The present research studied benzoic acid change in water and its Raman spectra in temperature rising period using hydrothermal diamond anvil cell and Raman spectrum technique. The hydrothermal diamon danvil cell is the most useful instrument to observe sample in-situation under high temperature and high pressure. The authors can get effective results from this instrument and pursue further research. The method of Raman spectra is the most useful measure tool and it can detect the material according to the spectrum. The result showed that there was no change in characteristic vibrational Raman peak of benzoic acid in the lower temperature period and there was no reaction between benzoic acid and water. In the process of temperature rising period, the characteristic vibrational Raman peak of benzoic acid becamewe aker. During the process, benzoic acid began to dissolve in water, but no chemical reaction happened. The reason for weaker Ramanpeak of benzoic acid is the dissolution.The characteristic vibrational Raman peak of carboxyl disappeared at 150℃, which showed that decarboxylic reaction occurred on benzoic acid. But the main Raman peak of benzoic acid existed which showed that no chemical reaction existed. And then benzoic acid disappeared when temperature ascended to 170℃. When the temperature of system dropped to room temperature, a kind of crystal appeared. The characteristic vibrational Raman peak of this kind of crystal showed that the crystal contained benzene ring, showing that dutrex appeared. At the same time the authors did not find the characteristic vibrational Raman peak of carboxyl, so the crystal was not benzoic acid. The whole research showed that: dutrex can disappear and be regained in the process of dissolution and recrystallization, but carboxyl cannot.