CN108997932B - Water-based insulating paint and preparation method thereof - Google Patents
Water-based insulating paint and preparation method thereof Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D183/00—Coating compositions based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon, with or without sulfur, nitrogen, oxygen, or carbon only; Coating compositions based on derivatives of such polymers
- C09D183/10—Block or graft copolymers containing polysiloxane sequences
- C09D183/12—Block or graft copolymers containing polysiloxane sequences containing polyether sequences
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
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- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/08—Anti-corrosive paints
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/18—Fireproof paints including high temperature resistant paints
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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- C08L2201/02—Flame or fire retardant/resistant
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- C08L2201/08—Stabilised against heat, light or radiation or oxydation
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- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
- C08L2205/035—Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend
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Abstract
The invention provides a water-based insulating paint which is prepared from the following components in parts by weight: 60-70 parts of polyether modified dimethylol hydantoin organic silicon polycondensate, 20-30 parts of polyurethane modified hyperbranched polyethyleneimine, 5-10 parts of surface modified nano boron fiber, 1-5 parts of defoaming agent, 1-5 parts of flatting agent, 1-3 parts of neutralization stabilizer, 1-5 parts of cosolvent and 20-30 parts of water. The invention also discloses a preparation method of the water-based insulating paint. The water-based insulating paint prepared by the invention has more excellent electrical property, heat resistance, chemical resistance, mechanical property and flame retardance, and is safer and more environment-friendly to use.
Description
Technical Field
The invention relates to the technical field of insulating paint, in particular to water-based insulating paint and a preparation method thereof.
Background
In recent years, along with the spread of motors and electric appliances, an insulating varnish, which is one of indispensable materials for electric devices and motors, has been developed rapidly. The insulating paint is an insulating material which takes high molecular polymer as a matrix and can be solidified into an insulating film or an insulator, and is a special coating. It not only has insulating property, but also has the functions of impregnation and sealing, can be permeated into various different matrixes, and can play an insulating role in various motor electric appliances.
At present, insulating paint on the market mainly has two types of oil and water, the oil insulating paint has excellent comprehensive performance and good insulating performance, but toxic and harmful organic solvents which are easy to volatilize are needed to be used in the manufacturing and using processes, and the insulating paint is easy to volatilize, has large smell, is unpleasant to smell, has high cost, has strict operation requirements, is not easy to clean, is easy to pollute the environment and threatens the health of people. The waterborne insulating paint generally uses waterborne acrylic resin, waterborne polyurethane resin, waterborne epoxy resin and waterborne polyester resin as film forming substances, uses water as a solvent, and is the preferred choice for future insulating paints due to low comprehensive cost, low toxicity, safe use and storage, excellent dielectric property, convenient use, good permeability and high bonding strength. However, the water-based insulating paint in the prior art is generally added with a cosolvent, is made water-based by adding an emulsifier, or is prepared into a water-based system by introducing acrylic acid or acrylate monomers, still possibly causes harm to people and environment, is inflammable and explosive, has potential safety hazards in transportation and storage, has poor insulating property and high temperature resistance, has the problem of hydrolysis caused by long-term storage, and has low mechanical strength after curing.
Therefore, it is imperative to develop a water-based insulating paint with more excellent electrical properties, heat resistance, chemical resistance, mechanical properties and flame retardance.
Disclosure of Invention
The invention mainly aims to provide the water-based insulating paint and the preparation method thereof, wherein the preparation method is simple and feasible, has low dependence on equipment, is easy to obtain raw materials, is low in price and is suitable for large-scale production. The water-based insulating paint prepared by the preparation method overcomes the technical problems that the water-based insulating paint in the prior art is poor in hydrolysis resistance and storage stability, low in mechanical strength after curing, poor in heat resistance and high in water absorption rate, and has better electrical properties, heat resistance, chemical resistance, mechanical properties and flame retardance, and the added cosolvent or organic micromolecules generated in the curing process can remain in the motor, damage is caused to antirust oil on the bearing in the using process, rusting of the bearing is accelerated, the motor generates noise, and the water-based insulating paint has poor electrical insulation properties.
In order to achieve the purpose, the invention provides water-based insulating paint which is prepared from the following components in parts by weight: 60-70 parts of polyether modified dimethylol hydantoin organic silicon polycondensate, 20-30 parts of polyurethane modified hyperbranched polyethyleneimine, 5-10 parts of surface modified nano boron fiber, 1-5 parts of defoaming agent, 1-5 parts of flatting agent, 1-3 parts of neutralization stabilizer, 1-5 parts of cosolvent and 20-30 parts of water.
Preferably, the defoaming agent is selected from one or more of polyoxyethylene polyoxypropylene ether, polydimethylsiloxane and polyoxypropylene glycerol ether; the leveling agent is preferably one or more of a polyacrylate leveling agent, a cellulose acetate butyrate leveling agent and a polyvinyl butyral leveling agent; the neutralizing stabilizer is selected from one or more of 2-amino-2-methyl-1-propanol, triethanolamine, dimethylethanolamine and ammonia water; the cosolvent is selected from one or more of ethanol, isopropanol, ethylene glycol and n-butanol.
Preferably, the preparation method of the polyether modified dimethylol hydantoin organosilicon polycondensate comprises the following steps:
i, adding dimethylolhydantoin, 1-chloropropylmethyldiethoxysilane, a high-boiling-point solvent and a catalyst dibutyltin dilaurate into a three-necked bottle provided with a stirrer, a thermometer and a constant-pressure dropping funnel, raising the temperature to 75-85 ℃, then dropwise adding distilled water, stirring and reacting for 15-18 hours at the temperature of 90-100 ℃, and then performing rotary evaporation to remove the high-boiling-point solvent to obtain an intermediate product;
and II, dissolving the intermediate product obtained in the step I and monoamino polyether in an organic solvent to form a solution, adding an alkaline catalyst into the solution, stirring and reacting for 6-8 hours at the temperature of 50-60 ℃, and then removing the solvent by rotary evaporation to obtain the polyether modified dimethylol hydantoin organosilicon polycondensate.
Preferably, the mass ratio of the dimethylolhydantoin, the 1-chloropropylmethyldiethoxysilane, the high-boiling-point solvent, the dibutyltin dilaurate and the distilled water in the step I is 1:1.12 (6-10): 0.3-0.6: 0.1-0.4.
Preferably, the high boiling point solvent is selected from one or more of dimethyl sulfoxide, N-dimethylformamide and N-methylpyrrolidone.
Preferably, the mass ratio of the intermediate product, the monoamino polyether, the organic solvent and the alkaline catalyst in the step II is (1-2) to (8-12) to (0.3-0.6).
Preferably, the organic solvent is selected from one or more of isopropanol, dichloromethane, tetrahydrofuran and acetone; the basic catalyst is selected from one or more of triethylamine, triphenylphosphine and tetrabutylammonium bromide.
Preferably, the preparation method of the polyurethane modified hyperbranched polyethyleneimine comprises the following steps: adding waterborne polyurethane, hyperbranched polyethyleneimine and dibutyltin dilaurate into dimethyl sulfoxide, stirring and reacting for 5-7 hours at 60-70 ℃, precipitating in ethanol, carrying out suction filtration, and removing a solvent by rotary evaporation to obtain the polyurethane modified hyperbranched polyethyleneimine.
Preferably, the mass ratio of the waterborne polyurethane to the hyperbranched polyethyleneimine to the dibutyltin dilaurate to the dimethyl sulfoxide is 1 (2-4) to (0.3-0.6) to (10-15).
Preferably, the preparation method of the surface modified nano boron fiber comprises the following steps: dispersing the nano boron fiber in ethanol, adding 1,3, 5-tri [3- (trimethoxysilyl) propyl ] -1,3, 5-triazine-2, 4,6(1H,3H,5H) -trione, stirring and reacting for 4-6 hours at 50-60 ℃, centrifuging, and washing for 3-5 times by using ethyl acetate to obtain the surface modified nano boron fiber.
Preferably, the mass ratio of the nano boron fiber to the ethanol to the 1,3, 5-tri [3- (trimethoxysilyl) propyl ] -1,3, 5-triazine-2, 4,6(1H,3H,5H) -trione is (3-5): 1 (10-15): 1.
Preferably, the preparation method of the water-based insulating paint comprises the following steps: uniformly mixing polyether modified dimethylol hydantoin organic silicon polycondensate, polyurethane modified hyperbranched polyethyleneimine, surface modified nano boron fiber and cosolvent according to a proportion to prepare mixed slurry, then adding a defoaming agent, a flatting agent, a neutralization stabilizer and water, and mixing again to obtain the water-based insulating paint.
Due to the application of the technical scheme, the invention has the following beneficial effects:
(1) the preparation method of the water-based insulating paint disclosed by the invention is simple and feasible, has low dependence on equipment, is easy to obtain raw materials, is low in price and is suitable for large-scale production.
(2) The water-based insulating paint disclosed by the invention overcomes the technical problems that the added cosolvent or organic micromolecules generated in the curing process can remain in a motor more or less in the water-based insulating paint in the prior art, the antirust oil on a bearing is damaged in the using process, the rusting of the bearing is accelerated, the motor generates noise, the hydrolysis resistance is poor, the storage stability is poor, the mechanical strength is not high after curing, the heat resistance is poor, the water absorption rate is high, and the electrical insulating performance is poor, and the water-based insulating paint has more excellent electrical performance, heat resistance, chemical resistance, mechanical performance and flame retardance.
(3) The water-based insulating paint disclosed by the invention combines the advantages of organic silicon and polyether film-forming polymers, and introduces a hydantoin structure, so that the paint has excellent insulating property, film-forming property, wear resistance, weather resistance and ultraviolet aging resistance; the molecular chain contains more active hydroxyl and amino structures, so that the bridging capacity is enhanced, and the mechanical stability and the weather resistance of the paint film are obviously improved. By adding polyurethane modified hyperbranched polyethyleneimine, the adhesive force between a paint film and a matrix and the comprehensive performance of the paint are further improved; adding surface modified boron fiber to further improve the strength and hardness of the paint film; all the components have synergistic effect, so that the waterborne insulating paint has excellent comprehensive performance.
Detailed Description
The following description is presented to disclose the invention so as to enable any person skilled in the art to practice the invention. The preferred embodiments in the following description are given by way of example only, and other obvious variations will occur to those skilled in the art.
The raw materials used in the examples of the present invention were purchased from Mobei (Shanghai) Biotech limited.
Example 1
The water-based insulating paint is prepared from the following components in parts by weight: 60 parts of polyether modified dimethylol hydantoin organic silicon polycondensate, 20 parts of polyurethane modified hyperbranched polyethyleneimine, 5 parts of surface modified nano boron fiber, 1 part of polyoxyethylene polyoxypropylene amine ether, 1 part of polyacrylate flatting agent, 1 part of 2-amino-2-methyl-1-propanol, 1 part of ethanol and 20 parts of water.
The preparation method of the polyether modified dimethylol hydantoin organic silicon polycondensate comprises the following steps:
i, adding 10g of dimethylolhydantoin, 11.2g of 1-chloropropylmethyldiethoxysilane, 60g of dimethyl sulfoxide and 3g of dibutyltin dilaurate serving as a catalyst into a three-necked bottle provided with a stirrer, a thermometer and a constant-pressure dropping funnel, raising the temperature to 75 ℃, dropwise adding 1g of distilled water, stirring and reacting for 15 hours at the temperature of 90 ℃, and then removing the dimethyl sulfoxide by rotary evaporation to obtain an intermediate product;
II, dissolving 10g of the intermediate product prepared in the step I and 10g of monoamino polyether in 80g of isopropanol to form a solution, adding 3g of triethylamine into the solution, stirring and reacting at 50 ℃ for 6 hours, and then removing the solvent by rotary evaporation to obtain the polyether modified dimethylol hydantoin organosilicon polycondensate.
The preparation method of the polyurethane modified hyperbranched polyethyleneimine comprises the following steps: 10g of waterborne polyurethane, 20g of hyperbranched polyethyleneimine and 3g of dibutyltin dilaurate are added into 100g of dimethyl sulfoxide, stirred and reacted for 5 hours at 60 ℃, then precipitated in ethanol, filtered, and subjected to rotary evaporation to remove the solvent, so that polyurethane modified hyperbranched polyethyleneimine is obtained.
The preparation method of the surface modified nano boron fiber comprises the following steps: dispersing 30g of nano boron fiber in 100g of ethanol, adding 10g of 1,3, 5-tri [3- (trimethoxysilyl) propyl ] -1,3, 5-triazine-2, 4,6(1H,3H,5H) -trione, stirring and reacting for 4 hours at 50 ℃, centrifuging, and washing 3 times by using ethyl acetate to obtain the surface modified nano boron fiber.
The preparation method of the water-based insulating paint comprises the following steps: uniformly mixing polyether modified dimethylol hydantoin organic silicon polycondensate, polyurethane modified hyperbranched polyethyleneimine, surface modified nano boron fiber and ethanol in proportion to prepare mixed slurry, then adding polyoxyethylene polyoxypropylene amine ether, a polyacrylate leveling agent, 2-amino-2-methyl-1-propanol and water, and mixing again to obtain the water-based insulating paint.
Example 2
The water-based insulating paint is prepared from the following components in parts by weight: 63 parts of polyether modified dimethylol hydantoin organic silicon polycondensate, 23 parts of polyurethane modified hyperbranched polyethyleneimine, 6 parts of surface modified nano boron fiber, 2 parts of polydimethylsiloxane, 2 parts of cellulose acetate leveling agent, 2 parts of triethanolamine, 2 parts of isopropanol and 23 parts of water.
The preparation method of the polyether modified dimethylol hydantoin organic silicon polycondensate comprises the following steps:
i, adding 10g of dimethylolhydantoin, 11.2g of 1-chloropropylmethyldiethoxysilane, 70g of N, N-dimethylformamide and 4g of dibutyltin dilaurate serving as a catalyst into a three-necked bottle provided with a stirrer, a thermometer and a constant-pressure dropping funnel, raising the temperature to 78 ℃, dropwise adding 2g of distilled water, stirring and reacting at 93 ℃ for 16 hours, and then removing the N, N-dimethylformamide by rotary evaporation to obtain an intermediate product;
II, dissolving 13g of the intermediate product obtained in the step I and 10g of monoamino polyether in 90g of dichloromethane to form a solution, adding 4g of triphenylphosphine into the solution, stirring and reacting at 53 ℃ for 6.5 hours, and then removing the solvent by rotary evaporation to obtain the polyether modified dimethylol hydantoin organosilicon polycondensate.
The preparation method of the polyurethane modified hyperbranched polyethyleneimine comprises the following steps: 10g of waterborne polyurethane, 25g of hyperbranched polyethyleneimine and 4g of dibutyltin dilaurate are added into 115g of dimethyl sulfoxide, stirred and reacted for 5.5 hours at 63 ℃, and then precipitated in ethanol, filtered, and subjected to rotary evaporation to remove the solvent, so that the polyurethane modified hyperbranched polyethyleneimine is obtained.
The preparation method of the surface modified nano boron fiber comprises the following steps: dispersing 35g of nano boron fiber in 125g of ethanol, adding 10g of 1,3, 5-tri [3- (trimethoxysilyl) propyl ] -1,3, 5-triazine-2, 4,6(1H,3H,5H) -trione, stirring and reacting for 5 hours at 53 ℃, centrifuging, and washing for 4 times by using ethyl acetate to obtain the surface modified nano boron fiber.
The preparation method of the water-based insulating paint comprises the following steps: uniformly mixing polyether modified dimethylol hydantoin organic silicon polycondensate, polyurethane modified hyperbranched polyethyleneimine, surface modified nano boron fiber and isopropanol in proportion to prepare mixed slurry, then adding polydimethylsiloxane, cellulose acetate butyrate leveling agent, triethanolamine and water, and mixing again to obtain the water-based insulating paint.
Example 3
The water-based insulating paint is prepared from the following components in parts by weight: 65 parts of polyether modified dimethylol hydantoin organic silicon polycondensate, 25 parts of polyurethane modified hyperbranched polyethyleneimine, 8 parts of surface modified nano boron fiber, 3 parts of polyoxypropylene glycerol ether, 3 parts of polyvinyl butyral flatting agent, 3 parts of dimethylethanolamine, 3 parts of ethylene glycol and 25 parts of water.
The preparation method of the polyether modified dimethylol hydantoin organic silicon polycondensate comprises the following steps:
i, adding 10g of dimethylolhydantoin, 11.2g of 1-chloropropylmethyldiethoxysilane, 80g of N-methylpyrrolidone and 5g of dibutyltin dilaurate serving as a catalyst into a three-necked bottle provided with a stirrer, a thermometer and a constant-pressure dropping funnel, raising the temperature to 80 ℃, dropwise adding 3g of distilled water, stirring and reacting for 16.5 hours at the temperature of 95 ℃, and then carrying out rotary evaporation to remove the N-methylpyrrolidone to obtain an intermediate product;
II, dissolving 16g of the intermediate product prepared in the step I and 10g of monoamino polyether in 100g of tetrahydrofuran to form a solution, adding 5g of tetrabutylammonium bromide into the solution, stirring and reacting at 56 ℃ for 7 hours, and then performing rotary evaporation to remove the solvent to obtain the polyether modified dimethylol hydantoin organosilicon polycondensate.
The preparation method of the polyurethane modified hyperbranched polyethyleneimine comprises the following steps: 10g of waterborne polyurethane, 30g of hyperbranched polyethyleneimine and 5g of dibutyltin dilaurate are added into 140g of dimethyl sulfoxide, stirred and reacted for 6 hours at 66 ℃, and then precipitated in ethanol, filtered, and subjected to rotary evaporation to remove the solvent, so that polyurethane modified hyperbranched polyethyleneimine is obtained.
The preparation method of the surface modified nano boron fiber comprises the following steps: dispersing 40g of nano boron fiber in 140g of ethanol, adding 10g of 1,3, 5-tri [3- (trimethoxysilyl) propyl ] -1,3, 5-triazine-2, 4,6(1H,3H,5H) -trione, stirring and reacting for 5.2 hours at 57 ℃, centrifuging, and washing for 5 times by using ethyl acetate to obtain the surface modified nano boron fiber.
The preparation method of the water-based insulating paint comprises the following steps: uniformly mixing polyether modified dimethylol hydantoin organic silicon polycondensate, polyurethane modified hyperbranched polyethyleneimine, surface modified nano boron fiber and ethylene glycol in proportion to prepare mixed slurry, then adding polyoxypropylene glycerol ether, a polyvinyl butyral flatting agent, dimethylethanolamine and water, and mixing again to obtain the water-based insulating paint.
Example 4
The water-based insulating paint is prepared from the following components in parts by weight: 68 parts of polyether modified dimethylol hydantoin organic silicon polycondensate, 28 parts of polyurethane modified hyperbranched polyethyleneimine, 9 parts of surface modified nano boron fiber, 4 parts of defoaming agent, 4 parts of flatting agent, 3 parts of neutralization stabilizer, 5 parts of cosolvent and 29 parts of water; the defoaming agent is a mixture formed by mixing polyoxyethylene polyoxypropylene ether, polydimethylsiloxane and polyoxypropylene glycerol ether according to the mass ratio of 1:2: 3; the leveling agent is a mixture formed by mixing a polyacrylate leveling agent, a cellulose acetate butyrate leveling agent and a polyvinyl butyral leveling agent according to a mass ratio of 2:2: 1; the neutralization stabilizer is a mixture formed by mixing 2-amino-2-methyl-1-propanol, triethanolamine, dimethylethanolamine and ammonia water according to the mass ratio of 2:1:3: 1; the cosolvent is a mixture formed by mixing ethanol, isopropanol, ethylene glycol and n-butanol according to the mass ratio of 1:1:2: 1.
The preparation method of the polyether modified dimethylol hydantoin organic silicon polycondensate comprises the following steps:
i, adding 10g of dimethylolhydantoin, 11.2g of 1-chloropropylmethyldiethoxysilane, 95g of high-boiling-point solvent and 5.8g of dibutyltin dilaurate serving as a catalyst into a three-necked bottle provided with a stirrer, a thermometer and a constant-pressure dropping funnel, raising the temperature to 83 ℃, dropwise adding 3.8g of distilled water, stirring and reacting for 17 hours at the temperature of 98 ℃, and then performing rotary evaporation to remove the high-boiling-point solvent to obtain an intermediate product; the high-boiling-point solvent is a mixture formed by mixing dimethyl sulfoxide, N-dimethylformamide and N-methylpyrrolidone according to the mass ratio of 2:1: 3;
II, dissolving 19g of the intermediate product prepared in the step I and 10g of monoamino polyether in 115g of organic solvent to form a solution, adding 5.7g of an alkaline catalyst into the solution, stirring and reacting at 58 ℃ for 7.5 hours, and then removing the solvent by rotary evaporation to obtain the polyether modified dimethylol hydantoin organosilicon polycondensate; the organic solvent is a mixture formed by mixing isopropanol, dichloromethane and tetrahydrofuran according to a mass ratio of 1:3: 5; the basic catalyst is a mixture formed by mixing triethylamine, triphenylphosphine and tetrabutylammonium bromide according to the mass ratio of 2:3: 1.
The preparation method of the polyurethane modified hyperbranched polyethyleneimine comprises the following steps: 10g of waterborne polyurethane, 38g of hyperbranched polyethyleneimine and 6g of dibutyltin dilaurate are added into 146g of dimethyl sulfoxide, stirred and reacted for 6.5 hours at 68 ℃, then precipitated in ethanol, filtered, and subjected to rotary evaporation to remove the solvent, so that the polyurethane modified hyperbranched polyethyleneimine is obtained.
The preparation method of the surface modified nano boron fiber comprises the following steps: dispersing 48g of nano boron fiber in 146g of ethanol, adding 10g of 1,3, 5-tris [3- (trimethoxysilyl) propyl ] -1,3, 5-triazine-2, 4,6(1H,3H,5H) -trione, stirring and reacting at 58 ℃ for 5.8 hours, centrifuging, and washing with ethyl acetate for 5 times to obtain the surface modified nano boron fiber.
The preparation method of the water-based insulating paint comprises the following steps: uniformly mixing polyether modified dimethylol hydantoin organic silicon polycondensate, polyurethane modified hyperbranched polyethyleneimine, surface modified nano boron fiber and cosolvent according to a proportion to prepare mixed slurry, then adding a defoaming agent, a flatting agent, a neutralization stabilizer and water, and mixing again to obtain the water-based insulating paint.
Example 5
The water-based insulating paint is prepared from the following components in parts by weight: 70 parts of polyether modified dimethylol hydantoin organic silicon polycondensate, 30 parts of polyurethane modified hyperbranched polyethyleneimine, 10 parts of surface modified nano boron fiber, 5 parts of polyoxyethylene polyoxypropylene amine ether, 5 parts of polyacrylate flatting agent, 3 parts of ammonia water, 5 parts of n-butyl alcohol and 30 parts of water.
The preparation method of the polyether modified dimethylol hydantoin organic silicon polycondensate comprises the following steps:
i, adding 10g of dimethylolhydantoin, 11.2g of 1-chloropropylmethyldiethoxysilane, 100g of dimethyl sulfoxide and 6g of dibutyltin dilaurate serving as a catalyst into a three-necked bottle provided with a stirrer, a thermometer and a constant-pressure dropping funnel, raising the temperature to 85 ℃, dropwise adding 4g of distilled water, stirring and reacting for 18 hours at the temperature of 100 ℃, and then removing the dimethyl sulfoxide by rotary evaporation to obtain an intermediate product;
and II, dissolving 20g of the intermediate product prepared in the step I and 10g of monoamino polyether in 120g of isopropanol to form a solution, adding 6g of triethylamine into the solution, stirring and reacting at 60 ℃ for 8 hours, and then removing the solvent by rotary evaporation to obtain the polyether modified dimethylol hydantoin organosilicon polycondensate.
The preparation method of the polyurethane modified hyperbranched polyethyleneimine comprises the following steps: 10g of waterborne polyurethane, 40g of hyperbranched polyethyleneimine and 6g of dibutyltin dilaurate are added into 150g of dimethyl sulfoxide, stirred and reacted for 7 hours at 70 ℃, then precipitated in ethanol, filtered, and subjected to rotary evaporation to remove the solvent, so that polyurethane modified hyperbranched polyethyleneimine is obtained.
The preparation method of the surface modified nano boron fiber comprises the following steps: dispersing 50g of nano boron fiber into 150g of ethanol, adding 10g of 1,3, 5-tri [3- (trimethoxysilyl) propyl ] -1,3, 5-triazine-2, 4,6(1H,3H,5H) -trione, stirring and reacting for 6 hours at 60 ℃, centrifuging, and washing for 5 times by using ethyl acetate to obtain the surface modified nano boron fiber.
The preparation method of the water-based insulating paint comprises the following steps: uniformly mixing polyether modified dimethylol hydantoin organic silicon polycondensate, polyurethane modified hyperbranched polyethyleneimine, surface modified nano boron fiber and n-butyl alcohol in proportion to prepare mixed slurry, adding polyoxyethylene polyoxypropylene amine ether, a polyacrylate flatting agent, ammonia water and water, and mixing again to obtain the water-based insulating paint.
Comparative example
The present example provides a water-based insulating paint, its formula and preparation method are the same as those of the Chinese invention patent CN 105348502B
Example 1.
The aqueous insulating paints prepared in examples 1 to 5 and comparative example were subjected to performance tests, the test methods and the test results are shown in Table 1.
TABLE 1
As can be seen from Table 1, the waterborne insulating paint disclosed by the embodiment of the invention has better stability and more excellent electrical properties.
The foregoing shows and describes the general principles, essential features, and advantages of the invention. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, which are merely illustrative of the principles of the invention, but that various changes and modifications may be made without departing from the spirit and scope of the invention, which fall within the scope of the invention as claimed. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (9)
1. The water-based insulating paint is characterized by being prepared from the following components in parts by weight: 60-70 parts of polyether modified dimethylol hydantoin organic silicon polycondensate, 20-30 parts of polyurethane modified hyperbranched polyethyleneimine, 5-10 parts of surface modified nano boron fiber, 1-5 parts of defoaming agent, 1-5 parts of flatting agent, 1-3 parts of neutralization stabilizer, 1-5 parts of cosolvent and 20-30 parts of water;
the preparation method of the polyether modified dimethylol hydantoin organosilicon polycondensate comprises the following steps:
i, adding dimethylolhydantoin, 1-chloropropylmethyldiethoxysilane, a high-boiling-point solvent and a catalyst dibutyltin dilaurate into a three-necked bottle provided with a stirrer, a thermometer and a constant-pressure dropping funnel, raising the temperature to 75-85 ℃, then dropwise adding distilled water, stirring and reacting for 15-18 hours at the temperature of 90-100 ℃, and then performing rotary evaporation to remove the high-boiling-point solvent to obtain an intermediate product;
and II, dissolving the intermediate product obtained in the step I and monoamino polyether in an organic solvent to form a solution, adding an alkaline catalyst into the solution, stirring and reacting for 6-8 hours at the temperature of 50-60 ℃, and then removing the solvent by rotary evaporation to obtain the polyether modified dimethylol hydantoin organosilicon polycondensate.
2. The water-based insulating paint according to claim 1, wherein the defoaming agent is selected from one or more of polyoxyethylene polyoxypropylene amine ether, polydimethylsiloxane and polyoxypropylene glycerol ether; the flatting agent is one or more of a polyacrylate flatting agent, a cellulose acetate butyrate flatting agent and a polyvinyl butyral flatting agent; the neutralizing stabilizer is selected from one or more of 2-amino-2-methyl-1-propanol, triethanolamine, dimethylethanolamine and ammonia water; the cosolvent is selected from one or more of ethanol, isopropanol, ethylene glycol and n-butanol.
3. The aqueous insulating paint according to claim 1, wherein the mass ratio of the dimethylolhydantoin, the 1-chloropropylmethyldiethoxysilane, the high-boiling-point solvent, the dibutyltin dilaurate and the distilled water in step I is 1:1.12 (6-10): 0.3-0.6): 0.1-0.4.
4. The water-based insulating paint according to claim 1, wherein the high boiling point solvent is selected from one or more of dimethyl sulfoxide, N-dimethylformamide and N-methylpyrrolidone; the organic solvent is selected from one or more of isopropanol, dichloromethane, tetrahydrofuran and acetone; the basic catalyst is selected from one or more of triethylamine, triphenylphosphine and tetrabutylammonium bromide.
5. The water-based insulating paint according to claim 1, wherein the mass ratio of the intermediate product, the monoamino polyether, the organic solvent and the basic catalyst in the step II is (1-2):1 (8-12): 0.3-0.6.
6. The water-based insulating paint according to claim 1, wherein the preparation method of the polyurethane modified hyperbranched polyethyleneimine comprises the following steps: adding waterborne polyurethane, hyperbranched polyethyleneimine and dibutyltin dilaurate into dimethyl sulfoxide, stirring and reacting for 5-7 hours at 60-70 ℃, precipitating in ethanol, carrying out suction filtration, and removing a solvent by rotary evaporation to obtain the polyurethane modified hyperbranched polyethyleneimine.
7. The water-based insulating paint according to claim 6, wherein the mass ratio of the water-based polyurethane to the hyperbranched polyethyleneimine to the dibutyltin dilaurate to the dimethylsulfoxide is 1 (2-4) to (0.3-0.6) to (10-15).
8. The water-based insulating paint according to claim 1, wherein the preparation method of the surface-modified nano boron fiber comprises the following steps: dispersing nano boron fibers in ethanol, adding 1,3, 5-tri [3- (trimethoxysilyl) propyl ] -1,3, 5-triazine-2, 4,6(1H,3H,5H) -trione, stirring and reacting for 4-6 hours at 50-60 ℃, centrifuging, and washing for 3-5 times by using ethyl acetate to obtain surface modified nano boron fibers; the mass ratio of the nano boron fiber to the ethanol to the 1,3, 5-tri [3- (trimethoxysilyl) propyl ] -1,3, 5-triazine-2, 4,6(1H,3H,5H) -trione is (3-5): 1 (10-15): 1.
9. A method for preparing the water-based insulating paint according to any one of claims 1 to 8, characterized by comprising the steps of: uniformly mixing polyether modified dimethylol hydantoin organic silicon polycondensate, polyurethane modified hyperbranched polyethyleneimine, surface modified nano boron fiber and cosolvent according to a proportion to prepare mixed slurry, then adding a defoaming agent, a flatting agent, a neutralization stabilizer and water, and mixing again to obtain the water-based insulating paint.
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| WO2007091961A1 (en) * | 2006-02-10 | 2007-08-16 | Akzo Nobel N.V. | Microspheres |
| CN107779073A (en) * | 2017-11-17 | 2018-03-09 | 广东华兹卜新材料科技有限公司 | A kind of hot water resistance woodcare paint |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| WO2007091961A1 (en) * | 2006-02-10 | 2007-08-16 | Akzo Nobel N.V. | Microspheres |
| CN107779073A (en) * | 2017-11-17 | 2018-03-09 | 广东华兹卜新材料科技有限公司 | A kind of hot water resistance woodcare paint |
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Denomination of invention: A water-based insulating paint and its preparation method Effective date of registration: 20230404 Granted publication date: 20200811 Pledgee: Bank of China Limited Zaozhuang Branch Pledgor: Shandong Shengyu coating Co.,Ltd. Registration number: Y2023980037343 |
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