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Citation: ZHANG Jin-Shu, CHENG Bo-Wen, REN Yuan-Lin. Synthesis and Characterization of 1,4-Di(O,O-diethyl thiophosphoryl imine) benzene[J]. Chinese Journal of Applied Chemistry, ;2007, 24(7): 832-834. shu

Synthesis and Characterization of 1,4-Di(O,O-diethyl thiophosphoryl imine) benzene

1.
Tianjin Municipal Key Laboratory of Fiber Modification and Functional Fiber, Tianjin Polytechnic University, Tianjin 300160

Corresponding author: REN Yuan-Lin,
Received Date: 18 August 2006
Available Online: 10 November 2006

Diethylthiophosphoryl chloride (A) was synthesized by reacting phosphorus thiochloride with anhydrous alcohol in the presence of NaOH,and then a novel phosphorus-nitrogen-and sulfur-containing flame retardant,1,4-di(O,O-diethyl thiophosphoryl imine) benzene (B),was synthesized via the reaction of diethylthiophosphoryl chloride with p-phenylenediamine.Compound B was characterized by elemental analysis,IR,¹H NMR and MS.The thermal properties of compound B were researched based on TG and DSC curves,and the influence factors such as the solvent and catalyst on the reaction rate and the yield of compound B were also studied.The thermal property studies indicate that the mass loss of compound B was 54.39% at 242.2~750℃,and when the temperature was 1 000℃,there was 25.11% char residue left,which showed that the title compound has a good thermal stability and char forming capability.Using acetonitrile as the solvent instead of trichloromethane or 1,2-dichloethane gave higher yield.During the synthesis,the yield was very low when triethylamine was used as acid acceptor alone,and when a little amount of 4-dimethylaminopyridine (DMAP) was added at the same time,the yield could be 81%.
- fire retardant,
- phosphorus thiochloride,
- di(O,O-diethyl thiophosphoryl imine) benzene,
- synthesis
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