High-thermal-conductivity and high-heat-resistance environment-friendly impregnated resin paint and preparation method thereof

Abstract

The application belongs to the field of high polymer materials, and discloses a high-heat-conducting and high-heat-resistant environment-friendly impregnated resin paint and a preparation method thereof.The high-heat-conducting and high-heat-resistant environment-friendly impregnated resin paint is composed of the following components by weight: silicon-based modified paste 40-70%, hydroquinone polymerization inhibitor 0.3%, molecular weight regulator 0.5-3%, wetting and leveling agent 1.7%, catalyst 1.8%, propylene ester active agent 22.1-52.1%, and crosslinking agent 1.6%.The silicon-based modified paste is composed of the following components: polyester imine resin 20-50%, propylene ester active agent 14%, heat-conducting filler 35-65%, rheological modifier 0.5%, and dispersant 0.5%.The silicon-based modified paste is prepared by the following steps: sequentially putting all raw materials into a stirrer, and stirring, homogenizing and dispersing to obtain the silicon-based modified paste.The impregnated resin paint has the advantages of high heat conduction, high heat resistance and the like.

Description

TECHNICAL FIELD

[0001] The present application belongs to the field of high polymer materials, and particularly relates to a high-heat-conducting and high-heat-resistant environment-friendly impregnating resin paint and a preparation method thereof. BACKGROUND

[0002] Insulating paint is a functional coating made of high molecular resin as the main film-forming material by adding solvents, additives and functional fillers. Its core function is to provide insulation protection for electrical / electronic components to prevent current leakage, arc discharge or short circuit, while also having heat resistance, moisture resistance, corrosion resistance and other properties to ensure long-term stable operation of the equipment.

[0003] The existing insulating paint products have various problems, such as weak adhesion to the substrate, low filling efficiency of the paint, and difficulty in completely filling the small pores inside the material, resulting in the formation of a "weak zone" inside the insulating layer. Low heat conduction efficiency of the insulating layer can cause heat accumulation and exacerbate abnormal temperature rise of the equipment, and the lack of filling rate and the accumulation of temperature rise can further limit the heat resistance of the insulating paint. When heat cannot be effectively dispersed, the material is prone to aging in a high-temperature environment, ultimately reducing its heat resistance rating and shortening the service life of the equipment.

[0004] Most of the existing resin insulating paints have high viscosity, and organic solvents are used in the preparation process, which can only withstand heat of about 180℃ or below, and some raw material components use epoxy and anhydride, which are unstable and have a high tackifying coefficient. SUMMARY

[0005] The present application aims to solve the above technical problems and provides an environment-friendly insulating paint with high heat conductivity, high heat resistance and comprehensive performance.

[0006] To achieve the above-mentioned application purposes, the present application provides the following technical solutions:

[0007] In a first aspect, the present application provides a high-heat-conducting and high-heat-resistant environment-friendly impregnating resin paint, which is composed of the following components by weight: silicon-based modified paste 40-70%, hydroquinone polymerization inhibitor 0.3%, molecular weight regulator 0.5-3%, wetting and leveling agent 1.7%, catalyst 1.8%, propylene ester active agent 22.1-52.1%, and crosslinking agent 1.6%.

[0008] The silicon-based modified paste is composed of the following components by weight: polyester imine resin 20-50%, propylene ester active agent 14%, heat-conducting filler 35-65%, rheological modifier 0.5%, and dispersant 0.5%.

[0009] The silicon-based modified paste is prepared by the following steps: all raw materials are sequentially put into a stirrer, and then stirred, homogenized and dispersed to obtain the silicon-based modified paste.

[0010] Preferably, the stirring speed during the preparation of the silicon-based modified paste is 600-1000 rpm, and the stirring time is 60-120 minutes.

[0011] Preferably, the molecular weight regulator is an a-methyl styrene dimer.

[0012] Preferably, the wetting and leveling agent is TEGO 4100.

[0013] Preferably, the catalyst is isooctoate. More preferably, the catalyst is one or more of manganese isooctoate, copper isooctoate, and iron isooctoate.

[0014] Preferably, the crosslinking agent is a peroxide, more preferably one or more of 3,3-bis (tert-butyl peroxy) -3,3,5-trimethylcyclohexane, dicumyl peroxide (DCP), tert-butyl benzene peroxide (TBPB), and benzoyl peroxide (PBO).

[0015] Preferably, the thermally conductive filler is one or more of nano- or micro-sized silicon dioxide, fumed silica, aluminum oxide powder, boron nitride, and magnesium oxide.

[0016] Preferably, the rheological modifier is one or more of bentonite, silicate, anti-settling wax, and polyurea.

[0017] Preferably, the dispersant is a high molecular weight copolymer alkyl ammonium salt, more preferably one or more of BYK-9076, BYK-190, and BYK-26475.

[0018] Preferably, the acrylate active agent is one or more of 2-hydroxyethyl methacrylate, 1-ethylene glycol-2-methacrylate, 2-ethylene glycol-2-methacrylate, 3-ethylene glycol-2-methacrylate, hexanediol diacrylate (HDDA), and diallyl phthalate (DAP).

[0019] In a second aspect, the present application provides a method for preparing the high-thermal-conductivity and high-heat-resistance environmentally friendly impregnation resin paint, comprising the following steps:

[0020] S1. Adding a hydroquinone polymerization inhibitor, a molecular weight regulator, and a wetting and leveling agent to the silicon-based modified paste, dispersing and shearing the mixture, increasing the temperature, and then decreasing the temperature to below 40℃, and then adding a catalyst and a crosslinking agent and mixing uniformly;

[0021] S2. Adding an acrylate active agent, filtering, and discharging.

[0022] Preferably, in the step S1, the dispersing speed is 600-1000 rpm, and the dispersing time is 30-60 minutes.

[0023] Preferably, in the step S1, the temperature is raised to 70-80℃, and the temperature is kept for 30 minutes-1 hour.

[0024] Preferably, the silicon-based modified slurry is prepared by mixing all raw materials and then stirring and dispersing uniformly.

[0025] Preferably, the stirring and dispersing speed is 600-1000 rpm. The dispersing time is preferably 60-120 minutes.

[0026] The polyester resin is imidized to improve the heat resistance of the resin. The molecular weight regulator expands the branch chain, improves the molecular weight, the film forming density and the toughness, improves the corrosion resistance, and improves the bonding strength and the electrical insulation strength. The wetting and leveling agent improves the surface tension, improves the permeability and the thermal conductivity. The acrylate active agent adjusts the viscosity, and participates in the curing to reduce the shrinkage. The crosslinking agent initiates ring opening below 120℃, gels at 100-110℃, greatly improves the amount of hanging paint and the filling property to the motor winding, further improves the thermal conductivity and reduces the motor temperature rise. The thermal conductive filler improves the thermal conductivity and the heat resistance of the film forming material, so that it can withstand heat above 220℃. The dispersant improves the coating ability of the thermal conductive filler and the resin.

[0027] Compared with the prior art, the present application introduces a thermal conductive material, an acrylate active agent and an unsaturated polyester imine resin to react, to obtain an environmentally friendly, solvent-free, VOC-free, non-flammable and non-explosive high-solid and low-viscosity insulation impregnating resin. The components synergistically improve the thermal conductivity and heat resistance, and also have good adhesion, toughness, bonding strength and electrical strength, and have excellent comprehensive performance. DETAILED DESCRIPTION

[0028] The technical solutions of the present application will be further described below in combination with specific embodiments, but the present application is not limited to the following embodiments.

[0029] Unless otherwise specified, the instruments or reagents used in the examples are conventional instruments or reagents in the art, which are conventional products that can be purchased on the market. Unless otherwise specified, the specific experimental operations involved in this paper are understood or known by those skilled in the art according to their mastery of common knowledge or conventional technical means, and will not be described one by one.

[0030] The preparation method of the polyester imine resin is as follows:

[0031] New pentanediol 50g, propylene glycol 45g, tris (2-hydroxyethyl) isocyanurate 35g, terephthalic acid 60g and butyl titanate 0.5g are added into a reaction bottle, start to heat to melt the material, start to stir; continue to heat to 200℃, and keep the temperature to react, until the material system becomes clear, the acid value is less than 10mgKOH / g, then reduce the temperature; when the temperature drops to 160℃, add trimellitic anhydride 100g, diamino diphenyl methane 40g, continue to heat to 200℃, and keep the temperature to react, until the acid value is 60mgKOH / g, vacuum, reduce pressure to extract the residual solvent, reduce the temperature; when the temperature drops to 150℃, add ethylene glycol butyl ether 140g, when the temperature drops below 60℃, add water-based amino resin methyl etherified melamine resin 33g, adjust the pH to 7.0-9.0 with neutralizer dimethyl ethanolamine 25g, to obtain water-soluble polyester imine resin. The water-soluble resin is a viscous transparent liquid with a solid content of 70%.

[0032] The α-methyl styrene dimer is a commercially available product.

[0033] The dispersants BYK-9076, BYK-190 and BYK-26475 are commercially available products from BYK, Germany.

[0034] The wetting and leveling agent TEGO 4100 is a commercially available product from Degussa, Germany.

[0035] Example 1

[0036] 1. Preparation of silicon-based modified paste

[0037] (1) The following raw material components are prepared according to weight percentage:

[0038] Polyester imine resin 50%;

[0039] 3-ethyleneglycol-2-methacrylate 14%;

[0040] Nano-silicon dioxide 35%;

[0041] Bentonite 0.5%;

[0042] Dispersant BYK-9076 0.5%.

[0043] (2) All raw materials are sequentially put into a stirrer, and stirred, homogenized and dispersed at a speed of 600 revolutions per minute for 120 minutes to obtain a silicon-based modified paste.

[0044] 2. Preparation of environmentally friendly impregnating resin paint

[0045] (1) The following raw material components are prepared according to weight percentage:

[0046] Silicon-based modified paste 40%;

[0047] hydroquinone polymerization inhibitor 0.3%;

[0048] a-methylstyrene dimer 0.5%;

[0049] wetting and leveling agent TEGO 4100 1.7%;

[0050] manganese isooctoate 1.8%;

[0051] 2-hydroxyethyl methacrylate 52.1%;

[0052] 3,3-bis(tert-butylperoxy)-3,3,5-trimethylcyclohexane 1.6%.

[0053] (2) Add the polymerization inhibitor, molecular weight regulator, and wetting and leveling agent to the silicon-based modified slurry, disperse and shear the mixture, the dispersion speed is 600 rpm, the dispersion time is 60 minutes, the temperature is raised to 70°C for 1 hour, the temperature is lowered to below 40°C, the catalyst and crosslinking agent are added and uniformly mixed; add the acrylate active agent to adjust the viscosity and participate in the curing to reduce shrinkage, filter, and discharge. The test shows that the solid content of the finished product is 99.1%, and the viscosity is less than 30 mPa·S (23±0.5°C).

[0054] Example 2

[0055] 1. Preparation of silicon-based modified slurry

[0056] (1) Prepare the following raw material components:

[0057] polyester imine resin 30%;

[0058] 1-ethylene glycol-2-methacrylate 14%;

[0059] boron nitride 55%;

[0060] polyurea 0.5%;

[0061] dispersant BYK-190 0.5%.

[0062] (2) Put all the raw materials into a stirrer in turn, stir and homogenize at a speed of 800 rpm for 80 minutes to obtain a silicon-based modified slurry.

[0063] 2. Preparation of environmentally friendly impregnated resin paint

[0064] (1) Prepare the following raw material components by weight percentage:

[0065] silicon-based modified slurry 50%;

[0066] hydroquinone polymerization inhibitor 0.3%;

[0067] Alpha-methylstyrene dimer 2%;

[0068] Wetting and levelling agent TEGO 4100 1.7%;

[0069] Copper isooctoate 1.8%;

[0070] 2-Hydroxyethyl methacrylate 42.1%;

[0071] Dicumyl peroxide 1.6%.

[0072] (2) Add a polymerization inhibitor, a molecular weight regulator, and a wetting and levelling agent to the silicon-based modified slurry, disperse and shear the mixture, the dispersion speed is 800 revolutions per minute, the dispersion time is 50 minutes, the temperature is raised to 75°C and maintained for 45 minutes, the temperature is lowered to below 40°C, a catalyst and a crosslinking agent are added and uniformly mixed, an acrylate active agent is added to adjust the viscosity and participate in curing to reduce shrinkage, filtration is performed, and the product is discharged. After testing, the solid content of the finished product is 99.3%, and the viscosity is less than 30 mPa·S (23±0.5°C).

[0073] Example 3

[0074] 1. Preparation of a silicon-based modified slurry

[0075] (1) Prepare the following raw material components by weight percentage:

[0076] Polyester imine resin 20%;

[0077] 2-Ethylene glycol-2-methacrylate 14%;

[0078] Alumina powder 65%;

[0079] Silicate 0.5%;

[0080] Dispersant BYK-26475 0.5%.

[0081] (2) Put all the raw materials into a stirrer in turn, stir and homogenize at a speed of 1000 revolutions per minute for 60 minutes, and obtain a silicon-based modified slurry.

[0082] 2. Preparation of an environmentally friendly impregnated resin paint

[0083] (1) Prepare the following raw material components by weight percentage:

[0084] Silicon-based modified slurry 70%;

[0085] P-phenylenediamine polymerization inhibitor 0.3%;

[0086] Alpha-methylstyrene dimer 3%;

[0087] Wetting and levelling agent TEGO 4100 1.7%;

[0088] Iron isooctoate 1.8%;

[0089] 2-Hydroxyethyl methacrylate 22.1%;

[0090] Tert-butyl benzene peroxide 1.6%.

[0091] (2) The polymerization inhibitor, the molecular weight regulator, and the wetting and leveling agent are added to the silicon-based modified paste, the mixture is dispersed and sheared, the dispersion speed is 1000 rpm, the dispersion time is 30 minutes, the temperature is raised to 80°C and kept for 30 minutes, the temperature is lowered to below 40°C, the catalyst and the crosslinking agent are added and uniformly mixed, the acrylate active agent is added to adjust the viscosity and participate in the curing to reduce the shrinkage, and then the mixture is filtered and discharged. The solid content of the finished product is 99.7%, and the viscosity is lower than 30 mPa·S (23±0.5°C).

[0092] Comparative Example

[0093] 1. The following resin paint raw material components are prepared according to the weight percentage:

[0094] Polyester imine resin 55%;

[0095] Hydroquinone polymerization inhibitor 0.3%;

[0096] Alpha-methyl styrene dimer 2.5%;

[0097] Wetting and leveling agent TEGO 4100 1.7%;

[0098] Copper isooctoate 1.8%;

[0099] 2-Hydroxyethyl methacrylate 37.1%;

[0100] Dicumyl peroxide 1.6%.

[0101] 2. The preparation steps are as follows:

[0102] The polymerization inhibitor, the molecular weight regulator, and the wetting and leveling agent are added to the polyester imine resin, the mixture is dispersed and sheared, the dispersion speed is 800 rpm, the dispersion time is 50 minutes, the temperature is raised to 70°C and kept for 1 hour, the temperature is lowered to below 40°C, the catalyst and the crosslinking agent are added and uniformly mixed, the acrylate active agent is added to adjust the viscosity, and then the mixture is filtered and discharged.

[0103] Product performance test

[0104] The impregnated resin paint prepared in the above Examples 1-3 and Comparative Example is tested to detect its various performances.

[0105] 1. VOC detection

[0106] Detection method: GB / T 23985-2009 "Paint and varnish Determination of the content of volatile organic compounds (VOC) by difference method"

[0107] Detection results: The detection results of the impregnated resin paint of examples 1-3 are shown in table 1.

[0108] 2. Microwave temperature rise detection

[0109] The winding temperature rise of the impregnated insulation paint was detected by microwave temperature rise experiment.

[0110] Detection results: The temperature rise results of the samples of examples 1-3 and the comparative example are shown in table 1.

[0111] Table 1. Microwave temperature rise detection results

[0112]

[0113] As can be seen from table 1, compared with the comparative example, the winding temperature rise results of the impregnated insulation paint of examples 1-3 are decreased, indicating that its heat dissipation performance is good, the thermal conductivity is excellent, the energy loss is less, and it is more conducive to electrical stability.

[0114] 3. Detection of heat resistance

[0115] Detection method: GB / T 27761-2011 "Thermogravimetric analyzer weight loss and residual amount test method"

[0116] Detection results: The heat resistance of the motor winding system using the impregnated resin paint of examples 1-3 is increased from 180℃ before modification (comparative example) to ≥220℃, and even up to 260℃, and the product does not soften, crack or carbonize, and the TGA is ≥270℃. The results are shown in table 2 below.

[0117] Table 2. Heat resistance results

[0118]

[0119] 4. Detection of bonding strength and electrical performance

[0120] Detection method: GB / T 7354-2018 "High voltage test technology Partial discharge measurement"

[0121] GB / T 1981.2-2009 "Paint for electrical insulation Part 2: Test methods"

[0122] Detection results: The detection results of the impregnated resin paint of examples 1-3 and the comparative example are shown in table 3.

[0123] Table 3. Bonding strength and electrical performance results

[0124]

[0125] As shown in Table 3, the adhesive strength of the resin paints of Examples 1-3 is higher than that of the comparative example. The electrical strength and PDIV partial discharge values indicate that the insulating paint of the present application has a higher high electrical strength, which means that the insulating paint can withstand higher voltage without being punctured, has excellent insulation performance, effectively prevents current leakage and short circuit, and ensures the safe operation of the equipment. Compared with the comparative example, the voltage resistance of Examples 1-3 is stronger, which can enable the electronic equipment to work in a more severe voltage environment, thereby improving the reliability and service life of the equipment. In addition, the PDIV partial discharge starting voltage of Examples 1-3 is also higher compared with the comparative example, which indicates that it has excellent corona resistance. The above electrical performance test results show that the insulating paint of the present application has excellent performance in terms of insulation performance, voltage resistance, corona resistance, insulation stability and anti-interference ability, and can ensure the safe, stable and reliable operation of electronic equipment.

[0126] The above is only a preferred embodiment of the present application, and does not limit the present application in any form. Any simple modification, equivalent change and modification of the above embodiment without departing from the technical solution of the present application, according to the technical essence of the present application, are still within the scope of the technical solution of the present application.

Claims

1. A high thermal conductivity and high heat resistance environmentally friendly impregnating resin paint, characterized in that, The composition is as follows by weight: modified pulp 40-70%, hydroquinone polymerization inhibitor 0.3%, molecular weight regulator 0.5-3%, wetting and leveling agent 1.7%, catalyst 1.8%, propylene ester active agent 22.1-52.1%, cross-linking agent 1.6%; The modified slurry is composed of the following components by weight percentage: 20-50% polyester imide resin, 14% propylene ester active agent, 35-65% thermal conductive filler, 0.5% rheology regulator, and 0.5% dispersant; The modified pulp is prepared by the following steps: all raw materials are sequentially put into a stirrer, stirred and homogenized to obtain a modified pulp; The acrylic ester active agent is one or more of 2-hydroxyethyl methacrylate, 1-ethylene glycol-2-methacrylate, 2-ethylene glycol-2-methacrylate, 3-ethylene glycol-2-methacrylate, hexanediol diacrylate, and diallyl phthalate; The rheology regulator is one or more of bentonite, silicate, anti-settling wax, and polyurea; The dispersant is a high molecular weight copolymer alkyl ammonium salt; The molecular weight regulator is α-methylstyrene dimer.

2. The high thermal conductivity and high heat resistance environmentally friendly impregnating resin paint according to claim 1, characterized in that: During the preparation of the modified pulp, the stirring speed is 600-1000 rpm and the stirring time is 60-120 minutes.

3. The high thermal conductivity and high heat resistance environmentally friendly impregnating resin paint according to claim 1, characterized in that: The catalyst is isooctanoate.

4. The high thermal conductivity and high heat resistance environmentally friendly impregnating resin paint according to claim 3, characterized in that: The catalyst is one or more of manganese isooctanoate, copper isooctanoate and iron isooctanoate.

5. The high thermal conductivity and high heat resistance environmentally friendly impregnating resin paint according to claim 1, characterized in that: The crosslinking agent is a peroxide.

6. The high thermal conductivity and high heat resistance environmentally friendly impregnating resin varnish according to claim 5, characterized in that: The cross-linking agent is one or more of 3,3-bis(tert-butylperoxy)-3,3,5-trimethylcyclohexane, dicumyl peroxide, tert-butylbenzene peroxide, and benzoyl peroxide.

7. The high thermal conductivity and high heat resistance environmentally friendly impregnating resin varnish according to claim 1, characterized in that: The thermally conductive filler is one or more of nano- or micron-sized silicon dioxide, fumed silicon dioxide, aluminum oxide powder, boron nitride, and magnesium oxide.

8. The high thermal conductivity and high heat resistance environmentally friendly impregnating resin varnish according to claim 1, characterized in that: The wetting and leveling agent is TEGO 4100.

9. The high thermal conductivity and high heat resistance environmentally friendly impregnating resin varnish according to claim 1, characterized in that: The dispersant is one or more of BYK-9076 and BYK-190.

10. A method for preparing the high thermal conductivity and high heat resistance environmentally friendly impregnating resin varnish according to any one of claims 1 to 9, characterized in that: The following steps are involved: S1. Add hydroquinone polymerization inhibitor, molecular weight regulator, and wetting and leveling agent to the modified pulp, disperse and shear the mixture, heat it up, cool it down to below 40°C, and then add catalyst and cross-linking agent and mix them evenly; S2. Add propylene ester surfactant, filter, and discharge.

11. The method according to claim 10, characterized in that In the step S1, the dispersion speed is 600-1000 rpm, and the dispersion time is 30-60 minutes.

12. The method according to claim 10, characterized in that In the step S1, the temperature is raised to 70-80° C. and kept warm for 30 minutes to 1 hour.

13. The method according to claim 10, characterized in that During the preparation of the modified slurry, the stirring and dispersing speed is 600 to 1000 rpm, and the dispersing time is 60 to 120 minutes.

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