CN101921529B - Heat-resistant solvent-free immersion paint and preparation method thereof - Google Patents

Heat-resistant solvent-free immersion paint and preparation method thereof Download PDF

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CN101921529B
CN101921529B CN 201010256437 CN201010256437A CN101921529B CN 101921529 B CN101921529 B CN 101921529B CN 201010256437 CN201010256437 CN 201010256437 CN 201010256437 A CN201010256437 A CN 201010256437A CN 101921529 B CN101921529 B CN 101921529B
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amino
benzene oxygen
benzene
epoxy resin
heat
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CN101921529A (en
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虞鑫海
陈梅芳
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Donghua University
Shanghai Ruitu Electronic Material Co Ltd
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Donghua University
Shanghai Ruitu Electronic Material Co Ltd
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Abstract

The invention relates to a heat-resistant solvent-free immersion paint which comprises the following components in percentage by weight: 10%-15% of organosilicon polyfunctional epoxy resin, 15%-35% of silicon-free polyfunctional epoxy resin, 5%-10% of curing agent and 45%-65% of reactive diluent. The preparation method thereof comprises the following steps: adding the organosilicon polyfunctional epoxy resin, the reactive diluent and the silicon-free polyfunctional epoxy resin into a kettle, reacting for 0.5h at the temperature of 100 DEG C, cooling, adding the curing agent, and evenly stirring at room temperature, thus obtaining sticky liquid, i.e. the heat-resistant solvent-free immersion paint. The preparation process is simple, the cost is low, and the industrialized production can be easily realized; the room-temperature longitudinal shear strength of the heat-resistant solvent-free immersion paint is high; and the heat-resistant solvent-free immersion paint has excellent heat resistance, strong hydrophobic property and wide application prospects in the fields of high-power traction electric machines, high-power generators, drilling motors, mining motors and the like.

Description

Heat-resistant solvent-free immersion paint and preparation method thereof
Technical field
The invention belongs to the preparation field of organic polymer and insulating material, particularly relate to a kind of heat-resistant solvent-free immersion paint and preparation method thereof.
Background technology
Insulating impregnating varnish is a kind of liquid resin system; Through the dipping operation, permeate, be filled among the space and pore of coil, wire casing or other insulant, whole through solidifying for insulation with the winding wire bonding; And form the successive insulation layer in the surface, have performances such as dielectric, machinery and anti-environment.Miniaturized, lightweight along with electrical equipment have proposed resistant to elevated temperatures requirement to impregnating varnish; In addition, mostly commercially available insulating impregnating varnish is that solvent-borne type is arranged, and most solvents all have certain murder by poisoning to human body; Do not meet environmental protection requirement; And the filling effect of lacquer liquid is not good, and the product over-all properties is poor, thereby solvent-free paint becomes one of developing direction of insulating impregnating varnish.
The heat-resistant solvent-free insulating impregnating varnish generally should possess following characteristic: (1) is long storage period, and the usage period is long after mixing; (2) solidification value is low, and reactive behavior is higher; (3) the lacquer fluid viscosity is low; (4) the cured product thermotolerance is high; (5) paint film excellent combination property.Recently, the research of heat-resistant solvent-free insulating impregnating varnish obtains bigger progress, and that main type comprises is silicone based, diphenyl ether, polyimide, polyester-imide class, epoxy resin and unsaturated polyester class.
In recent years, domestic each motor factory dipping is developed to solvent-free paint by non-solvent paint, few solvent paint with lacquer gradually.Because solvent-free paint is than non-solvent paint and lack the paint film that solvent paint more can obtain continuous densification, pore-free, therefore has higher electromechanical properties.Domestic solvent-free paint is existing for a long time in the application of motor dipping, but all occurs such as package stability badly mostly, coats with lacquer crisp firmly problems such as (poor flexibility) after liquid-solidization.
Along with improving constantly of scientific and technological level, fields such as specific type of electric machine, Aeronautics and Astronautics are increasingly high to the insulating material performance demands, aspect insulating impregnating varnish, just proposed requirements such as high temperature resistant, solvent-free.
As everyone knows; Epoxy resin has many good performances: the adhesiveproperties that (1) is good: bonding strength is high; Bonding wide, the bonding strength of it and many metals (like iron, steel, copper, aluminium, metal alloy etc.) or non-metallic material (like glass, pottery, timber, plastics etc.) is very high, have in addition surpass by the intensity of sticking material itself; Therefore can be used in many stress members, is one of staple of structure-type tackiness agent; (2) good processing properties: the variety of the handiness of Formulaion of epoxy resin, complete processing and product properties is the most outstanding in the macromolecular material; (3) satisfactory stability performance: the curing of epoxy resin mainly is the ring opening polyaddition that relies on epoxy group(ing); Therefore do not produce low-molecular material in the solidification process; Its cure shrinkage is one of kind minimum in the thermosetting resin; Be generally 1%-2%, if select suitable filler that shrinking percentage is reduced to about 0.2%; Epoxy resin main chain after the curing is ehter bond, phenyl ring, three-dimensional crosslinking structure, therefore has excellent resistance to acids and bases; (4) good electrical insulation properties, the groove that is widely used in motor is carved insulation, major insulation, wire enamel, impregnating varnish etc.
[research [J] the Northwestern Polytechnical University journal of C level single-component solvent-free insulating impregnating varnish such as Zuo Ruilin; 2003; 21 (2): 144-147] a kind of preparation method of solvent-free insulated impregnating varnish is disclosed; Be primarily characterized in that: (DA IP) is matrix resin with DAIP, and epoxy acrylate (V E) is a properties-correcting agent, synthesized a kind of novel C level single-component solvent-free insulating impregnating varnish; Utilize DTA (DSC), fourier infrared conversion spectrum to analyze (FT IR), thermogravimetic analysis (TGA) methods such as (TG), characterized systematically the performance of lacquer liquid and cured product thereof.But the fragility of paint film is big, adhesive property is not ideal enough, is difficult to apply and the big production of mass-producing.
Li Qiang army etc. [research [J] of H level unsaturated polyester-imide solvent-free immersion paint. insulating material, 2005, (3): 11-13] a kind of preparation method of solvent-free insulated impregnating varnish disclosed; Be primarily characterized in that: on the basis of unsaturated heat-resistant polyester resin; Adopt and introduce the imine group closed-end technology, reduce reactive group, optimize backbone structure; Make a kind of imine modified saturated heat-resistant polyester H level solvent-free immersion paint; It has been carried out traditional performance tests such as package stability, drying property and electrical strength, and detected dielectric dissipation factor and MWD etc., its molecular structure has been characterized with methods such as ir spectra, thermal weight losses.But, still unexposed its part key starting material, and the viscosity of lacquer liquid is bigger than normal, and manufacturability is bad, in practical application, is still waiting further to improve Journal of Sex Research.
Summary of the invention
Technical problem to be solved by this invention provides a kind of heat-resistant solvent-free immersion paint and preparation method thereof, and the preparation technology of this heat-resistant solvent-free immersion paint is simple, cost is low, help realizing suitability for industrialized production; And the room temperature tensile shearing resistance of this heat-resistant solvent-free immersion paint also has excellent thermotolerance up to 20.4MPa, and pyrolysated Tonset temperature is up to 398 ℃, and hydrophobicity is (rate of moisture absorption≤0.03% by force; Water-intake rate≤0.5%), in fields such as superpower traction electric machine, high-power generator, drilling motor, mining motors, has broad application prospects.
A kind of heat-resistant solvent-free immersion paint of the present invention, its component comprises: mass percent is that organosilicon polyfunctional epoxy resin, the mass percent of 10%-15% is that the no silicon polyfunctional epoxy resin of 15%-35%, solidifying agent, the mass percent that mass percent is 5%-10% are the reactive thinner of 45%-65%.
The general formula of described organosilicon polyfunctional epoxy resin is:
Figure BDA0000024632340000031
Wherein-E is:
M is not more than 3 natural number; N is not more than 10 natural number.
Described no silicon polyfunctional epoxy resin is selected from N, N, N ', N '-four glycidyl group-4,4 '-MDA, N; N, N ', N '-four glycidyl group-4,4, N, N; N ', N '-four glycidyl group-3,3 '-dimethyl--4,4 '-MDA, thermoplastic phenolic epoxy resin, N, N; N ', N ', O-five glycidyls-4,4 '-diamino--4 " hydroxyl tritane, N; N, O-triglycidyl group-4-amino-phenol, 4,5-epoxy cyclohexane-1, one or more in the 2-dioctyl phthalate 2-glycidyl ester.
Described solidifying agent be selected from pyromellitic acid anhydride, oxygen support two phthalic anhydrides, 3,3 ', 4,4 '-tetracarboxylic acid UVNUL MS-40 dianhydride, biphenyl dianhydride, 2,2-is two, and [4-(3; The 4-di carboxyl phenyloxy) phenyl] propane dianhydride, 2, two [4-(3, the 4-di carboxyl phenyloxy) phenyl] hexafluoropropane dianhydrides of 2-, phthalic anhydride, maleic anhydride, Nai Dike acid anhydrides, Dyhard RU 100,4,4,4,4 '-MDA, 4; 4 '-benzidine, 3,3 '-diaminodiphenylsulfone(DDS), 3,3 '-dimethyl--4,4 '-MDA, 2; Two [4-(3-amino-benzene oxygen) phenyl] propane, 2 of 2-, two [4-(3-amino-benzene oxygen) phenyl] HFC-236fas of 2-, 4,3,4 '-diaminodiphenyl oxide, 3; 3 '-diaminodiphenyl oxide, 1, two (3-amino-benzene oxygen) benzene, 2 of 4-, two (4-amino-benzene oxygen) cyanobenzenes, 2 of 6-, two (3-amino-benzene oxygen) cyanobenzenes, 2 of 6-; Two (4-amino-benzene oxygen) toluene, 2 of 6-, two (4-amino-benzene oxygen) phenylfluoroforms, 2 of 6-, two (4-amino-benzene oxygen) toluene, 2 of 5-, two (4-amino-benzene oxygen) tert-butylbenzenes, 2 of 5-; 5-di-t-butyl-1, two (4-amino-benzene oxygen) benzene, 4,4 of 4-'-two (4-amino-benzene oxygen) UVNUL MS-40,4,4 '-two (4-amino-benzene oxygen) sulfobenzide, 4; 4 '-two (3-amino-benzene oxygen) UVNUL MS-40,4,4 '-two (3-amino-benzene oxygen) sulfobenzide, 1, two (2-trifluoromethyl-4-amino-benzene oxygen) benzene, 1 of 4-, two (2-trifluoromethyl-4-amino-benzene oxygen) benzene, 2 of 3-; Two [4-(2-trifluoromethyl-4-amino-benzene oxygen) phenyl] propane, 2 of 2-, two [4-(2-trifluoromethyl-4-amino-benzene oxygen) phenyl] HFC-236fas, 2 of 2-, two (2-trifluoromethyl-4-amino-benzene oxygen) toluene, 2 of 5-, two (2-trifluoromethyl-4-amino-benzene oxygen) tert.-butylbenzenes, 2 of 5-; 5-di-t-butyl-1, two (2-trifluoromethyl-4-amino-benzene oxygen) benzene, 4,4 of 4-'-two (2-trifluoromethyl-4-amino-benzene oxygen) sulfobenzide, 4,4 '-two (2-trifluoromethyls-4-amino-benzene oxygen)-3; 3 ' 5,5 '-tetramethyl diphenyl sulfone, 4,4 '-two (2-trifluoromethyl-4-amino-benzene oxygen) biphenyl, 4,4 '-two (2-trifluoromethyls-4-amino-benzene oxygen)-3; 3 ' 5,5 '-tetramethyl biphenyl, 4,4 '-two (2-trifluoromethyl-4-amino-benzene oxygen) phenyl ether, 4,4 '-two (4-amino-benzene oxygen) phenyl ether, 4; 4 '-two (3-amino-benzene oxygen) phenyl ether, 4,4 '-two (3-amino-benzene oxygen) diphenyl sulfide, 4,4 '-two (4-amino-benzene oxygen) diphenyl sulfide, 4,4 '-two (4-amino-benzene oxygens)-3; 3 ' 5,5 '-tetramethyl biphenyl, 4,4 '-two (3-amino-benzene oxygens)-3,3 ' 5; 5 '-tetramethyl biphenyl, 2, two [4-(4-amino-benzene oxygen) phenyl] propane, 2 of 2-, two [4-(4-amino-benzene oxygen) phenyl] HFC-236fas, 1 of 2-, two (3-amino-benzene oxygen) benzene, 1 of 3-; Two (4-amino-benzene oxygen) benzene, 1 of 3-, two (4-amino-benzene oxygen) benzene, 4,4 of 4-'-diamino--4 " hydroxyl tritane, 3,3 '-diamino--4; 4 '-dihydroxybiphenyl, 3,3 '-dihydroxyl-4,4 '-benzidine, 2, two (the 3-amino-4-hydroxy phenyl) propane, 2 of 2-; two (the 3-amino-4-hydroxy phenyl) HFC-236fas, 3,3 of 2-'-diamino--4,4 '-dihydroxy diphenylsulphone, 3, one or more in the 5-diaminobenzoic acid; This solidifying agent is used with the ultrafine powder state, and its median size is not more than 0.5 micron.
Described reactive thinner is selected from o-phthalic acid diglycidyl ester, tetrahydrophthalic acid 2-glycidyl ester, diglycidyl Hydrogenated Bisphenol A 99, adjacent benzene two sad diglycidyl ether, titanium dioxide vinyl cyclohexane, bicyclopentadiene dioxide, 3; 4-epoxy group(ing) heptanaphthenic acid-3 '; 4 '-epoxy group(ing) hexamethylene methyl esters, 3; 4-epoxy group(ing)-6-methyl cyclohexane formic acid-3 ', 4 '-in the epoxy group(ing)-6-methyl cyclohexane methyl esters, titanium dioxide dicyclo amyl ether, resorcinol diglycidyl ether one or more.
The preparation method of a kind of heat-resistant solvent-free immersion paint of the present invention comprises:
(1) the organosilicon diamines is put into reaction kettle, be heated to 60 ℃, add bisphenol A type epoxy resin while stirring; Behind the stirring reaction 0.5 hour; Be warming up to 100 ℃, continued stirring reaction 0.5 hour, obtain the heavy-gravity organosilicon polyfunctional epoxy resin; Wherein, the ratio of the epoxy group(ing) mole number in the amino mole number in the organosilicon diamines and the bisphenol A type epoxy resin is 1: 4-5;
(2) with above-mentioned organosilicon polyfunctional epoxy resin, reactive thinner with do not have the silicon polyfunctional epoxy resin and add in the reaction kettle, in 100 ℃ of reactions after 0.5 hour, cooling; Add solidifying agent, under the room temperature, stir; Obtain viscous liquid, be heat-resistant solvent-free immersion paint.
Described organosilicon diamines, its molecular structural formula is:
Figure BDA0000024632340000041
Wherein, n is not more than 10 natural number (being provided by Shanghai Ruitu Electronic Materials Co., Ltd.).
Described bisphenol A type epoxy resin is selected from one or both (resin processing plant provides by the Wuxi) among E-51 (oxirane value is 0.51), the E-44 (oxirane value is 0.44).
Described solidifying agent is used with the ultrafine powder state, and its median size is not more than 0.5 micron.
Beneficial effect
(1) preparation technology of the present invention is simple, cost is low, easy to operate, the reaction raw materials convenient sources can be accomplished the preparation process in general-purpose equipment, help realizing suitability for industrialized production;
(2) the viscosity controllability of this heat-resistant solvent-free immersion paint is good, can in broad scope, regulate good manufacturability;
(3) this heat-resistant solvent-free immersion paint environmental friendliness, paint film are fine and close continuously, and pin hole is few, excellent combination properties such as electrical insulation properties and mechanical property;
(4) this lacquer package stability is good, and the room temperature storage phase reached more than 6 months;
(5) adhesive property of this lacquer is excellent, and the room temperature tensile shearing resistance also has excellent thermotolerance up to 20.4MPa, and pyrolysated Tonset temperature is up to 398 ℃, and hydrophobicity is (rate of moisture absorption≤0.03% by force; Water-intake rate≤0.5%), in fields such as superpower traction electric machine, high-power generator, drilling motor, mining motors, has broad application prospects.
Description of drawings
Fig. 1 is the molecular structural formula of organosilicon diamines;
Fig. 2 is the thermal weight loss collection of illustrative plates of the heat-resistant solvent-free immersion paint cured article of embodiment 1.
Embodiment
Below in conjunction with specific embodiment, further set forth the present invention.Should be understood that these embodiment only to be used to the present invention is described and be not used in the restriction scope of the present invention.Should be understood that in addition those skilled in the art can do various changes or modification to the present invention after the content of having read the present invention's instruction, these equivalent form of values fall within the application's appended claims institute restricted portion equally.
Embodiment 1
With 47.0 gram (0.1 mole) α, ω-two aminopropyl poly methylsiloxane organosilicon diamines is put into reaction kettle, is heated to 60 ℃, adds 157.0 gram E-51 bisphenol A type epoxy resins (oxirane value is 0.51) while stirring; Behind the stirring reaction 0.5 hour, be warming up to 100 ℃, continued stirring reaction 0.5 hour, obtain the heavy-gravity organosilicon polyfunctional epoxy resin; Add 1000.0 gram o-phthalic acid diglycidyl esters and 326.0 grams 3,4-epoxy group(ing) heptanaphthenic acid-3 ', 4 '-epoxy group(ing) hexamethylene methyl esters reactive thinner, 306.0 gram N; N, N ', N '-four glycidyl group-4,4 '-MDA do not have the silicon polyfunctional epoxy resin and add in the reaction kettle;, cool off after 0.5 hour in 100 ℃ of reactions, adding 54.0 grams 3,3 '; 4,4 '-tetracarboxylic acid UVNUL MS-40 dianhydride and 150.0 gram dicy-curing agent powder, under the room temperature, stir; Obtain viscous liquid, be heat-resistant solvent-free immersion paint, note is made HTV-1.
Get an amount of HTV-1 heat-resistant solvent-free immersion paint, and evenly be coated in the test piece of standard stainless steel, superimposed; Clamp, put into convection oven and be cured, its technology is for to begin to be warming up to 100 ℃ from room temperature; Insulation reaction 2 hours continues to be warming up to 120 ℃, insulation reaction 1 hour; Continue to be warming up to 160 ℃, insulation reaction 2 hours naturally cools to room temperature.Recording the room temperature tensile shearing resistance is 20.4MPa.
Get an amount of HTV-1 heat-resistant solvent-free immersion paint, on polytetrafluoroethylene film, push away film, place air blast heat drying case to be heating and curing; Make the square solids sample that is of a size of 5mm * 5mm * 1mm, curing process is: begin to be warming up to 100 ℃ from room temperature, insulation reaction 2 hours; Continue to be warming up to 120 ℃, insulation reaction 1 hour continues to be warming up to 160 ℃; Insulation reaction 2 hours naturally cools to room temperature.
The square sample of above-mentioned exsiccant is weighed after (W1), be soaked in the deionized water (25 ℃), after 72 hours, take out, dry the surface with filter paper, weigh (W2), calculating water-intake rate is 0.32%.
The square sample of above-mentioned exsiccant is weighed after (G1), be positioned over climatic chamber (85 ℃, RH85%) in, after 72 hours, take out, dry the surface with filter paper, weigh (G2), calculating rate of moisture absorption is 0.02%.
In addition, the thermal weight loss collection of illustrative plates of HTV-1 heat-resistant solvent-free immersion paint cured article is as shown in Figure 2, and its pyrolysated Tonset temperature is 398 ℃, and is visible, and this impregnating varnish has excellent high thermal resistance.
Other performance of HTV-1 heat-resistant solvent-free immersion paint is following: viscosity 65s (4# flow cup, 25 ℃); Gelation time 48min (110 ℃); Bonding strength 67.5N (spiral tube method); Cured article volume specific resistance 3.5 * 10 11Ω cm; The room temperature storage phase is no less than 6 months (viscosimetry).
Embodiment 2
With 47.0 gram (0.1 mole) α, ω-two aminopropyl poly methylsiloxane organosilicon diamines is put into reaction kettle, is heated to 60 ℃, adds 227.0 gram E-44 bisphenol A type epoxy resins (oxirane value is 0.44) while stirring; Behind the stirring reaction 0.5 hour, be warming up to 100 ℃, continued stirring reaction 0.5 hour, obtain the heavy-gravity organosilicon polyfunctional epoxy resin; Add 322.6 gram m-phthalic acid diglycidylethers, 200.0 gram diglycidyl Hydrogenated Bisphenol A 99s and 300.0 grams 3,4-epoxy group(ing) heptanaphthenic acid-3 ', 4 '-epoxy group(ing) hexamethylene methyl esters reactive thinner, 339.8 gram N; N, O-triglycidyl group-4-amino-phenol and 300.0 gram N, N, N '; N '-four glycidyl group-3,3 '-dimethyl--4,4 '-MDA does not have the silicon polyfunctional epoxy resin and adds in the reaction kettle; After 0.5 hour, cooling adds 30.0 grams 4 in 100 ℃ of reactions; 4 '-diaminodiphenylsulfone(DDS) and 61.4 gram dicy-curing agent powder, under the room temperature, stir; Obtain viscous liquid, be heat-resistant solvent-free immersion paint, note is made HTV-2.
Get an amount of HTV-2 heat-resistant solvent-free immersion paint, and evenly be coated in the test piece of standard stainless steel, superimposed; Clamp, put into convection oven and be cured, its technology is for to begin to be warming up to 100 ℃ from room temperature; Insulation reaction 2 hours continues to be warming up to 120 ℃, insulation reaction 1 hour; Continue to be warming up to 160 ℃, insulation reaction 2 hours naturally cools to room temperature.Recording the room temperature tensile shearing resistance is 19.7MPa.
Get an amount of HTV-2 heat-resistant solvent-free immersion paint, on polytetrafluoroethylene film, push away film, place air blast heat drying case to be heating and curing; Make the square solids sample that is of a size of 5mm * 5mm * 1mm, curing process is: begin to be warming up to 100 ℃ from room temperature, insulation reaction 2 hours; Continue to be warming up to 120 ℃, insulation reaction 1 hour continues to be warming up to 160 ℃; Insulation reaction 2 hours naturally cools to room temperature.
The square sample of above-mentioned exsiccant is weighed after (W1), be soaked in the deionized water (25 ℃), after 72 hours, take out, dry the surface with filter paper, weigh (W2), calculating water-intake rate is 0.45%.
The square sample of above-mentioned exsiccant is weighed after (G1), be positioned over climatic chamber (85 ℃, RH85%) in, after 72 hours, take out, dry the surface with filter paper, weigh (G2), calculating rate of moisture absorption is 0.03%.
Other performance of HTV-2 heat-resistant solvent-free immersion paint is following: viscosity 54s (4# flow cup, 25 ℃); Gelation time 39min (110 ℃); Bonding strength 66.2N (spiral tube method); Cured article pyrolysated Tonset temperature is 375 ℃; Cured article volume specific resistance 1.3 * 10 11Ω cm; The room temperature storage phase is no less than 6 months (viscosimetry).

Claims (7)

1. heat-resistant solvent-free immersion paint, its component comprises: mass percent is that organosilicon polyfunctional epoxy resin, the mass percent of 10%-15% is that the no silicon polyfunctional epoxy resin of 15%-35%, solidifying agent, the mass percent that mass percent is 5%-10% are the reactive thinner of 45%-65%;
Wherein, the general formula of organosilicon polyfunctional epoxy resin is:
Figure FDA0000144011270000011
Wherein-E is:
Figure FDA0000144011270000012
M is not more than 3 natural number; N is not more than 10 natural number;
No silicon polyfunctional epoxy resin is selected from N, N, N ', N '-four glycidyl group-4,4 '-MDA, N; N, N ', N '-four glycidyl group-4,4, N, N; N ', N '-four glycidyl group-3,3 '-dimethyl--4,4 '-MDA, thermoplastic phenolic epoxy resin, N, N; N ', N ', O-five glycidyls-4,4 '-diamino--4 " hydroxyl tritane, N; N, O-triglycidyl group-4-amino-phenol, 4,5-epoxy cyclohexane-1, one or more in the 2-dioctyl phthalate 2-glycidyl ester.
2. a kind of heat-resistant solvent-free immersion paint according to claim 1 is characterized in that: described solidifying agent be selected from pyromellitic acid anhydride, oxygen support two phthalic anhydrides, 3,3 ', 4,4 '-tetracarboxylic acid UVNUL MS-40 dianhydride, biphenyl dianhydride, 2; Two [4-(3, the 4-di carboxyl phenyloxy) phenyl] the propane dianhydrides, 2 of 2-, two [4-(3, the 4-di carboxyl phenyloxy) phenyl] hexafluoropropane dianhydrides of 2-, phthalic anhydride, maleic anhydride, Nai Dike acid anhydrides, Dyhard RU 100,4,4,4; 4 '-MDA, 4,4 '-benzidine, 3,3 '-diaminodiphenylsulfone(DDS), 3,3 '-dimethyl--4,4 '-MDA, 2; Two [4-(3-amino-benzene oxygen) phenyl] propane, 2 of 2-, two [4-(3-amino-benzene oxygen) phenyl] HFC-236fas of 2-, 4,3,4 '-diaminodiphenyl oxide, 3; 3 '-diaminodiphenyl oxide, 1, two (3-amino-benzene oxygen) benzene, 2 of 4-, two (4-amino-benzene oxygen) cyanobenzenes, 2 of 6-, two (3-amino-benzene oxygen) cyanobenzenes, 2 of 6-; Two (4-amino-benzene oxygen) toluene, 2 of 6-, two (4-amino-benzene oxygen) phenylfluoroforms, 2 of 6-, two (4-amino-benzene oxygen) toluene, 2 of 5-, two (4-amino-benzene oxygen) tert-butylbenzenes, 2 of 5-; 5-di-t-butyl-1, two (4-amino-benzene oxygen) benzene, 4,4 of 4-'-two (4-amino-benzene oxygen) UVNUL MS-40,4,4 '-two (4-amino-benzene oxygen) sulfobenzide, 4; 4 '-two (3-amino-benzene oxygen) UVNUL MS-40,4,4 '-two (3-amino-benzene oxygen) sulfobenzide, 1, two (2-trifluoromethyl-4-amino-benzene oxygen) benzene, 1 of 4-, two (2-trifluoromethyl-4-amino-benzene oxygen) benzene, 2 of 3-; Two [4-(2-trifluoromethyl-4-amino-benzene oxygen) phenyl] propane, 2 of 2-, two [4-(2-trifluoromethyl-4-amino-benzene oxygen) phenyl] HFC-236fas, 2 of 2-, two (2-trifluoromethyl-4-amino-benzene oxygen) toluene, 2 of 5-, two (2-trifluoromethyl-4-amino-benzene oxygen) tert.-butylbenzenes, 2 of 5-; 5-di-t-butyl-1, two (2-trifluoromethyl-4-amino-benzene oxygen) benzene, 4,4 of 4-'-two (2-trifluoromethyl-4-amino-benzene oxygen) sulfobenzide, 4,4 '-two (2-trifluoromethyls-4-amino-benzene oxygen)-3; 3 ' 5,5 '-tetramethyl diphenyl sulfone, 4,4 '-two (2-trifluoromethyl-4-amino-benzene oxygen) biphenyl, 4,4 '-two (2-trifluoromethyls-4-amino-benzene oxygen)-3; 3 ' 5,5 '-tetramethyl biphenyl, 4,4 '-two (2-trifluoromethyl-4-amino-benzene oxygen) phenyl ether, 4,4 '-two (4-amino-benzene oxygen) phenyl ether, 4; 4 '-two (3-amino-benzene oxygen) phenyl ether, 4,4 '-two (3-amino-benzene oxygen) diphenyl sulfide, 4,4 '-two (4-amino-benzene oxygen) diphenyl sulfide, 4,4 '-two (4-amino-benzene oxygens)-3; 3 ' 5,5 '-tetramethyl biphenyl, 4,4 '-two (3-amino-benzene oxygens)-3,3 ' 5; 5 '-tetramethyl biphenyl, 2, two [4-(4-amino-benzene oxygen) phenyl] propane, 2 of 2-, two [4-(4-amino-benzene oxygen) phenyl] HFC-236fas, 1 of 2-, two (3-amino-benzene oxygen) benzene, 1 of 3-; Two (4-amino-benzene oxygen) benzene, 1 of 3-, two (4-amino-benzene oxygen) benzene, 4,4 of 4-'-diamino--4 " hydroxyl tritane, 3,3 '-diamino--4; 4 '-dihydroxybiphenyl, 3,3 '-dihydroxyl-4,4 '-benzidine, 2, two (the 3-amino-4-hydroxy phenyl) propane, 2 of 2-; two (the 3-amino-4-hydroxy phenyl) HFC-236fas, 3,3 of 2-'-diamino--4,4 '-dihydroxy diphenylsulphone, 3, one or more in the 5-diaminobenzoic acid.
3. a kind of heat-resistant solvent-free immersion paint according to claim 1; It is characterized in that: described reactive thinner is selected from o-phthalic acid diglycidyl ester, tetrahydrophthalic acid 2-glycidyl ester, diglycidyl Hydrogenated Bisphenol A 99, adjacent benzene two sad diglycidyl ether, titanium dioxide vinyl cyclohexane, bicyclopentadiene dioxide, 3; 4-epoxy group(ing) heptanaphthenic acid-3 '; 4 '-epoxy group(ing) hexamethylene methyl esters, 3; 4-epoxy group(ing)-6-methyl cyclohexane formic acid-3 ', 4 '-in the epoxy group(ing)-6-methyl cyclohexane methyl esters, titanium dioxide dicyclo amyl ether, resorcinol diglycidyl ether one or more.
4. the preparation method of a kind of heat-resistant solvent-free immersion paint according to claim 1 comprises:
(1) the organosilicon diamines is put into reaction kettle, be heated to 60 ℃, add bisphenol A type epoxy resin while stirring; Behind the stirring reaction 0.5 hour; Be warming up to 100 ℃, continued stirring reaction 0.5 hour, obtain the heavy-gravity organosilicon polyfunctional epoxy resin; Wherein, the ratio of the epoxy group(ing) mole number in the amino mole number in the organosilicon diamines and the bisphenol A type epoxy resin is 1: 4-5;
(2) with above-mentioned organosilicon polyfunctional epoxy resin, reactive thinner with do not have the silicon polyfunctional epoxy resin and add in the reaction kettle, in 100 ℃ of reactions after 0.5 hour, cooling; Add solidifying agent, under the room temperature, stir; Obtain viscous liquid, be heat-resistant solvent-free immersion paint.
5. the preparation method of a kind of heat-resistant solvent-free immersion paint according to claim 4 is characterized in that: described organosilicon diamines, and its molecular structural formula is:
Wherein, n is not more than 10 natural number.
6. the preparation method of a kind of heat-resistant solvent-free immersion paint according to claim 4, it is characterized in that: described bisphenol A type epoxy resin is selected from one or both among E-51, the E-44.
7. the preparation method of a kind of heat-resistant solvent-free immersion paint according to claim 4 is characterized in that: described solidifying agent is used with the ultrafine powder state, and its median size is not more than 0.5 micron.
CN 201010256437 2010-08-18 2010-08-18 Heat-resistant solvent-free immersion paint and preparation method thereof Expired - Fee Related CN101921529B (en)

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