CN112143015A - Preparation method of black covering film - Google Patents
Preparation method of black covering film Download PDFInfo
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- CN112143015A CN112143015A CN202011129060.5A CN202011129060A CN112143015A CN 112143015 A CN112143015 A CN 112143015A CN 202011129060 A CN202011129060 A CN 202011129060A CN 112143015 A CN112143015 A CN 112143015A
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- 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
- C08J7/00—Chemical treatment or coating of shaped articles made of macromolecular substances
- C08J7/04—Coating
- C08J7/0427—Coating with only one layer of a composition containing a polymer binder
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- 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
- C08J7/00—Chemical treatment or coating of shaped articles made of macromolecular substances
- C08J7/04—Coating
- C08J7/044—Forming conductive coatings; Forming coatings having anti-static properties
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D179/00—Coating compositions based on 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 C09D161/00 - C09D177/00
- C09D179/04—Polycondensates having nitrogen-containing heterocyclic rings in the main chain; Polyhydrazides; Polyamide acids or similar polyimide precursors
- C09D179/08—Polyimides; Polyester-imides; Polyamide-imides; Polyamide acids or similar polyimide precursors
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/24—Electrically-conducting paints
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- 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
- C08J2367/00—Characterised by the use of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Derivatives of such polymers
- C08J2367/02—Polyesters derived from dicarboxylic acids and dihydroxy compounds
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- 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
- C08J2479/00—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 C08J2461/00 - C08J2477/00
- C08J2479/04—Polycondensates having nitrogen-containing heterocyclic rings in the main chain; Polyhydrazides; Polyamide acids or similar polyimide precursors
- C08J2479/08—Polyimides; Polyester-imides; Polyamide-imides; Polyamide acids or similar polyimide precursors
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- 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
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K3/08—Metals
- C08K2003/0862—Nickel
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- 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
- C08K2201/00—Specific properties of additives
- C08K2201/001—Conductive additives
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- 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
- C08K2201/00—Specific properties of additives
- C08K2201/017—Additives being an antistatic agent
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/04—Antistatic
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
- C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
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Abstract
The invention discloses a preparation method of a black covering film, which comprises the steps of preparing a carbon black solution, mixing the carbon black solution with a polyimide solution, mixing 4, 4-diaminodiphenyl ether and N, N-dimethylacetamide, then mechanically stirring, adding pyromellitic dianhydride, adding conductive flaky nickel powder and graphite micro-sheets, uniformly coating the solution on a PET film, and drying the solvent by gradient temperature rise. The volume resistivity of the black covering film obtained by the invention is about 8.7 multiplied by 106Omega cm, the conductivity is obviously improved compared with the traditional covering film, the antistatic effect is achieved, a black covering film sample is cut into a strip shape of 8cm multiplied by 7mm, the tensile strength is 124.1MPa by adopting a peel strength tester, and the strength is far higher than that of the traditional covering film.
Description
Technical Field
The invention belongs to the field of membrane materials, and particularly relates to a preparation method of a black covering membrane.
Background
Because LEDs have the advantages of energy saving and long service life, coupled with the increase in brightness, the range of applications extends from previous labeling applications to the lighting industry: including automotive lighting, indoor lighting, outdoor lighting, etc., so that the demand for LEDs has increased substantially; the application of the LED in electronic terminal products is also increasing, and besides consumer electronics, the LED is mainly used in the backlight of the display, and due to the light weight and cost competition of the display, the LED will be the mainstream trend in the future. Because the terminal application is more and more abundant, the market has more and more strong demand for the black covering film, compared with the common covering film, it is opaque, not reflecting the back light, therefore this kind of covering film can strengthen the contrast of the luminous source, help to raise the working efficiency of the photoelectric component; in addition, the black covering film has excellent light shielding performance and excellent confidentiality, can cover the Flexible Printed Circuit (FPC) circuit and ensure that light cannot penetrate through, and is suitable for mobile phones, digital cameras and other occasions sensitive to light. However, the traditional black covering film has poor antistatic capability and low tensile strength.
Disclosure of Invention
The invention provides a preparation method of a black covering film, aiming at the problems of poor antistatic capability and low tensile strength of the traditional black covering film.
The invention is realized in such a way that a preparation method of the black covering film comprises the following steps:
step one, adding butanone into a carbon black dispersing agent, stirring and dissolving, adding carbon black in a corresponding proportion to enable the final solid content of the carbon black to be 25%, adding glass beads, and placing on a dispersion machine to swing for 4 hours for dispersion;
step two, according to the volume ratio of 1: 1, taking a polyimide solution with the solid content of 20 percent and taking a carbon black solution with the solid content of 25 percent, and mixing and stirring for 2 hours;
thirdly, placing the conductive flaky nickel powder in a constant-temperature oven to be dried for 2 hours at the temperature of 100 ℃;
step four, heating the muffle furnace to 1000 ℃, putting the expandable graphite into the muffle furnace by using a quartz beaker, heating the expandable graphite in the muffle furnace for 15s, mixing the expanded graphite and ethanol according to the mass ratio of 1: 1000, stirring for 2 hours under ultrasonic, sanding, filtering, and drying to obtain graphite micro-sheets;
step five, mixing 4, 4-diaminodiphenyl ether and N, N-dimethylacetamide according to the mass ratio of 3: 70, mechanically stirring for 1 hour, controlling the reaction temperature at 15-20 ℃, adding pyromellitic dianhydride according to the mass ratio of 1: 1 of 4, 4-diaminodiphenyl ether, and continuously stirring for reaction for 2 hours;
step six, mixing the solution obtained in the step two and the solution obtained in the step five according to the volume ratio of 1: 1, adding 20g of the conductive flaky nickel powder obtained in the step three into every 1L of the mixed solution, controlling the reaction temperature to be 15-20 ℃, and mechanically stirring for 30 minutes;
step seven, adding 10g of the graphite microchip obtained in the step four into every 1L of the solution obtained in the step six, performing ultrasonic dispersion treatment on the mixed solution for 2 hours, and standing for 5 hours at the dispersion temperature of 20-30 ℃;
step eight, uniformly coating the solution obtained in the step seven on a PET film, and adjusting the gap of a coating head to obtain a coated film with the thickness of 0.5-0.7 mm after the solvent is dried;
and step nine, drying the solvent by adopting gradient temperature rise.
Further, in the second step, the stirring speed is 200 revolutions per minute, and the temperature is 15-20 ℃.
And further, in the fourth step, the graphite is ground until the particle size of the graphite is 30-50 microns after being stirred for 2 hours under 30kHZ ultrasonic.
And further, adding the pyromellitic dianhydride in the fifth step for three to five times, wherein the addition is finished within 0.4h, and the stirring speed is 270 revolutions per minute.
Further, in the seventh step, 50kHZ ultrasonic treatment is adopted.
Further, the flow of gradient temperature rise drying is as follows:
drying at 35 ℃ for 1 hour, then drying at 40 ℃ for 1 hour, then drying at 45 ℃ for 30 minutes, and then drying at 50 ℃ for 30 minutes.
The black overcoat layer of the present invention has a volume resistivity of about 8.7X 106Omega cm, the conductivity is obviously improved compared with the traditional covering film, the antistatic effect is achieved, a black covering film sample is cut into a strip shape of 8cm multiplied by 7mm, the tensile strength is 124.1MPa by adopting a peel strength tester, and the strength is far higher than that of the traditional covering film.
Drawings
Fig. 1 is a flow chart of a method for preparing a black cover film according to an embodiment of the present invention.
Detailed Description
In order to further understand the contents, features and effects of the present invention, the following embodiments are illustrated and described in detail with reference to the accompanying drawings.
The structure of the present invention will be described in detail below with reference to the accompanying drawings.
The invention is realized in such a way that a preparation method of a black covering film comprises the following steps:
s101, adding a carbon black dispersing agent into Methyl Ethyl Ketone (MEK), stirring and dissolving, adding carbon black in a corresponding proportion to enable the final solid content of the carbon black to be 25%, adding glass beads, and placing on a dispersion machine to swing for 4 hours for dispersion;
in the embodiment, a carbon black polymer hyperdispersant F423 of an Auner Polymer Co., Ltd, Fushan City is adopted;
s102, mixing and stirring a polyimide solution with a solid content of 20% and a carbon black solution with a solid content of 25% for 2 hours at a temperature of 15-20 ℃ at 200 revolutions per minute according to a volume ratio of 1: 1;
s103, placing the Conductive Flaky Nickel Powder (CFNP) in a constant-temperature oven to be dried for 2 hours at the temperature of 100 ℃;
in this example, Conductive Flake Nickel Powder (CFNP) of Shanghaineco metallic Material Co., Ltd is used, and the specification is 1.1g/cm3。
S104, heating a muffle furnace to 1000 ℃, putting expandable graphite into the muffle furnace by using a quartz beaker, heating the expandable graphite in the muffle furnace for 15S, mixing the expanded graphite and ethanol in a mass ratio of 1: 1000, stirring for 2 hours under 30kHZ ultrasonic sound, grinding until the particle size of the graphite is 30-50 microns, and performing suction filtration and drying to obtain graphite micro-sheets;
s105, mixing 4, 4-diaminodiphenyl ether and N, N-dimethylacetamide according to the mass ratio of 3: 70, mechanically stirring for 1 hour, controlling the reaction temperature to be between 15 and 20 ℃, adding pyromellitic dianhydride three to five times within 0.4 hour according to the mass ratio of the pyromellitic dianhydride to the 4, 4-diaminodiphenyl ether of 1: 1, and continuously stirring for reaction for 2 hours at 270 revolutions per minute;
s106, mixing the solution obtained in the step S102 and the solution obtained in the step S105 according to the volume ratio of 1: 1, adding 20g of the conductive flaky nickel powder obtained in the step S103 into every 1L of the mixed solution, controlling the reaction temperature to be 15-20 ℃, and mechanically stirring for 30 minutes;
s107, adding 10g of the graphite microchip obtained in the step S104 into every 1L of the solution obtained in the step S106, and carrying out 50kHZ ultrasonic dispersion treatment for 2 hours after the mixed solution is subjected to dispersion at the dispersion temperature of 20-30 ℃ and standing for 5 hours;
s108, uniformly coating the solution obtained in the step S107 on a PET film, and adjusting the gap of a coating head to obtain a coated film with the thickness of 0.5-0.7 mm after the solvent is dried;
and S109, drying the solvent by adopting gradient temperature rise.
The flow of gradient temperature rise drying is as follows:
drying at 35 ℃ for 1 hour, then drying at 40 ℃ for 1 hour, then drying at 45 ℃ for 30 minutes, and then drying at 50 ℃ for 30 minutes.
In the examples of the present invention, the temperature not particularly specified is room temperature.
The black overcoat layer of the present invention has a volume resistivity of about 8.7X 106Omega cm, the conductivity is obviously improved compared with the traditional covering film, the antistatic effect is achieved, a black covering film sample is cut into a strip shape of 8cm multiplied by 7mm, the tensile strength is 124.1MPa by adopting a peel strength tester, and the strength is far higher than that of the traditional covering film.
The above description is only for the preferred embodiment of the present invention, and is not intended to limit the present invention in any way, and all simple modifications, equivalent changes and modifications made to the above embodiment according to the technical spirit of the present invention are within the scope of the technical solution of the present invention.
Claims (6)
1. A preparation method of a black covering film is characterized by comprising the following steps:
step one, adding a carbon black dispersing agent into butanone, stirring and dissolving, adding carbon black to ensure that the final solid content of the carbon black is 25%, adding glass beads, placing on a dispersion machine, and swinging for 4 hours to obtain a carbon black solution;
step two, according to the volume ratio of 1: 1, taking a polyimide solution with the solid content of 20 percent and taking a carbon black solution with the solid content of 25 percent, and mixing and stirring for 2 hours;
thirdly, placing the conductive flaky nickel powder in a constant-temperature oven to be dried for 2 hours at the temperature of 100 ℃;
step four, heating the muffle furnace to 1000 ℃, putting the expandable graphite into the muffle furnace by using a quartz beaker, heating the expandable graphite in the muffle furnace for 15s, mixing the expanded graphite and ethanol according to the mass ratio of 1: 1000, stirring for 2 hours under ultrasonic waves, sanding, filtering, and drying to obtain graphite micro-sheets;
step five, mixing 4, 4-diaminodiphenyl ether and N, N-dimethylacetamide according to the mass ratio of 3: 70, mechanically stirring for 1 hour, controlling the reaction temperature at 15-20 ℃, adding pyromellitic dianhydride according to the mass ratio of 1: 1 of 4, 4-diaminodiphenyl ether, and continuously stirring for reaction for 2 hours;
step six, mixing the solution obtained in the step two and the solution obtained in the step five according to the volume ratio of 1: 1, adding 20g of the conductive flaky nickel powder obtained in the step three into every 1L of the mixed solution, controlling the reaction temperature to be 15-20 ℃, and mechanically stirring for 30 minutes;
step seven, adding 10g of the graphite microchip obtained in the step four into every 1L of the solution obtained in the step six, performing ultrasonic dispersion treatment on the mixed solution for 2 hours, and standing for 5 hours at the dispersion temperature of 20-30 ℃;
step eight, uniformly coating the solution obtained in the step seven on a PET film, and adjusting the gap of a coating head to obtain a coated film with the thickness of 0.5-0.7 mm after the solvent is dried;
and step nine, drying the solvent by adopting gradient temperature rise.
2. The method for preparing the black cover film according to claim 1, wherein the stirring speed in the second step is 200 rpm, and the temperature is 15 ℃ to 20 ℃.
3. The method for preparing the black covering film according to claim 1, wherein in the fourth step, the graphite is frosted to have a particle size of 30 to 50 μm after being stirred for 2 hours under 30kHZ ultrasound.
4. The method for preparing a black cover film according to claim 1, wherein the pyromellitic dianhydride is added in three to five times in 0.4 hour, and the stirring speed is 270 rpm.
5. The method for preparing the black cover film according to claim 1, wherein in the seventh step, 50kHZ ultrasonic treatment is adopted.
6. The method for preparing the black cover film according to claim 1, wherein the step of gradient temperature rise drying comprises the following steps:
drying at 35 ℃ for 1 hour, then drying at 40 ℃ for 1 hour, then drying at 45 ℃ for 30 minutes, and then drying at 50 ℃ for 30 minutes.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202011129060.5A CN112143015A (en) | 2020-10-21 | 2020-10-21 | Preparation method of black covering film |
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| CN202011129060.5A CN112143015A (en) | 2020-10-21 | 2020-10-21 | Preparation method of black covering film |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115093607A (en) * | 2022-07-06 | 2022-09-23 | 杭州临安德昌静电科技有限公司 | High-dispersity antistatic agent for plastic alloy and preparation method thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104151582A (en) * | 2014-07-17 | 2014-11-19 | 哈尔滨工业大学 | Method for preparing graphene-polyimide conductive black film |
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2020
- 2020-10-21 CN CN202011129060.5A patent/CN112143015A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104151582A (en) * | 2014-07-17 | 2014-11-19 | 哈尔滨工业大学 | Method for preparing graphene-polyimide conductive black film |
Non-Patent Citations (1)
| Title |
|---|
| 李建军等: "《塑料配方设计（第三版）》", 30 September 2019, 中国轻工业出版社 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115093607A (en) * | 2022-07-06 | 2022-09-23 | 杭州临安德昌静电科技有限公司 | High-dispersity antistatic agent for plastic alloy and preparation method thereof |
| CN115093607B (en) * | 2022-07-06 | 2024-02-02 | 杭州临安德昌静电科技有限公司 | High-dispersity antistatic agent for plastic alloy and preparation method thereof |
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Application publication date: 20201229 |