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Method for analyzing components in N-Phosphonomethyl aminodiacetic acid (PMIDA) mother solution

A technology for the analysis of diglyphosate mother liquor, which is applied in the field of chemical analysis, and can solve the problems of comprehensive analysis of diglyphosate mother liquor, difficult processing, and inaccurate determination results.

Inactive Publication Date: 2012-10-03
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 components in N-Phosphonomethyl aminodiacetic acid (PMIDA) mother solution
  • Method for analyzing components in N-Phosphonomethyl aminodiacetic acid (PMIDA) mother solution
  • Method for analyzing components in N-Phosphonomethyl aminodiacetic acid (PMIDA) mother solution

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] A kind of analytical method of bisphosphonate mother liquor composition, wherein nitrilotriacetic acid is measured by the following method:

[0028] Instrument: Shimadzu high performance liquid chromatograph (with UV detector)

[0029] Chromatographic column: DIKMA ODS-3, 250×4.5mm, 5μm

[0030] Mobile phase: 0.1%KH 2 PO 4 , with H 3 PO 3 Adjust pH=2.0

[0031] Flow rate: 0.8mL / min

[0032] UV: 195nm

[0033] Injection volume: 20μL

[0034] Standard solution determination:

[0035] Take nitrilotriacetic acid (AR, the purity of the purchased nitrilotriacetic acid sample is 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 into a 50mL volumetric flask. In a 100mL volumetric flask, add mobile phase to dilute to the mark, shake well, filter through a microporous membrane, and inject. The nitrilotriacetic acid peak area was 67886.

[0036] S...

Embodiment 2

[0064] A kind of analytical method of bisphosphonate mother liquor composition, wherein nitrilotriacetic acid is measured by the following method:

[0065] Instrument: Shimadzu high performance liquid chromatograph (with UV detector)

[0066] Chromatographic column: InertsilODS-4, 250×4.5mm, 5μm

[0067] Mobile phase: 0.15%H 3 PO 4 Aqueous solution, pH=3.0

[0068] Flow rate: 0.6mL / min

[0069] UV: 195nm

[0070] Injection volume: 20μL

[0071] Standard solution determination:

[0072] Take nitrilotriacetic acid (AR, the purity of the purchased nitrilotriacetic acid sample is 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 this solution into a 50mL volumetric flask. In a 100mL volumetric flask, add mobile phase to dilute to the mark, shake well, filter through a microporous membrane, and inject. The nitrilotriacetic acid peak area was 66428.

[0073] Sampl...

Embodiment 3

[0079] A kind of analytical method of bisphosphonate mother liquor composition, wherein nitrilotriacetic acid is measured by the following method:

[0080] Instrument: Shimadzu high performance liquid chromatograph (with UV detector)

[0081] Chromatographic column: DIKMA ODS-3, 250×4.5mm, 5μm

[0082] Mobile phase: 0.2%KH 2 PO 4 , with H 3 PO 4 Adjust pH=2.0

[0083] Flow rate: 1.5mL / min

[0084] UV: 195nm

[0085] Injection volume: 20μL

[0086] Standard solution determination:

[0087] Take nitrilotriacetic acid (AR, the purity of the purchased nitrilotriacetic acid sample is 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 into a 50mL volumetric flask. In a 100mL volumetric flask, add mobile phase to dilute to the mark, shake well, filter through a microporous membrane, and inject. The nitrilotriacetic acid peak area was 66101.

[0088] S...

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Abstract

The invention discloses a method for analyzing components in an N-Phosphonomethyl aminodiacetic acid (PMIDA) mother solution and relates to a component analysis method for a mother solution generated by producing the PMIDA by using iminodiacetonitrile to serve as a main raw material. The method includes the steps of independently measuring contents of the PMIDA, a nitrilotriacetic acid and an iminodiacetic acid in the mother solution, measuring polybasic acids of the PMIDA, a phosphoric acid and a phosphorous acid and the like in a substep mode, simultaneously strengthening a weak acid by adding calcium chloride, quantificationally releasing inactive hydrogen, then 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, a hydrochloric acid and the phosphoric acid according to reaction laws and interrelations of various substances. By means of verification, the method is accurate, comprehensive, scientific and reasonable, the operation is simple, reliable evidences are provided for recycle and comprehensive usage of the PMIDA mother solution, and the method has a good popularizing value.

Description

[0001] The present invention is a divisional application of the invention patent application with the patent application number 201010552827.5 and the application date on November 22, 2010, and the title is "An analysis method for the composition of bisphosphonate mother liquor". technical field [0002] The invention relates to a method for analyzing the composition of bisphosphonate mother liquor, in particular to a method for analyzing the composition of a mother liquor produced when bisphosphonate is produced by using iminodiacetonitrile as the main raw material, and belongs to the field of chemical analysis. Background technique [0003] Diglyphosate (N-(phosphomethyl)iminodiacetic acid) It is an intermediate for the production of glyphosate (N-phosphonomethylglycine) with iminodiacetonitrile as raw material (IDA method). Glyphosate is a widely used organophosphine herbicide, which has the characteristics of high efficiency, broad spectrum, low toxicity and safety, and...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N21/31G01N21/79
Inventor 罗延谷胡欣
Owner CHONGQING UNISPLENDOUR CHEM
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