CN101367846B - Percolation extraction method for raffinose - Google Patents
Percolation extraction method for raffinose Download PDFInfo
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Abstract
The present invention discloses a percolation extraction method of raffinose. Utilizing extraction solvent for extraction, the method includes the following processes: degreased cotton seed meal is used as material, methanol aqueous solution or ethanol aqueous solution, the volume percentage concentration of which is 70 percent to 85 percent, is used as the extraction solvent, which is added into a percolation column containing the degreased cotton seed meal under the temperature of 50 DEG C to 70 DEG C, and after the degreased cotton seed meal is sufficiently swelled, the extraction solvent flows through the percolation column in order to collect percolated extract at an outlet. In the percolated extract, the extraction rate of the raffinose is more than 95 percent. The method has the advantages of high extraction rate, little solvent consumption, low production cost, easy industrialized production, and the like.
Description
Technical field
The present invention relates to a kind of extracting method of raffinose, belong to technical field of chemical engineering.
Background technology
Raffinose (Raffinose) claims raffinose (Melitriose), raffinose again, by semi-lactosi, glucose and fructose be combined into, belongs to oligose, is non-reducing sugar.Find that after deliberation raffinose is the fabulous nutrition source of probiotics such as bifidus bacillus, Lactobacillus acidophilus in the human intestinal, can promote their propagation, thereby suppress the growth of spoilage organism in the enteron aisle, and reduce the formation of poisonous tunning.The bifidobacterium fermentation raffinose produces a large amount of short chain fatty acids, can stimulate intestines peristalsis, increases the ight soil degree of wetting and keep certain osmotic pressure, thereby prevent the generation of constipation.In addition, raffinose can improve the digestive function of human body, promotes the absorption of human body to calcium, thereby strengthens body immunity, to preventing disease with anti-ageingly have a positive effect.Raffinose also can be used as human body and animal lives organ transplantation with protecting the main component of carrying liquid and prolonging the viable bacteria body synergistic agent of survival time at normal temperatures.Acidproof, the good heat resistance of raffinose can not lump under 90% relative humidity in moisture absorption yet, itself can be used as foodstuff additive and use, and improve the processing characteristics of food, prevent the product brown stain, improve the quality of products, and prolong the quality guaranteed period of product.Raffinose has been widely used in industries such as food, medicine and makeup at present because of having good physicochemical property and physiologically active.
Raffinose is very wide in natural distribution, it is the widest oligose that except that sucrose, in plant, distributes, it extensively is present in beet, cottonseed, honey, Caulis et Folium Brassicae capitatae, yeast, potato, grape, wheat class, corn and the fabaceous seed, wherein the content in cottonseed is the highest, is about 4～9%.Cottonseed benevolence produces a large amount of byproducts---degreasing cottonseed meal after being extracted Oleum Gossypii semen, the content of raffinose remains unchanged substantially in the degreasing cottonseed meal, and therefore, degreasing cottonseed meal cake is the splendid raw material of industrial production raffinose.
In the prior art, produce raffinose from the degreasing cottonseed meal, will not containing behind the direct condensing crystal of raffinose raffinate of pigment repeatedly usually, recrystallization obtains.As magnify people such as illuminate (from no body of gland cottonseed, extract the research of raffinose, Chinese oil, 1996,5,7-9) disclosed from no body of gland cottonseed the technology of extraction raffinose, the extraction yield of raffinose is 58.8%, product purity is more than 97%.Chinese patent application 200710014172.4 disclosed a kind of methods of extracting raffinose in cottonseed meal, the raffinose product yield is also very low.Owing to comprise raffinose, albumen, salinity, gossypol pigment and monose and sucrose etc. in the degreasing cottonseed meal, after the solvent extraction, albumen wherein, salinity, gossypol pigment and impurity such as other monose or sucrose still exist, and the existence of these impurity can cause raffinose crystallization difficulty, if before the raffinose crystal refining, do not remove these impurity in advance, then must pass through repeatedly recrystallization and could obtain high purity raffinose, must cause lower raffinose yield like this.Also be lower than 60% even if extract the extraction yield of raffinose (not needing to handle through decolouring) from no body of gland absorbent cotton, the material waste seriously can not be used for commercial scale production in the production technique of this method.
Therefore, in order to realize suitability for industrialized production high purity raffinose from the degreasing cottonseed meal, need to reduce cost, improve yield, simplify flow process, can consider from the following aspects: (1) adopts the method for lower production cost, high raffinose extraction yield in leach the process that obtains raffinose raffinate from the degreasing cottonseed meal with organic solvent; (2) before to the raffinose crystal refining, raffinose raffinate is purified, promptly to raffinose raffinate decolour, deproteinated, desalination and remove monose and processing such as sucrose, and adopt the purifying technique of optimizing as far as possible; (3) adopt the raffinose process for refining of optimizing.
In the prior art, the extracting method that obtains raffinose from the degreasing cottonseed meal mainly contains water extraction, water-containing organic solvent extraction method and enzymolysis-alcoholic solution extraction method etc.At present, from the degreasing cottonseed meal, extract raffinose, the most frequently used method be with alcoholic solution as extracting solvent, adopt static leaching method to extract to the degreasing cottonseed meal.As people such as Wang Xingguo (research of raffinose extracting method in the degreasing cottonseed meal, Chinese oil, 2005,3,57-60) disclose raffinose extract technology in a kind of cottonseed meal, as extracting solvent, stirring is at a certain temperature isolated extraction solution after extracting with ethanolic soln.After the extracted many times, united extraction solution also filters, and obtains raffinose raffinate.Solvent load is big in this static state leaching method, cause difficulty and cause the solvent waste to solvent recuperation, the utilization ratio of solvent is low simultaneously, effective constituent leaches not exclusively, for guaranteeing to have higher extraction yield, generally needs the extraction of long-time and repeated multiple times, cause foreign matter content rising in the extract, composition complicates, and the later separation purification difficult is difficult to prepare high purity product.Therefore, adopt existing common technology utilization to extract solvent and extract the method that obtains raffinose raffinate from the degreasing cottonseed meal, can not take into account high extraction and low cost, especially solvent consumption is huge, and the cost that reclaims solvent also increases.
In the prior art,, mainly be that single wherein certain class impurity is removed the report respectively of method to the relevant report that raffinose raffinate is purified.As: (1) removes pigment: the decoloring method of raffinose raffinate mainly is to use the powder activated carbon decolorizing.Beam stands the new people of grade, and (cottonseed double liquid phase extraction process methanol is the decolouring of middle raffinose extracting solution mutually, food and fermentation industries, 2007,4,73-76) and people such as Jin Qingzhe (decolouring of raffinose raffinate and gossypol removal, Chinese oil, 2005,4,47-49) a kind of method that Powdered Activated Carbon is added static decolouring in the tank reactor that raffinose raffinate is housed is disclosed, from solution, isolate gac after decolouring is finished and obtain destainer; (2) remove freshen: ion exchange resin and nanofiltration desalination (Lip river iron man etc., the application of ion exchange resin in the syrup desalination, Chinese beet sugar industry, 2000,1,3-5 are mainly adopted in desalination; Wang Xiaolin etc., the experimental study of using nanofiltration membrane sepn sugar and salt, membrane science and technology, 2001,1,44-48); (3) remove Deproteinization: mainly adopt ultra-filtration membrane to separate, (cottonseed double liquid phase extraction process methanol is the decolouring of middle raffinose extracting solution mutually as people such as Liang Lixin, food and fermentation industries, 2007,4,73-76) reported and a kind ofly made the protein denaturation precipitation, adopted ultra-filtration membrane to separate again and finish the method that raffinose extracting solution deproteinated is handled by adding plumbic acetate; (4) the common technology of removing monose and sucrose is finished in the crystalline process simultaneously.These methods can only be removed single impurity, and itself there is a such-and-such problem, mainly contain: use a large amount of Powdered Activated Carbons just can reach satisfied decolorizing effect as needing in (1), simultaneously Powdered Activated Carbon can not reuse, and easily residues in to be difficult to finish in the solution of decolouring back and remove; Can produce a large amount of spent acid and salkali waste during ion exchange resin column resin regeneration (2), cause environmental pollution, and the used facility investment of nanofiltration membrane separation is big, it is short that separatory membrane easily pollutes the life-span; (3) use of plumbic acetate can bring heavy-metal residual in, and it is big that ultra-filtration membrane separates used facility investment, and it is short that separatory membrane easily pollutes the life-span; (4) remove monose and sucrose in the crystallization in, mean that final acquisition high purity raffinose must be by repeatedly recrystallization realization, cause low raffinose yield, therefore, iff with removing these a series of operations such as pigment, salinity, albumen, monose and sucrose in the prior art, still can not obtain ideal raffinose yield simply in conjunction with purifying raffinose raffinate.The raffinose purification process is still needed and will further be optimized and simplify.
In the prior art, the raffinose process for refining adopts crystallization or precipitation to realize usually.U.S. Pat 6224684 discloses with pure water as recrystallisation solvent, a kind of with the crystallizer of circulation device in the method and apparatus of crystallization raffinose.In this invention, adopt pure water as recrystallisation solvent, the mass percentage concentration of initial raffinose is 60%, in crystallisation process, because the solubleness of raffinose in pure water is big, makes that the viscosity of crystallization solution is excessive, cause crystallization rate to descend, only temperature fall time just needs 50 hours more than, and the yield of simultaneously final raffinose is also lower.
Generally speaking, under the prior art condition, realize industrialization from the degreasing cottonseed meal (low cost, high yield, quick-reading flow sheets) production high purity raffinose, need respectively or on the whole raffinose extracting method, raffinose raffinate purification process and raffinose process for refining to be improved, wherein the improvement of raffinose extracting method being seemed is even more important, because the composition in the raffinose raffinate has determined the follow-up purification and the difficulty for the treatment of process.The method of from the degreasing cottonseed meal, extracting raffinose that a kind of technology is simple, have high cottonseed extraction yield, the content height of raffinose in the raffinose raffinate that obtains, the kind and the content of impurity are few, can help to simplify and purify and treating process, and improve to purify simultaneously and treating process in the yield of raffinose, the yield of final raising (high purity) raffinose product.
Summary of the invention
It is the improvement that raw material extracts the method that obtains raffinose raffinate that the present invention is primarily aimed at the degreasing cottonseed meal, aims to provide a kind of to the raffinose extraction yield height in the degreasing cottonseed meal, extraction solvent consumption extracting method few, simple to operate.
A kind of percolation extraction method of raffinose comprises with the degreasing cottonseed meal being that prepared using extracts solvent extraction, and the extracting solution that obtains obtains raffinose through purification and aftertreatment, it is characterized in that, the process that solvent extraction is extracted in described utilization is as follows:
(1) raw material degreasing cottonseed meal is packed into the diacolation post, adds in the diacolation post and extract solvent, soaked 30～60 minutes at 50～70 ℃, the volume of the extraction solvent of adding is 0.6～1 times of degreasing cottonseed meal stacking volume.
(2) under the keeping warm mode, carrying out diacolation operation in the diacolation post, add the extraction solvent continuously in the diacolation post when collecting percolate, is 3～5 times of degreasing cottonseed meal stacking volume until the volume of the percolate of collecting.
Degreasing cottonseed meal stacking volume: the degreasing cottonseed meal is packed into the diacolation post, and the degreasing cottonseed meal is in the volume under the free accumulation state, and its apparent density is a tap density; The tap density of degreasing cottonseed meal is about 0.77g/ml, i.e. per kilogram degreasing cottonseed meal stacking volume is about 1300ml.
It is that 70～85% methanol aqueous solution or concentration expressed in percentage by volume are that 70～85% aqueous ethanolic solution is for extracting solvent that the present invention preferably adopts concentration expressed in percentage by volume, because under 50～70 ℃, methanol aqueous solution or the solubleness in aqueous ethanolic solution of raffinose under this concentration is big, simultaneously, other composition meltage therein is little in the degreasing cottonseed meal, therefore methanol aqueous solution under this concentration or aqueous ethanolic solution are to the selective extraction rate height of the raffinose in the degreasing cottonseed meal, and the content of impurity is few in the raffinose raffinate, thereby improves the purity of raffinose in the extraction yield that improves raffinose.
The volume that is used to soak the extraction solvent of swelling degreasing cottonseed meal among the present invention is 0.6～1 times of degreasing cottonseed meal stacking volume, guarantees that the degreasing cottonseed meal can be fully immersed in to extract in the solvent.
The flow velocity of the extraction solvent of in the diacolation post, adding continuously among the present invention be preferably 0.2～1.0 times of degreasing cottonseed meal stacking volume/hour.In this flow rates, both can guarantee to extract solvent and the degreasing cottonseed meal has sufficient duration of contact, improve the utilization ratio of extracting solvent, can take into account throughput again.
The diacolation post that uses among the present invention can be a single-column, also can be the multicolumn series connection.During the multicolumn serial operation, after last post diacolation post diacolation is finished with deionized water reclaim obtain dilute methanol or Diluted Alcohol solution can be directly as the back swelling solvent of a diacolation post, avoid the distillation removal process of solvent, greatly reduce production energy consumption.
In order to improve the utilising efficiency of solvent, also can recycle in the following manner: with the deionized water diacolation post of flowing through from top to bottom solvent, control flow velocity be 0.5～1.5 times of degreasing cottonseed meal stacking volume/hour, collect the exit and contain the mixing liquid that extracts solvent and water, handle through distillation and reclaim solvent.
In the present invention, in the extracting solution that the degreasing cottonseed meal obtains after diacolation extracts, the content of raffinose is higher, with the butt is benchmark, the mass percent of raffinose can reach 35～40%, and the raffinose extraction yield is higher than 95%, and residual extraction solvent can be reclaimed fully in the cottonseed meal simultaneously.
The present invention adopts percolation to extract raffinose from the degreasing cottonseed meal, rely on and extract solvent and the inside and outside concentration difference of degreasing cottonseed meal fibrocyte, make solute from the main body of born of the same parents' internal diffusion outside born of the same parents mutually in, solvent is joined in the diacolation post for a part continuously, cell peripheral is the higher extracting solution of concentration originally, constantly replaced, keeping the inside and outside maximum concentration gradient of cell, quicken the stripping mass transfer by novel solvent or lower concentration extracting solution.And solvent from up to down flows equably, and infiltration is being carried out simultaneously with diffusion, and each layer raw material and solvent or extracting solution all keep certain concentration difference, therefore can significantly improve extraction rate and extraction effect, reduce solvent consumption simultaneously.
Because raffinose is soluble in water, aqueous ethanol, aqueous acetone isopolarity solvent, and other composition such as the equal water soluble of Partial Protein, carbohydrate and salt in the degreasing cottonseed meal, wherein the gossypol pigment can extract with 70% aqueous acetone, among the present invention, adopt aqueous ethanol or aqueous methanol as extracting solvent, this type of extracts solvent to the raffinose selectivity is good, perviousness is strong, leaching yield is high, security is good.
The useful effect that the present invention has is:
Method of the present invention not only can significantly reduce the consumption that extracts solvent under the prerequisite that guarantees certain raffinose extraction yield, reduce the energy consumption of solvent recuperation, and, the extraction solvent can be reclaimed fully, reduce the loss and the production cost of solvent greatly, help suitability for industrialized production.
The further processing of the raffinose raffinate that utilizes the present invention to obtain finally obtains the process of raffinose (high purity), comprises that wherein each step can adopt existing techniques in realizing.Below provide one of its implementation method, concrete operations are as follows:
(a) decolouring:
After the percolate that the present invention is obtained carries out concentration, adding water, to be made into solid content be 10% solution, regulate pH value to 4～6,30～60 ℃, join in the fixed bed that adsorbent A is housed with the flow velocity of 0.5～3BV/h, the effluent liquid that collection obtains is a destainer, is 5～10BV until the destainer volume of collecting.
Describedly add water to be made into solid content be in 10% the solution, solid content be meant quality that solution is dried to constant weight account for dry before the per-cent of solution quality, the also quality percentage composition sum of all solutes in the ie in solution, because composition more complicated in the solution, also may occur suspending or precipitation, when calculating the solution total mass, refer to the total mass of mixed system, promptly also comprise the quality of foreign material such as suspension or precipitation.
BV: bed volume refers to the bed volume that adsorbent A is loaded in the ADSORPTION IN A FIXED BED post;
BV/h: the volume of moving phase that per hour flows through the bed of adsorbent A filling is the multiple of fixed bed volume BV;
Described adsorbent A is that granulated active carbon, nonpolar macroporous type polystyrene polymeric adsorbent, low-pole macroporous type polystyrene polymeric adsorbent, nonpolar macroporous type acrylic acid series polymeric adsorbent, low-pole macroporous type acrylic acid series polymeric adsorbent, nonpolar gel type polystyrene are that polymeric adsorbent, low-pole gel type polystyrene are polymeric adsorbent, nonpolar gel-type acrylic acid series polymeric adsorbent or low-pole gel-type acrylic acid series polymeric adsorbent.
(b) fractionation by adsorption:
The destainer that 2～4B ' V ' is obtained via step (a), feed with the flow velocity of 0.5～3B ' V '/h and to make raffinose be adsorbed agent B absorption in the fixed bed that adsorbent B is housed, use again deionized water with the flow velocity drip washing fixed bed of 0.5～3B ' V '/h to reclaim the destainer in the fixed bed space, leacheate that obtains and destainer merge to be applied mechanically, use 2～4B ' V ' desorbing agent adsorbent B to be carried out desorb at last with the flow velocity of 0.5～3B ' V '/h, obtain containing the elutriant of raffinose, the temperature of adsorption separation process is controlled at 40～80 ℃; Elutriant obtains the raffinose crude product through removal of solvents;
Described desorbing agent is that concentration expressed in percentage by volume is that 20～60% methanol aqueous solution or concentration expressed in percentage by volume are 20～60% aqueous ethanolic solution;
B ' V ': bed volume refers to the bed volume that adsorbent B is loaded in the ADSORPTION IN A FIXED BED post;
B ' V '/h: the volume of moving phase that per hour flows through the bed of adsorbent B filling is the multiple of fixed bed volume B ' V ';
Described adsorbent B is that nonpolar macroporous type polystyrene polymeric adsorbent, nonpolar macroporous type acrylic acid series polymeric adsorbent, nonpolar gel type polystyrene are that polymeric adsorbent, nonpolar gel-type acrylic acid series polymeric adsorbent, granulated active carbon, bonding have C
18Silica gel or bonding C is arranged
30Silica gel.
(c) crystallization:
It is after 60～80% methanol aqueous solution or concentration expressed in percentage by volume are 60～80% aqueous ethanolic solution being dissolved in concentration expressed in percentage by volume under 50～85 ℃ that step (b) is obtained the raffinose crude product, rate of temperature fall with 0.5～2 ℃/min is cooled to 30～50 ℃, add raffinose crystal grain and induce crystallization, crystal separate out the back be cooled to 5～30 ℃ with the rate of temperature fall of 0.5～2 ℃/min after growing the grain 2～24 hours, get the raffinose elaboration 30～40 ℃ of vacuum-dryings after leaching crystal.
Embodiment
Below, describe content of the present invention in detail by embodiment, but the present invention is not limited thereto.
Embodiment 1: the percolate of preparation raffinose
The degreasing cottonseed meal (wherein, the mass percent of raffinose is 3.9%) be the screening of 1.8mm sieve through sieve aperture, take by weighing 1000 gram cottonseed meal and pack the diacolation post into (in the Φ 5.6cm * 70cm), filling evenly its stacking volume of back is about 1300 milliliters, add 780 ml volumes percentage concentrations again and be 75% aqueous ethanolic solution in the diacolation post, 55 ℃ are soaked down and made its abundant swelling in 30 minutes.Under the keeping warm mode, open diacolation column outlet valve, add concentration expressed in percentage by volume simultaneously from the diacolation column top continuously and be 75% aqueous ethanolic solution, the control flow velocity is in 12 ml/min, until collecting 4200 milliliters of percolates.Percolate by analysis, solid content (quality when solid content is meant solution is dried to constant weight account for dry before the per-cent of solution quality, be 4.2% down together), wherein, with butt (butt is meant the solid quality that obtains after the solution drying, and the quality summation of the whole solutes in the ie in solution is together following) meter, the mass percent of raffinose is 38.2%, and the raffinose extraction yield is 95.8%.
Add from the diacolation column top with deionized water, residual ethanol in the displacement cottonseed meal, the control flow velocity is 20 ml/min, collects the alcohol of exit lower concentration, again by concentrating and mode such as rectifying reclaims ethanol.
Embodiment 2: the percolate of preparation raffinose
The degreasing cottonseed meal (wherein, the mass percent of raffinose is 3.9%) be the screening of 1.8mm sieve through sieve aperture, taking by weighing 3000 gram cottonseed meal is respectively charged into the diacolation post of three same sizes (in the Φ 5.6cm * 70cm), the filling evenly mean value of the stacking volume of its degreasing cottonseed meal of back is about 1260 milliliters.At first, the about 760 ml volumes percentage concentrations of adding are 75% aqueous ethanolic solution in the diacolation post, and 55 ℃ of following immersions made the abundant swelling of degreasing cottonseed meal in 30 minutes.Under the keeping warm mode, open first diacolation column outlet valve, and be that 75% aqueous ethanolic solution adds continuously from the diacolation column top with concentration expressed in percentage by volume, the control flow velocity reaches 4000 milliliters until the percolate of collecting and ends in 8 ml/min.
Add from the diacolation column top with deionized water, residual ethanol in the displacement cottonseed meal, the control flow velocity is 20 ml/min, collects 760 milliliters of ethanol extracts, simultaneously it is fed continuously in second diacolation post, feed the back immersion under 55 ℃ that finishes and made the abundant swelling of degreasing cottonseed meal in 30 minutes.The control flow velocity is in 8 ml/min, and feeding concentration expressed in percentage by volume from second diacolation column top is 75% aqueous ethanolic solution, reaches 4000 milliliters until the percolate of collecting and ends.
Add from the diacolation column top with deionized water, residual ethanol in the displacement cottonseed meal, the control flow velocity is 20 ml/min, collects 760 milliliters of ethanol extracts, simultaneously it is fed continuously in the 3rd diacolation post, feeding finishes to soak under 55 ℃ and made the abundant swelling of degreasing cottonseed meal in 30 minutes.The control flow velocity is in 8 ml/min, feeds concentration expressed in percentage by volume from the 3rd diacolation column top and be 75% aqueous ethanolic solution, reaches 4000 milliliters up to the percolate of collecting and ends.
Merge all percolates, by analysis, solid content is 4.8%, and wherein, in butt, the mass percent of raffinose is 36.5%, and the raffinose extraction yield is 98%.
Add from the diacolation column top with deionized water at last, residual ethanol in the displacement cottonseed meal, the control flow velocity is 20 ml/min, collects the 760 milliliters of aqueous ethanolic solutions in exit separately.
Embodiment 3: the preparation high purity raffinose
(a) will be concentrated into original volume 1/10 by 1900 milliliters of percolates that embodiment 1 method prepares, and add water and be mixed with solution (wherein solid content is 10%), add mass percentage concentration and be 5% salt acid for adjusting pH value to 5.
About 230 gram granulated active carbons (adsorbent A) are packed into and are of a size of in the adsorption column of Φ 5.6cm * 40cm, and post bed volume BV is 980mL.
By the ADSORPTION IN A FIXED BED post of granulated active carbon is housed, temperature is controlled at 40 ℃ with the flow velocity of the 1.0BV/h aqueous solution after with above-mentioned adjusting pH value.Collecting the effluent liquid (being destainer) of sample process on the ADSORPTION IN A FIXED BED post, is 10BV until the destainer of collecting, its color more shallow (colour is less than 10% of last sample aqueous solution colour).In butt, cottonseed saccharic amount per-cent is 50.6% in the destainer.With the flow velocity flushing adsorption column of 1.5BV deionized water with 1.0BV/h, collect in the water lotion that obtains and also contain a spot of raffinose, can continue recycled.Whole process, adsorption column temperature are controlled at 40 ℃.The effusive destainer of last sample process is analyzed through HPLC, and the raffinose rate of recovery is 95%.
Be 60% the aqueous ethanolic solution flow velocity flushing adsorption column with 1.0BV/h with the concentration expressed in percentage by volume of 2BV at last, elutriant is a scarlet; With the ethanol in the deionized water displacement adsorption column, the decolouring that adsorption column regeneration can directly be entered is next time operated again.
(b) the 1700 pretreated HZ816 resins of gram (adsorbent B) are packed into and are of a size of in the adsorption column of Φ 5.6cm * 97cm, post bed volume B ' V ' is about 2400mL.Last sample liquid is the raffinose destainer of step (a) gained, and wherein solid content is 10%.Flow velocity with 1.0B ' V '/h feeds above-mentioned raffinose destainer 2.5B ' V ' continuously in the ADSORPTION IN A FIXED BED post, also contain a small amount of raffinose in the effluent liquid that last sample process is collected, and can directly recycle.Last sample finishes, and earlier with the flow velocity flushing adsorption column of 2B ' V ' deionized water with 1.5B ' V '/h, removes the destainer of adsorption column internal adsorption agent voids left, and the water lotion that obtains can be recycled; Again with 2B ' V ' concentration expressed in percentage by volume be 40% aqueous ethanolic solution with 1.0B ' V '/h flow velocity flushing adsorption column, desorb HZ816 resin, the raffinose in the wash-out HZ816 resin is collected the elutriant that obtains containing raffinose.The adsorption column temperature is controlled at 60 ℃ in the whole process.The spray-dried raffinose crude product that obtains of elutriant, analyzing wherein through HPLC, the mass percent of raffinose is 80%.
Use 2B ' V ' deionized water to make the HZ816 resin regeneration at last with the ethanol in the flow velocity displacement adsorption column of 2B ' V '/h.
(c) gained raffinose crude product being dissolved in 500 ml volumes percentage concentrations under 80 ℃ is 70% aqueous ethanolic solution, slowly cooling cooling, and rate of temperature fall is 1 ℃/min.Add 170～200 order raffinose crystal grain (being crystal seed), 1.0 grams after being cooled to 40 ℃ and induce crystallization, continue slowly to be cooled to 15 ℃ with same speed again, growing the grain 12 hours, filter, washing leaching cake, filter cake gets the raffinose elaboration in 40 ℃ of following vacuum-dryings, and crystalline mother solution and destainer merge to be applied mechanically.
Analyze through HPLC, cottonseed saccharic amount per-cent is 98.2% in the gained raffinose elaboration.
Claims (4)
1. the percolation extraction method of a raffinose comprises with the degreasing cottonseed meal being that prepared using extracts solvent extraction, and the extracting solution that obtains obtains raffinose through purification and aftertreatment, it is characterized in that, the process that solvent extraction is extracted in described utilization is as follows:
(1) raw material degreasing cottonseed meal is packed into the diacolation post, adds in the diacolation post and extract solvent, soaked 30～60 minutes at 50～70 ℃, the volume of the extraction solvent of adding is 0.6～1 times of degreasing cottonseed meal stacking volume;
(2) under the keeping warm mode, carrying out diacolation operation in the diacolation post, add the extraction solvent continuously in the diacolation post when collecting percolate, is 3～5 times of degreasing cottonseed meal stacking volume until the volume of the percolate of collecting;
Wherein, described extraction solvent is that concentration expressed in percentage by volume is that 70～85% methanol aqueous solution or concentration expressed in percentage by volume are 70～85% aqueous ethanolic solution.
2. percolation extraction method according to claim 1 is characterized in that: the flow velocity of the extraction solvent of in the diacolation post, adding continuously be 0.2～1.0 times of degreasing cottonseed meal stacking volume/hour.
3. percolation extraction method according to claim 1 is characterized in that: described diacolation post is single-column or multicolumn series connection.
4. percolation extraction method according to claim 1, it is characterized in that: afterwards in step (2), with deionized water with 0.5～1.5 times of degreasing cottonseed meal stacking volume/hour the flow velocity diacolation post of flowing through, collect the exit and contain the mixing liquid that extracts solvent and water, handle the recovery solvent through distillation.
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| CN101265280A (en) * | 2007-04-13 | 2008-09-17 | 北京中棉紫光生物科技有限公司 | Method for extracting raffinose from cottonseed scum |
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| CN101265280A (en) * | 2007-04-13 | 2008-09-17 | 北京中棉紫光生物科技有限公司 | Method for extracting raffinose from cottonseed scum |
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