Process for preparing high-purity raffinose from degreased cottonseed meal

A technology of degreasing cottonseed and raffinose, which is applied in the field of chemical engineering, can solve the problems of low raffinose yield, large amount of solvent, and high solution viscosity, etc., to reduce the loss of raffinose, reduce solvent consumption, and accelerate dissolution and mass transfer Effect

Active Publication Date: 2009-02-25
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, using methanol with a concentration of 40-100% by weight to extract the rough material of raffinose, dissolving the crude material with dilute acid, decolorizing, and then directly Concentration and crystallization, and finally high-purity raffinose is obtained through multiple recrystallization treatments, but the yield of the final raffinose product is very low
[0009] There are such and such problems in the method of each single process adopted above, and the main problems are: as in (1), the amount of solvent used in the alcohol solvent static leaching method is large, which causes difficulties for solvent recovery and causes solvent waste. Simultaneously, the utilization of solvent The extraction rate is low, and the active ingredients are not fully leached. In order to ensure a high extraction rate, it generally takes a long time and repeated extractions, resulting in an increase in the content of impurities in the extract, complex components, difficult subsequent separation and purification, and difficult to prepare high-purity product; in (2), a large amount of powdered activated carbon needs to be used to achieve a satisfactory decolorization effect, and powdered activated carbon cannot be reused at the same time, and it is easy to remain in the solution after decolorization and it is difficult to complete removal; when the ion exchange resin column resin in (3) is regenerated Can produce a large amount of waste acid and waste alkali, cause environmental pollution, and the used equipment investment of nanofiltration membrane separation is big, and separation membrane is easy to pollute life-span short; The equipment investment is large, and the separation membrane is easy to pollute and has a short life; (5) removes monosaccharides and sucrose in the crystallization, which means that finally obtaining high-purity raffinose must be realized through multiple recrystallizations, resulting in low raffinose yield; (6) ) when using pure water as the crystallization solvent, the larger solubility of raffinose in pure water will cause the solution viscosity to be too large in the crystallization process, so that the crystallization rate will decline, and only the cooling time will need as much as 50 hours. The yield is also lower
[0010] Therefore, even if the organic solvent leaching in the prior art is used to obtain the raffinose extract, decolorization of the raffinose extract, desalination, deproteinization, removal of monosaccharides and sucrose, crystallization and refining, these series of processes are combined to prepare high-purity cottonseed sugar, still not getting the desired raffinose yield
Moreover, such a process route is quite long, has many steps, cumbersome operation, and high production cost, and is not suitable for industrialized production.

Method used

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  • Process for preparing high-purity raffinose from degreased cottonseed meal

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0063] (1) Degreased cottonseed meal (wherein the mass percentage 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 it evenly Its bulk volume is about 560 milliliters, then add 350 milliliters of ethanol aqueous solution with a volume percentage concentration of 75% to the percolation column, soak for 30 minutes at 55°C to fully swell the defatted cottonseed meal, open the outlet valve of the percolation column, and simultaneously The extraction solvent was continuously added to the top of the column, and the flow rate was controlled to be 168 ml / hour until the volume of the percolation extract collected was 1900 ml. After analysis, the percolation liquid has a solid content of 4.2%; on a dry basis, the mass percentage of raffinose is 38.2%.

[0064] Finally, add deionized water from the top of the percolation column to replace the residual ethanol in the defatted cottonseed meal, control the fl...

Embodiment 2

[0074] (1) Degreased cottonseed meal (wherein the mass percentage 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 it evenly The bulk volume is about 560 milliliters, then add 350 milliliters of ethanol aqueous solution with a volume percentage concentration of 85% to the percolation column, soak for 40 minutes at 70°C to fully swell the defatted cottonseed meal, open the outlet valve of the percolation column, and simultaneously The extraction solvent was continuously added to the top of the column, and the flow rate was controlled to be 450 ml / hour until the volume of the percolation extract collected was 2200 ml. The percolation liquid was analyzed by HPLC, and the solid content was 4.0%, and the mass percentage of raffinose was 33.7% on a dry basis.

[0075] Finally, add deionized water from the top of the percolation column to replace the residual ethanol in the defatted cottonseed meal,...

Embodiment 3

[0078] (1), (2) operating conditions are identical with embodiment 1.

[0079] (3) Put about 1700 grams of HZ802 resin (adsorbent B) into an adsorption column with a size of Φ5.6cm×97cm, and the column bed volume B'V' is about 2400mL.

[0080] Pass the decolorized solution obtained in step (2) into a fixed bed with HZ802 resin (adsorbent B) at a flow rate of 1.5B'V' / h, the sample loading volume is about 2.0B'V', and the temperature is controlled at 40 ℃, the raffinose is adsorbed by the HZ802 resin, and the effluent collected during the sample loading process also contains a small amount of raffinose, which can be directly recycled.

[0081] After loading the sample, wash the adsorption column with 2B'V' deionized water at a flow rate of 1.5B'V' / h to remove the decolorization solution remaining in the adsorbent voids in the adsorption column. The obtained washing solution can be recycled, and finally use 3B' The volume percent concentration of V' is 40% ethanol aqueous soluti...

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Abstract

The invention discloses a technique for preparing high-purity raffinose from degreasing cotton seed meal, which takes alcoholic solution as extraction solvent to extract the degreasing cotton seed meal by percolation, and extracting solution of the raffinose is obtained; then, the extracting solution of the raffinose is absorbed by a static bed which is filled with different sorbents to separate and remove impurities; at last, the crude product of the raffinose is dissolved in the alcoholic solution for crystallization, so that white styliform raffinose crystalloid is obtained; the purity of the raffinose is over 98%, and the total yield of the raffinose is higher than 70%. The technique has short operational path, low requirements for production equipment, good quality on the obtained raffinose products, high yield and low production cost, and facilitates industrial mass production.

Description

technical field [0001] The invention belongs to the technical field of chemical engineering, in particular to a process for preparing raffinose from defatted cottonseed meal. Background technique [0002] Raffinose, also known as Melitriose and raffinose, is composed of galactose, glucose and fructose. It is an oligosaccharide and a non-reducing sugar. Its structural formula is as follows: [0003] [0004] Research has found that raffinose is an excellent nutrient source for beneficial bacteria such as Bifidobacterium and Lactobacillus acidophilus in the human intestinal tract, which can promote their proliferation, thereby inhibiting the growth of spoilage bacteria in the intestinal tract and reducing the formation of toxic fermentation products. Bifidobacteria ferment raffinose to produce a large amount of short-chain fatty acids, which can stimulate intestinal peristalsis, increase stool moisture and maintain a certain osmotic pressure, thereby preventing constipation...

Claims

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Application Information

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IPC IPC(8): C07H3/06C07H1/08C13K13/00
Inventor 任其龙杨亦文苏云苏宝根鲍宗必邢华斌吴彩娟朱魏
Owner ZHEJIANG UNIV
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