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Study on Synthesis and Reaction Kinetics of Diphenyl Phosphorazidate by Phase Transfer Catalysis

Author: LiLei
Tutor: ZhaoJianHong
School: Zhengzhou University
Course: Chemical processes
Keywords: Azide diphenyl phosphate Phase Transfer Catalysis Synthesis Reaction kinetics
CLC: TQ203.2
Type: Master's thesis
Year: 2008
Downloads: 28
Quote: 0
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Abstract


Azide diphenyl phosphate (DPPA) as a colorless non-explosive oily liquid, is an important organic phosphorus reagent because it has a higher reaction activity, is widely used in the synthesis of organic compounds and drugs. There are poor product quality, after the process is complex, higher costs due to the current the DPPA production process (solvent), the research process is simple, mild conditions, post-processing is simple, good quality products, low-cost the DPPA synthesis of new process to become necessary. The chlorinated diphenyl phosphate (DPCP) and sodium azide as a raw material, carried out a detailed study of the phase transfer catalytic synthesis of DPPA process, the main contents include: the establishment of the of product qualitative and quantitative analysis methods, phase transfer catalyst selection phase transfer catalytic synthesis optimization of process conditions and apparent kinetic studies. The research results have certain the academic theoretical significance and better prospects for industrial applications. Phase transfer catalysis system by DPCP and sodium azide as raw material analysis method rarely reported, seeking a reliable method of analysis DPPA content through the synthesis process is of great significance. In this paper, the phase transfer catalyst synthesis DPPA background, the choice of C 18 (150 mm x 4.6 mm id) column, V (methanol): V (water) = 70:30 as mobile phase, established a way to quickly and accurate determination of the DPPA content. The effects of different catalysts, different stirring rates and different feeding methods impact on the synthesis reaction, the the DPCP synthesis DPPA preferred phase transfer catalyst is tetraethyl ammonium bromide, and a preferred stirring rate of 1700 r / min. Optimum conditions based on the use of orthogonal experimental design and fine single factor experiments: the use of refined DPCP; reaction time 13 h; catalyst amount of tetraethyl ammonium bromide 4.4 wt.%; Sodium azide and of DPCP the feed molar ratio 1.9:1; reaction temperature of 35 ° C. 4 repeats the process conditions under the experimental results show that the product yield above 88%, the content is stable at more than 96%. Study phase transfer catalyst presence of tetraethyl ammonium bromide, obtained by DPCP, sodium azide synthetic DPPA apparent kinetic reaction is a reaction, reaction apparent activation energy Ea = 5.086 kJ / mol The pre-exponential factor A = 1.256 h the -1 . 35 ℃ under optimum conditions when any reaction time raw DPCP conversion rate calculated by the kinetic equation, the maximum relative deviation of the calculated and experimental values ​​of less than 10%, indicating that the resulting kinetic equation can be better used in guidance the DPPA synthesis process.

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CLC: > Industrial Technology > Chemical Industry > Basic Organic Chemistry Industry > General issues > Chemical reaction process > Catalytic process
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