Anti-sticky PVB film and its preparation method and application

Abstract

The present invention discloses an anti-sticking PVB film, a preparation method, and applications thereof. The anti-sticking PVB film comprises the following raw materials in parts by weight: 100 parts of PVB resin, 30-40 parts of a plasticizer, 0.05-0.15 parts of an adhesion modifier, 2-6 parts of isooctyl palmitate, and 0.1-0.7 parts of a silicone release agent. The addition of isooctyl palmitate and the silicone release agent to the anti-sticking PVB film not only provides internal lubrication, improving the processing performance of the PVB film, but also enhances the anti-blocking properties of the PVB film without affecting the adhesion between the PVB film and laminated glass, or the optical properties of the laminated glass, such as light transmittance and haze.

Description

Technical Field

[0001] The present invention relates to the field of polymer sheets, and in particular to an anti-stickiness PVB film and a preparation method and application thereof. Background Art

[0002] Due to its high safety performance, PVB laminated glass has been widely used in the architectural and automotive sectors. However, due to the high content of plasticizers and hydroxyl groups in PVB films, they are prone to self-adhesion when laminated together, requiring storage at low temperatures to prevent adhesion. Storage at room temperature can cause PVB films to soften, exacerbating adhesion between sheets and reducing operability during laminated glass assembly. The process often requires operators to spend considerable time separating the adhered PVB films, severely impacting laminated glass production efficiency.

[0003] Chinese patent CN106164010A discloses a method for preventing PVB self-adhesion by printing a pattern of concave and convex shapes on the surface of PVB film through an embossing process. However, this method is energy-intensive, requires significant equipment investment, and requires a large floor space, making it a less-than-ideal approach. Other methods, such as applying a powder (such as sodium bicarbonate) to the film surface and chemically treating the PVB film surface with acid, reduce adhesion between films, but this surface treatment affects the adhesion between the film and the glass, making it less desirable.

[0004] Therefore, it is necessary to further enhance the anti-adhesion property of PVB film so that the PVB film can be easily operated when preparing laminated glass. Summary of the Invention

[0005] In order to overcome the adhesion problem of existing PVB films, one of the purposes of the present invention is to provide an anti-adhesive PVB film; a second purpose of the present invention is to provide a method for preparing the anti-adhesive PVB film; and a third purpose of the present invention is to provide applications of the anti-adhesive PVB film.

[0006] In order to achieve the above object, the technical solution adopted by the present invention is:

[0007] The first aspect of the present invention provides an anti-sticking PVB film, comprising the following raw materials in parts by weight: 100 parts of PVB resin, 30-40 parts of plasticizer, 0.05-0.15 parts of adhesion regulator, 2-6 parts of isooctyl palmitate, and 0.1-0.7 parts of silicone release agent.

[0008] The inventors have found that adding isooctyl palmitate to PVB film can reduce the adhesion of PVB film, and isooctyl palmitate has an internal plasticizing effect, which can reduce the initial viscosity and improve the processing performance of PVB film. In addition, by adding an organosilicon release agent to the PVB film, the stacking adhesion between PVB films can be further improved. The present invention obtains a PVB laminated glass intermediate mold with anti-adhesion properties by adding an organosilicon release agent and isooctyl palmitate to the PVB system, and does not adversely affect the optical and bonding properties of the laminated glass. The present invention can be used for PVB films of various specifications and structures, including but not limited to one or more layers of PVB film, wedge-shaped or uniform thickness PVB film, and other functional films such as heat insulation film, sound insulation film, color film, gradient color film, etc.

[0009] Preferably, the anti-stickiness PVB film further comprises the following raw materials in parts by weight: 0.2-1 parts of antioxidant and 0.1-1.2 parts of ultraviolet absorber.

[0010] Preferably, the degree of polymerization of the PVB resin is 1200-2800; further preferably, the degree of polymerization of the PVB resin is 1200-2200; further preferably, the degree of polymerization of the PVB resin is 1500-2000; further preferably, the degree of polymerization of the PVB resin is 1700; the PVB resin in this specific degree of polymerization range is selected to meet the mechanical property requirements of the film, such as tensile strength and elongation at break, while having good processing fluidity and penetration resistance.

[0011] Preferably, the hydroxyl content of the PVB resin is 17.8-19.2 wt %. Selecting a PVB resin with this hydroxyl content range can ensure that the PVB film maintains good adhesion to the glass while also having good flexibility, penetration resistance and impact resistance.

[0012] Preferably, the acetyl content of the PVB resin is 0.2-2 wt %. Selecting a PVB resin with this acetyl content can improve the moisture resistance of the PVB film.

[0013] Preferably, the plasticizer includes at least one of phthalate, adipate, sebacic acid ester, triethylene glycol ester, and tetraethylene glycol ester; further preferably, the plasticizer includes at least one of triethylene glycol ester and tetraethylene glycol ester; in some preferred embodiments of the present invention, the plasticizer is triethylene glycol diisooctanoate (3GO).

[0014] Preferably, the antioxidant is a mixture of a hindered phenol antioxidant and a phosphite antioxidant; further preferably, the mass ratio of the hindered phenol antioxidant to the phosphite antioxidant is 1:(0.5-1.5); still further preferably, the mass ratio of the hindered phenol antioxidant to the phosphite antioxidant is 1:(0.8-1.2); in some preferred embodiments of the present invention, the mass ratio of the hindered phenol antioxidant to the phosphite antioxidant is 1:1.

[0015] Further preferably, the hindered phenol antioxidant includes at least one of 2,6-di-tert-butyl-p-methylphenol (BHT), β-(4-hydroxy-3,5-di-tert-butylphenyl) propionate (antioxidant 1076), pentaerythritol tetrakis[methyl-β-(3,5-di-tert-butyl-4-hydroxyphenyl) propionate] (antioxidant 1010), N,N'-hexamethylenebis(3,5-di-tert-butyl-4-hydroxyphenylpropionamide) (antioxidant 1098), and triethylene glycol bis-3-(3-tert-butyl-4-hydroxy-5-methylphenyl) acrylate (antioxidant 245); even further preferably, the hindered phenol antioxidant includes at least one of antioxidant 1076, antioxidant 1010, and antioxidant 1098; in some preferred embodiments of the present invention, the hindered phenol antioxidant is antioxidant 1010.

[0016] Further preferably, the phosphite antioxidant includes at least one of phenyl isooctyl phosphite (ODPP), tris(2,4-di-tert-butylphenyl) phosphite (antioxidant 168), bisphenol A phosphite, and triphenyl phosphite (TPP); in some preferred embodiments of the present invention, the phosphite antioxidant is antioxidant 168.

[0017] Preferably, the ultraviolet absorber includes at least one of benzophenone, benzotriazole, and triazine ultraviolet absorbers; further preferably, the ultraviolet absorber is a benzotriazole ultraviolet absorber; even further preferably, the benzotriazole ultraviolet absorber includes at least one of 2-(2'-hydroxy-5'-methylphenyl)benzotriazole (UV-P), (2'-hydroxy-3'-tert-butyl-5'-methylphenyl)-5-chlorobenzotriazole (UV-326), 2-(2'-hydroxy-3', 5'-di-tert-butylphenyl)-5-chlorobenzotriazole (UV-327), and 2-(2'-hydroxy-3', 5'-dipentylphenyl)benzotriazole (UV-328); in some preferred embodiments of the present invention, the ultraviolet absorber is UV-326.

[0018] Preferably, the adhesion regulator includes at least one of alkali metal and alkaline earth metal salts; further preferably, the adhesion regulator is at least one of alkaline earth metal salts; alkaline earth metal salts include at least one of potassium acetate, magnesium acetate, potassium formate, magnesium formate, sodium acetate, magnesium propionate, magnesium 2-ethylbutyrate, magnesium 2-ethylhexanoate, and potassium 2-ethyl acetate; in some preferred embodiments of the present invention, the adhesion regulator is magnesium acetate and potassium acetate; the hydrogen bonding between the PVB film and the laminated glass is controlled by the alkali metal and alkaline earth metal salts, thereby controlling the adhesion between the PVB film and the glass.

[0019] Preferably, the silicone release agent includes at least one of polydimethylsiloxane, methyl hydrogen silicone oil, polydiethylsiloxane, and polymethylphenylsiloxane; further preferably, the silicone release agent is at least one of methyl hydrogen silicone oil and polydimethylsiloxane; even further preferably, the silicone release agent is methyl hydrogen silicone oil. Choosing methyl hydrogen silicone oil as a special silicone release agent can make the PVB film hydrophobic and moisture-proof, have high light transmittance, and good anti-sticking properties.

[0020] Preferably, the thickness of the anti-stick PVB film is 0.38-1.52 mm.

[0021] Preferably, the raw materials for preparing the anti-sticking PVB film also include water, and the amount of water used is 0.1-1 parts by mass; in the preparation process of the anti-sticking PVB film, water is first mixed with the adhesion regulator to dissolve the adhesion regulator, and then the adhesion regulator is mixed with other components.

[0022] The anti-sticking PVB film of the present invention may further contain additives such as light stabilizers, flame retardants, antistatic agents, pigments, dyes, surfactants, fluorescent brighteners, photochromic and thermochromic materials, and infrared absorbers as needed. These additives may be used alone or in combination of two or more.

[0023] A second aspect of the present invention provides a method for preparing the above-mentioned anti-sticking PVB film, comprising the following steps:

[0024] The raw materials except the adhesion regulator and the PVB resin are mixed to obtain a plasticizer composition; the plasticizer composition, the adhesion regulator and the PVB resin are added into an extruder for mixing and extruding to obtain the anti-stickiness PVB film.

[0025] Preferably, the extruder is a venting twin-screw extruder, and the extruder is provided with two vents, one for natural exhaust and the other for exhaust under a gauge pressure condition of a vacuum degree of -0.02 MPa to -0.1 MPa.

[0026] More preferably, the extrusion temperature of the vented twin-screw extruder is 40-190° C., and the screw speed is 50-200 r / min.

[0027] A third aspect of the present invention provides use of the above-mentioned anti-sticking PVB film in laminated glass.

[0028] The beneficial effects of the present invention are:

[0029] In the anti-sticking PVB film of the present invention, the addition of isooctyl palmitate and the silicone release agent not only has an internal lubricating effect, thereby improving the processing performance of the PVB film, but also improves the anti-sticking property of the PVB film, without affecting the bonding force between the PVB film and the laminated glass, or the optical properties of the laminated glass, such as the light transmittance and haze. DETAILED DESCRIPTION

[0030] The present invention is further described in detail below using specific examples. Unless otherwise specified, the raw materials, reagents, and apparatus used in the examples and comparative examples are available from conventional commercial sources or by conventional methods. Unless otherwise specified, all experimental or testing methods are conventional in the art.

[0031] Example 1

[0032] The specific steps of the preparation method of the anti-sticky PVB film of this embodiment are as follows:

[0033] (1) 0.16 parts by weight of antioxidant 1010, 0.16 parts by weight of antioxidant 168, 0.3 parts by weight of ultraviolet absorber UV-326, 4 parts by weight of isooctyl palmitate, 0.5 parts by weight of methyl hydrogen silicone oil and 34.5 parts by weight of 3GO plasticizer were mixed to prepare a 3GO composition;

[0034] (2) 0.08 parts by weight of potassium acetate and 0.01 parts by weight of magnesium acetate were mixed and dissolved in 0.6 parts by weight of deionized water to prepare a metal ion aqueous solution;

[0035] (3) The 3GO composition, metal ion aqueous solution, and 100 parts by weight of PVB resin prepared above were plasticized and mixed by a 90-type twin-screw extruder at a temperature of 150°C and a screw speed of 120 rpm. The vacuum degree of the exhaust port of the extruder was -0.08 MPa, and then extruded through a 160°C die head into a 0.76 mm thick film.

[0036] Example 2

[0037] The preparation method of the anti-sticking PVB film of this embodiment refers to that of Example 1, except that the amounts of raw material components are different. The raw material components of this embodiment are shown in Table 1 below.

[0038] Example 3

[0039] The preparation method of the anti-sticking PVB film of this embodiment refers to that of Example 1, except that the amounts of raw material components are different. The raw material components of this embodiment are shown in Table 1 below.

[0040] Example 4

[0041] The preparation method of the anti-sticking PVB film of this embodiment refers to that of Example 1, except that the amounts of raw material components are different. The raw material components of this embodiment are shown in Table 1 below.

[0042] Example 5

[0043] The preparation method of the anti-sticking PVB film of this embodiment refers to that of Example 1, except that the amounts of raw material components are different. The raw material components of this embodiment are shown in Table 1 below.

[0044] Comparative Example 1

[0045] The preparation method of the anti-stickiness PVB film of this comparative example refers to that of Example 1, except that the amounts of raw material components are different. The raw material components of this comparative example are shown in Table 1 below.

[0046] Comparative Example 2

[0047] The preparation method of the anti-stickiness PVB film of this comparative example refers to that of Example 1, except that the amounts of raw material components are different. The raw material components of this comparative example are shown in Table 1 below.

[0048] Comparative Example 3

[0049] The preparation method of the anti-stickiness PVB film of this comparative example refers to that of Example 1, except that the amounts of raw material components are different. The raw material components of this comparative example are shown in Table 1 below.

[0050] Comparative Example 4

[0051] The preparation method of the anti-stickiness PVB film of this comparative example refers to that of Example 1, except that the amounts of raw material components are different. The raw material components of this comparative example are shown in Table 1 below.

[0052] Comparative Example 5

[0053] The preparation method of the anti-stickiness PVB film of this comparative example refers to that of Example 1, except that the amounts of raw material components are different. The raw material components of this comparative example are shown in Table 1 below.

[0054] Table 1

[0055]

[0056] The above embodiments and comparative examples were subjected to performance tests:

[0057] (1) Impact value

[0058] The adhesion between PVB film and glass was evaluated according to the knock value test in GB / T 32020-2015 5.4.6. The results are shown in Table 2 below.

[0059] (2) Penetration resistance test

[0060] Tested according to GB / T 5137.1-2020 6 anti-penetration test.

[0061] (3) Transmittance and haze

[0062] Tested according to GB / T 2410-2008.

[0063] (4) Adhesion test

[0064] This test measures the self-adhesion strength of PVB film. Two sheets of PVB film are cut into 2.5cm x 15cm dimensions and completely laminated together. A 0.1mm thick layer of PET film is then laminated on each surface of the PVB film laminate. The PET and PVB film laminate is then placed between two panes of glass. The laminate is then pressed in a sheet press at a temperature of 20-25°C and a pressure of 0.25 MPa for 15 minutes. The PVB laminate is then removed, peeled back 2cm from the end, and clamped in the fixture of an electronic universal testing machine. The peel speed is set to 100mm / min, and the 180° peel strength of the two PVB films is measured at a temperature of 23°C and a humidity of 30%.

[0065] Table 2 Performance test results

[0066]

[0067] The data in Table 2 above show that the addition of isooctyl palmitate and a silicone release agent did not significantly affect the light transmittance and haze of the film. The peel forces of Comparative Examples 1, 2, and 5 were significantly greater than those of the other experimental examples, indicating that the addition of isooctyl palmitate and a silicone release agent provided a certain degree of anti-adhesion effect. Comparative Examples 3 and 4 show that excessive amounts of isooctyl palmitate and a silicone release agent can affect the penetration resistance of laminated glass. Therefore, the appropriate addition of isooctyl palmitate and a silicone release agent ensures both acceptable penetration resistance and good anti-adhesion properties.

[0068] The above embodiments are only preferred embodiments of the present invention and are not intended to limit the present invention. Any modifications, equivalent replacements, improvements, etc. made within the spirit and principles of the present invention should be included in the scope of protection of the present invention.

Claims

1. An anti-adhesive PVB film, characterized in that: The preparation method comprises the following raw materials in parts by weight: 100 parts of PVB resin, 30-40 parts of plasticizer, 0.05-0.15 parts of adhesion regulator, 2-6 parts of isooctyl palmitate, and 0.1-0.7 parts of silicone release agent; The organic silicon release agent includes at least one of polydimethylsiloxane, methyl hydrogen silicone oil, polydiethylsiloxane, and polymethylphenylsiloxane.

2. The anti-adhesive PVB film according to claim 1, characterized in that: The invention also comprises the following raw materials in parts by weight: 0.2-1 parts by weight of an antioxidant and 0.1-1.2 parts by weight of an ultraviolet absorber.

3. The anti-stickiness PVB film according to claim 1 or 2, characterized in that: The polymerization degree of the PVB resin is 1200-2800.

4. The anti-stickiness PVB film according to claim 1 or 2, characterized in that: The hydroxyl content of the PVB resin is 17.8-19.2 wt %.

5. The anti-stickiness PVB film according to claim 1 or 2, characterized in that: The acetyl content of the PVB resin is 0.2-2 wt %.

6. The anti-adhesive PVB film according to claim 2, characterized in that: The antioxidant is a mixture of hindered phenol antioxidants and phosphite antioxidants.

7. The anti-stickiness PVB film according to claim 1 or 2, characterized in that: The adhesion modifier includes an alkaline earth metal salt.

8. The method for preparing the anti-stickiness PVB film according to any one of claims 1 to 7, characterized in that: The following steps are involved: The raw materials except the adhesion regulator and the PVB resin are mixed to obtain a plasticizer composition; the plasticizer composition, the adhesion regulator and the PVB resin are added into an extruder for mixing and extruding to obtain the anti-stickiness PVB film.

9. Use of the anti-stickiness PVB film according to any one of claims 1 to 7 in laminated glass.

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