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Sulfur containing cage-like organic phosphate/ammonium polyphosphate compounded polyolefin fire retardant and preparation method thereof

An organic phosphate and ammonium polyphosphate technology, applied in the field of polyolefin flame retardants, can solve the problems of a large amount of inorganic flame retardants, human health and environmental hazards, and the decline of the mechanical properties of the matrix, and achieves high flame retardant efficiency, Good moisture absorption and good compatibility

Active Publication Date: 2020-02-18
NANJING UNIV OF AERONAUTICS & ASTRONAUTICS
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] At present, the most widely used polyolefin flame retardants usually include various inorganic flame retardants and organic halogen flame retardants, but these flame retardants have very obvious defects: large amount of inorganic flame retardants, poor dispersion and lead to The mechanical properties of the matrix have declined; although the organic halogen flame retardant has a good flame retardant effect, it will release a large amount of toxic substances such as hydrogen halide when the matrix is ​​burned, which is harmful to human health and the environment.

Method used

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  • Sulfur containing cage-like organic phosphate/ammonium polyphosphate compounded polyolefin fire retardant and preparation method thereof
  • Sulfur containing cage-like organic phosphate/ammonium polyphosphate compounded polyolefin fire retardant and preparation method thereof
  • Sulfur containing cage-like organic phosphate/ammonium polyphosphate compounded polyolefin fire retardant and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] Step 1: Add 54.46 g (0.4 mol) of pentaerythritol and 100 mL of solvent benzene into a four-neck flask equipped with stirring, thermometer, and condenser, stir and heat to reflux temperature (90°C) under nitrogen protection, and weigh sulfur trichloride Phosphorus 42.42mL (0.4mol), quickly drop half of the weighed amount of phosphorus trichloride, and slowly add the other half dropwise from the addition funnel, stir and react for about 7 hours until the white solid product is completely precipitated. Cool to room temperature, filter the product with dichloromethane or chloroform, wash, and then dry in a vacuum oven at 80°C to obtain white powdery intermediate A.

[0032] Step 2: Add 21.21 g (0.2 mol) of phosphorus trichloride and 100 mL of anhydrous acetonitrile into a four-necked flask equipped with stirring, a thermometer, and a condenser, mix at room temperature until the system is stable, and then add the first step 78.42g (0.4mol) of the synthesized intermediate A w...

Embodiment 2

[0045] Step 1: Add 44.93g (0.33mol) of pentaerythritol and 100mL of solvent benzene into a four-neck flask equipped with a stirring, thermometer, and condenser tube, stir and heat to reflux temperature (80°C) under nitrogen protection, and weigh sulfur trichloride Phosphorus 67.76g (0.4mol), quickly drop half of the weighed amount of phosphorus trichloride, and slowly add the other half dropwise from the addition funnel, stir and react for about 7 hours until the white solid product is completely precipitated. Cool to room temperature, filter the product with dichloromethane or chloroform, wash, and then dry in a vacuum oven at 80°C to obtain white powdery intermediate A.

[0046] Step 2: Add 33.88 g (0.2 mol) of phosphorus trichloride and 100 mL of anhydrous acetonitrile into a four-necked flask equipped with stirring, a thermometer, and a condenser, mix at room temperature until the system is stable, and then add the first step 64.69g (0.33mol) of the synthesized intermediat...

Embodiment 3

[0058] Step 1: Add 49.01 g (0.36 mol) of pentaerythritol and 100 mL of solvent benzene into a four-necked flask equipped with stirring, thermometer, and condenser, stir and heat to reflux temperature (80°C) under nitrogen protection, and weigh sulfur trichloride Phosphorus 67.76g (0.4mol), quickly drop half of the weighed amount of phosphorus trichloride, and slowly add the other half dropwise from the addition funnel, stir and react for about 7 hours until the white solid product is completely precipitated. Cool to room temperature, filter the product with dichloromethane or chloroform, wash, and then dry in a vacuum oven at 80°C to obtain white powdery intermediate A.

[0059] Step 2: Add 33.88 g (0.2 mol) of phosphorus trichloride and 100 mL of anhydrous acetonitrile into a four-necked flask equipped with stirring, a thermometer, and a condenser, mix at room temperature until the system is stable, and then add the first step 70.57g (0.36mol) of the synthesized intermediate ...

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Abstract

The invention relates to a sulfur containing cage-like organic phosphate / ammonium polyphosphate compounded polyolefin fire retardant and a preparation method thereof. The preparation method comprisesfollowing steps: reacting pentaerythritol with thiophosphoryl chloride under certain conditions, and after reactions, filtering, washing, and drying the reaction product to obtain a white powdery intermediate A; reacting the intermediate A with thiophosphoryl chloride under certain conditions for a while, cooling, carrying out rotary evaporation and drying to obtain a white powdery intermediate B;reacting the intermediate B with diethylamine under certain conditions, filtering, washing, and drying to obtain a white powdery product namely sulfur containing cage-like organic phosphate; compounding the white powdery product namely sulfur containing cage-like organic phosphate with ammonium polyphosphate according to a certain ratio t obtain a white solid namely the sulfur containing cage-like organic phosphate / ammonium polyphosphate compounded polyolefin fire retardant. The fire retardant is prepared by compounding a nitrogen fire retardant, a phosphorus fire retardant, and a sulfur fireretardant, the synergistic fire-retardant effect is excellent, and the fire retardant is not dissolved by water and most of organic solvents, and has a good fire retardant effect on multiple polyolefin materials.

Description

technical field [0001] The invention relates to the technical field of polyolefin flame retardants, in particular to a sulfur-containing cage organic phosphate / ammonium polyphosphate compound polyolefin flame retardant and a preparation method thereof. Background technique [0002] Polyolefin is obtained by the single polymerization or copolymerization of various olefins such as ethylene and propylene. It is a kind of thermoplastic synthetic resin with excellent performance. It has abundant raw materials and low price. It has excellent chemical resistance, heat resistance and electrical insulation. With good mechanical properties and processing properties, it has been widely used in medical equipment, electronics, building materials, aerospace and other fields since its inception, and has become an indispensable basic material in various industrial fields. However, the application of polyolefin is extremely limited by its flammability defect, and it is easy to generate molte...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08K5/5399C08K3/32C08L23/12C08L23/06C08L23/08C07F9/6574
CPCC08K5/5399C08K3/32C07F9/65748C08K2003/323C08L2201/02C08L2201/22C08L23/12C08L23/06C08L23/0853
Inventor 周金堂易鹏术
Owner NANJING UNIV OF AERONAUTICS & ASTRONAUTICS
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