CN103756602A - Acrylate pressure-sensitive adhesive for protective film and preparation method thereof - Google Patents
Acrylate pressure-sensitive adhesive for protective film and preparation method thereof Download PDFInfo
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Abstract
The invention discloses an acrylate pressure-sensitive adhesive for a protective film and a preparation method thereof. The acrylate pressure-sensitive adhesive is formed mainly by mixing the following raw materials in parts by weight: 100 parts of polymer A, 5-50 parts of polymer B and 0.2-2 parts of compound C, wherein the polymer A is a polymer containing a crosslinkable functional group, and the glass transition temperature is minus 10-minus 65 DEG C; the polymer B is a polymer without crosslinkable functional group and formed by copolymerization or homopolymerization of monomers with glass transition temperature lower than zero, or formed by copolymerization of a hard monomer and a soft monomer; and the compound C is an amino-containing compound, a polyvalent metal compound or an isocyanate group-containing compound. In the invention, the acrylate pressure-sensitive adhesive with the performance of rubber type pressure-sensitive adhesive is synthesized by use of ethyl acetate, and has good initial adhesion, stripping resistance and permanent adhesion; and moreover, the energy consumption is low since plasticization is not required in the processing process, an arene solvent is not required for dissolution, thus the harm to human is reduced while the fire is avoided, and the acrylate pressure-sensitive adhesive is not aged easily under heating and illumination.
Description
Technical Field
The invention relates to a pressure-sensitive adhesive, in particular to an acrylate pressure-sensitive adhesive for a protective film and a preparation method thereof.
Background
The pressure-sensitive adhesive is an adhesive closely related to daily life of people, and is one of the most widely applied adhesives with the largest output at present. The pressure-sensitive adhesive is distinguished from the main chemical components of the pressure-sensitive adhesive, and can be divided into rubber pressure-sensitive adhesive, thermoplastic elastic pressure-sensitive adhesive, polyacrylate pressure-sensitive adhesive, polyvinyl ether pressure-sensitive adhesive, organic silicon pressure-sensitive adhesive and the like. At present, rubber-type pressure-sensitive adhesives are prepared from natural rubber or synthetic rubber in combination with appropriate tackifying resins, softeners and the like. The rubber is a main component, which endows the pressure-sensitive adhesive with enough cohesive strength, good tensile strength and elongation; the tackifying resin enables the pressure-sensitive adhesive to have certain adhesiveness, and the softening agent is used for reducing the bulk viscosity of the pressure-sensitive adhesive and improving the initial adhesion at low temperature. The process is to plasticate and dissolve natural rubber, and then to add tackifying resin and plasticizer. The process has the following difficulties: 1. in the plastication process, the plasticizing degree of the natural rubber is difficult to control, and the energy consumption is high; 2. aromatic hydrocarbon solvents such as toluene are used for dissolving the rubber. As is well known, aromatic hydrocarbon solvents are harmful to human bodies, stimulate central nerves of brains and narcotize coma, and although some processes adopt a method of reducing the using amount of aromatic hydrocarbon to reduce the harm to the human bodies, new danger is brought because solvent gasoline is used, and fire disasters are easy to happen; 3. because unsaturated bonds exist on the molecular chain of the natural rubber, the natural rubber is easy to age under heating and illumination, so that the natural rubber cannot be used. Disclosure of Invention
In order to overcome the defects of the prior art, the invention aims to provide the acrylate pressure-sensitive adhesive for the protective film, which is synthesized by using ethyl acetate, has the performance similar to that of a rubber type pressure-sensitive adhesive, namely has good initial adhesion, stripping force and permanent adhesion, does not need to be plasticized in the processing process, has low energy consumption, does not need aromatic hydrocarbon solvents to be dissolved, reduces the harm to people and avoids the danger of fire, and is not easy to age under heat and light.
The invention also aims to provide a preparation method of the acrylate pressure-sensitive adhesive for the protective film.
The technical scheme adopted by the invention for realizing the aim is as follows:
the acrylate pressure-sensitive adhesive for the protective film is characterized by being mainly prepared from the following raw materials in parts by weight:
100 parts of a polymer A;
5-50 parts of a polymer B;
0.2-2 parts of a compound C;
wherein,
the polymer A is a polymer containing crosslinkable functional groups, and the glass transition temperature of the polymer A is between-10 ℃ and-65 ℃;
the polymer B is a polymer without crosslinkable functional groups, and is formed by copolymerization or homopolymerization of monomers with the glass transition temperature lower than zero, or copolymerization of hard monomers and soft monomers;
the compound C is an amino group-containing compound, a polyvalent metal compound or an isocyanate group-containing compound.
The high or low glass transition temperature is an important index reflecting the softness and brittleness of the polymer. The higher homopolymer glass transition temperature of the monomer is called a hard monomer, which increases the hardness and tensile strength of the copolymer resin. As the hard monomer, there are usually used methyl acrylate (8 ℃ C.), vinyl acetate (22 ℃ C.), styrene (80 ℃ C.), acrylonitrile (97 ℃ C.), methyl methacrylate (105 ℃ C.), acrylamide (165 ℃ C.), etc. Monomers having a glass transition temperature of-20 ℃ to-70 ℃ are generally called soft monomers, and commonly used soft monomers include ethyl acrylate (-22 ℃), butyl acrylate (-55 ℃), isooctyl acrylate (-70 ℃) and the like.
As a preferred embodiment of the present invention, the polymer A comprises the following raw materials, by weight, 0-30 parts of ethylenically unsaturated acid, 80-95 parts of acrylate, and 0.5-10 parts of monomer containing crosslinkable functional group; the polymer B comprises the following raw materials, by weight, 60-100 parts of acrylate and 0-20 parts of methacrylate monomer;
as a preferable scheme of the invention, the polymer A is prepared from the following raw materials in parts by weight: 80-95 parts of acrylate monomer, 5-20 parts of methacrylate monomer or acrylic acid; 0.5-10 parts of acrylate monomers; 0.2-1 part of initiator; 100 portions of ethyl acetate and 150 portions of polymer B, wherein the polymer B is prepared from the following raw materials in parts by weight: 60-100 parts of acrylate monomer; 1-15 parts of a methacrylate monomer; 0.2-1 part of initiator; 100 portions of ethyl acetate and 150 portions of ethyl acetate.
In a preferred embodiment of the present invention, the acrylate monomer is one or more of methyl acrylate, ethyl acrylate, butyl acrylate, and isooctyl acrylate.
In a preferred embodiment of the present invention, the methacrylate monomer is one or more of methyl methacrylate, ethyl methacrylate, and butyl methacrylate.
In a preferred embodiment of the present invention, the hydroxy acrylate monomer is acrylamide and its derivatives, and the acrylamide derivative is preferably one or more selected from hydroxyethyl acrylate, hydroxypropyl acrylate, hydroxybutyl acrylate and hydroxymethyl acrylamide.
As a preferred embodiment of the present invention, the initiator is azobisisobutyronitrile;
as a preferable scheme of the invention, the acrylate pressure-sensitive adhesive for the protective film further comprises tackifying resin and plasticizer, wherein the dosage of the tackifying resin is 1-30 parts by weight, and the dosage of the plasticizer is 1-10 parts by weight;
in a preferred embodiment of the present invention, the tackifier resin is one of rosin, C5, C9 petroleum resin, and terpene. Among them, rosin is the best, followed by C5 petroleum resin, and terpene has the worst performance.
In a preferred embodiment of the present invention, the plasticizer is dibutyl phthalate, dioctyl phthalate, mineral oil, or the like.
As a preferable embodiment of the present invention, an amine group-containing compound such as polyamine, polyamine coupling agent, etc.; examples are as follows: 3, 3-dichloro-4, 4-diphenylmethanediamine (MOCA), propyleneglycolbis- (4, 4' -diamino) benzoate, polyoxypropylenediamine, triethylenetetramine, etc.
The polyvalent metal compound is butyl titanate, a condensate thereof, or the like, and is exemplified by: butyl titanate, a condensate of butyl titanate and acetylacetone, calcium acetate, aluminum acetylacetonate, and the like.
The isocyanate-containing substance is a substance containing two or more isocyanate groups as a terminal, and is exemplified by the following: polyoxypropylene diisocyanate, 1, 6-hexamethylene diisocyanate, isophorone diisocyanate, and the like.
The invention also aims to provide a preparation method of the acrylate pressure-sensitive adhesive for the protective film, which comprises the following specific steps:
the method is characterized by comprising the following steps:
1) synthesis of Polymer A: adding ethyl acetate into a reaction kettle, starting stirring, adding 20 parts of mixed monomer consisting of acrylate monomer and methacrylate monomer or acrylic acid and acrylic hydroxy ester monomer, and simultaneously adding 0.1 part of initiator; heating to 78 deg.C, maintaining for 0.5-1 hr, and adding the rest monomer containing 0.2-0.4 weight parts of initiator for 3-3.5 hr; after the addition, the temperature is kept for 60 minutes, and the initiator is replenished every three ten minutes; keeping the temperature for 1.5 hours after the initiator is added, cooling and discharging;
2) synthesis of Polymer B: adding ethyl acetate into a reaction kettle, starting stirring, adding 20 parts of mixed monomer consisting of acrylate monomer and methacrylate monomer, and simultaneously adding 0.1 part of initiator; heating to 78 deg.C, maintaining for 0.5-1 hr, and adding the rest monomer containing 0.2-0.4 weight parts of initiator for 3-3.5 hr; after the addition, the temperature is kept for 60 minutes, and the initiator is replenished every three ten minutes; keeping the temperature for 1.5 hours after the initiator is added, cooling and discharging;
3) and (2) mixing the polymer A prepared in the step 1) and the polymer B and the compound C prepared in the step 2) according to the proportion of the first object of the invention, and uniformly mixing to obtain the acrylate pressure-sensitive adhesive for the protective film.
In a preferred embodiment of the present invention, in step 3, the acrylate pressure-sensitive adhesive for a protective film further comprises a tackifying resin and a plasticizer, wherein the amount of the tackifying resin is 1 to 30 parts by weight, and the amount of the plasticizer is 1 to 10 parts by weight.
The invention has the beneficial effects that:
1. the invention uses non-crosslinkable polymer, so the plasticizer is used a little, thus reducing the exudation of small molecules; the two polymers are blended together, one polymer is crosslinked into a network structure, the other polymer still exists in a thermoplastic state in a cured species and does not participate in crosslinking polymerization, so that a novel semi-interpenetrating network polymer is formed, the cured substance has toughness and rigidity, and the formed pressure-sensitive adhesive is ensured to have good initial adhesion, stripping force and permanent adhesion, and the three keep good balance. Meanwhile, plasticization is not needed in the processing process, the energy consumption is low, an aromatic solvent is not needed for dissolution, the harm to people is reduced, the fire danger is avoided, and the aging is not easy to occur under the heating and illumination.
2. The acrylate pressure-sensitive adhesive for the protective film can be coated on various base materials including PP, PE, OPP, PET, PVDC, PA, paper and aluminum foil, and can be used as the protective film for the protection of processing, transportation and storage.
Detailed Description
The present invention will be described in further detail with reference to specific embodiments.
A preparation method of acrylate pressure-sensitive adhesive for a protective film comprises the steps of taking a polymer A, a polymer B, a compound C and optionally tackifying resin and/or plasticizer as raw materials, mixing according to a formula proportion, and uniformly mixing to obtain the acrylate pressure-sensitive adhesive for the protective film.
Wherein,
firstly, the preparation of the polymer A comprises the following embodiments 1-5:
example 1:
the polymer A is prepared from the following raw materials in parts by weight: 70 parts of acrylate monomer, 12 parts of methacrylate monomer and 3 parts of acrylate monomer; 0.3 part of an initiator; and 100 parts of ethyl acetate. The acrylate monomer is methyl acrylate, the methacrylate monomer is methyl methacrylate, the acrylate monomer is hydroxyethyl acrylate, and the initiator is azobisisobutyronitrile.
Synthesis of Polymer A: adding ethyl acetate into a reaction kettle, starting stirring, adding 20 parts of mixed monomer consisting of the monomers, and simultaneously adding 0.1 part of initiator; heating to 78 deg.C, keeping the temperature for 0.5 h, adding the rest monomer containing 0.2 weight parts of initiator dropwise, and feeding for 3 h; after the addition, the temperature is kept for 60 minutes, and the initiator is replenished every three ten minutes; keeping the temperature for 1.5 hours after the initiator is added, cooling and discharging;
example 2:
the polymer A is prepared from the following raw materials in parts by weight: 65 parts of acrylate monomer and 5 parts of methacrylate monomer; 3 parts of acrylic acid and 15 parts of acrylic hydroxy ester monomer; 0.8 part of an initiator; and 100 parts of ethyl acetate.
Synthesis of Polymer A: adding ethyl acetate into a reaction kettle, starting stirring, adding 20 parts of mixed monomer consisting of the monomers, and simultaneously adding 0.1 part of initiator; heating to 78 deg.C, keeping the temperature for 1 hour, dripping the rest monomer containing 0.3 weight part of initiator, and feeding for 3.5 hours; after the addition, the temperature is kept for 60 minutes, and the initiator is replenished every three ten minutes; keeping the temperature for 1.5 hours after the initiator is added, cooling and discharging.
Example 3:
the polymer A is prepared from the following raw materials in parts by weight: 80 parts of acrylate monomer and 12 parts of methacrylate monomer; 5 parts of acrylic acid and 15 parts of acrylic hydroxy ester monomer; 0.3 part of an initiator; and 100 parts of ethyl acetate.
The synthesis of polymer a was the same as in example 1.
Example 4:
the polymer A is prepared from the following raw materials in parts by weight: 90 parts of acrylate monomer, 3 parts of acrylic acid and 15 parts of acrylic hydroxy ester monomer; 0.3 part of an initiator; and 100 parts of ethyl acetate.
The synthesis of polymer a was the same as in example 1.
Example 5:
the polymer A is prepared from the following raw materials in parts by weight: 82 parts of acrylate monomer and 10 parts of hydroxyl acrylate monomer; 0.3 part of an initiator; and 100 parts of ethyl acetate.
The synthesis of polymer a was the same as in example 1.
Secondly, the preparation of the polymer B comprises examples 6 to 7, which are specifically as follows:
example 6:
the polymer B is prepared from the following raw materials in parts by weight: 89 parts of acrylate monomer and 12 parts of methacrylate monomer; 0.3 part of an initiator; and 100 parts of ethyl acetate. The acrylate monomer is methyl acrylate, and the methacrylate monomer is methyl methacrylate;
synthesis of Polymer B: adding ethyl acetate into a reaction kettle, starting stirring, adding 20 parts of mixed monomer consisting of the monomers, and simultaneously adding 0.1 part of initiator; heating to 78 deg.C, keeping the temperature for 0.5 h, adding the rest monomer containing 0.1 weight part of initiator dropwise, and feeding for 3 h; after the addition, the temperature is kept for 60 minutes, and the initiator is replenished every three ten minutes; keeping the temperature for 1.5 hours after the initiator is added, cooling and discharging;
example 7:
the polymer B is prepared from the following raw materials in parts by weight: 100 parts of acrylate monomer; 0.5 part of an initiator; and 100 parts of ethyl acetate.
The synthesis of polymer B was the same as in example 6.
And thirdly, the compound C is polyoxypropylene diisocyanate, the tackifying resin is rosin, and the plasticizer is dibutyl phthalate.
Fourthly, detecting a product formula table and strength:
the composite base materials are polyester film, polyethylene film, polypropylene film and aluminizer which are processed by corona;
the test method comprises the following steps: uniformly coating on plastic film (such as polyester film) with 12 mm wire bar, blowing water with electric blower, compounding with another polyethylene film to obtain PET/PE composite film, curing in 60 deg.C oven for 24 hr, taking out, sampling and measuring according to GB/T8808.
The initial adhesion, the peeling force and the permanent adhesion are simultaneously detected, and the specific product formula and the detection result are shown in tables 1 to 5
TABLE 1
TABLE 2
TABLE 3
TABLE 4
TABLE 5
Remarking: in tables 1-5, Δ, the film was attached to the mirror plate, cooled to room temperature for 24 hours at 80 ℃ and torn off, and no fog was observed if the glue was removed; the check mark has no fog and does not drop glue; 1m means that the film is placed for one month at normal temperature after being pasted.
As can be seen from tables 1 to 5, the invention has good initial adhesion, peeling force and permanent adhesion, and has the performance similar to rubber type pressure sensitive adhesive.
The above embodiments are only preferred embodiments of the present invention, and the protection scope of the present invention is not limited thereby, and any insubstantial changes and substitutions made by those skilled in the art based on the present invention are within the protection scope of the present invention.
Claims (10)
1. The acrylate pressure-sensitive adhesive for the protective film is characterized by being mainly prepared from the following raw materials in parts by weight:
100 parts of a polymer A;
5-50 parts of a polymer B;
0.2-2 parts of a compound C;
wherein,
the polymer A is a polymer containing crosslinkable functional groups, and the glass transition temperature of the polymer A is between-10 ℃ and-65 ℃;
the polymer B is a polymer without crosslinkable functional groups, and is formed by copolymerization or homopolymerization of monomers with the glass transition temperature lower than zero, or copolymerization of hard monomers and soft monomers;
the compound C is an amino group-containing compound, a polyvalent metal compound or an isocyanate group-containing compound.
2. The acrylate pressure-sensitive adhesive for protective films according to claim 1, characterized in that:
the polymer A comprises the following raw materials, by weight, 0-30 parts of ethylenically unsaturated acid, 80-95 parts of acrylate and 0.5-10 parts of monomer containing crosslinkable functional groups; the unsaturated acid containing ethylenic bond is methacrylate monomer or acrylic acid, and the monomer containing crosslinkable functional group is acrylic acid hydroxy ester monomer;
the polymer B comprises the following raw materials, by weight, 60-100 parts of acrylate and 0-20 parts of methacrylate monomer.
3. The acrylate pressure-sensitive adhesive for protective films according to claim 2, characterized in that:
the polymer A is prepared from the following raw materials in parts by weight: 80-95 parts of acrylate monomer, 5-20 parts of methacrylate monomer or acrylic acid; 0.5-10 parts of acrylate monomers; 0.2-1 part of initiator; 100 portions of ethyl acetate and 150 portions of ethyl acetate;
the polymer B is prepared from the following raw materials in parts by weight: 60-100 parts of acrylate monomer; 1-15 parts of a methacrylate monomer; 0.2-1 part of initiator; 100 portions of ethyl acetate and 150 portions of ethyl acetate.
4. The acrylate pressure-sensitive adhesive for protective films according to claim 3, characterized in that: the acrylate monomer is one or more than two of methyl acrylate, ethyl acrylate, butyl acrylate and isooctyl acrylate.
5. The acrylate pressure-sensitive adhesive for protective films according to claim 3, characterized in that: the methacrylate monomer is one or more than two of methyl methacrylate, ethyl methacrylate and butyl methacrylate.
6. The acrylate pressure-sensitive adhesive for protective films according to claim 3, characterized in that: the acrylic acid hydroxyl ester monomer is acrylamide and derivatives thereof, and the acrylamide derivatives are preferably one or more of hydroxyethyl acrylate, hydroxypropyl acrylate, hydroxybutyl acrylate or hydroxymethyl acrylamide.
7. The acrylate pressure-sensitive adhesive for protective films according to claim 1, characterized in that: the acrylate pressure-sensitive adhesive for the protective film also comprises tackifying resin and/or plasticizer, wherein the using amount of the tackifying resin is 1-30 parts by weight, and the using amount of the plasticizer is 1-10 parts by weight.
8. The acrylate pressure-sensitive adhesive for protective films according to claim 1, characterized in that:
the compound C is a compound containing amino, in particular polyamine; or,
the compound C is a polyvalent metal compound, specifically butyl titanate and a condensation compound thereof; or,
the compound C is a compound containing isocyanate groups, specifically a compound containing two or more blocked isocyanate groups.
9. The method for preparing the acrylate pressure-sensitive adhesive for protective films according to claim 1 or 3, characterized by comprising the steps of:
1) synthesis of Polymer A: adding ethyl acetate into a reaction kettle, starting stirring, adding 20 parts of mixed monomer consisting of acrylate monomer and methacrylate monomer or acrylic acid and acrylic hydroxy ester monomer, and simultaneously adding 0.1 part of initiator; heating to 78 deg.C, maintaining for 0.5-1 hr, and adding the rest mixed monomer containing 0.2-0.4 weight parts of initiator for 3-3.5 hr; after the addition, the temperature is kept for 60 minutes, and the initiator is replenished every three ten minutes; keeping the temperature for 1.5 hours after the initiator is added, cooling and discharging;
2) synthesis of Polymer B: adding ethyl acetate into a reaction kettle, starting stirring, adding 20 parts of mixed monomer consisting of acrylate monomer and methacrylate monomer, and simultaneously adding 0.1 part of initiator; heating to 78 deg.C, maintaining for 0.5-1 hr, and adding the rest mixed monomer containing 0.2-0.4 weight parts of initiator for 3-3.5 hr; after the addition, the temperature is kept for 60 minutes, and the initiator is replenished every three ten minutes; keeping the temperature for 1.5 hours after the initiator is added, cooling and discharging;
3) mixing the polymer A prepared in the step 1), the polymer B prepared in the step 2) and the compound C according to the proportion in the claim 1, and uniformly mixing to obtain the acrylate pressure-sensitive adhesive for the protective film.
10. The method for preparing the acrylate pressure-sensitive adhesive for protective films according to claim 9, comprising the steps of: in step 3, the acrylate pressure-sensitive adhesive for the protective film further comprises tackifying resin and a plasticizer, wherein the using amount of the tackifying resin is 1-30 parts by weight, and the using amount of the plasticizer is 1-10 parts by weight.
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| CN106543348A (en) * | 2016-11-22 | 2017-03-29 | 博立尔化工（扬州）有限公司 | A kind of acrylic resin with environment-friendlyplasticizer plasticizer with excellent compatibility |
| CN108795342A (en) * | 2018-06-20 | 2018-11-13 | 烟台保立佳新材料有限公司 | A kind of polyethylene protective film pressure sensitive adhesive and its preparation process that can eliminate fisheye |
| CN109536048A (en) * | 2018-10-11 | 2019-03-29 | 福建鸿利印刷材料工贸有限公司 | A kind of environmental protection composite membrane and its glue and preparation method that use |
| CN110041860A (en) * | 2019-05-14 | 2019-07-23 | 平湖铂淳胶粘技术有限公司 | A kind of pressure-sensitive adhesive and preparation method thereof with high peeling force |
| WO2020216170A1 (en) * | 2019-04-24 | 2020-10-29 | 歌尔股份有限公司 | Diaphragm for use in micro sound-generating apparatus, and micro sound-generating apparatus |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103756602B (en) | 2016-04-20 |
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