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Preparation method of phosphorus-containing triazole compound and application of phosphorus-containing triazole compound in flame-retardant polylactic acid

A technology for triazoles and compounds, which is applied in the field of preparation of phosphorus-containing triazole compounds, can solve the problems of high addition amount, influence on material properties, etc., and achieves the effects of short cycle, easy post-processing and simple synthesis process

Active Publication Date: 2019-03-08
FUJIAN NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the common intumescent flame retardant system needs a very high additive amount to have good flame retardant performance, which also means that it will affect various properties of the material

Method used

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  • Preparation method of phosphorus-containing triazole compound and application of phosphorus-containing triazole compound in flame-retardant polylactic acid
  • Preparation method of phosphorus-containing triazole compound and application of phosphorus-containing triazole compound in flame-retardant polylactic acid
  • Preparation method of phosphorus-containing triazole compound and application of phosphorus-containing triazole compound in flame-retardant polylactic acid

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] 0.1mol DOPO, 96ml (1.5mol) CH 2 Cl 2 Add it into a three-necked flask equipped with a thermometer and a mechanical stirrer. After the raw materials are evenly mixed, add 13.9ml (0.1mol) of triethylamine. After the raw materials are completely dissolved, add 3-amino-1,2,4-triazol azole 0.1mol, then add 9.6ml (0.1mol) CCl dropwise 4 , the temperature of the solution was controlled at about 5±1°C during the dropwise addition. After the dropwise addition was completed, it was reacted at room temperature for 20 hours. Finally, the resulting solution was filtered with suction, and the filter cake was taken and washed with CH 2 Cl 2 Wash once, dry at 45°C, wash twice with deionized water, and dry at 50°C to obtain a phosphorus-containing triazole compound with a yield of 69%.

Embodiment 2

[0028] 0.1mol DOPO, 96m (1.5mol) CH 2 Cl 2 Add it into a three-necked flask equipped with a thermometer and a mechanical stirrer. After the raw materials are evenly mixed, add 13.9ml (0.1mol) of triethylamine. After the raw materials are completely dissolved, add 3-amino-1,2,4-triazol azole 0.1mol, then add 9.6ml (0.1mol) CCl dropwise 4 , the temperature of the solution was controlled at 10±1°C during the dropwise addition. After the dropwise addition was completed, it was reacted at room temperature for 20 hours. Finally, the resulting solution was filtered with suction, and the filter cake was taken and washed with CH 2 Cl 2 Wash once, dry at 45°C, wash twice with deionized water, and dry at 50°C to obtain a phosphorus-containing triazole compound with a yield of 68%.

Embodiment 3

[0030] 0.1mol DOPO, 96ml (1.5mol) CH 2 Cl 2 Add it into a three-necked flask equipped with a thermometer and a mechanical stirrer. After the raw materials are evenly mixed, add 13.9ml (0.1mol) of triethylamine. After the raw materials are completely dissolved, add 3-amino-1,2,4-triazol azole 0.1mol, then add 9.6ml (0.1mol) CCl dropwise 4 , the temperature of the solution was controlled at 14±1°C during the dropwise addition. After the dropwise addition was completed, it was reacted at room temperature for 20 hours. Finally, the resulting solution was suction-filtered, and the filter cake was taken and washed with CH 2 Cl 2 Wash once, dry at 45°C, wash twice with deionized water, and dry at 50°C to obtain a phosphorus-containing triazole compound with a yield of 60%.

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Abstract

The invention discloses a preparation method of phosphorus-containing triazole compound and application of the phosphorus-containing triazole compound in flame-retardant polylactic acid. The preparation method includes: putting DOPO (9,10-dihydro-9-oxa-10-phosphaphenanthrene-10- oxide) and CH2C12 into a three-opening flask, adding a certain amount of triethylamine, adding 3-amino-1,2,4-triazole after materials in the flask are dissolved, adding CCl4 dropwise, extracting and filtering after reaction is cover, taking filter cakes, washing and drying to obtain the phosphorus-containing triazole compound. The preparation method of the phosphorus-containing triazole compound is simple in processing steps and postprocessing processes, the obtained phosphorus-containing triazole compound is highin purity. The phosphorus-containing triazole compound can be applied to the flame-retardant polylactic acid and is highly compatible with the polylactic acid, a flame-retardant polylactic acid material prepared from the phosphorus-containing triazole compound is excellent in flame retarding performance and has better flame retarding performance as compared with pure polylactic acid, which means that D-ATA has a great flame-retardant effect on the polylactic acid under the condition of low addition amount.

Description

technical field [0001] The invention relates to a preparation method and application of phosphorus-containing triazole compounds, in particular to a preparation method of phosphorus-containing triazole and its application on flame-retardant polylactic acid. Background technique [0002] Polylactic acid (PLA) is polymerized from small molecular lactic acid and has the characteristics of good biocompatibility, biodegradability, high transparency, high strength, and easy processing. However, pure polylactic acid has poor heat resistance and is easy to burn. The oxygen index can only reach about 20%. The material has the requirement of high flame retardant level. Therefore, improving the flame retardancy of polylactic acid has become a hot spot in the current study of material properties. Commonly used flame retardant modifiers for polylactic acid include: halogen compounds, inorganic and nano compounds, intumescent compounds and synergistic compounds. At present, most of the...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08K5/5399C08L67/04C07F9/6574
CPCC07F9/657181C08K5/5399C08L2201/02C08L67/04
Inventor 简荣坤艾远芳夏龙庞付渠
Owner FUJIAN NORMAL UNIV
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