Environment-friendly flame-retardant PBS ecological integrated wallboard material and preparation method thereof
By adding a core-shell flame retardant to PBS, the problems of PBS's flammability and insufficient mechanical strength are solved, improving the flame retardant performance and mechanical strength of the eco-integrated wall panel, making it suitable for large-scale production and expanding its applications.
Patent Information
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- FUZHOU UNIV
- Filing Date
- 2026-04-02
- Publication Date
- 2026-05-29
AI Technical Summary
PBS material is flammable and lacks sufficient mechanical strength, posing a fire safety hazard and limiting its application in eco-friendly integrated wall panels.
A core-shell flame retardant is added during the melting process of PBS. By modifying fumed silica with KH560 and hybridizing nano-silicon nitride with aluminum hypophosphite, a core-shell structure is formed, which improves flame retardant performance and mechanical strength.
It significantly improves the flame retardant properties and mechanical strength of PBS eco-integrated wall panels, simplifies the preparation process, is suitable for large-scale production, is environmentally friendly and pollution-free, and expands the functionality of eco-integrated wall panels.
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Abstract
Description
Technical Field
[0001] This invention belongs to the field of polymer composite materials, specifically relating to an environmentally friendly flame-retardant PBS eco-integrated wall panel material and its preparation method. Background Technology
[0002] Eco-integrated wall panels are a new type of prefabricated wall material that integrates multiple functions such as structure, insulation, and decoration. They typically use environmentally friendly materials such as bamboo and wood fiber, natural stone powder, carbon crystal powder, and PVC powder, and are formed through processes such as high-temperature fusion and hot-pressing. They not only possess core advantages such as outstanding environmental friendliness and high installation efficiency, but also have multiple functions including excellent waterproofing, moisture resistance, fire resistance, sound insulation, heat insulation, and easy cleaning, solving problems such as mold growth and difficulty in cleaning associated with traditional materials.
[0003] Polybutylene succinate (PBS), as a fully biodegradable polyester, shows great potential in the field of eco-friendly wall panels. However, PBS itself is a flammable material with a low limiting oxygen index, a high calorific value during combustion, and significant dripping, posing a significant fire safety hazard. Furthermore, its insufficient mechanical strength further restricts its application in interior decorative wall materials that require both safety and structural stability. Summary of the Invention
[0004] The purpose of this invention is to provide an environmentally friendly flame-retardant PBS eco-integrated wall panel material and its preparation method. The method involves adding a core-shell flame retardant during the melting process of PBS for blending, which imparts good flame-retardant properties to the polymer matrix while further improving its mechanical strength.
[0005] To achieve the above objectives, the present invention adopts the following technical solution: An environmentally friendly flame-retardant PBS eco-integrated wall panel material, the preparation method of which includes the following steps: (1) Disperse the silane coupling agent KH560 in an ethanol solution by ultrasonication, then add fumed silica, adjust the pH to 5, and react by heating and stirring to obtain KH560-SiO2 hybrid sol; (2) Add aluminum hypophosphite (AHP) to the KH560-SiO2 hybrid sol obtained in step (1), disperse it by ultrasonication, and then heat and stir it to react. After washing and drying, a white powdery intermediate AHP@SiO2 is obtained. (3) Disperse the silane coupling agent KH560 in an ethanol solution by ultrasonication, then add nano silicon nitride, adjust the pH to 5, then heat and stir the reaction, and then wash and dry to obtain modified silicon nitride (Si3N4-g-KH560). (4) The intermediate AHP@SiO2 obtained in step (2) is ultrasonically dispersed in isopropanol, and then the modified silicon nitride obtained in step (3) is added. The mixture is ultrasonically dispersed to form a uniform suspension. Then, it is continuously heated and stirred with intermittent ultrasonication. After washing, drying and grinding, the core-shell flame retardant AHP@SiO2 / Si3N4 is obtained. (5) Polybutylene succinate and the core-shell flame retardant AHP@SiO2 / Si3N4 obtained in step (4) are melt-blended in a torque rheometer. The resulting blend is then hot-pressed and melted before being cold-pressed to obtain the environmentally friendly flame-retardant PBS eco-integrated wall panel material.
[0006] Furthermore, in step (1), the amount of silane coupling agent used is 5% of the mass of fumed silica.
[0007] Furthermore, in step (2), the amount of aluminum hypophosphite used is 10 times the mass of fumed silica in the KH560-SiO2 hybrid sol.
[0008] Furthermore, the concentration of the ethanol solution in steps (1) and (3) is 95 wt%.
[0009] Furthermore, in step (3), the amount of silane coupling agent used is 5% of the mass of nano-silicon nitride.
[0010] Furthermore, the ultrasonic dispersion time in steps (1) to (3) is 45 min.
[0011] Furthermore, the heating and stirring reaction in steps (1) to (3) is carried out at a temperature of 50°C, a stirring rate of 30 r / min, and a stirring time of 12 h.
[0012] Furthermore, the drying temperature in steps (2) and (3) is 60°C and the drying time is 24 h.
[0013] Furthermore, the mass ratio of the intermediate AHP@SiO2 to the modified silicon nitride used in step (4) is 10:1.5.
[0014] Furthermore, in step (4), the time for the first ultrasonic dispersion is 15 min, and the time for the second ultrasonic dispersion is 30 min.
[0015] Furthermore, the heating and stirring temperature in step (4) is 50°C, the stirring rate is 30 r / min, and the stirring time is 6 h. During this period, ultrasonication is performed for 5 min every 1 h to avoid the destruction of the intermediate structure due to uneven dispersion of components as much as possible.
[0016] Further, the mass percentage ratio of polybutylene succinate to core-shell flame retardant AHP@SiO2 / Si3N4 used in step (5) is (80-95):(5-20).
[0017] Furthermore, the processing temperature of the melt blending reaction in step (5) is 135°C, the rotor speed is 60 r / min, and the time is 10 min.
[0018] Furthermore, the hot pressing melting temperature in step (5) is 135°C, the pressure is 10 MPa, and the time is 10 min.
[0019] Furthermore, the cold pressing temperature in step (5) is room temperature, the pressure is 10 MPa, and the time is 10 min.
[0020] This invention utilizes a series of environmentally friendly and pollution-free raw materials to prepare environmentally friendly flame-retardant PBS eco-integrated wall panel materials through melt blending, significantly improving the mechanical and flame-retardant properties of the polymer. The beneficial effects of this invention are as follows: (1) This invention uses PBS, inorganic aluminum hypophosphite, fumed silica and nano silicon nitride as raw materials, KH560 as modifier, and prepares core-shell flame retardant by surface multiple grafting. Then, it efficiently prepares ecological integrated wall panel material by melt blending and cold pressing. Its preparation process technology is mature, the steps are clear, the conditions are mild and easy to control, and the recycling method is environmentally friendly and pollution-free. It is suitable for large-scale continuous production, which greatly expands the functionality of traditional ecological integrated wall panels and has good industrialization prospects and social and economic benefits.
[0021] (2) In this invention, KH560 is used as a surface grafting modifier. The silanol generated after hydrolysis of KH560 forms Si-O-Si covalent bonds with the hydroxyl groups on the surface of SiO2, and effectively bridges the micron core aluminum hypophosphite with the nano shell fumed silica, thereby improving the overall compatibility. The nano silicon nitride grafted on the KH560 surface can not only chemically crosslink with the intermediate layer (SiO2-KH560), but its long-chain alkane part (-(CH2)3-) is chemically similar to and compatible with the methylene chain of PBS. It can generate good entanglement and wetting through van der Waals forces, thereby improving the compatibility with the PBS matrix.
[0022] (3) The present invention designs a core-shell structure flame retardant constructed in steps. The structure is constructed sequentially by one-step in-situ method, which simplifies the process. The gas phase flame retardancy of aluminum hypophosphite and the condensed phase char formation and barrier effect of nano SiO2 / Si3N4 produce a "phosphorus-silicon-nitrogen" synergistic flame retardant effect. It is like a multifunctional "reinforced particle": the outer shell nano silicon nitride grafted KH560 is fixed on the surface of the middle layer through chemical action. It has extremely high hardness and thermal stability. As a strong physical barrier, it can effectively delay the transfer of heat and oxygen inward and protect the internal structure. The middle shell nano silicon dioxide grafted KH560 constructs an organic-inorganic hybrid network on the surface of aluminum hypophosphite, like an "adhesive" and "buffer layer". The core micron inorganic aluminum hypophosphite serves as the second flame retardant barrier. Attached Figure Description
[0023] Figure 1 The FTIR spectrum of the core-shell flame retardant AHP@SiO2 / Si3N4 prepared in Example 1.
[0024] Figure 2 The image shows a SEM image of the core-shell flame retardant AHP@SiO2 / Si3N4 prepared in Example 1.
[0025] Figure 3 The image shows a cross-section of the environmentally friendly flame-retardant PBS eco-integrated wall panel material prepared in Example 1.
[0026] Figure 4 The image shows a cross-section of the environmentally friendly flame-retardant PBS eco-integrated wall panel material prepared in Example 1 after combustion. Detailed Implementation
[0027] An environmentally friendly flame-retardant PBS eco-integrated wall panel material, the preparation method of which includes the following steps: (1) Disperse 5% by mass of silane coupling agent KH560 in 95wt% ethanol solution by ultrasonication for 45 min, then add fumed silica, adjust pH to 5, and then heat and stir at 50℃ and 30 r / min for 12 h to obtain KH560-SiO2 hybrid sol. (2) Add aluminum hypophosphite (AHP) with a mass of 10 times that of fumed silica to the KH560-SiO2 hybrid sol obtained in step (1), disperse it by ultrasonication for 45 min, and then heat and stir it at 50℃ and 30 r / min for 12 h. After washing, dry it at 60℃ for 24 h to obtain a white powdery intermediate AHP@SiO2. (3) Disperse 5% by mass of nano-silicon nitride silane coupling agent KH560 in a 95wt% ethanol solution by ultrasonication for 45 min, then add nano-silicon nitride, adjust the pH to 5, and then heat and stir the reaction at 50℃ and 30 r / min for 12 h. After washing, dry at 60℃ for 24 h to obtain modified silicon nitride (Si3N4-g-KH560). (4) The intermediate AHP@SiO2 obtained in step (2) was ultrasonically dispersed in isopropanol for 15 min. Then, the modified silicon nitride obtained in step (3) was added at a mass ratio of intermediate AHP@SiO2 to modified silicon nitride of 10:1.5. The mixture was ultrasonically dispersed for 30 min to form a uniform suspension. Then, it was continuously heated and stirred at 50°C and 30 r / min for 6 h, with ultrasonication for 5 min every 1 h. After washing, it was vacuum dried at 60°C for 24 h and ground to obtain the core-shell flame retardant AHP@SiO2 / Si3N4. (5) Based on a weight percentage of 100%, 80-95% polybutylene succinate and 5-20% of the core-shell flame retardant AHP@SiO2 / Si3N4 obtained in step (4) are added to a torque rheometer and melt-blended at 135°C and 60 r / min for 10 min. The resulting blend is then hot-pressed at 135°C and 10 MPa for 10 min, and then cold-pressed at room temperature and 10 MPa for 10 min to obtain an environmentally friendly flame-retardant PBS ecological integrated wall panel material.
[0028] To make the content of this invention easier to understand, the technical solution of this invention will be further described below with reference to specific embodiments, but this invention is not limited thereto.
[0029] The raw materials used in the examples are: polybutylene succinate (99% purity), fumed silica (99% purity), silane coupling agent KH560 (99% purity), aluminum hypophosphite (98% purity), and nano-silicon nitride (99% purity). Before the experiment, each raw material particle was placed in a vacuum drying oven at 60°C and 0MPa for 12 hours to remove the influence of moisture. Example 1
[0030] (1) Disperse 5% by mass of silane coupling agent KH560 of fumed silica in a 95wt% ethanol solution by ultrasonication for 45 min, then transfer the fumed silica to the dispersion, adjust the pH to 5, and then heat and stir at 50℃ and 30 r / min for 12 h to obtain KH560-SiO2 hybrid sol. (2) Add 10 times the mass of fumed silica aluminum hypophosphite to KH560-SiO2 hybrid sol, ultrasonically disperse for 45 min, then heat and stir at 50℃ and 30 r / min for 12 h, and finally centrifuge and wash, and vacuum dry at 60℃ for 24 h to obtain white powder intermediate AHP@SiO2. (3) Disperse 5% by mass of nano-silicon nitride silane coupling agent KH560 in a 95wt% ethanol solution by ultrasonication for 45 min, then transfer the nano-silicon nitride to the dispersion, adjust the pH to 5, and then heat and stir at 50℃ and 30 r / min for 12 h. Finally, wash by centrifugation and vacuum dry at 60℃ for 24 h to obtain modified silicon nitride Si3N4-g-KH560; (4) The intermediate AHP@SiO2 was ultrasonically dispersed in isopropanol for 15 min, and then Si3N4-g-KH560 obtained in step (3) was added at a mass ratio of 10:1.5. The mixture was ultrasonically dispersed for another 30 min to form a uniform suspension. Then it was heated and stirred at 50℃ and 30 r / min for 6 h, with an interval of 1 h and 5 min of ultrasonication during the process. Finally, it was centrifuged and washed, vacuum dried at 60℃ for 24 h, and then ground to obtain the core-shell flame retardant AHP@SiO2 / Si3N4. (5) According to the weight, 80 parts of polybutylene succinate (PBS) and 20 parts of core-shell flame retardant AHP@SiO2 / Si3N4 were added to a torque rheometer and melt-blended for 10 min at 135℃ and a rotor speed of 60 r / min to obtain an environmentally friendly flame-retardant PBS blend. Then, the obtained environmentally friendly flame-retardant PBS blend was hot-pressed and melted at 135℃ and 10 MPa for 10 min, and then cold-pressed at room temperature and 10 MPa for 10 min to obtain an environmentally friendly flame-retardant PBS ecological integrated wall panel material.
[0031] Figure 1 The image shows the FTIR spectrum of the prepared core-shell flame retardant AHP@SiO2 / Si3N4. The image shows the spectrum at 2380 cm⁻¹. -1 1190 cm -1 The peaks at 1010 cm-1 represent the characteristic peaks of the pH and P=O stretching vibrations of the aluminum hypophosphite matrix, respectively. Compared to the matrix aluminum hypophosphite, it can be seen that after multiple surface grafting treatments, AHP@SiO2 / Si3N4 exhibits higher peak values at 1010 -1 935 cm -1 890 cm -1 A new characteristic peak was generated at 890 cm⁻¹. -1 The peak at 10¹⁰ cm⁻¹ corresponds to the Si-N stretching vibration of silicon nitride. -1The peak at 890 cm⁻¹ corresponds to the characteristic peak of PO-Si, indicating that aluminum hypophosphite underwent a cross-linking reaction with the epoxy functional groups. -1 The peak at this location is a characteristic peak of Si-ON / Al, indicating that KH560 forms a bond with the powder surface.
[0032] Figure 2 SEM images of the prepared core-shell flame retardant AHP@SiO2 / Si3N4 are shown. As can be seen, the particles exhibit a micron-sized, near-spherical or irregular mass structure, determined by the micron-sized aluminum hypophosphite core. Furthermore, due to the coating of nano-silica and silicon nitride, its surface is much rougher than that of bare aluminum hypophosphite. On the rough silica substrate, even smaller nano-silicon nitride particles can be observed, uniformly attached to or embedded in the shell surface in the form of "islands" or "protrusions," serving as additional reinforcing points.
[0033] Figure 3 The image shows a cross-section of the prepared environmentally friendly flame-retardant PBS eco-integrated wall panel material. As can be seen from the image, its overall structure exhibits a heterogeneous, uneven, and rough surface, with a relatively uniform texture. AHP@SiO2 / Si3N4 particles are attached to the PBS matrix in clusters, with an irregular porous surface that is tightly bonded to the continuous structure.
[0034] Figure 4 The image shows a SEM image of the prepared environmentally friendly flame-retardant PBS eco-integrated wall panel material after combustion. As can be seen from the image, it exhibits a typical "sea-island" structure, with the continuous gray matrix being the residual carbon phase, and the bright white / black spherical pores / particles dispersed within it being the second phase. Example 2
[0035] The difference is that in step (5), the amount of polybutylene succinate (PBS) is 85 parts and the amount of core-shell flame retardant AHP@SiO2 / Si3N4 is 15 parts, and the other operations are the same as in Example 1. Example 3
[0036] The difference is that in step (5), the amount of polybutylene succinate (PBS) is 90 parts and the amount of core-shell flame retardant AHP@SiO2 / Si3N4 is 10 parts, and the other operations are the same as in Example 1. Example 4
[0037] The difference is that in step (5), the amount of polybutylene succinate (PBS) is 95 parts and the amount of core-shell flame retardant AHP@SiO2 / Si3N4 is 5 parts, and the other operations are the same as in Example 1.
[0038] Comparative Example 1 By weight, 100 parts of polybutylene succinate (PBS) were added to a torque rheometer and melt-blended for 10 min at 135°C and a rotor speed of 60 r / min to obtain pure PBS polymer. The obtained pure PBS polymer was then hot-pressed and melted at 135°C and 10 MPa for 10 min, and then cold-pressed at room temperature and 10 MPa for 10 min to obtain pure PBS eco-integrated wall panel material.
[0039] Comparative Example 2 (1) According to the weight, 95 parts of polybutylene succinate (PBS), 4 parts of aluminum hypophosphite (AHP), 0.4 parts of fumed silica and 0.6 parts of nano silicon nitride were added to a torque rheometer and melt-blended for 10 min at 135℃ and a rotor speed of 60 r / min to obtain PBS / SiO2 / Si3N4 blend. Then, the obtained PBS / SiO2 / Si3N4 blend was hot-pressed and melted at 135℃ and 10 MPa for 10 min, and then cold-pressed at room temperature and 10 MPa for 10 min to obtain PBS / SiO2 / Si3N4 eco-integrated wall panel material.
[0040] Comparative Example 3 (1) Disperse 5% by mass of silane coupling agent KH560 of fumed silica in a 95wt% ethanol solution by ultrasonication for 45 min, then transfer the fumed silica to the dispersion, adjust the pH to 5, and then heat and stir at 50℃ and 30 r / min for 12 h to obtain KH560-SiO2 hybrid sol. (2) Add 10 times the mass of fumed silica aluminum hypophosphite to KH560-SiO2 hybrid sol and ultrasonically disperse for 45 min. Then heat and stir at 50℃ and 30 r / min for 12 h. Finally, wash by centrifugation and vacuum dry at 60℃ for 24 h to obtain white powder intermediate AHP@SiO2. (3) Disperse 5% by mass of nano-silicon nitride silane coupling agent KH560 in a 95wt% ethanol solution by ultrasonication for 45 min, then transfer the nano-silicon nitride to the dispersion, adjust the pH to 5, and then heat and stir at 50℃ and 30 r / min for 12 h. Finally, wash by centrifugation and vacuum dry at 60℃ for 24 h to obtain modified silicon nitride Si3N4-g-KH560; (4) According to the weight parts, 95 parts of polybutylene succinate (PBS), 4.4 parts of intermediate AHP@SiO2, and 0.6 parts of Si3N4-g-KH560 were added to a torque rheometer and melt-blended for 10 min at 135℃ and a rotor speed of 60 r / min to obtain PBS / AHP@SiO2 / Si3N4-g-KH560 blend. Then, the obtained PBS / AHP@SiO2 / Si3N4-g-KH560 blend was hot-pressed and melted at 135℃ and 10 MPa for 10 min, and then cold-pressed at room temperature and 10 MPa for 10 min to obtain PBS / AHP@SiO2 / Si3N4-g-KH560 eco-integrated wall panel material.
[0041] Comparative Example 4 (1) Disperse 5% by mass of silane coupling agent KH560 of fumed silica in a 95wt% ethanol solution by ultrasonication for 45 min, then transfer the fumed silica to the dispersion, adjust the pH to 5, and then heat and stir at 50℃ and 30 r / min for 12 h to obtain KH560-SiO2 hybrid sol. (2) 5% by mass of nano-silicon nitride silane coupling agent KH560 was ultrasonically dispersed in a 95wt% ethanol solution for 45 min. Then, the nano-silicon nitride was transferred to the dispersion, the pH was adjusted to 5, and then heated and stirred at 50℃ and 30 r / min for 12 h. Finally, after centrifugation and washing, it was vacuum dried at 60℃ for 24 h to obtain modified silicon nitride Si3N4-g-KH560. (3) Disperse the KH560-SiO2 hybrid sol in isopropanol by ultrasonication for 15 min, then add the Si3N4-g-KH560 obtained in step (3) at a mass ratio of 10:1.5, continue ultrasonic dispersion for 30 min to form a uniform suspension, then heat and stir at 50℃ and stirring rate of 30 r / min for 6 h, with ultrasonication for 5 min every 1 h during the period, finally centrifuge and wash, vacuum dry at 60℃ for 24 h and grind to obtain core-shell flame retardant SiO2 / Si3N4; (4) According to the weight, 95 parts of polybutylene succinate (PBS), 4 parts of aluminum hypophosphite, and 1 part of core-shell flame retardant SiO2 / Si3N4 were added to a torque rheometer and melt-blended for 10 min at 135°C and a rotor speed of 60 r / min to obtain a flame-retardant PBS / AHP / SiO2 / Si3N4 blend. Then, the obtained environmentally friendly flame-retardant PBS blend was hot-pressed and melted at 135°C and 10 MPa for 10 min, and then cold-pressed at room temperature and 10 MPa for 10 min to obtain PBS / AHP / SiO2 / Si3N4 eco-integrated wall panel material.
[0042] Performance testing: Density was tested using ρ = m / ΔV, where ΔV is the volume change obtained by immersing the sample in a graduated cylinder; water absorption was tested according to GB / T1034-2008 Water Absorption of Plastics; tensile strength was tested according to GB / T 1040.2-2006 Bending Properties of Plastics; flame retardancy rating was tested according to GB / T 529-2008 Flame Retardancy of Plastics; Oxygen Index (LOI) was tested according to GB / T 1410-2006 Oxygen Index of Plastics; the results are shown in Table 1.
[0043] Table 1 Performance test results of eco-friendly integrated wall panel material samples
[0044] As shown in Table 1, comparing the data from Examples 1-4, the flame retardancy rating and oxygen index of the resulting eco-integrated wall panel material gradually increased with the increase in the amount of core-shell flame retardant, but the tensile strength showed a trend of first increasing and then decreasing. This is because, in the core-shell flame retardant, the outer shell nano-silicon nitride possesses extremely high hardness and thermal stability, serving as a robust physical barrier to effectively protect the internal structure; the middle shell nano-silica can construct an organic-inorganic hybrid network between the components; and the core micron-sized inorganic aluminum hypophosphite can serve as a second flame retardant barrier. Simultaneously, the KH560 grafted onto the surface of the nano-silicon nitride promoted the interaction with PBS resin, reducing the distance between the core-shell flame retardant and the polymer chains, thereby improving the tensile strength. However, with the increase in the amount of core-shell flame retardant, agglomeration occurred within the material, causing a decrease in the tensile strength. Overall, the eco-integrated wall panel material prepared in Example 3 exhibited the best overall performance. In contrast, the pure PBS wall panel material prepared in Comparative Example 1 without the addition of core-shell flame retardant showed significantly weaker tensile strength, flame retardant rating, and oxygen index than the composite wall panel material prepared in the Examples with the addition of core-shell flame retardant. In Comparative Example 2, the flame retardants of each component were not surface modified, which significantly reduced the tensile strength, flame retardant rating, and oxygen index of the composite material. As can be seen from the data of Comparative Examples 3 and 4, the absence of orderly grafting of KH560-SiO2, aluminum hypophosphite, and Si3N4-g-KH560 also significantly affected the tensile strength, flame retardant rating, and oxygen index of the composite material.
[0045] The above description is only a preferred embodiment of the present invention. All equivalent changes and modifications made within the scope of the claims of the present invention should be included in the scope of the present invention.
Claims
1. A method for preparing an environmentally friendly flame-retardant PBS eco-integrated wall panel material, characterized in that, Includes the following steps: (1) Disperse silane coupling agent KH560 in ethanol solution by ultrasonication, then add fumed silica, adjust pH to 5, and react by heating and stirring to obtain KH560-SiO2 hybrid sol; (2) Add aluminum hypophosphite to the KH560-SiO2 hybrid sol obtained in step (1), disperse it by ultrasonication, and then heat and stir it to react. After washing and drying, a white powdery intermediate AHP@SiO2 is obtained. (3) Disperse silane coupling agent KH560 in ethanol solution by ultrasonication, then add nano silicon nitride, adjust pH to 5, then heat and stir the reaction, and then wash and dry to obtain modified silicon nitride. (4) The intermediate AHP@SiO2 obtained in step (2) is ultrasonically dispersed in isopropanol, and then the modified silicon nitride obtained in step (3) is added. The mixture is ultrasonically dispersed to form a uniform suspension. Then, it is continuously heated and stirred with intermittent ultrasonication. After washing, drying and grinding, the core-shell flame retardant AHP@SiO2 / Si3N4 is obtained. (5) Polybutylene succinate and the core-shell flame retardant AHP@SiO2 / Si3N4 obtained in step (4) are melt-blended, and the resulting blend is hot-pressed and then cold-pressed to obtain the environmentally friendly flame-retardant PBS ecological integrated wall panel material.
2. The preparation method of the environmentally friendly flame-retardant PBS eco-integrated wall panel material according to claim 1, characterized in that, The concentration of the ethanol solution in step (1) is 95 wt%; the amount of silane coupling agent is 5% of the mass of fumed silica; the temperature of the heating and stirring reaction is 50 °C, the stirring rate is 30 r / min, and the stirring time is 12 h.
3. The preparation method of the environmentally friendly flame-retardant PBS eco-integrated wall panel material according to claim 1, characterized in that, In step (2), the amount of aluminum hypophosphite used is 10 times the mass of fumed silica in the KH560-SiO2 hybrid sol; the heating and stirring reaction temperature is 50℃, the stirring rate is 30 r / min, and the stirring time is 12 h.
4. The preparation method of the environmentally friendly flame-retardant PBS eco-integrated wall panel material according to claim 1, characterized in that, In step (3), the concentration of the ethanol solution is 95 wt%, and the amount of silane coupling agent is 5% of the mass of nano-silicon nitride; the temperature of the heating and stirring reaction is 50 °C, the stirring rate is 30 r / min, and the stirring time is 12 h.
5. The preparation method of the environmentally friendly flame-retardant PBS eco-integrated wall panel material according to claim 1, characterized in that, The mass ratio of intermediate AHP@SiO2 to modified silicon nitride used in step (4) is 10:1.5; the heating and stirring temperature is 50℃, the stirring rate is 30 r / min, the stirring time is 6 h, and ultrasonication is performed for 5 min every 1 h during the process.
6. The preparation method of the environmentally friendly flame-retardant PBS eco-integrated wall panel material according to claim 1, characterized in that, The mass percentage ratio of polybutylene succinate to core-shell flame retardant AHP@SiO2 / Si3N4 used in step (5) is (80-95):(5-20).
7. The preparation method of the environmentally friendly flame-retardant PBS eco-integrated wall panel material according to claim 1, characterized in that, The processing temperature for the melt blending reaction in step (5) is 135°C and the time is 10 min.
8. The method for preparing the environmentally friendly flame-retardant PBS eco-integrated wall panel material according to claim 1, characterized in that, The hot pressing melting temperature in step (5) is 135°C, the pressure is 10 MPa, and the time is 10 min.
9. The method for preparing the environmentally friendly flame-retardant PBS eco-integrated wall panel material according to claim 1, characterized in that, The cold pressing process in step (5) is performed at room temperature, with a pressure of 10 MPa and a time of 10 min.
10. The environmentally friendly flame-retardant PBS eco-integrated wall panel material prepared by the method according to any one of claims 1-9.