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

Inactive Publication Date: 2009-02-18
ZHEJIANG UNIV
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  • Abstract
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Problems solved by technology

Chinese patent application 200710014172.4 discloses a method for extracting raffinose from cottonseed meal, and the yield of raffinose is also very low
In the existing refining technology, although

Method used

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  • Crystallization preparation method for high purity raffinose

Examples

Experimental program
Comparison scheme
Effect test

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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Abstract

The present invention discloses a crystallization method for preparing high-purity raffinose. C1 to C3 alcohol aqueous solution is adopted as crystallizing solvent, raffinose in the form of small crystal particles is used as inoculating seeds to induce crystallization, and after two to twenty four hours of grain growing, the high-purity raffinose is obtained by filtration and drying. The purity of the obtained raffinose product can reach over 99 percent, and the crystallization yield can reach over 80 percent. The method has the advantages of simple technique, low production cost and easy industrialized production.

Description

technical field [0001] The invention relates to a method for preparing high-purity raffinose by crystallization of crude raffinose, belonging to the technical field of industrial crystallization. Background technique [0002] Raffinose, also known as Melitriose, is composed of galactose, glucose and fructose. It is an oligosaccharide and a non-reducing sugar. Its structural formula is as follows: [0003] [0004] Raffinose is widely found in beet, cottonseed, honey, cabbage, yeast, potato, grape, wheat, corn and the seeds of legumes. It is the most widely distributed oligosaccharide in plants except sucrose. One of the main components of polysaccharides. Among them, the content of raffinose is the highest in cottonseed, about 4-9%, about 1.0% in sugar beet, and about 1.3% in soybean. These raw materials are all important sources for extracting raffinose. Because the human digestive enzyme system lacks α-galactosidase that can decompose raffinose, raffinose can pass thr...

Claims

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Application Information

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IPC IPC(8): C07H3/06C13K13/00B01D9/04
Inventor 任其龙邢华斌苏宝根鲍宗必
Owner ZHEJIANG UNIV
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