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Process for preparing glyphosate intermediate N-Phosphonomethyl iminodiacetic acid by applying N-Phosphonomethyl iminodiacetic acid waste water

A glyphosate and glyphosate technology are applied in the field of preparing glyphosate intermediate glyphosate by applying bisphosphonate wastewater to achieve the effects of reducing process steps, reducing equipment used in the process and saving energy.

Inactive Publication Date: 2013-03-06
南通泰仓化学新材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] There are no literature reports addressing the above-mentioned problems

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0012] In a 5000L enamel reaction kettle, put 2400kg of recovered mother liquid wastewater and 1300kg of 80% iminodiacetic acid into it. After starting the stirring and cooling water system, directly add 1350kg of 98% phosphine trichloride dropwise, control the temperature of the kettle to less than 60°C, and Keep a vacuum of -0.02MPa in the kettle, keep it warm for 0.5 hours after dropping, raise the temperature to 110°C, add 800kg of formaldehyde dropwise, and keep reflux, after the dropwise addition, keep warm for 2 hours, add 1000kg of washing water for recycling, and cool to room temperature The finished product of diglyphosate is obtained by discharging and pressure filtration, and the product yield is about 89% (diglyphosate to iminodiacetonitrile).

[0013] Calculate waste water amount and utilization below according to embodiment 1, analyze as follows:

[0014] According to 5000L enamel kettle as the approximate amount of wastewater produced by the condensation kettle...

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Abstract

The invention discloses a process for preparing glyphosate intermediate N-Phosphonomethyl iminodiacetic acid by applying N-Phosphonomethyl iminodiacetic acid waste water. The process is characterized in that the reaction process comprises the following steps of: after mixing quantitative iminodiacetic acid and acid water (or washing water) in a reaction kettle, controlling that the temperature is less than 80 DEG C (preferably less than 60 DEG C) and dropwise adding phosphorus trichloride; mastering that the vacuum degree is -0.01 to -0.1 MPa (preferably -0.01 MPa to -0.03 MPa); preserving heat for 0.5-10 hours (preferably 0.5-2 hours) after the dropwise addition is finished; heating to 90-120 DEG C (preferably 105-112 DEG C); reflowing while dropwise adding formaldehyde; preserving heat for 0.5-5 hours (preferably 1-2 hours) after dropwise adding; adding quantitative clear water in the reaction kettle; and measuring a normal pH (Potential of Hydrogen) value of solution in the kettle and then discharging and performing filter pressing to obtain the N-Phosphonomethyl iminodiacetic acid. The process has the advantages of capabilities of saving energy, reducing process steps and reducing equipment used by the process, environmental friendliness and emission reduction.

Description

technical field [0001] The invention belongs to the field of pharmaceutical and pesticide intermediates, and mainly relates to a process for preparing diglyphosate, a glyphosate intermediate, by mechanically applying diglyphosate wastewater. Background technique [0002] IDA method glyphosate is a broad-spectrum killing systemic herbicide. This herbicide was first registered by Monsanto Company in the United States and has been widely used in the world. Later, Monsanto Company used it on corn, soybean and other grain and oil crops. Gene science methods have cultivated crop seeds with glyphosate-resistant genes, which has greatly promoted the large-scale spraying of glyphosate for weed control, and the amount of glyphosate has also risen sharply. Moreover, the drug is degraded into harmless substances in the soil, and the harm to the environment is relatively light, so it is an excellent herbicide. [0003] During the process of glyphosate preparation, a large amount of acid...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/38
Inventor 鲍菊篱
Owner 南通泰仓化学新材料有限公司