CN101255299B - Environment protection heat-proof acrylic resin insulation paint - Google Patents
Environment protection heat-proof acrylic resin insulation paint Download PDFInfo
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- CN101255299B CN101255299B CN2007103025509A CN200710302550A CN101255299B CN 101255299 B CN101255299 B CN 101255299B CN 2007103025509 A CN2007103025509 A CN 2007103025509A CN 200710302550 A CN200710302550 A CN 200710302550A CN 101255299 B CN101255299 B CN 101255299B
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Abstract
The invention discloses an environment-friendly heat-proof acrylic resin insulating coating, comprising nm inorganic modified acrylic acid latex, nm acrylic acid resin, inorganic filler, curing agent, wherein the weight ratio of nm inorganic modified acrylic acid latex, nm acrylic acid resin, inorganic filler and curing agent is 10-40:20-40:20-40:5-15. The coating has no chromate and the adhesiveforce thereof can be 1 lever, and the interface resistance is above 800 omega.mm<SUP>2</SUP>, with excellent waterproof and antirust property. The coating does not come off after annealing at 750 degree with good interface resistance and corrosion resistance.
Description
Technical field
The invention belongs to environment protection heat-proof coating, particularly be a kind of nano modified acrylic resin environmental protection insulation compound that electrical steel coatings uses.
Background technology
Up to the present, the prescription that forms the technology of a layer insulating and coating on electrical sheet has had many, mainly comprises inorganic, organic and half inorganic three major types.Coating the earliest mainly is that chromic salt and phosphoric acid salt form one deck mineral membrane on electrical sheet.Although the excellent heat resistance of mineral membrane, its water tolerance, shock resistance, tack are all very poor.In order to address the above problem, developed the compo that comprises organic and inorganic two main ingredients gradually, obtain half inorganic paint, this class prescription has made full use of good water-fast, the insulation of good welding property of mineral membrane and resistance toheat and organic membrane, shock resistance and adhesion property.For example mentioned being used for applies electrical sheet to form the coating of insulation layer in U.S. Pat 4238534, US4844753, US5624749, the Chinese patent 98125437, all adopts this class half inorganic paint prescription.The large-scale at home and abroad electrical steel of half inorganic paint manufacturing enterprise has obtained to use widely.The subject matter that this type of insulation compound exists is to have adopted harmful organic solvent and chromic salt, and along with the increasingly stringent of environmental practice, the application of such coating is restricted.
For satisfying the environmental requirement of coating, the insulation compound of environment-friendly type becomes the emphasis of domestic and international research and development gradually.Chinese patent 01113541.7,03132101.1 and 200610038817.3 adopts and adds the insulation compound that mineral filler has prepared the chromium-free environment-friendly type in the acrylic resin.Wherein, 01113541.7 acrylic resin that adopts is the particle of diameter 0.1-0.4 μ m, and the particle diameter of mineral filler is 0.1-0.5 μ m; 03132101.1 prepare acrylic resin with 200610038817.3 employing alcoholic solvent systems, but do not stipulate the granularity of resin, the particle diameter of mineral filler is 0.01-0.5 μ m.Adopt the ACRYLIC EMULSION film forming, need to add film coalescence aid and just can obtain dense film, because the less stable of Emulsion acrylic resin, viscosity changes greatly, is difficult to satisfy the requirement of electrical steel dense film technology of preparing.Application present situation according to present electric steel insulating coating, coating needs hot setting, and electrical steel product need pass through high temperature annealing, and the acrylic resin temperature tolerance is relatively poor, and acrylic resin influences the insulating property of siliconized plate through being easy to generate the dry linting phenomenon after the decomposition behind the high temperature annealing.
Summary of the invention
Technical problem to be solved by this invention provides a kind of environment protection heat-proof acrylic resin insulation paint that is not easy dry linting.
The technical scheme of technical solution problem of the present invention is: a kind of environment protection heat-proof acrylic resin insulation paint, comprise nano inorganic modified acrylic acid emulsion, nanometer acrylic resin, mineral filler, solidifying agent, the mass ratio of described nano inorganic modified acrylic acid emulsion, nanometer acrylic resin, mineral filler, solidifying agent is 10-40: 20-40: 20-40: 5-15.
Described nano inorganic modified acrylic acid emulsion prepares by following method:
A) comonomer, emulsifying agent, buffer reagent, linking agent, solvent, the pre-emulsification of stirring are not less than 1 hour and form pre-newborn body, the mass ratio of comonomer, emulsifying agent, buffer reagent, linking agent, solvent is: 50～70: 1: 1～2: 0.5～5: 80～100.
B) initiator and nano inorganic properties-correcting agent are added in the entry, form the properties-correcting agent suspension, the mass ratio of initiator, nano inorganic properties-correcting agent, water is 1.5: 1～10: 30.
C) under the situation of stirring at room, get pre-newborn body, the 10-30 weight part properties-correcting agent suspension of 10～30 weight parts, mix, be warming up to 78-85 ℃, with the 0.2-0.3 kilogram/pre-newborn body of hour dropping 70-90 weight part and the mixing solutions of 50-70 weight part properties-correcting agent suspension, after dripping off, with the 0.1-0.3 kilogram/hour speed drip 10-30 weight part properties-correcting agent suspension, be warmed up to 85-95 ℃ with 5-20 ℃/hour speed then, slaking 0.5-1.5 hour, be cooled to 50-60 ℃, the pH value of regulating emulsion with weak base is 7-8, gets final product.
Described nano inorganic properties-correcting agent is silicon sol, titanium colloidal sol, zirconium colloidal sol, nano silicon oxide, nano aluminium oxide, nano zircite, nano-titanium oxide is a kind of or several mixture.
Described initiator is that letex polymerization initiator commonly used gets final product, and what the present invention adopted is ammonium persulphate.
Described comonomer is methyl methacrylate, vinylformic acid, butyl acrylate and vinylbenzene; Emulsifying agent is the compound system of sodium lauryl sulphate and alkylphenol polyoxyethylene; Buffer reagent is a sodium bicarbonate; Linking agent is a N hydroxymethyl acrylamide; Solvent is a water.
Described nanometer acrylic resin can be bought from the market, also can prepare with following method:
In organic solvents such as butanols with methyl methacrylate, vinylformic acid, monomers such as butyl acrylate, hydroxyethyl methylacrylate, vinylbenzene, polymerization is not less than 4 hours under 80-85 ℃ of condition, gets final product.
For improve the nanometer acrylic resin dispersiveness, can also in the nanometer acrylic resin for preparing, add the polyalcohols solvent, disperse to be not less than 1 hour with 500～1500 rev/mins rotating speeds.Described polyvalent alcohol is ethylene glycol, glycerol, sorbyl alcohol and ethylene glycol etc.
Described mineral filler is zinc phosphate, aluminum phosphate, kaolin, titanium dioxide is a kind of or several mixtures, and for guaranteeing the homogeneity of coating, above-mentioned inorganic powder is preferably controlled particle diameter at 0.5～2 micron;
Described solidifying agent is melamine resin, aminoresin or the Resins, epoxy of high methyl-etherified.
In order to improve the use properties of coating, also can in coating, add flow agent, sanitas, thickening material.
Preparation method of the present invention be for will take by weighing various compositions in the coating, mixing and stirring, and then add deionized water, and adjusting viscosity is 15-29 second, sand milling disperses to get final product more than 30 minutes.
The present invention is by the water-borne acrylic resin and the emulsion combination of nano-scale, obtain dense organic film, improve the resistance toheat of film by emulsion parcel nano particle, organic composition decomposes behind the high temperature annealing, the inorganic nanoparticles that discharges can be bonded together inorganic filler particle, has reduced the dry linting phenomenon.
The present invention does not compared with prior art contain chromic salt, sticking power reaches 1 grade, and interlamination resistance is greater than 800 Ω .mm
2, water-fast, rustless property is outstanding, dry linting and still keep good interlamination resistance and solidity to corrosion not after 750 ℃ of annealing.
Description of drawings
Fig. 1 is embodiment 1 a coating pattern under the electron microscope.
Fig. 2 is embodiment 1 a coating polarization curve.
Fig. 3 is embodiment 2 coating patterns under the electron microscope.
In Fig. 2,1 is the acrylic resin coating, and 2 is nanometer acrylic resin coating.
Embodiment:
Below in conjunction with embodiment the present invention is described in detail.
Sticking power of the present invention detects according to the GB2522-88 standard;
Interlamination resistance detects according to the GB2522-88 standard;
Water-fastly, antirust detect according to the GB/3826-1999 standard;
The described material of embodiment " part " all refers to weight part.
Embodiment 1:
1, the preparation of nano inorganic modified acrylic acid emulsion:
A) get the sodium lauryl sulphate of 20 parts of butyl acrylates, 13 parts of methyl methacrylates, 28 parts of vinylbenzene, 2.7 parts, 1 part in vinylformic acid and the compound emulsifying agent of alkylphenol polyoxyethylene, 1 part of sodium bicarbonate, 0.5 part of N hydroxymethyl acrylamide, 80 parts of water, under the condition of room temperature, mix and stirred 1 hour, form pre-newborn body.
B) 1.5 parts of ammonium persulphates and 1 part of silicon sol are added in 30 parts of water, under the condition of room temperature, mix and stirred 1 hour, form the properties-correcting agent suspension.
C) under the situation of stirring at room, 10 parts pre-newborn bodies, 10 parts of properties-correcting agent suspensions are mixed, be warming up to 78-85 ℃, drip 70 parts the pre-newborn body and the mixing solutions of 70 parts of properties-correcting agent suspensions with 0.2 kilogram/hour, after dripping off, drip 10 parts of properties-correcting agent suspensions with 0.1 kilogram/hour speed again, after being added dropwise to complete, be warmed up to 85-95 ℃ with 5 ℃/hour speed then, slaking 0.5 hour, be cooled to 50-60 ℃, the pH value of regulating emulsion with ammoniacal liquor is 7-8, gets final product.
2, the preparation of environmental protection coating material
With 3 parts of nano inorganic modified acrylic acid emulsions, 3 parts of commercial nanometer acrylic resins, 3 parts of zinc phosphates, the melamine resin of 1 part of high methyl-etherified adds water and adjusts viscosity to 18 second, and sand milling gets final product.
Embodiment 2:
1, the preparation of nano inorganic modified acrylic acid emulsion:
A) get the sodium lauryl sulphate of 28 parts of butyl acrylates, 15 parts of methyl methacrylates, 24 parts of vinylbenzene, 3 parts, 1 part in vinylformic acid and the compound emulsifying agent of alkylphenol polyoxyethylene, 2 parts of sodium bicarbonates, 2 parts of N hydroxymethyl acrylamides, 90 parts of water, under the condition of room temperature, mix and stirred 1.5 hours, form pre-newborn body.
B) 1.5 parts of ammonium persulphates and 5 parts of nano silicon oxides are added in 30 parts of water, under the condition of room temperature, mix and stirred 1 hour, form the properties-correcting agent suspension.
C) under the situation of stirring at room, 10 parts pre-newborn bodies, 20 parts of properties-correcting agent suspensions are mixed, be warming up to 78-85 ℃, drip 90 parts the pre-newborn body and the mixing solutions of 50 parts of properties-correcting agent suspensions with 0.3 kilogram/hour, after dripping off, drip 20 parts of properties-correcting agent suspensions with 0.2 kilogram/hour speed again, after being added dropwise to complete, be warmed up to 90-95 ℃ with 10 ℃/hour speed then, slaking 1 hour, be cooled to 50-60 ℃, the pH value of regulating emulsion with ammoniacal liquor is 7-8, gets final product.
2, the preparation of environmental protection coating material
With 1 part of nano inorganic modified acrylic acid emulsion, 2 parts of commercial nanometer acrylic resins, 2 parts of aluminum phosphates, 0.5 part of Resins, epoxy adds water and adjusts viscosity to 29 second, and sand milling gets final product.
Embodiment 3:
1, the preparation of nano inorganic modified acrylic acid emulsion:
A) get the sodium lauryl sulphate of 25 parts of butyl acrylates, 13 parts of methyl methacrylates, 22 parts of vinylbenzene, 3 parts, 1 part in vinylformic acid and the compound emulsifying agent of alkylphenol polyoxyethylene, 1.2 parts of sodium bicarbonates, 4 parts of N hydroxymethyl acrylamides, 85 parts of water, under the condition of room temperature, mix and stirred 2 hours, form pre-newborn body.
B) 1.5 parts of ammonium persulphates and 10 parts of zirconium colloidal sols are added in 30 parts of water, under the condition of room temperature, mix and stirred 1 hour, form the properties-correcting agent suspension.
C) under the situation of stirring at room, 10 parts pre-newborn bodies, 30 parts of properties-correcting agent suspensions are mixed, be warming up to 78-85 ℃, drip 90 parts the pre-newborn body and the mixing solutions of 70 parts of properties-correcting agent suspensions with 0.3 kilogram/hour, after dripping off, drip 30 parts of properties-correcting agent suspensions with 0.3 kilogram/hour speed again, after being added dropwise to complete, be warmed up to 90-95 ℃ with 15 ℃/hour speed then, slaking 1.5 hours, be cooled to 50-60 ℃, the pH value of regulating emulsion with ammoniacal liquor is 7-8, gets final product.
2, the preparation of environmental protection coating material
With 1 part of nano inorganic modified acrylic acid emulsion, 4 parts of commercial nanometer acrylic resins, 4 parts of kaolin, the melamine resin of 1.5 parts of high methyl-etherifieds adds water and adjusts viscosity to 25 second, and sand milling gets final product.
Embodiment 4:
1, the preparation of nano inorganic modified acrylic acid emulsion:
A) get the sodium lauryl sulphate of 24 parts of butyl acrylates, 15 parts of methyl methacrylates, 20 parts of vinylbenzene, 2 parts, 1 part in vinylformic acid and the compound emulsifying agent of alkylphenol polyoxyethylene, 1.5 parts of saleratus, 5 parts of N hydroxymethyl acrylamides, 100 parts of water, under the condition of room temperature, mix and stirred 2.5 hours, form pre-newborn body.
B) 1.5 parts of ammonium persulphates and 8 parts of nano silicon oxides, nano aluminium oxide, nano zircite, nano-titanium oxide mixtures are added in 20 parts of water, under the condition of room temperature, mix and stirred 1.5 hours, form the properties-correcting agent suspension, the weight ratio of nano silicon oxide, nano aluminium oxide, nano zircite, nano-titanium oxide is 1: 1: 1 in the mixture: 1.
C) under the situation of stirring at room, 10 parts pre-newborn bodies, 25 parts of properties-correcting agent suspensions are mixed, be warming up to 78-85 ℃, drip 90 parts the pre-newborn body and the mixing solutions of 60 parts of properties-correcting agent suspensions with 0.3 kilogram/hour, after dripping off, drip 25 parts of properties-correcting agent suspensions with 0.3 kilogram/hour speed again, after being added dropwise to complete, be warmed up to 90-95 ℃ with 20 ℃/hour speed then, slaking 1.5 hours, be cooled to 50-60 ℃, the pH value of regulating emulsion with ammoniacal liquor is 7-8, gets final product.
2, the preparation of environmental protection coating material
With 1 part of nano inorganic modified acrylic acid emulsion, 3 parts of commercial nanometer acrylic resins, 4 parts is the mixture of zinc phosphate, aluminum phosphate, kaolin, titanium dioxide, 1 part of aminoresin, add water and adjust viscosity to 25 second, sand milling gets final product, and the weight ratio of zinc phosphate, aluminum phosphate, kaolin, titanium dioxide is 1: 1: 1 in the mixture.
Embodiment 5:
Except that the nanometer acrylic resin was following method preparation, all the other were identical with embodiment 2.
The preparation of nanometer acrylic resin:
With 50 parts of methyl methacrylates, 3 parts in vinylformic acid, 12 parts of butyl acrylates, hydroxyethyl methylacrylate are dissolved in 40 parts of propyl carbinols for 20 parts, and 80～85 ℃ of condition polymerizations 4 hours, obtaining particle diameter was nano level acrylic resin.
Embodiment 6:
Except that in the nanomaterial grade acrylic resin that makes, adding glycerol, to disperse to be not less than 1 hour with 1000 rev/mins rotating speeds, the weight ratio of nano level acrylic resin and glycerol is outside 9: 1, all the other are identical with embodiment 5.
Embodiment 7:
Remove adding flow agent 505 in coating, outside nano anti-corrosive agent, the thickening material Natvosol, all the other are identical with embodiment 6.
Embodiment 8:
Remove in the b operation of the preparation of nano inorganic modified acrylic acid emulsion, do not add outside the nano inorganic properties-correcting agent, all the other are identical with embodiment 1.
The coating that embodiment 1-8 is made is coated in the electrical sheet surface, and 300 ℃ solidified 1.5 minutes, and its performance is as shown in table 1:
| Sticking power | Interlamination resistance Ω .mm 2 | Water-fast, antirust | ||
| Before the annealing | After the | |||
| Embodiment | ||||
| 1 | 1 | ＞800 | ＞600 | 7 |
| |
1 | ＞800 | ＞500 | 8 |
| |
1 | ＞800 | ＞500 | 8 |
| |
1 | ＞800 | ＞500 | 8 |
| Embodiment 5 | 1 | ＞800 | ＞500 | 8 |
| Embodiment 6 | 1 | ＞800 | ＞500 | 8 |
| Embodiment 7 | 1 | ＞800 | ＞500 | 7 |
| Embodiment 8 | 1 | ＞800 | ≈100 | 6 |
It is acrylic resin modified to contain more nano inorganic among the embodiment 1, so the interlamination resistance of annealing back coating is higher.Compare with embodiment 8, all embodiment interlamination resistances after annealing of adding the nano modified acrylic resin significantly improve.
The SEM pattern of embodiment 1 coating as shown in Figure 1, the polarization curve of 750 ℃ of annealing coating after 2 hours as shown in Figure 2, the SEM pattern of embodiment 2 coatings as shown in Figure 3, Fig. 1, Fig. 3 show the coating even compact, have good adhesion property and electric property, solidity to corrosion significantly improves than embodiment 8.
Claims (6)
1. environment protection heat-proof acrylic resin insulation paint, comprise nanometer acrylic resin, mineral filler, solidifying agent, it is characterized in that: also comprise the nano inorganic modified acrylic acid emulsion in the coating, the mass ratio of described nano inorganic modified acrylic acid emulsion, nanometer acrylic resin, mineral filler, solidifying agent is 10-40: 20-40: 20-40: 5-15;
Described solidifying agent is aminoresin or Resins, epoxy;
Described nano inorganic modified acrylic acid emulsion prepares by following method:
A) comonomer, emulsifying agent, buffer reagent, linking agent, solvent are stirred pre-emulsification and be not less than 1 hour pre-newborn body of formation, the mass ratio of comonomer, emulsifying agent, buffer reagent, linking agent, solvent is: 50 ~ 70: 1: 1 ~ 2: 0.5 ~ 5: 80 ~ 100;
B) initiator and nano inorganic properties-correcting agent are added in the entry, form the properties-correcting agent suspension, the mass ratio of initiator, nano inorganic properties-correcting agent, water is 1.5: 1 ~ 10: 30;
C) under the situation of stirring at room, get pre-newborn body, the 10-30 weight part properties-correcting agent suspension of 10 ~ 30 weight parts, mix, be warming up to 78-85 ℃, slowly drip the pre-newborn body of 70-90 weight part and the mixing solutions of 50-70 weight part properties-correcting agent suspension, after dripping off, slowly drip 10-30 weight part properties-correcting agent suspension, be warmed up to 85-95 ℃ with 5-20 ℃/hour speed then, slaking 0.5-1.5 hour, be cooled to 50-60 ℃, the pH value of regulating emulsion with weak base is 7-8, gets final product;
Described nano inorganic properties-correcting agent is silicon sol, titanium colloidal sol, zirconium colloidal sol, nano silicon oxide, nano aluminium oxide, nano zircite, nano-titanium oxide is a kind of or several mixture;
Described comonomer is methyl methacrylate, vinylformic acid, butyl acrylate and vinylbenzene;
Described linking agent is a N hydroxymethyl acrylamide.
2. a kind of environment protection heat-proof acrylic resin insulation paint according to claim 1 is characterized in that: described nanometer acrylic resin is following method preparation:
With methyl methacrylate, vinylformic acid, the polymerization under 80-85 ℃ of condition of butyl acrylate, hydroxyethyl methylacrylate, vinylbenzene is not less than 4 hours, gets final product in organic solvent.
3. a kind of environment protection heat-proof acrylic resin insulation paint according to claim 2 is characterized in that: add the polyalcohols solvent in the nanometer acrylic resin for preparing, disperse to be not less than 1 hour with 500 ~ 1500 rev/mins rotating speeds.
4. a kind of environment protection heat-proof acrylic resin insulation paint according to claim 3 is characterized in that: described polyvalent alcohol is ethylene glycol, glycerol, sorbyl alcohol and ethylene glycol.
5. a kind of environment protection heat-proof acrylic resin insulation paint according to claim 1 is characterized in that: described mineral filler is zinc phosphate, aluminum phosphate, kaolin, titanium dioxide is a kind of or several mixtures.
6. a kind of environment protection heat-proof acrylic resin insulation paint according to claim 1 is characterized in that: add flow agent, sanitas, thickening material in coating.
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| CN2007103025509A CN101255299B (en) | 2007-12-28 | 2007-12-28 | Environment protection heat-proof acrylic resin insulation paint |
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| CP02 | Change in the address of a patent holder |
Address after: 243003 8 Jiuhua Road, Yushan, Ma'anshan, Anhui Co-patentee after: University of Science and Technology Beijing Patentee after: Ma'anshan Iron and Steel Co., Ltd. Co-patentee after: Ma'anshan Jinke Special Coating Co., Ltd. Address before: 243003 intellectual property department, technology center, No. 8 Hunan West Road, Yushan, Ma'anshan, Anhui Co-patentee before: University of Science and Technology Beijing Patentee before: Ma'anshan Iron and Steel Co., Ltd. Co-patentee before: Ma'anshan Jinke Special Coating Co., Ltd. |
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| CP02 | Change in the address of a patent holder |