Method for preparing cooperative flame retardant nylon 6

Abstract

The invention discloses a method for preparing cooperative flame retardant nylon 6, which comprises the following steps: adding a sodium hydroxide aqueous solution in an aluminum nitrate and magnesiumnitrate aqueous solution to react at room temperature; then adding a dissolved sodium stearate aqueous solution in the reaction system and then keeping the reaction; filtering, washing and drying theproduct to obtain modified lamellar magnesium aluminum bihydroxide powder; respectively weighing microcapsule red phosphorus, the modified lamellar magnesium aluminum bihydroxide powder and nylon 6 granules and drying; premixing the three dried materials; fusing, blending, extruding and granulating in a double-screw rod extruder; drying to obtain a cooperative flame retardant nylon 6 master granule. The invention uses ammonium persulphate as an initiating agent, and an ignition point of the prepared microcapsule red phosphorus exceeds 450DEG C; when the vertical combustion performance of a nylon 6 composite material reaches the V-0 level, and LOI reaches more than 28 percent, the consumption of flame retardant agents is less, and all used flame retardant agents are cheap halogen-free flame retardant agents, thereby reducing the cost.

Description

technical field

[0001] The invention belongs to the preparation of flame-retardant composite materials, in particular to a preparation method of synergistic flame-retardant nylon 6. Background technique

[0002] Nylon 6 is one of the most widely used engineering plastics at present. It has excellent mechanical strength, wear resistance, self-lubricating property, corrosion resistance and molding processability. However, the limiting oxygen index of nylon PA6 is only about 22%. At the same time, when it is heated and burned, it is particularly prone to melt dripping, which ignites other combustibles, causing the fire to spread further, causing casualties and property losses. Therefore, it is necessary to Make the necessary flame retardant modification to it.

[0003] Since 1971, when Miyata et al first published related reports about layered double hydroxides (LDHs) in public journals, the application reports about it have been increasing year by year. If an organic anion i...

Examples

preparation example Construction

[0013] In conjunction with accompanying drawing, the preparation method of synergistic flame-retardant nylon 6 of the present invention, its steps are as follows:

[0014] The first step is to add sodium hydroxide aqueous solution to aluminum nitrate and magnesium nitrate aqueous solution to react at room temperature, and the reaction time is 1.5 to 3 hours; then add dissolved sodium stearate aqueous solution to the aforementioned reaction system to continue the reaction , the reaction time is 1.5 to 3 hours; the product is filtered, washed and dried to obtain the modified layered magnesium aluminum hydroxide powder. Wherein, the molar ratio of sodium stearate, aluminum nitrate and magnesium nitrate is 0.8~1.2:1:3.

[0015] The second step is to weigh microcapsule red phosphorus, modified layered magnesium aluminum hydroxide powder and nylon 6 pellets respectively, and dry them; wherein microcapsule red phosphorus, layered magnesium aluminum hydroxide powder and nylon 6 pellet...

Embodiment 1

[0018] The preparation method of synergistic flame-retardant nylon 6 of the present invention, its steps are as follows:

[0019] Step 1: Mix 60g of melamine and 119.05g of formaldehyde solution (36%), react at pH=9, 80°C for 25 minutes to prepare a prepolymer; add 5.5g of ammonium persulfate and the prepolymer to 300g of red In 1.2L aqueous solution of phosphorus (about 5000 mesh), the pH value is adjusted to 5, the temperature is controlled at 55°C, and the reaction is carried out for 1.5h; the product is filtered, washed, and dried to obtain microencapsulated red phosphorus;

[0020] Step 2: At room temperature, add 3L of 1.5M sodium hydroxide aqueous solution to 3L of 2M aluminum nitrate and 6M magnesium nitrate aqueous solution, and react for 1.5h; Sodium fatty acid aqueous solution, reacted for 1.5h; the product was filtered, washed, and dried to obtain the modified layered magnesium aluminum hydroxide powder;

[0021] Step 3: Weigh 30g of microcapsule red phosphorus, 3...

Embodiment 2

[0025] The preparation method of synergistic flame-retardant nylon 6 of the present invention, its steps are as follows:

[0026] The first step: mix 60g of melamine and 119.05g of formaldehyde solution (36%), react at pH=9, 95°C for 45min to prepare a prepolymer; add 5.5g of potassium persulfate and the prepolymer to 360g of red In 1.2L aqueous solution of phosphorus (about 5000 mesh), adjust the pH value to 6, control the temperature at 75°C, and react for 1.5h; filter, wash and dry the product to obtain microencapsulated red phosphorus;

[0027] Step 2: At room temperature, add 3L of 1.5M sodium hydroxide aqueous solution to 3L of 2M aluminum nitrate and 6M magnesium nitrate aqueous solution, and react for 1.5h; Sodium fatty acid aqueous solution, reacted for 1.5h; the product was filtered, washed, and dried to obtain the modified layered magnesium aluminum hydroxide powder;

[0028] Step 3: Weigh 36g of microcapsule red phosphorus, 30g of modified layered magnesium alumin...

technical field

[0001] The invention belongs to the preparation of flame-retardant composite materials, in particular to a preparation method of synergistic flame-retardant nylon 6. Background technique

[0002] Nylon 6 is one of the most widely used engineering plastics at present. It has excellent mechanical strength, wear resistance, self-lubricating property, corrosion resistance and molding processability. However, the limiting oxygen index of nylon PA6 is only about 22%. At the same time, when it is heated and burned, it is particularly prone to melt dripping, which ignites other combustibles, causing the fire to spread further, causing casualties and property losses. Therefore, it is necessary to Make the necessary flame retardant modification to it.

[0003] Since 1971, when Miyata et al first published related reports about layered double hydroxides (LDHs) in public journals, the application reports about it have been increasing year by year. If an organic anion i...

Examples

preparation example Construction

[0013] In conjunction with accompanying drawing, the preparation method of synergistic flame-retardant nylon 6 of the present invention, its steps are as follows:

[0014] The first step is to add sodium hydroxide aqueous solution to aluminum nitrate and magnesium nitrate aqueous solution to react at room temperature, and the reaction time is 1.5 to 3 hours; then add dissolved sodium stearate aqueous solution to the aforementioned reaction system to continue the reaction , the reaction time is 1.5 to 3 hours; the product is filtered, washed and dried to obtain the modified layered magnesium aluminum hydroxide powder. Wherein, the molar ratio of sodium stearate, aluminum nitrate and magnesium nitrate is 0.8~1.2:1:3.

[0015] The second step is to weigh microcapsule red phosphorus, modified layered magnesium aluminum hydroxide powder and nylon 6 pellets respectively, and dry them; wherein microcapsule red phosphorus, layered magnesium aluminum hydroxide powder and nylon 6 pellet...

Embodiment 1

[0018] The preparation method of synergistic flame-retardant nylon 6 of the present invention, its steps are as follows:

[0019] Step 1: Mix 60g of melamine and 119.05g of formaldehyde solution (36%), react at pH=9, 80°C for 25 minutes to prepare a prepolymer; add 5.5g of ammonium persulfate and the prepolymer to 300g of red In 1.2L aqueous solution of phosphorus (about 5000 mesh), the pH value is adjusted to 5, the temperature is controlled at 55°C, and the reaction is carried out for 1.5h; the product is filtered, washed, and dried to obtain microencapsulated red phosphorus;

[0020] Step 2: At room temperature, add 3L of 1.5M sodium hydroxide aqueous solution to 3L of 2M aluminum nitrate and 6M magnesium nitrate aqueous solution, and react for 1.5h; Sodium fatty acid aqueous solution, reacted for 1.5h; the product was filtered, washed, and dried to obtain the modified layered magnesium aluminum hydroxide powder;

[0021] Step 3: Weigh 30g of microcapsule red phosphorus, 3...

Embodiment 2

[0025] The preparation method of synergistic flame-retardant nylon 6 of the present invention, its steps are as follows:

[0026] The first step: mix 60g of melamine and 119.05g of formaldehyde solution (36%), react at pH=9, 95°C for 45min to prepare a prepolymer; add 5.5g of potassium persulfate and the prepolymer to 360g of red In 1.2L aqueous solution of phosphorus (about 5000 mesh), adjust the pH value to 6, control the temperature at 75°C, and react for 1.5h; filter, wash and dry the product to obtain microencapsulated red phosphorus;

[0027] Step 2: At room temperature, add 3L of 1.5M sodium hydroxide aqueous solution to 3L of 2M aluminum nitrate and 6M magnesium nitrate aqueous solution, and react for 1.5h; Sodium fatty acid aqueous solution, reacted for 1.5h; the product was filtered, washed, and dried to obtain the modified layered magnesium aluminum hydroxide powder;

[0028] Step 3: Weigh 36g of microcapsule red phosphorus, 30g of modified layered magnesium alumin...

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