Thermal and fire insulation material and method for producing the same

Abstract

The application discloses a kind of heat-insulating fireproof materials and preparation method thereof, from top to bottom sequentially include first encapsulation layer, first fireproof support layer, first viscose layer, heat-insulating layer, second viscose layer, second fireproof support layer and second encapsulation layer;The first viscose layer, second viscose layer are independently made of the following raw materials respectively: amino-terminated hyperbranched polyimide, acrylic modified poly (ether ether ketone), 1,3-bis (oxymethylene methyl) -5- (2-propenyl) -1,3,5-triazine-2,4,6 (1H,3H,5H) -trione, 1,1,3,3-tetramethyl-1,3-divinyl disilazane, 3- (1,1-difluoro-2-propylene-1-yl) -2 (1H) -quinoxaline ketone, 2- (1-propylene-2-yl) benzo [d] oxazole, terpene resin, initiator, solvent.The material heat-insulating fireproof effect is remarkable, and mechanical mechanical property and high temperature resistance are sufficient.

Description

Technical Field

[0001] This invention relates to the field of fireproof materials technology, and in particular to a heat-insulating fireproof material and its preparation method. Background Technology

[0002] New energy batteries are one of the most important components of new energy electric vehicles. With the increasing popularity of new energy electric vehicles, the safety of these batteries is receiving growing attention. Vehicle-mounted new energy batteries have large capacities and high motor power. The rapid charging and discharging of these batteries results in a heavy thermal load on the battery system. The accumulation of heat inside the battery causes a rapid rise in temperature. When the thermal load reaches a certain level, thermal runaway can easily occur, leading to fires and / or explosions. Furthermore, because thermal runaway typically reacts very quickly and with tremendous force, it poses a serious threat to the safety of drivers and passengers.

[0003] To effectively control thermal runaway and avoid serious safety accidents, thermal and fire-resistant materials are typically used to create thermal and fire-resistant barriers between the battery cells and modules in new energy battery packs. These materials make efficient use of the limited space within the battery pack, allowing heat-generating components to coexist with heat-sensitive components within a confined space. Furthermore, in extreme thermal runaway scenarios, they maximally prevent the runaway component from causing thermal shock to other normal components, thus minimizing the risk of larger-area thermal runaway. Therefore, the performance of thermal and fire-resistant materials directly affects the safety, efficiency, and cycle life of the power battery.

[0004] Existing heat-insulating and fire-resistant materials suffer from limitations in heat-insulating and fire-resistant performance, insufficient mechanical and temperature resistance, and a need for further service life extension. To address these issues, Chinese invention patent document CN103342845B discloses a fire-resistant material comprising a matrix resin, a foaming agent, and a flame retardant. The weight percentages of the components are: polyolefin 15%–60%, foaming agent 0.5%–30%, and flame retardant 20%–80%; the foaming agent is aluminum hydroxide. This invention provides a fire-resistant material with improved processing fluidity and ease of processing, and features lightweight, flame retardancy, heat insulation, and low cost. However, its high-temperature resistance and mechanical properties still require further improvement.

[0005] It is evident that there is still a need in this field to develop a heat-insulating and fire-resistant material with significant heat insulation and fireproofing effects, sufficient mechanical and high-temperature resistance, and a long service life. Summary of the Invention

[0006] The main objective of this invention is to provide a heat-insulating and fire-resistant material with significant heat insulation and fireproofing effects, sufficient mechanical and high-temperature resistance, and a long service life.

[0007] To achieve the above objectives, the present invention provides a heat-insulating and fire-resistant material, comprising, from top to bottom, a first encapsulation layer, a first fire-resistant support layer, a first adhesive layer, a heat-insulating layer, a second adhesive layer, a second fire-resistant support layer, and a second encapsulation layer; the first adhesive layer and the second adhesive layer are independently made from the following raw materials in parts by weight: 10-15 parts of amino-terminated hyperbranched polyimide, 15-25 parts of acrylic acid-modified polyetheretherketone, and 1,3-bis(epoxyethylenemethyl)-5 3-5 parts of 1,1,3,3-tetramethyl-1,3-divinyldisilazane, 1-3 parts of 3-(1,1-difluoro-2-propen-1-yl)-2(1H)-quinoxalone, 1-3 parts of 2-(1-propen-2-yl)benzo[d]oxazole, 8-10 parts of terpene resin, 1-2 parts of initiator, and 30-50 parts of solvent.

[0008] Preferably, there are no special requirements regarding the source of the amino-terminated hyperbranched polyimide. In one embodiment of the present invention, the amino-terminated hyperbranched polyimide is prepared according to the method of Example 1 in Chinese Invention Patent CN107789677B.

[0009] Preferably, there are no special requirements for the source of the acrylic-modified polyether ether ketone. In one embodiment of the present invention, the acrylic-modified polyether ether ketone is prepared according to the method of Example 1 in Chinese Invention Patent CN109337019B.

[0010] Preferably, the terpene resin is terpene resin T-80.

[0011] Preferably, the initiator is azobisisobutyronitrile; and the solvent is at least one of N,N-dimethylformamide and N-methylpyrrolidone.

[0012] Preferably, both the first encapsulation layer and the second encapsulation layer are made of any one of PET film, PP film, PE film, PVC film, PI film, and single-sided aluminized PET film.

[0013] Preferably, the first fireproof support layer and the second fireproof support layer are independently made of woven fabrics, braided fabrics or non-woven fabrics composed of aramid fibers, glass fibers, mullite fibers, basalt fibers, carbon fibers and other fibers with flame-retardant functions.

[0014] Preferably, the heat insulation layer is formed by pressing the following raw materials in parts by weight: 8-12 parts fumed silica, 10-20 parts aerogel particles, 1-3 parts infrared shading agent, 8-12 parts heat-resistant filler, and 0.5-2.5 parts chopped fibers.

[0015] Preferably, the fumed silica is hydrophobic nano-sized fumed silica DECONS® E-65.

[0016] Preferably, the aerogel particles are one or more of silica aerogel, phenolic aerogel, or polyimide aerogel; the average diameter of the aerogel particles is 0.5-10 μm.

[0017] Preferably, the silica aerogel is CABOT silica aerogel.

[0018] Preferably, the infrared shading agent is at least one of silicon carbide, anatase titanium dioxide, carbon black, and potassium hexatitanate whiskers; the particle size of the infrared shading agent is 800-1200 mesh.

[0019] Preferably, the heat-resistant filler is at least one of calcium carbonate, talc, mica, wollastonite, and bauxite; the particle size of the heat-resistant filler is 1000-1300 mesh.

[0020] Preferably, the chopped fiber is at least one of basalt chopped fiber, carbon chopped fiber, mullite chopped fiber, glass chopped fiber, and rock wool chopped fiber.

[0021] Preferably, the average diameter of the chopped fibers is 9-13 μm and the chopped length is 3-6 mm.

[0022] Another object of the present invention is to provide a method for preparing the aforementioned heat-insulating and fire-resistant material, comprising the following steps:

[0023] Step S1: Mix all the raw materials of the heat insulation layer evenly and place them in a mold. Press the mold with a press and then cut the resulting sample into the required shape using a laser.

[0024] Step S2: After mixing all the raw materials of the first adhesive layer evenly, apply it to one side of the first fireproof support layer to form the first adhesive layer. After mixing all the raw materials of the second adhesive layer evenly, apply it to one side of the second fireproof support layer to form the second adhesive layer. Then, attach the first adhesive layer and the second adhesive layer to the upper and lower surfaces of the heat insulation layer respectively and heat cure them to form the second adhesive layer.

[0025] Step S3: Place the material prepared in step S2 into a packaging bag, first evacuate it, then heat press it, then release the pressure and open the mold, and finally cut the sealing edge to a suitable width to obtain the heat insulation and fireproof material.

[0026] Preferably, the thermosetting temperature in step S2 is 110-130℃ and the time is 20-30 min.

[0027] Preferably, the hot pressing pressure in step S3 is 0.1-1 MPa, the temperature is 85-110℃, and the time is 10-20 s.

[0028] Due to the application of the above technical solution, the present invention has the following beneficial effects:

[0029] (1) The method for preparing heat-insulating and fireproof materials disclosed in this invention is simple, easy to operate and control, low in energy consumption, low in dependence on equipment, high in preparation efficiency and finished product qualification rate, suitable for continuous large-scale production, and has high promotion and application value.

[0030] (2) The heat insulation and fireproof material disclosed in this invention adopts a structural design that includes a first encapsulation layer, a first fireproof support layer, a first adhesive layer, a heat insulation layer, a second adhesive layer, a second fireproof support layer and a second encapsulation layer from top to bottom, which reduces temperature exchange and improves the heat insulation and fireproof effect; the setting of the fireproof support layer can also improve the mechanical properties of the material and avoid the damage caused by thermal shock during thermal runaway.

[0031] (3) The heat-insulating and fire-resistant material disclosed in this invention is wherein the heat-insulating layer is formed by pressing the following raw materials in parts by weight: 8-12 parts of fumed silica, 10-20 parts of aerogel particles, 1-3 parts of infrared shading agent, 8-12 parts of heat-resistant filler, and 0.5-2.5 parts of chopped fiber. Through the synergistic effect of the raw materials, the resulting material has significant heat-insulating and fire-resistant effects, sufficient high-temperature resistance, and a long service life; the addition of chopped fiber can be evenly dispersed in the heat-insulating layer, thereby enhancing the formability of the heat-insulating layer and improving the mechanical properties of the material.

[0032] (4) The heat-insulating and fire-resistant material disclosed in this invention is made of the following raw materials in parts by weight, independently of each other: 10-15 parts of amino-terminated hyperbranched polyimide, 15-25 parts of acrylic acid-modified polyether ether ketone, 3-5 parts of 1,3-bis(epoxyethylenemethyl)-5-(2-propenyl)-1,3,5-triazine-2,4,6(1H,3H,5H)-trione, 0.5-0.8 parts of 1,1,3,3-tetramethyl-1,3-divinyldisilazane, 1-3 parts of 3-(1,1-difluoro-2-propen-1-yl)-2(1H)-quinoxalone, 1-3 parts of 2-(1-propen-2-yl)benzo[d]oxazole, 8-10 parts of terpene resin, 1-2 parts of initiator, and 30-50 parts of solvent. Through the synergistic effect of various raw materials, hyperbranched polyimide, polyetheretherketone, triazine ketone, silazane, fluoroquinoxalone, benzoxazole, and terpene resin structures are simultaneously introduced into the adhesive layer structure. Under the multiple effects of electronic effects, steric hindrance effects, and conjugation effects, the resulting adhesive layer has good bonding performance, excellent high temperature resistance, and good heat insulation and fire resistance. It effectively avoids delamination during the use of the material, thereby improving the overall structural strength of the material and extending its service life. Detailed Implementation

[0033] The following description is intended to disclose the invention and enable those skilled in the art to implement it. The preferred embodiments described below are merely examples, and other obvious variations will occur to those skilled in the art.

[0034] The phenolic aerogel described in the various embodiments of the present invention is a phenolic aerogel prepared according to the method of Example 1 in Chinese Invention Patent Document CN201910814350.4; the polyimide aerogel is a polyimide aerogel prepared according to the method of Example 1 in Chinese Invention Patent Document CN201910988262.6. Example 1

[0035] A heat-insulating and fire-resistant material, comprising, from top to bottom, a first encapsulation layer, a first fire-resistant support layer, a first adhesive layer, a heat-insulating layer, a second adhesive layer, a second fire-resistant support layer, and a second encapsulation layer; the first adhesive layer and the second adhesive layer are independently made from the following raw materials in parts by weight: 10 parts of amino-terminated hyperbranched polyimide, 15 parts of acrylic acid-modified polyetheretherketone, 3 parts of 1,3-bis(epoxyethylenemethyl)-5-(2-propenyl)-1,3,5-triazine-2,4,6(1H,3H,5H)-trione, 0.5 parts of 1,1,3,3-tetramethyl-1,3-divinyldisilazane, 1 part of 3-(1,1-difluoro-2-propen-1-yl)-2(1H)-quinoxalone, 1 part of 2-(1-propen-2-yl)benzo[d]oxazole, 8 parts of terpene resin, 1 part of initiator, and 30 parts of solvent.

[0036] The amino-terminated hyperbranched polyimide is prepared according to the method of Example 1 in Chinese Invention Patent CN107789677B; the source of the acrylic acid-modified polyether ketone is not particularly required. In one embodiment of the present invention, the acrylic acid-modified polyether ketone is prepared according to the method of Example 1 in Chinese Invention Patent CN109337019B; the terpene resin is terpene resin T-80.

[0037] The initiator is azobisisobutyronitrile; the solvent is N,N-dimethylformamide; both the first encapsulation layer and the second encapsulation layer are made of PET film.

[0038] The first fireproof support layer and the second fireproof support layer are independently made of woven fabric composed of aramid fibers; the heat insulation layer is made of the following raw materials pressed in parts by weight: 8 parts fumed silica, 10 parts aerogel particles, 1 part infrared shading agent, 8 parts heat-resistant filler, and 0.5 parts chopped fibers.

[0039] The fumed silica is hydrophobic nano-sized fumed silica DECONS® E-65; the aerogel particles are silica aerogel with an average diameter of 0.5 μm; the silica aerogel is CABOT silica aerogel; the infrared opacifier is silicon carbide with a particle size of 800 mesh; the heat-resistant filler is calcium carbonate with a particle size of 1000 mesh; the chopped fibers are basalt chopped fibers with an average diameter of 9 μm and a chopped length of 3 mm.

[0040] A method for preparing the aforementioned heat-insulating and fire-resistant material includes the following steps:

[0041] Step S1: Mix all the raw materials of the heat insulation layer evenly and place them in a mold. Press the mold with a press and then cut the resulting sample into the required shape using a laser.

[0042] Step S2: After mixing all the raw materials of the first adhesive layer evenly, apply it to one side of the first fireproof support layer to form the first adhesive layer. After mixing all the raw materials of the second adhesive layer evenly, apply it to one side of the second fireproof support layer to form the second adhesive layer. Then, attach the first adhesive layer and the second adhesive layer to the upper and lower surfaces of the heat insulation layer respectively and heat cure them to form the second adhesive layer.

[0043] Step S3: Place the material prepared in step S2 into a packaging bag, first evacuate it, then heat press it, then release the pressure and open the mold, and finally cut the sealing edge to a suitable width to obtain the heat insulation and fireproof material.

[0044] In step S2, the thermosetting temperature is 110℃ and the time is 20min; in step S3, the hot pressing pressure is 0.1MPa, the temperature is 85℃, and the time is 10s. Example 2

[0045] A heat-insulating and fire-resistant material, comprising, from top to bottom, a first encapsulation layer, a first fire-resistant support layer, a first adhesive layer, a heat-insulating layer, a second adhesive layer, a second fire-resistant support layer, and a second encapsulation layer; the first adhesive layer and the second adhesive layer are independently made from the following raw materials in parts by weight: 11 parts of amino-terminated hyperbranched polyimide, 18 parts of acrylic acid-modified polyetheretherketone, and 1,3-bis(epoxyethylenemethyl)-5-(2-propanediol). 3.5 parts of alkenyl)-1,3,5-triazine-2,4,6(1H,3H,5H)-trione, 0.6 parts of 1,1,3,3-tetramethyl-1,3-divinyldisilazane, 1.5 parts of 3-(1,1-difluoro-2-propen-1-yl)-2(1H)-quinoxalone, 1.5 parts of 2-(1-propen-2-yl)benzo[d]oxazole, 8.5 parts of terpene resin, 1.2 parts of initiator, and 35 parts of solvent.

[0046] The amino-terminated hyperbranched polyimide is prepared according to the method of Example 1 in Chinese Invention Patent CN107789677B; the acrylic acid-modified polyether ether ketone is prepared according to the method of Example 1 in Chinese Invention Patent CN109337019B; the terpene resin is terpene resin T-80; the initiator is azobisisobutyronitrile; the solvent is N-methylpyrrolidone; both the first encapsulation layer and the second encapsulation layer are made of PP film; the first fireproof support layer and the second fireproof support layer are independently made of woven fabric composed of glass fiber.

[0047] The heat insulation layer is formed by pressing the following raw materials in parts by weight: 9 parts fumed silica, 12 parts aerogel particles, 1.5 parts infrared shading agent, 9 parts heat-resistant filler, and 1 part chopped fiber; the fumed silica is hydrophobic nano-sized fumed silica DECONS® E-65; the aerogel particles are phenolic aerogel with an average diameter of 2 μm; the infrared shading agent is anatase titanium dioxide with a particle size of 900 mesh; the heat-resistant filler is talc with a particle size of 1100 mesh; and the chopped fiber is carbon chopped fiber with an average diameter of 10 μm and a chopped length of 4 mm.

[0048] A method for preparing the aforementioned heat-insulating and fire-resistant material includes the following steps:

[0049] Step S1: Mix all the raw materials of the heat insulation layer evenly and place them in a mold. Press the mold with a press and then cut the resulting sample into the required shape using a laser.

[0050] Step S2: After mixing all the raw materials of the first adhesive layer evenly, apply it to one side of the first fireproof support layer to form the first adhesive layer. After mixing all the raw materials of the second adhesive layer evenly, apply it to one side of the second fireproof support layer to form the second adhesive layer. Then, attach the first adhesive layer and the second adhesive layer to the upper and lower surfaces of the heat insulation layer respectively and heat cure them to form the second adhesive layer.

[0051] Step S3: Place the material prepared in step S2 into a packaging bag, first evacuate it, then heat press it, then release the pressure and open the mold, and finally cut the sealing edge to a suitable width to obtain the heat insulation and fireproof material.

[0052] In step S2, the thermosetting temperature is 115℃ and the time is 23min; in step S3, the hot pressing pressure is 0.4MPa, the temperature is 95℃, and the time is 12s. Example 3

[0053] A heat-insulating and fire-retardant material, comprising, from top to bottom, a first encapsulation layer, a first fire-retardant support layer, a first adhesive layer, a heat-insulating layer, a second adhesive layer, a second fire-retardant support layer, and a second encapsulation layer; the first adhesive layer and the second adhesive layer are independently made from the following raw materials in parts by weight: 13 parts of amino-terminated hyperbranched polyimide, 20 parts of acrylic acid-modified polyetheretherketone, and 1,3-bis(epoxyethylenemethyl)-5-( 4 parts of 2-propenyl)-1,3,5-triazine-2,4,6(1H,3H,5H)-trione, 0.65 parts of 1,1,3,3-tetramethyl-1,3-divinyldisilazane, 2 parts of 3-(1,1-difluoro-2-propen-1-yl)-2(1H)-quinoxalone, 2 parts of 2-(1-propen-2-yl)benzo[d]oxazole, 9 parts of terpene resin, 1.5 parts of initiator, and 40 parts of solvent.

[0054] The amino-terminated hyperbranched polyimide is prepared according to the method of Example 1 in Chinese Invention Patent CN107789677B; the acrylic acid-modified polyether ether ketone is prepared according to the method of Example 1 in Chinese Invention Patent CN109337019B; the terpene resin is terpene resin T-80; the initiator is azobisisobutyronitrile; the solvent is N,N-dimethylformamide; both the first encapsulation layer and the second encapsulation layer are made of PE film; the first fireproof support layer and the second fireproof support layer are independently made of nonwoven fabric composed of mullite fibers.

[0055] The heat insulation layer is formed by pressing the following raw materials in parts by weight: 10 parts fumed silica, 15 parts aerogel particles, 2 parts infrared shading agent, 10 parts heat-resistant filler, and 1.5 parts chopped fibers; the fumed silica is hydrophobic nano-sized fumed silica DECONS® E-65; the aerogel particles are polyimide aerogel; the average diameter of the aerogel particles is 6 μm.

[0056] The infrared shading agent is carbon black; the particle size of the infrared shading agent is 1000 mesh; the heat-resistant filler is mica; the particle size of the heat-resistant filler is 1150 mesh; the chopped fiber is mullite chopped fiber; the average diameter of the chopped fiber is 11 μm, and the chopped length is 4.5 mm.

[0057] A method for preparing the aforementioned heat-insulating and fire-resistant material includes the following steps:

[0058] Step S1: Mix all the raw materials of the heat insulation layer evenly and place them in a mold. Press the mold with a press and then cut the resulting sample into the required shape using a laser.

[0059] Step S2: After mixing all the raw materials of the first adhesive layer evenly, apply it to one side of the first fireproof support layer to form the first adhesive layer. After mixing all the raw materials of the second adhesive layer evenly, apply it to one side of the second fireproof support layer to form the second adhesive layer. Then, attach the first adhesive layer and the second adhesive layer to the upper and lower surfaces of the heat insulation layer respectively and heat cure them to form the second adhesive layer.

[0060] Step S3: Place the material prepared in step S2 into a packaging bag, first evacuate it, then heat press it, then release the pressure and open the mold, and finally cut the sealing edge to a suitable width to obtain the heat insulation and fireproof material.

[0061] In step S2, the thermosetting temperature is 120℃ and the time is 25min; in step S3, the hot pressing pressure is 0.6MPa, the temperature is 100℃, and the time is 15s. Example 4

[0062] A heat-insulating and fire-retardant material, comprising, from top to bottom, a first encapsulation layer, a first fire-retardant support layer, a first adhesive layer, a heat-insulating layer, a second adhesive layer, a second fire-retardant support layer, and a second encapsulation layer; the first adhesive layer and the second adhesive layer are independently made from the following raw materials in parts by weight: 14 parts of amino-terminated hyperbranched polyimide, 24 parts of acrylic acid-modified polyetheretherketone, and 1,3-bis(epoxyethylenemethyl)-5-(2-propylene) 4.5 parts of 1,1,3,3-tetramethyl-1,3-divinyldisilazane, 2.5 parts of 3-(1,1-difluoro-2-propen-1-yl)-2(1H)-quinoxalone, 2.5 parts of 2-(1-propen-2-yl)benzo[d]oxazole, 9.5 parts of terpene resin, 1.8 parts of initiator, and 45 parts of solvent.

[0063] The amino-terminated hyperbranched polyimide is prepared according to the method of Example 1 in Chinese Invention Patent CN107789677B; the acrylic acid-modified polyether ether ketone is prepared according to the method of Example 1 in Chinese Invention Patent CN109337019B; the terpene resin is terpene resin T-80; the initiator is azobisisobutyronitrile; the solvent is a mixture of N,N-dimethylformamide and N-methylpyrrolidone in a mass ratio of 3:5; both the first encapsulation layer and the second encapsulation layer are made of PVC film; the first fireproof support layer and the second fireproof support layer are independently made of woven fabric composed of basalt fiber.

[0064] The heat insulation layer is formed by pressing the following raw materials in parts by weight: 11 parts fumed silica, 18 parts aerogel particles, 2.5 parts infrared shading agent, 11 parts heat-resistant filler, and 2 parts chopped fibers; the fumed silica is hydrophobic nano-sized fumed silica DECONS® E-65; the aerogel particles are a mixture of silica aerogel, phenolic aerogel, and polyimide aerogel in a mass ratio of 1:2:1; the average diameter of the aerogel particles is 9 μm; the silica aerogel is CABOT silica aerogel; the infrared shading agent is a mixture of silicon carbide, anatase titanium dioxide, carbon black, and potassium hexatitanate whiskers in a mass ratio of 1:1:2:1; the particle size of the infrared shading agent is 1100 mesh.

[0065] The heat-resistant filler is a mixture of calcium carbonate, talc, mica, wollastonite, and bauxite in a mass ratio of 1:2:3:2:2; the particle size of the heat-resistant filler is 1250 mesh; the chopped fibers are a mixture of basalt chopped fibers, carbon chopped fibers, mullite chopped fibers, glass chopped fibers, and rock wool chopped fibers in a mass ratio of 1:1:3:5:2; the average diameter of the chopped fibers is 12 μm, and the chopped length is 5.5 mm.

[0066] A method for preparing the aforementioned heat-insulating and fire-resistant material includes the following steps:

[0067] Step S1: Mix all the raw materials of the heat insulation layer evenly and place them in a mold. Press the mold with a press and then cut the resulting sample into the required shape using a laser.

[0068] Step S2: After mixing all the raw materials of the first adhesive layer evenly, apply it to one side of the first fireproof support layer to form the first adhesive layer. After mixing all the raw materials of the second adhesive layer evenly, apply it to one side of the second fireproof support layer to form the second adhesive layer. Then, attach the first adhesive layer and the second adhesive layer to the upper and lower surfaces of the heat insulation layer respectively and heat cure them to form the second adhesive layer.

[0069] Step S3: Place the material prepared in step S2 into a packaging bag, first evacuate it, then heat press it, then release the pressure and open the mold, and finally cut the sealing edge to a suitable width to obtain the heat insulation and fireproof material.

[0070] In step S2, the thermosetting temperature is 125℃ and the time is 28min; in step S3, the hot pressing pressure is 0.9MPa, the temperature is 108℃, and the time is 18s. Example 5

[0071] A heat-insulating and fire-retardant material, comprising, from top to bottom, a first encapsulation layer, a first fire-retardant support layer, a first adhesive layer, a heat-insulating layer, a second adhesive layer, a second fire-retardant support layer, and a second encapsulation layer; the first adhesive layer and the second adhesive layer are independently made from the following raw materials in parts by weight: 15 parts of amino-terminated hyperbranched polyimide, 25 parts of acrylic acid-modified polyetheretherketone, 5 parts of 1,3-bis(epoxyethylenemethyl)-5-(2-propenyl)-1,3,5-triazine-2,4,6(1H,3H,5H)-trione, 0.8 parts of 1,1,3,3-tetramethyl-1,3-divinyldisilazane, 3 parts of 3-(1,1-difluoro-2-propen-1-yl)-2(1H)-quinoxalone, 3 parts of 2-(1-propen-2-yl)benzo[d]oxazole, 10 parts of terpene resin, 2 parts of initiator, and 50 parts of solvent.

[0072] The amino-terminated hyperbranched polyimide is prepared according to the method of Example 1 in Chinese Invention Patent CN107789677B; the acrylic acid-modified polyether ether ketone is prepared according to the method of Example 1 in Chinese Invention Patent CN109337019B; the terpene resin is terpene resin T-80; the initiator is azobisisobutyronitrile; the solvent is N,N-dimethylformamide; both the first encapsulation layer and the second encapsulation layer are made of PI film; the first fireproof support layer and the second fireproof support layer are independently made of nonwoven fabric composed of carbon fiber.

[0073] The heat insulation layer is formed by pressing the following raw materials in parts by weight: 12 parts fumed silica, 20 parts aerogel particles, 3 parts infrared shading agent, 12 parts heat-resistant filler, and 2.5 parts chopped fibers; the fumed silica is hydrophobic nano-sized fumed silica DECONS® E-65; the aerogel particles are silica aerogel; the average diameter of the aerogel particles is 10 μm; the silica aerogel is CABOT silica aerogel; the infrared shading agent is potassium hexatitanate whiskers; the particle size of the infrared shading agent is 1200 mesh.

[0074] The heat-resistant filler is bauxite; the particle size of the heat-resistant filler is 1300 mesh; the chopped fiber is rock wool chopped fiber; the average diameter of the chopped fiber is 13μm and the chopped length is 6mm.

[0075] A method for preparing the aforementioned heat-insulating and fire-resistant material includes the following steps:

[0076] Step S1: Mix all the raw materials of the heat insulation layer evenly and place them in a mold. Press the mold with a press and then cut the resulting sample into the required shape using a laser.

[0077] Step S2: After mixing all the raw materials of the first adhesive layer evenly, apply it to one side of the first fireproof support layer to form the first adhesive layer. After mixing all the raw materials of the second adhesive layer evenly, apply it to one side of the second fireproof support layer to form the second adhesive layer. Then, attach the first adhesive layer and the second adhesive layer to the upper and lower surfaces of the heat insulation layer respectively and heat cure them to form the second adhesive layer.

[0078] Step S3: Place the material prepared in step S2 into a packaging bag, first evacuate it, then heat press it, then release the pressure and open the mold, and finally cut the sealing edge to a suitable width to obtain the heat insulation and fireproof material.

[0079] In step S2, the thermosetting temperature is 130℃ and the time is 30min; in step S3, the hot pressing pressure is 1MPa, the temperature is 110℃, and the time is 20s.

[0080] Comparative Example 1

[0081] This invention provides a heat-insulating and fire-resistant material, which is similar to Example 1, except that it does not contain 1,3-bis(epoxyethylenemethyl)-5-(2-propenyl)-1,3,5-triazine-2,4,6(1H,3H,5H)-trione and 1,1,3,3-tetramethyl-1,3-divinyldisilazane.

[0082] Comparative Example 2

[0083] The present invention provides a heat-insulating and fire-resistant material, which is similar to that of Example 1, except that it does not contain 3-(1,1-difluoro-2-propen-1-yl)-2(1H)-quinoxalone and 2-(1-propen-2-yl)benzo[d]oxazole.

[0084] The heat-insulating and fire-resistant material samples prepared in Examples 1-5 and Comparative Examples 1-2 were subjected to relevant performance tests. To control variables, the thickness of each layer in each heat-insulating and fire-resistant material sample was controlled as follows: first encapsulation layer 0.1 mm, first fire-resistant support layer 0.4 mm, first adhesive layer 0.02 mm, heat insulation layer 2 mm, second adhesive layer 0.02 mm, second fire-resistant support layer 0.4 mm, and second encapsulation layer 0.1 mm. The test results are shown in Table 1, and the test methods are as follows:

[0085] (1) Flame retardancy: tested according to UL-94.

[0086] (2) Ablation resistance: The material was continuously burned with an oxyacetylene flame at 1300℃, and the time it took to burn through was recorded. The gas pressure was about 0.4 MPa.

[0087] (3) Thermal conductivity: Tested according to GB / T10295-2008.

[0088] As can be seen from Table 1, the heat-insulating and fire-retardant material disclosed in the embodiments of the present invention has superior fire resistance and heat insulation performance compared with the comparative product, and better ablation performance. The addition of bis(epoxyethylenemethyl)-5-(2-propenyl)-1,3,5-triazine-2,4,6(1H,3H,5H)-trione, 1,1,3,3-tetramethyl-1,3-divinyldisilazane, 3-(1,1-difluoro-2-propen-1-yl)-2(1H)-quinoxalone and 2-(1-propen-2-yl)benzo[d]oxazole are all beneficial to improving the above-mentioned performance.

[0089] Table 1

[0090] project Flame retardancy ablation resistance thermal conductivity unit class min W / (m·K) Example 1 V-0 >40min 0.050 Example 2 V-0 >42min 0.046 Example 3 V-0 >45min 0.041 Example 4 V-0 >46min 0.038 Example 5 V-0 >51min 0.034 Comparative Example 1 V-1 <30min 0.092 Comparative Example 2 V-1 <25min 0.079

[0091] The foregoing has shown and described the basic principles, main features, and advantages of the present invention. Those skilled in the art should understand that the present invention is not limited to the above embodiments. The embodiments and descriptions in the specification are merely principles of the invention. Various changes and modifications can be made to the invention without departing from its spirit and scope, and all such changes and modifications fall within the scope of the claimed invention. The scope of protection claimed by the appended claims and their equivalents is defined.

Claims

1. A thermal and fire barrier material, characterized in that, From top to bottom, it comprises a first encapsulation layer, a first fireproof support layer, a first adhesive layer, a heat insulation layer, a second adhesive layer, a second fireproof support layer and a second encapsulation layer; the first adhesive layer and the second adhesive layer are independently made of the following raw materials in parts by weight: amino-terminated hyperbranched polyimide 10-15 parts, acrylic modified polyether ether ketone 15-25 parts, 1,3-bis(oxymethylene methyl)-5-(2-propenyl)-1,3,5-triazine-2,4,6(1H,3H,5H)-trione 3-5 parts, 1,1,3,3-tetramethyl-1,3-divinyl disilazane 0.5-0.8 parts, 3-(1,1-difluoro-2-propen-1-yl)-2(1H)-quinoxalinone 1-3 parts, 2-(1-propen-2-yl)benzo[d]oxazole 1-3 parts, terpene resin 8-10 parts, initiator 1-2 parts, solvent 30-50 parts; the heat insulation layer is pressed from the following raw materials in parts by weight: fumed silica 8-12 parts, aerogel particles 10-20 parts, infrared light shielding agent 1-3 parts, heat-resistant filler 8-12 parts, chopped fiber 0.5-2.5 parts.

2. A thermally insulating fireproof material according to claim 1, characterized in that The terpene resin is terpene resin T-80; the initiator is azobisisobutyronitrile; and the solvent is at least one of N,N-dimethylformamide and N-methylpyrrolidone.

3. The thermally insulating fireproof material according to claim 1, characterized in that, The first encapsulation layer and the second encapsulation layer are each made of any one of PET film, PP film, PE film, PVC film, PI film and single-sided aluminum-coated PET film.

4. The fire protective thermal insulation material of claim 1, wherein The first fireproof support layer and the second fireproof support layer are each made of woven fabric, knitted fabric or non-woven fabric composed of aramid fiber, glass fiber, mullite fiber, basalt fiber and carbon fiber.

5. The thermally insulating fireproof material according to claim 1, characterized in that, The fumed silica is hydrophobic nanoscale fumed silica DECONS®E-65; the aerogel particles are one or more of silica aerogel, phenolic aerogel and polyimide aerogel; the average diameter of the aerogel particles is 0.5-10 μm; and the silica aerogel is CABOT silica aerogel.

6. The thermally insulating fireproof material according to claim 1, characterized in that, The infrared light shielding agent is at least one of silicon carbide, anatase titanium dioxide, carbon black and potassium hexatitanate whisker; the particle size of the infrared light shielding agent is 800-1200 mesh; the heat-resistant filler is at least one of calcium carbonate, talcum powder, mica, wollastonite and bauxite; and the particle size of the heat-resistant filler is 1000-1300 mesh.

7. The thermally insulating fire protective material of claim 1, wherein, The chopped fiber is at least one of basalt chopped fiber, carbon chopped fiber, mullite chopped fiber, glass chopped fiber and rock wool chopped fiber; the average diameter of the chopped fiber is 9-13 μm, and the chopped length is 3-6 mm.

8. A process for the preparation of a thermal and fire barrier material according to any one of claims 1 to 7, characterized in that, The method comprises the following steps: S1, mixing the raw materials of the heat insulation layer uniformly, placing them in a mold and pressing them into shape by a press to obtain a sample which is cut into a desired shape by a laser; Step S2, after mixing the raw materials of the first adhesive layer uniformly, the first adhesive layer is formed by coating on one side of the first fireproof support layer; after mixing the raw materials of the second adhesive layer uniformly, the second adhesive layer is formed by coating on one side of the second fireproof support layer; then the first adhesive layer and the second adhesive layer are respectively pasted with the upper and lower surfaces of the heat insulation layer and hot-cured to form; Step S3, the material prepared in step S2 is placed in a packaging bag, vacuumized, then hot-pressed, then pressure-released and opened, finally the edge sealing mold is cut to a proper width to obtain the heat insulation and fireproof material.

9. The method of claim 8, wherein the heat- and flame-resistant material is prepared by mixing the heat- and flame-resistant material with a solvent, and then drying the mixture. The hot-curing forming temperature in step S2 is 110-130℃, and the time is 20-30min; the pressure of the hot-pressing in step S3 is 0.1-1MPa, the temperature is 85-110℃, and the time is 10-20s.