CN115305023A - Transparent or semitransparent adhesive film material, preparation method and application thereof - Google Patents

Abstract

The invention provides a method for preparing a transparent or translucent adhesive film material. In the invention, polyorganosiloxane, boron-containing compound, linear silicone oil and auxiliary agents are mixed, reacted, and dried to obtain a transparent or translucent adhesive film. Adhesive film material. When subjected to external impact, it has better energy absorption rate and stress response ability. And when the material is damaged, the damaged part will undergo self-healing repair again through the intermolecular force of the internal structure. At the same time, it can be glued to any substrate without unnecessary trouble. The invention has the advantages of simple preparation process, low cost, readily available raw materials, non-toxic materials, convenient handling and the like. The present invention also provides a transparent or translucent adherent film material and application thereof.

Description

A transparent or translucent adhesive film material, its preparation method and application

technical field

The invention belongs to the technical field of film materials, and in particular relates to a transparent or translucent adhesive film material, its preparation method and application.

Background technique

With the development of science and technology, membrane materials have many uses in various fields such as agriculture, industry, and medicine. For example, in electronic products, film materials are required to have excellent electrical conductivity and light transmittance; in packaging products, film materials are required to have excellent mechanical properties; in some high-temperature application fields, good heat resistance is also required .

However, usually the flexible membrane material is thin and easily damaged by external force. Once damaged, its service life will inevitably be reduced. This situation has led to restrictions on the use of flexible membrane materials in many fields. To solve the problem of service life, fillers are usually added to flexible film materials. The addition of fillers increases the mechanical properties but causes a decrease in light transmittance, which also limits the application of film materials in electronic products. However, separate film materials also need to add adhesives to adhere to the surface substrate during specific applications, which also greatly increases the trouble. Therefore, research on new flexible composite membrane materials is still an important topic in this field.

Contents of the invention

The purpose of the present invention is to provide a transparent or translucent adhesive film material, its preparation method and application. The film material in the present invention has good adhesion and can realize self-healing after being damaged by strong external force , to prolong the service life of the material.

The invention provides a method for preparing a transparent or translucent adhesive film material, comprising the following steps:

A) mixing dihydroxy-terminated polydimethylsiloxane, a boron-containing compound, and tetraisopropyl titanate for reaction to obtain a first reaction solution;

Mixing divinyl-terminated polydimethylsiloxane, linear silicone oil, catalyst and reinforcing filler, and reacting to obtain a second reaction liquid;

mixing isocyanate and hydroxyacrylate to react, and mixing the obtained reactant with an initiator to carry out radical polymerization reaction to obtain a third reaction solution;

B) stirring and mixing the first reaction solution, the second reaction solution and the third reaction solution to obtain a primary reaction product;

C) Forming the primary reaction product into a film to obtain a transparent or translucent adhereable film material.

Preferably, the boron-containing compound is one or more of boron oxide, borate, boric acid compound, borate ester compound and trimethoxyboroxane;

The mass ratio of the dihydroxy-terminated polydimethylsiloxane, boron-containing compound and tetraisopropyl titanate is (2.5-27.5):(0.5-1):(0-0.04).

Preferably, the reaction temperature for obtaining the first reaction liquid in the step A) is 70-200°C, and the reaction time for obtaining the first reaction liquid in the step A) is 12-24 hours.

Preferably, the linear silicone oil is methyl hydrogen-containing silicone oil; the catalyst is platinum complex Pt(0)·1.5[CH ₂ =CH(CH ₃ ) ₂ Si] ₂ O; the reinforcing filler is white carbon black;

The mass ratio of the divinyl-terminated polydimethylsiloxane, linear silicone oil, catalyst and reinforcing filler is (0.5-1): (0.5-2.5): (0.0005-0.003): (0.0001-0.001) .

Preferably, the reaction temperature for obtaining the second reaction liquid in the step A) is 20-30° C.; the reaction time for obtaining the second reaction liquid in the step A) is 0.5-1 hour.

Preferably, the isocyanate is polyisocyanate; the hydroxyacrylate is 2-hydroxyethyl methacrylate, and the initiator is an azo compound initiator;

The molar ratio of the isocyanate to the hydroxyacrylate is 1:(0.95-1.05); the mass ratio of the reactant to the initiator is (100-1000):1.

Preferably, the mass ratio of the first reaction solution, the second reaction solution and the third reaction solution is (1-9):(1-9):(1-9);

The stirring and mixing temperature in the step B) is 20-30° C.; the stirring and mixing time in the step B) is 5-15 minutes. .

Preferably, the step C) pours the primary reaction product into a mold to dry to obtain a transparent or translucent adhered film material;

The drying temperature is 50-120° C.; the drying time is 3-24 hours.

The present invention provides a transparent or translucent adhesive film material prepared by the above-mentioned preparation method.

The present invention provides the use of a transparent or translucent adhereable film material as described above in electronic products.

The invention provides a method for preparing a transparent or translucent adhesive film material, comprising the following steps: A) mixing dihydroxy-terminated polydimethylsiloxane, a boron-containing compound and tetraisopropyl titanate, performing a reaction to obtain a first reaction solution; mixing divinyl-terminated polydimethylsiloxane, linear silicone oil, a catalyst and a reinforcing filler, performing a reaction to obtain a second reaction solution; mixing isocyanate and hydroxyacrylate, Carrying out the reaction, mixing the obtained reactant with the initiator to carry out a free radical polymerization reaction to obtain a third reaction solution; B) stirring and mixing the first reaction solution, the second reaction solution and the third reaction solution to obtain a primary reaction product; C ) forming a film of the primary reaction product to obtain a transparent or translucent adhereable film material. The invention mixes polyorganosiloxane, boron-containing compound, linear silicone oil and auxiliary agents, reacts, and dries to obtain a transparent or translucent adhesive film material. When subjected to external impact, it has better energy absorption rate and stress response ability. And when the material is damaged, the damaged part will undergo self-healing repair again through the intermolecular force of the internal structure. At the same time, it can be glued to any substrate without unnecessary trouble. The invention has the advantages of simple preparation process, low cost, readily available raw materials, non-toxic materials, convenient handling and the like.

Description of drawings

In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the following will briefly introduce the drawings that need to be used in the description of the embodiments or the prior art. Obviously, the accompanying drawings in the following description are only It is an embodiment of the present invention, and those skilled in the art can also obtain other drawings according to the provided drawings on the premise of not paying creative efforts.

Fig. 1 is a curve of the mechanical properties of the membrane material in Example 1 of the present invention during the self-healing process of the damage with time.

Detailed ways

The invention provides a method for preparing a transparent or translucent adhesive film material, comprising the following steps:

A) mixing dihydroxy-terminated polydimethylsiloxane, a boron-containing compound, and tetraisopropyl titanate for reaction to obtain a first reaction solution;

Mixing divinyl-terminated polydimethylsiloxane, linear silicone oil, catalyst and reinforcing filler, and reacting to obtain a second reaction liquid;

mixing isocyanate and hydroxyacrylate to react, and mixing the obtained reactant with an initiator to carry out radical polymerization reaction to obtain a third reaction liquid;

B) stirring and mixing the first reaction solution, the second reaction solution and the third reaction solution to obtain a primary reaction product;

C) Forming the primary reaction product into a film to obtain a transparent or translucent adhereable film material.

In the present invention, firstly, polydimethylsiloxane, boron-containing compound and tetraisopropyl titanate are mixed and reacted to obtain a first reaction solution.

In the present invention, following formula I and formula II provide the example of a reaction process:

In the present invention, the boron-containing compound is one or more of boron oxide, borate, boric acid compound, borate ester compound and trimethoxyboroxane; The mass ratio of base siloxane, boron-containing compound and tetraisopropyl titanate is preferably (2.5-27.5): (0.5-1): (0-0.04), more preferably (5-25): (0.6- 0.8): (0-0.03), most preferably (10-20): (0.6-0.7): (0-0.02).

In the present invention, the reaction temperature of this step is preferably 70-200°C, more preferably 100-150°C, such as 70°C, 80°C, 90°C, 100°C, 110°C, 120°C, 130°C, 140°C , 150°C, 160°C, 170°C, 180°C, 190°C, 200°C, preferably the range value with any of the above-mentioned values as the upper limit or lower limit; the reaction time of this step is preferably 12 to 24 hours, more preferably 15 ~20 hours.

Divinyl-terminated polydimethylsiloxane, linear silicone oil, catalyst and reinforcing filler are mixed and reacted to obtain a second reaction liquid; the following formula III provides an example of a reaction process:

The present invention uses bisvinyl-terminated PDMS and hydrogen-containing methyl silicone oil for cross-linking reaction, which greatly increases the cross-linking density on the basis of the original system, thereby improving the tensile properties of the membrane material and the puncture resistance of the membrane, and the performance The material has dimensional stability, is puncture-resistant when punctured at high speed, and has a high energy absorption rate when subjected to high-speed impact.

In the present invention, the linear silicone oil is methyl hydrogen-containing silicone oil; the catalyst is platinum complex Pt(0)·1.5[CH ₂ =CH(CH ₃ ) ₂ Si] ₂ O; the reinforcing filler is White carbon black, the white carbon black can be fumed white carbon black and precipitated white carbon black. Fumed white carbon black uses SiCl ₄ as raw material, burns at high temperature (1000-1200°C) in a hydrogen-oxygen flow, and generates SiO ₂ as a reinforcing filler. Precipitated white carbon black uses water glass (sodium silicate aqueous solution) as raw material, and reacts with hydrochloric acid or sulfuric acid to form SiO ₂ , which is filtered, dried, and ground to obtain a reinforcing filler. The rubber compound reinforced by fumed silica has better transparency, while the rubber compound reinforced by precipitation method is translucent.

In the present invention, the mass ratio of the divinyl-terminated polydimethylsiloxane, linear silicone oil, catalyst and reinforcing filler is (0.5-1): (0.5-2.5): (0.0005-0.003): (0.0001-0.001), more preferably (0.6-0.8): (1-2): (0.001-0.002): (0.0005-0.0008).

In the present invention, the reaction temperature of this step is preferably 20-30°C, such as 20°C, 21°C, 22°C, 23°C, 24°C, 25°C, 26°C, 27°C, 28°C, 29°C, 30°C °C is preferably a range value with any of the above-mentioned numerical values as the upper or lower limit; the reaction time of this step is preferably 0.5 to 1 hour, more preferably 0.6 to 0.8 hours.

The isocyanate is mixed with the hydroxy acrylate to react, and the obtained reactant is mixed with an initiator to carry out a free radical polymerization reaction to obtain a third reaction solution; the following formula IV and formula V provide an example of one of the reaction processes:

The present invention introduces the purpose of 2-(((butylamino) carbonyl) oxo) butyl methacrylate to improve the adhesion performance of film materials: 2-(((butylamino) carbonyl) oxo) methyl Butyl acrylate contains a carbamate group, which can form intermolecular hydrogen bonds with the surface groups of different substrates, and adhere the composite film material to different substrates, reducing a lot of unnecessary post-processing, etc. Trouble. The adhesion strength of pure PDMS membrane material on glass is only 1.28kPa, which has almost no adhesion ability. With the addition of 2-(((butylamino) carbonyl) oxo) butyl methacrylate, the adhesion strength on the glass can reach 151kPa, and it can even reach 171kPa on the aluminum substrate, which greatly improves the adhesion of the material. Attached performance.

In the present invention, the isocyanate is polyisocyanate, such as propyl isocyanate and/or butyl isocyanate; the hydroxy acrylate is -2-hydroxyethyl methacrylate, and the initiator is preferably diisocyanate Nitrogen compound initiator; such as one or more of azobisisobutyronitrile, azobisisoheptanonitrile and dimethyl azobisisobutyrate.

The preferred molar ratio of the isocyanate to hydroxyacrylate is 1:(0.95-1.05), more preferably 1:1; the mass ratio of the reactant to the initiator is preferably (100-1000):1, more preferably (200～800): 1, such as 100: 1, 200: 1, 300: 1, 400: 1, 500: 1, 600: 1, 700: 1, 800: 1, 900: 1, 1000: 1, preferably It is a range value with any of the above-mentioned numerical values as the upper limit or the lower limit.

In the present invention, the temperature of the condensation polymerization reaction between the isocyanate and hydroxyacrylate is preferably 15-30°C, more preferably 20-25°C, such as 15°C, 20°C, 25°C, 30°C, preferably at the above-mentioned Any numerical value is a range value of the upper limit or the lower limit; the time for the condensation polymerization reaction of the isocyanate and hydroxyacrylate is preferably 6-18 hours, more preferably 9-12 hours.

In the present invention, the temperature of the radical polymerization reaction is preferably 50-120°C, more preferably 60-100°C, such as 50°C, 60°C, 70°C, 80°C, 90°C, 100°C, 110°C, 120°C is preferably a range value with any of the above-mentioned values as the upper limit or lower limit; the time for the radical polymerization reaction is preferably 18 to 36 hours, more preferably 20 to 26 hours.

After obtaining the above-mentioned first reaction liquid, second reaction liquid and third reaction liquid, the present invention stirs and mixes the three reaction liquids according to a certain ratio to obtain primary reaction products.

In the present invention, the mass ratio of the first reaction liquid, the second reaction liquid and the third reaction liquid is (1-9): (1-9): (1-9), more preferably (2-8 ): (2～8): (2～8), most preferably (3～5): (3～5): (3～5)

The stirring and mixing temperature is preferably 20-30° C., more preferably 20-25° C.; the stirring and mixing time is preferably 5-15 minutes, more preferably 10 minutes.

After the primary reaction product is obtained, the present invention preferably puts it into an ultrasonic cleaner for defoaming treatment, and then pours it into a mold for drying.

In the present invention, the drying temperature is preferably 50-120°C, more preferably 60-100°C, such as 50°C, 60°C, 70°C, 80°C, 90°C, 100°C, 110°C, 120°C , is preferably a range value with any of the above-mentioned values as the upper limit or lower limit; the drying time is preferably 3-24 hours, more preferably 5-20 hours, most preferably 10-15 hours.

The present invention also provides a transparent or translucent adhesive film material, which is prepared according to the above-mentioned preparation method. The energy absorption rate of the transparent or translucent adhesive film material in the present invention is 42.77-81.51%. , the light transmittance is 60.6-99.35%, the haze is 3.52-65.8%, the maximum puncture distance can reach 4cm, and it has good adhesion strength on the surface of glass, metal and organic polymer.

The transparent or translucent adhesive film material in the present invention is mainly used in the field of electronic products.

The invention provides a method for preparing a transparent or translucent adhesive film material, comprising the following steps: A) mixing dihydroxy-terminated polydimethylsiloxane, a boron-containing compound and tetraisopropyl titanate, performing a reaction to obtain a first reaction solution; mixing divinyl-terminated polydimethylsiloxane, linear silicone oil, a catalyst and a reinforcing filler, performing a reaction to obtain a second reaction solution; mixing isocyanate and hydroxyacrylate, Carrying out the reaction, mixing the obtained reactant with the initiator to carry out a free radical polymerization reaction to obtain a third reaction solution; B) stirring and mixing the first reaction solution, the second reaction solution and the third reaction solution to obtain a primary reaction product; C ) forming a film of the primary reaction product to obtain a transparent or translucent adhereable film material. The invention mixes polyorganosiloxane, boron-containing compound, linear silicone oil and auxiliary agents, reacts, and dries to obtain a transparent or translucent adhesive film material. When subjected to external impact, it has better energy absorption rate and stress response ability. And when the material is damaged, the damaged part will undergo self-healing repair again through the intermolecular force of the internal structure. At the same time, it can be glued to any substrate without unnecessary trouble. The invention has the advantages of simple preparation process, low cost, readily available raw materials, non-toxic materials, convenient handling and the like.

In order to further illustrate the present invention, a transparent or translucent adhesive film material provided by the present invention, its preparation method and application will be described in detail below in conjunction with the examples, but it should not be construed as limiting the protection scope of the present invention.

Example 1

Mix 17g of dihydroxy-terminated polydimethylsiloxane with a molecular weight of 4000 and 1g of trimethoxyboroxane evenly, add 0.08g of tetraisopropyl titanate, and stir at a constant speed at 90°C for 8 hours to obtain the first a reaction solution.

Mix 8g of bisvinyl-terminated polydimethylsiloxane and 8g of methylhydrogen silicone oil evenly with 0.1g of additive (platinum complex Pt(0)·1.5[CH ₂ =CH(CH ₃ ) ₂ Si ] ₂ O as a catalyst, precipitated silica as a filler), and stirred at 25° C. for 10 minutes to obtain a second reaction solution.

1 mol of n-butyl isocyanate and 1 mol of 2-hydroxyethyl methacrylate were stirred at 25°C for 6 hours and mixed evenly. Add 15.2mg of azobisisobutyronitrile to the resulting 2-(((butylamino)carbonyl)oxo)butyl methacrylate, and stir at 60°C for 24h to obtain poly 2-(((butylamino)carbonyl ) oxo) butyl methacrylate. The resulting solution was washed twice in deionized water and ethyl acetate in sequence to obtain a third reaction solution.

Take 11.64g of the first reaction solution, and stir with the second reaction solution and 0.9g of the third reaction solution at 25°C for 10 minutes to obtain the primary reaction product.

The primary reaction products were poured into molds respectively, and dried at 80° C. for 24 hours. The primary reaction product is dried to obtain a translucent and adherent composite film.

self-healing properties

The translucent flexible composite film prepared in Example 1 was made into a dumbbell shape, and the width of the narrow parallel part was 6 mm. The thickness is 2 mm, and the mechanical properties of the composite membrane materials are tested with a WSN-10kN universal tensile machine (Changchun Intelligent, China). The tensile rate of the uniaxial tension was 50mm/min, and all the samples were tested at room temperature using a 100N load cell. Take the dumbbell-shaped spline of New Example 1, cut the narrow parallel part vertically with a blade, stick the two parts of the damaged surface tightly, put it at room temperature for self-healing, and then carry out the mechanical performance test under the same conditions at different times. The results are shown in figure 1. The healing efficiency of the material can reach 86.32% after 12 hours, and 93.96% after 60 hours, which proves the excellent self-healing performance of the membrane material.

energy absorption rate

The translucent flexible composite film prepared in Example 1 was subjected to an impact mechanical test using an LLY-53 protective material impact tester at 25°C. The test method is as follows: the composite film is made into a cylindrical shape with a diameter of 8cm and a thickness of 5mm, and placed on a blank polyester fiber fabric, and then the composite film and fabric are placed on a circular impact base, and the 5kg weight is lifted from 20cm , 40cm, 60cm, 80cm, 100cm height free fall, impact with the composite film, the impact sensor in the circular base records the impact force.

The blank fabric control test was subjected to impact testing. The test method is as follows: put a blank polyester fiber fabric on a circular impact base, and drop a 5kg weight freely from a height of 20cm, 40cm, 60cm, 80cm, and 100cm to impact the control film. The impact sensor in the circular base Record the force of impact.

Calculate the energy absorption rate by the energy absorption rate calculation formula shown in formula I,

Among them, N ₁ is the impact force of the hammer passing through the composite film and fabric, and N ₂ is the impact force of the weight passing through the blank fabric. The experimental results are shown in Table 2. Table 2 shows the energy absorption rate of the composite membrane at different heights.

Table 2 Energy absorption rate of composite membranes tested at different heights

It can be seen from Table 2 that the film prepared by the present invention has good energy absorption rate.

Transmittance and Haze

The translucent flexible composite film prepared in Example 1 was made into a thickness of 100 nm, and the transmittance test was carried out under the WGW photo-haze meter.

The light transmittance and haze are calculated by the formulas shown in formulas II and III,

Among them, T1 is the incident light flux, _T2 is the transmitted light flux, T3 is the scattered light flux _of the instrument, and T4 is the scattered light flux _of the sample _. The results are shown in Table 3, and Table 3 shows the light transmittance and haze of the composite film.

Table 3 Light transmittance and haze of translucent flexible composite film

Adhesive strength

Spread the translucent flexible composite film prepared in Example 1 evenly on two 2.5 × 6 × 0.5 cm glass plates (or different substrates) before curing, stick the glass plates (different substrates) together, and give 0.1 MPa pressure. After the reaction solution is completely cured, a lap shear test is performed to characterize the adhesion.

The adhesion strength was calculated by the calculation formula shown in Formula II.

Where F is the tensile force and S is the contact area. The experimental results are shown in Table 4, and Table 4 shows the adhesion strength on different substrates.

The adhesive strength of composite membrane material on different base materials in the embodiment 1 of table 4

As a comparison, the adhesion strengths of pure PDMS, PDMS+IHP and the membrane material of the present invention are shown in Table 5

shown.

Table 5 Adhesion strength of different materials on glass substrates

Example 2

Mix 15g of dihydroxy-terminated polydimethylsiloxane with a molecular weight of 6000 and 1g of trimethoxyboroxane evenly, add 0.04g of tetraisopropyl titanate, and stir at a constant speed for 6 hours at 100°C to obtain the first a reaction solution.

Mix 6g of bisvinyl-terminated polydimethylsiloxane and 6g of methylhydrogen silicone oil evenly with 0.1g of additive (platinum complex Pt(0)·1.5[CH ₂ =CH(CH ₃ ) ₂ Si ] ₂ O as a catalyst, fumed silica as a filler), and stirred at 25° C. for 10 minutes to obtain a second reaction solution.

Stir 2 mol of n-propyl isocyanate and 2 mol of hydroxyethyl acrylate at 25°C for 6 h and mix well. Add 14.3 mg of azobisisobutyronitrile to the resulting 2-(((propylamino)carbonyl)oxy)butyl acrylate and stir at 60°C for 24h to obtain poly-2-(((propylamino)carbonyl)oxy Generation) butyl acrylate. The resulting solution was washed twice in deionized water and ethyl acetate in sequence to obtain a third reaction solution.

Take 8 g of the first reaction solution, 1.2 g of the third reaction solution and the second reaction solution and stir at 25° C. for 10 minutes to obtain a primary reaction product.

The primary reaction products were poured into molds respectively, and dried at 80° C. for 24 hours. The primary reaction product is dried to obtain a transparent and flexible composite film.

The transparent flexible composite film prepared in Example 2 was made into a thickness of 100 nm, and the transmittance test was carried out under the WGW photo-haze meter. The results are shown in Table 6, and Table 6 shows the light transmittance and haze of the composite film.

The light transmittance and the haze of the transparent flexible composite film in the embodiment 2 of table 6

It can be seen from Table 5 that the film prepared by the present invention has good light transmittance.

Example 3

Mix 15g of dihydroxy-terminated polydimethylsiloxane with a molecular weight of 6000 and 1g of trimethoxyboroxane evenly, then add 0.08g of tetraisopropyl titanate, and stir at a constant speed at 100°C for 6 hours to obtain first reaction solution.

Mix 4g of bisvinyl-terminated polydimethylsiloxane and 8g of methyl hydrogen silicone oil with 0.1g of additive (platinum complex Pt(0)·1.5[CH ₂ =CH(CH ₃ ) ₂ Si ] ₂ O as a catalyst, precipitated silica as a filler), and stirred at 25° C. for 10 minutes to obtain a second reaction solution.

Stir 1 mol amyl isocyanate and 1 mol hydroxyethyl methacrylate at 25°C for 6 h and mix well. Add 9.5 mg of azobisisoheptanonitrile to the resulting 2-(((pentylamino)carbonyl)oxo)butyl methacrylate and stir at 60°C for 24h to obtain poly 2-(((pentylamino)carbonyl ) oxo) butyl methacrylate. The resulting solution was washed twice in deionized water and ethyl acetate in sequence to obtain a third reaction solution.

Take 8 g of the first reaction solution, stir 0.6 g of the third reaction solution and the second reaction solution at 25° C. for 10 minutes to obtain a primary reaction product.

The primary reaction products were poured into molds respectively, and dried at 80° C. for 24 hours. The primary reaction product is dried to obtain a translucent flexible composite film.

Example 4

Mix 18g of dihydroxy-terminated polydimethylsiloxane with a molecular weight of 5000 and 1g of trimethoxyboroxane evenly, then add 0.08g of tetraisopropyl titanate, and stir at a constant speed at 90°C for 8 hours to obtain first reaction solution.

Mix 2.4g of bisvinyl-terminated polydimethylsiloxane, 9.6g of methyl hydrogen silicone oil, and 0.1g of additive (platinum complex Pt(0)·1.5[CH ₂ =CH(CH ₃ ) ₂ Si] ₂ O as a catalyst, precipitated white carbon as a filler), and stirred at 25° C. for 10 minutes to obtain a second reaction solution.

1 mol of hexamethylene diisocyanate and 1 mol of 2-hydroxyethyl methacrylate were stirred at 25°C for 6 hours and mixed uniformly. Add 11.2mg of dimethyl azobisisobutyrate to the resulting 2-(((hexamethyleneethylamino)carbonyl)oxy)butyl methacrylate and stir at 60°C for 24h to obtain poly 2-( ((Hexamethyleneethylamino)carbonyl)oxo)butyl methacrylate. The resulting solution was washed twice in deionized water and ethyl acetate in sequence to obtain a third reaction solution.

Take 8 g of the first reaction solution, stir 0.5 g of the third reaction solution and the second reaction solution at 25° C. for 10 minutes to obtain a primary reaction product.

The primary reaction products were poured into molds respectively, and dried at 80° C. for 24 hours. The primary reaction product is dried to obtain a translucent flexible composite film.

Example 5

Mix 17g of dihydroxy-terminated polydimethylsiloxane with a molecular weight of 45,000 and 1g of trimethoxyboroxane evenly, add 0.4g of tetraisopropyl titanate, and stir at a constant speed at 90°C for 8 hours to obtain the first a reaction solution.

Mix 5g of bisvinyl-terminated polydimethylsiloxane and 5g of methylhydrogen silicone oil evenly with 0.1g of additive (platinum complex Pt(0)·1.5[CH ₂ =CH(CH ₃ ) ₂ Si ] ₂ O as a catalyst, precipitated silica as a filler), and stirred at 25° C. for 10 minutes to obtain a second reaction solution.

1 mol of diphenylmethane diisocyanate and 1 mol of 2-hydroxyethyl methacrylate were stirred at 25°C for 6 hours and mixed uniformly. Add 9.6 mg of azobisisobutyronitrile to the resulting 2-(((diphenylmethylethylamino)carbonyl)oxy)butyl methacrylate and stir at 60°C for 24 hours to obtain poly 2-(((di Benzylethylamino)carbonyl)oxo)butyl methacrylate. The resulting solution was washed twice in deionized water and ethyl acetate in sequence to obtain a third reaction solution.

Take 10 g of the first reaction solution, and stir with the second reaction solution at 25° C. for 10 minutes to obtain the primary reaction product.

The primary reaction products were poured into molds respectively, and dried at 80° C. for 24 hours. The primary reaction product is dried to obtain a translucent flexible composite film.

Example 6

Mix 17g of dihydroxy-terminated polydimethylsiloxane with a molecular weight of 8000 and 1g of trimethoxyboroxane evenly, add 0.02g of tetraisopropyl titanate, and stir at a constant speed at 90°C for 8 hours to obtain the first a reaction solution.

Mix 3g of divinyl-terminated polydimethylsiloxane and 9g of methyl hydrogen silicone oil evenly with 0.1g of additive (platinum complex Pt(0)·1.5[CH ₂ =CH(CH ₃ ) ₂ Si ] ₂ O as a catalyst, precipitated silica as a filler), and stirred at 25° C. for 10 minutes to obtain a second reaction solution.

Stir 1 mol of toluene diisocyanate and 1 mol of hydroxyethyl acrylate at 25°C for 6 hours and mix well. Add 11.4mg of azobisisoheptanonitrile to the resulting 2-(((tolylethylamino)carbonyl)oxy)butyl acrylate, and stir at 60°C for 24h to obtain poly 2-(((tolylethylamino)carbonyl ) oxo) butyl acrylate. The resulting solution was washed twice in deionized water and ethyl acetate in sequence to obtain a third reaction solution.

Take 6g of the first reaction solution, 2g of the third reaction solution and the second reaction solution and stir at 25° C. for 10 minutes to obtain a primary reaction product.

The primary reaction products were poured into molds respectively, and dried at 80° C. for 24 hours. The primary reaction product is dried to obtain a translucent flexible composite film.

Example 7

Mix 17g of dihydroxy-terminated polydimethylsiloxane with a molecular weight of 9000 and 1g of trimethoxyboroxane evenly, then add 0.064g of tetraisopropyl titanate, and stir at a constant speed at 90°C for 8 hours to obtain first reaction solution.

Mix 3g of divinyl-terminated polydimethylsiloxane and 9g of methyl hydrogen silicone oil evenly with 0.1g of additive (platinum complex Pt(0)·1.5[CH ₂ =CH(CH ₃ ) ₂ Si ] ₂ O as a catalyst, precipitated silica as a filler), and stirred at 25° C. for 10 minutes to obtain a second reaction solution.

1 mol of dicyclohexylmethane diisocyanate and 1 mol of 2-hydroxyethyl methacrylate were stirred at 25°C for 6 hours and mixed uniformly. Add 15.1 mg of azobisisobutyronitrile to the resulting 2-(((dicyclohexylmethaneamino)carbonyl)oxo)butyl methacrylate and stir at 60°C for 24h to obtain poly 2-(((dicyclohexyl Methaneamino)carbonyl)oxo)butyl methacrylate. The resulting solution was washed twice in deionized water and ethyl acetate to obtain the third reaction solution

Take 8 g of the first reaction solution, 3 g of the third reaction solution and the second reaction solution and stir at 25° C. for 10 minutes to obtain a primary reaction product.

The primary reaction products were poured into molds respectively, and dried at 80° C. for 24 hours. The primary reaction product is dried to obtain a translucent flexible composite film.

The above is only a preferred embodiment of the present invention, it should be pointed out that, for those of ordinary skill in the art, without departing from the principle of the present invention, some improvements and modifications can also be made, and these improvements and modifications can also be made. It should be regarded as the protection scope of the present invention.

Claims (10)

1. A method for preparing a transparent or translucent adhesive film material, comprising the following steps: A) mixing dihydroxy-terminated polydimethylsiloxane, a boron-containing compound, and tetraisopropyl titanate for reaction to obtain a first reaction solution; Mixing divinyl-terminated polydimethylsiloxane, linear silicone oil, catalyst and reinforcing filler, and reacting to obtain a second reaction liquid; mixing isocyanate and hydroxyacrylate to react, and mixing the obtained reactant with an initiator to carry out radical polymerization reaction to obtain a third reaction solution; B) stirring and mixing the first reaction solution, the second reaction solution and the third reaction solution to obtain a primary reaction product; C) Forming the primary reaction product into a film to obtain a transparent or translucent adhereable film material. 2. The preparation method according to claim 1, wherein the boron-containing compound is one or more of boron oxide, borate, boric acid compound, borate ester compound and trimethoxyboroxane kind; The mass ratio of the dihydroxy-terminated polydimethylsiloxane, boron-containing compound and tetraisopropyl titanate is (2.5-27.5):(0.5-1):(0-0.04). 3. The preparation method according to claim 2, characterized in that, the reaction temperature for obtaining the first reaction solution in the step A) is 70-200° C., and the reaction temperature for obtaining the first reaction solution in the step A) is The best time is 12 to 24 hours. 4. The preparation method according to claim 1, wherein the linear silicone oil is methyl hydrogen-containing silicone oil; the catalyst is a platinum complex Pt(0)·1.5[CH ₂ =CH(CH ₃ ) ₂ Si] ₂ O; The reinforcing filler is white carbon black; The mass ratio of the divinyl-terminated polydimethylsiloxane, linear silicone oil, catalyst and reinforcing filler is (0.5-1): (0.5-2.5): (0.0005-0.003): (0.0001-0.001) . 5. The preparation method according to claim 4, characterized in that, the reaction temperature for obtaining the second reaction solution in the step A) is 20 to 30° C.; the reaction temperature for obtaining the second reaction solution in the step A) The time is 0.5 to 1 hour. 6. preparation method according to claim 1, is characterized in that, described isocyanate is polyisocyanate; Described hydroxyl acrylate is methacrylate-2-hydroxyethyl ester, and described initiator is azo compound initiator ; The molar ratio of the isocyanate to the hydroxyacrylate is 1:(0.95-1.05); the mass ratio of the reactant to the initiator is (100-1000):1. 7. The preparation method according to claim 1, characterized in that, the mass ratio of the first reaction solution, the second reaction solution and the third reaction solution is (1～9):(1～9):(1 ~9); The stirring and mixing temperature in the step B) is 20-30° C.; the stirring and mixing time in the step B) is 5-15 minutes. 8. The preparation method according to claim 7, characterized in that, in the step C), the primary reaction product is poured into a mold and dried to obtain a transparent or translucent adhesive film material; The drying temperature is 50-120° C.; the drying time is 3-24 hours. 9. The transparent or translucent adhesive film material prepared by the preparation method according to any one of claims 1-8. 10. Use of the transparent or translucent adhesive film material according to claim 9 in electronic products.

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