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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- Prior art keywords
- polyimide
- hours
- insulating varnish
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- solvent
- Prior art date
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- 229920001721 polyimide Polymers 0.000 title claims abstract description 19
- 239000004642 Polyimide Substances 0.000 title claims abstract description 15
- 239000002966 varnish Substances 0.000 title claims abstract description 15
- 239000002114 nanocomposite Substances 0.000 title claims abstract description 13
- 238000002360 preparation method Methods 0.000 title claims abstract description 9
- 239000002904 solvent Substances 0.000 claims abstract description 11
- 239000000463 material Substances 0.000 claims abstract description 8
- 239000011858 nanopowder Substances 0.000 claims abstract description 7
- 239000011347 resin Substances 0.000 claims abstract description 6
- 229920005989 resin Polymers 0.000 claims abstract description 6
- 229920005575 poly(amic acid) Polymers 0.000 claims abstract description 5
- 238000006243 chemical reaction Methods 0.000 claims abstract description 4
- 150000004985 diamines Chemical class 0.000 claims abstract description 4
- 239000009719 polyimide resin Substances 0.000 claims abstract description 4
- 238000003756 stirring Methods 0.000 claims abstract description 4
- 150000008064 anhydrides Chemical class 0.000 claims abstract 2
- 230000015556 catabolic process Effects 0.000 claims abstract 2
- 238000010227 cup method (microbiological evaluation) Methods 0.000 claims abstract 2
- 238000006731 degradation reaction Methods 0.000 claims abstract 2
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 21
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 claims description 8
- FXHOOIRPVKKKFG-UHFFFAOYSA-N N,N-Dimethylacetamide Chemical compound CN(C)C(C)=O FXHOOIRPVKKKFG-UHFFFAOYSA-N 0.000 claims description 7
- 150000008065 acid anhydrides Chemical class 0.000 claims description 6
- 239000000126 substance Substances 0.000 claims description 4
- 238000001816 cooling Methods 0.000 claims description 2
- 238000000227 grinding Methods 0.000 claims description 2
- 239000000843 powder Substances 0.000 claims description 2
- 239000008096 xylene Substances 0.000 claims 4
- 239000002245 particle Substances 0.000 claims 2
- 229910018072 Al 2 O 3 Inorganic materials 0.000 claims 1
- 229910004298 SiO 2 Inorganic materials 0.000 claims 1
- 150000001412 amines Chemical class 0.000 claims 1
- 230000007774 longterm Effects 0.000 abstract description 4
- 238000000354 decomposition reaction Methods 0.000 abstract description 2
- 239000003973 paint Substances 0.000 abstract 1
- 229920001817 Agar Polymers 0.000 description 2
- 239000008272 agar Substances 0.000 description 2
- 238000009792 diffusion process Methods 0.000 description 2
- 239000004922 lacquer Substances 0.000 description 2
- 230000005855 radiation Effects 0.000 description 2
- 238000004804 winding Methods 0.000 description 2
- HLBLWEWZXPIGSM-UHFFFAOYSA-N 4-Aminophenyl ether Chemical compound C1=CC(N)=CC=C1OC1=CC=C(N)C=C1 HLBLWEWZXPIGSM-UHFFFAOYSA-N 0.000 description 1
- 241000024287 Areas Species 0.000 description 1
- 230000003460 anti-nuclear Effects 0.000 description 1
- 239000002826 coolant Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- ANSXAPJVJOKRDJ-UHFFFAOYSA-N furo[3,4-f][2]benzofuran-1,3,5,7-tetrone Chemical compound C1=C2C(=O)OC(=O)C2=CC2=C1C(=O)OC2=O ANSXAPJVJOKRDJ-UHFFFAOYSA-N 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Landscapes
- Paints Or Removers (AREA)
Abstract
本发明公开一种聚酰亚胺/无机纳米复合绝缘漆及其制备方法，本绝缘漆由聚酰亚胺树脂、无机纳米粉体、溶剂组成。其制备方法为：将溶剂称入反应釜中，加入二元胺；分批加入二元酸酐，于室温下搅拌3～5小时；升至50～85℃降解，至物料粘度下降至2.0～4.0分钟(23±2℃，4号杯法)为止；于室温下，在上述聚酰胺酸树脂中加入无机非金属纳米粉体，分散2～48小时，再研磨24～96小时即可。这种绝缘漆经烘焙固化成膜后，在空气中的分解温度在585～610℃之间，长期耐热性不低于300℃，导热系数在0.40～0.70W/(m·K)之间，350℃时的体积电阻率不低于1.0×108Ω·m。The invention discloses a polyimide/inorganic nano composite insulating varnish and a preparation method thereof. The insulating varnish is composed of polyimide resin, inorganic nano powder and a solvent. The preparation method is as follows: weigh the solvent into the reaction kettle, add diamine; add dibasic anhydride in batches, stir at room temperature for 3-5 hours; rise to 50-85°C for degradation, until the viscosity of the material drops to 2.0-4.0 Minutes (23±2°C, No. 4 cup method); at room temperature, add inorganic non-metallic nanopowder to the above polyamic acid resin, disperse for 2-48 hours, and then grind for 24-96 hours. After the insulating paint is baked and solidified into a film, its decomposition temperature in the air is between 585 and 610°C, its long-term heat resistance is not lower than 300°C, and its thermal conductivity is between 0.40 and 0.70W/(m·K). , and the volume resistivity at 350°C is not less than 1.0×10 8 Ω·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)
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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| CN (1) | CN100350003C (en) |
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 | A flexible and wear-resistant surge-resistant insulating coating |
| 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 | A kind of polyimide coating with functional material and method for preparing functional polyimide material using the 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 | Preparation method of polyimide/clay photosensitive nanocomposite material |
-
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 | Preparation method of polyimide/clay photosensitive nanocomposite material |
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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