Method for production of phosphonomethylglycin
A technology of phosphonomethyliminodiacetic acid and sulfurous acid, which is applied in chemical instruments and methods, compounds of Group 5/15 elements of the periodic table, organic chemistry, etc. Complexity, etc.
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example 1
[0029] 38 g of N-phosphonomethyliminodiacetic acid and 0.92 g of ammonium molybdate tetrahydrate were suspended in 100 ml of water, and the suspension was warmed to 65°C. Then 20.6 g of a 30% strength hydrogen peroxide solution were added dropwise within 30 minutes, and stirring was continued at 65° C. for 1 hour, during which time a clear solution was formed. h 2 o 2 The test was negative. At 40°C, add this N-oxide solution dropwise to 10 mL of SO in 30 min. 2 in saturated aqueous solution. Continuous gas evolution was observed. Even when the N-oxide is being metered in, a colorless precipitate still forms. Stirring was then continued for 1 hour at 40°C. The separated precipitate was filtered and dried at room temperature. In this way, 23.2 g of N-phosphonomethylglycine were isolated with a purity of 96%. This corresponds to a yield of 79%, based on the amount of N-phosphonomethyliminodiacetic acid used.
example 2
[0031] 38 g of N-phosphonomethyliminodiacetic acid and 0.92 g of ammonium molybdate tetrahydrate were suspended in 100 ml of water, and the suspension was warmed to 65°C. Then 20.6 g of a 30% strength hydrogen peroxide solution were added dropwise within 30 minutes, and stirring was continued at 65° C. for 1 hour, during which time a clear solution was formed. h 2 o 2 The test was negative. The solution was cooled to room temperature. This N-oxide solution was added dropwise within 30 minutes to the 2 and N 2 of the mixture in 10 ml of water. During N-oxide addition, more SO 2 and N 2 The mixture is metered into this solution. Continuous gas evolution was observed and the temperature climbed to 55°C. The mixture was then stirred at 5°C for 30 minutes. The separated precipitate was filtered and dried. In this way, 22.0 g of N-phosphonomethylglycine were isolated with a purity of 98%. This corresponds to a yield of 76%, based on the amount of N-phosphonomethyliminodi...
example 3
[0033] 60 g of N-phosphonomethyliminodiacetic acid and 1.23 g of ammonium molybdate tetrahydrate were suspended in 75 ml of water, and the suspension was warmed to 55°C. Then 19.8 g of a 50% strength hydrogen peroxide solution were added dropwise within 15 minutes, and stirring was continued at 65° C. for 1.5 hours, during which time a clear solution was formed. In the next step, 2 mL of saturated SO 2 The solution and 15% of the prepared N-oxide solution were introduced into a reaction vessel at 40°C. This N-oxide is then added dropwise such that the generated CO 2 The molar amount of is about 70% of the molar amount of N-oxide that has been added dropwise. Thus, for example, 1.7 liters of CO are formed after a total of 30% of the N-oxide solution has been introduced 2 . This metering method prevents the build-up of N-oxides in the solution. If CO 2 release rate slows down, add SO 2 solution makes CO 2 The amount of formed corresponds to about 70% of the N-oxide that ...
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