Efficient flame-retardant polyester material and preparation method thereof
By adding a graded micro/nanostructured aerogel to the polyester material, a double barrier of carbon/SiO2 is formed, the problems of existing phosphorus-containing flame retardant polyesters in thermal and mechanical properties are solved, and the combination of efficient flame retardant properties and structural integrity is achieved, while avoiding environmental pollution.
Patent Information
- Application Number
- CN202510200898.5
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-02-24
- Publication Date
- 2025-06-17
AI Technical Summary
The existing phosphorus-containing flame retardant polyesters have problems of degradation in thermal or mechanical properties and serious melting and dripping. At the same time, halogen-containing flame retardant has a great impact on the environment, and it is necessary to improve its efficient flame retardant performance through halogen-free modification.
By adding a graded micro/nanostructured aerogel to the polyester material, a double barrier of carbon/SiO2 is formed, giving it excellent fire resistance and maintaining structural integrity in the flame. This aerogel forms a multiphase nanostructure through the steps of delignin and in-situ mineralization of willow particles to construct a graded micro/nanostructured aerogel.
The efficient flame retardant properties of polyester materials are achieved, structural integrity is maintained, thermal and mechanical properties are reduced, and environmental pollution is avoided.
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Abstract
Description
Technical Field
[0001] The present invention relates to the field of polyester materials, and particularly relates to a highly flame-retardant polyester material and a preparation method thereof. Background Art
[0002] Polyester materials are materials with relatively comprehensive properties. They have good transparency and high gloss; they have good airtightness and fragrance retention. Compared with general materials, polyester materials have relatively better mechanical properties, with better tensile strength and impact strength. Polyester materials also have excellent resistance to weak acids and oils, and at the same time have advantages such as non-toxicity and good chemical resistance stability. Due to these many advantages, polyester materials are used as high-grade packaging materials for various textiles, precision instruments, and electrical components. However, with the development of society and economy, the functional requirements for polyester materials are getting higher and higher, and high-efficiency flame retardancy is one of them. Currently, the flame retardants used for polyester flame retardant modification on the market are mainly halogen-containing and phosphorus-containing flame retardants. Among them, phosphorus is the most effective flame retardant element, and the flame retardants can be copolymer type or blend type flame retardants. However, the existing phosphorus-containing flame-retardant polyesters have difficult-to-solve problems such as a decrease in thermal performance or mechanical properties and serious melting dripping. At the same time, halogen-containing flame retardants also have a greater impact on the environment. Therefore, it is an urgent problem to improve the high-efficiency flame retardant performance of polyester by halogen-free modification. Summary of the Invention
[0003] Technical problems to be solved: The purpose of the present invention is to provide a highly flame-retardant polyester material. The polyester material is added with a hierarchical micro / nano-structured aerogel, and its self-formed carbon / SiO2 double barrier can endow it with excellent fire resistance and maintain structural integrity in the flame.
[0004] Technical solution: A highly flame-retardant polyester material, in parts by weight, includes the following components: 100 parts of polyester chips, 10-25 parts of flame-retardant filler, and 5-10 parts of tackifier; The flame-retardant filler is an aerogel with a hierarchical micro / nano structure. Further, the preparation method of the flame-retardant filler is as follows: Step 1: Soak willow wood particles in an acidic sodium hypochlorite solution, heat to 80-90°C, and keep for 7-8 h until the wood particles are fully bleached to obtain delignified willow wood particles; Step 2: Wash the delignified willow wood particles with 100°C hot water for 10-20 min and then perform freeze-drying to obtain willow wood particles with micro and nano pores; Step 3: Mix cetyltrimethylammonium bromide, urea, acetic acid hydrate, and deionized water evenly, slowly add methyltrimethoxysilane, and continue stirring to obtain a mixed solution; Step 4: Immerse the willow wood particles with micro- and nano-pores in the mixed solution, degas at 0.1 MPa for 30 - 40 min, then reduce the pressure to atmospheric pressure, repeat seven times, and then polymerize at 80 °C for 11 - 13 h to form a gel; Step 5: Wash the gel 3 - 4 times with methyltrimethoxysilane solution, and then replace the solvent with hexane three times; Step 6: Dry at 50 - 100 °C for 2 h to obtain the flame retardant filler. Further, in Step 1, the concentration of the acidic sodium hypochlorite solution is 2.00 wt%, and the pH is adjusted to 4.6 with acetic acid. Further, in Step 1, during the soaking process, the acidic sodium hypochlorite solution is replaced every 2 h. Further, in Step 3, the mass ratio of cetyltrimethylammonium bromide, urea, acetic acid hydrate, deionized water, and methyltrimethoxysilane is 1:(2 - 5):(0.5 - 2):100:(0.5 - 2). Further, in Step 5, the methyltrimethoxysilane solution is a mixture of methyltrimethoxysilane and ethanol with a mass ratio of 1:2. The preparation method of the above high-efficiency flame retardant polyester material is as follows: S1: Mix the polyester chips, flame retardant filler, and tackifier, and stir in a blender until evenly mixed; S2: Place it in an oven and dry at a temperature of 150 - 170 °C for 4 - 6 h; S3: Put the dried material into an extruder for extrusion and plasticization, and the heating temperature in the extruder is 260 - 265 °C; S4: Mold the plasticized material, and the high-efficiency flame retardant polyester material is obtained after output. Further, in Step S4, the molding temperature is 255 - 265 °C, the molding pressure is 20 - 30 MPa, and the molding time is 45 s. Beneficial effects: 1. The hierarchical micro / nano-structured aerogel is added to the polyester material of the present invention, and its self-formed carbon / SiO2 double barrier can endow it with excellent fire resistance and maintain structural integrity in the flame. 2. In the present invention, the hierarchical micro / nano-structured aerogel is obtained by delignifying willow wood particles to form willow wood particles with micro- and nano-pores. Initially, methyltrimethoxysilane forms a silane layer in the willow wood particles, and the long-chain polyamine provides electrostatic interaction, effectively eliminating the microphase separation defects and promoting the multi-scale interfacial bonding between methyltrimethoxysilane and the willow wood particle framework. Subsequently, the in-situ mineralization of methyltrimethoxysilane under alkaline conditions results in the growth of polymethylsilsesquioxane particles on the willow wood particle framework, forming a multiphase nanostructure. As the reaction proceeds, a continuous mesoporous network is formed, and through drying, nano-scale heterogeneous assembly is achieved, constructing the hierarchical micro / nano-structured aerogel. Through delignification, in-situ mineralization and. Detailed implementation manners The present invention provides an efficient flame-retardant polyester material and its preparation method. To make the objectives, technical solutions and effects of the present invention clearer and more definite, the following will further elaborate on the present invention in conjunction with embodiments. It should be understood that the specific embodiments described herein are only used to explain the present invention and are not used to limit the present invention. Example 1 A preparation method of an efficient flame-retardant polyester material, calculated by weight, the preparation steps are as follows: Step 1: Immerse willow wood particles in an acidic sodium hypochlorite solution with a concentration of 2.00 wt% and a pH of 4.6, heat to 85 °C, and keep for 8 h until the wood particles are fully bleached to obtain delignified willow wood particles; during the immersion process, replace the acidic sodium hypochlorite solution every 2 h; Step 2: Wash the delignified willow wood particles with 100 °C hot water for 20 min and then perform freeze-drying to obtain willow wood particles with micro- and nano-pores; Step 3: Mix cetyltrimethylammonium bromide, urea, acetic acid hydrate and deionized water evenly, then slowly add methyltrimethoxysilane and continue stirring to obtain a mixed solution; the mass ratio of cetyltrimethylammonium bromide, urea, acetic acid hydrate, deionized water and methyltrimethoxysilane is 1:2:1:100:1; Step 4: Immerse the willow wood particles with micro- and nano-pores in the mixed solution, degas at 0.1 MPa for 35 min, then reduce the pressure to atmospheric pressure, repeat seven times, and then polymerize at 80 °C for 12 h to form a gel; Step 5: Wash the gel 4 times with a methyltrimethoxysilane solution, and then replace the solvent with hexane three times; the methyltrimethoxysilane solution is a mixture of methyltrimethoxysilane and ethanol with a mass ratio of 1:2; Step 6: Dry at 80 °C for 2 h to obtain the flame-retardant filler; Step 7: Mix 100 parts of polyester chips, 20 parts of flame retardant filler and 8 parts of tackifier, and stir in a blender until evenly mixed; Step 8: Place it in an oven and dry at a temperature of 160 °C for 6 h; Step 9: Put the dried material into an extruder for extrusion and plasticization, and the heating temperature in the extruder is 265 °C; Step 10: Carry out compression molding on the plasticized material, the compression molding temperature is 260 °C, the compression molding pressure is 25 MPa, and the compression molding time is 45 s. The high-efficiency flame retardant polyester material is obtained as the output. Example 2 A preparation method of a high-efficiency flame retardant polyester material, calculated by weight, the preparation steps are as follows: Step 1: Immerse willow wood particles in an acidic sodium hypochlorite solution with a concentration of 2.00 wt% and a pH of 4.6, heat to 85 °C, and keep for 8 h until the wood particles are fully bleached to obtain delignified willow wood particles; During the immersion process, replace the acidic sodium hypochlorite solution every 2 h; Step 2: Rinse the delignified willow wood particles with 100 °C hot water for 20 min and then perform freeze-drying to obtain willow wood particles with micro- and nano-pores; Step 3: Mix cetyltrimethylammonium bromide, urea, acetic acid hydrate and deionized water evenly, slowly add methyltrimethoxysilane, and continue to stir to obtain a mixed solution; The mass ratio of cetyltrimethylammonium bromide, urea, acetic acid hydrate, deionized water and methyltrimethoxysilane is 1:4:1:100:1.5; Step 4: Immerse the willow wood particles with micro- and nano-pores in the mixed solution, degas at 0.1 MPa for 35 min, then reduce the pressure to atmospheric pressure, repeat seven times, and then polymerize at 80 °C for 12 h to form a gel; Step 5: Wash the gel 4 times with a methyltrimethoxysilane solution, and then replace the solvent with hexane three times; The methyltrimethoxysilane solution is a mixture of methyltrimethoxysilane and ethanol with a mass ratio of 1:2; Step 6: Dry at 80 °C for 2 h to obtain the flame retardant filler; Step 7: Mix 100 parts of polyester chips, 20 parts of flame retardant filler and 8 parts of tackifier, and stir in a blender until evenly mixed; Step 8: Place it in an oven and dry at a temperature of 160 °C for 6 h; Step 9: Put the dried material into an extruder for extrusion and plasticization, and the heating temperature in the extruder is 265 °C; Step 10: Carry out compression molding on the plasticized material, the compression molding temperature is 260 °C, the compression molding pressure is 25 MPa, and the compression molding time is 45 s. The high-efficiency flame retardant polyester material is obtained as the output. Example 3 A preparation method of an efficient flame-retardant polyester material, by weight, the preparation steps are as follows: Step 1: Immerse the willow wood particles in an acidic sodium hypochlorite solution with a concentration of 2.00 wt% and a pH of 4.6, heat to 85 °C, and keep for 8 h until the wood particles are fully bleached to obtain delignified willow wood particles; during the immersion process, replace the acidic sodium hypochlorite solution every 2 h; Step 2: Rinse the delignified willow wood particles with 100 °C hot water for 20 min and then perform freeze-drying to obtain willow wood particles with micro- and nano-pores; Step 3: Mix cetyltrimethylammonium bromide, urea, acetic acid hydrate, and deionized water evenly, and slowly add methyltrimethoxysilane, and continue stirring to obtain a mixed solution; the mass ratio of cetyltrimethylammonium bromide, urea, acetic acid hydrate, deionized water, and methyltrimethoxysilane is 1:5:1:100:1.5; Step 4: Immerse the willow wood particles with micro- and nano-pores in the mixed solution, degas at 0.1 MPa for 35 min, then reduce the pressure to atmospheric pressure, repeat seven times, and then polymerize at 80 °C for 12 h to form a gel; Step 5: Wash the gel 4 times with a methyltrimethoxysilane solution, and then replace the solvent with hexane three times; the methyltrimethoxysilane solution is a mixture of methyltrimethoxysilane and ethanol with a mass ratio of 1:2; Step 6: Dry at 80 °C for 2 h to obtain the flame-retardant filler; Step 7: Mix 100 parts of polyester chips, 20 parts of flame-retardant filler, and 8 parts of tackifier, and stir in a blender to mix evenly; Step 8: Put it into an oven and dry at a temperature of 160 °C for 6 h; Step 9: Put the dried material into an extruder for extrusion and plasticization, and the heating temperature in the extruder is 265 °C; Step 10: Mold the plasticized material, the molding temperature is 260 °C, the molding pressure is 25 MPa, and the molding time is 45 s, and the output is the efficient flame-retardant polyester material. Example 4 A preparation method of an efficient flame-retardant polyester material, by weight, the preparation steps are as follows: Step 1: Immerse the willow wood particles in an acidic sodium hypochlorite solution with a concentration of 2.00 wt% and a pH of 4.6, heat to 85 °C, and keep for 8 h until the wood particles are fully bleached to obtain delignified willow wood particles; during the immersion process, replace the acidic sodium hypochlorite solution every 2 h; Step 2: Rinse the delignified willow wood particles with 100 °C hot water for 20 min and then perform freeze-drying to obtain willow wood particles with micro- and nano-pores; Step 3: After mixing cetyltrimethylammonium bromide, urea, acetic acid hydrate, and deionized water evenly, slowly add methyltrimethoxysilane and continue stirring to obtain a mixed solution; the mass ratio of cetyltrimethylammonium bromide, urea, acetic acid hydrate, deionized water, and methyltrimethoxysilane is 1:4:1:100:2; Step 4: Immerse the willow wood particles with micro- and nano-pores in the mixed solution, degas at 0.1 MPa for 35 min, then reduce the pressure to atmospheric pressure, repeat seven times, and then polymerize at 80 °C for 12 h to form a gel; Step 5: Wash the gel 4 times with methyltrimethoxysilane solution, and then replace the solvent with hexane three times; the methyltrimethoxysilane solution is a mixture of methyltrimethoxysilane and ethanol with a mass ratio of 1:2; Step 6: Dry at 80 °C for 2 h to obtain the flame retardant filler; Step 7: Mix 100 parts of polyester chips, 20 parts of flame retardant filler, and 8 parts of tackifier, and stir in a blender to mix evenly; Step 8: Place in an oven and dry at a temperature of 160 °C for 6 h; Step 9: Put the dried material into an extruder for extrusion and plasticization, and the heating temperature in the extruder is 265 °C; Step 10: Carry out molding pressing on the plasticized material, the molding pressing temperature is 260 °C, the molding pressing pressure is 25 MPa, and the molding pressing time is 45 s, and the high-efficiency flame retardant polyester material is obtained as the output. Example 5 A preparation method of a high-efficiency flame retardant polyester material, in parts by weight, the preparation steps are as follows: Step 1: Immerse the willow wood particles in an acidic sodium hypochlorite solution with a concentration of 2.00 wt% and a pH of 4.6, heat to 85 °C, and keep for 8 h until the wood particles are fully bleached to obtain delignified willow wood particles; during the immersion process, replace the acidic sodium hypochlorite solution every 2 h; Step 2: Rinse the delignified willow wood particles with 100 °C hot water for 20 min and then perform freeze-drying to obtain willow wood particles with micro- and nano-pores; Step 3: After mixing cetyltrimethylammonium bromide, urea, acetic acid hydrate, and deionized water evenly, slowly add methyltrimethoxysilane and continue stirring to obtain a mixed solution; the mass ratio of cetyltrimethylammonium bromide, urea, acetic acid hydrate, deionized water, and methyltrimethoxysilane is 1:4:1:100:1.5; Step 4: Immerse the willow wood particles with micro- and nano-pores in the mixed solution, degas at 0.1 MPa for 35 min, then reduce the pressure to atmospheric pressure, repeat seven times, and then polymerize at 80 °C for 11 h to form a gel; Step 5: Wash the gel 4 times with methyltrimethoxysilane solution, and then replace the solvent with hexane three times; the methyltrimethoxysilane solution is a mixture of methyltrimethoxysilane and ethanol with a mass ratio of 1:2. Step 6: Dry at 80 °C for 2 h to obtain the flame retardant filler. Step 7: Mix 100 parts of polyester chips, 20 parts of flame retardant filler and 8 parts of tackifier, and stir in a blender until evenly mixed; Step 8: Place in an oven and dry at a temperature of 160 °C for 6 h. Step 9: Put the dried material into an extruder for extrusion and plasticization, and the heating temperature in the extruder is 265 °C. Step 10: Carry out molding pressing on the plasticized material, the molding pressing temperature is 260 °C, the molding pressing pressure is 25 MPa, and the molding pressing time is 45 s, and the high-efficiency flame retardant polyester material is obtained as the output. Example 6 Step 1: Immerse the willow wood particles in an acidic sodium hypochlorite solution with a concentration of 2.00 wt% and a pH of 4.6, heat to 85 °C, and keep for 8 h until the wood particles are fully bleached to obtain delignified willow wood particles; during the immersion process, replace the acidic sodium hypochlorite solution every 2 h. Step 2: Wash the delignified willow wood particles with 100 °C hot water for 20 min and then perform freeze-drying to obtain willow wood particles with micro- and nano-pores. Step 3: Mix cetyltrimethylammonium bromide, urea, acetic acid hydrate and deionized water evenly, slowly add methyltrimethoxysilane, and continue to stir to obtain a mixed solution; the mass ratio of cetyltrimethylammonium bromide, urea, acetic acid hydrate, deionized water and methyltrimethoxysilane is 1:4:1:100:1.5. Step 4: Immerse the willow wood particles with micro- and nano-pores in the mixed solution, degas at 0.1 MPa for 35 min, then reduce the pressure to atmospheric pressure, repeat seven times, and then polymerize at 80 °C for 13 h to form a gel. Step 5: Wash the gel 4 times with methyltrimethoxysilane solution, and then replace the solvent with hexane three times; the methyltrimethoxysilane solution is a mixture of methyltrimethoxysilane and ethanol with a mass ratio of 1:2. Step 6: Dry at 80 °C for 2 h to obtain the flame retardant filler. Step 7: Mix 100 parts of polyester chips, 20 parts of flame retardant filler and 8 parts of tackifier, and stir in a blender until evenly mixed; Step 8: Place in an oven and dry at a temperature of 160 °C for 6 h. Step 9: Put the dried material into an extruder for extrusion and plasticization, and the heating temperature in the extruder is 265 °C. Step 10: The plasticized material is subjected to compression molding at a temperature of 260 °C, a pressure of 25 MPa, and a time of 45 s, and the high-efficiency flame-retardant polyester material is obtained as the output. Example 7 Step 1: Soak the willow wood particles in an acidic sodium hypochlorite solution with a concentration of 2.00 wt% and a pH of 4.6, heat to 85 °C, and keep for 8 h until the wood particles are fully bleached to obtain delignified willow wood particles; during the soaking process, replace the acidic sodium hypochlorite solution every 2 h; Step 2: Rinse the delignified willow wood particles with 100 °C hot water for 20 min and then perform freeze-drying to obtain willow wood particles with micro- and nano-pores; Step 3: Mix cetyltrimethylammonium bromide, urea, acetic acid monohydrate, and deionized water evenly, then slowly add methyltrimethoxysilane and continue stirring to obtain a mixed solution; the mass ratio of cetyltrimethylammonium bromide, urea, acetic acid monohydrate, deionized water, and methyltrimethoxysilane is 1:4:1:100:1.5; Step 4: Immerse the willow wood particles with micro- and nano-pores in the mixed solution, degas at 0.1 MPa for 35 min, then reduce the pressure to atmospheric pressure, repeat seven times, and then polymerize at 80 °C for 12 h to form a gel; Step 5: Wash the gel 4 times with a methyltrimethoxysilane solution, and then replace the solvent with hexane three times; the methyltrimethoxysilane solution is a mixture of methyltrimethoxysilane and ethanol with a mass ratio of 1:2; Step 6: Dry at 80 °C for 2 h to obtain the flame-retardant filler; Step 7: Mix 100 parts of polyester chips, 10 parts of flame-retardant filler, and 8 parts of tackifier, and stir in a blender to mix evenly; Step 8: Put it into an oven and dry at a temperature of 160 °C for 6 h; Step 9: Put the dried material into an extruder for extrusion and plasticization, and the heating temperature in the extruder is 265 °C; Step 10: The plasticized material is subjected to compression molding at a temperature of 260 °C, a pressure of 25 MPa, and a time of 45 s, and the high-efficiency flame-retardant polyester material is obtained as the output. Example 8 Step 1: Soak the willow wood particles in an acidic sodium hypochlorite solution with a concentration of 2.00 wt% and a pH of 4.6, heat to 85 °C, and keep for 8 h until the wood particles are fully bleached to obtain delignified willow wood particles; during the soaking process, replace the acidic sodium hypochlorite solution every 2 h; Step 2: Rinse the delignified willow wood particles with 100 °C hot water for 20 min and then perform freeze-drying to obtain willow wood particles with micro- and nano-pores; Step 3: After mixing cetyltrimethylammonium bromide, urea, acetic acid hydrate and deionized water evenly, slowly add methyltrimethoxysilane and continue stirring to obtain a mixed solution; the mass ratio of cetyltrimethylammonium bromide, urea, acetic acid hydrate, deionized water and methyltrimethoxysilane is 1:4:1:100:1.5; Step 4: Immerse the willow wood particles with micro- and nano-pores in the mixed solution, degas at 0.1 MPa for 35 min, then reduce the pressure to atmospheric pressure, repeat seven times, and then polymerize at 80 °C for 12 h to form a gel; Step 5: Wash the gel 4 times with methyltrimethoxysilane solution, and then replace the solvent with hexane three times; the methyltrimethoxysilane solution is a mixture of methyltrimethoxysilane and ethanol with a mass ratio of 1:2; Step 6: Dry at 80 °C for 2 h to obtain the flame retardant filler; Step 7: Mix 100 parts of polyester chips, 25 parts of flame retardant filler and 8 parts of tackifier, and stir in a blender to mix evenly; Step 8: Put it into an oven and dry at a temperature of 160 °C for 6 h; Step 9: Put the dried material into an extruder for extrusion and plasticization, and the heating temperature in the extruder is 265 °C; Step 10: Carry out molding pressing on the plasticized material, the molding pressing temperature is 260 °C, the molding pressing pressure is 25 MPa, and the molding pressing time is 45 s, and the high-efficiency flame retardant polyester material is obtained as the output. Comparative Example 1 The difference between this example and Example 2 is that willow wood particles with micro- and nano-pores are directly added. Specifically: A preparation method of a high-efficiency flame retardant polyester material, calculated by weight, the preparation steps are as follows: Step 1: Immerse the willow wood particles in an acidic sodium hypochlorite solution with a concentration of 2.00 wt% and a pH of 4.6, heat to 85 °C, and keep for 8 h until the wood particles are fully bleached to obtain delignified willow wood particles; during the immersion process, replace the acidic sodium hypochlorite solution every 2 h; Step 2: Wash the delignified willow wood particles with 100 °C hot water for 20 min and then perform freeze-drying to obtain willow wood particles with micro- and nano-pores; Step 7: Mix 100 parts of polyester chips, 20 parts of willow wood particles with micro- and nano-pores and 8 parts of tackifier, and stir in a blender to mix evenly; Step 8: Put it into an oven and dry at a temperature of 160 °C for 6 h; Step 9: Put the dried material into an extruder for extrusion and plasticization, and the heating temperature in the extruder is 265 °C; Step 10: The plasticized material is subjected to compression molding at a temperature of 260 °C, a pressure of 25 MPa, and a time of 45 s, and the output is the high-efficiency flame-retardant polyester material. The tensile strength and elongation at break are tested according to the ASTM D638-2014 standard. The sheet size (mm) is 200×20, and the tensile speed is 50 mm / min. Table 1 Characterization of the mechanical properties of the materials in each example Measure the flame retardancy of the above examples: The flame retardancy includes the UL-94 flame retardant rating and the peak heat release rate, and the results are shown in Table 2 below: Table 2 Characterization of the flame retardancy of the materials in each example
Claims
1. A highly efficient flame-retardant polyester material, characterized in that: The composition comprises the following components by weight: 100 parts of polyester chips, 10-25 parts of flame retardant filler, and 5-10 parts of tackifier; The flame retardant filler is an aerogel with a hierarchical micro / nano structure.
2. A highly efficient flame retardant polyester material according to claim 1, characterized in that: The preparation method of the flame retardant filler is as follows: Step 1: Soak the willow wood particles in an acidic sodium hypochlorite solution, heat it to 80-90°C, and keep it for 7-8 hours until the wood particles are fully bleached to obtain delignified willow wood particles; Step 2: The delignified willow wood particles are rinsed with 100° C. hot water for 10-20 min and then freeze-dried to obtain willow wood particles with micro- and nano-pores; Step 3: After uniformly mixing hexadecyltrimethylammonium bromide, urea, hydrated acetic acid and deionized water, slowly adding methyltrimethoxysilane and continuing to stir to obtain a mixed solution; Step 4: Immerse the willow wood particles with micro- and nano-pores in the mixed solution, degas for 30-40 minutes at 0.1 MPa, and then reduce the pressure to atmospheric pressure, repeat seven times, and polymerize at 80°C for 11-13 hours to form a gel; Step 5: Wash the gel 3-4 times with methyltrimethoxysilane solution, and then replace the solvent with hexane three times; Step 6: Dry at 50-100°C for 2 hours to obtain the flame retardant filler.
3. A highly efficient flame retardant polyester material according to claim 2, characterized in that: In step 1, the concentration of the acidic sodium hypochlorite solution is 2.00 wt %, and the pH is adjusted to 4.6 with acetic acid.
4. The high-efficiency flame-retardant polyester material according to claim 2, characterized in that: In the step 1, during the soaking process, the acidic sodium hypochlorite solution is replaced every 2 hours.
5. The high-efficiency flame-retardant polyester material according to claim 2, characterized in that: In the step 3, the mass ratio of hexadecyltrimethylammonium bromide, urea, hydrated acetic acid, deionized water and methyltrimethoxysilane is 1:(2-5):(0.5-2):100:(0.5-2).
6. The high-efficiency flame-retardant polyester material according to claim 2, characterized in that: The methyltrimethoxysilane solution in step 5 is a mixture of methyltrimethoxysilane and ethanol in a mass ratio of 1:
2.
7. A method for preparing a high-efficiency flame-retardant polyester material according to any one of claims 1 to 6, characterized in that: The preparation steps are as follows: S1: Mix the polyester chips, flame retardant filler and tackifier in a blender to mix them evenly; S2: Place in an oven and dry at 150-170°C for 4-6 hours; S3: putting the dried material into an extruder for extrusion plasticization, and the heating temperature in the extruder is 260-265°C; S4: The plasticized material is molded and output to obtain a highly efficient flame-retardant polyester material.
8. The method for preparing a high-efficiency flame-retardant polyester material according to claim 7, characterized in that: In step S4, the molding temperature is 255-265° C., the molding pressure is 20-30 MPa, and the molding time is 45 seconds.