CN101950601B - Composite of mineral insulating oil and modified nanoparticle powder as well as application and preparation method thereof - Google Patents

Composite of mineral insulating oil and modified nanoparticle powder as well as application and preparation method thereof Download PDF

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CN101950601B
CN101950601B CN2010102406721A CN201010240672A CN101950601B CN 101950601 B CN101950601 B CN 101950601B CN 2010102406721 A CN2010102406721 A CN 2010102406721A CN 201010240672 A CN201010240672 A CN 201010240672A CN 101950601 B CN101950601 B CN 101950601B
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powder
nano
insulating oil
mineral insulating
compound
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CN101950601A (en
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李剑
廖瑞金
杨丽君
孙才新
唐炬
陈伟根
杜林�
王有元
张晓星
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Chongqing University
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Abstract

The invention provides a composite of mineral insulating oil and modified nanometer powder as well as application and a preparation method thereof. The composite comprises mineral insulating oil and nanometer powder. The preparation method of the nanometer modified insulating oil comprises the following steps: carrying out surface treatment on the nanometer powder; mixing the dehydrated and degassed mineral insulating oil with the nanometer powder performed with surface treatment; carrying out ultrasonic oscillation on mixed insulating oil; and adding the oscillated mixture into a planetary ball mill, and processing by a wet milling process. The invention adds the nanoparticle powder into the mineral insulating oil to form nanometer liquid dielectric, improves the dielectric property of the insulating oil and can strengthen the cooling effect of a transformer winding coil; in addition, the nanometer powder is much smaller than impurity particles in the insulating oil, can form a stable sol system with a liquid medium and does not form a breakdownsmall bridge under the action of the external electric field so as to improve the dielectric strength of the insulating oil.

Description

The compound of mineral insulating oil and modified nano powder and application thereof and preparation method
Technical field
The present invention relates to the insulating oil technical field, be specifically related to a kind of mineral oil compound, the application of this mineral oil compound in the preparation insulating oil, and the preparation method of this mineral oil compound.
Background technology
Insulating oil is important liquid insulating medium, in electric equipments such as transformer, uses in a large number.Power transformer is one of equipment crucial in the electric power netting safe running, and the serious accident of transformer not only can cause self damaging, also can the interrupt power supply.The deterioration of transformer built-in electrical insulation medium and the main cause of the transformer fault that the insulation breakdown that causes causes often.Along with improving constantly of transmission voltage grade, the oilpaper compound inslation more and more is difficult to satisfy the strict demand of voltage levels to big capacity, miniaturization, high stability insulation system.And to the oilpaper compound inslation deficiency that the aging damage characteristic is familiar with under electromagnetic field, thermal stress effect; And, further increased the difficulty of transformer insulated design and manufacturing to the shortage of the correlation theory foundation of the aspects such as space charge effect of the discharge mechanism of paper oil insulation, medium.Therefore, the mechanism of research oilpaper compound inslation system aging and destruction is improved and raising insulating material performance, and development of new High Performance Insulation material is the developing direction of high reliability high-tension transformer manufacturing technology.
Mineral insulating oil has good electric insulation and advantages such as cooling performance and less cost concurrently, but along with the improving constantly of current power transmission grade, the electrical insulation properties of mineral insulating oil is had higher requirement.
Summary of the invention
In view of this, in order to address the above problem, the present invention provides the compound of a kind of mineral insulating oil and nano-powder, prepares insulating oil with this compound, can improve the dielectric property of insulating oil.
The objective of the invention is to realize like this, the compound of mineral insulating oil and nano-powder comprises mineral insulating oil and nano-powder.
Further, said nano-powder is one or more in tri-iron tetroxide, aluminium nitride, alundum (Al, di-iron trioxide, zinc oxide, the magnesia;
Further, the following surface treatment of said nano-powder process:
A) nano-powder is mixed with absolute ethyl alcohol;
B) add silane coupler, the quality of silane coupler is 1%~10% of a nano-powder quality;
C) mixed liquor with step B gained carries out ultrasonic dispersion and stirring under 40 ℃~70 ℃;
D) absolute ethyl alcohol cleans nano-powder, and is dry in vacuum oven then;
E) dried nano-powder grinds to form powdery;
Further, the quality of said nano-powder is 0.001%~5% of a nano modification mineral insulation oil quality;
Further, the diameter of said nano-powder is 40nm~600nm.
The present invention also discloses the application of compound in the preparation insulating oil of above-mentioned mineral insulating oil and nano-powder.
The present invention also provides the preparation method as the compound of the mineral insulating oil of nano modification mineral insulating oil and nano-powder, comprises the steps:
1) nano-powder is carried out surface treatment;
2) will through dewatering, the mineral insulating oil of degasification and surface treated nano-powder mix;
3) with step 2) mixture that obtains carries out sonic oscillation;
4) mixture after the oscillation treatment is added in the planetary ball mill, adopt wet grinding to handle, obtain the compound of mineral insulating oil and nano-powder.
Further, also comprise the steps: after the step 4)
5) will pass through the nano modification mineral insulating oil and carry out vacuumize and vacuum degassing, sealing is preserved;
Further, said step 1) comprises the steps:
A) nano-powder is mixed with absolute ethyl alcohol;
B) add silane coupler, the quality of silane coupler is 1%~10% of a nano-powder quality;
C) mixed liquor with step B gained carries out ultrasonic dispersion and stirring under 40 ℃~70 ℃;
D) absolute ethyl alcohol cleans nano-powder, and is dry in vacuum oven then;
E) dried nano-powder grinds to form powdery;
Further, in the said step 3), frequency of ultrasonic is 40kHz, and power density is 18W/cm 2, the temperature of sonic oscillation is 40-60 ℃, duration of oscillation is 30-60min.
Compared with prior art, the present invention has following advantage: in traditional mineral insulating oil, add nano-powder and can form a kind of liquid nano dielectric, it not only can improve the dielectric property of insulating oil, and can strengthen the thermolysis of Transformer Winding coil.And nano-powder is much littler than the foreign particle in the insulating oil, can form the stable sols system with liquid medium, under the effect of electric field, can not form the puncture foot bridge outside, thereby improves insulating oil dielectric strength.The present invention adds nano-powder with mineral insulating oil and obtains, and nano-powder can stably be distributed in the mineral insulating oil through surface modification treatment; The compound of mineral insulating oil of the present invention and nano-powder promptly can be used as the nano modification mineral insulating oil; It has good physics and chemistry and dielectric property; The all performance index of nano modification mineral insulating oil all meet the standard GB 2536-90 of mineral transformer oil, and frequency breakdown voltage, lightning impulse voltage and the local incipient discharge voltage of relatively outstanding is mixture all can improve 10%~40% on the basis of not adding nano-powder mineral insulation oil sample.
Other advantages of the present invention, target; To in specification subsequently, set forth to a certain extent with characteristic; And to a certain extent,, perhaps can from practice of the present invention, obtain instruction based on being conspicuous to those skilled in the art to investigating of hereinafter.
Embodiment
Below will carry out detailed description to the preferred embodiments of the present invention.
As the mineral insulating oil of nano modification mineral insulating oil and the compound of nano-powder, comprise mineral insulating oil and nano-powder, in addition, also can add additives such as oxidation inhibitor, matal deactivator as required.
Said mineral insulating oil can be selected existing 25# or 10# mineral insulating oil for use, and said nano-powder is one or more in the inorganic nanometer powders such as tri-iron tetroxide, aluminium nitride, alundum (Al, di-iron trioxide, zinc oxide, magnesia; The quality of said nano-powder is 0.001%~5% of a nano modification mineral insulation oil quality; The diameter of said nano-powder is 10nm~600nm, the following surface treatment of said nano-powder process:
1) nano-powder is mixed with absolute ethyl alcohol, ratio is with the 10g nano-powder: the 200mL absolute ethyl alcohol is advisable;
2) add silane coupler again, it is a kind of among KH550, KH560, the KH570 that said silane coupler can be selected model, and the silane coupler quality that is added is 1%~10% of a nano-powder quality;
3) mixed liquor is carried out ultrasonic dispersion and stirring under 40 ℃~70 ℃, the reaction time is 1.5-3 hour;
4) clean nano-powder repeatedly with absolute ethyl alcohol, dry in vacuum oven then;
5) dried nano-powder is ground to form powdery, for use.
Embodiment 1
(1) be the Fe about 40nm with diameter 3O 4(tri-iron tetroxide) nano-powder carries out surface treatment, and in the treatment step, the quality that adds silane coupler KH550 is 2% of a nano-powder quality, under 50 ℃ of water-baths, carries out ultrasonic dispersion, carries out mechanical agitation simultaneously, and the reaction time is 1.5 hours;
(2) will through dewatering, the mineral insulating oil and the surface treated Fe of degasification 3O 4Nano-powder mixes, and the quality of nano-powder is 0.1% of a mineral insulation oil quality.
(3) adopt the method for sonic oscillation to handle in mixed mixture, ultrasonic frequency is 40kHz, and power density is 18W/cm 2, the temperature of sonic oscillation is 50 ℃, duration of oscillation is 60min.
(4) mixture after the oscillation treatment is added in the planetary ball mill, adopt wet grinding to handle, rotating speed is 150r/min, processing time 30min.
(5) the nano modification mineral insulating oil after the above processing is carried out vacuumize and vacuum degassing, sealing is preserved.
Embodiment 2
(1) be that AlN (aluminium nitride) nano-powder about 100nm carries out surface treatment with diameter; In the treatment step, the quality that splashes into silane coupler is a nano-powder quality 4%, then mixed solution is carried out ultrasonic dispersion under 60 ℃ of water-baths; Carry out mechanical agitation simultaneously, the reaction time is 2 hours;
(2) will through dewatering, the mineral insulating oil and the surface treated AlN nano-powder of degasification mix, the quality of nano-powder is 0.01% of a mineral insulation oil quality.
(3) adopt the method for sonic oscillation to handle in mixed mixture, ultrasonic frequency is 40kHz, and power density is 18W/cm 2, the temperature of sonic oscillation is 60 ℃, duration of oscillation is 30min.
(4) mixture after the oscillation treatment is added in the planetary ball mill, adopt wet grinding to handle, rotating speed is 150r/min, processing time 60min.
(5) the nano modification mineral insulating oil after the above processing is carried out vacuumize and vacuum degassing, sealing is preserved.
Embodiment 3
(1) be the Al about 600nm with diameter 2O 3(alundum (Al) nano-powder carries out surface treatment, and in the treatment step, the quality that splashes into silane coupler is a nano-powder quality 10%, and mixed solution is carried out ultrasonic dispersion under 50 ℃ of water-baths, and the reaction time is 3 hours.
(2) will through dewatering, the mineral insulating oil and the surface treated Al of degasification 2O 3Nano-powder mixes, and the quality of nano-powder is 0.5% of a mineral insulation oil quality.
(3) adopt the method for sonic oscillation to handle in mixed mixture, ultrasonic frequency is 40kHz, and power density is 18W/cm 2, the temperature of sonic oscillation is 50 ℃, duration of oscillation is 20min.
(4) mixture after the oscillation treatment is added in the planetary ball mill, adopt wet grinding to handle, rotating speed is 150r/min, processing time 60min.
(5) the nano modification mineral insulating oil after the above processing is carried out vacuumize and vacuum degassing, sealing is preserved.
Embodiment 4
(1) be the Fe about 10nm with diameter 2O 3(di-iron trioxide) and Fe 3O 4(tri-iron tetroxide) nano-powder carries out surface treatment, and in the treatment step, the quality that adds silane coupler is 2% of a nano-powder quality, under 50 ℃ of water-baths, carries out ultrasonic dispersion, carries out mechanical agitation simultaneously, and the reaction time is 2.5 hours;
(2) will through dewatering, the mineral insulating oil and the surface treated Fe of degasification 2O 3And Fe 3O 4The nano-powder that mixes mixes, and the quality of nano-powder is 0.001% of a mineral insulation oil quality.
(3) adopt the method for sonic oscillation to handle in mixed mixture, ultrasonic frequency is 40kHz, and power density is 18W/cm 2, the temperature of sonic oscillation is 50 ℃, duration of oscillation is 10min.
(4) mixture after the oscillation treatment is added in the planetary ball mill, adopt wet grinding to handle, rotating speed is 180r/min, processing time 40min.
(5) the nano modification mineral insulating oil after the above processing is carried out vacuumize and vacuum degassing, sealing is preserved.
Embodiment 5
(1) be AlN (aluminium nitride), Al about 300nm with diameter 2O 3(alundum (Al) nano-powder carries out surface treatment, and in the treatment step, the quality that adds silane coupler is 2% of a nano-powder quality, under 50 ℃ of water-baths, carries out ultrasonic dispersion, carries out mechanical agitation simultaneously, and the reaction time is 2.5 hours;
(2) will through dewatering, mineral insulating oil and the surface treated AlN and the Al of degasification 2O 3The nano-powder that nano-powder mixes mixes, and the quality of nano-powder is 5% of a mineral insulation oil quality.
(3) adopt the method for sonic oscillation to handle in mixed mixture, ultrasonic frequency is 40kHz, and power density is 18W/cm 2, the temperature of sonic oscillation is 60 ℃, duration of oscillation is 60min.
(4) mixture after the oscillation treatment is added in the planetary ball mill, adopt wet grinding to handle, rotating speed is 200r/min, processing time 30min.
(5) the nano modification mineral insulating oil after the above processing is carried out vacuumize and vacuum degassing, sealing is preserved.
The leading indicator of the nano modification mineral insulating oil of the present invention's preparation is following:
Figure BSA00000210585600061
The above is merely the preferred embodiments of the present invention, is not limited to the present invention, and obviously, those skilled in the art can carry out various changes and modification and not break away from the spirit and scope of the present invention the present invention.Like this, belong within the scope of claim of the present invention and equivalent technologies thereof if of the present invention these are revised with modification, then the present invention also is intended to comprise these changes and modification interior.

Claims (8)

1. the compound of mineral insulating oil and nano-powder is characterized in that: comprise mineral insulating oil and nano-powder;
The following surface treatment of said nano-powder process:
A) nano-powder is mixed with absolute ethyl alcohol;
B) add silane coupler, the quality of silane coupler is 1%~10% of a nano-powder quality;
C) mixed liquor with step B gained carries out ultrasonic dispersion and stirring under 40 ℃~70 ℃;
D) nano-powder after the modification of absolute ethyl alcohol clean surface, dry in vacuum oven then;
E) dried nano-powder grinds to form powdery.
2. the compound of mineral insulating oil as claimed in claim 1 and nano-powder is characterized in that: said nano-powder is one or more in tri-iron tetroxide, aluminium nitride, alundum (Al, di-iron trioxide, zinc oxide, the magnesia.
3. the compound of mineral insulating oil as claimed in claim 2 and nano-powder is characterized in that: the quality of said nano-powder be mineral insulating oil and nano-powder the compound quality 0.001%~5%.
4. like the compound of each described mineral insulating oil and nano-powder in the claim 1 to 3, it is characterized in that: the diameter of said nano-powder is 10nm~600nm.
5. like the application in the preparation insulating oil of the compound of each described mineral insulating oil and nano-powder in the claim 1 to 4.
6. the preparation method of the compound of mineral insulating oil and nano-powder is characterized in that: comprise the steps:
1) nano-powder is carried out surface treatment;
2) will through dewatering, the mineral insulating oil of degasification and surface treated nano-powder mix;
3) with step 2) mixture that obtains carries out sonic oscillation;
4) mixture after the oscillation treatment is added in the planetary ball mill, adopt wet grinding to handle, obtain the compound of mineral insulating oil and nano-powder;
Said step 1) comprises the steps:
A) nano-powder is mixed with absolute ethyl alcohol;
B) add silane coupler, the quality of silane coupler is 1%~10% of a nano-powder quality;
C) mixed liquor with step B gained carries out ultrasonic dispersion and stirring under 40 ℃~70 ℃;
D) nano-powder after the modification of absolute ethyl alcohol clean surface, dry in vacuum oven then;
E) dried nano-powder grinds to form powdery, and is for use.
7. the preparation method of the compound of mineral insulating oil as claimed in claim 6 and nano-powder is characterized in that: also comprise the steps: after the step 4)
5) mineral insulating oil of gained after the step 4) and the compound of nano-powder are carried out vacuumize and vacuum degassing, sealing is preserved.
8. like the preparation method of the compound of each described mineral insulating oil and nano-powder in the claim 6 to 7, it is characterized in that: in the said step 3), frequency of ultrasonic is 40kHz, and power density is 18W/cm 2, the temperature of sonic oscillation is 40-60 ℃, duration of oscillation is 10-60min.
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CN105132079B (en) * 2015-07-08 2018-10-19 清华大学 A kind of preparation method of the particle modified transformer oil of aluminum nitride nanometer
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