A kind of EPE thermal insulation material and preparation method thereof

Abstract

This application discloses an EPE thermal insulation material and its preparation method. The EPE thermal insulation material comprises an EPE layer, a PE coating layer, and an aluminum foil layer. The EPE layer comprises the following components by weight: 100 parts of LDPE resin pellets; 20-35 parts of polyvinyl butyral; 5-10 parts of a compatibilizer; 5-20 parts of a foaming agent; 1-3 parts of a nucleating agent; and 1-5 parts of an anti-shrinkage agent. The compatibilizer comprises at least maleic anhydride-grafted PE. The melt index of the LDPE resin pellets is 1.5-8 g / 10 min at 190°C / 2.16 kg. The EPE thermal insulation material exhibits excellent toughness and heat resistance, making it suitable for more complex applications.

Description

Technical Field

[0001] The present application relates to the field of EPE materials, and in particular to an EPE thermal insulation material and a preparation method thereof. Background Art

[0002] EPE (Polyethylene Polyethylene Foam) is a new environmentally friendly material. Made primarily of polyethylene resin and a foaming agent, it boasts lightweight, flexible construction, shock absorption, sound insulation, and thermal insulation. It is used not only in construction applications such as wall sound insulation, roof insulation, and floor insulation, but also in packaging, sports equipment, yachts, automobiles, and electronics. EPE building materials are non-toxic, odorless, easy to process, and recyclable, meeting modern demands for environmental protection and energy conservation.

[0003] In construction and packaging, high requirements are placed on the toughness of EPE materials. However, existing EPE materials have poor toughness and are prone to cracking during bending. Summary of the Invention

[0004] In order to improve the toughness of EPE materials and reduce the problem of cracking during bending, the present application provides an EPE thermal insulation material and a preparation method thereof.

[0005] In a first aspect, the present application provides an EPE thermal insulation material, comprising an EPE layer, a PE coating layer, and an aluminum foil layer, wherein the raw materials of the EPE layer include the following components in parts by weight:

[0006] LDPE resin pellets: 100 parts;

[0007] Polyvinyl butyral: 20-35 parts;

[0008] Compatibilizer: 5-10 parts;

[0009] Foaming agent: 5-20 parts;

[0010] Nucleating agent: 1 to 3 parts;

[0011] Anti-shrinkage agent: 1-5 parts;

[0012] The compatibilizer includes at least maleic anhydride grafted PE; and under the conditions of 190° C. / 2.16 kg, the melt index of the LDPE resin pellets is 1.5-8 g / 10 min.

[0013] By employing this technical solution, an appropriate amount of polyvinyl butyral (PVB) is incorporated into the LDPE base resin. With the help of the compatibilizer maleic anhydride grafted onto POE, a relatively uniform PVB dispersed phase is formed within the LDPE resin. These micro-dispersed phases inhibit crack propagation and improve toughness. Furthermore, as a polar compound, PVB exhibits a certain degree of flexibility and ductility. The introduction of more chain segments into the base resin imparts higher toughness and impact resistance.

[0014] In addition, the doping of polar resin can enhance the molecular interaction force between the EPE layer and the PE coating layer, thereby improving the bonding performance.

[0015] Preferably, the hydroxyl value of the polyvinyl butyral is 11 to 20%.

[0016] In the present application, a low hydroxyl value is not conducive to improving its toughness, but an excessively high hydroxyl value is likely to affect the foaming rate and heat resistance of EPE.

[0017] Preferably, the compatibilizer is selected from maleic anhydride grafted POE and maleic anhydride grafted PE in a mass ratio of 1 to 3:1.

[0018] The use of two maleic anhydride-modified polymers in this application can further improve toughness and tensile strength. This may be because maleic anhydride-grafted POE has a strong affinity for polyvinyl butyral, while maleic anhydride-grafted PE has a good affinity for LDPE. The two can work together to improve the compatibility and mutual penetration between the two phases, forming a more uniform mixed phase and improving the toughness and tensile strength of the base resin.

[0019] Preferably, the foaming agent is butane.

[0020] Preferably, the nucleating agent includes one of silicon dioxide, calcium carbonate and talc.

[0021] Preferably, the particle size of the nucleating agent is 0.1 to 1 μm.

[0022] Preferably, the anti-shrinkage agent is monoglyceride.

[0023] Preferably, the raw materials of the EPE thermal insulation material further include 1-2 parts of GY-2013 organosilicon flame retardant.

[0024] Silicone flame retardants offer high thermal stability, long-lasting flame retardancy, and the ability to maintain flame retardancy even in humid environments. Furthermore, the GY-2013 silicone flame retardant used in this application contains epoxy and phosphate functional groups, which can bond with fabric molecules, making it less susceptible to dripping and resulting in superior flame retardancy.

[0025] Preferably, the polyvinyl butyral is boron hybrid polyvinyl butyral, which is mainly made of the following ingredients:

[0026] Polyvinyl butyral: 100 parts;

[0027] Boric acid: 0.5-2 parts;

[0028] Titanium acetylacetonate: 0.05 to 0.1 parts.

[0029] EPE materials have a loose molecular structure and average heat resistance. At high temperatures (60-80°C), internal bubbles expand and increase in volume, causing softening and deformation. To overcome this problem, this application uses boric acid to hybridize polyvinyl butyral. Under the catalysis of titanium acetylacetonate, boron-containing segments are introduced into the polyvinyl butyral to form a hybrid cross-linked network, which can enhance the heat resistance and tensile strength of the EPE material.

[0030] In addition, when the EPE material is subjected to high temperature, the boron hybrid polyvinyl butyral can be combined with the silicone flame retardant to form a silicon-boron flame retardant layer, which covers the surface of the EPE material and has a good flame retardant effect.

[0031] Preferably, the boron hybrid polyvinyl butyral is prepared according to the following method:

[0032] Dissolve polyvinyl butyral and boric acid in ethanol solution, stir evenly, then add titanium acetylacetonate, mix and heat to 50-60°C for reaction, and obtain the product after the reaction is completed.

[0033] Preferably, the reaction time is 3 to 5 hours.

[0034] In a second aspect, the present application provides a method for preparing an EPE thermal insulation material, comprising the following steps:

[0035] Preparation of masterbatch: LDPE resin pellets, polyvinyl butyral and compatibilizer are mixed evenly, extruded at 180±5℃, cooled, pelletized and dried to obtain masterbatch;

[0036] Preparation of EPE layer: Mix the masterbatch with other raw materials evenly, add them into the extrusion foaming machine, and extrude, cool and shape them to obtain the EPE layer;

[0037] Aluminum foil composite: Use the cast film process to spread the PE film on the surface of the EPE layer to obtain the PE film layer, and then composite the aluminum foil on the surface of the PE film layer. After cooling and solidification, the EPE thermal insulation material is obtained.

[0038] Preferably, the LDPE resin pellets used in the EPE layer have a melt index of 1.2 to 2.5 g / 10 min (190° C. / 2.16 kg).

[0039] Preferably, the raw material of the PE coating layer is coating-grade PE.

[0040] Preferably, the thickness of the EPE layer is 1 to 10 mm.

[0041] Preferably, the thickness of the PE coating layer is 10 to 15 μm

[0042] In summary, this application has the following beneficial effects:

[0043] 1. This application uses polyvinyl butyral to modify the PE base resin, which can effectively improve the problems of poor toughness and tensile strength of EPE materials and improve their performance.

[0044] 2. This application uses a combination of maleic anhydride grafted PE and maleic anhydride grafted POE as a compatibilizer, which can further promote the formation of a mixed phase between polyvinyl butyral and PE resin, thereby improving the toughness and tensile strength of the EPE material.

[0045] 3. By adopting boron-hybridized polyvinyl butyral, the present application can significantly improve the human resistance of EPE materials and prevent softening and deformation at high temperatures; at the same time, it can be combined with the organic silicone flame retardant of the present application to significantly improve its flame retardant effect. DETAILED DESCRIPTION

[0046] Preparation Example of Boron Hybrid Polyvinyl Butyral

[0047] Preparation Example 1: A boron hybrid polyvinyl butyral was prepared according to the following method:

[0048] Dissolve 10 kg of polyvinyl butyral (hydroxyl value 13-17%) and 120 g of boric acid in ethanol solution, stir evenly, then add 10 g of titanium acetylacetonate, mix, and heat to 55°C for reaction. After 4 hours, distill to recover ethanol, and filter and dry to obtain the product.

[0049] Preparation Example 2: A boron hybrid polyvinyl butyral was prepared according to the following method:

[0050] Dissolve 10 kg of polyvinyl butyral (hydroxyl value 11.5-13.5%) and 50 g of boric acid in ethanol solution, stir evenly, then add 5 g of titanium acetylacetonate, mix and heat to 55°C for reaction, distill and recover ethanol after 4 hours, filter and dry to obtain the product.

[0051] Preparation Example 3: A boron hybrid polyvinyl butyral was prepared according to the following method:

[0052] Dissolve 10 kg of polyvinyl butyral (hydroxyl value 17.5-20%) and 200 g of boric acid in ethanol solution, stir evenly, then add 10 g of titanium acetylacetonate, mix and heat to 55 ° C for reaction, distill and recover ethanol after 5 hours, filter and dry to obtain the product.

[0053] Example

[0054] Example 1, an EPE thermal insulation material, is prepared according to the following steps:

[0055] Preparation of masterbatch: 100 kg of LDPE resin pellets (grade 2426H, melt index of 1.9 g / 10 min), 25 kg of boron-hybridized polyvinyl butyral obtained in Preparation Example 1, 5 kg of maleic anhydride-grafted POE (grafting rate 1.0-1.3 MA%, melt index 0.6-2.0 g / 10 min (190°C, 2.16 kg)) and 2 kg of maleic anhydride-grafted PE (grafting rate 0.7%, melt index 1.2 g / 10 min (190°C, 2.16 kg)) were mixed evenly, extruded at 180±5°C, cooled, pelletized and dried to obtain masterbatch.

[0056] Preparation of EPE layer: The masterbatch prepared above was mixed evenly with 15 kg of butane, 2 kg of silica (D50 is 0.5 μm), 4 kg of monoglyceride, and 1.8 kg of GY-2013 silicone flame retardant, and added to an extrusion foaming machine. After extrusion, cooling, and shaping, an EPE layer with a thickness of 5 mm was obtained;

[0057] Aluminum foil composite: Use LDPE (brand 1C7A, coating grade) as raw material, add it into the casting machine, spread the PE film on the surface of the EPE layer at 330±5℃ to obtain the PE film layer, composite the aluminum foil on the surface of the PE film layer, and cool and solidify to obtain the EPE thermal insulation material.

[0058] Example 2, an EPE thermal insulation material, is prepared according to the following steps:

[0059] Preparation of masterbatch: 100 kg of LDPE resin pellets (grade 2426H, melt index of 1.9 g / 10 min), 35 kg of boron-hybridized polyvinyl butyral obtained in Preparation Example 2, 6 kg of maleic anhydride-grafted POE (grafting rate 1.0-1.3 MA%, melt index 0.6-2.0 g / 10 min (190°C, 2.16 kg)) and 3 kg of maleic anhydride-grafted PE (grafting rate 0.7%, melt index 1.2 g / 10 min (190°C, 2.16 kg)) were mixed evenly, extruded at 180±5°C, cooled, pelletized and dried to obtain masterbatch.

[0060] Preparation of EPE layer: The masterbatch prepared above was mixed evenly with 20 kg of butane, 3 kg of silica (D50 is 0.5 μm), 5 kg of monoglyceride, and 2 kg of GY-2013 silicone flame retardant, and added to an extrusion foaming machine. After extrusion, cooling, and shaping, an EPE layer with a thickness of 5 mm was obtained;

[0061] Aluminum foil composite: Use LDPE (brand 1C7A, coating grade) as raw material, add it into the casting machine, spread the PE film on the surface of the EPE layer at 330±5℃ to obtain the PE film layer, composite the aluminum foil on the surface of the PE film layer, and cool and solidify to obtain the EPE thermal insulation material.

[0062] Example 3, an EPE thermal insulation material, is prepared according to the following steps:

[0063] Preparation of masterbatch: 100 kg of LDPE resin pellets (grade 2426K, melt index of 4.0 g / 10 min), 20 kg of boron-hybridized polyvinyl butyral obtained in Preparation Example 3, 3 kg of maleic anhydride grafted POE (grafting rate 1.0-1.3 MA%, melt index 0.6-2.0 g / 10 min (190°C, 2.16 kg)) and 3 kg of maleic anhydride grafted PE (grafting rate 0.7%, melt index 1.2 g / 10 min (190°C, 2.16 kg)) were mixed evenly, extruded at 180±5°C, cooled, pelletized and dried to obtain masterbatch.

[0064] Preparation of EPE layer: The masterbatch prepared above was mixed evenly with 8 kg of butane, 1 kg of silica (D50 is 0.5 μm), 5 kg of monoglyceride, and 1 kg of GY-2013 silicone flame retardant, and added to an extrusion foaming machine. After extrusion, cooling, and shaping, an EPE layer with a thickness of 5 mm was obtained;

[0065] Aluminum foil composite: Use LDPE (brand 1C7A, coating grade) as raw material, add it into the casting machine, spread the PE film on the surface of the EPE layer at 330±5℃ to obtain the PE film layer, composite the aluminum foil on the surface of the PE film layer, and cool and solidify to obtain the EPE thermal insulation material.

[0066] Example 4 is an EPE thermal insulation material, which differs from Example 1 in that an equal amount of polyvinyl butyral with a hydroxyl value of 21.5-23.5% is used to replace the polyvinyl butyral with a hydroxyl value of 17.5-20%.

[0067] Example 5, an EPE thermal insulation material, differs from Example 1 in that an equal amount of maleic anhydride grafted POE is used instead of maleic anhydride grafted PE.

[0068] Example 6, an EPE thermal insulation material, differs from Example 1 in that an equal amount of maleic anhydride grafted PE is used instead of maleic anhydride grafted POE.

[0069] Example 7, an EPE thermal insulation material, differs from Example 1 in that an equal amount of FCA-107 organosilicon flame retardant is used instead of GY-2013 organosilicon flame retardant.

[0070] Example 8, an EPE thermal insulation material, differs from Example 1 in that an equal amount of unmodified polyvinyl butyral (hydroxyl value 13-17%) is used to replace the boron-hybridized polyvinyl butyral obtained in Preparation Example 1.

[0071] Comparative Example

[0072] Comparative Example 1 is an EPE thermal insulation material, which differs from Example 8 in that an equal amount of LDPE resin pellets is used to replace polyvinyl butyral in the raw materials of the EPE layer.

[0073] Performance testing

[0074] Test 1: Tensile Properties: The tensile strength and elongation at break of the EPE layer were tested in accordance with GB / T 1040.1-2018, "Determination of Tensile Properties of Plastics," to characterize its toughness. Five tests were performed per group, and the average values were calculated.

[0075] Test 2: Heat Resistance: The load deformation temperature of the EPE layer was tested according to GB / T 1634.2-2019, "Plastics - Determination of Deflection Temperature under Load," at a pressure of 0.45 MPa. Five tests were performed per group, and the average value was calculated.

[0076] Test 3: Flame retardant performance: The flame retardant grade of the EPE layer is determined according to the vertical method specified in GB / T 2408-2021 "National Standard for Determination of Combustion Properties".

[0077] Table 1. Test results

[0078]

[0079]

[0080] Analysis of test results:

[0081] (1) It can be seen from Examples 1 to 8 and Comparative Example 1 in combination with Table 1 that the present application significantly improves the toughness and tensile properties of the EPE material by incorporating polyvinyl butyral into the LDPE resin, which is beneficial to improving the bending properties of the EPE material during use. In addition, the load deformation temperature of the EPE material is also increased, reducing the probability of deformation under thermal conditions. The reason may be that by incorporating an appropriate amount of polyvinyl butyral into the LDPE base resin, under the action of the compatibilizer maleic anhydride grafted POE, a relatively uniform polyvinyl butyral dispersed phase can be formed in the LDPE resin. These tiny dispersed phases can play a role in hindering crack propagation and improving toughness. At the same time, polyvinyl butyral, as a polar compound, has certain flexibility and ductility. Introducing more chain segments into the base resin gives it higher toughness and impact resistance.

[0082] In addition, the polar groups contained in polyvinyl butyral can form intermolecular forces such as hydrogen bonds with the base resin system, thereby improving the heat resistance of EPE materials.

[0083] (2) Combining Examples 1 and 4 with Table 1, it can be seen that the use of polyvinyl butyral with an excessively high hydroxyl value can lead to a decrease in the tensile properties and heat resistance of the EPE layer. This may be because an excessively high hydroxyl value increases the viscosity of the system, resulting in a decrease in the resin processing performance and a decrease in the EPE foaming rate and uniformity. At the same time, excessive polar groups easily generate free radicals under thermal conditions, triggering thermal aging reactions, leading to molecular chain breakage and structural damage, resulting in a decrease in heat resistance.

[0084] (3) Combining Examples 1 and 5-6 with Table 1, it can be seen that the use of maleic anhydride-grafted PE and maleic anhydride-grafted POE polymers for compounding is beneficial to improving the tensile properties of EPE materials. This may be because the two compatibilizers have higher affinity with PE and polyvinyl butyral, respectively, which helps to reduce the interfacial energy, promote the mixing and dispersion of the two phases, form a small dispersed phase, and promote the improvement of toughness and tensile properties.

[0085] (4) Combining Example 1 and Example 7 with Table 1, it can be seen that compared with other organosilicon flame retardants, the flame retardant performance of GY-2013 organosilicon flame retardant is more outstanding.

[0086] (5) Combining Examples 1 and 7 with Table 1, it can be seen that the use of boron-hybridized polyvinyl butyral can significantly improve tensile properties and heat resistance. This may be because the introduction of BOB segments into polyvinyl butyral forms a hybrid cross-linked network, which can enhance the structural strength of the base resin and improve heat resistance and tensile strength.

[0087] This specific embodiment is merely an explanation of the present application and is not a limitation of the present application. After reading this specification, those skilled in the art may make non-creative modifications to the present embodiment as needed, but as long as they are within the scope of the claims of the present application, they are protected by the patent law.

Claims

1. An EPE thermal insulation material, comprising an EPE layer, a PE coating layer and an aluminum foil layer, characterized in that: The EPE layer raw materials include the following components in parts by weight: LDPE resin pellets: 100 parts; Polyvinyl butyral: 20-35 parts; Compatibilizer: 5-10 parts; Foaming agent: 5-20 parts; Nucleating agent: 1 to 3 parts; Anti-shrinkage agent: 1-5 parts; The compatibilizer is selected from maleic anhydride grafted POE and maleic anhydride grafted PE in a mass ratio of 1 to 3:1; at 190° C. / 2.16 kg, the melt index of the LDPE resin pellets is 1.5 to 8 g / 10 min.

2. The EPE thermal insulation material according to claim 1, characterized in that: The hydroxyl value of the polyvinyl butyral is 11 to 20%.

3. The EPE thermal insulation material according to claim 1, characterized in that: The foaming agent is butane.

4. The EPE thermal insulation material according to claim 1, characterized in that: The nucleating agent includes one or more of silicon dioxide, calcium carbonate, and talc.

5. The EPE thermal insulation material according to claim 1, characterized in that: The anti-shrinkage agent is monoglyceride.

6. The EPE thermal insulation material according to claim 1, characterized in that: The polyvinyl butyral is boron hybrid polyvinyl butyral, which is mainly made of the following components: Polyvinyl butyral: 100 parts; Boric acid: 0.5-2 parts; Titanium acetylacetonate: 0.05 to 0.1 parts.

7. The EPE thermal insulation material according to claim 6, characterized in that: The boron hybrid polyvinyl butyral is prepared according to the following method: Dissolve polyvinyl butyral and boric acid in ethanol solution, stir evenly, then add titanium acetylacetonate, mix and heat to 50-60°C for reaction, and obtain the product after the reaction is completed.

8. A method for preparing an EPE thermal insulation material according to any one of claims 1 to 7, characterized in that: The steps include: Preparation of masterbatch: LDPE resin pellets, polyvinyl butyral and compatibilizer are mixed evenly, extruded at 180±5℃, cooled, pelletized and dried to obtain masterbatch; Preparation of EPE layer: Mix the masterbatch with other raw materials evenly, add them into the extrusion foaming machine, and extrude, cool and shape them to obtain the EPE layer; Aluminum foil composite: Use the cast film process to spread the PE film on the surface of the EPE layer to obtain the PE film layer, and then composite the aluminum foil on the surface of the PE film layer. After cooling and solidification, the EPE thermal insulation material is obtained.

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