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Flame-retardant agent containing spirane structure and having antioxidant function and preparation method

A technology of spiral ring structure and flame retardant, which is applied in the field of flame retardants and can solve problems such as threats to life safety

Inactive Publication Date: 2016-10-12
CHANGZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, it is a flammable substance, which is easy to burn and generates a lot of heat, which poses a great threat to people's life safety. In order to reduce the occurrence of fires, researchers from all over the world have devoted themselves to the research of flame retardant materials and developed a A series of flame retardants with good flame retardant properties

Method used

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  • Flame-retardant agent containing spirane structure and having antioxidant function and preparation method
  • Flame-retardant agent containing spirane structure and having antioxidant function and preparation method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Under protective gas, 76.65g of phosphorus oxychloride was added to a four-necked flask with a thermometer and a stirring device and stirred, and the temperature of the system was raised to 80 °C, then 6.81g of pentaerythritol (PER) was weighed, and the PER powder was divided into 3 times of addition, each addition was added to a four-necked flask at an interval of 20 min, and the reaction was performed at a constant temperature for 20 h at the above temperature, and the reaction solution was concentrated, suction filtered, washed, and dried to obtain a pentaerythritol spirocyclic phosphate intermediate (SPDPC), which was produced. The rate was 91.5%. Weigh 3g of intermediate SPDPC and add 30mL of acetonitrile, stir and dissolve, then weigh 15.14g of hindered amine and 1.38g of potassium carbonate, dissolve in 80mL of acetonitrile and then add dropwise to the above reaction system, add dropwise for 30min, dropwise add After the completion of the reaction at 110 ° C for ...

Embodiment 2

[0030] Under protective gas, 91.98g of phosphorus oxychloride was added to a four-necked flask with a thermometer and a stirring device and stirred, and the temperature of the system was raised to 80 °C, then 6.81g of pentaerythritol (PER) was weighed, and the PER powder was divided into Add 3 times, add each feeding interval 30min to a four-necked flask, react at a constant temperature for 20h at the above temperature, concentrate the reaction solution, suction filter, wash, dry, obtain pentaerythritol spirocyclic phosphate intermediate (SPDPC), produce The rate was 94.7%. Weigh 3g of intermediate SPDPC and add 30mL of acetonitrile, stir and dissolve, then weigh 22.72g of hindered amine and 2.07g of potassium carbonate, dissolve in 120mL of acetonitrile and then add dropwise to the above reaction system, add dropwise for 30min, dropwise add After the completion of the reaction at 110°C for 24 hours, the reaction solution was concentrated, filtered, washed and dried to obtain ...

Embodiment 3

[0032] 76.65g of phosphorus oxychloride was added to a four-necked flask with a thermometer and a stirring device under protective gas, and the temperature of the system was raised to 90°C, then 6.81g of pentaerythritol (PER) was weighed, and the PER powder was divided into Add 3 times, add each feeding interval 30min into a four-necked flask, react at a constant temperature for 24h at the above temperature, concentrate the reaction solution, suction filter, wash and dry to obtain a pentaerythritol spirocyclic phosphate intermediate (SPDPC), which is produced. The rate was 93.8%. Weigh 3g of intermediate SPDPC and add 60mL of acetonitrile, stir and dissolve, then weigh 15.14g of hindered amine and 1.38g of potassium carbonate, dissolve in 160mL of acetonitrile and then add dropwise to the above reaction system, add dropwise for 1h, dropwise add After the completion of the reaction at 120°C for 28 hours, the reaction solution was concentrated, filtered, washed and dried to obta...

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Abstract

The invention relates to a flame-retardant agent containing a spirane structure and having an antioxidant function and a preparation method, and belongs to the technical field of flame-retardant agents. High-activity phosphoryl chloride on phosphorus oxychloride and hydroxyl groups on pentaerythritol have nucleophilic substitution reaction to prepare a spirocyclic phosphate intermediate SPDPC, then active chlorine on SPDPC and alcoholic hydroxyl groups on hindered amine are used for nucleophilic substitution reaction, and the flame-retardant agent containing the spirane structure and having the antioxidant function is formed. The spirocyclic phosphate structure contains pentaerythritol units and can provide sufficient carbon sources for an expansion flame-retardant system. Besides, the hindered amine can effectively capture active radials generated during decomposition of polymer, and chain reaction is delayed.

Description

technical field [0001] The invention relates to a flame retardant containing a spiro ring structure with antioxidant function and a preparation method, and belongs to the technical field of flame retardants. Background technique [0002] Polypropylene polymer materials are closely related to people's lives. Based on its excellent transparency, chemical resistance, heat resistance, folding resistance and high strength, it has been widely used in automobiles, electrical appliances, textiles, national defense, medical Sanitary equipment, composite coating, packing tape and other fields. However, it is a flammable substance, which is easy to burn and generates a lot of heat, which poses a great threat to people's life safety. A series of flame retardants with good flame retardant properties. [0003] A series of spiro phosphate flame retardants obtained by reacting pentaerythritol with phosphorus oxychloride or phosphorus trichloride have better flame retardancy, thermal stabi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08K5/5399
CPCC08K5/5399
Inventor 李锦春李雄杰刘雨邹国享赵彩霞
Owner CHANGZHOU UNIV
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