CN100350003C - 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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- CN100350003C CN100350003C CNB2005100071309A CN200510007130A CN100350003C CN 100350003 C CN100350003 C CN 100350003C CN B2005100071309 A CNB2005100071309 A CN B2005100071309A CN 200510007130 A CN200510007130 A CN 200510007130A CN 100350003 C CN100350003 C CN 100350003C
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Abstract
The present invention discloses polyimide and inorganic nanometer powder compounded insulating paint, and a preparation method thereof. The insulating paint is composed of polyimide resin, inorganic nanometer powder and a solvent. The preparation method comprises the following steps: weighing the solvent, adding the solvent into a reaction kettle and adding diamine; adding diacid anhydride and stirring at room temperature for 3 to 5 hours; raising the temperature to 50 to 85 DEG C for degradation until the viscosity of the materials falls for 2.0 to 4.0 minutes (23 plus/minus 2 DEG C, No. 4 cup method); adding an inorganic nonmetal nanometer powder to polyamic acid resin for dispersion for 2 to 48 hours and grinding for 24 to 96 hours to obtain the insulating paint. After being baked and solidified into a film, the insulating paint exposed to the air has the decomposition temperature of 585 to 610 DEG C, the long-term thermal endurance at least 300 DEG C, the heat conduction coefficient of 0.40 to 0.70W/(m. K), and the volume resistivity at least 1.0*10<8> omega m.
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 is the polyimide resin component: weight percent content is 3.0～10%, 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 is the inorganic nanometer powder component: weight percent content is 0.5～15.0%, and median size is the inorganic non-metallic nano-powder of 10nm～200nm.
Component 3 is a solvent: weight percent content is 75～90% solvent, and it consists of N,N-DIMETHYLACETAMIDE, dimethylbenzene and/or toluene, wherein N,N-DIMETHYLACETAMIDE: dimethylbenzene and/or toluene=40～60: 60～40, and its ratio is a weight ratio.
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 polyimide/inorganic nano-composite insulating varnish.
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, degree makes 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, and promptly obtained polyimide/inorganic nano-composite insulating varnish.
Claims (2)
1. polyimide/inorganic nano-composite insulating varnish is characterized in that containing following three kinds of components:
Component 1 is the polyimide resin component: weight percent content is 3.0～10%, 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 is the inorganic nanometer powder component: weight percent content is 0.5～15.0%, and median size is the SiO of 10nm～200nm
2And/or Al
2O
3Powder;
Component 3 is a solvent: weight percent content is 75～90% solvent, and it consists of N,N-DIMETHYLACETAMIDE, dimethylbenzene and/or toluene, wherein N,N-DIMETHYLACETAMIDE: dimethylbenzene and/or toluene=40～60: 60～40, and its ratio is a weight ratio.
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:
Solvent N,N-DIMETHYLACETAMIDE, dimethylbenzene and/or toluene are weighed in the reactor, and N,N-DIMETHYLACETAMIDE, dimethylbenzene and/or toluene consumption add diamine for 75～90% of the reaction total amount, are 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: adopts No. 4 agar diffusion methods in 23 ± 2 ℃ of mensuration down, viscosity is till 2.0～4.0 minutes; Under room temperature, adding median size in 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 again 24～96 hours, promptly obtain polyimide/inorganic nano-composite insulating varnish.
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 |
Applications Claiming Priority (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 |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1718658A CN1718658A (en) | 2006-01-11 |
| CN100350003C true CN100350003C (en) | 2007-11-21 |
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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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Families Citing this family (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 |
| 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 |
| CN102412027B (en) * | 2011-12-12 | 2013-01-23 | 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 |
| 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 |
| CN111253856B (en) * | 2020-03-11 | 2021-10-15 | 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 |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1258690A (en) * | 2000-01-05 | 2000-07-05 | 浙江大学 | Preparation of composite nanometer polyimide/clay film with very low thermal expansion coefficient |
| CN1424355A (en) * | 2002-12-25 | 2003-06-18 | 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
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1258690A (en) * | 2000-01-05 | 2000-07-05 | 浙江大学 | Preparation of composite nanometer polyimide/clay film with very low thermal expansion coefficient |
| CN1424355A (en) * | 2002-12-25 | 2003-06-18 | 上海交通大学 | Polyimide/clay photosensitive nano composite material preparation |
Non-Patent Citations (1)
| Title |
|---|
| 溶胶-凝胶法制备可溶性聚酰亚胺/二氧化硅纳米复合材料的研究I.溶胶-凝胶转变过程和反应机理的研究 杨勇，朱子康 漆宗，漆宗能.功能材料 1999 * |
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| CN1718658A (en) | 2006-01-11 |
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