CN102732359B - Preparation method for ferroferric oxide nanoparticle modified transformer oil - Google Patents
Preparation method for ferroferric oxide nanoparticle modified transformer oil Download PDFInfo
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- CN102732359B CN102732359B CN 201210215030 CN201210215030A CN102732359B CN 102732359 B CN102732359 B CN 102732359B CN 201210215030 CN201210215030 CN 201210215030 CN 201210215030 A CN201210215030 A CN 201210215030A CN 102732359 B CN102732359 B CN 102732359B
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- 239000002105 nanoparticle Substances 0.000 title claims abstract description 106
- 238000002360 preparation method Methods 0.000 title claims abstract description 24
- SZVJSHCCFOBDDC-UHFFFAOYSA-N ferrosoferric oxide Chemical compound O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 title abstract 8
- 238000012986 modification Methods 0.000 claims abstract description 53
- 230000004048 modification Effects 0.000 claims abstract description 53
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 36
- 238000006243 chemical reaction Methods 0.000 claims abstract description 33
- 239000008367 deionised water Substances 0.000 claims abstract description 33
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 33
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 20
- 238000001291 vacuum drying Methods 0.000 claims abstract description 17
- 239000012535 impurity Substances 0.000 claims abstract description 12
- BCKXLBQYZLBQEK-KVVVOXFISA-M Sodium oleate Chemical compound [Na+].CCCCCCCC\C=C/CCCCCCCC([O-])=O BCKXLBQYZLBQEK-KVVVOXFISA-M 0.000 claims abstract description 9
- 238000000967 suction filtration Methods 0.000 claims abstract description 9
- 239000011259 mixed solution Substances 0.000 claims description 32
- 239000012299 nitrogen atmosphere Substances 0.000 claims description 32
- NMCUIPGRVMDVDB-UHFFFAOYSA-L iron dichloride Chemical compound Cl[Fe]Cl NMCUIPGRVMDVDB-UHFFFAOYSA-L 0.000 claims description 24
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 claims description 24
- 230000010355 oscillation Effects 0.000 claims description 24
- 239000000243 solution Substances 0.000 claims description 24
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 16
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 16
- 239000007864 aqueous solution Substances 0.000 claims description 16
- 229960000935 dehydrated alcohol Drugs 0.000 claims description 16
- 229910052708 sodium Inorganic materials 0.000 claims description 16
- 239000011734 sodium Substances 0.000 claims description 16
- 238000010792 warming Methods 0.000 claims description 16
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 8
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 8
- 239000007789 gas Substances 0.000 claims description 8
- 239000007788 liquid Substances 0.000 claims description 8
- 239000012528 membrane Substances 0.000 claims description 8
- 229910052757 nitrogen Inorganic materials 0.000 claims description 8
- 239000001301 oxygen Substances 0.000 claims description 8
- 229910052760 oxygen Inorganic materials 0.000 claims description 8
- 239000011148 porous material Substances 0.000 claims description 8
- 229960004756 ethanol Drugs 0.000 claims 1
- 238000000034 method Methods 0.000 abstract description 7
- 239000000126 substance Substances 0.000 abstract description 2
- 238000010438 heat treatment Methods 0.000 abstract 1
- 230000007774 longterm Effects 0.000 abstract 1
- 239000002994 raw material Substances 0.000 abstract 1
- 150000003839 salts Chemical class 0.000 abstract 1
- 238000001132 ultrasonic dispersion Methods 0.000 abstract 1
- 239000006185 dispersion Substances 0.000 description 5
- 239000011554 ferrofluid Substances 0.000 description 4
- 238000009413 insulation Methods 0.000 description 3
- 230000015556 catabolic process Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000000835 fiber Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 238000009825 accumulation Methods 0.000 description 1
- 238000000975 co-precipitation Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000003701 mechanical milling Methods 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000004381 surface treatment Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
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Abstract
The present invention relates to a preparation method for ferroferric oxide nanoparticle modified transformer oil, and belongs to the technical field of energy sources. According to the preparation method, firstly ferroferric oxide nanoparticles are prepared in an alcohol-water solution, and sodium oleate is adopted to carry out surface modification on the ferroferric oxide nanoparticles after heating; deionized water and absolute alcohol are adopted to wash and remove salts and other substances from the reaction system; the obtained ferroferric oxide nanoparticles and a transformer oil are mixed and subjected to ultrasonic dispersion, and impurities and water are removed through processes of suction filtration and vacuum drying to obtain the ferroferric oxide nanoparticle modified transformer oil. The preparation method of the present invention has the following advantages that: the raw materials are easy to obtain and inexpensive, the prepared ferroferric oxide nanoparticle modifiedtransformer oil has good electrical performance and excellent long term stability, and stability and reliability of the ferroferric oxide nanoparticle modified transformer oil during service are ensured.
Description
Technical field
The present invention relates to a kind of preparation method of ferriferrous oxide nano-particle modification transformer oil, belong to energy technology field.
Background technology
Current power industry all adopts transformer oil as insulation, heat-eliminating medium with high-voltage, high-power transformer.Along with the raising of voltage range, capacity, people more and more need a kind of insulation and the more excellent medium of heat dispersion.Research accumulation by forefathers, nowadays people have had very deep understanding to the performance of transformer oil and as much as possible brought into play insulation, the heat sinking function of transformer oil in engineering practices, and the in the last few years rise of nanotechnology, so that people begin to seek nanotechnology possible application in transformer oil.According to existing result of study, after the impurity such as the fiber of micro-meter scale add in the transformer oil, the impurity such as fiber align under the effect of electrical forces, in transformer oil, form the electrode that " foot bridge " and bridge joint are in different potentials, so that the insulating property decrease of transformer oil, therefore traditional idea is thought, should pure as much as possible, not contain tramp material as the transformer oil of dielectric.But nanoparticle has the nano level yardstick, be added in the transformer oil after, can not cause " foot bridge " phenomenon, namely can not reduce original insulating property of transformer oil.And according to research, in the breakdown process of transformer oil, ferriferrous oxide nano-particle has trapped electron, stop the effect of streamer development, thereby improved the insulating property of transformer oil in some situation.On the other hand, the ferriferrous oxide nano-particle yardstick of producing by chemical coprecipitation has superparamagnetism about 10nm, and modification transformer oil prepared therefrom is a kind of ferrofluid.According to Curie law: magnetic reduces when temperature raises, and therefore near the ferrofluid focus is heated and magnetic reduces, and heated ferrofluid is replaced by near cold ferrofluid, thus the conduction of realization heat, and this process is also referred to as the magnetic thermal convection.To sum up, use ferriferrous oxide nano-particle modification transformer oil, can not reduce original insulating property of transformer oil, and in some cases even can improve the electric property of transformer oil, simultaneously because additional magnetic thermal convection process, transformer oil after the modification will have better heat dispersion, and visible ferriferrous oxide nano-particle modification transformer oil technology has bright prospect.But ferriferrous oxide nano-particle is inorganic molecule on the one hand, can not combine with the transformer oil molecule and form stable dispersion system, nanoparticle is easy to reunite on the other hand, and ferriferrous oxide nano-particle has the easier reunion of magnetic, so dispersiveness and the permanent stability of ferriferrous oxide nano-particle in transformer oil are to limit a large important problem of its practical application.
Summary of the invention
The objective of the invention is to propose a kind of preparation method of ferriferrous oxide nano-particle modification transformer oil, at first adopt suitable technique to prepare nanoparticle, take again surface treatment and dispersion technology, to improve the permanent stability of transformer oil.
The preparation method of the ferriferrous oxide nano-particle modification transformer oil that the present invention proposes may further comprise the steps:
(1) preparation ferriferrous oxide nano-particle:
(1-1) the dose volume percentage concentration is the aqueous ethanolic solution of 1:5 in container, passes into nitrogen in aqueous ethanolic solution, to discharge the oxygen in the reaction system;
(1-2) under sonic oscillation and nitrogen atmosphere, in aqueous ethanolic solution, add iron trichloride, make the molecular volume concentration of iron trichloride between 0.01mol/L～0.1mol/L, then add iron protochloride, the iron protochloride that adds and the mol ratio of iron trichloride are 0.5, obtain mixed solution;
(1-3) under sonic oscillation and nitrogen atmosphere, above-mentioned mixed solution is warming up to 50 ℃-60 ℃, drip ammoniacal liquor, the pH value that makes mixed solution is 11, is incubated 30 minutes;
(1-4) under sonic oscillation and nitrogen atmosphere, the mixed solution of step (1-3) is warming up to 80 ℃-85 ℃, the mass body volume concentrations that adds 80 ℃ is the sodium oleate-aqueous solution of 0.04 grams per milliliter, the adding mol ratio of sodium oleate-aqueous solution is: sodium oleate: iron protochloride=0.6:1 is incubated 30 minutes;
(1-5) in nitrogen atmosphere, make above-mentioned reaction system naturally cool to room temperature;
(2) clean ferriferrous oxide nano-particle:
(2-1) magnet is attached to outside the reaction vessel of step (1), makes ferriferrous oxide nano-particle under magneticaction, be adsorbed on container inner wall near the place of magnet, pour out simultaneously liquid wherein;
(2-2) remove magnet, add deionized water in reaction vessel, the deionized water of adding is dissolved in the deionized water ferriferrous oxide nano-particle substantially, repeating step (2-1) three to four times;
(2-3) replace deionized water, repeating step (2-2) three to four times with dehydrated alcohol;
(3) ferriferrous oxide nano-particle that contains a small amount of dehydrated alcohol with step (2-3) adds in the transformer oil, the volume ratio that adds is: ferriferrous oxide nano-particle: transformer oil=1:(1～45), obtain ferriferrous oxide nano-particle modification transformer oil;
(4) use the suction filtration device, the ferriferrous oxide nano-particle modification transformer oil that step (3) is obtained passes through the filter membrane of 0.22 micron pore size, removes impurity;
(5) the ferriferrous oxide nano modification transformer oil of step (4) is put into vacuum drying oven, 10～100 pascal pressures, 60 ℃～90 ℃ lower vacuum-drying 24～48 hours, remove moisture and gas in the ferriferrous oxide nano modification transformer oil, obtain finished product ferriferrous oxide nano-particle modification transformer oil.
The preparation method of the ferriferrous oxide nano-particle modification transformer oil that the present invention proposes, its advantage is:
Preparation method of the present invention, employed material is easy to obtain, and makes low cost product; The used equipment of preparation process is conventional equipment; Prepared ferriferrous oxide nano-particle modification transformer oil has good electric property (the purer transformer oil of alternating current breakdown intensity has improved 10%), and owing to taked suitable nanoparticle technology of preparing, process for treating surface and dispersion technology, have excellent permanent stability, humid test (90 ℃) through a week, and after 1 year leave standstill, ferriferrous oxide nano-particle is good being dispersed in the transformer oil still, finds the precipitation of nanoparticle in the transformer oil bottom.Compare with the prior art that obtains nanoparticle by ball mill and be dispersed in the transformer oil, the resulting ferriferrous oxide nano-particle permanent stability of preparation method of the present invention are good, and nanoparticle yardstick little (10 microns) is even, has avoided simultaneously the introducing of impurity in the mechanical milling process.
Embodiment
The preparation method of the ferriferrous oxide nano-particle modification transformer oil that the present invention proposes may further comprise the steps:
(1) preparation ferriferrous oxide nano-particle:
(1-1) the dose volume percentage concentration is the aqueous ethanolic solution of 1:5 in container, passes into nitrogen in aqueous ethanolic solution, to discharge the oxygen in the reaction system;
(1-2) under sonic oscillation and nitrogen atmosphere, in aqueous ethanolic solution, add iron trichloride, make the molecular volume concentration of iron trichloride between 0.01mol/L～0.1mol/L, then add iron protochloride, the iron protochloride that adds and the mol ratio of iron trichloride are 0.5, obtain mixed solution;
(1-3) under sonic oscillation and nitrogen atmosphere, above-mentioned mixed solution is warming up to 50 ℃-60 ℃, drip ammoniacal liquor, the pH value that makes mixed solution is 11, is incubated 30 minutes;
(1-4) under sonic oscillation and nitrogen atmosphere, the mixed solution of step (1-3) is warming up to 80 ℃-85 ℃, the mass body volume concentrations that adds 80 ℃ is the sodium oleate-aqueous solution of 0.04 grams per milliliter, the adding mol ratio of sodium oleate-aqueous solution is: sodium oleate: iron protochloride=0.6:1 is incubated 30 minutes;
(1-5) in nitrogen atmosphere, make above-mentioned reaction system naturally cool to room temperature;
(2) clean ferriferrous oxide nano-particle:
(2-1) magnet is attached to outside the reaction vessel of step (1), makes ferriferrous oxide nano-particle under magneticaction, be adsorbed on container inner wall near the place of magnet, pour out simultaneously liquid wherein;
(2-2) remove magnet, add deionized water in reaction vessel, the deionized water of adding is dissolved in the deionized water ferriferrous oxide nano-particle substantially, repeating step (2-1) three to four times;
(2-3) replace deionized water, repeating step (2-2) three to four times with dehydrated alcohol;
(3) ferriferrous oxide nano-particle that contains a small amount of dehydrated alcohol with step (2-3) adds in the transformer oil, the volume ratio that adds is: ferriferrous oxide nano-particle: transformer oil=1:(1～45), obtain ferriferrous oxide nano-particle modification transformer oil;
(4) use the suction filtration device, the ferriferrous oxide nano-particle modification transformer oil that step (3) is obtained passes through the filter membrane of 0.22 micron pore size, removes impurity;
(5) the ferriferrous oxide nano modification transformer oil of step (4) is put into vacuum drying oven, 10～100 pascal pressures, 60 ℃～90 ℃ lower vacuum-drying 24～48 hours, remove moisture and gas in the ferriferrous oxide nano modification transformer oil, obtain finished product ferriferrous oxide nano-particle modification transformer oil.
Below introduce the embodiment of the inventive method:
Embodiment 1
(1) preparation ferriferrous oxide nano-particle:
(1-1) the dose volume percentage concentration is the aqueous ethanolic solution of 1:5 in container, passes into nitrogen in aqueous ethanolic solution, to discharge the oxygen in the reaction system;
(1-2) under sonic oscillation and nitrogen atmosphere, in aqueous ethanolic solution, add iron trichloride, make the molecular volume concentration of iron trichloride at 0.05mol/L, then add iron protochloride, the iron protochloride that adds and the mol ratio of iron trichloride are 0.5, obtain mixed solution;
(1-3) under sonic oscillation and nitrogen atmosphere, above-mentioned mixed solution is warming up to 55 ℃, drip ammoniacal liquor, the pH value that makes mixed solution is 11, is incubated 30 minutes;
(1-4) under sonic oscillation and nitrogen atmosphere, the mixed solution of step (1-3) is warming up to 85 ℃, the mass body volume concentrations that adds 80 ℃ is the sodium oleate-aqueous solution of 0.04 grams per milliliter, and the adding mol ratio of sodium oleate-aqueous solution is: sodium oleate: iron protochloride=0.6:1 is incubated 30 minutes;
(1-5) in nitrogen atmosphere, make above-mentioned reaction system naturally cool to room temperature;
(2) clean ferriferrous oxide nano-particle:
(2-1) magnet is attached to outside the reaction vessel of step (1), makes ferriferrous oxide nano-particle under magneticaction, be adsorbed on container inner wall near the place of magnet, pour out simultaneously liquid wherein;
(2-2) remove magnet, add deionized water in reaction vessel, the deionized water of adding is dissolved in the deionized water ferriferrous oxide nano-particle substantially, repeating step (2-1) three to four times;
(2-3) replace deionized water, repeating step (2-2) three to four times with dehydrated alcohol;
(3) ferriferrous oxide nano-particle that contains a small amount of dehydrated alcohol with step (2-3) adds in the transformer oil, and the volume ratio of adding is: ferriferrous oxide nano-particle: transformer oil=1:30 obtains ferriferrous oxide nano-particle modification transformer oil;
(4) use the suction filtration device, the ferriferrous oxide nano-particle modification transformer oil that step (3) is obtained passes through the filter membrane of 0.22 micron pore size, removes impurity;
(5) the ferriferrous oxide nano modification transformer oil of step (4) is put into vacuum drying oven, 100 pascal pressures, 90 ℃ of lower vacuum-drying 48 hours, remove moisture and gas in the ferriferrous oxide nano modification transformer oil, obtain finished product ferriferrous oxide nano-particle modification transformer oil.
Embodiment 2
(1) preparation ferriferrous oxide nano-particle:
(1-1) the dose volume percentage concentration is the aqueous ethanolic solution of 1:5 in container, passes into nitrogen in aqueous ethanolic solution, to discharge the oxygen in the reaction system;
(1-2) under sonic oscillation and nitrogen atmosphere, in aqueous ethanolic solution, add iron trichloride, make the molecular volume concentration of iron trichloride at 0.05mol/L, then add iron protochloride, the iron protochloride that adds and the mol ratio of iron trichloride are 0.5, obtain mixed solution;
(1-3) under sonic oscillation and nitrogen atmosphere, above-mentioned mixed solution is warming up to 55 ℃, drip ammoniacal liquor, the pH value that makes mixed solution is 11, is incubated 30 minutes;
(1-4) under sonic oscillation and nitrogen atmosphere, the mixed solution of step (1-3) is warming up to 85 ℃, the mass body volume concentrations that adds 80 ℃ is the sodium oleate-aqueous solution of 0.04 grams per milliliter, and the adding mol ratio of sodium oleate-aqueous solution is: sodium oleate: iron protochloride=0.6:1 is incubated 30 minutes;
(1-5) in nitrogen atmosphere, make above-mentioned reaction system naturally cool to room temperature;
(2) clean ferriferrous oxide nano-particle:
(2-1) magnet is attached to outside the reaction vessel of step (1), makes ferriferrous oxide nano-particle under magneticaction, be adsorbed on container inner wall near the place of magnet, pour out simultaneously liquid wherein;
(2-2) remove magnet, add deionized water in reaction vessel, the deionized water of adding is dissolved in the deionized water ferriferrous oxide nano-particle substantially, repeating step (2-1) three to four times;
(2-3) replace deionized water, repeating step (2-2) three to four times with dehydrated alcohol;
(3) ferriferrous oxide nano-particle that contains a small amount of dehydrated alcohol with step (2-3) adds in the transformer oil, and the volume ratio of adding is: ferriferrous oxide nano-particle: transformer oil=1:15 obtains ferriferrous oxide nano-particle modification transformer oil;
(4) use the suction filtration device, the ferriferrous oxide nano-particle modification transformer oil that step (3) is obtained passes through the filter membrane of 0.22 micron pore size, removes impurity;
(5) the ferriferrous oxide nano modification transformer oil of step (4) is put into vacuum drying oven, 100 pascal pressures, 90 ℃ of lower vacuum-drying 48 hours, remove moisture and gas in the ferriferrous oxide nano modification transformer oil, obtain finished product ferriferrous oxide nano-particle modification transformer oil.
Embodiment 3
(1) preparation ferriferrous oxide nano-particle:
(1-1) the dose volume percentage concentration is the aqueous ethanolic solution of 1:5 in container, passes into nitrogen in aqueous ethanolic solution, to discharge the oxygen in the reaction system;
(1-2) under sonic oscillation and nitrogen atmosphere, in aqueous ethanolic solution, add iron trichloride, make the molecular volume concentration of iron trichloride at 0.05mol/L, then add iron protochloride, the iron protochloride that adds and the mol ratio of iron trichloride are 0.5, obtain mixed solution;
(1-3) under sonic oscillation and nitrogen atmosphere, above-mentioned mixed solution is warming up to 55 ℃, drip ammoniacal liquor, the pH value that makes mixed solution is 11, is incubated 30 minutes;
(1-4) under sonic oscillation and nitrogen atmosphere, the mixed solution of step (1-3) is warming up to 85 ℃, the mass body volume concentrations that adds 80 ℃ is the sodium oleate-aqueous solution of 0.04 grams per milliliter, and the adding mol ratio of sodium oleate-aqueous solution is: sodium oleate: iron protochloride=0.6:1 is incubated 30 minutes;
(1-5) in nitrogen atmosphere, make above-mentioned reaction system naturally cool to room temperature;
(2) clean ferriferrous oxide nano-particle:
(2-1) magnet is attached to outside the reaction vessel of step (1), makes ferriferrous oxide nano-particle under magneticaction, be adsorbed on container inner wall near the place of magnet, pour out simultaneously liquid wherein;
(2-2) remove magnet, add deionized water in reaction vessel, the deionized water of adding is dissolved in the deionized water ferriferrous oxide nano-particle substantially, repeating step (2-1) three to four times;
(2-3) replace deionized water, repeating step (2-2) three to four times with dehydrated alcohol;
(3) ferriferrous oxide nano-particle that contains a small amount of dehydrated alcohol with step (2-3) adds in the transformer oil, and the volume ratio of adding is: ferriferrous oxide nano-particle: transformer oil=1:10 obtains ferriferrous oxide nano-particle modification transformer oil;
(4) use the suction filtration device, the ferriferrous oxide nano-particle modification transformer oil that step (3) is obtained passes through the filter membrane of 0.22 micron pore size, removes impurity;
(5) the ferriferrous oxide nano modification transformer oil of step (4) is put into vacuum drying oven, 100 pascal pressures, 90 ℃ of lower vacuum-drying 48 hours, remove moisture and gas in the ferriferrous oxide nano modification transformer oil, obtain finished product ferriferrous oxide nano-particle modification transformer oil.
Embodiment 4
(1) preparation ferriferrous oxide nano-particle:
(1-1) the dose volume percentage concentration is the aqueous ethanolic solution of 1:5 in container, passes into nitrogen in aqueous ethanolic solution, to discharge the oxygen in the reaction system;
(1-2) under sonic oscillation and nitrogen atmosphere, in aqueous ethanolic solution, add iron trichloride, make the molecular volume concentration of iron trichloride at 0.03mol/L, then add iron protochloride, the iron protochloride that adds and the mol ratio of iron trichloride are 0.5, obtain mixed solution;
(1-3) under sonic oscillation and nitrogen atmosphere, above-mentioned mixed solution is warming up to 55 ℃, drip ammoniacal liquor, the pH value that makes mixed solution is 11, is incubated 30 minutes;
(1-4) under sonic oscillation and nitrogen atmosphere, the mixed solution of step (1-3) is warming up to 85 ℃, the mass body volume concentrations that adds 80 ℃ is the sodium oleate-aqueous solution of 0.04 grams per milliliter, and the adding mol ratio of sodium oleate-aqueous solution is: sodium oleate: iron protochloride=0.6:1 is incubated 30 minutes;
(1-5) in nitrogen atmosphere, make above-mentioned reaction system naturally cool to room temperature;
(2) clean ferriferrous oxide nano-particle:
(2-1) magnet is attached to outside the reaction vessel of step (1), makes ferriferrous oxide nano-particle under magneticaction, be adsorbed on container inner wall near the place of magnet, pour out simultaneously liquid wherein;
(2-2) remove magnet, add deionized water in reaction vessel, the deionized water of adding is dissolved in the deionized water ferriferrous oxide nano-particle substantially, repeating step (2-1) three to four times;
(2-3) replace deionized water, repeating step (2-2) three to four times with dehydrated alcohol;
(3) ferriferrous oxide nano-particle that contains a small amount of dehydrated alcohol with step (2-3) adds in the transformer oil, and the volume ratio of adding is: ferriferrous oxide nano-particle: transformer oil=1:10 obtains ferriferrous oxide nano-particle modification transformer oil;
(4) use the suction filtration device, the ferriferrous oxide nano-particle modification transformer oil that step (3) is obtained passes through the filter membrane of 0.22 micron pore size, removes impurity;
(5) the ferriferrous oxide nano modification transformer oil of step (4) is put into vacuum drying oven, 100 pascal pressures, 90 ℃ of lower vacuum-drying 48 hours, remove moisture and gas in the ferriferrous oxide nano modification transformer oil, obtain finished product ferriferrous oxide nano-particle modification transformer oil.
Embodiment 5
(1) preparation ferriferrous oxide nano-particle:
(1-1) the dose volume percentage concentration is the aqueous ethanolic solution of 1:5 in container, passes into nitrogen in aqueous ethanolic solution, to discharge the oxygen in the reaction system;
(1-2) under sonic oscillation and nitrogen atmosphere, in aqueous ethanolic solution, add iron trichloride, make the molecular volume concentration of iron trichloride at 0.07mol/L, then add iron protochloride, the iron protochloride that adds and the mol ratio of iron trichloride are 0.5, obtain mixed solution;
(1-3) under sonic oscillation and nitrogen atmosphere, above-mentioned mixed solution is warming up to 55 ℃, drip ammoniacal liquor, the pH value that makes mixed solution is 11, is incubated 30 minutes;
(1-4) under sonic oscillation and nitrogen atmosphere, the mixed solution of step (1-3) is warming up to 85 ℃, the mass body volume concentrations that adds 80 ℃ is the sodium oleate-aqueous solution of 0.04 grams per milliliter, and the adding mol ratio of sodium oleate-aqueous solution is: sodium oleate: iron protochloride=0.6:1 is incubated 30 minutes;
(1-5) in nitrogen atmosphere, make above-mentioned reaction system naturally cool to room temperature;
(2) clean ferriferrous oxide nano-particle:
(2-1) magnet is attached to outside the reaction vessel of step (1), makes ferriferrous oxide nano-particle under magneticaction, be adsorbed on container inner wall near the place of magnet, pour out simultaneously liquid wherein;
(2-2) remove magnet, add deionized water in reaction vessel, the deionized water of adding is dissolved in the deionized water ferriferrous oxide nano-particle substantially, repeating step (2-1) three to four times;
(2-3) replace deionized water, repeating step (2-2) three to four times with dehydrated alcohol;
(3) ferriferrous oxide nano-particle that contains a small amount of dehydrated alcohol with step (2-3) adds in the transformer oil, and the volume ratio of adding is: ferriferrous oxide nano-particle: transformer oil=1:10 obtains ferriferrous oxide nano-particle modification transformer oil;
(4) use the suction filtration device, the ferriferrous oxide nano-particle modification transformer oil that step (3) is obtained passes through the filter membrane of 0.22 micron pore size, removes impurity;
(5) the ferriferrous oxide nano modification transformer oil of step (4) is put into vacuum drying oven, 100 pascal pressures, 90 ℃ of lower vacuum-drying 48 hours, remove moisture and gas in the ferriferrous oxide nano modification transformer oil, obtain finished product ferriferrous oxide nano-particle modification transformer oil.
Claims (1)
1. the preparation method of a ferriferrous oxide nano-particle modification transformer oil is characterized in that this preparation method may further comprise the steps:
(1) preparation ferriferrous oxide nano-particle:
(1-1) volume ratio of preparation ethanol and water is 1: 5 aqueous ethanolic solution in container, passes into nitrogen in aqueous ethanolic solution, with the oxygen in the discharge reaction system;
(1-2) under sonic oscillation and nitrogen atmosphere, in aqueous ethanolic solution, add iron trichloride, make the molecular volume concentration of iron trichloride between 0.01mol/L～0.1mol/L, then add iron protochloride, the iron protochloride that adds and the mol ratio of iron trichloride are 0.5, obtain mixed solution;
(1-3) under sonic oscillation and nitrogen atmosphere, above-mentioned mixed solution is warming up to 50 ℃-60 ℃, drip ammoniacal liquor, the pH value that makes mixed solution is 11, is incubated 30 minutes;
(1-4) under sonic oscillation and nitrogen atmosphere, the mixed solution of step (1-3) is warming up to 80 ℃-85 ℃, the mass body volume concentrations that adds 80 ℃ is the sodium oleate-aqueous solution of 0.04 grams per milliliter, the adding mol ratio of sodium oleate-aqueous solution is: sodium oleate: iron protochloride=0.6: 1 is incubated 30 minutes;
(1-5) in nitrogen atmosphere, make above-mentioned reaction system naturally cool to room temperature;
(2) clean ferriferrous oxide nano-particle:
(2-1) magnet is attached to outside the reaction vessel of step (1), makes ferriferrous oxide nano-particle under magneticaction, be adsorbed on container inner wall near the place of magnet, pour out simultaneously liquid wherein;
(2-2) remove magnet, add deionized water in reaction vessel, the deionized water of adding is dissolved in the deionized water ferriferrous oxide nano-particle substantially, repeating step (2-1) three to four times;
(2-3) replace deionized water, repeating step (2-2) three to four times with dehydrated alcohol;
(3) ferriferrous oxide nano-particle that contains a small amount of dehydrated alcohol with step (2-3) adds in the transformer oil, the volume ratio that adds is: ferriferrous oxide nano-particle: transformer oil=1:(1～45), obtain ferriferrous oxide nano-particle modification transformer oil;
(4) use the suction filtration device, the ferriferrous oxide nano-particle modification transformer oil that step (3) is obtained passes through the filter membrane of 0.22 micron pore size, removes impurity;
(5) the ferriferrous oxide nano-particle modification transformer oil of step (4) is put into vacuum drying oven, 10～100 pascal pressures, 60 ℃～90 ℃ lower vacuum-drying 24～48 hours, remove moisture and gas in the ferriferrous oxide nano-particle modification transformer oil, obtain finished product ferriferrous oxide nano-particle modification transformer oil.
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| CN105974097B (en) * | 2016-05-04 | 2017-10-20 | 西安交通大学 | A kind of nano modification transformer oil method for analyzing stability |
| CN106635253B (en) * | 2016-08-26 | 2019-10-18 | 重庆大学 | A kind of monodisperse ferriferrous oxide nano-particle improved plant insulating oil preparation method |
| CN110669565A (en) * | 2019-09-10 | 2020-01-10 | 浙江中博润滑油有限公司 | Preparation method of nano modified transformer oil with high breakdown voltage |
| CN112951526B (en) * | 2021-03-23 | 2022-07-12 | 国网吉林省电力有限公司电力科学研究院 | Preparation method of nanoparticle modified insulating oil based on iron occurrence form |
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