CN116656211A - Water-based epoxy insulating paint and preparation method thereof - Google Patents

Water-based epoxy insulating paint and preparation method thereof Download PDF

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CN116656211A
CN116656211A CN202310699876.9A CN202310699876A CN116656211A CN 116656211 A CN116656211 A CN 116656211A CN 202310699876 A CN202310699876 A CN 202310699876A CN 116656211 A CN116656211 A CN 116656211A
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insulating paint
acetonitrile
parts
water
reaction
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CN116656211B (en
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沈庆
刘翔
汪太平
胡坤
张斌
张�杰
李淑心
陈明阳
李延东
张志强
黄永生
赵巨龙
胡可
房姗姗
杨娇娇
丁诗洋
崔玮
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Super High Voltage Branch Of State Grid Anhui Electric Power Co ltd
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Super High Voltage Branch Of State Grid Anhui Electric Power Co ltd
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Abstract

The invention discloses a water-based epoxy insulating paint and a preparation method thereof, which belong to the technical field of insulating paint and comprise the following raw materials in parts by weight: 50-60 parts of water-based epoxy resin, 9-11 parts of auxiliary agent, 10-16 parts of pigment and filler, 18-22 parts of curing agent, 0.3-0.5 part of defoamer, 0.4-0.6 part of flatting agent, 0.3-0.5 part of thickener and 20-30 parts of deionized water; mixing the raw materials in proportion, stirring at high speed for 3-4h, and grinding until the fineness is less than 20 mu m to obtain the water-based epoxy insulating paint. The epoxy insulating paint disclosed by the invention takes the aqueous epoxy resin as a matrix and water as a solvent, so that the epoxy insulating paint meets the environmental protection requirement; meanwhile, an auxiliary agent is added into the insulating paint, so that the insulating paint with high comprehensive performance, temperature resistance and flame retardance is finally obtained, and the insulating paint has higher application value and wider application range.

Description

Water-based epoxy insulating paint and preparation method thereof
Technical Field
The invention belongs to the technical field of insulating paint, and particularly relates to a water-based epoxy insulating paint and a preparation method thereof.
Background
The insulating paint is a necessary material in the aspect of electric power, is mainly used for some electrical equipment, effectively plays a role in insulating conductors, is based on high-molecular polymers, can be solidified into an insulating film or an insulating whole under certain conditions, and has good electric performance, thermal performance, mechanical performance and chemical performance. The high molecular polymer is mainly selected from epoxy, polyester, epoxy polyester and other varieties, wherein the epoxy resin is more, and the epoxy resin has the advantages of high adhesive force, good chemical resistance, good wear resistance, good insulating property and the like. In addition, with the increasing strictness of environmental protection requirements, epoxy insulating paint using aqueous epoxy resin as a matrix and water as a solvent is receiving more and more attention.
Because the coating formed by the epoxy resin is hard and brittle and not resistant to impact, the toughening agent needs to be added to improve the impact toughness of the coating, and the existing plasticizer has the problem of low compatibility of the epoxy resin, so that a higher toughening effect is difficult to realize. Furthermore, on certain specific electrical equipment, such as electrical machines, epoxy insulating paints are required to possess mechanical properties, flame retardant properties and heat resistance properties at the same time. 201010234600.6 in the prior art discloses a halogen-free flame-retardant high-temperature-resistant insulating paint for a motor, which comprises the following components in parts by weight: 100 parts of modified epoxy resin; 0.1 to 0.5 part of initiator; 10-30 parts of reactive diluent; 10-30 parts of nitrogen-containing hyperbranched polyphosphate; 5-20 parts of curing agent; 0.1 to 1 part of curing accelerator. The nitrogen-containing hyperbranched polyphosphate has lower compatibility with an epoxy resin matrix, and the flame retardant effect is difficult to meet the use requirement.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides a water-based epoxy insulating paint and a preparation method thereof.
The epoxy insulating paint disclosed by the invention takes the aqueous epoxy resin as a matrix and water as a solvent, so that the epoxy insulating paint meets the environmental protection requirement; meanwhile, an auxiliary agent is added into the insulating paint, the auxiliary agent contains polyethylene glycol long molecular chains, benzene rings, nitrogen-containing groups, phosphate groups and silicon-containing groups, the polyethylene glycol long molecular chains can play a role in toughening, and the benzene rings can improve the compatibility of the auxiliary agent and epoxy resin; the nitrogen-containing group, the phosphate group and the silicon-containing group are taken as the synergistic flame-retardant component of P, N, si, so that the flame-retardant functional characteristic of the insulating paint can be endowed, and the insulating paint with strong comprehensive performance and temperature-resistant flame-retardant functional characteristic is finally obtained along with the uniform distribution of the auxiliary agent in the insulating paint, so that the insulating paint has higher application value and wider application range.
The aim of the invention can be achieved by the following technical scheme:
the water-based epoxy insulating paint comprises the following raw materials in parts by weight: 50-60 parts of water-based epoxy resin, 9-11 parts of auxiliary agent, 10-16 parts of pigment and filler, 18-22 parts of curing agent, 0.3-0.5 part of defoamer, 0.4-0.6 part of flatting agent, 0.3-0.5 part of thickener and 20-30 parts of deionized water;
the preparation method of the water-based epoxy insulating paint comprises the following steps:
mixing the raw materials in proportion, stirring at high speed for 3-4h, and grinding until the fineness is less than 20 mu m to obtain the water-based epoxy insulating paint.
Further, the aqueous epoxy resin is any one of bisphenol a type epoxy resin, bisphenol F type epoxy resin, bisphenol S type epoxy resin.
Further, the curing agent is an anhydride or imidazole curing agent, such as: methyl tetrahydrophthalic anhydride, methyl hexahydrophthalic anhydride, 2-phenyl-4-methyl-5-hydroxymethyl imidazole, 1-benzyl-2-methylimidazole, and the like.
Further, the defoamer, the flatting agent and the thickener are all water-based substances; specifically, the aqueous defoamer comprises one or more of an organosilicon defoamer BYK-018, a polyether defoamer BYK-019 and a polyether modified silicon defoamer diGao TEGO-810; the water-based leveling agent comprises one or more of a modified polyether leveling agent TEGO-450 and a modified organosilicon leveling agent BYK-306; the aqueous thickener comprises one or more of cellulose thickener Natrosol HEC, polyacrylic thickener VISCOLAM330 and polyurethane thickener DOW company RM-8W.
Further, the auxiliary agent is prepared by the following steps:
s1, putting N-methyl ethylenediamine into a reaction kettle, vacuumizing, introducing nitrogen, repeatedly operating for three times (ensuring no air in the kettle), raising the temperature, introducing ethylene oxide step by step, controlling the reaction temperature to be 40 ℃ through pressurization, reacting for 2 hours, preserving heat for 1 hour after the reaction is finished, vacuumizing, cooling and discharging to obtain an intermediate product 1; the dosage ratio of N-methyl ethylenediamine to ethylene oxide is 7.4g to 8.8g;
-NH on N-methyl ethylenediamine 2 Reacting with ethylene oxide, and controlling the mol ratio of N-methyl ethylenediamine to ethylene oxide to be 1:2 to obtain an intermediate product 1 containing a dihydric alcohol structure through the following reaction process:
s2, adding a polyethylene glycol derivative and acetonitrile into a three-neck flask with a magnetic stirring device, magnetically stirring for 10min under the protection of nitrogen, adding potassium carbonate, potassium iodide and an intermediate product 1, heating, refluxing for 24h under the conditions of 85 ℃ and light shielding and nitrogen under normal pressure, and removing potassium carbonate and potassium iodide salt by suction filtration after the reaction is finished, and removing solvent acetonitrile by reduced pressure rotary evaporation to obtain an intermediate product 2; the ratio of polyethylene glycol derivative, acetonitrile, potassium carbonate, potassium iodide and intermediate 1 was 0.1mol:300mL:13.8g:1.8g:16.2g;
under the action of potassium carbonate and potassium iodide, terminal-Cl on a polyethylene glycol derivative molecular chain reacts with-NH-on an intermediate product 1 molecule (the nucleophilicity of secondary amine is stronger than that of alcoholic hydroxyl group) to obtain an intermediate product 2;
s3, sequentially adding acetonitrile, triethylamine (acid binding agent), phosphorus oxychloride and 4-dimethylaminopyridine (catalyst) into a three-neck flask, stirring and mixing uniformly at room temperature, slowly dropwise adding an acetonitrile solution of an intermediate product 2 into the three-neck flask (the dropwise adding speed is 4 mL/min), continuously stirring for 30min, heating to 60 ℃ for reaction for 3h, after the reaction is finished, adding toluene into the product after rotary evaporation to remove most of acetonitrile, stirring uniformly, extracting with hot distilled water, taking a water phase, performing primary drying on anhydrous magnesium sulfate, and continuously drying in a vacuum oven at 50 ℃ for 4-5h to obtain an intermediate product 3; acetonitrile, triethylamine, phosphorus oxychloride, 4-dimethylaminopyridine, intermediate 2 in a ratio of 150ml to 20.2g to 15.3g to 0.14g to 100ml; the concentration of the acetonitrile solution of the intermediate product 2 is 1mol/L;
under the action of 4-dimethylaminopyridine and triethylamine, the intermediate product 2 and phosphorus oxychloride undergo nucleophilic substitution reaction to generate cyclic phosphate, and the reaction process is as follows:
s4, uniformly mixing the intermediate product 3 with acetonitrile, adding the mixture into a reaction kettle, adding potassium carbonate and potassium iodide, and adding the mixture into N 2 Stirring and heating to 55 ℃ under protection, then dripping dimethyl phenyl silanol, pressurizing and heating after the dripping is completed, reacting for 6 hours at 75-80 ℃, filtering out potassium carbonate and potassium iodide salt after the reaction is finished, and removing solvent acetonitrile by reduced pressure rotary evaporation to obtain an auxiliary agent; the ratio of the amounts of intermediate 3, acetonitrile, potassium carbonate, potassium iodide and dimethylphenyl silanol was 0.1mol:200mL:13.8g:2.0g:15.2g;
intermediate 3 and dimethylphenyl silanol undergo the chemical reaction shown below to give the aid:
further, the polyethylene glycol derivative is prepared by the steps of:
adding methoxy polyethylene glycol and potassium carbonate into a three-neck round bottom flask with a magnetic stirring device, adding dichloromethane, heating, starting magnetic stirring after the temperature rises to 40-42 ℃, starting to dropwise add mixed solution of thionyl chloride and dichloromethane, condensing and refluxing for 24 hours at 42 ℃ after the dropwise addition is completed, removing potassium carbonate by suction filtration after the reaction is completed, and removing solvent dichloromethane and residual thionyl chloride by reduced pressure rotary evaporation to obtain polyethylene glycol derivatives; the dosage ratio of the mixture of methoxy polyethylene glycol, potassium carbonate, methylene dichloride, thionyl chloride and methylene dichloride is 0.1mol:13.8g:250mL:100mL; the concentration of the mixed solution of thionyl chloride and dichloromethane is 0.16g/mL;
under the condition of excessive thionyl chloride, the end-OH of methoxy polyethylene glycol is chloridized by thionyl chloride to obtain polyethylene glycol derivative containing end-Cl group, and the reaction process is as follows:
further, the degree of polymerization of methoxypolyethylene glycol is 12, and the relative molecular mass 560 is as shown in the above reaction scheme.
The obtained auxiliary agent contains polyethylene glycol long molecular chain, benzene ring, nitrogen-containing group, phosphate group and silicon-containing group from the molecular structure;
the main chain of the polyethylene glycol long molecular chain is a carbon-carbon single bond and a carbon-oxygen single bond, and the main chain has higher rotation freedom degree, so that the auxiliary agent is added into the insulating paint, the flexible polyethylene glycol long molecular chain can be inserted between epoxy resin molecular chains to play a toughening effect on an epoxy resin matrix, in addition, the benzene ring structure contained at the other end of the auxiliary agent molecule has higher compatibility with the epoxy resin molecular chain, the compatibility of the auxiliary agent and the epoxy resin matrix is improved, and the toughening effect of the auxiliary agent and the texture uniformity of the paint can be further improved; it should be further described that the nitrogen-containing group, the phosphate group and the silicon-containing group are effective flame retardant components of N, P, si respectively, so that different flame retardant mechanisms can be realized from a gas phase and a condensed phase, and a synergistic flame retardant effect is achieved, therefore, the addition of the auxiliary agent can endow the insulating paint with certain flame retardant and fireproof performance, and meanwhile, the heat resistance and the high temperature resistance can be improved;
in addition, the insulating paint of the invention takes the aqueous epoxy resin emulsion as a film forming matrix and water as a solvent, thereby meeting the environmental protection requirement; the added auxiliary agent molecules have extremely high water solubility, one end is a polyethylene glycol molecular chain, the other end is a benzene ring and a six-membered heterocycle, and the organic end and the epoxy resin have higher compatibility, so that the obtained auxiliary agent molecules can also serve as a surfactant, serve as bridge substances of the epoxy resin and solvent water, improve the texture uniformity of the insulating paint and the binding force of effective substances, further play the role of improving the integral performance of the insulating paint, and finally obtain the insulating paint with strong comprehensive performance and temperature resistance and flame retardance.
The invention has the beneficial effects that:
the epoxy insulating paint disclosed by the invention takes the aqueous epoxy resin as a matrix and water as a solvent, so that the epoxy insulating paint meets the environmental protection requirement; meanwhile, an auxiliary agent is added into the insulating paint, the auxiliary agent contains polyethylene glycol long molecular chains, benzene rings, nitrogen-containing groups, phosphate groups and silicon-containing groups, the polyethylene glycol long molecular chains can play a role in toughening, and the benzene rings can improve the compatibility of the auxiliary agent and epoxy resin; the nitrogen-containing group, the phosphate group and the silicon-containing group are taken as the synergistic flame-retardant component of P, N, si, so that the flame-retardant functional characteristic of the insulating paint can be endowed, and the insulating paint with strong comprehensive performance and temperature-resistant flame-retardant functional characteristic is finally obtained along with the uniform distribution of the auxiliary agent in the insulating paint, so that the insulating paint has higher application value and wider application range.
Detailed Description
The technical solutions of the embodiments of the present invention will be clearly and completely described below in conjunction with the embodiments of the present invention, and it is apparent that the described embodiments are only some embodiments of the present invention, not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Example 1
Preparation of polyethylene glycol derivatives:
adding 0.1mol of methoxy polyethylene glycol (polymerization degree is 12, relative molecular weight is 560) and 13.8g of potassium carbonate into a three-neck round bottom flask with a magnetic stirring device, adding 250mL of dichloromethane, heating, starting magnetic stirring after the temperature is raised to 40-42 ℃, beginning to dropwise add 100mL of mixed solution (with concentration of 0.16 g/mL) of thionyl chloride and dichloromethane, condensing and refluxing for 24h at 42 ℃ after the dropwise addition is completed, removing potassium carbonate by suction filtration after the reaction is completed, and removing solvent dichloromethane and residual thionyl chloride by rotary evaporation under reduced pressure to obtain polyethylene glycol derivatives.
Example 2
Preparing an auxiliary agent:
s1, putting 7.4g of N-methyl ethylenediamine into a reaction kettle, vacuumizing, introducing nitrogen, repeatedly operating for three times (ensuring no air in the kettle), raising the temperature, introducing 8.8g of ethylene oxide step by step, controlling the reaction temperature to 40 ℃ through pressurization, reacting for 2 hours, preserving heat for 1 hour after the reaction is finished, vacuumizing, cooling and discharging to obtain an intermediate product 1;
s2, adding 0.1mol of the polyethylene glycol derivative prepared in the example 1 and 300mL of acetonitrile into a three-neck flask with a magnetic stirring device, magnetically stirring for 10min under the protection of nitrogen, adding 13.8g of potassium carbonate, 1.8g of potassium iodide and 16.2g of intermediate 1, heating, refluxing for 24h under normal pressure under the conditions of 85 ℃ and light shielding and nitrogen, filtering to remove potassium carbonate and potassium iodide salt after the reaction is finished, and removing solvent acetonitrile by reduced pressure rotary evaporation to obtain an intermediate 2;
s3, sequentially adding 150mL of acetonitrile, 20.2g of triethylamine (acid binding agent), 15.3g of phosphorus oxychloride and 0.14g of 4-dimethylaminopyridine (catalyst) into a three-neck flask, stirring and mixing uniformly at room temperature, slowly dropwise adding 100mL of acetonitrile solution (with the concentration of 1 mol/L) of an intermediate product 2 into the three-neck flask (with the dropwise adding speed of 4 mL/min), continuously stirring for 30min, heating to 60 ℃ for reaction for 3h, after the reaction is finished, removing most of acetonitrile by rotary evaporation, adding toluene into the product, stirring uniformly, extracting with hot distilled water, taking a water phase, carrying out primary drying on anhydrous magnesium sulfate, and continuously drying in a vacuum oven at 50 ℃ for 4h to obtain an intermediate product 3;
s4, uniformly mixing 0.1mol of intermediate 3 and 200mL of acetonitrile, adding into a reaction kettle, and then13.8g of potassium carbonate and 2.0g of potassium iodide were added under N 2 Stirring and heating to 55 ℃ under protection, then dripping 15.2g of dimethyl phenyl silanol, pressurizing and heating after the dripping is completed, reacting for 6 hours at 75 ℃, removing potassium carbonate and potassium iodide salt by suction filtration after the reaction is finished, and removing solvent acetonitrile by reduced pressure rotary evaporation to obtain the auxiliary agent.
Example 3
Preparing an auxiliary agent:
s1, putting 14.8g of N-methyl ethylenediamine into a reaction kettle, vacuumizing, introducing nitrogen, repeatedly operating for three times (ensuring no air in the kettle), raising the temperature, introducing 17.6g of ethylene oxide step by step, controlling the reaction temperature to 40 ℃ through pressurization, reacting for 2 hours, preserving heat for 1 hour after the reaction is finished, vacuumizing, cooling and discharging to obtain an intermediate product 1;
s2, adding 0.2mol of the polyethylene glycol derivative prepared in the example 1 and 600mL of acetonitrile into a three-neck flask with a magnetic stirring device, magnetically stirring for 10min under the protection of nitrogen, adding 27.6g of potassium carbonate, 3.6g of potassium iodide and 32.4g of intermediate 1, heating, refluxing for 24h under normal pressure under the conditions of 85 ℃ and light shielding and nitrogen, filtering to remove potassium carbonate and potassium iodide salt after the reaction is finished, and removing solvent acetonitrile by reduced pressure rotary evaporation to obtain an intermediate 2;
s3, sequentially adding 300mL of acetonitrile, 40.4g of triethylamine (acid binding agent), 30.6g of phosphorus oxychloride and 0.28g of 4-dimethylaminopyridine (catalyst) into a three-neck flask, stirring and mixing uniformly at room temperature, slowly dropwise adding 200mL of acetonitrile solution (with the concentration of 1 mol/L) of an intermediate product 2 into the three-neck flask (with the dropwise adding speed of 4 mL/min), continuously stirring for 30min, heating to 60 ℃ for reaction for 3h, after the reaction is finished, removing most of acetonitrile by rotary evaporation, adding toluene into the product, stirring uniformly, extracting with hot distilled water, taking a water phase, carrying out primary drying on anhydrous magnesium sulfate, and then placing the obtained product into a vacuum oven at 50 ℃ for continuous drying for 5h to obtain an intermediate product 3;
s4, uniformly mixing 0.2mol of intermediate 3 and 400mL of acetonitrile, adding into a reaction kettle, adding 27.6g of potassium carbonate and 4.0g of potassium iodide, and adding into the mixture under N 2 Stirring under protection, heating to 55deg.C, dripping 30.4g dimethyl phenyl silanol, pressurizing, and heating to 80deg.CAfter the reaction is finished for 6 hours, removing potassium carbonate and potassium iodide salt by suction filtration, and removing solvent acetonitrile by reduced pressure rotary evaporation to obtain the auxiliary agent.
Example 4
The water-based epoxy insulating paint comprises the following raw materials in parts by weight: 50 parts of aqueous bisphenol A type epoxy resin, 9 parts of auxiliary agent prepared in example 2, 10 parts of pigment and filler, 18 parts of methyl tetrahydrophthalic anhydride, 0.3 part of organosilicon defoamer BYK-018, 0.4 part of modified polyether leveling agent TEGO-450, 0.3 part of cellulose thickener Natrosol HEC and 20 parts of deionized water;
the preparation method of the water-based epoxy insulating paint comprises the following steps:
mixing the raw materials in proportion, stirring at high speed for 3 hours, and grinding until the fineness is less than 20 mu m to obtain the water-based epoxy insulating paint.
Example 5
The water-based epoxy insulating paint comprises the following raw materials in parts by weight: 55 parts of aqueous bisphenol F type epoxy resin, 10 parts of auxiliary agent prepared in example 3, 13 parts of pigment and filler, 20 parts of methyl hexahydrophthalic anhydride, 0.4 part of polyether defoamer BYK-019, 0.5 part of modified organosilicon leveling agent BYK-306, 0.4 part of polyacrylic thickener VISCOLAM330 and 25 parts of deionized water;
the preparation method of the water-based epoxy insulating paint comprises the following steps:
mixing the raw materials in proportion, stirring at high speed for 3.5h, and grinding until the fineness is less than 20 mu m to obtain the water-based epoxy insulating paint.
Example 6
The water-based epoxy insulating paint comprises the following raw materials in parts by weight: 60 parts of aqueous bisphenol S-type epoxy resin, 11 parts of auxiliary agent prepared in example 2, 16 parts of pigment and filler, 22 parts of 2-phenyl-4-methyl-5-hydroxymethyl imidazole, 0.5 part of polyether modified silicon type defoamer TEGO-810, 0.6 part of modified polyether type flatting agent TEGO-450, 0.5 part of polyurethane thickener DOW company RM-8W and 30 parts of deionized water;
the preparation method of the water-based epoxy insulating paint comprises the following steps:
mixing the raw materials in proportion, stirring at high speed for 4 hours, and grinding until the fineness is less than 20 mu m to obtain the water-based epoxy insulating paint.
Comparative example
The auxiliary agent in the example 4 is replaced by polyethylene glycol, and the rest raw materials and the preparation process are unchanged, so that the water-based epoxy insulating paint is obtained.
The epoxy insulating paints obtained in examples 4 to 6 and comparative example were applied to tin plates, cured at about 100℃for 1 hour, at about 140℃for 2 hours, and then at about 170℃for 3 hours, and then tested for performance index, see the following table:
as can be seen from the data in the table, the insulating paint obtained by the invention has mechanical property, flame retardant property and insulating property, and has excellent comprehensive performance; according to the data of the comparative example, the addition of the auxiliary agent can play roles of toughening, improving flame retardant property and serving as a surfactant, so that the comprehensive performance of the insulating paint is improved.
In the description of the present specification, the descriptions of the terms "one embodiment," "example," "specific example," and the like, mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the present invention. In this specification, schematic representations of the above terms do not necessarily refer to the same embodiments or examples. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.
The foregoing is merely illustrative and explanatory of the invention, as various modifications and additions may be made to the particular embodiments described, or in a similar manner, by those skilled in the art, without departing from the scope of the invention or exceeding the scope of the invention as defined in the claims.

Claims (8)

1. The water-based epoxy insulating paint is characterized by comprising the following raw materials in parts by weight: 50-60 parts of water-based epoxy resin, 9-11 parts of auxiliary agent, 10-16 parts of pigment and filler, 18-22 parts of curing agent, 0.3-0.5 part of defoamer, 0.4-0.6 part of flatting agent, 0.3-0.5 part of thickener and 20-30 parts of deionized water;
wherein, the auxiliary agent is prepared by the following steps:
s1, putting N-methyl ethylenediamine into a reaction kettle, vacuumizing, introducing nitrogen, repeatedly operating for three times, raising the temperature, introducing ethylene oxide step by step, controlling the reaction temperature to be 40 ℃ through pressurization, reacting for 2 hours, preserving heat for 1 hour after the reaction is finished, vacuumizing, cooling and discharging to obtain an intermediate product 1;
s2, adding a polyethylene glycol derivative and acetonitrile into a three-neck flask with a magnetic stirring device, magnetically stirring for 10min under the protection of nitrogen, adding potassium carbonate, potassium iodide and an intermediate product 1, heating, refluxing for 24h under the conditions of 85 ℃ and light shielding and nitrogen under normal pressure, and removing potassium carbonate and potassium iodide salt by suction filtration after the reaction is finished, and removing solvent acetonitrile by reduced pressure rotary evaporation to obtain an intermediate product 2;
s3, sequentially adding acetonitrile, triethylamine, phosphorus oxychloride and 4-dimethylaminopyridine into a three-neck flask, stirring and mixing uniformly at room temperature, slowly dripping an acetonitrile solution of an intermediate product 2 into the three-neck flask, continuously stirring for 30min, heating to 60 ℃ for reaction for 3h, after the reaction is finished, removing most acetonitrile by rotary evaporation, adding toluene into the product, stirring uniformly, extracting with hot distilled water, taking a water phase, initially drying anhydrous magnesium sulfate, and continuously drying in a vacuum oven at 50 ℃ for 4-5h to obtain an intermediate product 3;
s4, reacting the intermediate product 3 with dimethylphenyl silanol to obtain the auxiliary agent.
2. An aqueous epoxy insulating varnish according to claim 1, wherein the ratio of N-methyl ethylenediamine to ethylene oxide in step S1 is 7.4 g/8.8 g.
3. The aqueous epoxy insulating varnish according to claim 1, wherein the ratio of polyethylene glycol derivative, acetonitrile, potassium carbonate, potassium iodide and intermediate 1 in step S2 is 0.1 mol/300 mL/13.8 g/1.8 g/16.2 g.
4. The aqueous epoxy insulating varnish according to claim 1, wherein the ratio of acetonitrile, triethylamine, phosphorus oxychloride, 4-dimethylaminopyridine and acetonitrile solution of intermediate 2 in step S3 is 150mL:20.2g:15.3g:0.14g:100mL; the concentration of the acetonitrile solution of the intermediate 2 was 1mol/L.
5. The aqueous epoxy insulating paint according to claim 1, wherein the specific process of step S4 is: mixing intermediate 3 with acetonitrile, adding into a reaction kettle, adding potassium carbonate and potassium iodide, and adding into N 2 Stirring and heating to 55 ℃ under protection, then dripping dimethyl phenyl silanol, pressurizing and heating after the dripping is completed, reacting for 6 hours at 75-80 ℃, removing potassium carbonate and potassium iodide salt by suction filtration after the reaction is finished, and removing solvent acetonitrile by reduced pressure rotary evaporation to obtain the auxiliary agent.
6. An aqueous epoxy insulating varnish according to claim 5, characterised in that the ratio of the amounts of intermediate 3, acetonitrile, potassium carbonate, potassium iodide and dimethylphenylsilanol is 0.1mol:200ml:13.8g:2.0g:15.2g.
7. The aqueous epoxy insulating varnish according to claim 1, wherein the polyethylene glycol derivative in step S2 is prepared by the steps of:
adding methoxy polyethylene glycol and potassium carbonate into a three-neck round bottom flask with a magnetic stirring device, adding dichloromethane, heating, starting magnetic stirring after the temperature rises to 40-42 ℃, starting to dropwise add mixed solution of thionyl chloride and dichloromethane, condensing and refluxing for 24 hours at 42 ℃ after the dropwise addition is completed, removing potassium carbonate by suction filtration after the reaction is completed, and removing solvent dichloromethane and residual thionyl chloride by reduced pressure rotary evaporation to obtain polyethylene glycol derivatives; the dosage ratio of the mixture of methoxy polyethylene glycol, potassium carbonate, methylene dichloride, thionyl chloride and methylene dichloride is 0.1mol:13.8g:250mL:100mL; the concentration of the mixed solution of thionyl chloride and methylene chloride was 0.16g/mL.
8. The preparation method of the aqueous epoxy insulating paint according to claim 1, which is characterized by comprising the following specific steps:
mixing the raw materials in proportion, stirring at high speed for 3-4h, and grinding until the fineness is less than 20 mu m to obtain the water-based epoxy insulating paint.
CN202310699876.9A 2023-06-14 Water-based epoxy insulating paint and preparation method thereof Active CN116656211B (en)

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