CN101921529A - Heat-resistant solvent-free immersion paint and preparation method thereof - Google Patents
Heat-resistant solvent-free immersion paint and preparation method thereof Download PDFInfo
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- CN101921529A CN101921529A CN 201010256437 CN201010256437A CN101921529A CN 101921529 A CN101921529 A CN 101921529A CN 201010256437 CN201010256437 CN 201010256437 CN 201010256437 A CN201010256437 A CN 201010256437A CN 101921529 A CN101921529 A CN 101921529A
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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
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, by the dipping operation, permeate, be filled among the space and pore of coil, wire casing or other insulant, through solidifying winding wire is bonded as insulation integral body, and, have performances such as dielectric, machinery and anti-environment in surface formation successive insulation layer.Miniaturization, lightweight along with electrical equipment have proposed resistant to elevated temperatures requirement to impregnating varnish; In addition, commercially available insulating impregnating varnish mostly has been solvent-borne type, 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) cured product thermotolerance height; (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 gradually with lacquer.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 more and more higher to the insulating material performance demands, just proposed requirements such as high temperature resistant, solvent-free aspect insulating impregnating varnish.
As everyone knows, Resins, epoxy has many good performances: the adhesiveproperties that (1) is good: the bonding strength height, bonding wide, the bonding strength of it and many metals (as iron, steel, copper, aluminium, metal alloy etc.) or non-metallic material (as glass, pottery, timber, plastics etc.) is very high, intensity that have even glue material itself above quilt, therefore can be used in many stress members, is one of main component of structure-type tackiness agent; (2) good processing properties: the diversity 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 Resins, epoxy 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%; Resins, epoxy 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 diallyl isophthalate, epoxy acrylate (V E) is a properties-correcting agent, has synthesized a kind of novel C level single-component solvent-free insulating impregnating varnish; Utilize differential thermal analysis (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 is 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 active 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 package stability, the test of traditional performance such as drying property and electrical strength, and detected dielectric dissipation factor and molecular weight distribution etc., use infrared spectra, methods such as thermal weight loss characterize its molecular structure.But, the crucial starting material of still unexposed its part, and the viscosity of lacquer liquid is bigger than normal, and manufacturability is bad, is still waiting further to improve Journal of Sex Research in actual applications.
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:
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 '-diaminodiphenylmethane, N, N, N ', N '-four glycidyl group-4,4, N, N, N ', N '-four glycidyl group-3,3 '-dimethyl-4,4 '-diaminodiphenylmethane, thermoplastic phenolic Resins, epoxy, 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 is selected from pyromellitic acid anhydride, oxygen supports two phthalic anhydrides, 3,3 ', 4,4 '-tetracarboxylic acid benzophenone dianhydride, biphenyl dianhydride, 2,2-is two, and [4-(3, the 4-di carboxyl phenyloxy) phenyl] the propane dianhydride, 2,2-is two, and [4-(3, the 4-di carboxyl phenyloxy) phenyl] hexafluoropropane dianhydride, phthalic anhydride, maleic anhydride, the Nai Dike acid anhydrides, Dyhard RU 100,4,4 '-diaminodiphenylsulfone(DDS), 4,4 '-diaminodiphenylmethane, 4,4 '-benzidine, 3,3 '-diaminodiphenylsulfone(DDS), 3,3 '-dimethyl-4,4 '-diaminodiphenylmethane, 2, two [4-(3-amino-benzene oxygen) phenyl] propane of 2-, 2, two [4-(3-amino-benzene oxygen) phenyl] HFC-236fa of 2-, 4,4 '-diaminodiphenyl oxide, 3,4 '-diaminodiphenyl oxide, 3,3 '-diaminodiphenyl oxide, 1, two (3-amino-benzene oxygen) benzene of 4-, 2, two (4-amino-benzene oxygen) cyanobenzenes of 6-, 2, two (3-amino-benzene oxygen) cyanobenzenes of 6-, 2, two (4-amino-benzene oxygen) toluene of 6-, 2, two (4-amino-benzene oxygen) phenylfluoroforms of 6-, 2, two (4-amino-benzene oxygen) toluene of 5-, 2, two (4-amino-benzene oxygen) tert-butylbenzenes of 5-, 2,5-di-t-butyl-1, two (4-amino-benzene oxygen) benzene of 4-, 4,4 '-two (4-amino-benzene oxygen) benzophenone, 4,4 '-two (4-amino-benzene oxygen) sulfobenzide, 4,4 '-two (3-amino-benzene oxygen) benzophenone, 4,4 '-two (3-amino-benzene oxygen) sulfobenzide, 1, two (2-trifluoromethyl-4-amino-benzene oxygen) benzene of 4-, 1, two (2-trifluoromethyl-4-amino-benzene oxygen) benzene of 3-, 2, two [4-(2-trifluoromethyl-4-amino-benzene oxygen) phenyl] propane of 2-, 2, two [4-(2-trifluoromethyl-4-amino-benzene oxygen) phenyl] HFC-236fa of 2-, 2, two (2-trifluoromethyl-4-amino-benzene oxygen) toluene of 5-, 2, two (2-trifluoromethyl-4-amino-benzene oxygen) tert.-butylbenzenes of 5-, 2,5-di-t-butyl-1, two (2-trifluoromethyl-4-amino-benzene oxygen) benzene of 4-, 4,4 '-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 of 2-, 2, two [4-(4-amino-benzene oxygen) phenyl] HFC-236fa of 2-, 1, two (3-amino-benzene oxygen) benzene of 3-, 1, two (4-amino-benzene oxygen) benzene of 3-, 1, two (4-amino-benzene oxygen) benzene of 4-, 4,4 '-diamino-4 " the hydroxyl tritane; 3,3 '-diamino-4; 4 '-dihydroxybiphenyl; 3; 3 '-dihydroxyl-4,4 '-benzidine; 2, two (the 3-amino-4-hydroxy phenyl) propane of 2-, 2, two (the 3-amino-4-hydroxy phenyl) HFC-236fa of 2-, 3,3 '-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, 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 reactor, 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 reactor, 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:
Wherein, 10 natural number (being provided by Shanghai Ruitu Electronic Materials Co., Ltd.) is provided n.
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 finished 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 regulate good manufacturability in broad scope;
(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) the adhesive property excellence of this lacquer, room temperature tensile shearing resistance also have 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 and limit the scope of the invention.Should be understood that in addition those skilled in the art can make various changes or modifications 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 reactor, be heated to 60 ℃, add 157.0 gram E-51 bisphenol A type epoxy resins (oxirane value is 0.51) while stirring, stirring reaction is after 0.5 hour, be warming up to 100 ℃, continue stirring reaction 0.5 hour, and obtained 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 '-diaminodiphenylmethane does not have the silicon polyfunctional epoxy resin and adds in the reactor, in 100 ℃ of reactions after 0.5 hour, cooling, adding 54.0 grams 3,3 ', 4,4 '-tetracarboxylic acid benzophenone 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, putting into convection oven is cured, its technology is for to begin to be warming up to 100 ℃ from room temperature, and 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 as shown in Figure 2, its pyrolysated Tonset temperature is 398 ℃, as seen, this impregnating varnish has excellent high thermal resistance.
Other performance of HTV-1 heat-resistant solvent-free immersion paint is as follows: 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 reactor, be heated to 60 ℃, add 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 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 '-diaminodiphenylmethane do not have the silicon polyfunctional epoxy resin and adds in the reactor, in 100 ℃ of reactions after 0.5 hour, cooling, add 30.0 gram 4,4s 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, putting into convection oven is cured, its technology is for to begin to be warming up to 100 ℃ from room temperature, and 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 as follows: 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 (9)
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%.
2. a kind of heat-resistant solvent-free immersion paint according to claim 1 is characterized in that: the general formula of described organosilicon polyfunctional epoxy resin is:
Wherein-E is:
M is not more than 3 natural number; N is not more than 10 natural number.
3. a kind of heat-resistant solvent-free immersion paint according to claim 1 is characterized in that: described no silicon polyfunctional epoxy resin is selected from N, N, N ', N '-four glycidyl group-4,4 '-diaminodiphenylmethane, N, N, N ', N '-four glycidyl group-4,4 '-diaminodiphenylsulfone(DDS), N, N, N ', N '-four glycidyl group-3,3 '-dimethyl-4,4 '-diaminodiphenylmethane, thermoplastic phenolic Resins, epoxy, 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.
4. a kind of heat-resistant solvent-free immersion paint according to claim 1, it is characterized in that: described solidifying agent is selected from pyromellitic acid anhydride, oxygen supports two phthalic anhydrides, 3,3 ', 4,4 '-tetracarboxylic acid benzophenone dianhydride, biphenyl dianhydride, 2,2-is two, and [4-(3, the 4-di carboxyl phenyloxy) phenyl] the propane dianhydride, 2,2-is two, and [4-(3, the 4-di carboxyl phenyloxy) phenyl] hexafluoropropane dianhydride, phthalic anhydride, maleic anhydride, the Nai Dike acid anhydrides, Dyhard RU 100,4,4 '-diaminodiphenylsulfone(DDS), 4,4 '-diaminodiphenylmethane, 4,4 '-benzidine, 3,3 '-diaminodiphenylsulfone(DDS), 3,3 '-dimethyl-4,4 '-diaminodiphenylmethane, 2, two [4-(3-amino-benzene oxygen) phenyl] propane of 2-, 2, two [4-(3-amino-benzene oxygen) phenyl] HFC-236fa of 2-, 4,4 '-diaminodiphenyl oxide, 3,4 '-diaminodiphenyl oxide, 3,3 '-diaminodiphenyl oxide, 1, two (3-amino-benzene oxygen) benzene of 4-, 2, two (4-amino-benzene oxygen) cyanobenzenes of 6-, 2, two (3-amino-benzene oxygen) cyanobenzenes of 6-, 2, two (4-amino-benzene oxygen) toluene of 6-, 2, two (4-amino-benzene oxygen) phenylfluoroforms of 6-, 2, two (4-amino-benzene oxygen) toluene of 5-, 2, two (4-amino-benzene oxygen) tert-butylbenzenes of 5-, 2,5-di-t-butyl-1, two (4-amino-benzene oxygen) benzene of 4-, 4,4 '-two (4-amino-benzene oxygen) benzophenone, 4,4 '-two (4-amino-benzene oxygen) sulfobenzide, 4,4 '-two (3-amino-benzene oxygen) benzophenone, 4,4 '-two (3-amino-benzene oxygen) sulfobenzide, 1, two (2-trifluoromethyl-4-amino-benzene oxygen) benzene of 4-, 1, two (2-trifluoromethyl-4-amino-benzene oxygen) benzene of 3-, 2, two [4-(2-trifluoromethyl-4-amino-benzene oxygen) phenyl] propane of 2-, 2, two [4-(2-trifluoromethyl-4-amino-benzene oxygen) phenyl] HFC-236fa of 2-, 2, two (2-trifluoromethyl-4-amino-benzene oxygen) toluene of 5-, 2, two (2-trifluoromethyl-4-amino-benzene oxygen) tert.-butylbenzenes of 5-, 2,5-di-t-butyl-1, two (2-trifluoromethyl-4-amino-benzene oxygen) benzene of 4-, 4,4 '-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 oxygen)-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 of 2-, 2, two [4-(4-amino-benzene oxygen) phenyl] HFC-236fa of 2-, 1, two (3-amino-benzene oxygen) benzene of 3-, 1, two (4-amino-benzene oxygen) benzene of 3-, 1, two (4-amino-benzene oxygen) benzene of 4-, 4,4 '-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 of 2-, 2, two (the 3-amino-4-hydroxy phenyl) HFC-236fa of 2-, 3,3 '-diamino-4,4 '-dihydroxy diphenylsulphone, 3, one or more in the 5-diaminobenzoic acid.
5. 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, the tetrahydrophthalic acid 2-glycidyl ester, the diglycidyl Hydrogenated Bisphenol A, adjacent benzene two sad diglycidyl ether, the 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 '-epoxy group(ing)-6-methyl cyclohexane methyl esters, titanium dioxide dicyclo amyl ether, in the resorcinol diglycidyl ether one or more.
6. the preparation method of a heat-resistant solvent-free immersion paint comprises:
(1) the organosilicon diamines is put into reactor, 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 reactor, 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.
7. the preparation method of a kind of heat-resistant solvent-free immersion paint according to claim 6 is characterized in that: described organosilicon diamines, and its molecular structural formula is:
Wherein, n is not more than 10 natural number.
8. the preparation method of a kind of heat-resistant solvent-free immersion paint according to claim 6, it is characterized in that: described bisphenol A type epoxy resin is selected from one or both among E-51, the E-44.
9. the preparation method of a kind of heat-resistant solvent-free immersion paint according to claim 6 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.
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| WO2021035905A1 (en) * | 2019-08-27 | 2021-03-04 | 中国船舶重工集团公司第七二五研究所 | Anti-rust weather-resistant functional gradient type bottom-face integrated coating, and method for preparing coating layer |
| CN112251108A (en) * | 2020-10-26 | 2021-01-22 | 衡阳拓创聚合新材料有限公司 | Solvent-free silicon modified elastic epoxy elastic floor coating |
| CN116640492A (en) * | 2023-05-31 | 2023-08-25 | 上海电气集团上海电机厂有限公司 | High-pressure solvent-free impregnating varnish with high storage stability and preparation method and application thereof |
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