Preparation method of fault diagnosis agent for transformer insulating oil
Fault diagnostic agents are prepared by a simple reaction of phenolic compounds, halogenated hydrocarbon compounds, alkali and solvent, which solves the problem of lag in power transformer fault monitoring and realizes rapid, economical and safe fault early warning. It is suitable for the industrial production of transformer insulating oil.
Patent Information
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-11-10
- Publication Date
- 2026-04-07
AI Technical Summary
In the existing technology, the fault monitoring methods for power transformers are lagging, lack complete diagnostic basis, and have long detection cycles, making it difficult to achieve rapid early warning of faults. Furthermore, there is a lack of fault warning and diagnostic agents suitable for insulating oil in oil-filled equipment.
A fault diagnostic agent was prepared by stirring a phenolic compound, a halogenated hydrocarbon compound, an alkali and a solvent under mild conditions. The high-purity fault diagnostic agent was obtained by simple extraction, distillation or chromatographic purification and then added to insulating oil for monitoring.
It enables rapid and sensitive fault diagnosis, reduces production costs and equipment investment, has good engineering applicability and safety, and is suitable for industrial production.
Smart Images
Figure CN121800624A_ABST
Abstract
Description
Technical Field
[0001] This invention belongs to the field of power equipment fault diagnosis technology, and specifically relates to a method for preparing a fault diagnosis agent for transformer insulating oil. Background Technology
[0002] Power transformers are critical equipment in power grid systems, and their operating status directly affects the safety and stability of the entire grid. Currently, fault monitoring methods based on oil chromatography suffer from drawbacks such as lag, incomplete diagnostic evidence, and long detection cycles, making it difficult to provide early warnings of rapidly evolving faults. Therefore, there is an urgent need in this field to develop a novel fault diagnostic agent capable of rapidly and sensitively responding to fault energy.
[0003] Currently, there is a lack of additives for use as fault early warning and diagnostic agents in the insulating oil of oil-filled equipment. Therefore, there is a need to develop a simple, environmentally friendly, and low-cost preparation method suitable for the industrial production of fault diagnostic agents for power equipment. Summary of the Invention
[0004] The purpose of this invention is to solve the above-mentioned problems and provide a method for preparing the fault diagnostic agent. This method has the advantages of simple steps, mild reaction conditions, and high product purity, and is suitable for large-scale preparation.
[0005] Specifically, the present invention provides a method for preparing a fault diagnostic agent for transformer insulating oil, wherein the reaction formula of the preparation method is:
[0006] The preparation method includes: mixing a phenolic compound, a halogenated hydrocarbon compound, an alkali, and a solvent and stirring the mixture to react; then, optionally cooling, optionally filtering, optionally concentrating the filtrate, and optionally purifying the mixture, to obtain a fault diagnosis agent having the structure of Formula 3; "optional" means that in a specific embodiment, this operation may or may not be performed.
[0007] The phenolic compound is a chiral phenol or a common phenolic compound having the structure of Formula 1, where R is hydrogen, aryl, or alkyl. 1 It is hydrogen, aryl, or alkyl; Halogenated hydrocarbons have the structure of formula 2, R 2 In X, X is chlorine, bromine, or iodine, and R 2 It is an alkyl group.
[0008] As a preferred embodiment, in the above-described method for preparing a fault diagnostic agent for transformer insulating oil, the alkali is an organic alkali or an inorganic alkali. More preferably, the organic alkali is triethylamine; and the inorganic alkali is potassium carbonate or cesium carbonate.
[0009] As a preferred embodiment, in the above-mentioned method for preparing a fault diagnostic agent for transformer insulating oil, the solvent is a polar solvent. More preferably, the polar solvent is tetrahydrofuran, acetonitrile, ethyl acetate, dichloromethane, etc. N , N One or more of dimethylformamide.
[0010] As a preferred embodiment, in the above-mentioned method for preparing a fault diagnostic agent for transformer insulating oil, the amounts of other components relative to 1.0 mol of phenolic compound are: 1.0~5.0 mol of halogenated hydrocarbon compound, 1.0~3.0 mol of alkali, and 10-2500 ml of solvent.
[0011] As a preferred embodiment, in the above-mentioned method for preparing a fault diagnostic agent for transformer insulating oil, the stirring reaction is carried out under an inert atmosphere or in an open air atmosphere.
[0012] As a preferred embodiment, the above-mentioned method for preparing a fault diagnostic agent for transformer insulating oil involves a reaction temperature of 50-120℃ and a reaction time of 1-50 hours, the reaction time of which can be adjusted according to the substrate type.
[0013] As a preferred embodiment, the above-mentioned method for preparing a fault diagnostic agent for transformer insulating oil involves purification by extraction, distillation, or chromatography.
[0014] In a preferred embodiment of the present invention, the phenolic compound in the above-described method for preparing a fault diagnostic agent for transformer insulating oil is ( S )-Binaphthol, wherein the halohydrocarbon compound is 1-bromononane, and the base is cesium carbonate.
[0015] Experiments have verified that within the addition range of 0.01wt% to 10wt%, the diagnostic agent has minimal impact on the key parameters of insulating oil (such as density, kinematic viscosity, breakdown voltage, etc.), and all indicators still meet the requirements of GB2536-2011 standard, demonstrating good engineering applicability and safety.
[0016] Compared with the prior art, the preparation method of the present invention has the following beneficial effects: 1. The preparation method of the fault diagnosis agent provided by the present invention has simple reaction steps, requires no complex equipment, and is easy to industrialize.
[0017] The preparation method of this invention involves mixing and stirring a phenolic compound, a halogenated hydrocarbon compound, a base, and a solvent to obtain the desired diagnostic agent. The entire process does not require complex chemical reaction steps, simplifying the production process and reducing operational difficulty. Due to the simplicity of the reaction steps, the method of this invention does not require special or complex reaction equipment; ordinary reaction vessels such as round-bottom flasks can complete the reaction process. This significantly reduces equipment investment and operating costs, facilitating large-scale industrial production.
[0018] 2. It uses inexpensive and readily available raw materials and does not use catalysts, resulting in low costs.
[0019] The phenolic compounds, halogenated hydrocarbons, bases, and solvents used in this invention are all commercially available and inexpensive chemicals, eliminating the need for expensive special materials and reducing raw material costs. Traditional chemical reactions often require catalysts to increase reaction rates and yields, but the method of this invention does not require any catalysts. This not only further reduces production costs but also avoids the environmental pollution and subsequent treatment problems that catalysts may cause. Considering all these factors, the preparation method of this invention achieves cost control in terms of raw materials, equipment, and processes, significantly reducing the overall production cost of fault diagnostic agents and improving economic efficiency.
[0020] 3. The reaction conditions are mild, the safety is high, and it is environmentally friendly.
[0021] The reaction temperature range of this invention is 50-120℃, and the reaction time is 1-50 hours. These conditions are relatively mild, eliminating the need for extreme conditions such as high temperature and high pressure, thus reducing energy consumption and equipment requirements, and also lowering operational risks. The mild reaction conditions and simple process flow make the entire production process safer, reducing potential safety hazards and protecting the health and safety of operators. The method of this invention does not use toxic or harmful catalysts, and the mild reaction conditions reduce the generation of harmful byproducts, lowering the environmental impact and meeting the requirements of green chemistry and sustainable development.
[0022] 4. The product has high purity and good compatibility with insulating oil.
[0023] Through appropriate purification steps (such as extraction, distillation, or chromatography), this invention can obtain high-purity fault diagnostic agents, ensuring product quality and performance. The fault diagnostic agents of this invention have good compatibility with transformer insulating oil, can be uniformly dispersed in the insulating oil, and can effectively perform fault diagnosis.
[0024] In summary, the preparation method of the present invention not only has technical advantages, but also performs well in terms of economy, safety and environmental protection, making it very suitable for industrial production and practical application.
[0025] The above description is merely an overview of the technical solution of the present invention. In order to better understand the technical means of the present invention and to implement it in accordance with the contents of the specification, and in order to make the above and other objects, features and advantages of the present invention more apparent and understandable, specific embodiments of the present invention are described below. Attached Figure Description
[0026] Figure 1 The 1H NMR spectrum of the target product of Example 1 is shown; Figure 2 The carbon NMR spectrum of the target product of Example 1 is shown. Detailed Implementation
[0027] The following description provides numerous specific details to offer a more thorough understanding of the technical solutions provided by this invention. However, it will be apparent to those skilled in the art that the technical solutions provided by this invention can be implemented without one or more of these details.
[0028] Example 1 This embodiment provides a method for preparing a fault diagnosis agent for transformer insulating oil.
[0029] The reaction formula is as follows:
[0030] Add the following ingredients sequentially to a 100mL round-bottom flask: S 1-Binaphthol (2.86 g, 10 mmol), 1-bromononane (6.18 g, 30 mmol), and cesium carbonate (Cs₂CO₃, 6.5 g, 20 mmol) were added, along with 20 mL of acetonitrile as a solvent. The reaction mixture was stirred at 50°C for 48 hours. After the reaction was complete, the system was cooled to room temperature. Subsequently, 50 mL of dichloromethane was added to the reaction solution, and insoluble solid impurities were removed by filtration. The filtrate was concentrated and purified by column chromatography (eluent: petroleum ether → ethyl acetate / petroleum ether = 1:100) to obtain the target product in 95% yield.
[0031] The target product was subjected to proton nuclear magnetic resonance spectroscopy using conventional methods. Figure 1 ), carbon spectrum ( Figure 2 The analysis yielded the following results: Hydrogen spectrum: 1 H NMR (400 MHz, chloroform- d ) δ 7.91 (d, J = 9.0 Hz, 2H), 7.83(d, J = 8.0 Hz, 2H), 7.39 (d, J= 9.0 Hz, 2H), 7.29 (m, 2H), 7.22 – 7.12 (m, 4H), 3.97 – 3.85 (m, 4H), 1.04 – 1.34 (m, 4H), 1.29 – 1.22 (m, 4H), 1.21 – 1.14 (m,4H), 1.14 – 1.06 (m, 4H), 1.04 – 0.94 (m, 8H), 0.91 – 0.84 (m, 10H). Carbon spectrum: 13 C NMR (101 MHz, chloroform-d) δ 154.7, 134.3, 129.4, 129.1,127.9, 126.1, 125.6, 123.5, 120.8, 116.0, 69.9, 32.0, 29.5, 29.3, 25.7, 22.8,14.3. Therefore, the target product was obtained in this embodiment.
[0032] Test case This test case demonstrates that the target product of Example 1 is suitable for overheating fault early warning in power oil-filled equipment.
[0033] During transformer operation, oil samples are periodically collected from the equipment for monitoring. Chiral chromatography is used to analyze the diagnostic reagents in the oil samples, determining the changes in the proportion of chiral isomers, particularly the change in the enantiomeric excess percentage. A quantitative relationship between the enantiomeric excess percentage of the diagnostic reagent and the overheating fault energy is obtained. o C: y = -0.011x + 1.0057, R 2 =0.981; 180 o C: y = -0.0129x + 1.0147, R 2 =0.9845; 190 o C: y = -0.0466x + 0.9802, R 2 =0.9787.
[0034] Based on the sample collection time interval and the rate of change of the enantiomeric excess percentage in the insulating oil, the quantitative relationship between the enantiomeric excess percentage of the diagnostic agent and the overheating fault energy is substituted into the above-mentioned formula. By comparing the y and x values under standard experimental conditions, the transformer overheating temperature and overheating duration can be derived, thereby realizing early warning of oil-filled equipment faults.
[0035] The above are merely preferred embodiments of the present invention and are not intended to limit the present invention. Various modifications and variations can be made to the present invention by those skilled in the art. Any modifications, equivalent substitutions, improvements, etc., made within the spirit and principles of the present invention should be included within the scope of protection of the present invention.
Claims
1. A method for preparing a fault diagnostic agent for transformer insulating oil, characterized in that, The general reaction formula for the preparation method is: The preparation method includes: mixing phenolic compounds, halogenated hydrocarbon compounds, alkali, and solvent and stirring the mixture to react; then, after optional cooling, optional filtration, optional filtrate concentration, and optional purification, a fault diagnosis agent with the structure of Formula 3 is obtained. The phenolic compound is a chiral phenol or a common phenolic compound having the structure of Formula 1, where R is hydrogen, aryl, or alkyl. 1 It is hydrogen, aryl, or alkyl; Halogenated hydrocarbons have the structure of formula 2, R 2 In X, X is chlorine, bromine, or iodine, and R 2 It is an alkyl group.
2. The method for preparing a fault diagnostic agent for transformer insulating oil according to claim 1, characterized in that, The alkali is an organic alkali or an inorganic alkali.
3. The method for preparing a fault diagnostic agent for transformer insulating oil according to claim 2, characterized in that, The organic base is triethylamine; the inorganic base is potassium carbonate or cesium carbonate.
4. The method for preparing a fault diagnostic agent for transformer insulating oil according to claim 1, characterized in that, The solvent is a polar solvent.
5. The method for preparing a fault diagnostic agent for transformer insulating oil according to claim 4, characterized in that, The polar solvent is tetrahydrofuran, acetonitrile, ethyl acetate, dichloromethane, N , N One or more of dimethylformamide.
6. The method for preparing a fault diagnostic agent for transformer insulating oil according to claim 1, characterized in that, Compared to 1.0 mol of phenolic compounds, the amounts of other components are: 1.0~5.0 mol of haloalkanes, 1.0~3.0 mol of alkali, and 10-2500 mL of solvent.
7. The method for preparing a fault diagnostic agent for transformer insulating oil according to claim 1, characterized in that, The stirring reaction is carried out under an inert atmosphere or in an open air atmosphere.
8. The method for preparing a fault diagnostic agent for transformer insulating oil according to claim 1, characterized in that, The reaction temperature is 50-120℃, and the reaction time is 1-50 hours.
9. The method for preparing a fault diagnostic agent for transformer insulating oil according to claim 1, characterized in that, Purification methods include extraction, distillation, or chromatography.
10. The method for preparing a fault diagnostic agent for transformer insulating oil according to claim 1, characterized in that, The phenolic compounds are ( S )-Binaphthol, wherein the halohydrocarbon compound is 1-bromononane, and the base is cesium carbonate.