tubing, extracts about 50mL oil sample, adjust the oil sample volume to 40m;
2) adjust 100mL medical glass needle tubing and keep the 10mL space, the methyl alcohol that adds the 5.0mL volume, under the uniform temperature condition through the certain hour oscillation extraction, after treating static layering, the methanol extraction liquid of 100mL medical glass needle tubing middle and upper part is transferred to is used for furfural in the medical glass needle tubing of 5.0mL volume and measures;
Described oscillation extraction reaches balance time 〉=3 minute, extraction temperature≤30 ℃.
Furfural component oscillation extraction method has following beneficial effect compared with prior art in a kind of insulating oil of the present invention: by the research success to furfural component oscillation extraction method in the insulating oil, for carrying out furfural content mensuration in the transformer oil, for good basis has been laid in the assessment of carrying out insulation ag(e)ing of transformer papery and insulation life.The inventive method has been utilized the succusion principle, and is simple and quick, and percentage extraction is stable, meets the quantitative test requirement, for good basis has been laid in follow-up instrumental analysis and the assessment of carrying out insulation ag(e)ing of transformer papery and insulation life.
Embodiment
Below in conjunction with embodiment furfural component oscillation extraction method and technology scheme in a kind of insulating oil of the present invention is further described.
Furfural component oscillation extraction method comprises the steps: in a kind of insulating oil of the present invention
1) in 100mL medical glass needle tubing, extracts about 50mL oil sample, adjust the oil sample volume to 40m;
2) adjust 100mL medical glass needle tubing and keep the 10mL space, the methyl alcohol that adds the 5.0mL volume, under the uniform temperature condition through the certain hour oscillation extraction, after treating static layering, the methanol extraction liquid of 100mL medical glass needle tubing middle and upper part is transferred to is used for furfural in the medical glass needle tubing of 5.0mL volume and measures;
Described oscillation extraction reaches balance time 〉=3 minute, extraction temperature≤30 ℃.
At ambient temperature through 5 minutes oscillation extraction balances, after static 5 minutes, the methanol extraction liquid of 100mL medical glass needle tubing middle and upper part is transferred to by 0.45 μ m needle-based oiliness filter membrane is used for furfural in the medical glass needle tubing of 5.0mL volume and measures.
Described oscillator is 275 times/min of reciprocating vibration frequency ± 5 times/min; Amplitude 35mm ± 3mm; Glass syringe is 100ml, 5 ml medical glass syringes, and impermeability is good, and the core plug does not have bite flexibly; Stainless steel syringe needle: No. 7 metal syringe needles; Syringe rubber sealing cap: good springiness is airtight; Filtering membrane is ф 40,0.45 μ m oiliness filter membranes; 0.45 μ m needle-based oiliness filter membrane; (is 75% still for medicine methyl alcohol?): the efficient liquid phase chromatographic analysis special agent; Isopropyl alcohol: chromatographically pure; Furfural: analyze pure.
Embodiment 1.
Extraction essence at material is to be extracted the dissolution equilibrium that material reaches under certain state in two kinds of mutual insoluble matters, in this case according to dissolution equilibrium analytical approach principle, utilizing the shaker vibration is dissolution equilibrium, carry out the research of furfural component oscillation extraction method in the insulating oil, its concrete method of work is as follows:
Shaker:
275 times/min of reciprocating vibration frequency ± 5 times/min; Amplitude 35mm ± 3mm.
Glass syringe:
100ml, 5 ml medical glass syringes, impermeability is good, and the core plug does not have bite flexibly.
Stainless steel syringe needle: No. 7 metal syringe needles.
Syringe rubber sealing cap: good springiness is airtight.
Filtering membrane:
ф 40,0.45 μ m oiliness filter membranes;
0.45 μ m needle-based oiliness filter membrane.
Medicine
Methyl alcohol: efficient liquid phase chromatographic analysis special agent.
Isopropyl alcohol: chromatographically pure.
Furfural: analyze pure.
Method of operating: in 100mL medical glass needle tubing, extract about 50mL oil sample, adjust the oil sample volume to 40mL, adjust 100mL medical glass needle tubing and keep the 10mL space, the methyl alcohol that adds the 5.0mL volume, under the uniform temperature condition through the certain hour oscillation extraction, after treating static layering, the methanol extraction liquid of 100mL medical glass needle tubing middle and upper part is transferred to is used for furfural in the medical glass needle tubing of 5.0mL volume and measures.
In insulating oil in the furfural component oscillation extraction method, relation to extraction quantity and duration of oscillation, temperature is to the influence of extraction, the effect of extracting of the oil sample of different furfural concentration carries out abundant experimental study, the minimum time of having found oscillation extraction to reach balance at last is no less than 3 minutes, percentage extraction is more stable at normal temperatures, extraction temperature generally should be lower than 30 ℃, the operating conditions of Que Dinging is at last: at ambient temperature through 5 minutes oscillation extraction balances, after static 5 minutes, the methanol extraction liquid of 100mL medical glass needle tubing middle and upper part is transferred to by 0.45 μ m needle-based oiliness filter membrane is used for furfural in the medical glass needle tubing of 5.0mL volume and measures.
By research success, for carrying out furfural content mensuration in the transformer oil, for good basis has been laid in the assessment of carrying out insulation ag(e)ing of transformer papery and insulation life to furfural component oscillation extraction method in the insulating oil.
The above only is preferred embodiment of the present invention, not in order to restriction the present invention, all any modifications of being done within the spirit and principles in the present invention, is equal to and replaces and improvement etc., all should be included within protection scope of the present invention.
Claims (3)
1. furfural component oscillation extraction method in the insulating oil, it is characterized in that: described method comprises the steps:
1) in 100mL medical glass needle tubing, extracts about 50mL oil sample, adjust the oil sample volume to 40m;
2) adjust 100mL medical glass needle tubing and keep the 10mL space, the methyl alcohol that adds the 5.0mL volume, under the uniform temperature condition through the certain hour oscillation extraction, after treating static layering, the methanol extraction liquid of 100mL medical glass needle tubing middle and upper part is transferred to is used for furfural in the medical glass needle tubing of 5.0mL volume and measures;
Described oscillation extraction reaches balance time 〉=3 minute, extraction temperature≤30 ℃.
2. furfural component oscillation extraction method in the exhausted insulating oil as claimed in claim 1, it is characterized in that: at ambient temperature through 5 minutes oscillation extraction balances, after static 5 minutes, the methanol extraction liquid of 100mL medical glass needle tubing middle and upper part is transferred to by 0.45 μ m needle-based oiliness filter membrane is used for furfural in the medical glass needle tubing of 5.0mL volume and measures.
3. furfural component oscillation extraction method in the exhausted insulating oil as claimed in claim 1, it is characterized in that: described oscillator is 275 times/min of reciprocating vibration frequency ± 5 times/min; Amplitude 35mm ± 3mm; Glass syringe is 100ml, 5 ml medical glass syringes, and impermeability is good, and the core plug does not have bite flexibly; Stainless steel syringe needle: No. 7 metal syringe needles; Syringe rubber sealing cap: good springiness is airtight; Filtering membrane is ф 40,0.45 μ m oiliness filter membranes; 0.45 μ m needle-based oiliness filter membrane; Medicine methyl alcohol: efficient liquid phase chromatographic analysis special agent; Isopropyl alcohol: chromatographically pure; Furfural: analyze pure.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201110020618 CN102175502A (en) | 2011-01-16 | 2011-01-16 | Method for oscillated extraction of furfural components from insulated oil |
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| Application Number | Priority Date | Filing Date | Title |
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| CN 201110020618 CN102175502A (en) | 2011-01-16 | 2011-01-16 | Method for oscillated extraction of furfural components from insulated oil |
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| CN102175502A true CN102175502A (en) | 2011-09-07 |
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| CN 201110020618 Pending CN102175502A (en) | 2011-01-16 | 2011-01-16 | Method for oscillated extraction of furfural components from insulated oil |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103323287A (en) * | 2013-06-04 | 2013-09-25 | 国家电网公司 | Automatic sampling device for sampling furfural in transformer oil and sampling method |
| CN104730184A (en) * | 2013-12-18 | 2015-06-24 | 上海宝钢工业技术服务有限公司 | Method for determining content of furfural and furan derivative in insulating oil |
| CN111537494A (en) * | 2020-05-09 | 2020-08-14 | 广东电网有限责任公司广州供电局 | Analysis method for furfural extraction effect in transformer oil |
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| US4510047A (en) * | 1983-12-14 | 1985-04-09 | Exxon Research And Engineering Co. | Selective extraction solvent recovery using regenerated cellulose membrane under reverse osmosis conditions |
| US5309776A (en) * | 1991-01-14 | 1994-05-10 | Mitsubishi Denki Kabushiki Kaisha | Method of diagnosing deterioration of insulating paper in oil-filled electric apparatus |
| JP3264427B2 (en) * | 1997-02-28 | 2002-03-11 | 財団法人中部電気保安協会 | Deterioration agent and method of deterioration of oil-immersed transformer |
| JP3892734B2 (en) * | 2002-02-08 | 2007-03-14 | 株式会社極東エレテック | Method and apparatus for extracting furfurals in oil |
| CN101887094A (en) * | 2010-06-30 | 2010-11-17 | 河南省电力公司济源供电公司 | Judging method of solid insulating and aging degrees of transformer |
| CN201701784U (en) * | 2010-06-23 | 2011-01-12 | 天津市电力公司 | Dedicated device used for extracting furfuraldehyde from transformer oil |
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2011
- 2011-01-16 CN CN 201110020618 patent/CN102175502A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4510047A (en) * | 1983-12-14 | 1985-04-09 | Exxon Research And Engineering Co. | Selective extraction solvent recovery using regenerated cellulose membrane under reverse osmosis conditions |
| US5309776A (en) * | 1991-01-14 | 1994-05-10 | Mitsubishi Denki Kabushiki Kaisha | Method of diagnosing deterioration of insulating paper in oil-filled electric apparatus |
| JP3264427B2 (en) * | 1997-02-28 | 2002-03-11 | 財団法人中部電気保安協会 | Deterioration agent and method of deterioration of oil-immersed transformer |
| JP3892734B2 (en) * | 2002-02-08 | 2007-03-14 | 株式会社極東エレテック | Method and apparatus for extracting furfurals in oil |
| CN201701784U (en) * | 2010-06-23 | 2011-01-12 | 天津市电力公司 | Dedicated device used for extracting furfuraldehyde from transformer oil |
| CN101887094A (en) * | 2010-06-30 | 2010-11-17 | 河南省电力公司济源供电公司 | Judging method of solid insulating and aging degrees of transformer |
Non-Patent Citations (2)
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| 《热力发电》 20081215 吴三毛等 变压器油中糠醛含量分析方法研究 , 第12期 * |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103323287A (en) * | 2013-06-04 | 2013-09-25 | 国家电网公司 | Automatic sampling device for sampling furfural in transformer oil and sampling method |
| CN104730184A (en) * | 2013-12-18 | 2015-06-24 | 上海宝钢工业技术服务有限公司 | Method for determining content of furfural and furan derivative in insulating oil |
| CN111537494A (en) * | 2020-05-09 | 2020-08-14 | 广东电网有限责任公司广州供电局 | Analysis method for furfural extraction effect in transformer oil |
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Application publication date: 20110907 |