Sodium diformate preparation method
A technology of sodium diformate and formic acid, which is applied in carboxylate preparation, organic chemistry, etc., can solve the problems of inability to obtain sodium diformate, instability, and difficulty in obtaining it, and achieve simple production process, small amount of evaporated water, and high product purity Effect
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Embodiment 1
[0031] Add 226g of formic acid with a mass fraction of 85% to a 500mL crystallizer equipped with a thermometer and a condensation reflux device, and slowly add 110g of 96% sodium carbonate at room temperature under stirring (100-150rpm speed). The rate of addition was controlled so that the temperature of the reaction mixture was within 90°C. After the feeding is completed, keep the crystallizer in a constant temperature circulating water bath, keep stirring (rotating speed 250-300rpm), and continue to react at 90°C for 0.5h. The reaction product is cooled at a cooling rate of 20°C / h under the stirring state of 200-250rpm. After crystals appear, the stirring speed is adjusted to 80-100rpm, and the end point temperature of cooling crystallization is 25°C. After crystallization, the crystals and mother liquor are separated by means of a vacuum filter. The wet sodium diformate yield was about 187.3 g. After drying in a drying oven at 60° C., 174.9 g of dry product are obtained....
Embodiment 2
[0033]Add 600g of formic acid with a mass fraction of 88% to a 1000mL crystallizer equipped with a thermometer and a condensation reflux device, and slowly add 270g of 98% sodium carbonate at room temperature under stirring (150-200rpm speed). The rate of addition was controlled so that the temperature of the reaction mixture was within 80°C. After the feeding is completed, keep the crystallizer in a constant temperature circulating water bath, keep stirring (rotating speed 250-300rpm), and continue to react at 80°C for 1.5h. The reaction product was cooled at a cooling rate of 15° C. / h under stirring at 200-250 rpm. When the temperature drops to 50°C, add a seed crystal with a theoretical yield of 3%, and adjust the rotation speed to 60-80rpm, continue to cool and crystallize at 15°C (increase the rotation speed at the later stage of crystallization to 120-150rpm), and separate the crystals with a vacuum filter and mother liquor. The wet sodium diformate yield was about 510...
Embodiment 3
[0035] Add 655g of formic acid with a mass fraction of 85% to a 1000mL crystallizer equipped with a thermometer and a condensing reflux device, and slowly add 210g of 96% sodium hydroxide at room temperature under stirring (rotating speed 200-250rpm). The rate of addition was controlled so that the temperature of the reaction mixture was within 40°C. After the feeding is completed, keep the crystallizer in a constant temperature circulating water bath, keep stirring (300-350 rpm), and continue to react at 40°C for 6h. The reaction product was cooled at a cooling rate of 5° C. / h under stirring at 200-250 rpm. When the temperature drops to 20°C, add a seed crystal with a theoretical yield of 0.1%, and adjust the rotation speed to 100-120rpm, continue cooling and crystallize at 10°C (increase the rotation speed at the later stage of crystallization to 150-180rpm), and separate the crystals with a vacuum filter and mother liquor. The wet sodium diformate yield was about 541 g. ...
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