CN109536078B - Hot melt adhesive film preparation method of vehicle FFC wire rod and hot melt adhesive film thereof - Google Patents
Hot melt adhesive film preparation method of vehicle FFC wire rod and hot melt adhesive film thereof Download PDFInfo
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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
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J7/00—Adhesives in the form of films or foils
- C09J7/50—Adhesives in the form of films or foils characterised by a primer layer between the carrier and the adhesive
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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
- C09D167/00—Coating compositions based on polyesters obtained by reactions forming a carboxylic ester link in the main chain; Coating compositions based on derivatives of such polymers
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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
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/60—Additives non-macromolecular
- C09D7/63—Additives non-macromolecular organic
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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
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/04—Non-macromolecular additives inorganic
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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
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/08—Macromolecular additives
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J167/00—Adhesives based on polyesters obtained by reactions forming a carboxylic ester link in the main chain; Adhesives based on derivatives of such polymers
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J7/00—Adhesives in the form of films or foils
- C09J7/20—Adhesives in the form of films or foils characterised by their carriers
- C09J7/22—Plastics; Metallised plastics
- C09J7/25—Plastics; Metallised plastics based on macromolecular compounds obtained otherwise than by reactions involving only carbon-to-carbon unsaturated bonds
- C09J7/255—Polyesters
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- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J7/00—Adhesives in the form of films or foils
- C09J7/30—Adhesives in the form of films or foils characterised by the adhesive composition
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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
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2237—Oxides; Hydroxides of metals of titanium
- C08K2003/2241—Titanium dioxide
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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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- C09J2467/00—Presence of polyester
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- C09J2467/00—Presence of polyester
- C09J2467/003—Presence of polyester in the primer coating
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
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- C09J2467/006—Presence of polyester in the substrate
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Abstract
The invention discloses a hot melt adhesive film preparation method of an FFC wire rod for a vehicle and a hot melt adhesive film thereof, wherein the method comprises the following steps: step A1, adding 20-40 parts by mass of medium molecular weight saturated polyester and 60-80 parts by mass of butanone-toluene solvent into a reaction kettle, stirring and dissolving, wherein the stirring speed is 500-1000 r/min; and step A2, cooling to room temperature after the reaction kettle in the step A1 is stirred and dissolved uniformly, then adding 0.1-5 parts of anti-blocking agent and 0.5-20 parts of low-temperature blocked isocyanate curing agent according to parts by weight, and stirring and dispersing uniformly. The primer is added with a low-temperature closed isocyanate curing agent, so that the chemical crosslinking of the primer on the PET polyester film and the hot melt adhesive is increased, the closed latent curing agent is used for the hot melt adhesive, the crosslinking degree and the cohesion of the hot melt adhesive are increased, and the cracking of the hot melt adhesive or the foaming and layering between the PET polyester film and the hot melt adhesive are avoided.
Description
Technical Field
The invention relates to the field of film manufacturing, in particular to a preparation method of a hot melt adhesive film of an automotive FFC wire rod and the hot melt adhesive film.
Background
The FFC Flat Cable is also called a Fexibe Flat Cable (FFC), namely a flexible Flat Cable, is a novel data Cable which is formed by clamping tinned Flat copper wires between an upper layer of insulating material and a lower layer of insulating material and pressing, and has the advantages of softness, random bending and folding and the like. The conventional FFC flat cable realizes hot-melt adhesion of an insulating material and a tinned flat copper wire through a hot-melt adhesive film.
The FFC wire for the vehicle is applied to a vehicle-mounted driving part in an engine compartment, and the FFC flat cable can be bent, moved and the like along with the movement of the vehicle-mounted driving part. However, the application of the existing hot melt adhesive film to the FFC wire for the vehicle has the following problems:
1. the adhesive force to the PET polyester film is not enough, the delamination problem of the hot melt adhesive and the PET polyester film is easy to occur, and even if the bottom coating treatment is carried out, the cracking problem of the bottom coating and the hot melt adhesive is easy to occur;
2. the cohesive force is not enough, the hot melt adhesive belongs to a thermoplastic cross-linking agent, the cross-linking degree is low, and the problem that the hot melt adhesive is easy to crack when the hot melt adhesive is applied to an automotive FFC wire rod with actions;
3. the strength of the bonded conductor is greatly influenced by temperature, and the bonding force of the conventional hot melt adhesive film is below 50g for the conventional 0.035mm 0.3mm (thickness and width) conductor under the room temperature test condition, belonging to thermoplastic bonding; under the conditions of high temperature (more than 50 ℃) and low temperature (less than-10 ℃), the stripping force of the hot melt adhesive film rapidly slides down, the problems of conductor and hot melt adhesive film separation and conductor fracture are easy to occur, and the requirements of vehicle-mounted FFC wires for driving action parts are difficult to meet;
4. the weather resistance is poor, the crosslinking degree of the hot melt adhesive film is low, the moisture absorption of the hot melt adhesive layer is high, and saturated polyester is easy to degrade, so that the PET polyester film and the hot melt adhesive are foamed and layered;
5. the anti-glue-overflow performance is poor, and the conventional thermoplastic hot-melt adhesive film is influenced by temperature, so that the hot-melt adhesive can gradually sink, the hot-melt adhesive overflows to the surface of the conductor, and the conductor is insulated from the connector.
Disclosure of Invention
The invention provides a preparation method of a hot melt adhesive film of an FFC wire rod for a vehicle and the hot melt adhesive film thereof for solving the problems.
In order to achieve the purpose, the invention adopts the following technical scheme:
a preparation method of a hot melt adhesive film of an FFC wire rod for a vehicle comprises the following steps:
A. preparing a primer:
step A1, adding 20-40 parts by mass of medium molecular weight saturated polyester and 60-80 parts by mass of butanone-toluene solvent into a reaction kettle, stirring and dissolving, wherein the stirring speed is 500-1000 r/min;
step A2, cooling to room temperature after the reaction kettle in the step A1 is stirred and dissolved uniformly, then adding 0.1-5 parts of anti-blocking agent and 0.5-20 parts of low-temperature closed isocyanate curing agent according to parts by weight, and stirring and dispersing uniformly;
step A3, adding 2-30 parts of isocyanate curing agent into the reaction kettle in the step A2 before coating according to the mass parts, and uniformly stirring and dispersing to obtain a primer;
B. preparing a hot melt adhesive:
step B1, adding 30-45 parts of high molecular weight saturated polyester a, 5-20 parts of high molecular weight saturated polyester B and 40-60 parts of toluene solvent into another reaction kettle according to parts by mass, heating to 60-80 ℃, and stirring for dissolving, wherein the stirring speed is 500-1000 r/min;
step B2, after stirring and dissolving the reaction kettle in the step B1, adding 0.5-10 parts of epoxy resin according to parts by weight, and stirring and dissolving uniformly;
step B3, adding 20-40 parts of flame retardant, 0-2.5 parts of anti-blocking agent and 1-3 parts of titanium dioxide into the reaction kettle in the step B2 in parts by mass, and then stirring and dispersing uniformly at a stirring speed of 1000 r/min;
step B4, grinding the reaction kettle in the step B3 to the fineness of less than 10 μm;
step B5, adding 0.5-8 parts of closed latent curing agent into the reaction kettle in the step B4 before coating according to parts by mass, and uniformly stirring and dispersing to obtain the hot melt adhesive;
C. coating, namely coating the primer on a PET (polyethylene terephthalate) polyester film, wherein the coating thickness of the primer is 0.5-2 mu m; then coating the hot melt adhesive, wherein the coating thickness of the hot melt adhesive is 15-100 mu m, and preparing a hot melt adhesive film of the vehicle FFC wire rod;
wherein the molecular weight of the medium molecular weight saturated polyester is less than that of the high molecular weight saturated polyester b, and the molecular weight of the high molecular weight saturated polyester b is less than that of the high molecular weight saturated polyester a.
The preparation method of the hot melt adhesive film of the FFC wire material for the vehicle is used for preparing the hot melt adhesive film of the FFC wire for the vehicle carrier tape action part. The prepared primer is a thermosetting primer, and a low-temperature closed isocyanate curing agent is added into the primer, so that the chemical crosslinking of the primer on the PET polyester film and the hot melt adhesive is increased, and the adhesive force of the primer on the PET polyester film and the hot melt adhesive under high and low temperature conditions is improved. The FFC wires are also known as flexible flat cables.
The hot melt adhesive uses an enclosed latent curing agent, so that the crosslinking degree and the cohesion of the hot melt adhesive are increased, the heat resistance and the hydrolysis resistance are improved, the fluidity of the adhesive layer is reduced, and the cracking of the hot melt adhesive or the foaming and layering between a PET (polyethylene terephthalate) polyester film and the hot melt adhesive are avoided; the method increases the adhesion of the hot melt adhesive to the conductor, improves the adhesion strength of the hot melt adhesive film under the conditions of high temperature (more than 50 ℃) and low temperature (less than-10 ℃), prevents the hot melt adhesive and the conductor from being separated due to the sharp sliding of the stripping force under the high and low temperature conditions, and prevents the hot melt adhesive from sinking and overflowing to the surface of the conductor under the influence of temperature to cause the insulation of the conductor and the connector, so that the hot melt adhesive meets the requirement of an FFC wire for a vehicle-mounted driving action part.
After the unsealing of the closed latent curing agent in the step B5, firstly, the hydroxyl of the high molecular weight saturated polyester B with the molecular weight smaller than that of the high molecular weight saturated polyester a and the hydroxyl of the epoxy resin are crosslinked, secondly, the epoxy group of the epoxy resin is cured, and thirdly, imidazole is crosslinked with the epoxy group of the epoxy resin, so that the adhesive force of the hot melt adhesive to the conductor is increased, and the foaming and layering between the PET polyester film and the hot melt adhesive caused by the large hygroscopicity of the hot melt adhesive layer and the degradation of the high molecular weight saturated polyester a and the high molecular weight saturated polyester B due to the low crosslinking degree are avoided.
Preferably, the molecular weight of the medium molecular weight saturated polyester is 3000-20000, and the glass transition temperature of the medium molecular weight saturated polyester is-40-30 ℃, so that the adhesive force to the PET polyester film is improved.
Preferably, the molecular weight of the high molecular weight saturated polyester a is 15000-40000, and the glass transition temperature of the high molecular weight saturated polyester a is-20-30 ℃; the molecular weight of the high molecular weight saturated polyester b is 15000-35000, and the glass transition temperature of the high molecular weight saturated polyester b is 50-120 ℃.
The high molecular weight saturated polyester a and the high molecular weight saturated polyester b have high molecular weight and excellent flexibility, and are particularly suitable for being used as hot melt adhesive matrix resin of FFC wires. The molecular weight of the high molecular weight saturated polyester a is 15000-40000, the glass transition temperature of the high molecular weight saturated polyester a is-20-30 ℃, and the flexibility is excellent. In order to improve the toughness and the glass transition temperature of the hot melt adhesive, high molecular weight saturated polyester b needs to be added.
Preferably, the deblocking temperature of the low-temperature blocked isocyanate curing agent in the step A2 is 60-130 ℃, and the low-temperature blocked isocyanate curing agent is HDI type or IPDI type; the isocyanate curing agent in the step A3 is HDI type or IPDI type.
The low-temperature closed isocyanate curing agent in the step A2 has good flexibility, increases chemical crosslinking on a PET polyester film and a hot melt adhesive after deblocking, improves cohesion, avoids cracking of a bottom coating of the prepared hot melt adhesive film, and is suitable for a working environment in which an FFC wire for a vehicle-mounted driving acting part needs to be bent, moved and the like along with the action of a vehicle-mounted carrier tape acting part.
The isocyanate curing agent in the step A3 is of HDI type or IPDI type, has excellent flexibility and weather resistance, and greatly increases the adhesive force of the base coat to the PET polyester film and promotes the chemical crosslinking of molecular weight saturated polyester in the base coat.
Preferably, the blocked latent curing agent of step B5 is an isocyanate curing agent having an imidazole type block, and has excellent adhesion to metal, mainly increasing adhesion to metal. The imidazole blocked isocyanate curing agent can be selected from HDI type, and has excellent flexibility and weather resistance.
Preferably, the epoxy resin in the step B2 is a high molecular epoxy resin, and the hydroxyl value of the epoxy resin in the step B2 is 180-200 mgKOH/g. Contains a large amount of hydroxyl, can react with the low-temperature closed isocyanate curing agent of the primer, and increases the chemical crosslinking of the hot melt adhesive on the primer; can also react with the closed latent curing agent of the hot melt adhesive to increase the crosslinking density of the hot melt adhesive and the adhesive force to the conductor.
Preferably, the anti-blocking agent comprises silica fume and wax powder, and the anti-blocking agent increases the anti-back-sticking performance of the hot melt adhesive and the primer.
Preferably, the micro silicon powder consists of silicon powders with various particle sizes.
Preferably, the flame retardant in the step B3 is a bromine-containing flame retardant or a halogen-free flame retardant, so that the flame retardance of the FFC wire is increased, and the flame retardant requirement of the wire VW-1 is met.
Preferably, the hot melt adhesive film prepared by the hot melt adhesive film preparation method of the FFC wire rod for the vehicle comprises a PET polyester film, a bottom coating and a hot melt adhesive layer, wherein the bottom coating is arranged between the PET polyester film and the hot melt adhesive layer; the primer is prepared through the steps A1 to A3, and the coating thickness of the primer is 0.5-2 mu m; the hot melt adhesive layer is prepared through the steps B1-B5, and the coating thickness of the hot melt adhesive layer is 15-100 mu m.
Drawings
The drawings are further illustrative of the invention and the content of the drawings does not constitute any limitation of the invention.
FIG. 1 is a schematic structural view of a hot melt adhesive film according to one embodiment of the present invention.
Wherein: a PET polyester film 1; a base coat layer 2; a hot melt adhesive layer 3.
Detailed Description
The technical scheme of the invention is further explained by the specific implementation mode in combination with the attached drawings.
The components and parts by mass of the primer of examples 1-12 are shown in Table 1.
TABLE 1
Examples 1-11 primers were prepared according to the following procedure:
step A1, adding medium-molecular-weight saturated polyester and a butanone-toluene solvent into a reaction kettle according to the mass parts in Table 1, and stirring for dissolving, wherein the stirring speed is 500-1000 r/min; the molecular weight of the medium molecular weight saturated polyester is 4000, and the glass transition temperature is-30 ℃;
step A2, cooling to room temperature after the reaction kettle in the step A1 is stirred and dissolved uniformly, then adding the anti-blocking agent and the low-temperature enclosed isocyanate curing agent according to the mass parts in the table 1, and stirring and dispersing uniformly;
step A3, adding an isocyanate curing agent into the reaction kettle in the step A2 before coating according to the mass parts in the table 1, and uniformly stirring and dispersing to obtain the primer.
Examples 1-12 hot melt adhesives were prepared according to the following steps:
step B1, adding 35 parts of high molecular weight saturated polyester a, 10 parts of high molecular weight saturated polyester B and 50 parts of toluene solvent into another reaction kettle according to the mass parts, heating to 70 ℃, and stirring for dissolving, wherein the stirring speed is 800 r/min; the molecular weight of the high molecular weight saturated polyester a is 30000, and the glass transition temperature is 10 ℃; the molecular weight of the high molecular weight saturated polyester b is 20000, and the glass transition temperature is 80 ℃;
step B2, after the reaction kettle in the step B1 is stirred and dissolved, adding 5 parts of epoxy resin according to the mass parts, and stirring and dissolving uniformly;
step B3, adding 30 parts of flame retardant, 2 parts of anti-blocking agent and 1 part of titanium dioxide into the reaction kettle in the step B2 according to the mass parts, and then stirring and dispersing uniformly at the stirring speed of 1000 r/min;
step B4, grinding the reaction kettle in the step B3 to the fineness of less than 10 μm;
and step B5, adding 5 parts of closed latent curing agent into the reaction kettle in the step B4 before coating according to the parts by mass, and uniformly stirring and dispersing to obtain the hot melt adhesive.
Examples 1-11 Hot melt adhesive films were prepared according to the following procedure:
the primer was coated on a PET polyester film 1 having a thickness of 25 μm, the coating thickness of the primer was 1 μm, and then a hot melt adhesive having a thickness of 35 μm was coated to prepare a hot melt adhesive film, as shown in fig. 1, with a primer layer 2 disposed between the PET polyester film 1 and a hot melt adhesive layer 3. The width of the hot melt adhesive film is 25.4mm, the hot melt adhesive surface and the adhesive surface are subjected to heat sealing, the heat sealing pressure is 0.5Mpa, the time is 1 second, the temperature is 180 ℃, and the hot melt adhesive film is cured for 1 hour after being subjected to heat sealing at 120 ℃.
Example 12 a hot melt adhesive film was prepared according to the following procedure:
a hot melt adhesive film was prepared by coating a hot melt adhesive having a thickness of 35 μm on a PET polyester film 1 having a thickness of 25 μm. The width of the hot melt adhesive film sample is 25.4mm, the hot melt adhesive surface and the adhesive surface are subjected to heat sealing, the heat sealing pressure is 0.5Mpa, the time is 1 second, the temperature is 180 ℃, and the hot melt adhesive film is cured for 1 hour after being subjected to heat sealing at 120 ℃.
The hot melt adhesive film samples prepared in the embodiments 1 to 12 are tested for the peeling strength of the base coat to the hot melt adhesive and the PET polyester film 1 at different temperatures;
placing the hot melt adhesive film samples prepared in the embodiments 1-12 for 1000 hours under the conditions of 85 ℃ and 85 humidity, and then testing the peel strength;
the yellowing resistance of the hot melt adhesive film samples prepared in examples 1 to 12 was measured.
The results of the measurements are shown in Table 2 below.
TABLE 2
From examples 1 to 12, it can be seen that the primer is added with the low-temperature blocked isocyanate curing agent, so that the chemical crosslinking of the primer on the PET polyester film 1 and the hot melt adhesive is increased, and the adhesion of the primer on the PET polyester film 1 and the hot melt adhesive under the high and low temperature conditions is improved. The low-temperature closed isocyanate curing agent has good flexibility, increases chemical crosslinking on the PET polyester film 1 and the hot melt adhesive after deblocking, improves cohesion, avoids cracking of the bottom coating 2 of the prepared hot melt adhesive film, and is suitable for a working environment in which an FFC (flexible flat cable) for a vehicle-mounted driving acting part needs to bend, move and the like along with the action of a vehicle-mounted carrier tape acting part. The isocyanate curing agent is HDI type or IPDI type, has excellent flexibility and weather resistance, greatly increases the adhesive force of the bottom coating 2 to the PET polyester film 1 and promotes the chemical crosslinking of the saturated polyester with the molecular weight in the bottom coating 2.
The components and parts by weight of the hot melt adhesives of examples 13-24 are shown in Table 3.
TABLE 3
Examples 13-24 primers were prepared according to the following procedure:
step A1, adding 20 parts of medium molecular weight saturated polyester and 60 parts of butanone-toluene solvent into a reaction kettle according to parts by mass, and stirring for dissolving, wherein the stirring speed is 500-1000 r/min; the molecular weight of the medium molecular weight saturated polyester is 15000, and the glass transition temperature is 25 ℃;
step A2, cooling to room temperature after the reaction kettle in the step A1 is stirred and dissolved uniformly, then adding 0.1 part of anti-blocking agent and 0.5 part of low-temperature blocked isocyanate curing agent according to the mass parts, and stirring and dispersing uniformly;
and step A3, adding 2 parts of isocyanate curing agent into the reaction kettle in the step A2 before coating according to the parts by mass, and uniformly stirring and dispersing to obtain the primer.
Examples 13-24 Hot melt adhesives were prepared according to the following steps:
step B1, adding the high molecular weight saturated polyester a, the high molecular weight saturated polyester B and a toluene solvent into another reaction kettle according to the mass parts in the table 3, heating to 60-80 ℃, and stirring for dissolving, wherein the stirring speed is 500-1000 r/min; the molecular weight of the high molecular weight saturated polyester a is 35000, and the glass transition temperature is-10 ℃; the molecular weight of the high molecular weight saturated polyester b is 20000, and the glass transition temperature is 100 ℃;
step B2, after the reaction kettle in the step B1 is stirred and dissolved, adding epoxy resin according to the mass parts in the table 3, and stirring and dissolving uniformly;
step B3, adding the flame retardant, the anti-blocking agent and the titanium dioxide into the reaction kettle in the step B2 according to the mass parts in the table 3, and then stirring and dispersing uniformly at the stirring speed of 1000 r/min;
step B4, grinding the reaction kettle in the step B3 to the fineness of less than 10 μm;
and step B5, adding the closed latent curing agent into the reaction kettle in the step B4 before coating according to the mass parts in the table 3, and uniformly stirring and dispersing to obtain the hot melt adhesive.
Examples 13-24 Hot melt adhesive films were prepared according to the following procedure:
the primer was coated on a PET polyester film 1 having a thickness of 25 μm, the coating thickness of the primer was 1 μm, and then a hot melt adhesive having a thickness of 35 μm was coated to prepare a hot melt adhesive film, as shown in fig. 1, with a primer layer 2 disposed between the PET polyester film 1 and a hot melt adhesive layer 3. The width of the hot melt adhesive film is 25.4mm, the hot melt adhesive surface and the adhesive surface are subjected to heat sealing, the heat sealing pressure is 0.5Mpa, the time is 1 second, the temperature is 180 ℃, and the hot melt adhesive film is cured for 1 hour after being subjected to heat sealing at 120 ℃.
The hot melt adhesive film samples prepared in examples 13 to 24 were tested for peel strength at-40 ℃ and 85 ℃ to observe the failure of the hot melt adhesive.
The hot melt adhesive film samples prepared in examples 13 to 24 were processed on a machine and pressed into FFC wires with conductor specifications of 0.035mm by 0.3mm,51 pin.
The FFC wire rods prepared in examples 13 to 24 were subjected to a reciprocal deflection test at 85 ℃ for 100 times/min and 10 ten thousand times, and then the conditions of the hot melt adhesive film and the conductor were observed: whether there is delamination or cracking, whether the conductor is broken, etc.
The FFC wires prepared in the examples 13 to 24 were placed under 85 ℃ and 85 humidity conditions for 2000 hours, and the problems of delamination and foaming of the FFC wires were observed.
The FFC wire prepared in the embodiment 13-24 is put on a connector, placed in an oven at 125 ℃, tested for 96 hours, and then whether hot melt adhesive exists on the surface of the conductor or not is detected.
The FFC wires prepared in examples 13 to 24 were tested for the strength of the adherent conductors at room temperature.
The results of the measurements are shown in Table 4 below.
TABLE 4
From examples 13 to 24, it can be seen that the high molecular weight saturated polyester a and the high molecular weight saturated polyester b have a large molecular weight and excellent flexibility, and are particularly suitable for being used as hot melt adhesive matrix resins for FFC wires. The molecular weight of the high molecular weight saturated polyester a is 15000-40000, the glass transition temperature of the high molecular weight saturated polyester a is-20-30 ℃, and the flexibility is excellent. In order to improve the toughness and the glass transition temperature of the hot melt adhesive, high molecular weight saturated polyester b needs to be added;
the epoxy resin in the step B2 is macromolecular epoxy resin, contains a large amount of hydroxyl, and can react with the low-temperature closed isocyanate curing agent of the primer, so that the chemical crosslinking of the primer by the hot melt adhesive is increased; the epoxy resin can also react with the closed latent curing agent of the hot melt adhesive to increase the crosslinking density of the hot melt adhesive and the adhesive force to the conductor;
the closed latent curing agent of the step B5 is an imidazole blocked isocyanate curing agent, has excellent adhesion to metal and mainly increases the adhesion to metal. After the unsealing of the closed latent curing agent in the step B5, firstly, the hydroxyl of the high molecular weight saturated polyester B with the molecular weight smaller than that of the high molecular weight saturated polyester a and the hydroxyl of the epoxy resin are crosslinked, secondly, the epoxy group of the epoxy resin is cured, and thirdly, imidazole is crosslinked with the epoxy group of the epoxy resin, so that the adhesive force of the hot melt adhesive to the conductor is increased, and the foaming and layering between the PET polyester film 1 and the hot melt adhesive caused by the large hygroscopicity of the hot melt adhesive layer and the degradation of the high molecular weight saturated polyester a and the high molecular weight saturated polyester B due to the low crosslinking degree are avoided. The imidazole blocked isocyanate curing agent can be selected from HDI type, and has excellent flexibility and weather 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 (7)
1. A preparation method of a hot melt adhesive film of an FFC wire rod for a vehicle is characterized by comprising the following steps:
A. preparing a primer:
step A1, adding 20-40 parts by mass of medium molecular weight saturated polyester and 60-80 parts by mass of butanone-toluene solvent into a reaction kettle, stirring and dissolving, wherein the stirring speed is 500-1000 r/min;
step A2, cooling to room temperature after the reaction kettle in the step A1 is stirred and dissolved uniformly, then adding 0.1-5 parts of anti-blocking agent and 0.5-20 parts of low-temperature closed isocyanate curing agent according to parts by weight, and stirring and dispersing uniformly;
step A3, adding 2-30 parts of isocyanate curing agent into the reaction kettle in the step A2 before coating according to the mass parts, and uniformly stirring and dispersing to obtain a primer;
B. preparing a hot melt adhesive:
step B1, adding 30-45 parts of high molecular weight saturated polyester a, 5-20 parts of high molecular weight saturated polyester B and 40-60 parts of toluene solvent into another reaction kettle according to parts by mass, heating to 60-80 ℃, and stirring for dissolving, wherein the stirring speed is 500-1000 r/min;
step B2, after stirring and dissolving the reaction kettle in the step B1, adding 0.5-10 parts of epoxy resin according to parts by weight, and stirring and dissolving uniformly;
step B3, adding 20-40 parts of flame retardant, 0-2.5 parts of anti-blocking agent and 1-3 parts of titanium dioxide into the reaction kettle in the step B2 in parts by mass, and then stirring and dispersing uniformly at a stirring speed of 1000 r/min;
step B4, grinding the reaction kettle in the step B3 to the fineness of less than 10 μm;
step B5, adding 0.5-8 parts of closed latent curing agent into the reaction kettle in the step B4 before coating according to parts by mass, and uniformly stirring and dispersing to obtain the hot melt adhesive;
C. coating, namely coating the primer on a PET (polyethylene terephthalate) polyester film, wherein the coating thickness of the primer is 0.5-2 mu m; then coating the hot melt adhesive, wherein the coating thickness of the hot melt adhesive is 15-100 mu m, and preparing a hot melt adhesive film of the vehicle FFC wire rod;
wherein the molecular weight of the medium molecular weight saturated polyester is less than that of the high molecular weight saturated polyester b, and the molecular weight of the high molecular weight saturated polyester b is less than that of the high molecular weight saturated polyester a;
the blocked latent curing agent in the step B5 is an imidazole blocked isocyanate curing agent, and the imidazole blocked isocyanate curing agent is HDI;
the epoxy resin in the step B2 is a high molecular epoxy resin, and the hydroxyl value of the epoxy resin in the step B2 is 180-200 mgKOH/g;
the deblocking temperature of the low-temperature blocked isocyanate curing agent in the step A2 is 60-130 ℃, and the low-temperature blocked isocyanate curing agent is HDI type or IPDI type;
the isocyanate curing agent in the step A3 is HDI type or IPDI type.
2. The method of preparing a hot melt adhesive film for FFC wires for vehicles according to claim 1, wherein:
the molecular weight of the medium molecular weight saturated polyester is 3000-20000, and the glass transition temperature of the medium molecular weight saturated polyester is-40-30 ℃.
3. The method of preparing a hot melt adhesive film for FFC wires for vehicles according to claim 1, wherein:
the molecular weight of the high molecular weight saturated polyester a is 15000-40000, and the glass transition temperature of the high molecular weight saturated polyester a is-20-30 ℃;
the molecular weight of the high molecular weight saturated polyester b is 15000-35000, and the glass transition temperature of the high molecular weight saturated polyester b is 50-120 ℃.
4. The method of preparing a hot melt adhesive film for FFC wires for vehicles according to claim 1, wherein: the anti-blocking agent comprises micro silicon powder and wax powder.
5. The method of preparing a hot melt adhesive film for FFC wires for vehicles according to claim 4, wherein: the micro silicon powder consists of silicon powders with various particle sizes.
6. The method of preparing a hot melt adhesive film for FFC wires for vehicles according to claim 1, wherein: the flame retardant in the step B3 is a bromine-containing flame retardant or a halogen-free flame retardant.
7. The hot melt adhesive film produced by the method for producing a hot melt adhesive film using the FFC wire for vehicles of any one of claims 1 to 6, characterized in that: the PET film comprises a PET polyester film, a bottom coating and a hot melt adhesive layer, wherein the bottom coating is arranged between the PET polyester film and the hot melt adhesive layer;
the primer is prepared through the steps A1 to A3, and the coating thickness of the primer is 0.5-2 mu m;
the hot melt adhesive layer is prepared through the steps B1-B5, and the coating thickness of the hot melt adhesive layer is 15-100 mu m.
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| CN110183982A (en) * | 2019-04-17 | 2019-08-30 | 广东莱尔新材料科技股份有限公司 | A kind of High-temp.-resistant hot-melt adhesive film and FFC wire rod for FFC wire rod |
| CN110527470A (en) * | 2019-08-29 | 2019-12-03 | 苏州瀚海新材料有限公司 | A kind of Adhesive composition for FFC |
| CN110982440B (en) * | 2019-12-20 | 2022-02-01 | 江门新时代胶粘科技有限公司 | Medical glove quick-binding adhesive tape and preparation method thereof |
| CN111019534B (en) * | 2019-12-24 | 2022-05-17 | 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 |
| CN114644747A (en) * | 2021-11-27 | 2022-06-21 | 长春富晟汽车技术研发有限公司 | Method for improving wet and heat aging resistance of PUR high-resilience foam |
| CN114196348A (en) * | 2021-11-29 | 2022-03-18 | 安徽创研新材料有限公司 | Environment-friendly hot melt adhesive film and preparation method thereof |
| CN114412328B (en) * | 2022-01-21 | 2024-08-20 | 广东嘉盛家具有限公司 | Composite solid wood door |
| CN114774011B (en) * | 2022-05-26 | 2024-08-27 | 广东莱尔新材料科技股份有限公司 | Double-sided hot melt adhesive film for FFC cable and preparation method thereof |
| CN116376464A (en) * | 2023-04-10 | 2023-07-04 | 杭州师范大学 | Hot melt adhesive film with high adhesive strength and high heat resistance, and preparation method and application thereof |
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