CN105085956A - Preparation method of black polyimide film with static electricity prevention and shielding functions - Google Patents
Preparation method of black polyimide film with static electricity prevention and shielding functions Download PDFInfo
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- CN105085956A CN105085956A CN201510564310.0A CN201510564310A CN105085956A CN 105085956 A CN105085956 A CN 105085956A CN 201510564310 A CN201510564310 A CN 201510564310A CN 105085956 A CN105085956 A CN 105085956A
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Abstract
The invention discloses a preparation method of a black polyimide film with static electricity prevention and shielding functions. The preparation method comprises steps as follows: an additive and polyamide acid are adopted, wherein the additive accounts for 0.5%-5% of polyamide acid in weight; the additive comprises nano-nickel powder, carbon black and a coupling agent, and nano-nickel powder accounts for 1%-8% of the total quantity of the additive; the carbon black accounts for 90%-98% of the total quantity of the additive; the coupling agent accounts for 1%-2% of the total quantity of the additive; polyamide acid is obtained from diamine and dianhydride through polycondensation in a solvent; during synthesizing, the nano-nickel powder, the carbon black and the coupling agent are dissolved in the solvent firstly, then respective required reacting weights of diamine and dianhydride are calculated in an equal molar ratio, polyamide acid is obtained through synthesis, and a product is obtained through defoaming and film casting. The product has the static electricity prevention effect, the volume resistivity of the product is 10<4>omega*cm-10<9>omega*cm, and meanwhile, the product has the excellent electromagnetic shielding effect and can be applied to the electronic fields such as a high-end flexible circuit board and the like.
Description
Technical field
The present invention relates to a kind of preparation method of Kapton, especially the preparation method of anti-electrostatic polyimide shielding black film, belongs to the antistatic film applications simultaneously with shield effectiveness.
Background technology
Kapton (PI film) is since the sixties in last century drops into application, and with the thermal characteristics of its excellence, dielectric properties and mechanical property etc. become the preferred material of the industrial circle such as electronics and space flight.Along with the development of electronic industry, more and more higher to polyimide characteristic requirements.
Due to the insulation characterisitic of commodity polymer material, in use unavoidably have electrostatic accumulation.Make troubles to life when electrostatic slightly gathers and inconvenience, and during severe accumulation, be not only just troublesome problem, sometimes even can cause casualties and the damage of equipment.Therefore the static hazard how eliminating macromolecular material is the important technology problem of people's constant quest for many years.Disclose in Chinese patent 20111002377.57 and add graphitized carbon black, antistatic polyimide film prepared by coupling agent, disclose in Chinese patent 201110265940.X and add carbon nanotube, polyaniline, antistatic polyimide film prepared by polyacrylic acid, 201410341743.5 disclose the antistatic polyimide film adding carbon graphite alkene and prepare, 20140421364.7 disclose one side painting graphene oxide to prepare the anlistatig Kapton of one side, simultaneously Chinese patent 20120277962.2 discloses the black polyamide thin film adding carbon black and coupling agent and prepare, these patents all serve the single premium properties such as antistatic black film, but effect in shielding is also not obvious, and anti-electrostatic has the polyimide black film of electromagnetic shielding action simultaneously, can be applied to and need the electronic applications such as the high-end flexible circuit board shielded to external electrical field is more responsive.
Summary of the invention
The object of the invention is in order to solve above-mentioned the deficiencies in the prior art provide a kind of can anti-electrostatic can play electromagnetic shielding action anti-electrostatic polyimide shielding black film preparation method.
To achieve these goals, the preparation method of the anti-electrostatic polyimide shielding black film designed by the present invention, comprise and adopt additive and polyamic acid, wherein additive accounts for the weight ratio in polyamic acid is 0.5% ~ 5%; Described additive is made up of nano-nickel powder, carbon black and coupling agent, and wherein nano-nickel powder accounts for 1% ~ 8% of additive total amount; Carbon black accounts for 90% ~ 98% of additive total amount; Coupling agent accounts for 1% ~ 2% of additive total amount, and the powder size diameter of nano-nickel powder is 0.15nm to 10nm simultaneously.
Described coupling agent is silane coupling agent, one or more specifically in γ-aminopropyl triethoxysilane, γ-(2,3 epoxy third oxygen) propyl trimethoxy silicane, γ-methacryloxypropyl trimethoxy silane, N-β-(aminoethyl)-γ-aminopropyltrimethoxysilane, N-β (aminoethyl)-γ-aminopropyl dimethoxy silane or vinyltrimethoxy silane.
Described polyamic acid is by the polycondensation and obtaining in a solvent of diamines and dianhydride, wherein said diamines is 4, one or more in 4-diaminodiphenyl oxide (ODA), Ursol D (PPD), 4,4-diaminodiphenyl-methanes (MDA);
Dianhydride is one or more in pyromellitic acid anhydride (PMDA), bibenzene tetracarboxylic dianhydride (BPDA), ketone acid anhydride (BTDA), diphenyl ether tetraformic dianhydride (ODPA);
Solvent is one or more in N,N-DIMETHYLACETAMIDE (DMAC), N-Methyl pyrrolidone (NMP), dimethyl formamide (DMF);
During synthesis, first these three kinds of additives of nano-nickel powder, carbon black and coupling agent are dissolved in a solvent, then diamines and dianhydride are calculated reacting weight required separately by equimolar ratio, synthesis obtains polyamic acid, in its building-up process, first the diamines needed for calculating is put into reactor, and by dissolution with solvents, and then add calculate needed for dianhydride 99% in reactor; The dianhydride of the remainder 1% not yet added when finally adding building-up reactions, reaches 90000 ± 5000CP with the viscosity controlling final reaction resultant, then deaeration casting film-forming.
By a kind of anti-electrostatic polyimide shielding black film that preparation method of the present invention obtains, its advantage is the common effect in conjunction with metal nano nickel powder and graphitized carbon black, nano-nickel powder mainly plays the anti-static effect of electromagnetic shielding action and part, carbon black plays anti-static effect and painted effect, realize the effect of anti-electrostatic black film, coupling agent mainly plays and promotes dispersion, the effect that stabilization process is produced, the Kapton of final preparation not only has the effect of anti-electrostatic, and its volume specific resistance is 10
4Ω cm ~ 10
9Ω cm, has good effectiveness simultaneously, and its effectiveness of shielding adopts coaxial method of testing to be measured as 40dB ~ 45dB, can be applied to the electronic applications such as high-end flexible circuit board.
Embodiment
Below in conjunction with embodiment, the present invention is further described.
Embodiment 1:
The preparation method of a kind of anti-electrostatic polyimide shielding black film that the present embodiment provides, comprise and adopt additive and polyamic acid, wherein additive accounts for the weight ratio in polyamic acid is 0.5%; Described additive is made up of nano-nickel powder, carbon black and coupling agent, and wherein the ratio of nano-nickel powder, carbon black, coupling agent three kinds of additives is 2%:97%:1%.Described coupling agent is γ-aminopropyl triethoxysilane, and described polyamic acid is by the polycondensation and obtaining in N,N-DIMETHYLACETAMIDE of 4,4-diaminodiphenyl oxide and pyromellitic acid anhydride.
During synthesis, first nano-nickel powder, carbon black, coupling agent three kinds of additives are dispersed in organic solvent N,N-DIMETHYLACETAMIDE, then by 4,4-diaminodiphenyl oxide and pyromellitic acid anhydride calculate reacting weight required separately by equimolar ratio, and synthesis obtains polyamic acid, in its building-up process, first by 4 needed for calculating, 4-diaminodiphenyl oxide puts into reactor, and uses dimethylacetamide amine solvent, and then add calculate required pyromellitic acid anhydride 99% in reactor; The pyromellitic acid anhydride of the remainder 1% not yet added when finally adding building-up reactions, reaches 90000 ± 5000CP with the viscosity controlling final reaction resultant, then deaeration casting film-forming.
The volume specific resistance of the anti-electrostatic polyimide shielding black film of the present embodiment gained is 10
8Ω cm, its effectiveness of shielding adopts coaxial method of testing to be measured as 45dB.
Embodiment 2:
The preparation method of a kind of anti-electrostatic polyimide shielding black film that the present embodiment provides, comprise and adopt additive and polyamic acid, wherein additive accounts for the weight ratio in polyamic acid is 2%; Described additive is made up of nano-nickel powder, carbon black and coupling agent, and wherein the ratio of nano-nickel powder, carbon black, coupling agent three kinds of additives is 2%:97%:1%.Described coupling agent is γ-methacryloxypropyl trimethoxy silane, and described polyamic acid is by the polycondensation and obtaining in N,N-DIMETHYLACETAMIDE of Ursol D and pyromellitic acid anhydride.
Synthetic method is identical with embodiment 1, and the volume specific resistance of the anti-electrostatic polyimide shielding black film of the present embodiment gained is 10
7Ω cm, its effectiveness of shielding adopts coaxial method of testing to be measured as 43dB.
Embodiment 3:
The preparation method of a kind of anti-electrostatic polyimide shielding black film that the present embodiment provides, comprise and adopt additive and polyamic acid, wherein additive accounts for the weight ratio in polyamic acid is 5%; Described additive is made up of nano-nickel powder, carbon black and coupling agent, and wherein the ratio of nano-nickel powder, carbon black, coupling agent three kinds of additives is 2%:97%:1%.Described coupling agent is γ-aminopropyl triethoxysilane, and described polyamic acid is by the polycondensation and obtaining in N-Methyl pyrrolidone of 4,4-diaminodiphenyl oxide and diphenyl ether tetraformic dianhydride.
Synthetic method is identical with embodiment 1, and the volume specific resistance of the anti-electrostatic polyimide shielding black film of the present embodiment gained is 10
6Ω cm, its effectiveness of shielding adopts coaxial method of testing to be measured as 40dB.
Embodiment 4:
The preparation method of a kind of anti-electrostatic polyimide shielding black film that the present embodiment provides, comprise and adopt additive and polyamic acid, wherein additive accounts for the weight ratio in polyamic acid is 4%; Described additive is made up of nano-nickel powder, carbon black and coupling agent, and wherein the ratio of nano-nickel powder, carbon black, coupling agent three kinds of additives is 1%:97%:2%.Described coupling agent is N-β-(aminoethyl)-γ-aminopropyltrimethoxysilane, and described polyamic acid is by the polycondensation and obtaining in dimethyl formamide of 4,4-diaminodiphenyl-methane and ketone acid anhydride.
Synthetic method is identical with embodiment 1, and the volume specific resistance of the anti-electrostatic polyimide shielding black film of the present embodiment gained is 10
5Ω cm, its effectiveness of shielding adopts coaxial method of testing to be measured as 45dB.
Embodiment 5:
The preparation method of a kind of anti-electrostatic polyimide shielding black film that the present embodiment provides, comprise and adopt additive and polyamic acid, wherein additive accounts for the weight ratio in polyamic acid is 2%; Described additive is made up of nano-nickel powder, carbon black and coupling agent, and wherein the ratio of nano-nickel powder, carbon black, coupling agent three kinds of additives is 3%:95%:2%.Described coupling agent is γ-aminopropyl triethoxysilane, and described polyamic acid is by the polycondensation and obtaining in N,N-DIMETHYLACETAMIDE of 4,4-diaminodiphenyl oxide and diphenyl ether tetraformic dianhydride.
Synthetic method is identical with embodiment 1, and the volume specific resistance of the anti-electrostatic polyimide shielding black film of the present embodiment gained is 10
4Ω cm, its effectiveness of shielding adopts coaxial method of testing to be measured as 42dB.
Embodiment 6:
The preparation method of a kind of anti-electrostatic polyimide shielding black film that the present embodiment provides, comprise and adopt additive and polyamic acid, wherein additive accounts for the weight ratio in polyamic acid is 3%; Described additive is made up of nano-nickel powder, carbon black and coupling agent, and wherein the ratio of nano-nickel powder, carbon black, coupling agent three kinds of additives is 1%:98%:1%.Described coupling agent is γ-aminopropyl triethoxysilane, and described polyamic acid is by the polycondensation and obtaining in N-Methyl pyrrolidone of 4,4-diaminodiphenyl oxide and ketone acid anhydride.
Synthetic method is identical with embodiment 1, and the volume specific resistance of the anti-electrostatic polyimide shielding black film of the present embodiment gained is 10
9Ω cm, its effectiveness of shielding adopts coaxial method of testing to be measured as 45dB.
Claims (3)
1. a preparation method for anti-electrostatic polyimide shielding black film, is characterized in that: comprise and adopt additive and polyamic acid, wherein additive accounts for the weight ratio in polyamic acid is 0.5% ~ 5%;
Described additive is made up of nano-nickel powder, carbon black and coupling agent, and wherein nano-nickel powder accounts for 1% ~ 8% of additive total amount; Carbon black accounts for 90% ~ 98% of additive total amount; Coupling agent accounts for 1% ~ 2% of additive total amount;
Described polyamic acid is by the polycondensation and obtaining in a solvent of diamines and dianhydride, wherein said diamines is 4,4-diaminodiphenyl oxide, Ursol D, 4, one or more in 4-diaminodiphenyl-methane, dianhydride is one or more in pyromellitic acid anhydride, bibenzene tetracarboxylic dianhydride, ketone acid anhydride, diphenyl ether tetraformic dianhydride, and solvent is one or more in N,N-DIMETHYLACETAMIDE, N-Methyl pyrrolidone, dimethyl formamide;
During synthesis, first these three kinds of additives of nano-nickel powder, carbon black and coupling agent are dissolved in a solvent, then diamines and dianhydride are calculated reacting weight required separately by equimolar ratio, synthesis obtains polyamic acid, in its building-up process, first the diamines needed for calculating is put into reactor, and by dissolution with solvents, and then add calculate needed for dianhydride 99% in reactor; The dianhydride of the remainder 1% not yet added when finally adding building-up reactions, reaches 90000 ± 5000CP with the viscosity controlling final reaction resultant, then deaeration casting film-forming.
2. the preparation method of anti-electrostatic polyimide shielding black film according to claim 1, is characterized in that the powder size diameter of described nano-nickel powder is 0.15nm to 10nm.
3. the preparation method of anti-electrostatic polyimide shielding black film according to claim 1 and 2, it is characterized in that described coupling agent is silane coupling agent, one or more specifically in γ-aminopropyl triethoxysilane, γ-(2,3 epoxy third oxygen) propyl trimethoxy silicane, γ-methacryloxypropyl trimethoxy silane, N-β-(aminoethyl)-γ-aminopropyltrimethoxysilane, N-β (aminoethyl)-γ-aminopropyl dimethoxy silane or vinyltrimethoxy silane.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105491788A (en) * | 2016-01-14 | 2016-04-13 | 苏州城邦达力材料科技有限公司 | Graphene heat radiation type shielding film and preparation method thereof |
| CN108239398A (en) * | 2016-12-23 | 2018-07-03 | 财团法人纺织产业综合研究所 | Plastic composition and preparation method thereof is with using the optical element made by it |
| CN109437905A (en) * | 2018-11-27 | 2019-03-08 | 宁波今山新材料有限公司 | A kind of preparation method of tear-resistant graphite film |
| CN110358295A (en) * | 2019-08-22 | 2019-10-22 | 深圳先进技术研究院 | It is a kind of with electromagnetic shielding and the polyimide composite film of thermally conductive function and preparation method thereof |
| CN111566151A (en) * | 2018-01-16 | 2020-08-21 | 韩国爱思开希可隆Pi股份有限公司 | Black polyimide film and preparation method thereof |
| CN113045898A (en) * | 2021-03-25 | 2021-06-29 | 广东工业大学 | Composite polyimide film and preparation method thereof |
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| CN101074291A (en) * | 2007-05-31 | 2007-11-21 | 上海市合成树脂研究所 | Production of black polyamide thin film |
| CN102120826A (en) * | 2011-01-21 | 2011-07-13 | 南京工业大学 | Preparation method of antistatic polyimide film |
| CN103725000A (en) * | 2013-12-26 | 2014-04-16 | 北京工商大学 | High-temperature polymer-based electromagnetic shielding functionally gradient material |
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2015
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| CN101074291A (en) * | 2007-05-31 | 2007-11-21 | 上海市合成树脂研究所 | Production of black polyamide thin film |
| CN102120826A (en) * | 2011-01-21 | 2011-07-13 | 南京工业大学 | Preparation method of antistatic polyimide film |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105491788A (en) * | 2016-01-14 | 2016-04-13 | 苏州城邦达力材料科技有限公司 | Graphene heat radiation type shielding film and preparation method thereof |
| CN105491788B (en) * | 2016-01-14 | 2019-02-19 | 苏州城邦达力材料科技有限公司 | A kind of graphene heat radiating type screened film and preparation method thereof |
| CN108239398A (en) * | 2016-12-23 | 2018-07-03 | 财团法人纺织产业综合研究所 | Plastic composition and preparation method thereof is with using the optical element made by it |
| CN108239398B (en) * | 2016-12-23 | 2021-02-26 | 财团法人纺织产业综合研究所 | Method for producing optical element |
| CN111566151A (en) * | 2018-01-16 | 2020-08-21 | 韩国爱思开希可隆Pi股份有限公司 | Black polyimide film and preparation method thereof |
| CN111566151B (en) * | 2018-01-16 | 2022-11-25 | 韩国爱思开希可隆Pi股份有限公司 | Black polyimide film and preparation method thereof |
| CN109437905A (en) * | 2018-11-27 | 2019-03-08 | 宁波今山新材料有限公司 | A kind of preparation method of tear-resistant graphite film |
| CN109437905B (en) * | 2018-11-27 | 2021-08-17 | 宁波今山新材料有限公司 | Preparation method of tear-resistant graphite film |
| CN110358295A (en) * | 2019-08-22 | 2019-10-22 | 深圳先进技术研究院 | It is a kind of with electromagnetic shielding and the polyimide composite film of thermally conductive function and preparation method thereof |
| CN113045898A (en) * | 2021-03-25 | 2021-06-29 | 广东工业大学 | Composite polyimide film and preparation method thereof |
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| CN105085956B (en) | 2018-01-30 |
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Effective date of registration: 20211123 Address after: 315176 88 Kesheng Road, jishigang Town, Haishu District, Ningbo City, Zhejiang Province Patentee after: NINGBO JINSHAN NEW MATERIAL Co.,Ltd. Address before: 315217 plant 4, qianqianchen Industrial Park, Yunlong Town, Yinzhou District, Ningbo City, Zhejiang Province (Ningbo Jinshan Electronic Materials Co., Ltd.) Patentee before: NINGBO CEN ELECTRONIC MATERIAL CO.,LTD. |