CN115216243A - Environment-friendly high-viscosity hot melt adhesive film and preparation method thereof - Google Patents
Environment-friendly high-viscosity hot melt adhesive film and preparation method thereof Download PDFInfo
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- CN115216243A CN115216243A CN202210827488.XA CN202210827488A CN115216243A CN 115216243 A CN115216243 A CN 115216243A CN 202210827488 A CN202210827488 A CN 202210827488A CN 115216243 A CN115216243 A CN 115216243A
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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
- C09J7/00—Adhesives in the form of films or foils
- C09J7/30—Adhesives in the form of films or foils characterised by the adhesive composition
- C09J7/35—Heat-activated
-
- 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
- C09J151/00—Adhesives based on graft polymers in which the grafted component is obtained by reactions only involving carbon-to-carbon unsaturated bonds; Adhesives based on derivatives of such polymers
- C09J151/06—Adhesives based on graft polymers in which the grafted component is obtained by reactions only involving carbon-to-carbon unsaturated bonds; Adhesives based on derivatives of such polymers grafted on to homopolymers or copolymers of aliphatic hydrocarbons containing only one carbon-to-carbon double bond
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
-
- 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
- C09J2301/00—Additional features of adhesives in the form of films or foils
- C09J2301/40—Additional features of adhesives in the form of films or foils characterized by the presence of essential components
- C09J2301/408—Additional 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
Abstract
The invention discloses an environment-friendly high-viscosity hot melt adhesive film and a preparation method thereof, wherein the preparation method comprises the following steps: (1) Adding the low-density polyethylene grafted acrylic acid-2-hydroxyethyl ester copolymer, the amino acid modified maleic anhydride grafted polyethylene, butyl rubber, microcrystalline wax and sodium stearate into a mixer, and uniformly stirring to obtain a rubber material; (2) Putting the uniformly mixed rubber material obtained in the step (1) into a charging hopper of a double-screw extruder, sequentially passing through six heating zones of the double-screw extruder, and fully plasticizing by the screw extruder to obtain a molten composition; (3) And (3) extruding the molten composition obtained in the step (2) through a die head to obtain a molten film, and cooling and shaping the molten film through a casting roller and a cooling roller to form the hot melt adhesive film. The hot melt adhesive film prepared by the invention does not contain solvent, has little pollution and good adhesion.
Description
Technical Field
The invention relates to the technical field of hot melt adhesive films, in particular to an environment-friendly high-viscosity hot melt adhesive film and a preparation method thereof.
Background
The hot melt adhesive, also called hot melt adhesive material, is a meltable adhesive, needs no other solvent in the bonding process, is solid at normal temperature, is heated and melted into a liquid adhesive material, and can complete bonding within a few seconds after being pressed and cooled after an adherend is coated and wetted.
The hot melt adhesive film belongs to one kind of hot melt adhesive, and as one new kind of adhesive, it has high adhering force, no pollution, convenient operation and easy storage, so that it is used widely. Hot-melt adhesive films are generally prepared from saturated polyolefin materials, such as Polyethylene (PE), ethylene-vinyl acetate (EVA), polyolefin elastomers (POE), etc. The preparation method is that the polyolefin material and the auxiliary agent are melted and blended in a double screw extruder, extruded and granulated, and finally the film is formed in a film-making device. In order to increase the adhesive properties of the hot melt adhesive film, an auxiliary agent is usually added to facilitate adhesion. However, most of the bonding aids contain polar functional groups, such as ester functional groups, acid functional groups, ether functional groups, residual acidic substances and the like, and may release a large amount of toxic and harmful gases at high temperature, which is not environment-friendly.
Disclosure of Invention
The invention aims to provide an environment-friendly high-viscosity hot melt adhesive film and a preparation method thereof aiming at the defects in the prior art.
In order to achieve the purpose, the technical scheme provided by the invention is as follows:
an environment-friendly high-viscosity hot melt adhesive film comprises the following components:
40-60 parts of low-density polyethylene grafted acrylic acid-2-hydroxyethyl ester copolymer,
30-50 parts of amino acid modified maleic anhydride grafted polyethylene,
1-5 parts by weight of butyl rubber,
5-10 parts by weight of microcrystalline wax,
0.1 to 1.5 weight portions of sodium stearate.
Further, the low density polyethylene grafted 2-hydroxyethyl acrylate copolymer is prepared by the following method: under the nitrogen atmosphere, adding metered hydroxyethyl acrylate, AIBN and xylene into a reactor, stirring for dissolving, adding low-density polyethylene, accelerating stirring to uniformly mix reactants, swelling for 40min at 50 ℃ on a rotary evaporator, heating to 80 ℃ for continuing to react for 2.5h, extracting a product in a Soxhlet extractor for 12h by using acetone, extracting for 48h by using distilled water, and finally performing vacuum drying at 60 ℃ to obtain the low-density polyethylene grafted acrylic acid-2-hydroxyethyl copolymer.
Further, the mass ratio of the hydroxyethyl acrylate, the AIBN, the xylene, and the low density polyethylene is 4:0.3:8:100.
further, the amino acid-modified maleic anhydride-grafted polyethylene is prepared by the following method: adding the amino acid and the maleic anhydride grafted polyethylene into a stirrer in proportion, fully stirring at the rotating speed of 250r/min for 10min, and then transferring into a double-screw extruder for granulation.
Further, the mass ratio of the amino acid to the maleic anhydride-grafted polyethylene is 2.
Further, the temperatures from the feed inlet to the head of the double-screw extruder are respectively as follows: 160 ℃, 170 ℃, 180 ℃, 190 ℃,200 ℃ and the screw rotation speed of 250r/min.
The preparation method of the environment-friendly high-viscosity hot melt adhesive film comprises the following steps:
(1) Adding low-density polyethylene grafted acrylic acid-2-hydroxyethyl ester copolymer, amino acid modified maleic anhydride grafted polyethylene, butyl rubber, microcrystalline wax and sodium stearate into a mixer, stirring at 200 ℃ and a rotation speed of 120r/min for 30min to obtain a rubber material;
(2) Putting the uniformly mixed rubber material obtained in the step (1) into a charging hopper of a double-screw extruder, sequentially passing through six heating zones of the double-screw extruder, and fully plasticizing by the screw extruder to obtain a molten composition;
(3) And (3) extruding the molten composition obtained in the step (2) through a die head to obtain a molten film, and cooling and shaping through a casting roller and a cooling roller to form the hot melt adhesive film.
Further, in the six heating zones in the step (2), the temperature of the first heating zone is 160 ℃, the temperature of the second heating zone is 180 ℃, the temperature of the third heating zone is 180 ℃, the temperature of the fourth heating zone is 190 ℃, and the temperature of the fifth heating zone is 210 ℃; the temperature of the sixth heating zone is 220 ℃; the rotating speed of the screw is 150r/min;
further, the temperature of the die head in the step (3) is controlled to be 220 ℃, the temperature of the casting roll is controlled to be 120-150 ℃, and the temperature of the cooling roll is controlled to be 40-60 ℃.
Compared with the prior art, the invention has the beneficial effects that:
1. the hot melt adhesive film disclosed by the invention does not contain a solvent, is low in pollution and has good adhesion.
2. Polyethylene (PE) is one of important general-purpose plastics, but PE is a nonpolar polymer, and has poor compatibility with inorganic substances and polar polymers and poor adhesion. The low-density polyethylene grafted acrylic acid-2-hydroxyethyl ester copolymer of the invention has the advantages that the grafted polymer hardly changes the framework structure of PE, simultaneously polar monomers with various functions are grafted to a PE main chain, the grafted polymer contains three functional groups of double bonds, vinegar groups and lifting groups, the polymerization activity is higher, the original characteristics of PE are maintained, and the compatibility of PE is improved.
3. Amino acid modified maleic anhydride grafted polyethylene obtained by reacting an amino acid with maleic anhydride grafted polyethylene, the modified polyolefin having physical properties similar to linear low density polyolefin resins of the same density and melt index, the use of such binder resins in a co-extruded structure providing a higher thermal stability than ethylene-vinyl acetate based binder resins.
4. The modified polyolefin and the low-density polyethylene grafted acrylic acid-2-hydroxyethyl ester copolymer have good compatibility, and can be better crosslinked during bonding and compounding under the blending of other components, so that the bonding strength is improved, and the product has better bonding performance.
Detailed Description
The technical solutions in the embodiments of the present invention will be described clearly and completely in conjunction with the detailed description of the invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be obtained by a person skilled in the art without making any creative effort based on the embodiments in the present invention, belong to the protection scope of the present invention.
Example 1
(1) Preparing a low-density polyethylene grafted acrylic acid-2-hydroxyethyl ester copolymer: adding 4 parts by weight of hydroxyethyl acrylate, 0.3 part by weight of AIBN and 8.5 parts by weight of xylene into a reactor in a nitrogen atmosphere, stirring for dissolving, adding 100 parts by weight of low-density polyethylene, stirring at an accelerated speed to uniformly mix reactants, swelling for 40min at 50 ℃ on a rotary evaporator, heating to 80 ℃, continuing to react for 2.5h, extracting the product in a Soxhlet extractor for 12h by using acetone, extracting with distilled water for 48h, and finally drying in vacuum at 60 ℃ to obtain the low-density polyethylene grafted acrylic acid-2-hydroxyethyl ester copolymer.
Preparing amino acid modified maleic anhydride grafted polyethylene: adding 2 parts by weight of amino acid and 100 parts by weight of maleic anhydride grafted polyethylene into a stirrer in proportion, fully stirring at the rotating speed of 250r/min for 10min, and then transferring into a double-screw extruder for granulation, wherein the temperatures from a feed inlet of the double-screw extruder to a machine head are respectively as follows: 160 ℃, 170 ℃, 180 ℃, 190 ℃,200 ℃ and the screw rotating speed of 250r/min
(2) Adding 50 parts by weight of low-density polyethylene grafted acrylic acid-2-hydroxyethyl copolymer, 40 parts by weight of amino acid modified maleic anhydride grafted polyethylene, 3 parts by weight of butyl rubber, 8 parts by weight of microcrystalline wax and 1 part by weight of sodium stearate into a mixer, stirring for 30min at 200 ℃ and a rotating speed of 120r/min to obtain a rubber material;
(3) Putting the rubber material into a charging hopper of a double-screw extruder, and sequentially passing through six heating zones of the double-screw extruder, wherein the temperature of a first heating zone is 160 ℃, the temperature of a second heating zone is 180 ℃, the temperature of a third heating zone is 180 ℃, the temperature of a fourth heating zone is 190 ℃, and the temperature of a fifth heating zone is 210 ℃; the temperature of the sixth heating zone is 220 ℃; the rotating speed of the screw is 150r/min, and the mixture is fully plasticized by a screw extruder to obtain a molten composition;
(4) And (4) extruding the molten composition obtained in the step (3) through a die head to obtain a molten film, and cooling and shaping through a casting roller and a cooling roller, wherein the temperature of the die head is 220 ℃, the temperature of the casting roller is 130 ℃, and the temperature of the cooling roller is 50 ℃ to form the hot melt adhesive film.
Example 2
The difference from example 1 is that:
60 parts by weight of low-density polyethylene grafted acrylic acid-2-hydroxyethyl ester copolymer,
50 parts by weight of amino acid modified maleic anhydride grafted polyethylene,
the weight portion of the butyl rubber is 5 portions,
the microcrystalline wax is 10 parts by weight of,
sodium stearate was 1.5 parts by weight.
Wherein the die head temperature is 220 ℃, the casting roll temperature is 120 ℃, and the cooling roll temperature is 40 ℃.
Example 3
The difference from example 1 is that:
40 parts by weight of a low-density polyethylene grafted acrylic acid-2-hydroxyethyl ester copolymer,
30 parts of amino acid modified maleic anhydride grafted polyethylene,
1 part by weight of butyl rubber is added,
the microcrystalline wax is 5 parts by weight of the wax,
sodium stearate is 0.1 part by weight.
Wherein the die temperature is 220 ℃, the casting roll temperature is 150 ℃, and the cooling roll temperature is 60 ℃.
Comparative example 1
Adding 50 parts by weight of modified polyethylene, 40 parts by weight of maleic anhydride grafted polyethylene, 3 parts by weight of butyl rubber, 8 parts by weight of microcrystalline wax and 1 part by weight of sodium stearate into a mixer, stirring at 200 ℃ and a rotating speed of 120r/min for 30min to obtain a rubber material; putting the rubber material into a hopper of a double-screw extruder, and sequentially passing through six heating zones of the double-screw extruder, wherein the temperature of a first heating zone is 160 ℃, the temperature of a second heating zone is 180 ℃, the temperature of a third heating zone is 180 ℃, the temperature of a fourth heating zone is 190 ℃, and the temperature of a fifth heating zone is 210 ℃; the temperature of the sixth heating zone is 220 ℃; the rotating speed of the screw is 150r/min, and the mixture is fully plasticized by a screw extruder to obtain a molten composition; and extruding the molten composition through a die head to obtain a molten film, and cooling and shaping the molten film through a casting roller and a cooling roller, wherein the temperature of the die head is 220 ℃, the temperature of the casting roller is 130 ℃, and the temperature of the cooling roller is 50 ℃ to form the hot melt adhesive film.
Performance testing
The hot melt adhesives prepared in examples 1-3 and comparative example 1 were placed on a pressure forming machine to prepare samples having a thickness of about 120um, a length of 100mm and a width of 25mm, the samples were placed between two pieces of TPO having a length of 200mm and a width of 30mm, and then were pressed and ironed in a constant temperature oven at 200 ℃, cooled and left to stand for 24 hours for use. T-peel strength measurements were made in a tensile tester at a speed of 100mm/min, with the execution standard GB/T2791-1995. The test results are shown in table 1.
TABLE 1
Those skilled in the art to which the present invention pertains can also make appropriate changes and modifications to the above-described embodiments, based on the disclosure of the above description. Therefore, the present invention is not limited to the specific embodiments disclosed and described above, and modifications and variations of the present invention are also intended to fall within the scope of the appended claims.
Claims (9)
1. An environment-friendly high-viscosity hot melt adhesive film is characterized in that: comprises the following components:
40-60 parts of low-density polyethylene grafted acrylic acid-2-hydroxyethyl ester copolymer,
30-50 parts of amino acid modified maleic anhydride grafted polyethylene,
1-5 parts by weight of butyl rubber,
5-10 parts by weight of microcrystalline wax,
0.1-1.5 parts of sodium stearate.
2. The environment-friendly high-viscosity hot-melt adhesive film according to claim 1, wherein: the low-density polyethylene grafted acrylic acid-2-hydroxyethyl ester copolymer is prepared by the following method: under the nitrogen atmosphere, adding metered hydroxyethyl acrylate, AIBN and xylene into a reactor, stirring for dissolving, adding low-density polyethylene, accelerating stirring to uniformly mix reactants, swelling for 40min at 50 ℃ on a rotary evaporator, heating to 80 ℃ for continuing to react for 2.5h, extracting a product in a Soxhlet extractor for 12h by using acetone, extracting for 48h by using distilled water, and finally performing vacuum drying at 60 ℃ to obtain the low-density polyethylene grafted acrylic acid-2-hydroxyethyl copolymer.
3. The environment-friendly high-viscosity hot-melt adhesive film according to claim 2, wherein: the mass ratio of the hydroxyethyl acrylate, the AIBN, the xylene and the low-density polyethylene is 4:0.3:8:100.
4. the environment-friendly high-viscosity hot-melt adhesive film according to claim 1, wherein: the amino acid modified maleic anhydride grafted polyethylene is prepared by the following method: adding the amino acid and the maleic anhydride grafted polyethylene into a stirrer according to a proportion, fully stirring at a rotating speed of 250r/min for 10min, and then transferring into a double-screw extruder for granulation.
5. The environment-friendly high-viscosity hot-melt adhesive film according to claim 4, wherein: the mass ratio of the amino acid to the maleic anhydride grafted polyethylene is 2.
6. The environment-friendly high-viscosity hot melt adhesive film as claimed in claim 4, wherein: the temperature from the feed inlet of the double-screw extruder to the machine head is respectively as follows: 160 ℃, 170 ℃, 180 ℃, 190 ℃,200 ℃ and the screw rotation speed of 250r/min.
7. The method for preparing the environment-friendly high-viscosity hot melt adhesive film according to any one of claims 1 to 6, wherein the method comprises the following steps: the method comprises the following steps:
(1) Adding low-density polyethylene grafted acrylic acid-2-hydroxyethyl ester copolymer, amino acid modified maleic anhydride grafted polyethylene, butyl rubber, microcrystalline wax and sodium stearate into a mixer, stirring at 200 ℃ and a rotation speed of 120r/min for 30min to obtain a rubber material;
(2) Putting the rubber material uniformly mixed in the step (1) into a charging hopper of a double-screw extruder, sequentially passing through six heating zones of the double-screw extruder, and fully plasticizing by the screw extruder to obtain a molten composition;
(3) And (3) extruding the molten composition obtained in the step (2) through a die head to obtain a molten film, and cooling and shaping the molten film through a casting roller and a cooling roller to form the hot melt adhesive film.
8. The method for preparing the environment-friendly high-viscosity hot melt adhesive film according to claim 7, wherein the method comprises the following steps: in the six heating zones in the step (2), the temperature of the first heating zone is 160 ℃, the temperature of the second heating zone is 180 ℃, the temperature of the third heating zone is 180 ℃, the temperature of the fourth heating zone is 190 ℃, and the temperature of the fifth heating zone is 210 ℃; the temperature of the sixth heating zone is 220 ℃; the rotation speed of the screw is 150r/min.
9. The environment-friendly high-viscosity hot melt adhesive film as claimed in claim 7, wherein: in the step (3), the temperature of the die head is controlled to be 220 ℃, the temperature of the casting roller is controlled to be 120-150 ℃, and the temperature of the cooling roller is controlled to be 40-60 ℃.
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Citations (6)
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| CN1338496A (en) * | 2001-04-30 | 2002-03-06 | 中国兵器工业第五三研究所 | Components, preparing process and usage of hot-fusible adhesive |
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2022
- 2022-07-14 CN CN202210827488.XA patent/CN115216243A/en active Pending
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| CN1338496A (en) * | 2001-04-30 | 2002-03-06 | 中国兵器工业第五三研究所 | Components, preparing process and usage of hot-fusible adhesive |
| JP2006089626A (en) * | 2004-09-24 | 2006-04-06 | Nof Corp | Hot-melt adhesive composition |
| JP2006183000A (en) * | 2004-12-28 | 2006-07-13 | Sanyo Chem Ind Ltd | Reactive hot-melt adhesive |
| CN108456497A (en) * | 2018-02-26 | 2018-08-28 | 合肥远科服装设计有限公司 | A kind of dress lining cloth hot melt adhesive and preparation method thereof |
| CN109439240A (en) * | 2018-11-17 | 2019-03-08 | 金丽丹 | A kind of preparation method of heat resistant type PP hot melt adhesive |
| CN111676594A (en) * | 2020-05-25 | 2020-09-18 | 界首市天鸿新材料股份有限公司 | Antibacterial and high-temperature-resistant polypropylene melt-blown nonwoven material |
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