A steel fireproof and heat-insulating partition wall and a preparation method thereof

Abstract

The application relates to the technical field of foamed materials, and discloses a steel fireproof heat-insulating partition wall and a preparation method thereof. The preparation steps are as follows: step 1: methyl vinyl silicone rubber, hydrogen-containing silicone oil, composite filler, foaming agent, sodium bicarbonate, vulcanizing agent and kast catalyst are uniformly mixed to obtain a filling material; step 2: a steel keel frame is placed in a mold, the filling material is added, and foaming vulcanization is carried out to obtain a wallboard; step 3: the wallboard is assembled with fireproof glass on both sides to obtain a steel fireproof heat-insulating partition wall; the filling material comprises the following components in parts by weight: 100 parts of methyl vinyl silicone rubber, 10-15 parts of hydrogen-containing silicone oil, 55-76 parts of composite filler, 3-4 parts of foaming agent, 5-6 parts of sodium bicarbonate, 1-2 parts of vulcanizing agent and 0.1-0.2 parts of kast catalyst.

Description

Technical Field

[0001] This invention relates to the field of foamed materials technology, and discloses a steel-reinforced fireproof and heat-insulating partition wall and its preparation method. Background Technology

[0002] Partition walls are easy to install and reusable, and are commonly used for interior partitioning and decoration in buildings, providing fire protection and heat insulation in the event of a fire. However, the fire resistance of existing glass walls used for fireproofing and heat insulation needs improvement, and their impact resistance is insufficient. Therefore, it is necessary to further introduce wall panels with steel frame structures.

[0003] To further optimize thermal insulation and impact resistance, foamed silicone rubber is used as a filler between wall panels with a steel frame. Foamed silicone rubber has advantages such as relatively low density and good thermal stability; its internal pore structure significantly affects both thermal insulation and impact resistance, requiring strict control. In conclusion, researching a steel-framed fireproof and thermally insulated partition wall with excellent fire resistance and impact resistance, and its preparation method, is of great significance. Summary of the Invention

[0004] The purpose of this invention is to provide a steel fireproof and heat-insulating partition wall and its preparation method, so as to solve the problems mentioned in the background art.

[0005] To solve the above-mentioned technical problems, the present invention provides the following technical solution: a method for preparing a steel-reinforced fireproof and heat-insulating partition wall, comprising the following steps:

[0006] Step 1: Mix methyl vinyl silicone rubber, hydrogen-containing silicone oil, composite filler, foaming agent, sodium bicarbonate, vulcanizing agent, and cassiterite catalyst evenly to obtain the filler;

[0007] Step 2: Place the steel keel frame in the mold, add filler, foam and vulcanize to obtain the wall panel;

[0008] Step 3: Assemble fireproof glass by overlapping the wall panels on both sides to obtain a tempered fireproof and heat-insulating partition wall.

[0009] In a more optimized manner, the steel keel frame is composed of intersecting steel keels in an "I" shape.

[0010] More preferably, the filler comprises the following components, by weight: 100 parts methyl vinyl silicone rubber, 10-15 parts hydrogen-containing silicone oil, 55-76 parts composite filler, 3-4 parts foaming agent, 5-6 parts sodium bicarbonate, 1-2 parts vulcanizing agent, and 0.1-0.2 parts cassette catalyst.

[0011] In a more optimized manner, the composite filler comprises the following components, by weight: 30-40 parts modified hydrotalcite, 20-30 parts modified glass beads, and 5-6 parts modified zinc oxide.

[0012] In a more optimized manner, the preparation of the modified hydrotalcite includes the following steps:

[0013] S1.1: Add polyvinyl alcohol to water, add urea, heat to 95~100℃ and stir until homogeneous; add phosphoric acid dropwise, keep warm and react for 3~4 hours; cool to room temperature, add ethanol to precipitate the product, dry, and obtain phosphate-modified polyvinyl alcohol.

[0014] S1.2: Take anhydrous magnesium sulfate and aluminum sulfate octadecahydrate, add them to water and stir evenly to obtain a mixed salt solution; take sodium hydroxide and anhydrous sodium carbonate, add them to water and stir evenly to obtain a mixed alkali solution; take phosphate-modified polyvinyl alcohol, add it to water and heat and stir to dissolve, maintain 70~75℃, stir and add the mixed salt solution and mixed alkali solution dropwise at the same time, stir for 2~3 hours, keep warm and let stand for 30~60 minutes, then filter, wash and dry to obtain intercalated hydrotalcite;

[0015] S1.3: Take intercalated hydrotalcite, add an aqueous ethanol solution, add vinyltrimethoxysilane, heat to 60~70℃ and stir for 4~6 hours, filter to obtain solid, dry to obtain modified hydrotalcite.

[0016] In a more optimized manner, the phosphate-modified polyvinyl alcohol comprises the following raw materials, by mass parts: 10-15 parts polyvinyl alcohol, 100-150 parts water, 20-30 parts urea, and 15-20 parts 85% phosphoric acid;

[0017] The intercalated hydrotalcite comprises the following raw materials, by mass: 5-10 parts anhydrous magnesium sulfate, 8-15 parts aluminum sulfate octadecylhydrate, 1-3 parts sodium hydroxide, 6-10 parts anhydrous sodium carbonate, and 10-15 parts phosphate-modified polyvinyl alcohol.

[0018] The modified hydrotalcite comprises the following raw materials, by mass: 10-15 parts intercalated hydrotalcite, 50-60 parts of 60wt% aqueous ethanol solution, and 1-2 parts of vinylsilane coupling agent.

[0019] In a more optimized manner, the preparation of the modified glass beads includes the following steps: adding hollow glass microspheres into hydrofluoric acid solution, stirring at 20~30℃ for 2~3h, filtering to obtain solid, washing, and drying to obtain hydroxylated glass beads;

[0020] Hydroxylated glass beads and hydroxyl-terminated methyl vinyl silicone oil were added to benzene and stirred until homogeneous. Glutaraldehyde was added, and the mixture was stirred at 60-70°C for 2-3 hours. The solid was filtered, washed, and dried to obtain modified glass beads.

[0021] More preferably, the hydroxylated glass beads comprise the following raw materials, by mass parts: 10-15 parts hollow glass microspheres and 50-60 parts 0.5 wt% hydrofluoric acid solution (aqueous solution).

[0022] The modified glass beads comprise the following raw materials, by mass: 10-15 parts hydroxylated glass beads, 5-8 parts hydroxyl-terminated methyl vinyl silicone oil, and 10-20 parts glutaraldehyde.

[0023] In a more optimized manner, the preparation of the modified zinc oxide includes the following steps: taking zinc oxide, 3-(2,3-epoxypropoxy)propyltrimethoxysilane, methylphenyldimethoxysilane, dimethylvinylethoxysilane, and a mixed solvent of toluene and acetone (volume ratio 1:1), stirring evenly, adding dilute KOH aqueous solution dropwise, reacting at 50~55℃ for 8~12h, gradually increasing the temperature to remove the liquid generated in the reaction system, filtering, washing, and drying to obtain modified zinc oxide.

[0024] In a more optimized manner, the modified zinc oxide comprises the following raw materials, by mass parts: 40-50 parts zinc oxide, 15-25 parts 3-(2,3-epoxypropoxy)propyltrimethoxysilane, 5-15 parts methylphenyldimethoxysilane, 5-15 parts dimethylvinylethoxysilane, and 8-12 parts dilute KOH aqueous solution.

[0025] A more optimized foaming vulcanization process is to foam and vulcanize at 240~250℃ for 15~20 minutes.

[0026] Compared with the prior art, the beneficial effects achieved by the present invention are: adding filler to the wall panel improves the thermal insulation performance and impact resistance; the filler matrix is ​​methyl vinyl silicone rubber, which has good thermal stability; and the present solution introduces composite fillers, including modified hydrotalcite, modified glass beads and modified zinc oxide. Since the fillers have different morphologies, the complexity of the heat conduction path is increased, thereby improving the thermal insulation performance.

[0027] The modified hydrotalcite is intercalated with phosphate-modified polyvinyl alcohol. Hydrotalcite itself has good fire resistance. The phosphate ester can enhance the fire resistance and heat resistance, while the polyvinyl alcohol can act as a dispersant and foaming agent to enhance the uniformity and density of the cells, thereby improving the overall mechanical properties. At the same time, the modified hydrotalcite contains double bonds, which can participate in the pre-crosslinking of subsequent steps, improve its own dispersibility and increase the degree of crosslinking of the rubber matrix.

[0028] The modified glass beads have a hollow structure, which improves thermal insulation performance and promotes uniform nucleation of bubbles during foaming, thereby reducing the pore size. The modified glass beads are grafted with hydroxyl-terminated methyl vinyl silicone oil, which improves compatibility with the rubber matrix and introduces a long-chain double-bond structure to improve the cross-linking network formed during subsequent pre-cross-linking, improves toughness and extends the heat conduction path, which helps to improve the overall impact resistance and thermal insulation performance.

[0029] Modified zinc oxide itself is a vulcanization accelerator. Modification with 3-(2,3-epoxypropoxy)propyltrimethoxysilane, methylphenyldimethoxysilane, and dimethylvinylethoxysilane improves its dispersibility in the rubber matrix, promotes vulcanization, and introduces a multi-active organosilicon tackifying system to increase the viscosity of the rubber matrix and enhance the strength of the cell walls, so that it will not break or merge during the foaming process, thus obtaining a more uniform foam structure.

[0030] All three fillers contain double bond structures and can participate in the pre-crosslinking process in subsequent steps. The amount of fillers added needs to be controlled. Excessive addition can lead to problems such as excessive crosslinking, decreased thermal insulation performance, and excessive viscosity, which in turn leads to a decrease in performance.

[0031] This solution also introduces hydrogen-containing silicone oil, which can pre-crosslink with the double bonds of various raw materials in the rubber matrix under the action of a catalyst. Since this reaction can be carried out at a lower temperature, it improves the problem of uneven bubble pore size caused by direct high-temperature foaming.

[0032] In summary, this solution optimizes the pore structure and improves the thermal insulation performance and impact resistance of the filler by introducing three types of fillers and hydrogen-containing silicone oil. Detailed Implementation

[0033] The technical solutions in the embodiments of the present invention will be clearly and completely described below. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of the present invention.

[0034] It should be noted that there are no special restrictions on the suppliers of any of the raw materials involved in this invention. Exemplary examples include: ethanol (CAS: 64-17-5); methyl vinyl silicone rubber (110-0, Hesheng Silicon Industry Co., Ltd.); hydrogen-containing silicone oil (GHQGY01, Shanhai Chemical); zinc oxide (4203, Jiyesheng); foaming agent (OBSH foaming agent, Jiaxing Jinhe Chemical Co., Ltd.); caster catalyst (KS301000, Shenzhen Xinyongsheng New Materials Co., Ltd.); vinyltrimethoxysilane. (CAS: 2768-02-7); Hollow glass microspheres (Zhongke Yali H40HS, true density 0.4g / cc); Hydroxyl-terminated methyl vinyl silicone oil (Anhui Aiyota Silicone Oil Co., Ltd. IOTA1203V); Vulcanizing agent (CAS: 133-14-2); Polyvinyl alcohol (S30196, Shanghai Yuanye Biotechnology Co., Ltd.); Urea (S30375, Shanghai Yuanye Biotechnology Co., Ltd.); 85% phosphoric acid (Shandong Yukang Chemical Co., Ltd.); Dilute KOH aqueous solution (0.5M);

[0035] Unless otherwise specified, all figures below are parts by weight or mass ratios.

[0036] Example 1: S1: Take 10 parts of polyvinyl alcohol, add 100 parts of water, heat and stir to dissolve, add 25 parts of urea, heat to 95°C, add 16 parts of 85% phosphoric acid dropwise over 30 min, keep the reaction at the temperature for 4 h, cool to room temperature, add anhydrous ethanol until the product precipitates, dry, and obtain phosphate ester modified polyvinyl alcohol.

[0037] S2: Take 6 parts of anhydrous magnesium sulfate and 12 parts of aluminum sulfate octadecahydrate, add 50 parts of water and stir evenly to obtain a mixed salt solution; take 2 parts of sodium hydroxide and 8 parts of anhydrous sodium carbonate, add 50 parts of water and stir evenly to obtain a mixed alkali solution; weigh 12 parts of phosphate-modified polyvinyl alcohol, add 100 parts of water, heat and stir to dissolve, maintain 70℃, stir and simultaneously add the mixed salt solution and mixed alkali solution, stir for 3 hours, place at 75℃ for 30 minutes, filter, wash and dry to obtain intercalated hydrotalcite;

[0038] S3: Take 10 parts of intercalated hydrotalcite, add 60 parts of 60wt% ethanol aqueous solution, add 1 part of vinyltrimethoxysilane, heat to 70℃ and stir for 4 hours, filter to obtain solid, dry to obtain modified hydrotalcite.

[0039] S4: Add 10 parts of hollow glass microspheres to 50 parts of 0.5wt% hydrofluoric acid solution, stir at 25℃ for 3h, filter to collect solid, wash and dry to obtain hydroxylated glass beads;

[0040] S5: Take 12 parts of hydroxylated glass beads and 6 parts of hydroxyl-terminated methyl vinyl silicone oil and add them to 100 parts of benzene and stir evenly. Add 15 parts of glutaraldehyde and stir at 70°C for 2 hours. Filter to obtain the solid, wash and dry to obtain modified glass beads.

[0041] S6: Take 50 parts of zinc oxide, 15 parts of 3-(2,3-epoxypropoxy)propyltrimethoxysilane, 10 parts of methylphenyldimethoxysilane, 10 parts of dimethylvinylethoxysilane, and 100 parts of a mixed solvent of toluene and acetone (volume ratio 1:1). Stir well, add 12 parts of dilute KOH aqueous solution dropwise, react at 50℃ for 10h, gradually increase the temperature to remove the liquid generated in the reaction system, filter, wash, and dry to obtain modified zinc oxide;

[0042] S7: Add 35 parts modified hydrotalcite, 12 parts hydrogen-containing silicone oil, 25 parts modified glass beads, and 5 parts modified zinc oxide to 100 parts methyl vinyl silicone rubber, mix at 130℃ for 10 min, add 3 parts foaming agent, 5 parts sodium bicarbonate, 1 part vulcanizing agent, and 0.1 parts caster catalyst, open mill at 60℃ for 10 min, and foam vulcanize at 250℃ for 15 min to obtain the filler.

[0043] Example 2: S1: Take 15 parts of polyvinyl alcohol, add 100 parts of water, heat and stir to dissolve, add 30 parts of urea, heat to 95°C, add 20 parts of 85% phosphoric acid dropwise for 30 min, keep the reaction at the temperature for 4 h, cool to room temperature, add anhydrous ethanol to precipitate the product, dry, and obtain phosphate ester modified polyvinyl alcohol.

[0044] S2: Take 10 parts of anhydrous magnesium sulfate and 15 parts of aluminum sulfate octadecahydrate, add 80 parts of water and stir evenly to obtain a mixed salt solution; take 3 parts of sodium hydroxide and 10 parts of anhydrous sodium carbonate, add 80 parts of water and stir evenly to obtain a mixed alkali solution; weigh 15 parts of phosphate-modified polyvinyl alcohol, add 100 parts of water, heat and stir to dissolve, maintain 70℃, stir and simultaneously add the mixed salt solution and mixed alkali solution, stir for 3 hours, place at 75℃ for 30 minutes, filter, wash and dry to obtain intercalated hydrotalcite;

[0045] S3: Take 15 parts of intercalated hydrotalcite, add 60 parts of 60wt% ethanol aqueous solution, add 2 parts of vinyltrimethoxysilane, heat to 70℃ and stir for 4 hours, filter to obtain solid, dry to obtain modified hydrotalcite.

[0046] S4: Add 15 parts of hollow glass microspheres to 60 parts of 0.5wt% hydrofluoric acid solution, stir at 25℃ for 3h, filter to collect solid, wash and dry to obtain hydroxylated glass beads;

[0047] S5: Take 15 parts of hydroxylated glass beads and 8 parts of hydroxyl-terminated methyl vinyl silicone oil and add them to 100 parts of benzene and stir evenly. Add 20 parts of glutaraldehyde and stir at 70°C for 2 hours. Filter to obtain the solid, wash and dry to obtain modified glass beads.

[0048] S6: Take 50 parts of zinc oxide, 25 parts of 3-(2,3-epoxypropoxy)propyltrimethoxysilane, 5 parts of methylphenyldimethoxysilane, 5 parts of dimethylvinylethoxysilane, and 100 parts of a mixed solvent of toluene and acetone (volume ratio 1:1). Stir well, add 12 parts of dilute KOH aqueous solution dropwise, react at 50℃ for 10 h, gradually increase the temperature to remove the liquid generated in the reaction system, filter, wash, and dry to obtain modified zinc oxide;

[0049] S7: Add 40 parts modified hydrotalcite, 15 parts hydrogen-containing silicone oil, 20 parts modified glass beads, and 5 parts modified zinc oxide to 100 parts methyl vinyl silicone rubber, mix at 130℃ for 10 min, add 3 parts foaming agent, 5 parts sodium bicarbonate, 1 part vulcanizing agent, and 0.1 parts caster catalyst, start mill at 60℃ for 10 min, and foam vulcanize at 250℃ for 15 min to obtain the filler.

[0050] Comparative Example 1 (without adding hydrogen-containing silicone oil, the rest of the methods and steps are the same as in Example 1): S1: Take 10 parts of polyvinyl alcohol, add 100 parts of water, heat and stir to dissolve, add 25 parts of urea, heat to 95°C, add 16 parts of 85% phosphoric acid dropwise after 30 min, keep the reaction at the temperature for 4 h, cool to room temperature, add anhydrous ethanol until the product precipitates, dry, and obtain phosphate ester modified polyvinyl alcohol;

[0051] S2: Take 6 parts of anhydrous magnesium sulfate and 12 parts of aluminum sulfate octadecahydrate, add 50 parts of water and stir evenly to obtain a mixed salt solution; take 2 parts of sodium hydroxide and 8 parts of anhydrous sodium carbonate, add 50 parts of water and stir evenly to obtain a mixed alkali solution; weigh 12 parts of phosphate-modified polyvinyl alcohol, add 100 parts of water, heat and stir to dissolve, maintain 70℃, stir and simultaneously add the mixed salt solution and mixed alkali solution, stir for 3 hours, place at 75℃ for 30 minutes, filter, wash and dry to obtain intercalated hydrotalcite;

[0052] S3: Take 10 parts of intercalated hydrotalcite, add 60 parts of 60wt% ethanol aqueous solution, add 1 part of vinyltrimethoxysilane, heat to 70℃ and stir for 4 hours, filter to obtain solid, dry to obtain modified hydrotalcite.

[0053] S4: Add 10 parts of hollow glass microspheres to 50 parts of 0.5wt% hydrofluoric acid solution, stir at 25℃ for 3h, filter to collect solid, wash and dry to obtain hydroxylated glass beads;

[0054] S5: Take 12 parts of hydroxylated glass beads and 6 parts of hydroxyl-terminated methyl vinyl silicone oil and add them to 100 parts of benzene and stir evenly. Add 15 parts of glutaraldehyde and stir at 70°C for 2 hours. Filter to obtain the solid, wash and dry to obtain modified glass beads.

[0055] S6: Take 50 parts of zinc oxide, 15 parts of 3-(2,3-epoxypropoxy)propyltrimethoxysilane, 10 parts of methylphenyldimethoxysilane, 10 parts of dimethylvinylethoxysilane, and 100 parts of a mixed solvent of toluene and acetone (volume ratio 1:1). Stir well, add 12 parts of dilute KOH aqueous solution dropwise, react at 50℃ for 10h, gradually increase the temperature to remove the liquid generated in the reaction system, filter, wash, and dry to obtain modified zinc oxide;

[0056] S7: Add 35 parts modified hydrotalcite, 25 parts modified glass beads, and 5 parts modified zinc oxide to 100 parts methyl vinyl silicone rubber, mix at 130℃ for 10 min, add 3 parts foaming agent, 5 parts sodium bicarbonate, 1 part vulcanizing agent, and 0.1 parts caster catalyst, start milling at 60℃ for 10 min, and foam vulcanize at 250℃ for 15 min to obtain the filler.

[0057] Comparative Example 2 (no zinc oxide modification, the rest of the methods and steps are the same as in Example 1): S1: Take 10 parts of polyvinyl alcohol, add 100 parts of water, heat and stir to dissolve, add 25 parts of urea, heat to 95°C, add 16 parts of 85% phosphoric acid dropwise after 30 min, keep the reaction at the temperature for 4 h, cool to room temperature, add anhydrous ethanol until the product precipitates, dry, and obtain phosphate ester modified polyvinyl alcohol.

[0058] S2: Take 6 parts of anhydrous magnesium sulfate and 12 parts of aluminum sulfate octadecahydrate, add 50 parts of water and stir evenly to obtain a mixed salt solution; take 2 parts of sodium hydroxide and 8 parts of anhydrous sodium carbonate, add 50 parts of water and stir evenly to obtain a mixed alkali solution; weigh 12 parts of phosphate-modified polyvinyl alcohol, add 100 parts of water, heat and stir to dissolve, maintain 70℃, stir and simultaneously add the mixed salt solution and mixed alkali solution, stir for 3 hours, place at 75℃ for 30 minutes, filter, wash and dry to obtain intercalated hydrotalcite;

[0059] S3: Take 10 parts of intercalated hydrotalcite, add 60 parts of 60wt% ethanol aqueous solution, add 1 part of vinyltrimethoxysilane, heat to 70℃ and stir for 4 hours, filter to obtain solid, dry to obtain modified hydrotalcite.

[0060] S4: Add 10 parts of hollow glass microspheres to 50 parts of 0.5wt% hydrofluoric acid solution, stir at 25℃ for 3h, filter to collect solid, wash and dry to obtain hydroxylated glass beads;

[0061] S5: Take 12 parts of hydroxylated glass beads and 6 parts of hydroxyl-terminated methyl vinyl silicone oil and add them to 100 parts of benzene and stir evenly. Add 15 parts of glutaraldehyde and stir at 70°C for 2 hours. Filter to obtain the solid, wash and dry to obtain modified glass beads.

[0062] S6: Add 35 parts modified hydrotalcite, 12 parts hydrogen-containing silicone oil, 25 parts modified glass beads, 5 parts zinc oxide, and 15 parts modified hollow glass microspheres to 100 parts methyl vinyl silicone rubber. Mix at 130℃ for 10 min. Add 3 parts foaming agent, 5 parts sodium bicarbonate, 1 part vulcanizing agent, and 0.1 parts caster catalyst. Open mill at 60℃ for 10 min. High temperature foaming and vulcanization at 250℃ for 15 min to obtain the filler.

[0063] Comparative Example 3 (the amount of modified zinc oxide added is increased, and the rest of the methods and steps are the same as in Example 1): S1: Take 10 parts of polyvinyl alcohol, add 100 parts of water, heat and stir to dissolve, add 25 parts of urea, heat to 95°C, add 16 parts of 85% phosphoric acid dropwise for 30 min, keep the reaction at the temperature for 4 h, cool to room temperature, add anhydrous ethanol until the product precipitates, dry, and obtain phosphate ester modified polyvinyl alcohol;

[0064] S2: Take 6 parts of anhydrous magnesium sulfate and 12 parts of aluminum sulfate octadecahydrate, add 50 parts of water and stir evenly to obtain a mixed salt solution; take 2 parts of sodium hydroxide and 8 parts of anhydrous sodium carbonate, add 50 parts of water and stir evenly to obtain a mixed alkali solution; weigh 12 parts of phosphate-modified polyvinyl alcohol, add 100 parts of water, heat and stir to dissolve, maintain 70℃, stir and simultaneously add the mixed salt solution and mixed alkali solution, stir for 3 hours, place at 75℃ for 30 minutes, filter, wash and dry to obtain intercalated hydrotalcite;

[0065] S3: Take 10 parts of intercalated hydrotalcite, add 60 parts of 60wt% ethanol aqueous solution, add 1 part of vinyltrimethoxysilane, heat to 70℃ and stir for 4 hours, filter to obtain solid, dry to obtain modified hydrotalcite.

[0066] S4: Add 10 parts of hollow glass microspheres to 50 parts of 0.5wt% hydrofluoric acid solution, stir at 25℃ for 3h, filter to collect solid, wash and dry to obtain hydroxylated glass beads;

[0067] S5: Take 12 parts of hydroxylated glass beads and 6 parts of hydroxyl-terminated methyl vinyl silicone oil and add them to 100 parts of benzene and stir evenly. Add 15 parts of glutaraldehyde and stir at 70°C for 2 hours. Filter to obtain the solid, wash and dry to obtain modified glass beads.

[0068] S6: Take 50 parts of zinc oxide, 15 parts of 3-(2,3-epoxypropoxy)propyltrimethoxysilane, 10 parts of methylphenyldimethoxysilane, 10 parts of dimethylvinylethoxysilane, and 100 parts of a mixed solvent of toluene and acetone (volume ratio 1:1). Stir well, add 12 parts of dilute KOH aqueous solution dropwise, react at 50℃ for 10h, gradually increase the temperature to remove the liquid generated in the reaction system, filter, wash, and dry to obtain modified zinc oxide;

[0069] S7: Add 35 parts modified hydrotalcite, 12 parts hydrogen-containing silicone oil, 25 parts modified glass beads, and 10 parts modified zinc oxide to 100 parts methyl vinyl silicone rubber, mix at 130℃ for 10 min, add 3 parts foaming agent, 5 parts sodium bicarbonate, 1 part vulcanizing agent, and 0.1 parts caster catalyst, start mill at 60℃ for 10 min, and foam vulcanize at 250℃ for 15 min to obtain the filler.

[0070] Comparative Example 4 (the preparation method of the modified glass beads was changed, and the other steps were the same as in Example 1): S1: Take 10 parts of polyvinyl alcohol, add 100 parts of water, heat and stir to dissolve, add 25 parts of urea, heat to 95°C, add 16 parts of 85% phosphoric acid dropwise after 30 min, keep the reaction at the temperature for 4 h, cool to room temperature, add anhydrous ethanol until the product precipitates, dry, and obtain phosphate ester modified polyvinyl alcohol;

[0071] S2: Take 6 parts of anhydrous magnesium sulfate and 12 parts of aluminum sulfate octadecahydrate, add 50 parts of water and stir evenly to obtain a mixed salt solution; take 2 parts of sodium hydroxide and 8 parts of anhydrous sodium carbonate, add 50 parts of water and stir evenly to obtain a mixed alkali solution; weigh 12 parts of phosphate-modified polyvinyl alcohol, add 100 parts of water, heat and stir to dissolve, maintain 70℃, stir and simultaneously add the mixed salt solution and mixed alkali solution, stir for 3 hours, place at 75℃ for 30 minutes, filter, wash and dry to obtain intercalated hydrotalcite;

[0072] S3: Take 10 parts of intercalated hydrotalcite, add 60 parts of 60wt% ethanol aqueous solution, add 1 part of vinyltrimethoxysilane, heat to 70℃ and stir for 4 hours, filter to obtain solid, dry to obtain modified hydrotalcite.

[0073] S4: Take 10 parts of hollow glass microspheres, add 60 parts of 60wt% ethanol aqueous solution, add 1 part of vinyltrimethoxysilane, heat to 70℃ and stir for 4 hours, filter to obtain solid, dry to obtain modified glass beads.

[0074] S5: Take 50 parts of zinc oxide, 15 parts of 3-(2,3-epoxypropoxy)propyltrimethoxysilane, 10 parts of methylphenyldimethoxysilane, 10 parts of dimethylvinylethoxysilane, and 100 parts of a mixed solvent of toluene and acetone (volume ratio 1:1). Stir well, add 12 parts of dilute KOH aqueous solution dropwise, react at 50℃ for 10h, gradually increase the temperature to remove the liquid generated in the reaction system, filter, wash, and dry to obtain modified zinc oxide;

[0075] S6: Add 35 parts modified hydrotalcite, 12 parts hydrogen-containing silicone oil, 25 parts modified glass beads, and 5 parts modified zinc oxide to 100 parts methyl vinyl silicone rubber, mix at 130℃ for 10 min, add 3 parts foaming agent, 5 parts sodium bicarbonate, 1 part vulcanizing agent, and 0.1 parts caster catalyst, open mill at 60℃ for 10 min, and foam vulcanize at 250℃ for 15 min to obtain the filler.

[0076] Performance test: Take the filler prepared in Examples 1-2 and Comparative Examples 1-4; (1) Prepare a sample with a thickness of 2 mm and test its heat insulation: fix one side of the sample on a heat source of 500℃ for 5 min, measure the temperature of the other side, and calculate the temperature difference; (2) Apply a pressure of 1 MPa and measure the thickness change of the sample to evaluate the bubble density and mechanical properties; see Table 1 for details;

[0077] Table 1:

[0078] Temperature difference / °C Change / % Example 1 399 13.0 Example 2 398 13.2 Comparative Example 1 355 17.6 Comparative Example 2 360 15.5 Comparative Example 3 341 7.9 Comparative Example 4 367 15.9

[0079] Conclusions: Comparative Example 1, lacking the pre-crosslinking step due to the absence of hydrogen-containing silicone oil, resulted in inferior bubble uniformity and stability compared to the Examples, thus affecting its thermal insulation performance. Comparative Example 2, without zinc oxide modification, suffered from decreased performance due to changes in dispersibility and overall viscosity. Comparative Example 3, by increasing the amount of modified zinc oxide, resulted in increased viscosity, reduced bubble quantity, excessive density, and increased filler content, leading to decreased thermal insulation. Comparative Example 4, by altering the preparation method of modified glass beads and using vinyltrimethoxysilane modification, lacked long-chain silicone oil, resulting in changes in the crosslinking network and inferior performance compared to the Examples. In summary, the filler prepared by this scheme exhibits good fireproof and thermal insulation capabilities, uniform pores, and excellent mechanical properties and stability.

[0080] Finally, it should be noted that the above descriptions are merely preferred embodiments of the present invention and are not intended to limit the present invention. Although the present invention has been described in detail with reference to the foregoing embodiments, those skilled in the art can still modify the technical solutions described in the foregoing embodiments or make equivalent substitutions for some of the technical features. Any modifications, equivalent substitutions, improvements, etc., made within the spirit and principles of the present invention should be included within the protection scope of the present invention.

Claims

1. A method for preparing a steel-reinforced fireproof and heat-insulating partition wall, characterized in that: It comprises the following steps: Step 1: uniformly mix methyl vinyl silicone rubber, hydrogen-containing silicone oil, composite filler, foaming agent, sodium bicarbonate, vulcanizing agent and Kast catalyst to obtain a filling material; Step 2: place a steel keel frame in a mold, add the filling material, and foam and vulcanize to obtain a wallboard; Step 3: assemble fireproof glass on both sides of the wallboard to obtain a steel fireproof heat-insulating partition wall; The composite filler comprises the following components in parts by weight: 30-40 parts of modified hydrotalcite, 20-30 parts of modified glass beads and 5-6 parts of modified zinc oxide. The preparation of the modified hydrotalcite comprises the following steps: S1.1: add polyvinyl alcohol into water, add urea, heat to 95-100 DEG C and stir until uniform; drop phosphoric acid and keep reacting for 3-4 hours; cool to room temperature, add ethanol to precipitate the product, and dry to obtain phosphate-modified polyvinyl alcohol; S1.2: take anhydrous magnesium sulfate and aluminum sulfate octadecahydrate, add water and stir until uniform to obtain a mixed salt solution; take sodium hydroxide and anhydrous sodium carbonate, add water and stir until uniform to obtain a mixed alkali solution; take phosphate-modified polyvinyl alcohol, add water, heat and stir until dissolved, keep the temperature at 70-75 DEG C, drop the mixed salt solution and the mixed alkali solution while stirring for 2-3 hours, keep for 30-60 minutes, then filter, wash and dry to obtain intercalated hydrotalcite; S1.3: take the intercalated hydrotalcite, add an ethanol aqueous solution and vinyltrimethoxysilane, heat to 60-70 DEG C and stir for 4-6 hours, then filter, dry and obtain modified hydrotalcite; The preparation of the modified glass beads comprises the following steps: S2.1: add hollow glass microbeads into a hydrofluoric acid solution, stir at 20-30 DEG C for 2-3 hours, filter, wash and dry to obtain hydroxylated glass beads; S2.2: take the hydroxylated glass beads and hydroxyl-terminated methyl vinyl silicone oil, add benzene and stir until uniform, add glutaraldehyde, stir at 60-70 DEG C for 2-3 hours, filter, wash and dry to obtain modified glass beads; The preparation of the modified zinc oxide comprises the following steps: take zinc oxide, 3-(2,3-epoxypropoxy) propyl trimethoxysilane, methyl phenyl dimethoxysilane, dimethyl vinyl ethoxy silane, a mixed solvent of toluene and acetone, stir until uniform, drop dilute KOH aqueous solution, react at 50-55 DEG C for 8-12 hours, gradually increase the temperature to remove the liquid generated in the reaction system, filter, wash and dry to obtain modified zinc oxide; The filling material comprises the following components in parts by weight: 100 parts of methyl vinyl silicone rubber, 10-15 parts of hydrogen-containing silicone oil, 55-76 parts of composite filler, 3-4 parts of foaming agent, 5-6 parts of sodium bicarbonate, 1-2 parts of vulcanizing agent and 0.1-0.2 parts of Kast catalyst. The phosphate-modified polyvinyl alcohol comprises the following raw materials in parts by mass: 10-15 parts of polyvinyl alcohol, 100-150 parts of water, 20-30 parts of urea and 15-20 parts of 85% phosphoric acid. ​ ​ 2. The method for preparing a steel fireproof and heat insulation partition wall according to claim 1, characterized in that: ​ The intercalated hydrotalcite comprises the following raw materials in parts by mass: 5-10 parts of anhydrous magnesium sulfate, 8-15 parts of aluminum sulfate octadecahydrate, 1-3 parts of sodium hydroxide, 6-10 parts of anhydrous sodium carbonate, and 10-15 parts of phosphate ester modified polyvinyl alcohol; The modified hydrotalcite comprises the following raw materials in parts by mass: 10-15 parts of the intercalated hydrotalcite, 50-60 parts of 60wt% ethanol aqueous solution, and 1-2 parts of vinyl silane coupling agent.

3. The method for preparing a steel fireproof and heat insulation partition wall according to claim 1, characterized in that: The hydroxylated glass beads comprise the following raw materials in parts by mass: 10-15 parts of hollow glass microbeads and 50-60 parts of 0.5wt% hydrofluoric acid solution; The modified glass beads comprise the following raw materials in parts by mass: 10-15 parts of the hydroxylated glass beads, 5-8 parts of hydroxyl-terminated methyl vinyl silicone oil, and 10-20 parts of glutaraldehyde.

4. The method for preparing a steel-reinforced fireproof and heat-insulating partition wall according to claim 1, characterized in that: The modified zinc oxide comprises the following raw materials in parts by mass: 40-50 parts of zinc oxide, 15-25 parts of 3-(2,3-epoxypropoxy)propyl trimethoxysilane, 5-15 parts of methyl phenyl dimethoxysilane, 5-15 parts of dimethyl vinyl ethoxysilane, and 8-12 parts of dilute KOH aqueous solution.

5. The partition wall prepared by the preparation method of the steel fireproof and heat-insulating partition wall according to any one of claims 1-4.