A kind of riboflavin purification process
A riboflavin and process technology, applied in the field of chemical engineering, can solve the problems of D impurity generation, exceeding the standard, etc.
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Embodiment 1
[0020] Embodiment 1: a kind of riboflavin purification process, it comprises following processing steps:
[0021] S1, in the there-necked flask of 1000ml, add 5% (w / v) hydrochloric acid 800ml and purity be 50g of the riboflavin crude product of 80%, after the riboflavin crude product dissolves completely, add 0.05% (w / w) iron powder, Heating to reflux for 4 hours, after the reflux reaction, the mixture in the three-neck flask was cooled, filtered, and dried to obtain a filter cake;
[0022] S2. Dissolving the filter cake in 27% (w / v) 100ml of hydrochloric acid, heating to 60°C, reacting for 1.5h, and filtering while hot, to obtain a filtrate;
[0023] S3. Add 0.05% (w / w) iron powder to the filtrate, quickly pour it into 1000ml deionized water, and precipitate crystals; then heat up to 92°C for crystal transformation; keep stirring for 1h, filter after cooling, and wash with water to obtain purity A 99.5% riboflavin product.
Embodiment 2
[0024] Embodiment 2: get the raw material identical with embodiment 1, operation method is exactly the same as above, but do not add iron powder, make the riboflavin product that purity is 99.2%.
[0025] The high-purity riboflavin product obtained in Example 1 and Example 2 is assayed and analyzed, and the analysis results are shown in Table 1.
[0026] Table 1: Riboflavin purification process experimental data table
[0027]
[0028] As can be seen from the data in Table 1: the riboflavin purification process without iron powder reducing agent, the obtained riboflavin product D impurity (hydroxymethyl riboflavin) exceeds the standard.
Embodiment 3
[0029] Embodiment 3: a kind of riboflavin purification process, it comprises following processing steps:
[0030] S1. In a 1000ml there-necked flask, add 800ml of 5% (w / v) hydrochloric acid and 50g of crude riboflavin with a purity of 80%. After the crude riboflavin is completely dissolved, add 3g of ferrous sulfate heptahydrate and heat to reflux for reaction 6h, after the reflux reaction was completed, the mixture in the there-necked flask was cooled, filtered, and dried to obtain a filter cake;
[0031] S2, dissolving the filter cake in 27% (w / v) 100ml hydrochloric acid, heating to 50°C, reacting for 1.6h, and filtering while hot to obtain a filtrate;
[0032] S3. Add 3g of ferrous sulfate heptahydrate to the filtrate, quickly pour it into 1000ml of deionized water, and precipitate crystals; then heat up to 90°C for crystal transformation; keep stirring for 1h, filter after cooling, and wash with water to obtain a purity of 99.4 % riboflavin products.
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