CN104774572B - A kind of protection film for automobile and preparation method thereof - Google Patents

A kind of protection film for automobile and preparation method thereof Download PDF

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Publication number
CN104774572B
CN104774572B CN201510083195.5A CN201510083195A CN104774572B CN 104774572 B CN104774572 B CN 104774572B CN 201510083195 A CN201510083195 A CN 201510083195A CN 104774572 B CN104774572 B CN 104774572B
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sensitive adhesive
pressure sensitive
preparation
monomer
automobile
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CN104774572A (en
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葛允林
张曙明
耿有为
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CHUZHOU YUNLIN DIGITAL IMAGING SUPPLIES CO LTD
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CHUZHOU YUNLIN DIGITAL IMAGING SUPPLIES CO LTD
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Abstract

The present invention relates to a kind of protection film for automobile and preparation method thereof, protection film for automobile composition is followed successively by by PVC film, acrylate glue and release liners, acrylate glue is a kind of anti-disconnected glue pressure sensitive adhesive, it is using acrylic acid PolyTHF ester as function monomer, obtained with soft monomer and hard monomer copolymerization, acrylic acid PolyTHF ester monomer has the Long carbon chain of ehter bond, it is flexible relatively good, the anti-disconnected glue pressure sensitive adhesive of gained can be good at resisting tension failure, be conducive to preventing fracture of glue etc. during stretch bending, thus the protection film for automobile of the present invention can be very good to apply and automobile adhesive film field.

Description

A kind of protection film for automobile and preparation method thereof
Technical field
The present invention relates to a kind of lacquer painting diaphragm and preparation method thereof, more particularly to a kind of anti-scratch lacquer painting diaphragm and its Preparation method.
Background technology
Since being born from automobile, the step that the mankind pursue automobile maintenance never stops.In order to make love car bright all the time such as new, People design a lot of ways, and improve lacquer painting brightness, the waxing of reduction lacquer painting damage and are born.It is more permanent, effective in order to pursue Protecting effect, there is envelope glaze, the appearance of coating technique.But with the prosperity of science and technology, the requirement that we conserve to body of a motor car It is more and more, easier, more practical, more fashion, then body paint mask also just take advantage of a situation and raw.
Pressure-sensitive adhesive be a class to pressure-sensitive adhesive, only need to apply certain pressure with regard to adherend table can be moistened Face and the class adhesive that can produce adhesive strength, are characterized in viscous easy, that takes off is not difficult, and stripping is without damaging, in the long period Inner glue layer will not be solid, so pressure sensitive adhesive is also referred to as adhesive sticker, it is of wide application.Because automobile adhesive film is in the process of patch In, lacquer painting is not that the pressure sensitive adhesive on plane, pad pasting has stretching, and pressure sensitive adhesive has disconnected glue during stretching May, just have a strong impact on the caking property and the transparency of pad pasting.
The content of the invention
It is an object of the invention to provide a kind of protection film for automobile and preparation method thereof, protection film for automobile composition be followed successively by by PVC film, acrylate glue and release liners, acrylate glue are a kind of anti-disconnected glue pressure sensitive adhesive, are using acrylic acid PolyTHF ester as work( Energy monomer, is obtained, acrylic acid PolyTHF ester monomer has the Long carbon chain of ehter bond with soft monomer and hard monomer copolymerization, flexible Relatively good, the anti-disconnected glue pressure sensitive adhesive of gained can be good at resisting tension failure, be conducive to preventing the glue during stretch bending Fracture etc., thus the present invention protection film for automobile can be very good apply and automobile adhesive film field.
A kind of protection film for automobile, composition is followed successively by by PVC film, acrylate glue and release liners, it is characterized in that:The acrylic acid Glue is anti-disconnected glue pressure sensitive adhesive, is mainly obtained by soft monomer, hard monomer and function monomer copolymerization, the function monomer is poly- for acrylic acid Tetrahydrofuran ester, its molecular structural formula is:
Wherein n=3~10;
The anti-disconnected glue pressure sensitive adhesive is not broken in the case of stretching 300%, and 180 ° of separation strengths are 2.0~4.0 pounds/ 25mm。
A kind of protection film for automobile as described above, the soft monomer is that ethyl acrylate, butyl acrylate, acrylic acid are different pungent One or more in ester;Described hard monomer is acrylamide.
A kind of preparation method of protection film for automobile, it is characterized in that comprising the following steps:
1) preparation of disconnected glue pressure sensitive adhesive is resisted
A, function monomer acrylic acid PolyTHF ester preparation;
PTMG is dissolved in dichloromethane, is then added drop-wise in propylene isoxazolecarboxylic acid and reacts, generation third Olefin(e) acid PolyTHF ester;
B, anti-disconnected glue pressure sensitive adhesive preparation;
Raw materials by weight portion is calculated as:
By soft monomer and hard monomer dissolving in a solvent, then 1/3rd of mixed solution are added in reactor, is risen Temperature adds initiator, remaining mixed solution is then added dropwise to 70~90 DEG C, the completion of dropping in 2~3h, then starts that work(is added dropwise Energy monomeric acrylic PolyTHF ester, time for adding is 0.5~1h, continues to react after 1~2h, is cooled to room temperature;Add and hand over Join agent stirring, discharging produces anti-disconnected glue pressure sensitive adhesive;
2) preparation of disconnected shellac varnish surface protective film is resisted;
In the anti-disconnected glue pressure sensitive adhesive of PVC film one side coating, drying is finally pressed with release liners.
In a kind of preparation method of protection film for automobile as described above, step a, the equal molecule of number of PTMG Measure as 600~2000;The concentration that PTMG is dissolved in dichloromethane is 20~30wt%;Poly- tetrahydrochysene is barked ether of muttering Glycol is 1~1.3 with the mol ratio of propylene isoxazolecarboxylic acid:1;Reaction temperature is 10~30 DEG C, 2~3h of reaction time, course of reaction The middle hydrogen chloride gas produced with triethylamine during absorbing reaction, triethylamine is 1 with the mol ratio of propylene isoxazolecarboxylic acid:1;Instead Product is answered through extract and separate, vacuum distillation and vacuum drying.
In a kind of preparation method of protection film for automobile as described above, step b, described initiator is azo-bis-isobutyl cyanide Or ABVN;Described crosslinking agent is polyisocyanates;Described solvent is ethyl acetate.
A kind of preparation method of protection film for automobile as described above, it is characterised in that step 2) in, the anti-disconnected glue of coating The amount of pressure sensitive adhesive is 40~60g/m2, drying temperature is 40~120 DEG C, and drying time is 8~12min.
Beneficial effect:
A kind of protection film for automobile and preparation method thereof, protection film for automobile composition is followed successively by by PVC film, acrylate glue and release Paper, acrylate glue is a kind of anti-disconnected glue pressure sensitive adhesive, is using acrylic acid PolyTHF ester as function monomer, with soft monomer and hard list Body copolymerization is obtained, and acrylic acid PolyTHF ester monomer has the Long carbon chain of ehter bond, flexible relatively good, and the anti-disconnected glue laminated of gained is quick Glue can be good at resisting tension failure, be conducive to preventing fracture of glue etc. during stretch bending, thus the vapour of the present invention Car diaphragm can be very good to apply and automobile adhesive film field.
Embodiment
The invention will be further elucidated with reference to specific embodiments.It should be understood that these embodiments are merely to illustrate this hair Bright rather than limitation the scope of the present invention.In addition, it is to be understood that after the content of the invention lectured has been read, art technology Personnel can make various changes or modifications to the present invention, and these equivalent form of values equally fall within the application appended claims and limited Fixed scope.
A kind of protection film for automobile of the present invention, composition is followed successively by by PVC film, acrylate glue and release liners, and acrylate glue is Anti- disconnected glue pressure sensitive adhesive, mainly by one or more of, hard in soft monomer ethyl acrylate, butyl acrylate, Isooctyl acrylate monomer Monomeric acrylamide and function monomer copolymerization and obtain, function monomer is acrylic acid PolyTHF ester, and its molecular structural formula is:
Wherein n=3~10;
Anti- disconnected glue pressure sensitive adhesive is not broken in the case of stretching 300%, and 180 ° of separation strengths are 2.0~4.0 pounds/25mm.
Embodiment 1
A kind of preparation method of protection film for automobile, comprises the following steps:
1) preparation of disconnected glue pressure sensitive adhesive is resisted
A, function monomer acrylic acid PolyTHF ester preparation;
Number-average molecular weight is dissolved in dichloromethane for 600 PTMGs, acrylic acid acyl is then added drop-wise to Reacted in chlorine, the concentration that PTMG is dissolved in dichloromethane is 20wt%;Poly- tetrahydrochysene is barked ether glycol and third of muttering The mol ratio of olefin(e) acid acyl chlorides is 1:1;Reaction temperature is 10 DEG C, reaction time 2h, with triethylamine come absorbing reaction in course of reaction During the hydrogen chloride gas that produces, triethylamine is 1 with the mol ratio of propylene isoxazolecarboxylic acid:1;Reaction product through extract and separate, subtract Pressure distillation and vacuum drying, generate acrylic acid PolyTHF ester, and its molecular structural formula is:
Wherein n=3;
B, anti-disconnected glue pressure sensitive adhesive preparation;
Raw materials by weight portion is calculated as:
Soft monomer ethyl acrylate and hard monomer acrylamide are dissolved in solvent ethyl acetate, then by mixed solution 1/3rd add in reactors, be warming up to 70 DEG C, add initiator azo-bis-isobutyl cyanide, remaining mixing is then added dropwise molten Liquid, the completion of dropping in 2h, then start that function monomer acrylic acid PolyTHF ester is added dropwise, time for adding is 0.5h, continues anti- Answer after 1h, be cooled to room temperature;The stirring of crosslinking agent polyisocyanates is added, discharging produces anti-disconnected glue pressure sensitive adhesive, resists disconnected glue pressure sensitive adhesive It is not broken in the case of stretching 300%, 180 ° of separation strengths are 2.0 pounds/25mm;
2) preparation of protection film for automobile;
In the anti-disconnected glue pressure sensitive adhesive of PVC film one side coating, the amount of the anti-disconnected glue pressure sensitive adhesive of coating is 40g/m2, drying, drying temperature Spend for 40 DEG C, drying time is 8min, is finally pressed with release liners.
Embodiment 2
A kind of preparation method of protection film for automobile, comprises the following steps:
1) preparation of disconnected glue pressure sensitive adhesive is resisted
A, function monomer acrylic acid PolyTHF ester preparation;
Number-average molecular weight is dissolved in dichloromethane for 2000 PTMGs, acrylic acid acyl is then added drop-wise to Reacted in chlorine, the concentration that PTMG is dissolved in dichloromethane is 30wt%;Poly- tetrahydrochysene is barked ether glycol and third of muttering The mol ratio of olefin(e) acid acyl chlorides is 1.3:1;Reaction temperature is 30 DEG C, reaction time 3h, absorbs anti-with triethylamine in course of reaction The hydrogen chloride gas produced during answering, triethylamine is 1 with the mol ratio of propylene isoxazolecarboxylic acid:1;Reaction product through extract and separate, Vacuum distillation and vacuum drying, generate acrylic acid PolyTHF ester, and its molecular structural formula is:
Wherein n=10;
B, anti-disconnected glue pressure sensitive adhesive preparation;
Raw materials by weight portion is calculated as:
Soft monomer butyl acrylate and hard monomer acrylamide are dissolved in solvent ethyl acetate, then by mixed solution 1/3rd add in reactors, be warming up to 90 DEG C, add initiator ABVN, remaining mixing is then added dropwise molten Liquid, the completion of dropping in 3h, then start that function monomer acrylic acid PolyTHF ester is added dropwise, time for adding is 1h, continues to react After 2h, room temperature is cooled to;The stirring of crosslinking agent polyisocyanates is added, discharging produces anti-disconnected glue pressure sensitive adhesive, and anti-disconnected glue pressure sensitive adhesive exists It is not broken in the case of stretching 300%, 180 ° of separation strengths are 4.0 pounds/25mm;
2) preparation of protection film for automobile;
In the anti-disconnected glue pressure sensitive adhesive of PVC film one side coating, the amount of the anti-disconnected glue pressure sensitive adhesive of coating is 60g/m2, drying, drying temperature Spend for 120 DEG C, drying time is 12min, is finally pressed with release liners.
Embodiment 3
A kind of preparation method of protection film for automobile, comprises the following steps:
1) preparation of disconnected glue pressure sensitive adhesive is resisted
A, function monomer acrylic acid PolyTHF ester preparation;
Number-average molecular weight is dissolved in dichloromethane for 1000 PTMGs, acrylic acid acyl is then added drop-wise to Reacted in chlorine, the concentration that PTMG is dissolved in dichloromethane is 25wt%;Poly- tetrahydrochysene is barked ether glycol and third of muttering The mol ratio of olefin(e) acid acyl chlorides is 1.1:1;Reaction temperature is 20 DEG C, reaction time 2.5h, is absorbed in course of reaction with triethylamine The hydrogen chloride gas produced in course of reaction, triethylamine is 1 with the mol ratio of propylene isoxazolecarboxylic acid:1;Reaction product is through extraction point From, vacuum distillation and vacuum drying, acrylic acid PolyTHF ester is generated, its molecular structural formula is:
Wherein n=4;
B, anti-disconnected glue pressure sensitive adhesive preparation;
Raw materials by weight portion is calculated as:
Soft monomer Isooctyl acrylate monomer and hard monomer acrylamide are dissolved in solvent ethyl acetate, then will mix molten / 3rd of liquid are added in reactor, are warming up to 75 DEG C, add initiator azo-bis-isobutyl cyanide, remaining mixing is then added dropwise Solution, the completion of dropping in 2.5h, then start that function monomer acrylic acid PolyTHF ester is added dropwise, time for adding is 0.6h, after After continuous reaction 1.5h, room temperature is cooled to;The stirring of crosslinking agent polyisocyanates is added, discharging produces anti-disconnected glue pressure sensitive adhesive, resists disconnected glue Pressure sensitive adhesive is not broken in the case of stretching 300%, and 180 ° of separation strengths are 2.5 pounds/25mm;
2) preparation of protection film for automobile;
In the anti-disconnected glue pressure sensitive adhesive of PVC film one side coating, the amount of the anti-disconnected glue pressure sensitive adhesive of coating is 45g/m2, drying, drying temperature Spend for 80 DEG C, drying time is 9min, is finally pressed with release liners.
Embodiment 4
A kind of preparation method of protection film for automobile, comprises the following steps:
1) preparation of disconnected glue pressure sensitive adhesive is resisted
A, function monomer acrylic acid PolyTHF ester preparation;
Number-average molecular weight is dissolved in dichloromethane for 1200 PTMGs, acrylic acid acyl is then added drop-wise to Reacted in chlorine, the concentration that PTMG is dissolved in dichloromethane is 22wt%;Poly- tetrahydrochysene is barked ether glycol and third of muttering The mol ratio of olefin(e) acid acyl chlorides is 1.2:1;Reaction temperature is 15 DEG C, reaction time 2.2h, is absorbed in course of reaction with triethylamine The hydrogen chloride gas produced in course of reaction, triethylamine is 1 with the mol ratio of propylene isoxazolecarboxylic acid:1;Reaction product is through extraction point From, vacuum distillation and vacuum drying, acrylic acid PolyTHF ester is generated, its molecular structural formula is:
Wherein n=5;
B, anti-disconnected glue pressure sensitive adhesive preparation;
Raw materials by weight portion is calculated as:
Wherein the mass ratio of ethyl acrylate and butyl acrylate is 1:1;
Soft monomer ethyl acrylate and butyl acrylate and hard monomer acrylamide are dissolved in solvent ethyl acetate, so 1/3rd of mixed solution are added in reactor afterwards, 78 DEG C are warming up to, initiator ABVN is added, is then added dropwise Remaining mixed solution, the completion of dropping in 2h, then start that function monomer acrylic acid PolyTHF ester is added dropwise, time for adding is 0.8h, continues to react after 2h, is cooled to room temperature;The stirring of crosslinking agent polyisocyanates is added, discharging produces anti-disconnected glue pressure sensitive adhesive, Anti- disconnected glue pressure sensitive adhesive is not broken in the case of stretching 300%, and 180 ° of separation strengths are 2.5 pounds/25mm;
2) preparation of protection film for automobile;
In the anti-disconnected glue pressure sensitive adhesive of PVC film one side coating, the amount of the anti-disconnected glue pressure sensitive adhesive of coating is 42g/m2, drying, drying temperature Spend for 100 DEG C, drying time is 10min, is finally pressed with release liners.
Embodiment 5
A kind of preparation method of protection film for automobile, comprises the following steps:
1) preparation of disconnected glue pressure sensitive adhesive is resisted
A, function monomer acrylic acid PolyTHF ester preparation;
Number-average molecular weight is dissolved in dichloromethane for 1100 PTMGs, acrylic acid acyl is then added drop-wise to Reacted in chlorine, the concentration that PTMG is dissolved in dichloromethane is 26wt%;Poly- tetrahydrochysene is barked ether glycol and third of muttering The mol ratio of olefin(e) acid acyl chlorides is 1:1;Reaction temperature is 30 DEG C, reaction time 2h, with triethylamine come absorbing reaction in course of reaction During the hydrogen chloride gas that produces, triethylamine is 1 with the mol ratio of propylene isoxazolecarboxylic acid:1;Reaction product through extract and separate, subtract Pressure distillation and vacuum drying, generate acrylic acid PolyTHF ester, and its molecular structural formula is:
Wherein n=6;
B, anti-disconnected glue pressure sensitive adhesive preparation;
Raw materials by weight portion is calculated as:
Wherein the mass ratio of ethyl acrylate, butyl acrylate and Isooctyl acrylate monomer is 2:1:1;
Soft monomer ethyl acrylate, butyl acrylate and Isooctyl acrylate monomer and hard monomer acrylamide are dissolved in solvent In ethyl acetate, then 1/3rd of mixed solution are added in reactor, 75 DEG C are warming up to, initiator azo two is added different Heptonitrile, is then added dropwise remaining mixed solution, the completion of dropping in 2h, then starts that function monomer acrylic acid PolyTHF is added dropwise Ester, time for adding is 1h, continues to react after 2h, is cooled to room temperature;The stirring of crosslinking agent polyisocyanates is added, discharging is produced anti- Disconnected glue pressure sensitive adhesive, anti-disconnected glue pressure sensitive adhesive is not broken in the case of stretching 300%, and 180 ° of separation strengths are 2.8 pounds/25mm;
2) preparation of protection film for automobile;
In the anti-disconnected glue pressure sensitive adhesive of PVC film one side coating, the amount of the anti-disconnected glue pressure sensitive adhesive of coating is 50g/m2, drying, drying temperature Spend for 90 DEG C, drying time is 8min, is finally pressed with release liners.
Embodiment 6
A kind of preparation method of protection film for automobile, comprises the following steps:
1) preparation of disconnected glue pressure sensitive adhesive is resisted
A, function monomer acrylic acid PolyTHF ester preparation;
Number-average molecular weight is dissolved in dichloromethane for 1800 PTMGs, acrylic acid acyl is then added drop-wise to Reacted in chlorine, the concentration that PTMG is dissolved in dichloromethane is 26wt%;Poly- tetrahydrochysene is barked ether glycol and third of muttering The mol ratio of olefin(e) acid acyl chlorides is 1.1:1;Reaction temperature is 10 DEG C, reaction time 3h, absorbs anti-with triethylamine in course of reaction The hydrogen chloride gas produced during answering, triethylamine is 1 with the mol ratio of propylene isoxazolecarboxylic acid:1;Reaction product through extract and separate, Vacuum distillation and vacuum drying, generate acrylic acid PolyTHF ester, and its molecular structural formula is:
Wherein n=8;
B, anti-disconnected glue pressure sensitive adhesive preparation;
Raw materials by weight portion is calculated as:
Wherein the mass ratio of butyl acrylate and Isooctyl acrylate monomer is 1:2;
Soft monomer butyl acrylate and Isooctyl acrylate monomer and hard monomer acrylamide are dissolved in solvent ethyl acetate, Then 1/3rd of mixed solution are added in reactor, is warming up to 88 DEG C, added initiator azo-bis-isobutyl cyanide, then drip Plus remaining mixed solution, the completion of dropping in 2.8h, then start that function monomer acrylic acid PolyTHF ester is added dropwise, during dropwise addition Between be 0.8h, continue react 1h after, be cooled to room temperature;The stirring of crosslinking agent polyisocyanates is added, discharging produces anti-disconnected glue laminated quick Glue, anti-disconnected glue pressure sensitive adhesive is not broken in the case of stretching 300%, and 180 ° of separation strengths are 4.0 pounds/25mm;
2) preparation of protection film for automobile;
In the anti-disconnected glue pressure sensitive adhesive of PVC film one side coating, the amount of the anti-disconnected glue pressure sensitive adhesive of coating is 60g/m2, drying, drying temperature Spend for 110 DEG C, drying time is 11min, is finally pressed with release liners.

Claims (6)

1. a kind of protection film for automobile, composition is followed successively by by PVC film, acrylate glue and release liners, it is characterized in that:The acrylate glue For anti-disconnected glue pressure sensitive adhesive, mainly obtained by soft monomer, hard monomer and function monomer copolymerization, the function monomer is acrylic acid poly- four Hydrogen furans ester, its molecular structural formula is:
Wherein n=3~10;
The anti-disconnected glue pressure sensitive adhesive is not broken in the case of stretching 300%, and 180 ° of separation strengths are 2.0~4.0 pounds/25mm;
The preparing raw material of the anti-disconnected glue pressure sensitive adhesive is calculated by weight as:
2. a kind of protection film for automobile according to claim 1, it is characterised in that the soft monomer is ethyl acrylate, third One or more in olefin(e) acid butyl ester, Isooctyl acrylate monomer;Described hard monomer is acrylamide.
3. a kind of preparation method of protection film for automobile as claimed in claim 1 or 2, it is characterized in that comprising the following steps:
1) preparation of disconnected glue pressure sensitive adhesive is resisted
A, function monomer acrylic acid PolyTHF ester preparation;
PTMG is dissolved in dichloromethane, is then added drop-wise in acryloyl chloride and reacts, generation acrylic acid gathers Tetrahydrofuran ester;
B, anti-disconnected glue pressure sensitive adhesive preparation;
By soft monomer and hard monomer dissolving in a solvent, then 1/3rd of mixed solution are added in reactor, is warming up to 70~90 DEG C, initiator is added, remaining mixed solution is then added dropwise, the completion of dropping in 2~3h, then start that function list is added dropwise Body acrylic acid PolyTHF ester, time for adding is 0.5~1h, continues to react after 1~2h, is cooled to room temperature;Add crosslinking agent Stirring, discharging produces anti-disconnected glue pressure sensitive adhesive;
2) preparation of protection film for automobile;
In the anti-disconnected glue pressure sensitive adhesive of PVC film one side coating, drying is finally pressed with release liners.
4. the preparation method of a kind of protection film for automobile according to claim 3, it is characterised in that in step a, poly- tetrahydrochysene furan Mutter ether glycol number-average molecular weight be 600~2000;PTMG be dissolved in concentration in dichloromethane for 20~ 30wt%;The mol ratio of PTMG and acryloyl chloride is 1~1.3:1;Reaction temperature is 10~30 DEG C, during reaction Between 2~3h, the hydrogen chloride gas produced with triethylamine during absorbing reaction in course of reaction, triethylamine and acryloyl chloride Mol ratio is 1:1;Reaction product is through extract and separate, vacuum distillation and vacuum drying.
5. the preparation method of a kind of protection film for automobile according to claim 3, it is characterised in that in step b, described draws It is azodiisobutyronitrile or ABVN to send out agent;Described crosslinking agent is polyisocyanates;Described solvent is acetic acid second Ester.
6. a kind of preparation method of protection film for automobile according to claim 3, it is characterised in that step 2) in, it is described to apply The amount for covering anti-disconnected glue pressure sensitive adhesive is 40~60g/m2, drying temperature is 40~120 DEG C, and drying time is 8~12min.
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CN106381085A (en) * 2016-11-04 2017-02-08 太仓金煜电子材料有限公司 Polyvinyl chloride protection film and production method thereof
CN111992477A (en) * 2020-08-06 2020-11-27 东风汽车集团有限公司 Method for manufacturing automobile logo
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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