CN102277079A - Non-pinhole rapid direct-welding polyurethane enamelled wire insulating varnish with high heat grade and preparation method thereof - Google Patents
Non-pinhole rapid direct-welding polyurethane enamelled wire insulating varnish with high heat grade and preparation method thereof Download PDFInfo
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- CN102277079A CN102277079A CN2011102197133A CN201110219713A CN102277079A CN 102277079 A CN102277079 A CN 102277079A CN 2011102197133 A CN2011102197133 A CN 2011102197133A CN 201110219713 A CN201110219713 A CN 201110219713A CN 102277079 A CN102277079 A CN 102277079A
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Abstract
The invention relates to non-pinhole rapid direct-welding polyurethane enamelled wire insulating varnish with high heat grade and a preparation method thereof. The preparation method comprises the following steps: preparing polyester resin; synthesizing blocked isocyanate resin by using trimethylolpropane (TMP), diphenylmethane diisocyanate (MDI), phenol or m-cresol through a two-step method; and mixing paint by using 20 parts of polyester resin, 50 parts of blocked isocyanate resin, 15 parts of dimethylbenzene, 10 parts of phenol and 5 parts of n-butyl alcohol by weight at 60-70 DEG C to prepare the enamelled wire insulating varnish. The enamelled wire insulating varnish has the following advantages: the prepared enamelled wire has high heat resistance, the heat grade can reach 180, the soft breakdown is over 230 DEG C and the heat shock temperature is 200 DEG C (the testing method refers to IEC60851); the enamelled wire can be directly welded at 330 DEG C and no residues are produced after direct welding; the enamelled wire is resistant to kneading and tensile salt-water pinholes in water; the loss of flues in an oven is less and obvious lysate is not produced on the surface of the enamelled wire; and when the product is used for preparing the enamelled wire, the process redundancy is wide and the steady process production is convenient to realize.
Description
Technical field
The present invention relates to a kind of polyurethane enamelled wire insullac, quick beading polyurethane paint wire-covering insullac of especially a kind of high heat-stage free of pinholes and preparation method thereof.
Background technology
Polyurethane enamelled wire insullac is to introduce carbamate groups on the basis of polyester lacquer, because carbamate groups at high temperature can decompose, thereby making the enameled wire of making not need to remove in advance paint film just can directly weld, simplified generation technology greatly, and polyurethane enamelled wire has the low characteristics of dielectric loss under high frequency, has therefore obtained utilization widely in all kinds of electronic devices and components.
But polyurethane enamelled wire also has significant disadvantage, the resistance toheat that is it is not good, can introduce the high-temperature resistant group for the thermotolerance that improves it and improve thermotolerance, but this significantly reduces its straight weldering again, and reduced the salt water resistance pinhole characteristics of enameled wire.Therefore be necessary to provide a kind of polyurethane enamelled wire of good combination property.
Summary of the invention
The objective of the invention is to overcome the shortcoming on the existing polyurethane enamelled wire insullac performance, provide a kind of straight weldering good, the salt water resistance pinhole characteristics is good, the softening temperature height that punctures, and thermal level is the preparation method of the quick beading polyurethane paint wire-covering insullac of high heat-stage free of pinholes more than 180 grades.
The polyurethane enamelled wire insullac that provides aforesaid method to make is provided a further object of the present invention.
The object of the invention is achieved through the following technical solutions: the preparation method of the quick beading polyurethane paint wire-covering insullac of a kind of high heat-stage free of pinholes comprises following content:
(1) preparation of vibrin: adopt glycerine, ethylene glycol, m-phthalic acid synthesizing polyester resin, wherein the mol ratio of glycerine and ethylene glycol is 1:1～1:1.1, hydroxyl and carboxylic acid group's mol ratio is 1.2:1～1.5:1 synthesizing polyester resin intermediate, wherein, glycerine: ethylene glycol the best is 1:1, and mol ratio the best of hydroxyl and carboxylic acid group is 1.5:1;
(2) with TriMethylolPropane(TMP) (TMP), diphenylmethanediisocyanate (MDI), phenol or meta-cresol adopt the synthetic sealing of two-step approach isocyanate resin, mol ratio is TMP:MDI: phenol=1:3:9, wherein phenol is the excessive and double solvent of doing, earlier with MDI and the synthetic MDI that seals of phenol, generate the sealing isocyanate resin with TMP reaction again, adding meta-cresol and dimethylbenzene, to be diluted to solids content be 43%～45% standby;
(3) with 20 weight part vibrin, 50 weight parts sealing isocyanate resin, 15 weight part dimethylbenzene, 10 weight part phenol, 5 weight part propyl carbinols stirred 2 hours under 60～70 ℃ of conditions, were cooled to 45 ℃ of paints and became the quick beading polyurethane paint wire-covering insullac of high heat-stage free of pinholes.
On the such scheme basis, the concrete preparation method of described vibrin: in reactor A, add glycerine, ethylene glycol, terephthalic acid, account for total charging capacity 0.04% zinc acetate, account for the 0.02% positive butyl (tetra) titanate heat temperature raising to 220 ℃ of total charging capacity, control 105 ℃ of column top temperatures and following, when no cut distillates, under the vacuum tightness of-0.6kg, vacuumize, keep 210 ℃ of still temperature, distillate until no cut, the solids content that adding meta-cresol, dimethylbenzene are diluted to vibrin is 45%, and 23 ℃ of viscosity 800 ~ 1000mpas are standby.
On the such scheme basis, described blocked isocyanate adopts two-step approach:
The first step with the one-NCO of phenol sealing MDI, is 1:1～1:1.2 by the equivalence ratio of controlling phenol and MDI earlier, and phenol is dropped among the reactor B, then MDI is dropped in the reactor fast 40 ~ 60 ℃ of control still temperature, stirring reaction 3 hours;
Second step added TMP in aforesaid reaction vessel, be warming up to naturally and react when stopping, and was heated to 138 ~ 140 ℃, and transparent to material, the solids content that adding meta-cresol and dimethylbenzene are diluted to blocked isocyanate is 45%, and 23 ℃ of viscosity 2500 ~ 3500mpas are standby.
In the content of the present invention, described MDI adopts 2, and 4 '-MDI content is 50% and above MDI, and is as shown below:
Figure
2,4 '-MDI
Since 100% 2,4 '-MDI is difficult to obtain, generally be and 4, the mixture of 4 '-MDI,
Figure
4,4 '-MDI
2, the content of 4 '-MDI is high more good more.
The ideal structure formula of blocked isocyanate resin is:
TMP:DMI: phenol=1:3:3
The present invention carries a kind of product that utilizes above-mentioned preparation method to make, described vibrin 20 weight parts, blocked isocyanate resin 50 weight parts, add 15 weight part dimethylbenzene, 10 weight part phenol, 5 weight part propyl carbinol paint to solids contents are 30% the quick beading polyurethane paint wire-covering insullac of high heat-stage.
Can be according to producing needs, the adding weight part of regulating the solvent part in proportion obtains the quick beading polyurethane paint wire-covering insullac of high heat-stage of different solid contents.
Compared with prior art, the quick beading polyurethane paint wire-covering insullac made from the present invention of high heat-stage free of pinholes has following advantage:
(1) the enameled wire resistance toheat height of making, thermal level can reach 180 grades, the softening puncture more than 230 ℃, heat is dashed level 200 ℃ of temperature (testing method is with reference to IEC 60851).
(2) enameled wire of making directly weldering property is good, can be 330 ℃ of straight weldering, and straight postwelding does not have residue.
(3) the enameled wire saline infusion needle pore property excellence of making, stretching salt solution pin hole in anti-rubbing and the water.
When (4) making enameled wire with this product, the stack losses in baker is fewer, and the enameled wire surface does not have tangible lysate to produce.
(5) the technology remaining is wide, is convenient to realize sane explained hereafter.
Embodiment
Comparative example 1
With 130 grades of common urethane (such as Shanghai Sheng Ran Insulation Materials Co 814/30), produce the polyurethane enamelled wire of paste paint film.
Comparative example 2
With 155 grades of common urethane (such as Shanghai Sheng Ran Insulation Materials Co 815/30), produce the polyurethane enamelled wire of paste paint film.
Comparative example 3
With 180 grades of common urethane (such as Shanghai Sheng Ran Insulation Materials Co 816/30), produce the polyurethane enamelled wire of paste paint film.
Comparative example 4
Get 20 parts in vibrin, (single stage method is synthetic to add 50 parts of blocked isocyanate resins, the trade mark of MDI is the MDI-50 of Yantai ten thousand China), add 15 parts of dimethylbenzene during 70 ℃ of still temperature, 10 parts of meta-cresols, 5 parts of propyl carbinols stirred 3 hours, and blowing filters when being cooled to 45 ℃, made that to contain admittedly be the polyurethane enamelled wire that 30% polyurethane paint is produced the paste paint film.
Embodiment 1
Get 20 parts in vibrin, (two-step approach is synthetic to add 50 parts of blocked isocyanate resins, the trade mark of MDI is the MDI-50 of Yantai ten thousand China), add 15 parts of dimethylbenzene during 70 ℃ of still temperature, 10 parts of meta-cresols, 5 parts of propyl carbinols stirred 3 hours, and blowing filters when being cooled to 45 ℃, made that to contain admittedly be the polyurethane enamelled wire that 30% polyurethane paint is produced the paste paint film.
Embodiment 2
Get 20 parts in vibrin, (two-step approach is synthetic to add 50 parts of blocked isocyanate resins, the trade mark of MDI is the SUPRASEC 3051 of HUNTSMAN), add 15 parts of dimethylbenzene during 70 ℃ of still temperature, 10 parts of meta-cresols, 5 parts of propyl carbinols stirred 3 hours, and blowing filters when being cooled to 45 ℃, made that to contain admittedly be the polyurethane enamelled wire that 30% polyurethane paint is produced the paste paint film.
Embodiment 3
Get 20 parts in vibrin, (two-step approach is synthetic to add 50 parts of blocked isocyanate resins, the trade mark of MDI is the DESMODUR 2460M of BAYER), add 15 parts of dimethylbenzene during 70 ℃ of still temperature, 10 parts of meta-cresols, 5 parts of propyl carbinols stirred 3 hours, and blowing filters when being cooled to 45 ℃, made that to contain admittedly be the polyurethane enamelled wire that 30% polyurethane paint is produced the paste paint film.
The preparation of enameled wire line-transect:
Be coated with line equipment: plum reaches QHW 4/1
Processing parameter:
Baker import: 350 ℃; In the middle of the baker: 380 ℃; Baker outlet: 420 ℃; Recirculation blower: 1000RPM; Waste discharge blower fan: 800RPM;
The speed of a motor vehicle: 115 m/min
Japanning passage: 7
The enameled wire specification is 0.20mm.
Following table is comparative example and embodiment performance test tabulation:
| ? | Comparative example 1 | Comparative example 2 | Comparative example 3 | Comparative example 4 | Embodiment 1 | Embodiment 2 | Embodiment 3 |
| Conductor diameter | 0.199 | 0.199 | 0.200 | 0.199 | 0.199 | 0.200 | 0.200 |
| The enameled wire external diameter | 0.230 | 0.231 | 0.231 | 0.230 | 0.232 | 0.231 | 0.233 |
| Straight weldering property: 375 ℃, 3 seconds | OK | OK | OK | OK | OK | OK | OK |
| Straight weldering property: 350 ℃, 3 seconds | OK | NG | NG | OK | OK | OK | OK |
| Straight weldering property: 330 ℃, 3 seconds | NG | NG | NG | NG | OK | OK | OK |
| Normality salt solution pin hole | OK | OK | OK | OK | OK | OK | OK |
| Rubbing salt solution pin hole | OK | OK | NG | OK | OK | OK | OK |
| Stretching salt solution pin hole in the water | NG | NG | NG | OK | OK | OK | OK |
| Softening puncture ℃ | 170 | 200 | 230 | 230 | 230 | 230 | 230 |
| Thermal shocking ℃ | 155 | 175 | 230 | 230 | 230 | 230 | 230 |
| Enameled wire surface lysate | Less | Many | Many | Many | Seldom | Seldom | Seldom |
Annotate:
Adopt Pb-free solder in the test of straight weldering property, test method is with reference to JIS C 3003.
The test method of softening puncture and thermal shocking is with reference to IEC 60851.
The testing method of enameled wire surface lysate is: with the enameled wire of a clean blank sheet of paper wiping baker outlet one minute, the amount of observing blank sheet of paper adhesion lysate, this test only is a simultaneous test.
As can be seen from the above table: all there are the many problems of enameled wire surface lysate in comparative example 1 to 4, and comparative example 1 to 4 can not satisfy the requirement of straight weldering property fully.
Use the quick beading polyurethane paint wire-covering insullac of high heat-stage free of pinholes of the inventive method preparation, the enameled wire of making can directly weld down at 330 ℃, and the no residue in enameled wire surface behind the scolding tin; Saline infusion needle pore property excellence, stretching salt solution pin hole in anti-rubbing and the water; The softening temperature that punctures can reach more than 230 ℃, and the heatproof index is 180 grades.
Claims (6)
1. the preparation method of the quick beading polyurethane paint wire-covering insullac of high heat-stage free of pinholes, its feature comprises following content:
The preparation of vibrin: adopt glycerine, ethylene glycol, m-phthalic acid synthesizing polyester resin, wherein the mol ratio of glycerine and ethylene glycol is 1:1～1:1.1, and hydroxyl and carboxylic acid group's mol ratio is 1.2:1～1.5:1;
With TriMethylolPropane(TMP) (TMP), diphenylmethanediisocyanate (MDI), phenol or meta-cresol adopt the synthetic sealing of two-step approach isocyanate resin, mol ratio is TMP:MDI: phenol=1:3:9, wherein phenol is the excessive and double solvent of doing, earlier with MDI and the synthetic MDI that seals of phenol, generate the sealing isocyanate resin with TMP reaction again, adding meta-cresol and dimethylbenzene, to be diluted to solids content be 43%～45% standby;
With 20 weight part vibrin, 50 weight parts sealing isocyanate resin, 15 weight part dimethylbenzene, 10 weight part phenol, 5 weight part propyl carbinols become the quick beading polyurethane paint wire-covering insullac of high heat-stage free of pinholes 60～70 ℃ of paints.
2. according to the preparation method of the quick beading polyurethane paint wire-covering insullac of claims 1 described high heat-stage free of pinholes, it is characterized in that: the concrete preparation method of described vibrin: in reactor, add glycerine, ethylene glycol, terephthalic acid, account for 0.04% zinc acetate of total charging capacity, account for 0.02% the positive butyl (tetra) titanate heat temperature raising to 220 ℃ of total charging capacity, control 105 ℃ of column top temperatures and following, when no cut distillates, under the vacuum tightness of-0.6kg, vacuumize, keep 210 ℃ of still temperature, distillate until no cut, add meta-cresol, the solids content that dimethylbenzene is diluted to vibrin is 45%, and 23 ℃ of viscosity 800 ~ 1000mpas are standby.
3. according to the preparation method of the quick beading polyurethane paint wire-covering insullac of claims 1 described high heat-stage free of pinholes, it is characterized in that described blocked isocyanate adopts two-step approach:
The first step with the one-NCO of phenol sealing MDI, is 1:1～1:1.2 by the equivalence ratio of controlling phenol and MDI earlier, and phenol is dropped in the reactor, then MDI is dropped in the reactor fast 40 ~ 60 ℃ of control still temperature, stirring reaction 3 hours;
Second step added TMP in aforesaid reaction vessel, be warming up to naturally and react when stopping, and was heated to 138 ~ 140 ℃, and transparent to material, the solids content that adding meta-cresol and dimethylbenzene are diluted to blocked isocyanate is 45%, and 23 ℃ of viscosity 2500 ~ 3500mpas are standby.
4. according to the preparation method of claims 1 or the quick beading polyurethane paint wire-covering insullac of 3 described high heat-stage free of pinholes, it is characterized in that described MDI adopts 2,4 '-MDI content is 50% and above MDI.
5. product that the preparation method who utilizes the quick beading polyurethane paint wire-covering insullac of the described high heat-stage free of pinholes of one of claims 1 to 4 makes, it is characterized in that with described vibrin 20 weight parts, blocked isocyanate resin 50 weight parts, add 15 weight part dimethylbenzene, 10 weight part phenol, 5 weight part propyl carbinol paint to solids contents are 30% the quick beading polyurethane paint wire-covering insullac of high heat-stage.
6. according to claims 5 described products, it is characterized in that the adding weight part of regulating the solvent part in proportion obtains the quick beading polyurethane paint wire-covering insullac of high heat-stage of different solid contents according to producing needs.
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Cited By (6)
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| CN102604384A (en) * | 2012-02-29 | 2012-07-25 | 苏州巨峰电气绝缘系统股份有限公司 | Universal refrigerant resistant solvent-free impregnating resin for high and low voltage motor and preparation method thereof |
| CN103773187A (en) * | 2014-01-20 | 2014-05-07 | 南通钰成光电科技有限公司 | Enamelled wire coating for electric appliance and preparation method thereof |
| CN104017476A (en) * | 2014-05-30 | 2014-09-03 | 百川化工(如皋)有限公司 | Production method of 180-level polyurethane wire enamel |
| CN104087142A (en) * | 2014-07-15 | 2014-10-08 | 王锶源 | Heat-resistant insulating paint |
| CN109135545A (en) * | 2018-08-20 | 2019-01-04 | 安徽晟然绝缘材料有限公司 | Zero salt water pin hole polyurethane wire enamel of one kind and preparation method thereof |
| CN109486378A (en) * | 2018-11-07 | 2019-03-19 | 苏州太湖电工新材料股份有限公司 | The flame retardant type insulated paint and its preparation method and application of resistance to ATF oil for electric vehicle |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102604384A (en) * | 2012-02-29 | 2012-07-25 | 苏州巨峰电气绝缘系统股份有限公司 | Universal refrigerant resistant solvent-free impregnating resin for high and low voltage motor and preparation method thereof |
| CN103773187A (en) * | 2014-01-20 | 2014-05-07 | 南通钰成光电科技有限公司 | Enamelled wire coating for electric appliance and preparation method thereof |
| CN104017476A (en) * | 2014-05-30 | 2014-09-03 | 百川化工(如皋)有限公司 | Production method of 180-level polyurethane wire enamel |
| CN104017476B (en) * | 2014-05-30 | 2016-02-24 | 百川化工(如皋)有限公司 | A kind of production method of 180 level polyurethane enamelled wire paints |
| CN104087142A (en) * | 2014-07-15 | 2014-10-08 | 王锶源 | Heat-resistant insulating paint |
| CN109135545A (en) * | 2018-08-20 | 2019-01-04 | 安徽晟然绝缘材料有限公司 | Zero salt water pin hole polyurethane wire enamel of one kind and preparation method thereof |
| CN109486378A (en) * | 2018-11-07 | 2019-03-19 | 苏州太湖电工新材料股份有限公司 | The flame retardant type insulated paint and its preparation method and application of resistance to ATF oil for electric vehicle |
| CN109486378B (en) * | 2018-11-07 | 2020-08-04 | 苏州太湖电工新材料股份有限公司 | ATF oil-resistant flame-retardant insulating paint for electric automobile and preparation method and application thereof |
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Application publication date: 20111214 |