Fireproof environment-friendly sealing flexible material and preparation method thereof

Abstract

The invention discloses a fireproof environment-friendly sealing flexible material and a preparation method thereof. On one hand, the invention provides a fireproof environment-friendly sealing flexible material which comprises a component A and a component B, the component A is prepared from the following raw material components in parts by mass: 100 parts of methyl vinyl silicone rubber, 62 to 68 parts of melamine coated ammonium polyphosphate, 14 to 18 parts of nano kaolin and 24 to 28 parts of elastomer polyurethane prepolymer; the component B is prepared from the following raw material components in parts by mass: 44 to 48 parts of vinyl silicone oil, 24 to 28 parts of hydrogen-containing silicone oil, 10 to 14 parts of a Karstedt catalyst, 18 to 22 parts of modified magnesium hydroxide, 12 to 16 parts of nano titanium dioxide and 44 to 48 parts of an IPDI (isophorone diisocyanate) polyurethane prepolymer. On the other hand, the invention provides a preparation method of the fireproof environment-friendly sealing flexible material. The material provided by the invention has the advantages of excellent flame retardant property, excellent flexibility and sealing property, and excellent aging resistance.

Description

Technical Field

[0001] This application relates to the field of fireproof materials technology, and in particular to a fireproof, environmentally friendly, and flexible sealing material and its preparation method. Background Technology

[0002] With the rapid development of industrial technology, the market demand for sealing materials has been surging year by year. In particular, the development of the power industry and the new energy vehicle industry in recent years has led to a continuous increase in the demand for flexible sealing materials. For example, various joints in the power industry, joints and seams in voltage equipment, and battery compartments in new energy vehicles all require the use of flexible sealing materials. Based on these demands, new requirements have been placed on the performance of flexible sealing materials, requiring them to possess excellent sealing performance and good electrical insulation properties.

[0003] Existing flexible sealing materials are mainly based on various silicone materials, divided into solid sealing materials and paste sealing materials, with various silicones as the main component. While these sealing materials possess excellent flexibility, and their sealing and insulation properties are relatively good, they lack flame retardancy, have relatively poor wear resistance, and insufficient resistance to photothermal aging, making them difficult to apply in the power industry and new energy vehicle industry. Although existing technologies can effectively improve the above-mentioned properties of silicone materials by incorporating various flame retardants and functional fillers, this leads to a decrease in sealing performance. Silicone materials are relatively expensive, difficult to deeply cure, and the incorporation of various flame retardants and fillers further widens the gaps between the molecular chains, thus affecting their sealing performance. While other existing sealing materials have certain advantages over silicone materials in other properties, their flexibility is far inferior.

[0004] Therefore, designing a sealing material that can meet current fire-retardant requirements and has excellent flexibility and sealing performance is a technical problem that urgently needs to be solved in this field. Summary of the Invention

[0005] In order to solve at least one of the above-mentioned technical problems and to develop a flexible sealing material with excellent flame retardant properties, excellent flexibility and sealing properties, and good aging resistance, this application provides a fireproof and environmentally friendly flexible sealing material and its preparation method.

[0006] On one hand, this application provides a fire-resistant, environmentally friendly, and flexible sealing material, comprising component A and component B. The mass ratio of each raw material component in component A includes: 100 parts methyl vinyl silicone rubber, 62-68 parts melamine-coated ammonium polyphosphate, 14-18 parts nano-kaolin, and 24-28 parts elastomer polyurethane prepolymer. The mass ratio of each raw material component in component B includes: 44-48 parts vinyl silicone oil, 24-28 parts hydrogen-containing silicone oil, 10-14 parts Karstedt catalyst, 18-22 parts modified magnesium hydroxide, 12-16 parts nano-titanium dioxide, and 44-48 parts IPDI polyurethane prepolymer. The elastomer polyurethane prepolymer is a polyurethane prepolymer prepared by isocyanate-grafted POE elastomer and bio-based polyol, and the IPDI polyurethane prepolymer is a polyurethane prepolymer prepared by IPDI trimer curing agent and bio-based polyol. The mass ratio of component A to component B is 1:0.95-1.2.

[0007] Optionally, the mass ratio of component A to component B is 1:1 to 1.1.

[0008] Optionally, the preparation of the isocyanate-grafted POE elastomer includes the following steps:

[0009] Sa, according to the mass ratio of 100:0.3:3.5~4.5, accurately weigh POE polyolefin elastomer, dicumyl peroxide and 1-(1-isocyano-1-methylethyl)-3-isopropenylbenzene, mix thoroughly to obtain premix;

[0010] Sb. The premix obtained in step Sa is added to a twin-screw extruder and melt-extruded to granulate, thereby obtaining isocyanate-grafted POE elastomer. The extrusion granulation process parameters are as follows: Zone 1 145℃, Zone 2 155℃, Zone 3 165℃, Zone 4 170℃, Zone 5 160℃, Zone 6 155℃, and the screw speed is 200~220rpm.

[0011] Optionally, the preparation of the elastomer polyurethane prepolymer includes the following steps:

[0012] S1-a. According to the mass ratio of 100:32~36:4~5, accurately weigh the isocyanate-grafted POE elastomer, bio-based polyol and delayed amine catalyst, and mix them thoroughly to obtain the premix.

[0013] S1-b: Heat the premix obtained in step S1-a to 80~85℃ and keep it at that temperature for more than 1 hour, then heat it to 155~160℃ and keep it at that temperature for 1~1.5 hours to obtain the elastomer polyurethane prepolymer.

[0014] Optionally, the preparation of the IPDI polyurethane prepolymer includes the following steps:

[0015] S2-a. According to the mass ratio of 100:38~42:5~6:2, accurately weigh IPDI trimer curing agent, bio-based polyol, delayed amine catalyst and quaternary ammonium salt, and mix them thoroughly to obtain a premix.

[0016] S2-b: Heat the premix obtained in step S2-a to 90°C and keep it at that temperature for more than 5 hours to obtain IPDI polyurethane prepolymer.

[0017] Further optionally, the delayed amine catalyst is selected from delayed amine catalyst A400.

[0018] Optionally, the IPDI trimer curing agent may be Z4470 IPDI trimer curing agent.

[0019] Alternatively, the quaternary ammonium salt may be selected from 2-hydroxypropyltrimethylammonium salt.

[0020] Optionally, component B may further include expanded vermiculite powder, wherein the amount of expanded vermiculite powder is 20-24 parts.

[0021] Secondly, this application provides a method for preparing the aforementioned fire-resistant and environmentally friendly flexible sealing material, comprising the following steps:

[0022] S1. Preparation of elastomer polyurethane prepolymer;

[0023] S2. Preparation of IPDI polyurethane prepolymer;

[0024] S3. Weigh the remaining raw materials according to the formula, mix methyl vinyl silicone rubber, melamine-coated ammonium polyphosphate and nano kaolin, add them to the mixer, and mix at 95~100℃ for more than 2 hours to obtain the compound.

[0025] S4. Mix the elastomer polyurethane prepolymer obtained in step S1 with the compound liquid obtained in step S3, and then stir and mix at a speed of 2000~2500 rpm for more than 30 minutes to obtain component A.

[0026] S5. Mix the IPDI polyurethane prepolymer obtained in step S2 with the remaining raw materials of component B, and then stir at 1200~1500 rpm for more than 30 minutes to obtain component B.

[0027] In summary, the present invention has at least one of the following beneficial technical effects:

[0028] 1. This application uses addition-cure silicone as the main body and introduces elastomeric polyurethane prepolymer and IPDI polyurethane prepolymer. Through a specific ratio design, a two-component flexible sealing material is prepared. After curing, it can form a dense elastomeric polyurethane and IPDI polyurethane cross-linked network in the silicone, effectively filling the gaps between the silicone molecular chains and greatly improving the sealing performance. In addition, elastomeric polyurethane has relatively excellent flexibility, and IPDI polyurethane also has a certain degree of flexibility. Under a specific ratio design, the constructed material system has excellent flexibility, which is not inferior to pure silicone material. The polyurethane cross-linked network, which also has plasticity, can significantly improve the wear resistance of the material.

[0029] 2. This application introduces an IPDI polyurethane crosslinking network into the material system, combined with nano-titanium dioxide filler, which can significantly improve the material's resistance to photothermal aging while ensuring the material's mechanical properties, thus giving the material better durability.

[0030] 3. The sealing material of this application introduces two different polyurethane crosslinking networks, both of which use bio-based polyols, which can form a dense char layer skeleton. The sealing material of this application uses melamine-coated ammonium polyphosphate and modified magnesium hydroxide to form an inorganic intumescent flame retardant ratio, and combines it with nano-kaolin as a synergist. It can work synergistically with the char layer skeleton to form a flame retardant system with excellent flame retardant performance, so that the material has excellent fireproof and flame retardant effects. Detailed Implementation

[0031] The present application will be further described in detail below with reference to the embodiments.

[0032] This application provides a fire-resistant, environmentally friendly, and flexible sealing material, comprising component A and component B. The component A comprises the following components in the following mass ratios: 100 parts methyl vinyl silicone rubber, 62-68 parts melamine-coated ammonium polyphosphate, 14-18 parts nano-kaolin, and 24-28 parts elastomer polyurethane prepolymer. The component B comprises the following components in the following mass ratios: 44-48 parts vinyl silicone oil, 24-28 parts hydrogen-containing silicone oil, 10-14 parts Karstedt catalyst, 18-22 parts modified magnesium hydroxide, 12-16 parts nano-titanium dioxide, and 44-48 parts IPDI polyurethane prepolymer. The elastomer polyurethane prepolymer is a polyurethane prepolymer prepared by isocyanate-grafted POE elastomer and bio-based polyol, and the IPDI polyurethane prepolymer is a polyurethane prepolymer prepared by IPDI trimer curing agent and bio-based polyol. The mass ratio of component A to component B is 1:0.95-1.2.

[0033] The preparation method of the above-mentioned fire-resistant and environmentally friendly flexible sealing material includes the following steps:

[0034] S1. Preparation of elastomer polyurethane prepolymer;

[0035] S2. Preparation of IPDI polyurethane prepolymer;

[0036] S3. Weigh the remaining raw materials according to the formula, mix methyl vinyl silicone rubber, melamine-coated ammonium polyphosphate and nano kaolin, add them to the mixer, and mix at 95~100℃ for more than 2 hours to obtain the compound.

[0037] S4. Mix the elastomer polyurethane prepolymer obtained in step S1 with the compound liquid obtained in step S3, and then stir and mix at a speed of 2000~2500 rpm for more than 30 minutes to obtain component A.

[0038] S5. Mix the IPDI polyurethane prepolymer obtained in step S2 with the remaining raw materials of component B, and then stir at 1200~1500 rpm for more than 30 minutes to obtain component B.

[0039] When using, simply mix the two components thoroughly according to the ratio to form a paste. The material of this application can be completely cured within 72 hours at room temperature to form a flexible seal.

[0040] Prior to this application, existing flame-retardant flexible sealing materials were primarily flame-retardant systems made by physical blending of silicone or elastic polyurethane materials with inorganic flame retardants. Silicone materials have poor mechanical fatigue resistance; the addition of flame retardants increases the gaps between molecular chains, leading to a decrease in sealing performance. Furthermore, silicone materials have insufficient aging resistance, resulting in unsatisfactory durability with long-term use. Elastic polyurethane materials have significantly lower insulation performance than silicone materials; the addition of flame retardants results in insufficient flexibility, making them prone to breakage after prolonged bending and puncture.

[0041] The applicant, through reasonable formulation design, selected two specific polyurethane prepolymers, fused them with addition-cured silicone and a specific flame-retardant system, and designed the composite material of this application, which effectively solves many problems existing in the prior art.

[0042] The following are preparation examples and embodiments of this application.

[0043] The main raw materials used in the embodiments of this application are all commercially available.

[0044] Among them, methyl vinyl silicone rubber, 112 raw rubber, was purchased from Guangzhou Shisheng Chemical Co., Ltd.; vinyl silicone oil, 1000CS type, was purchased from Hubei Longsheng Sihai New Material Co., Ltd.; hydrogen-containing silicone oil was purchased from Shandong Longhui Chemical Co., Ltd.; Karstedt catalyst was purchased from Hubei Shineng Chemical Technology Co., Ltd.; 1-(1-isocyano-1-methylethyl)-3-isopropenylbenzene was purchased from Shanghai Jizhi Biochemical Technology Co., Ltd.; POE polyolefin elastomer was purchased from Nanchang Yingfeng Chemical Co., Ltd.; bio-based polyol, FH-3185, was purchased from Zhangjiagang Feihang Technology Co., Ltd.; Z4470 IPDI trimer curing agent was purchased from Guangzhou Haoyi New Material Technology Co., Ltd.; delayed amine catalyst A400 was purchased from Xindian Chemical Materials (Shanghai) Co., Ltd.; 2-hydroxypropyltrimethylammonium salt was purchased from Suzhou Weidu Chemical Co., Ltd.; rutile nano titanium dioxide, 15~30nm, was purchased from Beijing Deco Island Gold Technology Co., Ltd.; melamine-coated ammonium polyphosphate, with a phosphorus content of about 30% and an average particle size of 5μm, was purchased from Shanghai Huanyang Chemical Technology Co., Ltd.; nano kaolin, with a particle size of 10~100nm, was purchased from Qingdao Taiyang Sheng Chemical Co., Ltd.; modified magnesium hydroxide, SS-MH6PG, D50, with a particle size of 1.0~2.0μm and a hexagonal flake morphology, was purchased from Qinghe County Ruijiang Metal Materials Co., Ltd.; expanded vermiculite powder, with a particle size of 100~300μm, was purchased from Lingshou County Zhanteng Mineral Products Processing Plant.

[0045] The following is a preparation example of this application.

[0046] Preparation Example 1

[0047] The preparation of the isocyanate-grafted POE elastomer in this example includes the following steps:

[0048] Sa, according to the mass ratio of 100:0.3:3.5, accurately weigh POE polyolefin elastomer, dicumyl peroxide and 1-(1-isocyano-1-methylethyl)-3-isopropenylbenzene, mix thoroughly to obtain premix;

[0049] Sb. The premix obtained in step Sa is added to a twin-screw extruder and melt-extruded to granulate, thereby obtaining isocyanate-grafted POE elastomer. The extrusion granulation process parameters are as follows: Zone 1 145℃, Zone 2 155℃, Zone 3 165℃, Zone 4 170℃, Zone 5 160℃, Zone 6 155℃, and the screw speed is 200 rpm.

[0050] Preparation Example 2

[0051] The preparation of the isocyanate-grafted POE elastomer in this example includes the following steps:

[0052] Sa, according to the mass ratio of 100:0.3:4.5, accurately weigh POE polyolefin elastomer, dicumyl peroxide and 1-(1-isocyano-1-methylethyl)-3-isopropenylbenzene, mix thoroughly to obtain the premix;

[0053] Sb. The premix obtained in step Sa is added to a twin-screw extruder and melt-extruded to granulate, thereby obtaining isocyanate-grafted POE elastomer. The extrusion granulation process parameters are as follows: Zone 1 145℃, Zone 2 155℃, Zone 3 165℃, Zone 4 170℃, Zone 5 160℃, Zone 6 155℃, and the screw speed is 220 rpm.

[0054] Preparation Example 3

[0055] The preparation of the elastomer polyurethane prepolymer in this example includes the following steps:

[0056] S1-a, according to the mass ratio of 100:32:4, accurately weigh the isocyanate-grafted POE elastomer, bio-based polyol and delayed amine catalyst a400, and mix them thoroughly to obtain the premix.

[0057] S1-b: Heat the premix obtained in step S1-a to 80~85℃ and keep it at that temperature for 1 hour, then heat it to 155~160℃ and keep it at that temperature for 1 hour to obtain the elastomer polyurethane prepolymer.

[0058] The isocyanate-grafted POE elastomer of Preparation Example 1 was selected.

[0059] Preparation Example 4

[0060] The preparation of the elastomer polyurethane prepolymer in this example includes the following steps:

[0061] S1-a, according to the mass ratio of 100:36:5, accurately weigh the isocyanate-grafted POE elastomer, bio-based polyol and delayed amine catalyst a400, and mix them thoroughly to obtain the premix.

[0062] S1-b: Heat the premix obtained in step S1-a to 80~85℃ and keep it at that temperature for 1 hour, then heat it to 155~160℃ and keep it at that temperature for 1 hour to obtain the elastomer polyurethane prepolymer.

[0063] The isocyanate-grafted POE elastomer of Preparation Example 1 was selected.

[0064] Preparation Example 5

[0065] The preparation of the elastomer polyurethane prepolymer in this example includes the following steps:

[0066] S1-a, according to the mass ratio of 100:34:4.6, accurately weigh the isocyanate-grafted POE elastomer, bio-based polyol and delayed amine catalyst a400, and mix them thoroughly to obtain the premix;

[0067] S1-b: Heat the premix obtained in step S1-a to 80~85℃ and keep it at that temperature for 1 hour, then heat it to 155~160℃ and keep it at that temperature for 1.5 hours to obtain the elastomer polyurethane prepolymer.

[0068] The isocyanate-grafted POE elastomer of Preparation Example 1 was selected.

[0069] Preparation Example 6

[0070] The difference between this preparation example and preparation example 5 is that the isocyanate-grafted POE elastomer of preparation example 2 is used.

[0071] Preparation Example 7

[0072] The preparation of the IPDI polyurethane prepolymer in this example includes the following steps:

[0073] S2-a, according to the mass ratio of 100:38:5:2, accurately weigh Z4470 IPDI trimer curing agent, bio-based polyol, delayed amine catalyst a400 and 2-hydroxypropyltrimethylformate ammonium salt, and mix them thoroughly to obtain a premix;

[0074] S2-b: Heat the premix obtained in step S2-a to 90°C and keep it at that temperature for 5 hours to obtain IPDI polyurethane prepolymer.

[0075] Preparation Example 8

[0076] The preparation of the IPDI polyurethane prepolymer in this example includes the following steps:

[0077] S2-a, according to the mass ratio of 100:42:6:2, accurately weigh Z4470 IPDI trimer curing agent, bio-based polyol, delayed amine catalyst a400 and 2-hydroxypropyltrimethylformate ammonium salt, and mix them thoroughly to obtain a premix;

[0078] S2-b: Heat the premix obtained in step S2-a to 90°C and keep it at that temperature for 5 hours to obtain IPDI polyurethane prepolymer.

[0079] Preparation Example 9

[0080] The preparation of the IPDI polyurethane prepolymer in this example includes the following steps:

[0081] S2-a, according to the mass ratio of 100:40:5.4:2, accurately weigh Z4470 IPDI trimer curing agent, bio-based polyol, delayed amine catalyst a400 and 2-hydroxypropyltrimethylformate ammonium salt, and mix them thoroughly to obtain the premix;

[0082] S2-b: Heat the premix obtained in step S2-a to 90°C and keep it at that temperature for 5 hours to obtain IPDI polyurethane prepolymer.

[0083] The following are embodiments of this application.

[0084] The preparation of the fire-resistant, environmentally friendly, and flexible sealing material according to this application includes the following steps:

[0085] S1. Select the corresponding elastomer polyurethane prepolymer;

[0086] S2. Select the corresponding IPDI polyurethane prepolymer;

[0087] S3. Weigh the remaining raw materials according to the formula, mix methyl vinyl silicone rubber, melamine-coated ammonium polyphosphate and nano kaolin, add them to the mixer, and mix at 95~100℃ for 2 hours to obtain the compound solution.

[0088] S4. Mix the elastomer polyurethane prepolymer obtained in step S1 with the compound liquid obtained in step S3, and then stir at 2000 rpm for 30 min to obtain component A.

[0089] S5. Mix the IPDI polyurethane prepolymer obtained in step S2 with the remaining raw materials of component B, and then stir at 1200 rpm for 30 minutes to obtain component B.

[0090] Example 1

[0091] The fire-resistant and environmentally friendly sealing flexible material of this embodiment is prepared by fully mixing component A and component B in a ratio of 1:0.95.

[0092] The mass proportions of each raw material component in Component A include: 100 parts methyl vinyl silicone rubber, 62 parts melamine-coated ammonium polyphosphate, 14 parts nano kaolin, and 24 parts elastomer polyurethane prepolymer.

[0093] The mass proportions of each raw material component in Component B include: 44 parts vinyl silicone oil, 24 parts hydrogen-containing silicone oil, 10 parts Karstedt catalyst, 18 parts modified magnesium hydroxide, 12 parts nano titanium dioxide, and 44 parts IPDI polyurethane prepolymer.

[0094] In this embodiment, the elastomer polyurethane prepolymer of Preparation Example 3 and the IPDI polyurethane prepolymer of Preparation Example 7 were selected.

[0095] Example 2

[0096] The fire-resistant and environmentally friendly sealing flexible material of this embodiment is prepared by fully mixing component A and component B in a ratio of 1:0.95.

[0097] The mass proportions of each raw material component in Component A include: 100 parts methyl vinyl silicone rubber, 68 parts melamine-coated ammonium polyphosphate, 18 parts nano kaolin, and 28 parts elastomer polyurethane prepolymer.

[0098] The mass proportions of each raw material component in Component B include: 48 parts vinyl silicone oil, 28 parts hydrogen-containing silicone oil, 14 parts Karstedt catalyst, 22 parts modified magnesium hydroxide, 16 parts nano titanium dioxide, and 48 parts IPDI polyurethane prepolymer.

[0099] In this embodiment, the elastomer polyurethane prepolymer of Preparation Example 3 and the IPDI polyurethane prepolymer of Preparation Example 7 were selected.

[0100] Example 3

[0101] The fire-resistant and environmentally friendly sealing flexible material of this embodiment is prepared by fully mixing component A and component B in a ratio of 1:0.95.

[0102] The mass proportions of each raw material component in Component A include: 100 parts methyl vinyl silicone rubber, 65 parts melamine-coated ammonium polyphosphate, 15 parts nano kaolin, and 26 parts elastomer polyurethane prepolymer.

[0103] The mass proportions of each raw material component in Component B include: 46 parts vinyl silicone oil, 26 parts hydrogen-containing silicone oil, 12 parts Karstedt catalyst, 20 parts modified magnesium hydroxide, 14 parts nano titanium dioxide, and 45 parts IPDI polyurethane prepolymer.

[0104] In this embodiment, the elastomer polyurethane prepolymer of Preparation Example 3 and the IPDI polyurethane prepolymer of Preparation Example 7 were selected.

[0105] Example 4

[0106] The fire-resistant and environmentally friendly sealing flexible material of this embodiment is prepared by fully mixing component A and component B in a ratio of 1:0.95.

[0107] The mass proportions of each raw material component in Component A include: 100 parts methyl vinyl silicone rubber, 65 parts melamine-coated ammonium polyphosphate, 15 parts nano kaolin, and 26 parts elastomer polyurethane prepolymer.

[0108] The mass proportions of each raw material component in Component B include: 46 parts vinyl silicone oil, 26 parts hydrogen-containing silicone oil, 12 parts Karstedt catalyst, 20 parts modified magnesium hydroxide, 14 parts nano titanium dioxide, 45 parts IPDI polyurethane prepolymer, and 20 parts expanded vermiculite powder.

[0109] In this embodiment, the elastomer polyurethane prepolymer of Preparation Example 3 and the IPDI polyurethane prepolymer of Preparation Example 7 were selected.

[0110] Example 5

[0111] The fire-resistant and environmentally friendly sealing flexible material of this embodiment is prepared by fully mixing component A and component B in a 1:1 ratio.

[0112] The mass proportions of each raw material component in Component A include: 100 parts methyl vinyl silicone rubber, 65 parts melamine-coated ammonium polyphosphate, 15 parts nano kaolin, and 26 parts elastomer polyurethane prepolymer.

[0113] The mass proportions of each raw material component in Component B include: 46 parts vinyl silicone oil, 26 parts hydrogen-containing silicone oil, 12 parts Karstedt catalyst, 20 parts modified magnesium hydroxide, 14 parts nano titanium dioxide, 45 parts IPDI polyurethane prepolymer, and 24 parts expanded vermiculite powder.

[0114] In this embodiment, the elastomer polyurethane prepolymer of Preparation Example 3 and the IPDI polyurethane prepolymer of Preparation Example 7 were selected.

[0115] Example 6

[0116] The difference between this embodiment and Example 5 is that this embodiment selects the elastomer polyurethane prepolymer of Preparation Example 4 and the IPDI polyurethane prepolymer of Preparation Example 8.

[0117] Example 7

[0118] The difference between this embodiment and Example 5 is that this embodiment selects the elastomer polyurethane prepolymer of Preparation Example 5 and the IPDI polyurethane prepolymer of Preparation Example 9.

[0119] Example 8

[0120] The difference between this embodiment and Example 5 is that this embodiment selects the elastomer polyurethane prepolymer of Preparation Example 6 and the IPDI polyurethane prepolymer of Preparation Example 9.

[0121] Example 9

[0122] The difference between this embodiment and embodiment 8 is that the fire-resistant and environmentally friendly sealing flexible material in this embodiment is prepared by fully mixing component A and component B in a ratio of 1:1.1.

[0123] Example 10

[0124] The difference between this embodiment and embodiment 8 is that the fire-resistant and environmentally friendly sealing flexible material in this embodiment is prepared by fully mixing component A and component B in a ratio of 1:1.2.

[0125] Comparative Example 1

[0126] This application uses Example 5 of the invention patent with publication number CN108203525A and invention titled "An Expandable Flexible Fireproof Material and Its Application" as Comparative Example 1.

[0127] Comparative Example 2

[0128] The fire-resistant and environmentally friendly flexible sealing material in this comparative example is prepared by fully mixing component A and component B in a 1:1 ratio.

[0129] The mass proportions of each raw material component in Component A include: 100 parts of methyl vinyl silicone rubber, 65 parts of melamine-coated ammonium polyphosphate, and 15 parts of nano-kaolin.

[0130] The mass proportions of each raw material component in Component B include: 46 parts vinyl silicone oil, 26 parts hydrogen-containing silicone oil, 12 parts Karstedt catalyst, 20 parts modified magnesium hydroxide, 14 parts nano titanium dioxide, and 24 parts expanded vermiculite powder.

[0131] Comparative Example 3

[0132] The difference between this comparative example and Example 8 is that an equal amount of IPDI polyurethane prepolymer is used to replace the elastomer polyurethane prepolymer.

[0133] Comparative Example 4

[0134] The difference between this comparative example and Example 8 is that an equal amount of elastomeric polyurethane prepolymer is used to replace the IPDI polyurethane prepolymer.

[0135] The performance of the products in Examples 1-10 and Comparative Examples 1-4 was tested. The materials of Examples 1-10 and Comparative Examples 2-4 were cured into specimens with a size of 25cm×5cm×5mm. The material of Comparative Example 1 was also made into a specimen of the same size. The flexibility, mechanical fatigue, sealing and flame retardancy of the specimens were tested respectively.

[0136] Among them, flexibility is tested for whether cracks appear when bent at 90°.

[0137] Mechanical fatigue is tested by bending at 75° for 3000 times to see if cracks appear. If cracks appear, the number of bends that caused the cracks is recorded.

[0138] The leak rate of the nitrogen seal under a pressure of 50 MPa was tested according to the method described in GB / T12385-2008.

[0139] The oxygen index was tested according to the method described in ASTM D2863.

[0140] The results are shown in Table 1 below.

[0141] Table 1. Performance test results of products from Examples 1-10 and Comparative Examples 1-4

[0142] Flexible (90° bending) Mechanical fatigue Leakage rate (%) Oxygen index (%) Example 1 Intact and without cracks Intact and without cracks 0.18 32.4 Example 2 Intact and without cracks Intact and without cracks 0.17 33.1 Example 3 Intact and without cracks Intact and without cracks 0.15 33.0 Example 4 Intact and without cracks Intact and without cracks 0.12 33.2 Example 5 Intact and without cracks Intact and without cracks 0.09 33.3 Example 6 Intact and without cracks Intact and without cracks 0.08 33.3 Example 7 Intact and without cracks Intact and without cracks 0.06 33.3 Example 8 Intact and without cracks Intact and without cracks 0.04 33.3 Example 9 Intact and without cracks Intact and without cracks 0.02 33.3 Example 10 Intact and without cracks Intact and without cracks 0.09 33.4 Comparative Example 1 cracking 314 cracks 1.22 28.2 Comparative Example 2 Intact and without cracks 271 cracks 5.41 27.6 Comparative Example 3 fracture 44 cracks 0.64 33.2 Comparative Example 4 Intact and without cracks 752 cracks 0.41 33.3

[0143] The samples from Examples 1-10 and Comparative Examples 1-4 were subjected to aging treatment, and their various properties were then tested. The results are shown in Table 2 below. Aging parameters: temperature 85℃, humidity 100%, UV intensity 0.45W / m 2 Under these conditions, the treatment lasted for 30 days.

[0144] Table 2. Results of Aging Resistance Tests for Examples 1-10 and Comparative Examples 1-4

[0145] Flexible (90° bending) Mechanical fatigue Leakage rate (%) Example 1 Intact and without cracks Intact and without cracks 0.20 Example 2 Intact and without cracks Intact and without cracks 0.19 Example 3 Intact and without cracks Intact and without cracks 0.17 Example 4 Intact and without cracks Intact and without cracks 0.15 Example 5 Intact and without cracks Intact and without cracks 0.10 Example 6 Intact and without cracks Intact and without cracks 0.09 Example 7 Intact and without cracks Intact and without cracks 0.08 Example 8 Intact and without cracks Intact and without cracks 0.06 Example 9 Intact and without cracks Intact and without cracks 0.04 Example 10 Intact and without cracks Intact and without cracks 0.11 Comparative Example 1 fracture 109 cracks 3.44 Comparative Example 2 cracking 92 cracks 9.69 Comparative Example 3 fracture 46 cracks 0.65 Comparative Example 4 Intact and without cracks 305 cracks 0.98

[0146] As can be seen from the data in Table 1, the samples of Examples 1-10 of this application exhibit superior flexibility compared to Comparative Examples 1 and 2 of the prior art. They can withstand 90° bending, and their mechanical fatigue resistance is significantly better than that of Comparative Examples 1 and 2. Their sealing performance is also superior, and their flame retardancy is significantly better than that of the materials in Comparative Examples 1 and 2. Therefore, it is evident that the fire-resistant and environmentally friendly sealing flexible material of this application demonstrates a significant improvement in overall performance compared to existing products.

[0147] As can be seen from the data in Tables 1 and 2, the samples of Examples 1-10 of this application show a significant improvement in resistance to damp heat aging compared to Comparative Examples 1 and 2 of the prior art. After aging treatment, there is no significant decrease in any of the properties. Therefore, the fire-resistant and environmentally friendly sealing flexible material of this application, through specific design, effectively solves the problem of insufficient resistance to damp heat aging.

[0148] Comparing the data from Examples 1-10 in Tables 1 and 2, it can be seen that the performance of products from Examples 9-10 is slightly better than that of product from Example 8, while the performance of products from Examples 6-8 is significantly better than that of products from Examples 3-5, and the performance of products from Examples 3-5 is better than that of products from Examples 1-2. This demonstrates that by optimizing the raw material ratio and the polyurethane prepolymer ratio, the various properties of the material can be significantly improved. Furthermore, the addition of a certain amount of expanded vermiculite powder further enhances the fatigue resistance and flame retardancy of the material. Additionally, the cured performance of the material is highly correlated with the ratio of component A to component B; a ratio of 1:1 to 1.1 between components A and B results in relatively better performance after curing.

[0149] By comparing the data from Example 10 and Comparative Examples 3-4 in Table 1, it can be seen that in the design of this application, the two polyurethane prepolymers are incorporated into the system in a specific ratio to form a dense polyurethane cross-linked network, which is the core of the excellent performance of the material in this application. No single type of polyurethane network can achieve the effect of this application. In addition, the hygrothermal aging resistance of this application is provided by the polyurethane cross-linked network formed by the IPDI polyurethane prepolymer. Therefore, there is no need to add antioxidants or other additives. Only the UV stabilizer nano-titanium dioxide is needed to ensure that the material of this application has excellent aging resistance after curing.

[0150] The above are all preferred embodiments of this application, and are not intended to limit the scope of protection of this application. Therefore, all equivalent changes made in accordance with the structure, shape and principle of this application should be covered within the scope of protection of this application.

Claims

1. A fire-resistant, environmentally friendly, flexible sealing material, characterized in that, The product comprises two components, A and B. The mass ratio of each raw material component in component A is as follows: 100 parts methyl vinyl silicone rubber, 62-68 parts melamine-coated ammonium polyphosphate, 14-18 parts nano-kaolin, and 24-28 parts elastomer polyurethane prepolymer. The mass ratio of each raw material component in component B is as follows: 44-48 parts vinyl silicone oil, 24-28 parts hydrogen-containing silicone oil, 10-14 parts Karstedt catalyst, 18-22 parts modified magnesium hydroxide, 12-16 parts nano-titanium dioxide, and 44-48 parts IPDI polyurethane prepolymer. The elastomer polyurethane prepolymer is a polyurethane prepolymer prepared by isocyanate-grafted POE elastomer and bio-based polyol, and the IPDI polyurethane prepolymer is a polyurethane prepolymer prepared by IPDI trimer curing agent and bio-based polyol. The mass ratio of component A to component B is 1:0.95-1.

2.

2. The fire-resistant, environmentally friendly, and flexible sealing material according to claim 1, characterized in that, The mass ratio of component A to component B is 1:1 to 1.

1.

3. The fire-resistant, environmentally friendly, and flexible sealing material according to claim 1, characterized in that, The preparation of the isocyanate-grafted POE elastomer includes the following steps: Sa, according to the mass ratio of 100:0.3:3.5~4.5, accurately weigh POE polyolefin elastomer, dicumyl peroxide and 1-(1-isocyano-1-methylethyl)-3-isopropenylbenzene, mix thoroughly to obtain premix; Sb. The premix obtained in step Sa is added to a twin-screw extruder and melt-extruded to granulate, thereby obtaining isocyanate-grafted POE elastomer. The extrusion granulation process parameters are as follows: Zone 1 145℃, Zone 2 155℃, Zone 3 165℃, Zone 4 170℃, Zone 5 160℃, Zone 6 155℃, and the screw speed is 200~220rpm.

4. The fire-resistant, environmentally friendly, and flexible sealing material according to claim 1, characterized in that, The preparation of the elastomer polyurethane prepolymer includes the following steps: S1-a. According to the mass ratio of 100:32~36:4~5, accurately weigh the isocyanate-grafted POE elastomer, bio-based polyol and delayed amine catalyst, and mix them thoroughly to obtain the premix. S1-b: Heat the premix obtained in step S1-a to 80~85℃ and keep it at that temperature for more than 1 hour, then heat it to 155~160℃ and keep it at that temperature for 1~1.5 hours to obtain the elastomer polyurethane prepolymer.

5. The fire-resistant, environmentally friendly, and flexible sealing material according to claim 1, characterized in that, The preparation of the IPDI polyurethane prepolymer includes the following steps: S2-a. According to the mass ratio of 100:38~42:5~6:2, accurately weigh IPDI trimer curing agent, bio-based polyol, delayed amine catalyst and quaternary ammonium salt, and mix them thoroughly to obtain a premix. S2-b: Heat the premix obtained in step S2-a to 90°C and keep it at that temperature for more than 5 hours to obtain IPDI polyurethane prepolymer.

6. The fire-resistant, environmentally friendly, and flexible sealing material according to claim 4 or 5, characterized in that, The delayed amine catalyst used is the delayed amine catalyst a400.

7. The fire-resistant, environmentally friendly, and flexible sealing material according to claim 5, characterized in that, The IPDI trimer curing agent used is Z4470 IPDI trimer curing agent.

8. The fire-resistant, environmentally friendly, and flexible sealing material according to claim 5, characterized in that, The quaternary ammonium salt is selected from 2-hydroxypropyltrimethylformate ammonium salt.

9. The fire-resistant, environmentally friendly, and flexible sealing material according to claim 1, characterized in that, Component B also includes expanded vermiculite powder, and the amount of expanded vermiculite powder used is 20-24 parts.

10. A method for preparing a fire-resistant, environmentally friendly, and flexible sealing material according to any one of claims 1 to 9, characterized in that, Includes the following steps: S1. Preparation of elastomer polyurethane prepolymer; S2. Preparation of IPDI polyurethane prepolymer; S3. Weigh the remaining raw materials according to the formula, mix methyl vinyl silicone rubber, melamine-coated ammonium polyphosphate and nano kaolin, add them to the mixer, and mix at 95~100℃ for more than 2 hours to obtain the mixed rubber solution. S4. Mix the elastomer polyurethane prepolymer obtained in step S1 with the compound liquid obtained in step S3, and then stir and mix at a speed of 2000~2500 rpm for more than 30 minutes to obtain component A. S5. Mix the IPDI polyurethane prepolymer obtained in step S2 with the remaining raw materials of component B, and then stir and mix at a speed of 1200~1500 rpm for more than 30 minutes to obtain component B.