A live-line insulating cleaning agent for 500kV and above voltage level and a preparation method thereof

Abstract

The application belongs to the field of high-voltage power equipment cleaning, and provides a live insulation cleaning agent for 500kV and above voltage grades and a preparation method thereof. The application constructs a pre-dehydration insulation continuous phase by isododecane and polydimethylsiloxane, forms a nano reverse micelle dispersed phase by silanization n-decyl glucoside and dimethyl carbonate, and filters into an agent through airtight low-moisture mixing, so as to realize the consideration of cleaning wetting, dispersion stability, low-moisture insulation and processing fluidity, solve the problem that the dispersion stability and insulation performance and the fluidity and wetting performance of a high-voltage live cleaning system are difficult to unify, and be suitable for live insulation cleaning of 500kV and above power equipment.

Description

Technical Field

[0001] This invention relates to the field of live-line cleaning agents for high-voltage power equipment, specifically to a live-line insulating cleaning agent for voltage levels of 500kV and above and its preparation method. Background Technology

[0002] Transmission and transformation equipment with voltage levels of 500kV and above operates long-term in outdoor or complex industrial environments. Insulators, bushings, busbar connections, and external insulation surfaces easily accumulate dust, salt spray, oil, and moisture, forming a complex contamination layer. When using live-line cleaning agents for uninterrupted maintenance, they not only need sufficient electrical insulation safety margin but also need to maintain low moisture content, low conductivity micro-areas, and low residue during spraying, spreading, and evaporation. In high-voltage scenarios, the cleaning and wetting ability, dispersion stability, processing fluidity, and insulation retention ability of the cleaning agent are interdependent; any imbalance can lead to insufficient contamination removal, uneven wetting, or fluctuations in insulation condition. Therefore, developing an insulation cleaning system suitable for high-voltage live-line operations—characterized by low moisture content, stable dispersion, easy filtration, and good wetting and cleaning capabilities—is of great significance for improving the efficiency of power equipment maintenance, reducing the need for power outages for repairs, and ensuring the long-term operation of external insulation.

[0003] Existing technologies for cleaning live-line insulation have proposed various combinations of solvents, surfactants, and spraying processes, but the problem of simultaneously stabilizing insulation performance and cleaning / wetting performance remains. For example, Chinese patent CN105296244A discloses a live-line cleaning agent for insulators, which uses dimethyl carbonate, ethylene glycol derivatives, nonionic surfactants, dispersants, and polymethylsiloxane to improve the cleaning effect of insulators; however, this type of solution contains a large number of polar solubilizers and surfactants, and if the moisture and dispersed phase states are not adequately controlled, localized polar micro-regions can easily form in high-voltage operating environments. Another example is Chinese patent CN112226301A, which describes a live-line insulation cleaning agent for electrical and mechanical equipment and mentions existing solutions containing trichloroethylene, anhydrous ethanol, surfactants, and antistatic agents in the background; while such systems can improve the convenience of decontamination or maintenance, there are still difficulties in coordinating volatility safety, ionic components, residue control, and high-voltage insulation maintenance. Summary of the Invention

[0004] The purpose of this invention is to provide a live insulating cleaning agent for voltage levels of 500kV and above and its preparation method, thereby solving the problem that it is difficult to simultaneously achieve both dispersion stability and insulation performance, as well as processing fluidity and cleaning wetting performance in current high-voltage live cleaning systems.

[0005] Existing systems often introduce polar components to enhance wetting and dispersion, but this can easily weaken insulation retention. To enhance insulation, dispersion and cleaning spread can be reduced. This invention achieves a synergistic balance between two types of side effects by matching the ratio of the pre-dehydrated insulating continuous phase and the silanized n-decyl glucoside reverse micelle dispersed phase and by preparing the system in a closed, low-moisture environment. This results in the mutual weakening of these two types of side effects and the synergistic balance between cleaning, wetting, dispersion stability, and insulation retention.

[0006] To achieve the above objectives, the present invention provides the following technical solution:

[0007] A live-line insulation cleaning agent for voltage levels of 500kV and above, comprising, based on 100 parts by weight of the total weight of the live-line insulation cleaning agent, the live-line insulation cleaning agent consists of the following components and process residues that are unavoidably introduced during the preparation process:

[0008] Isododecane is the remainder after deducting the other components and the process residues, and its final content is 71.37-92.80 parts by weight;

[0009] Polydimethylsiloxane 2.00-8.00 parts by weight;

[0010] Dimethyl carbonate, 5.00-18.00 parts by weight;

[0011] 0.20-2.50 parts by weight of silanized n-decyl glucoside;

[0012] Moisture content: 0.005-0.030 parts by weight;

[0013] Process residual components: 0-0.10 parts by weight;

[0014] The above contents are the final contents of the corresponding components in the charged insulating cleaning agent. The total final contents of isododecane, polydimethylsiloxane, dimethyl carbonate, silanized n-decyl glucoside, water and the process residue components are 100 parts by weight.

[0015] The silanized n-decyl glucoside is obtained by reacting n-decyl glucoside with 3-glycidyl etheroxypropyltrimethoxysilane. The silanized n-decyl glucoside is the average silanized product formed after the hydroxyl group in the n-decyl glucoside molecule undergoes a ring-opening reaction with the epoxy group of 3-glycidyl etheroxypropyltrimethoxysilane. Its quality control indicators include silicon content, moisture content and unreacted 3-glycidyl etheroxypropyltrimethoxysilane residue in the product.

[0016] The process residues are the process residues introduced into the final filtrate from the product obtained in step B6, the filtration step, the step of removing part of the dimethyl carbonate under reduced pressure, and the final filtration step, excluding isododecane, polydimethylsiloxane, dimethyl carbonate, silanized n-decyl glucoside, and water in the final charged insulating cleaning agent. The process residues include unreacted 3-glycidyl etheroxypropyltrimethoxysilane, n-decyl glucoside-related residues, siloxane condensation-related components, and inorganic salt residues introduced into the filtrate after filtration in step A4, step C3, or step S5.

[0017] Furthermore, the silanized n-decyl glucoside and the dimethyl carbonate form a silanized n-decyl glucoside reverse micelle intermediate in isododecane, and form a reverse micelle dispersed phase in the charged insulating cleaning agent. The reverse micelle dispersed phase has a D50 particle size of 20-80 nm and a polydispersity index of 0.08-0.30.

[0018] The silanized n-decyl glucoside is a cleaning and wetting component.

[0019] Furthermore, the silanized n-decyl glucoside reverse micelle intermediate is prepared by the following steps:

[0020] A1. To provide the silanized n-decyl glucoside;

[0021] A2. By weight, add 100 parts isododecane, 5-35 parts dimethyl carbonate and 0.5-8 parts silanized n-decyl glucoside to a sealed stirring container.

[0022] A3. Stir for 0.5-3.0 h at 20-35℃ and 1000-4000 r / min under a nitrogen protective atmosphere;

[0023] A4. Add 0.5-5.0 parts by weight of anhydrous sodium sulfate and contact for dehydration for 0.5-2.0 hours, then filter to remove the anhydrous sodium sulfate;

[0024] A5. Control the moisture content of the obtained dispersion to be 0.005-0.030 wt%, the D50 particle size to be 20-80 nm, and the polydispersity index to be 0.08-0.30, to obtain the silanized n-decyl glucoside reverse micelle intermediate.

[0025] Furthermore, the silanized n-decyl glucoside in step A1 is prepared through the following steps:

[0026] B1. Add n-decyl glucoside, anhydrous potassium carbonate, and dimethyl carbonate to the reaction vessel to form a reaction system;

[0027] B2. With the molar amount of n-decyl glucoside as 1, the molar amount of 3-glycidyl etheroxypropyltrimethoxysilane is 0.10-0.60, and the molar amount of anhydrous potassium carbonate is 0.01-0.08.

[0028] B3. The solid content of the reaction system is controlled to be 20.00-60.00 wt%;

[0029] B4. Under a nitrogen protective atmosphere, 3-glycidyl etheroxypropyltrimethoxysilane is added to the reaction system and reacted at 55-80°C for 4-10 h;

[0030] B5. Using the reaction solution from step B4 as the test object, the reaction is stopped when the residual amount of unreacted 3-glycidyl ether oxypropyltrimethoxysilane is 0.05-0.50 wt%.

[0031] B6. Filter to remove anhydrous potassium carbonate, remove part of dimethyl carbonate under reduced pressure, and control the silicon content in the product to be 0.20-2.50 wt% and the moisture content to be 0.005-0.100 wt% to obtain the silanized n-decyl glucoside.

[0032] Furthermore, the isododecane and the polydimethylsiloxane are first prepared into a pre-dehydrated insulating continuous phase, which is prepared through the following steps:

[0033] C1. By weight, 100 parts by weight of isododecane are mixed with 2.75-40.00 parts by weight of polydimethylsiloxane;

[0034] C2. Add 0.5-5.0 parts by weight of anhydrous sodium sulfate and stir at 20-35℃ for 0.5-4.0 hours;

[0035] C3. Filter to remove anhydrous sodium sulfate;

[0036] C4. Control the moisture content of the obtained liquid phase to 0.005-0.020wt% to obtain the pre-dehydrated insulating continuous phase.

[0037] Furthermore, the mass ratio of the silanized n-decyl glucoside to the dimethyl carbonate is 1:6 to 1:25; in the electrically insulating cleaning agent, the free silanized n-decyl glucoside accounts for 0-20.00 wt% of the total silanized n-decyl glucoside, and the dispersed phase with a particle size greater than 1.00 μm accounts for 0-5.00 vol% of the total dispersed phase.

[0038] Furthermore, the charged insulating cleaning agent does not contain 1,1,2-trichloro-1,2,2-trifluoroethane, dichloromethane, 1,1,1-trichloroethane, or carbon tetrachloride, nor does it contain any ionic antistatic additives.

[0039] As a concept of this invention, the present invention employs a design that combines a pre-dehydrated insulating continuous phase with a silanized n-decyl glucoside reverse micelle dispersion phase, primarily to achieve a synergistic balance between insulation retention and cleaning, wetting, and dispersibility. Existing live-line cleaning systems typically increase polar solvents or surface-active structures to improve dispersion stability and wetting spreadability; however, polar microregions and residual moisture can increase the risk of insulation fluctuations under high-voltage environments. To improve insulation performance, there is a tendency to increase the proportion of non-polar continuous phases and reduce the content of polar components, thereby weakening dirt wetting, interfacial penetration, and dispersion retention. This cleaning agent forms a low-moisture insulating continuous phase through isododecane and polydimethylsiloxane, and then forms a nanoscale reverse micelle dispersion phase through silanized n-decyl glucoside and dimethyl carbonate in isododecane. This confines the wetting components within a stable dispersion structure, reducing the adverse effects of free polar components, and maintains a balance between flowability and cleaning effect through moisture, particle size, and polydispersity index control.

[0040] This invention also discloses a method for preparing a live insulating cleaning agent for voltage levels of 500kV and above, comprising the following steps:

[0041] S1. Provides a silanized n-decyl glucoside reverse micelle intermediate, wherein the silanized n-decyl glucoside reverse micelle intermediate is a reverse micelle intermediate formed by silanized n-decyl glucoside, dimethyl carbonate and isododecane;

[0042] S2. Providing a pre-dehydrated insulating continuous phase, said pre-dehydrated insulating continuous phase being obtained by dehydrating and mixing isododecane and polydimethylsiloxane;

[0043] S3. The silanized n-decyl glucoside reverse micelle intermediate is mixed with the pre-dehydrated insulating continuous phase at a mass ratio of 1:0.4 to 1:3.0;

[0044] S4. Stir at 20-35℃ and 300-1500 r / min for 0.5-2.0 h;

[0045] S5. Filter to obtain the charged insulating cleaning agent;

[0046] The electrical insulating cleaning agent has a moisture content of 0.005-0.030 wt%, and the reverse micelle dispersed phase in the electrical insulating cleaning agent has a D50 particle size of 20-80 nm and a polydispersity index of 0.08-0.30.

[0047] Furthermore, in step S3, the mass ratio of the silanized n-decyl glucoside reverse micelle intermediate to the pre-dehydrated insulating continuous phase is 1:0.4 to 1:3.0, the mixing temperature is 20-35℃, the stirring rate is 300-1500 r / min, and the mixing time is 0.5-2.0 h.

[0048] Furthermore, after step S4, a quality control step is included, which includes detecting the moisture content of the charged insulating cleaning agent, the D50 particle size and polydispersity index of the reverse micelle dispersed phase in the charged insulating cleaning agent.

[0049] Furthermore, the preparation process of the silanized n-decyl glucoside reverse micelle intermediate provided in step S1 and step S3 are both carried out in a closed explosion-proof stirring device. The operating temperature of the closed explosion-proof stirring device is 20-35℃, and the oxygen content in the gas phase inside the device is 0.1-5.0 vol.

[0050] Furthermore, the filtration in step S4 includes end filtration with a pore size of 0.20-1.00 μm, and the dispersed phase with a particle size greater than 1.00 μm after filtration accounts for 0-5.00 vol of the total dispersed phase.

[0051] Furthermore, in the preparation of silanized n-decyl glucoside, n-decyl glucoside and anhydrous potassium carbonate are added to dimethyl carbonate to form a reaction system. Taking the molar amount of n-decyl glucoside as 1, the molar amount of 3-glycidyl etheroxypropyltrimethoxysilane is controlled to be 0.10-0.60, the molar amount of anhydrous potassium carbonate is controlled to be 0.01-0.08, and the solid content of the reaction system is controlled to be 20.00-60.00 wt%. Under a nitrogen protective atmosphere, 3-glycidyl etheroxypropyltrimethoxysilane is added to the reaction system and reacted at 55-80℃ for 4-10 h. After the reaction, the system is filtered to remove anhydrous potassium carbonate and partially removed by dimethyl carbonate under reduced pressure to obtain silanized n-decyl glucoside for the preparation of reverse micelle intermediates.

[0052] Furthermore, the structure of the obtained silanized n-decyl glucoside was determined, and the sample to be tested was the product obtained in step B6; the detection items included² 9 SiNMR, FTIR and silicon elemental content detection;² 9 SiNMR recorded trimethoxysilyl silicon signals in the range of -40ppm to -43ppm and siloxane condensation-related silicon signals in the range of -48ppm to -67ppm. FTIR recorded epoxy group characteristic absorption signals, Si-OC related absorption signals, and Si-O-Si related absorption signals. Silicon element content detection recorded the mass fraction of silicon in the sample. The above detection data, together with the amount of unreacted 3-glycidyl etheroxypropyltrimethoxysilane residue, served as the quality control data for this batch of silanized n-decyl glucoside before it entered the reverse micelle intermediate preparation step.

[0053] Furthermore, the residual amount of unreacted 3-glycidyl etheroxypropyltrimethoxysilane was detected by external standard chromatography. The test sample was either the reaction solution from step B4 or the product obtained from step B6. The test sample was diluted with dimethyl carbonate and then injected. The retention time and peak area of ​​the corresponding peaks in the 3-glycidyl etheroxypropyltrimethoxysilane standard and the test sample were recorded. The mass fraction of unreacted 3-glycidyl etheroxypropyltrimethoxysilane in the test sample was calculated based on the external standard curve of the standard. The obtained mass fraction was used as the judgment data for stopping the reaction in step B5 and releasing the product in step B6.

[0054] Furthermore, the silanized n-decyl glucoside reverse micelle intermediate was subjected to dynamic light scattering detection by direct loading of the intermediate stock solution at a test temperature of 25±0.1℃. The detection data included intensity distribution particle size, volume distribution particle size, D50 particle size, polydispersity index, and number of test repetitions. Within the same batch, samples were taken from the silanized n-decyl glucoside reverse micelle intermediate obtained in step A5 and the mixture after stirring in step S4 and before filtration in step S5 for testing. The D50 particle size and polydispersity index before and after mixing were used to characterize the particle size retention state of the reverse micelle dispersed phase in the system before final filtration.

[0055] Further, before mixing in step S3, based on the measured mass fractions of dimethyl carbonate and silanized n-decyl glucoside in the silanized n-decyl glucoside reverse micelle intermediate, and the measured mass fractions of isododecane and polydimethylsiloxane in the pre-dehydrated insulating continuous phase, the weighed mass of the silanized n-decyl glucoside reverse micelle intermediate and the pre-dehydrated insulating continuous phase are calculated. For components introduced by only one source phase, the target final content is equal to the measured mass fraction of that component in the corresponding source phase multiplied by the mass percentage of that source phase in the final mixture. For components such as isododecane and water introduced by two source phases, the target final content is equal to the sum of the products of the measured mass fraction of that component in each source phase and the mass percentage of the corresponding source phase in the final mixture. The obtained weighed mass is used for feeding in step S3, and simultaneously meets the mass ratio range of step S3, so that step S5... The final contents of dimethyl carbonate, silanized n-decyl glucoside, water, polydimethylsiloxane, and isododecane in the obtained electrically insulating cleaning agent fall within the corresponding ranges.

[0056] Furthermore, the moisture content was determined using the Karl Fischer coulometric method. The test samples were taken from the silanized n-decyl glucoside obtained in step B6, the silanized n-decyl glucoside reverse micelle intermediate obtained in step A5, the pre-dehydrated insulating continuous phase obtained in step C4, and the charged insulating cleaning agent obtained in step S5. For each test sample, the sample mass, titration endpoint charge, converted moisture mass, and moisture mass fraction were recorded. The obtained moisture mass fraction was used as the quality control data for steps B6, A5, C4, and S5, respectively.

[0057] Furthermore, in step S5, the final filtration uses the liquid phase mixed in step S3 as the object to be filtered, with a pore size of 0.20-1.00 μm. The filtered filtrate is used as the final charged insulating cleaning agent. The volume fraction of the dispersed phase with a particle size greater than 1.00 μm is detected in the filtrate. The detection data includes the sample batch number, pore size, sample state before detection, particle size distribution curve, total volume of all dispersed phases, and volume of dispersed phase with a particle size greater than 1.00 μm. The ratio of the volume of dispersed phase with a particle size greater than 1.00 μm to the total volume of all dispersed phases is used as the dispersed phase control result after final filtration.

[0058] Furthermore, the proportion of free silanized n-decyl glucoside was detected using the charged insulating cleaning agent obtained in step S5 as the test sample. The test sample was divided into unseparated sample and separated sample. The unseparated sample was used to determine the total amount of silanized n-decyl glucoside. The separated sample was centrifuged to obtain a continuous phase liquid, which was used to determine the content of free silanized n-decyl glucoside. The ratio of the mass of free silanized n-decyl glucoside to the total mass of silanized n-decyl glucoside was used as the free proportion data, and together with the D50 particle size and polydispersity index of the reverse micelle dispersed phase, it was used as the final product batch release data.

[0059] Furthermore, using the live insulation cleaning agent and its volatile residues obtained in step S5 as the testing objects, the volume resistivity, power frequency breakdown voltage, dielectric loss factor, corrosivity, flash point, and cleaning rate of the liquid sample are recorded, and the mass fraction of the volatile residues is recorded for the volatile residue sample. The preparation process of the test sample includes taking the filtrate obtained in step S5, mixing it uniformly in a sealed container, dispensing it into liquid samples according to the same batch, and taking another batch of filtrate to prepare volatile residue samples according to the volatile residue test conditions. The obtained test data, together with the moisture content, D50 particle size, polydispersity index, and volume fraction of dispersed phase with a particle size greater than 1.00 μm of the batch, constitute the product quality record for live insulation cleaning applications at voltage levels of 500 kV and above.

[0060] Furthermore, before feeding materials, the gas phase space inside the sealed explosion-proof mixing equipment is replaced with nitrogen. The oxygen content of the gas phase inside the equipment after replacement is detected by an oxygen content detector. The detection point is set in the gas phase space of the equipment. The detection data includes the oxygen content before replacement, the oxygen content after replacement, the oxygen content during the intermediate preparation process in step S1, and the oxygen content during the mixing process in step S3. The gas phase oxygen content inside the equipment is controlled at 0.1-5.0 vol% before the intermediate preparation or final mixing operation is carried out. The obtained oxygen content record and the working temperature record are used together as the operation record of the sealed explosion-proof mixing equipment.

[0061] As another aspect of this invention, the present invention employs a method of first preparing a silanized n-decyl glucoside reverse micelle intermediate, followed by low-temperature closed-loop mixing and filtration with a pre-dehydrated insulating continuous phase. This method is primarily used to achieve, fix, or amplify the aforementioned synergistic effects. Directly mixing the wetting component, polar solvent, and non-polar insulating phase can easily lead to localized aggregation, moisture introduction, and uncontrolled particle size, causing the cleaning / wetting and insulation processes to mutually constrain each other. Excessive dehydration or reducing the amount of wetting component will limit contamination spread and dispersion stability. This method, through silanization reaction, reverse micelle intermediate construction, pre-dehydrated insulating continuous phase preparation, mass-ratio mixing, low-temperature stirring, and end-filtration, sequentially controls reaction residue, moisture, particle size, polydispersity index, and the proportion of large-particle-size dispersed phases. This ensures that the wetting structure remains dispersible within the insulating continuous phase, and that the oxygen content control and operating temperature of the sealed explosion-proof equipment jointly improve the stability of the preparation process.

[0062] The pre-dehydrated insulating continuous phase formed by isododecane and polydimethylsiloxane mainly serves as a low-moisture insulation retainer and a flowing medium. While increasing the proportion of this continuous phase alone helps reduce the influence of polar micro-regions, it weakens the wetting penetration and dispersion of contaminants. The reverse micelle dispersed phase formed by silanized n-decyl glucoside and dimethyl carbonate mainly serves as a cleaning and wetting agent and an interface spreading agent. Increasing the proportion of this dispersed phase or free wetting components alone may introduce local polar aggregation, moisture sensitivity, and changes in flow state. This invention uses the mass ratio of silanized n-decyl glucoside to dimethyl carbonate, the reverse micelle D50 particle size, the polydispersity index, the moisture content, and end-filtering to jointly regulate the wetting function, allowing it to be carried by the nano-dispersed phase and distributed within the insulating continuous phase. This balances the mutually restrictive performance in high-voltage live cleaning scenarios.

[0063] Beneficial technical effects

[0064] 1. By pre-forming a pre-dehydrated insulating continuous phase with isododecane and polydimethylsiloxane and controlling the moisture content of the continuous phase, the adverse effects of free water and polar micro-regions in the system on insulation retention can be reduced. At the same time, it provides the continuous medium required for the flow and spread of the cleaning agent, making it more suitable for cleaning and maintenance of high-voltage live external insulation surfaces.

[0065] 2. By first forming a reverse micelle intermediate in isododecane with silanized n-decyl glucoside and dimethyl carbonate, and then introducing them into the final mixing system, the cleaning and wetting components can be stably carried in the form of a dispersed phase, reducing the risk of local aggregation caused by excessive free wetting components, thereby taking into account dirt wetting, dirt dispersion and insulation continuous phase stability.

[0066] 3. By controlling the moisture content, D50 particle size, polydispersity index, proportion of free silanized n-decyl glucoside, and volume fraction of dispersed phase with a particle size greater than 1.00 μm, the composition, dispersion state, and post-filtration state of the prepared cleaning agent can be verified, which is beneficial to improving the stability of the preparation process for different batches.

[0067] 4. By completing the preparation and final mixing of the reverse micelle intermediate in a closed, explosion-proof stirring device, and by combining nitrogen replacement, working temperature and gas phase oxygen content recording, the preparation can be completed under low moisture, low temperature mixing and explosion-proof control conditions, reducing the impact of volatile solvent operation fluctuations on product quality and preparation safety. Attached Figure Description

[0068] Figure 1 This is a DLS intensity-weighted particle size distribution diagram of the electrically insulating cleaning agent of the present invention.

[0069] Figure 2 This is a cumulative volume distribution diagram of DLS in the electrically insulating cleaning agent of the present invention.

[0070] Figure 3 This is a statistical chart of the D50 particle size of the electrically insulating cleaning agent of the present invention.

[0071] Figure 4 This is a statistical chart of the polydispersity index (PDI) of the electrically insulating cleaning agent of the present invention.

[0072] Figure 5 This is a statistical chart showing the proportion of free silanized n-decyl glucoside in the electrically insulating cleaning agent of this invention.

[0073] Figure 6 This is a graph showing the correlation between the free state ratio and D50 particle size of the charged insulating cleaning agent of this invention.

[0074] Figure 7 The 2nd silanized n-decyl glucoside of this invention 9 Si NMR spectrum overlay.

[0075] Figure 8 The 2nd silanized n-decyl glucoside of this invention 9 Si NMR normalized peak area statistics.

[0076] Figure 9This is a superimposed FTIR absorption spectrum of the silanized n-decyl glucoside of the present invention.

[0077] Figure 10 This is a statistical chart of the normalized area of ​​the FTIR characteristic peaks of the silanized n-decyl glucoside of the present invention.

[0078] Figure 11 This is a graph showing the correlation between the volume resistivity and D50 particle size of the electrically insulating cleaning agent of this invention.

[0079] Figure 12 This is a correlation diagram between the power frequency breakdown voltage and PDI of the electrically insulating cleaning agent of the present invention.

[0080] Figure 13 This is a correlation diagram between the moisture content and dielectric loss factor of the electrically insulating cleaning agent of the present invention.

[0081] Figure 14 This is a graph showing the dynamic contact angle of the electrically insulating cleaning agent of the present invention changing over time.

[0082] Figure 15 This is a statistical chart showing the standard dirt layer cleaning rate of the electrically insulating cleaning agent of the present invention.

[0083] Figure 16 This is a graph showing the correlation between the 60 s contact angle and the cleaning rate of the electrically insulating cleaning agent of this invention.

[0084] Figure 17 This is a macroscopic optical photograph of the charged insulating cleaning agent in Example 1.

[0085] Figure 18 This is a SEM image of the residual layer after the charged insulating cleaning agent from Example 1 has evaporated following drop application; Figure 18 a is a low-magnification SEM image of the residual layer of the electrically insulating cleaning agent in Example 1; Figure 18 b and Figure 18 c is a medium-to-high magnification SEM image of the residual layer of the electrically insulating cleaning agent in Example 1; Figure 18 d is a SEM image of the cross-section or local interface of the residual layer of the charged insulating cleaning agent in Example 1.

[0086] Figure 19 This is a TEM characterization image of the reverse micelle dispersion phase of the charged insulating cleaning agent in Example 1; Figure 19 a is a bright-field TEM image of the reverse micelle dispersion phase of the charged insulating cleaning agent in Example 1; Figure 19 b is a magnified TEM image of the reverse micelle dispersion phase of the charged insulating cleaning agent in Example 1. Detailed Implementation

[0087] To make the objectives, technical solutions, and advantages of the embodiments of the present invention clearer, the technical solutions of the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings.

[0088] Example 1

[0089] Overall production scale and product form

[0090] This embodiment prepares 1000.00g of liquid cleaning agent for live insulation applications at voltage levels of 500kV and above. Based on a total weight of 100 parts by weight of the cleaning agent, the composition includes 92.795 parts by weight of isododecane, 2.00 parts by weight of polydimethylsiloxane, 5.00 parts by weight of dimethyl carbonate, 0.20 parts by weight of silanized n-decyl glucoside, 0.005 parts by weight of water, and 0.000 parts by weight of unavoidable process residues, totaling 100 parts by weight. The product of this embodiment is a low-viscosity, filterable liquid used for cleaning contaminant layers on external insulation surfaces.

[0091] Raw materials, components or material specifications

[0092] Isododecane was a commercially available high-purity liquid with a purity ≥99.0% and a moisture content ≤0.005 wt%. Polydimethylsiloxane was a commercially available low-viscosity liquid with a kinematic viscosity of 5 mm² / s at 25°C and a moisture content ≤0.010 wt%. Dimethyl carbonate was a commercially available anhydrous liquid with a purity ≥99.5% and a moisture content ≤0.010 wt%. n-Decyl glucoside was a commercially available industrial-grade raw material with an active ingredient content ≥98.0%. 3-Glycidyl etheroxypropyltrimethoxysilane was a commercially available high-purity raw material with a purity ≥98.0%. Anhydrous potassium carbonate and anhydrous sodium sulfate were both commercially available analytical-grade solids, dried at 105°C for 2 hours and cooled to 25°C in a drying container before use. Nitrogen gas had a purity ≥99.99%.

[0093] Steps B1 to B6: Preparation of silanized n-decyl glucoside

[0094] Decyl glucoside, anhydrous potassium carbonate, and dimethyl carbonate were added to a reaction vessel equipped with mechanical stirring, reflux condenser, and nitrogen inlet to form a reaction system. Taking the molar amount of decyl glucoside as 1, the molar amount of 3-glycidyl etheroxypropyltrimethoxysilane was 0.10, and the molar amount of anhydrous potassium carbonate was 0.01, with the solid content of the reaction system controlled at 20.00 wt%. Under a nitrogen protective atmosphere, the mixture was stirred at 300 rpm for 20 min, and then 3-glycidyl etheroxypropyltrimethoxysilane was added to the reaction system over 30 min. The temperature was raised to 55 °C and the reaction was carried out for 4 h. During the reaction, a slight positive pressure of nitrogen was maintained at atmospheric pressure, and reflux condenser was used to maintain stability. The endpoint was determined by external standard chromatography, with the residual amount of unreacted 3-glycidyl etheroxypropyltrimethoxysilane being 0.05 wt%. After the reaction was completed, anhydrous potassium carbonate was removed by filtration at 25°C, and some dimethyl carbonate was removed under reduced pressure at 40°C and 8 kPa to obtain silanized n-decyl glucoside. In this example, the silanized n-decyl glucoside contained 0.20 wt% silicon and 0.005 wt% water.

[0095] Steps A1 to A5: Preparation of the silanized n-decyl glucoside reverse micelle intermediate

[0096] The silanized n-decyl glucoside obtained in step B6 was used as raw material A1. 100 parts by weight of isododecane, 12.5 parts by weight of dimethyl carbonate, and 0.5 parts by weight of silanized n-decyl glucoside were added to a sealed stirred container. After purging the container with nitrogen, the mixture was stirred at 20°C and 1000 rpm for 0.5 h. After stirring, 0.5 parts by weight of anhydrous sodium sulfate was added, and dehydration was continued at 20°C for 0.5 h. Then, the anhydrous sodium sulfate was removed by filtration through a 0.45 μm solvent-resistant filter membrane to obtain the silanized n-decyl glucoside reverse micelle intermediate. In this example, the intermediate had a moisture content of 0.005 wt%, a D50 particle size of 20 nm, and a polydispersity index of 0.08.

[0097] Steps C1 to C4: Preparation of the pre-dehydrated insulating continuous phase

[0098] By weight, 100 parts by weight of isododecane and 3.8 parts by weight of polydimethylsiloxane were added to a dry, sealed stirring vessel and stirred for 15 minutes at 20°C and 500 rpm. Then, 0.5 parts by weight of anhydrous sodium sulfate were added, and stirring continued at 20°C for 0.5 hours. After stirring, the anhydrous sodium sulfate was removed by filtration through a 0.45 μm solvent-resistant membrane to obtain a pre-dehydrated insulating continuous phase. The moisture content of the pre-dehydrated insulating continuous phase in this embodiment was 0.005 wt%.

[0099] Steps S1 to S5: Preparation of the live insulating cleaning agent

[0100] This embodiment provides a silanized n-decyl glucoside reverse micelle intermediate and a pre-dehydrated insulating continuous phase. Based on the measured composition of the intermediate and the continuous phase, the mass of both phases is calculated to ensure that the final cleaning agent contains isododecane, polydimethylsiloxane, dimethyl carbonate, silanized n-decyl glucoside, and water at the levels set in this embodiment. The silanized n-decyl glucoside reverse micelle intermediate and the pre-dehydrated insulating continuous phase are added to a sealed explosion-proof mixing device at a mass ratio of 1:1.21. Before adding the materials, the gas phase space of the device is purged with nitrogen, resulting in a gas phase oxygen content of 0.1 vol%. The mixture is stirred for 0.5 hours at 20°C and 300 r / min, maintaining a sealed environment and atmospheric pressure nitrogen protection during the stirring process. After stirring, end-point filtration is performed with a pore size of 0.20 μm, and the filtrate is the live insulating cleaning agent of this embodiment.

[0101] Quality testing methods and results

[0102] Moisture content was determined using the Karl Fischer coulometric method, with each sample analyzed in triplicate. The final cleaning agent moisture content in this embodiment was 0.005 ± 0.001 wt%. The silanized n-decyl glucoside reverse micelle intermediate and the final pre-filtration mixture were subjected to dynamic light scattering analysis using a direct loading method at 24.9 °C. The final cleaning agent reverse micelle dispersed phase had a D50 particle size of 20 ± 1 nm and a polydispersity index of 0.08 ± 0.01. The dispersed phase with a particle size greater than 1.00 μm accounted for 0.00 vol% of the total dispersed phase. Free silanized n-decyl glucoside accounted for 0.00 wt% of the total silanized n-decyl glucoside.² 9 SiNMR recorded a trimethoxysilylsilane signal at -43 ppm and a siloxane condensation-related silicon signal at -67 ppm. FTIR recorded a weakened characteristic absorption signal of epoxy groups, a Si-OC related absorption signal, and a Si-O-Si related absorption signal. The silicon content detection results were consistent with the quality control results in step B6. After the liquid samples were sealed and dispensed, the volume resistivity, power frequency breakdown voltage, dielectric loss factor, corrosivity, flash point, and cleaning rate were recorded. For volatile residue samples, the mass fraction of volatile residues was recorded. All detection records, along with moisture, D50 particle size, and polydispersity index, formed the batch quality record.

[0103] Features and application scenarios of this embodiment

[0104] This embodiment uses a relatively mild low-wetting component and a low dimethyl carbonate ratio. The reverse micelle dispersed phase has a small particle size, strict moisture control, and a small end filter pore size, making it suitable for cleaning and maintenance scenarios of high-voltage external insulation equipment that are sensitive to moisture and require stable dispersion after filtration.

[0105] Example 2

[0106] Overall production scale and product form

[0107] This embodiment prepares 1000.00g of liquid cleaning agent for live insulation surfaces with voltage levels of 500kV and above. Based on a total weight of 100 parts by weight of the live insulation cleaning agent, the composition includes 71.610 parts by weight of isododecane, 8.00 parts by weight of polydimethylsiloxane, 17.88 parts by weight of dimethyl carbonate, 2.48 parts by weight of silanized n-decyl glucoside, 0.030 parts by weight of water, and 0.000 parts by weight of unavoidable process residues, totaling 100 parts by weight. The product of this embodiment is a highly wetting component-loaded liquid, used for cleaning external insulation surfaces with thick contaminant layers and requiring enhanced spreading and contaminant-carrying capacity.

[0108] Raw materials, components or material specifications

[0109] Isododecane was a commercially available high-purity liquid with a purity ≥99.0% and moisture content ≤0.005 wt%. Polydimethylsiloxane was a commercially available low-viscosity liquid with a kinematic viscosity of 10 mm² / s at 25°C and moisture content ≤0.010 wt%. Dimethyl carbonate was a commercially available anhydrous liquid with a purity ≥99.5% and moisture content ≤0.010 wt%. n-Decyl glucoside was a commercially available industrial-grade raw material with an active ingredient content ≥98.0%. 3-Glycidyl etheroxypropyltrimethoxysilane was a commercially available high-purity raw material with a purity ≥98.0%. Anhydrous potassium carbonate and anhydrous sodium sulfate were both commercially available analytical-grade solids, dried at 105°C for 2 hours and cooled to 25°C in a drying container before use. Nitrogen gas purity ≥99.99%.

[0110] Steps B1 to B6: Preparation of silanized n-decyl glucoside

[0111] Decyl glucoside, anhydrous potassium carbonate, and dimethyl carbonate were added to a reaction vessel equipped with mechanical stirring, reflux condenser, and nitrogen inlet to form a reaction system. Taking the molar amount of decyl glucoside as 1, the molar amount of 3-glycidyl etheroxypropyltrimethoxysilane was 0.60, and the molar amount of anhydrous potassium carbonate was 0.08, with the solid content of the reaction system controlled at 60.00 wt%. Under a nitrogen protective atmosphere, the mixture was stirred at 600 rpm for 20 min, and then 3-glycidyl etheroxypropyltrimethoxysilane was added to the reaction system over 60 min. The temperature was raised to 80 °C and the reaction was carried out for 10 h. During the reaction, a slight positive pressure of nitrogen was maintained at atmospheric pressure, and reflux condenser was used to maintain stability. The endpoint was determined by external standard chromatography, with the residual amount of unreacted 3-glycidyl etheroxypropyltrimethoxysilane being 0.50 wt%. After the reaction was completed, anhydrous potassium carbonate was removed by filtration at 30°C, and some dimethyl carbonate was removed under reduced pressure at 45°C and 6 kPa to obtain silanized n-decyl glucoside. In this example, the silanized n-decyl glucoside contained 2.50 wt% silicon and 0.100 wt% water.

[0112] Steps A1 to A5: Preparation of the silanized n-decyl glucoside reverse micelle intermediate

[0113] The silanized n-decyl glucoside obtained in step B6 was used as raw material A1. 100 parts by weight of isododecane, 35 parts by weight of dimethyl carbonate, and 4.86 parts by weight of silanized n-decyl glucoside were added to a sealed stirred container. After purging the container with nitrogen, the mixture was stirred at 35°C and 4000 rpm for 3.0 h. After stirring, 5.0 parts by weight of anhydrous sodium sulfate were added, and the mixture was further dehydrated at 35°C for 2.0 h. The anhydrous sodium sulfate was then removed by filtration through a 1.00 μm solvent-resistant filter membrane to obtain the silanized n-decyl glucoside reverse micelle intermediate. In this example, the intermediate had a moisture content of 0.030 wt%, a D50 particle size of 80 nm, and a polydispersity index of 0.30.

[0114] Steps C1 to C4: Preparation of the pre-dehydrated insulating continuous phase

[0115] By weight, 100 parts by weight of isododecane and 38.90 parts by weight of polydimethylsiloxane were added to a dry, sealed stirring vessel and stirred for 30 minutes at 35°C and 900 rpm. Then, 5.0 parts by weight of anhydrous sodium sulfate were added, and stirring continued at 35°C for 4.0 hours. After stirring, the anhydrous sodium sulfate was removed by filtration through a 1.00 μm solvent-resistant membrane to obtain a pre-dehydrated insulating continuous phase. The moisture content of the pre-dehydrated insulating continuous phase in this embodiment was 0.020 wt%.

[0116] Steps S1 to S5: Preparation of the live insulating cleaning agent

[0117] This embodiment provides a silanized n-decyl glucoside reverse micelle intermediate and a pre-dehydrated insulating continuous phase. Based on the measured composition of the intermediate and the continuous phase, the mass of both phases is calculated to ensure that the final cleaning agent contains isododecane, polydimethylsiloxane, dimethyl carbonate, silanized n-decyl glucoside, and water at the levels set in this embodiment. The silanized n-decyl glucoside reverse micelle intermediate and the pre-dehydrated insulating continuous phase are added to a sealed, explosion-proof mixing device at a mass ratio of 1:0.4. Before adding the materials, the gas phase space of the device is purged with nitrogen, resulting in a gas phase oxygen content of 5.0 vol%. The mixture is stirred at 35°C and 1500 r / min for 2.0 h, maintaining a sealed environment and atmospheric pressure nitrogen protection during the stirring process. After stirring, end-point filtration is performed with a pore size of 1.00 μm, and the filtrate is the live insulating cleaning agent of this embodiment.

[0118] Quality testing methods and results

[0119] Moisture content was determined using the Karl Fischer coulometric method, with each sample analyzed in triplicate. The final cleaning agent moisture content in this embodiment was 0.030 ± 0.002 wt%. The silanized n-decyl glucoside reverse micelle intermediate and the final pre-filtration mixture were subjected to dynamic light scattering analysis using a direct loading method at 25.1℃. The final cleaning agent reverse micelle dispersed phase had a D50 particle size of 80 ± 3 nm and a polydispersity index of 0.30 ± 0.02. Dispersed phase particles larger than 1.00 μm accounted for 5.00 vol% of the total dispersed phase. Free silanized n-decyl glucoside accounted for 20.00 wt% of the total silanized n-decyl glucoside.² 9 SiNMR recorded a trimethoxysilylsilane signal at -40 ppm and a siloxane condensation-related silicon signal at -48 ppm. FTIR recorded a weakened characteristic absorption signal of epoxy groups, a Si-OC related absorption signal, and a Si-O-Si related absorption signal. The silicon content detection results were consistent with the quality control results in step B6. After the liquid samples were sealed and dispensed, the volume resistivity, power frequency breakdown voltage, dielectric loss factor, corrosivity, flash point, and cleaning rate were recorded. For volatile residue samples, the mass fraction of volatile residues was recorded. All detection records, along with moisture, D50 particle size, and polydispersity index, formed a batch quality record.

[0120] Features and application scenarios of this embodiment

[0121] This embodiment uses a high-load wetting component and dimethyl carbonate ratio, with a high proportion of polydimethylsiloxane in the continuous phase, and a high mixing time and stirring rate. It is suitable for high-voltage external insulation cleaning applications where the contaminant layer has strong adhesion and requires enhanced wetting, spreading, and contaminant dispersion capabilities.

[0122] Example 3

[0123] Overall production scale and product form

[0124] This embodiment prepares 1000.00g of liquid cleaning agent for live insulation surfaces with voltage levels of 500kV and above. Based on a total weight of 100 parts by weight of the cleaning agent, the composition includes 80.985 parts by weight of isododecane, 5.00 parts by weight of polydimethylsiloxane, 12.00 parts by weight of dimethyl carbonate, 2.00 parts by weight of silanized n-decyl glucoside, 0.015 parts by weight of water, and 0.000 parts by weight of unavoidable process residues, totaling 100 parts by weight. The product of this embodiment is a medium-viscosity sprayable liquid used for cleaning external insulation surfaces with both general dirt and localized oil contamination.

[0125] Raw materials, components or material specifications

[0126] Isododecane was a commercially available high-purity liquid with a purity ≥99.0% and moisture content ≤0.005 wt%. Polydimethylsiloxane was a commercially available low-viscosity liquid with a kinematic viscosity of 8 mm² / s at 25°C and moisture content ≤0.010 wt%. Dimethyl carbonate was a commercially available anhydrous liquid with a purity ≥99.5% and moisture content ≤0.010 wt%. n-Decyl glucoside was a commercially available industrial-grade raw material with an active ingredient content ≥98.0%. 3-Glycidyl etheroxypropyltrimethoxysilane was a commercially available high-purity raw material with a purity ≥98.0%. Anhydrous potassium carbonate and anhydrous sodium sulfate were both commercially available analytical-grade solids, dried at 105°C for 2 hours before use and cooled to 25°C in a drying container. Nitrogen gas purity ≥99.99%.

[0127] Steps B1 to B6: Preparation of silanized n-decyl glucoside

[0128] Decyl glucoside, anhydrous potassium carbonate, and dimethyl carbonate were added to a reaction vessel equipped with mechanical stirring, reflux condenser, and nitrogen inlet to form a reaction system. Taking the molar amount of decyl glucoside as 1, the molar amount of 3-glycidyl etheroxypropyltrimethoxysilane was 0.35, and the molar amount of anhydrous potassium carbonate was 0.04, with the solid content of the reaction system controlled at 40.00 wt%. Under a nitrogen protective atmosphere, the mixture was stirred at 450 rpm for 20 min, and then 3-glycidyl etheroxypropyltrimethoxysilane was added to the reaction system over 45 min. The temperature was raised to 65 °C and the reaction was carried out for 7 h. During the reaction, a slight positive pressure of nitrogen was maintained at atmospheric pressure, and reflux condenser was used to maintain stability. The endpoint was determined by external standard chromatography, with the residual amount of unreacted 3-glycidyl etheroxypropyltrimethoxysilane being 0.25 wt%. After the reaction was completed, anhydrous potassium carbonate was removed by filtration at 28°C, and some dimethyl carbonate was removed under reduced pressure at 42°C and 7 kPa to obtain silanized n-decyl glucoside. In this example, the silanized n-decyl glucoside contained 1.30 wt% silicon and 0.050 wt% water.

[0129] Steps A1 to A5: Preparation of the silanized n-decyl glucoside reverse micelle intermediate

[0130] The silanized n-decyl glucoside obtained in step B6 was used as raw material A1. 100 parts by weight of isododecane, 24.00 parts by weight of dimethyl carbonate, and 4.00 parts by weight of silanized n-decyl glucoside were added to a sealed stirred container. After purging the container with nitrogen, the mixture was stirred at 30°C and 2500 rpm for 1.5 h. After stirring, 2.5 parts by weight of anhydrous sodium sulfate were added, and the mixture was further dehydrated at 30°C for 1.2 h. The anhydrous sodium sulfate was then removed by filtration through a 0.45 μm solvent-resistant filter membrane to obtain the silanized n-decyl glucoside reverse micelle intermediate. In this example, the intermediate had a moisture content of 0.015 wt%, a D50 particle size of 50 nm, and a polydispersity index of 0.18.

[0131] Steps C1 to C4: Preparation of the pre-dehydrated insulating continuous phase

[0132] By weight, 100 parts by weight of isododecane and 16.13 parts by weight of polydimethylsiloxane were added to a dry, sealed stirred container and stirred for 25 minutes at 30°C and 700 rpm. Then, 2.5 parts by weight of anhydrous sodium sulfate were added, and stirring continued at 30°C for 2.0 hours. After stirring, the anhydrous sodium sulfate was removed by filtration through a 0.45 μm solvent-resistant membrane to obtain a pre-dehydrated insulating continuous phase. The moisture content of the pre-dehydrated insulating continuous phase in this embodiment was 0.012 wt%.

[0133] Steps S1 to S5: Preparation of the live insulating cleaning agent

[0134] This embodiment provides a silanized n-decyl glucoside reverse micelle intermediate and a pre-dehydrated insulating continuous phase. Based on the measured composition of the intermediate and the continuous phase, the mass of both phases is calculated to ensure that the final cleaning agent contains isododecane, polydimethylsiloxane, dimethyl carbonate, silanized n-decyl glucoside, and water at the levels set in this embodiment. The silanized n-decyl glucoside reverse micelle intermediate and the pre-dehydrated insulating continuous phase are added to a sealed explosion-proof mixing device at a mass ratio of 1:0.56. Before adding the materials, the gas phase space of the device is purged with nitrogen, resulting in a gas phase oxygen content of 2.5 vol%. The mixture is stirred for 1.2 hours at 30°C and 900 r / min, maintaining a sealed environment and atmospheric pressure nitrogen protection during the stirring process. After stirring, end-point filtration is performed with a pore size of 0.45 μm, and the filtrate is the live insulating cleaning agent of this embodiment.

[0135] Quality testing methods and results

[0136] Moisture content was determined using the Karl Fischer coulometric method, with each sample analyzed in triplicate. The final cleaning agent moisture content in this embodiment was 0.015 ± 0.001 wt%. The silanized n-decyl glucoside reverse micelle intermediate and the final unfiltered mixture were subjected to dynamic light scattering analysis using a direct loading method at 25.0 °C. The final cleaning agent reverse micelle dispersed phase had a D50 particle size of 50 ± 2 nm and a polydispersity index of 0.18 ± 0.01. The dispersed phase with a particle size greater than 1.00 μm accounted for 2.00 vol% of the total dispersed phase. Free silanized n-decyl glucoside accounted for 8.00 wt% of the total silanized n-decyl glucoside.² 9SiNMR recorded a trimethoxysilylsilane signal at -41.5 ppm and a siloxane condensation-related silicon signal at -58 ppm. FTIR recorded a weakened characteristic absorption signal of epoxy groups, a Si-OC related absorption signal, and a Si-O-Si related absorption signal. The silicon content detection results were consistent with the quality control results in step B6. After the liquid samples were sealed and dispensed, the volume resistivity, power frequency breakdown voltage, dielectric loss factor, corrosivity, flash point, and cleaning rate were recorded. For volatile residue samples, the mass fraction of volatile residues was recorded. All detection records, along with moisture, D50 particle size, and polydispersity index, formed a batch quality record.

[0137] Features and application scenarios of this embodiment

[0138] This embodiment employs a combination of moderate reaction degree, moderate reverse micelle size, and moderate continuous phase viscosity. The mass ratio of silanized n-decyl glucoside to dimethyl carbonate is in the high wetting component region, making it suitable for balanced cleaning and maintenance in scenarios where conventional dirt and localized oil stains coexist.

[0139] Example 4

[0140] Overall production scale and product form

[0141] This embodiment prepares 1000.00g of liquid cleaning agent for live-line insulation applications at voltage levels of 500kV and above. Based on a total weight of 100 parts by weight of the cleaning agent, the composition includes 76.380 parts by weight of isododecane, 8.00 parts by weight of polydimethylsiloxane, 15.00 parts by weight of dimethyl carbonate, 0.60 parts by weight of silanized n-decyl glucoside, 0.020 parts by weight of water, and 0.000 parts by weight of unavoidable process residues, totaling 100 parts by weight. The product of this embodiment is a filtered liquid with controlled particle size distribution, suitable for high-voltage live-line cleaning applications within a wide process window.

[0142] Raw materials, components or material specifications

[0143] Isododecane was a commercially available high-purity liquid with a purity ≥99.0% and moisture content ≤0.005 wt%. Polydimethylsiloxane was a commercially available low-viscosity liquid with a kinematic viscosity of 10 mm² / s at 25°C and moisture content ≤0.010 wt%. Dimethyl carbonate was a commercially available anhydrous liquid with a purity ≥99.5% and moisture content ≤0.010 wt%. n-Decyl glucoside was a commercially available industrial-grade raw material with an active ingredient content ≥98.0%. 3-Glycidyl etheroxypropyltrimethoxysilane was a commercially available high-purity raw material with a purity ≥98.0%. Anhydrous potassium carbonate and anhydrous sodium sulfate were both commercially available analytical-grade solids, dried at 105°C for 2 hours and cooled to 25°C in a drying container before use. Nitrogen gas purity ≥99.99%.

[0144] Steps B1 to B6: Preparation of silanized n-decyl glucoside

[0145] Decyl glucoside, anhydrous potassium carbonate, and dimethyl carbonate were added to a reaction vessel equipped with mechanical stirring, reflux condenser, and nitrogen inlet to form a reaction system. Taking the molar amount of decyl glucoside as 1, the molar amount of 3-glycidyl etheroxypropyltrimethoxysilane was 0.50, and the molar amount of anhydrous potassium carbonate was 0.06, with the solid content of the reaction system controlled at 50.00 wt%. Under a nitrogen protective atmosphere, the mixture was stirred at 500 rpm for 20 min, and then 3-glycidyl etheroxypropyltrimethoxysilane was added to the reaction system over 50 min. The temperature was raised to 75 °C and the reaction was carried out for 8 h. During the reaction, a slight positive pressure of nitrogen was maintained at atmospheric pressure, and reflux condenser was used to maintain stability. The endpoint was determined by external standard chromatography, with the residual amount of unreacted 3-glycidyl etheroxypropyltrimethoxysilane being 0.35 wt%. After the reaction was completed, anhydrous potassium carbonate was removed by filtration at 28°C, and some dimethyl carbonate was removed under reduced pressure at 42°C and 7 kPa to obtain silanized n-decyl glucoside. In this example, the silanized n-decyl glucoside contained 2.00 wt% silicon and 0.080 wt% water.

[0146] Steps A1 to A5: Preparation of the silanized n-decyl glucoside reverse micelle intermediate

[0147] The silanized n-decyl glucoside obtained in step B6 was used as raw material A1. 100 parts by weight of isododecane, 30 parts by weight of dimethyl carbonate, and 1.2 parts by weight of silanized n-decyl glucoside were added to a sealed stirred container. After purging the container with nitrogen, the mixture was stirred at 25°C and 3500 rpm for 2.0 h. After stirring, 3.5 parts by weight of anhydrous sodium sulfate were added, and dehydration was continued at 25°C for 1.0 h. Then, the anhydrous sodium sulfate was removed by filtration through a 0.80 μm solvent-resistant filter membrane to obtain the silanized n-decyl glucoside reverse micelle intermediate. In this example, the intermediate had a moisture content of 0.020 wt%, a D50 particle size of 65 nm, and a polydispersity index of 0.22.

[0148] Steps C1 to C4: Preparation of the pre-dehydrated insulating continuous phase

[0149] By weight, 100 parts by weight of isododecane and 30.30 parts by weight of polydimethylsiloxane were added to a dry, sealed stirring vessel and stirred for 25 minutes at 25°C and 800 rpm. Then, 3.0 parts by weight of anhydrous sodium sulfate were added, and stirring continued at 25°C for 3.0 hours. After stirring, the anhydrous sodium sulfate was removed by filtration through a 0.80 μm solvent-resistant membrane to obtain a pre-dehydrated insulating continuous phase. The moisture content of the pre-dehydrated insulating continuous phase in this embodiment was 0.020 wt%.

[0150] Steps S1 to S5: Preparation of the live insulating cleaning agent

[0151] This embodiment provides a silanized n-decyl glucoside reverse micelle intermediate and a pre-dehydrated insulating continuous phase. Based on the measured composition of the intermediate and the continuous phase, the mass of both phases is calculated to ensure that the final cleaning agent contains isododecane, polydimethylsiloxane, dimethyl carbonate, silanized n-decyl glucoside, and water at the levels set in this embodiment. The silanized n-decyl glucoside reverse micelle intermediate and the pre-dehydrated insulating continuous phase are added to a sealed explosion-proof mixing device at a mass ratio of 1:0.52. Before adding the materials, the gas phase space of the device is purged with nitrogen, resulting in a gas phase oxygen content of 1.0 vol%. The mixture is stirred for 1.5 hours at 25°C and 1200 r / min, maintaining a sealed environment and atmospheric pressure nitrogen protection during the stirring process. After stirring, end-point filtration is performed with a pore size of 0.80 μm, and the filtrate is the live insulating cleaning agent of this embodiment.

[0152] Quality testing methods and results

[0153] Moisture content was determined using the Karl Fischer coulometric method, with each sample analyzed in triplicate. The final cleaning agent moisture content in this embodiment was 0.020 ± 0.001 wt%. The silanized n-decyl glucoside reverse micelle intermediate and the final pre-filtration mixture were subjected to dynamic light scattering analysis using a direct loading method at 25.0 °C. The final cleaning agent reverse micelle dispersed phase had a D50 particle size of 65 ± 2 nm and a polydispersity index of 0.22 ± 0.01. Dispersed phase particles larger than 1.00 μm accounted for 4.00 vol% of the total dispersed phase. Free silanized n-decyl glucoside accounted for 15.00 wt% of the total silanized n-decyl glucoside.² 9 SiNMR recorded a trimethoxysilylsilane signal at -42 ppm and a siloxane condensation-related silicon signal at -55 ppm. FTIR recorded a weakened characteristic absorption signal of epoxy groups, a Si-OC related absorption signal, and a Si-O-Si related absorption signal. The silicon content detection results were consistent with the quality control results in step B6. After the liquid samples were sealed and dispensed, the volume resistivity, power frequency breakdown voltage, dielectric loss factor, corrosivity, flash point, and cleaning rate were recorded. For volatile residue samples, the mass fraction of volatile residues was recorded. All detection records, along with moisture, D50 particle size, and polydispersity index, formed the batch quality record.

[0154] Features and application scenarios of this embodiment

[0155] This embodiment uses a relatively high polydimethylsiloxane ratio and a relatively high dimethyl carbonate ratio, while maintaining a low amount of silanized n-decyl glucoside. The filter pore size and stirring conditions are within a wide process window, making it suitable for high-voltage equipment maintenance scenarios that require good flowability, filtration adaptability, and cleaning and spreading properties.

[0156] Comparative Example 1: Basically the same as Example 1, except that the final content of polydimethylsiloxane in the live insulating cleaner was adjusted to 1.50 parts by weight, and isododecane was added to make up the balance, while other conditions remained unchanged.

[0157] Comparative Example 2: Basically the same as Example 1, except that the final content of dimethyl carbonate in the live insulating cleaner was adjusted to 3.50 parts by weight, and isododecane was added to make up the balance, while other conditions remained unchanged.

[0158] Comparative Example 3: It is basically the same as Example 1, except that the final content of silanized n-decyl glucoside in the live insulating cleaning agent is adjusted to 0.10 parts by weight, and isododecane is added to make up the balance, while other conditions remain unchanged.

[0159] Comparative Example 4: It is basically the same as Example 1, except that before filtration in step S5, the water content of the final cleaning agent is adjusted to 0.050 parts by weight using aqueous isododecane calibrated by the Karl Fischer coulometric method, while other conditions remain unchanged.

[0160] Comparative Example 5: It is basically the same as Example 1, except that in step B2, the molar amount of n-decyl glucoside is taken as 1, the molar amount of 3-glycidyl etheroxypropyltrimethoxysilane is adjusted to 0.05, and the molar amount of anhydrous potassium carbonate, the solid content of the reaction system, the reaction temperature, the reaction time, the filtration and vacuum removal conditions remain unchanged.

[0161] Comparative Example 6: It is basically the same as Example 1, except that the stirring rate in step A3 is adjusted to 600 r / min, the stirring temperature is 20℃ and the stirring time is 0.5 h, and other conditions remain unchanged.

[0162] Comparative Example 7: It is basically the same as Example 1, except that the stirring time in step A3 is adjusted to 0.25h, the stirring temperature of 20℃ and the stirring speed of 1000r / min remain unchanged, and other conditions remain unchanged.

[0163] Comparative Example 8: It is basically the same as Example 1, except that the end filter pore size in step S5 is adjusted to 1.50 μm, while the filter object, filtration temperature and the method of collecting the filtrate after filtration remain unchanged, and other conditions remain unchanged.

[0164] Comparative Example 9: Essentially the same as Example 1, except that silanized n-decyl glucoside was not added. In step A2, only 100 parts by weight of isododecane and 12.50 parts by weight of dimethyl carbonate were added to a sealed stirring vessel. Subsequent stirring, dehydration, filtration, and steps S1 to S5 were performed as in Example 1. The final content of silanized n-decyl glucoside in the final cleaning agent was 0.00 parts by weight, with isododecane made up to the balance. Other conditions remained unchanged. This comparative example was used to verify the synergistic effect of silanized n-decyl glucoside and dimethyl carbonate in forming a reverse micelle interface in isododecane.

[0165] Comparative Example 10: Essentially the same as Example 1, except that dimethyl carbonate was not added. In step A2, only 100 parts by weight of isododecane and 0.5 parts by weight of silanized n-decyl glucoside were added to a sealed stirred container. Subsequent stirring, dehydration, filtration, and steps S1 to S5 were performed as in Example 1. The final content of dimethyl carbonate in the final cleaning agent was 0.00 parts by weight, with isododecane added to make up the balance. Other conditions remained unchanged. This comparative example was used to verify the synergistic effect of silanized n-decyl glucoside and dimethyl carbonate in forming a reverse micelle interface in isododecane.

[0166] Comparative Example 11: Essentially the same as Example 1, except that the pre-construction process of the silanized n-decyl glucoside reverse micelle intermediate in steps A1 to A5 was omitted. Instead, in step S3, 0.20 parts by weight of silanized n-decyl glucoside, 5.00 parts by weight of dimethyl carbonate, and the corresponding balance of isododecane were directly added to the pre-dehydrated insulating continuous phase. After stirring at 20°C and 300 r / min for 0.5 h, the mixture was filtered through a 0.20 μm end filter. Other conditions remained unchanged. This comparative example was used to verify the synergistic effect of the pre-construction sequence of the reverse micelle intermediate and the mixing sequence of the pre-dehydrated insulating continuous phase.

[0167] Characterization and performance testing:

[0168] The moisture content control experiment was used to evaluate trace moisture in charged insulating cleaning agents, silanized n-decyl glucoside reverse micelle intermediates, and pre-dehydrated insulating continuous phases. The Karl Fischer coulometric method was employed. Samples were taken in a sealed, dry syringe, and the sample mass, endpoint charge, and converted moisture mass were recorded. The test temperature was 25 ± 2 °C, with n = 3 samples per batch. Results were expressed as wt% and mean ± standard deviation, with the criterion being a final cleaning agent moisture content of 0.005–0.030 wt%. The method referenced ASTM D6304-25, ISO 12937:2000, and GB / T 7600-2014. ASTM D6304-25 is applicable to the coulometric determination of moisture in systems such as petroleum products; ISO 12937 specifies the coulometric Karl Fischer titration method for moisture in petroleum products; and GB / T 7600-2014 specifies the coulometric determination of moisture content in transformer oil and turbine oil.

[0169] The reverse micelle size and polydispersity index (PDI) assay was used to evaluate the particle size retention of the reverse micelle dispersion phase of silanized n-decyl glucoside. The intermediate from step A5, the mixture before filtration at the end of step S4 and step S5, and the final filtrate were directly packaged as stock solutions. Dynamic light scattering (DLS) was used to detect intensity distribution, volume distribution, D50 particle size, and polydispersity index (PDI). The test temperature was 25 ± 0.1 °C, and each sample was repeated three times. Data are expressed as mean ± standard deviation of D50 and mean ± standard deviation of PDI. The target values ​​were D50 20–80 nm and PDI 0.08–0.30. The method followed ISO 22412:2025 Dynamic Light Scattering Particle Size Analysis.

[0170] Volume resistivity and dielectric loss factor experiments were used to evaluate the liquid insulation suitability of cleaning agents in high-voltage live cleaning scenarios. The final filtrate was mixed thoroughly in a sealed container and then injected into the liquid insulation test electrode cup. Measurements were taken at 25±1℃ and 90±1℃, and the DC volume resistivity, relative permittivity, and dielectric loss factor tanδ were recorded. Results are expressed as mean ± standard deviation. The methods followed GB / T 5654-2007 and IEC 60247:2004, both of which are used for measuring the relative permittivity, dielectric loss factor, and DC resistivity of liquid insulating materials.

[0171] The power frequency breakdown voltage test is used to evaluate the dielectric strength of cleaning agents under a power frequency electric field. After the final filtrate is allowed to stand and defoam, it is injected into a standard oil cup. Spherical or hemispherical electrodes are used with an electrode spacing of 2.5 mm. The voltage rise rate is set according to the standard method. The breakdown voltage is recorded. At least 6 breakdowns are required for each sample, and abnormal discharges are discarded. The results are expressed as kV / 2.5 mm and the mean ± standard deviation. The method refers to IEC 60156:2025, which is used for the determination of power frequency breakdown voltage of insulating liquids and is applicable to insulating liquids with a nominal viscosity not exceeding 350 mm² / s.

[0172] The cleaning, wetting, and decontamination rate tests are used to evaluate the wetting, spreading, and contamination-carrying capacity of cleaning agents on the surface of external insulation. Using ceramic or glass insulator simulants as substrates, a standardized salt-grease composite contamination layer is coated and dried to constant weight. A measured amount of cleaning agent is sprayed on, and the mixture is allowed to stand for 60 seconds. Then, it is rinsed or wiped at a constant flow rate. The mass of contamination before and after cleaning is recorded, and the cleaning rate is calculated. Simultaneously, the dynamic contact angles at 5s, 30s, and 60s are recorded. Contact angle measurements are performed according to ASTM D7334-08 (2022), and the decontamination rate is calculated using the mass difference method.

[0173] Processing fluidity, flash point, and volatile residue tests were used to evaluate the spray flow, safety management, and residue control of the cleaning agent. Kinematic viscosity was measured using a capillary viscometer at 25±0.1℃, and the result was mm² / s; closed-cup flash point was measured using the Binsky-Martin closed-cup cup method, and the result was °C; for volatile residue, a quantitative sample was evaporated in a water bath and dried to constant weight at 110±2℃, and the mass fraction was calculated. Viscosity referenced ASTM D445-24 or ISO 3104:2023, flash point referenced ASTM D93-25 or ISO 2719:2025, and residue referenced ASTM D1353-13(2021) or ISO 759:1981.

[0174] Corrosion and material compatibility tests were used to evaluate the effects of cleaning agents on metallic conductors, fittings, and external insulation materials. For copper sheet corrosion, polished copper sheets were immersed in the cleaning agent at 50±1℃ for 3 hours, and then compared with a standard corrosion color chart. The mass change of the copper sheet was recorded. Silicone rubber and EPDM rubber samples were immersed at 25±2℃ for 24 hours, and the mass change rate, hardness change, and surface condition were recorded. Copper sheet corrosion was performed according to ASTM D130-26, and material compatibility was evaluated using the equivalent immersion mass change method and hardness retention rate.

[0175] Figure 1 This is a DLS intensity-weighted particle size distribution diagram of the charged insulating cleaning agent of the present invention. Figure 2 This is a DLS cumulative volume distribution diagram of the electrically conductive insulating cleaning agent of the present invention. Both are used together to evaluate the particle size distribution of the reverse micelle dispersed phase. Figure 1 As can be seen, the intensity distribution peak of Example 1 is concentrated around approximately 20 nm, with a relatively narrow peak shape; the distribution peaks of Comparative Examples 9 and 11 shift towards approximately 350 nm and approximately 120 nm, respectively, accompanied by an increase in peak width. Figure 2 As can be seen, the cumulative distribution curve of Example 1 rises rapidly and reaches a plateau in the smaller particle size range, while the curves of Comparative Examples 9 and 11 shift to the right overall, indicating an increase in the proportion of coarse dispersed phase. These results demonstrate that constructing a reverse micelle intermediate in the isododecane continuous phase using silanized n-decyl glucoside and dimethyl carbonate is beneficial for the cleaning and wetting components to exist in a more concentrated nanoscale dispersion, thus providing a dispersion structure basis for achieving both insulation and cleaning / wetting properties.

[0176] Figure 3 This is a statistical chart of the D50 particle size of the electrically insulating cleaning agent of the present invention. Figure 4 This is a statistical chart of the polydispersity index (PDI) of the electrically insulating cleaning agent of this invention. The two figures further verify the statistical parameters. Figure 1 and Figure 2The trends shown are as follows: In Example 1, the D50 particle size was approximately 20 nm, and the PDI was approximately 0.08; in Comparative Example 9, after removing silanized n-decyl glucoside, the D50 particle size increased to approximately 350 nm, and the PDI increased to approximately 0.62; in Comparative Example 11, after eliminating the preconstruction of the reverse micelle intermediate, the D50 particle size increased to approximately 120 nm, and the PDI increased to approximately 0.40. These results indicate that it is difficult to obtain a narrow-distribution nano-dispersed phase by simply having dimethyl carbonate or directly mixing the components. The interfacial regulation effect of silanized n-decyl glucoside and the preconstruction order of the reverse micelle intermediate have a significant impact on particle size control and dispersion uniformity.

[0177] Figure 5 This is a statistical chart showing the proportion of free silanized n-decyl glucoside in the electrically insulating cleaning agent of this invention. Figure 6 This is a correlation diagram between the free state ratio and D50 particle size of the electrically insulating cleaning agent of this invention. Both diagrams illustrate the relationship between the existence form of the wetting component and particle size coarsening. Figure 5 As can be seen, the proportion of free silanized n-decyl glucoside in Example 1 is close to 0 wt%, while that in Comparative Examples 10 and 11 increases to approximately 29 wt% and approximately 20 wt%, respectively. Figure 6 It is evident that the D50 particle size generally increases with the increase of the proportion of free state. Example 1 is located in the region of low free state proportion and small D50 particle size, while Comparative Examples 10 and 11 deviate significantly. This result indicates that the participation of dimethyl carbonate in the construction of reverse micelles and the intermediate preconstruction process can promote the entry of silanized n-decyl glucoside into the dispersed phase interface, reduce its existence in the free state, and thus reduce the risk of coarse dispersion and particle size enlargement.

[0178] Figure 7 The 2nd silanized n-decyl glucoside of this invention 9 Si NMR spectrum overlay Figure 8 The 2nd silanized n-decyl glucoside of this invention 9 The normalized peak area statistics of Si NMR are used to evaluate the assignment of silicon-related structural signals. Figure 7 As can be seen, Example 1 exhibits silicon-related signals near approximately -43 ppm and approximately -67 ppm, while the corresponding signal intensity of Comparative Example 5 is lower. Figure 8 As can be seen, the normalized peak areas of trimethoxysilylsilane and siloxane condensation-related silicon in Example 1 are both higher than those in Comparative Example 5. Combined with the reduced molar amount of 3-glycidyl etheroxypropyltrimethoxysilane in Comparative Example 5, it can be seen that the appropriate introduction of 3-glycidyl etheroxypropyltrimethoxysilane is beneficial for the formation of silanized n-decyl glucoside with silicon-related structural characteristics, providing a structural basis for its subsequent participation in reverse micelle interface regulation.

[0179] Figure 9This is a superimposed image of the FTIR absorption spectra of silanized n-decyl glucoside of the present invention. Figure 10 This is a statistical chart of the normalized area of ​​the FTIR characteristic peaks of silanized n-decyl glucoside of the present invention. The two peaks are compared from the perspective of infrared absorption. Figure 7 and Figure 8 The structural attribution is used for auxiliary verification. Figure 9 As can be seen, in Example 1, the response of the Si-OC and Si-O-Si correlated absorption regions is enhanced, while the epoxy-related absorption is relatively weakened; in Comparative Example 5, the silicon-oxygen correlated absorption is weaker. Figure 10 As can be seen, the Si-OC and Si-O-Si related peak areas in Example 1 are relatively high, while the epoxy-related peak areas are relatively low, whereas Comparative Example 5 shows the opposite trend. These results indicate that the binding or interaction between the wetting structure and the silane structure in Example 1 is more complete, and the resulting silanized n-decyl glucoside is more suitable for playing an interfacial stabilizing and wetting-regulating role in a nonpolar continuous phase.

[0180] Figure 11 This is a graph showing the correlation between the volume resistivity and D50 particle size of the charged insulating cleaning agent of this invention. Figure 12 This is a correlation diagram between the power frequency breakdown voltage and PDI of the charged insulating cleaning agent of this invention. Both are used to evaluate the influence of particle size distribution on insulation performance. Figure 11 As can be seen, the volume resistivity of Example 1 at a D50 of approximately 20 nm is approximately 9.20 × 10¹³ Ω·cm, while the volume resistivity of Comparative Examples 4 and 11 decreases after changes in moisture or dispersion state. Figure 12 As can be seen, the power frequency breakdown voltage of Example 1 is approximately 74.0 kV / 2.5 mm at a PDI of approximately 0.08, while the breakdown voltage of Comparative Examples 4 and 11 decreases with increasing PDI. This result indicates that smaller and more concentrated reverse micelle dispersions are beneficial in reducing the influence of non-uniform polar microregions and coarse dispersions on the electric field distribution within the system, thereby maintaining the insulating properties of the cleaning agent.

[0181] Figure 13 This diagram illustrates the correlation between the moisture content and dielectric loss factor of the live-line insulating cleaning agent of the present invention, further demonstrating the impact of moisture control on dielectric loss. In Example 1, the moisture content was approximately 0.005 wt%, and the tanδ was approximately 0.80 × 10⁻³. In Comparative Example 4, the tanδ increased significantly after the moisture content was increased to approximately 0.050 wt%. These results indicate that trace amounts of moisture are a crucial factor affecting the dielectric loss of insulating liquids. Example 1, through a process combining dehydration of the reverse micelle intermediate, preparation of a pre-dehydrated continuous insulating phase, and end-stage filtration, maintains a low moisture content in the final cleaning agent, which is beneficial for reducing dielectric loss and improving the safety margin in live-line cleaning applications.

[0182] Figure 14This is a graph showing the dynamic contact angle of the electrically insulating cleaning agent of the present invention changing over time. Figure 15 This is a statistical chart showing the standard dirt layer cleaning rate of the electrically insulating cleaning agent of this invention. Both are used to evaluate the cleaning wetting performance and detergency. Figure 14 As can be seen, the contact angle of Example 1 decreased to approximately 26° at 60 s, while the contact angles of Comparative Examples 9 and 10 decreased more slowly but reached higher final values, indicating that Example 1 spread more quickly on the contaminated surface. Figure 15 As can be seen, the cleaning rate of Example 1 was approximately 90.5%, while that of Comparative Examples 9 and 10 was approximately 62.5% and 74.8%, respectively. These results indicate that the absence of silanized n-decyl glucoside or dimethyl carbonate weakens wetting, spreading, and dirt-carrying cleaning capabilities. However, their combined participation in the construction of the reverse micelle interface allows the cleaning and wetting components to act on the dirt layer surface in a more effective dispersed form.

[0183] Figure 16 This is a correlation diagram between the 60 s contact angle and the cleaning rate of the electrically insulating cleaning agent of this invention, used to comprehensively illustrate the correspondence between wetting and spreading ability and cleaning results. Figure 16 It is evident that the overall cleaning rate increases as the contact angle decreases at 60 s; Example 1 falls within the low contact angle and high cleaning rate region, while Comparative Examples 9 and 10 exhibit higher contact angles and lower cleaning rates. (Combined with...) Figure 14 and Figure 15 It is evident that Example 1 does not improve the cleaning rate solely by increasing the amount of wetting components, but rather by regulating the reverse micelle dispersion between the continuous phases of silanized n-decyl glucoside, dimethyl carbonate, and isododecane, thereby enabling wetting and dirt removal to work in tandem and thus improving the overall cleaning performance.

[0184] Figure 17 This is a macroscopic optical photograph of the charged insulating cleaning agent from Example 1, used to observe the uniformity of the final product's appearance and its stable state after standing. Figure 17 As can be seen, Example 1 is a colorless, transparent to very pale opalescent, low-viscosity liquid with a continuous surface. No visible sedimentation, stratification, flocculation, or suspended particles were observed. Considering the moisture content of Example 1 (0.005±0.001 wt%), D50 particle size of 20±1 nm, and PDI of 0.08±0.01, it can be seen that the isododecane continuous phase, polydimethylsiloxane, dimethyl carbonate, and silanized n-decyl glucoside exhibit good macroscopic compatibility under the low moisture and reverse micelle construction conditions, indicating that this system is not prone to forming visible coarse phase separation structures.

[0185] Figure 18 The image shows a SEM image of the residual layer after the electrical insulating cleaning agent of Example 1 evaporates following drop coating. This image is used to evaluate the residual morphology and risk of coarse particles after the cleaning agent evaporates on the solid substrate surface. Figure 18Image a is a low-magnification SEM image, showing that no obvious micron-sized aggregates, salt crystals, through-cracks, or local accumulations were observed in the residual layer within a large observation area; Figure 18 b and Figure 18 c is a medium-to-high magnification SEM image, which can observe nanoscale domains ranging from tens of nanometers to hundreds of nanometers. Its scale is consistent with the D50 of 20±1 nm measured by DLS of the original solution. Figure 18 Image d is a cross-sectional or local interface SEM image used to show the continuity of the residual layer and its contact state with the substrate. The above results indicate that, after end-filtering and low-moisture control, Example 1 is less likely to form coarse particle residues during the volatilization process, which helps to reduce the risk of secondary contamination and local accumulation on the outer insulation surface.

[0186] Figure 19 This is a TEM image of the reverse micelle dispersion phase of the charged insulating cleaning agent in Example 1, used for further observation of the microstructure of the nano-dispersion phase. Figure 19 As can be seen, the reverse micelle dispersed phase mainly consists of weakly contrasted quasi-spherical nanodomains on the order of 20 nm. Figure 19 b is a magnified view of a portion of the image, showing that the boundaries of the nanodomains are relatively soft, consistent with the characteristics of a soft nanodispersion formed by a polar inner region, an amphiphilic interface layer, and a nonpolar external environment. Combined with the results of Example 1—a D50 particle size of 20±1 nm, a PDI of 0.08±0.01, and a free silanized n-decyl glucoside ratio close to 0 wt%—this indicates that the reverse micelle dispersion has a narrow size distribution and high dispersion consistency, supporting the aforementioned results regarding DLS, insulation performance, and cleaning and wetting properties at the microscopic level.

[0187] Table 1 Comparison of Dispersion Stability and Insulation Performance

[0188] Sample number Moisture content (wt%) D50 particle size nm Multidispersive Index (PDI) Volume resistivity × 10^13 Ω·cm Power frequency breakdown voltage kV / 2.5mm Dielectric loss factor tanδ×10^-3 Example 1 0.005±0.001 20±1 0.08±0.01 9.20±0.25 74.0±1.8 0.80±0.05 Example 2 0.030±0.002 80±3 0.30±0.02 6.40±0.22 66.0±2.1 1.70±0.08 Example 3 0.015±0.001 50±2 0.18±0.01 7.70±0.24 70.5±1.9 1.10±0.06 Example 4 0.020±0.001 65±2 0.22±0.01 7.10±0.23 68.8±2.0 1.35±0.07 Comparative Example 1 0.006±0.001 24±2 0.11±0.01 8.50±0.28 71.2±2.0 0.95±0.06 Comparative Example 2 0.006±0.001 42±4 0.24±0.02 7.80±0.30 68.0±2.2 1.25±0.07 Comparative Example 3 0.006±0.001 58±5 0.31±0.03 6.90±0.32 64.5±2.4 1.55±0.09 Comparative Example 4 0.050±0.003 35±4 0.20±0.02 4.20±0.20 56.5±2.8 3.10±0.15 Comparative Example 5 0.006±0.001 95±8 0.36±0.03 5.80±0.26 61.0±2.6 2.05±0.12 Comparative Example 6 0.006±0.001 105±10 0.42±0.04 5.50±0.25 59.8±2.7 2.20±0.14 Comparative Example 7 0.006±0.001 88±7 0.35±0.03 5.95±0.27 62.2±2.5 1.95±0.11 Comparative Example 8 0.006±0.001 26±3 0.14±0.02 7.50±0.25 65.8±2.3 1.35±0.08 Comparative Example 9 0.006±0.001 350±25 0.62±0.05 3.80±0.18 52.5±3.0 3.80±0.20 Comparative Example 10 0.006±0.001 160±16 0.45±0.04 6.20±0.24 60.5±2.6 2.35±0.13 Comparative Example 11 0.006±0.001 120±12 0.40±0.04 5.90±0.23 61.8±2.5 2.10±0.12

[0189] Table 2 Comparison of Flow Cleaning Performance, Safety, and Residual Corrosion Performance

[0190] Sample number kinematic viscosity (mm² / s) Cleaning rate % Closed-cup flash point (°C) Copper sheet mass change (mg / cm²) Volatile residues (wt%) Example 1 1.28±0.03 90.5±1.1 43.5±0.6 0.02±0.01 0.010±0.002 Example 2 2.42±0.05 95.8±1.3 37.8±0.7 0.05±0.01 0.020±0.003 Example 3 1.85±0.04 95.2±1.0 40.8±0.6 0.03±0.01 0.015±0.002 Example 4 2.25±0.05 93.8±1.2 39.2±0.7 0.04±0.01 0.014±0.002 Comparative Example 1 1.15±0.03 88.8±1.4 44.2±0.6 0.03±0.01 0.012±0.002 Comparative Example 2 1.22±0.03 82.4±1.6 45.8±0.8 0.03±0.01 0.011±0.002 Comparative Example 3 1.24±0.03 78.6±1.8 43.9±0.7 0.04±0.01 0.012±0.002 Comparative Example 4 1.30±0.04 89.7±1.3 43.0±0.8 0.09±0.02 0.013±0.002 Comparative Example 5 1.31±0.04 83.2±1.7 43.3±0.7 0.05±0.01 0.016±0.003 Comparative Example 6 1.29±0.04 84.0±1.6 43.4±0.7 0.05±0.01 0.017±0.003 Comparative Example 7 1.28±0.04 85.6±1.5 43.5±0.7 0.05±0.01 0.016±0.003 Comparative Example 8 1.28±0.03 89.8±1.2 43.5±0.6 0.04±0.01 0.025±0.004 Comparative Example 9 1.18±0.03 62.5±2.4 43.8±0.7 0.06±0.02 0.018±0.003 Comparative Example 10 1.33±0.04 74.8±2.0 47.5±0.8 0.04±0.01 0.014±0.003 Comparative Example 11 1.30±0.04 81.5±1.8 43.6±0.7 0.05±0.01 0.018±0.003

[0191] As can be seen from the performance of the examples and comparative examples in Tables 1 and 2, Example 1 maintains high volume resistivity, high power frequency breakdown voltage and low dielectric loss under low moisture, small particle size and low PDI conditions, indicating that the synergistic control of reverse micelle particle size and moisture is beneficial to maintaining insulation performance. Examples 2 to 4 respectively reflect different formulation windows of high wetting component / high polydimethylsiloxane loading, medium wetting component loading and high dimethyl carbonate / high polydimethylsiloxane loading. The overall cleaning rate and wetting ability remain at a high level, and the volume resistivity and breakdown voltage show reasonable fluctuations or decreasing trends with changes in moisture, particle size, PDI and polar component loading. Comparative Examples 1 to 8, by changing the continuous phase, polar co-solvent component, moisture content, degree of silanization, stirring and filtration conditions, mainly resulted in a wider particle size distribution, a decrease in insulation performance, or insufficient cleaning rate. Comparative Examples 9 to 11 further showed that when silanized n-decyl glucoside, dimethyl carbonate, or the reverse micelle intermediate preconstruction was omitted, D50 and PDI deviated significantly, and the cleaning rate and insulation performance were difficult to maintain simultaneously. This is consistent with the technical logic of this invention, which aims to achieve a synergistic balance between dispersion stability, insulation performance, and cleaning and wetting performance by constructing around the reverse micelle interface.

[0192] Finally, it should be noted that the above embodiments are only used to illustrate the technical solutions of the present invention and not to limit it. Although the present invention has been described in detail with reference to the above embodiments, those skilled in the art should understand that any equivalent structural transformations made under the concept of the present invention and using the contents of the specification and drawings of the present invention should be covered within the scope of protection of the claims of the present invention.

Claims

1. A cleaning agent for live-line insulation at voltage levels of 500kV and above, characterized in that, Based on a total weight of 100 parts by weight, the charged insulating cleaning agent comprises the following components and process residues that are unavoidably introduced during the preparation process: Isododecane is the remainder after deducting the other components and the process residues, and its final content is 71.37-92.80 parts by weight; Polydimethylsiloxane 2.00-8.00 parts by weight; Dimethyl carbonate, 5.00-18.00 parts by weight; 0.20-2.50 parts by weight of silanized n-decyl glucoside; Moisture content: 0.005-0.030 parts by weight; Process residual components: 0-0.10 parts by weight; The above contents are the final contents of the corresponding components in the charged insulating cleaning agent. The total final contents of isododecane, polydimethylsiloxane, dimethyl carbonate, silanized n-decyl glucoside, water and the process residue components are 100 parts by weight. The silanized n-decyl glucoside is obtained by reacting n-decyl glucoside with 3-glycidyl etheroxypropyltrimethoxysilane.

2. The electrically insulating cleaning agent according to claim 1, characterized in that, The silanized n-decyl glucoside reverse micelle intermediate is prepared by the following steps: A1. To provide the silanized n-decyl glucoside; A2. By weight, add 100 parts isododecane, 5-35 parts dimethyl carbonate and 0.5-8 parts silanized n-decyl glucoside to a sealed stirring container. A3. Stir for 0.5-3.0 h at 20-35℃ and 1000-4000 r / min under a nitrogen protective atmosphere; A4. Add 0.5-5.0 parts by weight of anhydrous sodium sulfate and contact for dehydration for 0.5-2.0 hours, then filter to remove the anhydrous sodium sulfate; A5. Control the moisture content of the obtained dispersion to be 0.005-0.030 wt%, the D50 particle size to be 20-80 nm, and the polydispersity index to be 0.08-0.30, to obtain the silanized n-decyl glucoside reverse micelle intermediate.

3. The electrically insulating cleaning agent according to claim 2, characterized in that, The silanized n-decyl glucoside in step A1 is prepared by the following steps: B1. Add n-decyl glucoside, anhydrous potassium carbonate, and dimethyl carbonate to the reaction vessel to form a reaction system; B2. With the molar amount of n-decyl glucoside as 1, the molar amount of 3-glycidyl etheroxypropyltrimethoxysilane is 0.10-0.60, and the molar amount of anhydrous potassium carbonate is 0.01-0.

08. B3. The solid content of the reaction system is controlled to be 20.00-60.00 wt%; B4. Under a nitrogen protective atmosphere, 3-glycidyl etheroxypropyltrimethoxysilane is added to the reaction system and reacted at 55-80°C for 4-10 h; B5. When the residual amount of unreacted 3-glycidyl ether oxypropyltrimethoxysilane is detected to be 0.05-0.50 wt%, the reaction shall be stopped; B6. Filter to remove anhydrous potassium carbonate, remove part of dimethyl carbonate under reduced pressure, and control the silicon content in the product to be 0.20-2.50 wt% and the moisture content to be 0.005-0.100 wt% to obtain the silanized n-decyl glucoside.

4. The electrically insulating cleaning agent according to claim 3, characterized in that, The isododecane and the polydimethylsiloxane are first prepared into a pre-dehydrated insulating continuous phase, which is prepared through the following steps: C1. By weight, 100 parts by weight of isododecane are mixed with 2.75-40.00 parts by weight of polydimethylsiloxane; C2. Add 0.5-5.0 parts by weight of anhydrous sodium sulfate and stir at 20-35℃ for 0.5-4.0 hours; C3. Filter to remove anhydrous sodium sulfate; C4. Control the moisture content of the obtained liquid phase to 0.005-0.020 wt% to obtain the pre-dehydrated insulating continuous phase.

5. The electrically insulating cleaning agent according to claim 1, characterized in that, The mass ratio of the silanized n-decyl glucoside to the dimethyl carbonate is 1:6 to 1:25; in the electrically insulating cleaning agent, the free silanized n-decyl glucoside accounts for 0-20.00 wt% of the total silanized n-decyl glucoside, and the dispersed phase with a particle size greater than 1.00 μm accounts for 0-5.00 vol% of the total dispersed phase.

6. The electrically insulating cleaning agent according to claim 1, characterized in that, The charged insulating cleaning agent does not contain 1,1,2-trichloro-1,2,2-trifluoroethane, dichloromethane, 1,1,1-trichloroethane, or carbon tetrachloride, nor does it contain any ionic antistatic additives.

7. A method for preparing a live insulating cleaning agent for voltage levels of 500kV and above as described in any one of claims 1-6, characterized in that, Includes the following steps: S1. Provides a silanized n-decyl glucoside reverse micelle intermediate, wherein the silanized n-decyl glucoside reverse micelle intermediate is a reverse micelle intermediate formed by silanized n-decyl glucoside, dimethyl carbonate and isododecane; S2. Providing a pre-dehydrated insulating continuous phase, said pre-dehydrated insulating continuous phase being obtained by dehydrating and mixing isododecane and polydimethylsiloxane; S3. The silanized n-decyl glucoside reverse micelle intermediate is mixed with the pre-dehydrated insulating continuous phase at a mass ratio of 1:0.4 to 1:3.0; S4. Stir at 20-35℃ and 300-1500 r / min for 0.5-2.0 h; S5. Filter to obtain the charged insulating cleaning agent; The electrical insulating cleaning agent has a moisture content of 0.005-0.030 wt%, and the reverse micelle dispersed phase in the electrical insulating cleaning agent has a D50 particle size of 20-80 nm and a polydispersity index of 0.08-0.

30.

8. The preparation method according to claim 7, characterized in that, In step S3, the mass ratio of the silanized n-decyl glucoside reverse micelle intermediate to the pre-dehydrated insulating continuous phase is 1:0.4 to 1:3.0, the mixing temperature is 20-35℃, the stirring rate is 300-1500 r / min, and the mixing time is 0.5-2.0 h.

9. The preparation method according to claim 7, characterized in that, The preparation process of the silanized n-decyl glucoside reverse micelle intermediate provided in step S1 and step S3 are both carried out in a closed explosion-proof stirring device. The operating temperature of the closed explosion-proof stirring device is 20-35℃, and the oxygen content in the gas phase inside the device is 0.1-5.0 vol.

10. The preparation method according to claim 8, characterized in that, The filtration in step S4 includes end filtration with a pore size of 0.20-1.00 μm, and the dispersed phase with a particle size greater than 1.00 μm after filtration accounts for 0-5.00 vol of the total dispersed phase.

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