Method for analyzing mother liquor of N-(phosphonomethyl) iminodiacetic acid (PMIDA)

A kind of technology of bisphosphonate mother and analytical method, applied in the field of chemical analysis

Inactive Publication Date: 2011-04-27
CHONGQING UNISPLENDOUR CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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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 iminodiacetic acid content 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 the solution, mainly use lead nitrate standard solution for complexometric titration, with pH 9.0 buffer solution and arsenazo as indicators 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, in the prior art, use nitrogen determination method to measure nitrilotriacetic acid content, but nitrogen-containing compound is more in the mother liquor, interferes Large, there is also an acid-base complexometric titration method, 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 titrate with alkali standard solution. There are also chromazurin S-hexadecyltrimethylammonium bromide as an indicator, titrated with copper nitrate standard solution at pH = 6, but the composition of diglyphosate is complex, and the nitrilotriacetic acid and bisphosphonate contained in the mother liquor Glyphosate has complexation property, which interferes with complexometric titration, and nitrilotriacetic acid is also acidic, and is a polyacid, which, like other acidic substances in the mother liquor, can react with alkali, so the determination of nitrilotriacetic acid is carried out by the above chemical analysis method. The content of acetic acid will be interfered by other substances in the mother liquor, making the measurement 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

Method used

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  • Method for analyzing mother liquor of N-(phosphonomethyl) iminodiacetic acid (PMIDA)
  • Method for analyzing mother liquor of N-(phosphonomethyl) iminodiacetic acid (PMIDA)
  • Method for analyzing mother liquor of N-(phosphonomethyl) iminodiacetic acid (PMIDA)

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Instrument: Shimadzu high performance liquid chromatography (with UV detector)

[0028] Chromatographic column: DIKMA ODS-3, 250×4.5mm, 5μm

[0029] Mobile phase: 0.1% KH 2 PO 4 , with H 3 PO 3 Adjust pH=2.0

[0030] Flow rate: 0.8mL / min

[0031] UV: 195nm

[0032] Injection volume: 20μL

[0033] Determination of standard solution:

[0034] Take nitrilotriacetic acid (AR, the purchased nitrilotriacetic acid sample has a purity of 98%) as the reference substance, weigh 0.1155g into a 50mL volumetric flask, add water to dissolve and dilute to the mark, shake well, and accurately draw 1mL of the solution in the In a 100mL volumetric flask, add mobile phase to dilute to the mark, shake well, filter through a microporous membrane, and inject the sample. The peak area of ​​nitrilotriacetic acid is 67886.

[0035] Sample determination:

[0036] Accurately draw 5mL of the mother solution into a 50mL volumetric flask, add mobile phase to dilute to the mark, shake wel...

Embodiment 2

[0057] Instrument: Shimadzu high performance liquid chromatography (with UV detector)

[0058] Chromatographic column: InertsilODS-4, 250×4.5mm, 5μm

[0059] Mobile phase: 0.15%H 3 PO 4 Aqueous solution, pH=3.0

[0060] Flow rate: 0.6mL / min

[0061] UV: 195nm

[0062] Injection volume: 20μL

[0063] Determination of standard solution:

[0064] Take nitrilotriacetic acid (AR, the purchased nitrilotriacetic acid sample has a purity of 98%) as the reference substance, weigh 0.1000g into a 50mL volumetric flask, add water to dissolve and dilute to the mark, shake well, and accurately draw 1mL of the solution in the In a 100mL volumetric flask, add mobile phase to dilute to the mark, shake well, filter through a microporous membrane, and inject the sample. The peak area of ​​nitrilotriacetic acid is 66428.

[0065] Sample determination:

[0066] Accurately draw 5mL of the mother solution into a 50mL volumetric flask, add mobile phase to dilute to the mark, shake well, pre...

Embodiment 3

[0071] Instrument: Shimadzu high performance liquid chromatography (with UV detector)

[0072] Chromatographic column: DIKMA ODS-3, 250×4.5mm, 5μm

[0073] Mobile phase: 0.2% KH 2 PO 4 , with H 3 PO 4 Adjust pH=2.0

[0074] Flow rate: 1.5mL / min

[0075] UV: 195nm

[0076] Injection volume: 20μL

[0077] Determination of standard solution:

[0078] Take nitrilotriacetic acid (AR, the purchased nitrilotriacetic acid sample has a purity of 98%) as the reference substance, weigh 0.1155g into a 50mL volumetric flask, add water to dissolve and dilute to the mark, shake well, and accurately draw 1mL of the solution in the In a 100mL volumetric flask, add mobile phase to dilute to the mark, shake well, filter through a microporous membrane, and inject the sample. The peak area of ​​nitrilotriacetic acid is 66101.

[0079] Sample determination:

[0080] Accurately draw 5mL of the mother solution into a 50mL volumetric flask, add mobile phase to dilute to the mark, shake wel...

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Abstract

The invention relates to a method for analyzing a mother liquor of N-(phosphonomethyl)iminodiacetic acid (PMIDA), in particular to a method for analyzing the mother liquor generated during producing the PMIDA by taking iminodiacetonitrile as a raw material. The method comprises the steps of independently measuring contents of PMIDA, nitrilotriacetic acid and iminodiacetic acid in the mother liquor and measuring polybasic acids such as PMIDA, phosphoric acid, phosphorous acid and the like step by step, strengthening the weak acid by adding calcium chloride to release inactive hydrogen quantificationally and measuring the phosphoric acid, the nitrilotriacetic acid and the PMIDA and skillfully measuring the contents of the iminodiacetic acid, the PMIDA, the nitrilotriacetic acid, the phosphorous acid, hydrochloric acid and the phosphoric acid in the mother liquor of PMIDA according to the reaction law and interrelation of substances. The verification shows that the method v is accurate, comprehensive, scientific and reasonable, is simple to operate and provides reliable ground for recycling and comprehensively utilizing the mother liquor of PMIDA and has good application 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) 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 types of her...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N21/31G01N21/79
Inventor 胡欣罗延谷曹强董远萍
Owner CHONGQING UNISPLENDOUR CHEM
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