The preparation method of glyphosate
A technology of glyphosate and chloromethylphosphonic acid, which is applied in the chemical industry, can solve the problems of low production cost, large amount of waste water, and difficulty in recycling, and achieve the effects of improving yield and quality, reducing material loss and reducing production cost.
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Embodiment 1
[0024] Example 1. Preparation of monosodium chloromethylphosphonic acid
[0025] Quickly add 278 grams (2 moles) of newly distilled phosphorus trichloride and 180 grams (6 moles) of paraformaldehyde into the reaction vessel, and slowly increase the temperature from room temperature to 80°C within 1.5 hours. After the paraformaldehyde is completely dissolved, the temperature is increased Incubate the reaction at 100°C for 8 hours, then cool the reaction solution to room temperature, add 11.2 g of anhydrous aluminum trichloride, slowly increase the temperature from room temperature to 180°C within 2 hours, keep the temperature for 4 hours, and then distill the by-product dichloride Methane, dichloromethyl ether and excess formaldehyde, the residue is cooled to room temperature, add 200 mL of water, hydrolyze at 70°C for 2 hours until the solid is completely dissolved, filter to remove a small amount of insoluble black residue, decolor the filtrate with activated carbon, and adjust t...
Embodiment 2
[0029] Example 2. Preparation of disodium aminomethylphosphonic acid
[0030] Add 621 grams of chloromethylphosphonic acid monosodium salt aqueous solution prepared in Example 1 (the mass percentage of chloromethylphosphonic acid monosodium salt is 45.68%, 1.89 moles) into the reaction kettle, and then add liquid ammonia (18.66) Mol), heat to 80°C, keep the temperature in the kettle at 1.5MPa and keep the reaction for 6 hours, monitor the reaction progress by high performance liquid chromatography, and stop when the residual amount of chloromethylphosphonic acid monosodium salt is less than 0.3% In the reaction, the residual ammonia gas in the system is eliminated to obtain 750 grams of an aqueous solution of disodium aminomethylphosphonic acid, in which the mass percentage of disodium aminomethylphosphonic acid is 36.64%, and the yield is 95%. The obtained aminomethylphosphonic acid disodium salt aqueous solution does not need to be purified, and can be directly used as a raw ma...
Embodiment 3
[0031] Example 3. Preparation of disodium aminomethylphosphonic acid
[0032] Add 621 grams of chloromethylphosphonic acid monosodium salt aqueous solution prepared in Example 1 (the mass percentage of chloromethylphosphonic acid monosodium salt is 45.68%, 1.89 moles) into the reaction kettle, and then add ammonia (18.66 moles) ), the temperature is raised to 80℃, and the reaction is kept for 6 hours under the condition of 1.5MPa in the kettle. The reaction progress is monitored by high performance liquid chromatography, and the reaction is stopped when the residual amount of chloromethylphosphonic acid monosodium salt is less than 0.3% , Exclude the residual ammonia in the system to obtain 750 grams of aminomethylphosphonic acid disodium salt aqueous solution, in which the mass percentage of aminomethylphosphonic acid disodium salt is 36.64%, and the yield is 95%. The obtained aminomethylphosphonic acid disodium salt aqueous solution does not need to be purified, and can be dire...
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