Improved pmida energy-saving synthesis method
A synthesis method, the technology of diglyphosate, which is applied in the field of energy-saving synthesis of diglyphosate, can solve the problems of inconvenient production process, shortage of precious metal resources, and high requirements for equipment materials, so as to reduce equipment and operation costs, improve raw material utilization, The effect of shortening the process flow
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Embodiment 1
[0033] Prepare a 250ml three-necked flask equipped with a small magnet, a reflux condenser, a thermometer, and a constant pressure dropping funnel, and add 22.8g of iminodiacetonitrile and 22.8g of water with a mass fraction of 95% in the flask. Raise the temperature to 60°C, dissolve 20g of sodium hydroxide with a mass fraction of 99% in 67.2g of water and add it dropwise to the flask. ℃-85℃, keep warm for 0.5h, raise the temperature to 90℃-95℃, keep warm for 0.5h; raise the temperature above 100℃, deamination for 1.5h. After the end, the temperature began to drop, and when the temperature dropped to 60° C., 76.7 g of hydrochloric acid with a mass fraction of 31% was added dropwise for acidification. Afterwards, 22.4 g of phosphorous acid with a mass fraction of 98% was added to the iminodiacetic acid filtrate, and the acidification temperature was maintained for hot filtration, and the filtrate was filtered into another 250 ml three-neck flask.
[0034] Raise the temperatur...
Embodiment 2
[0037]Prepare a 250ml three-necked flask equipped with a small magnet, a reflux condenser, a thermometer, and a constant pressure dropping funnel, and add 22.8g of iminodiacetonitrile and 22.8g of water with a mass fraction of 95% in the flask. Raise the temperature to 60°C, then dissolve 20g of sodium hydroxide with a mass fraction of 99% in 57.2g of water and add it dropwise to the flask. Heat to 80°C-85°C, keep warm for 0.5h, raise the temperature to 90°C-95°C, keep warm for 0.5h; raise the temperature to above 100°C, deamination for 1.5h. After the end, the temperature began to drop, and when the temperature dropped to 60° C., 78.7 g of hydrochloric acid with a mass fraction of 31% was added dropwise for acidification. Afterwards, 22.4 g of phosphorous acid with a mass fraction of 98% was added to the iminodiacetic acid filtrate, and the acidification temperature was maintained for hot filtration, and the filtrate was filtered into another 250 ml three-neck flask.
[0038...
Embodiment 3
[0041] Prepare a 250ml three-necked flask equipped with a small magnet, a reflux condenser, a thermometer, and a constant pressure dropping funnel, and add 22.8g of iminodiacetonitrile and 22.8g of water with a mass fraction of 95% in the flask. Stirring was carried out to form a suspension. Afterwards, 20 g of sodium hydroxide with a mass fraction of 99% was dissolved in 57.2 g of water and then transferred to a constant pressure dropping funnel, and the temperature was raised to 60° C. to start adding the sodium hydroxide solution dropwise. ℃-75℃, keep warm for 0.5h, raise the temperature to 80℃-85℃, keep warm for 0.5h, raise the temperature to 90℃-95℃, keep warm for 0.5h; raise the temperature to above 100℃, deamination for 1.5h. After the end, the temperature began to drop, and when the temperature dropped to 60° C., 78.7 g of hydrochloric acid with a mass fraction of 31% was added dropwise for acidification. After that, 20.5 g of phosphorous acid with a mass fraction of ...
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