CN108084902A - A kind of viscous metal power is high, the Halogen hot melt adhesive film of good flame resistance and preparation method thereof - Google Patents
A kind of viscous metal power is high, the Halogen hot melt adhesive film of good flame resistance and preparation method thereof Download PDFInfo
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- CN108084902A CN108084902A CN201711372503.1A CN201711372503A CN108084902A CN 108084902 A CN108084902 A CN 108084902A CN 201711372503 A CN201711372503 A CN 201711372503A CN 108084902 A CN108084902 A CN 108084902A
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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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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/18—Fireproof paints including high temperature resistant paints
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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
- 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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- 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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- 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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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K2003/026—Phosphorus
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- 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
- C08K2003/2217—Oxides; Hydroxides of metals of magnesium
- C08K2003/2224—Magnesium hydroxide
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- 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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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/017—Additives being an antistatic agent
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/02—Flame or fire retardant/resistant
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- 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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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/22—Halogen free composition
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- 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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- C09J2203/00—Applications of adhesives in processes or use of adhesives in the form of films or foils
- C09J2203/326—Applications of adhesives in processes or use of adhesives in the form of films or foils for bonding electronic components such as wafers, chips or semiconductors
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- C09J2301/00—Additional features of adhesives in the form of films or foils
- C09J2301/10—Additional features of adhesives in the form of films or foils characterized by the structural features of the adhesive tape or sheet
- C09J2301/12—Additional features of adhesives in the form of films or foils characterized by the structural features of the adhesive tape or sheet by the arrangement of layers
- C09J2301/122—Additional features of adhesives in the form of films or foils characterized by the structural features of the adhesive tape or sheet by the arrangement of layers the adhesive layer being present only on one side of the carrier, e.g. single-sided adhesive tape
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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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- C09J2301/00—Additional features of adhesives in the form of films or foils
- C09J2301/30—Additional features of adhesives in the form of films or foils characterized by the chemical, physicochemical or physical properties of the adhesive or the carrier
- C09J2301/304—Additional features of adhesives in the form of films or foils characterized by the chemical, physicochemical or physical properties of the adhesive or the carrier the adhesive being heat-activatable, i.e. not tacky at temperatures inferior to 30°C
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- C09J2301/00—Additional features of adhesives in the form of films or foils
- C09J2301/30—Additional features of adhesives in the form of films or foils characterized by the chemical, physicochemical or physical properties of the adhesive or the carrier
- C09J2301/312—Additional features of adhesives in the form of films or foils characterized by the chemical, physicochemical or physical properties of the adhesive or the carrier parameters being the characterizing feature
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- C09J2301/00—Additional features of adhesives in the form of films or foils
- C09J2301/40—Additional features of adhesives in the form of films or foils characterized by the presence of essential components
- C09J2301/408—Additional features of adhesives in the form of films or foils characterized by the presence of essential components additives as essential feature of the adhesive layer
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- C09J2467/00—Presence of polyester
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- C09J2467/00—Presence of polyester
- C09J2467/006—Presence of polyester in the substrate
Abstract
The invention discloses a kind of viscous metal power is high, Halogen hot melt adhesive film of good flame resistance and preparation method thereof, including polyester film, refractory coating and viscous metal coating, the refractory coating is arranged between polyester film and viscous metal coating;According to mass percent, the raw material of the viscous metal coating includes 50~80% saturated polyester resin A, 5~30% saturated polyester resin B, 4~10% halogen-free flame retardants A, 6~10% halogen-free flame retardants B, 0.2~2% isocyanates and 0.5~8% filler.Using polyester film as basilar memebrane, refractory coating and viscous metal coating are coated in polyester film, the viscous metal coating for being arranged at outer layer has metal stronger viscous force, the refractory coating for being arranged at internal layer has higher anti-flammability, so as to while anti-flammability is improved, still there is stronger viscous metal power to the tin plating flat copper wire of package.
Description
Technical field
The present invention relates to field of thin film fabrication more particularly to a kind of viscous metal power height, the Halogen hot melt adhesive films of good flame resistance
And preparation method thereof.
Background technology
FFC winding displacements are also known as Fexibe Flat Cable (FFC), i.e. flexible flat cable, are a kind of upper and lower two layers insulation
The upper tin plating flat copper wire of folder, new types of data cable made of pressing have softness among material, and random bending fold, thickness is thin,
Constitution is small, and link is simple, convenient disassembly, the advantages that easily solving to be electromagnetically shielded (EMI), is now widely used for such as plotter, sweeps
Retouch the various electronic products such as instrument, sound equipment, liquid crystal electric appliance signal transmission and plate between connect, in modern electronic equipment almost without
Place does not exist.
Existing FFC winding displacements are to realize insulating materials and the hot melt adhesion of tin plating flat copper wire, hot melt by hot melt adhesive film
Glued membrane is that certain thickness film is made with the material of fusible bonding adherend, is placed between adherend, implements hot melt adhesion,
During the production gluing of hot melt adhesive film, halogen-free flame retardants is added, Halogen hot melt adhesive film is made, it is made to be used after finished product
FFC winding displacements can be allowed in the process with flame retardant effect, and avoid halogen fire proofing that from generating substantial amounts of smog during fire-retardant
With toxic corrosive hydrogen halides gas, secondary hazards are caused into.But existing Halogen hot melt adhesive film is when improving flame retardant property
Its viscous metal power can be caused to be greatly reduced, existing technique is promoted while can not realizing flame retardant property and viscous metal power.
The content of the invention
It is an object of the invention to propose a kind of high viscous metal power, the Halogen hot melt adhesive film of good flame resistance and its preparation side
Method while anti-flammability is improved, has the tin plating flat copper wire of package stronger viscous metal power.
For this purpose, the present invention uses following technical scheme:
A kind of viscous metal power is high, the Halogen hot melt adhesive film of good flame resistance, is applied including polyester film, refractory coating and viscous metal
Layer, the refractory coating are arranged between polyester film and viscous metal coating;
According to mass percent, the raw material of the viscous metal coating includes 50~80% saturated polyester resin A, and 5~30%
Saturated polyester resin B, 4~10% halogen-free flame retardants A, 6~10% halogen-free flame retardants B, 0.2~2% isocyanates and 0.5~
8% filler;
According to mass percent, the raw material of the refractory coating includes 10~30% saturated polyester resin A, and 40~60% is full
With polyester resin C, 5~15% halogen-free flame retardants A, 15~25% halogen-free flame retardants B, 0.2~2% isocyanates and 0.5~8%
Filler;
Wherein, the glass transition temperature of the saturated polyester resin A is -20~10 DEG C, and softening point is 75~85 DEG C, molecular weight
For 45000~60000, hydroxyl value is 3~4mgKOH/g;
The glass transition temperature of the saturated polyester resin B is 30~50 DEG C, and softening point is 100~110 DEG C, and molecular weight is
20000~30000, hydroxyl value is 2~4mgKOH/g;
The glass transition temperature of the saturated polyester resin C is 85~100 DEG C, and softening point is 130~150 DEG C, and molecular weight is
10000~20000, hydroxyl value is 2~3mgKOH/g.
The viscous metal power is high, the Halogen hot melt adhesive film of good flame resistance is placed in insulating materials and very thin tin plating flat copper wire
Between, FFC winding displacements are made in pressing, realize insulating materials and the hot melt adhesion of very thin tin plating flat copper wire.Made with polyester film
For basilar memebrane, refractory coating and viscous metal coating are coated in polyester film, be arranged at the viscous metal coating of outer layer have to metal compared with
Strong viscous force, the refractory coating for being arranged at internal layer have higher anti-flammability, thus while anti-flammability is improved, to package
Tin plating flat copper wire still have stronger viscous metal power.
In the viscous metal coating, mass percent shared by saturated polyester resin A is bigger than saturated polyester resin B, because
Glass transition temperature for saturated polyester resin A is low, and molecular weight is high, to the strong adhesive force of metal;But correspondingly, saturated polyester resin
The softening point temperature of A is low, poor heat resistance, therefore adds in the high saturated polyester resin B of a certain amount of glass transition temperature, saturated polyester
For the glass transition temperature of resin B at 30~50 DEG C, glass temperature range is appropriate, and softening point temperature is high, the mass percent occupied
It is small so that the mixed viscous metal coatings of saturated polyester resin A and saturated polyester resin B are keeping the strong adhesive force to metal
On the premise of, improve softening point temperature and heat resistance.
In the refractory coating, mass percent shared by saturated polyester resin C is bigger than saturated polyester resin A, because
The softening point temperature of saturated polyester resin C is high, can greatly improve the heat resistance of refractory coating;And Halogen hinders in refractory coating
The mass percent that combustion agent A and halogen-free flame retardants B is accounted for is big, greatly improves the anti-flammability of refractory coating.The refractory coating
The middle suitable saturated polyester resin A of incorporation, is conducive to the refractory coating and is attached to polyester film.
Preferably, the thickness of the polyester film is 10 μm~65 μm, and the thickness of the refractory coating is 5 μm~25 μm,
The thickness of the viscous metal coating is 4 μm~18 μm.It is suitable that the thickness of polyester film, refractory coating and viscous metal coating is set,
Be conducive to improve the anti-flammability of Halogen hot melt adhesive film and viscous metal power.
Preferably, the halogen-free flame retardants A is inorganic phosphorus type flame retardant or organic phosphates fire retardant;The inorganic Phosphorus resistance
It is red phosphorus or ammonium polyphosphate to fire agent;Organic phosphates fire retardant is phosphoric acid ester or phosphorous heterocylic compound;
The phosphoric acid ester is triphenyl phosphate, p isopropylbenzoic acid base phenylester, two base ester of phosphoric acid tert-butyl benzene, four aryl are sub-
Any one in aryl biphosphonate, resorcin phosphate, tetraphenyl bisphenol A- bisphosphates or two kinds of combinations;The phosphorus
Heterocyclic compound is any one in monocyclic phosphorous heterocylic compound, phosphorus spiro-compound, cage modle phosphorus compound.
Red phosphorus is good inorganic combustion inhibitor, while the still fire-resistant synergistic in aluminium hydroxide/magnesium hydroxide flame retardant system
Agent, the flame retarding efficiency height of red phosphorus, dosage is few, smoke amount is low, small toxicity.Ammonium polyphosphate has the function of expandable flame retardant, therefore more favourable
Yu Jiangyan and anti-dripping melt although being solid, are easy to disperse in polyalcohol.
Organic phosphates fire retardant have high flame retardant, few additive, it is small to finished product material properties affect the characteristics of, have it is fire-retardant and
Dual function is plasticized, fire retardant can be enable to fully achieve flow processability non-halogen, in improvement plastic shaping and reduce ablation,
Improve heat aging performance, improve heat distortion temperature, and can inhibit the residue after burning.Organic phosphates fire retardant can be phosphate
Class or phosphorous heterocylic compound, phosphoric acid ester can be triphenyl phosphate, p isopropylbenzoic acid base phenylester, two base ester of phosphoric acid tert-butyl benzene,
Four aryl arlydene biphosphonates, resorcin phosphate or tetraphenyl bisphenol A- bisphosphates, phosphorous heterocylic compound can be single
Ring phosphorous heterocylic compound, phosphorus spiro-compound or cage modle phosphorus compound.
Preferably, the halogen-free flame retardants B is nitrogenated flame retardant, and the nitrogenated flame retardant is melamine, cyanuric acid, three
Any one in the derivative of poly cyanamid, dicyandiamide, thiocarbamide, urea and its derivative or two kinds of combinations;The melamine
Derivative be Melamine Polyphosphate, melamine phosphate, any one in melamine cyanurate.
Nitrogenated flame retardant has many advantages, such as highly effective flame-retardant, is halogen-free, corrosion-free effect, thus reduces machinery and be corroded
Problem;Ultraviolet resistance shines, and good electrical property is colour-fast, no blooming, recyclable recycling.Nitrogenated flame retardant can be melamine, cyanogen
Uric acid, the derivative of melamine, dicyandiamide, thiocarbamide, urea and its derivative, the derivative of the melamine can be trimerization
Cyanamide polyphosphate, melamine phosphate or melamine cyanurate.
The halogen-free flame retardants A and halogen-free flame retardants B are used in mixed way, and are enhancing the same of the anti-flammability of Halogen hot melt adhesive film
When, the plasticity of Halogen hot melt adhesive film is also improved, hot melt adhesion effect is more preferable, in turn avoids the corrosiveness to tin plating flat copper wire.
Preferably, the halogen-free flame retardants B is metal oxyhydroxide based flame retardant or metal boride fire retardant;It is described
Metal oxyhydroxide based flame retardant is aluminium hydroxide or magnesium hydroxide;The metal boride fire retardant is zinc borate or boric acid
Barium.Aluminium hydroxide or magnesium hydroxide have good flame retardant effect, while can also play the role of smoke suppressant, safe and non-toxic, high
The advantages that thermal stability is good during warm working.Zinc borate or barium borate effectively improve flame retardant property, and can adjust Halogen hot melt adhesive
The electric property of film.
Preferably, the isocyanates is aromatic isocyanate, aliphatic isocyanates, room temperature reaction type isocyanates
With the one or more in blocked isocyanate.Isocyanates plays solidification, under room temperature can with containing active group (hydroxyl
Base, carboxyl, amido, epoxy group etc.) resin coexists steadily in the long term, after solvent volatilization, film after Overheating Treatment this latent cure
Agent release-NCO group and on molecular resin chain hydroxyl, carboxyl, amino groups react and to form crosslinking, nothing can be significantly improved
Adhesive force, color stability and resistance to retort sterilization ability of halogen hot melt adhesive film etc., wherein aliphatic isocyanate cross-linking agent has
Excellent anti-yellowing property.
The room temperature reaction type isocyanates can be toluene di-isocyanate(TDI) (TDI) and its dimer, tripolymer, 2,4- bis-
Methylenebis phenyl isocyanate (MDI) and its dimer, tripolymer, hexamethylene diisocyanate (HDI) and its dimer, three
Aggressiveness, isophorone diisocyanate (IPDI) and its dimer, tripolymer, phenylenedimethylidyne diisocyanate (XDI) and secondly
The addition product of aggressiveness, tripolymer or above-mentioned isocyanates;The blocked isocyanate can be phenol, polyether Glycols with it is upper
State the blocked isocyanate of the room temperature reaction type isocyanates synthesis.
Preferably, the polyester film is biaxially oriented polyester film;The filler is wollastonite, mica, kaolin, cunning
Mountain flour and titanium dioxide.Biaxially oriented polyester film has good antistatic property and heat resistance, is conducive to be coated with, and improves viscous metal
The adhesive force of coating and refractory coating.
Preferably, the preparation method of high, good flame resistance the Halogen hot melt adhesive film of the viscous metal power, comprises the following steps:
Step A is coated with the refractory coating on the polyester film, controls the coating thickness of the refractory coating in 5 μ
M~25 μm, and it is dry;
Step B is coated with the viscous metal coating on the refractory coating, controls the coating thickness of the viscous metal coating
At 4 μm~18 μm, and it is dry, the viscous metal power height, the Halogen hot melt adhesive film of good flame resistance is made.
The preparation method of high, good flame resistance the Halogen hot melt adhesive film of the viscous metal power is that polyester film is put into coating machine,
Equipped with a plurality of for gluing the deflector roll of coating, first pass through deflector roll and the refractory coating is coated on the polyester film, then apply again
Metal coating is glued described in cloth, you can the viscous metal power height, the Halogen hot melt adhesive film of good flame resistance is made, it is simple for process easy to operate.
Preferably, the step A is further included:
The preparation of the viscous metal coating, according to mass percent, by 50~80% saturated polyester resin A, 5~
The 30% saturated polyester resin B, 4~10% halogen-free flame retardants A, 6~10% halogen-free flame retardants B and 0.5~8%
When filler is small with the Rate Dispersion 2 of 2400r/min, 0.2~2% isocyanates is then placed into the speed of 1200r/min point
It dissipates 30 minutes, is finally ground twice, every time grinding 30 minutes, the viscous metal coating is made;
The preparation of the refractory coating, according to mass percent, by 10~30% saturated polyester resin A, 40~
The 60% saturated polyester resin C, 5~15% halogen-free flame retardants A, 15~25% halogen-free flame retardants B and 0.5~
When 8% filler is small with the Rate Dispersion 2 of 2400r/min, 0.2~2% isocyanates is then placed into the speed of 1200r/min
It is 30 minutes scattered, it is finally ground twice, every time grinding 30 minutes, the refractory coating is made.Above-mentioned raw materials are by scattered
Grinding, mixing are more uniformly distributed.
Preferably, in the step A, the drying temperature for controlling the refractory coating is 160 ± 10 DEG C;
In the step B, the drying temperature for controlling the viscous metal coating is 140 ± 10 DEG C;
Also, the drying temperature of the refractory coating is higher than the drying temperature of the viscous metal coating.
Ensure that the oven temperature of coating machine is 20 DEG C high during metal coating more viscous than coating when being coated with refractory coating, so as to drop
The dissolvent residual total amount of low Halogen hot melt adhesive film, more Environmental Safety.
Description of the drawings
The present invention will be further described for attached drawing, but the content in attached drawing does not form any limitation of the invention.
Fig. 1 is the Halogen hot melt adhesive film structure diagram of the one of embodiment of the present invention.
Wherein:Polyester film 1;Refractory coating 2;Viscous metal coating 3.
Specific embodiment
Technical solution to further illustrate the present invention below with reference to the accompanying drawings and specific embodiments.
Embodiment X1~X5 prepares viscous metal coating 3 and refractory coating according to the different raw material components of table 1 and proportioning
2, as shown in Figure 1;
The glass transition temperature of saturated polyester resin A in table 1 is -10 DEG C, and softening point is 75 DEG C, molecular weight 50000, hydroxyl
It is worth for 3.5mgKOH/g;The glass transition temperature of saturated polyester resin B is 40 DEG C, and softening point is 105 DEG C, molecular weight 20000, hydroxyl
It is worth for 2mgKOH/g;The glass transition temperature of saturated polyester resin C is 100 DEG C, and softening point is 150 DEG C, molecular weight 10000, hydroxyl
It is worth for 2mgKOH/g.
Table 1
Different Halogen hot melt adhesive films is made further according to following steps, as shown in Figure 1:
Step 1 glues the preparation of metal coating 3, described full by the saturated polyester resin A according to the proportioning shown in table 1
During with polyester resin B, the halogen-free flame retardants A, the halogen-free flame retardants B and filler small with the Rate Dispersion 2 of 2400r/min,
Then isocyanates is placed into the Rate Dispersion 30 minutes of 1200r/min, is finally ground twice, every time 30 points of grinding
The viscous metal coating 3 is made in clock;
The preparation of refractory coating 2, according to the proportioning shown in table 1, by the saturated polyester resin A, the saturated polyester tree
Fat C, the halogen-free flame retardants A, the halogen-free flame retardants B and during filler small with the Rate Dispersion 2 of 2400r/min, then put again
Enter isocyanates with the Rate Dispersion 30 minutes of 1200r/min, finally ground twice, every time grinding 30 minutes, institute is made
State refractory coating 2.
Step 2 is coated with the refractory coating 2 on the polyester film 1 that thickness is 50 μm, controls the heat-resisting painting
The coating thickness of layer 2 is at 20 μm, and the drying in the case where oven temperature is 160 DEG C.
Step 3 is coated with the viscous metal coating 3 on the refractory coating 2 that thickness is 20 μm, controls the viscous gold
Belong to the coating thickness of coating 3 at 15 μm, and it is dry in the case where oven temperature is 140 DEG C, the Halogen hot melt adhesive film is made after dry.
Following performance test is carried out to Halogen hot melt adhesive film obtained, the results are shown in Table 4:
(1) appearance
There are bubble-free, pin hole, particle in the surface of range estimation Halogen hot melt adhesive film.
(2) back of the body is viscous
It is entirely fitted on the non-corona surface of PET with the viscous metal coating 3 of Halogen hot melt adhesive film, the specification of model is
50mmX200mm, the counterweight of smooth placement 5kg on this model, placed in 50 DEG C of baking oven 48 it is small when after test sample plate
Peeling force, the peeling rate 50mm/min of puller system, peel value be less than 0.2N/5cm, be qualification.
(3) it is to the test method of the adhesive force of copper wire:Two pieces of tablets up and down of tablet pressing machine are adjusted to 100 DEG C,
Pressure is adjusted to below or equal to 0.1Mpas, the peeling force of 3 seconds test sample plates of pressing time, peeling rate 50mm/min, attached
Put forth effort to be greater than or equal to 20g/0.3mm, be qualification.
(4) it is to the test method of the adhesive force of PET:Two pieces of tablets up and down of tablet pressing machine are adjusted to 100 DEG C, pressure
Power is adjusted to below or equal to 0.1Mpas, the peeling force of 3 seconds test sample plates of pressing time, peeling rate 50mm/min, attachment
Power is more than 10N/IN, is qualification.
(5) flame retardant rating of Halogen hot melt adhesive film is divided according to UL-94, fire-retardant highest ranking is VTM-0, secondly VTM-
1, VTM-2, HB etc..
(6) according to specified in GB/T10004-2008 national standards:Dissolvent residual total amount≤5.0mg/m2。
Embodiment Y1~Y7 prepares viscous metal coating 3 and refractory coating according to the different raw material components of table 2 and proportioning
2;
The glass transition temperature of saturated polyester resin A in table 2 is -10 DEG C, and softening point is 75 DEG C, molecular weight 50000, hydroxyl
It is worth for 3.5mgKOH/g;The glass transition temperature of saturated polyester resin B is 40 DEG C, and softening point is 105 DEG C, molecular weight 20000, hydroxyl
It is worth for 2mgKOH/g;The glass transition temperature of saturated polyester resin C is 100 DEG C, and softening point is 150 DEG C, molecular weight 10000, hydroxyl
It is worth for 2mgKOH/g.
Table 2
Halogen hot melt adhesive film is made according to following steps in embodiment Y1:
Step 1, the preparation of refractory coating 2, according to the proportioning shown in table 2, by the saturated polyester resin A, the saturation
Polyester resin C, the halogen-free flame retardants A, the halogen-free flame retardants B and during filler small with the Rate Dispersion 2 of 2400r/min, so
Isocyanates is placed into afterwards with the Rate Dispersion 30 minutes of 1200r/min, is finally ground twice, every time grinding 30 minutes,
The refractory coating 2 is made.
Step 2 is coated with the refractory coating 2 on the polyester film 1 that thickness is 50 μm, controls the heat-resisting painting
The coating thickness of layer 2 is at 20 μm, and, dry after the obtained Halogen hot melt adhesive film dry in the case where oven temperature is 160 DEG C.
Above-mentioned performance test is carried out to Halogen hot melt adhesive film obtained, the results are shown in Table 4.
Difference is made in proportionings of the embodiment Y2~Y6 according to the step 1 to three and table 2 of embodiment X1~X5
Halogen hot melt adhesive film, and above-mentioned performance test is carried out to Halogen hot melt adhesive film obtained, the results are shown in Table 4.
Halogen hot melt adhesive film is made according to following steps in embodiment Y7:
Step 1 glues the preparation of metal coating 3, described full by the saturated polyester resin A according to the proportioning shown in table 2
During with polyester resin B, the halogen-free flame retardants A, the halogen-free flame retardants B and filler small with the Rate Dispersion 2 of 2400r/min,
Then isocyanates is placed into the Rate Dispersion 30 minutes of 1200r/min, is finally ground twice, every time 30 points of grinding
The viscous metal coating 3 is made in clock;
The preparation of refractory coating 2, according to the proportioning shown in table 1, by the saturated polyester resin A, the saturated polyester tree
Fat C, the halogen-free flame retardants A, the halogen-free flame retardants B and during filler small with the Rate Dispersion 2 of 2400r/min, then put again
Enter isocyanates with the Rate Dispersion 30 minutes of 1200r/min, finally ground twice, every time grinding 30 minutes, institute is made
State refractory coating 2.
Step 2 is coated with the refractory coating 2 on the polyester film 1 that thickness is 50 μm, controls the heat-resisting painting
The coating thickness of layer 2 is at 20 μm, and the drying in the case where oven temperature is 140 DEG C.
Step 3 is coated with the viscous metal coating 3 on the refractory coating 2 that thickness is 20 μm, controls the viscous gold
Belong to the coating thickness of coating 3 at 15 μm, and it is dry in the case where oven temperature is 130 DEG C, the Halogen hot melt adhesive film is made after dry.
Above-mentioned performance test is carried out to Halogen hot melt adhesive film obtained, the results are shown in Table 4.
Saturated polyester resin A, the saturated polyester resin B of different glass temperature of the embodiment Z1~Z6 according to table 3
With polyester resin C, component, proportioning are identical with embodiment X1, prepare viscous metal coating 3 and refractory coating 2;
And according to the step 1 of embodiment X1 to three, different Halogen hot melt adhesive films is made, and to Halogen obtained
Hot melt adhesive film carries out above-mentioned performance test, and the results are shown in Table 4.
The softening point of saturated polyester resin A in table 3 is 75 DEG C, molecular weight 50000, hydroxyl value 3.5mgKOH/g;It is full
Softening point with polyester resin B is 105 DEG C, molecular weight 20000, hydroxyl value 2mgKOH/g;The softening point of saturated polyester resin C
For 150 DEG C, molecular weight 10000, hydroxyl value 2mgKOH/g.
Table 3
Table 4
As shown in Table 4, Halogen hot melt adhesive made from embodiment Y1 is low to the adhesive force of copper wire, by embodiment X1~X5 and
The comparison of embodiment Y1 understands that viscous metal coating 3 has the tin plating flat copper wire of package on stronger viscous metal power, and viscous metal
Mass percent shared by saturated polyester resin A in coating 3 is bigger, and it is stronger to glue metal power;
Halogen hot melt adhesive made from embodiment Y2 is low to the adhesive force of PET, passes through embodiment X1~X5's and embodiment Y2
Comparison is understood, suitable saturated polyester resin A is mixed in refractory coating 2, is conducive to the refractory coating 2 and is attached to polyester film
1, improve adhesive force of the Halogen hot melt adhesive to PET;
Halogen hot melt adhesive made from embodiment Y3 causes softening point low because viscous metal coating 3 lacks saturated polyester resin B,
It is viscous to there is the back of the body, poor fire;By the comparison of embodiment X1~X5 and embodiment Y3, glue in metal coating 3 and add in centainly
The high saturated polyester resin B of the glass transition temperature of amount, on the premise of keeping to the strong adhesive force of metal, improves softening point temperature
Degree and heat resistance;
Halogen hot melt adhesive made from embodiment Y4 because in refractory coating 2 mass percent shared by saturated polyester resin A it is excessive,
Cause softening point low, the back of the body occur and glue, poor fire;Pass through the comparison of embodiment X1~X5 and embodiment Y4, saturated polyester
Mass percent shared by resin C is bigger than saturated polyester resin A, can be significantly because the softening point temperature of saturated polyester resin C is high
Ground improves the heat resistance of refractory coating 2, avoids causing to go out when softening point is low because mass percent shared by saturated polyester resin A is excessive
Now the back of the body is viscous;
Halogen hot melt adhesive made from embodiment Y5 is because of mass percent mistake shared by saturated polyester resin B in viscous metal coating 3
Greatly, cause low to the adhesive force of copper wire;By the comparison of embodiment X1~X5 and embodiment Y5, viscous metal coating 3 is embezzled
With polyester resin A shared by mass percent it is bigger than saturated polyester resin B, avoid to the decline of the adhesive force of copper wire;
What Halogen hot melt adhesive made from embodiment Y6 was accounted for because gluing halogen-free flame retardants A and halogen-free flame retardants B in metal coating 3
Mass percent is excessive, causes low to the adhesive force of copper wire;By the comparison of embodiment X1~X5 and embodiment Y6, gold is glued
The mass percent that halogen-free flame retardants A and halogen-free flame retardants B are accounted in category coating 3 is small, avoids the adhesive force decline to copper wire;
Halogen hot melt adhesive made from embodiment Y7 is more viscous than being coated with because drying temperature is low, and when being coated with refractory coating 2
The temperature difference is less than 20 DEG C during metal coating 3, therefore dissolvent residual total amount is excessive;Pass through the comparison of embodiment X1~X5 and embodiment Y7
It understands, the oven temperature of coating machine is 20 DEG C high during metal coating 3 more viscous than coating when being coated with refractory coating 2, so as to reduce nothing
The dissolvent residual total amount of halogen hot melt adhesive film;
By the comparison of embodiment Z1~Z3 and embodiment Z4, if in refractory coating 2 saturated polyester resin A glass
It is excessively high to change temperature, adhesive force of the Halogen hot melt adhesive film to PET can be reduced;If the glass of saturated polyester resin A in viscous metal coating 3
It is excessively high to change temperature, adhesive force of the Halogen hot melt adhesive film to copper wire can be reduced;
By the comparison of embodiment Z1~Z3 and embodiment Z5, if in refractory coating 2 saturated polyester resin C glass
It is too low to change temperature, Halogen hot melt adhesive film is present with the viscous situation of the back of the body;
By the comparison of embodiment Z1~Z3 and embodiment Z6, if gluing the glass of saturated polyester resin B in metal coating 3
Glass temperature is excessively high, can reduce adhesive force of the Halogen hot melt adhesive film to copper wire.
The technical principle of the present invention is described above in association with specific embodiment.These descriptions are intended merely to explain the present invention's
Principle, and limiting the scope of the invention cannot be construed in any way.Based on explanation herein, the technology of this field
Personnel would not require any inventive effort the other specific embodiments that can associate the present invention, these modes are fallen within
Within protection scope of the present invention.
Claims (10)
1. a kind of viscous metal power is high, the Halogen hot melt adhesive film of good flame resistance, applied including polyester film, refractory coating and viscous metal
Layer, the refractory coating are arranged between polyester film and viscous metal coating, it is characterised in that:
According to mass percent, the raw material of the viscous metal coating includes 50~80% saturated polyester resin A, 5~30% saturations
Polyester resin B, 4~10% halogen-free flame retardants A, 6~10% halogen-free flame retardants B, 0.2~2% isocyanates and 0.5~8% are filled out
Material;
According to mass percent, the raw material of the refractory coating includes 10~30% saturated polyester resin A, and 40~60% saturations are gathered
Ester resin C, 5~15% halogen-free flame retardants A, 15~25% halogen-free flame retardants B, 0.2~2% isocyanates and 0.5~8% are filled out
Material;
Wherein, the glass transition temperature of the saturated polyester resin A is -20~10 DEG C, and softening point is 75~85 DEG C, and molecular weight is
45000~60000, hydroxyl value is 3~4mgKOH/g;
The glass transition temperature of the saturated polyester resin B is 30~50 DEG C, and softening point is 100~110 DEG C, molecular weight 20000
~30000, hydroxyl value is 2~4mgKOH/g;
The glass transition temperature of the saturated polyester resin C is 85~100 DEG C, and softening point is 130~150 DEG C, molecular weight 10000
~20000, hydroxyl value is 2~3mgKOH/g.
2. viscous metal power according to claim 1 is high, the Halogen hot melt adhesive film of good flame resistance, it is characterised in that:It is described poly-
The thickness of ester film is 10 μm~65 μm, and the thickness of the refractory coating is 5 μm~25 μm, and the thickness of the viscous metal coating is
4 μm~18 μm.
3. viscous metal power according to claim 1 is high, the Halogen hot melt adhesive film of good flame resistance, it is characterised in that:The nothing
Halogen fire retardant A is inorganic phosphorus type flame retardant or organic phosphates fire retardant;The inorganic phosphorus type flame retardant is red phosphorus or ammonium polyphosphate;
Organic phosphates fire retardant is phosphoric acid ester or phosphorous heterocylic compound;
The phosphoric acid ester is triphenyl phosphate, p isopropylbenzoic acid base phenylester, two base ester of phosphoric acid tert-butyl benzene, four aryl arlydene
Any one in biphosphonate, resorcin phosphate, tetraphenyl bisphenol A- bisphosphates or two kinds of combinations;The phosphorus heterocycle
Compound is any one in monocyclic phosphorous heterocylic compound, phosphorus spiro-compound, cage modle phosphorus compound.
4. viscous metal power according to claim 1 is high, the Halogen hot melt adhesive film of good flame resistance, it is characterised in that:The nothing
Halogen fire retardant B is nitrogenated flame retardant, and the nitrogenated flame retardant is melamine, cyanuric acid, the derivative of melamine, double cyanogen
Any one in amine, thiocarbamide, urea and its derivative or two kinds of combinations;
The derivative of the melamine is Melamine Polyphosphate, in melamine phosphate, melamine cyanurate
Any one.
5. viscous metal power according to claim 1 is high, the Halogen hot melt adhesive film of good flame resistance, it is characterised in that:The nothing
Halogen fire retardant B is metal oxyhydroxide based flame retardant or metal boride fire retardant;The metal oxyhydroxide class is fire-retardant
Agent is aluminium hydroxide or magnesium hydroxide;The metal boride fire retardant is zinc borate or barium borate.
6. viscous metal power according to claim 1 is high, the Halogen hot melt adhesive film of good flame resistance, it is characterised in that:It is described different
Cyanate is in aromatic isocyanate, aliphatic isocyanates, room temperature reaction type isocyanates and blocked isocyanate
It is one or more.
7. viscous metal power according to claim 1 is high, the Halogen hot melt adhesive film of good flame resistance, it is characterised in that:It is described poly-
Ester film is biaxially oriented polyester film;
The filler is wollastonite, mica, kaolin, talcum powder and titanium dioxide.
8. the preparation side of high, good flame resistance the Halogen hot melt adhesive film of viscous metal power according to claim 1 to 7 any one
Method, which is characterized in that comprise the following steps:
Step A is coated with the refractory coating on the polyester film, control the coating thickness of the refractory coating 5 μm~
25 μm, and it is dry;
Step B is coated with the viscous metal coating on the refractory coating, controls the coating thickness of the viscous metal coating in 4 μ
M~18 μm, and it is dry, the viscous metal power height, the Halogen hot melt adhesive film of good flame resistance is made.
9. the preparation method of high, good flame resistance the Halogen hot melt adhesive film of viscous metal power according to claim 8, feature exist
In the step A is further included:
The preparation of the viscous metal coating, according to mass percent, by 50~80% saturated polyester resin A, 5~30% institutes
State saturated polyester resin B, 4~10% halogen-free flame retardants A, 6~10% halogen-free flame retardants B and 0.5~8% filler with
When the Rate Dispersion 2 of 2400r/min is small, then places into 0.2~2% isocyanates and divided with the Rate Dispersion 30 of 1200r/min
Clock is finally ground twice, every time grinding 30 minutes, and the viscous metal coating is made;
The preparation of the refractory coating, according to mass percent, by 10~30% saturated polyester resin A, 40~60% institutes
State saturated polyester resin C, 5~15% halogen-free flame retardants A, 15~25% halogen-free flame retardants B and 0.5~8% filler
When small with the Rate Dispersion 2 of 2400r/min, 0.2~2% isocyanates is then placed into the Rate Dispersion 30 of 1200r/min
Minute, it is finally ground twice, every time grinding 30 minutes, the refractory coating is made.
10. the preparation method of high, good flame resistance the Halogen hot melt adhesive film of viscous metal power according to claim 8, feature
It is:
In the step A, the drying temperature for controlling the refractory coating is 160 ± 10 DEG C;
In the step B, the drying temperature for controlling the viscous metal coating is 140 ± 10 DEG C;
Also, the drying temperature of the refractory coating is higher than the drying temperature of the viscous metal coating.
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Application publication date: 20180529 |