CN102936341A - Polyimide resin synthesis method - Google Patents
Polyimide resin synthesis method Download PDFInfo
- Publication number
- CN102936341A CN102936341A CN2012103743064A CN201210374306A CN102936341A CN 102936341 A CN102936341 A CN 102936341A CN 2012103743064 A CN2012103743064 A CN 2012103743064A CN 201210374306 A CN201210374306 A CN 201210374306A CN 102936341 A CN102936341 A CN 102936341A
- Authority
- CN
- China
- Prior art keywords
- powder mixture
- heat conducting
- nano powder
- conducting nano
- polyamic acid
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Landscapes
- Macromolecular Compounds Obtained By Forming Nitrogen-Containing Linkages In General (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The present invention discloses a polyimide resin synthesis method. The polyimide resin comprises a thermally conductive nanometer powder mixture and a resin solid, wherein the resin solid is polyamic acid, and the thermally conductive nanometer powder mixture is a mixture of three thermally conductive nanometer powders such as Al2O3, NB and AlN, and is 10-30% of the total amount of the resin solid. During synthesis, pyromellitic dianhydride reacts with 4,4'-diaminodiphenyl ether to obtain polyamic acid, the grinded thermally conductive nanometer powder mixture is added to the polyamic acid according to a certain proportion, then pyromellitic dianhydride is added to control a viscosity of the final reaction product to reach 85000-95000 CP, and deaeration slobbering film formation is performed to obtain the finished product. According to the polyimide resin synthesized by the method, a thermal conductivity coefficient can be more than three times the thermal conductivity coefficient of the ordinary polyimide film, excellent electrical property, excellent thermal property and excellent mechanical property are provided, and a storage life of the electronic component can be substantially improved.
Description
Technical field
The present invention relates to a kind of synthetic method of polyimide resin.
Background technology
Polyimide (PI) is the high-performance polymer material of a class take imide ring as constitutional features; have good dielectric properties, mechanical property, thermal stability and solvent resistance etc.; in microelectronics industry, be widely used, become the novel material that electronic component connects and protects.Development along with the ic manufacturing technology level, the size of super large-scale integration is dwindled gradually, metal interconnected resistance, electric capacity (Rc) cause signal transmission delay and crosstalk and the heating of electronic original part, directly affect performance of devices and work-ing life.In order to address the above problem, polyimide material is had higher requirement---reduce specific inductivity and promote heat conductivility.
At present the thermal conductivity Kapton basically all pass through the inorganics that specific inductivity is lower and polyimide compound, make it to disperse at nano level, thereby the effect by nano-grade inorganics produces special performance or the performance of polyimide is improved, but all undesirable aspect heat conduction, can't satisfy the demand of the electronic component of microelectronics industry.
Summary of the invention
The objective of the invention is provides excellent electrical properties, thermal characteristics and the mechanical property that a kind of thermal conductivity is high, have in order to solve above-mentioned the deficiencies in the prior art, can increase substantially the synthetic method of polyimide resin in the work-ing life of electronic component.
To achieve these goals, the synthetic method of a kind of polyimide resin provided by the invention, comprise and adopt heat conducting nano powder mixture and resin solid thing, it is characterized in that described resin solid thing is by pyromellitic acid anhydride (PMDA) and 4, the resulting polyamic acid of 4'-diaminodiphenyl oxide (ODA) building-up reactions (PAA), described heat conducting nano powder mixture is Al
2O
3The mixture of (aluminium sesquioxide), NB (boronation nitrogen) and three kinds of heat conducting nano powders of AlN (aluminium nitride), the consisting of of its weight part: Al
2O
3: 10 parts-40 parts, NB:20 part-50 part, AlN:20 part-60 part, the heat conducting nano powder mixture accounts for the 10%-30% of resin solid thing total amount; When synthetic, at first to pyromellitic acid anhydride (PMDA) and 4,4 '-diaminodiphenyl oxide (ODA) calculates required separately reacting weight (wherein: PMDA: molecular weight 218.12 by equimolar ratio; ODA molecular weight: 200.24), and synthesizing polyamides acid (PAA), in its building-up process, to calculate first required 4,4'-diaminodiphenyl oxide (ODA) places reactor, and then the 90%-95% that add to calculate required pyromellitic acid anhydride (PMDA) total amount joins in the reactor with 4, and 4 '-diaminodiphenyl oxide (ODA) carries out building-up reactions, obtains polyamic acid (PAA); The heat conducting nano powder mixture need grind after mixing, makes diameter of particle reach D
90＜1um, in reacted polyamic acid, add according to the above ratio the heat conducting nano powder mixture after grinding, and then the pyromellitic acid anhydride of the remaining 5%-10% that not yet adds when adding building-up reactions, viscosity with control final reaction resultant reaches 90000 ± 5000CP, and then deaeration salivation film forming gets final product.
The optimal selection of the proportioning components of described heat conducting nano powder mixture is: Al
2O
330 parts, 40 parts of NB, AlN30 part.
With pyromellitic acid anhydride (PMDA) and 4, in the building-up process of 4 '-diaminodiphenyl oxide (ODA) synthesizing polyamides acid (PAA), also can adopt DMAC as the middle envrionment conditions of reaction.
Reach desirable heat conduction polyimide, key point is to select the suitable mineral powder with thermal conductivity, and need multiple mineral powder mixing use with thermal conductivity, its ratio cooperates the most key, and simultaneously total inorganics shared ratio in polyimide is also extremely important.
A kind of polyimide resin that obtains by method of the present invention, its advantage is: thermal conductivity reaches more than 3 times of common Kapton, the excellent electrical properties that is connected with, thermal characteristics and the mechanical property that not only have Kapton, as packaged material, can increase substantially the work-ing life of electronic component simultaneously.Can be widely used in poly-edge radiator element, heating circuit, energy source device (battery, sun power), ceramic radiating fin etc.
Embodiment
The present invention is further described below in conjunction with embodiment.
Embodiment 1:
The synthetic method of a kind of polyimide resin that present embodiment is described, described resin solid thing is by pyromellitic acid anhydride (PMDA) and 4, the resulting polyamic acid of 4 '-diaminodiphenyl oxide (ODA) building-up reactions (PAA), described heat conducting nano powder mixture is Al
2O
3The mixture of (aluminium sesquioxide), NB (boronation nitrogen) and three kinds of heat conducting nano powders of AlN (aluminium nitride), ratio is take listed as parts by weight as Al
2O
330 parts, NB40 part, AlN30 part, total amount be 1 ((part ratio mix, the heat conducting nano powder mixture accounts for 10% of resin solid thing total amount; When synthetic, at first to pyromellitic acid anhydride (PMDA) and 4,4 '-diaminodiphenyl oxide (ODA) calculates required separately reacting weight (wherein: PMDA: molecular weight 218.12 by equimolar ratio; ODA molecular weight: 200.24), and synthesizing polyamides acid (PAA), in its building-up process, to calculate first required 4,4'-diaminodiphenyl oxide (ODA) places reactor, and then add to calculate 90% of required pyromellitic acid anhydride (PMDA) total amount and join in the reactor with 4,4 '-diaminodiphenyl oxide (ODA) carries out building-up reactions, obtains polyamic acid (PAA); The heat conducting nano powder mixture need grind after mixing, makes diameter of particle reach D
90＜1um, in reacted polyamic acid, add according to the above ratio the heat conducting nano powder mixture after grinding, and then the pyromellitic acid anhydride of the remaining 5%-10% that not yet adds when adding building-up reactions, viscosity with control final reaction resultant reaches 90000 ± 5000CP, and then deaeration salivation film forming gets final product.After tested, reach performance index as shown in table 1 below.
Table 1:
Obtain polyimide resin by the present embodiment method, its advantage is: thermal conductivity reaches more than 3 times of common Kapton, the excellent electrical properties that is connected with, thermal characteristics and the mechanical property that not only have Kapton, as packaged material, can increase substantially the work-ing life of electronic component simultaneously.
Embodiment 2:
The synthetic method of a kind of polyimide resin that present embodiment provides, described heat conducting nano powder mixture is Al2O340%, NB50%, AlN60%, the heat conducting nano powder mixture accounts for 30% of resin solid thing total amount, in polyamic acid (PAA) building-up process, pyromellitic acid anhydride (PMDA) add-on is for calculating 95% of total amount.After tested, can reach performance index as shown in table 2 below:
Table 2:
Embodiment 3:
The synthetic method of a kind of polyimide resin that present embodiment provides, described heat conducting nano powder mixture is Al
2O
310%, NB20%, AlN20%, heat conducting nano powder mixture account for 20% of resin solid thing total amount, and in polyamic acid (PAA) building-up process, pyromellitic acid anhydride (PMDA) add-on reaches 93%.After tested, can reach performance index as shown in table 3 below.
Table 3:
Claims (2)
1. the synthetic method of a polyimide resin, comprise and adopt heat conducting nano powder mixture and resin solid thing, it is characterized in that described resin solid thing is by pyromellitic acid anhydride and 4, the resulting polyamic acid of 4'-diaminodiphenyl oxide building-up reactions, described heat conducting nano powder mixture is Al
2O
3, NB and three kinds of heat conducting nano powders of AlN mixture, the consisting of of its weight part: Al
2O
3: 10 parts-40 parts, NB:20 part-50 part, AlN:20 part-60 part, the heat conducting nano powder mixture accounts for the 10%-30% of resin solid thing total amount; When synthetic, at first to pyromellitic acid anhydride and 4, the 4'-diaminodiphenyl oxide calculates required separately reacting weight by equimolar ratio, and the synthetic polyamic acid that obtains, in its building-up process, will calculate first requiredly 4, the 4'-diaminodiphenyl oxide places reactor, and then the 90%-95% that add to calculate required pyromellitic acid anhydride total amount joins in the reactor and carries out building-up reactions with 4,4'-diaminodiphenyl oxide; The heat conducting nano powder mixture need grind after mixing, makes diameter of particle reach D
90＜1um, in reacted polyamic acid, add according to the above ratio the heat conducting nano powder mixture after grinding, and then the pyromellitic acid anhydride of the remaining 5%-10% that not yet adds when adding building-up reactions, viscosity with control final reaction resultant reaches 90000 ± 5000CP, and then deaeration salivation film forming gets final product.
2. the synthetic method of a kind of polyimide resin according to claim 1, the proportioning components that it is characterized in that described heat conducting nano powder mixture is Al
2O
330 parts, 40 parts of NB, AlN30 part.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2012103743064A CN102936341A (en) | 2012-09-27 | 2012-09-27 | Polyimide resin synthesis method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2012103743064A CN102936341A (en) | 2012-09-27 | 2012-09-27 | Polyimide resin synthesis method |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN102936341A true CN102936341A (en) | 2013-02-20 |
Family
ID=47695269
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2012103743064A Pending CN102936341A (en) | 2012-09-27 | 2012-09-27 | Polyimide resin synthesis method |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN102936341A (en) |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103923330A (en) * | 2014-04-30 | 2014-07-16 | 山东中天华德科技发展有限公司 | Method for preparing high-thermal conductivity polyimide/magnesium oxide composite film |
| CN105315664A (en) * | 2014-07-24 | 2016-02-10 | 中国石油化工股份有限公司 | Polyamide acid composition with controllable viscosity, and preparation method and applications thereof |
| CN105315462A (en) * | 2014-07-24 | 2016-02-10 | 中国石油化工股份有限公司 | Polyamide acid composition, and preparation method and applications thereof |
| CN106366334A (en) * | 2016-08-30 | 2017-02-01 | 宁波今山电子材料有限公司 | Preparation method of polyimide film with low dielectric constant and low dielectric loss factor |
| CN106832280A (en) * | 2017-02-27 | 2017-06-13 | 华烁科技股份有限公司 | A kind of thermoplasticity conducting liquid crystal Kapton and preparation method thereof |
| CN107400360A (en) * | 2017-06-28 | 2017-11-28 | 徐昌霞 | A kind of microelectronic device polyimides/aluminium nitride hybridized film and preparation method thereof |
| CN108117655A (en) * | 2016-11-30 | 2018-06-05 | 达胜科技股份有限公司 | Method for producing polyimide film, and polyimide film |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4590258A (en) * | 1983-12-30 | 1986-05-20 | International Business Machines Corporation | Polyamic acid copolymer system for improved semiconductor manufacturing |
| US5502156A (en) * | 1994-07-28 | 1996-03-26 | The United States Of America As Represented By The Administrator Of The National Aeronautics And Space Administration | Electrically conducting polyimide film containing tin complexes |
| CN101168598A (en) * | 2007-10-08 | 2008-04-30 | 江阴市云达电子新材料有限公司 | Method for preparing ultra-thick polyimide film with high heat conductivity and low thermal expansion coefficient |
| CN102020848A (en) * | 2009-09-17 | 2011-04-20 | 新扬科技股份有限公司 | Polyamide acid composition and application thereof |
-
2012
- 2012-09-27 CN CN2012103743064A patent/CN102936341A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4590258A (en) * | 1983-12-30 | 1986-05-20 | International Business Machines Corporation | Polyamic acid copolymer system for improved semiconductor manufacturing |
| US5502156A (en) * | 1994-07-28 | 1996-03-26 | The United States Of America As Represented By The Administrator Of The National Aeronautics And Space Administration | Electrically conducting polyimide film containing tin complexes |
| CN101168598A (en) * | 2007-10-08 | 2008-04-30 | 江阴市云达电子新材料有限公司 | Method for preparing ultra-thick polyimide film with high heat conductivity and low thermal expansion coefficient |
| CN102020848A (en) * | 2009-09-17 | 2011-04-20 | 新扬科技股份有限公司 | Polyamide acid composition and application thereof |
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103923330A (en) * | 2014-04-30 | 2014-07-16 | 山东中天华德科技发展有限公司 | Method for preparing high-thermal conductivity polyimide/magnesium oxide composite film |
| CN105315664A (en) * | 2014-07-24 | 2016-02-10 | 中国石油化工股份有限公司 | Polyamide acid composition with controllable viscosity, and preparation method and applications thereof |
| CN105315462A (en) * | 2014-07-24 | 2016-02-10 | 中国石油化工股份有限公司 | Polyamide acid composition, and preparation method and applications thereof |
| CN105315462B (en) * | 2014-07-24 | 2018-09-14 | 中国石油化工股份有限公司 | Polyamic acid composition and its preparation method and application |
| CN106366334A (en) * | 2016-08-30 | 2017-02-01 | 宁波今山电子材料有限公司 | Preparation method of polyimide film with low dielectric constant and low dielectric loss factor |
| CN106366334B (en) * | 2016-08-30 | 2021-08-10 | 宁波今山新材料有限公司 | Preparation method of polyimide film with low dielectric constant and low dielectric loss factor |
| CN108117655A (en) * | 2016-11-30 | 2018-06-05 | 达胜科技股份有限公司 | Method for producing polyimide film, and polyimide film |
| CN106832280A (en) * | 2017-02-27 | 2017-06-13 | 华烁科技股份有限公司 | A kind of thermoplasticity conducting liquid crystal Kapton and preparation method thereof |
| CN107400360A (en) * | 2017-06-28 | 2017-11-28 | 徐昌霞 | A kind of microelectronic device polyimides/aluminium nitride hybridized film and preparation method thereof |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102936341A (en) | Polyimide resin synthesis method | |
| CN105385106B (en) | A kind of preparation method of high heat conductivity insulation composite | |
| JP5723498B1 (en) | Polyimide resin composition and thermally conductive adhesive film using the same | |
| CN102948264B (en) | Circuit board use plywood and metallic substrates circuit substrate | |
| JP5707052B2 (en) | Resin composite composition and use thereof | |
| CN105575464B (en) | A kind of organic curing resistance slurry and preparation method thereof | |
| CN102977603B (en) | High temperature resistance high heat conduction PPS/PPO alloy and preparation method thereof | |
| CN103224705A (en) | Nano-modified polyimide composite film and preparation method thereof | |
| CN102702743A (en) | High-toughness high-heat-conduction epoxy-imine resin system and preparation method and application thereof | |
| CN102093665B (en) | Heat conduction insulating casting glue and preparation method thereof | |
| CN113337230B (en) | High-thermal-conductivity semi-cured adhesive film for metal substrate and preparation method thereof | |
| CN110776716A (en) | Epoxy plastic packaging material for high-thermal-conductivity and high-magnetic-induction packaging and preparation method and application thereof | |
| CN110862597A (en) | PE-BN-AlN electric insulation high thermal conductivity composite material and preparation method thereof | |
| CN105061764B (en) | A kind of thermoset polyimide resin and its composite laminate and their preparation method and application | |
| CN114644815B (en) | Lithium battery insulating film for new energy automobile and preparation method thereof | |
| Zhang et al. | Cyanate ester composites containing surface functionalized BN particles with grafted hyperpolyarylamide exhibiting desirable thermal conductivities and a low dielectric constant | |
| CN115044205B (en) | High-mechanical-strength heat-conducting polyimide film and preparation method thereof | |
| Kumar et al. | Thermal conductive epoxy adhesive composites filled with carbon-based particulate fillers: a comparative study | |
| CN103524995A (en) | Insulating plastic with high thermal conductivity | |
| Li et al. | Flexible and thermally conductive epoxy‐dispersed liquid crystal composites filled with functionalized boron nitride nanosheets | |
| JP2013040062A (en) | Hexagonal boron nitride powder, thermally conductive resin composition containing the same, and molded product obtained by the resin composition | |
| TWI558740B (en) | Thermal conductive resin and thermal interface material comprising the same | |
| CN115785864A (en) | PI-Al 2 O 3 Preparation method of PI-BN codoped high-thermal-conductivity epoxy resin composite material | |
| CN101921479B (en) | Cyanate resin base composite material and preparation method thereof | |
| JP5536723B2 (en) | Epoxy resin composition, molded body and sheet material |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C12 | Rejection of a patent application after its publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20130220 |