High-strength flame-retardant soundproof and heat-insulating composite material and preparation method thereof

By innovatively combining modified flame retardants and binders, the problem of imbalance in the high strength, flame retardancy, sound insulation, and heat insulation properties of composite materials has been solved, achieving efficient flame retardancy and sound and heat insulation effects, and improving the stability and mechanical properties of the materials.

CN120365731BActive Publication Date: 2025-12-16ZHEJIANG FULAI NEW MATERIAL CO LTD +1
View PDF 3 Cites 0 Cited by

Patent Information

Application Number
CN202510735963.4
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2025-06-04
Publication Date
2025-12-16
Estimated Expiration
2045-06-04

AI Technical Summary

Technical Problem

Existing composite materials, while balancing high strength, flame retardancy, sound insulation, and heat insulation, suffer from performance imbalances and cannot operate stably under complex working conditions. Furthermore, traditional materials are easily combustible in fires and have poor heat and sound insulation effects, affecting personnel safety and user experience.

Method used

By combining modified flame retardants and binders, a highly cross-linked network is constructed through nitrogen-phosphorus synergistic flame retardancy and star-shaped topology, combined with the steric hindrance and chemical bonding of silanes, thereby improving the dispersibility and interfacial stability of the flame retardants. At the same time, a highly cross-linked network is constructed using thiol-epoxy click reaction to enhance the tensile properties of the material.

Benefits of technology

It achieves a synergistic improvement in high strength, flame retardancy, sound insulation, and heat insulation performance. The material forms a dense carbon layer at high temperature, which prevents heat and oxygen transfer, improves tensile strength and ductility, avoids stress concentration, and maintains material stability.

✦ Generated by Eureka AI based on patent content.

Smart Images

  • Figure SMS_7
    Figure SMS_7
Patent Text Reader

Abstract

The application discloses a high-strength flame-retardant sound-proof and heat-insulation composite material and a preparation method thereof, and belongs to the technical field of high polymer materials. The high-strength flame-retardant sound-proof and heat-insulation composite material comprises the following raw materials in parts by weight: 40-60 parts of polyurethane resin, 10-15 parts of polyvinylpyrrolidone, 10-15 parts of ceramic hollow microbeads, 6-10 parts of ceramic fiber, 5-8 parts of a bonding agent, 1-3 parts of a modified flame retardant and 2-4 parts of an anti-aging agent. The high-strength flame-retardant sound-proof and heat-insulation composite material prepared by the application has excellent heat-insulation, sound-proof, tensile property and flame-retardant property.
Need to check novelty before this filing date? Find Prior Art

Description

TECHNICAL FIELD

[0001] The present application relates to the technical field of high polymer materials, in particular to a high-strength flame-retardant sound and heat insulation composite material and a preparation method thereof. BACKGROUND

[0002] In today's many fields, such as building, aerospace, automobile manufacturing, etc., the comprehensive performance requirements for materials are increasingly stringent, especially the composite materials that need to have high strength, flame retardation, sound insulation and heat insulation performance. In the field of building, with the acceleration of urbanization, high-rise buildings and intensive residential buildings are emerging, and the performance requirements for composite materials are also increasing.

[0003] However, the existing composite materials have many shortcomings when meeting various performance requirements. On the one hand, many traditional composite materials can meet certain strength requirements, but have poor flame retardation performance, and when facing fire, they are easy to burn and have poor heat and sound insulation effects, which not only cannot gain time for personnel to escape, but also exacerbate the spread of fire and noise, causing great threat to personnel life safety and living comfort. On the other hand, some composite materials have high strength, but poor sound and heat insulation effects, and cannot effectively insulate external noise and heat, which will transmit external high temperature and noise into the internal space, affecting the use experience. In addition, some composite materials have good flame retardation, sound and heat insulation performance, but their strength is greatly reduced, which cannot meet the mechanical performance requirements in actual application, resulting in unbalanced overall performance of the materials and instability in complex working conditions.

[0004] Chinese invention patent with publication number CN113563771A discloses a crack-resistant sound insulation composite material and a preparation method thereof. The crack-resistant sound insulation composite material comprises the following raw materials by weight: hollow glass microspheres 5-20%, modified polycarboxylic acid water reducer 0.2-0.5%; the vacuum degree of the hollow glass microspheres is 0.2 g / cm 3 , and the particle size is 80 μm; the modified polycarboxylic acid water reducer is prepared by reacting polycarboxylic acid water reducer and silane coupling agent containing amino groups at the end in a weight ratio of 1:2-5 under the action of organic weak base; the crack-resistant sound insulation composite material prepared by the patent has excellent sound insulation, heat insulation, strong adhesion, anti-ultraviolet, and is not easy to crack and fall off, etc. However, the flame retardation effect of the composite material is poor. SUMMARY

[0005] In view of the deficiencies of the prior art, the purpose of the present application is to provide a high-strength flame-retardant sound and heat insulation composite material and a preparation method thereof.

[0006] To achieve the above-mentioned purpose, the present application realizes the following technical solutions:

[0007] A high-strength flame-retardant sound and heat insulation composite material comprises the following raw materials by weight:

[0008] Polyurethane resin 40-60 parts, polyvinylpyrrolidone 10-15 parts, ceramic hollow microsphere 10-15 parts, ceramic fiber 6-10 parts, adhesive 5-8 parts, modified flame retardant 1-3 parts, antioxidant 2-4 parts;

[0009] The modified flame retardant is prepared by the following method:

[0010] S1: pentaerythritol reacts with 3,6-dimethyl-1,4-dioxane-2,5-dione under the catalysis of stannous octoate to generate a four-arm star compound;

[0011] S2: 2-piperazine carboxylic acid reacts with diphenyl phosphinic chloride to generate a nitrogen-phosphorus compound;

[0012] S3: the four-arm star compound reacts with the nitrogen-phosphorus compound under the action of p-toluenesulfonic acid to generate a nitrogen-phosphorus modified four-arm star compound;

[0013] S4: the nitrogen-phosphorus modified four-arm star compound reacts with octadecyldimethylmethoxysilane to generate a modified flame retardant.

[0014] In step S1, the molar ratio of pentaerythritol to 3,6-dimethyl-1,4-dioxane-2,5-dione is 1:(12-20).

[0015] In step S2, the molar ratio of 2-piperazine carboxylic acid to diphenyl phosphinic chloride is 1:(2-2.5).

[0016] In step S3, the molar ratio of the four-arm star compound to the nitrogen-phosphorus compound is 1:(1.8-2.2).

[0017] In step S4, the molar ratio of the nitrogen-phosphorus modified four-arm star compound to octadecyldimethylmethoxysilane is 1:(2-2.5).

[0018] The adhesive is prepared by the following method:

[0019] A1: castor oil reacts under the action of formic acid and H2O2 to generate an epoxy compound;

[0020] A2: the epoxy compound reacts with (1,4-phenylenebis(1,3,2-dioxaborolan-2,4-diyl)) dimethyl sulfide to generate an adhesive.

[0021] In step A1, the mass ratio of castor oil to formic acid is 1:3.

[0022] In step A2, the mass ratio of the epoxy compound to (1,4-phenylenebis(1,3,2-dioxaborolan-2,4-diyl)) dimethyl sulfide is 2:1.

[0023] The anti-aging agent is one of UV-531 and UV-326.

[0024] A preparation method of a high-strength flame-retardant soundproof and heat-insulating composite material, comprising the following steps:

[0025] (1) Take the following components by weight parts: polyurethane resin 40-60 parts, polyvinylpyrrolidone 10-15 parts, ceramic hollow microbeads 10-15 parts, ceramic fiber 6-10 parts, binder 5-8 parts, modified flame retardant 1-3 parts, and anti-aging agent 2-4 parts;

[0026] (2) Mix the polyurethane resin, polyvinylpyrrolidone, binder, modified flame retardant, and anti-aging agent to obtain a mixture A; grind the ceramic fiber and then mix it with the ceramic hollow microbeads to obtain a mixture B;

[0027] (3) Mix the mixture A and the mixture B uniformly, extrude them through an extruder, and cool and shape them to obtain the high-strength flame-retardant soundproof and heat-insulating composite material.

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

[0029] (1) The modified flame retardant prepared in the present application realizes high-efficiency flame retardation through nitrogen-phosphorus synergistic flame retardation and star-shaped topological structure, and the introduction of silane significantly improves the dispersion uniformity and interface stability of the flame retardant in the matrix through steric hindrance dispersion and chemical bonding.

[0030] (2) The binder in the present application constructs a high-crosslinking network through thiol-epoxy click reaction, and utilizes the dynamic flexibility of the long-chain alkyl of castor oil and the reversible rupture and recombination of borate ester bond to synergistically improve the tensile properties of the soundproof and heat-insulating material. DETAILED DESCRIPTION

[0031] The present application will be further described below in conjunction with examples, but the present application is not limited to these examples.

[0032] Example 1: Preparation of modified flame retardant

[0033] S1: Under nitrogen protection, 1200 g of DMF, 0.1 mol of pentaerythritol and 1.2 mol of 3,6-dimethyl-1,4-dioxane-2,5-dione were added into a reactor, stirred and mixed, heated to 130°C, stirred for 15 min, then 10 g of stannous octoate catalyst was added, reacted for 20 h, then cooled to room temperature, distilled at 60°C under reduced pressure for 2 h to obtain a crude product, the crude product was added into 500 ml of chloroform, stirred and mixed, then 500 ml of cold methanol was added, and the precipitate was separated by standing and filtering, then washed with methanol three times (500 ml each time), and vacuum dried at 60°C for 5 h to obtain a four-arm star-shaped compound with a number average molecular weight of 1762; the reaction equation is as follows:

[0034] .

[0035] S2: Under nitrogen protection, 200 ml of dichloromethane and 0.2 mol of diphenylphosphine chloride were added into a reactor, stirred and mixed, then 100 ml of a dichloromethane solution of 2-piperazine carboxylic acid (0.1 mol of 2-piperazine carboxylic acid dissolved in 100 ml of dichloromethane) was slowly added dropwise, and 0.3 mol of triethylamine was slowly added dropwise for 10 min, after the dropwise addition was completed, refluxed for 4 h, then cooled to room temperature, distilled at 35°C under reduced pressure for 45 min, washed with deionized water three times (200 ml each time), filtered, and vacuum dried at 60°C for 4 h to obtain a nitrogen-phosphorus compound; the reaction equation is as follows:

[0036] .

[0037] S3: Under nitrogen protection, 1200 g of toluene, 0.1 mol of the four-arm star-shaped compound and 0.18 mol of the nitrogen-phosphorus compound were added into a reactor, stirred and mixed, heated to 80°C, then 15 g of p-toluenesulfonic acid was added, reacted for 6 h (a water trap was used to remove the generated water during the reaction), then cooled to room temperature, slowly added saturated sodium bicarbonate solution to adjust the pH to neutral, stirred for 30 min, separated the layers by standing, transferred the organic phase to a rotary evaporator, distilled at 60°C under reduced pressure for 4 h, and vacuum dried at 70°C for 10 h to obtain a nitrogen-phosphorus modified four-arm star-shaped compound; the number average molecular weight was 2633; the reaction equation is as follows:

[0038] .

[0039] S4: 800 ml of toluene, 0.1 mol of nitrogen-phosphorus modified four-armed star compound was added into the reactor, stirred for 1 h, then 0.2 mol of octadecyldimethylmethoxysilane, 0.2 mol of triethylamine was added, after reaction at 60°C for 6 h, centrifugation, washing with deionized water for 3 times (500 ml each time), filtration, vacuum drying at 70°C for 12 h to obtain the modified flame retardant; the number average molecular weight is 3224; the reaction equation is as follows:

[0040] .

[0041] Example 2 Preparation of modified flame retardant:

[0042] S1: Under nitrogen protection, 1200 g of DMF, 0.1 mol of pentaerythritol and 1.6 mol of 3,6-dimethyl-1,4-dioxane-2,5-dione were added into the reactor, stirred and mixed, heated to 130°C, stirred for 15 min, then 10 g of catalyst stannous octoate was added, reacted for 24 h, then cooled to room temperature, distilled at 60°C under reduced pressure for 2 h to obtain a crude product, the crude product was added into 500 ml of chloroform, stirred and mixed, then 500 ml of cold methanol was added, and the precipitate was separated by standing, filtered, then washed with methanol for 3 times (500 ml each time), vacuum dried at 60°C for 5 h to obtain a four-armed star compound, and the number average molecular weight was 2318;

[0043] S2: Under nitrogen protection, 200 ml of dichloromethane, 0.22 mol of diphenylphosphine chloride was added into the reactor, stirred and mixed, then 100 ml of 2-piperazine carboxylic acid dichloromethane solution (0.1 mol of 2-piperazine carboxylic acid was dissolved in 100 ml of dichloromethane) was slowly added dropwise, dropwise for 20 min, then 0.3 mol of triethylamine was slowly added dropwise, dropwise for 10 min, after dropwise addition, refluxed for 5 h, then cooled to room temperature, distilled at 35°C under reduced pressure for 45 min, washed with deionized water for 3 times (200 ml each time), filtered, vacuum dried at 60°C for 4 h to obtain a nitrogen-phosphorus compound;

[0044] S3: Under nitrogen protection, 1200 g of toluene, 0.1 mol of four-armed star compound, 0.2 mol of nitrogen-phosphorus compound was added into the reactor, stirred and mixed, heated to 90°C, then 15 g of p-toluenesulfonic acid was added, reacted for 5 h (water generated during the reaction was removed using a water trap), then cooled to room temperature, slowly added saturated sodium bicarbonate solution to adjust pH to neutral, stirred for 30 min, separated into layers by standing, the organic phase was transferred to a rotary evaporator, distilled at 60°C under reduced pressure for 4 h, vacuum dried at 70°C for 10 h to obtain a nitrogen-phosphorus modified four-armed star compound; the number average molecular weight is 3291;

[0045] S4: 800 ml of toluene, 0.1 mol of nitrogen-phosphorus modified four-armed star compound was added into the reactor, stirred for 1 h, then 0.22 mol of octadecyldimethylmethoxysilane, 0.2 mol of triethylamine was added, reacted at 70°C for 5 h, then centrifuged, washed with deionized water for 3 times (500 ml each time), filtered, and vacuum dried at 70°C for 12 h to obtain the modified flame retardant; the number average molecular weight was 3913.

[0046] Example 3 Preparation of modified flame retardant:

[0047] S1: Under nitrogen protection, 1200 g of DMF, 0.1 mol of pentaerythritol and 2 mol of 3,6-dimethyl-1,4-dioxane-2,5-dione were added into the reactor, stirred and mixed uniformly, heated to 130°C, stirred for 15 min, then 10 g of catalyst stannous octoate was added, reacted for 26 h, then cooled to room temperature, distilled at 60°C under reduced pressure for 2 h to obtain a crude product, the crude product was added into 500 ml of chloroform, stirred and mixed uniformly, then 500 ml of cold methanol was added, precipitated and separated, filtered, then washed with methanol for 3 times (500 ml each time), and vacuum dried at 60°C for 5 h to obtain a four-armed star compound; the number average molecular weight was 2984;

[0048] S2: Under nitrogen protection, 200 ml of dichloromethane, 0.25 mol of diphenylphosphine chloride was added into the reactor, stirred and mixed uniformly, then 100 ml of 2-piperazine carboxylic acid dichloromethane solution (0.1 mol of 2-piperazine carboxylic acid was dissolved in 100 ml of dichloromethane) was slowly added dropwise, dropwise for 20 min, then 0.3 mol of triethylamine was slowly added dropwise, dropwise for 10 min, after the dropwise addition was completed, refluxed for 6 h, then cooled to room temperature, distilled at 35°C under reduced pressure for 45 min, washed with deionized water for 3 times (200 ml each time), filtered, and vacuum dried at 60°C for 4 h to obtain a nitrogen-phosphorus compound;

[0049] S3: Under nitrogen protection, 1200 g of toluene, 0.1 mol of four-armed star compound, 0.22 mol of nitrogen-phosphorus compound was added into the reactor, stirred and mixed uniformly, heated to 100°C, then 15 g of p-toluenesulfonic acid was added, reacted for 4 h (water generated during the reaction was removed using a water trap), then cooled to room temperature, slowly added saturated sodium bicarbonate solution to adjust the pH to neutral, stirred thoroughly for 30 min, separated into layers, the organic phase was transferred to a rotary evaporator, distilled at 60°C under reduced pressure for 4 h, and vacuum dried at 70°C for 10 h to obtain a nitrogen-phosphorus modified four-armed star compound; the number average molecular weight was 4060;

[0050] S4: 800 ml of toluene, 0.1 mol of nitrogen-phosphorus modified four-armed star-shaped compound was added into the reactor, stirred for 1 h, then 0.25 mol of octadecyl dimethyl methoxysilane, 0.2 mol of triethylamine was added, reacted at 80℃ for 4 h, then centrifuged, washed with deionized water for 3 times (500 ml each time), filtered, and vacuum dried at 70℃ for 12 h to obtain the modified flame retardant; the number average molecular weight was 4681.

[0051] Example 4 Preparation of adhesive:

[0052] A1: 200 ml of DMF, 10 g of castor oil, and 2 g of strong acid cation exchange resin were added into the reactor, stirred and mixed uniformly, heated to 50℃, then 30 g of formic acid and 90 g of 30 wt% H2O2 solution were mixed uniformly, the mixed solution of formic acid and H2O2 solution was slowly added dropwise, and the dropping was maintained for 20 min, after 8 h of reaction, the upper clear liquid was transferred to a separatory funnel, petroleum ether was added for extraction three times (300 ml each time), and 50℃ reduced pressure distillation was carried out for 5 h to obtain an epoxy compound; the reaction equation is shown as follows:

[0053] .

[0054] A2: Under nitrogen protection, 200 ml of anhydrous DMF, 20 g of the epoxy compound, and 10 g of (1,4-phenylene bis (1,3,2-dioxaborolan-2,4-diyl)) dimethylthiol were added into the reactor, stirred and mixed uniformly, then 5 g of triethylamine was added, heated to 80℃ for 6 h, then cooled to room temperature, 1M hydrochloric acid was added to adjust the pH value to 7, 200 ml of ice water was added and stirred, a precipitate was separated out, filtered, and vacuum dried at 60℃ for 6 h to obtain an adhesive; the reaction equation is shown as follows:

[0055] .

[0056] Example 5 Preparation of high-strength flame-retardant sound and heat insulation composite material:

[0057] (1) Take: polyurethane resin 400 g, polyvinylpyrrolidone 100 g, ceramic hollow microsphere 100 g, ceramic fiber 60 g, adhesive (prepared in example 4) 50 g, modified flame retardant (prepared in example 1) 10 g, antioxidant (UV-531) 20 g;

[0058] (2) The polyurethane resin, polyvinylpyrrolidone, adhesive, modified flame retardant, and antioxidant were mixed, the stirring speed was 500 r / min, and the stirring was carried out for 30 min to obtain a mixture A; the ceramic fiber was ground and then mixed with the ceramic hollow microsphere, the stirring speed was 800 r / min, and the stirring was carried out for 50 min to obtain a mixture B;

[0059] (3) Mix mixture A and mixture B uniformly, stirring speed is 600 r / min, stirring for 40 min, extrude through double screw extruder, feeding section, compression section, homogenization section and die temperature are 150℃, 170℃, 185℃ and 170℃ respectively, cool and shape, to obtain high-strength flame-retardant sound and heat insulation composite material.

[0060] Example 6 Preparation of high-strength flame-retardant sound and heat insulation composite material:

[0061] (1) Weigh by weight: polyurethane resin 500g, polyvinylpyrrolidone 120g, ceramic hollow microsphere 120g, ceramic fiber 80g, adhesive (prepared in example 4) 60g, modified flame retardant (prepared in example 2) 20g, antioxidant (UV-326) 30g;

[0062] (2) Mix polyurethane resin, polyvinylpyrrolidone, adhesive, modified flame retardant, antioxidant, stirring speed is 500 r / min, stirring for 30 min, to obtain mixture A; grind ceramic fiber and mix with ceramic hollow microsphere, stirring speed is 800 r / min, stirring for 50 min, to obtain mixture B;

[0063] (3) Mix mixture A and mixture B uniformly, stirring speed is 600 r / min, stirring for 40 min, extrude through double screw extruder, feeding section, compression section, homogenization section and die temperature are 150℃, 170℃, 185℃ and 170℃ respectively, cool and shape, to obtain high-strength flame-retardant sound and heat insulation composite material.

[0064] Example 7 Preparation of high-strength flame-retardant sound and heat insulation composite material:

[0065] (1) Weigh by weight: polyurethane resin 600g, polyvinylpyrrolidone 150g, ceramic hollow microsphere 150g, ceramic fiber 100g, adhesive (prepared in example 4) 80g, modified flame retardant (prepared in example 3) 30g, antioxidant (UV-531) 40g;

[0066] (2) Mix polyurethane resin, polyvinylpyrrolidone, adhesive, modified flame retardant, antioxidant, stirring speed is 500 r / min, stirring for 30 min, to obtain mixture A; grind ceramic fiber and mix with ceramic hollow microsphere, stirring speed is 800 r / min, stirring for 50 min, to obtain mixture B;

[0067] (3) The mixture A and mixture B are mixed evenly, the stirring speed is 600 r / min, stirring for 40 min, extruded by double screw extruder, the feeding section, compression section, homogenization section and die temperature are 150℃, 170℃, 185℃ and 170℃ respectively, and then cooled to form, to obtain the high-strength flame-retardant soundproof and heat-insulating composite material.

[0068] Comparative Example 1

[0069] The raw material composition and preparation method of the high-strength flame-retardant soundproof and heat-insulating composite material are basically the same as those of Example 6, except that the modified flame retardant is replaced by an equal weight of the nitrogen-phosphorus modified four-arm star-shaped compound prepared in step S3 of Example 2.

[0070] Comparative Example 2

[0071] The raw material composition and preparation method of the high-strength flame-retardant soundproof and heat-insulating composite material are basically the same as those of Example 6, except that the modified flame retardant is replaced by an equal weight of the modified flame retardant prepared by the following method:

[0072] The preparation method of the modified flame retardant is basically the same as that of Example 2, except that the addition amount of the nitrogen-phosphorus compound in step S3 is increased to 0.4 mol.

[0073] Comparative Example 3

[0074] The raw material composition and preparation method of the high-strength flame-retardant soundproof and heat-insulating composite material are basically the same as those of Example 6, except that the modified flame retardant is replaced by an equal weight of the modified flame retardant prepared by the following method:

[0075] The preparation method of the modified flame retardant is basically the same as that of Example 2, except that the octadecyldimethylmethoxysilane in step S4 is replaced by an equal molar amount of methoxy(dimethyl)octylsilane.

[0076] Comparative Example 4

[0077] The raw material composition and preparation method of the high-strength flame-retardant soundproof and heat-insulating composite material are basically the same as those of Example 6, except that the modified flame retardant is replaced by an equal weight of the modified flame retardant prepared by the following method:

[0078] The preparation method of the modified flame retardant is basically the same as that of Example 2, except that the 2-piperazine carboxylic acid in step S2 is replaced by an equal molar amount of (S)-3-piperidine carboxylic acid.

[0079] Comparative Example 5

[0080] The raw material composition and preparation method of the high-strength flame-retardant soundproof and heat-insulating composite material are basically the same as those of Example 6, except that the adhesive is replaced by an equal weight of the adhesive prepared by the following method:

[0081] The preparation method of the adhesive is basically the same as that of Example 4, except that the castor oil in step A1 is replaced by an equal mass of glycerol monooleate.

[0082] Comparative Example 6

[0083] The raw material composition and preparation method of the high-strength flame-retardant sound and heat insulation composite material are basically the same as those of Example 6, except that the adhesive is replaced by an equal weight of the adhesive prepared by the following method:

[0084] The preparation method of the adhesive is basically the same as that of Example 4, except that the castor oil in step A1 is replaced by an equal mass of glycerol monooleate.

[0085] Comparative Example 7

[0086] The raw material composition and preparation method of the high-strength flame-retardant sound and heat insulation composite material are basically the same as those of Example 6, except that the adhesive is replaced by an equal weight of the adhesive prepared by the following method:

[0087] The preparation method of the adhesive is basically the same as that of Example 4, except that the (1,4-phenylenebis(1,3,2-dioxaborolan-2,4-diyl)) dimercaptan in step A2 is replaced by an equal mass of 1,4-benzenedimercaptan.

[0088] The polyurethane resin used in the present application is WANNATE® 6087F produced by Wanhua Chemical Group Co., Ltd.; the polyvinylpyrrolidone is PVP K30; the ceramic hollow microsphere is E-SPHERES produced by Dalian Yibang Technology Co., Ltd.; the ceramic fiber is a 1050 type ceramic fiber from Shandong Haoyang Energy-saving Material Co., Ltd., with a fiber diameter of 2-4 μm, an Al2O3 content of 46 wt%, and a SiO2 content of 52 wt%; and the strong acidic cation exchange resin is a polymer of divinylbenzene and sodium vinylbenzenesulfonate, with a brand name of Amberlite® IMAC HP1110 resin produced by Sinopharm Chemical Reagent Co., Ltd.

[0089] The high-strength flame-retardant sound and heat insulation composite materials prepared in Examples 5-7 and Comparative Examples 1-7 are subjected to tensile property testing according to GB / T 1040.1-2006; flame-retardant property testing is performed using a horizontal and vertical combustion tester according to ASTM-D3801 standard, with a sample size of 127 mm x 13 mm x 10 mm; thermal conductivity testing is performed according to GB / T 10295-2008; and sound insulation performance testing is performed according to GB / Z27764-2011 method (sound source frequency of 400 Hz). The test results are shown in Table 1.

[0090] Table 1 Performance test data table

[0091]

[0092] As can be seen from Table 1, the high-strength flame-retardant sound and heat insulation composite material prepared by the application has good mechanical properties, flame-retardant properties, sound insulation and heat insulation properties.

[0093] The modified flame retardant prepared in the application has a unique star-shaped molecular structure, which has higher thermal stability and can form a more dense crosslinked carbon layer than linear polymers at high temperatures; at the same time, the star-shaped molecular structure realizes good dispersion of nitrogen and phosphorus elements through chemical bonding, produces synergistic flame-retardant effect of gas phase and condensed phase during combustion, and forms a dense three-dimensional network carbon layer. In addition, the introduction of silane further promotes the formation of a dense silicon-carbon composite carbon layer, effectively isolating heat and oxygen transmission; the introduction of octadecyl dimethyl methoxysilane improves the dispersibility and compatibility of the flame retardant in the matrix, and the long chain of octadecyl prevents the flame retardant from agglomerating through physical steric hindrance, promoting its dispersion in the matrix material and avoiding stress concentration caused by excessive local concentration. Good dispersibility and compatibility avoid stress cracking caused by the flame retardant as a "defect point", and improve the tensile strength of the material.

[0094] The epoxy groups in the adhesive prepared in the application form a three-dimensional network structure with the boron-containing crosslinking agent, and a high-crosslinking-density skeleton is constructed through thiol-epoxy click reaction, significantly improving the tensile strength. At the same time, the long fatty chain of castor oil endows the molecular chain segment with dynamic flexibility, avoiding brittle fracture of traditional rigid crosslinking systems. The borate ester bond (B-O) contained in the adhesive has reversible dynamic properties and can be broken and recombined under external force, absorbing energy and preventing stress concentration, so that the material exhibits high ductility when stretched. The temperature responsiveness of the borate ester bond allows it to dynamically recombine at high temperatures, relieving thermal stress; the crosslinking network remains rigid at low temperatures, avoiding brittle fracture.

[0095] The above is only a preferred embodiment of the application and is not intended to limit the application; however, for ordinary skilled persons in the art, some minor changes, modifications and equivalent changes made to the above disclosed technical content without departing from the scope of the technical solutions of the application are equivalent embodiments of the application; at the same time, any equivalent changes, modifications and evolution of the above embodiments made according to the essential technology of the application are still within the protection scope of the technical solutions of the application.

Claims

1. A high strength fire-retardant acoustical and thermal insulation composite material, characterized in that, The raw materials include the following components by weight: polyurethane resin 40-60 parts, polyvinylpyrrolidone 10-15 parts, ceramic hollow microsphere 10-15 parts, ceramic fiber 6-10 parts, adhesive 5-8 parts, modified flame retardant 1-3 parts, antioxidant 2-4 parts; The modified flame retardant is prepared by the following method: S1: pentaerythritol reacts with 3,6-dimethyl-1,4-dioxane-2,5-dione under the catalysis of stannous octoate to generate a four-arm star compound; S2: 2-piperazine carboxylic acid reacts with diphenyl phosphinic chloride to generate a nitrogen phosphorus compound; S3: the four-arm star compound reacts with the nitrogen phosphorus compound under the action of p-toluenesulfonic acid to generate a nitrogen phosphorus modified four-arm star compound; S4: the nitrogen phosphorus modified four-arm star compound reacts with octadecyldimethylmethoxysilane to generate a modified flame retardant; In step S1, the molar ratio of pentaerythritol to 3,6-dimethyl-1,4-dioxane-2,5-dione is 1:(12-20); In step S2, the molar ratio of 2-piperazine carboxylic acid to diphenyl phosphinic chloride is 1:(2-2.5); In step S3, the molar ratio of the four-arm star compound to the nitrogen phosphorus compound is 1:(1.8-2.2); In step S4, the molar ratio of the nitrogen phosphorus modified four-arm star compound to octadecyldimethylmethoxysilane is 1:(2-2.5); The adhesive is prepared by the following method: A1: castor oil reacts under the action of formic acid and H2O2 to generate an epoxy compound; A2: the epoxy compound reacts with (1,4-phenylenebis(1,3,2-dioxaborolan-2,4-diyl)) dimethyl sulfide to generate an adhesive.

2. A high strength fire-retardant sound and heat insulating composite material according to claim 1, characterized in that, In step A1, the mass ratio of castor oil to formic acid is 1:

3.

3. A high strength fire-retardant sound and heat insulating composite material according to claim 1, characterized in that, In step A2, the mass ratio of the epoxy compound to (1,4-phenylenebis(1,3,2-dioxaborolan-2,4-diyl)) dimethyl sulfide is 2:

1.

4. The high strength fire resistant sound and heat insulating composite material according to claim 1, wherein, The antioxidant is one of UV-531 and UV-326.

5. A method for preparing a high-strength flame-retardant, sound-insulating, and heat-insulating composite material according to any one of claims 1-4, characterized in that, The method includes the following steps: (1) weigh the following components by weight parts: polyurethane resin 40-60 parts, polyvinylpyrrolidone 10-15 parts, ceramic hollow microsphere 10-15 parts, ceramic fiber 6-10 parts, adhesive 5-8 parts, modified flame retardant 1-3 parts, antioxidant 2-4 parts; (2) mix polyurethane resin, polyvinylpyrrolidone, adhesive, modified flame retardant, and antioxidant to obtain mixture A; grind the ceramic fiber and then mix it with the ceramic hollow microsphere to obtain mixture B; (3) mix mixture A and mixture B uniformly, extrude through an extruder, and cool to form a high-strength flame-retardant sound and heat insulation composite material.

Citation Information

Patent Citations

  • Anti-cracking sound- insulation composite material and preparation method thereof

    CN113563771A

  • Nitrogen-containing saturated heterocyclic compound

    CN103562191A

  • Purpose of multi-arm star copolymer used as diverting agent for fracturing and preparation method of multi-arm star copolymer

    CN105154058A