CN100467557C - Production of cryogenic direct-welding polyurethane envelope without pinhole - Google Patents
Production of cryogenic direct-welding polyurethane envelope without pinhole Download PDFInfo
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- CN100467557C CN100467557C CNB2007100197607A CN200710019760A CN100467557C CN 100467557 C CN100467557 C CN 100467557C CN B2007100197607 A CNB2007100197607 A CN B2007100197607A CN 200710019760 A CN200710019760 A CN 200710019760A CN 100467557 C CN100467557 C CN 100467557C
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Abstract
A low-temperature straight-welding polyurethane wire enamel without pin hole is carried out by preparing hydroxide radical component, preparing enclosed component and formulating wire enamel. It can be used for extended or bended zero pin hole below 340degree.
Description
Technical field
But the present invention relates to a kind of preparation method of polyurethane wire enamel of cryogenic direct-welding free of pinholes.
Background technology
Wire enamel is that a class is specifically designed to the electric insulation coating that coats enameled wire.Polyurethane wire enamel and the polyurethane enamelled wire that is coated thereof have following characteristics because of its distinctive chemical structure:
The first, directly weldering property is good, polyurethane enamelled wire when welding, needn't remove paint film layer in advance, and scolding tin temperature low (about 375 ℃), speed fast (about 3 seconds);
The second, dyeability is good, and polyurethane wire enamel can be miscible with multiple dyestuff, makes various colored enameled wires, is applicable to the occasion of many solder joints;
Three, high frequency performance is good, and the dielectric loss angle tangent of paint film under high frequency is smaller, can be used for preparing the corona-resistant wire enamel that variable-frequency motor is used through modification;
But the 4th low-temperature and high-speed is coated with line, and storing temperature is lower about 100 ℃ than polyester enameled wire, is coated with linear velocity simultaneously and also wants fast 2～4 times, has improved production efficiency widely.
Exist advantage, especially its cryogenic direct-welding of above-mentioned uniqueness based on polyurethane wire enamel, make polyurethane enamelled wire be widely used in light current electric product fields such as the more colour TV of solder joint, instrument, the accurate coil of computer, household electrical appliance.The polyurethane wire enamel market demand increases sharply in recent years, and annual growth is about 10% according to incompletely statistics, and more and more replaces polyester wire enamel in a lot of application scenarios.Polyurethane wire enamel shared share in the wire enamel total amount increases year by year, and is present about 40% by rising to 10% of the beginning of the nineties in last century, therefore very good according to the market outlook of ammonia ester wire enamel.
Increasing of the increase of polyurethane wire enamel market demand and use occasion, especially the frequent update of all kinds of electric products, require polyurethane wire enamel not only more reliable and more stable on performance, more need to develop the service requirements that extraordinary polyurethane wire enamels such as cryogenic direct-welding, high heat-resisting, anti-high frequency satisfy emerging special occasions simultaneously.The straight weldering performance of polyurethane enamelled wire provides great convenience for the welding of enameled wire, yet the general scolding tin temperature of existing homemade polyurethane wire enamel is about 370 ℃, the lower occasion of components and parts thermotolerance around base material and welding causes the distortion of base material and coil rack, components and parts are impaired and produce waste product possibly on every side.Both at home and abroad seldom about the research report of the cryogenic direct-welding aspect of performance of polyurethane wire enamel.USP3988251, USP4110297, USP4115342 have reported a kind of polyurethane wire enamel of low temperature scolding tin, adopt the masked isocyanate component of 25-27% polyurethane polyester resin (including the hydroxyl of 4-10%) and 23-25%, adding that solvent and Preparation of Catalyst form.The enameled wire scolding tin temperature that is coated is 285 ℃ to 315 ℃, and softening puncture temperature is 230 ℃.But domestic CN1597815A has reported the well H level polyurethane enamelled wire lacquer of cryogenic direct-welding of a kind of saline infusion needle permeability, mainly adopts three (2-hydroxyethyl) isocyanuric acid ester, TriMethylolPropane(TMP) and 2-methyl propanediol modification preparation.The enameled wire scolding tin temperature that is coated reaches 375 ℃ (1.5-2.5 seconds), and salt solution 3% pin hole that stretches is 0-2 holes, and the softening temperature that punctures is greater than 240 ℃.This patent stresses to have reported the heat-resisting level of polyurethane wire enamel, and other improves, and does not have big improvement for the reduction of scolding tin temperature and the 3% pin hole aspect of performance that stretches.The at present domestic patent report that does not also have about low temperature scolding tin (being lower than 370 ℃) polyurethane wire enamel.
Summary of the invention
The present invention seeks to: but a kind of preparation method of polyurethane wire enamel of cryogenic direct-welding free of pinholes is provided, can not be higher than directly weldering under 340 ℃ the condition with the enameled wire that wire enamel coated of this method preparation, and realize that enameled wire stretches or bending zero pin hole.
Technical scheme of the present invention is: but a kind of preparation method of polyurethane wire enamel of cryogenic direct-welding free of pinholes comprises the following steps:
(1) hydroxy component preparation: hydroxy component carries out melt co-polycondensation earlier by monoprotic acid, aromatic dibasic acid, Tetra hydro Phthalic anhydride, hexanodioic acid, polyvalent alcohol, dibasic alcohol and generates polyester polyol resin, and then No. 1 mixed solvent that adds some amount mixes and forms.The mass ratio of each reactant is in the component: monoprotic acid: aromatic dibasic acid: Tetra hydro Phthalic anhydride: adipic acid: polyvalent alcohol: dibasic alcohol: No. 1 mixed solvent equals 1:(0.1～0.9): (0.5～1.9): (0.2～0.9): (0.8～2.5): (0.1～0.9): (5～8).Monoprotic acid be stearic acid, Palmiticacid, myristic acid, lauric one or more.Aromatic dibasic acid is one or more of terephthalic acid, m-phthalic acid.Polyvalent alcohol is one or more of glycerine, TriMethylolPropane(TMP), tetramethylolmethane.Dibasic alcohol is one or more of neopentyl glycol, 2-methyl propanediol, ethylene glycol, glycol ether.No. 1 mixed solvent is the mixture of cresols, aromatic solvent naphtha, dimethylbenzene, and its mass ratio is (2.5～4.0): (0.5～1.5): (0.5～1.5).Catalyzer is organic titanium-antimony mixture, and its consumption is 0.2%～1.5% of a reactant quality.The preparation technology of hydroxy component is: 100 ℃ to 180 ℃ were reacted 1-3 hours, 180 ℃ to 200 ℃ were reacted 1-3 hours, keep 200 ℃ of reactions 1-3 hours, 200 ℃ and 0.01-0.09MPa negative pressure extracted dimethylbenzene 10 minutes to 40 minutes, add cresols and between 180 ℃ to 200 ℃, reacted 1-2 hours, add mixed solvent and promptly make hydroxy component.The technical indicator of prepared polyester polyol resin is: acid number 1-3mgKOH/g, and hydroxyl value 130-300mgKOH/g, number-average molecular weight 3000-6000 (gel permeation chromatography, solvents tetrahydrofurane), molecular weight distributing index is (1.9～2.3).
(2) closure component preparation: closure is formed by aromatic diisocyanate, trivalent alcohol, phenols encapsulant and No. 2 mixed solvent reactions.The mass ratio of each reactant is in the component: 4,4 '-diphenylmethanediisocyanate: trivalent alcohol: the phenols encapsulant: No. 2 mixed solvent equals (2～6): (0.2～0.6): (2～5): (3～5).Trivalent alcohol is one or more of glycerine, TriMethylolPropane(TMP), three (2-hydroxyethyl isocyanuric acid ester).The phenols encapsulant is one or more in xylenol, the cresols.No. 2 mixed solvents are the mixture of cresols, dimethyl formamide, dimethylbenzene, and its mass ratio is (0.5～1.0): (3～5): (3～5).Closure preparation technology is: earlier 4,4 '-diphenylmethanediisocyanate, trivalent alcohol, No. 2 mixed solvents were reacted 2～4 hours at 60 ℃-80 ℃, add the phenols encapsulant then, at 125 ℃～140 ℃, reacted 4～6 hours, be cooled to 50 ℃ and promptly make closure.Prepared closure technical indicator is the appearance transparent viscous liquid, and residual isocyano-content is less than 0.1% to 0.5%, and the quality guaranteed period is more than 1 year.
(3) lacquer liquid preparation: the preparation technology of polyurethane wire enamel is: is (1～1.9) with hydroxy component, closure component and No. 3 mixed solvents according to mass ratio: (1～1.9): mix (1～3), the zinc naphthenate that adds lacquer liquid total amount 0.2% to 1% again, at 30 ℃～80 ℃, stirred 2 to 3 hours, and made polyurethane wire enamel after removing by filter suspended impurity.No. 3 mixed solvents are the mixture of cresols, phenol, aromatic solvent naphtha, dimethyl formamide, and its mass ratio is (1～1.5): (1～1.5): (2～3): (0.8～1.2).The technical indicator of prepared polyurethane wire enamel is: solid content 25% to 40% (180 ℃ of surveys), and viscosity 17 seconds to 60 seconds (25 ℃ of surveys), outward appearance is light to the xanchromatic transparent viscous liquid.
Advantage of the present invention is:
1. in the hydroxy component formulating of recipe, introduce a certain amount of fatty monoprotic acid, comprise stearic acid, Palmiticacid, myristic acid, lauric one or more, flexible side group can connected on the polyester polyol molecular chain, reduce the straight weldering temperature of paint film, improve paint film adhesion, improve the stretching and the bending saline infusion needle permeability energy of paint film.
2, specific hydroxy component prescription and the production technique of design can obtain acid number 1-3mgKOH/g, hydroxyl value 130-300mgKOH/g, the polyester polyol resin of number-average molecular weight 3000-6000.Wherein an amount of phthalic acid anhydride component replaces aromatic dibasic acid can play reduction straight weldering temperature and improves and soften the dual function that punctures temperature; An amount of trivalent alcohol can make paint film obtain satisfied crosslinking degree, improves the mechanical property and the withstand voltage properties of paint film.
3, in the production technique of hydroxy component, adopting organic titanium-antimony mixture is catalyzer, can make that the generated time of polyester polyol shortens to 5-8 hours in the hydroxy component, is about half of existing industrial production cycle, has reduced energy consumption and worker consumption.
4, adding a certain amount of cresols at hydroxy component production technique latter stage reacted 1-2 hours between 180 ℃ to 200 ℃, purpose is to obtain the polyester polyol that molecular weight distributing index is stabilized in (1.9～2.3) scope, can improve the quality stability of wire enamel and coat enameled wire nargin scope.
5, in closure preparation, design specific prescription and one-step method production process and can obtain package stability and reach closure work in-process more than 1 year, and then improved the package stability of wire enamel finished product, stablized the quality of product.
6, in lacquer man's skill of polyurethane wire enamel, adopt dimethyl formamide partly to replace dimethylbenzene can play the dual function of solvent and thinner, viscosity and the solid content that can regulate lacquer liquid in very wide scope are to satisfy different be coated with Wiring technology (felt and die methods) and the different requirements that are coated with line equipment (horizontal and vertical), the wire range of enameled wire can be widened and be 0.015mm～2.0mm, can reduce simultaneously the consumption of toxic phenol again, be beneficial to environmental protection.
Below in conjunction with embodiment the present invention is further described:
Embodiment
Embodiment one:
(1) preparation of hydroxy component:
10 kilograms of stearic acid, 2 kilograms of terephthalic acids, 10 kilograms of Tetra hydro Phthalic anhydrides, 3 kilograms of hexanodioic acids, 12 kilograms of glycerine, 3 kilograms of neopentyl glycol, organic titanium-0.3 kilogram and 5 kilograms dimethylbenzene of antimony composite catalyst are added in the reactor successively.Start heating unit, even temperature reaction is 2 hours between 100 ℃～180 ℃; 180 ℃ to 200 ℃ even temperature reactions 2 hours; Keep 200 ℃ of reactions 2 hours; 200 ℃ and 0.03-0.09MPa negative pressure extracted dimethylbenzene 10 minutes; Add 10 kilograms of cresols at last and between 180 ℃ to 200 ℃, reacted 1 hour, add 19 kilograms in cresols, 13 kilograms of aromatic solvent naphthas, dimethylbenzene successively and stir for 12 kilograms, be cooled to room temperature and make hydroxy component.The technical indicator of measuring polyester polyol resin in the hydroxy component is: acid number 2.2mgKOH/g, and hydroxyl value 220mgKOH/g, number-average molecular weight 4500, molecular weight distributing index is 2.1.
(2) preparation of closure component:
In reactor, add 4,10 kilograms of 4 '-diphenylmethanediisocyanates, 1.1 kilograms of TriMethylolPropane(TMP)s, 11 kilograms of xylenols, 0.8 kilogram in cresols, 4.5 kilograms of dimethyl formamides, 4.5 kilograms of dimethylbenzene.70 ℃ of reactions 4 hours, be warming up to 135 ℃ then, reacted 5 hours, be cooled to 50 ℃ and promptly make closure.The closure technical indicator is the appearance transparent viscous liquid, and residual isocyano-content is less than 0.2%, stores turbid phenomenon not occur after 1 year.
(3) preparation of polyurethane wire enamel and enameled wire performance:
With 30 kilograms of hydroxy components, 29 kilograms of closure components, 4.5 kilograms in cresols, 4.5 kilograms of phenol, 9 kilograms of aromatic solvent naphthas, 3 kilograms of dimethyl formamides, 0.4 kilogram of zinc naphthenate, 40 ℃, stirred 3 hours, make polyurethane wire enamel after removing by filter suspended impurity.
The technical indicator of prepared polyurethane wire enamel is: solid content 29% (180 ℃ of surveys), and viscosity 25 seconds (25 ℃ of surveys), outward appearance is light to the xanchromatic transparent viscous liquid.
Coat the enameled wire of line footpath 0.23mm, the enameled wire external diameter is 0.255mm, the enameled wire any surface finish; 340 ℃ of scolding tin times less than 1 second, the no residue in scolding tin surface; Stretch 3% or 5% or and the bending condition under the salt solution pin hole be zero hole; It is 175 ℃ that heat is dashed, 30min, and ID does not split; Average voltage breakdown is 5000 volts under the room temperature.
Embodiment two:
(1) preparation of hydroxy component:
9 kilograms of Palmiticacid, 2 kilograms of terephthalic acids, 11 kilograms of Tetra hydro Phthalic anhydrides, 2.5 kilograms of hexanodioic acids, 13 kilograms of TriMethylolPropane(TMP)s, 2.5 kilograms of Diethylene Glycols, organic titanium-0.3 kilogram and 5 kilograms dimethylbenzene of antimony composite catalyst are added in the reactor successively.Start heating unit, even temperature reaction is 2 hours between 100 ℃～180 ℃; 180 ℃ to 200 ℃ even temperature reactions 2 hours; Keep 200 ℃ of reactions 2 hours; 200 ℃ and 0.03-0.09MPa negative pressure extracted dimethylbenzene 10 minutes; Add 10 kilograms of cresols at last and between 180 ℃ to 200 ℃, reacted 1 hour, add 19 kilograms in cresols, 13 kilograms of aromatic solvent naphthas, dimethylbenzene successively and stir for 12 kilograms, be cooled to room temperature and make hydroxy component.The technical indicator of measuring polyester polyol resin in the hydroxy component is: acid number 1.9mgKOH/g, and hydroxyl value 230mgKOH/g, number-average molecular weight 5500, molecular weight distributing index is 2.2.
(2) preparation of closure component:
In reactor, add 4,10 kilograms of 4 '-diphenylmethanediisocyanates, 0.3 kilogram of glycerine, 1.1 kilograms of three (hydroxyethyl) isocyanuric acid esters, 11 kilograms of xylenols, 0.8 kilogram in cresols, 4.5 kilograms of dimethyl formamides, 4.5 kilograms of dimethylbenzene.70 ℃ of reactions 4 hours, be warming up to 135 ℃ then, reacted 5 hours, be cooled to 50 ℃ and promptly make closure.The closure technical indicator is the appearance transparent viscous liquid, and residual isocyano-content is less than 0.3%, stores turbid phenomenon not occur after 1 year.
(3) preparation of polyurethane wire enamel and enameled wire performance:
With 31 kilograms of hydroxy components, 32 kilograms of closure components, 4.5 kilograms in cresols, 4.5 kilograms of phenol, 9 kilograms of aromatic solvent naphthas, 3 kilograms of dimethyl formamides, 0.4 kilogram of zinc naphthenate, 40 ℃, stirred 3 hours, make polyurethane wire enamel after removing by filter suspended impurity.
The technical indicator of prepared polyurethane wire enamel is: solid content 32% (180 ℃ of surveys), and viscosity 30 seconds (25 ℃ of surveys), outward appearance is light to the xanchromatic transparent viscous liquid.
Coat the enameled wire of line footpath 0.50mm, the enameled wire external diameter is 0.555mm, the enameled wire any surface finish; 340 ℃ of scolding tin times less than 1.5 seconds, the no residue in scolding tin surface; Stretch 3% or 5% or and the bending condition under the salt solution pin hole be zero hole; It is 175 ℃ that heat is dashed, 30min, and 1D does not split; Average voltage breakdown is 11000 volts under the room temperature.
Claims (4)
1. but the preparation method of the polyurethane wire enamel of a cryogenic direct-welding free of pinholes comprises the following steps:
(1) hydroxy component preparation: hydroxy component carries out melt co-polycondensation earlier by monoprotic acid, aromatic dibasic acid, Tetra hydro Phthalic anhydride, hexanodioic acid, polyvalent alcohol, dibasic alcohol and generates polyester polyol resin, and then No. 1 mixed solvent that adds some amount mixes and forms;
The mass ratio of each reactant is in the component: monoprotic acid: aromatic dibasic acid: Tetra hydro Phthalic anhydride: adipic acid: polyvalent alcohol: dibasic alcohol: No. 1 mixed solvent equals 1:(0.1～0.9): (0.5～1.9): (0.2～0.9): (0.8～2.5): (0.1～0.9): (5～8);
Monoprotic acid be stearic acid, Palmiticacid, myristic acid, lauric one or more;
Aromatic dibasic acid is one or more of terephthalic acid, m-phthalic acid;
Polyvalent alcohol is one or more of glycerine, TriMethylolPropane(TMP), tetramethylolmethane;
Dibasic alcohol is one or more of neopentyl glycol, 2-methyl propanediol, ethylene glycol, glycol ether;
No. 1 mixed solvent is the mixture of cresols, aromatic solvent naphtha, dimethylbenzene, and its mass ratio is (2.5～4.0): (0.5～1.5): (0.5～1.5);
Catalyzer is organic titanium-antimony mixture, and its consumption is 0.2%～1.5% of a reactant quality;
The preparation technology of hydroxy component is: 100 ℃ to 180 ℃ were reacted 1-3 hours, 180 ℃ to 200 ℃ were reacted 1-3 hours, keep 200 ℃ of reactions 1-3 hours, 200 ℃ and 0.01-0.09MPa negative pressure extracted dimethylbenzene 10 minutes to 40 minutes, add cresols and between 180 ℃ to 200 ℃, reacted 1-2 hours, add mixed solvent and promptly make hydroxy component;
(2) closure component preparation: closure is formed by aromatic diisocyanate, trivalent alcohol, phenols encapsulant and No. 2 mixed solvent reactions;
The mass ratio of each reactant is in the component: 4,4 '-diphenylmethanediisocyanate: trivalent alcohol: the phenols encapsulant: No. 2 mixed solvent equals (2～6): (0.2～0.6): (2～5): (3～5);
Trivalent alcohol is one or more of glycerine, TriMethylolPropane(TMP), three (2-hydroxyethyl isocyanuric acid ester);
The phenols encapsulant is one or more in xylenol, the cresols;
No. 2 mixed solvents are the mixture of cresols, dimethyl formamide, dimethylbenzene, and its mass ratio is (0.5～1.0): (3～5): (3～5);
Closure preparation technology is: earlier 4,4 '-diphenylmethanediisocyanate, trivalent alcohol, No. 2 mixed solvents were reacted 2～4 hours at 60 ℃-80 ℃, add the phenols encapsulant then, at 125 ℃～140 ℃, reacted 4～6 hours, be cooled to 50 ℃ and promptly make closure;
(3) lacquer liquid preparation: the preparation technology of polyurethane wire enamel is: is (1～1.9) with hydroxy component, closure component and No. 3 mixed solvents according to mass ratio: (1～1.9): mix (1～3), the zinc naphthenate that adds lacquer liquid total amount 0.2% to 1% again, at 30 ℃～80 ℃, stirred 2 to 3 hours, and made polyurethane wire enamel after removing by filter suspended impurity;
No. 3 mixed solvents are the mixture of cresols, phenol, aromatic solvent naphtha, dimethyl formamide, and its mass ratio is (1～1.5): (1～1.5): (2～3): (0.8～1.2).
2. but the preparation method of the polyurethane wire enamel of cryogenic direct-welding free of pinholes according to claim 1, it is characterized in that: in the described step (1), the technical indicator of prepared polyester polyol resin is: acid number 1-3mgKOH/g, hydroxyl value 130-300mgKOH/g, number-average molecular weight 3000-6000 (gel permeation chromatography, solvents tetrahydrofurane), molecular weight distributing index is (1.9～2.3).
3. but the preparation method of the polyurethane wire enamel of cryogenic direct-welding free of pinholes according to claim 1, it is characterized in that: in the described step (2), prepared closure technical indicator is the appearance transparent viscous liquid, residual isocyano-content is less than 0.1% to 0.5%, and the quality guaranteed period is more than 1 year.
4. but the preparation method of the polyurethane wire enamel of cryogenic direct-welding free of pinholes according to claim 1, it is characterized in that: in the described step (3), the technical indicator of prepared polyurethane wire enamel is: solid content 25% to 40% (180 ℃ of surveys), viscosity 17 seconds to 60 seconds (25 ℃ of surveys), outward appearance is light to the xanchromatic transparent viscous liquid.
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| CNB2007100197607A CN100467557C (en) | 2007-02-08 | 2007-02-08 | Production of cryogenic direct-welding polyurethane envelope without pinhole |
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| CNB2007100197607A CN100467557C (en) | 2007-02-08 | 2007-02-08 | Production of cryogenic direct-welding polyurethane envelope without pinhole |
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2007
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