A kind of organic silicon insulating paint and preparation method thereof

Abstract

The present application relates to an organic silicon insulating varnish, and relates to the field of insulating varnishes, which comprises the following components by mass: 100-200 parts of a polymer modifier, 60-80 parts of hydrophobic mesoporous silica, 300-500 parts of fluorine nitrogen modified polysiloxane, and 80-100 parts of an active diluent. The present application has the effect of improving the insulating performance and weather resistance of the organic silicon insulating varnish.

Description

Technical Field

[0001] The present application relates to the field of insulating varnishes, and in particular to an organic silicon insulating varnish and a preparation method thereof. Background Art

[0002] Insulating varnish is a coating with excellent electrical insulation properties. It is an indispensable material in motors and electrical equipment. The quality and service life of motors and other electrical equipment depend to a large extent on the insulating varnish used. Insulating varnish has good electrochemical, thermal, mechanical and chemical properties. It is mostly varnish and also colored paint. Insulating varnish is a special varnish among varnishes. It is based on high molecular polymers and can be cured into an insulating film or an insulating whole under certain conditions. It is an important insulating material.

[0003] With the continuous advancement of science and technology, motors and electrical appliances are developing towards miniaturization and environmental protection. Therefore, people have put forward higher and higher requirements on the quality and environmental protection of insulating paint. Silicone resin materials are a kind of polymer materials with silicon-oxygen bonds as the main chain structure and organic groups as side groups. Silicone resin materials have good stability and insulation properties, but in actual use, the high temperature and high humidity environment faced by the motor will reduce the performance and service life of the insulating paint, and the insulation performance cannot meet the requirements of the working environment, so it needs to be improved. Summary of the invention

[0004] In order to improve the insulation performance of organic silicon insulating varnish, the present application provides an organic silicon insulating varnish and a preparation method thereof.

[0005] The present application provides an organic silicon insulating varnish and a preparation method thereof using the following technical solutions:

[0006] In the first aspect, the present application provides an organic silicon insulating varnish, which adopts the following technical solution:

[0007] An organic silicon insulating varnish comprising the following components in parts by weight:

[0008] Polymer modifier 100-200 parts

[0009] 60-80 parts of hydrophobic mesoporous silica

[0010] Fluorine nitrogen modified polysiloxane 300-500 parts

[0011] Active diluent 80-100 parts.

[0012] Fluorine-nitrogen modified polysiloxane reduces the surface energy of the molecule by introducing fluorine atoms and nitrogen atoms, thereby improving the hydrophobicity and weather resistance of the silicone insulating varnish, thereby improving the insulation performance; the polymer modifier has good flexibility, adhesion and wear resistance, which can reinforce the fluorine-nitrogen modified polysiloxane and improve the stability of the silicone insulating varnish, thereby improving the insulation performance of the silicone insulating varnish; hydrophobic mesoporous silica has good insulation performance and thermal stability, which can synergize with fluorine-nitrogen modified polysiloxane and polymer modifier to improve the insulation performance and weather resistance of the silicone insulating varnish; the active diluent has good reactivity and dilution capacity, which can further improve the insulation performance of the silicone insulating varnish.

[0013] Preferably, the polymer modifier includes polycaprolactone triol, polyurethane prepolymer and 2-ethyl methacrylate.

[0014] Polycaprolactone triol has good hydrophobic properties and can introduce hydrophobic side chains into the molecules of polyurethane prepolymers to reduce water penetration, thereby improving the insulating properties and weather resistance of silicone insulating varnishes; 2-ethyl methacrylate introduces acrylates into the surface of polymer modifiers. Acrylates have good durability and weather resistance, which can improve the insulating properties and weather resistance of silicone insulating varnishes.

[0015] Preferably, the polyurethane prepolymer comprises isophorone diisocyanate, p-methoxyphenol and diethanolamine.

[0016] Polyurethane prepolymer is synthesized by isophorone diisocyanate, p-methoxyphenol and diethanolamine. Isophorone diisocyanate and p-methoxyphenol have good hydrophobicity and weather resistance, which can improve the stability of fluorine-nitrogen modified polysiloxane, thereby improving the insulation performance and weather resistance of silicone insulating paint.

[0017] Preferably, the mass ratio of the polycaprolactone triol, the polyurethane prepolymer and 2-ethyl methacrylate is (0.05-0.15):1:0.2.

[0018] The organic silicon insulating varnish prepared according to the above mass ratio has good insulating properties and weather resistance.

[0019] Preferably, the reaction raw materials of the hydrophobic mesoporous silica include ethyl orthosilicate, heptadecafluorodecyltriethoxysilane and potassium aluminum sulfate dodecahydrate.

[0020] By reacting ethyl orthosilicate and heptadecafluorodecyltriethoxysilane, mesoporous silica with a rich pore structure can be obtained. The introduced fluorine atoms reduce the surface energy of the mesoporous silica and improve the hydrophobicity and thermal stability of the mesoporous silica. Potassium aluminum sulfate dodecahydrate can introduce an aluminum source on the surface of the mesoporous silica, thereby loading alumina on the surface of the mesoporous silica. Alumina has good insulating and hydrophobic properties and can synergize with mesoporous silica. The obtained hydrophobic mesoporous silica has good insulating and thermal insulation properties, thereby improving the insulating properties and weather resistance of the silicone insulating paint.

[0021] Preferably, the hydrophobic mesoporous silica is prepared by the following steps:

[0022] Mixing and dispersing ethyl orthosilicate and heptadecafluorodecyltrimethoxysilane in anhydrous ethanol to obtain a silicon-based dispersion, adding ammonia water to the silicon-based dispersion to obtain a silicon-based reaction liquid, reacting in a water bath with stirring to obtain a crude product, filtering and washing the crude product, calcining and grinding the washed crude product to obtain a product;

[0023] Potassium aluminum sulfate dodecahydrate and the product are dispersed in deionized water to obtain a suspension, the suspension is stirred for reaction, filtered and washed to obtain a modified product, the modified product is calcined and then ground, and sieved to obtain hydrophobic mesoporous silica.

[0024] The hydrophobic mesoporous silica prepared according to the above steps has good insulation properties and weather resistance.

[0025] Preferably, the fluorine-nitrogen modified polysiloxane includes fluorine-containing olefins, polymethylhydrogensilazane and phenyl polytrimethylsiloxane.

[0026] By introducing fluorine atoms into fluorine-containing olefins, the surface energy of fluorine-nitrogen modified polysiloxane can be reduced, and stability and weather resistance can be improved; phenyl polytrimethylsilane has good hydrophobic properties, and polymethylhydrogensilazane has good corrosion resistance, antioxidant properties and high temperature resistance. The fluorine-nitrogen modified polysiloxane obtained by compounding the two has good weather resistance and insulation properties.

[0027] Preferably, the mass ratio of the fluorine-containing olefin, polymethylhydrogensilazane and phenylpolytrimethylsiloxane is (0.1-0.2):1:0.8.

[0028] The organic silicon insulating varnish prepared according to the above steps has good insulating performance and weather resistance.

[0029] Preferably, the reaction raw materials of the active diluent include methacryloyl chloride and anhydrous benzyl alcohol.

[0030] The active diluent prepared by methacryloyl chloride and anhydrous benzyl alcohol has good reactivity and dilution capacity, can regulate the compatibility between the components of the silicone insulating varnish, improve the stability of the silicone insulating varnish, and thus improve the insulation performance and weather resistance.

[0031] In a second aspect, the present application provides a method for preparing an organic silicon insulating varnish, using the following technical solution:

[0032] A preparation method for organic silicon insulating varnish, wherein the organic silicon insulating varnish is prepared by the following steps:

[0033] The polymer modifier and the fluorine-nitrogen modified polysiloxane are mixed and melted to obtain the modified polysiloxane, the hydrophobic mesoporous silica and the active diluent are added into the modified polysiloxane and stirred, and the organic silicon insulating varnish is obtained after cooling.

[0034] The organic silicon insulating varnish prepared according to the above steps has good weather resistance and insulating properties.

[0035] In summary, the present application includes at least one of the following beneficial technical effects:

[0036] 1. Fluorine-nitrogen modified polysiloxane reduces the surface energy of the molecule by introducing fluorine atoms and nitrogen atoms, thereby improving the hydrophobicity and weather resistance of the silicone insulating varnish, thereby improving the insulation performance; the polymer modifier has good flexibility, adhesion and wear resistance, which can reinforce the fluorine-nitrogen modified polysiloxane and improve the stability of the silicone insulating varnish, thereby improving the insulation performance of the silicone insulating varnish; hydrophobic mesoporous silica has good insulation performance and thermal stability, which can cooperate with fluorine-nitrogen modified polysiloxane and polymer modifier to improve the insulation performance and weather resistance of the silicone insulating varnish; the active diluent has good reactivity and dilution ability, which can further improve the insulation performance of the silicone insulating varnish.

[0037] 2. Polymer modifiers, hydrophobic mesoporous silica and fluorine-nitrogen modified polysiloxane have good hydrophobic properties and heat resistance, which can improve the weather resistance of silicone insulating paint, thereby improving the insulating properties of silicone insulating paint. DETAILED DESCRIPTION

[0038] The present application discloses an organic silicon insulating varnish and a preparation method thereof. The present application is further described in detail below in conjunction with the embodiments:

[0039] Example 1

[0040] Preparation of polymer modifiers

[0041] 224 g of isophorone diisocyanate (CAS No. 4098-71-9), 1.5 g of p-methoxyphenol, 0.5 g of dibutyltin dilaurate and 500 g of ethyl acetate were dispersed in a four-necked flask, 75 g of diethanolamine was added dropwise to the four-necked flask within 30 min, and the four-necked flask was stirred at a speed of 200 r / min in a 50° C. water bath for 2 h to obtain a polyurethane prepolymer; 12 g of polycaprolactone triol (CAS No.: 39 280-09-6), the addition was completed within 30 minutes, the four-necked flask was stirred at a speed of 200r / min for 2 hours in a 60°C water bath to obtain a modified polyurethane; the modified polyurethane was heated to 80°C, 48g of 2-ethyl methacrylate (CAS No.: 97-63-2) was added dropwise within 1 hour, the reaction was stirred at a speed of 200r / min for 3 hours in a 80°C water bath to obtain a product solution, the product solution was subjected to reduced pressure distillation to remove the solvent, and a polymer modifier was obtained.

[0042] Preparation of hydrophobic mesoporous silica

[0043] 160g of ethyl orthosilicate and 90g of heptadecafluorodecyltrimethoxysilane are mixed and dispersed in 200mL of anhydrous ethanol to obtain a silicon-based dispersion liquid, 10mL of 1mol / L ammonia water is added to the silicon-based dispersion liquid to obtain a silicon-based reaction liquid, and the crude product is reacted under stirring in a water bath to obtain the crude product, the crude product is filtered, washed with deionized water, and the washed crude product is calcined and ground to obtain the product; 50g of potassium aluminum sulfate dodecahydrate and 120g of the product are dispersed in 500mL of deionized water to obtain a suspension, the suspension is stirred for reaction, filtered, washed with deionized water to obtain a modified product, the modified product is calcined and ground, and passed through a 100-mesh sieve to obtain hydrophobic mesoporous silica.

[0044] Preparation of fluorine-nitrogen modified polysiloxane

[0045] Polymethylhydrogensilazane (CAS No.: 475645-84-2) and fluorine-containing olefins were subjected to reduced pressure distillation under nitrogen protection to remove residual water in the raw materials to obtain anhydrous polymethylhydrogensilazane and anhydrous fluorine-containing olefins; under nitrogen protection, 315.79 g of anhydrous polymethylhydrogensilazane and 31.58 g of anhydrous fluorine-containing olefins were mixed to obtain a fluorine-modified silane mixture, 5 g of chloroplatinic acid was added to the fluorine-modified silane mixture, and the mixture was reacted in an oil bath at 70°C. The reaction mixture was stirred for 5 hours to obtain a fluorine-containing silazane; 252.63 g of phenyl polytrimethoxysilane (CAS No.: 73559-47-4) and 1 mL of 1 mol / L hydrochloric acid were added to the fluorine-containing silazane, and the mixture was stirred at a speed of 200 r / min in an oil bath at 80°C for 2 hours, and the fluorine-modified silane mixture after the reaction was rotary evaporated to obtain a polymer modifier; the above-mentioned fluorine-containing olefin is hexafluoro-2-butene (CAS No.: 407-60-3).

[0046] Preparation of reactive diluent

[0047] 100 g of methacryloyl chloride (CAS No.: 920-46-7), 100 g of anhydrous benzyl alcohol (CAS No.: 100-51-6) and 0.5 g of an inhibitor are mixed to obtain a reactant, and the reactant is reacted in an 80° C. oil bath for 2 h to obtain a reaction product, a 1 mol / L sodium bicarbonate aqueous solution is added to the reaction product for washing, followed by washing with a 0.1 mol / L sodium hydroxide aqueous solution, and finally washing with deionized water, and after standing, the active diluent organic solution is obtained by layering; the active diluent organic solution is subjected to reduced pressure distillation to obtain an active diluent.

[0048] Preparation of silicone insulating varnish

[0049] 100 g of a polymer modifier and 300 g of fluorine-nitrogen modified polysiloxane were mixed and melted to obtain modified polysiloxane, 60 g of hydrophobic mesoporous silica and 80 g of an active diluent were added to the modified polysiloxane and stirred for 30 minutes, and then the organic silicone insulating varnish was obtained after cooling.

[0050] Example 2

[0051] Preparation of polymer modifiers

[0052] 224 g of isophorone diisocyanate (CAS No. 4098-71-9), 1.5 g of p-methoxyphenol, 0.5 g of dibutyltin dilaurate and 500 g of ethyl acetate were dispersed in a four-necked flask, 75 g of diethanolamine was added dropwise to the four-necked flask within 30 min, and the four-necked flask was stirred at a speed of 200 r / min in a 50° C. water bath for 2 h to obtain a polyurethane prepolymer; 33.33 g of polycaprolactone triol (CAS No.: 3 9280-09-6), the addition was completed within 30 minutes, the four-necked flask was stirred at a speed of 200r / min for 2 hours in a 60°C water bath to obtain a modified polyurethane; the modified polyurethane was heated to 80°C, 44.45g of 2-ethyl methacrylate (CAS No.: 97-63-2) was added dropwise within 1 hour, the reaction was stirred at a speed of 200r / min for 3 hours in a 80°C water bath to obtain a product solution, the product solution was subjected to reduced pressure distillation to remove the solvent, and a polymer modifier was obtained.

[0053] Preparation of hydrophobic mesoporous silica

[0054] 160g of ethyl orthosilicate and 90g of heptadecafluorodecyltrimethoxysilane are mixed and dispersed in 200mL of anhydrous ethanol to obtain a silicon-based dispersion liquid, 10mL of 1mol / L ammonia water is added to the silicon-based dispersion liquid to obtain a silicon-based reaction liquid, and the crude product is reacted under stirring in a water bath to obtain the crude product, the crude product is filtered, washed with deionized water, and the washed crude product is calcined and ground to obtain the product; 50g of potassium aluminum sulfate dodecahydrate and 120g of the product are dispersed in 500mL of deionized water to obtain a suspension, the suspension is stirred for reaction, filtered, washed with deionized water to obtain a modified product, the modified product is calcined and ground, and passed through a 100-mesh sieve to obtain hydrophobic mesoporous silica.

[0055] Preparation of fluorine-nitrogen modified polysiloxane

[0056] Polymethylhydrogen silazane (CAS No.: 475645-84-2) and fluorine-containing olefins are respectively subjected to reduced pressure distillation under nitrogen protection to remove residual water in the raw materials to obtain anhydrous polymethylhydrogen silazane and anhydrous fluorine-containing olefins; under nitrogen protection, 300g of anhydrous polymethylhydrogen silazane and 60g of anhydrous fluorine-containing olefins are mixed to obtain a fluorine-modified silane mixture, 5g of chloroplatinic acid is added to the fluorine-modified silane mixture, and the mixture is reacted in an oil bath at 70°C for 5h to obtain a fluorine-containing silazane; 240g of phenyl polytrimethoxysilane (CAS No.: 73559-47-4) and 1mL of 1mol / L hydrochloric acid are added to the fluorine-containing silazane, and the mixture is stirred and reacted at a speed of 200r / min for 2h under an oil bath condition of 80°C, and the fluorine-modified silane mixture after the reaction is rotary evaporated to obtain a polymer modifier; the above-mentioned fluorine-containing olefin is hexafluoro-2-butene (CAS No.: 407-60-3).

[0057] Preparation of active diluent

[0058] 100 g of methacryloyl chloride (CAS No.: 920-46-7), 100 g of anhydrous benzyl alcohol (CAS No.: 100-51-6) and 0.5 g of an inhibitor are mixed to obtain a reactant, and the reactant is reacted in an 80° C. oil bath for 2 h to obtain a reaction product, a 1 mol / L sodium bicarbonate aqueous solution is added to the reaction product for washing, followed by washing with a 0.1 mol / L sodium hydroxide aqueous solution, and finally washing with deionized water, and after standing, the active diluent organic solution is obtained by layering; the active diluent organic solution is subjected to reduced pressure distillation to obtain an active diluent.

[0059] Preparation of silicone insulating varnish

[0060] 200 g of a polymer modifier and 500 g of fluorine-nitrogen modified polysiloxane were mixed and melted to obtain modified polysiloxane, 80 g of hydrophobic mesoporous silica and 100 g of an active diluent were added to the modified polysiloxane and stirred for 30 minutes, and then the organic silicone insulating varnish was obtained after cooling.

[0061] Example 3

[0062] Preparation of polymer modifiers

[0063] 224 g of isophorone diisocyanate (CAS No. 4098-71-9), 1.5 g of p-methoxyphenol, 0.5 g of dibutyltin dilaurate and 500 g of ethyl acetate were dispersed in a four-necked flask, 75 g of diethanolamine was added dropwise to the four-necked flask within 30 min, and the four-necked flask was stirred at 200 r / min in a 50° C. water bath for 2 h to obtain a polyurethane prepolymer; 46.15 g of polycaprolactone triol (CAS No.: 3 9280-09-6), the addition was completed within 30 minutes, the four-necked flask was stirred at a speed of 200r / min for 2 hours in a 60°C water bath to obtain a modified polyurethane; the modified polyurethane was heated to 80°C, 23.08g of 2-ethyl methacrylate (CAS No.: 97-63-2) was added dropwise within 1 hour, the reaction was stirred at a speed of 200r / min for 3 hours in a 80°C water bath to obtain a product solution, the product solution was subjected to reduced pressure distillation to remove the solvent, and a polymer modifier was obtained.

[0064] Preparation of hydrophobic mesoporous silica

[0065] 160g of tetraethyl orthosilicate and 90g of heptadecafluorodecyltrimethoxysilane are mixed and dispersed in 200mL of anhydrous ethanol to obtain a silicon-based dispersion liquid, 10mL of 1mol / L ammonia water is added to the silicon-based dispersion liquid to obtain a silicon-based reaction liquid, and the crude product is reacted under stirring in a water bath to obtain the crude product, the crude product is filtered, washed with deionized water, and the washed crude product is calcined and ground to obtain the product; 50g of potassium aluminum sulfate dodecahydrate and 120g of the product are dispersed in 500mL of deionized water to obtain a suspension, the suspension is stirred for reaction, filtered, washed with deionized water to obtain a modified product, the modified product is calcined and ground, and passed through a 100-mesh sieve to obtain hydrophobic mesoporous silica.

[0066] Preparation of fluorine-nitrogen modified polysiloxane

[0067] Polymethylhydrogensilazane (CAS No.: 475645-84-2) and fluorine-containing olefins were subjected to reduced pressure distillation under nitrogen protection to remove residual water in the raw materials to obtain anhydrous polymethylhydrogensilazane and anhydrous fluorine-containing olefins; under nitrogen protection, 307.69 g of anhydrous polymethylhydrogensilazane and 46.15 g of anhydrous fluorine-containing olefins were mixed to obtain a fluorine-modified silane mixture, 5 g of chloroplatinic acid was added to the fluorine-modified silane mixture, and the mixture was reacted in an oil bath at 70°C. The reaction mixture was stirred for 5 hours to obtain a fluorine-containing silazane; 246.16 g of phenyl polytrimethoxysilane (CAS No.: 73559-47-4) and 1 mL of 1 mol / L hydrochloric acid were added to the fluorine-containing silazane, and the mixture was stirred at a speed of 200 r / min in an oil bath at 80°C for 2 hours, and the fluorine-modified silane mixture after the reaction was rotary evaporated to obtain a polymer modifier; the above-mentioned fluorine-containing olefin is hexafluoro-2-butene (CAS No.: 407-60-3).

[0068] Preparation of active diluent

[0069] 100 g of methacryloyl chloride (CAS No.: 920-46-7), 100 g of anhydrous benzyl alcohol (CAS No.: 100-51-6) and 0.5 g of an inhibitor are mixed to obtain a reactant, and the reactant is reacted in an 80° C. oil bath for 2 h to obtain a reaction product, a 1 mol / L sodium bicarbonate aqueous solution is added to the reaction product for washing, followed by washing with a 0.1 mol / L sodium hydroxide aqueous solution, and finally washing with deionized water, and after standing, the active diluent organic solution is obtained by layering; the active diluent organic solution is subjected to reduced pressure distillation to obtain an active diluent.

[0070] Preparation of silicone insulating varnish

[0071] 150 g of a polymer modifier and 400 g of fluorine-nitrogen modified polysiloxane were mixed and melted to obtain modified polysiloxane, 70 g of hydrophobic mesoporous silica and 90 g of an active diluent were added to the modified polysiloxane and stirred for 30 minutes, and then the organic silicone insulating varnish was obtained after cooling.

[0072] Example 4

[0073] Example 4 is based on Example 3. The only difference between Example 4 and Example 3 is that in Example 4, the amount of polycaprolactone triol used is 4.92 g, the amount of polyurethane prepolymer used is 245.9 g, and the amount of 2-ethyl methacrylate used is 49.18 g.

[0074] Example 5

[0075] Example 5 is based on Example 3. The only difference between Example 5 and Example 3 is that in Example 5, the amount of polycaprolactone triol used is 42.85 g, the amount of polyurethane prepolymer used is 214.3 g, and the amount of 2-ethyl methacrylate used is 42.85 g.

[0076] Example 6

[0077] Example 6 is based on Example 3. The only difference between Example 6 and Example 3 is that in Example 6, the amount of fluorine-containing olefin used is 16.22 g, the amount of polymethylhydrogensilazane used is 324.32 g, and the amount of phenyl polytrimethylsiloxane used is 259.46 g.

[0078] Example 7

[0079] Example 7 is based on Example 3. The only difference between Example 7 and Example 3 is that in Example 7, the amount of fluorine-containing olefin used is 85.71 g, the amount of polymethylhydrogensilazane used is 285.71 g, and the amount of phenyl polytrimethylsiloxane used is 228.58 g.

[0080] Example 8

[0081] Example 8 is based on Example 3. The only difference between Example 8 and Example 3 is that in Example 8, the polycaprolactone triol in the step of preparing the polymer modifier is replaced by propylene glycol.

[0082] Example 9

[0083] Example 9 is based on Example 3. The only difference between Example 9 and Example 3 is that in Example 9, 2-ethyl methacrylate in the step of preparing the polymer modifier is replaced by acrylate.

[0084] Example 10

[0085] Example 10 is based on Example 3. The only difference between Example 10 and Example 3 is that in Example 10, the fluorine-containing olefin in the step of preparing fluorine-nitrogen-modified polysiloxane is replaced by butene.

[0086] Embodiment 11

[0087] Example 11 is based on Example 3. The only difference between Example 11 and Example 3 is that in Example 11, the polymethylhydrogensilazane in the step of preparing fluorine-nitrogen-modified polysiloxane is replaced by methyltriethoxysilane.

[0088] Example 12

[0089] Example 12 is based on Example 3. The only difference between Example 12 and Example 3 is that in Example 12, phenyl polytrimethylsiloxane in the step of preparing fluorine-nitrogen modified polysiloxane is replaced by methyltriethoxysilane.

[0090] Example 13

[0091] Example 13 is based on Example 3. The only difference between Example 13 and Example 3 is that in Example 13, no heptadecafluorodecyltrimethoxysilane is added in the step of preparing the hydrophobic mesoporous silica.

[0092] Embodiment 14

[0093] Example 14 is based on Example 3. The only difference between Example 14 and Example 3 is that in Example 14, potassium aluminum sulfate dodecahydrate is not added for alumina loading in the step of preparing hydrophobic mesoporous silica.

[0094] Comparative Example 1

[0095] Comparative Example 1 is based on Example 3, and the only difference between Comparative Example 1 and Example 3 is that the polymer modifier in Comparative Example 1 is replaced by polyurethane.

[0096] Comparative Example 2

[0097] Comparative Example 2 is based on Example 3, and the only difference between Comparative Example 2 and Example 3 is that in Comparative Example 2, the fluorine-nitrogen-modified polysiloxane is replaced by phenyl polytrimethylsiloxane.

[0098] Comparative Example 3

[0099] Comparative Example 3 is based on Example 3, and the only difference between Comparative Example 3 and Example 3 is that in Comparative Example 3, the hydrophobic mesoporous silica is replaced by nano-silica.

[0100] Comparative Example 4

[0101] Comparative Example 4 is based on Example 3. The only difference between Comparative Example 4 and Example 3 is that in Comparative Example 4, the active diluent is replaced by silicone diluent X-13.

[0102] Performance testing

[0103] The test was carried out according to GB / 15022.2-2007 Resin-based active composites for electrical insulation Part 2: Test methods, where the test conditions were: (1) at 25°C and 50% humidity; (2) at 200°C and 50% humidity; (3) immersed in water at 25°C for 24 hours;

[0104] The volume resistivity of the samples was tested under the above three conditions. Three samples were prepared for each sample for testing. The average value was taken after measurement and the results are recorded in Table 1.

[0105] Table 1 Insulation performance and weather resistance test results of silicone insulating varnish

[0106]

[0107] It can be seen from Table 1 that the volume resistivity under the environmental conditions of Examples 1-3 is greater than 2.1×1015 Ω·cm, volume resistivity at 200℃ is greater than 4.3×10 14 Ω·cm, after immersion in water at 25℃ for 24h, the volume resistivity is greater than 1.2×10 10 Ω·cm, it can be seen that the organic silicon insulating paint prepared in the present application has good insulating properties and weather resistance.

[0108] As shown in Table 1, the difference between Examples 4 and 5 and Example 3 is that the mass ratio of polycaprolactone triol, polyurethane prepolymer and 2-ethyl methacrylate in Example 4 is 0.02:1:0.2, and the mass ratio of polycaprolactone triol, polyurethane prepolymer and 2-ethyl methacrylate in Example 5 is 0.2:1:0.2. The volume resistivity under the environmental conditions in Examples 4 and 5 is less than 1.9×10 15 Ω·cm, volume resistivity at 200℃ is less than 4.1×10 14 Ω·cm, volume resistivity is less than 1.1×10 after immersion in water at 25℃ for 24h 10 Ω·cm, the volume resistivity under the environmental conditions in Example 3 is 2.4×10 15 Ω·cm, volume resistivity at 200℃ is 4.6×10 14 Ω·cm, volume resistivity after immersion in water at 25℃ for 24h is 1.5×10 10 Ω·cm, compared with Example 3, the insulation performance and weather resistance of Examples 4 and 5 are both reduced; this is because the mass ratio of polycaprolactone triol, polyurethane prepolymer and 2-ethyl methacrylate is not within the specified range, too much or too little polycaprolactone triol will affect the hydrophobicity and reaction performance of the polymer modifier, and destroying the distribution ratio of each component in the polymer modifier will reduce the stability and compatibility of the system, thereby reducing the insulation performance and weather resistance.

[0109] As shown in Table 1, the only difference between Examples 6 and 7 and Example 3 is that the mass ratio of fluorinated olefin, polymethylhydrogen silazane and phenyl polytrimethylsiloxane in Example 6 is 0.05:1:0.8, and the mass ratio of fluorinated olefin, polymethylhydrogen silazane and phenyl polytrimethylsiloxane in Example 7 is 0.3:1:0.8. The volume resistivity under the environmental conditions in Examples 6 and 7 is less than 2.0×10 15 Ω·cm, volume resistivity at 200℃ is less than 4.2×10 14 Ω·cm, volume resistivity is less than 1.1×10 after immersion in water at 25℃ for 24h 10Ω·cm, compared with Example 3, the insulation performance and weather resistance of Examples 6 and 7 are reduced; this is because the mass ratio of fluorine-containing olefin, polymethylhydrogensilazane and phenylpolytrimethylsiloxane is not within the specified range, too much or too little fluorine-containing olefin will affect the stability and reaction performance of fluorine-nitrogen modified polysiloxane, the system compatibility of fluorine-nitrogen modified polysiloxane is reduced, and thus the insulation performance and weather resistance are reduced.

[0110] As shown in Table 1, the only difference between Examples 8 and 9 and Example 3 is that the polycaprolactone triol in the step of preparing the polymer modifier in Example 8 is replaced by propylene glycol, and the 2-ethyl methacrylate in the step of preparing the polymer modifier in Example 9 is replaced by acrylate. The volume resistivity under the environmental conditions in Examples 8 and 9 is less than 1.9×10 15 Ω·cm, volume resistivity at 200℃ is less than 3.8×10 14 Ω·cm, volume resistivity is less than 0.9×10 after immersion in water at 25℃ for 24h 10 Ω·cm, compared with Example 3, the insulation performance and weather resistance of Examples 8 and 9 are both reduced; this is because the replacement of polycaprolactone triol with propylene glycol or 2-ethyl methacrylate with acrylate, the replacement of the polymer modifier component will reduce the reaction performance and hydrophobicity, the stability of the system is reduced, and thus the insulation performance and weather resistance are reduced.

[0111] As shown in Table 1, the only difference between Examples 10, 11, and 12 and Example 3 is that the fluorine-containing olefin in the step of preparing fluorine-nitrogen-modified polysiloxane in Example 10 is replaced by butene, the polymethylhydrogensilazane in the step of preparing fluorine-nitrogen-modified polysiloxane in Example 11 is replaced by methyltriethoxysilane, and the phenyl polytrimethylsiloxane in the step of preparing fluorine-nitrogen-modified polysiloxane in Example 12 is replaced by methyltriethoxysilane. The volume resistivity under the environmental conditions in Examples 10, 11, and 12 is less than 1.6×10 15 Ω·cm, volume resistivity at 200℃ is less than 3.5×10 14 Ω·cm, volume resistivity is less than 0.6×10 after immersion in water at 25℃ for 24h 10 Ω·cm, compared with Example 3, the insulation performance and weather resistance of Examples 10, 11, and 12 are reduced; this is because the components of the fluorine-nitrogen modified polysiloxane are replaced. If the introduction of fluorine atoms is lacking, the surface energy of the polymer increases, and the stability decreases. In the absence of the composite modification treatment of siloxane or phenylsilane, the crosslinking degree between the fluorine-nitrogen modified polysiloxane molecules is reduced, and the overall stability decreases, thereby reducing the insulation performance and weather resistance.

[0112] As shown in Table 1, the only difference between Examples 13 and 14 and Example 3 is that: in the step of preparing hydrophobic mesoporous silica in Example 13, no heptadecafluorodecyltrimethoxysilane is added; in the step of preparing hydrophobic mesoporous silica in Example 14, no potassium aluminum sulfate dodecahydrate is added for alumina loading; and the volume resistivity under the environmental conditions in Examples 13 and 14 is less than 1.6×10 15 Ω·cm, volume resistivity at 200℃ is less than 3.1×10 14 Ω·cm, volume resistivity is less than 0.3×10 after immersion in water at 25℃ for 24h 10 Ω·cm, compared with Example 3, the insulation performance and weather resistance of Examples 13 and 14 are both reduced; this is because the surface energy of the hydrophobic mesoporous silica is increased due to the lack of the introduction of heptadecafluorodecyltrimethoxysilane, and the hydrophobic performance and stability are reduced; alumina is not loaded on the surface of the mesoporous silica, and the hydrophobic mesoporous silica lacks the synergistic effect of mesoporous silica and alumina, and the hydrophobic performance and stability are reduced, thereby reducing the insulation performance and weather resistance.

[0113] As shown in Table 1, the difference between Comparative Example 1 and Example 3 is that the polymer modifier in Comparative Example 1 is replaced by polyurethane, and the volume resistivity under the environmental conditions in Comparative Example 1 is 1.1×10 15 Ω·cm, volume resistivity at 200℃ is 2.7×10 14 Ω·cm, volume resistivity after immersion in water at 25℃ for 24h is 0.09×10 10 Ω·cm, compared with Example 3, the insulation performance and weather resistance of Comparative Example 1 are significantly reduced; this is because the polymer modifier is replaced by polyurethane, the polyurethane lacks the composite modification of acrylate and hydrophobic polyol, the reactivity and compatibility of the polymer modifier molecules are reduced, and the overall stability of the silicone insulating paint is reduced, so that the insulation performance and weather resistance are significantly reduced.

[0114] As can be seen from Table 1, the difference between Comparative Example 2 and Example 3 is that the fluorine-nitrogen modified polysiloxane is replaced by phenyl polytrimethylsiloxane in Comparative Example 2, and the volume resistivity under the ambient conditions in Comparative Example 2 is 1.0×10 15 Ω·cm, volume resistivity at 200℃ is 2.5×10 14 Ω·cm, volume resistivity after immersion in water at 25℃ for 24h is 0.1×10 10Ω·cm, compared with Example 3, the insulation performance and weather resistance of Comparative Example 2 are significantly reduced; this is because the fluorine-nitrogen modified polysiloxane is replaced by phenyl polytrimethylsiloxane, which lacks the introduction of fluorine atoms and silazane structures, the surface energy of the molecule is increased, the hydrophobicity, antioxidant performance and high temperature resistance are reduced, and the overall stability of the silicone insulating paint is reduced, so that the insulation performance and weather resistance are significantly reduced.

[0115] As shown in Table 1, the difference between Comparative Example 3 and Example 3 is that the hydrophobic mesoporous silica is replaced by nano-silicon dioxide in Comparative Example 3, and the volume resistivity under the ambient conditions in Comparative Example 3 is 1.0×10 15 Ω·cm, volume resistivity at 200℃ is 2.4×10 14 Ω·cm, volume resistivity after immersion in water at 25℃ for 24h is 0.1×10 10 Ω·cm, compared with Example 3, the insulation performance and weather resistance of Comparative Example 3 are significantly reduced; this is because the hydrophobic mesoporous silica is replaced by nano-silica, lacks the introduction of fluorine-containing groups and the loading of alumina, the synergistic effect is weakened, the hydrophobicity and heat resistance are reduced, and the stability of the silicone insulating paint is reduced, thereby significantly reducing the insulation performance and weather resistance.

[0116] As shown in Table 1, the difference between Comparative Example 4 and Example 3 is that the reactive diluent in Comparative Example 4 is replaced by the organosilicon diluent X-13, and the volume resistivity under the ambient conditions in Comparative Example 4 is 0.9×10 15 Ω·cm, volume resistivity at 200℃ is 2.1×10 14 Ω·cm, volume resistivity after immersion in water at 25℃ for 24h is 0.07×10 10 Ω·cm, compared with Example 3, the insulation performance and weather resistance of Comparative Example 4 are significantly reduced; this is because the reactive diluent is replaced by the organosilicon diluent X-13, the reaction performance and dilution capacity of the organosilicon diluent X-13 are reduced, the compatibility between the components of the organosilicon insulating paint is weakened, and the stability is reduced, so that the insulation performance and weather resistance are significantly reduced.

[0117] This specific embodiment is only an explanation of the present application, and it is not a limitation of the present application. Through the above description, relevant staff can make various changes and modifications without deviating from the technical idea of ​​the present application. The technical scope of the present application is not limited to the content in the specification, and its technical scope must be determined according to the scope of the claims.

Claims

1. An organic silicon insulating varnish, characterized in that: The composition includes the following components in parts by weight: Polymer modifier 100-200 parts 60-80 parts of hydrophobic mesoporous silica Fluorine nitrogen modified polysiloxane 300-500 parts 80-100 parts of active diluent; The polymer modifier includes polycaprolactone triol, polyurethane prepolymer and 2-ethyl methacrylate; The polyurethane prepolymer comprises isophorone diisocyanate, p-methoxyphenol and diethanolamine; The mass ratio of the polycaprolactone triol, the polyurethane prepolymer and 2-ethyl methacrylate is (0.05-0.15):1:0.2; The reaction raw materials of the hydrophobic mesoporous silica include ethyl orthosilicate, heptadecafluorodecyltriethoxysilane and potassium aluminum sulfate dodecahydrate; The hydrophobic mesoporous silica is prepared by the following steps: Mixing and dispersing ethyl orthosilicate and heptadecafluorodecyltrimethoxysilane in anhydrous ethanol to obtain a silicon-based dispersion, adding ammonia water to the silicon-based dispersion to obtain a silicon-based reaction liquid, reacting in a water bath with stirring to obtain a crude product, filtering and washing the crude product, calcining and grinding the washed crude product to obtain a product; Dispersing potassium aluminum sulfate dodecahydrate and the product in deionized water to obtain a suspension, stirring the suspension to react, filtering and washing to obtain a modified product, calcining and then grinding the modified product, and sieving to obtain hydrophobic mesoporous silica; The fluorine-nitrogen modified polysiloxane includes fluorine-containing olefins, polymethyl hydrogen silazane and phenyl polytrimethyl siloxane; The mass ratio of the fluorine-containing olefin, polymethylhydrogensilazane and phenyl polytrimethylsiloxane is (0.1-0.2):1:0.8; The reaction raw materials of the active diluent include methacryloyl chloride and anhydrous benzyl alcohol.

2. A method for preparing the organic silicon insulating varnish as claimed in claim 1, characterized in that: The organosilicon insulating varnish is prepared by the following steps: The polymer modifier and the fluorine-nitrogen modified polysiloxane are mixed and melted to obtain the modified polysiloxane, the hydrophobic mesoporous silica and the active diluent are added into the modified polysiloxane and stirred, and the organic silicon insulating varnish is obtained after cooling.

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