CN106318995A - Method for preparing fructan and gluconic acid by using inulin - Google Patents
Method for preparing fructan and gluconic acid by using inulin Download PDFInfo
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- C12P19/00—Preparation of compounds containing saccharide radicals
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Abstract
The invention discloses a method for preparing fructan and gluconic acid by using inulin and belongs to the technical field of separation and purification. The method comprises the following steps: by taking commercially available inulin as a raw material, preparing a sucrase hydrating solution; preparing glucose oxidase treating fluid; preparing an ultrafiltration separating solution; preparing a gluconic acid separating solution; preparing a gluconic acid concentrated solution; preparing a fructan separating solution; preparing fructo-oligosaccharide powder and polyfructose powder, thus obtaining two fructan powder and gluconic acid solution with the mass percent concentration of 10 to 15 percent. According to the technical scheme provided by the invention, a product with high added value is produced by the operations of enzymatic hydrolysis, separation and concentration; the product is high in purity and definite in application; the quality of the product meets the requirement of market; used production equipment is industrial equipment, namely separating devices such as a nanofiltration device, an ultrafiltration device, a reverse osmosis device and an electrodialysis device; the production equipment is mild in separation condition and high in separation efficiency; the adopted raw materials and solvent can be completely utilized, and no three wastes are discharged; the method is a classical green technology and facilitates popularization and application.
Description
One, technical field
The invention belongs to separating and purifying technology field, be specifically related to a kind of utilize inulin to prepare levan and gluconic acid
Method.
Two, background technology
Inulin be birds of the same feather flock together right be 2～60, formed and with Portugal by β-(2,1) glycosidic bond dehydration polymerization with fructose units
The carbohydrate that grape sugar unit terminates.Inulin is preferable functional food ingredient, is the most also to produce oligofructose, Gao Guo
The very good material of the product such as syrup, fructose.Additionally, inulin also has controls blood fat, reduction blood glucose, the suction of promotion mineral
Receive, make intestinal bifidobacteria increase, anti-constipation and the treatment function such as obesity, thus be widely used in health product, DFA
The fields such as supplement, demand is the hugest.
The existing method preparing inulin, such as Application No. 201210565275.0, entitled " a kind of is former with dry Jerusalem artichoke
The method of inulin prepared by material ", the patent describe and prepare dry Jerusalem artichoke with Jerusalem artichoke or Herba Cichorii for raw material, then carry out countercurrent extraction,
Extracting solution, through remove impurity and activated carbon decolorizing, concentrates through NF membrane after entering ion exchange column desalination, then spray drying obtains height
The inulin of purity.The weak point of the method is: 1. activated carbon decolorizing non-selectivity, also sloughs part inulin during decolouring, impact
Inulin recovery rate；2. the inulin concentration after nanofiltration concentrates is only 20～30%, and directly carrying out spray drying needs to expend substantial amounts of
Energy；3. not sloughing the macromolecule impurities such as albumen, the purity of product is the highest, has a poor flavour；4. inulin terminal glucose is not excised,
Glucose is the high heating value carbon source that human body needs, unfavorable on diabetics and affect inulin local flavor.The most such as Application No.
201510152269.6, patent of invention entitled " method separating high Polyfructose. from inulin ", the patent describes with commonly
Level inulin is raw material, utilizes oligofructose and high Polyfructose. molten in dimethyl sulfoxide or dimethylformamide and alcohol or ketone solvent
The difference of Xie Du realizes the separation of the two, and precipitation is dried to obtain highly purified high Polyfructose..The weak point of the method is:
1. inulin is dissolved with organic solvent dimethyl sulfoxide or dimethylformamide.Owing to organic solvent boiling point is low, the response rate is low, solvent
Loss seriously and often easy firing blast, production environment must be the most explosion-proof；Additionally, many organic solvents have stimulation or poison to human body
Side effect, operator must close protection；Dimethyl sulfoxide and dimethylformamide are all with bitterness or off-odor, impact height
Polyfructose. local flavor；2. with dehydrated alcohol be second solvent separate high and low Polyfructose..Owing to dehydrated alcohol consumption is big, high volatility,
Being difficult to reclaim completely, therefore, production cost is higher；The most not reclaiming the oligofructose in supernatant, wasting can be as food
Additive and the valuable materials of enriching substance, add production cost.
Three, summary of the invention
The present invention be directed to the deficiency of existing inulin separating and purifying technology, it is provided that one prepares levan with inulin for raw material
And the method for gluconic acid.The method by enzymolysis, separate, the operation such as concentration, produce high-purity, the oligomeric fruit of high added value
Sugar, polyfructosan and gluconic acid product, increase economic efficiency.
The principle of the present invention is: inulin be birds of the same feather flock together right be 2～60, taken off by β-(2,1) glycosidic bond with fructose units
The carbohydrate that water is polymerized and terminates with glucose unit, the β-D-furan in the catalysis non-reducing sugar that saccharase can be special
Fructose glycosidic bond of muttering hydrolyzes, and may act on inulin, cuts terminal glucose, generates free glucose and the fruit of few a part glucose
Polysaccharide；Nanofiltration/ultrafiltration is under pressure reduction motive force effect, and molecular diameter can pass through less than the solute in nanofiltration/ultrafilter membrane aperture and receives
Filter/ultrafilter membrane, molecular diameter is then trapped more than the solute in nanofiltration/ultrafilter membrane aperture, the most just realizes separating；Fructus Vitis viniferae sugar
Son amount be only 180Da, inulin levan molecular weight distribution 342～9600Da, both significant differences, therefore can use nanofiltration/surpass
Filter is separated；Glucoseoxidase energy oxidation of beta-D-Glucose, generates electronegative gluconic acid；Electronegative Fructus Vitis viniferae
Saccharic acid under DC electric field effect, can by anion being had the anion exchange membrane of selective penetrated property to anode directional migration,
And levan neutral, then both separate；Reverse osmosis is under pressure reduction motive force effect, through hydrone, retains
Salt and the membrane separation technique of little molecule solute；Gluconic acid solution through electrodialysis separation and the poly through ultrafiltration/nanofiltration separation
Fructose and oligofructose solution, again through membrance concentration, obtain gluconic acid, oligofructose and polyfructosan concentrated solution the most respectively；Will
The oligofructose and the polyfructosan concentrated solution that obtain are spray-dried, and just prepare oligofructose and polyfructosan powder.
It is an object of the invention to be realized by following approach, a kind of side utilizing inulin to prepare levan and gluconic acid
Method, with commercially available inulin as raw material, through preparing saccharase hydrating solution, prepares glucoseoxidase treatment fluid, and preparation ultrafiltration divides
Chaotropic, prepares gluconic acid separation liquid, prepares gluconic acid concentrated solution, prepares levan separation liquid, prepares oligofructose powder
With the step of polyfructosan powder, prepare two kinds of levan powder and mass percentage concentration be 10～15% gluconic acid molten
Liquid.Its concrete processing step is as follows:
(1) saccharase hydrating solution is prepared
First in rustless steel enzymatic hydrolysis reaction still, pump into pure water, according still further to inulin quality and pure water volume ratio (kg/L)
It is the ratio of 1: 10～20, under agitation inulin is dissolved in pure water, then open the heat riser of this hydrolytic reaction pot,
The aqueous solution dissolving inulin is warming up to 40～45 DEG C and is incubated 10～15min, according to saccharase and inulin mass ratio (kg/
Kg) be 1: 150～300 ratio add saccharase, then temperature be 40～45 DEG C, mixing speed be 60～100r/min
Under the conditions of process 10～16h, just prepare saccharase hydrating solution, prepare glucoseoxidase treatment fluid for lower step.
(2) glucoseoxidase treatment fluid is prepared
After (1st) step completes, saccharase hydrating solution prepared by (1st) step is warming up to 50～60 DEG C and be incubated 10～
15min, adds glucose oxidation according to the ratio that glucoseoxidase and inulin mass ratio (kg/kg) are 1: 100～200
Enzyme, then temperature be 50～60 DEG C, mixing speed be to process 1～2h under conditions of 60～100r/min, just prepare Fructus Vitis viniferae
Carbohydrate oxidase treatment fluid, prepares ultra-filtration and separation liquid for lower step.
(3) ultra-filtration and separation liquid is prepared
After (2nd) step completes, glucoseoxidase treatment fluid prepared by (2nd) step is pumped into molecular cut off is 10000
～in the ultrafilter of 30000Da, carry out ultrafiltration for the first time under gauge pressure is 0.2～0.5MPa, until ultra-filter retentate for the first time
When being 1: 5～8 with the ratio (L/L) of first time ultrafiltration filtered solution volume only.Collect ultrafiltration filtered solution and first time for the first time respectively
Ultra-filter retentate, to the first time ultra-filter retentate collected, adds this trapped fluid volume 4～pure water of 6 times, again carries out the
Second ultrafiltration, second time ultra-filter retentate and second time ultrafiltration filtered solution when the gauge pressure of ultrafiltration for the second time and stopping second time ultrafiltration
The ratio of volume is all identical with ultrafiltration for the first time.After ultrafiltration completes for the second time, collect second time ultrafiltration filtered solution and second time respectively
Ultra-filter retentate.To the second time ultrafiltration filtered solution collected, merge with the first time ultrafiltration filtered solution collected, i.e. prepare ultrafiltration
Separate liquid, prepare gluconic acid separation liquid for lower step；To the second time ultra-filter retentate collected, dry after mixing with Semen Maydis powder
Dry, as feedstuff flavour enhancer.
(4) gluconic acid separation liquid is prepared
After (3rd) step completes, ultra-filtration and separation liquid pump prepared by (3rd) step is entered in cathodic coating electrodialyzer, at voltage be
150～200V, electric current is 1～3A, and intake pressure is 0.5～2kg/cm2Under conditions of carry out electrodialysis process and collect electric osmose
The liquid flowed out from concentrated water spout and fresh water mouth in parser.To the liquid flowed out from fresh water mouth collected, containing oligofructose and poly
Fructose, is levan solution, is used for preparing levan separation liquid；To the liquid flowed out from concentrated water spout collected, containing glucose
Acid, i.e. prepares gluconic acid separation liquid, prepares gluconic acid concentrated solution for lower step.
(5) gluconic acid concentrated solution is prepared
After (4th) step completes, the gluconic acid separation liquid pump (4th) step prepared enters in counter-osmosis device, is 0.7 in gauge pressure
～carry out reverse osmosis concentration under conditions of 0.9MPa, until in reverse osmosis trapped fluid gluconic acid mass percentage concentration reach 10～
When 15% only.Collect reverse osmosis filtered solution and trapped fluid respectively, to the reverse osmosis filtered solution collected, pump into wastewater disposal basin and carry out biochemistry
Process, rear discharge up to standard；To the reverse osmosis trapped fluid collected, it is gluconic acid mass percentage concentration and reaches the Portugal of 10～15%
Grape saccharic acid concentrated solution, is used for preparing protein coagulating agent, food preservative and cement water reducing agent etc..
(6) levan separation liquid is prepared
After (4th) step completes, the levan solution (4th) step prepared, pumping into molecular cut off is 800～1500Da
In nanofiltration/ultrafilter, under gauge pressure is 0.2～0.5MPa, carry out nanofiltration/ultrafiltration for the first time, until nanofiltration/ultrafiltration for the first time cuts
When to stay the ratio of liquid and first time nanofiltration/ultrafiltration filtered solution volume be 1: 5～8 (L/L) only.Collect nanofiltration/ultrafiltration for the first time respectively
Filtered solution and for the first time nanofiltration/ultra-filter retentate, to the first time nanofiltration/ultra-filter retentate collected, add this trapped fluid volume 4
～the pure water of 6 times, again carry out second time nanofiltration/ultrafiltration, for the second time gauge pressure of nanofiltration/ultrafiltration, and stop second time nanofiltration/
During ultrafiltration the ratio of second time nanofiltration/ultra-filter retentate and second time nanofiltration/ultrafiltration filtered solution volume all with first time nanofiltration/ultrafiltration
Identical.After nanofiltration/ultrafiltration completes for the second time, collect second time nanofiltration/ultrafiltration filtered solution respectively and second time nanofiltration/ultrafiltration retains
Liquid.To the second time nanofiltration/ultrafiltration filtered solution collected, merging with the first time nanofiltration/ultrafiltration filtered solution collected, this amalgamation liquid contains
Oligofructose, prepares oligofructose powder for lower step；To the second time nanofiltration/ultra-filter retentate collected, containing polyfructosan, use
Polyfructosan powder is prepared in lower step.To this amalgamation liquid collected and the second time nanofiltration/ultra-filter retentate of collection, it is collectively referred to as fruit
Polysaccharide separation liquid, i.e. prepares levan separation liquid.
(7) oligofructose powder and polyfructosan powder are prepared
After (6th) step completes, the amalgamation liquid of the nanofiltration containing the oligofructose/ultrafiltration filtered solution (6th) step prepared pumps into
Molecular cut off is in the nanofiltration device of 200～600Da, carries out nanofiltration concentration under conditions of gauge pressure is 0.7～0.9MPa, until
In nanofiltration trapped fluid, oligofructose mass percentage concentration reaches to stop when 15～20%.Collect nanofiltration filtered solution respectively and nanofiltration retains
Liquid, to the nanofiltration filtered solution collected, pumps into wastewater disposal basin and processes, rear discharge up to standard；To the nanofiltration trapped fluid collected, pump into spray dried
Dry machine, inlet temperature be 150～180 DEG C, leaving air temp be 90～100 DEG C, spraying centrifuge speed be 5000～8000r/
It is spray-dried under conditions of min, just prepares the oligofructose powder of white.(6) step collected containing polyfructosan
Nanofiltration/ultra-filter retentate for the second time, pumps in the ultrafilter that molecular cut off is 1000～2500Da, gauge pressure be 0.7～
It is concentrated by ultrafiltration under conditions of 0.9MPa, during until polyfructosan mass percentage concentration reaches 15～20% in ultra-filter retentate
Only.Collect ultrafiltration filtered solution and ultra-filter retentate respectively, to the ultrafiltration filtered solution collected, pump into wastewater disposal basin and process, heel row up to standard
Put；To the ultra-filter retentate collected, pump into spray dryer, inlet temperature be 150～180 DEG C, leaving air temp be 90～100
DEG C, spraying centrifuge speed be to be spray-dried under conditions of 5000～8000r/min, just prepare the polyfructosan of white
Powder.
After the present invention uses technique scheme, mainly have the following effects:
1, the technology of the present invention is with commercially available inulin as raw material, and the product of preparation is respectively the oligofructose powder of the degree of polymerization 2～9
Reaching the gluconic acid solution of 10～15% with the degree of polymerization polyfructosan powder more than 9 and mass percentage concentration, product is pure
Degree height, quality meets market demands.
2, the product purpose that the technology of the present invention is prepared is clear and definite, and wherein the strand of oligofructose is shorter, sugariness and dissolving
Degree is bigger, and physiologically active is significantly stronger than inulin, is more suitable for as diabetes patient, the food additive of obesity patient and supplement
Agent；Without oligofructose in polyfructosan, without sweet taste, without calorific value, it is suitable for use as the filler of old people food；Gluconic acid is then to use
Way protein coagulating agent widely, antidote and water reducer etc..
3, used by the inventive method, production equipment is industrial equipment, such as nanofiltration, ultrafiltration, reverse osmosis and electrodialysis etc.
Segregation apparatus, separation condition is gentle, and separation efficiency is high, can realize raw material all of, it is achieved whole recovery of solvent are sharp again
With, discharge without " three wastes ", be typical green public skill, be suitable for large-scale production.
Four, detailed description of the invention
Below in conjunction with detailed description of the invention, further illustrate the present invention.
Embodiment 1
(1) saccharase hydrating solution is prepared
First in rustless steel enzymatic hydrolysis reaction still, pump into pure water, according still further to inulin quality and pure water volume ratio (kg/L)
It is the ratio of 1: 10, under agitation inulin is dissolved in pure water, then open the heat riser of this hydrolytic reaction pot, by molten
The aqueous solution solving inulin is warming up to 40 DEG C and is incubated 10min, is 1: 150 according to saccharase and inulin mass ratio (kg/kg)
Ratio adds saccharase, then temperature be 40 DEG C, mixing speed be 60r/min under conditions of process 10h, just prepare sucrose
Enzyme hydrolysis solution, prepares glucoseoxidase treatment fluid for lower step.
(2) glucoseoxidase treatment fluid is prepared
After (1st) step completes, saccharase hydrating solution prepared by (1st) step is warming up to 50 DEG C and is incubated 10min, according to
Glucoseoxidase and inulin mass ratio (kg/kg) be 1: 100 ratio add glucoseoxidase, be then 50 in temperature
DEG C, mixing speed be to process 1h under conditions of 60r/min, just prepare glucoseoxidase treatment fluid, super for the preparation of lower step
Filter separates liquid.
(3) ultra-filtration and separation liquid is prepared
After (2nd) step completes, glucoseoxidase treatment fluid prepared by (2nd) step is pumped into molecular cut off is
In the ultrafilter of 10000Da, under gauge pressure is 0.2MPa, carry out ultrafiltration for the first time, until ultra-filter retentate is with for the first time for the first time
When the ratio (L/L) of ultrafiltration filtered solution volume is 1: 5 only.Collect ultrafiltration filtered solution and for the first time ultra-filter retentate for the first time respectively,
To collect first time ultra-filter retentate, add the pure water of this trapped fluid volume 4 times, again carry out second time ultrafiltration, second
The gauge pressure of secondary ultrafiltration and stop during second time ultrafiltration the ratio of second time ultra-filter retentate and second time ultrafiltration filtered solution volume all with
Ultrafiltration is identical for the first time.After ultrafiltration completes for the second time, collect second time ultrafiltration filtered solution and second time ultra-filter retentate respectively.Right
The second time ultrafiltration filtered solution collected, merges with the first time ultrafiltration filtered solution collected, i.e. prepares ultra-filtration and separation liquid, under being used for
Step prepares gluconic acid separation liquid；To the second time ultra-filter retentate collected, it is dried after mixing with Semen Maydis powder, as feedstuff flavour enhancing
Agent.
(4) gluconic acid separation liquid is prepared
After (3rd) step completes, ultra-filtration and separation liquid pump prepared by (3rd) step is entered in cathodic coating electrodialyzer, at voltage be
150V, electric current is 1A, and intake pressure is 0.5kg/cm2Under conditions of carry out electrodialysis process and collect in electrodialyzer from dense water
The liquid that mouth and fresh water mouth flow out.To the liquid flowed out from fresh water mouth collected, containing oligofructose and polyfructosan, it is fruit poly-
Sugar juice, is used for preparing levan separation liquid；To the liquid flowed out from concentrated water spout collected, containing gluconic acid, i.e. prepare Portugal
Grape saccharic acid separation liquid, prepares gluconic acid concentrated solution for lower step.
(5) gluconic acid concentrated solution is prepared
After (4th) step completes, the gluconic acid separation liquid pump (4th) step prepared enters in counter-osmosis device, in gauge pressure is
Reverse osmosis concentration is carried out, during until gluconic acid mass percentage concentration reaches 10% in reverse osmosis trapped fluid under conditions of 0.7MPa
Only.Collect reverse osmosis filtered solution and trapped fluid respectively, to the reverse osmosis filtered solution collected, pump into wastewater disposal basin and carry out biochemical treatment,
Discharge after up to standard；To collect reverse osmosis trapped fluid, be gluconic acid mass percentage concentration reach 10% gluconic acid dense
Contracting liquid, is used for preparing protein coagulating agent, food preservative and cement water reducing agent etc..
(6) levan separation liquid is prepared
After (4th) step completes, levan solution prepared by (4th) step, pump into the nanofiltration device that molecular cut off is 800Da
In, under gauge pressure is 0.2MPa, carry out nanofiltration for the first time, until nanofiltration trapped fluid and nanofiltration filtered solution volume for the first time for the first time
Ratio when being 1: 5 (L/L) only.Collect nanofiltration filtered solution and for the first time nanofiltration trapped fluid for the first time respectively, to the first time collected
Nanofiltration trapped fluid, adds the pure water of this trapped fluid volume 4 times, again carry out second time nanofiltration, the gauge pressure of nanofiltration for the second time, and
Stop second time nanofiltration trapped fluid during second time nanofiltration all identical with nanofiltration for the first time with the ratio of second time nanofiltration filtered solution volume.
After nanofiltration completes for the second time, collect second time nanofiltration filtered solution and second time nanofiltration trapped fluid respectively.The second time collected is received
Filter filtered solution, merges with the first time nanofiltration filtered solution collected, and this amalgamation liquid contains oligofructose, prepares oligofructose for lower step
Powder；To the second time nanofiltration trapped fluid collected, containing polyfructosan, prepare polyfructosan powder for lower step.Collection is somebody's turn to do
The second time nanofiltration trapped fluid of amalgamation liquid and collection, is collectively referred to as levan separation liquid, i.e. prepares levan separation liquid.
(7) oligofructose powder and polyfructosan powder are prepared
After (6th) step completes, the amalgamation liquid of the nanofiltration filtered solution containing oligofructose (6th) step prepared pumps into and retains point
Son amount is in the nanofiltration device of 200Da, carries out nanofiltration concentration under conditions of gauge pressure is 0.7MPa, until oligomeric in nanofiltration trapped fluid
Fructose mass percentage concentration reaches to stop when 15%.Collect nanofiltration filtered solution and nanofiltration trapped fluid respectively, the nanofiltration collected is filtered
Liquid, pumps into wastewater disposal basin and processes, rear discharge up to standard；To the nanofiltration trapped fluid collected, pump into spray dryer, in inlet temperature be
150 DEG C, leaving air temp be 90 DEG C, spraying centrifuge speed be to be spray-dried under conditions of 5000r/min, just prepare white
The oligofructose powder of color.The second time nanofiltration trapped fluid containing polyfructosan collecting (6) step, pumping into molecular cut off is
In the ultrafilter of 1000Da, it is concentrated by ultrafiltration under conditions of gauge pressure is 0.7MPa, until polyfructosan in ultra-filter retentate
Mass percentage concentration reaches to stop when 15%.Collect ultrafiltration filtered solution and ultra-filter retentate respectively, to the ultrafiltration filtered solution collected, pump
Enter wastewater disposal basin to process, rear discharge up to standard；To the ultra-filter retentate collected, pump into spray dryer, inlet temperature be 150 DEG C,
Leaving air temp is 90 DEG C, spraying centrifuge speed is to be spray-dried under conditions of 5000r/min, just prepares white many
Polyfructose. powder.
Embodiment 2
(1) saccharase hydrating solution is prepared
First in rustless steel enzymatic hydrolysis reaction still, pump into pure water, according still further to inulin quality and pure water volume ratio (kg/L)
It is the ratio of 1: 15, under agitation inulin is dissolved in pure water, then open the heat riser of this hydrolytic reaction pot, by molten
The aqueous solution solving inulin is warming up to 42 DEG C and is incubated 12min, is 1: 225 according to saccharase and inulin mass ratio (kg/kg)
Ratio adds saccharase, then temperature be 42 DEG C, mixing speed be 80r/min under conditions of process 13h, just prepare sucrose
Enzyme hydrolysis solution, prepares glucoseoxidase treatment fluid for lower step.
(2) glucoseoxidase treatment fluid is prepared
After (1st) step completes, saccharase hydrating solution prepared by (1st) step is warming up to 55 DEG C and is incubated 12min, according to
Glucoseoxidase and inulin mass ratio (kg/kg) be 1: 150 ratio add glucoseoxidase, be then 55 in temperature
DEG C, mixing speed be to process 1.5h under conditions of 80r/min, just prepare glucoseoxidase treatment fluid, prepare for lower step
Ultra-filtration and separation liquid.
(3) ultra-filtration and separation liquid is prepared
After (2nd) step completes, glucoseoxidase treatment fluid prepared by (2nd) step is pumped into molecular cut off is
In the ultrafilter of 20000Da, under gauge pressure is 0.4MPa, carry out ultrafiltration for the first time, until ultra-filter retentate is with for the first time for the first time
When the ratio (L/L) of ultrafiltration filtered solution volume is 1: 6.5 only.Collect ultrafiltration filtered solution and ultrafiltration for the first time for the first time respectively to retain
Liquid, to the first time ultra-filter retentate collected, adds the pure water of this trapped fluid volume 5 times, again carries out second time ultrafiltration, the
When the gauge pressure of second ultrafiltration and stopping second time ultrafiltration, second time ultra-filter retentate is equal with the ratio of second time ultrafiltration filtered solution volume
Identical with first time ultrafiltration.After ultrafiltration completes for the second time, collect second time ultrafiltration filtered solution and second time ultra-filter retentate respectively.
To the second time ultrafiltration filtered solution collected, merge with the first time ultrafiltration filtered solution collected, i.e. prepare ultra-filtration and separation liquid, be used for
Lower step prepares gluconic acid separation liquid；To the second time ultra-filter retentate collected, it is dried after mixing with Semen Maydis powder, increases as feedstuff
Taste agent.
(4) gluconic acid separation liquid is prepared
After (3rd) step completes, ultra-filtration and separation liquid pump prepared by (3rd) step is entered in cathodic coating electrodialyzer, at voltage be
175V, electric current is 2A, and intake pressure is 1.25kg/cm2Under conditions of carry out electrodialysis process and collect in electrodialyzer from dense
The liquid that the mouth of a river and fresh water mouth flow out.To the liquid flowed out from fresh water mouth collected, containing oligofructose and polyfructosan, it is fruit
Polysaccharide solution, is used for preparing levan separation liquid；To the liquid flowed out from concentrated water spout collected, containing gluconic acid, i.e. prepare
Gluconic acid separation liquid, prepares gluconic acid concentrated solution for lower step.
(5) gluconic acid concentrated solution is prepared
After (4th) step completes, the gluconic acid separation liquid pump (4th) step prepared enters in counter-osmosis device, in gauge pressure is
Reverse osmosis concentration is carried out, until gluconic acid mass percentage concentration reaches 12.5% in reverse osmosis trapped fluid under conditions of 0.8MPa
Time only.Collect reverse osmosis filtered solution and trapped fluid respectively, to the reverse osmosis filtered solution collected, pump into wastewater disposal basin and carry out at biochemistry
Reason, rear discharge up to standard；To the reverse osmosis trapped fluid collected, it is gluconic acid mass percentage concentration and reaches the glucose of 12.5%
Acid concentrated solution, is used for preparing protein coagulating agent, food preservative and cement water reducing agent etc..
(6) levan separation liquid is prepared
After (4th) step completes, levan solution prepared by (4th) step, pump into the ultrafiltration that molecular cut off is 1000Da
In device, under gauge pressure is 0.4MPa, carry out ultrafiltration for the first time, until ultra-filter retentate and ultrafiltration filtered solution for the first time for the first time
When long-pending ratio is 1: 6.5 (L/L) only.Collect for the first time ultrafiltration filtered solution and for the first time ultra-filter retentate respectively, to the collected
Ultra-filter retentate, adds the pure water of this trapped fluid volume 5 times, again carries out second time ultrafiltration, the table of ultrafiltration for the second time
Pressure, and stop during second time ultrafiltration the ratio of second time ultra-filter retentate and second time ultrafiltration filtered solution volume all with first time ultrafiltration
Identical.After ultrafiltration completes for the second time, collect second time ultrafiltration filtered solution and second time ultra-filter retentate respectively.To second collected
Secondary ultrafiltration filtered solution, merges with the first time ultrafiltration filtered solution collected, and this amalgamation liquid contains oligofructose, prepares oligomeric for lower step
Fructose powder；To the second time ultra-filter retentate collected, containing polyfructosan, prepare polyfructosan powder for lower step.To collection
This amalgamation liquid and the second time ultra-filter retentate of collection, be collectively referred to as levan separation liquid, i.e. prepare levan separation liquid.
(7) oligofructose powder and polyfructosan powder are prepared
After (6th) step completes, the amalgamation liquid of the nanofiltration containing the oligofructose/ultrafiltration filtered solution (6th) step prepared pumps into
Molecular cut off is in the nanofiltration device of 400Da, carries out nanofiltration concentration under conditions of gauge pressure is 0.8MPa, until nanofiltration trapped fluid
Middle oligofructose mass percentage concentration reaches to stop when 17.5%.Collect nanofiltration filtered solution and nanofiltration trapped fluid respectively, to collect
Nanofiltration filtered solution, pumps into wastewater disposal basin and processes, rear discharge up to standard；To the nanofiltration trapped fluid collected, pump into spray dryer, at air intake
Temperature is 165 DEG C, leaving air temp is 95 DEG C, spraying centrifuge speed is to be spray-dried under conditions of 6500r/min, just system
For the oligofructose powder going out white.The second time ultra-filter retentate containing polyfructosan collecting (6) step, pumps into and retains molecule
In the amount ultrafilter for 2000Da, it is concentrated by ultrafiltration under conditions of gauge pressure is 0.8MPa, until poly in ultra-filter retentate
Fructose mass percentage concentration reaches to stop when 17.5%.Collect ultrafiltration filtered solution and ultra-filter retentate respectively, to the ultrafiltration filter collected
Cross liquid, pump into wastewater disposal basin and process, rear discharge up to standard；To the ultra-filter retentate collected, pump into spray dryer, in inlet temperature be
165 DEG C, leaving air temp be 95 DEG C, spraying centrifuge speed be to be spray-dried under conditions of 6500r/min, just prepare white
The polyfructosan powder of color.
Embodiment 3
(1) saccharase hydrating solution is prepared
First in rustless steel enzymatic hydrolysis reaction still, pump into pure water, according still further to inulin quality and pure water volume ratio (kg/L)
It is the ratio of 1: 20, under agitation inulin is dissolved in pure water, then open the heat riser of this hydrolytic reaction pot, by molten
The aqueous solution solving inulin is warming up to 45 DEG C and is incubated 15min, is 1: 300 according to saccharase and inulin mass ratio (kg/kg)
Ratio adds saccharase, then temperature be 45 DEG C, mixing speed be 100r/min under conditions of process 16h, just prepare sugarcane
Carbohydrase hydrating solution, prepares glucoseoxidase treatment fluid for lower step.
(2) glucoseoxidase treatment fluid is prepared
After (1st) step completes, saccharase hydrating solution prepared by (1st) step is warming up to 60 DEG C and is incubated 15min, according to
Glucoseoxidase and inulin mass ratio (kg/kg) be 1: 200 ratio add glucoseoxidase, be then 60 in temperature
DEG C, mixing speed be to process 2h under conditions of 100r/min, just prepare glucoseoxidase treatment fluid, super for the preparation of lower step
Filter separates liquid.
(3) ultra-filtration and separation liquid is prepared
After (2nd) step completes, glucoseoxidase treatment fluid prepared by (2nd) step is pumped into molecular cut off is
In the ultrafilter of 30000Da, under gauge pressure is 0.5MPa, carry out ultrafiltration for the first time, until ultra-filter retentate is with for the first time for the first time
When the ratio (L/L) of ultrafiltration filtered solution volume is 1: 8 only.Collect ultrafiltration filtered solution and for the first time ultra-filter retentate for the first time respectively,
To collect first time ultra-filter retentate, add the pure water of this trapped fluid volume 6 times, again carry out second time ultrafiltration, second
The gauge pressure of secondary ultrafiltration and stop during second time ultrafiltration the ratio of second time ultra-filter retentate and second time ultrafiltration filtered solution volume all with
Ultrafiltration is identical for the first time.After ultrafiltration completes for the second time, collect second time ultrafiltration filtered solution and second time ultra-filter retentate respectively.Right
The second time ultrafiltration filtered solution collected, merges with the first time ultrafiltration filtered solution collected, i.e. prepares ultra-filtration and separation liquid, under being used for
Step prepares gluconic acid separation liquid；To the second time ultra-filter retentate collected, it is dried after mixing with Semen Maydis powder, as feedstuff flavour enhancing
Agent.
(4) gluconic acid separation liquid is prepared
After (3rd) step completes, ultra-filtration and separation liquid pump prepared by (3rd) step is entered in cathodic coating electrodialyzer, at voltage be
200V, electric current is 3A, and intake pressure is 2kg/cm2Under conditions of carry out electrodialysis process and collect in electrodialyzer from concentrated water spout
The liquid flowed out with fresh water mouth.To the liquid flowed out from fresh water mouth collected, containing oligofructose and polyfructosan, it is levan
Solution, is used for preparing levan separation liquid；To the liquid flowed out from concentrated water spout collected, containing gluconic acid, i.e. prepare Fructus Vitis viniferae
Saccharic acid separation liquid, prepares gluconic acid concentrated solution for lower step.
(5) gluconic acid concentrated solution is prepared
After (4th) step completes, the gluconic acid separation liquid pump (4th) step prepared enters in counter-osmosis device, in gauge pressure is
Reverse osmosis concentration is carried out, during until gluconic acid mass percentage concentration reaches 15% in reverse osmosis trapped fluid under conditions of 0.9MPa
Only.Collect reverse osmosis filtered solution and trapped fluid respectively, to the reverse osmosis filtered solution collected, pump into wastewater disposal basin and carry out biochemical treatment,
Discharge after up to standard；To collect reverse osmosis trapped fluid, be gluconic acid mass percentage concentration reach 15% gluconic acid dense
Contracting liquid, is used for preparing protein coagulating agent, food preservative and cement water reducing agent etc..
(6) levan separation liquid is prepared
After (4th) step completes, levan solution prepared by (4th) step, pump into the ultrafiltration that molecular cut off is 1500Da
In device, under gauge pressure is 0.5MPa, carry out ultrafiltration for the first time, until ultra-filter retentate and ultrafiltration filtered solution for the first time for the first time
When long-pending ratio is 1: 8 (L/L) only.Collect ultrafiltration filtered solution and for the first time ultra-filter retentate for the first time respectively, to first collected
Secondary ultra-filter retentate, adds the pure water of this trapped fluid volume 6 times, again carry out second time ultrafiltration, the gauge pressure of ultrafiltration for the second time,
And stop during second time ultrafiltration the ratio of second time ultra-filter retentate and second time ultrafiltration filtered solution volume all with first time ultrafiltration phase
With.After ultrafiltration completes for the second time, collect second time ultrafiltration filtered solution and second time ultra-filter retentate respectively.To the second time collected
Ultrafiltration filtered solution, merges with the first time ultrafiltration filtered solution collected, and this amalgamation liquid contains oligofructose, prepares oligomeric fruit for lower step
Icing Sugar end；To the second time ultra-filter retentate collected, containing polyfructosan, prepare polyfructosan powder for lower step.To collect
The second time ultra-filter retentate of this amalgamation liquid and collection, is collectively referred to as levan separation liquid, i.e. prepares levan separation liquid.
(7) oligofructose powder and polyfructosan powder are prepared
After (6th) step completes, the amalgamation liquid of the ultrafiltration filtered solution containing oligofructose (6th) step prepared pumps into and retains point
Son amount is in the nanofiltration device of 600Da, carries out nanofiltration concentration under conditions of gauge pressure is 0.9MPa, until oligomeric in nanofiltration trapped fluid
Fructose mass percentage concentration reaches to stop when 20%.Collect nanofiltration filtered solution and nanofiltration trapped fluid respectively, the nanofiltration collected is filtered
Liquid, pumps into wastewater disposal basin and processes, rear discharge up to standard；To the nanofiltration trapped fluid collected, pump into spray dryer, in inlet temperature be
180 DEG C, leaving air temp be 100 DEG C, spraying centrifuge speed be to be spray-dried under conditions of 8000r/min, just prepare
The oligofructose powder of white.The second time ultra-filter retentate containing polyfructosan collecting (6) step, pumping into molecular cut off is
In the ultrafilter of 2500Da, it is concentrated by ultrafiltration under conditions of gauge pressure is 0.9MPa, until polyfructosan in ultra-filter retentate
Mass percentage concentration reaches to stop when 20%.Collect ultrafiltration filtered solution and ultra-filter retentate respectively, to the ultrafiltration filtered solution collected, pump
Enter wastewater disposal basin to process, rear discharge up to standard；To the ultra-filter retentate collected, pump into spray dryer, inlet temperature be 180 DEG C,
Leaving air temp is 100 DEG C, spraying centrifuge speed is to be spray-dried under conditions of 8000r/min, just prepares white
Polyfructosan powder.
Claims (1)
1. one kind utilizes the method that inulin prepares levan and gluconic acid, it is characterised in that concrete processing step is as follows:
(1) saccharase hydrating solution is prepared
First in rustless steel enzymatic hydrolysis reaction still, pump into pure water, be 1 according still further to inulin quality and pure water volume ratio (kg/L):
The ratio of 10～20, is under agitation dissolved in inulin in pure water, then opens the heat riser of this hydrolytic reaction pot, by molten
The aqueous solution solving inulin is warming up to 40～45 DEG C and is incubated 10～15min, according to saccharase with inulin mass ratio (kg/kg) is
The ratio of 1: 150～300 adds saccharase, then temperature be 40～45 DEG C, mixing speed be 60～100r/min condition
Lower process 10～16h, just prepares saccharase hydrating solution, prepares glucoseoxidase treatment fluid for lower step；
(2) glucoseoxidase treatment fluid is prepared
After (1st) step completes, saccharase hydrating solution prepared by (1st) step is warming up to 50～60 DEG C and is incubated 10～15min,
Glucoseoxidase is added, then according to the ratio that glucoseoxidase and inulin mass ratio (kg/kg) are 1: 100～200
Temperature be 50～60 DEG C, mixing speed be to process 1～2h under conditions of 60～100r/min, just prepare glucoseoxidase
Treatment fluid, prepares ultra-filtration and separation liquid for lower step；
(3) ultra-filtration and separation liquid is prepared
After (2nd) step completes, glucoseoxidase treatment fluid prepared by (2nd) step is pumped into molecular cut off be 10000～
In the ultrafilter of 30000Da, under gauge pressure is 0.2～0.5MPa, carry out for the first time ultrafiltration, until for the first time ultra-filter retentate with
When the ratio (L/L) of ultrafiltration filtered solution volume is 1: 5～8 for the first time only, ultrafiltration filtered solution and first time for the first time are collected respectively super
Filter trapped fluid, to the first time ultra-filter retentate collected, adds this trapped fluid volume 4～pure water of 6 times, again carries out second
Secondary ultrafiltration, second time ultra-filter retentate and second time ultrafiltration filtered solution when the gauge pressure of ultrafiltration for the second time and stopping second time ultrafiltration
Long-pending ratio is all identical with ultrafiltration for the first time, after ultrafiltration completes for the second time, collects second time ultrafiltration filtered solution respectively and second time is super
Filter trapped fluid, to the second time ultrafiltration filtered solution collected, merges with the first time ultrafiltration filtered solution collected, i.e. prepares ultrafiltration and divide
Chaotropic, prepares gluconic acid separation liquid for lower step；To the second time ultra-filter retentate collected, it is dried after mixing with Semen Maydis powder,
As feedstuff flavour enhancer；
(4) gluconic acid separation liquid is prepared
After (3rd) step completes, ultra-filtration and separation liquid pump prepared by (3rd) step is entered in cathodic coating electrodialyzer, voltage be 150～
200V, electric current is 1～3A, and intake pressure is 0.5～2kg/cm2Under conditions of carry out electrodialysis process and collect in electrodialyzer
The liquid flowed out from concentrated water spout and fresh water mouth, to the liquid flowed out from fresh water mouth collected, containing oligofructose and polyfructosan, i.e.
For levan solution, it is used for preparing levan separation liquid；To the liquid flowed out from concentrated water spout collected, containing gluconic acid, i.e. make
For going out gluconic acid separation liquid, prepare gluconic acid concentrated solution for lower step；
(5) gluconic acid concentrated solution is prepared
After (4th) step completes, the gluconic acid separation liquid pump (4th) step prepared enters in counter-osmosis device, gauge pressure be 0.7～
Carry out reverse osmosis concentration under conditions of 0.9MPa, until in reverse osmosis trapped fluid gluconic acid mass percentage concentration reach 10～
When 15% only, collect reverse osmosis filtered solution and trapped fluid respectively, to the reverse osmosis filtered solution collected, pump into wastewater disposal basin and carry out biochemistry
Process, rear discharge up to standard；To the reverse osmosis trapped fluid collected, it is gluconic acid mass percentage concentration and reaches the Portugal of 10～15%
Grape saccharic acid concentrated solution, is used for preparing protein coagulating agent, food preservative and cement water reducing agent etc.；
(6) levan separation liquid is prepared
After (4th) step completes, the levan solution (4th) step prepared, pumping into molecular cut off is 800～1500Da receive
In filter/ultrafilter, under gauge pressure is 0.2～0.5MPa, carry out nanofiltration/ultrafiltration for the first time, until nanofiltration/ultrafiltration for the first time retains
When the ratio of liquid and first time nanofiltration/ultrafiltration filtered solution volume is 1: 5～8 (L/L) only, nanofiltration for the first time/ultrafiltration filter is collected respectively
Cross liquid and for the first time nanofiltration/ultra-filter retentate, to the first time nanofiltration/ultra-filter retentate collected, add this trapped fluid volume 4～
The pure water of 6 times, carries out second time nanofiltration/ultrafiltration, for the second time gauge pressure of nanofiltration/ultrafiltration again, and stops second time nanofiltration/super
During filter the ratio of second time nanofiltration/ultra-filter retentate and second time nanofiltration/ultrafiltration filtered solution volume all with first time nanofiltration/ultrafiltration phase
With, after nanofiltration/ultrafiltration completes for the second time, collect second time nanofiltration/ultrafiltration filtered solution respectively and second time nanofiltration/ultrafiltration retains
Liquid, to the second time nanofiltration/ultrafiltration filtered solution collected, merges with the first time nanofiltration/ultrafiltration filtered solution collected, and this amalgamation liquid contains
Oligofructose, prepares oligofructose powder for lower step；To the second time nanofiltration/ultra-filter retentate collected, containing polyfructosan, use
Prepare polyfructosan powder in lower step, to this amalgamation liquid collected and the second time nanofiltration/ultra-filter retentate of collection, be collectively referred to as fruit
Polysaccharide separation liquid, i.e. prepares levan separation liquid；
(7) oligofructose powder and polyfructosan powder are prepared
After (6th) step completes, the amalgamation liquid of the nanofiltration containing the oligofructose/ultrafiltration filtered solution (6th) step prepared pumps into and retains
Molecular weight is in the nanofiltration device of 200～600Da, carries out nanofiltration concentration under conditions of gauge pressure is 0.7～0.9MPa, until nanofiltration
In trapped fluid, oligofructose mass percentage concentration reaches to stop when 15～20%, collects nanofiltration filtered solution and nanofiltration trapped fluid respectively,
To the nanofiltration filtered solution collected, pump into wastewater disposal basin and process, rear discharge up to standard；To the nanofiltration trapped fluid collected, pump into spray drying
Machine, inlet temperature be 150～180 DEG C, leaving air temp be 90～100 DEG C, spraying centrifuge speed be 5000～8000r/min
Under conditions of be spray-dried, just prepare white oligofructose powder, to (6) step collect containing polyfructosan second
Secondary nanofiltration/ultra-filter retentate, pumps in the ultrafilter that molecular cut off is 1000～2500Da, is 0.7～0.9MPa in gauge pressure
Under conditions of be concentrated by ultrafiltration, until when in ultra-filter retentate, polyfructosan mass percentage concentration reaches 15～20% only, point
Not Shou Ji ultrafiltration filtered solution and ultra-filter retentate, to collect ultrafiltration filtered solution, pump into wastewater disposal basin process, up to standard after discharge；Right
The ultra-filter retentate collected, pumps into spray dryer, inlet temperature be 150～180 DEG C, leaving air temp be 90～100 DEG C, spray
Mist centrifuge speed is to be spray-dried under conditions of 5000～8000r/min, just prepares the polyfructosan powder of white.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106947000A (en) * | 2017-04-25 | 2017-07-14 | 寰龙特种糖业有限公司 | A kind of preparation method of high-purity polyfructosan |
| CN109645297A (en) * | 2019-01-02 | 2019-04-19 | 旬阳县太极缘生物科技有限公司 | The minimizing technology of mono-and di-saccharides in a kind of honey raisin tree fruit juice |
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| CN101538591A (en) * | 2009-04-29 | 2009-09-23 | 重庆大学 | Method for preparing gluconic acid from mother liquor of xylose crystalline liquid |
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| CN101538591A (en) * | 2009-04-29 | 2009-09-23 | 重庆大学 | Method for preparing gluconic acid from mother liquor of xylose crystalline liquid |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106947000A (en) * | 2017-04-25 | 2017-07-14 | 寰龙特种糖业有限公司 | A kind of preparation method of high-purity polyfructosan |
| CN106947000B (en) * | 2017-04-25 | 2019-05-07 | 凡秘能特种糖业有限公司 | A kind of preparation method of high-purity polyfructosan |
| CN109645297A (en) * | 2019-01-02 | 2019-04-19 | 旬阳县太极缘生物科技有限公司 | The minimizing technology of mono-and di-saccharides in a kind of honey raisin tree fruit juice |
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