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Preparation method of N-phosphonomethyliminodiacetic acid

A technology of bisphosphonate and iminodiacetic acid, which is applied in the chemical industry, can solve the problems of complicated operation, only 91% actual yield, and many bisphosphonate wastewater, etc., and achieves the effect of simple operation and improved yield.

Active Publication Date: 2012-03-14
ANHUI COSTAR BIOCHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] Patent CN 1916005A reports the method of using iminodiacetonitrile to synthesize diglyphosate. This method needs to control the pressure change, and the operation is relatively complicated. At the same time, the yield of diglyphosate is not high, only about 90%.
[0004] Patent US 005688994A reports the technology of using iminodiacetic acid sodium salt as a raw material to synthesize diglyphosate. The process can reduce the cost, but after the reaction, there is a lot of diglyphosate wastewater, and the actual yield is only about 91%.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Add 140g of iminodiacetic acid with a mass concentration of 95% into a 1000ml four-necked flask equipped with a thermometer, a stirrer, and a condenser tube, and simultaneously add 129.5g of hydrochloric acid with a mass percentage concentration of 31%, and 100g of water, start heating and stirring, and heat up Start to add 33g of paraformaldehyde in 2 times at 100°C, and drop 117g of phosphorous acid solution with a mass percentage concentration of 70% within 30 minutes at the same time. to room temperature, followed by filtration and washing with water to obtain 241g of wet powder of diglyphosate and 278g of mother liquor; then dry at 100°C to obtain 213.5g of dry powder of diglyphosate with a content of 98.1%, and the content of diglyphosate in mother liquor is 1.87%. Using iminodiacetic acid as a benchmark, the yield of diglyphosate was 94.6%.

Embodiment 2

[0025] Add 140g of iminodiacetic acid with a content of 95% into a 1000ml four-necked flask equipped with a thermometer, a stirrer, and a condenser, and simultaneously add 170g of hydrochloric acid with a mass percentage concentration of 31%, and 10g of water, and start heating and stirring. Raise the temperature to 130°C and start adding 45g of paraformaldehyde in 10 times. At the same time, dropwise add 176g of phosphorous acid solution with a mass percentage concentration of 70% within 60 minutes. to room temperature, filtered, and washed with water to obtain 241 g of diglyphosate wet powder and 300 g of mother liquor; the diglyphosate wet powder was dried at 100° C. to obtain 219.2 g of diglyphosate dry powder with a content of 98.2%, and the content of diglyphosate in the mother liquor was 1.51% , Taking iminodiacetic acid as a benchmark to calculate the yield of diglyphosate 96.7%.

Embodiment 3

[0027] Add 140g of iminodiacetic acid with a content of 95% into a 1000ml four-neck flask equipped with a thermometer, a stirrer, and a condenser, and simultaneously add 150g of hydrochloric acid with a mass percentage concentration of 31%, and 50g of water, and start heating and stirring. Raise the temperature to 110°C and start to add 40g of paraformaldehyde in 6 times. At the same time, dropwise add 146g of phosphorous acid solution with a mass percentage concentration of 70% within 40 minutes. to room temperature, filtered, and washed with water to obtain 236 g of wet powder of diglyphosate and 290 g of mother liquor; the wet powder of diglyphosate was dried at 100°C to obtain 216.6 g of dry powder of diglyphosate with a content of 98.6%, and the content of diglyphosate in the mother liquor was 1.63% , Taking iminodiacetic acid as a benchmark to calculate the yield of diglyphosate 96.1%.

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Abstract

The invention discloses a preparation method of N-phosphonomethyliminodiacetic acid, and the method comprises the following steps: mixing iminodiacetic acid, acidic catalyst and water, then stirring, heating to more than 100 DEG C, then adding paraformaldehyde and adding phosphorous acid within 30-60min, keeping the temperature to perform a reaction for 2-7h to obtain the suspending liquid of N-phosphonomethyliminodiacetic acid and finally preparing N-phosphonomethyliminodiacetic acid by cooling, filtrating, washing and drying. The purity of the N-phosphonomethyliminodiacetic acid prepared bythe method of the invention is more than 98% and the product yield is more than 94.5%.

Description

technical field [0001] The invention belongs to the field of chemical industry, and in particular relates to a preparation method of a fine chemical product bisglyphosate. Background technique [0002] Glyphosate is the organophosphine herbicide with the largest output and sales volume in the world. It has the characteristics of high efficiency, broad spectrum, low toxicity and safety. In recent years, due to the large-scale promotion of glyphosate-resistant genetically modified crops, making its application more convenient, the market demand for glyphosate has grown rapidly, and it has continuously replaced other types of herbicides. It has occupied the first place in the world's pesticide sales for many years. In the 1970s, the United States developed the technology of synthesizing diglyphosate and glyphosate from iminodiacetic acid as a raw material, and this technology became the conventional method for preparing glyphosate - the iminodiacetic acid (IDA) method. [0003...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F9/38
Inventor 薛谊方红新李健葛九敢王红明
Owner ANHUI COSTAR BIOCHEM CO LTD
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