Highly efficient flame retardant film and its production process

Abstract

The application provides a high-efficiency flame-retardant film and a production process thereof, and relates to the technical field of flame-retardant films.A high-efficiency flame-retardant film comprises a surface layer, a core layer and an inner layer.The surface layer comprises the following raw materials in parts by mass: 10-40 parts of copolymerized PP, 7-36 parts of a flame retardant, 0.4-1.5 parts of an anti-UV agent, 0.01-0.1 parts of an anti-aging agent, 0.5-3 parts of an anti-sticking agent and 0.2-3 parts of titanium white masterbatch.The flame-retardant film provided by the application has excellent flame-retardant performance.

Description

Technical Field

[0001] This invention relates to the field of flame retardant film technology, and in particular to a high-efficiency flame retardant film and its manufacturing process. Background Technology

[0002] Flame-retardant film is a thin-film material with fire-resistant properties, widely used in various fields such as construction, transportation, electronics, and new energy. In the event of a fire, flame-retardant film effectively isolates flames and ignition sources, reduces heat transfer, lowers the surface temperature of the material, and slows down further degradation. Its main function is to protect materials and personnel safety by inhibiting and delaying the combustion of plastics. Traditional halogenated flame retardants may release toxic gases during combustion, while halogen-free flame retardant additives reduce smoke emissions and are more environmentally friendly. Summary of the Invention

[0003] Based on the technical problems existing in the background technology, the present invention proposes a high-efficiency flame-retardant film and its production process.

[0004] The present invention proposes a high-efficiency flame-retardant film, comprising a surface layer, a core layer, and an inner layer.

[0005] Preferably, the surface layer comprises the following raw materials in parts by weight: 10-40 parts copolymer PP, 7-36 parts flame retardant, 0.4-1.5 parts UV stabilizer, 0.01-0.1 parts anti-aging agent, 0.5-3 parts anti-sticking agent, and 0.2-3 parts titanium dioxide masterbatch.

[0006] Preferably, the thickness of the surface layer is 1.0-1.5 μm.

[0007] Preferably, the core layer comprises the following raw materials in parts by weight: 150-200 parts PP, 100-180 parts flame retardant, 6-10 parts UV stabilizer, 0.1-1 part anti-aging agent, and 3-16 parts titanium dioxide masterbatch.

[0008] Preferably, the thickness of the core layer is 26-28 μm.

[0009] Preferably, the inner layer comprises the following raw materials in parts by weight: 10-40 parts PP, 5-35 parts flame retardant, 0.4-1.5 parts UV stabilizer, 0.01-0.1 parts anti-aging agent, 0.5-3 parts anti-sticking agent, and 0.2-3 parts titanium dioxide masterbatch.

[0010] Preferably, the thickness of the inner layer is 1.0-1.5 μm.

[0011] More preferably, the flame retardant includes modified attapulgite, hydroxide, polycarbosilane, and POE.

[0012] More preferably, the method for preparing the flame retardant includes the following steps:

[0013] S1. The modified attapulgite clay is dispersed in solvent A and ultrasonically treated to obtain mixed solution A; mixed solution A is added to hydroxide, mixed evenly, and then dried to obtain mixture A;

[0014] S2. Disperse polycarbosilane in solvent B and stir until homogeneous to obtain mixed solution B; add mixed solution B to mixture A, mix until homogeneous, and then dry to obtain mixture B;

[0015] S3. Disperse γ-methacryloxypropyltrimethoxysilane in solvent C and stir until homogeneous to obtain mixed solution C; add mixed solution C to mixture B, mix until homogeneous, and then dry to obtain mixture C;

[0016] S4. Mix POE with mixture C until homogeneous to obtain the flame retardant.

[0017] More preferably, in S1, solvent A is selected from one or more of ethanol and water.

[0018] More preferably, in S1, the preparation of modified attapulgite clay includes the following steps: after the attapulgite clay is treated at high temperature, it is dispersed in a methanol solution, graphene is added, a solvothermal reaction is carried out, and the clay is washed and dried to obtain modified attapulgite clay.

[0019] More preferably, the high-temperature treatment includes calcination at 400-550°C for 2-3 hours.

[0020] More preferably, the solvothermal reaction includes a reaction at 130-150°C for 8-12 hours.

[0021] More preferably, the mass ratio of attapulgite clay to graphene is (5-10):1.

[0022] More preferably, in S1, the hydroxide includes one or more of magnesium hydroxide and aluminum hydroxide.

[0023] More preferably, the mass ratio of magnesium hydroxide to aluminum hydroxide is (1-3):(1-3).

[0024] More preferably, in S2, solvent B is selected from one or more of methanol and toluene.

[0025] More preferably, in S3, solvent C is selected from one or more of ethanol and acetone.

[0026] More preferably, in S3, the mass ratio of γ-methacryloyloxypropyltrimethoxysilane to mixture B is (0.5-2):100.

[0027] More preferably, the mass ratio of the modified attapulgite clay, hydroxide, polycarbosilane, and POE is (1-5):100:(5-10):(15-20).

[0028] More preferably, the ethylene content in the copolymer PP is 1-4%.

[0029] More preferably, the copolymer PP has a melt index of 4-16 g / 10 min at 230°C and 2.16 kg.

[0030] More preferably, the melt index of the PP at 230℃ and 2.16kg is 1.5-2.0g / 10min.

[0031] More preferably, the UV-resistant agent is selected from one or more of UV-242, UV-284, and UV-531.

[0032] More preferably, the anti-aging agent is selected from one or more of antioxidant 1098 and antioxidant 1010.

[0033] More preferably, the anti-sticking agent is selected from one or more of silica, talc, zeolite, limestone, erucamide, and oleamide.

[0034] More preferably, the titanium dioxide content in the titanium dioxide masterbatch is 50-60%.

[0035] This invention also proposes a production process for a high-efficiency flame-retardant film, comprising the following steps:

[0036] S1. Mix the raw materials of the surface layer, core layer and inner layer evenly, and then extrude them together to obtain a melt;

[0037] S2. The melt is cast, stretched longitudinally, stretched transversely, wound up, and slit to obtain a high-efficiency flame-retardant film.

[0038] Preferably, in S1, the extrusion temperature is 230-250℃.

[0039] Preferably, in S2, the longitudinal stretching ratio is 4.5-5.5.

[0040] Preferably, in S2, the stretching ratio of the horizontal stretch is 9-10.

[0041] The beneficial effects of this invention are as follows:

[0042] This invention relates to a high-efficiency flame-retardant film, comprising a surface layer, a core layer, and an inner layer. The surface layer comprises copolymer PP, flame retardant, UV stabilizer, anti-aging agent, anti-sticking agent, and titanium dioxide masterbatch. The core layer comprises PP, flame retardant, UV stabilizer, anti-aging agent, and titanium dioxide masterbatch. The inner layer comprises PP, flame retardant, UV stabilizer, anti-aging agent, anti-sticking agent, and titanium dioxide masterbatch. The various raw materials in each layer work synergistically to prepare a flame-retardant film that not only has excellent flame-retardant properties but also a certain degree of wear resistance.

[0043] By controlling the thickness of the surface layer to 1.0-1.5μm, the core layer to 26-28μm, and the inner layer to 1.0-1.5μm, the resulting flame-retardant film has a thickness of about 30μm, which can be widely used for coating building materials, decorative materials, floor tiles, and electronic products.

[0044] The flame-retardant film prepared by this invention is a halogen-free flame-retardant film. The "halogen" in halogen-free flame-retardant film refers to halogen elements (including F, Cl, Br, I, At, and Ts) in the periodic table. During combustion, the halogen-free flame-retardant film forms a char layer, preventing heat transfer and oxygen contact, thus achieving a flame-retardant effect. Because it contains no halogen elements, it does not release harmful gases during combustion, complying with international environmental regulations and being environmentally friendly and human health-friendly. The flame retardant includes modified attapulgite, hydroxide, polycarbosilane, and POE. The raw materials work synergistically. By controlling the raw material ratio and preparation process, the obtained flame retardant has good compatibility with the resin, resulting in a flame-retardant film with excellent flame-retardant properties and a certain degree of toughness. The halogen-free flame-retardant film produces less smoke, has a lower density, and is less costly during combustion, while also generating fewer toxic and corrosive gases. The halogen-free flame-retardant film prepared by this invention has a thickness of approximately 30 μm and a density of approximately 0.92 g / cm³. 3 It also has a VTM-0 flame retardant rating.

[0045] This invention adds titanium dioxide masterbatch to the surface layer, core layer, and inner layer. The titanium dioxide masterbatch is similar to resin particles, has good dispersibility, and mixes more evenly, ensuring stable product color.

[0046] This invention adds anti-sticking agents to both the surface and inner layers. By selecting anti-sticking agents with different components for synergistic effects, on the one hand, it helps to create an uneven surface structure on the film, making it easier to peel off when the film layers come into contact with each other; on the other hand, the addition of organic anti-sticking agents has little impact on the transparency of the film and also has a slip-enhancing function, giving the film a low coefficient of friction, preventing scratches on the film surface, and maintaining a high gloss. By using a mixture of anti-sticking agents with different components, this invention can utilize the slip-enhancing effect of organic anti-sticking agents and the anti-sticking properties of inorganic anti-sticking agents, while reducing their respective negative impacts, thus providing both an opening function and a certain degree of slip resistance. Attached Figure Description

[0047] Figure 1 This is a schematic diagram of the high-efficiency flame-retardant membrane structure proposed in this invention, where 1 is the surface layer, 2 is the core layer, and 3 is the inner layer. Detailed Implementation

[0048] The technical solution of the present invention will be described in detail through specific embodiments.

[0049] Unless otherwise specified, all materials and reagents used in the following examples are commercially available.

[0050] Example 1

[0051] A high-efficiency flame-retardant film, comprising a surface layer, a core layer, and an inner layer;

[0052] The surface layer comprises the following raw materials in parts by weight: 25 parts copolymer PP, 20 parts flame retardant, 0.5 parts UV stabilizer, 0.05 parts anti-aging agent, 2 parts anti-sticking agent, and 0.5 parts titanium dioxide masterbatch. The surface layer thickness is 1.0 μm. The melt index of the copolymer PP at 230℃ and 2.16 kg is 4.5 g / 10 min.

[0053] The core layer comprises the following raw materials in parts by weight: 185 parts PP, 160 parts flame retardant, 7 parts UV stabilizer, 0.5 parts anti-aging agent, and 10 parts titanium dioxide masterbatch. The core layer has a thickness of 28 μm.

[0054] The inner layer comprises the following raw materials in parts by weight: 25 parts PP, 20 parts flame retardant, 0.5 parts UV stabilizer, 0.05 parts anti-aging agent, 2.5 parts anti-sticking agent, and 0.5 parts titanium dioxide masterbatch. The thickness of the inner layer is 1.0 μm.

[0055] The UV-resistant agent is UV-531; the anti-aging agent is antioxidant 1098; and the anti-sticking agent is composed of silica, limestone, erucamide, and oleamide in a mass ratio of 1:1:1:1.

[0056] The method for preparing the flame retardant includes the following steps:

[0057] S1. After treating attapulgite clay at 450℃ for 2 hours, it is dispersed in methanol solution, graphene is added, and the mixture is reacted with solvent at 140℃ for 10 hours. After washing and drying, modified attapulgite clay is obtained, wherein the mass ratio of attapulgite clay to graphene is 5:1. The modified attapulgite clay is dispersed in ethanol and ultrasonically treated to obtain mixed solution A. Magnesium hydroxide and aluminum hydroxide are mixed at a mass ratio of 1:3 to obtain hydroxide. Mixed solution A is added to the hydroxide, and after mixing evenly, it is dried to obtain mixture A.

[0058] S2. Disperse polycarbosilane in toluene and stir until homogeneous to obtain mixed solution B; add mixed solution B to mixture A, mix until homogeneous, and then dry to obtain mixture B;

[0059] S3. Disperse γ-methacryloxypropyltrimethoxysilane in ethanol and stir until homogeneous to obtain mixed solution C; add mixed solution C to mixture B, mix until homogeneous, and then dry to obtain mixture C; wherein, the mass ratio of γ-methacryloxypropyltrimethoxysilane to mixture B is 1:100.

[0060] S4. Mix POE with mixture C until homogeneous to obtain the flame retardant;

[0061] The mass ratio of modified attapulgite clay, hydroxide, polycarbosilane, and POE is 3:100:5:15.

[0062] A production process for a high-efficiency flame-retardant film includes the following steps:

[0063] S1. Mix the raw materials of the surface layer, core layer and inner layer evenly, and extrude them together to obtain a melt at an extrusion temperature of 240℃.

[0064] S2. The melt is cast, stretched longitudinally, stretched transversely, wound up, and cut to obtain the following: the stretching ratio of the longitudinal stretch is 4.5, and the stretching ratio of the transverse stretch is 9.5.

[0065] According to the test, the high-efficiency flame retardant film prepared in this embodiment has a flame retardant rating of VTM-0, a friction coefficient of 0.15, and an abrasion amount of 1.23% as tested according to GB / T 1689-2014.

[0066] Example 2

[0067] A high-efficiency flame-retardant film, comprising a surface layer, a core layer, and an inner layer;

[0068] The surface layer comprises the following raw materials in parts by weight: 10 parts copolymer PP, 7 parts flame retardant, 0.4 parts UV stabilizer, 0.02 parts anti-aging agent, 0.5 parts anti-sticking agent, and 0.2 parts titanium dioxide masterbatch. The surface layer thickness is 1.0 μm. The melt index of the copolymer PP at 230℃ and 2.16 kg is 4.5 g / 10 min.

[0069] The core layer comprises the following raw materials in parts by weight: 150 parts PP, 120 parts flame retardant, 6 parts UV stabilizer, 0.3 parts anti-aging agent, and 5 parts titanium dioxide masterbatch. The core layer has a thickness of 28 μm.

[0070] The inner layer comprises the following raw materials in parts by weight: 10 parts PP, 7 parts flame retardant, 0.4 parts UV stabilizer, 0.02 parts anti-aging agent, 0.5 parts anti-sticking agent, and 0.2 parts titanium dioxide masterbatch. The thickness of the inner layer is 1.0 μm.

[0071] The UV stabilizer, anti-aging agent, and flame retardant described are the same as those in Example 1.

[0072] The anti-sticking agent is composed of talc, erucamide, and oleamide in a mass ratio of 1:0.5:1.

[0073] The production process of the high-efficiency flame-retardant film is the same as that in Example 1.

[0074] According to the test, the high-efficiency flame retardant film prepared in this embodiment has a flame retardant rating of VTM-0, a friction coefficient of 0.18, and an wear rate of 1.75% according to GB / T 1689-2014.

[0075] Example 3

[0076] A high-efficiency flame-retardant film, comprising a surface layer, a core layer, and an inner layer;

[0077] The surface layer comprises the following raw materials in parts by weight: 40 parts copolymer PP, 36 parts flame retardant, 1.5 parts UV stabilizer, 0.05 parts anti-aging agent, 3 parts anti-sticking agent, and 2 parts titanium dioxide masterbatch. The surface layer thickness is 1.5 μm. The melt index of the copolymer PP at 230℃ and 2.16 kg is 4.5 g / 10 min.

[0078] The core layer comprises the following raw materials in parts by weight: 200 parts PP, 180 parts flame retardant, 8 parts UV stabilizer, 1 part anti-aging agent, and 15 parts titanium dioxide masterbatch. The core layer has a thickness of 27 μm.

[0079] The inner layer comprises the following raw materials in parts by weight: 40 parts PP, 35 parts flame retardant, 1.5 parts UV stabilizer, 0.05 parts anti-aging agent, 3 parts anti-sticking agent, and 2 parts titanium dioxide masterbatch. The thickness of the inner layer is 1.5 μm.

[0080] The UV-resistant agent, anti-aging agent, and anti-sticking agent are the same as those in Example 1.

[0081] The preparation method of the flame retardant differs from that of Example 1 only in that the mass ratio of modified attapulgite clay, hydroxide, polycarbosilane, and POE is 5:100:6:18.

[0082] The production process of the high-efficiency flame-retardant film is the same as that in Example 1.

[0083] According to the test, the high-efficiency flame retardant film prepared in this embodiment has a flame retardant rating of VTM-0, a friction coefficient of 0.14, and an abrasion rate of 1.08% according to GB / T 1689-2014.

[0084] Example 4

[0085] A high-efficiency flame-retardant film, comprising a surface layer, a core layer, and an inner layer;

[0086] The surface layer comprises the following raw materials in parts by weight: 35 parts copolymer PP, 20 parts flame retardant, 1 part UV stabilizer, 0.05 parts anti-aging agent, 2 parts anti-sticking agent, and 1 part titanium dioxide masterbatch. The surface layer thickness is 1.5 μm. The melt index of the copolymer PP at 230℃ and 2.16 kg is 4.5 g / 10 min.

[0087] The core layer comprises the following raw materials in parts by weight: 180 parts PP, 150 parts flame retardant, 7 parts UV stabilizer, 0.5 parts anti-aging agent, and 8 parts titanium dioxide masterbatch. The core layer has a thickness of 27 μm.

[0088] The inner layer comprises the following raw materials in parts by weight: 35 parts PP, 20 parts flame retardant, 1 part UV stabilizer, 0.05 parts anti-aging agent, 2 parts anti-sticking agent, and 1 part titanium dioxide masterbatch. The thickness of the inner layer is 1.5 μm.

[0089] The UV stabilizer, anti-aging agent, anti-sticking agent, and flame retardant are the same as in Example 1.

[0090] The production process of the high-efficiency flame-retardant film is the same as that in Example 1.

[0091] According to the test, the high-efficiency flame retardant film prepared in this embodiment has a flame retardant rating of VTM-0, a friction coefficient of 0.15, and a wear rate of 1.25% according to GB / T 1689-2014.

[0092] Comparative Example 1

[0093] The difference between Comparative Example 1 and Example 1 is that the flame retardant is a commercially available flame retardant (Zhongmei Magnesium Industry ZM W-QYHM-MX-4), and the anti-sticking agent is composed of silica and limestone in a mass ratio of 1:1.

[0094] According to the test, the flame retardant film prepared in Comparative Example 1 has a flame retardant rating of VTM-1, a friction coefficient of 0.25, and a wear rate of 2.42% according to GB / T 1689-2014.

[0095] In summary, the flame-retardant film provided by this invention has excellent flame-retardant properties and wear resistance.

[0096] The above description is only a preferred embodiment of the present invention, but the scope of protection of the present invention is not limited thereto. Any equivalent substitutions or modifications made by those skilled in the art within the scope of the technology disclosed in the present invention, based on the technical solution and inventive concept of the present invention, should be covered within the scope of protection of the present invention.

Claims

1. A high-efficiency flame-retardant film, characterized in that, It includes a surface layer, a core layer, and an inner layer; the surface layer includes the following raw materials in parts by weight: 10-40 parts copolymer PP, 7-36 parts flame retardant, 0.4-1.5 parts UV stabilizer, 0.01-0.1 parts anti-aging agent, 0.5-3 parts anti-sticking agent, and 0.2-3 parts titanium dioxide masterbatch; The method for preparing the flame retardant includes the following steps: S1. Modified attapulgite clay is dispersed in solvent A and ultrasonically treated to obtain mixed solution A; mixed solution A is added to hydroxide, mixed evenly, and then dried to obtain mixture A; S2. Disperse polycarbosilane in solvent B and stir until homogeneous to obtain mixed solution B; add mixed solution B to mixture A, mix until homogeneous, and then dry to obtain mixture B; S3. Disperse γ-methacryloxypropyltrimethoxysilane in solvent C and stir until homogeneous to obtain mixed solution C; add mixed solution C to mixture B, mix until homogeneous, and then dry to obtain mixture C; S4. Mix POE with mixture C until homogeneous to obtain the flame retardant; In S1, the preparation of modified attapulgite clay includes the following steps: after high-temperature treatment, attapulgite clay is dispersed in methanol solution, graphene is added, a solvothermal reaction is carried out, and the mixture is washed and dried to obtain modified attapulgite clay; the hydroxide includes one or more of magnesium hydroxide and aluminum hydroxide.

2. The high-efficiency flame-retardant film according to claim 1, characterized in that, The core layer comprises the following raw materials in parts by weight: 150-200 parts PP, 100-180 parts flame retardant, 6-10 parts UV stabilizer, 0.1-1 part anti-aging agent, and 3-16 parts titanium dioxide masterbatch.

3. The high-efficiency flame-retardant film according to claim 1, characterized in that, The inner layer comprises the following raw materials in parts by weight: 10-40 parts PP, 5-35 parts flame retardant, 0.4-1.5 parts UV stabilizer, 0.01-0.1 parts anti-aging agent, 0.5-3 parts anti-sticking agent, and 0.2-3 parts titanium dioxide masterbatch.

4. The high-efficiency flame-retardant film according to claim 1, characterized in that, The mass ratio of the modified attapulgite clay, hydroxide, polycarbosilane, and POE is (1-5):100:(5-10):(15-20).

5. The high-efficiency flame-retardant film according to claim 1, characterized in that, The copolymer PP has a melt index of 4-16 g / 10 min at 230℃ and 2.16 kg; the UV stabilizer is selected from one or more of UV-242, UV-284, and UV-531; the anti-aging agent is selected from one or more of antioxidant 1098 and antioxidant 1010; and the anti-sticking agent is selected from one or more of silica, talc, zeolite, limestone, erucamide, and oleamide.

6. A production process for the high-efficiency flame-retardant film according to any one of claims 1-5, characterized in that, Includes the following steps: A1. Mix the raw materials of the surface layer, core layer and inner layer evenly, and then extrude them together to obtain a melt; A2. The melt is cast, stretched longitudinally, stretched laterally, wound up, and slit to obtain a high-efficiency flame-retardant film.

7. The production process according to claim 6, characterized in that, In step A1, the extrusion temperature is 230-250℃.

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