CN101899258A - Method for preparing polyester wire coating enamel - Google Patents
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- CN101899258A CN101899258A CN 201010245909 CN201010245909A CN101899258A CN 101899258 A CN101899258 A CN 101899258A CN 201010245909 CN201010245909 CN 201010245909 CN 201010245909 A CN201010245909 A CN 201010245909A CN 101899258 A CN101899258 A CN 101899258A
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Abstract
The invention discloses a method for preparing polyester wire coating enamel, which is characterized by comprising the following steps of: (1) performing degradation and polycondensation reaction on recovered polyester bottle crushed aggregates and polyalcohol according to a mass ratio of 3:(0.5-2) so as to obtain a hydroxy resin in the presence of a catalyst, and preparing the hydroxy resin and a solvent into solution of hydroxy resin according to a mass ratio of 4:(5-7); (2) performing hydroxymethylation and etherification reaction on raw materials of melamine, urea, benzoguanamine, 37 percent formaldehyde, methanol, isopropanol and n-butyl alcohol to obtain a modified etherfied amino resin; and (3) mixing the solution of hydroxy resin, the modified etherfied amino resin and a mixed environment-friendly solvent according to a mass ratio of (1-2.5):(0.1-0.9):(0.3-1.0), adding tetrabutyl titanate which accounts for 0.2 to 1 percent of the total weight of liquid paint, stirring uniformly, filtering and removing the suspending impurities so as to prepare the polyester wire coating enamel at the temperature of between 30 and 80 DEG C. The inflection temperature of a dielectric loss curve of an enameled wire coated by the wire coating enamel prepared by the method is over 160 DEG C, zero pin hole in the process of stretching or bending the enameled wire is realized, and the production cost is 60 to 80 percent of that of the conventional like products.
Description
Technical field
The invention belongs to technical field of polymer materials, be specifically related to a kind of preparation method of polyester wire coating enamel.
Background technology
Polyester is that a kind of structure is the thermoplastic macromolecule material of polyethylene terephthalate.Because of it has the performance of many excellences, good processibility, and be widely used in the manufacturing of products such as man-made fiber, polyester bottles, polyester film, engineering plastics, plastic containers, wrapping material.The demand of the annual all kinds of polyester materials in the whole world reaches more than 8,000 ten thousand tons now according to investigations, and continues the speed cumulative year after year with 10%.Wherein the polyester for bottle demand is about more than 3,000 ten thousand tons, and annual growth is more than 20%.China is one of maximum polyester bottles demand state, and annual requirement is up to more than 400 ten thousand tons at present, and annual growth is more than 25%.A large amount of polyester materials uses and has caused a considerable number of waste and old polyester material, has formed immense pressure to physical environment.Therefore how these waste and old polyester materials are carried out manipulation of regeneration, reduce environmental pollution, turn waste into wealth simultaneously, realize that the recycling of polyester material precious resources has become research topic quite noticeable in recent years in the resource and environment field.
Wire enamel is the coating that a class is used for coating enameled wire specially, and wherein polyester wire coating enamel is the wire enamel kind of early using.The enameled wire that polyester wire coating enamel coated has good sticking power, insulativity and mechanical property, therefore becomes the principal item of wire enamel, accounts for about 50% of wire enamel total amount.It is the main raw material(s) preparation that present polyester wire coating enamel mainly adopts dimethyl terephthalate (DMT), ethylene glycol, glycerine.Adopt a large amount of dimethyl terephthalate (DMT) of this arts demand consumption and ethylene glycol, producing more methyl alcohol simultaneously has toxic byproduct, and these have toxic byproduct to need to reclaim, the material cost height, and production environment is polluted heavy.Need transesterify and two steps of polycondensation on the technology, the condensation temperature height, long reaction time, the production cycle, energy consumption and worker consumed greatly up to more than 24 hours.The polyester type enameled wire temperature classification that adopts this prepared is for only reaching the B level, and hot punching performance and salt water resistance pin hole performance are all not good enough.Therefore, development in recent years the polyester wire enamel kind of various modifications.
Modification kind comparatively successful in the modified poly ester wire enamel is exactly a polyesterimide wire enamel, and its temperature classification can reach F level, H level, even the C level.As US4179423, US4018742, US3975330, WO9203831, JP4202324, JP4183725, JP59174662 etc.The polyesterimide wire enamel of above-mentioned patent report all be with trimellitic acid 1,2-anhydride, three (α-hydroxyethyl) isocyanuric acid ester, 4,4 '-diaminodiphenyl-methane is material of main part preparation.US 5907028 has reported a kind of 180 grades of polyesterimide wire enamels, by three (α-hydroxyethyl) isocyanuric acid ester, 4,4 '-diaminodiphenyl-methane, methyl propanediol, trimellitic acid 1,2-anhydride, dimethyl terephthalate (DMT), dihydroxyphenyl propane be prepared from.The solvent that adopts in this patent is unique, as pimelinketone, propylene carbonate, benzylalcohol etc.Domestic patent about polyester wire coating enamel also has a small amount of report, has reported a kind of preparation method of high heat-stage non-pinhole polyesterimide enamelled wire insulating paint properties-correcting agent as patent 200610030956..Patent 200410010141.8 has been reported a kind of method that adopts Production of Terephthalic Acid polyester, polyesterimide wire enamel.Above-mentioned patent reports that all adopting the recovery polyester is the raw material preparing wire enamel.' polyester resin production polyester, the civilian technology that adopts terylene material, ethylene glycol, glycerine reaction to prepare wire enamel of reporting of polyesterimide wire enamel problem discussion ' one that " insulating material communication " first phase in 1998 delivers.But adopt this processing method terylene material depolymerization incomplete, molecular weight distribution is wide, and the wire enamel levelling property of production is poor.The present invention comes therefrom.
Summary of the invention
It is a kind of that the object of the invention is to provide
In order to solve these problems of the prior art, technical scheme provided by the invention is:
A kind of preparation method of polyester wire coating enamel is characterized in that said method comprising the steps of:
(1) making the raw materials quality ratio is 3: the recovery polyester bottles particle of (0.5～2), polyvalent alcohol obtain hydroxy resin by degraded, polycondensation under the condition that catalyzer exists, be 4 with hydroxy resin and solvent by mass ratio then: (5～7) are mixed with hydroxy resin solution; Described polyvalent alcohol is selected from one or more combination of glycerol, TriMethylolPropane(TMP), tetramethylolmethane, three (α-hydroxyethyl) isocyanuric acid ester, trolamine;
(2) be that raw material obtains the modification etherified amino resins by methylolation and etherification reaction with trimeric cyanamide, urea, benzoguanamine, 37% formaldehyde, methyl alcohol, Virahol, propyl carbinol, the mass ratio of described raw material is a trimeric cyanamide: urea: benzoguanamine: 37% formaldehyde: methyl alcohol: Virahol: propyl carbinol equals 1: (0.1～0.9): (0.2～1.1): (1.2～5.5): (1.0～3.5): (0.5～2.0): (0.5～2.0);
(3) the modification etherified amino resins of the hydroxy resin solution of step (1) acquisition, step (2) acquisition is (1～2.5) with mixed environment-friendly solvent according to mass ratio: (0.1～0.9): mix (0.3～1.0), add the tetrabutyl titanate that accounts for lacquer liquid total mass 0.2% to 1% again, at 30 ℃～80 ℃, stirring makes polyester wire coating enamel after removing by filter suspended impurity.
Preferably, catalyzer is selected from Lithium Sulphate or antimonous oxide in the described method steps (1), and described Lithium Sulphate added in the DeR stage, and described antimonous oxide added in the polycondensation stage; The consumption of described Lithium Sulphate or antimonous oxide is for reacting 0.05%～1.0% of the total mass that feeds intake.
Preferably, solvent comprises cresols, di-esters solvent DBE and dimethylbenzene in the described method steps (1), and the mass ratio of described cresols, DBE and dimethylbenzene is 1: (0.1～0.9): (0.1～0.9).
Preferably, the concrete steps that described method steps (1) obtains hydroxy resin are included in 100 ℃ to 200 ℃ reactions 1～3 hour, keep 200 ℃ of reactions 2～3 hours; Reaction back adds band ethylene glycol agent refluxing xylene and takes ethylene glycol out of, extracts dimethylbenzene 200 ℃ and 0.01～0.09MPa negative pressure then and obtains hydroxy resin.
Preferably, the hydroxy resin that described method steps (1) obtains is controlled at acid number 0.1～2mgKOH/g, hydroxyl value 130～280mg KOH/g, and number-average molecular weight 4500～6500, molecular weight distributing index is 1.9～2.3.
Preferably, the concrete steps that described method steps (2) obtains the modification etherified amino resins comprise 1/5 37% formaldehyde, trimeric cyanamide, urea, benzoguanamine, methyl alcohol, Virahol, propyl carbinol adds in the reaction flask, regulating the pH value with trolamine is 7.0～8.5, be heated to 50～60 ℃ and begin reaction, to be left simultaneously 4/5 37% formaldehyde with 2 quality branches/minute rate of addition join in the reaction flask, dropwise and react 2～3 hours again, regulating the pH value with cis-butenedioic anhydride then is 4.0～5.5, reflux 2～3 hours makes the modification etherified amino resins with the dehydration of toluene heating component distillation at last.
Preferably, the acid number of the modification etherified amino resins that described method steps (2) obtains is less than 5mgKOH/g, 25 ℃ viscosity for be coated with-4 glasss 60～150 seconds.
Preferably, described mixed environment-friendly solvent is that mass ratio is (1～2.0): (1～1.5): (1～3): the mixture of the di-esters solvent DBE of (0.8～1.2), 2-Butoxyethyl acetate, aromatic solvent naphtha, dimethyl formamide.
It is the preparation method of the polyester wire coating enamel of main raw material(s) to reclaim polyester bottles that the present invention obtains a kind of, the enameled wire dielectric loss knee point temperature that wire enamel coated with this method preparation can reach more than 160 ℃, and realize that enameled wire stretches or bending zero pin hole, production cost is 60%～80% of a present like product.
Why the present invention adopts the recovery polyester bottles is that main raw material(s) prepares the reason that polyester wire coating enamel is based on the following aspects: the first, a new way that the polyester bottles waste and scrap is recycled is provided; The second, recovery polyester bottles starting material are cheap and easy to get, can reduce the production cost of polyester wire coating enamel significantly, improve the polyester wire coating enamel competitiveness of product in market; Three, the number-average molecular weight of polyester bottles is about about 20,000, is convenient to adopt relatively-stationary reaction process, and the wire enamel of preparation is evenly distributed with the molecular resin amount, helps the stable of quality product.
Lacquer liquid total amount of the present invention is lacquer liquid total mass.The concrete steps of this method comprise:
(1) preparation of hydroxy resin and solution thereof:
Hydroxy resin is by reclaiming polyester bottles particle, polyvalent alcohol by degraded, polycondensating process generation hydroxy resin.Raw-material mass ratio is in the component: the polyester bottles particle: polyvalent alcohol equals 3: (0.5～2).Polyvalent alcohol is one or more of glycerol, TriMethylolPropane(TMP), tetramethylolmethane, three (α-hydroxyethyl) isocyanuric acid ester, trolamine.Catalyzer is Lithium Sulphate and antimonous oxide.Catalyzer uses by a certain percentage stage by stage, and Lithium Sulphate added in the DeR stage, and antimonous oxide added in the polycondensation stage.Two kinds of catalyst levelss are 0.05%～1.0% of the quality that always feeds intake.The agent of band ethylene glycol is a dimethylbenzene, and consumption is 5%～15% of total charging capacity.The preparation technology of hydroxy resin is: 100 ℃ to 200 ℃ were reacted 1-3 hour, keep 200 ℃ of reactions 2-3 hour, add band ethylene glycol agent dimethylbenzene then, keep and took ethylene glycol in 200 ℃ of backflow 1-3 hours out of, 200 ℃ and 0.01-0.09MPa negative pressure extracted dimethylbenzene 10 minutes to 40 minutes again, promptly made hydroxy resin.The technical indicator of prepared hydroxy resin is: acid number 0.1-2mg KOH/g, and hydroxyl value 130-280mg KOH/g, number-average molecular weight 4500-6500 (gel permeation chromatography, moving phase tetrahydrofuran (THF)), molecular weight distributing index is (1.9～2.3).
The mass ratio of resin and solvent is 4 in the hydroxy resin solution: (5～7).Solvent adopts the mixture of cresols, di-esters solvent DBE and dimethylbenzene, and its mass ratio is: 1: (0.1～0.9): (0.1～0.9).The preparation technology of hydroxy resin solution is: add cresols, kept under 190 ℃ 1-2 hour, di-esters solvent DBE and dimethylbenzene successively stir then, are cooled to below 60 ℃, promptly make hydroxy resin solution.
(2) preparation of modification etherified amino resins:
The modification etherified amino resins is prepared from by methylolation and etherification reaction by trimeric cyanamide, urea, benzoguanamine, 37% formaldehyde, methyl alcohol, Virahol, propyl carbinol.Each raw-material mass ratio is in the component: trimeric cyanamide: urea: benzoguanamine: 37% formaldehyde: methyl alcohol: Virahol: propyl carbinol equals 1: (0.1～0.9): (0.2～1.1): (1.2～5.5): (1.0～3.5): (0.5～2.0): (0.5～2.0).The preparation technology of modification etherified amino resins is: 37% formaldehyde with 1/5, trimeric cyanamide, urea, benzoguanamine, methyl alcohol, Virahol, propyl carbinol adds in the reaction flask, regulating the pH value with trolamine is 7.0～8.5, be heated to 50～60 ℃ and begin reaction, to be left simultaneously 4/5 37% formaldehyde with 2 quality branches/minute rate of addition join in the reaction flask, dropwise and react 2～3 hours again, regulating the pH value with cis-butenedioic anhydride then is 4.0～5.5, reflux 2～3 hours, with the dehydration of toluene heating component distillation, just make the modification etherify melamine resin at last.Technical indicator be acid number less than 5mg KOH/g, viscosity is for being coated with-4 glasss 60～150 seconds (25 ℃).
(3) preparation of polyester wire coating enamel
The preparation technology of wire enamel is: is (1～2.5) with hydroxy resin solution, modification etherified amino resins, mixed environment-friendly solvent according to mass ratio: (0.1～0.9): mix (0.3～1.0), the tetrabutyl titanate that adds lacquer liquid total amount 0.2% to 1% again, at 30 ℃～80 ℃, stirred 2 to 3 hours, and made polyester wire coating enamel after removing by filter suspended impurity.Mixed environment-friendly solvent is the mixture of di-esters solvent DBE, 2-Butoxyethyl acetate, aromatic solvent naphtha, dimethyl formamide, and its mass ratio is (1～2.0): (1～1.5): (1～3): (0.8～1.2).The technical indicator of prepared polyester wire coating enamel is: solid content 25% to 50% (180 ℃ of surveys), viscosity 20 seconds to 80 seconds (25 ℃ of surveys), outward appearance are yellowish to brown xanchromatic transparent viscous liquid.
With respect to scheme of the prior art, advantage of the present invention is:
1. the present invention is in the production technique of hydroxy resin, the main raw material(s) that adopts is for reclaiming the polyester bottles material, can reduce the production cost of polyester wire coating enamel significantly, production cost is 60%～80% of a present like product, and a new way that the polyester bottles waste and scrap is recycled is provided simultaneously.And adopt two kinds of catalyst sulfuric acid lithiums and antimonous oxide, and adding stage by stage and use, Lithium Sulphate added in the DeR stage, and antimonous oxide added in the polycondensation stage.Prepared hydroxy resin even molecular weight distribution helps the stable of wire enamel quality product.
2, technical solution of the present invention adopts a certain proportion of modification etherified amino resins and hydroxy resin preparation, improved the curing performance of resin, widen the enamelling technique nargin of wire enamel, the raising to a certain degree that thermotolerance, insulativity, machinery and the chemical resistance of paint film have been obtained.Adopt the mixed environment-friendly solvent of specified proportion partly to replace phenol, cresols and the xylenol dissolving resin of industry use at present and join lacquer, make the wire enamel that makes have excellent environmental-protecting performance.
Embodiment
Below in conjunction with specific embodiment such scheme is described further.Should be understood that these embodiment are used to the present invention is described and are not limited to limit the scope of the invention.The implementation condition that adopts among the embodiment can be done further adjustment according to the condition of concrete producer, and not marked implementation condition is generally the condition in the normal experiment.
The preparation of embodiment 1 polyester wire coating enamel
(1) preparation of hydroxy resin and solution thereof
Recovery polyester bottles particle 600 mass parts, TriMethylolPropane(TMP) 110 mass parts, catalyst sulfuric acid lithium 2.3 mass parts clean, dry, that pulverize are joined in the reactor successively.Earlier 100 ℃ to 200 ℃ reactions 2.5～3 hours, keep 200 ℃ of reactions 2 hours, the band ethylene glycol agent dimethylbenzene and The catalytic antimony trioxide 2.3 mass parts that add 60 mass parts then, keep 200 ℃ of backflows and took ethylene glycol in 2.5～3 hours out of, 200 ℃ and 0.01～0.09MPa negative pressure extracted dimethylbenzene 20 minutes to 30 minutes again, promptly made hydroxy resin.Add 490 mass parts cresols then, kept under 190 ℃ 1-2 hour, di-esters solvent DBE 250 mass parts and dimethylbenzene 240 mass parts successively stir then, are cooled to below 60 ℃, promptly make hydroxy resin solution.The technical indicator of prepared hydroxy resin is: acid number 0.6～0.8mgKOH/g, and hydroxyl value 260～280mgKOH/g, number-average molecular weight 4985 (gel permeation chromatography, moving phase tetrahydrofuran (THF)), molecular weight distributing index is 2.1.
(2) preparation of modification etherified amino resins
With trimeric cyanamide 100 mass parts, urea 30 mass parts, benzoguanamine 50 mass parts, 37% formaldehyde, 100 mass parts, methyl alcohol 300 mass parts, Virahol 100 mass parts, propyl carbinol 100 mass parts, put in the reaction flask, heated and stirred makes material melting, 37% formaldehyde with 400 mass parts dropwise drips with feed hopper again, regulating the pH value with trolamine is 7.0～8.5, be heated to 50～60 ℃ and begin reaction, treat that formaldehyde dropwises and react 2.5 hours again, regulating the pH value with cis-butenedioic anhydride then is 4.0～5.5, reflux 3 hours, with the dehydration of toluene heating component distillation, just make the melamine resin of modification at last.Technical indicator is that acid number is 3mg KOH/g, and viscosity is for being coated with-4 glasss 100 seconds (25 ℃).
(3) preparation of polyester wire coating enamel
With hydroxy resin solution 200 mass parts, modification etherified amino resins 40 mass parts, di-esters solvent DBE 18 mass parts, 2-Butoxyethyl acetate 16 mass parts, aromatic solvent naphtha 14 mass parts, dimethyl formamide 12 mass parts, tetrabutyl titanate 2.5 mass parts, at 50 ℃, stirred 3 hours, and made polyester wire coating enamel after removing by filter suspended impurity.The technical indicator of prepared polyester wire coating enamel is: solid content 40 ± 1% (180 ℃ of surveys), and viscosity 35 ± 1 seconds (25 ℃ of surveys), outward appearance is the xanchromatic transparent viscous liquid.Coat the enameled wire of line footpath 0.350mm, the enameled wire external diameter is 0.390mm, the enameled wire any surface finish; Stretch 3% or 5% or and the bending condition under the salt solution pin hole be zero hole; It is 200 ℃ that heat is dashed, 30min, and 1D does not split; Softening puncture is not puncture in 260 ℃, 2 minutes; Average voltage breakdown is 8000 volts under the room temperature; Dielectric loss point of inflexion on a curve temperature is 160 ℃.
The preparation of embodiment 2 polyester wire coating enamels
(1) preparation of hydroxy resin and solution thereof
Recovery polyester bottles particle 600 mass parts, three (α-hydroxyethyl) isocyanuric acid ester, 200 mass parts, catalyst sulfuric acid lithium 3.3 mass parts clean, dry, that pulverize are joined in the reactor successively.Earlier 100 ℃ to 200 ℃ reactions 2.5～3 hours, keep 200 ℃ of reactions 2 hours, the band ethylene glycol agent dimethylbenzene and The catalytic antimony trioxide 3.5 mass parts that add 75 mass parts then, keep 200 ℃ of backflows and took ethylene glycol in 2.5～3 hours out of, 200 ℃ and 0.01～0.09MPa negative pressure extracted dimethylbenzene 20 minutes to 30 minutes again, promptly made hydroxy resin.Add 585 mass parts cresols then, kept under 190 ℃ 1-2 hour, di-esters solvent DBE290 mass parts and dimethylbenzene 294 mass parts successively stir then, are cooled to below 60 ℃, promptly make hydroxy resin solution.The technical indicator of prepared hydroxy resin is: acid number 0.4～0.6mg KOH/g, and hydroxyl value 210～240mgKOH/g, number-average molecular weight 5955 (gel permeation chromatography, moving phase tetrahydrofuran (THF)), molecular weight distributing index is 2.2.
(2) preparation of modification etherified amino resins
With trimeric cyanamide 100 mass parts, urea 40 mass parts, benzoguanamine 40 mass parts, 37% formaldehyde, 100 mass parts, methyl alcohol 300 mass parts, Virahol 100 mass parts, propyl carbinol 100 mass parts, put in the reaction flask, heated and stirred makes material melting, 37% formaldehyde with 400 mass parts dropwise drips with feed hopper again, regulating the pH value with trolamine is 7.0～8.5, be heated to 50～60 ℃ and begin reaction, treat that formaldehyde dropwises and react 2.5 hours again, regulating the pH value with cis-butenedioic anhydride then is 4.0～5.5, reflux 3 hours, with the dehydration of toluene heating component distillation, just make the melamine resin of modification at last.Technical indicator is that acid number is 4mg KOH/g, and viscosity is for being coated with-4 glasss 90 seconds (25 ℃).
(4) preparation of polyester wire coating enamel
With hydroxy resin solution 200 mass parts, modification etherified amino resins 40 mass parts, di-esters solvent DBE 45 mass parts, 2-Butoxyethyl acetate 40 mass parts, aromatic solvent naphtha 35 mass parts, dimethyl formamide 30 mass parts, tetrabutyl titanate 3.5 mass parts, at 50 ℃, stirred 3 hours, and made polyester wire coating enamel after removing by filter suspended impurity.The technical indicator of prepared polyester wire coating enamel is: solid content 30 ± 1% (180 ℃ of surveys), and viscosity 23 ± 1 seconds (25 ℃ of surveys), outward appearance is the xanchromatic transparent viscous liquid.Coat the enameled wire of line footpath 0.1mm, the enameled wire external diameter is 0.122mm, the enameled wire any surface finish; Stretch 3% or 5% or and the bending condition under the salt solution pin hole be zero hole; It is 200 ℃ that heat is dashed, 30min, and 1D does not split; Softening puncture is not puncture in 290 ℃, 2 minutes; Average voltage breakdown is 5000 volts under the room temperature; Dielectric loss point of inflexion on a curve temperature is 180 ℃.
Above-mentioned example only is explanation technical conceive of the present invention and characteristics, and its purpose is to allow the people who is familiar with this technology can understand content of the present invention and enforcement according to this, can not limit protection scope of the present invention with this.All equivalent transformations that spirit is done according to the present invention or modification all should be encompassed within protection scope of the present invention.
Claims (8)
1. the preparation method of a polyester wire coating enamel is characterized in that said method comprising the steps of:
(1) making the raw materials quality ratio is 3: the recovery polyester bottles particle of (0.5～2), polyvalent alcohol obtain hydroxy resin by degraded, polycondensation under the condition that catalyzer exists, be 4 with hydroxy resin and solvent by mass ratio then: (5～7) are mixed with hydroxy resin solution; Described polyvalent alcohol is selected from one or more combination of glycerol, TriMethylolPropane(TMP), tetramethylolmethane, three (α-hydroxyethyl) isocyanuric acid ester, trolamine;
(2) be that raw material obtains the modification etherified amino resins by methylolation and etherification reaction with trimeric cyanamide, urea, benzoguanamine, 37% formaldehyde, methyl alcohol, Virahol, propyl carbinol, the mass ratio of described raw material is a trimeric cyanamide: urea: benzoguanamine: 37% formaldehyde: methyl alcohol: Virahol: propyl carbinol equals 1: (0.1～0.9): (0.2～1.1): (1.2～5.5): (1.0～3.5): (0.5～2.0): (0.5～2.0);
(3) the modification etherified amino resins of the hydroxy resin solution of step (1) acquisition, step (2) acquisition is (1～2.5) with mixed environment-friendly solvent according to mass ratio: (0.1～0.9): mix (0.3～1.0), add the tetrabutyl titanate that accounts for lacquer liquid total mass 0.2% to 1% again, at 30 ℃～80 ℃, stirring makes polyester wire coating enamel after removing by filter suspended impurity.
2. method according to claim 1 is characterized in that catalyzer is selected from Lithium Sulphate or antimonous oxide in the described method steps (1), and described Lithium Sulphate added in the DeR stage, and described antimonous oxide added in the polycondensation stage; The consumption of described Lithium Sulphate or antimonous oxide is for reacting 0.05%～1.0% of the total mass that feeds intake.
3. method according to claim 1 is characterized in that solvent comprises cresols, di-esters solvent DBE and dimethylbenzene in the described method steps (1), and the mass ratio of described cresols, DBE and dimethylbenzene is 1: (0.1～0.9): (0.1～0.9).
4. method according to claim 1 is characterized in that the concrete steps of described method steps (1) acquisition hydroxy resin are included in 100 ℃ to 200 ℃ reactions 1～3 hour, keeps 200 ℃ of reactions 2～3 hours; Reaction back adds band ethylene glycol agent refluxing xylene and takes ethylene glycol out of, extracts dimethylbenzene 200 ℃ and 0.01～0.09MPa negative pressure then and obtains hydroxy resin.
5. method according to claim 1 is characterized in that the hydroxy resin that described method steps (1) obtains is controlled at acid number 0.1～2mg KOH/g, hydroxyl value 130～280mg KOH/g, and number-average molecular weight 4500～6500, molecular weight distributing index is 1.9～2.3.
6. method according to claim 1, it is characterized in that concrete steps that described method steps (2) obtains the modification etherified amino resins comprise 1/5 37% formaldehyde, trimeric cyanamide, urea, benzoguanamine, methyl alcohol, Virahol, propyl carbinol adds in the reaction flask, regulating the pH value with trolamine is 7.0～8.5, be heated to 50～60 ℃ and begin reaction, to be left simultaneously 4/5 37% formaldehyde with 2 quality branches/minute rate of addition join in the reaction flask, dropwise and react 2～3 hours again, regulating the pH value with cis-butenedioic anhydride then is 4.0～5.5, reflux 2～3 hours makes the modification etherified amino resins with the dehydration of toluene heating component distillation at last.
7. method according to claim 1, the acid number that it is characterized in that the modification etherified amino resins that described method steps (2) obtains be less than 5mg KOH/g, 25 ℃ viscosity for be coated with-4 glasss 60～150 seconds.
8. method according to claim 1 is characterized in that described mixed environment-friendly solvent is that mass ratio is (1～2.0): (1～1.5): (1～3): the mixture of the di-esters solvent DBE of (0.8～1.2), 2-Butoxyethyl acetate, aromatic solvent naphtha, dimethyl formamide.
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| CN103709352A (en) * | 2013-12-12 | 2014-04-09 | 嘉兴市杭星精细化工有限公司 | Synthesis technology of highly-methylated melamine resin |
| CN103740230A (en) * | 2013-11-25 | 2014-04-23 | 铜陵天河特种电磁线有限公司 | Polyester modified wire enamel and preparation method thereof |
| CN103740268A (en) * | 2013-11-25 | 2014-04-23 | 铜陵天河特种电磁线有限公司 | Environment-friendly modified heat-resistant polyester wire enamel and preparation method thereof |
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| CN111793199A (en) * | 2020-08-07 | 2020-10-20 | 常熟理工学院 | Ultraviolet light cured resin using waste polyester plastic bottle as raw material and preparation method thereof |
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| CN103740230A (en) * | 2013-11-25 | 2014-04-23 | 铜陵天河特种电磁线有限公司 | Polyester modified wire enamel and preparation method thereof |
| CN103740268A (en) * | 2013-11-25 | 2014-04-23 | 铜陵天河特种电磁线有限公司 | Environment-friendly modified heat-resistant polyester wire enamel and preparation method thereof |
| CN103694757A (en) * | 2013-12-04 | 2014-04-02 | 铜陵三佳变压器有限责任公司 | Corona-resistant wire enamel for transformer and preparation method of corona-resistant wire enamel |
| CN103694757B (en) * | 2013-12-04 | 2016-04-13 | 铜陵三佳变压器有限责任公司 | A kind of transformer corona-resistant wire enamel and preparation method thereof |
| CN103709352A (en) * | 2013-12-12 | 2014-04-09 | 嘉兴市杭星精细化工有限公司 | Synthesis technology of highly-methylated melamine resin |
| CN103709352B (en) * | 2013-12-12 | 2015-08-12 | 嘉兴市杭星精细化工有限公司 | A kind of synthesis technique of highly methyl etherified melamine resin |
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| CN108822273B (en) * | 2018-05-17 | 2021-04-13 | 浙江新华新材料科技有限责任公司 | Benzoguanamine modified amino resin and preparation method thereof |
| CN111732877A (en) * | 2020-07-17 | 2020-10-02 | 迪马新材料科技（苏州）有限公司 | Modified polyester paint with good adhesive force and preparation method thereof |
| CN111793199A (en) * | 2020-08-07 | 2020-10-20 | 常熟理工学院 | Ultraviolet light cured resin using waste polyester plastic bottle as raw material and preparation method thereof |
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