Silicon-containing flame-retardant foot pad for automobile and preparation method of silicon-containing flame-retardant foot pad
By combining iron oxide with silica to prepare microcapsules and applying specific flame retardant coatings to the surface of the car foot pads, the problem of flammability of existing car foot pad materials is solved, and the flame retardant performance and stain resistance are significantly improved, and the flame retardant performance and anti-fouling properties are enhanced. Security and performance.
Patent Information
- Application Number
- CN202411499181.7
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2024-10-25
- Publication Date
- 2025-01-14
- Estimated Expiration
- 2044-10-25
AI Technical Summary
Existing automotive foot pad materials are flammable under high temperature or fire source, have insufficient flame retardant performance, pose safety hazards and may release harmful gases, affecting the air quality in the car.
Using the preparation method of silicon-containing flame retardant foot pads, microcapsules are prepared by compounding iron oxide with silica, and polypyrrole is wrapped on its surface to enhance thermal stability and residual carbon barrier performance; at the same time, coat the foot pads on the surface Flame retardant coatings, containing 9,10-dihydro-9-oxa-10-phosphophenophen-10-oxide and dodecanoheptyl methacrylate, improve hydrophobic properties and adhesion.
It significantly improves the flame retardant and stain-proof properties of the foot pads, enhances thermal stability and residual carbon barrier properties, inhibits the escape of harmful gases, and improves safety and use performance.
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Abstract
Description
Technical Field
[0001] The invention relates to the technical field of foot pads, in particular to a silicon-containing flame-retardant foot pad for automobiles and a preparation method thereof. Background Art
[0002] With the rapid development of the automobile industry, floor mats, as an important component in the car, not only need to have good wear resistance, anti-fouling and comfort, but also need to meet flame retardant properties to ensure the safety of the vehicle in the event of a fire. Currently, most of the car floor mats on the market are made of PVC, rubber and other materials. Although they have certain wear resistance and anti-slip properties, their flame retardant properties are generally poor. These materials are prone to melting, burning and other phenomena under the influence of high temperature or fire source, which may cause the spread of flames and bring great safety hazards to passengers and vehicles. In addition, traditional materials may release harmful gases during use, affecting the air quality in the car. Therefore, the development of a silicon-containing flame-retardant floor mat for automobiles with excellent performance has become an urgent need in the industry.
[0003] In order to solve the above problems and improve the flame retardancy of the foot pad, the present invention provides a silicon-containing flame retardant foot pad for automobiles and a preparation method thereof. Summary of the invention
[0004] The object of the present invention is to provide a silicon-containing flame-retardant foot pad for automobiles and a preparation method thereof, so as to solve the problems raised in the prior art.
[0005] To achieve the above object, the present invention provides the following technical solutions: A method for preparing a silicon-containing flame-retardant foot pad for an automobile comprises the following steps: Step 1: Take ferric chloride hexahydrate and deionized water, stir evenly to obtain ferric chloride hexahydrate solution; take anhydrous ethanol and deionized water, stir evenly, add silicon dioxide-iron oxide complex, ultrasonically disperse for 30-40 minutes, add pyrrole, ultrasonically disperse for 30-40 minutes, dropwise add ferric chloride hexahydrate solution, stir for 18-20 hours, add 3-mercaptopropionic acid and benzoin dimethyl ether, stir for 4-6 hours, filter, dry and grind to obtain flame retardant microcapsules; Step 2: taking polyester chips, ammonium polyphosphate, flame retardant microcapsules, and dispersants, blending, extruding, spinning, drawing, opening, combing, needling, and heat setting to obtain flame retardant needle-punched cloth; Step 3: Take the flame-retardant needle-punched cloth, and stack the buffer layer and leather on its upper surface in sequence, and glue them together to obtain a foot pad; Step 4: Apply the flame retardant coating to the surface of the foot pad, and then 2 Expose to ultraviolet light for 8-10 minutes to obtain a flame retardant foot pad.
[0006] More optimally, the preparation method of the flame retardant coating is: take flame retardant modified waterborne polyurethane, styrene acrylic emulsion, and emulsifier, stir for 60-70 minutes at 50-55°C to obtain a blended emulsion, add a crosslinking agent and a leveling agent, stir evenly, and obtain a flame retardant coating.
[0007] More optimally, the preparation method of the silica-iron oxide complex is: take silica and Tris-HCl buffer, ultrasonically disperse for 30-40 minutes to obtain a silica dispersion; take dopamine hydrochloride and Tris-HCl buffer, stir evenly, add the silica dispersion, ultrasonicate for 15-20 minutes, stir for 6-7 hours, add nano-ferric oxide, stir for 3-4 hours, wash, dry and grind to obtain a silica-iron oxide complex.
[0008] More optimally, the preparation method of the flame retardant modified waterborne polyurethane is: take 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide, trimethylolpropane, and acetone, stir evenly to obtain a mixed solution; take polyether diol, dihydroxy silicone oil, and toluene diisocyanate, pass nitrogen, stir for 30-40 minutes, heat to 75-80°C, react for 3.5-4 hours, cool to 70-75°C, add the mixed solution, stir evenly, react for 1-2 hours, cool to 60-63°C, add polyethylene glycol, react for 3-4 hours, cool to 20-25°C, drop a mixed solution of ethylenediamine, dodecafluoroheptyl methacrylate, and acetone, react for 50-70 minutes, and distill to obtain a flame retardant modified waterborne polyurethane.
[0009] More optimally, the flame retardant needle-punched cloth comprises the following components, by weight: 90-95 parts of polyester chips, 2-2.5 parts of ammonium polyphosphate, 2-3 parts of flame retardant microcapsules, and 2.5-3 parts of dispersant.
[0010] More optimally, the flame retardant coating comprises the following ingredients, by weight: 95-100 parts of flame retardant modified waterborne polyurethane, 20-25 parts of styrene acrylic emulsion, 2-3 parts of crosslinking agent, 3-4 parts of emulsifier, and 0.01-0.02 parts of leveling agent.
[0011] More optimally, the dispersant is ethylene bis stearic acid amide.
[0012] Compared with the prior art, the present invention has the following beneficial effects: (1) The present invention modifies the needle-punched cloth and uses flame-retardant microcapsules to enhance the flame retardant properties of the foot pad. The present invention composites iron oxide with silicon dioxide to enhance the dispersibility of silicon dioxide, and then wraps polypyrrole on its surface to further prepare it into microcapsules. The microcapsules will produce phosphorus-containing and nitrogen-containing groups when burned, improve the carbonization ability, thereby enhancing the thermal stability and barrier properties of the residual carbon, thereby further inhibiting the escape of harmful gases and enhancing the flame retardant properties of the silicon-containing flame-retardant foot pad.
[0013] (2) The present invention applies a flame retardant coating on the surface of the foot pad to enhance the flame retardancy of the foot pad. 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide is added to the flame retardant coating to improve the flame retardancy of the waterborne polyurethane, and dodecafluoroheptyl methacrylate is added to improve the hydrophobicity of the waterborne polyurethane and enhance the antifouling property of the foot pad. The present invention also adds 3-mercaptopropionic acid to the flame retardant microcapsule. 3-mercaptopropionic acid can react with dodecafluoroheptyl methacrylate in the flame retardant coating under ultraviolet light, thereby enhancing the adhesion of the coating and thus enhancing the performance of the foot pad. DETAILED DESCRIPTION
[0014] The technical solutions in the embodiments of the present invention are described clearly and completely below. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of them. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.
[0015] The sources of the substances involved in the present invention are not particularly limited, and exemplarily include: nano ferric oxide: average particle size: 50 nm, which can be purchased from Qinghe Chaotai Metal Materials Co., Ltd.; polyethylene glycol: model: PEG6397, which can be purchased from Changzhou Junxin Plastic Co., Ltd.; polyether diol: model: N210, number average molecular weight (Mn) = 1000, which can be purchased from Jining Baichuan Chemical Co., Ltd.; polyester chips: model: WK-801, which can be purchased from Kunshan Jinkaiwo Plastic Co., Ltd.; emulsifier: model: OP-10, which can be purchased from Shenzhen Boshun Chemical Co., Ltd.; crosslinking agent : Model: Epoxy curing agent R-2257, which can be purchased from Shandong Pinshang New Materials Co., Ltd.; Leveling agent: Model: G450, which can be purchased from Germany Digo; Dispersant: Ethylene bis stearic acid amide, Model: B-50, which can be purchased from Indonesia EBS; Styrene acrylic emulsion: Model: Y17677, which can be purchased from Shanghai Yuanye; Leather: PVC artificial leather, Model: YX-10, with a thickness of 0.5 mm, which can be purchased from Xiamen Yongdeyu Leather Co., Ltd.; Buffer layer: Soft polyurethane foam plastic, Model: mz1208, with a thickness of 10 mm, which can be purchased from Suzhou Maozhen New Materials Technology Co., Ltd.
[0016] Embodiment 1: A method for preparing a silicon-containing flame-retardant foot pad for an automobile, comprising the following steps: Step 1: Preparation of silica-iron oxide composite: Take 1g of silica and 100mL of Tris-HCl buffer, and ultrasonically disperse for 35min to obtain a silica dispersion; take 1.4g of dopamine hydrochloride and 200mL of Tris-HCl buffer, stir evenly, add the silica dispersion, ultrasonicate for 18min, stir for 6.5h, add 0.4g of nano-ferric oxide, stir for 3.5h, wash, dry and grind to obtain a silica-iron oxide complex; Step 2: Preparation of flame retardant microcapsules: Take 2g of ferric chloride hexahydrate and 50mL of deionized water, stir evenly to obtain ferric chloride hexahydrate solution; take 8mL of anhydrous ethanol and 32mL of deionized water, stir evenly, add 6.5g of silicon dioxide-iron oxide complex, ultrasonically disperse for 35min, add 0.22mL of pyrrole, ultrasonically disperse for 35min, dropwise add ferric chloride hexahydrate solution, stir for 19h, add 1g of 3-mercaptopropionic acid and 0.2g of benzoin dimethyl ether, stir for 5h, filter, dry and grind to obtain flame retardant microcapsules; Step 3: Preparation of flame retardant modified waterborne polyurethane: Take 12g of 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide, 3.5g of trimethylolpropane, and 25mL of acetone, stir evenly to obtain a mixed solution; take 52g of polyether diol, 5g of dihydroxy silicone oil, and 31g of toluene diisocyanate, pass nitrogen, stir for 35min, heat to 78°C, react for 3.8h, cool to 72°C, add the mixed solution, stir evenly, react for 1.5h, cool to 62°C, add 20g of polyethylene glycol, react for 3.5h, cool to 23°C, drop 2.2g of ethylenediamine, 8mL of dodecafluoroheptyl methacrylate, and a mixed solution of 20mL of acetone, react for 60min, and distill to obtain a flame-retardant modified waterborne polyurethane; Step 4: Preparation of flame retardant coating: Take flame retardant modified waterborne polyurethane, styrene acrylic emulsion and emulsifier, stir at 52°C for 65 minutes to obtain a blended emulsion, add a crosslinking agent and a leveling agent, stir evenly to obtain a flame retardant coating; The flame retardant coating comprises the following components, by weight: 98 parts of flame retardant modified waterborne polyurethane, 22 parts of styrene acrylic emulsion, 2.5 parts of crosslinking agent, 3.5 parts of emulsifier, and 0.015 parts of leveling agent; Step 5: Preparation of flame retardant needle punched fabric: Taking polyester chips, ammonium polyphosphate, flame retardant microcapsules and dispersants, blending, extruding, spinning, drawing, opening, carding, needling and heat setting to obtain flame retardant needle-punched cloth; The dispersant is ethylene bis stearic acid amide; The flame retardant needle-punched fabric comprises the following components, by weight: 92 parts of polyester chips, 2.2 parts of ammonium polyphosphate, 2.5 parts of flame retardant microcapsules, and 2.8 parts of dispersant; Step 6: Preparation of silicone flame retardant foot pads: Take the flame retardant needle-punched cloth, stack the buffer layer and leather on its upper surface in sequence, and glue them together to obtain a foot pad; apply the flame retardant coating on the surface of the foot pad, the thickness of the flame retardant coating is 150μm, and then 2 The product was exposed to ultraviolet light for 9 minutes to obtain a flame retardant foot pad.
[0017] Embodiment 2: A method for preparing a silicon-containing flame-retardant foot pad for an automobile, comprising the following steps: Step 1: Preparation of silica-iron oxide composite: Take 1g of silica and 100mL of Tris-HCl buffer, and ultrasonically disperse for 30min to obtain a silica dispersion; take 1.4g of dopamine hydrochloride and 200mL of Tris-HCl buffer, stir evenly, add the silica dispersion, ultrasonicate for 15min, stir for 6h, add 0.4g of nano-iron trioxide, stir for 3h, wash, dry and grind to obtain a silica-iron oxide complex; Step 2: Preparation of flame retardant microcapsules: Take 2g of ferric chloride hexahydrate and 50mL of deionized water, stir evenly to obtain ferric chloride hexahydrate solution; take 8mL of anhydrous ethanol and 32mL of deionized water, stir evenly, add 6.5g of silicon dioxide-iron oxide complex, ultrasonically disperse for 30min, add 0.22mL of pyrrole, ultrasonically disperse for 30min, dropwise add ferric chloride hexahydrate solution, stir for 18h, add 1g of 3-mercaptopropionic acid and 0.2g of benzoin dimethyl ether, stir for 4h, filter, dry and grind to obtain flame retardant microcapsules; Step 3: Preparation of flame retardant modified waterborne polyurethane: Take 12g of 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide, 3.5g of trimethylolpropane, and 25mL of acetone, stir evenly to obtain a mixed solution; take 52g of polyether diol, 5g of dihydroxy silicone oil, and 31g of toluene diisocyanate, pass nitrogen, stir for 30min, heat to 75°C, react for 3.5h, cool to 70°C, add the mixed solution, stir evenly, react for 1h, cool to 60°C, add 20g of polyethylene glycol, react for 3h, cool to 20°C, drop 2.2g of ethylenediamine, 8mL of dodecafluoroheptyl methacrylate, and a mixed solution of 20mL of acetone, react for 50min, and distill to obtain a flame-retardant modified waterborne polyurethane; Step 4: Preparation of flame retardant coating: Take flame retardant modified waterborne polyurethane, styrene acrylic emulsion and emulsifier, stir at 50°C for 60 minutes to obtain a blended emulsion, add a crosslinking agent and a leveling agent, stir evenly to obtain a flame retardant coating; The flame retardant coating comprises the following components, by weight: 95 parts of flame retardant modified waterborne polyurethane, 20 parts of styrene acrylic emulsion, 2 parts of crosslinking agent, 3 parts of emulsifier, and 0.01 parts of leveling agent; Step 5: Preparation of flame retardant needle punched fabric: Taking polyester chips, ammonium polyphosphate, flame retardant microcapsules and dispersants, blending, extruding, spinning, drawing, opening, carding, needling and heat setting to obtain flame retardant needle-punched cloth; The dispersant is ethylene bis stearic acid amide; The flame retardant needle-punched cloth comprises the following components, by weight: 90 parts of polyester chips, 2 parts of ammonium polyphosphate, 2 parts of flame retardant microcapsules, and 2.5 parts of dispersant; Step 6: Preparation of silicone flame retardant foot pads: Take the flame retardant needle-punched cloth, stack the buffer layer and leather on its upper surface in sequence, and glue them together to obtain a foot pad; apply the flame retardant coating on the surface of the foot pad, the thickness of the flame retardant coating is 150μm, and then 2 The product was exposed to ultraviolet light for 8 minutes to obtain a flame retardant foot pad.
[0018] Embodiment 3: A method for preparing a silicon-containing flame-retardant foot pad for an automobile, comprising the following steps: Step 1: Preparation of silica-iron oxide composite: Take 1g of silica and 100mL of Tris-HCl buffer, and ultrasonically disperse for 40min to obtain a silica dispersion; take 1.4g of dopamine hydrochloride and 200mL of Tris-HCl buffer, stir evenly, add the silica dispersion, ultrasonicate for 20min, stir for 7h, add 0.4g of nano-iron trioxide, stir for 4h, wash, dry and grind to obtain a silica-iron oxide complex; Step 2: Preparation of flame retardant microcapsules: Take 2g of ferric chloride hexahydrate and 50mL of deionized water, stir evenly to obtain ferric chloride hexahydrate solution; take 8mL of anhydrous ethanol and 32mL of deionized water, stir evenly, add 6.5g of silicon dioxide-iron oxide complex, ultrasonically disperse for 40min, add 0.22mL of pyrrole, ultrasonically disperse for 40min, dropwise add ferric chloride hexahydrate solution, stir for 20h, add 1g of 3-mercaptopropionic acid and 0.2g of benzoin dimethyl ether, stir for 6h, filter, dry and grind to obtain flame retardant microcapsules; Step 3: Preparation of flame retardant modified waterborne polyurethane: Take 12g of 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide, 3.5g of trimethylolpropane, and 25mL of acetone, stir evenly to obtain a mixed solution; take 52g of polyether diol, 5g of dihydroxy silicone oil, and 31g of toluene diisocyanate, pass nitrogen, stir for 40min, heat to 80°C, react for 4h, cool to 75°C, add the mixed solution, stir evenly, react for 2h, cool to 63°C, add 20g of polyethylene glycol, react for 4h, cool to 25°C, add dropwise a mixed solution of 2.2g of ethylenediamine, 8mL of dodecafluoroheptyl methacrylate, and 20mL of acetone, react for 70min, and distill to obtain a flame-retardant modified waterborne polyurethane; Step 4: Preparation of flame retardant coating: Take flame retardant modified waterborne polyurethane, styrene acrylic emulsion and emulsifier, stir at 55°C for 70 minutes to obtain a blended emulsion, add a crosslinking agent and a leveling agent, stir evenly to obtain a flame retardant coating; The flame retardant coating comprises the following components, by weight: 100 parts of flame retardant modified waterborne polyurethane, 25 parts of styrene acrylic emulsion, 3 parts of crosslinking agent, 4 parts of emulsifier, and 0.02 parts of leveling agent; Step 5: Preparation of flame retardant needle punched fabric: Taking polyester chips, ammonium polyphosphate, flame retardant microcapsules and dispersants, blending, extruding, spinning, drawing, opening, carding, needling and heat setting to obtain flame retardant needle-punched cloth; The dispersant is ethylene bis stearic acid amide; The flame retardant needle-punched fabric comprises the following components, by weight: 95 parts of polyester chips, 2.5 parts of ammonium polyphosphate, 3 parts of flame retardant microcapsules, and 3 parts of dispersant; Step 6: Preparation of silicone flame retardant foot pads: Take the flame retardant needle-punched cloth, stack the buffer layer and leather on its upper surface in sequence, and glue them together to obtain a foot pad; apply the flame retardant coating on the surface of the foot pad, the thickness of the flame retardant coating is 150μm, and then 2 The flame retardant foot pad was obtained by irradiating the surface of the foot pad with ultraviolet light for 10 minutes.
[0019] Comparative Example 1: No iron oxide is added, and the rest is the same as Example 1: Step 1: Preparation of modified silica: Take 1g of silica and 100mL of Tris-HCl buffer, and ultrasonically disperse for 35min to obtain a silica dispersion; take 1.4g of dopamine hydrochloride and 200mL of Tris-HCl buffer, stir evenly, add the silica dispersion, ultrasonically treat for 18min, stir for 9h, wash, dry, and grind to obtain modified silica; Step 2: Preparation of flame retardant microcapsules: Take 2g of ferric chloride hexahydrate and 50mL of deionized water, stir evenly to obtain ferric chloride hexahydrate solution; take 8mL of anhydrous ethanol and 32mL of deionized water, stir evenly, add 6.5g of modified silica, ultrasonically disperse for 35min, add 0.22mL of pyrrole, ultrasonically disperse for 35min, dropwise add ferric chloride hexahydrate solution, stir for 19h, add 1g of 3-mercaptopropionic acid and 0.2g of benzoin dimethyl ether, stir for 5h, filter, dry and grind to obtain flame retardant microcapsules; Step 3: Preparation of flame retardant modified waterborne polyurethane: Take 12g of 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide, 3.5g of trimethylolpropane, and 25mL of acetone, stir evenly to obtain a mixed solution; take 52g of polyether diol, 5g of dihydroxy silicone oil, and 31g of toluene diisocyanate, pass nitrogen, stir for 35min, heat to 78°C, react for 3.8h, cool to 72°C, add the mixed solution, stir evenly, react for 1.5h, cool to 62°C, add 20g of polyethylene glycol, react for 3.5h, cool to 23°C, drop 2.2g of ethylenediamine, 8mL of dodecafluoroheptyl methacrylate, and a mixed solution of 20mL of acetone, react for 60min, and distill to obtain a flame-retardant modified waterborne polyurethane; Step 4: Preparation of flame retardant coating: Take flame retardant modified waterborne polyurethane, styrene acrylic emulsion and emulsifier, stir at 52°C for 65 minutes to obtain a blended emulsion, add a crosslinking agent and a leveling agent, stir evenly to obtain a flame retardant coating; The flame retardant coating comprises the following components, by weight: 98 parts of flame retardant modified waterborne polyurethane, 22 parts of styrene acrylic emulsion, 2.5 parts of crosslinking agent, 3.5 parts of emulsifier, and 0.015 parts of leveling agent; Step 5: Preparation of flame retardant needle punched fabric: Taking polyester chips, ammonium polyphosphate, flame retardant microcapsules and dispersants, blending, extruding, spinning, drawing, opening, carding, needling and heat setting to obtain flame retardant needle-punched cloth; The dispersant is ethylene bis stearic acid amide; The flame retardant needle-punched fabric comprises the following components, by weight: 92 parts of polyester chips, 2.2 parts of ammonium polyphosphate, 2.5 parts of flame retardant microcapsules, and 2.8 parts of dispersant; Step 6: Preparation of silicone flame retardant foot pads: Take the flame retardant needle-punched cloth, stack the buffer layer and leather on its upper surface in sequence, and glue them together to obtain a foot pad; apply the flame retardant coating on the surface of the foot pad, the thickness of the flame retardant coating is 150μm, and then 2 The product was exposed to ultraviolet light for 9 minutes to obtain a flame retardant foot pad.
[0020] Comparative Example 2: Microcapsules were not prepared, and the rest was the same as Example 1: Step 1: Preparation of silica-iron oxide composite: Take 1g of silica and 100mL of Tris-HCl buffer, and ultrasonically disperse for 35min to obtain a silica dispersion; take 1.4g of dopamine hydrochloride and 200mL of Tris-HCl buffer, stir evenly, add the silica dispersion, ultrasonicate for 18min, stir for 6.5h, add 0.4g of nano-ferric oxide, stir for 3.5h, wash, dry and grind to obtain a silica-iron oxide complex; Step 2: Preparation of flame retardant modified waterborne polyurethane: Take 12g of 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide, 3.5g of trimethylolpropane, and 25mL of acetone, stir evenly to obtain a mixed solution; take 52g of polyether diol, 5g of dihydroxy silicone oil, and 31g of toluene diisocyanate, pass nitrogen, stir for 35min, heat to 78°C, react for 3.8h, cool to 72°C, add the mixed solution, stir evenly, react for 1.5h, cool to 62°C, add 20g of polyethylene glycol, react for 3.5h, cool to 23°C, drop 2.2g of ethylenediamine, 8mL of dodecafluoroheptyl methacrylate, and a mixed solution of 20mL of acetone, react for 60min, and distill to obtain a flame-retardant modified waterborne polyurethane; Step 4: Preparation of flame retardant coating: Take flame retardant modified waterborne polyurethane, styrene acrylic emulsion and emulsifier, stir at 52°C for 65 minutes to obtain a blended emulsion, add a crosslinking agent and a leveling agent, stir evenly to obtain a flame retardant coating; The flame retardant coating comprises the following components, by weight: 98 parts of flame retardant modified waterborne polyurethane, 22 parts of styrene acrylic emulsion, 2.5 parts of crosslinking agent, 3.5 parts of emulsifier, and 0.015 parts of leveling agent; Step 5: Preparation of flame retardant needle punched fabric: The polyester chips, ammonium polyphosphate, silicon dioxide-iron oxide compound and dispersant are blended, extruded, spun, drawn, opened, carded, needled and heat-set to obtain flame-retardant needle-punched fabric; The dispersant is ethylene bis stearic acid amide; The flame retardant needle-punched cloth comprises the following components, by weight: 92 parts of polyester chips, 2.2 parts of ammonium polyphosphate, 2.5 parts of silicon dioxide-iron oxide composite, and 2.8 parts of dispersant; Step 6: Preparation of silicone flame retardant foot pads: Take the flame retardant needle-punched cloth, stack the buffer layer and leather on its upper surface in sequence, and glue them together to obtain a foot pad; apply the flame retardant coating on the surface of the foot pad, the thickness of the flame retardant coating is 150μm, and then 2 The product was exposed to ultraviolet light for 9 minutes to obtain a flame retardant foot pad.
[0021] Comparative Example 3: No dodecafluoroheptyl methacrylate was added, and the rest was the same as Example 1: Step 1: Preparation of silica-iron oxide composite: Take 1g of silica and 100mL of Tris-HCl buffer, and ultrasonically disperse for 35min to obtain a silica dispersion; take 1.4g of dopamine hydrochloride and 200mL of Tris-HCl buffer, stir evenly, add the silica dispersion, ultrasonicate for 18min, stir for 6.5h, add 0.4g of nano-ferric oxide, stir for 3.5h, wash, dry and grind to obtain a silica-iron oxide complex; Step 2: Preparation of flame retardant microcapsules: Take 2g of ferric chloride hexahydrate and 50mL of deionized water, stir evenly to obtain ferric chloride hexahydrate solution; take 8mL of anhydrous ethanol and 32mL of deionized water, stir evenly, add 6.5g of silicon dioxide-iron oxide complex, ultrasonically disperse for 35min, add 0.22mL of pyrrole, ultrasonically disperse for 35min, dropwise add ferric chloride hexahydrate solution, stir for 19h, add 1g of 3-mercaptopropionic acid and 0.2g of benzoin dimethyl ether, stir for 5h, filter, dry and grind to obtain flame retardant microcapsules; Step 3: Preparation of flame retardant modified waterborne polyurethane: Take 12g of 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide, 3.5g of trimethylolpropane, and 25mL of acetone, stir evenly to obtain a mixed solution; take 52g of polyether diol, 5g of dihydroxy silicone oil, and 31g of toluene diisocyanate, pass nitrogen, stir for 35min, heat to 78°C, react for 3.8h, cool to 72°C, add the mixed solution, stir evenly, react for 1.5h, cool to 62°C, add 20g of polyethylene glycol, react for 3.5h, cool to 23°C, dropwise add a mixed solution of 2.2g of ethylenediamine and 20mL of acetone, react for 60min, and distill to obtain a flame-retardant modified waterborne polyurethane; Step 4: Preparation of flame retardant coating: Take flame retardant modified waterborne polyurethane, styrene acrylic emulsion and emulsifier, stir at 52°C for 65 minutes to obtain a blended emulsion, add a crosslinking agent and a leveling agent, stir evenly to obtain a flame retardant coating; The flame retardant coating comprises the following components, by weight: 98 parts of flame retardant modified waterborne polyurethane, 22 parts of styrene acrylic emulsion, 2.5 parts of crosslinking agent, 3.5 parts of emulsifier, and 0.015 parts of leveling agent; Step 5: Preparation of flame retardant needle punched fabric: Taking polyester chips, ammonium polyphosphate, flame retardant microcapsules and dispersants, blending, extruding, spinning, drawing, opening, carding, needling and heat setting to obtain flame retardant needle-punched cloth; The dispersant is ethylene bis stearic acid amide; The flame retardant needle-punched fabric comprises the following components, by weight: 92 parts of polyester chips, 2.2 parts of ammonium polyphosphate, 2.5 parts of flame retardant microcapsules, and 2.8 parts of dispersant; Step 6: Preparation of silicone flame retardant foot pads: Take the flame-retardant needle-punched cloth, stack a buffer layer and leather on its upper surface in sequence, and glue them together to obtain a foot pad; apply a flame-retardant coating on the surface of the foot pad, the thickness of the flame-retardant coating is 150 μm, and obtain a flame-retardant foot pad.
[0022] experiment: The flame retardant foot pads prepared in Example 1 to Example 3 and Comparative Example 1 to Comparative Example 3 were tested for performance. The flame retardant foot pads were tested for limiting oxygen index. The flame retardant foot pads were then placed in water, washed 10 times, each time for 30 minutes, dried, and the limiting oxygen index after washing was tested again. The flame retardant foot pads were cut into 60 mm × 25 mm specimens, and their mechanical properties were tested with reference to GB / T 1040.3-2006. The tensile speed was 100 mm / min, and the obtained data were as follows:
[0023] Conclusion: From the comparison of the data in the table, it can be seen that in Comparative Example 1, no iron oxide is added, silicon dioxide is easy to agglomerate, and the flame retardant properties of the foot pads are reduced. In Comparative Example 2, no microcapsules are prepared, and the flame retardant properties of the silicon-containing flame retardant foot pads are reduced. In Comparative Example 3, no dodecafluoroheptyl methacrylate is added. After multiple water washings, the adhesion of the coating is greatly reduced, and the flame retardant properties of the foot pads are reduced. Examples 1-3 of the present invention add dodecafluoroheptyl methacrylate, and 3-mercaptopropionic acid is also added to the flame retardant microcapsules. 3-mercaptopropionic acid can react with dodecafluoroheptyl methacrylate in the flame retardant coating under ultraviolet light, thereby enhancing the adhesion of the coating and thus enhancing the performance of the foot pads.
[0024] It will be apparent to those skilled in the art that the present invention is not limited to the details of the exemplary embodiments described above and that the present invention can be implemented in other specific forms without departing from the spirit or essential features of the present invention. Therefore, the embodiments should be considered exemplary and non-restrictive in all respects, and the scope of the present invention is defined by the appended claims rather than the above description, and it is intended that all changes falling within the meaning and scope of the equivalent elements of the claims be included in the present invention.
Claims
1. A method for preparing a silicon-containing flame-retardant foot pad for automobiles, characterized in that: The following steps are involved: Step 1: Take ferric chloride hexahydrate and deionized water, stir evenly to obtain ferric chloride hexahydrate solution; take anhydrous ethanol and deionized water, stir evenly, add silicon dioxide-iron oxide complex, ultrasonically disperse for 30-40 minutes, add pyrrole, ultrasonically disperse for 30-40 minutes, dropwise add ferric chloride hexahydrate solution, stir for 18-20 hours, add 3-mercaptopropionic acid and benzoin dimethyl ether, stir for 4-6 hours, filter, dry and grind to obtain flame retardant microcapsules; Step 2: taking polyester chips, ammonium polyphosphate, flame retardant microcapsules, and dispersants, blending, extruding, spinning, drawing, opening, combing, needling, and heat setting to obtain flame retardant needle-punched cloth; Step 3: Take the flame-retardant needle-punched cloth, and stack the buffer layer and leather on its upper surface in sequence, and glue them together to obtain a foot pad; Step 4: Apply the flame retardant coating to the surface of the foot pad, and then 2 Expose to ultraviolet light for 8-10 minutes to obtain a flame retardant foot pad.
2. The method for preparing a silicon-containing flame-retardant automotive foot pad according to claim 1, characterized in that: The preparation method of the flame retardant coating comprises: taking flame retardant modified waterborne polyurethane, styrene acrylic emulsion and emulsifier, stirring at 50-55° C. for 60-70 minutes to obtain a blended emulsion, adding a crosslinking agent and a leveling agent, stirring evenly to obtain the flame retardant coating.
3. The method for preparing a silicon-containing flame-retardant automotive foot pad according to claim 1, characterized in that: The preparation method of the silicon dioxide-iron oxide complex is as follows: silicon dioxide and Tris-HCl buffer are taken, ultrasonically dispersed for 30-40 minutes to obtain a silicon dioxide dispersion; dopamine hydrochloride and Tris-HCl buffer are taken, stirred evenly, added with the silicon dioxide dispersion, ultrasonicated for 15-20 minutes, stirred for 6-7 hours, added with nano-iron trioxide, stirred for 3-4 hours, washed, dried and ground to obtain the silicon dioxide-iron oxide complex.
4. The method for preparing a silicon-containing flame-retardant automotive foot pad according to claim 2, characterized in that: The preparation method of the flame retardant modified waterborne polyurethane comprises the following steps: taking 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide, trimethylolpropane and acetone, stirring evenly to obtain a mixed solution; taking polyether diol, dihydroxy silicone oil and toluene diisocyanate, passing nitrogen, stirring for 30-40 minutes, heating to 75-80°C, reacting for 3.5-4 hours, cooling to 70-75°C, adding the mixed solution, stirring evenly, reacting for 1-2 hours, cooling to 60-63°C, adding polyethylene glycol, reacting for 3-4 hours, cooling to 20-25°C, dropping a mixed solution of ethylenediamine, dodecafluoroheptyl methacrylate and acetone, reacting for 50-70 minutes, and distilling to obtain the flame retardant modified waterborne polyurethane.
5. The method for preparing a silicon-containing flame-retardant automotive foot pad according to claim 1, characterized in that: The flame retardant needle-punched cloth comprises the following components, by weight: 90-95 parts of polyester chips, 2-2.5 parts of ammonium polyphosphate, 2-3 parts of flame retardant microcapsules, and 2.5-3 parts of dispersant.
6. The method for preparing a silicon-containing flame-retardant automotive foot pad according to claim 2, characterized in that: The flame retardant coating comprises the following components, by weight: 95-100 parts of flame retardant modified waterborne polyurethane, 20-25 parts of styrene acrylic emulsion, 2-3 parts of crosslinking agent, 3-4 parts of emulsifier, and 0.01-0.02 parts of leveling agent.
7. The method for preparing a silicon-containing flame-retardant automotive foot pad according to claim 5, characterized in that: The dispersant is ethylene bis stearic acid amide.
8. The silicon-containing flame-retardant foot pad prepared according to the method for preparing a silicon-containing flame-retardant foot pad for automobiles according to any one of claims 1 to 7.
Citation Information
Patent Citations
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