CN116189962A - Modified alumina nano-screen and preparation method thereof, and modified alumina nano-screen insulating oil and preparation method thereof - Google Patents
Modified alumina nano-screen and preparation method thereof, and modified alumina nano-screen insulating oil and preparation method thereof Download PDFInfo
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- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 title claims abstract description 129
- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- 239000007787 solid Substances 0.000 claims abstract description 30
- 150000002148 esters Chemical class 0.000 claims abstract description 28
- 238000006243 chemical reaction Methods 0.000 claims abstract description 15
- 238000002156 mixing Methods 0.000 claims abstract description 15
- 239000003607 modifier Substances 0.000 claims abstract description 15
- 239000002243 precursor Substances 0.000 claims abstract description 14
- BNGXYYYYKUGPPF-UHFFFAOYSA-M (3-methylphenyl)methyl-triphenylphosphanium;chloride Chemical compound [Cl-].CC1=CC=CC(C[P+](C=2C=CC=CC=2)(C=2C=CC=CC=2)C=2C=CC=CC=2)=C1 BNGXYYYYKUGPPF-UHFFFAOYSA-M 0.000 claims abstract description 12
- ATRRKUHOCOJYRX-UHFFFAOYSA-N Ammonium bicarbonate Chemical compound [NH4+].OC([O-])=O ATRRKUHOCOJYRX-UHFFFAOYSA-N 0.000 claims abstract description 12
- 235000012501 ammonium carbonate Nutrition 0.000 claims abstract description 12
- 239000001099 ammonium carbonate Substances 0.000 claims abstract description 12
- 125000005521 carbonamide group Chemical group 0.000 claims abstract description 9
- -1 trimethylolpropane triester Chemical class 0.000 claims description 20
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 18
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 claims description 12
- 238000001354 calcination Methods 0.000 claims description 11
- 238000000034 method Methods 0.000 claims description 11
- 239000011259 mixed solution Substances 0.000 claims description 9
- 239000002904 solvent Substances 0.000 claims description 9
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 8
- 239000011261 inert gas Substances 0.000 claims description 7
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 6
- 238000007789 sealing Methods 0.000 claims description 6
- ZORQXIQZAOLNGE-UHFFFAOYSA-N 1,1-difluorocyclohexane Chemical compound FC1(F)CCCCC1 ZORQXIQZAOLNGE-UHFFFAOYSA-N 0.000 claims description 5
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 5
- 235000021355 Stearic acid Nutrition 0.000 claims description 5
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 5
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 claims description 5
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 claims description 5
- 230000035484 reaction time Effects 0.000 claims description 5
- 229940035049 sorbitan monooleate Drugs 0.000 claims description 5
- 235000011069 sorbitan monooleate Nutrition 0.000 claims description 5
- 239000001593 sorbitan monooleate Substances 0.000 claims description 5
- 239000008117 stearic acid Substances 0.000 claims description 5
- 239000012298 atmosphere Substances 0.000 claims description 4
- SNRUBQQJIBEYMU-UHFFFAOYSA-N dodecane Chemical compound CCCCCCCCCCCC SNRUBQQJIBEYMU-UHFFFAOYSA-N 0.000 claims description 4
- 229940094933 n-dodecane Drugs 0.000 claims description 4
- 229910052757 nitrogen Inorganic materials 0.000 claims description 4
- 229910052786 argon Inorganic materials 0.000 claims description 3
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims description 3
- 230000001105 regulatory effect Effects 0.000 claims description 3
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims 2
- 239000004202 carbamide Substances 0.000 claims 1
- 235000013877 carbamide Nutrition 0.000 claims 1
- 238000004519 manufacturing process Methods 0.000 claims 1
- 239000002086 nanomaterial Substances 0.000 abstract description 9
- 230000000694 effects Effects 0.000 abstract description 6
- 239000000654 additive Substances 0.000 abstract description 2
- 238000003837 high-temperature calcination Methods 0.000 abstract description 2
- 239000003921 oil Substances 0.000 description 130
- 238000001291 vacuum drying Methods 0.000 description 36
- 239000007788 liquid Substances 0.000 description 14
- 230000010355 oscillation Effects 0.000 description 14
- 238000001132 ultrasonic dispersion Methods 0.000 description 13
- 239000000203 mixture Substances 0.000 description 12
- 238000000643 oven drying Methods 0.000 description 11
- 230000000052 comparative effect Effects 0.000 description 10
- 239000008367 deionised water Substances 0.000 description 9
- 229910021641 deionized water Inorganic materials 0.000 description 9
- 239000002480 mineral oil Substances 0.000 description 9
- 235000010446 mineral oil Nutrition 0.000 description 9
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 7
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 6
- 238000001035 drying Methods 0.000 description 6
- 238000010438 heat treatment Methods 0.000 description 6
- 239000002105 nanoparticle Substances 0.000 description 6
- WXZMFSXDPGVJKK-UHFFFAOYSA-N pentaerythritol Chemical compound OCC(CO)(CO)CO WXZMFSXDPGVJKK-UHFFFAOYSA-N 0.000 description 6
- 239000005020 polyethylene terephthalate Substances 0.000 description 6
- 229920000139 polyethylene terephthalate Polymers 0.000 description 6
- 239000000243 solution Substances 0.000 description 6
- 238000005406 washing Methods 0.000 description 6
- 238000005119 centrifugation Methods 0.000 description 5
- NWGKJDSIEKMTRX-AAZCQSIUSA-N Sorbitan monooleate Chemical compound CCCCCCCC\C=C/CCCCCCCC(=O)OC[C@@H](O)[C@H]1OC[C@H](O)[C@H]1O NWGKJDSIEKMTRX-AAZCQSIUSA-N 0.000 description 4
- 238000011160 research Methods 0.000 description 4
- 238000012546 transfer Methods 0.000 description 4
- 230000017525 heat dissipation Effects 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- AFCARXCZXQIEQB-UHFFFAOYSA-N N-[3-oxo-3-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)propyl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(CCNC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 AFCARXCZXQIEQB-UHFFFAOYSA-N 0.000 description 2
- 230000006978 adaptation Effects 0.000 description 2
- 238000005054 agglomeration Methods 0.000 description 2
- 230000002776 aggregation Effects 0.000 description 2
- 150000003857 carboxamides Chemical class 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 239000012530 fluid Substances 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 238000001179 sorption measurement Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical group [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 239000012300 argon atmosphere Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008033 biological extinction Effects 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 239000012299 nitrogen atmosphere Substances 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 230000003014 reinforcing effect Effects 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 238000004804 winding Methods 0.000 description 1
Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B3/00—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties
- H01B3/18—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties mainly consisting of organic substances
- H01B3/20—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties mainly consisting of organic substances liquids, e.g. oils
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F27/00—Details of transformers or inductances, in general
- H01F27/08—Cooling; Ventilating
- H01F27/10—Liquid cooling
- H01F27/12—Oil cooling
- H01F27/125—Cooling by synthetic insulating and incombustible liquid
Abstract
The invention relates to the field of insulating oil additives, and particularly provides a modified alumina nano sieve and a preparation method thereof, and a modified alumina nano sieve insulating oil and a preparation method thereof. According to the invention, the white alumina nano sieve precursor solid is prepared through the mixing reaction of aluminum nitrate, ammonium carbonate and carbonamide, and then the alumina nano sieve is prepared through high-temperature calcination of the white alumina nano sieve precursor solid, meanwhile, in order to ensure that the nano sieve has good stability in insulating oil, the surface of the nano sieve is modified by using a surface modifier, and finally the modified alumina nano sieve is prepared. And further mixing the obtained modified alumina nano sieve with synthetic ester insulating oil to obtain the modified alumina nano sieve insulating oil. According to the invention, by changing the appearance of the nano material, the effect of the physicochemical properties of the nano material on the oil property of the synthetic ester insulating oil is more remarkable, and the modified alumina nano sieve insulating oil with high heat conducting property is obtained.
Description
Technical Field
The invention relates to the technical field of insulating oil additives, in particular to a modified alumina nano sieve and a preparation method thereof, and a modified alumina nano sieve insulating oil and a preparation method thereof.
Background
The insulating oil is an important insulating medium of the transformer, and plays roles of heat dissipation, insulation, arc extinction and the like in the operation process of the transformer. The heat generated during the operation of the transformer causes the insulating oil close to the iron core and the winding to expand and rise by heating, and the heat can be dissipated through the up-down convection of the insulating oil, thereby ensuring the normal operation of the transformer. Currently, the main stream of transformer oil comprises traditional mineral insulating oil, natural ester insulating oil, synthetic ester insulating oil and the like. However, the kinematic viscosity of the ester-based insulating oil is relatively high, the flow speed is slow compared with that of the mineral oil, and the heat dissipation performance is required to be enhanced. Therefore, in order to make the synthetic ester insulating oil have better heat dissipation performance of equipment, the heat conduction performance of the synthetic ester insulating oil can be effectively improved by adding solid nano particles with high heat conduction coefficient into the oil by utilizing the mechanism of reinforcing heat transfer by nano fluid and extremely high specific surface area and reactivity of nano particles.
At present, the research of adding nano materials into the synthetic ester insulating oil is less, most of the nano materials are nano fluids which take mineral oil as base liquid, the research result is not suitable for the synthetic ester insulating oil with different structures, and the properties of the nano modified synthetic ester are required to be measured and evaluated. In addition, the effect of different nano materials on the heat conduction characteristic of the insulating oil is different, and the nano materials with higher efficiency and better applicability are searched for aiming at the unique physical and chemical properties of the synthetic ester insulating oil so as to remarkably improve the heat conductivity of the synthetic ester insulating oil.
Disclosure of Invention
The invention aims to provide a modified alumina nano sieve and a preparation method thereof, and modified alumina nano sieve insulating oil and a preparation method thereof, wherein the surface of the alumina nano sieve is modified, so that the influence effect of the physicochemical property of a nano material on the insulating oil performance of the synthetic ester is more remarkable, and the insulating oil of the synthetic ester of the modified alumina nano sieve with high heat-conducting property is obtained.
In order to achieve the above object, the present invention provides the following technical solutions:
the invention provides a preparation method of a modified alumina nano sieve, which comprises the following steps:
(1) Mixing aluminum nitrate, ammonium carbonate and carbonamide in water to obtain a mixed solution, regulating the pH value of the mixed solution, and reacting to obtain a white aluminum oxide nano-screen precursor solid;
(2) Calcining the white alumina nano sieve precursor solid obtained in the step (1) in an inert gas atmosphere to obtain an alumina nano sieve;
(3) Mixing the alumina nano sieve obtained in the step (2) with a surface modifier in a solvent, and reacting under a sealing condition to obtain the modified alumina nano sieve.
Preferably, in the step (1), the molar ratio of the aluminum nitrate, the ammonium carbonate and the carbonamide is 1:1-3:1-3; the dosage ratio of the aluminum nitrate to the ammonium carbonate to the carbonamide to the water is 1 mol:1-3 mol:30-50 mL;
in the step (1), ammonia water is used for adjusting the pH value of the mixed solution to 8.5-9.5;
the reaction temperature in the step (1) is 40-50 ℃, and the reaction time is 12-24 h.
Preferably, the inert gas in the step (2) comprises nitrogen or argon;
the calcination temperature in the step (2) is 850-950 ℃ and the calcination time is 3-4 h.
Preferably, in the step (3), the mass ratio of the alumina nano sieve to the surface modifier is 1:1-3;
the dosage ratio of the alumina nano sieve to the surface modifier to the solvent in the step (3) is 1 g:1-3 g:30-60 mL;
the solvent in the step (3) comprises n-hexane or n-dodecane;
the surface modifier in the step (3) comprises sorbitan monooleate or stearic acid;
the reaction temperature in the step (3) is 30-50 ℃ and the reaction time is 2-3 h.
The invention also provides the modified alumina nano sieve prepared by the preparation method of the modified alumina nano sieve.
The invention also provides a preparation method of the modified alumina nano sieve insulating oil, which comprises the following steps: and mixing the modified alumina nano sieve obtained by the method with the synthetic ester insulating oil to obtain the modified alumina nano sieve insulating oil.
Preferably, the content of the modified alumina nano sieve is 0.01-0.15 vol% of the total amount of the synthetic ester insulating oil.
Preferably, the synthetic ester insulating oil comprises trimethylolpropane triester insulating oil or pentaerythritol ester insulating oil.
The invention also provides the modified alumina nano-screen insulating oil prepared by the preparation method of the modified alumina nano-screen insulating oil.
Compared with the prior art, the technical scheme of the invention has the following beneficial effects:
according to the invention, the alumina nano sieve with a porous structure is obtained by a precipitation method and a high-temperature calcination method, and meanwhile, in order to ensure that the nano sieve has good stability in insulating oil, a surface modifier is used for carrying out surface modification on the alumina nano sieve, and the surface modifier can form a coating structure on the surface of the alumina nano sieve, so that the compatibility of the alumina nano sieve in the insulating oil is enhanced, the agglomeration phenomenon is reduced, and the modified alumina nano sieve with extremely high specific surface area is obtained.
The modified alumina nano sieve provided by the invention has extremely high specific surface area, the surface of the modified alumina nano sieve can form an adsorption layer with high heat transfer efficiency with synthetic ester insulating oil, and meanwhile, the modified alumina nano sieve has high heat conductivity coefficient, so that the overall heat conductivity coefficient of the nano sieve insulating oil can be improved.
The invention changes the appearance of alumina nano particles with excellent thermal conductivity to be a loose and porous nano sieve structure. Compared with the nano alumina with the traditional structure, the modified alumina nano sieve has better effect on improving the heat conduction performance of the synthetic ester insulating oil. In addition, the invention takes the ester insulating oil synthesized by the modified alumina nano sieve as a research object, and enriches the research and application of the novel nano material of the nano sieve in the field of insulating oil.
Detailed Description
The invention provides a preparation method of a modified alumina nano sieve, which comprises the following steps:
(1) Mixing aluminum nitrate, ammonium carbonate and carbonamide in water to obtain a mixed solution, regulating the pH value of the mixed solution, and reacting to obtain a white aluminum oxide nano-screen precursor solid;
(2) Calcining the white alumina nano sieve precursor solid obtained in the step (1) in an inert gas atmosphere to obtain an alumina nano sieve;
(3) Mixing the alumina nano sieve obtained in the step (2) with a surface modifier in a solvent, and reacting under a sealing condition to obtain the modified alumina nano sieve.
In the invention, the molar ratio of the aluminum nitrate, the ammonium carbonate and the carbonamide in the step (1) is 1:1-3:1-3, preferably 1:1.5-2.5: 1.5 to 2.5; the dosage ratio of the aluminum nitrate, the ammonium carbonate, the carbonamide and the water is 1 mol:1-3 mol:30-50 mL, preferably 1mol:1.5 to 2.5mol:1.5 to 2.5mol: 35-45 mL;
in the step (1), ammonia water with mass fraction of 25% -50% is used for adjusting the pH value of the mixed solution to 8.5-9.5, the mass fraction of the ammonia water is preferably 35-40%, and the pH value is preferably 8.8-9.2;
the temperature of the reaction in the step (1) is 40-50 ℃, preferably 43-47 ℃; the reaction time is 12 to 24 hours, preferably 16 to 20 hours.
In the present invention, the reaction in the step (1) is performed in a reaction vessel;
and (3) after the reaction in the step (1), carrying out centrifugal separation on the mixture, washing the solid obtained by the centrifugal separation by using deionized water and absolute ethyl alcohol, and carrying out vacuum drying to obtain the white alumina nano-screen precursor solid.
In the present invention, the inert gas in the step (2) contains nitrogen or argon, preferably nitrogen;
the calcination temperature in the step (2) is 850-950 ℃, preferably 870-900 ℃; the calcination time is 3 to 4 hours, preferably 3.3 to 3.7 hours.
In the invention, in the step (2), the alumina nano sieve precursor solid is placed in a tube furnace to be calcined under the inert gas atmosphere.
In the invention, the mass ratio of the alumina nano sieve to the surface modifier in the step (3) is 1:1-3, preferably 1:1.5-2.5;
in the step (3), the dosage ratio of the alumina nano sieve to the surface modifier to the solvent is 1 g:1-3 g:30-60 mL, preferably 1g:1.5 g to 2.5g: 40-50 mL;
the solvent in the step (3) comprises n-hexane or n-dodecane, preferably n-hexane;
the surface modifier in step (3) comprises sorbitan monooleate or stearic acid, preferably sorbitan monooleate;
the temperature of the reaction in the step (3) is 30-50 ℃, preferably 35-45 ℃; the time is 2 to 3 hours, preferably 2.4 to 2.8 hours.
In the invention, after the reaction in the step (3), the mixture is centrifugally separated, the solid obtained by centrifugation is washed by deionized water and absolute ethyl alcohol, and the modified alumina nano-sieve is obtained after vacuum drying.
The invention also provides the modified alumina nano sieve prepared by the preparation method of the modified alumina nano sieve.
The invention also provides a preparation method of the modified alumina nano sieve insulating oil, which comprises the following steps: and mixing the modified alumina nano sieve obtained by the method with insulating oil to obtain the modified alumina nano sieve insulating oil.
In the present invention, the content of the modified alumina nano sieve is 0.01 to 0.15vol%, preferably 0.05 to 0.10vol% of the total amount of the insulating oil.
In the present invention, the insulating oil comprises trimethylolpropane triester insulating oil or pentaerythritol ester insulating oil.
According to the invention, the modified alumina nano sieve is mixed with insulating oil, an ultrasonic oscillator is used for dispersing a mixed oil sample, and vacuum drying is carried out after oscillation is finished to obtain the modified alumina nano sieve insulating oil;
the power of the ultrasonic vibration instrument is 1000-1500W, preferably 1200-1300W; the ultrasonic time is 0.5-2 h, preferably 1-1.5 h.
The invention also provides the modified alumina nano-screen insulating oil prepared by the preparation method of the modified alumina nano-screen insulating oil.
The technical solutions provided by the present invention are described in detail below with reference to examples, but they should not be construed as limiting the scope of the present invention.
Example 1
(1) 1g of aluminum nitrate (Al (NO) 3 ) 3 ·9H 2 O), 0.5g of ammonium carbonate ((NH) 4 ) 2 CO 3 ) 0.4g of carboxamide (CO (NH) 2 ) 2 ) Mix in 40mL deionized water, add 25% ammonia to adjust pH to 8.5. The solution was stirred uniformly and then transferred to a reaction vessel, and the solution was reacted at 50℃for 24 hours by heating in an oil bath. And after the reaction is finished, centrifuging the mixture by using a high-speed centrifuge, washing the solid obtained by centrifugation by using deionized water and absolute ethyl alcohol, taking the washed solid, and placing the solid into a vacuum drying oven for vacuum drying at 60 ℃ for 24 hours to obtain the white alumina nano-screen precursor solid.
(2) And (3) placing the nano-screen precursor into a tube furnace, calcining at a high temperature of 900 ℃ for 3 hours in a nitrogen atmosphere, and cooling to obtain the alumina nano-screen with the porous structure.
(3) Mixing an alumina nano sieve and sorbitan monooleate (Span 80) in 40mL of n-hexane, wherein the mass ratio of the alumina nano sieve to the Span80 is 1:2. the mixture was heated in a water bath at 40℃for 2h under sealing. And after heating, centrifugally separating the mixture, washing the solid obtained by centrifugation by using deionized water and absolute ethyl alcohol, taking the washed solid, and placing the solid into a vacuum drying oven for vacuum drying at 60 ℃ for 24 hours to obtain the modified alumina nano sieve.
Example 2
(1) 1g of aluminum nitrate (Al (NO) 3 ) 3 ·9H 2 O), 0.7g of ammonium carbonate ((NH) 4 ) 2 CO 3 ) 0.3g of carboxamide (CO (NH) 2 ) 2 ) Mixing in 50mL deionized water, and adding 50% ammonia water to the mixture to adjust the pH value to 9.0. The solution was stirred uniformly and then transferred to a reaction vessel, and the solution was reacted at 50℃for 20 hours by heating in an oil bath. And after the reaction is finished, centrifuging the mixture by using a high-speed centrifuge, washing the solid obtained by centrifugation by using deionized water and absolute ethyl alcohol, taking the washed solid, and placing the solid into a vacuum drying oven for vacuum drying at 60 ℃ for 24 hours to obtain the white alumina nano-screen precursor solid.
(2) And (3) placing the nano-screen precursor into a tube furnace, calcining at a high temperature of 850 ℃ for 4 hours in an argon atmosphere, and cooling to obtain the alumina nano-screen with the porous structure.
(3) Mixing an alumina nano sieve and stearic acid in 45mL of n-dodecane, wherein the mass ratio of the alumina nano sieve to the stearic acid is 1:2.5. the mixture was heated in a water bath at 40℃for 2.5h under sealing. And after heating, centrifugally separating the mixture, washing the solid obtained by centrifugation by using deionized water and absolute ethyl alcohol, taking the washed solid, and placing the solid into a vacuum drying oven for vacuum drying at 60 ℃ for 24 hours to obtain the modified alumina nano sieve.
Example 3
The modified alumina nano-sieve prepared in example 1 was added to trimethylolpropane triester (TMP triester) insulating oil, wherein the volume ratio of the modified alumina nano-sieve to the whole insulating oil was 0.05vol%. Ultrasonic dispersion is carried out on the nano-screen insulating oil for 1h by using an ultrasonic oscillator, and the ultrasonic power is set to be 1200W. And (3) after the oscillation is finished, placing the oil sample in a vacuum drying oven, and vacuum drying at 90 ℃ for 48 hours to obtain the alumina nano-sieve TMP triester insulating oil. The thermal conductivity of the oil samples at 25, 90 ℃ was tested using a TC3010 series liquid thermal conductivity meter to characterize their thermal conductivity.
Example 4
The modified alumina nano-sieve prepared in example 1 was added to TMP triester insulating oil, wherein the volume ratio of the modified alumina nano-sieve to the whole insulating oil was 0.10vol%. Ultrasonic dispersion is carried out on the nano-screen insulating oil for 1h by using an ultrasonic oscillator, and the ultrasonic power is set to be 1200W. And (3) after the oscillation is finished, placing the oil sample in a vacuum drying oven, and vacuum drying at 90 ℃ for 48 hours to obtain the modified alumina nano-screen TMP triester insulating oil. The thermal conductivity of the oil samples at 25, 90 ℃ was tested using a TC3010 series liquid thermal conductivity meter to characterize their thermal conductivity.
Example 5
The modified alumina nano-sieve prepared in example 1 was added to TMP triester insulating oil, wherein the volume ratio of the modified alumina nano-sieve to the whole insulating oil was 0.15vol%. Ultrasonic dispersion is carried out on the nano-screen insulating oil for 1h by using an ultrasonic oscillator, and the ultrasonic power is set to be 1200W. And (3) after the oscillation is finished, placing the oil sample in a vacuum drying oven, and vacuum drying at 90 ℃ for 48 hours to obtain the modified alumina nano-screen TMP triester insulating oil. The thermal conductivity of the oil samples at 25, 90 ℃ was tested using a TC3010 series liquid thermal conductivity meter to characterize their thermal conductivity.
Example 6
The modified alumina nano-sieve prepared in example 1 was added to pentaerythritol ester (PETP tetraester) insulating oil, wherein the volume ratio of the modified alumina nano-sieve to the whole insulating oil was 0.05vol%. Ultrasonic dispersion is carried out on the nano-screen insulating oil for 1h by using an ultrasonic oscillator, and the ultrasonic power is set to be 1200W. And (3) after the oscillation is finished, placing the oil sample in a vacuum drying oven, and vacuum drying at 90 ℃ for 48 hours to obtain the modified alumina nano-screen PETP tetraester insulating oil after the drying is finished. The thermal conductivity of the oil samples at 25, 90 ℃ was tested using a TC3010 series liquid thermal conductivity meter to characterize their thermal conductivity.
Example 7
The modified alumina nano-sieve prepared in example 1 was added to PETP tetraester insulating oil, wherein the volume ratio of the modified alumina nano-sieve to the whole insulating oil was 0.10vol%. Ultrasonic dispersion is carried out on the nano-screen insulating oil for 1h by using an ultrasonic oscillator, and the ultrasonic power is set to be 1200W. And (3) after the oscillation is finished, placing the oil sample in a vacuum drying oven, and vacuum drying at 90 ℃ for 48 hours to obtain the modified alumina nano-screen PETP tetraester insulating oil after the drying is finished. The thermal conductivity of the oil samples at 25, 90 ℃ was tested using a TC3010 series liquid thermal conductivity meter to characterize their thermal conductivity.
Example 8
The modified alumina nano-sieve prepared in example 1 was added to PETP tetraester insulating oil, wherein the volume ratio of the modified alumina nano-sieve to the whole insulating oil was 0.15vol%. Ultrasonic dispersion is carried out on the nano-screen insulating oil for 1h by using an ultrasonic oscillator, and the ultrasonic power is set to be 1200W. And (3) after the oscillation is finished, placing the oil sample in a vacuum drying oven, and vacuum drying at 90 ℃ for 48 hours to obtain the modified alumina nano-screen PETP tetraester insulating oil after the drying is finished. The thermal conductivity of the oil samples at 25, 90 ℃ was tested using a TC3010 series liquid thermal conductivity meter to characterize their thermal conductivity.
Comparative example 1
Taking washed and dried nano Al without morphology modification 2 O 3 Mixing with Span80 in 40mL of n-hexane, wherein nano Al 2 O 3 The mass ratio to Span80 is 1:2. the mixture was heated in a water bath at 40℃for 2h under sealing. Centrifuging the mixture after heating, washing the solid obtained by centrifuging by using deionized water and absolute ethyl alcohol, placing the washed solid in a vacuum drying oven, and vacuum drying at 60 ℃ for 24 hours to obtain the modified nano Al 2 O 3 。
Taking the nano Al with the surface modified 2 O 3 The nano particles account for 0.05vol% of the whole insulating oil. Ultrasonic dispersion is carried out on the nano-screen insulating oil for 1h by using an ultrasonic oscillator, and the ultrasonic power is set to be 1200W. After oscillation, the oil sample is placed in a vacuum drying oven and is dried in vacuum for 48 hours at 90 ℃ to obtain the modified nano Al after drying 2 O 3 TMP triester insulating oil. The thermal conductivity of the oil samples at 25, 90 ℃ was tested using a TC3010 series liquid thermal conductivity meter to characterize their thermal conductivity.
Comparative example 2
Taking the modified nano Al prepared in comparative example 1 2 O 3 The nano particles account for 0.10vol% of the whole insulating oil. Ultrasonic dispersion is carried out on the nano-screen insulating oil for 1h by using an ultrasonic oscillator, and the ultrasonic power is set to be 1200W. After oscillation, the oil sample is placed in a vacuum drying oven and is dried in vacuum for 48 hours at 90 ℃ to obtain the modified nano Al after drying 2 O 3 TMP triester insulating oil. The thermal conductivity of the oil samples at 25, 90 ℃ was tested using a TC3010 series liquid thermal conductivity meter to characterize their thermal conductivity.
Comparative example 3
Taking the modified nano Al prepared in comparative example 1 2 O 3 The nano particles account for 0.15vol% of the whole insulating oil. Ultrasonic dispersion is carried out on the nano-screen insulating oil for 1h by using an ultrasonic oscillator, and the ultrasonic power is set to be 1200W. After oscillation, the oil sample is placed in a vacuum drying oven and is dried in vacuum for 48 hours at 90 ℃ to obtain the modified nano Al after drying 2 O 3 TMP triester insulating oil. The thermal conductivity of the oil samples at 25, 90 ℃ was tested using a TC3010 series liquid thermal conductivity meter to characterize their thermal conductivity.
Comparative example 4
The modified alumina nano-sieve prepared in example 1 was added to TMP triester insulating oil, wherein the volume ratio of the modified alumina nano-sieve to the whole insulating oil was 0.2vol%. Ultrasonic dispersion is carried out on the modified alumina nano sieve insulating oil for 1h by using an ultrasonic oscillator, and the ultrasonic power is set to be 1200W. And (3) after the oscillation is finished, placing the oil sample in a vacuum drying oven, and vacuum drying at 90 ℃ for 48 hours to obtain the modified alumina nano-screen TMP triester insulating oil. The thermal conductivity of the oil samples at 25, 90 ℃ was tested using a TC3010 series liquid thermal conductivity meter to characterize their thermal conductivity.
Comparative example 5
The modified alumina nano-sieve prepared in example 1 was added to a Kelamani #45 mineral oil insulating oil, wherein the modified alumina nano-sieve was the entire insulatorThe volume ratio of the edge oil is 0.05vol%. Ultrasonic dispersion is carried out on the modified alumina nano sieve insulating oil for 1h by using an ultrasonic oscillator, and the ultrasonic power is set to be 1200W. After oscillation, placing the oil sample in a vacuum drying oven, and vacuum drying at 90deg.C for 48 hr to obtain Al 2 O 3 Nano-screen #45 mineral oil. The thermal conductivity of the oil samples at 25, 90 ℃ was tested using a TC3010 series liquid thermal conductivity meter to characterize their thermal conductivity.
Comparative example 6
The modified alumina nano-sieve prepared in example 1 was added to the clarituximab #45 mineral oil insulating oil, wherein the volume ratio of the modified alumina nano-sieve to the whole insulating oil was 0.10vol%. Ultrasonic dispersion is carried out on the modified alumina nano sieve insulating oil for 1h by using an ultrasonic oscillator, and the ultrasonic power is set to be 1200W. After oscillation, placing the oil sample in a vacuum drying oven, and vacuum drying at 90deg.C for 48 hr to obtain Al 2 O 3 Nano-screen #45 mineral oil. The thermal conductivity of the oil samples at 25, 90 ℃ was tested using a TC3010 series liquid thermal conductivity meter to characterize their thermal conductivity.
Comparative example 7
The modified alumina nano-sieve prepared in example 1 was added to the clarituximab #45 mineral oil insulating oil, wherein the modified alumina nano-sieve was 0.15vol% of the entire insulating oil. Ultrasonic dispersion is carried out on the modified alumina nano sieve insulating oil for 1h by using an ultrasonic oscillator, and the ultrasonic power is set to be 1200W. After oscillation, placing the oil sample in a vacuum drying oven, and vacuum drying at 90deg.C for 48 hr to obtain Al 2 O 3 Nano-screen #45 mineral oil. The thermal conductivity of the oil samples at 25, 90 ℃ was tested using a TC3010 series liquid thermal conductivity meter to characterize their thermal conductivity.
TABLE 1 results of thermal conductivity testing of oil samples of examples 3-8 and comparative examples 1-7 at 25℃and 90 ℃
From the above table data, it can be seen that the modified alumina nano-screen with porous structure is compared with solid single crystal modified nano-Al 2 O 3 The heat conductivity coefficient of the synthetic ester insulating oil is improved better, and the advantages of the nano sieve material provided by the invention are reflected. When the addition amount of the modified alumina nano sieve is 0.20vol%, the heat conductivity enhancement effect on TMP triester insulating oil is weakened, which indicates that too much nano sieve can increase the agglomeration phenomenon, the contact area between the nano material and the insulating oil is reduced, and the heat transfer is not facilitated. In addition, the effect of the nano sieve on improving the heat conductivity coefficient in #45 mineral oil is not obvious as that in synthetic ester, which shows that the nano sieve has higher structural adaptation degree with synthetic ester insulating oil, and the unique physical and chemical properties of the nano sieve and the synthetic ester insulating oil enable an adsorption layer formed on the surface of the synthetic ester to have higher heat transfer efficiency.
The foregoing is merely a preferred embodiment of the present invention and it should be noted that modifications and adaptations to those skilled in the art may be made without departing from the principles of the present invention, which are intended to be comprehended within the scope of the present invention.
Claims (9)
1. The preparation method of the modified alumina nano sieve is characterized by comprising the following steps of:
(1) Mixing aluminum nitrate, ammonium carbonate and carbonamide in water to obtain a mixed solution, regulating the pH value of the mixed solution, and reacting to obtain a white aluminum oxide nano-screen precursor solid;
(2) Calcining the white alumina nano sieve precursor solid obtained in the step (1) in an inert gas atmosphere to obtain an alumina nano sieve;
(3) Mixing the alumina nano sieve obtained in the step (2) with a surface modifier in a solvent, and reacting under a sealing condition to obtain the modified alumina nano sieve.
2. The method for preparing a modified alumina nano-screen according to claim 1, wherein the molar ratio of aluminum nitrate, ammonium carbonate and carbamide in the step (1) is 1:1-3:1-3; the dosage ratio of the aluminum nitrate to the ammonium carbonate to the carbonamide to the water is 1 mol:1-3 mol:30-50 mL;
in the step (1), ammonia water is used for adjusting the pH value of the mixed solution to 8.5-9.5;
the reaction temperature in the step (1) is 40-50 ℃, and the reaction time is 12-24 h.
3. The method for preparing a modified alumina nano-sieve according to claim 2, wherein the inert gas in the step (2) comprises nitrogen or argon;
the calcination temperature in the step (2) is 850-950 ℃ and the calcination time is 3-4 h.
4. The method for preparing a modified alumina nano-screen according to claim 1, 2 or 3, wherein the mass ratio of the alumina nano-screen to the surface modifier in the step (3) is 1:1-3;
the dosage ratio of the alumina nano sieve to the surface modifier to the solvent in the step (3) is 1 g:1-3 g:30-60 mL;
the solvent in the step (3) comprises n-hexane or n-dodecane;
the surface modifier in the step (3) comprises sorbitan monooleate or stearic acid;
the reaction temperature in the step (3) is 30-50 ℃ and the reaction time is 2-3 h.
5. A modified alumina nano-screen prepared by the method for preparing a modified alumina nano-screen according to any one of claims 1 to 4.
6. The preparation method of the modified alumina nano sieve insulating oil is characterized by comprising the following steps of: mixing the modified alumina nano-screen of claim 5 with a synthetic ester insulating oil to obtain a modified alumina nano-screen insulating oil.
7. The method for preparing a modified alumina nano-sieve insulating oil according to claim 6, wherein the content of the modified alumina nano-sieve is 0.01 to 0.15vol% of the total amount of the synthetic ester insulating oil.
8. The method for producing a modified alumina nano-screen insulating oil according to claim 6 or 7, wherein the synthetic ester insulating oil comprises trimethylolpropane triester insulating oil or pentaerythritol ester insulating oil.
9. The modified alumina nano-screen insulating oil prepared by the method for preparing the modified alumina nano-screen insulating oil according to any one of claims 6 to 8.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1865147A (en) * | 2005-05-18 | 2006-11-22 | 中国石油化工股份有限公司 | Nano alumina and its preparation method |
| CN107128961A (en) * | 2017-06-09 | 2017-09-05 | 福州大学 | A kind of preparation method and applications of the tabular alumina with loose structure |
| CN110451538A (en) * | 2019-08-20 | 2019-11-15 | 中铝山东有限公司 | A kind of preparation method of high-purity boehmite and high purity aluminium oxide |
| CN113462451A (en) * | 2021-06-29 | 2021-10-01 | 广西大学 | Preparation method of antioxidant rapeseed insulating oil |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1865147A (en) * | 2005-05-18 | 2006-11-22 | 中国石油化工股份有限公司 | Nano alumina and its preparation method |
| CN107128961A (en) * | 2017-06-09 | 2017-09-05 | 福州大学 | A kind of preparation method and applications of the tabular alumina with loose structure |
| CN110451538A (en) * | 2019-08-20 | 2019-11-15 | 中铝山东有限公司 | A kind of preparation method of high-purity boehmite and high purity aluminium oxide |
| CN113462451A (en) * | 2021-06-29 | 2021-10-01 | 广西大学 | Preparation method of antioxidant rapeseed insulating oil |
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