CN115011281A - High-viscosity metal hot-melt adhesive film and preparation method thereof - Google Patents

High-viscosity metal hot-melt adhesive film and preparation method thereof Download PDF

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Publication number
CN115011281A
CN115011281A CN202210414163.9A CN202210414163A CN115011281A CN 115011281 A CN115011281 A CN 115011281A CN 202210414163 A CN202210414163 A CN 202210414163A CN 115011281 A CN115011281 A CN 115011281A
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Prior art keywords
melt adhesive
adhesive film
hot
viscosity
metal
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Inventor
宾家荃
宾家齐
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Guangdong Huiqi New Material Co ltd
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Guangdong Huiqi New Material Co ltd
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Priority to CN202210414163.9A priority Critical patent/CN115011281A/en
Priority to PCT/CN2022/092761 priority patent/WO2023201795A1/en
Publication of CN115011281A publication Critical patent/CN115011281A/en
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    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09JADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J123/00Adhesives based on homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Adhesives based on derivatives of such polymers
    • C09J123/02Adhesives based on homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Adhesives based on derivatives of such polymers not modified by chemical after-treatment
    • C09J123/04Homopolymers or copolymers of ethene
    • C09J123/08Copolymers of ethene
    • C09J123/0846Copolymers of ethene with unsaturated hydrocarbons containing other atoms than carbon or hydrogen atoms
    • C09J123/0853Vinylacetate
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09JADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J11/00Features of adhesives not provided for in group C09J9/00, e.g. additives
    • C09J11/02Non-macromolecular additives
    • C09J11/04Non-macromolecular additives inorganic
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09JADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J7/00Adhesives in the form of films or foils
    • C09J7/10Adhesives in the form of films or foils without carriers
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09JADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J7/00Adhesives in the form of films or foils
    • C09J7/30Adhesives in the form of films or foils characterised by the adhesive composition
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/02Elements
    • C08K3/08Metals
    • C08K2003/0856Iron
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K2201/00Specific properties of additives
    • C08K2201/01Magnetic additives
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09JADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J2301/00Additional features of adhesives in the form of films or foils
    • C09J2301/40Additional features of adhesives in the form of films or foils characterized by the presence of essential components
    • C09J2301/408Additional 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
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02EREDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E10/00Energy generation through renewable energy sources
    • Y02E10/50Photovoltaic [PV] energy

Abstract

The invention relates to the field of hot melt adhesive film materials, in particular to a high-viscosity metal hot melt adhesive film, which comprises the following components in parts by mass: 50-80 parts of ethylene-vinyl acetate copolymer; 20-35 parts of high-viscosity metal resin; 5-10 parts of surface modified far infrared ceramic powder; 3-8 parts of permanent magnetic material powder; 1-4 parts of rosin derivatives; 0.1-1 part of functional assistant. The invention provides a high-viscosity hot melt adhesive film with excellent performance. The invention also provides a preparation method of the high-viscosity metal hot-melt adhesive film, which is simple in process and convenient and fast to operate.

Description

High-viscosity metal hot-melt adhesive film and preparation method thereof
Technical Field
The invention relates to the field of hot melt adhesive film materials, in particular to a high-viscosity metal-strength hot melt adhesive film and a preparation method thereof.
Background
The hot melt adhesive film is a film product with or without release paper, and can be conveniently operated continuously or intermittently. Can be widely used for bonding various fabrics, paper, high polymer materials and metals.
The existing hot melt adhesive film has poor metal adhesion force, and the metal adhesion force cannot be maintained for a long time, so that the hot melt adhesive film is separated due to the reduction or loss of the metal adhesion force of the hot melt adhesive film after the product is used for a period of time.
Disclosure of Invention
In order to solve the technical problems, the invention provides a high-viscosity hot-melt adhesive film with excellent performance.
The invention also provides a preparation method of the high-viscosity metal hot-melt adhesive film, which is simple in process and convenient and fast to operate.
The invention adopts the following technical scheme:
a hot melt adhesive film with high metal viscosity comprises the following components in parts by mass:
Figure BDA0003601446330000011
the technical proposal is further improved that the content of the vinyl acetate in the ethylene-vinyl acetate copolymer is 30 to 40 percent.
The technical proposal is further improved that the high-viscosity metal resin is bisphenol A epoxy resin.
The technical proposal is further improved that the glass transition temperature of the high-viscosity metal resin is 70-85 ℃, the softening point is 90-100 ℃, the molecular weight is 30000-41000, and the hydroxyl value is 4-5 mgKOH/g.
The technical proposal is further improved that the preparation method of the surface modified nano far infrared ceramic powder comprises the following steps: dissolving a coupling agent in the solution, performing ultrasonic dispersion for 10min, adjusting the pH value to 5-6, adding 10-25g of dried nano far-infrared ceramic powder after stirring for stabilization, performing ultrasonic dispersion for 20min, performing water bath at 65 ℃ for 20min, and finally drying, cooling and grinding the mixed solution to obtain the surface modified nano far-infrared ceramic powder.
The technical proposal is further improved in that the solution is a mixed solution of ethanol and water.
The technical proposal is further improved in that the rosin derivative is one of disproportionated rosin, acrylic acid rosin, maleic rosin, dehydroabietic acid and maleopimaric acid.
The technical proposal is further improved in that the permanent magnetic material powder is neodymium iron boron powder.
The technical proposal is further improved in that the auxiliary agent comprises one or a mixture of two of an ultraviolet absorbent, an antioxidant and a crosslinking agent.
A preparation method of a hot melt adhesive film with high viscous metal force comprises the following steps:
s1, uniformly mixing the raw materials in proportion, heating the mixture in a stirrer to 250-300 ℃ to melt the raw materials to obtain a uniformly mixed mixture;
s2, placing the mixture in a granulator for granulation and drying to obtain hot melt adhesive particles;
and S3, placing the hot melt adhesive particles in a film making forming machine to prepare the high-viscosity metal hot melt adhesive film.
The invention has the beneficial effects that:
1. the invention adopts bisphenol A type epoxy resin as the high-viscosity metal resin. Bisphenol A epoxy resin is a high molecular compound prepared by condensing bisphenol A and epichlorohydrin under an alkaline condition, washing with water, and removing a solvent. The epoxy group and the hydroxyl group endow the resin with reactivity, so that a cured resin has strong cohesive force and adhesive force; ether bonds and hydroxyl groups are polar groups, which contribute to improved wettability and adhesion; the benzene ring imparts heat resistance and rigidity to the polymer; the bond energy of the-C-O-bond is high, thereby improving the alkali resistance. Therefore, the matching use of the bisphenol A type epoxy resin and the ethylene-vinyl acetate copolymer can improve the metal adhesion force of the hot melt adhesive film and simultaneously can keep the metal adhesion force at a higher level for a long time.
2. The invention also introduces the surface modified far infrared ceramic powder and the permanent magnetic material powder, so that the invention can provide energy for far infrared emission and increase the emission intensity; secondly, the weak magnetic field has physiological activity to the organism, so that the product using the hot melt adhesive film has double health care functions of far infrared and magnetic field.
Detailed Description
The invention will now be further illustrated by reference to specific examples, which are intended to be illustrative of the invention and are not intended to be a further limitation of the invention.
A hot melt adhesive film with high metal viscosity comprises the following components in parts by mass: 50-80 parts of ethylene-vinyl acetate copolymer; 20-35 parts of high-viscosity metal resin; 5-10 parts of surface modified far infrared ceramic powder; 3-8 parts of permanent magnetic material powder; 1-4 parts of rosin derivatives; 0.1-1 part of functional assistant.
Further, the ethylene-vinyl acetate copolymer has a vinyl acetate content of 30% to 40%.
Further, the high-viscosity metal force resin includes, but is not limited to, bisphenol a type epoxy resin.
Furthermore, the glass transition temperature of the high-viscosity metal resin is 70-85 ℃, the softening point is 90-100 ℃, the molecular weight is 30000-41000, and the hydroxyl value is 4-5 mgKOH/g.
Further, the preparation method of the surface modified nano far infrared ceramic powder comprises the following steps: dissolving a coupling agent in the solution, performing ultrasonic dispersion for 10min, adjusting the pH value to 5-6, adding 10-25g of dried nano far-infrared ceramic powder after stirring for stabilization, performing ultrasonic dispersion for 20min, performing water bath at 65 ℃ for 20min, and finally drying, cooling and grinding the mixed solution to obtain the surface modified nano far-infrared ceramic powder.
Further, the solution is a mixed solution of ethanol and water.
Further, the rosin derivative includes, but is not limited to, one of disproportionated rosin, acrylic rosin, maleic rosin, dehydroabietic acid, and maleopimaric acid.
Further, the powder of the permanent magnetic material includes, but is not limited to, neodymium iron boron powder.
Further, the auxiliary agent includes but is not limited to one or a mixture of two of ultraviolet absorbent, antioxidant and crosslinking agent.
A preparation method of a hot melt adhesive film with high viscous metal force comprises the following steps:
s1, uniformly mixing the raw materials in proportion, heating the mixture in a stirrer to 250-300 ℃ to melt the raw materials to obtain a uniformly mixed mixture;
s2, placing the mixture in a granulator for granulation and drying to obtain hot melt adhesive particles;
and S3, placing the hot melt adhesive particles in a film making forming machine to prepare the high-viscosity metal hot melt adhesive film.
Example 1
A preparation method of a hot melt adhesive film with high viscous metal force comprises the following steps:
s1, 50 parts of ethylene-vinyl acetate copolymer; 20 parts of bisphenol A epoxy resin; 5 parts of surface modified far infrared ceramic powder; 3 parts of neodymium iron boron powder; 1 part of rosin derivative; 0.5 part of functional auxiliary agent is uniformly mixed according to the proportion, and the mixture is heated to 250 ℃ in a stirrer to melt the raw materials to obtain a uniformly mixed mixture;
s2, placing the mixture in a granulator for granulation and drying to obtain hot melt adhesive particles;
and S3, placing the hot melt adhesive particles in a film making forming machine to prepare the high-viscosity metal hot melt adhesive film.
Example 2
A preparation method of a hot melt adhesive film with high viscous metal force comprises the following steps:
s1, mixing 80 parts of ethylene-vinyl acetate copolymer; 35 parts of bisphenol A type epoxy resin; 10 parts of surface modified far infrared ceramic powder; 8 parts of neodymium iron boron powder; 4 parts of rosin derivative; 1 part of functional additive is uniformly mixed according to a proportion, and the mixture is heated to 300 ℃ in a stirrer to melt the raw materials to obtain a uniformly mixed mixture;
s2, placing the mixture in a granulator for granulation and drying to obtain hot melt adhesive particles;
and S3, placing the hot melt adhesive particles in a film making forming machine to prepare the high-viscosity metal hot melt adhesive film.
Comparative example 1
The components and steps are the same as those in example 1 except that the components of bisphenol a type epoxy resin, surface modified far infrared ceramic powder and neodymium iron boron powder are omitted.
Comparative example 2
The components and steps are the same as those in example 2 except that the components of bisphenol a type epoxy resin, surface modified far infrared ceramic powder and neodymium iron boron powder are omitted.
The hot melt adhesive films obtained in examples 1 to 2 and comparative examples 1 to 2 were subjected to adhesion test, tensile strength test and heat resistance test by the following test methods, as shown in Table 1.
The test method is as follows:
1. and (3) testing the instant metal adhesion force:
step 1: taking a sample of 25.4 × 150mm, generally 1 Pcs;
step 2: sticking transparent adhesive on PET surfaces at two ends of a sample, reserving a half, and sticking 2Pcs of a tinned wire and bare copper with specifications of 0.35mm multiplied by 0.30mm on the transparent adhesive in parallel with the cut edge of the sample;
and step 3: pressing at 170 deg.C at a speed of 1.5m/min and a pressure of 0.4mpa.s, and standing for 5 min;
and 4, step 4: 2cm of metal wires are pulled open and placed on an upper chuck of a tensile machine, a sample film is placed on a lower chuck, and the span between the chucks of the tensile machine is set to be 20mm (the speed is 100 mm/min);
and 5: the testing stroke is 50-70mm, the average force displayed by the tensile machine is recorded, the force is the metal bonding force (g/0.3mm) of the tested sample, and when the metal bonding force is more than or equal to 26g/0.3mm, the product reaches the qualified standard.
2. 85%, 145 ℃, 24 hour metal adhesion test:
step 1: taking a sample of 25.4 × 150mm, generally 1 Pcs;
step 2: adhering transparent adhesive to PET surfaces at two ends of a sample, reserving a half, and adhering 2Pcs of a tinned wire and bare copper with specifications of 0.35mm multiplied by 0.30mm to the transparent adhesive in parallel with the trimming edge of the sample;
and step 3: pressing at 170 deg.C at speed of 1.5m/min and pressure of 0.4mpa.s, and placing in oven at 85% and 145 deg.C for 24 hr;
and 4, step 4: 2cm of metal wires are pulled open and placed on an upper chuck of a tensile machine, a sample film is placed on a lower chuck, and the span between the chucks of the tensile machine is set to be 20mm (the speed is 100 mm/min);
and 5: the testing stroke is 50-70mm, the average force displayed by a tensile machine is recorded, the force is the metal adhesion force (g/0.3mm) of the tested sample, and when the metal adhesion force is more than or equal to 30g/0.3mm, the product reaches the qualified standard.
3. Tensile strength: the test specimens were stretched until they broke during the tensile test according to ISO 527-.
Figure BDA0003601446330000051
Figure BDA0003601446330000061
Variations and modifications to the above-described embodiments may also occur to those skilled in the art to which the invention pertains. Therefore, the above examples illustrate the detailed methods of the present invention, but the present invention is not limited to the specific embodiments disclosed and described above, and it is not intended that the present invention be implemented by relying on the above detailed methods, any modifications and variations of the present invention, equivalent substitutions of each raw material of the product of the present invention, addition of auxiliary components, selection of specific embodiments, etc., should also fall within the scope of the claims of the present invention.

Claims (10)

1. The hot melt adhesive film with high metal viscosity is characterized by comprising the following components in parts by mass:
Figure FDA0003601446320000011
2. a high viscous metal hot-melt adhesive film according to claim 1, wherein the ethylene-vinyl acetate copolymer has a vinyl acetate content of 30 to 40%.
3. A high viscous metal hot-melt adhesive film according to claim 1, wherein the high viscous metal resin is a bisphenol a type epoxy resin.
4. The high-viscosity hot-melt adhesive film as claimed in claim 1, wherein the high-viscosity resin has a glass transition temperature of 70-85 ℃, a softening point of 90-100 ℃, a molecular weight of 30000-41000 and a hydroxyl value of 4-5 mgKOH/g.
5. The high-viscosity metal hot-melt adhesive film as claimed in claim 1, wherein the preparation method of the surface-modified nano far-infrared ceramic powder comprises the following steps: dissolving a coupling agent in the solution, performing ultrasonic dispersion for 10min, adjusting the pH value to 5-6, adding 10-25g of dried nano far-infrared ceramic powder after stirring for stabilization, performing ultrasonic dispersion for 20min, performing water bath at 65 ℃ for 20min, and finally drying, cooling and grinding the mixed solution to obtain the surface modified nano far-infrared ceramic powder.
6. A high-tack hot-melt adhesive film according to claim 5, wherein the solution is a mixed solution of ethanol and water.
7. A hot-melt adhesive film with high cohesive force according to claim 1, wherein said rosin derivative is one of disproportionated rosin, acrylic rosin, maleated rosin, dehydroabietic acid, and maleopimaric acid.
8. A high viscous metal hot melt adhesive film according to claim 1, wherein the permanent magnetic material powder is neodymium iron boron powder.
9. A high-tack metal hot-melt adhesive film as claimed in claim 1, wherein the auxiliary agent comprises one or a mixture of two of an ultraviolet absorber, an antioxidant and a crosslinking agent.
10. The preparation method of the hot melt adhesive film with high viscous metal force is characterized by comprising the following steps:
s1, uniformly mixing the raw materials in proportion, heating the mixture in a stirrer to 250-300 ℃ to melt the raw materials to obtain a uniformly mixed mixture;
s2, placing the mixture in a granulator for granulation and drying to obtain hot melt adhesive particles;
and S3, placing the hot melt adhesive particles in a film making forming machine to prepare the high-viscosity metal hot melt adhesive film.
CN202210414163.9A 2022-04-18 2022-04-18 High-viscosity metal hot-melt adhesive film and preparation method thereof Pending CN115011281A (en)

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CN202210414163.9A CN115011281A (en) 2022-04-18 2022-04-18 High-viscosity metal hot-melt adhesive film and preparation method thereof
PCT/CN2022/092761 WO2023201795A1 (en) 2022-04-18 2022-05-13 Hot melt adhesive film having high-viscosity metal force and preparation method therefor

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Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1129640A (en) * 1995-10-21 1996-08-28 熊显耀 Far infrared melting plastic films and preparation thereof
CN103666352A (en) * 2012-09-20 2014-03-26 中国石油化工股份有限公司 Special-purpose adhesive for beer and beverage bottle cap gasket and preparation method thereof
CN104927707A (en) * 2015-05-27 2015-09-23 合肥卓元科技服务有限公司 High-temperature-resistant hot melt adhesive and preparation method for same
CN105385369A (en) * 2015-12-17 2016-03-09 江苏宇昊新能源科技有限公司 EVA film used for double glass photovoltaic module and preparation method thereof
US20190001635A1 (en) * 2015-08-06 2019-01-03 Fujimori Kogyo Co., Ltd. Hot-melt adhesive resin film and production method thereof

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Publication number Priority date Publication date Assignee Title
JP4333829B2 (en) * 2002-03-07 2009-09-16 日立化成ポリマー株式会社 Adhesive composition
CN103571392B (en) * 2013-10-24 2016-04-13 芜湖众力部件有限公司 A kind of Anti-corrosion hot melt adhesive for automotive upholstery
CN103571375A (en) * 2013-10-24 2014-02-12 芜湖众力部件有限公司 Epoxy resin hot melt adhesive
CN103756577B (en) * 2013-12-31 2015-08-19 广州鹿山新材料股份有限公司 A kind of PVC/ metal sticking hot melt adhesive film and preparation method thereof
CN108587508B (en) * 2018-03-29 2021-04-06 广东莱尔新材料科技股份有限公司 High-viscosity metal hot-melt adhesive film and preparation method thereof

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1129640A (en) * 1995-10-21 1996-08-28 熊显耀 Far infrared melting plastic films and preparation thereof
CN103666352A (en) * 2012-09-20 2014-03-26 中国石油化工股份有限公司 Special-purpose adhesive for beer and beverage bottle cap gasket and preparation method thereof
CN104927707A (en) * 2015-05-27 2015-09-23 合肥卓元科技服务有限公司 High-temperature-resistant hot melt adhesive and preparation method for same
US20190001635A1 (en) * 2015-08-06 2019-01-03 Fujimori Kogyo Co., Ltd. Hot-melt adhesive resin film and production method thereof
CN105385369A (en) * 2015-12-17 2016-03-09 江苏宇昊新能源科技有限公司 EVA film used for double glass photovoltaic module and preparation method thereof

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