A kind of fluorine-based dopo derivative flame retardant and preparation method thereof
A technology of derivatives and flame retardants, applied in the field of fluorine-based DOPO derivative flame retardants and their preparation, can solve problems such as adverse material properties and influence, and achieve the effects of low cost, simple process and easy availability of raw materials
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Embodiment 1
[0030] A kind of synthetic steps of fluorine-based DOPO derivative flame retardant is:
[0031] (1) Heat 19.3g of aminodimethylpentafluorophenylsilane and 8.2g of 2,3,5,6-tetrafluoro-p-benzaldehyde in 137g of ethanol at 70°C for 6h. The reaction system of intermediate product I;
[0032] (2) 17.3g of DOPO was added to the reaction system containing intermediate product I obtained in step (1) and heated at 70° C. for 4 h. After the reaction was finished, it was washed and dried to obtain a fluorine-based DOPO derivative flame retardant. Yield 87.4%.
[0033] The infrared test results are as follows:
[0034] FTIR (KBr): N-H stretching vibration peak 3410cm -1 , C-H stretching vibration peak 3085cm -1 , C-N characteristic peak 1288cm -1 , C-F characteristic peak 1100cm -1 , C-Si characteristic peak 1255cm -1 , P-O-C characteristic peak 1035cm -1 , P-O-Ph characteristic peak 1230cm -1 , P-Ph characteristic peak 1595cm -1 , P=O characteristic peak 1212cm -1 , the out-of...
Embodiment 2
[0038] A kind of synthetic steps of fluorine-based DOPO derivative flame retardant is:
[0039] (1) 28.9g of aminodimethylpentafluorophenylsilane and 12.3g of 2,3,5,6-tetrafluoro-p-benzaldehyde were heated in 330g of DMF at 70°C for 8h. After the reaction, the mixture containing The reaction system of intermediate product I;
[0040] (2) 25.9g of DOPO is added to the reaction system containing intermediate product I obtained in step (1) and heated at 70°C for 6h. After the reaction is finished, it is washed and dried to obtain a fluorine-based DOPO derivative flame retardant. Yield 86.9%.
[0041] The infrared test results are as follows:
[0042] FTIR (KBr): N-H stretching vibration peak 3415cm -1 , C-H stretching vibration peak 3070cm -1 , C-N characteristic peak 1286cm -1 , C-F characteristic peak 1100cm -1 , C-Si characteristic peak 1253cm -1 , P-O-C characteristic peak 1035cm -1 , P-O-Ph characteristic peak 1230cm -1 , P-Ph characteristic peak 1595cm -1 , P=O ch...
Embodiment 3
[0044] A kind of synthetic steps of fluorine-based DOPO derivative flame retardant is:
[0045] (1) 38.6g of aminodimethylpentafluorophenylsilane and 16.5g of 2,3,5,6-tetrafluoro-p-benzaldehyde were heated in 550.6g of DMSO at 70°C for 10h. After the reaction, Containing the reaction system of intermediate product I;
[0046] (2) 34.6g of DOPO was added to the reaction system containing intermediate product I obtained in step (1) and heated at 70°C for 8h. After the reaction was finished, it was washed and dried to obtain a fluorine-based DOPO derivative flame retardant. Yield 87.6%.
[0047] The infrared test results are as follows:
[0048] FTIR (KBr): N-H stretching vibration peak 3410cm -1 , C-H stretching vibration peak 3060cm -1 , C-N characteristic peak 1285cm -1 , C-F characteristic peak 1100cm -1 , C-Si characteristic peak 1252cm -1 , P-O-C characteristic peak 1030cm -1 , P-O-Ph characteristic peak 1230cm -1 , P-Ph characteristic peak 1595cm -1 , P=O charact...
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