CN115975559A - Adhesive resin, method for producing the same, and protective film - Google Patents
Adhesive resin, method for producing the same, and protective film Download PDFInfo
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- CN115975559A CN115975559A CN202211691436.0A CN202211691436A CN115975559A CN 115975559 A CN115975559 A CN 115975559A CN 202211691436 A CN202211691436 A CN 202211691436A CN 115975559 A CN115975559 A CN 115975559A
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Abstract
The invention provides an adhesive resin, a preparation method thereof and a protective film, and particularly relates to the technical field of high polymer materials. The adhesive resin comprises the following components in parts by weight: 70-90 parts of acrylic block copolymer, 5-15 parts of tackifying resin, 5-15 parts of maleic acid snore graft hydrogenated styrene block copolymer and 0.1-0.5 part of antioxidant; wherein the acrylic block copolymer is a living anionic polymer elastomer. The adhesive resin provided by the invention uses acrylic block copolymer with better polarity, the material is softer, the pure raw material has higher viscosity when being formed into a film, and the physical adsorption of an adhesive layer on a base material can be increased by adding less tackifying resin, so that the stripping force is improved; the viscosity change of different base materials is small, and the universality is better. The maleic acid ester grafted hydrogenated styrene block copolymer has better compatibility with polar material acrylic block copolymer, and keeps the relative stability of stripping force.
Description
Technical Field
The invention relates to the technical field of high polymer materials, in particular to adhesive resin, a preparation method thereof and a protective film.
Background
Protective films, which are generally composed of a pressure-sensitive adhesive layer, a core layer and an unwinding layer, are films for protecting vulnerable surfaces, and are intended for temporary surface protection of the surface of a protected substrate (metal plate, plastic plate, decorative plate, coated plate, etc.) during production, processing, transportation and storage. The main performance requirements of the industry for protective films are: proper and stable viscosity, easy uncoiling, few crystal points, easy tearing, no residual glue, no image, weather resistance and the like.
The adhesive layer is the core structure of the protective film and determines the main performance of the protective film product. Currently, the adhesive layers used in the industry are mainly classified into coating type solvent adhesives or hot melt adhesives and co-extrusion type self-adhesive adhesives according to the production process. The prior coextrusion self-adhesive mainly has the following defects:
1. the amount of tackifying resin is large, the viscosity is unstable, and the post-tackifying property is high;
2. the viscosity change of different base materials is large, especially the viscosity of the surface of a rough surface and a low surface energy base material is reduced quickly, and the universality is poor;
3. the compatibility with PE and PP materials commonly used for the protective film core layer is poor, so that the protective film is easy to glue residue in the using process and has poor weather resistance.
In view of the above, the present invention is particularly proposed.
Disclosure of Invention
It is an object of the present invention to provide a tackifying resin which aims at solving at least one of the above-mentioned technical drawbacks.
In order to solve the technical problems, the invention adopts the following technical scheme:
the invention provides a first aspect of adhesive resin, which comprises the following components in parts by weight:
70-90 parts of acrylic block copolymer, 5-15 parts of tackifying resin, 5-15 parts of maleic acid snore grafted hydrogenated styrene block copolymer and 0.1-0.5 part of antioxidant;
wherein the acrylic block copolymer is a living anionic polymer elastomer.
Optionally, the acrylic block copolymer comprises an acrylate copolymer in the A-B-A form and/or the A-B form.
Preferably, the acrylic block copolymer is ase:Sub>A triblock copolymer in an A-B-A shape, wherein the block A is PMMA, and the block B is PBA or P (BA/2 EHA).
Optionally, the melt flow index of the acrylic block copolymer at 190 ℃ under a load of 2.16kg is 3g/10 min-10 g/10min.
Optionally, the tackifying resin comprises at least one of a petroleum resin, a terpene-phenol resin, a styrene resin, a monomer resin, and a rosin resin.
Preferably, the softening point of the tackifying resin is between 90 ℃ and 160 ℃.
Preferably, the tackifying resin is at least one of hydrogenated carbon-nine petroleum resin, terpene-phenol resin and styrene resin.
Optionally, the grafting ratio of the maleic anhydride grafted hydrogenated styrene block copolymer is 0.1% to 0.35%.
Preferably, the maleic acid ester grafted hydrogenated styrene block copolymer has a diblock content of 0% to 30%.
Preferably, the melt flow index of the maleic acid ethylene grafted hydrogenated styrene block copolymer under the conditions of the temperature of 190 ℃ and the load of 2.16kg is 0.2g/10 min-14 g/10min.
Alternatively, the antioxidant comprises at least one of pentaerythrityl tetrakis [ beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionate ], diethyleneglycol bis [ beta- (3-tert-butyl-4-hydroxy-5-methylphenyl) propionate ], thioethylenebis [3- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionate ], tris (2, 4-di-tert-butylphenyl) phosphite, and pentaerythrityl tetrakis (3-laurylthiopropionate).
The second aspect of the invention provides a preparation method of the adhesive resin, wherein the adhesive resin is obtained by uniformly mixing an acrylic block copolymer, a tackifying resin, a maleic acid and glycerin grafted hydrogenated styrene block copolymer and an antioxidant, and extruding and granulating by a twin screw.
The invention provides a protective film, which comprises an adhesive layer, a core layer and an uncoiling layer, wherein the adhesive layer, the core layer and the uncoiling layer are sequentially attached;
wherein the adhesive layer is made of the adhesive resin of the first aspect.
Optionally, the core layer is made of a polyethylene and hydrogenated styrene block copolymer.
Preferably, the unrolling layer is made of high pressure low density polyethylene.
Optionally, the mass ratio of the polyethylene to the hydrogenated styrene block copolymer in the core layer is 1 to 4.
Preferably, the hydrogenated styrene block copolymer has a 1, 2-addition degree in a polybutadiene block precursor of 60 to 85% by mole.
Preferably, the hydrogenated styrene block copolymer has a diblock content of 0 to 15%.
Preferably, the hydrogenated styrene block copolymer has a melt flow index of 0.1g/10min to 40g/10min at a temperature of 190 ℃ under a load of 2.16 kg.
Compared with the prior art, the invention has at least the following beneficial effects:
the adhesive resin provided by the invention uses acrylic block copolymer with better polarity, the material is softer, the pure raw material has higher viscosity when being formed into a film, and the physical adsorption of an adhesive layer on a base material can be increased by adding less tackifying resin, so that the stripping force is improved; the viscosity change of different base materials is small, and the universality is better. The maleic acid ethylene glycol grafted hydrogenated styrene block copolymer has better compatibility with polar material acrylic block copolymer, improves the change of the peeling force in time or temperature in the adhesive layer, and keeps the relative stability of the peeling force.
The preparation method provided by the invention has the advantages of simple process, high degree of mechanization and good controllability, and is suitable for large-scale industrial production.
The protective film provided by the invention has higher viscosity on the surfaces of different base materials such as stainless steel, PVC, rock plates and the like, particularly protects better viscosity on rough rock plates, has smaller viscosity change on different base materials and has better universality.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention. The components of embodiments of the present invention may be arranged and designed in a wide variety of different configurations.
It should be noted that, in this document, relational terms such as first and second, and the like are used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Also, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus.
According to a first aspect of the present invention, there is provided an adhesive resin comprising the following components in parts by weight:
70-90 parts of acrylic block copolymer, 5-15 parts of tackifying resin, 5-15 parts of maleic acid snore grafted hydrogenated styrene block copolymer and 0.1-0.5 part of antioxidant;
wherein the acrylic block copolymer is a living anionic polymer elastomer.
The adhesive resin provided by the invention uses acrylic block copolymer with better polarity, the material is softer, the pure raw material has higher viscosity when being formed into a film, and the physical adsorption of an adhesive layer on a base material can be increased by adding less tackifying resin, so that the stripping force is improved; the viscosity change of different base materials is small, and the universality is better. The maleic acid ethylene glycol grafted hydrogenated styrene block copolymer has better compatibility with polar material acrylic block copolymer, improves the change of the peeling force in time or temperature in the adhesive layer, and keeps the relative stability of the peeling force.
In some embodiments of the present invention, the weight part of the acryl block copolymer in the adhesive resin is typically, but not limited to, 70 parts, 75 parts, 80 parts, 85 parts, or 90 parts; the parts by weight of the tackifying resin are typically, but not limited to, 5 parts, 7 parts, 9 parts, 11 parts, 13 parts, or 15 parts; the parts by weight of the maleic acid urea-grafted hydrogenated styrene block copolymer are typically, but not limited to, 5 parts, 7 parts, 9 parts, 11 parts, 13 parts or 15 parts; the weight portion of the antioxidant is typically, but not limited to, 0.1 part, 0.2 part, 0.3 part, 0.4 part or 0.5 part.
Optionally, the acrylic block copolymer comprises an acrylate copolymer in the A-B-A form and/or the A-B form.
Preferably, the acrylic block copolymer is ase:Sub>A triblock copolymer in ase:Sub>A-B-ase:Sub>A shape, wherein the block ase:Sub>A is pmmase:Sub>A, and the block B is pbase:Sub>A or P (base:Sub>A/2 ehase:Sub>A).
Optionally, the melt flow index of the acrylic block copolymer at 190 ℃ under a load of 2.16kg is 3g/10 min-10 g/10min. In some embodiments of the present invention, the acrylic block copolymer has a melt flow index of typically, but not limited to, 3g/10min, 4g/10min, 5g/10min, 6g/10min, 7g/10min, 8g/10min, 9g/10min, or 10g/10min at 190 ℃ under a load of 2.16 kg.
Optionally, the tackifying resin comprises at least one of a petroleum resin, a terpene phenolic resin, a styrenic resin, a monomeric resin, and a rosin resin.
Preferably, the softening point of the tackifying resin is between 90 ℃ and 160 ℃.
Preferably, the tackifying resin is at least one of hydrogenated carbon-nine petroleum resin, terpene-phenol resin and styrene resin.
Optionally, the grafting ratio of the maleic anhydride grafted hydrogenated styrene block copolymer is 0.1% to 0.35%. In some embodiments of the present invention, the graft ratio of the maleic anhydride grafted hydrogenated styrene block copolymer is typically, but not limited to, 0.1%, 0.15%, 0.2%, 0.25%, 0.3%, or 0.35%.
Preferably, the maleic acid ester grafted hydrogenated styrene block copolymer has a diblock content of 0% to 30%. In some embodiments of the present invention, the diblock content in the maleic acid ester-grafted hydrogenated styrene block copolymer is typically, but not limited to, 5%, 10%, 15%, 20%, 25%, or 30%.
Preferably, the melt flow index of the maleic acid ethylene grafted hydrogenated styrene block copolymer under the conditions of the temperature of 190 ℃ and the load of 2.16kg is 0.2g/10 min-14 g/10min. In some embodiments of the present invention, the melt flow index of the maleic acid/ethylene glycol grafted hydrogenated styrene block copolymer is typically but not limited to 0.2g/10min, 0.5g/10min, at a temperature of 190 ℃ under a load of 2.16kg,
1g/10min, 2g/10min, 5g/10min, 7g/10min, 9g/10min, 10g/10min, 12g/10min or 14g/10min.
Alternatively, the antioxidant comprises at least one of pentaerythrityl tetrakis [ beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionate ], diethyleneglycol bis [ beta- (3-tert-butyl-4-hydroxy-5-methylphenyl) propionate ], thioethylenebis [3- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionate ], tris (2, 4-di-tert-butylphenyl) phosphite, and pentaerythrityl tetrakis (3-laurylthiopropionate).
According to the preparation method of the adhesive resin provided by the second aspect of the invention, the acrylic block copolymer, the tackifying resin, the maleic acid snorkel grafted hydrogenated styrene block copolymer and the antioxidant are uniformly mixed, and the mixture is subjected to twin-screw extrusion granulation to obtain the adhesive resin.
The preparation method provided by the invention has the advantages of simple process, high degree of mechanization and good controllability, and is suitable for large-scale industrial production.
According to a third aspect of the present invention, there is provided a protective film comprising an adhesive layer, a core layer and an unwinding layer which are laminated in this order;
wherein the adhesive layer is made of the adhesive resin of the first aspect.
The protective film provided by the invention has higher viscosity on the surfaces of different base materials such as stainless steel, PVC, rock plates and the like, particularly protects better viscosity on rough rock plates, has smaller viscosity change on different base materials and has better universality.
Optionally, the core layer is made of a polyethylene and hydrogenated styrene block copolymer.
Conventional adhesive layers are based on Hydrogenated Styrene Block Copolymers (HSBC) and core layers are based on PE or PP. And co-extruding and film-blowing or tape-casting the viscous layer, the core layer and the uncoiling layer. HSBC and PE or PP compatibility are better, and the incomplete gluey phenomenon less appears in the protection film of making in the in-process of being heated. The acrylic block copolymer has poor compatibility with PE or PP, has certain compatibility with HSBC, and particularly has good compatibility with HSBC with high ethylene content, and the addition of HSBC with a certain amount of high ethylene content into the core layer can improve the compatibility with the adhesive layer and improve the weather resistance of the protective film.
Preferably, the unrolling layer is made of high pressure low density polyethylene.
Optionally, the mass ratio of the polyethylene to the hydrogenated styrene block copolymer in the core layer is 1 to 4.
Preferably, the hydrogenated styrene block copolymer has a 1, 2-addition degree in a polybutadiene block precursor of 60 to 85% by mole.
Preferably, the hydrogenated styrene block copolymer has a diblock content of 0 to 15%.
Preferably, the hydrogenated styrene block copolymer has a melt flow index of 0.1g/10min to 40g/10min at a temperature of 190 ℃ under a load of 2.16 kg.
Some embodiments of the present invention will be described in detail below with reference to examples. The embodiments and features of the embodiments described below can be combined with each other without conflict. The raw materials in the following examples and comparative examples were purchased from commercial sources unless otherwise specified.
The Shore A hardness of the acrylic block copolymer used in the following examples and comparative examples was 13, and the melt flow index was 6.2g/10min; the grafting ratio of the maleic acid urea grafted hydrogenated styrene block copolymer is 0.33 percent, and the melt flow index is 1.6g/10min; the softening point of the terpene-phenol resin is 115 ℃; the softening point of the styrene resin is 100 ℃; in the hydrogenated styrene block copolymer (SEBS), the styrene block content was 13wt.%, the diene block content was 7wt.%, the melt flow index was 3.5g/10min, and the glass transition temperature was-38 ℃.
Example 1
The embodiment provides an adhesive resin, which is composed of the following raw materials: 80kg of acrylic block copolymer, 10kg of maleic anhydride grafted hydrogenated styrene block copolymer, 10kg of terpene phenol resin and 0.4kg of antioxidant;
the main component of the antioxidant is pentaerythritol tetra (3-lauryl thiopropionate).
The raw materials are mixed and added into a double-screw extruder. The temperature of each zone of the double-screw extruder is 100-170 ℃; the rotating speed of the extruder is 300r/min, and then the viscous resin is obtained by drying (adding a powder isolating agent in the drying process to avoid agglomeration).
Example 2
This example provides an adhesive resin, which is composed of the following raw materials: 75kg of acrylic block copolymer, 10kg of maleic anhydride grafted hydrogenated styrene block copolymer, 15kg of terpene phenol resin and 0.4kg of antioxidant;
the main component of the antioxidant is pentaerythritol tetra (3-lauryl thiopropionate).
The raw materials are mixed and added into a double-screw extruder. The temperature of each zone of the double-screw extruder is 100-170 ℃; the rotating speed of the extruder is 300r/min, and then the viscous resin is obtained by drying (adding a powder isolating agent in the drying process to avoid agglomeration).
Example 3
This example provides an adhesive resin, which is composed of the following raw materials: 75kg of acrylic block copolymer, 15kg of maleic anhydride grafted hydrogenated styrene block copolymer, 10kg of terpene phenol resin and 0.4kg of antioxidant;
the main component of the antioxidant is pentaerythritol tetra (3-lauryl thiopropionate).
The raw materials are mixed and added into a double-screw extruder. The temperature of each zone of the double-screw extruder is 100-170 ℃; the rotating speed of the extruder is 300r/min, and then the viscous resin is obtained by drying (adding a powder isolating agent in the drying process to avoid agglomeration).
Example 4
The embodiment provides an adhesive resin, which is composed of the following raw materials: 90kg of acrylic block copolymer, 5kg of maleic anhydride grafted hydrogenated styrene block copolymer, 5kg of terpene phenol resin and 0.4kg of antioxidant;
the main component of the antioxidant is pentaerythritol tetra (3-lauryl thiopropionate).
The raw materials are mixed and added into a double-screw extruder. The temperature of each zone of the double-screw extruder is 100-170 ℃; the rotation speed of the extruder is 300r/min, and then the viscous resin is obtained by drying (adding a powder isolating agent in the drying process to avoid agglomeration).
Example 5
This example provides an adhesive resin, which is composed of the following raw materials: 75kg of acrylic block copolymer, 10kg of maleic anhydride grafted hydrogenated styrene block copolymer, 15kg of styrene resin and 0.4kg of antioxidant;
the main component of the antioxidant is pentaerythritol tetra (3-lauryl thiopropionate).
The raw materials are mixed and added into a double-screw extruder. The temperature of each zone of the double-screw extruder is 100-170 ℃; the rotation speed of the extruder is 300r/min, and then the viscous resin is obtained by drying (adding a powder isolating agent in the drying process to avoid agglomeration).
Comparative example 1
This comparative example provides an adhesive resin consisting of the following raw materials: 96kg of acrylic block copolymer, 4kg of maleic acid ethylene glycol grafted hydrogenated styrene block copolymer and 0.4kg of antioxidant;
the main component of the antioxidant is pentaerythritol tetra (3-lauryl thiopropionate).
The raw materials are mixed and added into a double-screw extruder. The temperature of each zone of the double-screw extruder is 100-170 ℃; the rotating speed of the extruder is 300r/min, and then the viscous resin is obtained by drying (adding a powder isolating agent in the drying process to avoid agglomeration).
Comparative example 2
The comparative example provides an adhesive resin consisting of the following raw materials: 70kg of acrylic block copolymer, 20kg of maleic acid urea grafted hydrogenated styrene block copolymer, 10kg of terpene phenol resin and 0.4kg of antioxidant;
the main component of the antioxidant is pentaerythritol tetra (3-lauryl thiopropionate).
The raw materials are mixed and added into a double-screw extruder. The temperature of each zone of the double-screw extruder is 100-170 ℃; the rotating speed of the extruder is 300r/min, and then the viscous resin is obtained by drying (adding a powder isolating agent in the drying process to avoid agglomeration).
Comparative example 3
This comparative example provides an adhesive resin consisting of the following raw materials: 25kg of terpene phenol resin, 75kg of SEBS and 0.4kg of antioxidant;
the main component of the antioxidant is pentaerythritol tetra (3-lauryl thiopropionate).
The raw materials are mixed and added into a double-screw extruder. The temperature of each zone of the double-screw extruder is 100-170 ℃; the rotation speed of the extruder is 300r/min, and then the viscous resin is obtained by drying (adding a powder isolating agent in the drying process to avoid agglomeration).
Test example 1
The adhesive resins obtained in examples 1 to 5 and comparative examples 1 to 3 were used as adhesive layers of protective films to obtain protective films of examples 6 to 10 and comparative examples 4 to 7, respectively.
The core layer was polyethylene and SEBS (styrene block content 19%; diblock content 7%; 1, 2-addition in molar terms in the polybutadiene block precursor 75%; melt flow index 2.8);
the uncoiling layer is polyethylene PE.
And co-extruding and blowing the three layers of raw materials, cooling and rolling to obtain the protective film. The thickness of the protective film adhesive layer is 5 μm, the core layer is 30 μm, and the uncoiling layer is 15 μm.
Table 1 lists the specific composition of the core layer and the unwinding layer in each protective film.
TABLE 1
Test example 2
The peel strength of the protective films of examples 6-10 and comparative examples 4-7 after being attached to different base materials for 20min at room temperature and after being thermally aged for 72h at 75 ℃ is measured according to the national standard GB/T2792; and the change of the phenomenon on the surface of the base material after the heat aging at 75 ℃ for 72 hours is observed and recorded, and the result is shown in Table 2.
TABLE 2
Finally, it should be noted that the above embodiments are only used for illustrating the technical solutions of the present invention, and not for limiting the same; although the present invention has been described in detail with reference to the foregoing embodiments, it should be understood by those skilled in the art that various changes in form and details may be made therein without departing from the spirit and scope of the invention; and the modifications or the substitutions do not make the essence of the corresponding technical solutions depart from the scope of the technical solutions of the embodiments of the present invention.
Claims (10)
1. The adhesive resin is characterized by comprising the following components in parts by weight:
70-90 parts of acrylic block copolymer, 5-15 parts of tackifying resin, 5-15 parts of maleic acid snore graft hydrogenated styrene block copolymer and 0.1-0.5 part of antioxidant;
wherein the acrylic block copolymer is a living anionic polymer elastomer.
2. The adhesive resin according to claim 1, wherein the acryl block copolymer comprises an acrylate copolymer of ase:Sub>A-B-ase:Sub>A type and/or ase:Sub>A-B type;
preferably, the acrylic block copolymer is ase:Sub>A triblock copolymer in an A-B-A shape, wherein the block A is PMMA, and the block B is PBA or P (BA/2 EHA).
3. The adhesive resin according to claim 1, wherein the acrylic block copolymer has a melt flow index of 3g/10min to 10g/10min at 190 ℃ under a load of 2.16 kg.
4. The tackifying resin of claim 1, wherein said tackifying resin comprises at least one of a petroleum resin, a terpene-phenolic resin, a styrenic resin, a monomeric resin, and a rosin resin;
preferably, the softening point of the tackifying resin is 90-160 ℃;
preferably, the tackifier resin is at least one of hydrogenated carbon-nonapetroleum resin, terpene-phenol resin and styrene resin.
5. The adhesive resin according to claim 1, wherein the maleic acid ester-grafted hydrogenated styrene block copolymer has a grafting ratio of 0.1% to 0.35%;
preferably, in the maleic acid ester grafted hydrogenated styrene block copolymer, the content of the diblock is 0-30%;
preferably, the melt flow index of the maleic acid ethylene grafted hydrogenated styrene block copolymer under the conditions of the temperature of 190 ℃ and the load of 2.16kg is 0.2g/10 min-14 g/10min.
6. The tackifying resin of claim 1, wherein said antioxidant comprises at least one of pentaerythrityl tetrakis [ beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionate ], diethyleneglycol bis [ beta- (3-tert-butyl-4-hydroxy-5-methylphenyl) propionate ], thioethylenebis [3- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionate ], tris (2, 4-di-tert-butylphenyl) phosphite, and pentaerythrityl tetrakis (3-laurylthiopropionate).
7. The method for preparing tackifying resin according to any one of claims 1 to 6, wherein said tackifying resin is obtained by mixing acrylic block copolymer, tackifying resin, maleic acid ethylene-grafted hydrogenated styrene block copolymer and antioxidant uniformly and extruding and pelletizing with twin screw.
8. The protective film is characterized by comprising an adhesive layer, a core layer and an uncoiling layer which are sequentially attached;
wherein the adhesive layer is made of the adhesive resin according to any one of claims 1 to 6.
9. The protective film of claim 8, wherein the core layer is made of a block copolymer of polyethylene and hydrogenated styrene;
preferably, the unrolling layer is made of high pressure low density polyethylene.
10. The protective film according to claim 9, wherein the mass ratio of the polyethylene to the hydrogenated styrene block copolymer in the core layer is 1 to 4;
preferably, in the hydrogenated styrene block copolymer, the 1, 2-addition degree in the polybutadiene block precursor is 60 to 85% in terms of mole number;
preferably, in the hydrogenated styrene block copolymer, the content of diblock is 0 to 15%;
preferably, the hydrogenated styrene block copolymer has a melt flow index of 0.1g/10min to 40g/10min at a temperature of 190 ℃ under a load of 2.16 kg.
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