CN111171750A - Hot melt adhesive film for automotive interior ceiling and production method thereof - Google Patents

Hot melt adhesive film for automotive interior ceiling and production method thereof Download PDF

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Publication number
CN111171750A
CN111171750A CN202010203856.4A CN202010203856A CN111171750A CN 111171750 A CN111171750 A CN 111171750A CN 202010203856 A CN202010203856 A CN 202010203856A CN 111171750 A CN111171750 A CN 111171750A
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Prior art keywords
parts
adhesive film
melt adhesive
hot melt
antioxidant
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CN202010203856.4A
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Chinese (zh)
Inventor
郭焕祥
单汝坤
朱维珍
王克强
周光远
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Yantai Zhenghai High Technology Co ltd
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Yantai Zhenghai High Technology Co ltd
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Priority to CN202010203856.4A priority Critical patent/CN111171750A/en
Publication of CN111171750A publication Critical patent/CN111171750A/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
    • C09J7/00Adhesives in the form of films or foils
    • C09J7/30Adhesives in the form of films or foils characterised by the adhesive composition
    • C09J7/35Heat-activated
    • 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
    • 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
    • C09J123/06Polyethene
    • 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
    • C09J7/00Adhesives in the form of films or foils
    • C09J7/10Adhesives in the form of films or foils without carriers
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2205/00Polymer mixtures characterised by other features
    • C08L2205/03Polymer mixtures characterised by other features containing three or more polymers in a blend

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Adhesives Or Adhesive Processes (AREA)

Abstract

The invention relates to a hot melt adhesive film for an automotive interior ceiling, which comprises main materials of polyethylene and a copolymer thereof, and auxiliary materials of polyisobutylene, tackifying resin, white carbon black, a coupling agent, a surfactant, an antioxidant and a stabilizer; the weight ratio is as follows: 10000 parts of polyethylene and copolymer thereof, 50-500 parts of polyisobutylene, and the weight ratio of tackifying resin, white carbon black, coupling agent and surfactant is 20-70: 30-80: 3-10: 1-5, 50-200 parts of a mixture prepared from the raw materials, 5-30 parts of an antioxidant and 10-100 parts of a stabilizer. Compared with the traditional adhesive film, the adhesive film disclosed by the invention has better adhesive strength, heat resistance and aging resistance.

Description

Hot melt adhesive film for automotive interior ceiling and production method thereof
Technical Field
The invention relates to a hot melt adhesive film and a production method thereof, in particular to a hot melt adhesive film for an automotive interior ceiling and a production method thereof.
Background
The automotive interior ceiling is divided into a dry method and a wet method, the middle layer is a PU foam board, the two surfaces of the middle layer are provided with glass fibers for reinforcement, and the upper surface and the lower surface of the middle layer are provided with fabric and back layer non-woven fabrics; the dry method adopts thermoplastic glue powder or a glue film as a bonding material, and the wet method adopts thermosetting liquid glue as a bonding material; since the liquid glue is generally a polyurethane material and contains many small molecular materials, the odor and VOC indexes are crossed and inferior to those of a dry ceiling.
The dry-method automobile interior ceiling adopts thermoplastic glue film or glue powder to bond the PU foam board, the glass fiber, the back non-woven fabric and the surface decorative material. The rubber powder is easy to generate dust in the using process, the working environment is poor, and the rubber powder is subjected to the fouling of operators. Glue films are gradually becoming the mainstream adhesive material for dry ceiling.
However, the dry ceiling has a problem of poor heat resistance and unsatisfactory adhesion strength because it is a thermoplastic adhesive material regardless of whether a rubber powder or a glue film is used. Therefore, the development of a hot melt adhesive film with good adhesiveness is a technical problem which needs to be solved urgently by the dry ceiling technology.
Disclosure of Invention
The invention aims to provide a hot melt adhesive film with better heat resistance and adhesiveness.
The technical scheme of the invention is as follows:
a hot melt adhesive film for an automotive interior ceiling is characterized in that a main material is polyethylene and a copolymer thereof, and an auxiliary material comprises polyisobutylene, tackifying resin, white carbon black, a coupling agent, a surfactant, an antioxidant and a stabilizer;
the weight ratio is as follows: 10000 parts of polyethylene and copolymer thereof, 50-500 parts of polyisobutylene, and the weight ratio of tackifying resin, white carbon black, coupling agent and surfactant is 20-70: 30-80: 3-10: 1-5, 50-200 parts of a mixture, 5-30 parts of an antioxidant and 10-100 parts of a stabilizer;
wherein,
3000-8000 parts of polyethylene and 7000-2000 parts of polyethylene copolymer;
the tackifying resin is one or more of 2402 tackifying resin, 202 tackifying resin, C9 petroleum resin, WL brominated resin and SP-1055 brominated resin;
the white carbon black is precipitated white carbon black;
the coupling agent is one or more of KH540, KH550, KH570, SI-69 and SI-75;
the surfactant is a cationic surfactant or a nonionic surfactant;
the antioxidant is one or more of 1010 antioxidant and 1076 antioxidant;
the stabilizer is one or more of magnesium oxide, calcium oxide and lead oxide.
Further, the auxiliary materials also contain 1-5 parts of microporous foaming agent, and the microporous foaming agent is one or more of OBSH, EMA80AH, WQFP-2, NBFP-1, KX-565 and other brands;
the production method of the hot melt adhesive film is characterized in that,
firstly, adding tackifying resin, white carbon black, a coupling agent and a surfactant in auxiliary materials according to the weight ratio of 20-70: 30-80: 3-10: 1-5, and then spray-drying to prepare the bonding modified filler (the other auxiliary materials are directly mixed with the main material);
then preparing the following ingredients in parts by weight: 50-500 parts of bonding modified filler, 10000 parts of polyethylene and copolymer thereof, 50-500 parts of polyisobutylene, 5-30 parts of antioxidant and 10-100 parts of stabilizer, and the components are melted, blended, extruded and granulated in a double-screw extruder;
the particles are put into hot melt adhesive film production equipment to prepare the hot melt adhesive film.
The raw materials of the hot melt adhesive film are subjected to melt blending modification by using resin containing special functional groups, so that a series of hot melt adhesive film raw materials with high bonding strength and heat resistance can be prepared. In addition, the low-magnification microsphere foaming agent is introduced into the preparation process of the hot melt adhesive film raw material, so that the density of the hot melt adhesive film raw material can be greatly reduced, and a new research approach for reducing the weight of the automobile hot melt adhesive film is added. The final hot melt adhesive film raw material is made into a film in the casting equipment, the film forming process is good, the appearance of the hot melt adhesive film is consistent with that of an original product, the prepared hot melt adhesive film not only has higher bonding strength than that of a traditional hot melt adhesive film, but also has the density reduced by 3% -10% than that of a traditional hot melt adhesive film product due to the action of microcellular foaming. On the other hand, the physical and mechanical properties, the heat resistance and the aging resistance of the novel hot melt adhesive film prepared by the invention, especially the aging condition of the bonding strength are improved compared with the original product.
Detailed Description
The PU foam board used for the automotive interior ceiling has low strength and is easy to break materials when testing the adhesive force, so that the schemes with good adhesive property are difficult to distinguish by testing numerical values, and the glass fiber also belongs to a reticular material and is not beneficial to the evaluation of the adhesive effect, so the polyethylene board and the steel board are adopted as the adhesive objects.
Example 1
Tackifying resin 2402, white carbon black SI-175, coupling agent KH550 and surfactant sodium dodecyl benzene sulfonate in a mass ratio of 50: 50: 10: 2, sequentially adding the mixture into a high-stirring machine, and drying the mixture in a drying machine after the samples are uniformly stirred to prepare the bonding modified filler for later use.
200 g of bonding modified filler, 2 g of microporous foaming agent OBSH [ 4, 4' -oxybis-benzenesulfonylhydrazide ], 10 kg of polyethylene, 100 g of polyisobutylene, 10 g of antioxidant 1010 and 10 g of magnesium oxide are melted and blended in a double-screw extruder, and extruded and granulated to obtain the hot melt adhesive film granules. And putting the hot melt adhesive film granules into casting equipment to prepare the hot melt adhesive film. The obtained hot-melt adhesive film was tested for its adhesive strength with polyethylene sheets and stainless steel sheets, physical and mechanical properties, heat resistance, aging resistance and adhesive strength after aging, see table 1.
Comparative example 1
10 kg of polyethylene, 100 g of polyisobutylene, 10 g of antioxidant 1010 and 10 g of magnesium oxide are melted and blended in a double-screw extruder, and then extruded and granulated. And putting the hot melt adhesive film granules into a film blowing machine to prepare the hot melt adhesive film. The obtained hot-melt adhesive film was tested for its adhesive strength with polyethylene sheets and stainless steel sheets, physical and mechanical properties, heat resistance, aging resistance and adhesive strength after aging, see table 1.
Example 2
WL brominated resin, white carbon black SI-175, a coupling agent KH570 and a surfactant sodium dodecyl benzene sulfonate are mixed according to the mass ratio of 70: 30: 10: 1, sequentially putting the materials into a high-stirring machine, and drying the materials in a drying machine after the samples are uniformly stirred to obtain the bonding modified filler for later use.
100 g of bonding modified filler, 1 g of microporous foaming agent EMA80AH, 10 kg of ethylene-vinyl acetate copolymer (EVA), 100 g of polyisobutylene, 10 g of antioxidant 1076 and 10 g of magnesium oxide are melted and blended in a double-screw extruder, and extruded and granulated. And putting the hot melt adhesive film granules into a film blowing machine to prepare the hot melt adhesive film. The obtained hot-melt adhesive film was tested for its adhesive strength with polyethylene sheets and stainless steel sheets, physical and mechanical properties, heat resistance, aging resistance and adhesive strength after aging, see table 1.
Comparative example 2
10 kg of ethylene-vinyl acetate copolymer (EVA), 100 g of polyisobutylene, 10 g of antioxidant 1076 and 10 g of magnesium oxide are melted and blended in a double-screw extruder, and then extruded and granulated. And (3) putting the hot melt adhesive film granules into a casting machine to prepare the hot melt adhesive film. The adhesion strength, physical and mechanical properties, heat resistance, aging resistance and adhesion strength after aging of the obtained hot melt adhesive film, polyethylene plate and stainless steel plate were tested, see table 1.
Example 3
Brominated resin SP-1055, white carbon black SI-175, a coupling agent SI-69 and a surfactant alkyl polyoxyethylene ether are mixed according to the mass ratio of 30: 70: 5: 1, sequentially adding the materials into a high-stirring machine, uniformly stirring the samples, and drying the samples in a drying machine to obtain the bonding modified filler for later use.
100 g of bonding modified filler, 5 g of microporous foaming agent WQFP-2, 5 kg of ethylene-vinyl acetate copolymer (EVA), 5 kg of polyethylene, 500 g of polyisobutylene, 5 g of antioxidant 1010 and 10 g of magnesium oxide are melted and blended in a double-screw extruder, and then extruded and granulated. And (3) putting the hot melt adhesive film granules into a casting machine to prepare the hot melt adhesive film. The obtained hot-melt adhesive film was tested for its adhesive strength with polyethylene sheets and stainless steel sheets, physical and mechanical properties, heat resistance, aging resistance and adhesive strength after aging, see table 1.
Comparative example 3
5 kg of ethylene-vinyl acetate copolymer (EVA), 5 kg of polyethylene, 500 g of polyisobutylene, 3 g of antioxidant 1010 and 8 g of magnesium oxide are melted and blended in a double-screw extruder, and then extruded and granulated. And (3) putting the hot melt adhesive film granules into a casting machine to prepare the hot melt adhesive film. The obtained hot-melt adhesive film was tested for its adhesive strength with polyethylene sheets and stainless steel sheets, physical and mechanical properties, heat resistance, aging resistance and adhesive strength after aging, see table 1.
Example 4
Tackifying resin 202, white carbon black SI-175, coupling agent SI-75 and surfactant polyoxyethylene sorbitan monooleate in a mass ratio of 70: 30: 3: and 5, sequentially adding the materials into a high-stirring machine, and drying in a drying machine after the samples are uniformly stirred to obtain the bonding modified filler for later use.
100 g of bonding modified filler, 3 g of microporous foaming agent NBFP-1, 7 kg of ethylene-vinyl acetate copolymer (EVA), 3 kg of polyethylene, 200 g of polyisobutylene, 20 g of antioxidant 1076 and 50g of calcium oxide are melted and blended in a double-screw extruder, and then extruded and granulated. And (3) putting the hot melt adhesive film granules into a casting machine to prepare the hot melt adhesive film. The obtained hot-melt adhesive film was tested for its adhesive strength with polyethylene sheets and stainless steel sheets, physical and mechanical properties, heat resistance, aging resistance and adhesive strength after aging, see table 1.
Comparative example 4
7 kg of ethylene-vinyl acetate copolymer (EVA), 3 kg of polyethylene, 200 g of polyisobutylene, 20 g of antioxidant 1076 and 50g of calcium oxide are melted and blended in a double-screw extruder, and then extruded and granulated. And (3) putting the hot melt adhesive film granules into a casting machine to prepare the hot melt adhesive film. The obtained hot-melt adhesive film was tested for its adhesive strength with polyethylene sheets and stainless steel sheets, physical and mechanical properties, heat resistance, aging resistance and adhesive strength after aging, see table 1.
Example 5
Tackifying resin C9, white carbon black SI-175, coupling agent KH540 and surfactant sorbitan fatty acid ester in a mass ratio of 20: 80: 5: 1, sequentially adding the raw materials into the aqueous solution, and drying in a dryer after the samples are uniformly stirred to obtain the bonding modified filler for later use.
50g of bonding modified filler, 1 g of microporous foaming agent KX-565, 4 kg of ethylene-vinyl acetate copolymer (EVA), 6 kg of polyethylene, 50g of polyisobutylene, 30 g of antioxidant 1010 and 100 g of lead oxide are melted and blended in a double-screw extruder, and then extruded and granulated. And putting the hot melt adhesive film granules into a film blowing machine to prepare the hot melt adhesive film. The obtained hot-melt adhesive film was tested for its adhesive strength with polyethylene sheets and stainless steel sheets, physical and mechanical properties, heat resistance, aging resistance and adhesive strength after aging, see table 1.
Comparative example 5
4 kg of ethylene-vinyl acetate copolymer (EVA), 6 kg of polyethylene, 50g of polyisobutylene, 30 g of antioxidant 1010 and 100 g of lead oxide are melted and blended in a double-screw extruder, and then extruded and granulated. And putting the hot melt adhesive film granules into a film blowing machine to prepare the hot melt adhesive film. The obtained hot-melt adhesive film was tested for its adhesive strength with polyethylene sheets and stainless steel sheets, physical and mechanical properties, heat resistance, aging resistance and adhesive strength after aging, see table 1.
Table 1 shows the properties of the hot melt adhesive films obtained in the examples and comparative examples of the present invention.
As can be seen from table 1, the examples are better than the corresponding comparative examples except for the elongation at break: the high-strength polyethylene alloy has high tensile strength, high bonding strength with a PE plate, high bonding strength with a stainless steel plate, high protection rate of the bonding strength with metal after aging for 48 hours at 100 ℃, and low density. In particular, the fabric is bonded with a stainless steel plate, the bonding width is 50mm, a weight of 50g is hung on the upper end of the fabric, the fabric is subjected to a high-temperature peeling test without falling off for 2 hours at 110 ℃, all the examples pass, all the comparative examples do not pass, and the scheme of the application is fully proved to have remarkable improvement on heat resistance.
TABLE 1 Properties of hot-melt adhesive films prepared according to different formulations
Figure 241787DEST_PATH_IMAGE002
Bonding strength with PE sheet: the tensile shear strength of the adhesive is measured according to GB/T7124-2008 (rigid material to rigid material);
bonding strength with stainless steel plate: the tensile shear strength of the adhesive is measured according to GB/T7124-2008 (rigid material to rigid material);
retention ratio of metal adhesion strength = (metal adhesion strength after aging/metal adhesion strength before aging) × 100%.

Claims (3)

1. A hot melt adhesive film for an automotive interior ceiling is characterized in that a main material is polyethylene and a copolymer thereof, and an auxiliary material comprises polyisobutylene, tackifying resin, white carbon black, a coupling agent, a surfactant, an antioxidant and a stabilizer;
the weight ratio is as follows: 10000 parts of polyethylene and copolymer thereof, 50-500 parts of polyisobutylene, and the weight ratio of tackifying resin, white carbon black, coupling agent and surfactant is 20-70: 30-80: 3-10: 1-5, 50-200 parts of a mixture, 5-30 parts of an antioxidant and 10-100 parts of a stabilizer;
wherein,
3000-8000 parts of polyethylene and 7000-2000 parts of polyethylene copolymer;
the tackifying resin is one or more of 2402 tackifying resin, 202 tackifying resin, C9 petroleum resin, WL brominated resin and SP-1055 brominated resin;
the white carbon black is precipitated white carbon black;
the coupling agent is one or more of KH540, KH550, KH570, SI-69 and SI-75;
the surfactant is a cationic surfactant or a nonionic surfactant;
the antioxidant is one or more of 1010 antioxidant and 1076 antioxidant;
the stabilizer is one or more of magnesium oxide, calcium oxide and lead oxide.
2. The hot melt adhesive film for an automotive interior ceiling as claimed in claim 1, wherein the formulation further comprises 1 to 5 parts of a microcellular foaming agent, and the microcellular foaming agent is one or more of OBSH, EMA80AH, WQFP-2, NBFP-1 and KX-565.
3. The method for producing a hot melt adhesive film for an automotive interior ceiling as claimed in claim 1,
firstly, mixing tackifying resin, white carbon black, a coupling agent and a surfactant according to the weight ratio of 20-70: 30-80: 3-10: 1-5, and then spray drying to prepare the bonding modified filler;
then preparing the following ingredients in parts by weight: 50-500 parts of bonding modified filler, 3000-10000 parts of polyethylene, 50-500 parts of polyisobutylene, 5-30 parts of antioxidant and 10-100 parts of stabilizer, and the components are melted, blended, extruded and granulated in a double-screw extruder;
the particles are put into hot melt adhesive film production equipment to prepare the hot melt adhesive film.
CN202010203856.4A 2020-03-21 2020-03-21 Hot melt adhesive film for automotive interior ceiling and production method thereof Pending CN111171750A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114350280A (en) * 2022-01-18 2022-04-15 鑫序高分子材料(苏州)有限公司 High-temperature-resistant hot-melt adhesive film and preparation method thereof
CN114369426A (en) * 2022-01-04 2022-04-19 江苏斯尔邦石化有限公司 Hot melt adhesive film composition and preparation method and application thereof

Citations (3)

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Publication number Priority date Publication date Assignee Title
JP2000297265A (en) * 1999-04-15 2000-10-24 Taoka Chem Co Ltd Hot-melt adhesive composition
CN103254803A (en) * 2013-05-21 2013-08-21 上海海优威电子技术有限公司 Micro-foaming polyolefin solar photovoltaic module film
CN108034368A (en) * 2017-12-15 2018-05-15 中国科学院长春应用化学研究所 A kind of VOC free automobile using hot melt adhesive film and preparation method thereof

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CN103254803A (en) * 2013-05-21 2013-08-21 上海海优威电子技术有限公司 Micro-foaming polyolefin solar photovoltaic module film
CN108034368A (en) * 2017-12-15 2018-05-15 中国科学院长春应用化学研究所 A kind of VOC free automobile using hot melt adhesive film and preparation method thereof

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114369426A (en) * 2022-01-04 2022-04-19 江苏斯尔邦石化有限公司 Hot melt adhesive film composition and preparation method and application thereof
CN114369426B (en) * 2022-01-04 2023-05-12 江苏斯尔邦石化有限公司 Hot melt adhesive film composition and preparation method and application thereof
CN114350280A (en) * 2022-01-18 2022-04-15 鑫序高分子材料(苏州)有限公司 High-temperature-resistant hot-melt adhesive film and preparation method thereof

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