Crystallization preparation method for high purity raffinose
A raffinose, high-purity technology, applied in the production of sugar, solution crystallization, oligosaccharides, etc., can solve the problems of unsuitability for industrial production, low raffinose yield, low raffinose product yield, etc., and achieves easy industrialization. The effect of high production, high yield and low production cost
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Embodiment 1
[0046] Embodiment 1: prepare raffinose crude product:
[0047] (a). Degreased cottonseed meal (wherein the mass percent content of raffinose is 3.9%) is sieved through a 1.8mm sieve, weighs 435 grams and puts it into a percolation column (Φ3.5cm×70cm), and fills After uniformity, its bulk volume is about 560 milliliters, then add 350 milliliters of volume percent concentration to the percolation column and be 75% ethanol aqueous solution, soak at 55 ℃ for 30 minutes to make the defatted cottonseed meal fully swell, open the percolation column outlet valve, and simultaneously Continuously add extraction solvent from the top of the percolation column, and control the flow rate to be 168 ml / hour until the volume of the percolation extract collected is 1900 ml. The percolating liquid is analyzed, and solid content (solid content refers to the percentage that the quality when solution is dried to constant weight accounts for the percentage of solution mass before drying, the same b...
Embodiment 2
[0055] Embodiment 2: the preparation of high-purity raffinose
[0056] In a clean three-necked flask with a reflux condenser, add 100 grams of raffinose crude product with a purity of 80% and 500 milliliters of methanol aqueous solution with a volume concentration of 70% prepared by the method in Example 1, start stirring, and heat up to 65 ℃, after completely dissolving, first slowly cool down to 40°C at a rate of 0.5°C / min, add 0.5 g of 170-200 mesh raffinose (ie crystal seed) to induce crystallization, and then continue to slowly cool down to 10°C at the same speed , grow the crystal for 12 hours at this temperature. Then, the crystalline solid was filtered again, and the filter cake was washed with a small volume concentration of 70% methanol solution, and dried in a vacuum oven at 40°C for 6 hours to obtain 65.2 grams of white needle-shaped raffinose pentahydrate crystals, which were analyzed by HPLC. The purity is 98.7%, and the yield is 80.5%.
Embodiment 3
[0057] Embodiment 3: the preparation of high-purity raffinose
[0058] In a clean three-necked flask with a reflux condenser, add 100 grams of raffinose crude product with a purity of 80% and 400 milliliters of ethanol aqueous solution with a volume concentration of 60% obtained by the method in Example 1, start stirring, and heat up to 75 ℃, after it is completely dissolved, slowly cool down to 45°C at a speed of 1°C / min, add 0.6 g of 170-200 mesh raffinose (ie, seed crystal) to induce crystallization, and then continue to slowly cool down to 20°C at the same speed , grow crystals at this temperature for 24 hours. Finally, the crystalline solid was filtered, the filter cake was washed with a small amount of 70% ethanol solution, and dried in a vacuum oven at 40°C for 8 hours to obtain 63.8 grams of white needle-shaped raffinose pentahydrate crystals, which were analyzed by HPLC and had a purity of 98.2% , yield 78.4%.
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