A novel preparation method of phosphorus pentafluoride（PF5） is introduced in details in the article. Phosphorus pentafluoride is mainly used to synthesize lithium ion battery electrolyte salt. In the experiment mesn...A novel preparation method of phosphorus pentafluoride（PF5） is introduced in details in the article. Phosphorus pentafluoride is mainly used to synthesize lithium ion battery electrolyte salt. In the experiment mesneproduct- hexafluorophosphoric acid（HPF6） was firstly prepared-from phosphorus pentoxide（P2O5） and anhydrous hydrogen fluoride（HF）, according to the chemical stoichiometrics, the optimum amount of excess HF used was about 60% and the optimum reaction time was 4 h; then HPF6 was dehydrated by oleum with an excess amount of 35%-- 40% which was heated for 40--50 min at 150 ℃; thus HPF6 was decomposed to a mixture of gases containing PF5; impurity gases were removed through condensation in the presence of cooling water at 0 ℃, then PF5 of high purity was eventually prepared. The production was characterized by inffared（IR） spectrometry and gas chromatography-mass spectroscopy-selected ion monitoring（GC-MS-SIM）. Eventual results indicate that PF5 prepared by the novel method has a high target purity and a low amount of impurity and water.展开更多
In this paper a modified two-step procedure for synthesis of N-（1-naphthyl） suecinimide （NaS） was developed, and the molecular structure of NaS was properly characterized by XRD, FT-IR, 1H NMR, DSC, etc. The resul...In this paper a modified two-step procedure for synthesis of N-（1-naphthyl） suecinimide （NaS） was developed, and the molecular structure of NaS was properly characterized by XRD, FT-IR, 1H NMR, DSC, etc. The results show that the melting point of our product is 159 ℃-160.5 ℃, and the characteristic infrared absorption band of carbonyl group splits into two peaks （1705cm^-3/1779cm^-3）, which are found to be quite different from the documented data （rap 147℃ -149℃; IR C=0-1700cm^-3）. Besides, photophysical spectroscopy was found to be powerful to study the molecular structure and crystal morphology of NaS compound.展开更多
基金Supported by the National Basic Research Program of China(No.2007CB613607)
文摘A novel preparation method of phosphorus pentafluoride（PF5） is introduced in details in the article. Phosphorus pentafluoride is mainly used to synthesize lithium ion battery electrolyte salt. In the experiment mesneproduct- hexafluorophosphoric acid（HPF6） was firstly prepared-from phosphorus pentoxide（P2O5） and anhydrous hydrogen fluoride（HF）, according to the chemical stoichiometrics, the optimum amount of excess HF used was about 60% and the optimum reaction time was 4 h; then HPF6 was dehydrated by oleum with an excess amount of 35%-- 40% which was heated for 40--50 min at 150 ℃; thus HPF6 was decomposed to a mixture of gases containing PF5; impurity gases were removed through condensation in the presence of cooling water at 0 ℃, then PF5 of high purity was eventually prepared. The production was characterized by inffared（IR） spectrometry and gas chromatography-mass spectroscopy-selected ion monitoring（GC-MS-SIM）. Eventual results indicate that PF5 prepared by the novel method has a high target purity and a low amount of impurity and water.
基金Natural Science Foundation of China (50273014, 29928003)Natural Science Foundation of Tianjin (03380261).
文摘In this paper a modified two-step procedure for synthesis of N-（1-naphthyl） suecinimide （NaS） was developed, and the molecular structure of NaS was properly characterized by XRD, FT-IR, 1H NMR, DSC, etc. The results show that the melting point of our product is 159 ℃-160.5 ℃, and the characteristic infrared absorption band of carbonyl group splits into two peaks （1705cm^-3/1779cm^-3）, which are found to be quite different from the documented data （rap 147℃ -149℃; IR C=0-1700cm^-3）. Besides, photophysical spectroscopy was found to be powerful to study the molecular structure and crystal morphology of NaS compound.
