A kind of silicon-containing dopo derivative flame retardant and preparation method thereof
A technology of derivatives and flame retardants, which is applied in the field of silicon-containing DOPO derivatives flame retardants and its preparation, can solve the problems of impact and unfavorable material properties, and achieve the effects of simple process, low cost and good thermal stability
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Embodiment 1
[0030] A kind of synthetic steps of silicon-containing DOPO derivative flame retardant is:
[0031] (1) Heat 7.2g of aminodimethylpentafluorophenylsilane and 4.3g of 3,5-difluoropyridine-4-carbaldehyde in 80.4g of ethanol at 75°C for 6h. After the reaction, an intermediate product containing The reaction system of I;
[0032] (2) Add 6.5g of DOPO to the reaction system containing intermediate product I obtained in step (1) and heat at 75° C. for 4 hours. After the reaction, wash and dry to obtain a silicon-containing DOPO derivative flame retardant , yield 85.5%.
[0033] The infrared test results are as follows:
[0034] FTIR (KBr): N-H stretching vibration peak 3415cm -1 , C-H stretching vibration peak 3080cm -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 1231cm -1 , P-Ph characteristic peak 1595cm -1 , P=O characteristic peak 1212cm ...
Embodiment 2
[0038] A kind of synthetic steps of silicon-containing DOPO derivative flame retardant is:
[0039] (1) Heat 12.1g of aminodimethylpentafluorophenylsilane and 7.2g of 3,5-difluoropyridine-4-carbaldehyde in 192.5g of DMF at 75°C for 7h. After the reaction, an intermediate product containing The reaction system of I;
[0040] (2) Add 10.8g of DOPO to the reaction system containing the intermediate product I obtained in step (1) and heat at 75°C for 5h. After the reaction, wash and dry to obtain a silicon-containing DOPO derivative flame retardant , yield 84.9%.
[0041] The infrared test results are as follows:
[0042] FTIR (KBr): N-H stretching vibration peak 3410cm -1 , C-H stretching vibration peak 3070cm -1 , C-N characteristic peak 1288cm -1 , C-F characteristic peak 1100cm -1 , C-Si characteristic peak 1250cm -1 , P-O-C characteristic peak 1035cm -1 , P-O-Ph characteristic peak 1231cm -1 , P-Ph characteristic peak 1595cm -1 , P=O characteristic peak 1212cm -1 ,...
Embodiment 3
[0044] A kind of synthetic steps of silicon-containing DOPO derivative flame retardant is:
[0045] (1) 24.1g of aminodimethylpentafluorophenylsilane and 14.3g of 3,5-difluoropyridine-4-carbaldehyde were heated in 538g of DMSO at 75°C for 8h. After the reaction, intermediate product I was obtained. reaction system;
[0046] (2) Add 21.6g of DOPO to the reaction system containing intermediate product I obtained in step (1) and heat at 75°C for 6h. After the reaction is finished, wash and dry to obtain a silicon-containing DOPO derivative flame retardant , yield 86.1%.
[0047] The infrared test results are as follows:
[0048] FTIR (KBr): N-H stretching vibration peak 3415cm -1 , C-H stretching vibration peak 3075cm -1 , C-N characteristic peak 1288cm -1 , C-F characteristic peak 1100cm -1 , C-Si characteristic peak 1255cm -1 , P-O-C characteristic peak 1038cm -1 , P-O-Ph characteristic peak 1231cm -1 , P-Ph characteristic peak 1595cm -1 , P=O characteristic peak 1214...
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