CN115322709A - Hot melt adhesive film with high metal adhesion and good flame retardance and preparation method thereof - Google Patents
Hot melt adhesive film with high metal adhesion and good flame retardance and preparation method thereof Download PDFInfo
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- CN115322709A CN115322709A CN202210809883.5A CN202210809883A CN115322709A CN 115322709 A CN115322709 A CN 115322709A CN 202210809883 A CN202210809883 A CN 202210809883A CN 115322709 A CN115322709 A CN 115322709A
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- adhesive film
- melt adhesive
- hot melt
- good flame
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- 239000004831 Hot glue Substances 0.000 title claims abstract description 38
- 229910052751 metal Inorganic materials 0.000 title claims abstract description 21
- 239000002184 metal Substances 0.000 title claims abstract description 21
- 238000002360 preparation method Methods 0.000 title abstract description 7
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 39
- 239000000203 mixture Substances 0.000 claims abstract description 35
- 239000003063 flame retardant Substances 0.000 claims abstract description 31
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 claims abstract description 28
- 238000001816 cooling Methods 0.000 claims abstract description 20
- 239000000463 material Substances 0.000 claims abstract description 15
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 15
- 235000012239 silicon dioxide Nutrition 0.000 claims abstract description 15
- 239000005062 Polybutadiene Substances 0.000 claims abstract description 14
- 229920002857 polybutadiene Polymers 0.000 claims abstract description 14
- 229920003225 polyurethane elastomer Polymers 0.000 claims abstract description 14
- 238000005266 casting Methods 0.000 claims abstract description 13
- 239000003085 diluting agent Substances 0.000 claims abstract description 11
- -1 polyethylene Polymers 0.000 claims abstract description 11
- RSWGJHLUYNHPMX-UHFFFAOYSA-N Abietic-Saeure Natural products C12CCC(C(C)C)=CC2=CCC2C1(C)CCCC2(C)C(O)=O RSWGJHLUYNHPMX-UHFFFAOYSA-N 0.000 claims abstract description 9
- 239000004698 Polyethylene Substances 0.000 claims abstract description 9
- KHPCPRHQVVSZAH-HUOMCSJISA-N Rosin Natural products O(C/C=C/c1ccccc1)[C@H]1[C@H](O)[C@@H](O)[C@@H](O)[C@@H](CO)O1 KHPCPRHQVVSZAH-HUOMCSJISA-N 0.000 claims abstract description 9
- 229920000573 polyethylene Polymers 0.000 claims abstract description 9
- 239000011347 resin Substances 0.000 claims abstract description 9
- 229920005989 resin Polymers 0.000 claims abstract description 9
- KHPCPRHQVVSZAH-UHFFFAOYSA-N trans-cinnamyl beta-D-glucopyranoside Natural products OC1C(O)C(O)C(CO)OC1OCC=CC1=CC=CC=C1 KHPCPRHQVVSZAH-UHFFFAOYSA-N 0.000 claims abstract description 9
- 229920001577 copolymer Polymers 0.000 claims abstract description 8
- 238000007493 shaping process Methods 0.000 claims abstract description 7
- 238000000034 method Methods 0.000 claims description 13
- 239000005543 nano-size silicon particle Substances 0.000 claims description 7
- VTHJTEIRLNZDEV-UHFFFAOYSA-L magnesium dihydroxide Chemical compound [OH-].[OH-].[Mg+2] VTHJTEIRLNZDEV-UHFFFAOYSA-L 0.000 claims description 6
- 239000000347 magnesium hydroxide Substances 0.000 claims description 6
- 229910001862 magnesium hydroxide Inorganic materials 0.000 claims description 6
- DURPTKYDGMDSBL-UHFFFAOYSA-N 1-butoxybutane Chemical compound CCCCOCCCC DURPTKYDGMDSBL-UHFFFAOYSA-N 0.000 claims description 4
- HJEORQYOUWYAMR-UHFFFAOYSA-N 2-[(2-butylphenoxy)methyl]oxirane Chemical compound CCCCC1=CC=CC=C1OCC1OC1 HJEORQYOUWYAMR-UHFFFAOYSA-N 0.000 claims description 4
- 239000004593 Epoxy Substances 0.000 claims description 4
- 229910019142 PO4 Inorganic materials 0.000 claims description 4
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims description 4
- GOOHAUXETOMSMM-UHFFFAOYSA-N Propylene oxide Chemical compound CC1CO1 GOOHAUXETOMSMM-UHFFFAOYSA-N 0.000 claims description 4
- 239000010452 phosphate Substances 0.000 claims description 4
- 229910052698 phosphorus Inorganic materials 0.000 claims description 4
- 239000011574 phosphorus Substances 0.000 claims description 4
- REZAIYDMQVPNCA-UHFFFAOYSA-N (3-hydroxyphenyl) dihydrogen phosphate Chemical compound OC1=CC=CC(OP(O)(O)=O)=C1 REZAIYDMQVPNCA-UHFFFAOYSA-N 0.000 claims description 3
- WRXFONORSZHETC-UHFFFAOYSA-N phenyl propan-2-yl hydrogen phosphate Chemical compound CC(C)OP(O)(=O)OC1=CC=CC=C1 WRXFONORSZHETC-UHFFFAOYSA-N 0.000 claims description 3
- XZZNDPSIHUTMOC-UHFFFAOYSA-N triphenyl phosphate Chemical compound C=1C=CC=CC=1OP(OC=1C=CC=CC=1)(=O)OC1=CC=CC=C1 XZZNDPSIHUTMOC-UHFFFAOYSA-N 0.000 claims description 3
- QXONIHMUSQFKJU-UHFFFAOYSA-N 2-(prop-1-enoxymethyl)oxirane Chemical compound CC=COCC1CO1 QXONIHMUSQFKJU-UHFFFAOYSA-N 0.000 claims description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 claims description 2
- SZIMYNVBPPNTMU-UHFFFAOYSA-N tert-butyl phenyl hydrogen phosphate Chemical compound CC(C)(C)OP(O)(=O)OC1=CC=CC=C1 SZIMYNVBPPNTMU-UHFFFAOYSA-N 0.000 claims description 2
- 239000002313 adhesive film Substances 0.000 abstract description 9
- 229910052736 halogen Inorganic materials 0.000 abstract description 7
- 150000002367 halogens Chemical class 0.000 abstract description 7
- 239000000945 filler Substances 0.000 abstract description 6
- 239000003795 chemical substances by application Substances 0.000 abstract description 3
- 239000006185 dispersion Substances 0.000 abstract 1
- 230000001070 adhesive effect Effects 0.000 description 6
- 239000012796 inorganic flame retardant Substances 0.000 description 5
- 238000012360 testing method Methods 0.000 description 5
- 238000003825 pressing Methods 0.000 description 4
- 239000000853 adhesive Substances 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- DXZMANYCMVCPIM-UHFFFAOYSA-L zinc;diethylphosphinate Chemical compound [Zn+2].CCP([O-])(=O)CC.CCP([O-])(=O)CC DXZMANYCMVCPIM-UHFFFAOYSA-L 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 238000005034 decoration Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000011256 inorganic filler Substances 0.000 description 1
- 229910003475 inorganic filler Inorganic materials 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- FKMFNQXZJGJRJG-UHFFFAOYSA-N tert-butyl phenyl phosphono phosphate Chemical compound CC(C)(C)OP(=O)(OC1=CC=CC=C1)OP(=O)(O)O FKMFNQXZJGJRJG-UHFFFAOYSA-N 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
Classifications
-
- 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
- C09J151/00—Adhesives based on graft polymers in which the grafted component is obtained by reactions only involving carbon-to-carbon unsaturated bonds; Adhesives based on derivatives of such polymers
- C09J151/06—Adhesives based on graft polymers in which the grafted component is obtained by reactions only involving carbon-to-carbon unsaturated bonds; Adhesives based on derivatives of such polymers grafted on to homopolymers or copolymers of aliphatic hydrocarbons containing only one carbon-to-carbon double bond
-
- 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
-
- 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
-
- 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
-
- 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
- C09J7/10—Adhesives in the form of films or foils without carriers
-
- 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
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/014—Additives containing two or more different additives of the same subgroup in C08K
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/02—Flame or fire retardant/resistant
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/22—Halogen free composition
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Inorganic Chemistry (AREA)
- Extrusion Moulding Of Plastics Or The Like (AREA)
- Adhesives Or Adhesive Processes (AREA)
Abstract
The invention discloses a hot melt adhesive film with high metal adhesion and good flame retardance and a preparation method thereof, wherein the preparation method comprises the following steps: according to the weight parts, a polybutadiene polyurethane elastomer/nano-silica organic-inorganic hybrid material, a polyethylene grafted acrylic acid-2-hydroxyethyl ester copolymer, rosin resin and a flame retardant are dispersed, and a reactive diluent is added for dispersion to obtain a mixture; putting the mixture into a charging hopper of a double-screw extruder, and fully plasticizing the mixture by the screw extruder to obtain a molten composition; and extruding the molten composition through a die head to obtain a molten film, and cooling and shaping the molten film through a casting roller and a cooling roller to form the hot melt adhesive film. According to the invention, other fillers are not required to be added, the silicon dioxide not only serves as a curing agent, but also plays a role of an inorganic nano filler, inorganic and organic flame retardant components are combined, the compatibility with an organic adhesive film main body component is better, halogen is not contained, the flame retardance is good, the metal adhesion is high, and the mechanical property is good.
Description
Technical Field
The invention relates to the technical field of hot melt adhesive films, in particular to a hot melt adhesive film with high metal adhesion and good flame retardance and a preparation method thereof.
Background
The hot melt adhesive film belongs to one kind of hot melt adhesive, and as one new kind of adhesive, it has high adhering force, no pollution, convenient operation and easy storage, so that it is used widely.
With the development of automobile, decoration and electrical industries in China, the market puts higher requirements on hot melt adhesive film products, and the hot melt adhesive film is expected to meet the index requirements of flame retardance, environmental protection, mechanical property and the like while ensuring the bonding capability.
In the prior art, a halogen-containing flame retardant is added into a system, and the halogen-containing flame retardant has good compatibility with an inorganic system, but generates halogen gas during combustion and has great influence on the environment, so the halogen-containing flame retardant is forbidden in many occasions, and many products require that the halogen-containing flame retardant cannot be used, and the halogen-free flame retardant is required to be adopted. The halogen-free flame retardant is usually an inorganic flame retardant, and the addition amount of the halogen-free flame retardant needs to be large to achieve a good effect, but a large amount of inorganic filler can reduce the adhesive property and the mechanical property of the hot melt adhesive film, so that a plurality of technical problems are brought to hot melt adhesive film manufacturers in the process of granulating and preparing the material and using the material by an end user.
Disclosure of Invention
The invention aims to provide a hot melt adhesive film with high metal adhesion and good flame retardance and a preparation method thereof aiming at the defects in the prior art, wherein the hot melt adhesive film does not contain halogen, has good flame retardance, and is high in metal adhesion and good in mechanical property.
In order to realize the purpose, the technical scheme provided by the invention is as follows:
a hot melt adhesive film with high metal adhesion and good flame retardance is characterized in that: comprises the following components:
50-80 parts of polyethylene grafted acrylic acid-2-hydroxyethyl ester copolymer,
10-30 parts of polybutadiene polyurethane elastomer/nano silicon dioxide organic-inorganic hybrid material,
1 to 5 parts by weight of rosin resin,
8-15 parts by weight of a flame retardant,
1-5 parts of reactive diluent.
Further, the reactive diluent is an epoxy reactive diluent, and the epoxy reactive diluent is one or more of epoxypropane butyl ether, butyl phenyl glycidyl ether and propenyl glycidyl ether.
Further, the flame retardant is a mixture of nano flaky magnesium hydroxide and an organic phosphorus flame retardant, the organic phosphorus flame retardant is a phosphate compound, and the phosphate is one or more of triphenyl phosphate, isopropyl phenyl phosphate, tert-butyl phenyl phosphate and resorcinol phosphate.
Further, the content of silica in the polybutadiene polyurethane elastomer/nano silica organic-inorganic hybrid material is 5wt%.
The preparation method of the hot melt adhesive film with high metal adhesion and good flame retardance comprises the following steps:
(1) According to the weight parts, the polybutadiene polyurethane elastomer/nano-silica organic-inorganic hybrid material, the polyethylene grafted acrylic acid-2-hydroxyethyl ester copolymer, the rosin resin and the flame retardant are dispersed for 3 hours at the speed of 1500r/min, and the mixture is continuously dispersed for 30 minutes at the speed of 1000r/min by adding the reactive diluent to obtain a mixture;
(2) Putting the mixture obtained in the step (1) into a charging hopper of a double-screw extruder, and fully plasticizing the mixture by the screw extruder to obtain a molten composition;
(3) And (3) extruding the molten composition obtained in the step (2) through a die head to obtain a molten film, and cooling and shaping through a casting roller and a cooling roller to form the hot melt adhesive film.
Further, the temperatures from the feed inlet to the head of the twin-screw extruder in the step (2) are respectively as follows: 150 ℃, 180 ℃, 200 ℃, 220 ℃, 230 ℃, 250 ℃ and the screw rotating speed of 230r/min.
Further, the temperature of the die head is controlled to be 250 ℃, the temperature of the casting roll is controlled to be 120-150 ℃, and the temperature of the cooling roll is controlled to be 40-60 ℃ in the step (3).
Compared with the prior art, the invention has the beneficial effects that:
1. according to the invention, no other filler is required to be added into the system, and the silicon dioxide not only serves as a curing agent, but also plays a role of an inorganic nano filler, so that the metal bonding capability of the hot melt adhesive film is improved, and the flame retardant property of the hot melt adhesive film is also improved.
2. The inorganic flame-retardant component and the organic flame-retardant component are combined, so that the organic flame-retardant adhesive film has better compatibility with the main component of the organic adhesive film, the flame-retardant effect is improved, the influence of the flame retardant on the adhesive property and the mechanical property of the adhesive film is reduced, and the performance influence and the process difficulty caused by adding a large amount of inorganic flame retardant in the prior art are eliminated in the production and use processes of the adhesive film.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the specific embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The reagents or instruments used in the present invention are not indicated by manufacturers, and are all conventional products commercially available.
Example 1
(1) Dispersing 20 parts by weight of polybutadiene polyurethane elastomer/nano-silica organic-inorganic hybrid material, 60 parts by weight of polyethylene grafted acrylic acid-2-hydroxyethyl ester copolymer, 3 parts by weight of rosin resin, 4 parts by weight of nano-flaky magnesium hydroxide and 8 parts by weight of triphenyl phosphate at the speed of 1500r/min for 3 hours, adding 3 parts by weight of propylene oxide butyl ether, and continuously dispersing at the speed of 1000r/min for 30 minutes to obtain a mixture; wherein, the content of the silicon dioxide in the polybutadiene polyurethane elastomer/nano silicon dioxide organic-inorganic hybrid material is 5wt%.
(2) Putting the mixture obtained in the step (1) into a charging hopper of a double-screw extruder, wherein the temperatures from a charging opening to a machine head of the double-screw extruder are respectively as follows: 150 ℃, 180 ℃, 200 ℃, 220 ℃, 230 ℃, 250 ℃ and the screw rotating speed of 230r/min, and fully plasticizing by a screw extruder to obtain the molten composition.
(3) Extruding the molten composition obtained in the step (2) through a die head to obtain a molten film, cooling and shaping the molten film through a casting roller and a cooling roller to form the hot-melt adhesive film, wherein the temperature of the die head is controlled to be 250 ℃, the temperature of the casting roller is controlled to be 150 ℃, and the temperature of the cooling roller is controlled to be 50 ℃.
Example 2
(1) Dispersing 10 parts by weight of polybutadiene polyurethane elastomer/nano-silica organic-inorganic hybrid material, 50 parts by weight of polyethylene grafted acrylic acid-2-hydroxyethyl ester copolymer, 1 part by weight of rosin resin, 2 parts by weight of nano-flaky magnesium hydroxide and 6 parts by weight of isopropyl phenyl phosphate at a speed of 1500r/min for 3 hours, adding 3 parts by weight of butyl phenyl glycidyl ether, and continuously dispersing at a speed of 1000r/min for 30 minutes to obtain a mixture; wherein, the content of the silicon dioxide in the polybutadiene polyurethane elastomer/nano silicon dioxide organic-inorganic hybrid material is 5wt%.
(2) Putting the mixture obtained in the step (1) into a charging hopper of a double-screw extruder, wherein the temperatures from a charging opening to a machine head of the double-screw extruder are respectively as follows: 150 ℃, 180 ℃, 200 ℃, 220 ℃, 230 ℃, 250 ℃ and the screw rotating speed of 230r/min, and fully plasticizing by a screw extruder to obtain the molten composition.
(3) Extruding the molten composition obtained in the step (2) through a die head to obtain a molten film, cooling and shaping the molten film through a casting roller and a cooling roller to form the hot-melt adhesive film, wherein the temperature of the die head is controlled to be 250 ℃, the temperature of the casting roller is controlled to be 120 ℃, and the temperature of the cooling roller is controlled to be 40 ℃.
Example 3
(1) Dispersing 30 parts by weight of polybutadiene polyurethane elastomer/nano silicon dioxide organic-inorganic hybrid material, 80 parts by weight of polyethylene grafted acrylic acid-2-hydroxyethyl ester copolymer, 5 parts by weight of rosin resin, 5 parts by weight of nano flaky magnesium hydroxide, 10 parts by weight of tert-butyl phenyl diphosphate and 5 parts by weight of resorcinol phosphate at the speed of 1500r/min for 3 hours, adding 3 parts by weight of butyl phenyl glycidyl ether, and continuously dispersing at the speed of 1000r/min for 30 minutes to obtain a mixture; wherein, the content of the silicon dioxide in the polybutadiene polyurethane elastomer/nano silicon dioxide organic-inorganic hybrid material is 5wt%.
(2) Putting the mixture obtained in the step (1) into a charging hopper of a double-screw extruder, wherein the temperatures from a charging opening to a machine head of the double-screw extruder are respectively as follows: 150 ℃, 180 ℃, 200 ℃, 220 ℃, 230 ℃, 250 ℃ and the screw rotating speed of 230r/min, and fully plasticizing by a screw extruder to obtain the molten composition.
(3) Extruding the molten composition obtained in the step (2) through a die head to obtain a molten film, cooling and shaping the molten film through a casting roller and a cooling roller to form the hot-melt adhesive film, wherein the temperature of the die head is controlled to be 250 ℃, the temperature of the casting roller is controlled to be 150 ℃, and the temperature of the cooling roller is controlled to be 60 ℃.
Comparative example 1
(1) According to the weight parts, 20 parts of polybutadiene polyurethane elastomer, 60 parts of polyethylene, 3 parts of rosin resin, 12 parts of nano flaky magnesium hydroxide and 2 parts of silicon dioxide are dispersed for 3 hours at the speed of 1500r/min, 3 parts of propylene oxide butyl ether is added and continuously dispersed for 30 minutes at the speed of 1000r/min, and a mixture is obtained.
(2) Putting the mixture obtained in the step (1) into a charging hopper of a double-screw extruder, wherein the temperatures from a charging opening to a machine head of the double-screw extruder are respectively as follows: 150 ℃, 180 ℃, 200 ℃, 220 ℃, 230 ℃, 250 ℃ and the screw rotating speed of 230r/min, and fully plasticizing by a screw extruder to obtain the molten composition.
(3) Extruding the molten composition obtained in the step (2) through a die head to obtain a molten film, cooling and shaping the molten film through a casting roller and a cooling roller to form the hot-melt adhesive film, wherein the temperature of the die head is controlled to be 250 ℃, the temperature of the casting roller is controlled to be 150 ℃, and the temperature of the cooling roller is controlled to be 50 ℃.
The hot melt adhesive films obtained in examples 1 to 3 and comparative example 1 were subjected to the test, and the test results are shown in Table 1.
(1) Appearance: the surface of the hot melt adhesive film was visually observed for the presence of bubbles and particles.
(2) The method for testing the adhesion of the copper wire comprises the following steps: adjusting the upper and lower flat plates of the flat plate pressing machine to 100 ℃, adjusting the pressure to be less than or equal to 0.1Mpas, testing the peeling force of the sample plate within 3 seconds of pressing time, wherein the peeling speed is 50mm/min, and the adhesive force is greater than or equal to 20g/0.3mm, thus obtaining the qualified product.
(3) The test method for adhesion to PET is: adjusting the upper and lower flat plates of the flat plate pressing machine to 100 ℃, adjusting the pressure to be less than or equal to 0.1Mpas, testing the peeling force of the sample plate within 3 seconds of pressing time, wherein the peeling speed is 50mm/min, and the adhesive force is more than 10N/IN, thus obtaining the qualified product.
(4) According to the flame retardant rating of UL-94 for the halogen-free hot melt adhesive film, the highest flame retardant rating is VTM-0, then VTM-1, VTM-2, HB and the like.
TABLE 1
According to the invention, no other filler is required to be added into the system, and the silicon dioxide not only serves as a curing agent, but also plays a role of an inorganic nano filler, so that the metal bonding capability and the flame retardant property of the hot melt adhesive film are improved. The inorganic flame-retardant component and the organic flame-retardant component are combined, so that the organic flame-retardant adhesive film has better compatibility with the main component of the organic adhesive film, the flame-retardant effect is improved, the influence of the flame retardant on the adhesive property and the mechanical property of the adhesive film is reduced, and the performance influence and the process difficulty caused by adding a large amount of inorganic flame retardant in the prior art are eliminated in the production and use processes of the adhesive film.
Although the invention has been described with reference to specific embodiments, it will be understood by those skilled in the art that various changes in form and details may be made therein without departing from the spirit and scope of the invention.
Claims (10)
1. A hot melt adhesive film with high metal adhesion and good flame retardance is characterized in that: comprises the following components:
50-80 parts of polyethylene grafted acrylic acid-2-hydroxyethyl ester copolymer,
10-30 parts of polybutadiene polyurethane elastomer/nano silicon dioxide organic-inorganic hybrid material,
1 to 5 parts by weight of rosin resin,
8-15 parts by weight of a flame retardant,
1-5 parts of reactive diluent.
2. The hot melt adhesive film with high metal adhesion and good flame retardancy as claimed in claim 1, wherein: the reactive diluent is an epoxy reactive diluent.
3. The hot melt adhesive film with high viscous metal force and good flame retardancy as claimed in claim 2, wherein: the epoxy active diluent is one or more of epoxypropane butyl ether, butyl phenyl glycidyl ether and propenyl glycidyl ether.
4. The hot melt adhesive film with high metal adhesion and good flame retardancy as claimed in claim 1, wherein: the flame retardant is a mixture of nano flaky magnesium hydroxide and an organic phosphorus flame retardant.
5. The hot melt adhesive film with high metal adhesion and good flame retardancy as claimed in claim 4, wherein: the organic phosphorus flame retardant is a phosphate compound.
6. The hot melt adhesive film with high viscous metal force and good flame retardance as claimed in claim 5, wherein: the phosphate is one or more of triphenyl phosphate, isopropyl phenyl phosphate, tert-butyl phenyl phosphate and resorcinol phosphate.
7. The hot melt adhesive film with high viscous metal force and good flame retardancy as claimed in claim 1, wherein: the content of silicon dioxide in the polybutadiene polyurethane elastomer/nano silicon dioxide organic-inorganic hybrid material is 5wt%.
8. The method for preparing a hot-melt adhesive film with high viscous metal force and good flame retardancy according to any one of claims 1 to 7, wherein the method comprises the following steps: the method comprises the following steps:
(1) According to the weight parts, the polybutadiene polyurethane elastomer/nano-silica organic-inorganic hybrid material, the polyethylene grafted acrylic acid-2-hydroxyethyl ester copolymer, the rosin resin and the flame retardant are dispersed for 3 hours at the speed of 1500r/min, and the mixture is continuously dispersed for 30 minutes at the speed of 1000r/min by adding the reactive diluent to obtain a mixture;
(2) Putting the mixture obtained in the step (1) into a charging hopper of a double-screw extruder, and fully plasticizing the mixture by the screw extruder to obtain a molten composition;
(3) And (3) extruding the molten composition obtained in the step (2) through a die head to obtain a molten film, and cooling and shaping the molten film through a casting roller and a cooling roller to form the hot melt adhesive film.
9. The method for preparing a hot-melt adhesive film with high metal adhesion and good flame retardance according to claim 8, wherein the method comprises the following steps: the temperature from the feed inlet of the double-screw extruder to the head in the step (2) is respectively as follows: 150 ℃, 180 ℃, 200 ℃, 220 ℃, 230 ℃, 250 ℃ and the screw rotating speed of 230r/min.
10. The method for preparing a hot melt adhesive film with high metal adhesion and good flame retardance according to claim 8, wherein the method comprises the following steps: in the step (3), the temperature of the die head is controlled to be 250 ℃, the temperature of the casting roller is controlled to be 120-150 ℃, and the temperature of the cooling roller is controlled to be 40-60 ℃.
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