Method for determining synthesized intermediate and product in wastewater in TATB production by liquid chromatogram

Abstract

The invention relates to a method for determining synthesized intermediate and product in wastewater in TATB production by liquid chromatogram, belonging to the technical field of chemical analysis. The method comprises the following steps: firstly, preparing standard solutions of phloroglucinol, TETNB and TATB standard substances by using liquid phase chromatogram mobile phase; secondly, treating the TATB wastewater, regulating pH to be neutral, extracting to-be-detected substance, drying the to-be-detected substance, adding the liquid phase chromatogram mobile phase for dissolving, filtering through a microfiltration membrane to remove impurity to obtain a liquid phase chromatogram detection sample; thirdly, performing liquid phase chromatographic analysis on the standard solutions, and drawing a standard curve; and fourthly, respectively analyzing the samples by using the liquid phase chromatogram, comparing the analysis result with the standard curve to determine the intermediate and the product in the TATB wastewater. Trace amount of intermediate related substances, such as phloroglucinol, TETNB and the product, namely TATB in the TATB wastewater can be accurately detected by using the method disclosed by the invention, and the defects in the prior art are filled.

Description

technical field [0001] The present invention relates to a method for the determination of triaminotrinitrobenzene (TATB) synthetic intermediates and products in waste water by liquid chromatography, in particular, to a liquid chromatography method for the determination of three types of waste water produced in the TATB production process. The methods of phloroglucinol, 1,3,5-trimethoxy-2,4,6-trinitrobenzene (TETNB) and TATB belong to the field of chemical analysis. Background technique [0002] The chlorine content of triaminotrinitrobenzene (TATB) can obviously affect the thermal stability of TATB, in order to solve the influence of chlorine impurity in the traditional production TATB method, generally adopt in the prior art with phloroglucinol as raw material, through nitration , alkylation and amination to produce chlorine-free TATB, but the production process has brought unavoidable environmental problems——waste water, which is mainly nitrification waste water, alkylatio...

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Problems solved by technology

[0002] The chlorine content of triaminotrinitrobenzene (TATB) can obviously affect the thermal stability of TATB, in order to solve the influence of chlorine impurity in the traditional production TATB method, generally adopt in the prior art with phloroglucinol as raw material, through nitration , alkylation and amination to produce chlorine-free TATB, but the production process has brought unavoidable environmental problems——waste water, which is mainly nitrification waste water, alkylation waste water and amination waste water

Ultraviolet spectrophotometry is a relatively classic method, but its sensitivity is not high. Because the related substances of intermediates in TATB wastewater have extremely similar absorption peaks, it is easy to cause interference, which is not conducive to the simultaneous analysis of multi-component intermediates.

Thin-layer chromatography has high sensitivity and good selectivity, but poor repeatability and cumbersome detection steps

The reagents used in the permanent stop titration method are highly toxic and the technology is difficult to master, and what is measured is the total amount of organic matter in TATB wastewater. It cannot distinguish the types of intermediate-related substances in TATB wastewater, and is not suitable for multi-component intermediates in TATB wastewater. Analysis of related substanc

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