CN113913233A - Method for modifying plant insulating oil by octaaniline propyl polysilsesquioxane - Google Patents
Method for modifying plant insulating oil by octaaniline propyl polysilsesquioxane Download PDFInfo
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- C—CHEMISTRY; METALLURGY
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- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M169/00—Lubricating compositions characterised by containing as components a mixture of at least two types of ingredient selected from base-materials, thickeners or additives, covered by the preceding groups, each of these compounds being essential
- C10M169/04—Mixtures of base-materials and additives
- C10M169/041—Mixtures of base-materials and additives the additives being macromolecular compounds only
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
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- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M155/00—Lubricating compositions characterised by the additive being a macromolecular compound containing atoms of elements not provided for in groups C10M143/00 - C10M153/00
- C10M155/02—Monomer containing silicon
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- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M169/00—Lubricating compositions characterised by containing as components a mixture of at least two types of ingredient selected from base-materials, thickeners or additives, covered by the preceding groups, each of these compounds being essential
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- C10M2207/00—Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
- C10M2207/40—Fatty vegetable or animal oils
- C10M2207/401—Fatty vegetable or animal oils used as base material
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- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2229/00—Organic macromolecular compounds containing atoms of elements not provided for in groups C10M2205/00, C10M2209/00, C10M2213/00, C10M2217/00, C10M2221/00 or C10M2225/00 as ingredients in lubricant compositions
- C10M2229/04—Siloxanes with specific structure
- C10M2229/05—Siloxanes with specific structure containing atoms other than silicon, hydrogen, oxygen or carbon
- C10M2229/052—Siloxanes with specific structure containing atoms other than silicon, hydrogen, oxygen or carbon containing nitrogen
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- C10N2030/00—Specified physical or chemical properties which is improved by the additive characterising the lubricating composition, e.g. multifunctional additives
- C10N2030/08—Resistance to extreme temperature
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- C10N2030/00—Specified physical or chemical properties which is improved by the additive characterising the lubricating composition, e.g. multifunctional additives
- C10N2030/10—Inhibition of oxidation, e.g. anti-oxidants
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- C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
- C10N2040/00—Specified use or application for which the lubricating composition is intended
- C10N2040/14—Electric or magnetic purposes
- C10N2040/16—Dielectric; Insulating oil or insulators
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Abstract
The invention relates to a method for modifying vegetable insulating oil by octaaniline propyl polysilsesquioxane, which comprises the following steps: s1 preparation of octaanilinopropylsilsesquioxane nanoparticles: s2 preparation of polysilsesquioxane modified vegetable insulating oil: s2-1: drying, dehydrating and degassing the vegetable insulating oil in a vacuum drying oven; s2-2: forming a mixture containing the modified nanoparticles and the vegetable insulating oil; s2-3: ensuring that the modified polysilsesquioxane nano particles are fully dispersed in the insulating oil; s2-4: and obtaining the polysilsesquioxane modified vegetable insulating oil. The nano modification is carried out by using the vegetable insulating oil, the initial oxidation temperature of the vegetable insulating oil can be greatly increased, the stability is greatly enhanced, and the breakdown voltage, the dielectric loss factor, the insulating property and the heat conducting property of the insulating oil are also enhanced.
Description
Technical Field
The invention belongs to the technical field of improvement of stability of vegetable insulating oil, and particularly relates to a method for modifying vegetable insulating oil by octaaniline propyl polysilsesquioxane.
Background
Insulating oil is used in a large amount as an important liquid insulating medium in electrical equipment such as transformers. The traditional mineral insulating oil has excellent physical and chemical properties and electrical insulation and cooling characteristics, can play roles in insulation, heat dissipation and cooling, electric arc extinguishing and the like, and is widely applied to oil-immersed power transformers for nearly one hundred years. However, the mineral insulating oil has a low ignition point, may cause fire or explosion accidents under the condition of transformer overheating or internal short circuit failure, cannot meet the requirements of high fire resistance in places such as mines, military facilities and high-rise buildings, has poor biodegradability, is a non-environment-friendly liquid insulating material, and can cause serious pollution and damage to the surrounding environment once leakage occurs. In addition, mineral insulating oil is a non-renewable petroleum product, and the use of a large amount of mineral insulating oil can occupy limited petroleum resources, so that the shortage and exhaustion of the petroleum resources are further aggravated. Therefore, the vegetable insulating oil which has the advantages of environmental protection, renewable resources, excellent fireproof performance and the like receives wide attention.
In chinese patent document CN102732359A, a preparation method of a ferroferric oxide nanoparticle modified transformer oil is disclosed, which comprises the steps of firstly preparing ferroferric oxide nanoparticles by a suitable process, mixing the ferroferric oxide nanoparticles with mineral transformer oil, performing ultrasonic dispersion, and removing impurities and moisture through suction filtration and vacuum drying processes to obtain the ferroferric oxide nanoparticle modified transformer oil, so as to improve the long-term stability of the transformer oil.
In chinese patent document CN109749814A, a method for modifying silica-coated ferriferrous oxide nanoparticles is disclosed, which comprises preparing silica-coated ferriferrous oxide nanoparticles by a suitable process, adding ethanol, oleic acid surfactant 2 and silane coupling agent, and obtaining oleic acid-coated SiO under the condition of a constant temperature water bath of 60-90 ℃2@Fe3O4And adding the nano particles into the insulating oil under a certain condition, and drying in vacuum to obtain the high-thermal-conductivity nano plant insulating oil.
Currently, the main research on nano insulating oil focuses on using traditional mineral oil as a base fluid, so as to form a stable colloid and improve the stability of the stable colloid. However, the physical and chemical properties of the vegetable insulating oil are obviously different from those of mineral insulating oil which mainly comprises naphthenic hydrocarbon and aromatic hydrocarbon, the physical and chemical properties and the electrical properties of the two kinds of insulating oil show different trends due to the addition of the nano particles, and the physical and chemical electrical properties of the two kinds of nano modified insulating oil have obvious difference due to the difference of molecular structures of the two kinds of insulating oil. However, the current vegetable insulating oil nano-modification technology is still lack of research.
The nanoparticles such as ferroferric oxide proposed in the above-mentioned chinese patent document CN102732359A are inorganic particles, and cannot be combined with transformer oil molecules to form a stable dispersion system. On the other hand, the nano particles are easy to agglomerate, and the ferroferric oxide nano particles have magnetism and are easy to agglomerate, so that the dispersibility and the long-term stability of the nano particles in the transformer oil cause a great important problem of limiting the application of the nano particles. In addition, after the semiconductor nanoparticles exceed a certain mass fraction, the nanoparticles can significantly improve the heat conductivity of the insulating oil, the nano insulating oil with the concentration is easy to form small bridges under an electric field to reduce the breakdown characteristic of the insulating oil, and meanwhile, the semiconductor material can increase the electrical conductivity and the dielectric loss of the insulating oil, so that a nano material which has the heat conductivity, the insulating strength and the dielectric loss parameters at the same time needs to be found.
Disclosure of Invention
The invention aims to provide a method for modifying vegetable insulating oil by octaaniline propyl polysilsesquioxane, which is suitable for vegetable insulating oil, remarkably improves the oxidation stability of the vegetable insulating oil and does not influence dielectric physicochemical properties such as dielectric loss factors of the vegetable insulating oil.
In order to solve the technical problems, the technical scheme adopted by the invention is that the method for modifying the vegetable insulating oil by the octaaniline propyl polysilsesquioxane comprises the following steps:
s1 preparation of octaanilinopropylsilsesquioxane nanoparticles:
s1-1: dissolving aniline propyl siloxane A in a solvent B, adding a catalyst C, uniformly stirring, and standing for 7-20 days to obtain a crude cage octaaniline propyl polysiloxane acid salt solid;
wherein the weight ratio of the aniline propyl siloxane A to the solvent B is 1: 100-8: 100, respectively; the weight ratio of the catalyst C to the aniline propyl siloxane A is 80: 100-150: 100, respectively;
s1-2: washing the crude cage-type octaaniline propyl polysilsesquioxane acid salt solid obtained in the step S1-1 by using a solvent B, and performing vacuum drying to obtain a refined cage-type octaaniline propyl polysilsesquioxane acid salt solid;
s1-3: adding the refined cage octaaniline propyl polysilsesquioxane acid salt solid in the step S1-2 into a solvent D, adding organic amine E, stirring and mixing, filtering, pouring the filtrate into water for precipitation and purification, filtering, and drying in vacuum to obtain cage octaaniline propyl polysilsesquioxane; wherein the weight ratio of the acid salt of the aniline propyl polysilsesquioxane to the solvent D is 0.5: 100-20: 100, the dosage of water for precipitation and purification is 6 to 12 times of the volume of the organic amine E;
obtaining modified polysilsesquioxane nano particles;
s2 preparation of polysilsesquioxane modified vegetable insulating oil:
s2-1: drying, dehydrating and degassing the vegetable insulating oil in a vacuum drying oven at 70-90 ℃ under a vacuum degree of-0.05-0.13 MPa for 36-48 hours;
s2-2: adding the modified polysilsesquioxane nanoparticles obtained in the step S1-3 to the vegetable insulating oil obtained in the step S2-1 to form a mixture containing the modified nanoparticles and the vegetable insulating oil;
s2-3: ultrasonically oscillating the mixture obtained in the step S2-2 at 50-70 ℃ for 20-30 minutes to ensure that the modified polysilsesquioxane nanoparticles are fully dispersed in the insulating oil;
s2-4: and (4) dehydrating and degassing the polysilsesquioxane nanoparticle modified vegetable insulating oil obtained in the step S2-3, wherein the drying temperature is 70-90 ℃, the vacuum degree is-0.05-0.13 MPa, and the drying time is 24-36h, so that the polysilsesquioxane modified vegetable insulating oil is obtained.
By adopting the technical method, the vegetable insulating oil is subjected to nano modification, so that the initial oxidation temperature of the vegetable insulating oil can be greatly increased, the stability is greatly enhanced, and the breakdown voltage, the dielectric loss factor, the insulating property and the heat conducting property of the insulating oil are also enhanced. Compared with the prior nanometer modification technology, the nanometer material provided by the invention has the advantages that the effect of improving the oxidation stability is more obvious, the addition amount is small, and other properties of the vegetable insulating oil cannot be influenced.
In a preferred embodiment of the present invention, the synthesis of the cage-type octaanilinopropylsilsesquioxane salt in step S1-1 is performed in an atmosphere of air, nitrogen, argon or helium.
In a preferred embodiment of the present invention, the synthesis of the cage-type octaanilinopropylsilsesquioxane salt in step S1-1 is performed under an atmosphere of air nitrogen or argon.
In a preferred embodiment of the present invention, in step S1-1, the solvent B is one or a mixture of several of methanol, ethanol, propanol, isopropanol, acetone, dimethyl sulfoxide, and N-methylpyrrolidone.
In the step S1-1, the catalyst C is one or a mixture of several of hydrochloric acid, nitric acid, sulfuric acid, phosphoric acid, formic acid and acetic acid in any proportion.
In a preferred embodiment of the present invention, in step S1-3, the solvent D is one or a mixture of acetone, dimethyl sulfoxide, tetrahydrofuran, and N-methylpyrrolidone in any ratio.
As a preferred technical solution of the present invention, in the step S1-3, the organic amine E is one or a mixture of several of trimethylamine, triethylamine, diethyltriamine, ethylenediamine, methylamine, and triethyldiamine in any proportion.
In the preferred embodiment of the present invention, in step S2-4, the obtained vegetable insulating oil is stored in a jar in a sealed state.
In a preferred embodiment of the present invention, in the step S2-1, the vegetable insulating oil is jatropha curcas vegetable insulating oil.
The jatropha curcas oil has rich sources, low cost and high content of monounsaturated fatty acid, and is a natural crop with great application potential in plant insulating oil. The jatropha curcas is also called jatropha curcas, jatropha curcas and jatropha curcas, is a jatropha curcas in Euphorbiaceae, belongs to deciduous shrub or small arbor, and has strong drought tolerance. The oil content of the seed kernel of the jatropha curcas is 40-60 percent, the maximum oil content can reach 66.32 percent, and the seed kernel can be prepared into excellent oil materials after being processed. The jatropha curcas has large planting area, wide distribution range and rich resources, is mainly distributed in provinces such as Yunnan, Sichuan, Guangxi, Guangdong, Guizhou, Hainan and the like, and has natural distribution area of about 1.1 kilohm. Therefore, the preparation of the vegetable insulating oil based on the jatropha curcas oil has important research significance.
The existing research shows that the proportion of various main fatty acids after the hydrolysis of the jatropha curcas oil is approximately: oleic acid (35.27%), linoleic acid (40.51%), pentadecanoic acid (15.82%) and stearic acid (8.41%), of which the monounsaturated fatty acid content is comparatively high, are preferred for the preparation of vegetable insulating oils. However, due to the large amount of unsaturated bonds contained in the jatropha curcas oil, the vegetable insulating oil is easily affected by external conditions such as light, temperature, moisture, oxygen and the like during storage and use, and thus is deteriorated. The deterioration of the vegetable insulating oil will deteriorate to generate more acidic substances than the mineral insulating oil, will adversely affect the support and insulation materials impregnated with the vegetable oil in the construction of the transformer, and severely limit the application and development of the vegetable insulating oil.
The polysilsesquioxane nano molecule is added to carry out nano modification on the jatropha curcas plant insulating oil, so that the initial oxidation temperature of the jatropha curcas plant insulating oil is increased, and the stability is greatly improved.
The cage type Polysilsesquioxane (POSS) provided by the invention enables a novel material with a unique organic-inorganic hybrid structure to be developed in recent years. The composite material has the characteristics of nanoscale size, uniform particle size, good structural designability and solubility, thermal oxidation stability of inorganic materials, excellent mechanical properties, easy processing of organic materials, good toughness, low density and the like. POSS molecules contain a large number of inorganic silica rigid frameworks and multi-end active groups, and after the POSS molecules react with substances, the flexibility of the POSS molecules can be restrained, a rigid structure taking POSS as a core is formed, and the formed hybrid material is highly cross-linked in structure, so that the movement of a molecular chain segment structure is hindered, the POSS is not easy to deform and decompose, and the heat resistance of the material is remarkably improved. And the POSS taking the amino group as the active group can obviously improve the initial decomposition temperature of the unsaturated ester.
Therefore, the octaaniline propyl polysilsesquioxane nano molecule is added into the plant insulating oil (jatropha curcas plant insulating oil), so that the oxidation stability of the plant insulating oil can be remarkably improved, and the dielectric property of the insulating oil is also remarkably improved.
Detailed Description
The method for modifying the vegetable insulating oil by the octaaniline propyl polysilsesquioxane comprises the following steps:
s1 preparation of octaanilinopropylsilsesquioxane nanoparticles:
s1-1: dissolving aniline propyl siloxane A in a solvent B, adding a catalyst C, uniformly stirring, and standing for 7-20 days to obtain a crude cage octaaniline propyl polysiloxane acid salt solid;
wherein the weight ratio of the aniline propyl siloxane A to the solvent B is 1: 100-8: 100, respectively; the weight ratio of the catalyst C to the aniline propyl siloxane A is 80: 100-150: 100, respectively;
s1-2: washing the crude cage-type octaaniline propyl polysilsesquioxane acid salt solid obtained in the step S1-1 by using a solvent B, and performing vacuum drying to obtain a refined cage-type octaaniline propyl polysilsesquioxane acid salt solid;
s1-3: adding the refined cage octaaniline propyl polysilsesquioxane acid salt solid in the step S1-2 into a solvent D, adding organic amine E, stirring and mixing, filtering, pouring the filtrate into water for precipitation and purification, filtering, and drying in vacuum to obtain cage octaaniline propyl polysilsesquioxane; wherein the weight ratio of the acid salt of the aniline propyl polysilsesquioxane to the solvent D is 0.5: 100-20: 100, the dosage of water for precipitation and purification is 6 to 12 times of the volume of the organic amine E;
obtaining modified polysilsesquioxane nano particles;
s2 preparation of polysilsesquioxane modified vegetable insulating oil:
s2-1: drying, dehydrating and degassing the vegetable insulating oil in a vacuum drying oven at 70-90 ℃ under a vacuum degree of-0.05-0.13 MPa for 36-48 hours;
s2-2: adding the modified polysilsesquioxane nanoparticles obtained in the step S1-3 to the vegetable insulating oil obtained in the step S2-1 to form a mixture containing the modified nanoparticles and the vegetable insulating oil;
s2-3: ultrasonically oscillating the mixture obtained in the step S2-2 at 50-70 ℃ for 20-30 minutes to ensure that the modified polysilsesquioxane nanoparticles are fully dispersed in the insulating oil;
s2-4: and (4) dehydrating and degassing the polysilsesquioxane nanoparticle modified vegetable insulating oil obtained in the step S2-3, wherein the drying temperature is 70-90 ℃, the vacuum degree is-0.05-0.13 MPa, and the drying time is 24-36h, so that the polysilsesquioxane modified vegetable insulating oil is obtained.
In the step S1-1, the synthesis of the cage-type octaanilinopropylsilsesquioxane salt is performed under an atmosphere of air, nitrogen, argon or helium, preferably under an atmosphere of air nitrogen or argon.
In the step S1-1, the solvent B is one or a mixture of several of methanol, ethanol, propanol, isopropanol, acetone, dimethyl sulfoxide and N-methylpyrrolidone in any proportion.
In the step S1-1, the catalyst C is one or a mixture of several of hydrochloric acid, nitric acid, sulfuric acid, phosphoric acid, formic acid and acetic acid in any proportion.
In the step S1-3, the solvent D is one or a mixture of acetone, dimethyl sulfoxide, tetrahydrofuran and N-methylpyrrolidone in any proportion.
In the step S1-3, the organic amine E is one or a mixture of several of trimethylamine, triethylamine, diethyltriamine, ethylenediamine, methylamine, and triethyldiamine in any proportion.
In the step S2-4, the obtained vegetable insulating oil is stored in a jar in a sealed manner.
In the step S2-1, the vegetable insulating oil is jatropha curcas vegetable insulating oil.
Specifically, the method comprises the following steps: 2000mL three-neck flask, room temperature, nitrogen protection, electromagnetic stirring, sequentially adding 1200mL acetone and 0.2moL aniline propyl silane, then dropwise adding 68mL concentrated hydrochloric acid (concentration 38%), stirring for 24 hours, sealing and standing for 20 days, suction filtering, washing a filter cake for 3 times by using 5mL fresh acetone, and vacuum drying at normal temperature to obtain 28.5g of hydrochloride of cage octapolyaniline propyl silsesquioxane. Transferring hydrochloride of the cage octa-polyaniline propyl silsesquioxane into a 250mL three-neck flask, adding 100mL of dimethyl sulfoxide and 0.48moL of triethylamine under the condition of room temperature and under the protection of nitrogen, electromagnetically stirring for 6 hours, filtering, dropwise adding filtrate into 1500mL of water, precipitating and purifying, filtering, and drying in vacuum to obtain 21.6g of white solid, namely cage octa-polyaniline propyl silsesquioxane;
drying the jatropha curcas plant insulating oil in a vacuum drying oven at 80 ℃ under-0.1 MPa for 40 hours; adding 5g of modified polysilsesquioxane nanoparticles to 5kg of vegetable insulating oil to form a mixture containing the modified nanoparticles and the vegetable insulating oil; ultrasonically oscillating the obtained mixture at 50-70 ℃ for 20-30 minutes to ensure that polysilsesquioxane particles are fully dispersed in insulating oil; and then, dehydrating and degassing the polysilsesquioxane nanoparticle modified vegetable insulating oil, wherein the drying temperature is 80 ℃, the vacuum degree is-0.1 MPa, and the drying time is 36 hours, so that the polysilsesquioxane modified vegetable insulating oil is obtained. Through detection, the molecular chain decomposition rate of the modified jatropha curcas plant insulating oil is reduced by 62.6%, the oxygen diffusion rate is reduced by 42.8%, the electron confinement capability is improved by 37.1%, the initial oxidation temperature of the plant insulating oil is improved by 30 ℃ overall, and the oxidation stability is greatly improved.
The above-mentioned embodiments, objects, technical solutions and advantages of the present invention are further described in detail, it should be understood that the above-mentioned embodiments are only exemplary embodiments of the present invention, and are not intended to limit the present invention, and any modifications, equivalent substitutions, improvements and the like, such as changes in shape or material of some components, may be made within the spirit and principle of the present invention; are intended to be included within the scope of the present invention.
Claims (9)
1. The method for modifying the vegetable insulating oil by using octaaniline propyl polysilsesquioxane is characterized by comprising the following steps of:
s1 preparation of octaanilinopropylsilsesquioxane nanoparticles:
s1-1: dissolving aniline propyl siloxane A in a solvent B, adding a catalyst C, uniformly stirring, and standing for 7-20 days to obtain a crude cage octaaniline propyl polysiloxane acid salt solid;
wherein the weight ratio of the aniline propyl siloxane A to the solvent B is 1: 100-8: 100, respectively; the weight ratio of the catalyst C to the aniline propyl siloxane A is 80: 100-150: 100, respectively;
s1-2: washing the crude cage-type octaaniline propyl polysilsesquioxane acid salt solid obtained in the step S1-1 by using a solvent B, and performing vacuum drying to obtain a refined cage-type octaaniline propyl polysilsesquioxane acid salt solid;
s1-3: adding the refined cage octaaniline propyl polysilsesquioxane acid salt solid in the step S1-2 into a solvent D, adding organic amine E, stirring and mixing, filtering, pouring the filtrate into water for precipitation and purification, filtering, and drying in vacuum to obtain cage octaaniline propyl polysilsesquioxane; wherein the weight ratio of the acid salt of the aniline propyl polysilsesquioxane to the solvent D is 0.5: 100-20: 100, the dosage of water for precipitation and purification is 6 to 12 times of the volume of the organic amine E;
obtaining modified polysilsesquioxane nano particles;
s2 preparation of polysilsesquioxane modified vegetable insulating oil:
s2-1: drying, dehydrating and degassing the vegetable insulating oil in a vacuum drying oven at 70-90 ℃ under a vacuum degree of-0.05-0.13 MPa for 36-48 hours;
s2-2: adding the modified polysilsesquioxane nanoparticles obtained in the step S1-3 to the vegetable insulating oil obtained in the step S2-1 to form a mixture containing the modified nanoparticles and the vegetable insulating oil;
s2-3: ultrasonically oscillating the mixture obtained in the step S2-2 at 50-70 ℃ for 20-30 minutes to ensure that the modified polysilsesquioxane nanoparticles are fully dispersed in the insulating oil;
s2-4: and (4) dehydrating and degassing the polysilsesquioxane nanoparticle modified vegetable insulating oil obtained in the step S2-3, wherein the drying temperature is 70-90 ℃, the vacuum degree is-0.05-0.13 MPa, and the drying time is 24-36h, so that the polysilsesquioxane modified vegetable insulating oil is obtained.
2. The method for modifying vegetable insulating oil with octaanilinopropylsilylsesquioxane of claim 1, wherein in step S1-1, the synthesis of the cage-type octaanilinopropylsilylsesquioxane salt is performed under an atmosphere of air, nitrogen, argon or helium.
3. The method for modifying vegetable insulating oil with octaanilinopropylsilsesquioxane of claim 2, wherein in step S1-1, the synthesis of the cage-type octaanilinopropylsilsesquioxane salt is performed under an air nitrogen or argon atmosphere.
4. The method for modifying plant insulating oil by octa-anilinopropylsilsesquioxane of claim 1, wherein in step S1-1, the solvent B is one or a mixture of several of methanol, ethanol, propanol, isopropanol, acetone, dimethyl sulfoxide and N-methyl pyrrolidone at any ratio.
5. The method for modifying vegetable insulating oil by octaanilinopropylsilsesquioxane of claim 1, wherein in step S1-1, the catalyst C is one or a mixture of hydrochloric acid, nitric acid, sulfuric acid, phosphoric acid, formic acid and acetic acid.
6. The method for modifying plant insulating oil by octaanilinopropylsilsesquioxane of claim 1, wherein in step S1-3, the solvent D is one or a mixture of acetone, dimethyl sulfoxide, tetrahydrofuran and N-methylpyrrolidone.
7. The method for modifying vegetable insulating oil with octa-anilinopropylsilsesquioxane of claim 1, wherein in step S1-3, the organic amine E is one or a mixture of several of trimethylamine, triethylamine, diethyltriamine, ethylenediamine, methylamine, and triethyldiamine.
8. The method for modifying vegetable insulating oil with octaanilinopropylsilsesquioxane of any one of claims 1-7, wherein in said step S2-4, the obtained vegetable insulating oil is stored in a jar under sealed condition.
9. The method for modifying vegetable insulating oil with octanilino propyl polysilsesquioxane as set forth in any one of claims 1 to 7, wherein in said step S2-1, the vegetable insulating oil is a Jatropha curcas vegetable insulating oil.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1986605A (en) * | 2006-11-30 | 2007-06-27 | 南京大学 | Preparing method of cage anilino methyl sesquisiloxane octamer |
| CN105047257A (en) * | 2015-07-06 | 2015-11-11 | 重庆大学 | Method for preparing compounds containing modified fullerene nanoparticles and plant insulating oil |
| CN106635253A (en) * | 2016-08-26 | 2017-05-10 | 重庆大学 | Preparation method of monodisperse iron (II,III) oxide nanoparticle modified vegetable insulating oil |
| CN110747037A (en) * | 2019-10-30 | 2020-02-04 | 凉山德农生物能源股份有限公司 | Jatropha curcas insulating oil and preparation method thereof |
| CN111892971A (en) * | 2020-07-31 | 2020-11-06 | 云南电网有限责任公司电力科学研究院 | Preparation method of nano plant insulating oil |
-
2021
- 2021-10-10 CN CN202111178442.1A patent/CN113913233A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1986605A (en) * | 2006-11-30 | 2007-06-27 | 南京大学 | Preparing method of cage anilino methyl sesquisiloxane octamer |
| CN105047257A (en) * | 2015-07-06 | 2015-11-11 | 重庆大学 | Method for preparing compounds containing modified fullerene nanoparticles and plant insulating oil |
| CN106635253A (en) * | 2016-08-26 | 2017-05-10 | 重庆大学 | Preparation method of monodisperse iron (II,III) oxide nanoparticle modified vegetable insulating oil |
| CN110747037A (en) * | 2019-10-30 | 2020-02-04 | 凉山德农生物能源股份有限公司 | Jatropha curcas insulating oil and preparation method thereof |
| CN111892971A (en) * | 2020-07-31 | 2020-11-06 | 云南电网有限责任公司电力科学研究院 | Preparation method of nano plant insulating oil |
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