CN111635713A - Anti-adhesion binder, anti-adhesion hot melt adhesive film and FFC wire - Google Patents
Anti-adhesion binder, anti-adhesion hot melt adhesive film and FFC wire Download PDFInfo
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- CN111635713A CN111635713A CN202010489951.5A CN202010489951A CN111635713A CN 111635713 A CN111635713 A CN 111635713A CN 202010489951 A CN202010489951 A CN 202010489951A CN 111635713 A CN111635713 A CN 111635713A
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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
- C09J7/30—Adhesives in the form of films or foils characterised by the adhesive composition
- C09J7/35—Heat-activated
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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
- C09J11/02—Non-macromolecular additives
- C09J11/06—Non-macromolecular additives 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
- 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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- 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
- C09J7/20—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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- 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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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B7/00—Insulated conductors or cables characterised by their form
- H01B7/17—Protection against damage caused by external factors, e.g. sheaths or armouring
- H01B7/29—Protection against damage caused by extremes of temperature or by flame
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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
- C08L2201/00—Properties
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
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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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- 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
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
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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
- C09J2467/00—Presence of polyester
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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
- C09J2467/00—Presence of polyester
- C09J2467/006—Presence of polyester in the substrate
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- Chemical Kinetics & Catalysis (AREA)
- Inorganic Chemistry (AREA)
- Adhesives Or Adhesive Processes (AREA)
Abstract
An anti-sticking adhesive, an anti-sticking hot melt adhesive film and an FFC wire, the adhesive comprising: saturated polyester resin A, saturated polyester resin B, saturated polyester resin C, a flame retardant, a curing agent and a filler; the glass transition temperature of the saturated polyester resin A is 20-25 ℃; the glass transition temperature of the saturated polyester resin B is 50-60 ℃; the saturated polyester resin C is crystalline saturated polyester, and the glass transition temperature of the saturated polyester resin C is-45 to-20 ℃; a hot melt adhesive film comprising: an insulating layer, a precoat layer and a binder layer; an FFC wire material which presses the hot melt adhesive film to the surface of the conductor; the hot melt adhesive film prepared by the adhesive can adapt to the environment of 60 ℃, does not adhere after 7 days, and eliminates the influence of high temperature on the hot melt adhesive film; the hot melt adhesive film can also achieve the effect of long-term high temperature resistance after being matched with a conductor to form an FFC wire, and is placed for at least 85 hours in an environment of 115 ℃.
Description
Technical Field
The invention relates to the technical field of hot melt adhesive films, in particular to an anti-reverse-adhesion adhesive and an anti-reverse-adhesion hot melt adhesive film.
Background
In the prior art, a hot melt adhesive film is prepared for convenient storage and is often required to be rolled up, and in the rolling process, an adhesive layer in the hot melt adhesive film can contact an insulating layer; the hot melt adhesive film in the prior art needs to be stored in a shady and cool and light-proof environment, and needs to be prevented from a high-temperature environment all year round; because hot melt adhesive film exposes in sunshine or steam, can lead to the heating of the binder layer in the hot melt adhesive film, it is integrative with the insulating layer adhesion, and because the heat dissipation is not enough under the rolling state, the anti-phenomenon of gluing has more aggravated, is unfavorable for unreeling under the processing state. The hot melt adhesive film in the prior art is narrow in non-anti-sticking temperature range and easy to anti-stick in a high-temperature environment.
Disclosure of Invention
The invention aims to provide an anti-reverse-adhesion binder which is prepared by using saturated polyester resin A, saturated polyester resin B and saturated polyester resin C, matching the glass transition temperatures of the saturated polyester resin A, the saturated polyester resin B and the saturated polyester resin C, and selecting the saturated polyester resin C as a crystalline saturated polyester according to a system of the formula.
The invention also provides an anti-reverse-adhesion hot melt adhesive film, which comprises: an insulating layer, a precoat layer and a binder layer; the adhesive layer is made of the adhesive.
The invention also provides an FFC wire, which is used for laminating the hot melt adhesive film on the outer surface of the conductor.
In order to achieve the purpose, the invention adopts the following technical scheme:
an anti-reverse-adhesion binder comprises the following components in percentage by weight: 35-40% of saturated polyester resin A, 10-15% of saturated polyester resin B, 1-5% of saturated polyester resin C, 35-45% of flame retardant, less than 1% of curing agent and the balance of filler;
the glass transition temperature of the saturated polyester resin A is 20-25 ℃;
the glass transition temperature of the saturated polyester resin B is 50-60 ℃;
the saturated polyester resin C is a crystalline saturated polyester, and the glass transition temperature of the saturated polyester resin C is-45 to-20 ℃.
Preferably, the flame retardant comprises: at least one of a bromine-based flame retardant, a phosphorus-based flame retardant, a nitrogen-based flame retardant, a metal hydroxide-based flame retardant, a metal oxide flame retardant and a metal boride flame retardant.
Preferably, the curing agent is one or a combination of two or more of aromatic isocyanate, aliphatic isocyanate, room temperature reactive isocyanate and blocked isocyanate.
Preferably, the room temperature reactive isocyanate comprises: any one or combination of a dimer of diisocyanate or a polymer thereof, a dimer of 2, 4-diphenylmethane diisocyanate or a polymer thereof, a dimer of hexamethylene diisocyanate or a polymer thereof, a dimer of isophorone diisocyanate or a polymer thereof, a dimer of xylylene diisocyanate or a polymer thereof, and an adduct of the above isocyanates.
Preferably, the filler comprises: at least one of fumed silica, titanium dioxide and talc.
An anti-tack hot melt adhesive film, comprising: an insulating layer, a precoat layer and a binder layer;
the insulating layer, the precoating layer and the binder layer are sequentially attached from top to bottom; the adhesive layer is made of the adhesive.
Preferably, the precoat layer is prepared by mixing at least a coupling agent and an isocyanate; the content ratio of the coupling agent to the isocyanate is 1: (20-100).
Preferably, the insulating layer is a PET insulating layer.
Preferably, the thickness of the insulating layer is 12-50 μm; the thickness of the pre-coating layer is 1-3 mu m; the thickness of the adhesive layer is 20-50 mu m.
An FFC wire is laminated on the outer surface of a conductor by using the prepared hot melt adhesive film.
The invention has the beneficial effects that:
according to the anti-reverse-adhesion binder, the saturated polyester resin A, the saturated polyester resin B and the saturated polyester resin C are matched, the state and Tg of polyester are strictly controlled, and the glass transition temperature of the saturated polyester resin A is 20-25 ℃; the glass transition temperature of the saturated polyester resin B is 50-60 ℃; the saturated polyester resin C is crystalline saturated polyester, the glass transition temperature of the saturated polyester resin C is-45 to-20 ℃, the anti-reverse-adhesion effect of the material can be improved, the hot melt adhesive film can not be reversely adhered after being taken out after 7 days when being placed in an environment of 60 ℃, and the influence of high temperature in summer on the hot melt adhesive film can be eliminated; meanwhile, after the hot melt adhesive film is matched with a conductor to form the FFC wire, the effect of long-term high temperature resistance can be achieved, and the FFC wire can be placed at 115 ℃ for at least 85 hours and is suitable for products for marine transportation.
Detailed Description
The technical solution of the present invention is further explained by the following embodiments.
An anti-reverse-adhesion binder comprises the following components in percentage by weight: 35-40% of saturated polyester resin A, 10-15% of saturated polyester resin B, 1-5% of saturated polyester resin C, 35-45% of flame retardant, less than 1% of curing agent and the balance of filler;
the glass transition temperature of the saturated polyester resin A is 20-25 ℃;
the glass transition temperature of the saturated polyester resin B is 50-60 ℃;
the saturated polyester resin C is a crystalline saturated polyester, and the glass transition temperature of the saturated polyester resin C is-45 to-20 ℃.
In the scheme, the anti-reverse-adhesion binder is prepared by matching saturated polyester resin A, saturated polyester resin B and saturated polyester resin C, strictly controlling the state and Tg of polyester, wherein the glass transition temperature of the saturated polyester resin A is 20-25 ℃; the glass transition temperature of the saturated polyester resin B is 50-60 ℃; the saturated polyester resin C is crystalline saturated polyester, the glass transition temperature of the saturated polyester resin C is-45 to-20 ℃, the anti-reverse-adhesion effect of the material can be improved, the hot melt adhesive film can not be reversely adhered after being taken out after 7 days when being placed in an environment of 60 ℃, and the influence of high temperature in summer on the hot melt adhesive film can be eliminated; meanwhile, after the hot melt adhesive film is matched with a conductor to form the FFC wire, the effect of long-term high temperature resistance can be achieved, and the FFC wire can be placed at 115 ℃ for at least 85 hours and is suitable for products for marine transportation.
Preferably, the flame retardant comprises: at least one of a bromine-based flame retardant, a phosphorus-based flame retardant, a nitrogen-based flame retardant, a metal hydroxide-based flame retardant, a metal oxide flame retardant and a metal boride flame retardant.
Brominated flame retardants such as polybrominated diphenyl ethers, tribromophenols, brominated phthalic anhydrides, brominated bisphenol A, brominated alcohols, brominated polymers, and other brominated flame retardants such as pentabromotoluene, hexabromocyclododecane, decabromodiphenylethane, dibromophenylglycidyl ether ethyl brominated flame retardant monomers, and the like.
The phosphorus flame retardant can be inorganic phosphorus flame retardant or organic phosphorus flame retardant; wherein the inorganic phosphorus flame retardant can be red phosphorus or ammonium polyphosphate; the organic phosphorus flame retardant can be phosphate or a phosphorus heterocyclic compound; examples of the phosphoric acid esters include triphenyl phosphate, ethylphenyl phosphate, t-butylphenyl phosphate, tetraarylarylene diphosphate, resorcinol phosphate, tetraphenyl bisphenol A-diphosphate, etc.; the phosphorus heterocyclic compound may be, for example, a monocyclic phosphorus heterocyclic compound, a phosphorus spiro compound and a cage-type phosphorus compound.
The nitrogen flame retardant can be melamine, cyanuric acid, melamine derivatives, dicyandiamide, urea and derivatives thereof; derivatives of melamine such as melamine polyphosphate, melamine phosphate, melamine cyanurate.
The metal hydroxide flame retardant may be aluminum hydroxide or magnesium hydroxide.
The metal oxide may be antimony trioxide, antimony oxide, iron oxide, tin oxide, etc.
The metal boride flame retardant can be zinc borate or barium borate.
The flame retardant used in the adhesive of the present invention may be one or a mixture of several of the above flame retardants. Preferred are bromine-based flame retardants or phosphorus-based flame retardants.
Preferably, the curing agent is one or a combination of two or more of aromatic isocyanate, aliphatic isocyanate, room temperature reactive isocyanate and blocked isocyanate.
The isocyanate is used as a curing agent, and may be one or a mixture of aromatic isocyanate, aliphatic isocyanate, room temperature-reactive isocyanate, and blocked (high temperature-deblocking) isocyanate. The room temperature reactive isocyanate may be Toluene Diisocyanate (TDI) and its dimer, trimer, 2, 4-diphenylmethane diisocyanate (MDI) and its dimer, trimer, Hexamethylene Diisocyanate (HDI) and its dimer, trimer, isophorone diisocyanate (IPDI) and its dimer, trimer, Xylylene Diisocyanate (XDI) and its dimer, trimer, or adduct of the above isocyanates; the blocked isocyanate can be blocked isocyanate synthesized by phenol, polyether diol and the room-temperature reaction type isocyanate.
Preferably, the room temperature reactive isocyanate comprises: any one or combination of a dimer of diisocyanate or a polymer thereof, a dimer of 2, 4-diphenylmethane diisocyanate or a polymer thereof, a dimer of hexamethylene diisocyanate or a polymer thereof, a dimer of isophorone diisocyanate or a polymer thereof, a dimer of xylylene diisocyanate or a polymer thereof, and an adduct of the above isocyanates.
Preferably, the filler comprises: at least one of fumed silica, titanium dioxide and talc.
An anti-tack hot melt adhesive film, comprising: an insulating layer, a precoat layer and a binder layer;
the insulating layer, the precoating layer and the binder layer are sequentially attached from top to bottom; the adhesive layer is made of the adhesive.
Preferably, the precoat layer is prepared by mixing at least a coupling agent and an isocyanate;
the content ratio of the coupling agent to the isocyanate is 1: (20-100).
The precoat layer can promote the combination degree between the insulating layer and the adhesive layer, and prevent the poor compatibility of the insulating layer and the adhesive layer from affecting the performance.
Preferably, the insulating layer is a PET insulating layer.
Preferably, the thickness of the insulating layer is 12-50 μm; the thickness of the pre-coating layer is 1-3 mu m; the thickness of the adhesive layer is 20-50 mu m.
An FFC wire is laminated on the outer surface of a conductor by using the prepared hot melt adhesive film.
And (3) performance testing:
anti-tack: a roll of 120mm multiplied by 500m adhesive film is placed into a 60-degree oven in a simulation mode; and taking out the adhesive film after 7 days, and putting the adhesive film on a machine for unreeling. When the whole roll of the adhesive film is 500m, the adhesive film can be unwound, and the whole roll of the adhesive film can be pulled out to avoid sticking the PET on the back, namely the PET is qualified. When the adhesive film is degummed and sticky at a certain position and can not be unwound, the adhesive film is unqualified.
Heat resistance: after the adhesive film is pressed on the bare copper conductor for molding, the two ends of the wire rod are cut to be flat, so that the conductor is completely wrapped in the adhesive film and is level; the wire rod was placed in an oven at 115 ℃ and the time taken to observe the exposure of the conductor in the wire rod from the adhesive film was recorded every hour, and the heat resistance of the adhesive film was confirmed from the time taken to expose the conductor.
PET adhesion force: taking 2 adhesive films, pressing the adhesive surfaces of the 2 adhesive films to be opposite to the adhesive films at the temperature of 180 ℃ to enable the 2 adhesive films to be adhered together, cutting the pressed sample plate into a sample plate with the length of 1 inch, and performing a stripping test on the adhesive surfaces by using a tensile machine at the stripping speed of 100 mm/min. If the peeling force is more than 1kg/IN, the product is qualified; otherwise, the product is not qualified.
Adhesion of the metal conductor: the FFC forming machine presses the bare copper conductor with the specification of 0.035X0.3 at the temperature of 180 ℃ and the speed of 1.5 m/min. Then, performing an adhesion test on a single conductor by using a pulling machine at a speed of 200mm/min, wherein the qualification is that the adhesion requirement is more than 20 g; otherwise, the product is not qualified.
Example A:
example A was prepared according to Table 1 by mixing saturated polyester resin A, saturated polyester resin B, saturated polyester resin C, flame retardant, curing agent and filler.
Wherein the glass transition temperature of the saturated polyester resin A is 22 ℃; the glass transition temperature of the saturated polyester resin B is 50 ℃; the saturated polyester resin C is crystalline saturated polyester, and the glass transition temperature of the saturated polyester resin C is-37 ℃; the flame retardant is inorganic phosphorus flame retardant; the curing agent is room temperature reaction type isocyanate and is the combination of diisocyanate and 2, 4-diphenylmethane diisocyanate; the filler is hydrophobic silicon dioxide and titanium dioxide. Printing a precoating layer prepared from a coupling agent and isocyanate (the content ratio of the coupling agent to the isocyanate is 1: 20) on a PET (polyethylene terephthalate) insulating layer by a printer and curing, coating a binder on the precoating layer by a coating machine and curing to prepare a hot melt adhesive film; the hot melt adhesive films obtained were subjected to performance tests, as shown in table 2.
TABLE 1 formulation of example A
TABLE 2 comparison of the Properties of example A
| Performance of | Comparative example A1 | Comparative example A2 | Comparative example A3 | Example A1 |
| Anti-tack property | Fail to be qualified | Fail to be qualified | Fail to be qualified | Qualified |
| Heat resistance (h) | 3 | 24 | 55 | 96 |
| Adhesion of PET | Fail to be qualified | Fail to be qualified | Qualified | Qualified |
| Adhesion of metallic conductors | Fail to be qualified | Fail to be qualified | Qualified | Qualified |
Description of the drawings:
1. as can be seen from comparison between the comparative example A1 and the example A1, in the scheme, the Tg of the saturated polyester resin A is controlled to be 20-25 ℃, and the saturated polyester resin B and the saturated polyester resin C can be matched, so that the anti-reverse viscosity of the adhesive layer is effectively improved; comparative example a1, however, was poor in anti-tack performance due to the absence of addition of saturated polyester resin a, and was readily adhered to the back side PET; and as the main resin, because the adhesive system lacks the saturated polyester resin A, the proportion of the comparative example A1 is not balanced, the heat resistance is insufficient, and the adhesive can be placed at 115 ℃ for 2 hours.
2. As shown by comparing the comparative example A2 with the example A1, the comparative example A2 does not add the saturated polyester resin B, but the Tg of the saturated polyester resin B is 50-60 ℃, so that after the saturated polyester resin A and the saturated polyester resin C are matched, the adhesive capacity of the adhesive film is improved, the adhesiveness of the hot melt adhesive film to PET and metal at the processing temperature of 175-190 ℃ is further improved, and the reverse adhesion at the normal temperature (0-40 ℃) is prevented. The absence of the saturated polyester resin B in comparative example a2 resulted in a hot melt adhesive film having poor anti-tack properties at normal temperature and poor adhesion to PET and metal.
3. Comparative example A3 in this case, the saturated polyester resin C is a crystalline saturated polyester, as can be seen by comparing comparative example A3 with example A1; because the saturated polyester resin CTg is low, the adhesive force to the base material and the metal conductor is excellent, and after the saturated polyester resin A and the saturated polyester resin B are matched, the adhesive force is not sensitive to the transportation temperature below 60 ℃ in a stable state, so that the anti-reverse adhesion can be improved. In contrast, comparative example A3, in which the saturated polyester resin C was not added, was poor in anti-tack property and heat resistance, and was left alone at 115 ℃ for 55 hours.
In conclusion, in the embodiment a1, the saturated polyester resin a, the saturated polyester resin B and the saturated polyester resin C are added at the same time; wherein the Tg of the saturated polyester resin A is 20-25 ℃; the Tg of the saturated polyester resin B is 50-60 ℃; the saturated polyester resin C is a crystalline saturated polyester, and the Tg of the saturated polyester resin C is-45 to-20 ℃. The anti-reverse viscosity, heat resistance and base material adhesion of the product can be improved simultaneously by matching with a flame retardant, a curing agent and a filler; the prepared adhesive film can still be normally unwound in an environment of 60 ℃, so that the anti-sticking phenomenon of products can not occur, and the anti-sticking phenomenon of the adhesive film in the hot weather or direct solar radiation environment in the prior art is avoided; meanwhile, after the prepared material is pressed into an FFC wire, the prepared material has stable heat resistance and can stay for 96 hours in an environment of 115 ℃ without being separated from a conductor.
Example B:
example B was prepared by mixing 40% saturated polyester resin a, 10% saturated polyester resin B, 5% saturated polyester resin C, 40% flame retardant, 1% curing agent, and the balance filler, by weight.
Wherein, the Tg of the saturated polyester resin a, the saturated polyester resin B and the saturated polyester resin C are shown in table 3; the saturated polyester resin C is a crystalline saturated polyester. The flame retardant is inorganic phosphorus flame retardant; the curing agent is room temperature reaction type isocyanate and is the combination of diisocyanate and 2, 4-diphenylmethane diisocyanate; the filler is hydrophobic silicon dioxide and titanium dioxide. Printing a precoating layer prepared from a coupling agent and isocyanate (the content ratio of the coupling agent to the isocyanate is 1: 20) on a PET (polyethylene terephthalate) insulating layer by a printer and curing, coating a binder on the precoating layer by a coating machine and curing to prepare a hot melt adhesive film; the hot melt adhesive film obtained was subjected to anti-tack and heat resistance tests, as shown in table 3.
TABLE 3 glass transition temperature of saturated polyester resin A in example B
Description of the drawings:
as can be seen from the comparison of comparative example B with example B, the Tg of the saturated polyester resin A in comparative example B1 and comparative example B2 is out of the range of 20 to 25 ℃, and although the Tg of the saturated polyester resin B is within 50 to 60 ℃ and the Tg of the saturated polyester resin C is within-45 to-20 ℃, the comparative example B1 and comparative example B2 are equivalent to the large difference in performance between examples B1 and B3; as in comparative example B1, the Tg of its saturated polyester resin a was 2 ℃ lower than that of example B1, but the anti-tack of comparative example B1 was poor; the stripping of comparative example B1 resulted in a slight anti-sticking phenomenon, which is not in accordance with the harsh requirements of the present protocol; in the comparative example B2, the Tg of the saturated polyester resin A is 3 ℃ higher than that of the example B3, so that the conductor is exposed from the adhesive film after the saturated polyester resin A stays for 72 hours in an environment of 115 ℃, and the thermal stability is reduced from 90 hours to 72 hours; in the examples B1-B3, the Tg of the saturated polyester resin A is within the range of 20-25 ℃, and the performances of the saturated polyester resin A such as non-tack, high heat resistance and high adhesion are satisfied, which indicates that the Tg of the saturated polyester resin A is within the range of 20-25 ℃.
Example C:
example C was prepared by mixing 40% saturated polyester resin a, 10% saturated polyester resin B, 5% saturated polyester resin C, 40% flame retardant, 1% curing agent, and the balance filler, by weight.
Wherein the glass transition temperatures of the saturated polyester resin a, the saturated polyester resin B and the saturated polyester resin C are shown in table 4; the saturated polyester resin C is a crystalline saturated polyester. The flame retardant is inorganic phosphorus flame retardant; the curing agent is room temperature reaction type isocyanate and is the combination of diisocyanate and 2, 4-diphenylmethane diisocyanate; the filler is hydrophobic silicon dioxide and titanium dioxide. Printing a precoating layer prepared from a coupling agent and isocyanate (the content ratio of the coupling agent to the isocyanate is 1: 20) on a PET (polyethylene terephthalate) insulating layer by a printer and curing, coating a binder on the precoating layer by a coating machine and curing to prepare a hot melt adhesive film; the hot melt adhesive films obtained were subjected to performance tests, as shown in table 4.
TABLE 4 glass transition temperature of saturated polyester resin B in example C
Description of the drawings:
as can be seen from the comparison of comparative example C with example C, the Tg of the saturated polyester resin B in comparative example C1 and comparative example C2 is outside the range of 50 to 60 ℃; likewise, both pairs of ratios exhibited performance defects, as in comparative example C1, since the Tg of its saturated polyester resin B was 3 ℃ lower than that of example C1, the 3 ℃ difference resulted in a decrease in the anti-blocking property of comparative example C1, and a slight anti-blocking phenomenon occurred, although there was less influence in heat resistance and substrate adhesion. The Tg of the saturated polyester resin B in comparative example C2 was 2 ℃ higher than that of example C3, but it exhibited moderate tack-free behavior at 60 ℃. In the embodiments C1-C3, the Tg of the saturated polyester resin B is controlled within the range of 50-60 ℃, and the performances of the saturated polyester resin B can meet the requirements of no reverse adhesion, high heat resistance and high adhesion, which indicates that the Tg of the saturated polyester resin B in the formula system is within the range of 50-60 ℃ to improve the reverse adhesion resistance.
Example D:
example D was prepared by mixing 40% saturated polyester resin a, 10% saturated polyester resin B, 5% saturated polyester resin C, 40% flame retardant, 1% curing agent, and the balance filler, by weight.
Wherein the glass transition temperatures of the saturated polyester resin a, the saturated polyester resin B and the saturated polyester resin C are shown in table 5; the saturated polyester resin C is a crystalline saturated polyester. The flame retardant is inorganic phosphorus flame retardant; the curing agent is room temperature reaction type isocyanate and is the combination of diisocyanate and 2, 4-diphenylmethane diisocyanate; the filler is hydrophobic silicon dioxide and titanium dioxide. Printing a precoating layer prepared from a coupling agent and isocyanate (the content ratio of the coupling agent to the isocyanate is 1: 20) on a PET (polyethylene terephthalate) insulating layer by a printer and curing, coating a binder on the precoating layer by a coating machine and curing to prepare a hot melt adhesive film; the hot melt adhesive films obtained were subjected to performance tests, as shown in table 5.
TABLE 5 glass transition temperature of saturated polyester resin C of example D
Description of the drawings:
as can be seen from comparison of comparative examples D1-D2 with examples D1-D3, the Tg of the crystalline saturated polyester resin C has a large influence on the properties of the hot melt adhesive film; the comparison example D, no matter higher or lower than 5 ℃, can affect the anti-reverse viscosity and heat resistance of the hot melt adhesive film; comparative example D1 wherein the Tg of saturated polyester resin C was 5 ℃ lower than that of example D1, but this difference eventually resulted in comparative example D1 having poor anti-tack effect and the heat resistance decreased from 92h to 74h of example D1; comparative example D2 wherein the Tg of saturated polyester resin C was 5 ℃ higher than that of example D3, but this difference eventually led to deterioration of the anti-tack effect of comparative example D2 and a decrease in heat resistance from 88h to 73h of example D3. In examples D1-D3, the crystalline saturated polyester resin C had a Tg of-45 to-20 ℃ and satisfied non-blocking, high heat resistance and high adhesion, indicating that the saturated polyester resin C had a Tg in the range of-45 to-20 ℃ in the present formulation system to improve anti-blocking and heat resistance.
By integrating the embodiments A-D, the anti-reverse-adhesion binder is prepared by matching saturated polyester resin A, saturated polyester resin B and saturated polyester resin C, strictly controlling the state and Tg of polyester, wherein the Tg of the saturated polyester resin A is 20-25 ℃; the Tg of the saturated polyester resin B is 50-60 ℃; the saturated polyester resin C is crystalline saturated polyester, the Tg of the saturated polyester resin C is-45 to-20 ℃, and the anti-reverse-adhesion effect of the material can be improved; the hot melt adhesive film can not be anti-sticky after being taken out after 7 days when being put into an environment of 60 ℃; meanwhile, after the FFC wire is formed, the effect of long-term high temperature resistance can be achieved, and the FFC wire can be stored for at least more than 85 hours in an environment at 115 ℃.
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 anti-reverse-adhesion adhesive is characterized by comprising the following components in percentage by weight: 35-40% of saturated polyester resin A, 10-15% of saturated polyester resin B, 1-5% of saturated polyester resin C, 35-45% of flame retardant, less than 1% of curing agent and the balance of filler;
the glass transition temperature of the saturated polyester resin A is 20-25 ℃;
the glass transition temperature of the saturated polyester resin B is 50-60 ℃;
the saturated polyester resin C is a crystalline saturated polyester, and the glass transition temperature of the saturated polyester resin C is-45 to-20 ℃.
2. The adhesive of claim 1, wherein the flame retardant comprises: at least one of a bromine-based flame retardant, a phosphorus-based flame retardant, a nitrogen-based flame retardant, a metal hydroxide-based flame retardant, a metal oxide flame retardant and a metal boride flame retardant.
3. The adhesive according to claim 1, wherein the curing agent is one or a combination of two or more of aromatic isocyanate, aliphatic isocyanate, room temperature-reactive isocyanate, and blocked isocyanate.
4. The binder of claim 3 wherein the room temperature reactive isocyanate comprises: any one or combination of a dimer of diisocyanate or a polymer thereof, a dimer of 2, 4-diphenylmethane diisocyanate or a polymer thereof, a dimer of hexamethylene diisocyanate or a polymer thereof, a dimer of isophorone diisocyanate or a polymer thereof, a dimer of xylylene diisocyanate or a polymer thereof, and an adduct of the above isocyanates.
5. The bonding agent of claim 1, wherein the filler comprises: at least one of fumed silica, titanium dioxide and talc.
6. An anti-tack hot melt adhesive film, comprising: an insulating layer, a precoat layer and a binder layer;
the insulating layer, the precoating layer and the binder layer are sequentially attached from top to bottom; the adhesive layer is made of the adhesive of any one of claims 1 to 5.
7. A hot melt adhesive film according to claim 6, wherein said precoat layer is prepared by mixing at least a coupling agent and an isocyanate;
the content ratio of the coupling agent to the isocyanate is 1: (20-100).
8. The hot melt adhesive film as claimed in claim 7, wherein the insulating layer is a PET insulating layer.
9. The hot melt adhesive film as claimed in claim 8, wherein the thickness of the insulating layer is 12 to 50 μm;
the thickness of the pre-coating layer is 1-3 mu m;
the thickness of the adhesive layer is 20-50 mu m.
10. An FFC wire, wherein the hot melt adhesive film produced according to claim 6 is laminated to the outer surface of a conductor.
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