CN112111077A - Polyimide black film with high insulation strength and high blackness and preparation method thereof - Google Patents
Polyimide black film with high insulation strength and high blackness and preparation method thereof Download PDFInfo
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- CN112111077A CN112111077A CN202010864598.4A CN202010864598A CN112111077A CN 112111077 A CN112111077 A CN 112111077A CN 202010864598 A CN202010864598 A CN 202010864598A CN 112111077 A CN112111077 A CN 112111077A
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- 229920001721 polyimide Polymers 0.000 title claims abstract description 35
- 239000004642 Polyimide Substances 0.000 title claims abstract description 22
- 238000009413 insulation Methods 0.000 title claims abstract description 17
- 238000002360 preparation method Methods 0.000 title abstract description 8
- 239000000975 dye Substances 0.000 claims abstract description 66
- 239000002904 solvent Substances 0.000 claims abstract description 25
- 239000000178 monomer Substances 0.000 claims abstract description 22
- GTDPSWPPOUPBNX-UHFFFAOYSA-N ac1mqpva Chemical compound CC12C(=O)OC(=O)C1(C)C1(C)C2(C)C(=O)OC1=O GTDPSWPPOUPBNX-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000001045 blue dye Substances 0.000 claims abstract description 12
- 150000004985 diamines Chemical class 0.000 claims abstract description 12
- 239000001044 red dye Substances 0.000 claims abstract description 12
- 239000001043 yellow dye Substances 0.000 claims abstract description 12
- AJDUTMFFZHIJEM-UHFFFAOYSA-N n-(9,10-dioxoanthracen-1-yl)-4-[4-[[4-[4-[(9,10-dioxoanthracen-1-yl)carbamoyl]phenyl]phenyl]diazenyl]phenyl]benzamide Chemical compound O=C1C2=CC=CC=C2C(=O)C2=C1C=CC=C2NC(=O)C(C=C1)=CC=C1C(C=C1)=CC=C1N=NC(C=C1)=CC=C1C(C=C1)=CC=C1C(=O)NC1=CC=CC2=C1C(=O)C1=CC=CC=C1C2=O AJDUTMFFZHIJEM-UHFFFAOYSA-N 0.000 claims abstract description 11
- 239000002994 raw material Substances 0.000 claims abstract description 3
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 claims description 15
- 239000011324 bead Substances 0.000 claims description 15
- 229910052726 zirconium Inorganic materials 0.000 claims description 15
- 229920005575 poly(amic acid) Polymers 0.000 claims description 14
- 238000000034 method Methods 0.000 claims description 11
- 238000010008 shearing Methods 0.000 claims description 10
- 239000000010 aprotic solvent Substances 0.000 claims description 8
- 238000000227 grinding Methods 0.000 claims description 8
- VLDPXPPHXDGHEW-UHFFFAOYSA-N 1-chloro-2-dichlorophosphoryloxybenzene Chemical compound ClC1=CC=CC=C1OP(Cl)(Cl)=O VLDPXPPHXDGHEW-UHFFFAOYSA-N 0.000 claims description 7
- CBCKQZAAMUWICA-UHFFFAOYSA-N 1,4-phenylenediamine Chemical compound NC1=CC=C(N)C=C1 CBCKQZAAMUWICA-UHFFFAOYSA-N 0.000 claims description 6
- FXHOOIRPVKKKFG-UHFFFAOYSA-N N,N-Dimethylacetamide Chemical compound CN(C)C(C)=O FXHOOIRPVKKKFG-UHFFFAOYSA-N 0.000 claims description 6
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 6
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 6
- 238000002156 mixing Methods 0.000 claims description 6
- 239000011248 coating agent Substances 0.000 claims description 4
- 238000000576 coating method Methods 0.000 claims description 4
- 238000001816 cooling Methods 0.000 claims description 4
- ZUOUZKKEUPVFJK-UHFFFAOYSA-N diphenyl Chemical compound C1=CC=CC=C1C1=CC=CC=C1 ZUOUZKKEUPVFJK-UHFFFAOYSA-N 0.000 claims description 4
- 238000001914 filtration Methods 0.000 claims description 4
- 239000000758 substrate Substances 0.000 claims description 3
- VQVIHDPBMFABCQ-UHFFFAOYSA-N 5-(1,3-dioxo-2-benzofuran-5-carbonyl)-2-benzofuran-1,3-dione Chemical compound C1=C2C(=O)OC(=O)C2=CC(C(C=2C=C3C(=O)OC(=O)C3=CC=2)=O)=C1 VQVIHDPBMFABCQ-UHFFFAOYSA-N 0.000 claims description 2
- 235000010290 biphenyl Nutrition 0.000 claims description 2
- 239000004305 biphenyl Substances 0.000 claims description 2
- YMHQVDAATAEZLO-UHFFFAOYSA-N cyclohexane-1,1-diamine Chemical compound NC1(N)CCCCC1 YMHQVDAATAEZLO-UHFFFAOYSA-N 0.000 claims description 2
- 239000011261 inert gas Substances 0.000 claims description 2
- NTNWKDHZTDQSST-UHFFFAOYSA-N naphthalene-1,2-diamine Chemical compound C1=CC=CC2=C(N)C(N)=CC=C21 NTNWKDHZTDQSST-UHFFFAOYSA-N 0.000 claims description 2
- 239000007787 solid Substances 0.000 claims description 2
- 239000010408 film Substances 0.000 description 35
- 239000000243 solution Substances 0.000 description 15
- 239000006229 carbon black Substances 0.000 description 12
- 230000000052 comparative effect Effects 0.000 description 6
- 239000000843 powder Substances 0.000 description 6
- 229910000831 Steel Inorganic materials 0.000 description 5
- 239000003292 glue Substances 0.000 description 5
- 239000002245 particle Substances 0.000 description 5
- 239000010959 steel Substances 0.000 description 5
- 238000002834 transmittance Methods 0.000 description 5
- 239000004677 Nylon Substances 0.000 description 4
- 239000006185 dispersion Substances 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 229920001778 nylon Polymers 0.000 description 4
- 238000004321 preservation Methods 0.000 description 4
- 238000003756 stirring Methods 0.000 description 4
- 238000012360 testing method Methods 0.000 description 3
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 2
- 230000007423 decrease Effects 0.000 description 2
- ZHDTXTDHBRADLM-UHFFFAOYSA-N hydron;2,3,4,5-tetrahydropyridin-6-amine;chloride Chemical compound Cl.NC1=NCCCC1 ZHDTXTDHBRADLM-UHFFFAOYSA-N 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 238000007790 scraping Methods 0.000 description 2
- 239000013039 cover film Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000004043 dyeing Methods 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 238000001746 injection moulding Methods 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/18—Manufacture of films or sheets
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G73/00—Macromolecular compounds obtained by reactions forming a linkage containing nitrogen with or without oxygen or carbon in the main chain of the macromolecule, not provided for in groups C08G12/00 - C08G71/00
- C08G73/06—Polycondensates having nitrogen-containing heterocyclic rings in the main chain of the macromolecule
- C08G73/10—Polyimides; Polyester-imides; Polyamide-imides; Polyamide acids or similar polyimide precursors
- C08G73/1042—Copolyimides derived from at least two different tetracarboxylic compounds or two different diamino compounds
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G73/00—Macromolecular compounds obtained by reactions forming a linkage containing nitrogen with or without oxygen or carbon in the main chain of the macromolecule, not provided for in groups C08G12/00 - C08G71/00
- C08G73/06—Polycondensates having nitrogen-containing heterocyclic rings in the main chain of the macromolecule
- C08G73/10—Polyimides; Polyester-imides; Polyamide-imides; Polyamide acids or similar polyimide precursors
- C08G73/1067—Wholly aromatic polyimides, i.e. having both tetracarboxylic and diamino moieties aromatically bound
- C08G73/1071—Wholly aromatic polyimides containing oxygen in the form of ether bonds in the main chain
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2379/00—Characterised by the use of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing nitrogen with or without oxygen, or carbon only, not provided for in groups C08J2361/00 - C08J2377/00
- C08J2379/04—Polycondensates having nitrogen-containing heterocyclic rings in the main chain; Polyhydrazides; Polyamide acids or similar polyimide precursors
- C08J2379/08—Polyimides; Polyester-imides; Polyamide-imides; Polyamide acids or similar polyimide precursors
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
Abstract
The invention discloses a polyimide black film with high insulation strength and high blackness, which comprises the following raw materials: the high-temperature resistant solvent type organic dye comprises a high-temperature resistant solvent type organic dye, a diamine monomer and a dianhydride monomer, wherein the weight of the high-temperature resistant solvent type organic dye is 0.5-2% of the total weight of the diamine monomer and the dianhydride monomer, and the high-temperature resistant solvent type organic dye is blue dye, red dye and yellow dye. The invention also discloses a preparation method of the polyimide black film with high insulation strength and high blackness. The invention has high insulating strength, high blackness and good shielding property.
Description
Technical Field
The invention relates to the technical field of polyimide, in particular to a polyimide black film with high insulation strength and high blackness and a preparation method thereof.
Background
Polyimide films are widely used in the fields of electronic and electrical products, aerospace and the like because of their excellent heat resistance, insulation, dimensional stability and the like, and are called gold films. The black polyimide film derived therefrom is also widely used, for example, as a black cover film, a black tape, a black light-shielding sheet, etc. Compared with the common polyimide film, the black polyimide film has the characteristics of opacity and good confidentiality.
However, the black polyimide film in the current market is basically dyed by carbon black, and the carbon black has the advantages of low cost, good dyeing property and convenient operation. However, since the conductivity of carbon black is very good, the insulation strength of the polyimide black film prepared by using the carbon black is much lower than that of the common polyimide film, and the use requirements of high-end customers cannot be met. Meanwhile, the dispersion of the carbon black is difficult, and part of the carbon black which is not dispersed or aggregated after dispersion forms large particles, so that black particles and holes are formed on the film surface, and the quality and the yield of the film are seriously influenced.
Disclosure of Invention
Based on the technical problems in the background art, the invention provides the polyimide black film with high insulating strength and high blackness and the preparation method thereof.
The invention provides a polyimide black film with high insulation strength and high blackness, which comprises the following raw materials: the high-temperature resistant solvent type organic dye comprises a high-temperature resistant solvent type organic dye, a diamine monomer and a dianhydride monomer, wherein the weight of the high-temperature resistant solvent type organic dye is 0.5-2% of the total weight of the diamine monomer and the dianhydride monomer, and the high-temperature resistant solvent type organic dye is blue dye, red dye and yellow dye.
Preferably, the high-temperature solvent-resistant organic dye has stable performance at the temperature of 250-350 ℃.
The high-temperature resistant solvent type organic dye is not easy to decompose at the temperature of 250-350 ℃, stays in an injection molding machine at the temperature of 300 ℃ for 5min, and has no light color and higher color retention rate after being extruded.
Preferably, the blue dye is at least one of dye RR blue, dye 3R blue, dye AP blue, dye 2B blue.
Preferably, the red dye is at least one of dye H5B red, dye E2G red, dye HFG red, dye GK red, dye 2BP high temperature red.
Preferably, the yellow dye is at least one of dye 114 yellow, dye 8GF yellow, dye 3GL yellow.
The above blue, red and yellow dyes are commercially available.
Preferably, the content of the blue dye, the content of the red dye and the content of the yellow dye in the high-temperature solvent-resistant organic dye are respectively 70-80%, 15-20% and 0-15%.
The specific ratio of the blue dye, the red dye and the yellow dye in the high temperature solvent resistant organic dye can be adjusted according to the required color of the polyimide, such as: in the yellow polyimide with higher p-Phenylenediamine (PDA) content, the proportion of the yellow dye can be properly reduced or even not added, and the proportion of the blue dye and the red dye is properly increased to obtain the required blackness.
Preferably, the diamine monomer is at least one of p-phenylenediamine, 4-diaminodiphenyl ether, cyclohexanediamine and naphthalenediamine.
Preferably, the dianhydride monomer is at least one of pyromellitic dianhydride, biphenyl dianhydride, and benzophenone tetracarboxylic dianhydride.
The invention also provides a preparation method of the polyimide black film with high insulation strength and high blackness, which comprises the following steps:
s1, mixing a blue dye, a red dye, a yellow dye and an aprotic solvent, then shearing and dispersing, adding zirconium beads for grinding, and filtering the zirconium beads to obtain a color paste;
s2, adding color paste into an aprotic solvent in which a diamine monomer is dissolved in an inert gas range, uniformly mixing, and adding a dianhydride monomer for reaction to obtain a polyamic acid solution; and defoaming the polyamic acid solution, coating the defoamed polyamic acid solution on the surface of the substrate, removing the solvent and imidizing, cooling and stripping to obtain the polyimide black film with high insulating strength and high blackness.
Preferably, in S1, the color paste has a solid content of 5-20%.
Preferably, in S1, the material is dispersed by shearing at 2800 and 3200r/min for 0.4-0.6h, and then the material is ground by adding zirconium beads for 2-3 h.
Preferably, in S1, the weight ratio of the zirconium beads to the color paste is 1: 0.8-1.2.
Preferably, in S1, the zirconium beads have a diameter of 0.2 to 0.4 mm.
Preferably, in S1 and S2, the aprotic solvent is at least one of N, N-dimethylformamide, N-dimethylacetamide, and toluene.
Preferably, in S2, the weight ratio of the diamine monomer to the aprotic solvent is 1:9 to 11.
Preferably, in S2, the polyamic acid solution has a viscosity of 100-200 PaS.
Preferably, in S2, the procedure for solvent removal and imidization is: keeping the temperature at 160 ℃ for 3-5min at 140-; keeping the temperature at 280-300 ℃ for 2-3 min; finally, the temperature is maintained for 1-2min at 350 ℃ of 330-.
Has the advantages that:
the invention uses three high temperature resistant solvent organic dyes of blue, red and yellow to replace carbon black, which can greatly improve the insulation strength of the film while ensuring the blackness of the film. The black is modulated by using three high-temperature resistant solvent-based organic dyes of blue, red and yellow, and the film has the characteristics of high temperature resistance and fastness compared with other organic black dyes, can be properly adjusted according to the color change of a film substrate, so that the color fluctuation of a finished film is smaller, the problem that the black organic dye is easily decomposed at high temperature during imidization when the black organic dye is directly used can be avoided, and the problem that the polyimide film cannot reach the required color or blackness is avoided. The organic dye can be dissolved in the solvent, so that the dispersibility of the organic dye is better than that of carbon black, the generation of film surface defects is reduced, and the yield is improved; and the zirconium beads are used for grinding, so that the particles of the dye can be smaller, the dye can be more easily dissolved in the solvent, various dyes are uniformly mixed, and the yield is further improved. The invention has high insulating strength, high blackness and good shielding property, and can be suitable for black covering films and black anti-shielding materials with high insulating requirements.
Detailed Description
The technical solution of the present invention will be described in detail below with reference to specific examples.
Example 1
A preparation method of a polyimide black film with high insulation strength and high blackness comprises the following steps:
s1, mixing 7.5g of dye RR blue powder, 1.5g of dye H5B red powder, 1g of dye 114 yellow powder and 90g N, N-dimethylacetamide, then shearing and dispersing for 0.5H on a high-speed shearing dispersion machine by using a shearing disc at the speed of 1500r/min, then adding 100g of zirconium beads (the particle size is 0.3mm), grinding for 3H at the speed of 3000r/min by replacing a nylon grinding disc, and filtering the zirconium beads by using a 300-mesh nylon filter screen to obtain a color paste;
s2, in a 500mL three-hole flask, 20.0g of 4, 4-diaminodiphenyl ether (ODA) and 200g N, N-dimethylacetamide were added, and N was purged2Stirring for 0.5h, after the ODA is completely dissolved, adding 4.1g of color paste into the solution, and stirring uniformly; then adding pyromellitic dianhydride (PMDA) for three times, wherein the total mass of the PMDA is 21 g; adding 7.0g of the mixture every time, and adding the mixture once every 0.5 h; carrying out reaction and testing the viscosity, and obtaining the polyamic acid solution when the viscosity is 100-200 PaS;
placing the polyamic acid solution into a vacuum oven for defoaming, then uniformly coating the polyamic acid solution on a mirror steel plate, adjusting the distance between scrapers to be 75 mu m, scraping out a glue film, sequentially placing the glue film steel plate into an oven at 150 ℃ for heat preservation for 4min, and placing the oven at 210 ℃ for heat preservation for 4 min; keeping the temperature of a 280 ℃ oven for 2 min; keeping the temperature of an oven at 340 ℃ for 1 min; taking out, cooling and stripping the film to obtain the polyimide black film with high insulation strength and high blackness, the thickness of which is about 15 mu m.
Example 2
A preparation method of a polyimide black film with high insulation strength and high blackness comprises the following steps:
s1, mixing 8g of dye 3R blue, 1.7g of dye 2BP high-temperature red, 0.3g of dye 114 yellow powder and 90g N, N-dimethylacetamide, then shearing and dispersing for 0.5h on a high-speed shearing dispersion machine by using a shearing disc at the speed of 1500R/min, then adding 100g of zirconium beads (the particle size is 0.3mm), grinding for 3h by replacing a nylon grinding disc at the speed of 3000R/min, and filtering the zirconium beads by using a 300-mesh nylon filter screen to obtain color paste;
s2, in a 500mL three-hole flask, 15g of 4, 4-diaminodiphenyl ether (ODA), 5g of p-Phenylenediamine (PDA) and 200g N, N-dimethylacetamide were added, and N was passed through2Stirring for 0.5h, adding 4.6g of color paste into the solution after the solution is completely dissolved, and uniformly stirring; then adding pyromellitic dianhydride (PMDA) for three times, wherein the total mass of the PMDA26.1 g; adding 8.7g each time, and adding once every 0.5 h; carrying out reaction and testing the viscosity, and obtaining the polyamic acid solution when the viscosity is 100-200 PaS;
placing the polyamic acid solution into a vacuum oven for defoaming, then uniformly coating the polyamic acid solution on a mirror steel plate, adjusting the distance between scrapers to be 75 mu m, scraping out a glue film, sequentially placing the glue film steel plate into a 160 ℃ oven for heat preservation for 4min, and placing the glue film steel plate into a 200 ℃ oven for heat preservation for 4 min; keeping the temperature of an oven at 290 ℃ for 2 min; keeping the temperature of a baking oven at 350 ℃ for 1 min; taking out, cooling and stripping the film to obtain the polyimide black film with high insulation strength and high blackness, the thickness of which is about 15 mu m.
Comparative example 1
The procedure of example 1 was repeated except that "7.5 g of RR blue powder as a dye, 1.5g of red powder as a dye H5B, and 1g of yellow powder as a dye" were replaced with 10g of carbon black.
Comparative example 2
The procedure of example 2 was repeated except that "8 g of dye 3R blue, 1.7g of dye 2BP high-temperature Red, and 0.3g of dye 114 yellow powder" were replaced with 10g of carbon black.
Blank example 1
The procedure of S2 in example 1 was repeated except that no color paste was added.
Blank example 2
The procedure of example 2 was repeated except that no color paste was added, i.e., S2.
Taking the films prepared in the examples 1-2, the comparative examples 1-2 and the blank examples 1-2, and detecting the insulating strength, the L value and the light transmittance of the films, wherein the light transmittance of the materials is tested according to GB/T2410-2008; GB/T1354.2-2009 test insulation strength; the L value was measured using a color difference meter and the results are shown in the following table:
| detection ofItem | Example 1 | Example 2 | Comparative example 1 | Comparative example 2 | Blank example 1 | Blank example 2 |
| Value of L | 12.64 | 9.36 | 12.31 | 8.79 | 64.63 | 56.37 |
| Dielectric strength (V/. mu.m) | 198 | 211 | 64 | 78 | 237 | 246 |
| Light transmittance% | 0.98 | 0.69 | 0.87 | 0.53 | 68 | 57 |
From the data of examples 1, 2 and comparative examples 1, 2 it can be seen that: the L value and the light transmittance of the black film prepared by using the three high-temperature resistant organic dyes are very close to those of the black film prepared by using the carbon black; but the dielectric strength is much higher than that of the black film prepared from carbon black.
From a comparison of examples 1, 2 and blanks 1, 2, it can be seen that: the addition of the organic dye slightly decreases the dielectric strength of the non-film, but greatly decreases the L value and light transmittance of the film.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the technical scope of the present invention, and the technical solutions and the inventive concepts thereof according to the present invention should be equivalent or changed within the scope of the present invention.
Claims (10)
1. The utility model provides a high dielectric strength high blackness polyimide black film which characterized in that, its raw materials include: the high-temperature resistant solvent type organic dye comprises a high-temperature resistant solvent type organic dye, a diamine monomer and a dianhydride monomer, wherein the weight of the high-temperature resistant solvent type organic dye is 0.5-2% of the total weight of the diamine monomer and the dianhydride monomer, and the high-temperature resistant solvent type organic dye is blue dye, red dye and yellow dye.
2. The black polyimide film with high insulation strength and high blackness as claimed in claim 1, wherein the high temperature solvent organic dye has stable performance at the temperature of 250 ℃ to 350 ℃; preferably, the blue dye is at least one of dye RR blue, dye 3R blue, dye AP blue, dye 2B blue; preferably, the red dye is at least one of dye H5B red, dye E2G red, dye HFG red, dye GK red, dye 2BP high temperature red; preferably, the yellow dye is at least one of dye 114 yellow, dye 8GF yellow, dye 3GL yellow.
3. The black polyimide film with high insulation strength and high blackness as claimed in claim 1 or 2, wherein the content of the blue dye, the content of the red dye and the content of the yellow dye in the solvent-type organic dye with high temperature resistance are respectively 70-80%, 15-20% and 0-15%.
4. The black polyimide film with high dielectric strength and high blackness as claimed in any one of claims 1 to 3, wherein the diamine monomer is at least one of p-phenylenediamine, 4-diaminodiphenyl ether, cyclohexanediamine, and naphthalenediamine.
5. The high dielectric strength high jetness polyimide black film according to any one of claims 1 to 4, wherein the dianhydride monomer is at least one of pyromellitic dianhydride, biphenyl dianhydride, and benzophenone tetracarboxylic dianhydride.
6. A method for preparing the polyimide black film with high dielectric strength and high blackness as claimed in any one of claims 1 to 5, comprising the following steps:
s1, mixing a blue dye, a red dye, a yellow dye and an aprotic solvent, then shearing and dispersing, adding zirconium beads for grinding, and filtering the zirconium beads to obtain a color paste;
s2, adding color paste into an aprotic solvent in which a diamine monomer is dissolved in an inert gas range, uniformly mixing, and adding a dianhydride monomer for reaction to obtain a polyamic acid solution; and defoaming the polyamic acid solution, coating the defoamed polyamic acid solution on the surface of the substrate, removing the solvent and imidizing, cooling and stripping to obtain the polyimide black film with high insulating strength and high blackness.
7. The method for preparing the polyimide black film with high insulating strength and high blackness as claimed in claim 6, wherein in S1, the solid content of the color paste is 5-20%; preferably, in S1, shearing and dispersing for 0.4-0.6h at the speed of 2800-3200r/min, then adding zirconium beads for grinding for 2-3 h; preferably, in S1, the weight ratio of the zirconium beads to the color paste is 1: 0.8-1.2; preferably, in S1, the zirconium beads have a diameter of 0.2 to 0.4 mm.
8. The method for preparing a black polyimide film having high dielectric strength and high jetness as claimed in claim 6 or 7, wherein the aprotic solvent is at least one of N, N-dimethylformamide, N-dimethylacetamide and toluene in S1 and S2.
9. The method for preparing a black polyimide film having high dielectric strength and high jetness as claimed in any one of claims 6 to 8, wherein in S2, the weight ratio of the diamine monomer to the aprotic solvent is 1:9 to 11; preferably, in S2, the polyamic acid solution has a viscosity of 100-200 PaS.
10. The method for preparing a black polyimide film with high dielectric strength and high jetness as claimed in any one of claims 6 to 9, wherein the procedures of removing the solvent and imidizing in S2 are as follows: keeping the temperature at 160 ℃ for 3-5min at 140-; keeping the temperature at 280-300 ℃ for 2-3 min; finally, the temperature is maintained for 1-2min at 350 ℃ of 330-.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010864598.4A CN112111077A (en) | 2020-08-25 | 2020-08-25 | Polyimide black film with high insulation strength and high blackness and preparation method thereof |
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| CN202010864598.4A CN112111077A (en) | 2020-08-25 | 2020-08-25 | Polyimide black film with high insulation strength and high blackness and preparation method thereof |
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| CN112111077A true CN112111077A (en) | 2020-12-22 |
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| CN202010864598.4A Pending CN112111077A (en) | 2020-08-25 | 2020-08-25 | Polyimide black film with high insulation strength and high blackness and preparation method thereof |
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| Country | Link |
|---|---|
| CN (1) | CN112111077A (en) |
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| US4822718A (en) * | 1982-09-30 | 1989-04-18 | Brewer Science, Inc. | Light absorbing coating |
| CN1214129A (en) * | 1996-09-27 | 1999-04-14 | 部鲁尔科学公司 | Ultra thin organic black matix |
| CN104040430A (en) * | 2011-12-30 | 2014-09-10 | 第一毛织株式会社 | Positive photosensitive resin composition |
| CN104211974A (en) * | 2014-08-14 | 2014-12-17 | 哈尔滨工业大学 | Making method of color polyimide film |
| CN105482115A (en) * | 2015-12-11 | 2016-04-13 | 宁波今山电子材料有限公司 | Method for preparing high-insulation and high-strength polyimide black film |
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2020
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4822718A (en) * | 1982-09-30 | 1989-04-18 | Brewer Science, Inc. | Light absorbing coating |
| CN1214129A (en) * | 1996-09-27 | 1999-04-14 | 部鲁尔科学公司 | Ultra thin organic black matix |
| CN104040430A (en) * | 2011-12-30 | 2014-09-10 | 第一毛织株式会社 | Positive photosensitive resin composition |
| CN104211974A (en) * | 2014-08-14 | 2014-12-17 | 哈尔滨工业大学 | Making method of color polyimide film |
| CN105482115A (en) * | 2015-12-11 | 2016-04-13 | 宁波今山电子材料有限公司 | Method for preparing high-insulation and high-strength polyimide black film |
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Application publication date: 20201222 |