CN113583737A - By using nano SiO2Preparation method of modified palm insulating oil - Google Patents
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Abstract
The invention provides a method for preparing a nano-SiO2Process for the preparation of modified palm insulating oil, SiO2When the nano particles are modified for the first time, removing SiO by dodecyl trimethoxy silane and oleic acid2surface-OH group to modify a large amount of nano SiO2The palm insulating oil is compatible, and the agglomeration phenomenon is reduced; SiO once modified by isobutanol2The nano particles are modified for the second time to further remove SiO2the-OH groups on the surface greatly improve the heat-conducting property and the insulation reliability of the insulating oil; in the second modification of SiO2Adding toluene diphenyl phosphate and alkylphenol polyoxyethylene into nano particles to prepare SiO2The nano particle mixed liquid is mixed with the filtered palm insulating oil, so that the heat conduction performance and the insulation reliability of the insulating oil are greatly improved; the ultrasonic dispersion in the step S5 is carried out for three times, next dispersion is carried out at certain time intervals, and the ultrasonic dispersion is carried out by adopting a mode of combining the interval dispersion and the multiple dispersion, so that the secondary modified SiO can be greatly improved2Thermal conductivity of the nanoparticles.
Description
Technical Field
The invention relates to the technical field of processing of insulating oil, in particular to a method for processing insulating oil by using nano SiO2A preparation method of modified palm insulating oil.
Background
Oil-filled power transformers are critical devices in the safe operation of power grids, and the failure of the oil-filled power transformers interrupts the power supply. The insulation performance of oil-filled transformers is mainly determined by the internal insulation consisting of insulating oil and insulating paper. The insulating oil plays roles of insulation, heat dissipation and cooling, and the guarantee of good operation characteristics of the insulating oil is very important for safe operation of the transformer. The performance of insulating oil is generally required to be 1) the density of the insulating oil is as low as possible so as to facilitate the precipitation of moisture and impurities in the oil; 2) the viscosity is moderate, the convection heat dissipation is influenced if the viscosity is too high, and the flash point is reduced if the viscosity is too low; 3) the flash point is as high as possible and is generally not lower than 136 ℃; 4) the freezing point should be as low as possible; 5) the lower the content of impurities such as acid, alkali, sulfur, ash and the like, the better the impurities are, so as to avoid the corrosion of the impurities on insulating materials, leads, oil tanks and the like as much as possible; 6) the degree of oxidation, usually expressed in acid value, which refers to the amount of potassium hydroxide (mg) required to absorb 1 g of the free acid in the oil, cannot be too high; 7) the stability, which is usually expressed as a precipitate in the acid value test, represents the resistance of the oil to ageing, should not be too low.
Palm oil is used as a novel breakdown-resistant, high-ignition-point and environment-friendly liquid dielectric medium and is used as transformer insulating oil. However, palm insulating oil has weak heat conductivity and is liable to cause local overheating of the transformer to cause failure, thereby limiting its application to large-sized power transformers. In view of this, the development of a high thermal conductivity palm insulating oil has important practical value. Nano SiO2The particles have excellent insulating property and heat conducting property, and the preparation method is mature, so that the particles are widely applied to preparing electric insulating materials. Nano SiO2The particles can be uniformly dispersed in the palm insulating oil, and therefore, the present invention uses the palm insulating oil and SiO2Nano SiO with high heat conductivity is prepared by using nano granules as raw material2Modified palm insulating oil.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide the utilization nanometer SiO with higher thermal conductivity than the traditional plant insulating oil, good long-term stability and high insulating reliability2A preparation method of modified palm insulating oil.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows: by using nano SiO2The preparation method of the modified palm insulating oil comprises the following steps:
step S1, adding SiO in the ball mill2Adding dodecyl trimethoxy silane into the nano particles, heating, mixing and ball-milling to obtain a mixture; the addition amount of the dodecyl trimethoxy silane is SiO25-15% of the weight of the nano particles;
step S2, adding oleic acid into the mixture obtained in the step S1, then continuing to heat up, stirring, then ultrasonically oscillating, and finally adding ethanol for washing to obtain the mixture containing SiO2A washing solution of nanoparticles;
step S3, filtering the SiO-containing material obtained in step S22Washing the nano particles, drying to obtain the primary modified SiO2Nanoparticles;
step S4, modifying the primary modified SiO obtained in step S32Uniformly mixing the nano particles with absolute ethyl alcohol, adding isobutanol, and uniformly stirring to obtain a mixed solution; the addition amount of the isobutanol is SiO subjected to primary modification235 to 45 percent of the weight of the nano particles;
step S5, the mixed solution obtained in the step S4 is subjected to ultrasonic dispersion and stirring at the temperature of 40-45 ℃ to obtain ultrasonic dispersion liquid(ii) a Centrifugally separating the ultrasonic dispersion, drying and grinding into powder to obtain the secondarily modified SiO2Nanoparticles;
step S6, the twice modified SiO obtained in step S52The nano particles, diphenyl cresylphosphate and alkylphenol polyoxyethylene ether are uniformly subjected to ultrasonic oscillation to obtain SiO2Mixing the nano particle liquid; the addition amount of the cresyl diphenyl phosphate is SiO subjected to secondary modification235 to 45 percent of the weight of the nano particles; the addition amount of the alkylphenol polyoxyethylene ether is SiO subjected to secondary modification225-35% of the weight of the nanoparticles;
step S7, filtering the palm insulating oil in vacuum, heating and mechanically stirring to obtain filtered palm insulating oil;
step S8, SiO obtained in step S62Adding the nano particle mixed solution, an antioxidant and a metal passivator into the filtered palm insulating oil, performing ultrasonic oscillation and vacuum drying to obtain the nano SiO2A modified palm insulating oil; the SiO2The addition amount of the nano particle mixed liquid is 0.025-0.150% of the weight of the filtered palm insulating oil, the addition amount of the antioxidant is 0.01-0.03% of the weight of the filtered palm insulating oil, and the addition amount of the metal deactivator is 0.01-0.05% of the weight of the filtered palm insulating oil.
Further, in the step S1, the temperature in the ball mill is controlled to be 60-65 ℃, and the ball milling time is 1.8-2.2 h.
Further, in the step S2, oleic acid is added into the mixture obtained in the step S1, then the temperature is continuously increased to 70-75 ℃, stirring is carried out, and then ultrasonic oscillation is carried out, wherein the ultrasonic frequency of an ultrasonic oscillation generator is 35-40 KHz, and the ultrasonic oscillation time is 1.2-1.6 hours; finally adding ethanol for washing to obtain the SiO-containing2A washing solution of nanoparticles.
Further, in the step S3, the SiO-containing material obtained in the step S2 is filtered2Drying the nano particle washing liquid in a vacuum drying oven at the vacuum degree of-0.06 MPa and the drying temperature of 80-85 ℃ to obtain the primary modified SiO2Nanoparticles.
Further, in the step S4The primary modified SiO obtained in step S32Uniformly mixing the nano particles and absolute ethyl alcohol, adding isobutanol, and uniformly stirring at the stirring speed of 200-250 r/min for 35-40 min to obtain a mixed solution; the addition amount of the isobutanol is SiO subjected to primary modification235 to 45 percent of the weight of the nano particles.
Further, in the step S5, the mixed solution obtained in the step S4 is subjected to ultrasonic dispersion and stirring at 40 to 45 ℃ to obtain an ultrasonic dispersion solution; during ultrasonic dispersion, the ultrasonic frequency of the ultrasonic oscillation generator is 35-38 KHz, and ultrasonic dispersion is carried out for three times, wherein each time is 25-30 min, and each time is 15 min; centrifugally separating the ultrasonic dispersion, drying in a vacuum drying oven, and grinding into powder to obtain the secondarily modified SiO2Nanoparticles.
Further, in the step S6, the twice modified SiO obtained in the step S52The nano particles, diphenyl cresyl phosphate and alkylphenol polyoxyethylene ether are subjected to ultrasonic oscillation uniformly, the ultrasonic frequency of an ultrasonic oscillation generator is 35-38 KHz, and the ultrasonic oscillation time is as follows: obtaining SiO in 45-55 min2Mixing the nano particle liquid; the addition amount of the cresyl diphenyl phosphate is SiO subjected to secondary modification235 to 45 percent of the weight of the nano particles; the addition amount of the alkylphenol polyoxyethylene ether is SiO subjected to secondary modification225-35% of the weight of the nano particles.
Further, in the step S7, the palm insulating oil is subjected to vacuum filtration, heated to 65-70 ℃, mechanically stirred at the stirring speed of 150-200 r/min for 40-45 min, and the filtered palm insulating oil is obtained.
Further, the antioxidant in step S8 is selected from one or more of 2, 6-tri-tert-butyl-4-methylphenol, 2, 6-di-tert-butylphenol, and 2, 6-di-tert-butyl-p-cresol.
Further, the metal passivator in step S8 is 2-methyl-benzotriazole.
The invention relates to a method for preparing a nano-SiO2Process for the preparation of modified palm insulating oil, SiO2When the nano particles are modified for the first time, dodecyl trimethoxy silane and dodecyl trimethoxy silane are addedOleic acid SiO removal2surface-OH group to modify a large amount of nano SiO2The palm oil is compatible with palm insulating oil, and all raw materials are uniformly dispersed, so that the agglomeration phenomenon is reduced; SiO once modified by isobutanol2The nano particles are modified for the second time to further remove SiO2the-OH groups on the surface reduce the agglomeration phenomenon and greatly improve the heat conduction performance and the insulation reliability of the insulating oil; in the second modification of SiO2Adding toluene diphenyl phosphate and alkylphenol polyoxyethylene into nano particles to prepare SiO2The nano particle mixed liquid is mixed with the filtered palm insulating oil, so that the heat conduction performance and the insulation reliability of the insulating oil can be greatly improved; nano SiO2Compared with unmodified insulating oil, the nano SiO prepared by the invention2The modified palm insulating oil has higher heat conductivity coefficient, and improves the insulating reliability.
The invention relates to a method for preparing a nano-SiO2The preparation method of the modified palm insulating oil comprises the steps of carrying out ultrasonic dispersion for three times in the step S5, carrying out next-time dispersion at certain intervals, carrying out ultrasonic dispersion in a mode of combining interval dispersion and multi-time dispersion, achieving a better ultrasonic dispersion effect, and greatly improving the secondary modified SiO2Thermal conductivity of the nanoparticles.
Detailed Description
The following examples may help one skilled in the art to more fully understand the present invention, but are not intended to limit the invention in any way.
The invention relates to a method for preparing a nano-SiO2The preparation method of the modified palm insulating oil adopts vegetable insulating oil as a main raw material, and specifically adopts the vegetable insulating oil as the palm oil;
the invention relates to a method for preparing a nano-SiO2The preparation method of the modified palm insulating oil comprises the following steps of (1) preparing a mixture of ethanol with the volume percentage of more than 99.5% by using absolute ethanol; the used reagents such as dodecyl trimethoxy silane, isobutyl alcohol, diphenyl cresyl phosphate, vinyl trimethoxy silane, alkylphenol ethoxylates and the like are all chemically pure;
the invention relates to a method for preparing a nano-SiO2The preparation method of the modified palm insulating oil comprises the steps that an instrument used for ultrasonic dispersion is a Wu Ji Reian JRA-1000MF type constant-temperature closed ultrasonic reactor; the vacuum drying apparatus is a vacuum drying oven with a vacuum pump;
the invention relates to a method for preparing a nano-SiO2Process for the preparation of modified palm insulating oil, SiO as used in step (1) of the examples below2The weight of the nanoparticles was 10 grams.
Example 1
By using nano SiO2The preparation method of the modified palm insulating oil comprises the following steps:
step S1, adding SiO in the ball mill2Adding dodecyl trimethoxy silane into the nano particles, heating, mixing and ball-milling, controlling the temperature in a ball mill to be 60 ℃, and ball-milling for 1.8 hours to obtain a mixture; the addition amount of the dodecyl trimethoxy silane is SiO25% of the weight of the nanoparticles;
step S2, adding oleic acid into the mixture obtained in the step S1, then continuing to heat to 70 ℃, stirring, and then ultrasonically oscillating, wherein the ultrasonic frequency of an ultrasonic oscillation generator is 35KHz, and the ultrasonic oscillation time is 1.2 h; finally adding ethanol for washing for more than three times to obtain the SiO-containing solution2A washing solution of nanoparticles;
step S3, filtering the SiO-containing material obtained in step S22The washing liquid of the nano particles is put in a vacuum drying oven for drying, the vacuum degree is-0.06 MPa, the drying temperature is 80 ℃, and the primary modified SiO is obtained2Nanoparticles;
step S4, modifying the primary modified SiO obtained in step S32Uniformly mixing the nano particles and absolute ethyl alcohol, adding isobutanol, and uniformly stirring at the stirring speed of 200r/min for 35min to obtain a mixed solution; the addition amount of the isobutanol is SiO subjected to primary modification235% of the weight of the nanoparticles;
step S5, performing ultrasonic dispersion and stirring on the mixed solution obtained in the step S4 at 40 ℃ to obtain an ultrasonic dispersion solution; during ultrasonic dispersion, the ultrasonic frequency of the ultrasonic oscillation generator is 35KHz, and the ultrasonic dispersion is carried out three times, each time for 25min, and each time interval15 min; centrifugally separating the ultrasonic dispersion, drying and grinding into powder to obtain the secondarily modified SiO2Nanoparticles;
step S6, the twice modified SiO obtained in step S52The nano particles, diphenyl cresyl phosphate and alkylphenol polyoxyethylene ether are subjected to ultrasonic oscillation uniformly, the ultrasonic frequency of an ultrasonic oscillation generator is 35KHz, and the ultrasonic oscillation time is as follows: for 45min, obtaining SiO2Mixing the nano particle liquid; the addition amount of the cresyl diphenyl phosphate is SiO subjected to secondary modification235% of the weight of the nanoparticles; the addition amount of the alkylphenol polyoxyethylene ether is SiO subjected to secondary modification225% of the weight of the nanoparticles;
step S7, filtering the palm insulating oil in vacuum, heating to 65 ℃, and mechanically stirring at the stirring speed of 150r/min for 40min to obtain filtered palm insulating oil;
step S8, SiO obtained in step S62Adding the nano particle mixed solution, an antioxidant and a metal passivator into the filtered palm insulating oil, performing ultrasonic oscillation and vacuum drying to obtain the nano SiO2A modified palm insulating oil; the SiO2The addition amount of the nano particle mixed liquid is 0.025% of the weight of the filtered palm insulating oil, the addition amount of the antioxidant is 0.01% of the weight of the filtered palm insulating oil, and the addition amount of the metal deactivator is 0.01% of the weight of the filtered palm insulating oil; the antioxidant is 2, 6-tri-tert-butyl-4-methylphenol, and the metal passivator is 2-methyl-benzotriazole.
Example 2
By using nano SiO2The preparation method of the modified palm insulating oil comprises the following steps:
step S1, adding SiO in the ball mill2Adding dodecyl trimethoxy silane into the nano particles, heating, mixing and ball-milling, controlling the temperature in a ball mill to be 65 ℃, and ball-milling for 2.2 hours to obtain a mixture; the addition amount of the dodecyl trimethoxy silane is SiO215% of the weight of the nanoparticles;
step S2, adding oleic acid into the mixture obtained in step S1, and then continuing to heat to 75 DEG CStirring, and then ultrasonically oscillating, wherein the ultrasonic frequency of an ultrasonic oscillation generator is 40KHz, and the ultrasonic oscillation time is 1.6 h; finally adding ethanol for washing for more than three times to obtain the SiO-containing solution2A washing solution of nanoparticles;
step S3, filtering the SiO-containing material obtained in step S22The washing liquid of the nano particles is placed in a vacuum drying oven for drying, the vacuum degree is-0.06 MPa, the drying temperature is 85 ℃, and the primary modified SiO is obtained2Nanoparticles;
step S4, modifying the primary modified SiO obtained in step S32Uniformly mixing the nano particles and absolute ethyl alcohol, adding isobutanol, and uniformly stirring at the stirring speed of 250r/min for 40min to obtain a mixed solution; the addition amount of the isobutanol is SiO subjected to primary modification245% of the weight of the nanoparticles;
step S5, performing ultrasonic dispersion and stirring on the mixed solution obtained in the step S4 at 45 ℃ to obtain an ultrasonic dispersion solution; during ultrasonic dispersion, the ultrasonic frequency of the ultrasonic oscillation generator is 38KHz, and ultrasonic dispersion is carried out for three times, each time is 30min, and each time interval is 15 min; centrifugally separating the ultrasonic dispersion, drying and grinding into powder to obtain the secondarily modified SiO2Nanoparticles;
step S6, the twice modified SiO obtained in step S52The nano particles, diphenyl cresyl phosphate and alkylphenol polyoxyethylene ether are subjected to ultrasonic oscillation uniformly, the ultrasonic frequency of an ultrasonic oscillation generator is 38KHz, and the ultrasonic oscillation time is as follows: 55min to obtain SiO2Mixing the nano particle liquid; the addition amount of the cresyl diphenyl phosphate is SiO subjected to secondary modification245% of the weight of the nanoparticles; the addition amount of the alkylphenol polyoxyethylene ether is SiO subjected to secondary modification235% of the weight of the nanoparticles;
step S7, filtering the palm insulating oil in vacuum, heating to 70 ℃, and mechanically stirring at the stirring speed of 200r/min for 45min to obtain filtered palm insulating oil;
step S8, SiO obtained in step S62Adding the mixed solution of the nano particles, the antioxidant and the metal passivator into the filtered palm insulating oil, ultrasonically oscillating and vacuum dryingTo obtain the nano SiO2A modified palm insulating oil; the SiO2The addition amount of the nano particle mixed liquid is 0.150% of the weight of the filtered palm insulating oil, the addition amount of the antioxidant is 0.03% of the weight of the filtered palm insulating oil, and the addition amount of the metal deactivator is 0.05% of the weight of the filtered palm insulating oil; the antioxidant is 2, 6-di-tert-butylphenol, and the metal passivator is 2-methyl-benzotriazole.
Example 3
By using nano SiO2The preparation method of the modified palm insulating oil comprises the following steps:
step S1, adding SiO in the ball mill2Adding dodecyl trimethoxy silane into the nano particles, heating, mixing and ball-milling, controlling the temperature in a ball mill to be 62 ℃, and ball-milling for 2 hours to obtain a mixture; the addition amount of the dodecyl trimethoxy silane is SiO210% of the weight of the nanoparticles;
step S2, adding oleic acid into the mixture obtained in the step S1, then continuing to heat to 72 ℃, stirring, and then ultrasonically oscillating, wherein the ultrasonic frequency of an ultrasonic oscillation generator is 38KHz, and the ultrasonic oscillation time is 1.4 h; finally adding ethanol for washing for more than three times to obtain the SiO-containing solution2A washing solution of nanoparticles;
step S3, filtering the SiO-containing material obtained in step S22The washing liquid of the nano particles is placed in a vacuum drying oven for drying, the vacuum degree is-0.06 MPa, the drying temperature is 82 ℃, and the primary modified SiO is obtained2Nanoparticles;
step S4, modifying the primary modified SiO obtained in step S32Uniformly mixing the nano particles and absolute ethyl alcohol, adding isobutanol, and uniformly stirring at the stirring speed of 220r/min for 38min to obtain a mixed solution; the addition amount of the isobutanol is SiO subjected to primary modification240% of the weight of the nanoparticles;
step S5, performing ultrasonic dispersion and stirring on the mixed solution obtained in the step S4 at 42 ℃ to obtain an ultrasonic dispersion solution; centrifugally separating the ultrasonic dispersion, drying and grinding into powder to obtain the secondarily modified SiO2Nanoparticles;
step S6, the twice modified SiO obtained in step S52The nano particles, diphenyl cresyl phosphate and alkylphenol polyoxyethylene ether are subjected to ultrasonic oscillation uniformly, the ultrasonic frequency of an ultrasonic oscillation generator is 36KHz, and the ultrasonic oscillation time is as follows: 50min to obtain SiO2Mixing the nano particle liquid; the addition amount of the cresyl diphenyl phosphate is SiO subjected to secondary modification240% of the weight of the nanoparticles; the addition amount of the alkylphenol polyoxyethylene ether is SiO subjected to secondary modification230% of the weight of the nanoparticles;
step S7, filtering the palm insulating oil in vacuum, heating to 68 ℃, and mechanically stirring at the stirring speed of 180r/min for 42min to obtain filtered palm insulating oil;
step S8, SiO obtained in step S62Adding the nano particle mixed solution, an antioxidant and a metal passivator into the filtered palm insulating oil, performing ultrasonic oscillation and vacuum drying to obtain the nano SiO2A modified palm insulating oil; the SiO2The addition amount of the nano particle mixed liquid is 0.085% of the weight of the filtered palm insulating oil, the addition amount of the antioxidant is 0.02% of the weight of the filtered palm insulating oil, and the addition amount of the metal deactivator is 0.03% of the weight of the filtered palm insulating oil; the antioxidant is 2, 6-di-tert-butyl-p-cresol, and the metal passivator is 2-methyl-benzotriazole.
Example 4
By using nano SiO2The preparation method of the modified palm insulating oil comprises the following steps:
step S1, adding SiO in the ball mill2Adding dodecyl trimethoxy silane into the nano particles, heating, mixing and ball-milling, controlling the temperature in a ball mill to be 62 ℃, and ball-milling for 2 hours to obtain a mixture; the addition amount of the dodecyl trimethoxy silane is SiO210% of the weight of the nanoparticles;
step S2, adding oleic acid into the mixture obtained in the step S1, then continuing to heat to 72 ℃, stirring, and then ultrasonically oscillating, wherein the ultrasonic frequency of an ultrasonic oscillation generator is 38KHz, and the ultrasonic oscillation time is 1.4 h; finally, theAdding ethanol for washing for more than three times to obtain the SiO-containing solution2A washing solution of nanoparticles;
step S3, filtering the SiO-containing material obtained in step S22The washing liquid of the nano particles is placed in a vacuum drying oven for drying, the vacuum degree is-0.06 MPa, the drying temperature is 82 ℃, and the primary modified SiO is obtained2Nanoparticles;
step S4, modifying the primary modified SiO obtained in step S32Uniformly mixing the nano particles and absolute ethyl alcohol, adding isobutanol, and uniformly stirring at the stirring speed of 220r/min for 38min to obtain a mixed solution; the addition amount of the isobutanol is SiO subjected to primary modification240% of the weight of the nanoparticles;
step S5, performing ultrasonic dispersion and stirring on the mixed solution obtained in the step S4 at 42 ℃ to obtain an ultrasonic dispersion solution; during ultrasonic dispersion, the ultrasonic frequency of the ultrasonic oscillation generator is 36KHz, and ultrasonic dispersion is carried out for three times, each time is 28min, and each time interval is 15 min; centrifugally separating the ultrasonic dispersion, drying and grinding into powder to obtain the secondarily modified SiO2Nanoparticles;
step S6, the twice modified SiO obtained in step S52The nano particles, diphenyl cresyl phosphate and alkylphenol polyoxyethylene ether are subjected to ultrasonic oscillation uniformly, the ultrasonic frequency of an ultrasonic oscillation generator is 36KHz, and the ultrasonic oscillation time is as follows: 50min to obtain SiO2Mixing the nano particle liquid; the addition amount of the cresyl diphenyl phosphate is SiO subjected to secondary modification240% of the weight of the nanoparticles; the addition amount of the alkylphenol polyoxyethylene ether is SiO subjected to secondary modification230% of the weight of the nanoparticles;
step S7, filtering the palm insulating oil in vacuum, heating to 68 ℃, and mechanically stirring at the stirring speed of 180r/min for 42min to obtain filtered palm insulating oil;
step S8, SiO obtained in step S62Adding the nano particle mixed solution, an antioxidant and a metal passivator into the filtered palm insulating oil, performing ultrasonic oscillation and vacuum drying to obtain the nano SiO2A modified palm insulating oil; the SiO2Addition of nanoparticle mixtureThe amount of the antioxidant is 0.085% of the weight of the filtered palm insulating oil, the addition amount of the antioxidant is 0.02% of the weight of the filtered palm insulating oil, and the addition amount of the metal deactivator is 0.03% of the weight of the filtered palm insulating oil; the antioxidant is 2, 6-di-tert-butyl-p-cresol, and the metal passivator is 2-methyl-benzotriazole.
Comparative example 1
By using nano SiO2The preparation method of the modified palm insulating oil comprises the following steps:
step S1, adding SiO in the ball mill2Adding dodecyl trimethoxy silane into the nano particles, heating, mixing and ball-milling, controlling the temperature in a ball mill to be 62 ℃, and ball-milling for 2 hours to obtain a mixture; the addition amount of the dodecyl trimethoxy silane is SiO210% of the weight of the nanoparticles;
step S2, adding oleic acid into the mixture obtained in the step S1, then continuing to heat to 72 ℃, stirring, and then ultrasonically oscillating, wherein the ultrasonic frequency of an ultrasonic oscillation generator is 38KHz, and the ultrasonic oscillation time is 1.4 h; finally adding ethanol for washing for more than three times to obtain the SiO-containing solution2A washing solution of nanoparticles;
step S3, filtering the SiO-containing material obtained in step S22The washing liquid of the nano particles is placed in a vacuum drying oven for drying, the vacuum degree is-0.06 MPa, the drying temperature is 82 ℃, and the primary modified SiO is obtained2Nanoparticles;
step S4, modifying the primary modified SiO obtained in step S32The nano particles, diphenyl cresyl phosphate and alkylphenol polyoxyethylene ether are subjected to ultrasonic oscillation uniformly, the ultrasonic frequency of an ultrasonic oscillation generator is 36KHz, and the ultrasonic oscillation time is as follows: 50min to obtain SiO2Mixing the nano particle liquid; the addition amount of the cresyl diphenyl phosphate is SiO subjected to primary modification240% of the weight of the nanoparticles; the addition amount of the alkylphenol polyoxyethylene is SiO modified for one time230% of the weight of the nanoparticles;
step S5, filtering the palm insulating oil in vacuum, heating to 68 ℃, and mechanically stirring at the stirring speed of 180r/min for 42min to obtain filtered palm insulating oil;
step S6, SiO obtained in step S42Adding the nano particle mixed solution, an antioxidant and a metal passivator into the filtered palm insulating oil, performing ultrasonic oscillation and vacuum drying to obtain the nano SiO2A modified palm insulating oil; the SiO2The addition amount of the nano particle mixed liquid is 0.085% of the weight of the filtered palm insulating oil, the addition amount of the antioxidant is 0.02% of the weight of the filtered palm insulating oil, and the addition amount of the metal deactivator is 0.03% of the weight of the filtered palm insulating oil; the antioxidant is 2, 6-di-tert-butyl-p-cresol, and the metal passivator is 2-methyl-benzotriazole.
Comparative example 2
By using nano SiO2The preparation method of the modified palm insulating oil comprises the following steps:
step S1, mixing SiO2Uniformly mixing the nano particles and absolute ethyl alcohol, adding isobutanol, and uniformly stirring at the stirring speed of 220r/min for 38min to obtain a mixed solution; the addition amount of the isobutanol is SiO240% of the weight of the nanoparticles;
step S2, performing ultrasonic dispersion and stirring on the mixed solution obtained in the step S1 at 42 ℃ to obtain an ultrasonic dispersion solution; during ultrasonic dispersion, the ultrasonic frequency of the ultrasonic oscillation generator is 36KHz, and ultrasonic dispersion is carried out for three times, each time is 28min, and each time interval is 15 min; centrifugally separating the ultrasonic dispersion, drying and grinding into powder to obtain the primary modified SiO2Nanoparticles;
step S3, modifying the primary modified SiO obtained in step S22The nano particles, diphenyl cresyl phosphate and alkylphenol polyoxyethylene ether are subjected to ultrasonic oscillation uniformly, the ultrasonic frequency of an ultrasonic oscillation generator is 36KHz, and the ultrasonic oscillation time is as follows: 50min to obtain SiO2Mixing the nano particle liquid; the addition amount of the cresyl diphenyl phosphate is SiO subjected to primary modification240% of the weight of the nanoparticles; the addition amount of the alkylphenol polyoxyethylene is SiO modified for one time230% of the weight of the nanoparticles;
step S4, filtering the palm insulating oil in vacuum, heating to 68 ℃, and mechanically stirring at the stirring speed of 180r/min for 42min to obtain filtered palm insulating oil;
step S5, SiO obtained in step S32Adding the nano particle mixed solution, an antioxidant and a metal passivator into the filtered palm insulating oil, performing ultrasonic oscillation and vacuum drying to obtain the nano SiO2A modified palm insulating oil; the SiO2The addition amount of the nano particle mixed liquid is 0.085% of the weight of the filtered palm insulating oil, the addition amount of the antioxidant is 0.02% of the weight of the filtered palm insulating oil, and the addition amount of the metal deactivator is 0.03% of the weight of the filtered palm insulating oil; the antioxidant is 2, 6-di-tert-butyl-p-cresol, and the metal passivator is 2-methyl-benzotriazole.
Comparative example 3
By using nano SiO2The preparation method of the modified palm insulating oil comprises the following steps:
step S1, adding SiO in the ball mill2Adding dodecyl trimethoxy silane into the nano particles, heating, mixing and ball-milling, controlling the temperature in a ball mill to be 62 ℃, and ball-milling for 2 hours to obtain a mixture; the addition amount of the dodecyl trimethoxy silane is SiO210% of the weight of the nanoparticles;
step S2, adding oleic acid into the mixture obtained in the step S1, then continuing to heat to 72 ℃, stirring, and then ultrasonically oscillating, wherein the ultrasonic frequency of an ultrasonic oscillation generator is 38KHz, and the ultrasonic oscillation time is 1.4 h; finally adding ethanol for washing for more than three times to obtain the SiO-containing solution2A washing solution of nanoparticles;
step S3, filtering the SiO-containing material obtained in step S22The washing liquid of the nano particles is placed in a vacuum drying oven for drying, the vacuum degree is-0.06 MPa, the drying temperature is 82 ℃, and the primary modified SiO is obtained2Nanoparticles;
step S4, modifying the primary modified SiO obtained in step S32Uniformly mixing the nano particles and absolute ethyl alcohol, adding isobutanol, and uniformly stirring at the stirring speed of 220r/min for 38min to obtain a mixed solution; the addition amount of the isobutanol is primary modificationSiO of (2)240% of the weight of the nanoparticles;
step S5, performing ultrasonic dispersion and stirring on the mixed solution obtained in the step S4 at 42 ℃ to obtain an ultrasonic dispersion solution; during ultrasonic dispersion, the ultrasonic frequency of the ultrasonic oscillation generator is 36KHz, and ultrasonic dispersion is carried out for three times, each time is 28min, and each time interval is 15 min; centrifugally separating the ultrasonic dispersion, drying and grinding into powder to obtain the secondarily modified SiO2Nanoparticles;
step S6, the twice modified SiO obtained in step S52The nano particles and the diphenyl cresyl phosphate are subjected to uniform ultrasonic oscillation, the ultrasonic frequency of an ultrasonic oscillation generator is 36KHz, and the ultrasonic oscillation time is as follows: 50min to obtain SiO2Mixing the nano particle liquid; the addition amount of the cresyl diphenyl phosphate is SiO subjected to secondary modification240% of the weight of the nanoparticles;
step S7, filtering the palm insulating oil in vacuum, heating to 68 ℃, and mechanically stirring at the stirring speed of 180r/min for 42min to obtain filtered palm insulating oil;
step S8, SiO obtained in step S62Adding the nano particle mixed solution, an antioxidant and a metal passivator into the filtered palm insulating oil, performing ultrasonic oscillation and vacuum drying to obtain the nano SiO2A modified palm insulating oil; the SiO2The addition amount of the nano particle mixed liquid is 0.085% of the weight of the filtered palm insulating oil, the addition amount of the antioxidant is 0.02% of the weight of the filtered palm insulating oil, and the addition amount of the metal deactivator is 0.03% of the weight of the filtered palm insulating oil; the antioxidant is 2, 6-di-tert-butyl-p-cresol, and the metal passivator is 2-methyl-benzotriazole.
Comparative example 4
By using nano SiO2The preparation method of the modified palm insulating oil comprises the following steps:
step S1, adding SiO in the ball mill2Adding dodecyl trimethoxy silane into the nano particles, heating, mixing and ball-milling, controlling the temperature in a ball mill to be 62 ℃, and ball-milling for 2 hours to obtain a mixture; addition of the said dodecyl trimethoxy silaneIn an amount of SiO210% of the weight of the nanoparticles;
step S2, adding oleic acid into the mixture obtained in the step S1, then continuing to heat to 72 ℃, stirring, and then ultrasonically oscillating, wherein the ultrasonic frequency of an ultrasonic oscillation generator is 38KHz, and the ultrasonic oscillation time is 1.4 h; finally adding ethanol for washing for more than three times to obtain the SiO-containing solution2A washing solution of nanoparticles;
step S3, filtering the SiO-containing material obtained in step S22The washing liquid of the nano particles is placed in a vacuum drying oven for drying, the vacuum degree is-0.06 MPa, the drying temperature is 82 ℃, and the primary modified SiO is obtained2Nanoparticles;
step S4, modifying the primary modified SiO obtained in step S32Uniformly mixing the nano particles and absolute ethyl alcohol, adding isobutanol, and uniformly stirring at the stirring speed of 220r/min for 38min to obtain a mixed solution; the addition amount of the isobutanol is SiO subjected to primary modification240% of the weight of the nanoparticles;
step S5, performing ultrasonic dispersion and stirring on the mixed solution obtained in the step S4 at 42 ℃ to obtain an ultrasonic dispersion solution; during ultrasonic dispersion, the ultrasonic frequency of the ultrasonic oscillation generator is 36KHz, and ultrasonic dispersion is carried out for three times, each time is 28min, and each time interval is 15 min; centrifugally separating the ultrasonic dispersion, drying and grinding into powder to obtain the secondarily modified SiO2Nanoparticles;
step S6, the twice modified SiO obtained in step S52The nano particles and alkylphenol ethoxylates are subjected to ultrasonic oscillation uniformly, the ultrasonic frequency of an ultrasonic oscillation generator is 36KHz, and the ultrasonic oscillation time is as follows: 50min to obtain SiO2Mixing the nano particle liquid; the addition amount of the alkylphenol polyoxyethylene ether is SiO subjected to secondary modification230% of the weight of the nanoparticles;
step S7, filtering the palm insulating oil in vacuum, heating to 68 ℃, and mechanically stirring at the stirring speed of 180r/min for 42min to obtain filtered palm insulating oil;
step S8, SiO obtained in step S62Adding the mixed solution of nano particles, antioxidant and metal deactivator into the filtered palmIn insulating oil, ultrasonic oscillation and vacuum drying are carried out to obtain the nano SiO2A modified palm insulating oil; the SiO2The addition amount of the nano particle mixed liquid is 0.085% of the weight of the filtered palm insulating oil, the addition amount of the antioxidant is 0.02% of the weight of the filtered palm insulating oil, and the addition amount of the metal deactivator is 0.03% of the weight of the filtered palm insulating oil; the antioxidant is 2, 6-di-tert-butyl-p-cresol, and the metal passivator is 2-methyl-benzotriazole.
Verification of the Nano SiO prepared in examples 1-4 and comparative examples 1-42The properties of the modified palm insulating oil are as follows:
firstly, detecting the nano SiO prepared in examples 1-4 and comparative examples 1-42The breakdown voltage of the modified palm insulating oil is measured by a voltage breakdown tester;
secondly, detecting the nano SiO prepared in the examples 1 to 4 and the comparative examples 1 to 42Measuring the thermal conductivity coefficient of the modified palm insulating oil by adopting a hot wire method;
the test results of examples 1 to 4 and comparative examples 1 to 4 are shown in the following tables 1 to 2.
TABLE 1
TABLE 2
According to the detection results, the invention utilizes the nano SiO2Process for the preparation of modified palm insulating oil, SiO2When the nano particles are modified for the first time, removing SiO by dodecyl trimethoxy silane and oleic acid2surface-OH group to modify a large amount of nano SiO2The palm oil is compatible with palm insulating oil, and all raw materials are uniformly dispersed, so that the agglomeration phenomenon is reduced; SiO once modified by isobutanol2The nano particles are secondarily modified to further removeSiO2the-OH groups on the surface reduce the agglomeration phenomenon and greatly improve the heat conduction performance and the insulation reliability of the insulating oil; in the second modification of SiO2Adding toluene diphenyl phosphate and alkylphenol polyoxyethylene into nano particles to prepare SiO2The nano particle mixed liquid is mixed with the filtered palm insulating oil, so that the heat conduction performance and the insulation reliability of the insulating oil can be greatly improved; the ultrasonic dispersion in the step S5 is carried out for three times, next dispersion is carried out at certain time intervals, the ultrasonic dispersion is carried out in a mode of combining the interval dispersion and the multiple dispersion, the ultrasonic dispersion effect is better, and the secondary modified SiO can be greatly improved2Thermal conductivity of the nanoparticles.
Although the invention has been described in detail hereinabove with respect to a general description and specific embodiments thereof, it will be apparent to those skilled in the art that modifications or improvements may be made thereto based on the invention. Accordingly, such modifications and improvements are intended to be within the scope of the invention as claimed.
Claims (10)
1. By using nano SiO2The preparation method of the modified palm insulating oil is characterized by comprising the following steps:
step S1, adding SiO in the ball mill2Adding dodecyl trimethoxy silane into the nano particles, heating, mixing and ball-milling to obtain a mixture; the addition amount of the dodecyl trimethoxy silane is SiO25-15% of the weight of the nano particles;
step S2, adding oleic acid into the mixture obtained in the step S1, then continuing to heat up, stirring, then ultrasonically oscillating, and finally adding ethanol for washing to obtain the mixture containing SiO2A washing solution of nanoparticles;
step S3, filtering the SiO-containing material obtained in step S22Washing the nano particles, drying to obtain the primary modified SiO2Nanoparticles;
step S4, modifying the primary modified SiO obtained in step S32Mixing the nanoparticles with anhydrous ethanol, and adding isobutanolStirring the alcohol uniformly to obtain a mixed solution; the addition amount of the isobutanol is SiO subjected to primary modification235 to 45 percent of the weight of the nano particles;
step S5, performing ultrasonic dispersion and stirring on the mixed solution obtained in the step S4 at the temperature of 40-45 ℃ to obtain an ultrasonic dispersion solution; centrifugally separating the ultrasonic dispersion, drying and grinding into powder to obtain the secondarily modified SiO2Nanoparticles;
step S6, the twice modified SiO obtained in step S52The nano particles, diphenyl cresylphosphate and alkylphenol polyoxyethylene ether are uniformly subjected to ultrasonic oscillation to obtain SiO2Mixing the nano particle liquid; the addition amount of the cresyl diphenyl phosphate is SiO subjected to secondary modification235 to 45 percent of the weight of the nano particles; the addition amount of the alkylphenol polyoxyethylene ether is SiO subjected to secondary modification225-35% of the weight of the nanoparticles;
step S7, filtering the palm insulating oil in vacuum, heating and mechanically stirring to obtain filtered palm insulating oil;
step S8, SiO obtained in step S62Adding the nano particle mixed solution, an antioxidant and a metal passivator into the filtered palm insulating oil, performing ultrasonic oscillation and vacuum drying to obtain the nano SiO2A modified palm insulating oil; the SiO2The addition amount of the nano particle mixed liquid is 0.025-0.150% of the weight of the filtered palm insulating oil, the addition amount of the antioxidant is 0.01-0.03% of the weight of the filtered palm insulating oil, and the addition amount of the metal deactivator is 0.01-0.05% of the weight of the filtered palm insulating oil.
2. The method of claim 1, wherein the SiO nanoparticles are used2The preparation method of the modified palm insulating oil is characterized in that in the step S1, the temperature in the ball mill is controlled to be 60-65 ℃, and the ball milling time is 1.8-2.2 hours.
3. The method of claim 1, wherein the SiO nanoparticles are used2A method for producing a modified palm insulating oil, characterized in that, in step S2, the palm insulating oil obtained in step S1Adding oleic acid into the mixture, then continuously heating to 70-75 ℃, stirring, and then ultrasonically oscillating, wherein the ultrasonic frequency of an ultrasonic oscillation generator is 35-40 KHz, and the ultrasonic oscillation time is 1.2-1.6 h; finally adding ethanol for washing to obtain the SiO-containing2A washing solution of nanoparticles.
4. The method of claim 1, wherein the SiO nanoparticles are used2The preparation method of the modified palm insulating oil is characterized in that in the step S3, the SiO-containing oil obtained in the step S2 is filtered2Drying the nano particle washing liquid in a vacuum drying oven at the vacuum degree of-0.06 MPa and the drying temperature of 80-85 ℃ to obtain the primary modified SiO2Nanoparticles.
5. The method of claim 1, wherein the SiO nanoparticles are used2A method for producing a modified palm insulating oil, characterized in that in step S4, the primary modified SiO obtained in step S3 is used2Uniformly mixing the nano particles and absolute ethyl alcohol, adding isobutanol, and uniformly stirring at the stirring speed of 200-250 r/min for 35-40 min to obtain a mixed solution; the addition amount of the isobutanol is SiO subjected to primary modification235 to 45 percent of the weight of the nano particles.
6. The method of claim 1, wherein the SiO nanoparticles are used2The preparation method of the modified palm insulating oil is characterized in that in the step S5, the mixed solution obtained in the step S4 is subjected to ultrasonic dispersion and stirring at the temperature of 40-45 ℃ to obtain an ultrasonic dispersion solution; during ultrasonic dispersion, the ultrasonic frequency of the ultrasonic oscillation generator is 35-38 KHz, and ultrasonic dispersion is carried out for three times, wherein each time is 25-30 min, and each time is 15 min; centrifugally separating the ultrasonic dispersion, drying in a vacuum drying oven, and grinding into powder to obtain the secondarily modified SiO2Nanoparticles.
7. The method of claim 1, wherein the SiO nanoparticles are used2The preparation method of the modified palm insulating oil is characterized in that in the step S6, the modified palm insulating oil is prepared byThe secondarily modified SiO obtained in step S52The nano particles, diphenyl cresyl phosphate and alkylphenol polyoxyethylene ether are subjected to ultrasonic oscillation uniformly, the ultrasonic frequency of an ultrasonic oscillation generator is 35-38 KHz, and the ultrasonic oscillation time is as follows: obtaining SiO in 45-55 min2Mixing the nano particle liquid; the addition amount of the cresyl diphenyl phosphate is SiO subjected to secondary modification235 to 45 percent of the weight of the nano particles; the addition amount of the alkylphenol polyoxyethylene ether is SiO subjected to secondary modification225-35% of the weight of the nano particles.
8. The method of claim 1, wherein the SiO nanoparticles are used2The preparation method of the modified palm insulating oil is characterized in that in the step S7, the palm insulating oil is subjected to vacuum filtration and heated to 65-70 ℃, and is mechanically stirred at the stirring speed of 150-200 r/min for 40-45 min, so that the filtered palm insulating oil is obtained.
9. The method of claim 1, wherein the SiO nanoparticles are used2The preparation method of the modified palm insulating oil is characterized in that the antioxidant in the step S8 is selected from one or more of 2, 6-tri-tert-butyl-4-methylphenol, 2, 6-di-tert-butylphenol and 2, 6-di-tert-butyl-p-cresol.
10. The method of claim 1, wherein the SiO nanoparticles are used2The preparation method of the modified palm insulating oil is characterized in that the metal passivator in the step S8 is 2-methyl-benzotriazole.
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