CN116285720A - Low-temperature cured silica gel protective film - Google Patents

Abstract

The invention discloses a low-temperature curing silica gel protective film, which comprises a substrate layer, an adhesive layer and a release layer arranged in sequence. The adhesive layer is obtained by baking and curing a silicone pressure-sensitive adhesive. The sensitive adhesive is obtained by stirring the following components in a reactor: 100 parts of A component, 80~120 parts of B component, 1~1.8 parts of silane coupling agent, 1.5~2.2 parts of Pt catalyst, 2-methyl- 3-8 parts of 3-butyne-2-alcohol, 75-150 parts of dilution solvent; the composition of the A component is: vinyl polysiloxane, hydrogen-containing polysiloxane and 3-chloropropyl triethyl Oxysilane, the components of the B component are: the reaction product of sodium silicate, chlorotrimethylsilane and isopropanol, hydrogen-containing polysiloxane, and tetramethyldivinyldisiloxane. The curing time of the silicone pressure-sensitive adhesive in the low-temperature curing silicone protective film of the present invention is reduced to less than 25 minutes at 50° C., which improves the production and rapid winding efficiency of the protective film.

Description

Low temperature curing silicone protective film

technical field

The invention relates to the technical field of silica gel protective films, in particular to a low-temperature curing silica gel protective film.

Background technique

Silicone protective film is a screen protective film mainly used to protect electronic products. Now the mainstream silicone protective film is PET silicone screen protective film. With the rapid development of electronic manufacturing technology, many manufacturing processes require protective films, such as: mobile phones , computers and various screen monitors, etc. The existing silicone protective film is limited by the curing time of the adhesive layer, and the winding time is relatively long, which is not conducive to improving production efficiency.

Contents of the invention

The technical problem to be solved by the present invention is to provide a low-temperature curing silica gel protective film, the curing time of the silicone pressure-sensitive adhesive in the low-temperature curing silica gel protective film is reduced to less than 25 minutes at 50°C, which improves the rapid yield of the protective film production. volume efficiency.

In order to achieve the above object, the technical solution adopted in the present invention is: a low-temperature curing silicone protective film, including a substrate layer, an adhesive layer and a release layer arranged in sequence, and the adhesive layer is made of silicone pressure-sensitive adhesive The adhesive is baked and cured. This silicone pressure-sensitive adhesive is obtained by stirring the following components in a reactor:

A component 100 parts,

B component 80~120 parts,

Silane coupling agent 1~1.8 parts,

1.5~2.2 parts of Pt catalyst,

2-methyl-3-butyn-2-ol 3~8 parts,

Dilute solvent 75~150 parts;

The composition of the A component is: 43-50 parts of vinyl polysiloxane, 13-20 parts of hydrogen-containing polysiloxane and 2-6 parts of 3-chloropropyltriethoxysilane,

The components of the B component are: 31-38 parts of the reaction product of sodium silicate, chlorotrimethylsilane and isopropanol, 20-34 parts of hydrogen-containing polysiloxane, tetramethyldivinyldisiloxane 1~8 parts of alkane.

The technical scheme further improved in the above-mentioned technical scheme is as follows:

1. In the above scheme, the viscosity of the component A at 25°C is 10000-50000mpa.s, and the content of non-volatile substances is 55%-65%.

2. In the above scheme, the viscosity of component B at 25°C is 5000-20000mpa.s, and the content of non-volatile substances is 55%-65%.

3. In the above solution, the platinum content in the Pt catalyst is 3000ppm-4000ppm; the platinum catalyst is a platinum catalyst coordinated with methylvinylsiloxane.

4. In the above scheme, the Pt catalyst is the use of siloxane oligomers containing long-chain alkyl and vinyl groups to carry out coordination exchange on the Karst catalyst to form platinum-a,w-bis(n-octyl base) catalyst for polymethylvinylsiloxane complexes.

5. In the above scheme, the solvent is a mixture of one or more of toluene, xylene, and ethyl acetate.

6. In the above solution, the silane coupling agent is r-glycidoxypropyltrimethoxysilane or r-methacryloxypropyltrimethoxysilane.

Due to the application of the above-mentioned technical solution, the present invention has the following advantages compared with the prior art:

The low-temperature curing silica gel protective film of the present invention is based on 3 to 8 parts of 2-methyl-3-butyn-2-ol, and the A component of the two-component contains 3-chloropropyltriethoxysilane, so that the silicone The curing time of the pressure-sensitive adhesive is reduced to less than 25 minutes at 50°C, which improves the efficiency of rapid winding in the production of protective films.

Description of drawings

Accompanying drawing 1 is the structure schematic diagram of low-temperature curing silica gel protective film of the present invention.

In the above drawings: 1. Substrate layer; 2. Adhesive layer; 3. Release layer.

Implementation

In the description of the present invention, it should be noted that the terms "center", "upper", "lower", "left", "right", "vertical", "horizontal", "inner", "outer" etc. The indicated orientation or positional relationship is based on the illustrated orientation or positional relationship, and is only for the convenience of describing the present invention and simplifying the description, rather than indicating or implying that the referred device or element must have a specific orientation, be configured in a specific orientation, and operations, and therefore cannot be construed as limiting the present invention; the terms "first", "second", and "third" are used for descriptive purposes only, and cannot be construed as indicating or implying relative importance; in addition, unless otherwise expressly Provisions and limitations, the terms "installation", "connection" and "connection" should be understood in a broad sense, for example, it can be a fixed connection, a detachable connection, or an integral connection; it can be a mechanical connection or an electrical connection ; It can be directly connected, or indirectly connected through an intermediary, and can be internally connected between two components. Those of ordinary skill in the art can understand the specific meanings of the above terms in the present invention in specific situations.

The present invention will be further described below in conjunction with embodiment:

Embodiments 1-4: A low-temperature curing silicone protective film, including a substrate layer, an adhesive layer and a release layer arranged in sequence, the adhesive layer is obtained by baking and curing a silicone pressure-sensitive adhesive, This silicone pressure-sensitive adhesive is obtained by stirring the following components in a reaction kettle, as described in Table 1:

Table 1

components Example 1 Example 2 Example 3 Example 4 A component 100 copies 100 copies 100 copies 100 copies B component 100 copies 85 copies 115 copies 105 copies A silane coupling agent 1 copy 1.5 servings 1.2 parts 1.5 servings Pt catalyst 2 copies 1.5 servings 2 copies 1.5 servings 2-Methyl-3-butyn-2-ol 4 parts 6 servings 4 parts 7 copies dilution solvent 100 copies 125 copies 100 copies 125 copies

;

The composition of above-mentioned A component, as described in table 2:

Table 2

components Example 1 Example 2 Example 3 Example 4 Vinyl polysiloxane 45 copies 50 copies 45 copies 50 copies Hydrogen polysiloxane 15 copies 18 copies 15 copies 18 copies 3-Chloropropyltriethoxysilane 3 copies 5 copies 3 copies 5 copies

;

The composition of above-mentioned B component, as described in table 3:

table 3

components Example 1 Example 2 Example 3 Example 4 Reaction product of sodium silicate with chlorotrimethylsilane and isopropanol 35 copies 32 copies 35 copies 32 copies Hydrogen polysiloxane 25 copies 30 copies 25 copies 30 copies Tetramethyldivinyldisiloxane 4 parts 6 servings 3 copies 6 servings

In Example 1, the viscosity of component A at 25°C is 10000-50000mpa.s, and the content of non-volatile substances is 55%-65%; the viscosity of component B at 25°C is 5000-20000mpa.s, and the content of non-volatile substances is 55%~65%; the platinum content in the Pt catalyst is 3000ppm~4000ppm; the platinum catalyst is a platinum catalyst coordinated with methylvinylsiloxane; the solvent is toluene and xylene mixed in a weight ratio of 1:1, the above The silane coupling agent is r-glycidyl etheroxypropyltrimethoxysilane.

In Example 2, the viscosity of component A at 25°C is 10000-50000mpa.s, and the content of non-volatile substances is 55%-65%; the viscosity of component B at 25°C is 5000-20000mpa.s, and the content of non-volatile substances is 55%~65%; Pt catalyst is the use of siloxane oligomers containing long-chain alkyl and vinyl groups to perform coordination exchange on Karlster catalysts to form platinum-a,w-bis(n-octyl) Catalyst for polymethylvinylsiloxane complex; the above solvent is mixed with toluene and ethyl acetate at a weight ratio of 1:2, and the above silane coupling agent is r-methacryloxypropyltrimethoxysilane.

In Example 3, the viscosity of component A at 25°C is 10000-50000mpa.s, and the content of non-volatile substances is 55%-65%; the viscosity of component B at 25°C is 5000-20000mpa.s, and the content of non-volatile substances is 55%~65%; the platinum content in the Pt catalyst is 3000ppm~4000ppm; the platinum catalyst is a platinum catalyst coordinated with methylvinylsiloxane; the solvent is toluene and xylene mixed in a weight ratio of 1:1, the above The silane coupling agent is r-glycidyl etheroxypropyltrimethoxysilane.

In Example 4, the viscosity of component A at 25°C is 10000-50000mpa.s, and the content of non-volatile substances is 55%-65%; the viscosity of component B at 25°C is 5000-20000mpa.s, and the content of non-volatile substances is 55%~65%; Pt catalyst is the use of siloxane oligomers containing long-chain alkyl and vinyl groups to perform coordination exchange on Karlster catalysts to form platinum-a,w-bis(n-octyl) Catalyst for polymethylvinylsiloxane complexes; the above-mentioned solvent is mixed with toluene and ethyl acetate at a weight ratio of 1:2, and the above-mentioned silane coupling agent is r-methacryloxypropyltrimethoxysilane .

A preparation method for the above-mentioned low-temperature curing silica gel protective film, comprising the following steps:

Step 1. Add the dilution solvent, component A and component B raw materials into the reaction kettle, and stir at room temperature to obtain a dispersion;

Step 2, adding silane coupling agent, Pt catalyst and 2-methyl-3-butyn-2-ol in sequence while stirring the dispersion, and mixing evenly to obtain a silicone pressure-sensitive adhesive;

Step 3: Coating the silicone pressure-sensitive adhesive on the base material, coating the pressure-sensitive adhesive on the surface of the base material by a tape coater, and curing the adhesive layer in an oven at a low temperature of 50°C after the coating is completed ;

Step 4: Paste a release film on the adhesive layer to prepare the low-temperature curing silicone protective film

The stirring time in the above step 1 is 1 hour.

Comparative Examples 1-3: A silicone protective film, including a substrate layer, an adhesive layer and a release layer arranged in sequence, the adhesive layer is obtained by baking and curing a silicone pressure-sensitive adhesive, the organic The silicone pressure-sensitive adhesive is obtained by stirring the following components in a reactor, as described in Table 4:

Table 4

components Comparative example 1 Comparative example 2 Comparative example 3 A component 100 copies 100 copies 100 copies B component 100 copies 85 copies 100 copies A silane coupling agent 1 copy 1.5 servings 1 copy Pt catalyst 2 copies 1.5 servings 2 copies 2-Methyl-3-butyn-2-ol - - 4 parts dilution solvent 100 copies 125 copies 100 copies

;

The composition of above-mentioned A component, as described in table 2:

table 5

components Comparative example 1 Comparative example 2 Comparative example 3 Vinyl polysiloxane 45 copies 50 copies 45 copies Hydrogen polysiloxane 15 copies 18 copies 15 copies 3-Chloropropyltriethoxysilane 3 copies - -

;

The composition of above-mentioned B component, as described in table 3:

Table 6

components Comparative example 1 Comparative example 2 Comparative example 3 Reaction product of sodium silicate with chlorotrimethylsilane and isopropanol 35 copies 32 copies 35 copies Hydrogen polysiloxane 25 copies 30 copies 25 copies Tetramethyldivinyldisiloxane 4 parts 6 servings 4 parts

In Comparative Example 1 and Comparative Example 3, the viscosity of component A at 25°C is 10000-50000mpa.s, and the content of non-volatile substances is 55%-65%; the viscosity of component B at 25°C is 5000-20000mpa.s, and the content of non-volatile The content of the active substance is 55%~65%; the platinum content in the Pt catalyst is 3000ppm~4000ppm; the platinum catalyst is a platinum catalyst coordinated with methylvinylsiloxane; the solvent is toluene and xylene according to the weight ratio of 1: 1 mixing, the above-mentioned silane coupling agent is r-glycidyl etheroxypropyl trimethoxysilane.

In Comparative Example 2, the viscosity of component A at 25°C is 10000-50000mpa.s, and the content of non-volatile substances is 55%-65%; the viscosity of component B at 25°C is 5000-20000mpa.s, and the content of non-volatile substances is 55%~65%; Pt catalyst is the use of siloxane oligomers containing long-chain alkyl and vinyl groups to perform coordination exchange on Karlster catalysts to form platinum-a,w-bis(n-octyl) Catalyst for polymethylvinylsiloxane complexes; the above-mentioned solvent is mixed with toluene and ethyl acetate at a weight ratio of 1:2, and the above-mentioned silane coupling agent is r-methacryloxypropyltrimethoxysilane .

The preparation method of the comparative example is the same as that of the embodiment.

For the silicone protective film obtained in the above-mentioned Examples 1-4 and Comparative Examples 1-3, the silicone pressure-sensitive adhesive in the silicone protective film was searched for the curing time at 50°C, and the test results were as follows:

Table 7

Test items Example 1 Example 2 Example 3 Example 4 Comparative example 1 Comparative example 2 Comparative example 3 Curing time at 50°C/min twenty two twenty four twenty one twenty three 35 41 32

;

As shown in the evaluation results in Table 7, the silicone pressure-sensitive adhesives in the silicone protective films of Examples 1 to 4 of the present invention have a curing time of 22 minutes, 24 minutes, 21 minutes, and 23 minutes at 50°C. The curing times of proportions 1 to 3 were 35 minutes, 41 minutes and 32 minutes respectively; the curing time of the silicone pressure-sensitive adhesive of the embodiment of the present invention was lower than that of the comparative example at 50°C.

The above-mentioned embodiments are only to illustrate the technical concept and characteristics of the present invention, and the purpose is to enable those skilled in the art to understand the content of the present invention and implement it accordingly, and not to limit the protection scope of the present invention. All equivalent changes or modifications made according to the spirit of the present invention shall fall within the protection scope of the present invention.

Claims (7)

1. A low-temperature curing silicone protective film, comprising a substrate layer (1), an adhesive layer (2) and a release layer (3) arranged in sequence, characterized in that: the adhesive layer (2) consists of The silicone pressure-sensitive adhesive is obtained by baking and curing. The silicone pressure-sensitive adhesive is obtained by stirring the following components in a reactor: A component 100 parts, B component 80~120 parts, Silane coupling agent 1~1.8 parts, 1.5~2.2 parts of Pt catalyst, 2-methyl-3-butyn-2-ol 3~8 parts, Dilute solvent 75~150 parts; The composition of the A component is: 43-50 parts of vinyl polysiloxane, 13-20 parts of hydrogen-containing polysiloxane and 2-6 parts of 3-chloropropyltriethoxysilane, The components of the B component are: 31-38 parts of the reaction product of sodium silicate, chlorotrimethylsilane and isopropanol, 20-34 parts of hydrogen-containing polysiloxane, tetramethyldivinyldisiloxane 1~8 parts of alkane. 2. The low-temperature curing silica gel protective film according to claim 1, characterized in that: the viscosity of the component A at 25°C is 10000-50000mpa.s, and the content of non-volatile substances is 55%-65%. 3. The low-temperature curing silicone protective film according to claim 1, characterized in that: the viscosity of the B component at 25°C is 5000-20000mpa.s, and the content of non-volatile substances is 55%-65%. 4. The low-temperature curing silica gel protective film according to claim 1, characterized in that: the platinum content in the Pt catalyst is 3000ppm-4000ppm; the platinum catalyst is a platinum catalyst coordinated with methylvinylsiloxane. 5. The low-temperature curing silica gel protective film according to claim 1, characterized in that: the Pt catalyst utilizes the siloxane oligomers containing long-chain alkyl and vinyl groups to carry out coordination exchange to the Carlster catalyst, Catalyst for platinum-a,w-bis(n-octyl)polymethylvinylsiloxane complexes. 6. The low-temperature curing silica gel protective film according to claim 1, characterized in that: the solvent is a mixture of one or more of toluene, xylene, and ethyl acetate. 7. The low-temperature curing silica gel protective film according to claim 1, characterized in that: the silane coupling agent is r-glycidyl etheroxypropyl trimethoxysilane or r-methacryloxypropyl trimethoxysilane Oxysilane.

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