CN1718658A - Polyimide/inorganic nano-composite insulating varnish and its preparation method - Google Patents
Polyimide/inorganic nano-composite insulating varnish and its preparation method Download PDFInfo
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- CN1718658A CN1718658A CN 200510007130 CN200510007130A CN1718658A CN 1718658 A CN1718658 A CN 1718658A CN 200510007130 CN200510007130 CN 200510007130 CN 200510007130 A CN200510007130 A CN 200510007130A CN 1718658 A CN1718658 A CN 1718658A
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Abstract
An insulating polyimide/inorganic nano-material paint is proportionally prepared from polyimide resin, inorganic nano-particles and solvent through adding binary amine to solvent, adding binary acid anhydride step by step, stirring, heating until the viscosity is lowered to 2.0-4.0, dispersing the inorganic non-metal nanoparticles in said polyamide resin, and grinding. Its durable high-temp resistance is more than 300 deg.C and its heat conductivity is 0.4-0.7 W/(m.K).
Description
Technical field
The present invention relates to a kind of polyimide/inorganic nano-composite insulating varnish and preparation method thereof.
Background technology
Polyimide insulative lacquer on the market is after the baked and cured film forming at present, and long-term heat resistance generally is not higher than 250 ℃, and for some special Application Areass, its thermotolerance still can not satisfy the requirement of some high-tech product; Its thermal conductivity is mostly lower, generally between 0.20～0.25W/ (mK), is unfavorable for the heat radiation of electrical equipment and electrical winding, micromodule, causes operating temperature further to raise, reliability decrease.
Summary of the invention
The object of the present invention is to provide polyimide/inorganic nano-composite insulating varnish of the high heat conduction of a kind of superhigh temperature resistant and preparation method thereof, the long-term heat resistance of this nano combined impregnating varnish is not less than 300 ℃, and thermal conductivity is common commercially available more than two times of polyimide insulative lacquer.
The high heat conduction polyimide/inorganic nano-composite insulating varnish of the superhigh temperature resistant that the present invention relates to is grouped into by following three one-tenth:
Component 1 (polyimide resin component): content 3.0～10% (weight percent) has following repetition chemical structure unit (molecular formula 1):
This repetition chemical structure unit changes molecular formula 2 into after high temperature cures film-forming:
R wherein
1For:
And/or
R
2For:
Component 2 (inorganic nanometer powder component): content is 0.5～15.0% (weight percent), and median size is the inorganic non-metallic nano-powder of 10nm～200nm.
Component 3 (solvent): content is the solvent of 75～90% (weight percents), and it consists of N,N-DIMETHYLACETAMIDE, dimethylbenzene and/or toluene, wherein N,N-DIMETHYLACETAMIDE: dimethylbenzene and/or toluene=(40～60): (60～40) (weight percent).
The preparation method of polyimide/inorganic nano-composite insulating varnish:
Solvent is weighed in the reactor, and solvent load adds diamine for 75～90% of the reaction total amount, is stirred to dissolving fully under the room temperature.Slowly add dibasic acid anhydride, the mol ratio of diamine and dibasic acid anhydride is 1.0mol: 1.01～1.03mol in batches.By giving reactor suitably cooling and control feed rate, make temperature of charge be no more than 45 ℃.Dibasic acid anhydride adds the back and stirred under room temperature 3～5 hours.Material viscosity rises to 50～85 ℃ of degradeds after reaching greatly, degrades to material viscosity to drop to 2.0～4.0 minutes till (23 ± 2 ℃, No. 4 agar diffusion methods).Obtain having the polyamic acid resin of structure shown in molecular formula 1, this resin changes the polyimide resin with structure shown in molecular formula 2 into after high temperature cures film-forming.
Under room temperature, adding median size in above-mentioned polyamic acid resin is the inorganic non-metallic nano-powder of 10nm～200nm, adopt the high speed dispersor high shear stress to disperse 2～48 hours down, ground 24～96 hours with grinding plant again, promptly obtain product of the present invention.
This insullac is after the baked and cured film forming, and aerial decomposition temperature is between 585～610 ℃, and long-term heat resistance is not less than 300 ℃, and thermal conductivity is between 0.40～0.70W/ (mK), and the volume specific resistance in the time of 350 ℃ is not less than 1.0 * 10
8Ω m.The polyimide/inorganic nano-composite insulating varnish that the present invention relates to is mainly used in the varnished insulation of making the superhigh temperature resistant insulated wire or being used for extraordinary superhigh temperature resistant, the electrical equipment and electrical of anti-nuclear radiation winding and handles.
Embodiment
Embodiment one
In the 100L reactor, be weighed into solvent 85Kg, solvent consist of N,N-DIMETHYLACETAMIDE: toluene=60: 40 (weight ratio), start stirring, add 4,4 '-diamino-diphenyl ether 15.00mol, be stirred to dissolving fully under the room temperature.Open the reactor water coolant, slowly add pyromellitic acid anhydride 15.30mol in batches, suitably cool off and the control feed rate, make temperature of charge be no more than 45 ℃ to the logical water coolant of reactor.Pyromellitic acid anhydride adds the back and stirred 4 hours under room temperature.Material viscosity rises to 85 ℃ of degradeds after reaching greatly, degrades to material viscosity to drop to 4.0 minutes till (23 ± 2 ℃, No. 4 agar diffusion methods).Obtain palm fibre to thick, the equal benzene type of red-brown polyamic acid resin.
Reduce to below 40 ℃, adding median size is the SiO of 10nm～50nm
2Powder 6.0Kg, ground 96 hours with ball-grinding machine after 2 hours with the high speed dispersor high speed dispersion again, obtained the high heat conduction polyimide of superhigh temperature resistant/nanometer SiO
2Composite insulating varnish.
This insullac through 350 ℃ cure 2 hours film-formings after, the aerial decomposition temperature of paint film is 605 ℃, long-term heat resistance is not less than 320 ℃, thermal conductivity is not less than 0.50W/ (mK), the volume specific resistance in the time of 350 ℃ is not less than 4.0～6.0 * 10
9Ω m.
Embodiment two
In embodiment one, be the Al of 20nm～50nm with median size
2O
3Powder 6.0Kg replaces nanometer SiO
2Powder, all the other proportion of raw materials, preparation technology are constant, can obtain the high heat conduction polyimide of superhigh temperature resistant/nanometer Al that another kind the present invention relates to
2O
3Compound insullac.
This insullac through 350 ℃ cure 2 hours film-formings after, the aerial decomposition temperature of paint film is 595 ℃, long-term heat resistance is not less than 300 ℃, thermal conductivity is not less than 0.60W/ (mK), the volume specific resistance in the time of 350 ℃ is not less than 2.0～6.0 * 10
8Ω m.
Claims (2)
1. polyimide/inorganic nano-composite insulating varnish is characterized in that containing following three kinds of components:
Component 1 (polyimide resin component): content 3.0～10% (weight percent) has following repetition chemical structure unit:
This repetition chemical structure unit changes into after high temperature cures film-forming:
R wherein
1For:
R
2For:
Component 2 (inorganic nanometer powder component): content is 0.5～15.0% (weight percent), and median size is the SiO of 10nm～200nm
2And/or Al
2O
3Powder;
Component 3 (solvent): content is the solvent of 75～90% (weight percents), and it consists of N,N-DIMETHYLACETAMIDE, dimethylbenzene and/or toluene, wherein N,N-DIMETHYLACETAMIDE: dimethylbenzene and/or toluene=(40～60): 60～40 (weight percents).
2. the preparation method of the described polyimide/inorganic nano-composite insulating varnish of claim 1 is characterized in that the preparation method adopts following steps:
The described solvent of claim 1 is weighed in the reactor, and solvent load adds diamine for 75～90% of the reaction total amount, is stirred to dissolving fully under the room temperature; Slowly add dibasic acid anhydride, the mol ratio of diamine and dibasic acid anhydride is 1.0mol: 1.01～1.03mol in batches; By giving reactor suitably cooling and control feed rate, make temperature of charge be no more than 45 ℃; Dibasic acid anhydride adds the back and stirred under room temperature 3～5 hours; Material viscosity rises to 50～85 ℃ of degradeds after reaching greatly, degrades to material viscosity to drop to 2.0～4.0 minutes till (23 ± 2 ℃, No. 4 agar diffusion methods); Under room temperature, adding median size in the described polyamic acid resin of claim 1 is the described inorganic non-metallic nano-powder of claim 1 of 10nm～200nm, adopt the high speed dispersor high shear stress to disperse 2～48 hours down, ground again 24～96 hours, promptly obtain product of the present invention.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2005100071309A CN100350003C (en) | 2005-01-21 | 2005-01-21 | Polyimide/inorganic nano-composite insulating varnish and its preparation method |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2005100071309A CN100350003C (en) | 2005-01-21 | 2005-01-21 | Polyimide/inorganic nano-composite insulating varnish and its preparation method |
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| Publication Number | Publication Date |
|---|---|
| CN1718658A true CN1718658A (en) | 2006-01-11 |
| CN100350003C CN100350003C (en) | 2007-11-21 |
Family
ID=35930609
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|---|---|---|---|
| CNB2005100071309A Expired - Fee Related CN100350003C (en) | 2005-01-21 | 2005-01-21 | Polyimide/inorganic nano-composite insulating varnish and its preparation method |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100440387C (en) * | 2006-09-04 | 2008-12-03 | 山东赛特电工材料有限公司 | Compound paint copper-in-aluminum enameled wire and its manufacturing method |
| CN102412027A (en) * | 2011-12-12 | 2012-04-11 | 江苏冰城电材股份有限公司 | Manufacturing method of H-level and 200-level electromagnetic wire |
| CN102079945B (en) * | 2009-11-26 | 2012-11-21 | 福保化学股份有限公司 | Surge-withstanding insulating paint with flexibility and attrition resistance |
| CN105802222A (en) * | 2016-04-22 | 2016-07-27 | 广东精达里亚特种漆包线有限公司 | Nanometer polyamide imide film containing inorganic oxide and preparation method of nanometer polyamide imide film |
| CN110229609A (en) * | 2019-05-23 | 2019-09-13 | 东南大学 | A method of the polyimide paint with functional material and use the coating preparation functional form polyimide material |
| CN111253856A (en) * | 2020-03-11 | 2020-06-09 | 江苏龙创新材料科技有限公司 | High-temperature-resistant and corona-resistant polyimide wire enamel and preparation method thereof |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1101415C (en) * | 2000-01-05 | 2003-02-12 | 浙江大学 | Preparation of composite nanometer polyimide/clay film with very low thermal expansion coefficient |
| CN1171952C (en) * | 2002-12-25 | 2004-10-20 | 上海交通大学 | Polyimide/clay photosensitive nano composite material preparation |
-
2005
- 2005-01-21 CN CNB2005100071309A patent/CN100350003C/en not_active Expired - Fee Related
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100440387C (en) * | 2006-09-04 | 2008-12-03 | 山东赛特电工材料有限公司 | Compound paint copper-in-aluminum enameled wire and its manufacturing method |
| CN102079945B (en) * | 2009-11-26 | 2012-11-21 | 福保化学股份有限公司 | Surge-withstanding insulating paint with flexibility and attrition resistance |
| CN102412027A (en) * | 2011-12-12 | 2012-04-11 | 江苏冰城电材股份有限公司 | Manufacturing method of H-level and 200-level electromagnetic wire |
| CN105802222A (en) * | 2016-04-22 | 2016-07-27 | 广东精达里亚特种漆包线有限公司 | Nanometer polyamide imide film containing inorganic oxide and preparation method of nanometer polyamide imide film |
| CN110229609A (en) * | 2019-05-23 | 2019-09-13 | 东南大学 | A method of the polyimide paint with functional material and use the coating preparation functional form polyimide material |
| CN110229609B (en) * | 2019-05-23 | 2021-06-25 | 东南大学 | Polyimide coating with functional material and method for preparing functional polyimide material by adopting coating |
| CN111253856A (en) * | 2020-03-11 | 2020-06-09 | 江苏龙创新材料科技有限公司 | High-temperature-resistant and corona-resistant polyimide wire enamel and preparation method thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN100350003C (en) | 2007-11-21 |
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