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 substances

The boiling points of related substances in intermediates in TATB wastewater are all higher than 300K, and it is generally difficult to regasify in the column, and the products after derivatization treatment are difficult to extract from wastewater, so gas chromatography and GC-MS are also not applicable

[0013] Due to the wide variety of TATB wastewater and complex matrix, the physical and chemical properties of each component are quite different, especially the nitrification wastewater is strongly acidic, with a pH far below 1, which will damage the pipeline of the chromatographic mass spectrometer, and it is not suitable for direct sample injection.

The content of intermediate-related substances in TATB wastewater is relatively low, especially for alkylation wastewater and amination wastewater, in which intermediate-related substances need to be enriched and treated; the solvent of alkylation wastewater and amination wastewater is mainly ethanol, because Ethanol is miscible with most organic solvents, and it cannot be enriched by liquid-liquid extraction; try solid-phase extraction, and the chromatographic behavior is poor

The various detection methods cannot detect trace intermediate related substances in TATB wastewater, therefore, there is currently no effective method that can detect trace intermediate related substances in TATB wastewater

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