CN115820155A - Super-thick high-temperature-resistant and voltage-resistant polyester hot melt adhesive film and preparation method thereof - Google Patents
Super-thick high-temperature-resistant and voltage-resistant polyester hot melt adhesive film and preparation method thereof Download PDFInfo
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- CN115820155A CN115820155A CN202211572692.8A CN202211572692A CN115820155A CN 115820155 A CN115820155 A CN 115820155A CN 202211572692 A CN202211572692 A CN 202211572692A CN 115820155 A CN115820155 A CN 115820155A
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- 238000009472 formulation Methods 0.000 description 4
- 239000003292 glue Substances 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- 229910052802 copper Inorganic materials 0.000 description 3
- 239000010949 copper Substances 0.000 description 3
- 239000000155 melt Substances 0.000 description 3
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 2
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
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- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 2
- 239000010931 gold Substances 0.000 description 2
- 229910052737 gold Inorganic materials 0.000 description 2
- 238000003475 lamination Methods 0.000 description 2
- 229910052698 phosphorus Inorganic materials 0.000 description 2
- 239000011574 phosphorus Substances 0.000 description 2
- 238000007747 plating Methods 0.000 description 2
- 229920000139 polyethylene terephthalate Polymers 0.000 description 2
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- YXRKNIZYMIXSAD-UHFFFAOYSA-N 1,6-diisocyanatohexane Chemical compound O=C=NCCCCCCN=C=O.O=C=NCCCCCCN=C=O.O=C=NCCCCCCN=C=O YXRKNIZYMIXSAD-UHFFFAOYSA-N 0.000 description 1
- 239000005995 Aluminium silicate Substances 0.000 description 1
- WKBOTKDWSSQWDR-UHFFFAOYSA-N Bromine atom Chemical compound [Br] WKBOTKDWSSQWDR-UHFFFAOYSA-N 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 239000012790 adhesive layer Substances 0.000 description 1
- 235000012211 aluminium silicate Nutrition 0.000 description 1
- 230000002238 attenuated effect Effects 0.000 description 1
- GDTBXPJZTBHREO-UHFFFAOYSA-N bromine Substances BrBr GDTBXPJZTBHREO-UHFFFAOYSA-N 0.000 description 1
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- 229910000019 calcium carbonate Inorganic materials 0.000 description 1
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- FPAFDBFIGPHWGO-UHFFFAOYSA-N dioxosilane;oxomagnesium;hydrate Chemical compound O.[Mg]=O.[Mg]=O.[Mg]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O FPAFDBFIGPHWGO-UHFFFAOYSA-N 0.000 description 1
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- 239000012943 hotmelt Substances 0.000 description 1
- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 description 1
- 238000010128 melt processing Methods 0.000 description 1
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Classifications
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A30/00—Adapting or protecting infrastructure or their operation
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E10/00—Energy generation through renewable energy sources
- Y02E10/50—Photovoltaic [PV] energy
Abstract
The invention discloses an ultra-thick high-temperature-resistant and voltage-resistant polyester hot melt adhesive film and a preparation method thereof, and relates to the technical field of flexible flat cables. The preparation method of the invention comprises the following steps: uniformly mixing all the raw materials of the first hot melt adhesive layer, adding the mixture into a double-screw extruder, extruding and granulating to obtain hot melt adhesive particles, putting the hot melt adhesive particles into a casting machine for heating and melting, coating the molten hot melt adhesive on the surface of the ink layer, and cooling to obtain the first hot melt adhesive layer; and coating a polyester hot melt adhesive on the surface of the first hot melt adhesive layer, and drying to form a second hot melt adhesive layer on the surface of the first hot melt adhesive layer to obtain the super-thick high-temperature-resistant voltage-resistant polyester hot melt adhesive film. According to the invention, the first hot melt adhesive layer with large thickness and good bending resistance can be prepared in an extrusion granulation and spraying manner, and meanwhile, the problem of back adhesion can be reduced by coating the second hot melt adhesive layer on the surface of the first hot melt adhesive layer, so that the problem that the FFC insulating hot melt adhesive film with large thickness is difficult to prepare by adopting a coating method at present is solved.
Description
Technical Field
The invention relates to the technical field of flexible flat cables, in particular to an ultra-thick high-temperature-resistant and voltage-resistant polyester hot melt adhesive film and a preparation method thereof.
Background
The FFC (flexible flat cable is called in English) is a novel data cable formed by pressing an FFC insulating hot melt adhesive film and an extremely thin tinned flat copper wire through a high-tech automatic equipment production line, and has the advantages of softness, free bending and folding, thin thickness, small volume, simple connection, convenience in disassembly, easiness in solving of electromagnetic shielding and the like.
The conventional FFC insulating hot melt adhesive film structure generally has three layers, i.e. a PET (polyethylene terephthalate, chemical formula of (cioh 804) n) insulating layer, a pre-coating ink layer and a hot melt adhesive layer. With the wider application range of the FFC, some industries need to use the FFC with higher resistance, and at the moment, in order to consider the safety, the FFC insulating hot melt adhesive film needs to have excellent voltage resistance. At present, one of the important methods for improving the voltage resistance of the FFC insulating hot melt adhesive film is to increase the voltage resistance by increasing the thickness of the hot melt adhesive layer, and as the thickness of the hot melt adhesive layer is thicker, the voltage resistance of the FFC insulating hot melt adhesive film is higher.
The FFC insulating hot melt adhesive film on the market at present is usually 40-80 μm thick, and is low in thickness, so that the hot melt adhesive film with large thickness is difficult to prepare, and the main reason is that the hot melt adhesive layer in the conventional FFC insulating hot melt adhesive film is mainly prepared in a solution coating mode, namely, various materials are emulsified and dispersed into hot melt adhesive liquid, then the hot melt adhesive liquid is coated on the pre-coating ink layer, and the hot melt adhesive layer is obtained through drying and rolling. The thickness of the hot melt adhesive layer manufactured by the coating method is about 50 mu m at one time, if the ultra-thick FFC insulating hot melt adhesive film needs to be obtained through multiple coating, the mode of obtaining the high-thickness hot melt adhesive layer by multiple coating not only can increase the production cost, but also can cause uncertainty and risk increase due to multiple coating, if an error occurs at one time, the whole product can be scrapped, and the FFC insulating hot melt adhesive film manufactured by the coating method is harder and has poor bending resistance, and a right-angle position is easy to scratch in the later processing punching process, so that the assembly connector can be influenced. Therefore, the FFC insulating hot melt adhesive film with large thickness cannot be easily prepared by the conventional coating method.
Disclosure of Invention
Aiming at the problems in the prior art, the invention aims to provide a preparation method of an ultra-thick high-temperature-resistant voltage-resistant film, which can be used for preparing a first hot-melt adhesive layer with large thickness and good bending resistance in an extrusion granulation and spraying manner, and can reduce the problem of back adhesion by coating a second hot-melt adhesive layer on the surface of the first hot-melt adhesive layer, thereby solving the problem that the FFC (flexible flat cable) insulating hot-melt adhesive film with large thickness is difficult to prepare by adopting a coating method at present.
The invention also aims to provide an ultra-thick high-temperature-resistant voltage-resistant cable which is prepared by the preparation method and has the advantages of large thickness, good voltage-resistant performance, good bending-resistant performance and high temperature resistance.
In order to achieve the purpose, the invention adopts the following technical scheme:
a preparation method of an ultra-thick high-temperature-resistant and voltage-resistant polyester hot melt adhesive film comprises the following steps:
(1) Uniformly mixing 35-75 parts by mass of saturated polyester resin A, 10-60 parts by mass of saturated polyester resin C, 10-30 parts by mass of first flame retardant, 1-4 parts by mass of dispersing agent and 1-10 parts by mass of first filler, adding the mixture into a double-screw extruder, and carrying out extrusion granulation to obtain hot melt adhesive granules;
(2) Mixing 35-75 parts of saturated polyester resin A, 10-40 parts of saturated polyester resin B and a solvent, and then emulsifying to obtain a resin solution; adding 5-30 parts of a second flame retardant and 1-10 parts of a second filler into the resin solution, uniformly dispersing to obtain a powder liquid, and grinding the powder liquid to obtain a semi-finished product solution; sequentially adding 1-10 parts of flatting agent and 1-10 parts of curing agent into the semi-finished product solution, and adding while dispersing to obtain the polyester hot melt adhesive;
(3) Putting hot melt adhesive particles into a casting machine for heating and melting to obtain molten hot melt adhesive, coating the molten hot melt adhesive on the surface of the insulating material which is pre-coated with the printing ink, and cooling to obtain a polyester hot melt adhesive film which is sequentially provided with a first hot melt adhesive layer, a printing ink layer and an insulating layer from top to bottom; the thickness of the first hot melt adhesive layer is 100-250 mu m;
(4) And (3) coating a polyester hot melt adhesive on the surface of the first hot melt adhesive layer, wherein the coating thickness of the polyester hot melt adhesive is 25-50 mu m, and forming a second hot melt adhesive layer on the surface of the first hot melt adhesive layer after drying to obtain the super-thick high-temperature-resistant voltage-resistant polyester hot melt adhesive film.
Preferably, in the step (2), the preparation method of the resin liquid is as follows: putting 35-75 parts of saturated polyester resin A, 10-40 parts of saturated polyester resin B and a solvent into an emulsifying machine, emulsifying, setting the rotating speed of the emulsifying machine to 200r/min before putting materials into the emulsifying machine, then putting the materials, after the feeding is finished, accelerating the rotating speed of the emulsifying machine to 300-800 r/min, emulsifying for 30-110 min, wherein the emulsifying temperature is 25-40 ℃, the environmental humidity is 30-50%, and obtaining a resin liquid after the emulsification is finished.
Preferably, in the step (2), the powdered liquid is prepared by the following method: adding 5-30 parts of second flame retardant and 1-10 parts of second filler into the resin liquid, and performing dispersion treatment at the dispersion speed of 300-700 r/min for 20-90 min, wherein the temperature is controlled at 20-35 ℃ and the environmental humidity is 30-50% in the dispersion process to obtain the powder body liquid.
Preferably, in the step (2), the semi-finished solution is prepared by the following method: grinding the powder liquid twice, wherein the grinding time is 20-80 min each time, and the temperature is 20-35 ℃ in the grinding process, so as to obtain a semi-finished product solution.
Preferably, in the step (2), when the leveling agent and the curing agent are added into the semi-finished product solution, the leveling agent is added firstly while dispersing, the dispersing speed is 300-800 r/min, and the dispersing time is 10-40 min; then adding a curing agent while dispersing, wherein the dispersing speed is 300-800 r/min, and the dispersing time is 10-40 min, so as to obtain the polyester hot melt adhesive.
Preferably, in the step (4), after the polyester hot melt adhesive is coated, drying is performed at a temperature of 130-150 ℃, and after drying, a second hot melt adhesive layer is formed on the surface of the first hot melt adhesive layer, so as to obtain the super-thick high-temperature-resistant voltage-resistant polyester hot melt adhesive film.
A super-thick high-temperature-resistant voltage-resistant polyester hot melt adhesive film is prepared by the preparation method of the super-thick high-temperature-resistant voltage-resistant polyester hot melt adhesive film and sequentially comprises a second hot melt adhesive layer, a first hot melt adhesive layer, an ink layer and an insulating layer from top to bottom;
according to the mass parts, the raw materials of the first hot melt adhesive layer comprise 35-75 parts of saturated polyester resin A, 10-60 parts of saturated polyester resin C, 10-30 parts of first flame retardant, 1-4 parts of dispersant and 1-10 parts of first filler;
the raw materials of the second hot melt adhesive layer comprise 35-75 parts of saturated polyester resin A, 10-40 parts of saturated polyester resin B, 1-10 parts of flatting agent, 5-30 parts of second flame retardant, 1-10 parts of flatting agent, 1-10 parts of second filler and 1-10 parts of curing agent.
Preferably, the glass transition temperature of the saturated polyester resin A is-10-80 ℃, the softening point is 100-160 ℃, the molecular weight is 36000-84000, and the hydroxyl value is 2-6 mgKOH/g;
the glass transition temperature of the saturated polyester resin C is 20-60 ℃, the softening point is 20-80 ℃, the molecular weight is 2200-42000, and the hydroxyl value is 1-4 mgKOH/g;
the glass transition temperature of the saturated polyester resin B is 0-36 ℃, the softening point is 3-80 ℃, the molecular weight is 18000-58000, and the hydroxyl value is 2-5 mgKOH/g;
preferably, the thickness of the insulating layer is 12 to 100 micrometers, the thickness of the ink layer is 1 to 2 micrometers, the thickness of the first hot melt adhesive layer is 100 to 250 micrometers, and the thickness of the second hot melt adhesive layer is 25 to 50 micrometers.
Preferably, the first flame retardant and the second flame retardant are respectively selected from any one or more of a bromine flame retardant, a phosphorus flame retardant, a nitrogen flame retardant, a metal hydroxide flame retardant, a metal oxide flame retardant and a metal boride flame retardant;
the leveling agent is an acrylic leveling agent and/or a fluorine leveling agent;
the curing agent is selected from any one or combination of more of aromatic isocyanate, aliphatic isocyanate, room temperature reaction type isocyanate and blocked isocyanate.
The effective results of the technical scheme are as follows:
1. the technical scheme provides a preparation method of an ultra-thick high-temperature-resistant voltage-resistant polyester hot melt adhesive film, wherein raw materials of a first hot melt adhesive layer are extruded and granulated by a double-screw extruder to obtain hot melt adhesive particles, and then the hot melt adhesive particles are heated and melted and then coated on the surface of an insulating material of pre-coated ink, and the first hot melt adhesive layer with the thickness of 100-250 mu m can be directly prepared by the method, so that the ultra-thick polyester hot melt adhesive film is prepared, repeated coating is not needed, the cost and the risk can be reduced, and meanwhile, the first hot melt adhesive layer prepared by the extrusion granulation and coating method in the technical scheme is softer than the hot melt adhesive layer prepared by a coating method, so that the bending resistance is good, and the ultra-thick high-temperature-resistant voltage-resistant polyester hot melt adhesive film can not be easily damaged in the later processing process. Therefore, the polyester hot melt adhesive film prepared by the technical scheme has large film thickness and good flexing resistance, and can be used as a polyester hot melt adhesive film for the gold plating treatment of oxygen-free copper conductors in the FFC industry.
2. This technical scheme is equipped with second hot melt adhesive layer on first hot melt adhesive layer's surface, through the interact of saturated polyester resin A, saturated polyester resin B and flatting agent in the second hot melt adhesive layer, can prevent that second hot melt adhesive layer from producing the problem of anti-sticking, is favorable to depositing and transporting, when using, opens a book easily to improve production efficiency.
Detailed Description
The technical solution of the present invention will be further described with reference to the following embodiments.
A preparation method of an ultra-thick high-temperature-resistant and voltage-resistant polyester hot melt adhesive film comprises the following steps:
(1) Uniformly mixing 35-75 parts by mass of saturated polyester resin A, 10-60 parts by mass of saturated polyester resin C, 10-30 parts by mass of first flame retardant, 1-4 parts by mass of dispersing agent and 1-10 parts by mass of first filler, adding the mixture into a double-screw extruder, and carrying out extrusion granulation to obtain hot melt adhesive granules;
(2) Mixing 35-75 parts of saturated polyester resin A, 10-40 parts of saturated polyester resin B and a solvent (the solvent in the technical scheme is composed of butanone and toluene in a mass ratio of 3; adding 5-30 parts of a second flame retardant and 1-10 parts of a second filler into the resin solution, uniformly dispersing to obtain a powder liquid, and grinding the powder liquid to obtain a semi-finished product solution; sequentially adding 1-10 parts of flatting agent and 1-10 parts of curing agent into the semi-finished product solution, and adding while dispersing to obtain the polyester hot melt adhesive;
(3) Putting hot melt adhesive particles into a casting machine for heating and melting to obtain molten hot melt adhesive, coating the molten hot melt adhesive on the surface of the insulating material which is pre-coated with the printing ink, and cooling to obtain a polyester hot melt adhesive film which is sequentially provided with a first hot melt adhesive layer, a printing ink layer and an insulating layer from top to bottom; the thickness of the first hot melt adhesive layer is 100-250 mu m;
(4) And (3) coating a polyester hot melt adhesive on the surface of the first hot melt adhesive layer, wherein the coating thickness of the polyester hot melt adhesive is 25-50 mu m, and forming a second hot melt adhesive layer on the surface of the first hot melt adhesive layer after drying to obtain the super-thick high-temperature-resistant voltage-resistant polyester hot melt adhesive film.
In the prior art, the hot melt adhesive layer in the hot melt adhesive film is mainly prepared in a solution coating mode, and the hot melt adhesive layer with larger thickness is obtained through multiple coating.
The technical scheme provides a preparation method of an ultra-thick high-temperature-resistant voltage-resistant polyester hot melt adhesive film, wherein raw materials of a first hot melt adhesive layer are extruded and granulated by a double-screw extruder to obtain hot melt adhesive particles, and then the hot melt adhesive particles are heated and melted and then coated on the surface of an insulating material of pre-coated ink, and the first hot melt adhesive layer with the thickness of 100-250 mu m can be directly prepared by the method, so that the ultra-thick polyester hot melt adhesive film is prepared, repeated coating is not needed, the cost and the risk can be reduced, and meanwhile, the first hot melt adhesive layer prepared by the extrusion granulation and coating method in the technical scheme is softer than the hot melt adhesive layer prepared by a coating method, so that the bending resistance is good, and the ultra-thick high-temperature-resistant voltage-resistant polyester hot melt adhesive film can not be easily damaged in the later processing process. Therefore, the polyester hot melt adhesive prepared by the technical scheme has large film thickness and good flexing resistance, and can be used as a polyester hot melt adhesive film for gold plating treatment of oxygen-free copper conductors in the FFC industry.
It is worth noting that the existing hot melt adhesive film for FFC is produced by adopting a coating process of a solution system because the used raw materials have low molecular weight and no processability, and meanwhile, the content of various types of powder (such as flame retardants and fillers) is high, and the various types of powder have no viscosity, so that the hot melt adhesive layer in the existing hot melt adhesive film is difficult to prepare by using a method of extrusion granulation and then pouring. In the preparation process of the first hot melt adhesive layer, the first hot melt adhesive layer can be prepared by adopting the processes of twin-screw extrusion, laminating and the like through the matching of the saturated polyester resin A, the saturated polyester resin C and the dispersing agent.
It is worth pointing out that because among this technical scheme first hot melt adhesive layer adopts the twin-screw to extrude and drench the preparation such as membrane and form, make first hot melt adhesive layer produce the problem that the back of the body glues (anti-sticking) easily under the higher environment of transportation and temperature, when polyester hot melt adhesive film deposits promptly, deposit after the polyester hot melt adhesive film rolling, under transportation or the higher environment of temperature, because the temperature is higher, first hot melt adhesive layer can produce a small amount of melting, and lead to the surface of first hot melt adhesive layer and insulating layer to glue together, be difficult for separating when using, lead to the production degree of difficulty to increase. Consequently, this technical scheme is equipped with second hot melt adhesive layer on first hot melt adhesive layer's surface, through the interact of saturated polyester resin A, saturated polyester resin B and flatting agent in the second hot melt adhesive layer for second hot melt adhesive layer can not produce the problem of anti-sticking basically, is favorable to depositing and transporting, when using, opens a book easily, thereby improves production efficiency.
Further, according to the technical scheme, the first hot melt adhesive layer and the second hot melt adhesive layer are arranged, and the polyester resins with different properties are simultaneously selected, so that the prepared polyester hot melt adhesive film has the properties of strong metal adhesion, good heat resistance and good voltage resistance. Moreover, because the total thickness of the first hot melt adhesive layer and the second hot melt adhesive layer in the technical scheme reaches 125-300 μm, the voltage resistance of the polyester hot melt adhesive film can be obviously improved, and the voltage resistance of the polyester hot melt adhesive film is higher along with the increase of the total thickness of the first hot melt adhesive layer and the second hot melt adhesive layer. Meanwhile, because the total thickness of the first hot melt adhesive layer and the second hot melt adhesive layer is thicker, the deeper the sinking depth of the metal conductor is when the FFC finished product is prepared by pressing, and the performance of metal adhesion can be further improved.
Further, in the step (1), in the extrusion step of preparing the hot melt adhesive pellets, the extrusion processing temperature of the twin-screw extruder is 80 to 200 ℃. When the extrusion processing temperature of the double-screw extruder is lower than 80 ℃, the hot melt adhesive system is not melted, and hot melt processing cannot be realized; when the extrusion processing temperature of the double-screw extruder is higher than 200 ℃, the melt strength of the hot melt adhesive system is too low, and the hot melt adhesive system does not have the processing performance and cannot extrude the melt. In the step of preparing the laminating film of the first hot melt adhesive layer in the step (3), the laminating processing temperature of a laminating machine is 120-200 ℃, when the laminating processing temperature of the laminating machine is lower than 120 ℃, the plasticization of a hot melt adhesive system is incomplete, the processing performance is poor, and the film forming is difficult; when the film spraying processing temperature of the film spraying machine is higher than 200 ℃, the melt strength of the hot melt adhesive system is too low, and the hot melt adhesive system does not have the processing performance and cannot be subjected to film spraying forming.
Specifically, in the actual use process, after the semi-finished product is obtained in the step (2), the semi-finished product solution, the leveling agent and the curing agent do not need to be mixed immediately, but the semi-finished product solution is hermetically stored, the storage temperature is controlled to be 20-30 ℃, the humidity of the environment in the storage area is controlled to be 30-50%, when the semi-finished product solution needs to be used, the semi-finished product solution, the leveling agent and the curing agent are mixed, and the polyester hot melt adhesive is obtained after the semi-finished product solution is uniformly dispersed. When the prepared polyester hot melt adhesive is used, the polyester hot melt adhesive is placed in an environment with the environmental humidity of 30-70%, and after HDI trimer capsules mainly containing methylcellulose are added, the glue is applied within the shelf life of 8 hours, so that various functions of the polyester hot melt adhesive can be exerted to the best, and the functions begin to be attenuated after 8 hours.
The preparation method of the super-thick high-temperature-resistant and voltage-resistant polyester hot melt adhesive film has the advantages of simple preparation process, high production safety and strong operability.
Further, in the step (2), the preparation method of the resin solution is as follows: putting 35-75 parts of saturated polyester resin A, 10-40 parts of saturated polyester resin B and a solvent into an emulsifying machine, emulsifying, setting the rotating speed of the emulsifying machine to 200r/min before putting the materials into the emulsifying machine, then putting the materials, after the materials are put into the emulsifying machine, increasing the rotating speed of the emulsifying machine to 300-800 r/min, emulsifying for 30-110 min, the emulsifying temperature is 25-40 ℃, the environmental humidity is 30-50%, and obtaining the resin liquid after the emulsification is finished.
In step (2), the powdered liquid is prepared as follows: adding 5-30 parts of second flame retardant and 1-10 parts of second filler into the resin liquid, and performing dispersion treatment at the dispersion speed of 300-700 r/min for 20-90 min, wherein the temperature is controlled at 20-35 ℃ and the environmental humidity is 30-50% in the dispersion process to obtain the powder body liquid.
In step (2), the semi-finished solution is prepared as follows: grinding the powder liquid twice, wherein the grinding time is 20-80 min each time, and the temperature is 20-35 ℃ in the grinding process, so as to obtain a semi-finished product solution.
Further, in the step (2), when the leveling agent and the curing agent are added into the semi-finished product solution, the leveling agent is added first, and the addition is carried out while dispersing, wherein the dispersing speed is 300-800 r/min, and the dispersing time is 10-40 min; then adding a curing agent while dispersing, wherein the dispersing speed is 300-800 r/min, and the dispersing time is 10-40 min, so as to obtain the polyester hot melt adhesive.
Further, in the step (4), after the polyester hot melt adhesive is coated, drying is performed at a temperature of 130 to 150 ℃, and after drying, a second hot melt adhesive layer is formed on the surface of the first hot melt adhesive layer, so as to obtain the ultra-thick high temperature resistant and voltage resistant polyester hot melt adhesive film.
A super-thick high-temperature-resistant voltage-resistant polyester hot melt adhesive film is prepared by the preparation method of the super-thick high-temperature-resistant voltage-resistant polyester hot melt adhesive film and sequentially comprises a second hot melt adhesive layer, a first hot melt adhesive layer, an ink layer and an insulating layer from top to bottom;
the raw materials of the first hot melt adhesive layer comprise, by mass, 35-75 parts of saturated polyester resin A, 10-60 parts of saturated polyester resin C, 10-30 parts of a first flame retardant, 1-4 parts of a dispersing agent and 1-10 parts of a first filler;
the raw materials of the second hot melt adhesive layer comprise 35-75 parts of saturated polyester resin A, 10-40 parts of saturated polyester resin B, 1-10 parts of flatting agent, 5-30 parts of second flame retardant, 1-10 parts of flatting agent, 1-10 parts of second filler and 1-10 parts of curing agent.
Further, the glass transition temperature of the saturated polyester resin A is-10 to 80 ℃, the softening point is 100 to 160 ℃, the molecular weight is 36000 to 84000, and the hydroxyl value is 2 to 6mgKOH/g;
the glass transition temperature of the saturated polyester resin C is 20-60 ℃, the softening point is 20-80 ℃, the molecular weight is 2200-42000, and the hydroxyl value is 1-4 mgKOH/g;
the glass transition temperature of the saturated polyester resin B is 0-36 ℃, the softening point is 3-80 ℃, the molecular weight is 18000-58000, and the hydroxyl value is 2-5 mgKOH/g;
it is worth to say that the saturated polyester resin A in the technical scheme is a saturated polyester resin with the softening point of 100-160 ℃ and the molecular weight of 36000-84000, and the softening point is high, so that the saturated polyester resin A has good heat resistance, and the high-temperature resistance of the polyester hot melt adhesive film can be obviously improved. The saturated polyester resin C is relatively cheap, and can reduce the cost. The saturated polyester resin B has a low softening point and a low molecular weight, and can further reduce the problem of anti-sticking.
Preferably, in the first hot-melt adhesive layer, the mass ratio of the saturated polyester resin a to the saturated polyester resin C is (35. If the content of the saturated polyester resin A in the first hot melt adhesive layer is too much, the molten polyester hot melt adhesive has strong fluidity, and the back adhesion is serious; if the content of the saturated polyester resin a is too small, the adhesion of the first hot-melt adhesive layer is low and the heat resistance is insufficient. Meanwhile, if the content of the saturated polyester resin C is too high, the fluidity of the molten polyester hot melt adhesive is too poor when the first hot melt adhesive layer is prepared, so that the prepared polyester hot melt adhesive film is relatively hard and has low adhesive force.
Preferably, in the second hot melt adhesive layer, the mass ratio of the saturated polyester resin a to the saturated polyester resin B is (35; if the content of the saturated polyester resin B is too large, the heat resistance of the polyester hot melt adhesive is too high, the second hot melt adhesive layer can be back-adhered, and if the content of the saturated polyester resin B is too small, the polyester hot melt adhesive is high in fluidity and low in heat resistance.
According to the polyester hot melt adhesive film prepared by the scheme, the saturated polyester resins with different molecular weights and soft critical points are selected and compounded for use, so that the prepared polyester hot melt adhesive film has the performances of strong metal adhesion, good heat resistance and good voltage resistance, and meanwhile, the hot melt adhesive film has high thickness and good bending resistance.
Preferably, the polyester hot melt adhesive film of the technical scheme has a processing temperature of 175-190 ℃ when the FFC wire is pressed with the metal wire.
Further, the thickness of the insulating layer is 12 to 100 μm, the thickness of the ink layer is 1 to 2 μm, the thickness of the first hot melt adhesive layer is 100 to 250 μm, and the thickness of the second hot melt adhesive layer is 25 to 50 μm.
It is worth explaining that the polyester hot melt adhesive film prepared by the technical scheme has thicker thickness, and can obviously improve the polyester hot melt adhesive film and the voltage resistance, so that the polyester hot melt adhesive film of the technical scheme can be used for coating tinned flat copper wires with larger resistance values and voltage values.
The first flame retardant and the second flame retardant are respectively selected from any one or more of a brominated flame retardant, a phosphorus flame retardant, a nitrogen flame retardant, a metal hydroxide flame retardant, a metal oxide flame retardant and a metal boride flame retardant;
the leveling agent is an acrylic leveling agent and/or a fluorine leveling agent;
the curing agent is selected from any one or combination of more of aromatic isocyanate, aliphatic isocyanate, room temperature reaction type isocyanate and blocked isocyanate.
Preferably, the first filler and the second filler in the technical scheme are respectively one or a combination of more of fumed silica, titanium dioxide, calcium carbonate, mica, talcum powder, wollastonite and kaolin.
Preferably, the dispersant used in the first hot-melt adhesive layer of the technical scheme is a polyacid copolymer, and because the ratio of the flame retardant to the first filler in the first hot-melt adhesive layer is large, the first hot-melt adhesive layer is easily layered, and meanwhile, the condition of uneven dispersion of particles can exist, and the polyacid copolymer is added to enable the flame retardant and the first filler to be uniformly dispersed, so that the first hot-melt adhesive layer is not layered.
The technical scheme of the invention is further illustrated by the following specific examples.
Examples 1 to 6
The preparation method of the super-thick high-temperature-resistant voltage-resistant polyester hot melt adhesive film in the embodiments 1 to 6 comprises the following steps:
(1) Uniformly mixing 35-75 parts by mass of saturated polyester resin A, 10-60 parts by mass of saturated polyester resin C, 10-30 parts by mass of first flame retardant, 1-4 parts by mass of dispersing agent and 1-10 parts by mass of first filler, adding the mixture into a double-screw extruder, and carrying out extrusion granulation to obtain hot melt adhesive granules; wherein the glass transition temperature of the saturated polyester resin A is 19 ℃, the softening point is 140 ℃, the molecular weight is 49466, and the hydroxyl value is 4.5mgKOH/g; the glass transition temperature of the saturated polyester resin C is 55 ℃, the softening point is 80 ℃, the molecular weight is 22347, and the hydroxyl value is 1.8mgKOH/g;
(2) Putting 35-75 parts of saturated polyester resin A, 10-40 parts of saturated polyester resin B and a solvent (consisting of butanone and toluene in a mass ratio of 3; adding 5-30 parts of a second flame retardant and 1-10 parts of a second filler into the resin liquid, performing dispersion treatment, wherein the dispersion speed is 300r/min, the dispersion time is 60min, the temperature is controlled to be 30 ℃ in the dispersion process, the environmental humidity is 40%, so as to obtain powder liquid, grinding the powder liquid twice, the grinding time is 60min each time, and the temperature is 28 ℃ in the grinding process, so as to obtain a semi-finished product solution; sequentially adding 1-10 parts of flatting agent and 1-10 parts of curing agent into the semi-finished product solution, wherein the dispersion speed is 600r/min, and obtaining the polyester hot melt adhesive; wherein, the glass transition temperature of the saturated polyester resin A used for preparing the polyester hot melt adhesive is 19 ℃, the softening point is 140 ℃, the molecular weight is 49466, and the hydroxyl value is 4.5mgKOH/g; the glass transition temperature of the saturated polyester resin B is 9 ℃, the softening point is 65 ℃, the molecular weight is 20153, and the hydroxyl value is 4.3mgKOH/g;
(3) Putting hot melt adhesive particles into a casting machine for heating and melting to obtain molten hot melt adhesive, coating the molten hot melt adhesive on the surface of the insulating material which is pre-coated with the printing ink, and cooling to obtain a polyester hot melt adhesive film which is sequentially provided with a first hot melt adhesive layer, a printing ink layer and an insulating layer from top to bottom; the thickness of the first hot melt adhesive layer is 150 micrometers;
(4) And (3) coating a polyester hot melt adhesive on the surface of the first hot melt adhesive layer, wherein the coating thickness of the polyester hot melt adhesive is 35 microns, and drying at 140 ℃ to form a second hot melt adhesive layer on the surface of the first hot melt adhesive layer to obtain the super-thick high-temperature-resistant voltage-resistant polyester hot melt adhesive film.
Specifically, the formulations of the first and second hot melt adhesive layers in examples 1-6 are shown in tables 1 and 2 below, respectively.
TABLE 1 formulation of the first hotmelt adhesive layers in examples 1-6 (unit: parts)
TABLE 2 formulation of the second hotmelt adhesive layer in examples 1-6 (unit: parts)
Specifically, the appearance, the back adhesion condition, the metal adhesion property and the voltage resistance of the polyester hot melt adhesive films prepared in examples 1 to 6 were respectively tested by the following test evaluation methods, and a double 85 ℃ high temperature and high humidity test, an 85 ℃ 96 hour occlusion connector test and a test were performed to determine whether a void phenomenon occurred, and the test evaluation results are shown in table 3 below. The specific test evaluation method is as follows:
(1) Appearance condition: and (4) visually observing the surface of the second hot melt adhesive layer to determine whether bubbles, pinholes and particles exist, and determining that the second hot melt adhesive layer is qualified if the bubbles, the pinholes and the particles exist.
(2) Back-sticking condition: and coating the second hot melt adhesive layer on the second hot melt adhesive layer surface of the finished polyester hot melt adhesive film of the first hot melt adhesive layer, flatly attaching the second hot melt adhesive layer on the non-corona surface of the insulating layer, wherein the specification of the sample plate is 50mm multiplied by 200mm, flatly placing a weight of 5kg on the sample plate, testing the stripping force of the sample plate after placing the sample plate in a drying oven at the temperature of 50 ℃ for 48 hours, and testing the qualified sample plate when the stripping speed of a tensile machine is 50mm/min and the stripping value is less than 0.2N/5 cm.
(3) Metal adhesion condition: pressing a round wire conductor with the diameter of 0.12mm under the temperature condition of 175-190 ℃, pressing a window position into a conductor with the thickness of 0.035mm multiplied by 0.3mm width by a machine or pressing a round wire conductor with the diameter of 0.28mm, pressing a window position into a conductor with the thickness of 0.1mm multiplied by 0.6mm by a machine, after pressing an FFC wire rod, testing the adhesive force of a single conductor at the window position of the FFC wire rod by using a tensile machine, wherein the peeling speed is 300mm/min, the standard is that the adhesive force of the pressed conductor with the thickness of 0.3mm is more than 20g/0.3mm, and the adhesive force of the pressed conductor with the thickness of 0.6mm is more than 60g/0.6mm.
(4) And (3) voltage resistance performance test: and placing the hot-pasted FFC wire in a voltage-resistant tester, and placing the FFC wire in a plug-in jig for testing, wherein the conductor and the conductor are AC500V for one minute, the conductor and the coating are tested for AC2000V for one minute below 0.060mm, the conductor and the coating are tested for AC5000V for one minute above 0.06mm, the leakage current is set to 10mA, and the insulating adhesive is qualified without generating electric arcs.
(5) Double 85 ℃ high temperature and high humidity test: pressing a round wire conductor with the diameter of 0.12mm under the temperature condition of 175-190 ℃, pressing the round wire conductor with the diameter of 0.035mm and the width of 0.3mm at the window position by a machine, designing the temperature to 85 ℃ and 85 humidity in a high-temperature high-humidity tester after pressing the round wire conductor into an FFC wire, then putting a sample plate in the FFC wire for 96 hours, taking out the sample plate to wipe off the surface water, testing the adhesive force of a single conductor at the window position of the FFC wire by a tensile machine, wherein the peeling speed is 200mm/min, and the standard is that the adhesive force for pressing the 0.3mm conductor is more than 20g/0.3mm.
(6) Whether the hole phenomenon appears or not: the hole phenomenon is actually a phenomenon of poor lamination, and is mainly because the glue does not fill the gaps at the edges of the conductors in the lamination process, the FFC wires can be cut from the window position of the FFC wires, the FFC wires are soaked in water for 30 minutes and then taken out, whether the FFC wires are subjected to water seepage or not is observed, and the phenomenon that the FFC wires are subjected to water seepage is a phenomenon with holes.
(7) 96 hour snap connector test at 85 ℃: the polyester hot melt adhesive films of examples 1 to 6 were respectively prepared into FFC wires, and the FFC wires were put on a connector and placed in an oven at 85 ℃ for 96 hours, and then the connector was taken out and pulled out, and whether the adhesive layers (i.e., the first hot melt adhesive layer and the second hot melt adhesive layer) of the FFC wires overflowed onto the surface of the conductor was observed under a secondary machine.
Table 3 test evaluation results of examples 1 to 6
As can be seen from the evaluation test results in Table 3, the surfaces of the polyester hot melt adhesive films prepared in examples 1 to 6 were all defects such as bubbles, pinholes, particles, etc., indicating good appearance; in the back adhesion test, the polyester hot melt adhesive films prepared in examples 1 to 6 were placed in an oven at 50 ℃ for 48 hours, and the peel values of the peel forces were all less than 0.2N/5cm, so that the back adhesion was negligible even at a high temperature of 50 ℃. From the results of the metal adhesion condition test, it can be seen that the metal adhesion performance of the polyester hot melt adhesive films of examples 1 to 6 is greater than the standard, and the adhesion of the polyester hot melt adhesive film prepared in example 1 to the conductor is the greatest, i.e., the metal adhesion performance is the best. From the voltage resistance test results, the voltage resistance of the polyester hot melt adhesive films of examples 1 to 6 all met the standard. From the results of the double 85 ℃ high temperature and high humidity test, it can be seen that the polyester hot melt adhesive films of examples 1 to 6 have strong high temperature resistance and high humidity resistance, i.e., good weather resistance, and the polyester hot melt adhesive films prepared by the formulation of example 1 have the best weather resistance, and after the polyester hot melt adhesive films are prevented in a high temperature and high humidity tester for 96 hours, the adhesive force to a single conductor reaches 55g/0.3mm, and the polyester hot melt adhesive films of examples 1 to 6 have lower reduction range of the adhesive force to the single conductor after the double 85 ℃ high temperature and high humidity test, so that the high temperature resistance is better. As can be seen from the results of the tests on the occurrence of voids, the polyester hot melt adhesive films of examples 1 to 6 did not exhibit the phenomenon of water permeation, i.e., did not have voids. As can be seen from the results of 96-hour snap connector tests at 85 ℃, none of the polyester hot melt adhesive films of examples 1-6 showed the situation where the adhesive overflowed onto the conductor, and thus it can be seen that the polyester hot melt adhesive films of examples 1-6 were good in high temperature resistance.
The technical principle of the present invention is described above in connection with specific embodiments. The description is made for the purpose of illustrating the principles of the invention and should not be construed in any way as limiting the scope of the invention. Based on the explanations herein, those skilled in the art will be able to conceive of other embodiments of the present invention without inventive effort, which would fall within the scope of the present invention.
Claims (10)
1. The preparation method of the super-thick high-temperature-resistant voltage-resistant polyester hot melt adhesive film is characterized by comprising the following steps of:
(1) Uniformly mixing 35-75 parts by mass of saturated polyester resin A, 10-60 parts by mass of saturated polyester resin C, 10-30 parts by mass of first flame retardant, 1-4 parts by mass of dispersing agent and 1-10 parts by mass of first filler, adding the mixture into a double-screw extruder, and extruding and granulating to obtain hot melt adhesive granules;
(2) Mixing 35-75 parts of saturated polyester resin A, 10-40 parts of saturated polyester resin B and a solvent, and then emulsifying to obtain a resin solution; adding 5-30 parts of a second flame retardant and 1-10 parts of a second filler into the resin solution, uniformly dispersing to obtain a powder liquid, and grinding the powder liquid to obtain a semi-finished product solution; sequentially adding 1-10 parts of flatting agent and 1-10 parts of curing agent into the semi-finished product solution, and adding while dispersing to obtain the polyester hot melt adhesive;
(3) Putting hot melt adhesive particles into a casting machine for heating and melting to obtain molten hot melt adhesive, coating the molten hot melt adhesive on the surface of the insulating material which is pre-coated with the printing ink, and cooling to obtain a polyester hot melt adhesive film which is sequentially provided with a first hot melt adhesive layer, a printing ink layer and an insulating layer from top to bottom; the thickness of the first hot melt adhesive layer is 100-250 mu m;
(4) And (3) coating a polyester hot melt adhesive on the surface of the first hot melt adhesive layer, wherein the coating thickness of the polyester hot melt adhesive is 25-50 mu m, and forming a second hot melt adhesive layer on the surface of the first hot melt adhesive layer after drying to obtain the super-thick high-temperature-resistant voltage-resistant polyester hot melt adhesive film.
2. The method for preparing the ultra-thick high temperature and voltage resistant polyester hot melt adhesive film according to claim 1, wherein in the step (2), the preparation method of the resin liquid comprises the following steps: putting 35-75 parts of saturated polyester resin A, 10-40 parts of saturated polyester resin B and a solvent into an emulsifying machine, emulsifying, setting the rotating speed of the emulsifying machine to 200r/min before putting the materials into the emulsifying machine, then putting the materials, after the materials are put into the emulsifying machine, increasing the rotating speed of the emulsifying machine to 300-800 r/min, emulsifying for 30-110 min, the emulsifying temperature is 25-40 ℃, the environmental humidity is 30-50%, and obtaining the resin liquid after the emulsification is finished.
3. The method for preparing the ultra-thick high temperature and voltage resistant polyester hot melt adhesive film according to claim 1, wherein in the step (2), the method for preparing the powdered liquid comprises the following steps: adding 5-30 parts of second flame retardant and 1-10 parts of second filler into the resin liquid, and performing dispersion treatment at the dispersion speed of 300-700 r/min for 20-90 min, wherein the temperature is controlled at 20-35 ℃ and the environmental humidity is 30-50% in the dispersion process to obtain the powder body liquid.
4. The method for preparing the ultra-thick high temperature and voltage resistant polyester hot melt adhesive film according to claim 1, wherein in the step (2), the semi-finished solution is prepared by the following steps: grinding the powder liquid twice, wherein the grinding time is 20-80 min each time, and the temperature is 20-35 ℃ in the grinding process to obtain a semi-finished product solution.
5. The preparation method of the ultra-thick high temperature and voltage resistant polyester hot melt adhesive film according to claim 1, wherein in the step (2), when the leveling agent and the curing agent are added to the semi-finished solution, the leveling agent is added first, and the addition is carried out while dispersing, wherein the dispersing speed is 300-800 r/min, and the dispersing time is 10-40 min; then adding a curing agent while dispersing, wherein the dispersing speed is 300-800 r/min, and the dispersing time is 10-40 min, so as to obtain the polyester hot melt adhesive.
6. The method for preparing the polyester hot melt adhesive film with the ultra-thick performance of high temperature resistance and voltage resistance as claimed in claim 1, wherein in the step (4), after the polyester hot melt adhesive is coated, the polyester hot melt adhesive is dried at the temperature of 130-150 ℃, and after the polyester hot melt adhesive is dried, a second hot melt adhesive layer is formed on the surface of the first hot melt adhesive layer, so that the polyester hot melt adhesive film with the ultra-thick performance of high temperature resistance and voltage resistance is prepared.
7. A super-thick high temperature and voltage resistant polyester hot melt adhesive film is characterized in that the super-thick high temperature and voltage resistant polyester hot melt adhesive film is prepared by the preparation method of the super-thick high temperature and voltage resistant polyester hot melt adhesive film of any one of claims 1 to 6 and sequentially comprises a second hot melt adhesive layer, a first hot melt adhesive layer, an ink layer and an insulating layer from top to bottom;
according to the mass parts, the raw materials of the first hot melt adhesive layer comprise 35-75 parts of saturated polyester resin A, 10-60 parts of saturated polyester resin C, 10-30 parts of first flame retardant, 1-4 parts of dispersant and 1-10 parts of first filler;
the raw materials of the second hot melt adhesive layer comprise 35-75 parts of saturated polyester resin A, 10-40 parts of saturated polyester resin B, 1-10 parts of flatting agent, 5-30 parts of second flame retardant, 1-10 parts of flatting agent, 1-10 parts of second filler and 1-10 parts of curing agent.
8. The ultra-thick high temperature and voltage resistant polyester hot melt adhesive film as claimed in claim 7, wherein the saturated polyester resin A has a glass transition temperature of-10 to 80 ℃, a softening point of 100 to 160 ℃, a molecular weight of 36000 to 84000, and a hydroxyl value of 2 to 6mgKOH/g;
the glass transition temperature of the saturated polyester resin C is 20-60 ℃, the softening point is 20-80 ℃, the molecular weight is 2200-42000, and the hydroxyl value is 1-4 mgKOH/g;
the glass transition temperature of the saturated polyester resin B is 0-36 ℃, the softening point is 3-80 ℃, the molecular weight is 18000-58000, and the hydroxyl value is 2-5 mgKOH/g.
9. The ultra-thick high temperature and voltage resistant polyester hot melt adhesive film according to claim 7, wherein the insulating layer has a thickness of 12-100 μm, the ink layer has a thickness of 1-2 μm, the first hot melt adhesive layer has a thickness of 100-250 μm, and the second hot melt adhesive layer has a thickness of 25-50 μm.
10. The ultra-thick high temperature and voltage resistant polyester hot melt adhesive film according to claim 7, wherein the first flame retardant and the second flame retardant are respectively selected from any one or more of a brominated flame retardant, a phosphorous flame retardant, a nitrogen flame retardant, a metal hydroxide flame retardant, a metal oxide flame retardant and a metal boride flame retardant;
the leveling agent is an acrylic leveling agent and/or a fluorine leveling agent;
the curing agent is selected from any one or combination of more of aromatic isocyanate, aliphatic isocyanate, room temperature reaction type isocyanate and blocked isocyanate.
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| WO2014000631A1 (en) * | 2012-06-26 | 2014-01-03 | 北京康得新复合材料股份有限公司 | Precoating film and preparation method thereof |
| WO2016021409A1 (en) * | 2014-08-04 | 2016-02-11 | 住友電気工業株式会社 | Adhesive composition, insulating film, insulating film production method, and flat cable |
| KR101976501B1 (en) * | 2017-11-03 | 2019-05-10 | 현대자동차 주식회사 | Insulating film and flexible flat cable |
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| CN110791219A (en) * | 2019-11-27 | 2020-02-14 | 广东莱尔新材料科技股份有限公司 | Preparation method of polyester hot melt adhesive film for FFC and polyester hot melt adhesive film |
| CN111019534A (en) * | 2019-12-24 | 2020-04-17 | 广东莱尔新材料科技股份有限公司 | Anti-hole polyester hot melt adhesive film for FFC wire and preparation method thereof |
| CN112195007A (en) * | 2020-10-12 | 2021-01-08 | 中瀚新材料科技有限公司 | Hot melt adhesive with low dielectric constant for high-frequency transmission, adhesive film thereof and preparation method |
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