CN110330901B - EVA hot melt adhesive with high bonding strength - Google Patents
EVA hot melt adhesive with high bonding strength Download PDFInfo
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- CN110330901B CN110330901B CN201910634147.9A CN201910634147A CN110330901B CN 110330901 B CN110330901 B CN 110330901B CN 201910634147 A CN201910634147 A CN 201910634147A CN 110330901 B CN110330901 B CN 110330901B
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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
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/04—Non-macromolecular additives inorganic
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- 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
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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
- C09J4/00—Adhesives based on organic non-macromolecular compounds having at least one polymerisable carbon-to-carbon unsaturated bond ; adhesives, based on monomers of macromolecular compounds of groups C09J183/00 - C09J183/16
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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
- C09J4/00—Adhesives based on organic non-macromolecular compounds having at least one polymerisable carbon-to-carbon unsaturated bond ; adhesives, based on monomers of macromolecular compounds of groups C09J183/00 - C09J183/16
- C09J4/06—Organic non-macromolecular compounds having at least one polymerisable carbon-to-carbon unsaturated bond in combination with a macromolecular compound other than an unsaturated polymer of groups C09J159/00 - C09J187/00
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- Inorganic Chemistry (AREA)
- Adhesives Or Adhesive Processes (AREA)
Abstract
The invention discloses an EVA hot melt adhesive with high bonding strength, which comprises the following raw materials in parts by weight: 100 parts of EVA resin, 8-19 parts of SBS thermoplastic elastomer, 4-11 parts of hydroxyl-terminated polyurethane resin, 0.2-1.3 parts of polyacrylamide, 0.15-0.8 part of 2-vinyl-1-benzofuran and hydrogenated C511-15 parts of petroleum resin, 5-13 parts of polyethylene wax, 1-3 parts of paraffin, 0.12-0.34 part of antioxidant, 0.01-0.1 part of benzoyl peroxide, 0.01-0.07 part of acrylic europium and 13-28 parts of filler. The EVA hot melt adhesive with high bonding strength provided by the invention has the advantages of high bonding strength, good high temperature resistance and excellent aging resistance.
Description
Technical Field
The invention relates to the technical field of adhesives, and particularly relates to an EVA hot melt adhesive with high bonding strength.
Background
The hot melt adhesive is an adhesive which takes thermoplastic resin as a base material, is added with a small amount of plasticizer, tackifier, filler, antioxidant and the like, is bonded by utilizing temperature change, has a plurality of excellent properties such as hundreds of solids, short curing time, simple and convenient operation, suitability for continuous industrial production and the like, and is widely applied to the fields of home decoration, wireless binding, plastic bonding and the like at present.
Hot melt adhesives can be classified into ethylene-vinyl acetate esters, styrene block elastomers, polyolefins, polyamides, polyesters, and the like, depending on the host resin. Ethylene-vinyl acetate (EVA) hot melt adhesives have the characteristics of excellent weather resistance, no toxicity, no pollution, simple and convenient preparation method and the like, are more hot melt adhesives used at present, but have the defects of low bonding strength and poor heat resistance, and seriously limit the application range of the hot melt adhesives.
Disclosure of Invention
The invention provides an EVA hot melt adhesive with high bonding strength, which aims to solve the technical problems in the background art.
The invention provides an EVA hot melt adhesive with high bonding strength, which comprises the following raw materials in parts by weight: 100 parts of EVA resin, 8-19 parts of SBS thermoplastic elastomer, 4-11 parts of hydroxyl-terminated polyurethane resin, 0.2-1.3 parts of polyacrylamide and 2-vinyl-1-benzofuran0.15-0.8 parts of pyran, hydrogenated C511-15 parts of petroleum resin, 5-13 parts of polyethylene wax, 1-3 parts of paraffin, 0.12-0.34 part of antioxidant, 0.01-0.1 part of benzoyl peroxide, 0.01-0.07 part of acrylic europium and 13-28 parts of filler.
Preferably, the mass content of VA in the EVA resin is 28-40 wt%.
Preferably, the SBS thermoplastic elastomer is SBS thermoplastic elastomer YH-792.
Preferably, the antioxidant is one or a mixture of more of antioxidant 1010, antioxidant 168, antioxidant 264 and antioxidant DLTP.
Preferably, the filler is a mixture of nano titanium dioxide and modified nano calcium carbonate; the modified nano calcium carbonate is prepared according to the following process: modifying the nano calcium carbonate by taking a silane coupling agent KH-570 as a modifier to obtain coupling agent modified nano calcium carbonate; adding coupling agent modified nano calcium carbonate into DMF, heating to 70-80 ℃, adding methacrylic acid-2-hydroxyethyl and azobisisobutyronitrile, stirring and reacting for 3-5h under the protection of nitrogen, then carrying out ultrasonic treatment for 50-100min, adding 3-isopropyl-dimethylbenzyl isocyanate (TMI), carrying out ultrasonic reaction for 30-50min, washing, and drying to obtain the modified nano calcium carbonate.
Preferably, the weight ratio of the modified nano calcium carbonate to the nano titanium dioxide is 5-12: 2-4.
Preferably, the weight ratio of the coupling agent modified nano calcium carbonate, 2-hydroxyethyl methacrylate, azobisisobutyronitrile and 3-isopropyl-dimethylbenzyl isocyanate TMI is 2-3: 2.5-4: 0.7-1: 4-6.5.
Preferably, the nano calcium carbonate is a mixture of chain-like nano calcium carbonate and needle-like nano calcium carbonate, and the weight ratio of the chain-like nano calcium carbonate to the needle-like nano calcium carbonate is 3-9: 1-2.
In the preparation process of the modified nano calcium carbonate, firstly, silane coupling agent KH-570 is taken as a modifying agent to modify the nano calcium carbonate, the coupling agent is introduced to the surface of the nano calcium carbonate to obtain the coupling agent modified nano calcium carbonate, then, the coupling agent modified nano calcium carbonate and 2-hydroxyethyl methacrylate are taken as raw materials, azobisisobutyronitrile is taken as an initiator to react the raw materials and the hydroxyl, 3-isopropyl-dimethylbenzyl isocyanate TMI is added to react the introduced hydroxyl with isocyanate, so that the silane coupling agent KH-570, the 2-hydroxyethyl methacrylate and the 3-isopropyl-dimethylbenzyl isocyanate TMI are introduced to the surface of the nano calcium carbonate to modify the surface of the nano calcium carbonate to obtain the modified nano calcium carbonate, the double bonds introduced into the surface of the nano calcium carbonate can react with raw materials in the system, and simultaneously, the chain structure introduced into the surface of the nano calcium carbonate can be wound with EVA, so that the acting force of the nano calcium carbonate and the EVA is improved, the contact area of the nano calcium carbonate and the EVA is increased, the mechanical property of the hot melt adhesive is further enhanced, the degradation of EVA macromolecules is delayed, and the high temperature resistance of the hot melt adhesive is improved; in the preferred mode, chain-shaped nano calcium carbonate and needle-shaped nano calcium carbonate in a specific proportion are specifically selected as nano calcium carbonate, and the nano calcium carbonate and the needle-shaped nano calcium carbonate are added into a system to play a synergistic effect, so that the bonding and stripping-resistant characteristics of the obtained hot melt adhesive are obviously improved, and the obtained hot melt adhesive is endowed with excellent bonding performance.
In the invention, the specific process of modifying the nano calcium carbonate by taking the silane coupling agent KH-570 as the modifying agent to obtain the coupling agent modified nano calcium carbonate can be as follows: adding nano calcium carbonate and a silane coupling agent KH-570 into a mixed solution of ethanol and water, wherein the weight ratio of the nano calcium carbonate to the silane coupling agent KH-570 is 10: 1.3-2, ultrasonic treatment for 20-30min, ultrasonic power of 200-300W, stirring at 65-75 ℃ for 2-5h, centrifuging at normal temperature at the rotating speed of 6000-8000r/min, and vacuum drying at 70-80 ℃ for 3-5h to obtain the coupling agent modified nano calcium carbonate.
The EVA hot melt adhesive with high bonding strength can be prepared according to the following process: uniformly mixing EVA resin, 2-vinyl-1-benzofuran, benzoyl peroxide, europium acrylate, a filler and an antioxidant, adding the mixture into a mixing roll, mixing for 5-12min at 90-100 ℃, adding the rest raw materials, adjusting the temperature to 85-95 ℃ under the condition of stirring, and mixing for 45-55min to obtain a material A; adding the material A into a double-screw extruder for extrusion, and cooling and granulating the extruded product to obtain the EVA hot melt adhesive with high bonding strength; in the preparation process, the antioxidant is preferentially added for mixing, so that the phenomenon of uneven mixing of the antioxidant is avoided, and the obtained hot melt adhesive has good ageing resistance.
Preferably, the rate of agitation is 20-35 rpm.
The EVA hot melt adhesive with high bonding strength is prepared from the raw materials, wherein EVA resin is used as a main material, and an SBS thermoplastic elastomer and hydroxyl-terminated polyurethane resin are added in a matching manner, and the proportion of the three is controlled, so that the three exert a synergistic effect, the cohesive strength of the hot melt adhesive is increased, the bonding strength of the obtained hot melt adhesive is improved, the high temperature resistance of the hot melt adhesive is improved, a small amount of polyacrylamide is added, the polyacrylamide can form a hydrogen bond with water, and meanwhile, N-H groups are contained in molecules, so that acidic substances can be absorbed, a small amount of free acetic acid contained in the EVA and acidic small molecular substances generated in an aging process can be effectively eliminated or neutralized, and the hot melt adhesive is endowed with excellent water vapor barrier capability and aging resistance; 2-vinyl-1-benzofuran and europium acrylate are added into a system and can react with EVA under the action of an initiator benzoyl peroxide, the 2-vinyl-1-benzofuran and the europium acrylate are introduced into EVA resin, the content of vinyl acetate in the EVA resin is adjusted, the polarity of the system is adjusted, the bonding property of the hot melt adhesive is obviously improved, and meanwhile, europium element is introduced to endow the hot melt adhesive with better high temperature resistance and aging resistance; compared with the prior art, the hot melt adhesive disclosed by the invention has excellent bonding strength, good high temperature resistance and excellent aging resistance.
Detailed Description
The technical solution of the present invention will be described in detail below with reference to specific examples.
Example 1
An EVA hot melt adhesive with high bonding strength comprises the following raw materials in parts by weight: 100 parts of EVA resin, 19 parts of SBS thermoplastic elastomer and terminal hydroxyl4 parts of base polyurethane resin, 0.9 part of polyacrylamide, 0.15 part of 2-vinyl-1-benzofuran and hydrogenated C515 parts of petroleum resin, 5 parts of polyethylene wax, 1.7 parts of paraffin, 0.15 part of antioxidant, 0.01 part of benzoyl peroxide, 0.07 part of acrylic europium and 28 parts of filler.
Example 2
An EVA hot melt adhesive with high bonding strength comprises the following raw materials in parts by weight: 100 parts of EVA resin, YH-7928 parts of SBS thermoplastic elastomer, 7 parts of hydroxyl-terminated polyurethane resin, 1.3 parts of polyacrylamide, 0.4 part of 2-vinyl-1-benzofuran and hydrogenated C511 parts of petroleum resin, 9 parts of polyethylene wax, 3 parts of paraffin, 10100.34 parts of antioxidant, 0.1 part of benzoyl peroxide, 0.01 part of acrylic europium and 21 parts of filler;
wherein the mass content of VA in the EVA resin is 40 wt%;
the filler is a mixture of nano titanium dioxide and modified nano calcium carbonate, and the weight ratio of the modified nano calcium carbonate to the nano titanium dioxide is 5: 4; the modified nano calcium carbonate is prepared according to the following process: modifying the nano calcium carbonate by taking a silane coupling agent KH-570 as a modifier to obtain coupling agent modified nano calcium carbonate; adding coupling agent modified nano calcium carbonate into DMF, heating to 70 ℃, adding 2-hydroxyethyl methacrylate and azobisisobutyronitrile, stirring and reacting for 5 hours under the protection of nitrogen, then performing ultrasonic treatment for 50 minutes, adding 3-isopropyl-dimethylbenzyl isocyanate (TMI), performing ultrasonic reaction for 50 minutes, washing, and drying to obtain the modified nano calcium carbonate; wherein the coupling agent modified nano calcium carbonate, 2-hydroxyethyl methacrylate, azobisisobutyronitrile and 3-isopropyl-dimethylbenzyl isocyanate TMI are in a weight ratio of 2: 4: 0.7: 6.5; the nano calcium carbonate is a mixture of chain-like nano calcium carbonate and needle-like nano calcium carbonate, and the weight ratio of the chain-like nano calcium carbonate to the needle-like nano calcium carbonate is 9: 1.
example 3
An EVA hot melt adhesive with high bonding strength comprises the following raw materials in parts by weight: 100 parts of EVA resin, YH-79212 parts of SBS thermoplastic elastomer, 11 parts of hydroxyl-terminated polyurethane resin, 0.2 part of polyacrylamide, 0.8 part of 2-vinyl-1-benzofuran,Hydrogenation of C511.5 parts of petroleum resin, 13 parts of polyethylene wax, 1 part of paraffin, 1680.2 parts of antioxidant, 0.14 part of antioxidant DLTP, 0.07 part of benzoyl peroxide, 0.02 part of europium acrylate and 13 parts of filler;
wherein the mass content of VA in the EVA resin is 28 wt%;
the filler is a mixture of nano titanium dioxide and modified nano calcium carbonate, and the weight ratio of the modified nano calcium carbonate to the nano titanium dioxide is 12: 2; the modified nano calcium carbonate is prepared according to the following process: modifying the nano calcium carbonate by taking a silane coupling agent KH-570 as a modifier to obtain coupling agent modified nano calcium carbonate; adding coupling agent modified nano calcium carbonate into DMF, heating to 80 ℃, adding 2-hydroxyethyl methacrylate and azobisisobutyronitrile, stirring and reacting for 3 hours under the protection of nitrogen, then performing ultrasonic treatment for 100 minutes, adding 3-isopropyl-dimethylbenzyl isocyanate (TMI), performing ultrasonic reaction for 30 minutes, washing, and drying to obtain the modified nano calcium carbonate; wherein the coupling agent modified nano calcium carbonate, 2-hydroxyethyl methacrylate, azobisisobutyronitrile and 3-isopropyl-dimethylbenzyl isocyanate TMI are in a weight ratio of 3: 2.5: 1: 4; the nano calcium carbonate is a mixture of chain-like nano calcium carbonate and needle-like nano calcium carbonate, and the weight ratio of the chain-like nano calcium carbonate to the needle-like nano calcium carbonate is 3: 2.
example 4
An EVA hot melt adhesive with high bonding strength comprises the following raw materials in parts by weight: 100 parts of EVA resin, 12 parts of SBS thermoplastic elastomer, 8.7 parts of hydroxyl-terminated polyurethane resin, 1 part of polyacrylamide, 0.65 part of 2-vinyl-1-benzofuran and hydrogenated C512 parts of petroleum resin, 10 parts of polyethylene wax, 2.1 parts of paraffin, 10100.1 parts of antioxidant, 1680.05 parts of antioxidant, 2640.05 parts of antioxidant, 0.05 part of antioxidant DLTP, 0.06 part of benzoyl peroxide, 0.04 part of europium acrylate and 21 parts of filler;
wherein the mass content of VA in the EVA resin is 32 wt%;
the SBS thermoplastic elastomer is an SBS thermoplastic elastomer YH-792;
the filler is a mixture of nano titanium dioxide and modified nano calcium carbonate, and the weight ratio of the modified nano calcium carbonate to the nano titanium dioxide is 7: 2; the modified nano calcium carbonate is prepared according to the following process: modifying the nano calcium carbonate by taking a silane coupling agent KH-570 as a modifier to obtain coupling agent modified nano calcium carbonate; adding coupling agent modified nano calcium carbonate into DMF, heating to 78 ℃, adding 2-hydroxyethyl methacrylate and azobisisobutyronitrile, stirring and reacting for 3.8h under the protection of nitrogen, then performing ultrasonic treatment for 85min, adding 3-isopropyl-dimethylbenzyl isocyanate (TMI), performing ultrasonic reaction for 40min, washing, and drying to obtain the modified nano calcium carbonate; wherein the weight ratio of the coupling agent modified nano calcium carbonate, 2-hydroxyethyl methacrylate, azobisisobutyronitrile and 3-isopropyl-dimethylbenzyl isocyanate TMI is 2.7: 3: 0.8: 5; the nano calcium carbonate is a mixture of chain-like nano calcium carbonate and needle-like nano calcium carbonate, and the weight ratio of the chain-like nano calcium carbonate to the needle-like nano calcium carbonate is 5: 1.4.
comparative example 1
The only difference from example 4 is that: the raw materials do not contain polyacrylamide.
Comparative example 2
The only difference from example 4 is that: the raw materials do not contain 2-vinyl-1-benzofuran and acrylic acid europium.
Comparative example 3
The only difference from example 4 is that: the modified nano calcium carbonate is prepared according to the following process: the silane coupling agent KH-570 is used as a modifier to modify the nano calcium carbonate to obtain the coupling agent modified nano calcium carbonate, namely the modified nano calcium carbonate.
Respectively pressing the hot melt adhesives in the embodiment 4 and the comparative examples 1-3 into films with the thickness of 1mm in a hot press at 160 ℃, cutting the films into 25 x 150mm, placing the cut films between two aluminum sheets (25 x 200mm), carrying out hot pressing on the hot press at 160 ℃ for 2min, wherein the pressure is 4MPa, folding 50mm parts, which are not glued, of the two aluminum sheets into right angles after cooling, forming a T shape with the 150mm part of the glue, and placing for 24h under test conditions to obtain test films; the peel strength was determined according to GB/T2791-1995 standard; performing the ring and ball softening point measurement according to GB/T15332-1994 standard;
determination of adhesive Strength: the adhesive strength of the hot melt adhesives of example 4 and comparative examples 1 to 3 was determined using a universal tester according to astm d 1002. The substrate dimensions were 150mm by 30mm by 2mm at room temperature, and the paste length was about 3 cm.
The results are shown in the following table:
the hot melt adhesives of example 4 and comparative example 4 exhibited substantially unchanged adhesive properties after 30 days of aging at 80 c, whereas the hot melt adhesives of comparative example 2 and comparative example 3 exhibited a decrease in adhesive properties after 30 days of aging at 70 c.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the technical scope of the present invention, and the technical solutions and the inventive concepts thereof according to the present invention should be equivalent or changed within the scope of the present invention.
Claims (7)
1. The EVA hot melt adhesive with high bonding strength is characterized by comprising the following raw materials in parts by weight: 100 parts of EVA resin, 8-19 parts of SBS thermoplastic elastomer, 4-11 parts of hydroxyl-terminated polyurethane resin, 0.2-1.3 parts of polyacrylamide, 0.15-0.8 part of 2-vinyl-1-benzofuran and hydrogenated C511-15 parts of petroleum resin, 5-13 parts of polyethylene wax, 1-3 parts of paraffin, 0.12-0.34 part of antioxidant, 0.01-0.1 part of benzoyl peroxide, 0.01-0.07 part of acrylic europium and 13-28 parts of filler;
the filler is a mixture of nano titanium dioxide and modified nano calcium carbonate; the modified nano calcium carbonate is prepared according to the following process: modifying the nano calcium carbonate by taking a silane coupling agent KH-570 as a modifier to obtain coupling agent modified nano calcium carbonate; adding coupling agent modified nano calcium carbonate into DMF, heating to 70-80 ℃, adding methacrylic acid-2-hydroxyethyl and azobisisobutyronitrile, stirring and reacting for 3-5h under the protection of nitrogen, then carrying out ultrasonic treatment for 50-100min, adding 3-isopropyl-dimethylbenzyl isocyanate (TMI), carrying out ultrasonic reaction for 30-50min, washing, and drying to obtain the modified nano calcium carbonate.
2. The EVA hot melt adhesive with high bonding strength of claim 1, wherein the mass content of VA in the EVA resin is 28-40 wt%.
3. The EVA hot melt adhesive with high adhesive strength of claim 1 or 2, wherein the SBS thermoplastic elastomer is SBS thermoplastic elastomer YH-792.
4. The EVA hot melt adhesive with high bonding strength of claim 1 or 2, wherein the antioxidant is one or a mixture of antioxidant 1010, antioxidant 168, antioxidant 264 and antioxidant DLTP.
5. The EVA hot melt adhesive with high bonding strength of claim 1, wherein the weight ratio of the modified nano calcium carbonate to the nano titanium dioxide is 5-12: 2-4.
6. The EVA hot melt adhesive with high bonding strength of claim 1, wherein the weight ratio of the coupling agent modified nano calcium carbonate, 2-hydroxyethyl methacrylate, azobisisobutyronitrile and 3-isopropyl-dimethylbenzyl isocyanate TMI is 2-3: 2.5-4: 0.7-1: 4-6.5.
7. The EVA hot melt adhesive with high bonding strength of claim 1, wherein the nano calcium carbonate is a mixture of chain-like nano calcium carbonate and needle-like nano calcium carbonate, and the weight ratio of the chain-like nano calcium carbonate to the needle-like nano calcium carbonate is 3-9: 1-2.
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| CN113403003A (en) * | 2021-06-23 | 2021-09-17 | 泉州中宝鞋材有限公司 | Formula and preparation method of high-hardness hot-melt adhesive sheet |
| CN113913131A (en) * | 2021-11-05 | 2022-01-11 | 龚郁蓉 | Modified EVA hot melt adhesive and preparation method thereof |
| CN114262582A (en) * | 2022-01-21 | 2022-04-01 | 广东汇齐新材料有限公司 | High-temperature-resistant EVA hot-melt adhesive film and preparation process thereof |
| CN115044348B (en) * | 2022-07-13 | 2023-05-16 | 广州市嘉雁粘合剂有限公司 | EMS (energy management system) label hot melt adhesive with strong stripping force and easy cutting and preparation method thereof |
| CN115044302B (en) * | 2022-07-18 | 2023-03-10 | 惠州艺都文化用品有限公司 | Modified EVA hot melt adhesive and precious metal commemorative coin are with hot tectorial membrane |
| CN117659914A (en) * | 2023-12-08 | 2024-03-08 | 东莞市欣美电子材料有限公司 | Pressure-sensitive adhesive applied to power battery and manufacturing method thereof |
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