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Method for preparing Phosphonomethyl iminodiacetic acid (PMIDA) through hydrolysis of imino diacetonitrile

The technology of iminodiacetonitrile and iminodiacetate is applied in the field of preparing bisphosphonate by hydrolysis of iminodiacetonitrile. Investment and energy consumption, the effect of short process route

Inactive Publication Date: 2008-07-09
SICHUAN BEIER CHEM GROUP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The price of diethanolamine fluctuates greatly, and there is a certain market risk
However, the preparation of iminodiacetic acid solid or iminodiacetic acid disodium salt solid requires processes such as concentration, crystallization, separation, washing, drying, etc., which lengthens the flow process, increases equipment investment and process operation
In the process of obtaining iminodiacetic acid disodium salt solid, the mother liquor will contain a certain amount of iminodiacetic acid disodium salt that is difficult to recover, which not only increases the amount of waste water, but also reduces the utilization rate of raw materials

Method used

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  • Method for preparing Phosphonomethyl iminodiacetic acid (PMIDA) through hydrolysis of imino diacetonitrile
  • Method for preparing Phosphonomethyl iminodiacetic acid (PMIDA) through hydrolysis of imino diacetonitrile

Examples

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Effect test

Embodiment 1

[0035] 84 grams of sodium hydroxide and 340 grams of water are mixed into a 20% sodium hydroxide solution (potassium hydroxide solution or other lye can also be used) with a mass percentage composition. Raise the temperature to 80°C, add 120 grams of iminodiacetonitrile with a mass percentage of 95% in four batches under the conditions of stirring and pressure of -0.01 to -0.04 MPa, and keep warm for 2 hours to obtain iminodiacetic acid Disodium salt solution, the released ammonia is absorbed by water. Add 50 grams of hydrochloric acid with a mass percentage of 36%, maintain the temperature at 95 to 105°C, control the pressure at -0.01 to -0.04MPa, add 168 grams of phosphorus trichloride with a mass percentage of 98%, and release HCl gas is absorbed by water. Then be warming up to 103 ℃, add 50 gram mass percentage composition and be 36% hydrochloric acid, dropwise add 162 gram mass percentage composition be 37% formaldehyde, after formaldehyde is added, maintain temperature ...

Embodiment 2

[0037] 85 grams of sodium hydroxide was mixed with 340 grams of water to make a 20% sodium hydroxide solution. Raise the temperature to 80° C., under the conditions of stirring and pressure of -0.01 to -0.04 MPa, add a total of 120 grams of 95% iminodiacetonitrile in four batches, and keep warm for 2 hours to prepare a solution of iminodiacetic acid disodium salt. The released ammonia is absorbed by water. Add 50 grams of 36% hydrochloric acid, control the pressure at -0.01 to -0.04 MPa, and add 168 grams of 98% phosphorus trichloride dropwise at a temperature of 50 to 80° C., and the released HCl gas is absorbed by water. Then the temperature was raised to 105° C., and 146 grams of 37% formaldehyde was added dropwise. After the formaldehyde was added, the temperature was maintained at 110° C. for 2 hours to complete the synthesis reaction of diglyphosate. After the synthesis liquid was processed, 201.4 grams of bisglyphosate with a purity greater than 98% were obtained. Oth...

Embodiment 3

[0039] 84 grams of sodium hydroxide was mixed with 340 grams of water to make a 20% sodium hydroxide solution. Raise the temperature to 80° C., under the conditions of stirring and pressure of -0.01 to -0.04 MPa, add a total of 120 grams of 95% iminodiacetonitrile in four batches, and keep warm for 2 hours to prepare a solution of iminodiacetic acid disodium salt. The released ammonia is absorbed by water. Under the maintenance temperature of 50-80°C, the pressure is controlled at -0.01--0.04 MPa, and 173 grams of 98% phosphorus trichloride is added dropwise, and the released HCl gas is absorbed by water. Then the temperature was raised to 110° C., and 146 grams of 37% formaldehyde was added dropwise. After the formaldehyde was added, the temperature was maintained at 110° C. for 2 hours to complete the synthesis reaction of diglyphosate. The synthetic solution was treated to obtain 207.7 grams of diglyphosate. Other operating conditions are with embodiment 1. The yield of ...

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Abstract

This invention discloses a method for preparing N-phosphonomethyl iminodiacetic acid (PMIDA) by iminodiacetonitrile hydrolysis. The method comprises: (1) hydrolyzing iminodiacetonitrile (greater than or equal to 95 wt.%) in an alkali solution under stirring at 20-100 deg.C and -(0.01-0.04) MPa to obtain iminodiacetate solution; (2) dropping phosphorous trichloride (1.0-1.5 mol times of iminodiacetonitrile) to the iminodiacetate solution at 20-100 deg.C and -(0.01-0.04) MPa with an acidic catalyst added before or after the phosphorous trichloride addition; (3) adding formaldehyde at a temperature not lower than 80 deg.C; (4) reacting at 100-120 deg.C for 1-7 h to obtain PMIDA suspension; (5) vacuum-distilling to recover formaldehyde; (6) crystallizing, separating, washing and drying to obtain PMIDA with a purity higher than 98%. The method has such advantages as simple process, low cost and high yield.

Description

Technical field: [0001] The present invention relates to a preparation method of a fine chemical product-diphosphine, in particular to a method for preparing diphosphine by hydrolysis of iminodiacetonitrile. Background technique: [0002] Glyphosate is the pesticide with the largest output and sales volume in the world, and diglyphosate is an important intermediate for the synthesis of glyphosate, which has a very broad international and domestic market. In the 1870s, the United States developed the technology of using iminodiacetic acid as raw material to synthesize diglyphosate and then glyphosate. Since then, this technology has become a conventional method for preparing glyphosate——iminodiacetic acid (IDA) Act. The IDA method is to react iminodiacetic acid with phosphorous acid and formaldehyde to prepare diglyphosate, and then oxidize it to obtain glyphosate. At present, the processing route of preparing bisglyphosate has the following several kinds: [0003] (1) Chl...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F9/38
Inventor 王国成陈贵林蔡忠安曾泉杨华崔卫东梁晓禽杨建华邓珍
Owner SICHUAN BEIER CHEM GROUP
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