CN115960652A - Composite nano material and preparation method and application thereof - Google Patents
Composite nano material and preparation method and application thereof Download PDFInfo
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- CN115960652A CN115960652A CN202310079162.8A CN202310079162A CN115960652A CN 115960652 A CN115960652 A CN 115960652A CN 202310079162 A CN202310079162 A CN 202310079162A CN 115960652 A CN115960652 A CN 115960652A
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- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 claims description 9
- WRIDQFICGBMAFQ-UHFFFAOYSA-N (E)-8-Octadecenoic acid Natural products CCCCCCCCCC=CCCCCCCC(O)=O WRIDQFICGBMAFQ-UHFFFAOYSA-N 0.000 claims description 8
- QGLWBTPVKHMVHM-KTKRTIGZSA-N (z)-octadec-9-en-1-amine Chemical compound CCCCCCCC\C=C/CCCCCCCCN QGLWBTPVKHMVHM-KTKRTIGZSA-N 0.000 claims description 8
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- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 claims description 8
- 239000008117 stearic acid Substances 0.000 claims description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 claims description 6
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- 238000000034 method Methods 0.000 claims description 5
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- 229920001174 Diethylhydroxylamine Polymers 0.000 claims description 3
- FVCOIAYSJZGECG-UHFFFAOYSA-N diethylhydroxylamine Chemical compound CCN(O)CC FVCOIAYSJZGECG-UHFFFAOYSA-N 0.000 claims description 3
- 238000005119 centrifugation Methods 0.000 claims description 2
- 125000000113 cyclohexyl group Chemical group [H]C1([H])C([H])([H])C([H])([H])C([H])(*)C([H])([H])C1([H])[H] 0.000 claims description 2
- 239000002244 precipitate Substances 0.000 claims description 2
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- 150000004667 medium chain fatty acids Chemical class 0.000 description 2
- WXZMFSXDPGVJKK-UHFFFAOYSA-N pentaerythritol Chemical compound OCC(CO)(CO)CO WXZMFSXDPGVJKK-UHFFFAOYSA-N 0.000 description 2
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- OHVLMTFVQDZYHP-UHFFFAOYSA-N 1-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)-2-[4-[2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidin-5-yl]piperazin-1-yl]ethanone Chemical compound N1N=NC=2CN(CCC=21)C(CN1CCN(CC1)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)=O OHVLMTFVQDZYHP-UHFFFAOYSA-N 0.000 description 1
- KZEVSDGEBAJOTK-UHFFFAOYSA-N 1-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)-2-[5-[2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidin-5-yl]-1,3,4-oxadiazol-2-yl]ethanone Chemical compound N1N=NC=2CN(CCC=21)C(CC=1OC(=NN=1)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)=O KZEVSDGEBAJOTK-UHFFFAOYSA-N 0.000 description 1
- JQMFQLVAJGZSQS-UHFFFAOYSA-N 2-[4-[2-(2,3-dihydro-1H-inden-2-ylamino)pyrimidin-5-yl]piperazin-1-yl]-N-(2-oxo-3H-1,3-benzoxazol-6-yl)acetamide Chemical compound C1C(CC2=CC=CC=C12)NC1=NC=C(C=N1)N1CCN(CC1)CC(=O)NC1=CC2=C(NC(O2)=O)C=C1 JQMFQLVAJGZSQS-UHFFFAOYSA-N 0.000 description 1
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- ZJCCRDAZUWHFQH-UHFFFAOYSA-N Trimethylolpropane Chemical compound CCC(CO)(CO)CO ZJCCRDAZUWHFQH-UHFFFAOYSA-N 0.000 description 1
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Landscapes
- Inorganic Insulating Materials (AREA)
Abstract
The invention belongs to the technical field of insulating materials, and particularly relates to a composite nano material as well as a preparation method and application thereof. The composite nano material comprises the following components in parts by weight: 0.3-1 part of nano particle Al 2 O 3 0.3 to 1 portion of nano TiO particle 2 1-3 parts of surfactant and 1-3 parts of polymerization inhibitor. The composite nano material prepared by the invention can obviously improve the thermal conductivity and the insulating strength of the synthetic ester insulating oil at the same time, and makes up the limitation of the nano material with single component in improving the performance of the synthetic ester insulating oil to a certain extent.
Description
Technical Field
The invention belongs to the technical field of insulating materials, and particularly relates to a composite nano material as well as a preparation method and application thereof.
Background
At present, most oil-immersed transformers use mineral insulating oil as an insulating medium, but the mineral oil cannot be degraded, which causes serious environmental pollution problems after leakage, and the non-regenerability of the mineral oil makes the mineral oil limited by shortage of petroleum resources, so that renewable and easily degradable synthetic ester insulating oil is one of excellent substitutes of the mineral oil, but the synthetic ester insulating oil has a short plate with inferior insulating strength to the mineral oil, and therefore how to obtain the synthetic ester insulating oil with higher electrical strength becomes one of the current research hotspots.
Because the nano particles have the characteristics of high small size effect, volume effect, quantum size, tunnel effect and the like, the insulating property and the heat conducting property of the synthetic ester insulating oil are improved by adding the nano particles into the synthetic ester insulating oil in the prior art. At present, the nano modified insulating oil basically adopts metal oxide nano particles as an additive material, and TiO is usually selected 2 、Fe 3 O 4 、Al 2 O 3 、SiO 2 SiC, znO, mgO, and the like. However, the nanometer material added in the nanometer insulating oil has single component, and cannot play a role in improving the performance in many aspects. Therefore, new composite insulating materials need to be explored to meet the special requirements of insulating oil performance improvement.
Disclosure of Invention
The invention aims to provide a composite nano material and a preparation method and application thereof. The composite nano material prepared by the invention can obviously improve the thermal conductivity and the insulating strength of the synthetic ester insulating oil at the same time, and makes up the limitation of a single-component nano material in the aspect of improving the performance of the synthetic ester insulating oil to a certain extent.
In order to achieve the purpose, the invention adopts the following technical scheme: a composite nano material comprises the following components in parts by weight: 0.3-1 part of nano particle Al 2 O 3 0.3 to 1 portion of nano TiO particle 2 1-3 parts of surfactant, 1-E3 parts of polymerization inhibitor.
Preferably, the nanoparticles Al 2 O 3 With nano-particle TiO 2 The mass ratio of (1): (1-2).
Preferably, the nanoparticles Al 2 O 3 The particle diameter of (2) is 1 to 20 μm.
Preferably, the nanoparticle TiO 2 The particle diameter of (A) is 1 to 30 μm.
Preferably, the surfactant comprises oleic acid, stearic acid and oleylamine.
More preferably, the mass ratio of oleic acid, stearic acid and oleylamine is 2:1:1.
preferably, the polymerization inhibitor comprises triethylamine, styrene and N, N-diethylhydroxylamine.
More preferably, the mass ratio of triethylamine, styrene and N, N-diethylhydroxylamine is 3:1:1.
a preparation method of the composite nano material comprises the following steps:
dissolving all the components in a solvent, stirring, performing ultrasonic dispersion, centrifuging, cleaning precipitates obtained by centrifuging, and drying to obtain the composite nano material.
Preferably, the preparation method at least comprises one of the following (1) to (6):
(1) The solvent is cyclohexane;
(2) The adding amount of the solvent is 6 to 15 times of the total mass of the composite nano material;
(3) The temperature of the ultrasonic dispersion is 40-70 ℃, and the time is 12-36 h;
(4) The rotation speed of the centrifugation is 2500-3000 rpm, and the time is 3-5 min;
(5) The cleaning is to select deionized water and absolute ethyl alcohol to respectively carry out cleaning for 2-5 times;
(6) The drying temperature is 80-90 ℃ and the drying time is 10-15 h.
An application of the composite nano material in preparing modified synthetic ester insulating oil.
The modified synthetic ester insulating oil comprises the composite nano material and synthetic ester insulating oil, wherein the concentration of the composite nano material in the synthetic ester insulating oil is 0.01 g/L-0.10 g/L.
The synthetic ester insulating oil comprises TMP triester (synthesized by esterifying medium-chain fatty acid with trimethylolpropane), PETP tetraester (synthesized by esterifying medium-chain fatty acid with pentaerythritol) and other conventional synthetic ester insulating oil components in the field.
The invention selects nano-particle Al 2 O 3 And nano TiO particle 2 As a component of the composite nano material, the two metal oxide nano particles can generate polarization phenomenon in the synthetic ester insulating oil, so that the two metal oxide nano particles are matched with each other to present synergistic action. Compared with single nano Al 2 O 3 And nano TiO 2 The composite use of the two components has better effect of improving the insulating property and the heat conducting property of the synthetic ester oil.
Compared with the prior art, the invention has the following beneficial effects:
the invention selects nano-particle Al 2 O 3 And nano-particle TiO 2 As a composite nano material component, the composite nano material makes up the limitation of a nano material with a single component in the aspect of improving the performance of the synthetic ester insulating oil to a certain extent. The composite nano material prepared by the invention can obviously improve the thermal conductivity and the insulating strength of the synthetic ester insulating oil at the same time.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
In the examples and comparative examples, the experimental methods used were conventional unless otherwise specified, and the materials, reagents and the like used were commercially available unless otherwise specified.
Example 1 composite nanomaterial of the invention and method for preparing the same
The components are as follows: 0.3 parts of nano-particle Al 2 O 3 0.3 part of nano TiO particle 2 1 part of a surfactant (the mass ratio of oleic acid to stearic acid to oleylamine is 2.
Wherein, the nano particles Al 2 O 3 Particle diameter of 1 μm, nano-particle TiO 2 Has a particle diameter of 30 μm.
The preparation method comprises the following steps:
dissolving all the components in 33ml of cyclohexane, uniformly stirring, putting the mixture into an ultrasonic oscillation instrument, continuously oscillating for 36 hours at 40 ℃ at a working frequency of 30s after stopping every 1min of ultrasonic oscillation, separating the mixed solution after the ultrasonic oscillation by adopting a high-speed centrifuge, setting the rotating speed to be 2500rpm for 5min, firstly washing the separated solid substance by using deionized water for 2 times, then washing the solid substance by using absolute ethyl alcohol for 2 times, and drying the washed solid substance in a vacuum drying box for 15 hours at a high temperature of 80 ℃ to prepare the composite nano material.
Example 2
The components are as follows: 0.5 parts of nano-particle Al 2 O 3 0.5 part of nano TiO particle 2 1.2 parts of a surfactant (the mass ratio of oleic acid, stearic acid and oleylamine is 2.
Wherein, the nano particles Al 2 O 3 Particle diameter of 10 μm, nano-particle TiO 2 Has a particle diameter of 10 μm.
The preparation method comprises the following steps:
dissolving all the components in 40ml of cyclohexane, uniformly stirring, putting the mixture into an ultrasonic oscillation instrument, continuously oscillating for 24 hours at 60 ℃ at a working frequency of 30s per 1min of ultrasonic oscillation, separating the mixed solution after the ultrasonic oscillation by adopting a high-speed centrifuge, setting the rotating speed to 3000rpm for 5min, cleaning the separated solid substance by using deionized water for 3 times, cleaning the solid substance by using absolute ethyl alcohol for 3 times, and drying the cleaned solid substance in a vacuum drying box at a high temperature of 90 ℃ for 12 hours to obtain the composite nano material.
Example 3
The components are as follows: 1 part of nano-particle Al 2 O 3 1 part of nano TiO particle 2 3 parts of a surfactant (the mass ratio of oleic acid, stearic acid and oleylamine is 2.
Wherein, the nano particles Al 2 O 3 Has a particle diameter of 20 mu m and is a nano-particle TiO 2 Has a particle diameter of 1 μm.
The preparation method comprises the following steps:
dissolving all the components in 50ml of cyclohexane, uniformly stirring, putting the mixture into an ultrasonic oscillation instrument, continuously oscillating for 12 hours at 70 ℃ at the working frequency of stopping 30s every 1min of ultrasound, then separating the mixed solution after ultrasonic oscillation by adopting a high-speed centrifuge, setting the rotating speed at 3000rpm for 5min, then washing the separated solid substance for 5 times by using deionized water, then washing the solid substance for 5 times by using absolute ethyl alcohol, and drying the washed solid substance in a vacuum drying box for 10 hours at the high temperature of 90 ℃ to obtain the composite nano material.
Example 4
The components are as follows: 0.5 parts of nano-particle Al 2 O 3 1 part of nano TiO particle 2 1.2 parts of a surfactant (the mass ratio of oleic acid, stearic acid and oleylamine is 2.
Wherein, the nano particles Al 2 O 3 Particle diameter of 10 μm, nano-particle TiO 2 Has a particle diameter of 10 μm.
The preparation method comprises the following steps:
dissolving all the components in 40ml of cyclohexane, uniformly stirring, putting the mixture into an ultrasonic oscillation instrument, continuously oscillating for 24 hours at 60 ℃ at a working frequency of 30s stopping every 1min of ultrasonic oscillation, separating the mixed solution after the ultrasonic oscillation by adopting a high-speed centrifuge, setting the rotating speed to 3000rpm for 5min, cleaning the separated solid substance by using deionized water for 3 times, cleaning the solid substance by using absolute ethyl alcohol for 3 times, and drying the cleaned solid substance in a vacuum drying oven at a high temperature of 90 ℃ for 12 hours to obtain the composite nano material.
Comparative example 1
The comparative example differs from example 2 only in that the same amount of Al nanoparticles is used 2 O 3 Substitutional nano-particle TiO 2 。
The preparation method refers to example 2.
Comparative example 2
The comparative example differs from example 2 only in that the same amount of nanoparticulate TiO was used 2 Substitutional nano particle Al 2 O 3 。
The preparation method refers to example 2.
Comparative example 3
Compared with the example 2, the comparative example only differs in that the nano-particle Al is replaced by the same amount of nano-SiC 2 O 3 。
The preparation method refers to example 2.
Comparative example 4
The comparative example differs from example 2 only in that the nanoparticles Al 2 O 3 Has a particle diameter of 30 μm.
The preparation method refers to example 2.
Comparative example 5
The comparative example differs from example 2 only in that the nanoparticulate TiO is 2 The weight portion of the additive is 3 portions.
The preparation method refers to example 2.
Comparative example 6
The components are as follows: 0.25 parts of nano-particle Al 2 O 3 0.75 part of nano TiO particle 2 1.2 parts of a surfactant (the mass ratio of oleic acid, stearic acid and oleylamine is 2.
Wherein, the nano particles Al 2 O 3 Particle diameter of 10 μm, nano-particle TiO 2 Has a particle diameter of 10 μm.
The comparative example differs from example 2 only in that the nanoparticles Al 2 O 3 With nano-particle TiO 2 The mass ratio of (1).
The preparation method refers to example 2.
Performance test
The composite nano-materials prepared in examples 1 to 4 and comparative examples 1 to 6 were added to synthetic ester insulating oil (TMP triester) to prepare composite nano-TMP triester in the following manner.
The preparation method of the composite nano TMP triester comprises the following steps:
the composite nano-materials prepared in examples 1 to 4 and comparative examples 1 to 6 were added to TMP triester at an addition concentration of 0.02g/L, and the mixed oil sample was subjected to ultrasonic oscillation for 1 hour by an ultrasonic dispersion method using 960W as ultrasonic power, and then the oscillated oil sample was placed in a vacuum drying oven and vacuum-dried at 90 ℃ for 48 hours to prepare composite nano-TMP triester.
Testing the heat conduction performance: the thermal conductivity of the composite nano TMP triester was tested using a high precision TC3010 series liquid thermal conductivity meter. In the process of measuring the thermal conductivity of the nano insulating oil, firstly, 25ml of oil sample is placed in a measuring groove of an instrument, the oil sample is heated at the speed of 2 ℃/s through a wire, the test time is within five minutes, the test is repeated for 8 times, and the thermal conductivity coefficients of 25 ℃ and 90 ℃ are obtained through software calculation.
And (3) testing the insulating property: the power frequency breakdown voltage of the oil sample is measured by using an insulating oil dielectric strength tester, so that the improvement capability of the composite nano material on the insulating property of the synthetic ester insulating oil is represented, and the higher the power frequency breakdown voltage is, the better the insulating property of the synthetic ester insulating oil is.
The results of the performance tests for each sample are shown in table 1.
TABLE 1 Heat conduction and Power frequency breakdown Voltage conditions for each sample
As can be seen from the data in Table 1, the composite nanomaterial prepared by the embodiment of the invention can significantly improve the thermal conductivity and the insulating property of the synthetic ester insulating oil, and the composite nanomaterial can be addedThe composite nano synthetic ester insulating oil prepared from the composite nano material has the highest coefficient of heat conductivity at 25 ℃ of 0.184Wm -1 K -1 The highest heat conductivity coefficient at 90 ℃ can reach 0.180Wm -1 K -1 And the highest power frequency breakdown voltage can reach 77.2kV.
Only single nano-particle Al is selected in the composite nano-materials of comparative examples 1-2 2 O 3 Or nano TiO particle 2 The prepared composite nano synthetic ester insulating oil has a thermal conductivity coefficient and a power frequency breakdown voltage lower than those of the embodiment. Single nano Al 2 O 3 The thermal conductivity of the synthetic ester insulating oil is obviously improved, and the breakdown voltage of the synthetic ester insulating oil is improved slightly; single nano TiO 2 2 The breakdown voltage of the synthetic ester insulating oil is obviously improved, and the thermal conductivity of the synthetic ester insulating oil is improved slightly; in comparative example 3, nano SiC which also has the function of improving the heat conductivity of the synthetic ester insulating oil is selected to replace nano Al 2 O 3 The prepared composite nano synthetic ester insulating oil has a thermal conductivity coefficient and a power frequency breakdown voltage lower than those of the embodiment, so that the nano particle Al is shown 2 O 3 With nano-particle TiO 2 The compound use of (2) can generate synergistic effect, and better heat-conducting property and insulating property are realized.
Nano-particle TiO added in comparative example 4 2 Of the particle diameter of comparative example 5 2 The weight parts of the nano-particles are not proper, the probability of nano-particle agglomeration is increased, and the thermal conductivity coefficient and the power frequency breakdown voltage of the prepared composite nano-synthetic ester insulating oil are lower than those of the embodiment; nanoparticle Al added in comparative example 6 2 O 3 With nano-particle TiO 2 The mass ratio of the composite nano synthetic ester insulating oil is not proper, and the thermal conductivity coefficient and the power frequency breakdown voltage of the prepared composite nano synthetic ester insulating oil are lower than those of the embodiment.
The foregoing embodiments are merely illustrative of the principles and utilities of the present invention and are not intended to limit the invention. Any person skilled in the art can modify or change the above-mentioned embodiments without departing from the spirit and scope of the present invention. Accordingly, it is intended that all equivalent modifications or changes which may be made by those skilled in the art without departing from the spirit and scope of the present invention as defined in the appended claims.
Claims (10)
1. The composite nano material is characterized by comprising the following components in parts by weight: 0.3-1 part of nano particle Al 2 O 3 0.3 to 1 portion of nano TiO particle 2 1-3 parts of surfactant and 1-3 parts of polymerization inhibitor.
2. The composite nanomaterial of claim 1, wherein the nanoparticles are Al 2 O 3 With nano-particle TiO 2 The mass ratio of (1): (1-2).
3. The composite nanomaterial of claim 1, wherein the nanoparticles are Al 2 O 3 The particle diameter of (A) is 1 to 20 μm.
4. The composite nanomaterial of claim 1, wherein the nanoparticle TiO is 2 The particle diameter of (A) is 1 to 30 μm.
5. The composite nanomaterial of claim 1, wherein the surfactant comprises oleic acid, stearic acid, and oleylamine.
6. The composite nanomaterial of claim 1, wherein the polymerization inhibitor comprises triethylamine, styrene, and N, N-diethylhydroxylamine.
7. A method for preparing a composite nanomaterial as defined in any of claims 1 to 6, comprising the steps of:
dissolving all the components in a solvent, stirring, performing ultrasonic dispersion, centrifuging, cleaning precipitates obtained by centrifuging, and drying to obtain the composite nano material.
8. The method according to claim 7, comprising at least one of the following (1) to (6):
(1) The solvent is cyclohexane;
(2) The adding amount of the solvent is 6 to 15 times of the total mass of the composite nano material;
(3) The temperature of the ultrasonic dispersion is 40-70 ℃, and the time is 12-36 h;
(4) The rotation speed of the centrifugation is 2500-3000 rpm, and the time is 3-5 min;
(5) The cleaning is to select deionized water and absolute ethyl alcohol to respectively carry out cleaning for 2 to 5 times;
(6) The drying temperature is 80-90 ℃, and the drying time is 10-15 h.
9. Use of a composite nanomaterial as defined in any of claims 1 to 6 in the preparation of a modified synthetic ester insulating oil.
10. A modified synthetic ester insulating oil comprising the composite nanomaterial of any of claims 1 to 6 and a synthetic ester insulating oil, wherein the concentration of the composite nanomaterial in the synthetic ester insulating oil is from 0.01g/L to 0.10g/L.
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