Study On The Synthesis Of Isooctyl Phosphates And Hydrolysis Kinetics Of Pyrophosphates

Nowadays, the spinning process of synthetic fiber is facing the transition from low to high speed and temperature, the change also sets higher demands for antistatic agent. Phosphates as a kind of antistatic agents has good solubility, thermal stability and acid-and-alkali-resistant ability, it can satisfy the requirements of the high speed spinning process, and the preparation is relatively simple and low cost.Isooctyl phosphate potassium salt, a kind of antistatic agents was synthesized by phosphating reaction of 2-ethylhexanol with phosphorus pentoxide in this thesis. The influence of different factors such as mole feed ratio, reaction temperature and time on the composition and performance of the outputs was discussed. Thus, the optimum synthesizing conditions were obtained, namely mole feed ratio 3 to 1, reaction temperature 70℃, and reaction time 4 hours. The influence of pyrophosphate on the analysis method and performance of product was also discussed, and hydrolysis is needed to transform pyrophosphates to phosphates.31P-NMR is used as a qualitative and quantitative analysis method for pyrophosphates. The analysis temperature was 27℃, analysis concentration was 0.05g P/0.5 mL DMSO. The chemical shifts of pyrophosphoric acid, pyrophosphate mono-ester, pyrophosphate di-ester were distinguished in 31P-NMR spectra. According to the research, the peak area could be used to quantitatively analyze the composition of the pyrophosphate, and the relative deviation is small. The range of applications of 31P-NMR in phosphate was extended.The kinetic study of the hydrolysis of butyl pyrophosphates was discussed in this paper. For practical reasons, power function model was adopted. Parameters of the proposed model equation were calculated by integration method combined with fourth order Runge-Kutta method and least square method. Finally, reaction order, apparent activation energies and pre-exponential factors of the hydrolysis reaction were obtained. The kinetic model was then verified by the comparison between experimental data and calculated one.The hydrolysis of isooctyl pyrophosphates,2-butoxyethyl pyrophosphates and 2-(2-butoxyethoxy)ethyl pyrophosphates was also studied. Using Gaussian, the optimized geometric configuration and charge distribution of pyrophosphates were obtained. Based on experimental results, the variation of the hydrolysis rate of different pyrophosphates was explained reasonably.