CN108048006A - A kind of solvent-type acrylic ester pressure-sensitive for being suitable for bonding TPU and preparation method thereof - Google Patents
A kind of solvent-type acrylic ester pressure-sensitive for being suitable for bonding TPU and preparation method thereof Download PDFInfo
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- CN108048006A CN108048006A CN201710692771.5A CN201710692771A CN108048006A CN 108048006 A CN108048006 A CN 108048006A CN 201710692771 A CN201710692771 A CN 201710692771A CN 108048006 A CN108048006 A CN 108048006A
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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
- 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
- C09J151/08—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 macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F2/00—Processes of polymerisation
- C08F2/12—Polymerisation in non-solvents
- C08F2/16—Aqueous medium
- C08F2/22—Emulsion polymerisation
- C08F2/24—Emulsion polymerisation with the aid of emulsifying agents
- C08F2/30—Emulsion polymerisation with the aid of emulsifying agents non-ionic
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F283/00—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G
- C08F283/06—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G on to polyethers, polyoxymethylenes or polyacetals
- C08F283/065—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G on to polyethers, polyoxymethylenes or polyacetals on to unsaturated polyethers, polyoxymethylenes or polyacetals
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- Adhesives Or Adhesive Processes (AREA)
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Abstract
The invention discloses a kind of solvent-type acrylic ester pressure-sensitive for being suitable for bonding TPU, which is made by including the following raw material：9~18 parts by weight of hard monomer, 31~37 parts by weight of soft monomer, 0.8~6 parts by weight of polar monomer, 0.6~4.5 parts by weight of polyether reactant type emulsifier, 0.08~0.3 parts by weight of initiator, 1~5% that hardener dose is solvent-type acrylic ester pressure-sensitive total weight.The solvent-type acrylic ester pressure-sensitive of the present invention has stronger adhesive force to TPU film; height holds viscous (200h is without displacement under the conditions of 25 DEG C) high peeling force (＞ 10N/25mm); solve the problems, such as existing acrylate pressure-sensitive adhesive to TPU material cohesions difference bonding loosely; and the fields such as mobile phone adhesive tape, protection film for automobile, body sticker can be widely used in without residue glue after removing.
Description
Technical field
The invention belongs to adhesive fields, and in particular to a kind of solvent-type acrylic ester pressure-sensitive for being suitable for bonding TPU
And preparation method thereof.
Background technology
TPU (thermoplastic polyurethane) film is using TPU materials as film article made of main raw material(s), is a kind of new
High-performance environment-friendly thin-film material, have intensity height, good toughness, resist cold, oil resistant, ageing-resistant, weatherability, it is environment-protecting and non-poisonous, can divide
The good characteristics such as solution.Since TPU film has the features such as easy to use, functional diversities, TPU is because of its superior performance and environmental protection
Concept is increasingly subject to the welcome of people.At present, every place using PVC, TPU can become the substitute of PVC.TPU is not only
Possess remarkable high-tension, high-tensile strength, tough and ageing-resistant characteristic, and be kind of a ripe environment-friendly materials.But TPU material tables
Face can be low, uses existing adhesive good bonding relatively difficult to achieve.
The content of the invention
The defects of being not easy to be bonded TPU the technical problem to be solved by the present invention is to overcome existing adhesive provides a kind of suitable
For being bonded the solvent-type acrylic ester pressure-sensitive of TPU.
It is a further object of the present invention to provide a kind of methods for preparing above-mentioned solvent-type acrylic ester pressure-sensitive.
In order to solve the above technical problem, the present invention provides following technical solutions：
A kind of solvent-type acrylic ester pressure-sensitive for being suitable for bonding TPU, is made by including the following raw material：
9~18 parts by weight of hard monomer；
31~37 parts by weight of soft monomer；
0.8~6 parts by weight of polar monomer；
0.6~4.5 parts by weight of polyether reactant type emulsifier；
0.08~0.3 parts by weight of initiator；
Hardener dose is the 1~5% of solvent-type acrylic ester pressure-sensitive total weight.
Preferably, the hard monomer be methyl acrylate, isobornyl methacrylate, in methyl methacrylate extremely
Few one kind.
Preferably, the soft monomer is at least one of Isooctyl acrylate monomer, butyl acrylate, ethyl acrylate.
Preferably, the polar monomer is methacrylic acid, acrylic acid, itaconic acid, hydroxy-ethyl acrylate, methacrylic acid
At least one of hydroxyl ethyl ester.
Preferably, the polyether reactant type emulsifier has following chemical structural formula
R is alkyl, and EO adds molal quantity 10~40.
Preferably, the initiator is azodiisobutyronitrile (AIBN), dibenzoyl peroxide (BPO) and/or peroxidating
Lauroyl (LPO).
Preferably, the curing agent is titanium acetylacetone and/or isocyanates.
Preferably, the raw material further includes the solvent of 45~60 parts by weight.
The present invention is added in using substep and prepares above-mentioned solvent-type acrylic ester pressure-sensitive, is specifically comprised the following steps：
(1) hard monomer, soft monomer, polar monomer, polyether reactant type emulsifier are mixed, obtains mix monomer；
(2) initiator is dissolved with solvent；
(3) a part of mix monomer and solvent are added in reaction vessel, is heated to 60~80 DEG C, adds a part and draw
Send out agent, insulation reaction；
(4) mix monomer of remainder and a part of initiator are added in into reaction vessel, after adding, through anti-after heat preservation
It should；
(5) reaction vessel, insulation reaction is added portionwise in the initiator of remainder；
(6) after the completion of reacting, cooling adds in curing agent, is mixed to get to the solvent-type acrylic ester pressure-sensitive.
Preferably, in step (3), mix monomer is added in by the 40~45% of mix monomer total amount, by initiator total amount
30~40% add in initiator；In step (4), initiator is added in by the 30~40% of initiator total amount.
Ethyl acetate, butyl acetate, hexamethylene, isopropanol can be selected in solvent, can be used alone or in combination.
Compared with prior art, the invention has the advantages that：
1st, the present invention has TPU film by cleverly introducing polyether structure, the solvent-type acrylic ester pressure-sensitive of preparation
There is stronger adhesive force, height is held viscous (200h is without displacement under the conditions of 25 DEG C) high peeling force (＞ 10N/25mm), solved existing
The problem of acrylate pressure-sensitive adhesive is bonded loosely to TPU material cohesions difference can be widely used in mobile phone adhesive tape, automobile protection
The fields such as film, body sticker.
2nd, solvent-type acrylic ester pressure-sensitive of the invention, which can be removed, has excellent performance, and has the characteristics that after removing without residue glue.
Specific embodiment
The preferred embodiment of the present invention is illustrated below, it should be understood that preferred embodiment described herein is only used
In the description and interpretation present invention, it is not intended to limit the present invention.
The polyether reactant type emulsifier of the present invention is selected from the ER serial reaction type emulsifiers of Ai Dike (ADEKA) productions,
With following chemical structural formula
R is alkyl, and EO (ethylene oxide) adds molal quantity 10~40.
In the ER serial reaction type emulsifiers, the EO of ER-40, which adds the EO that molal quantity is 40, ER-20, to be added molal quantity and is
20。
Embodiment 1
(1) first by Isooctyl acrylate monomer 37g, methyl acrylate 6.5g, isobornyl methacrylate 2.5g, acrylic acid
Hydroxyl ethyl ester 3g, acrylic acid 3g, ER-400.6g are uniformly mixed, and obtain mix monomer；
(2) take initiator A IBN 0.08g and ethyl acetate 1g mixed dissolutions uniform, obtain initiator solution；
(3) ethyl acetate 13.4g, butyl acetate 19.2g, hexamethylene 9.6g, isopropanol 4.8g is taken to be uniformly mixed, is mixed
Bonding solvent；
(4) 40% of mix monomer in step (1) is taken, takes the 33% of step (3) mixed solvent, is poured into equipped with stirring dress
It puts, in the reaction flask of thermometer and condenser pipe, is gradually heated to 70 DEG C, then will take initiator solution in step (2)
Start to react in 40% addition flask.
(5) notice that observation starts timing after minute bubbles occurs in reaction liquid level, by initiator in step (2) after 1h is reacted
40% and remaining mix monomer of solution are dropped evenly by constant pressure funnel into reaction system with mixed solvent, wait to drip
After finishing (2h), insulation reaction 1h.
(6) heat preservation completes 10% of initiator solution in backward reaction flask addition step (2), and reaction temperature rises to 76
DEG C, remaining initiator solution is added in after keeping the temperature 1h, keeps the temperature 3h.
(7) after reaction, cooling discharging obtains glue.
(8) step 7) is made glue to weigh, by the weight of glue, add in 2.5% titanium acetylacetone and 2.5% it is different
Cyanate (L-75 Bayers), is sufficiently stirred, obtains solvent-type acrylic ester pressure-sensitive.
Embodiment 2
(1) first by Isooctyl acrylate monomer 29g, ethyl acrylate 2g, methyl acrylate 14.5g, methyl methacrylate
3.5g, hydroxy-ethyl acrylate 1g, acrylic acid 2g, ER-404.5g are uniformly mixed, and obtain mix monomer；
(2) take initiator B PO 0.2g, LPO 0.1g and ethyl acetate 1g mixed dissolutions uniform, obtain initiator solution；
(3) ethyl acetate 16g, butyl acetate 23g, hexamethylene 11g, isopropanol 5g is taken to be uniformly mixed, obtains mixed solvent；
(4) 45% of mix monomer in step (1) is taken, takes the 33% of step (3) mixed solvent, is poured into equipped with stirring dress
It puts, in the reaction flask of thermometer and condenser pipe, is gradually heated to 70 DEG C, then will take initiator solution in step (2)
Start to react in 30% addition flask.
(5) notice that observation starts timing after minute bubbles occurs in reaction liquid level, by initiator in step (2) after 1h is reacted
40% and remaining mix monomer of solution are dropped evenly by constant pressure funnel into reaction system with mixed solvent, wait to drip
After finishing (2h), insulation reaction 1h.
(6) heat preservation completes 15% of initiator solution in backward reaction flask addition step (2), and reaction temperature rises to 76
DEG C, remaining initiator solution is added in after keeping the temperature 1h, keeps the temperature 3h.
(7) after reaction, cooling discharging obtains glue.
(8) step 7) is made glue to weigh, by the weight of glue, adds in 1% titanium acetylacetone and 1.5% isocyanide
Acid esters (L-75), is sufficiently stirred, and obtains solvent-type acrylic ester pressure-sensitive.
Embodiment 3
(1) first by Isooctyl acrylate monomer 37g, methyl acrylate 9g, hydroxy-ethyl acrylate 3g, itaconic acid 2g, ER-20
4.5g is uniformly mixed, and obtains mix monomer；
(2) take initiator A IBN 0.3g and ethyl acetate 1g mixed dissolutions uniform, obtain initiator solution；
(3) ethyl acetate 15.5g, butyl acetate 22.5g, hexamethylene 11g, isopropanol 4.5g is taken to be uniformly mixed, is mixed
Bonding solvent；
(4) 40% of mix monomer in step (1) is taken, takes the 28% of step (3) mixed solvent, is poured into equipped with stirring dress
It puts, in the reaction flask of thermometer and condenser pipe, is gradually heated to 70 DEG C, then will take initiator solution in step (2)
Start to react in 30% addition flask.
(5) notice that observation starts timing after minute bubbles occurs in reaction liquid level, by initiator in step (2) after 1h is reacted
30% and remaining mix monomer of solution are dropped evenly by constant pressure funnel into reaction system with mixed solvent, wait to drip
After finishing (2h), insulation reaction 1h.
(6) heat preservation completes 20% of initiator solution in backward reaction flask addition step (2), and reaction temperature rises to 76
DEG C, remaining initiator solution is added in after keeping the temperature 1h, keeps the temperature 3h.
(7) after reaction, cooling discharging obtains glue.
(8) step 7) is made glue to weigh, by the weight of glue, adds in 2% titanium acetylacetone and 1% isocyanic acid
Ester (L-75), is sufficiently stirred, and obtains solvent-type acrylic ester pressure-sensitive.
Embodiment 4
(1) first by Isooctyl acrylate monomer 31g, methyl acrylate 14.5g, isobornyl methacrylate 1g, acrylic acid
Hydroxyl ethyl ester 0.5g, acrylic acid 2g, ER-404.0g are uniformly mixed, and obtain mix monomer；
(2) take initiator B PO 0.1g, AIBN 0.1g and ethyl acetate 1g mixed dissolutions uniform, obtain initiator solution；
(3) ethyl acetate 15g, butyl acetate 23g, hexamethylene 10g, isopropanol 5g is taken to be uniformly mixed, obtains mixed solvent；
(4) 45% of mix monomer in step (1) is taken, takes the 28% of step (3) mixed solvent, is poured into equipped with stirring dress
It puts, in the reaction flask of thermometer and condenser pipe, is gradually heated to 70 DEG C, then will take initiator solution in step (2)
Start to react in 30% addition flask.
(5) notice that observation starts timing after minute bubbles occurs in reaction liquid level, by initiator in step (2) after 1h is reacted
40% and remaining mix monomer of solution are dropped evenly by constant pressure funnel into reaction system with mixed solvent, wait to drip
After finishing (2h), insulation reaction 1h.
(6) heat preservation completes 15% of initiator solution in backward reaction flask addition step (2), and reaction temperature rises to 76
DEG C, remaining initiator solution is added in after keeping the temperature 1h, keeps the temperature 3h.
(7) after reaction, cooling discharging obtains glue.
(8) step 7) is made glue to weigh, by the weight of glue, add in 0.5% titanium acetylacetone and 1.5% it is different
Cyanate (L-75), is sufficiently stirred, and obtains solvent-type acrylic ester pressure-sensitive.
Embodiment 5
(1) first by Isooctyl acrylate monomer 30g, butyl acrylate 5g, methyl acrylate 9g, methyl methacrylate 1g,
Hydroxyethyl methacrylate 0.4g, methacrylic acid 0.4g, ER-40 0.6g are uniformly mixed, and obtain mix monomer；
(2) take initiator B PO 0.2g, LPO 0.1g and ethyl acetate 1g mixed dissolutions uniform, obtain initiator solution；
(3) ethyl acetate 13.4g, butyl acetate 18.2g, hexamethylene 8.6g, isopropanol 4.8g is taken to be uniformly mixed, is mixed
Bonding solvent；
(4) 42% of mix monomer in step (1) is taken, takes the 30% of step (3) mixed solvent, is poured into equipped with stirring dress
It puts, in the reaction flask of thermometer and condenser pipe, is gradually heated to 70 DEG C, then will take initiator solution in step (2)
Start to react in 35% addition flask.
(5) notice that observation starts timing after minute bubbles occurs in reaction liquid level, by initiator in step (2) after 1h is reacted
40% and remaining mix monomer of solution are dropped evenly by constant pressure funnel into reaction system with mixed solvent, wait to drip
After finishing (2h), insulation reaction 1h.
(6) heat preservation completes 12.5% of initiator solution in backward reaction flask addition step (2), and reaction temperature rises to
76 DEG C, remaining initiator solution is added in after keeping the temperature 1h, keeps the temperature 3h.
(7) after reaction, cooling discharging obtains glue.
(8) step 7) is made glue to weigh, by the weight of glue, add in 0.5% titanium acetylacetone and 0.5% it is different
Cyanate (L-75), is sufficiently stirred, and obtains solvent-type acrylic ester pressure-sensitive.
Embodiment 6
(1) first by Isooctyl acrylate monomer 35g, methyl acrylate 14.5g, hydroxy-ethyl acrylate 3g, acrylic acid 1.5g,
ER-402.5g is uniformly mixed, and obtains mix monomer；
(2) take initiator B PO 0.2g, AIBN 0.1g and ethyl acetate 1g mixed dissolutions uniform, obtain initiator solution；
(3) ethyl acetate 16g, butyl acetate 23g, hexamethylene 11g, isopropanol 5g is taken to be uniformly mixed, obtains mixed solvent；
(4) 42% of mix monomer in step (1) is taken, takes the 30% of step (3) mixed solvent, is poured into equipped with stirring dress
It puts, in the reaction flask of thermometer and condenser pipe, is gradually heated to 70 DEG C, then will take initiator solution in step (2)
Start to react in 40% addition flask.
(5) notice that observation starts timing after minute bubbles occurs in reaction liquid level, by initiator in step (2) after 1h is reacted
40% and remaining mix monomer of solution are dropped evenly by constant pressure funnel into reaction system with mixed solvent, wait to drip
After finishing (2h), insulation reaction 1h.
(6) heat preservation completes 10% of initiator solution in backward reaction flask addition step (2), and reaction temperature rises to 76
DEG C, remaining initiator solution is added in after keeping the temperature 1h, keeps the temperature 3h.
(7) after reaction, cooling discharging obtains glue.
(8) step 7) is made glue to weigh, by the weight of glue, add in 2.5% titanium acetylacetone and 1.5% it is different
Cyanate (L-75), is sufficiently stirred, and obtains solvent-type acrylic ester pressure-sensitive.
Performance test：
Solvent-type acrylic ester pressure-sensitive is coated in PET release papers with 40 μm of coaters, its thickness control is existed
18~20um in 90 DEG C of dry 5min, takes out and is ridden over transparent TPU film on release PET with mounting film machine, glue is transferred to transparent
In TPU membrane, sample is positioned in 55 DEG C of baking ovens and cures 72h, last sample preparation test.
1 each embodiment performance characterization summary sheet of table
Embodiment described above is only that the preferred addition formulation content of the present invention is described, not to the present invention
Overall conception and protection domain are defined, and find out stripping of the solvent-type acrylic ester pressure-sensitive of the present invention on TPU from result
More than 10N/25mm is can reach from power, is held viscous more than 200h and without residue glue.
Finally it should be noted that：The foregoing is only a preferred embodiment of the present invention, is not intended to limit the invention,
Although the present invention is described in detail with reference to the foregoing embodiments, for those skilled in the art, still may be used
To modify to the technical solution recorded in foregoing embodiments or carry out equivalent substitution to which part technical characteristic.
Within the spirit and principles of the invention, any modifications, equivalent replacements and improvements are made should be included in the present invention's
Within protection domain.
Claims (10)
1. a kind of solvent-type acrylic ester pressure-sensitive for being suitable for bonding TPU, is made by including the following raw material：
9~18 parts by weight of hard monomer；
31~37 parts by weight of soft monomer；
0.8~6 parts by weight of polar monomer；
0.6~4.5 parts by weight of polyether reactant type emulsifier；
0.08~0.3 parts by weight of initiator；
Hardener dose is the 1~5% of solvent-type acrylic ester pressure-sensitive total weight.
2. solvent-type acrylic ester pressure-sensitive according to claim 1, it is characterised in that：The hard monomer is acrylic acid first
At least one of ester, isobornyl methacrylate, methyl methacrylate.
3. solvent-type acrylic ester pressure-sensitive according to claim 1, it is characterised in that：The soft monomer is different for acrylic acid
At least one of monooctyl ester, butyl acrylate, ethyl acrylate.
4. solvent-type acrylic ester pressure-sensitive according to claim 1, it is characterised in that：The polar monomer is methyl-prop
At least one of olefin(e) acid, acrylic acid, itaconic acid, hydroxy-ethyl acrylate, hydroxyethyl methacrylate.
5. solvent-type acrylic ester pressure-sensitive according to claim 1, it is characterised in that：The polyether reactant type emulsifier
With following chemical structural formula
R is alkyl, and EO adds molal quantity 10~40.
6. solvent-type acrylic ester pressure-sensitive according to claim 1, it is characterised in that：The initiator is different for azo two
Butyronitrile, dibenzoyl peroxide and/or lauroyl peroxide.
7. solvent-type acrylic ester pressure-sensitive according to claim 1, it is characterised in that：The curing agent is acetylacetone,2,4-pentanedione
Titanium and/or isocyanates.
8. solvent-type acrylic ester pressure-sensitive according to claim 1, it is characterised in that：The raw material further includes 45~60
The solvent of parts by weight.
9. the preparation method of any solvent-type acrylic ester pressure-sensitives of claim 1-8, includes the following steps：
(1) hard monomer, soft monomer, polar monomer, polyether reactant type emulsifier are mixed, obtains mix monomer；
(2) initiator is dissolved with solvent；
(3) a part of mix monomer and solvent are added in reaction vessel, is heated to 60~80 DEG C, adds a part of initiation
Agent, insulation reaction；
(4) mix monomer of remainder and a part of initiator are added in into reaction vessel, after adding, insulation reaction；
(5) reaction vessel, insulation reaction is added portionwise in the initiator of remainder；
(6) after the completion of reacting, cooling adds in curing agent, is mixed to get to the solvent-type acrylic ester pressure-sensitive.
10. preparation method according to claim 9, it is characterised in that：In step (3), by mix monomer total amount 40~
45% adds in mix monomer, and initiator is added in by the 30~40% of initiator total amount；
In step (4), initiator is added in by the 30~40% of initiator total amount.
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| CN114231216A (en) * | 2021-11-25 | 2022-03-25 | 肇庆新丰环保材料有限公司 | Ultra-light stripping solvent type acrylate pressure-sensitive adhesive |
| CN114621710A (en) * | 2020-12-10 | 2022-06-14 | 安佐化学有限公司 | Adhesive for invisible car cover and preparation method and application thereof |
| CN115141584A (en) * | 2021-08-02 | 2022-10-04 | 西安航天三沃化学有限公司 | Acrylate pressure-sensitive adhesive for TPU (thermoplastic polyurethane) automobile protective film and preparation method and use method thereof |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114621710A (en) * | 2020-12-10 | 2022-06-14 | 安佐化学有限公司 | Adhesive for invisible car cover and preparation method and application thereof |
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| CN115141584B (en) * | 2021-08-02 | 2023-11-07 | 西安航天三沃化学有限公司 | Acrylic pressure-sensitive adhesive for TPU automobile protective film, and preparation method and application method thereof |
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| CN115975555A (en) * | 2022-06-29 | 2023-04-18 | 西安航天三沃化学有限公司 | Cold-heat-resistant-replacement-wide-temperature-range pressure-sensitive adhesive for TPU (thermoplastic polyurethane) car cover and preparation method thereof |
| CN115975555B (en) * | 2022-06-29 | 2024-10-11 | 西安航天三沃化学有限公司 | Pressure-sensitive adhesive for TPU (thermoplastic polyurethane) vehicle cover with cold and hot resistance alternating wide temperature range and preparation method |
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Application publication date: 20180518 |