Preparation method of calcium glycerophosphate with high calcium content
A technology of calcium glycerophosphate and calcium dihydrogen phosphate, which is applied in the direction of phosphorus organic compounds, can solve the problem that the product cannot meet the needs of multiple industries at the same time, and achieve the effect of stable quality
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[0021] A preparation method of calcium glycerophosphate with high calcium content, comprising the following steps:
[0022] (i) Synthesis reaction
[0023] Put glycerol: calcium dihydrogen phosphate: phosphoric acid molar ratio equal to 1.5:0.1~0.2:1 into the reactor, and add citric acid of 1%~3% of the total weight of the above reactants at the same time to carry out the synthesis reaction, this reaction is For the esterification reaction, the above-mentioned components are all food-grade.
[0024] This reaction is carried out in two stages, the first stage: under normal pressure, the temperature is 80°C, keep for 0.5 hours; the first stage: the vacuum degree is 0.08MPa, the temperature is 140°C, keep for 7.5 hours.
[0025] A small amount of citric acid is added before the reaction, and the chelation of citric acid can increase the solubility of calcium dihydrogen phosphate, so that it can fully participate in the esterification reaction, which is beneficial to increase the...
Embodiment 1
[0037] Put 40 grams of glycerin, 8 grams of calcium dihydrogen phosphate, 32.7 grams of phosphoric acid, and 0.08 grams of citric acid into a reactor equipped with a condensing water separator and a stirrer. Turn on the stirring, fully stir for 20 minutes, start heating, and when the temperature rises to 80°C, keep it for 0.5 hours to ensure that the solid substances in the reaction raw materials are fully dissolved. Start vacuuming, and continue to raise the temperature until the vacuum degree is 0.08MPa and the temperature is 140°C, and it is kept for 7.5 hours.
[0038] After the esterification reaction is finished, the weight of water in the metering collector is 30.8 grams, and the weight of the esterification product in the reaction kettle is converted to about 50 grams. Let the product cool to about 80°C, add 200ml of pure water, and stir at 105°C under normal pressure for 2 hours to obtain an orange transparent acidic liquid.
[0039] Under stirring conditions, add 4%...
Embodiment 2
[0043] Put 141 grams of glycerin, 41 grams of calcium dihydrogen phosphate, 115.3 grams of phosphoric acid, and 5.6 grams of citric acid into a reaction kettle equipped with a condensing water separator and a stirrer. After stirring for 20 minutes, heat up to 80° C. and keep for 0.5 hour, and the solid matter in the reaction raw material is fully dissolved. Start vacuuming, and continue to raise the temperature until the vacuum degree is 0.08MPa and the temperature is 140°C, and it is kept for 7.5 hours.
[0044] After the esterification reaction is finished, the weight of water in the metering collector is 97.6 grams, and the weight of the esterification product in the reaction kettle is converted to about 205 grams. Let the product cool to about 80°C, add 820 ml of pure water, and stir at 110°C under normal pressure for 2 hours to obtain an orange transparent acidic liquid.
[0045] Under stirring conditions, add 4% (mass percentage concentration) of calcium hydroxide turbi...
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