Method for analyzing components of mother solution of glyphosine

Abstract

The invention discloses a method for analyzing components of mother solution of glyphosine, in particular a method for analyzing the components of mother solution generated by preparing the glyphosine from iminodiacetonitrile serving as a main raw material. In the method, the contents of N-(phosphonomethyl) iminodiacetic acid, nitrilotriacetic acid and iminodiacetic acid in the mother solution are independently measured, and polyacids such as the N-(phosphonomethyl) iminodiacetic acid, phosphoric acid, phosphorous acid and the like are measured stepwise; meanwhile, calcium chloride is added to strengthen weak acid, quantitative inactive hydrogen is released, and the phosphoric acid, nitrilotriacetic acid and the N-(phosphonomethyl) iminodiacetic acid are measured; and according to reaction rules and interrelation of substances, the contents of the iminodiacetic acid, the N-(phosphonomethyl) iminodiacetic acid, the nitrilotriacetic acid, the phosphorous acid, hydrochloric acid and the phosphoric acid are skillfully measured. Through verification, the method is accurate, comprehensive, scientific, reasonable, and easy to operate, provides a reliable basis for recycling and comprehensively utilizing the mother solution of the glyphosine, and has high promotion value.

Description

technical field [0001] The invention relates to a method for analyzing the components of diglyphosate mother liquor, in particular to a method for analyzing the components of mother liquor produced when diglyphosate is produced by using iminodiacetonitrile as the main raw material, and belongs to the field of chemical analysis. Background technique [0002] Diglyphosate (N-(phosphomethyl)iminodiacetic acid) [0003] It is an intermediate for the production of glyphosate (N-phosphonomethylglycine) from iminodiacetonitrile (IDA method). Glyphosate is a widely used organic phosphine herbicide, which has the characteristics of high efficiency, broad spectrum, low toxicity and safety, and is very effective in the control of perennial deep-rooted weeds. In recent years, due to the large-scale promotion of glyphosate-resistant genetically modified crops, making its use more convenient, the market demand for glyphosate has grown rapidly, and it has continuously replaced other typ...

AI Technical Summary

Problems solved by technology

However, it is very difficult to deal with diglyphosate mother liquor in production at present, the main reason is that the composition of the mother liquor is relatively complex, and there are no relevant reports on the comprehensive analysis of diglyphosate mother liquor, and the actual analysis of many components of diglyphosate mother liquor has not yet established analytical methods

At present, the determination of the content of iminodiacetic acid of a single component in the solution mainly adopts the acid-base titration method using methyl red as an indicator; the determination of the content of phosphorous acid, phosphoric acid and hydrochloric acid of a single component in the solution mainly adopts conventional methods Acid-base titration, directly titrate with alkali standard solution; for the determination of the content of diglyphosate in a single component in the solution, mainly use a buffer solution with a pH of 9.0, arsenazo (Ⅲ) as an indicator, and lead nitrate standard solution Complexometric titration; Mainly adopt sodium sulfite addition method etc. to the mensuration of formaldehyde content in the solution; To the mensuration of the nitrilotriacetic acid of single component, use nitrogen determination method to measure nitrilotriacetic acid content in the prior art, but in the mother liquor, nitrogen-containing compound is more There are many, large interference, and acid-base complexometric titration is also useful, that is, after dissolving nitrilotriacetic acid with alkali, adjust it with acid-base until methyl red just turns yellow, add zinc nitrate solution to form a complex to precipitate acid, and use alkali standard For solution titration, chrome azure S-hexadecyltrimethylammonium bromide is also used as an indicator, and copper nitrate standard solution is used for titration at pH = 6, but the composition of diglyphosate is complex, and the ammonia trimethylammonium contained in the mother liquor Both acetic acid and bisglyphosate have complexation properties, and there is interference with complexometric titration. Nitrilotriacetic acid is also acidic at the same time. It is a polyacid. Like other acidic substances in the mother liquor, it can react with alkali. Therefore, the above chemical analysis method The determination of nitrilotriacetic acid content will be interfered by other substances in the mother liquor, making the determination results inaccurate

Mo Qingkui's "Content Determination of Hydrochloric Acid and Phosphorous Acid in the Recovery Solution of Diglyphosate Production" is used to determine the content of hydrochloric acid and phosphorous acid in the distilled liquid of the synthesis reaction of diglyphosate. The distilled liquid has simple components, mainly containing hydrochloric acid, Phosphorous acid and formaldehyde, while the composition of the mother liquor is complex, the properties of several components have similarities, the analysis is difficult, and there is no relevant literature report

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