CN115637116A - High-temperature-resistant low-climbing protective film and preparation method thereof - Google Patents
High-temperature-resistant low-climbing protective film and preparation method thereof Download PDFInfo
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Abstract
The invention provides a high-temperature-resistant low-climbing protection film which comprises a base material layer, an adhesive layer and a release layer which are sequentially attached; the adhesive layer comprises an acrylic resin polymer, and the molecular weight of the acrylic resin polymer is between 50 and 70 ten thousand. The invention also provides a preparation method of the high-temperature-resistant low-climbing protective film. By adopting the acrylic resin polymer with larger molecular weight, the overall crosslinking density of the adhesive layer is improved, and thus the overall strength and modulus of the adhesive layer are improved.
Description
Technical Field
The invention relates to the field of protective films, in particular to a high-temperature-resistant low-climbing protective film and a preparation method thereof.
Background
When tiny components such as wafers are ground, various silicon wafers, packaging substrates, ceramics, glass, crystal fine electronic parts, glass, metal plates and the like are processed, a protective film is generally required to be adopted for fixing, and damage caused by component movement in a cutting process is avoided. In addition, when the local surface of a certain component needs to be polished in the etching, washing or coating process, in order to protect other parts which do not need to be processed from being influenced, the parts which do not need to be processed are firstly covered by the protective film, and then stripped after the processing is finished. However, the adhesive tape for fixing or covering 24288is high in adhesive strength, high in stripping force during processing, and acid-base etching and cleaning processes and high-temperature processes, so that a novel high-temperature-resistant low-climbing protective film needs to be designed to meet the requirements of high temperature resistance, low climbing and good adhesion on products.
Disclosure of Invention
In order to overcome the defects of the prior art, the first purpose of the invention is to provide a high-temperature-resistant low-climbing protection film, which comprises a base material layer, an adhesive layer and a release layer which are sequentially attached; the glue layer comprises an acrylic polymer, and the molecular weight of the acrylic polymer is between 50 and 70 ten thousand.
Preferably, the acrylic resin polymer comprises, in parts by weight:
preferably, the acrylic resin polymer comprises, in parts by weight:
preferably, the thickness of the substrate layer is 25-100 μm.
Preferably, the thickness of the release layer is 25-50 μm.
Preferably, the thickness of the glue layer is 20-50 μm.
Preferably, the thickness of the glue layer is 30 μm.
The second purpose of the invention is to provide a preparation method of the high temperature resistant low-climbing protection film, which comprises the following steps:
the method comprises the following steps: uniformly mixing isooctyl acrylate, n-butyl acrylate, methyl methacrylate, hydroxyethyl acrylate, glycidyl acrylate, acryloyl morpholine, an initiator and a solvent into a reaction kettle, heating and stirring at 66-67 ℃, cooling after 6h, and pouring out to obtain an acrylic resin polymer;
step two: adding an acrylic resin polymer, a curing agent and a solvent into a stirring barrel, and stirring at the speed of 500r/min for 20min to obtain an acrylic resin mixture;
step three: and coating the acrylic resin mixture on the substrate layer by adopting a coating device to form dry glue, coating a release layer, and baking for two days at 55 ℃ to obtain the high-temperature-resistant low-climbing protective film.
Preferably, in the third step, the thickness of the dry glue is controlled to be 20-50 μm.
Compared with the prior art, the invention has the beneficial effects that: the invention provides a high-temperature-resistant low-climbing protection film which comprises a base material layer, an adhesive layer and a release layer which are sequentially attached; the glue layer comprises an acrylic polymer, and the molecular weight of the acrylic polymer is between 50 and 70 ten thousand. The invention also provides a preparation method of the high-temperature-resistant low-climbing protective film. The invention adopts the acrylic resin polymer with larger molecular weight, and improves the overall crosslinking density of the adhesive layer, thereby improving the overall strength and modulus of the adhesive layer. At 60 ℃, the adhesive can still keep higher viscosity, so that acid and alkali liquid cannot permeate the surface of the base material, the adhesive layer structure cannot be damaged after baking at 200 ℃, and the peeling force cannot be increased too much and is still easier to peel after the adhesive layer structure is restored to normal temperature.
The foregoing description is only an overview of the technical solutions of the present invention, and in order to make the technical means of the present invention more clearly understood and to be implemented in accordance with the content of the description, the following detailed description of the preferred embodiments of the present invention is given. Specific embodiments of the present invention are given in detail by the following examples.
Detailed Description
The present invention is further described below with reference to specific embodiments, and it should be noted that, without conflict, any combination between the embodiments or technical features described below may form a new embodiment.
In the practical application process of the protective film, the following problems can occur: (1) When the temperature is high, the adhesive layer becomes soft and the fluidity is enhanced, so that the bonding strength between the adhesive layer and the attached object is reduced, and acid-base liquid can permeate into the surface of the attached object to corrode the attached object; (2) After high-temperature heating, the cohesion of the adhesive layer is damaged, and after the adhesive layer is recovered to normal temperature, the viscosity is increased more, and the residual adhesive is on the surface of an object to be pasted when the film is torn. In order to overcome the defects of the existing protective film, the acrylic resin polymer with larger molecular weight is adopted, and the overall crosslinking density of the adhesive layer is improved, so that the overall strength and modulus of the adhesive layer are improved; the high-temperature-resistant low-climbing protective film comprises a base material layer, an adhesive layer and a release layer which are sequentially attached; the glue layer comprises an acrylic polymer, and the molecular weight of the acrylic polymer is between 50 and 70 ten thousand. The protective film can still maintain higher stripping force at 60 ℃, and acid-base liquid cannot permeate to the surface of the base material; after the baking at the temperature of 200 ℃, the adhesive layer structure of the protective film cannot be damaged, and after the normal temperature is recovered, the peeling force cannot be increased too much and is still easy to peel.
In some embodiments, the acrylic polymer comprises, in parts by weight:
in some embodiments, the acrylic polymer comprises, in parts by weight:
in some embodiments, the substrate layer is made of a PET material and has a thickness of 25-100 μm. Preferably, the thickness of the base material layer is 50 μm, so that the stiffness of the protective film is moderate, and the protective film is convenient to use in a fitting manner.
In some embodiments, the release layer is a release film, and the thickness of the release layer is 25-50 μm. Preferably, the thickness of the release layer is 50 μm, so that the thickness of the release film is moderate and the application range is wider.
The adhesive layer is made by coating acrylic resin polymer, curing agent and solvent on the surface of the substrate layer, and in some embodiments, the thickness of the adhesive layer is 20-50 μm.
In some embodiments, the thickness of the glue layer is 30 μm in order to ensure the overall properties of the finally obtained protective film.
The invention also relates to a preparation method of the high-temperature-resistant low-climbing protection film, which comprises the following steps:
the method comprises the following steps: uniformly mixing isooctyl acrylate, n-butyl acrylate, methyl methacrylate, hydroxyethyl acrylate, glycidyl acrylate, acryloyl morpholine, an initiator and a solvent into a reaction kettle, heating and stirring at 66-67 ℃, cooling after 6h, and pouring out to obtain an acrylic resin polymer;
step two: adding an acrylic resin polymer, a curing agent and a solvent into a stirring barrel, and stirring at the speed of 500r/min for 20min to obtain an acrylic resin mixture;
step three: and coating the acrylic resin mixture on the substrate layer by adopting a coating device to form dry glue, coating a release layer, and baking for two days at 55 ℃ to obtain the high-temperature-resistant low-climbing protective film.
In order to ensure that the finally formed protective film has better high temperature resistance and low climbing performance, in some embodiments, in the third step, the thickness of the dry glue is controlled to be 20-50 μm.
Example one
A high-temperature-resistant low-climbing protection film comprises a base material layer, an adhesive layer and a release layer which are sequentially attached; the adhesive layer comprises an acrylic resin polymer, a curing agent and a solvent, and the adhesive layer comprises the following components in parts by weight: 50 parts of acrylic resin polymer, 2 parts of curing agent and 30 parts of solvent; the thickness of the base material layer is 50 μm, the thickness of the release film layer is 50 μm, and the thickness of the glue layer is 30 μm. The acrylic resin polymer is a copolymer formed by free radical polymerization of 40 parts of isooctyl acrylate, 20 parts of n-butyl acrylate, 10 parts of methyl methacrylate, 10 parts of hydroxyethyl acrylate, 1 part of glycidyl acrylate, 1 part of acryloyl morpholine, 1 part of initiator AIBN and 30 parts of solvent.
A preparation method of a high-temperature-resistant low-climbing protective film comprises the following steps:
the method comprises the following steps: uniformly mixing isooctyl acrylate, n-butyl acrylate, methyl methacrylate, hydroxyethyl acrylate, glycidyl acrylate, acryloyl morpholine, an initiator AIBN and a solvent into a reaction kettle, heating and stirring at 66-67 ℃, cooling after 6h, and pouring out to obtain an acrylic resin polymer;
step two: mixing acrylic resin polymer, curing agent and solvent, and stirring at 500r/min for 20min to obtain a glue layer mixture;
step three: and coating the adhesive layer mixture on the substrate layer by adopting a coating device, controlling the thickness of the dry adhesive to be 30 mu m, covering a release film, and baking at 55 ℃ for two days to obtain the high-temperature-resistant low-climbing protective film.
Wherein the curing agent is toluene diisocyanate, and the solvent is ethyl acetate.
Example two
A high-temperature-resistant low-climbing protection film comprises a base material layer, an adhesive layer and a release layer which are sequentially attached; the adhesive layer comprises an acrylic resin polymer, a curing agent and a solvent, and the adhesive layer comprises the following components in parts by weight: 50 parts of acrylic resin polymer, 2 parts of curing agent and 30 parts of solvent; the thickness of the base material layer is 50 μm, the thickness of the release film layer is 50 μm, and the thickness of the glue layer is 50 μm. The acrylic resin polymer is a copolymer obtained by free radical polymerization of 50 parts of isooctyl acrylate, 10 parts of n-butyl acrylate, 10 parts of methyl methacrylate, 10 parts of hydroxyethyl acrylate, 5 parts of glycidyl acrylate, 5 parts of acryloyl morpholine, 1 part of initiator AIBN and 30 parts of solvent.
A preparation method of a high-temperature-resistant low-climbing protective film comprises the following steps:
the method comprises the following steps: uniformly mixing isooctyl acrylate, n-butyl acrylate, methyl methacrylate, hydroxyethyl acrylate, glycidyl acrylate, acryloyl morpholine, an initiator and a solvent into a reaction kettle, heating and stirring at 66-67 ℃, cooling after 6h, and pouring out to obtain an acrylic resin polymer;
step two: mixing an acrylic resin polymer, a curing agent and a solvent, and stirring at 500r/min for 20min to obtain a glue layer mixture;
step three: and coating the adhesive layer mixture on the substrate layer by adopting a coating device, controlling the thickness of the dry adhesive to be 50 mu m, coating a release film, and baking at 55 ℃ for two days to obtain the high-temperature-resistant low-climbing protective film.
Wherein the curing agent is toluene diisocyanate, and the solvent is ethyl acetate.
EXAMPLE III
A high-temperature-resistant low-climbing protection film comprises a base material layer, an adhesive layer and a release layer which are sequentially attached; the adhesive layer comprises an acrylic resin polymer, a curing agent and a solvent, and the adhesive layer comprises the following components in parts by weight: 20 parts of acrylic resin polymer, 2 parts of curing agent and 30 parts of solvent; the thickness of the base material layer is 50 μm, the thickness of the release film layer is 50 μm, and the thickness of the adhesive layer is 45 μm. Wherein the acrylic resin polymer is a copolymer obtained by free radical polymerization of 20 parts of isooctyl acrylate, 50 parts of n-butyl acrylate, 10 parts of methyl methacrylate, 10 parts of hydroxyethyl acrylate, 3 parts of glycidyl acrylate, 1 part of acryloyl morpholine, 1 part of initiator AIBN and 30 parts of solvent.
A preparation method of a high-temperature-resistant low-climbing protection film comprises the following steps:
the method comprises the following steps: uniformly mixing isooctyl acrylate, n-butyl acrylate, methyl methacrylate, hydroxyethyl acrylate, acrylic acid, an initiator and a solvent into a reaction kettle, heating and stirring at 66-67 ℃, cooling after 6h, and pouring out to obtain an acrylic resin polymer;
step two: mixing an acrylic resin polymer, a curing agent and a solvent, and stirring at 500r/min for 20min to obtain a glue layer mixture;
step three: and coating the adhesive layer mixture on the substrate layer by adopting a coating device, controlling the thickness of the dry adhesive to be 45 mu m, coating a release film, and baking for two days at 55 ℃ to obtain the high-temperature-resistant low-climbing protective film.
Wherein the curing agent is toluene diisocyanate, and the solvent is ethyl acetate.
Example four
A high-temperature-resistant low-climbing protection film comprises a base material layer, an adhesive layer and a release layer which are sequentially attached; the adhesive layer comprises an acrylic resin polymer, a curing agent and a solvent, and the adhesive layer comprises the following components in parts by weight: 50 parts of acrylic resin polymer, 2 parts of curing agent and 30 parts of solvent; the thickness of the base material layer is 50 μm, the thickness of the release film layer is 50 μm, and the thickness of the glue layer is 20 μm. The acrylic resin polymer is a copolymer formed by free radical polymerization of 40 parts of isooctyl acrylate, 20 parts of n-butyl acrylate, 10 parts of methyl methacrylate, 10 parts of hydroxyethyl acrylate, 3 parts of glycidyl acrylate, 1 part of acryloyl morpholine, 1 part of initiator AIBN and 30 parts of solvent.
A preparation method of a high-temperature-resistant low-climbing protective film comprises the following steps:
the method comprises the following steps: uniformly mixing isooctyl acrylate, n-butyl acrylate, methyl methacrylate, hydroxyethyl acrylate, glycidyl acrylate, acryloyl morpholine, an initiator AIBN and a solvent into a reaction kettle, heating and stirring at 66-67 ℃, cooling after 6h, and pouring out to obtain an acrylic resin polymer;
step two: mixing acrylic resin polymer, curing agent and solvent, and stirring at 500r/min for 20min to obtain a glue layer mixture;
step three: and coating the adhesive layer mixture on the substrate layer by adopting a coating device, controlling the thickness of the dry adhesive to be 20 mu m, coating a release film, and baking for two days at 55 ℃ to obtain the high-temperature-resistant low-climbing protective film.
Wherein the curing agent is toluene diisocyanate, and the solvent is ethyl acetate.
Comparative example 1
A high-temperature-resistant low-climbing protection film comprises a base material layer, an adhesive layer and a release layer which are sequentially attached; the adhesive layer comprises an acrylic resin polymer, a curing agent and a solvent, and the adhesive layer comprises the following components in parts by weight: 50 parts of acrylic resin polymer, 2 parts of curing agent and 30 parts of solvent; the thickness of the base material layer is 50 μm, the thickness of the release film layer is 50 μm, and the thickness of the adhesive layer is 20 μm. The acrylic resin polymer is a copolymer formed by free radical polymerization of 40 parts of isooctyl acrylate, 20 parts of n-butyl acrylate, 10 parts of hydroxyethyl acrylate, 1 part of initiator AIBN and 30 parts of solvent.
A preparation method of a high-temperature-resistant low-climbing protective film comprises the following steps:
the method comprises the following steps: uniformly mixing isooctyl acrylate, n-butyl acrylate, an initiator AIBN and a solvent into a reaction kettle, heating and stirring at 66-67 ℃, cooling after 6 hours and pouring out to obtain an acrylic resin polymer;
step two: mixing acrylic resin polymer, curing agent and solvent, and stirring at 500r/min for 20min to obtain a glue layer mixture;
step three: and coating the adhesive layer mixture on the substrate layer by adopting a coating device, controlling the thickness of the dry adhesive to be 20 mu m, covering a release film, and baking at 55 ℃ for two days to obtain the high-temperature-resistant low-climbing protective film.
Wherein the curing agent is toluene diisocyanate, and the solvent is ethyl acetate.
Comparative example No. two
A high-temperature-resistant low-climbing protection film comprises a base material layer, an adhesive layer and a release layer which are sequentially attached; the adhesive layer comprises an acrylic resin polymer, a curing agent and a solvent, and the adhesive layer comprises the following components in parts by weight: 50 parts of acrylic resin polymer, 2 parts of curing agent and 30 parts of solvent; the thickness of the base material layer is 50 μm, the thickness of the release film layer is 50 μm, and the thickness of the adhesive layer is 20 μm. The acrylic resin polymer is a copolymer formed by free radical polymerization of 10 parts of methyl acrylate, 10 parts of methyl methacrylate, 10 parts of hydroxyethyl acrylate, 1 part of acryloyl morpholine, 1 part of initiator AIBN and 30 parts of solvent.
A preparation method of a high-temperature-resistant low-climbing protective film comprises the following steps:
the method comprises the following steps: uniformly mixing methyl acrylate, methyl methacrylate, hydroxyethyl acrylate, glycidyl acrylate, acryloyl morpholine, an initiator AIBN and a solvent into a reaction kettle, heating and stirring at 66-67 ℃, cooling after 6h, and pouring out to obtain an acrylic resin polymer;
step two: mixing acrylic resin polymer, curing agent and solvent, and stirring at 500r/min for 20min to obtain a glue layer mixture;
step three: and coating the adhesive layer mixture on the substrate layer by adopting a coating device, controlling the thickness of the dry adhesive to be 20 mu m, covering a release film, and baking at 55 ℃ for two days to obtain the high-temperature-resistant low-climbing protective film.
Wherein the curing agent is toluene diisocyanate, and the solvent is ethyl acetate.
Comparative example No. three
A high-temperature-resistant low-climbing protection film comprises a base material layer, an adhesive layer and a release layer which are sequentially attached; the adhesive layer comprises an acrylic resin polymer, a curing agent and a solvent, and the adhesive layer comprises the following components in parts by weight: 50 parts of acrylic resin polymer, 2 parts of curing agent and 30 parts of solvent; the thickness of the base material layer is 50 μm, the thickness of the release film layer is 50 μm, and the thickness of the adhesive layer is 30 μm. The acrylic resin polymer is a copolymer formed by free radical polymerization of 40 parts of isooctyl acrylate, 20 parts of n-butyl acrylate, 10 parts of methyl methacrylate, 10 parts of hydroxyethyl acrylate, 1 part of glycidyl acrylate, 1 part of initiator AIBN and 30 parts of solvent.
A preparation method of a high-temperature-resistant low-climbing protection film comprises the following steps:
the method comprises the following steps: uniformly mixing isooctyl acrylate, n-butyl acrylate, methyl methacrylate, hydroxyethyl acrylate, glycidyl acrylate, acryloyl morpholine, an initiator AIBN and a solvent into a reaction kettle, heating and stirring at 66-67 ℃, cooling after 6h, and pouring out to obtain an acrylic resin polymer;
step two: mixing acrylic resin polymer, curing agent and solvent, and stirring at 500r/min for 20min to obtain a glue layer mixture;
step three: and coating the adhesive layer mixture on the substrate layer by adopting a coating device, controlling the thickness of the dry adhesive to be 30 mu m, coating a release film, and baking for two days at 55 ℃ to obtain the high-temperature-resistant low-climbing protective film.
Wherein the curing agent is toluene diisocyanate, and the solvent is ethyl acetate.
The protective films prepared in examples one to four and comparative examples one to three were subjected to performance tests, respectively, to obtain the test results as in table 1 below.
The test method comprises the following steps: the peel force test is carried out according to an ASMTD3330 standard method, and the residual adhesive test method comprises the following steps: cutting the protective film into the size of the mobile phone glass, attaching two surfaces, rolling twice with a 2kg roller, standing for 20min, placing into a high-temperature oven at 200 ℃, taking out after half an hour, standing for 20min, tearing off the protective film, and observing whether the surface of the glass has residual glue by using a strong-light flashlight.
The method for testing the bonding performance comprises the following steps: cutting the protective film into 10-10 cm, tearing off the release film, lightly placing on plain glass, slightly pressing with force, and observing and recording the time (standard is less than or equal to 3 min) for the protective film to completely adhere to the glass surface (no obvious bubbles).
Table 1 table of test results of different examples
While embodiments of the invention have been disclosed above, it is not limited to the applications listed in the description and the embodiments, which are fully applicable in all kinds of fields of adaptation of the invention, and further modifications can be easily implemented by those skilled in the art, so that the invention is not limited to the specific details and the examples shown herein, without departing from the general concept defined by the claims and the scope of equivalents.
Claims (9)
1. The high-temperature-resistant low-climbing protection film is characterized by comprising a base material layer, an adhesive layer and a release layer which are sequentially attached; the glue layer comprises an acrylic polymer, and the molecular weight of the acrylic polymer is between 50 and 70 ten thousand.
2. The high temperature resistant low climb protection film of claim 1, wherein the acrylic polymer comprises in parts by weight:
3. the high temperature resistant low climb protection film of claim 2, wherein the acrylic polymer comprises in parts by weight:
4. the high temperature resistant low climb protection film of claim 1 wherein the substrate layer has a thickness of 25-100 μm.
5. The high temperature resistant low climbing protection film according to claim 1, wherein the thickness of the release layer is 25-50 μm.
6. The high temperature resistant low-climb protection film according to claim 1, wherein the thickness of the glue layer is 20-50 μm.
7. The high temperature resistant low climb protection film of claim 6, wherein the glue layer has a thickness of 30 μm.
8. The preparation method of the high temperature resistant low-climbing protection film according to claim 1, characterized by comprising the following steps:
the method comprises the following steps: uniformly mixing isooctyl acrylate, n-butyl acrylate, methyl methacrylate, hydroxyethyl acrylate, glycidyl acrylate, acryloyl morpholine, an initiator and a solvent into a reaction kettle, heating and stirring at 66-67 ℃, cooling after 6h, and pouring out to obtain an acrylic resin polymer;
step two: adding an acrylic resin polymer, a curing agent and a solvent into a stirring barrel, and stirring at the speed of 500r/min for 20min to obtain an acrylic resin mixture;
step three: and coating the acrylic resin mixture on the substrate layer by adopting a coating device to form dry glue, coating a release layer, and baking for two days at 55 ℃ to obtain the high-temperature-resistant low-climbing protective film.
9. The method for preparing the high temperature resistant and low climbing protection film according to claim 8, wherein in the third step, the thickness of the dry glue is controlled to be 20-50 μm.
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| CN116515415A (en) * | 2023-04-14 | 2023-08-01 | 太仓斯迪克新材料科技有限公司 | High-temperature-resistant ultraviolet visbreaking protective film and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110527453A (en) * | 2019-09-10 | 2019-12-03 | 皇冠（太仓）胶粘制品有限公司 | The bonding sheet based on acrylic acid series copolymer for 5G antenna processing procedure |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110527453A (en) * | 2019-09-10 | 2019-12-03 | 皇冠（太仓）胶粘制品有限公司 | The bonding sheet based on acrylic acid series copolymer for 5G antenna processing procedure |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116515415A (en) * | 2023-04-14 | 2023-08-01 | 太仓斯迪克新材料科技有限公司 | High-temperature-resistant ultraviolet visbreaking protective film and preparation method thereof |
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