CN105419684B - A kind of bonding of rubber to metal hot melt adhesive film and preparation method thereof - Google Patents
A kind of bonding of rubber to metal hot melt adhesive film and preparation method thereof Download PDFInfo
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- CN105419684B CN105419684B CN201510924923.0A CN201510924923A CN105419684B CN 105419684 B CN105419684 B CN 105419684B CN 201510924923 A CN201510924923 A CN 201510924923A CN 105419684 B CN105419684 B CN 105419684B
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- melt adhesive
- rubber
- adhesive film
- hot melt
- bonding
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J123/00—Adhesives based on homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Adhesives based on derivatives of such polymers
- C09J123/02—Adhesives 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
- C09J123/04—Homopolymers or copolymers of ethene
- C09J123/08—Copolymers of ethene
- C09J123/0846—Copolymers of ethene with unsaturated hydrocarbons containing other atoms than carbon or hydrogen atoms
- C09J123/0853—Vinylacetate
-
- 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
- C09J123/00—Adhesives based on homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Adhesives based on derivatives of such polymers
- C09J123/02—Adhesives 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
- C09J123/04—Homopolymers or copolymers of ethene
- C09J123/08—Copolymers of ethene
- C09J123/0807—Copolymers of ethene with unsaturated hydrocarbons only containing more than three carbon atoms
- C09J123/0815—Copolymers of ethene with aliphatic 1-olefins
-
- 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
-
- 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
- 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
-
- 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
- C09J2423/00—Presence of polyolefin
- C09J2423/04—Presence of homo or copolymers of ethene
- C09J2423/048—Presence of homo or copolymers of ethene in the pretreated surface to be joined
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Adhesive Tapes (AREA)
- Adhesives Or Adhesive Processes (AREA)
Abstract
The present invention relates to a kind of bonding of rubber to metal hot melt adhesive film, for adhesive rubber and metal, solvent-free release in production process, and preparation technology is simple can replace the pretreatment of metal surface technique of conventional liquid adhesive or complexity.The production process of this product includes following two steps：1) using EVA or POE resin as matrix, the polybutadiene that Grafting of Maleic Anhydride Onto Melt is modified, and granulating and drying, obtain hot-melt adhesive granules；2) hot-melt adhesive granules are well mixed with sulfur-donor, and prepare suitable depth hot melt adhesive film.The product of the present invention has excellent bonding force, while sulfur-donor discharges sulphur by the butadiene segment of addition and rubber co-vulcanization in high temperature, so as to also keep excellent bonding force with rubber by grafted maleic anhydride with metal.
Description
Technical field
The invention belongs to PUR technical field, and in particular to a kind of bonding of rubber to metal hot melt adhesive film.
Background technology
Metal to rubber, which is bonded in many industrial circles, demand, is carried out in such as mechanical engineering, building, ship, war industry
Belt armored vehicle bogie wheel, creeper tread land the bondings of glue and track bushings.Differed greatly due to rubber and metal-polar, it is necessary to
One layer of bonding agent could be preferably bonded.Conventional method has vulcanie method, brass or brass plating method, resorcinol formaldehyde body
System, phenolic resin method, polyisocyanic acid ester process, halogenated rubber method and containing extraordinary vulcanizing agent halogen polymer method and water accack method
Deng.These big Alternatives of traditional method are complex, it is necessary to which the pretreatment procedure such as polish, liquid adhesive often also has solvent
The problem of toxicity of volatilizing.
Hot melt adhesive film technique is simple, nontoxic, but is not a kind of new theory, only because adhesive technology reason, always
Used in some traditional fields, the bonding of certain material is difficult to break through all the time, such as rubber is bonding with metal.In view of rubber with
Metal adhesive at present the problems of, we are necessary to develop a kind of hot melt adhesive film of bonding of rubber to metal, make rubber-metal
There is good adhesive property.
The content of the invention
It is an object of the invention to provide a kind of hot melt adhesive film that rubber and metal can be made to have good bonding performance, and the heat
Melten gel film is nontoxic, odorlessness, and processing technology is simple, can substitute traditional bonding of rubber to metal technique.
The present invention to EVA or POE resin by being modified, and being made a kind of makes rubber and metal have good bonding performance
Hot melt adhesive film.
Bonding of rubber to metal hot melt adhesive film prepared by the present invention, it is characterised in that by the following raw material system by weight
It is standby to form：
100 parts of hot-melt adhesive granules
0.5-5 parts of sulfur-donor；
Wherein, hot-melt adhesive granules are prepared from by the following raw material by weight：
100 parts of EVA resin or POE resin
0.01-0.2 parts of peroxide initiator
0.5-10 parts of maleic anhydride modified polybutadiene.
Preferably, the fusing point of the EVA resin or POE resin is in the range of 50~105 DEG C, and melt index is 1~40g/
10min。
Preferably, described peroxide initiator is cumyl peroxide, the double (peroxidating of 2,5- dimethyl -2,5-
The tert-butyl group) hexane, benzoyl peroxide, mixture one or more kinds of in tert-butyl hydroperoxide carbonic acid -2- ethylhexyls.
Preferably, the cumyl peroxide is used as best results during peroxide initiator.
Preferably, described maleic anhydride modified polybutadiene number-average molecular weight is in the range of 2500-9900, maleic acid
Acid anhydride content is in the range of 3~20%.
Preferably, described sulfur-donor is following one or more kinds of mixtures：4,4`- dimorpholinyl disulfides
(DTDM), tetramethylthiuram disulfide (TMTD), tetramethylthiuram tetrasulfide (TMTT), 2- (4- morpholines base two is thio)
Benzothiazole (MDB).
Preferably, 4, the 4`- dimorpholinyl disulfides (DTDM), tetramethylthiuram disulfide (TMTD) mixing are used as sulphur
Best results during carrier.
The preparation method of the bonding of rubber to metal hot melt adhesive film of the present invention, it is characterised in that：Prepared by following two steps
Form：
1) EVA or POE resin using formula ratio is matrixes, and the peroxide initiator and maleic anhydride for adding formula ratio change
The polybutadiene of property, with double screw extruder fusion-grafting and granulates at 190 DEG C, obtains hot-melt adhesive granules；
2) sulfur-donor of formula ratio is added in the hot-melt adhesive granules of formula ratio, is well mixed, is prepared with the tape casting
Thickness is 0.3mm hot melt adhesive film.
The advantageous effects of the present invention are as follows：
1st, the preparation technology of hot melt adhesive film is simple, is bonded metal and rubber firm, solves metal rubber in the prior art
The problem of glue is difficult to be bonded.
2nd, smell or release Toxic will not be produced by preparing in material environmental protection used in hot melt adhesive film, process
Matter, and solvent-free volatilization, are conducive to the technological innovation of material.
3rd, hot melt adhesive film of the invention laminating is uniform, and bubble-free is produced in sulfidation, rubber and metal is had very well
Adhesive strength.
Embodiment
With reference to specific embodiment, the invention will be further described：
Embodiment 1
Step one, the EVA resin of 100 mass parts is taken, the wherein fusing point of EVA resin is 50 DEG C, and melt index is 40g/
10min, adds double (tert-butyl peroxide) hexanes of 2,5- dimethyl -2,5- and 5 mass fraction average molecular weights of 0.01 mass parts
The maleic anhydride modified polybutadiene for being 3% for 4500, maleic anhydride content, at 190 DEG C with twin-screw extrusion grafting simultaneously
Granulation drying；Step 2, weighs 100 mass parts steps one and granulates son, the DTDM of 0.5 mass parts of addition is well mixed, used
The tape casting, prepares the film that thickness is 0.3mm.Specific test result is shown in Table 1.
Embodiment 2
Step one, the POE resin of 100 mass parts is taken, the wherein fusing point of POE resin is 60 DEG C, and melt index is 15g/
10min, double (tert-butyl peroxide) hexanes of 2,5- dimethyl -2,5- of 0.2 mass parts of addition and 5 mass fraction average molecular weights are
7500th, maleic anhydride content is 20% maleic anhydride modified polybutadiene, is grafted and is made with twin-screw extrusion at 190 DEG C
Grain drying；Step 2, weighs 100 mass parts steps one and granulates son, the TMTD of 5 mass parts of addition is well mixed, using curtain coating
Method, prepares the film that thickness is 0.3mm.Specific test result is shown in Table 1.
Embodiment 3
Step one, the EVA resin of 100 mass parts is taken, the wherein fusing point of EVA resin is 105 DEG C, and melt index is 2g/
10min, the cumyl peroxide and 0.5 mass fraction average molecular weight for adding 0.05 mass parts is 9900, maleic anhydride content
For 6% maleic anhydride modified polybutadiene, it is grafted and granulation drying with twin-screw extrusion at 190 DEG C；Step 2, is weighed
100 mass parts steps one granulate son, and the DTDM of 0.5 mass parts of addition is well mixed, and using the tape casting, preparing thickness is
0.3mm film.Specific test result is shown in Table 1.
Embodiment 4
Step one, the EVA resin of 100 mass parts is taken, the wherein fusing point of EVA resin is 72 DEG C, and melt index is 20g/
10min, the cumyl peroxide and 5 mass fraction average molecular weights for adding 0.1 mass parts are that 5000, maleic anhydride content is
10% maleic anhydride modified polybutadiene, with twin-screw extrusion grafting and granulation drying at 190 DEG C；Step 2, is weighed
100 mass parts steps one granulate son, and the TMTD of 1 mass parts of addition is well mixed, using the tape casting, prepare thickness for 0.3mm
Film.Specific test result is shown in Table 1.
Embodiment 5
Step one, the EVA resin of 100 mass parts is taken, the wherein fusing point of EVA resin is 81 DEG C, and melt index is 3g/
10min, adds double (tert-butyl peroxide) hexanes of 2,5- dimethyl -2,5- and the peroxidating of 0.05 mass parts of 0.05 mass parts
Diisopropylbenzene (DIPB), 10 mass fraction average molecular weights are the maleic anhydride modified polybutadiene that 2500, maleic anhydride content is 17%,
With twin-screw extrusion grafting and granulation drying at 190 DEG C；Step 2, weighs 100 mass parts steps one and granulates son, addition
The TMTD of the 0.5 mass parts and DTDM of 0.5 mass parts is well mixed, and using the tape casting, prepares the film that thickness is 0.3mm.Tool
Body examination test result is shown in Table 1.
Embodiment 6
Step one, the POE resin of 100 mass parts is taken, the wherein fusing point of POE resin is 104 DEG C, and melt index is 1g/
10min, adds double (tert-butyl peroxide) hexanes of 2,5- dimethyl -2,5- and the peroxidating of 0.05 mass parts of 0.05 mass parts
Diisopropylbenzene (DIPB), 10 mass fraction average molecular weights are the maleic anhydride modified polybutadiene that 3100, maleic anhydride content is 8%,
With twin-screw extrusion grafting and granulation drying at 190 DEG C；Step 2, weighs 100 mass parts steps one and granulates son, addition
The TMTD of the 0.5 mass parts and DTDM of 0.5 mass parts is well mixed, and using the tape casting, prepares the film that thickness is 0.3mm.Tool
Body examination test result is shown in Table 1.
The hot melt adhesive film of the present invention is made using the tape casting, after 60-80 DEG C of vacuum press laminating precompressed, in high-pressure mercury
1-10min is radiated under lamp and completes solidification crosslinking, is concretely comprised the following steps：By ethylene-octene copolymer with other function additives by pre-
Mixing, melting extrusion, casting film-forming, finally wind finished product.Wherein, the UV solidification polyolefin optical film thicknesses of casting machine can
Root Ju is actually needed regulation, the use of more thickness is at present 0.2mm, the thickness of hot melt adhesive film of the present invention is 0.3mm.
Performance test scheme：
1. bonding force is tested
Method for making sample：By EPDM (ethylene propylene diene rubber)/hot melt adhesive film/aluminium sheet structure sample preparation, wherein EPDM sizes are width
2cm, thickness 2mm are spent, length is 10cm, and aluminium sheet size is width 2cm, and thickness 2mm, length is 5cm, in 160 degree of compression moldings
Machine pressurization 10min, pressure is 2MPa.
Method of testing：180 degree peels off rubber and aluminium sheet bonding force, and peeling rate is 100mm/min.
The hot melt adhesive film the performance test results of table 1
From the point of view of test result, peel strength size and selected substrate resin species, maleic anhydride modified polybutadiene
Molecular weight, maleic anhydride content, addition and carry sulphur body species and addition have larger contact, embodiment 1-6 is equal
There is preferable bonding force with EPDM rubber and metal aluminum sheet, wherein most preferably embodiment 3 and embodiment 6, peel strength is more than 100N/
cm。
In summary, product involved in the present invention has preferable bonding force with rubber and metal, and solvent-free
Volatilization, operating procedure is simple, and traditional rubber and metal adhesive method can be substituted in some fields.
The foregoing is only a specific embodiment of the invention, but protection scope of the present invention is not limited thereto, any
Those skilled in the art disclosed herein technical scope in, the change that can expect without creative work or
Replace, should all be included within the scope of the present invention.Therefore, protection scope of the present invention should be limited with claims
Fixed protection domain is defined.
Claims (7)
1. a kind of bonding of rubber to metal hot melt adhesive film, it is characterised in that be prepared from by the following raw material by weight：
100 parts of hot-melt adhesive granules
0.5-5 parts of sulfur-donor；
Wherein, hot-melt adhesive granules are prepared from by the following raw material by weight：
100 parts of EVA resin or POE resin
0.01-0.2 parts of peroxide initiator
0.5-10 parts of maleic anhydride modified polybutadiene；
Described sulfur-donor is following one or more kinds of mixtures：4,4`- dimorpholinyl disulfides, tetramethyl autumn
Lan Mu, tetramethylthiuram tetrasulfide, 2- (4- morpholines base two is thio) benzothiazole.
2. the bonding of rubber to metal hot melt adhesive film described in a Ju right 1, it is characterised in that：The EVA resin or POE resin it is molten
O'clock in the range of 50~105 DEG C, melt index is 1~40g/10min.
3. the bonding of rubber to metal hot melt adhesive film described in a Ju right 1, it is characterised in that：Described peroxide initiator was
Aoxidize diisopropylbenzene (DIPB), 2,5- dimethyl -2,5- double (tert-butyl peroxide) hexane, benzoyl peroxide, tert-butyl hydroperoxide carbon
One or more kinds of mixture in acid -2- ethylhexyls.
4. the bonding of rubber to metal hot melt adhesive film described in a Ju right 3, it is characterised in that：The cumyl peroxide is used as mistake
Best results during peroxide initiator.
5. the bonding of rubber to metal hot melt adhesive film described in a Ju right 1, it is characterised in that：Described maleic anhydride modified poly- fourth
Diene number-average molecular weight is in the range of 2500-9900, and maleic anhydride content is in the range of 3~20%.
6. the bonding of rubber to metal hot melt adhesive film described in a Ju right 1, it is characterised in that：The 4,4`- dimorpholinyl disulfides
(DTDM), tetramethylthiuram disulfide (TMTD) mixing is used as best results during sulfur-donor.
7. the preparation method of the bonding of rubber to metal hot melt adhesive film described in a Ju right 1-6 any one, it is characterised in that：Under
Two steps are stated to be prepared from：
1) EVA or POE resin using formula ratio is matrix, adds the peroxide initiator of formula ratio and maleic anhydride modified
Polybutadiene, with double screw extruder fusion-grafting and granulates at 190 DEG C, obtains hot-melt adhesive granules；
2) sulfur-donor of formula ratio is added in the hot-melt adhesive granules of formula ratio, is well mixed, thickness is prepared with the tape casting
For 0.3mm hot melt adhesive film.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201510924923.0A CN105419684B (en) | 2015-12-11 | 2015-12-11 | A kind of bonding of rubber to metal hot melt adhesive film and preparation method thereof |
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| CN201510924923.0A CN105419684B (en) | 2015-12-11 | 2015-12-11 | A kind of bonding of rubber to metal hot melt adhesive film and preparation method thereof |
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| CN105419684A CN105419684A (en) | 2016-03-23 |
| CN105419684B true CN105419684B (en) | 2017-08-11 |
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| CN108219692A (en) * | 2017-12-29 | 2018-06-29 | 江苏鹿山光电科技有限公司 | A kind of crosslinked EVA heat conduction packaging adhesive film and preparation method thereof |
| CN109066503A (en) * | 2018-07-02 | 2018-12-21 | 安徽坤和电气有限公司 | A kind of corrosion resistant high-strength plastic steel cable bridge |
| CN115287003A (en) * | 2022-08-04 | 2022-11-04 | 广东汇齐新材料有限公司 | Composite hot melt adhesive film for metal bonding and preparation method thereof |
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| CN104449462B (en) * | 2013-09-13 | 2019-03-15 | 湖北回天新材料股份有限公司 | A kind of automobile folding adhesive that wet-hot aging performance is excellent |
| 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 |
| CN103756581B (en) * | 2014-01-16 | 2015-06-10 | 南京红宝丽新材料有限公司 | PID (Potential Induced Degradation) resisting solar cell module packaging coating and preparation method thereof |
| CN104262543A (en) * | 2014-09-09 | 2015-01-07 | 沈阳化工大学 | Method for preparing maleic anhydride-grafted 1,2-polybutadiene |
| CN105111950B (en) * | 2015-09-28 | 2018-03-02 | 广州鹿山新材料股份有限公司 | A kind of EVA adhesive film and preparation method thereof |
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