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Reactive phosphorus-containing flame retardant and preparation method and application thereof

A flame retardant and reactive technology, applied in the field of flame retardants, can solve problems such as cumbersome process flow and complex synthesis methods of flame retardants, and achieve the effects of wide application range, excellent durability, and easy control

Active Publication Date: 2018-12-07
SICHUAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the synthesis method of the flame retardant is complex and the process is cumbersome, which limits its industrial application.

Method used

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  • Reactive phosphorus-containing flame retardant and preparation method and application thereof
  • Reactive phosphorus-containing flame retardant and preparation method and application thereof
  • Reactive phosphorus-containing flame retardant and preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] First, under the protection of nitrogen, add 0.2 mol of phosphorus oxychloride to 150 mL of tetrahydrofuran at 0~-5°C and mix well, then add 0.6 mol of triethylamine at this temperature, and then slowly add 50 mL of it dropwise within 2 hours After the dropwise addition of 0.2 mol of hydroxyethyl acrylate dissolved in tetrahydrofuran was completed, the reaction was continued at the temperature for 6 hours to obtain a solution of a single-substituted phosphorus-containing intermediate (III) containing a double bond structure. Add 0.2 mol of triethylamine to the intermediate (Ⅲ) solution obtained in the above step at room temperature, then slowly add 0.2 mol of 4,4-diaminodiphenyl ether dissolved in 60 mL of tetrahydrofuran dropwise within 2 hours, after the dropwise addition is completed Raise the temperature of the solution to 100°C and react for 8 hours. After the reaction, the liquid is removed by suction filtration, and the obtained yellow solid is washed with deioniz...

Embodiment 2

[0042] First, under the protection of nitrogen, add 0.22mol phosphorus oxychloride to 150mL acetonitrile at 0~-10℃ and mix well, then add 0.66mol pyridine at this temperature, then slowly add 50mL acetonitrile dropwise within 1.5h to dissolve 0.2mol of hydroxyethyl acrylate, after the dropwise addition, the reaction was continued at this temperature for 7 hours to obtain a solution of a single-substituted phosphorus-containing intermediate (Ⅲ) containing a double bond structure. Add 0.2 mol of pyridine to the solution of intermediate (Ⅲ) obtained in the above step at room temperature, then slowly add 0.2 mol of 4,4-diaminodiphenylmethane dissolved in 60 mL of acetonitrile dropwise within 2 hours, and dissolve the solution after the dropwise addition The temperature is raised to 90°C and reacted for 7 hours. After the reaction, the liquid is removed by suction filtration, and the obtained yellow solid is washed with deionized water for 3 to 4 times. After drying, the reactive ph...

Embodiment 3

[0044] First, under the protection of nitrogen, add 0.2 mol of phosphorus oxychloride to 150 mL of tetrahydrofuran at 0~-5°C and mix well, then add 0.7 mol of triethylamine at this temperature, and then slowly add 50 mL of it dropwise within 2 hours After the dropwise addition of 0.2 mol of hydroxyethyl acrylate dissolved in tetrahydrofuran was completed, the reaction was continued at the temperature for 6 hours to obtain a solution of a single-substituted phosphorus-containing intermediate (III) containing a double bond structure. Add 0.2 mol of triethylamine to the intermediate (Ⅲ) solution obtained in the above steps at room temperature, then slowly add 0.2 mol of 4,4-diaminodiphenyl ether dissolved in 60 mL of tetrahydrofuran dropwise within 2 hours, The temperature of the solution is raised to 85°C and reacted for 8 hours. After the reaction, the liquid is removed by suction filtration, and the obtained yellow solid is washed with deionized water for 3 to 4 times. After dr...

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Abstract

The invention provides a reactive phosphorus-containing flame retardant. The flame retardant contains unsaturated double bonds and can react with polymer, and phosphate and phosphamide structural units are further introduced based on the structure with the unsaturated double bonds. After the obtained flame retardant is applied to unsaturated polyester resin, the highest level of vertical burning UL-94 reaches the level of V-1-V-0, the maximum value of the limit oxygen index LOI is 33.0%, and the peak of heat release rate (PHRR) and total heat release (THR) in cone calorimetry tests are lower than the PHRR and THR of pure unsaturated polyester; after the obtained flame retardant is applied to unsaturated polyester glass fiber composite materials, the highest level of vertical burning UL-94reaches the level of V-1-V-0, and the maximum value of the limit oxygen index LOI is 40%. The reactive phosphorus-containing flame retardant has good flame retardancy and little influences on the mechanical properties of the materials. The invention also provides a preparation method of the flame retardant. The preparation method of the flame retardant is simple, and has mild conditions and easy control.

Description

technical field [0001] The invention belongs to the field of flame retardants, in particular to a reactive phosphorus-containing flame retardant and its preparation [0002] preparation methods and applications. Background technique [0003] Polymer materials are widely used in aerospace, household appliances, electronic information, and construction fields due to their many advantages such as abundant sources, easy processing, superior performance, and low price. However, most polymer materials are flammable materials, which are easy to cause fire and cause heavy losses to human life and property. Therefore, how to reduce the combustion performance of polymer materials has become a technical and social issue that people pay more and more attention to. At present, adding flame retardants to modify them is one of the important ways to endow these polymer materials with excellent flame retardancy, which also provides a broad market for the research and development of flame r...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08K5/5399C08K5/5398C08G79/04C08L67/06C08L85/02
CPCC08G79/04C08K5/5398C08K5/5399C08L67/06C08L2201/02C08L85/02
Inventor 王玉忠曹媛张文强尹学武史月全汪秀丽
Owner SICHUAN UNIV
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