A kind of high-efficiency flame retardant and preparation method thereof
A flame retardant and high-efficiency technology, applied in the field of high-efficiency flame retardants and their preparation, can solve problems such as influence and unfavorable material properties, and achieve the effects of good chemical stability, improved mechanical properties, and good flame retardant effect.
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Embodiment 1
[0028] The synthesis steps of an efficient flame retardant are:
[0029] (1) Heat 11.1g of tris(4-aminophenyl) phosphate and 16.0g of 4-trimethylsilylbenzaldehyde in 217.2g of ethanol at 80°C for 5h. After the reaction is over, the intermediate product I is obtained. The reaction system;
[0030] (2) Add 19.5 g of DOPO to the reaction system containing intermediate product I obtained in step (1) and heat it at 80°C for 4 hours. After the reaction, wash and dry to obtain a high-efficiency flame retardant with a yield of 85.9% .
[0031] The infrared test results are as follows:
[0032] FTIR (KBr): N-H stretching vibration peak 3405cm -1 , C-H stretching vibration peak 3070cm -1 , C-N characteristic peak 1288cm -1 , C-Si characteristic peak 1255cm -1 ,, P-O-C characteristic peak 1032cm -1 , P-O-Ph characteristic peak 1231cm -1 , P-Ph characteristic peak 1595cm -1 , P=O characteristic peak 1212cm -1 , The out-of-plane bending vibration peak of aromatic hydrogen 900cm -1 .
[0033] NMR s...
Embodiment 2
[0036] The synthesis steps of an efficient flame retardant are:
[0037] (1) Heat 18.6g of tris(4-aminophenyl) phosphate and 26.7g of 4-trimethylsilylbenzaldehyde in 544g of DMF at 80°C for 7h. After the reaction is over, the intermediate product I is obtained. reaction system;
[0038] (2) Add 32.4 g of DOPO to the reaction system containing intermediate product I obtained in step (1) and heat it at 80°C for 6 hours. After the reaction, wash and dry to obtain a high-efficiency flame retardant with a yield of 86.2% .
[0039] The infrared test results are as follows:
[0040] FTIR (KBr): N-H stretching vibration peak 3405cm -1 , C-H stretching vibration peak 3060cm -1 , C-N characteristic peak 1287cm -1 , C-Si characteristic peak 1255cm -1 ,, P-O-C characteristic peak 1033cm -1 , P-O-Ph characteristic peak 1231cm -1 , P-Ph characteristic peak 1595cm -1 , P=O characteristic peak 1213cm -1 , The out-of-plane bending vibration peak of aromatic hydrogen is 850cm -1 .
Embodiment 3
[0042] The synthesis steps of an efficient flame retardant are:
[0043] (1) Heat 37.1g of tris(4-aminophenyl) phosphate and 53.5g of 4-trimethylsilylbenzaldehyde in 1268g of DMSO at 80°C for 9h. After the reaction is over, the intermediate product I is obtained. reaction system;
[0044] (2) Add 64.9 g of DOPO to the reaction system containing intermediate product I obtained in step (1) and heat it at 80°C for 8 hours. After the reaction, wash and dry to obtain a high-efficiency flame retardant with a yield of 86.6% .
[0045] The infrared test results are as follows:
[0046] FTIR (KBr): N-H stretching vibration peak 3410cm -1 , C-H stretching vibration peak 3060cm -1 , C-N characteristic peak 1287cm -1 , C-Si characteristic peak 1254cm -1 ,, P-O-C characteristic peak 1033cm -1 , P-O-Ph characteristic peak 1231cm -1 , P-Ph characteristic peak 1595cm -1 , P=O characteristic peak 1213cm -1 , The out-of-plane bending vibration peak of aromatic hydrogen is 800cm -1 .
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