A kind of preparation method of ferrous glycinate without interfering ion
A technology of ferrous glycinate and interfering ions, which is applied in the preparation of organic compounds, chemical instruments and methods, and preparation of cyanide reactions. Long time and other problems, to achieve the effect of simple operation, increase yield and reduce reaction time
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[0030] A preparation method of ferrous glycinate without interfering ions, comprising the following steps:
[0031] ①Preparation of active ferrous oxide: under the condition of isolated air, heat ferrous oxalate to prepare active ferrous oxide, the heating temperature is 300-400°C, and the reaction time is 15-60 minutes;
[0032]
[0033] ②Synthesis reaction: In a reaction kettle, dissolve glycine in water to obtain a solution, add active ferrous oxide to the solution, and the reaction molar ratio of glycine, active ferrous oxide and water is 2~3:1:15~30 , and then, use paraffin or vegetable oil liquid seal or add one of the antioxidant vitamin C, citric acid, malic acid, reduced iron powder, acetic acid without interfering ions under the condition of filling nitrogen, argon or helium. Various, the amount of antioxidant added is 3% to 15% of the mass of glycine, then stirred and heated to 50-80°C, and reacted for 3-9 hours to obtain a reaction solution;
[0034]
[0035...
Embodiment 1
[0039] Weigh 0.1mol ferrous oxalate and heat it to 300°C in the absence of air, keep it for 60 minutes to react, after the reaction is completed, cool to room temperature to obtain active ferrous oxide; combine active ferrous oxide with weighed 0.25mol glycine, 0.75 Put 50g of citric acid into a 250ml Erlenmeyer flask, then add 50ml of deionized water to it, and add a certain amount of liquid paraffin to seal the water surface. Heat to 70°C in a water bath, and stir at constant temperature for 6 hours. After the reaction finishes, use a separatory funnel to separate the reaction solution from the liquid paraffin, filter the reaction solution, add 400ml of ethanol to the filtrate, leave it to stand for 4 hours to obtain a precipitate, and dry the precipitate at 50°C for 8 hours. 18.2 g of the ferrous glycinate product was obtained, with a yield of 75.9%. The detected total iron content is 21.0%, and the ferrous content is 20.5%. The ethanol separation solution was rectified a...
Embodiment 2
[0042] Weigh 1 mol of ferrous oxalate, heat it to 350°C in the absence of air, and keep it for 30 minutes for reaction. After the reaction is completed, cool to room temperature to obtain active ferrous oxide; put ferrous oxide, 3 mol of glycine and 10g of Vc into 1L In a three-necked flask, add 300mL of deionized water to it, and add a certain amount of soybean oil liquid seal on the water surface. Heat to 60°C in a water bath, and stir at constant temperature for 9 hours. After the reaction, use a separatory funnel to separate the reaction solution from the soybean oil, filter the reaction solution, add 1000 mL of methanol to the filtrate, leave it to stand for 2 hours to obtain a precipitate, and dry the precipitate at 70°C for 5 hours. 392g of the ferrous glycinate product was obtained, with a yield of 80.4%. The detected total iron content is 20.7%, and the ferrous content is 20.4%. Alcohol analysis liquid is rectified at 80°C for 1 hour to recover methanol, and the res...
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