CN104992749A - Modified fullerene nanoparticle and vegetable insulating oil-containing complex - Google Patents

Modified fullerene nanoparticle and vegetable insulating oil-containing complex Download PDF

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CN104992749A
CN104992749A CN201510389998.3A CN201510389998A CN104992749A CN 104992749 A CN104992749 A CN 104992749A CN 201510389998 A CN201510389998 A CN 201510389998A CN 104992749 A CN104992749 A CN 104992749A
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insulating oil
nano particle
modified fullerenes
vegetable insulating
fullerenes nano
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李剑
王飞鹏
杨丽君
陈伟根
廖瑞金
杜林�
王有元
周泉
赵学童
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Chongqing University
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Chongqing University
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Abstract

The invention relates to a modified fullerene nanoparticle and vegetable insulating oil-containing complex. The components of the modified fullerene nanoparticle and vegetable insulating oil-containing complex include vegetable insulating oil and modified fullerene nanoparticles; and the concentration of the modified fullerene nanoparticles in the vegetable insulating oil ranges from 50mg/L to 150mg/L. The complex is formed by the modified fullerene nanoparticles and the vegetable insulating oil; the modified fullerene nanoparticle and vegetable insulating oil-containing complex has secular stability, and no sediments will be generated in the complex; the dielectric property and electrical breakdown property of the modified fullerene nanoparticle and vegetable insulating oil-containing complex can be improved; and the modified fullerene nanoparticles have a free radical adsorption property, and therefore, the anti-acidification ability of the modified fullerene nanoparticle and vegetable insulating oil-containing complex can be improved.

Description

Containing the compound of modified fullerenes nano particle and vegetable insulating oil
Technical field
The present invention relates to insulating oil technical field, be specifically related to a kind of fullerene nanoparticle that uses as the formula of modifier modification vegetable insulating oil and preparation method.
Background technology
Insulating oil is important liquid insulating medium, uses in a large number in the electric equipments such as transformer.Vegetable insulating oil is the environmental type liquid insulating medium of a kind of renewable, high natural degradation rate, high burning-point.But there is a large amount of monounsaturated fatty acids and polyunsaturated fatty acid in vegetable insulating oil, oxidation stability is poor compared with mineral insulating oil.This makes vegetable insulating oil easily be subject to external condition in storage and use procedure, as the factors such as illumination, temperature, moisture, oxygen and metal impurities impact thus that acidifying occurs is rotten.The deterioration of vegetable insulating oil will produce the comparatively more acidic materials of mineral insulating oil, and this has a negative impact to the support and insulating material that impregnated in vegetable insulating oil in Transformer structure.Vegetable insulating oil dielectric dissipation factor is higher simultaneously, specific insulation is lower, and dielectric property are relatively weak compared with mineral insulating oil.
Chinese invention patent (grant number is CN 101901637 B) discloses the compound of a kind of vegetable insulating oil and modified nano powder and application thereof and preparation method, described compound comprises vegetable insulating oil and nano-powder, described compound is for the preparation of insulating oil, and described preparation method comprises the steps: to carry out surface treatment to nano-powder; By through dewatering, the vegetable insulating oil of degasification and the mixing of surface treated nano-powder; The insulating oil of mixing is carried out sonic oscillation; Mixture after oscillation treatment is added in planetary ball mill, adopts wet grinding to process.This invention adds nano-powder in vegetable insulating oil, as tri-iron tetroxide, aluminium nitride, alundum (Al2O3), di-iron trioxide, zinc oxide, magnesium oxide etc., liquid nano dielectric can be formed, it not only can improve the dielectric property of insulating oil, and can strengthen the thermolysis of Transformer Winding coil; And nano particle is more much smaller than the foreign particle in insulating oil, stable sol system can be formed with liquid medium, under the effect of external electric field, can not be formed and puncture foot bridge, thus improve insulating oil dielectric strength.But the compound of this vegetable insulating oil and modified nano powder is compared with mineral insulating oil, and its dielectric property are still relatively weak.
Therefore, improve thermal stability and the specific insulation of vegetable insulating oil further, reduce its dielectric dissipation factor and there is important Research Significance.
Summary of the invention
The technical problem to be solved in the present invention is, provide a kind of improve vegetable insulating oil dielectric property and the anti-acid ability improving vegetable insulating oil containing the compound of modified fullerenes nano particle and vegetable insulating oil.
In order to solve the problems of the technologies described above, the technical solution used in the present invention is, the component that should contain the compound of modified fullerenes nano particle and vegetable insulating oil comprises vegetable insulating oil and modified fullerenes nano particle; The concentration of described modified fullerenes nano particle in described vegetable insulating oil is 50mg/L ~ 150mg/L.
Adopt technique scheme, compound is formed by modified fullerenes nano particle and vegetable insulating oil, should generate without precipitation containing the compound long-term stability of modified fullerenes nano particle and vegetable insulating oil, and the dielectric property containing the compound of modified fullerenes nano particle and vegetable insulating oil obtained, electrically breakdown performance can obtain raising.Simultaneously due to the free radical absorption property that fullerene nanoparticle has, the anti-acid ability containing the compound of modified fullerenes nano particle and vegetable insulating oil can obtain raising.The compound containing modified fullerenes nano particle and vegetable insulating oil that the present invention is prepared by modified fullerenes nano particle has good physics and chemistry and dielectric property.
Further improvement of the present invention is, the component that should contain the compound of modified fullerenes nano particle and vegetable insulating oil also comprises additive composition.Use additive to improve reaction rate, shorten preparation time, thus reduce costs.
As preferred version of the present invention, the diameter of fullerene nanoparticle is 5nm ~ 100nm.
As preferred version of the present invention, described fullerene nanoparticle is C60.C60 is a kind of typical fullerene-based material, there is good conductivity and magnetic, can with a lot of material generation chemical reaction, the present invention utilizes its improved plant insulating oil, and the dielectric property, electrically breakdown performance and the Antacid effectiveness that make improved plant insulating oil namely contain the compound of modified fullerenes nano particle and vegetable insulating oil can obtain raising.
As preferred version of the present invention, described additive is antioxidant or matal deactivator.Use additive to improve reaction rate, shorten preparation time, thus reduce costs.
Compound containing modified fullerenes nano particle and vegetable insulating oil of the present invention is applied preparing in insulating oil.
The technical problem that the present invention also will solve is, provide a kind of improve vegetable insulating oil dielectric property and the anti-acid ability improving vegetable insulating oil containing the preparation method of the modified fullerenes nano particle of the middle use of the compound of modified fullerenes nano particle and vegetable insulating oil.
In order to solve the problems of the technologies described above, the technical solution used in the present invention is, this prepares the method for modified fullerenes nano particle, and concrete steps are as follows:
(A) fullerene nanoparticle is mixed with absolute ethyl alcohol;
(B) add oleic acid surfactant, the quality of oleic acid surfactant is 10% ~ 50% of the quality of fullerene nanoparticle, obtained mixed liquor;
(C) mixed liquor of step (B) gained is carried out ultrasonic disperse and mechanical agitation at 40 DEG C ~ 70 DEG C, obtained modified fullerenes nano particle;
(D) modified fullerenes nano particle obtained in washes of absolute alcohol step (C) is adopted, then dry in vacuum drying chamber;
(E) dried modified fullerenes nano particle is ground to form powdery, stand-by.
Further improvement of the present invention is, the technical process of this method of modifying needs to carry out in light protected environment.
Further improvement of the present invention is, in described step (C), hyperacoustic frequency is 35 ~ 45kHz, and power density is 15 ~ 20W/cm 2, the temperature of sonic oscillation is 40 ~ 70 DEG C, and mechanical agitation speed is 200 ~ 400rpm, and ultrasonic disperse and mechanical agitation time are 60 ~ 240min.
Further improvement of the present invention is, in described step (A), the concentration of described fullerene nanoparticle in described absolute ethyl alcohol is 0.03 ~ 0.06g/mL.
Another problem that the present invention also will solve is, provides a kind of preparation method containing the compound of modified fullerenes nano particle and vegetable insulating oil.
In order to solve the problems of the technologies described above, the technical solution used in the present invention is, should contain the preparation method of the compound of modified fullerenes nano particle and vegetable insulating oil, concrete steps comprise:
A () prepares raw material: fullerene nanoparticle forms modified fullerenes nano particle after carrying out surface modification, stand-by; Original vegetable insulating oil is carried out drying, dehydration, degassed process, baking temperature is 80 ~ 100 DEG C, and vacuum degree is-0.05 ~-0.13MPa, and drying time is 40 ~ 50h, stand-by;
B () adds modified fullerenes nano particle: add described modified fullerenes nano particle in the raw material obtained in step (a), forms the mixture containing modified fullerenes nano particle and vegetable insulating oil;
C () prepares compound: under the environment of lucifuge, by the mixture sonic oscillation process of gained in step (b), and the preliminary obtained compound containing modified fullerenes nano particle and vegetable insulating oil;
D () is dewatered degassed process: by fullerene nanoparticle improved plant insulating oil in step (c) through the degassed process of dehydration, baking temperature is 80 ~ 100 DEG C, vacuum degree is-0.05 ~-0.13MPa, drying time is 20 ~ 30h, obtains the compound containing modified fullerenes nano particle and vegetable insulating oil;
E () sealing is preserved: fullerene nanoparticle improved plant insulating oil step (d) obtained is cooled to room temperature, and lucifuge sealing and standing is preserved.
Further improvement of the present invention is, in described step (c), the process conditions of sonic oscillation process are: hyperacoustic frequency is 30 ~ 50kHz, and power density is 15 ~ 20W/cm 2, the temperature of sonic oscillation is 40 ~ 70 DEG C, and duration of oscillation is 30 ~ 60min.
Adopt technical scheme of the present invention, its beneficial effect produced is: the compound containing modified fullerenes nano particle and vegetable insulating oil of the present invention, can be used for preparing corresponding improved plant insulating oil, the vegetable insulating oil of the modification prepared by modified fullerenes nano particle obtained, is steady in a long-termly generated without precipitation.Use modified fullerenes nano particle to carry out modification to vegetable insulating oil, the dielectric property of the improved plant insulating oil of acquisition, electrically breakdown performance can obtain raising.Simultaneously due to the free radical absorption property that fullerene nanoparticle has, the anti-acid ability of improved plant insulating oil can obtain raising.The compound containing modified fullerenes nano particle and vegetable insulating oil that the present invention is prepared by modified fullerenes nano particle has good physics and chemistry and dielectric property, and acid number is lower than 0.01mg KOH/g, and specific insulation when 90 DEG C is higher than 12 × 10 10Ω m, dielectric constant is about 3.0; This compound is compared and is adopted the electric conductivity of compound as nano powder modified in tri-iron tetroxide, aluminium nitride, alundum (Al2O3), di-iron trioxide, zinc oxide, magnesium oxide etc. to have further raising.
Embodiment
Embodiment 1
Component containing the compound of modified fullerenes nano particle and vegetable insulating oil is: modified fullerenes nano particle and vegetable insulating oil, and the concentration of modified fullerenes nano particle in vegetable insulating oil is 50mg/L;
Concrete preparation process containing the compound of modified fullerenes nano particle and vegetable insulating oil is as follows:
(1) carry out surface modification to fullerene nanoparticle, the diameter of selected fullerene nanoparticle is the C60 of 5nm, and concrete steps comprise:
(A) under light protected environment, mixed by fullerene nanoparticle with absolute ethyl alcohol, ratio is add 10g fullerene nanoparticle in 200mL absolute ethyl alcohol;
(B) add oleic acid surfactant, the quality of oleic acid surfactant is 10% of fullerene nanoparticle quality, obtains mixed liquor;
(C) under light protected environment, carry out mechanical agitation by carrying out ultrasonic disperse in the water-bath of the mixed liquor of step (B) gained at 60 DEG C, hyperacoustic frequency is 40kHz, and power density is 15W/cm simultaneously 2, the temperature of sonic oscillation is 40 DEG C, and mechanical agitation speed is 200rpm, and ultrasonic disperse and mechanical agitation time are 120min, obtains modified fullerenes nano particle;
(D) with the absolute ethyl alcohol modified fullerenes nano particle that obtains of cleaning step (C) repeatedly, then dry in vacuum oven;
(E) dried modified fullerenes nano particle grinds to form powdery, stand-by.
(2) prepare the compound of modified fullerenes nano particle and vegetable insulating oil, concrete steps comprise:
A () prepares raw material: modified fullerenes nano particle obtained in step (E), stand-by; Primordial plant insulating oil is carried out drying, dehydration, degassed process in vacuum oil-filter, and baking temperature is 100 DEG C, and vacuum degree is-0.13MPa, and drying time is 40 hours, stand-by;
B () adds modified fullerenes nano particle: mixed with modified fullerenes nanoparticle powder by the vegetable insulating oil after process in step (a); The concentration of modified fullerenes nano particle in vegetable insulating oil is 50mg/L;
C () prepares compound: under the environment of lucifuge, and the mixture in step (b) is carried out sonic oscillation process; Hyperacoustic frequency is 40kHz, and power density is 15W/cm 2, the temperature of sonic oscillation is 40 DEG C, and duration of oscillation is 30min, the compound of obtained modified fullerenes nano particle and vegetable insulating oil;
D () is dewatered degassed process: by fullerene nanoparticle improved plant insulating oil in step (c) through the degassed process of dehydration, baking temperature is 100 DEG C, vacuum degree is-0.13MPa, drying time is 20h, obtains the compound containing modified fullerenes nano particle and vegetable insulating oil;
E () sealing is preserved: fullerene nanoparticle improved plant insulating oil step (d) obtained is cooled to room temperature, and lucifuge sealing and standing is preserved, and obtains the compound containing modified fullerenes nano particle and vegetable insulating oil.
Embodiment 2
Component containing the compound of modified fullerenes nano particle and vegetable insulating oil is: modified fullerenes nano particle and vegetable insulating oil, and the concentration of modified fullerenes nano particle in vegetable insulating oil is 100mg/L;
Concrete preparation process containing the compound of modified fullerenes nano particle and vegetable insulating oil is as follows:
(1) carry out surface modification to fullerene nanoparticle, the diameter of selected fullerene nanoparticle is the C60 of 50nm, and concrete steps comprise:
(A) under light protected environment, mixed by fullerene nanoparticle with absolute ethyl alcohol, ratio is add 10g fullerene nanoparticle in 200mL absolute ethyl alcohol;
(B) add oleic acid surfactant, the quality of oleic acid surfactant is 30% of fullerene nanoparticle quality, obtains mixed liquor;
(C) under light protected environment, carry out mechanical agitation by carrying out ultrasonic disperse in the water-bath of the mixed liquor of step (B) gained at 65 DEG C, hyperacoustic frequency is 40kHz, and power density is 18W/cm simultaneously 2, the temperature of sonic oscillation is 65 DEG C, and mechanical agitation speed is 300rpm, and ultrasonic disperse and mechanical agitation time are 240min, obtains modified fullerenes nano particle;
(D) with the absolute ethyl alcohol modified fullerenes nano particle that obtains of cleaning step (C) repeatedly, then dry in vacuum oven;
(E) dried modified fullerenes nano particle grinds to form powdery, stand-by.
(2) prepare the compound of modified fullerenes nano particle and vegetable insulating oil, concrete steps comprise:
A () prepares raw material: modified fullerenes nano particle obtained in step (E), stand-by; Primordial plant insulating oil is carried out drying, dehydration, degassed process in vacuum oil-filter, and baking temperature is 90 DEG C, and vacuum degree is-0.1MPa, and drying time is 48 hours, stand-by;
B () adds modified fullerenes nano particle: mixed with modified fullerenes nanoparticle powder by the vegetable insulating oil after process in step (a); The concentration of modified fullerenes nano particle in vegetable insulating oil is 100mg/L;
C () prepares compound: under light protected environment, and the mixture in step (b) is carried out sonic oscillation process; Hyperacoustic frequency is 40kHz, and power density is 18W/cm 2, the temperature of sonic oscillation is 65 DEG C, and duration of oscillation is 60min, the compound of obtained modified fullerenes nano particle and vegetable insulating oil;
D () is dewatered degassed process: by fullerene nanoparticle improved plant insulating oil in step (c) through the degassed process of dehydration, baking temperature is 90 DEG C, vacuum degree is-0.1MPa, and drying time is 24h, obtains the compound containing modified fullerenes nano particle and vegetable insulating oil;
E () sealing is preserved: fullerene nanoparticle improved plant insulating oil step (d) obtained is cooled to room temperature, and lucifuge sealing and standing is preserved, and obtains the compound containing modified fullerenes nano particle and vegetable insulating oil.
Embodiment 3
Component containing the compound of modified fullerenes nano particle and vegetable insulating oil is: modified fullerenes nano particle and vegetable insulating oil, and the concentration of modified fullerenes nano particle in vegetable insulating oil is 150mg/L;
Concrete preparation process containing the compound of modified fullerenes nano particle and vegetable insulating oil is as follows:
(1) carry out surface modification to fullerene nanoparticle, the diameter of selected fullerene nanoparticle is the C60 of 100nm, and concrete steps comprise:
(A) under light protected environment, mixed by fullerene nanoparticle with absolute ethyl alcohol, ratio is add 10g fullerene nanoparticle in 200mL absolute ethyl alcohol;
(B) add oleic acid surfactant, the quality of oleic acid surfactant is 50% of fullerene nanoparticle quality, obtains mixed liquor;
(C) under light protected environment, carry out mechanical agitation by carrying out ultrasonic disperse in the water-bath of the mixed liquor of step (B) gained at 70 DEG C, hyperacoustic frequency is 40kHz, and power density is 20W/cm simultaneously 2, the temperature of sonic oscillation is 70 DEG C, and mechanical agitation speed is 400rpm, and ultrasonic disperse and mechanical agitation time are 240min, obtains modified fullerenes nano particle;
(D) with the absolute ethyl alcohol modified fullerenes nano particle that obtains of cleaning step (C) repeatedly, then dry in vacuum oven;
(E) dried modified fullerenes nano particle grinds to form powdery, stand-by.
(2) prepare the compound of modified fullerenes nano particle and vegetable insulating oil, concrete steps comprise:
A () prepares raw material: modified fullerenes nano particle obtained in step (E), stand-by; Primordial plant insulating oil is carried out drying, dehydration, degassed process in vacuum oil-filter, and baking temperature is 80 DEG C, and vacuum degree is-0.05MPa, and drying time is 50 hours, stand-by;
B () adds modified fullerenes nano particle: mixed with modified fullerenes nanoparticle powder by the vegetable insulating oil after process in step (a); The concentration of modified fullerenes nano particle in vegetable insulating oil is 150mg/L;
C () prepares compound: under light protected environment, and the mixture in step (b) is carried out sonic oscillation process; Hyperacoustic frequency is 40kHz, and power density is 20W/cm 2, the temperature of sonic oscillation is 70 DEG C, and duration of oscillation is 60min, the compound of obtained modified fullerenes nano particle and vegetable insulating oil;
D () is dewatered degassed process: by fullerene nanoparticle improved plant insulating oil in step (c) through the degassed process of dehydration, baking temperature is 80 DEG C, vacuum degree is-0.05MPa, drying time is 30h, obtains the compound containing modified fullerenes nano particle and vegetable insulating oil;
E () sealing is preserved: fullerene nanoparticle improved plant insulating oil step (d) obtained is cooled to room temperature, and lucifuge sealing and standing is preserved, and obtains the compound containing modified fullerenes nano particle and vegetable insulating oil.
Contrasted by the compound containing modified fullerenes nano particle and vegetable insulating oil obtained in embodiment 1, embodiment 2 and embodiment 3, its performance comparison data are as table 1; Based on blank sample in table 1, oil, is the vegetable insulating oil not adding any nanometer additive.
Table 1 embodiment 1 and the contrast of embodiment 2 the performance test results
In sum, the compound containing modified fullerenes nano particle and vegetable insulating oil prepared by modified fullerenes nano particle has good physics and chemistry and dielectric property, compound containing modified fullerenes nano particle and vegetable insulating oil effectively can improve the specific insulation of vegetable insulating oil, reduce the dielectric loss of vegetable insulating oil, the performance improving insulating material for nanometer technology provides new approaches and new way.
Finally, it is also to be noted that what enumerate above is only several specific embodiments of the present invention.Obviously, the invention is not restricted to above embodiment, many distortion can also be had.All distortion that those of ordinary skill in the art can directly derive from content disclosed by the invention or associate, all should think protection scope of the present invention.

Claims (10)

1. contain a compound for modified fullerenes nano particle and vegetable insulating oil, it is characterized in that, the component that should contain the compound of modified fullerenes nano particle and vegetable insulating oil comprises vegetable insulating oil and modified fullerenes nano particle; The concentration of described modified fullerenes nano particle in described vegetable insulating oil is 50mg/L ~ 150mg/L.
2. the compound containing modified fullerenes nano particle and vegetable insulating oil according to claim 1, is characterized in that, the component that should contain the compound of modified fullerenes nano particle and vegetable insulating oil also comprises additive.
3. the compound containing modified fullerenes nano particle and vegetable insulating oil according to claim 1 and 2, it is characterized in that, the diameter of fullerene nanoparticle is 5nm ~ 100nm.
4. the compound containing modified fullerenes nano particle and vegetable insulating oil according to claim 3, it is characterized in that, described fullerene nanoparticle is C60.
5. the compound containing modified fullerenes nano particle and vegetable insulating oil according to claim 2, it is characterized in that, described additive is antioxidant or matal deactivator.
6. the compound containing modified fullerenes nano particle and vegetable insulating oil according to claim 4, is characterized in that, should apply preparing in insulating oil containing the compound of modified fullerenes nano particle and vegetable insulating oil.
7. prepare a method for modified fullerenes nano particle, comprise the following steps:
(A) fullerene nanoparticle is mixed with absolute ethyl alcohol;
(B) add oleic acid surfactant, the quality of oleic acid surfactant is 10% ~ 50% of the quality of fullerene nanoparticle, obtained mixed liquor;
(C) mixed liquor of step (B) gained is carried out ultrasonic disperse and mechanical agitation at 40 DEG C ~ 70 DEG C, obtained modified fullerenes nano particle;
(D) modified fullerenes nano particle obtained in washes of absolute alcohol step (C) is adopted, then dry in vacuum drying chamber;
(E) dried modified fullerenes nano particle is ground to form powdery, stand-by.
8. the method preparing modified fullerenes nano particle according to claim 7, is characterized in that, the technical process of this method of modifying needs to carry out in light protected environment.
9. the method preparing modified fullerenes nano particle according to claim 8, it is characterized in that, in described step (C), hyperacoustic frequency is 35 ~ 45kHz, power density is 15 ~ 20W/cm2, the temperature of sonic oscillation is 40 ~ 70 DEG C, and mechanical agitation speed is 200 ~ 400rpm, and ultrasonic disperse and mechanical agitation time are 120 ~ 240min.
10. the method preparing modified fullerenes nano particle according to claim 9, is characterized in that, in described step (A), the concentration of described fullerene nanoparticle in described absolute ethyl alcohol is 0.03 ~ 0.06g/mL.
CN201510389998.3A 2015-07-06 2015-07-06 Modified fullerene nanoparticle and vegetable insulating oil-containing complex Pending CN104992749A (en)

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Cited By (4)

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Publication number Priority date Publication date Assignee Title
CN106867679A (en) * 2017-03-20 2017-06-20 国家电网公司 A kind of sorbent regeneration process of the plant transformer oil of deterioration
CN111778087A (en) * 2020-07-10 2020-10-16 宜宾学院 Fullerene lubricating oil additive, preparation method and preparation method of lubricating oil
CN111785410A (en) * 2020-07-31 2020-10-16 云南电网有限责任公司电力科学研究院 Preparation method of nano-powder composite plant insulating oil
CN111849583A (en) * 2020-07-31 2020-10-30 云南电网有限责任公司电力科学研究院 Preparation method of nano plant insulating oil with high oxidation resistance

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Cited By (4)

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Publication number Priority date Publication date Assignee Title
CN106867679A (en) * 2017-03-20 2017-06-20 国家电网公司 A kind of sorbent regeneration process of the plant transformer oil of deterioration
CN111778087A (en) * 2020-07-10 2020-10-16 宜宾学院 Fullerene lubricating oil additive, preparation method and preparation method of lubricating oil
CN111785410A (en) * 2020-07-31 2020-10-16 云南电网有限责任公司电力科学研究院 Preparation method of nano-powder composite plant insulating oil
CN111849583A (en) * 2020-07-31 2020-10-30 云南电网有限责任公司电力科学研究院 Preparation method of nano plant insulating oil with high oxidation resistance

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Application publication date: 20151021