CN101586129A - Method of preparing sodium gluconate from xylose crystallization mother liquor - Google Patents
Method of preparing sodium gluconate from xylose crystallization mother liquor Download PDFInfo
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- CN101586129A CN101586129A CNA200910104241XA CN200910104241A CN101586129A CN 101586129 A CN101586129 A CN 101586129A CN A200910104241X A CNA200910104241X A CN A200910104241XA CN 200910104241 A CN200910104241 A CN 200910104241A CN 101586129 A CN101586129 A CN 101586129A
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Abstract
The invention discloses a method of preparing sodium gluconate from xylose crystallization mother liquor, relates to prepartion method of sodium gluconate. The invention uses indurtrial sewage of xylose crystallization mother liquor, through steps of dilution and nanofiltration, enzyme oxidation, anion exchange, washing concentrating and drying to obtain completed products. The invention uses indurtrial sewage of xylose crystallization mother liquor to produce product sodium gluconate with a purity of 96 to 98% and byproduct such as caramel color, waste is made as treaure, and waste source are made of full use, production cost is reduced; simple method, simple device, no waste residue is discharged in production process, clean production and target of energy saving and discharge reducing are implemented, and then production cost is reduced further. Products according to the invention can be used in industry of foods, chemistry, medicine, and light industry, and particularly suitable for using as nutritional supplements, curing agent and buffers for food industry.
Description
One, technical field
The invention belongs to the technical field of preparation Sunmorl N 60S, be specifically related to Preparation of Sodium Gluconate.
Two, background technology
Sunmorl N 60S claims sodium pentahydyoxycaproate again, is a kind of organic monoacid salt, and white or light yellow crystalline powder are soluble in water, be slightly soluble in alcohol, be insoluble to ether, nontoxic, being the good flavor agent that is, covering the effect of bitter taste and stink in addition, is good food-processing pH buffer reagent.Sodium in the Sunmorl N 60S has vital role to acid base equilibrium, the nervimuscular normal function of performance in the exosmosis pressure of keeping cell and capacity, the control agent, can effectively prevent the generation of low sodium syndromes.Sunmorl N 60S because of Heat stability is good, do not have deliquescence, good closing property of huge legendary turtle arranged, be widely used in the industrial sector of water conditioning, plating, metal and nonmetallic surface cleaning and manufacture of cement.Sunmorl N 60S is the basic material of preparation Gluconolactone, gluconate (zinc, copper, ferrous salt etc.), makes accessory substance, solidifying agent etc. in foodstuffs industry, is widely used.
The existing method for preparing Sunmorl N 60S, " with the research of cane molasses fermentative Production Sunmorl N 60S " literary composition as " China brewages " 2008 the 16th phases, disclosed method is to be raw material with the cane molasses, earlier make glucose solution, add nutritive salt KH then through pre-treatment (being ionized water dilution, activated carbon decolorizing, adjusting pH value, filtration)
2PO
4And MgSO
47H
2O and corn steep liquor, and through sterilization and regulate after pH value is 5.4～6.5, add the long wheat bran that aspergillus niger spore is arranged again ferment, at last after filtration, to make the Sunmorl N 60S transformation efficiency be 89% product for activated carbon decolorizing, vacuum concentration, suction filtration drying.The main shortcoming of this method is: cost is higher, intermediate steps is complicated, by product is many, asepticize processing requirement height, separation and purifying difficulty are big, make a low multiple use, product purity is not high, environmental stress is big.
Three, summary of the invention
The objective of the invention is weak point at existing preparation Sunmorl N 60S method, a kind of method for preparing Sunmorl N 60S from xylose crystallization mother liquor is provided, has the xylose crystallization mother liquor of making full use of trade waste resource, there is not " three wastes " discharging, operation steps is simple, equipment is practical, characteristics such as the Sunmorl N 60S purity height of preparing.
The principle of the invention: in preparation Xylitol depleted xylose crystallization mother liquor, contain 5～15% glucose, 1～5% semi-lactosi and pectinose.The present invention utilizes and contains the bigger solute of pigment equimolecular quantity (its molecular weight is generally greater than 2000Da) in the xylose crystallization mother liquor, and the characteristics of carbohydrate molecule amounts less (being generally hundreds of Da) such as wood sugar, semi-lactosi, pectinose, glucose, utilizing nanofiltration again is a kind of pressure drive membrane separation means between reverse osmosis and ultrafiltration, the pore diameter range of nanofiltration membrane is about several nanometers, so select for use suitable nanofiltration membrane just can remove the solute of macromolecule scope; Glucose in the nanofiltration liquid adopts immobilized glucose oxidase Choice of Resin oxidizing glucose, obtain the gluconic acid effluent liquid, and wood sugar, semi-lactosi etc. can be by this oxydasises, and mainly contain gluconic acid in the effluent liquid this moment, contain carbohydrates such as pectinose, semi-lactosi, wood sugar simultaneously yet; The formation negatively charged ion because gluconic acid dissociates in solution, and carbohydrates such as wood sugar are not charged, so can exchange on the resin with anionite-exchange resin, carbohydrates such as wood sugar are removed because of not separated by exchange; Exchange to gluconic acid on the resin column with separation and purification behind the NaOH eluant solution, obtain the higher Sunmorl N 60S product of purity.
The object of the present invention is achieved like this: a kind of method for preparing Sunmorl N 60S from xylose crystallization mother liquor, with the xylose crystallization mother liquor industrial effluent is raw material, make finished product through dilution and nanofiltration, oxydasis, anionresin, wash-out and the concentrated drying that reaches, concrete steps are as follows:
(1) dilution, nanofiltration
With the xylose crystallization mother liquor industrial effluent is raw material, and according to xylose crystallization mother liquor: the volume ratio of pure water is 1: 1～5 ratio, adds pure water, agitation and dilution in xylose crystallization mother liquor.Then the xylose crystallization mother liquor diluent being pumped in the nanofiltration device, is that the nanofiltration membrane of 1000～6000Da is carried out nanofiltration and handled with molecular weight cut-off, collects filtered solution and trapped fluid respectively.Filtered solution is the saccharide solution that contains wood sugar, glucose, semi-lactosi, pectinose etc.; Trapped fluid is the solution that contains macromolecule solutes such as pigment, pumps in the thermostat water bath, is concentrated into pulpous state under 80～100 ℃ of temperature, prepares caramel colorant.
(2) oxydasis
1. prepare the immobilized glucose oxidase resin column
(1) step was a carrier with cross-linked chitosan-Methionin resin after finishing, and by cross-linked chitosan-Methionin resin carrier amino: glucose oxidase: the mol ratio of glutaraldehyde is 1: (1.0 * 10
-4～2.0 * 10
-4): the ratio of (0.4～0.6), in cross-linked chitosan-Methionin resin carrier, add glucose oxidase and glutaraldehyde, regulating its pH value with Sodium phosphate dibasic-citrate buffer solution again is 3.0～5.0, adsorbed crosslinked 2～4 hours, and just made immobilized glucose oxidase (IGOD) resin.Then immobilized glucose oxidase (IGOD) resin that makes is enclosed in the constant temperature interlayer resin post, just makes the immobilized glucose oxidase resin column of constant temperature interlayer, be used for next step and carry out oxydasis.
2. oxydasis
(2)-1. the step finish after, (1) filtered solution that goes on foot collection is pumped into (2)-1. to be gone on foot in the immobilized glucose oxidase resin column of the constant temperature interlayer that makes, be under 35～45 ℃ the constant temperature in temperature, carry out oxydasis, the speed that pumps into of filtered liquid be 2～6 times of immobilized glucose oxidase resin volumes/hour, till no gluconic acid flows out in the oxydasis liquid of crossing post, collected the oxydasis liquid of post and the immobilized glucose oxidase resin behind the oxydasis respectively.Oxydasis liquid for collecting is used for next step and carries out ion-exchange; Immobilized glucose oxidase resin for collecting cleans with pure water, and is reusable.
(3) anionresin
1. prepare anion-exchange resin column
(2) step finish after, with D293 anionite-exchange resin, be filled in the ion exchange column, the deionization bubble that adds 3～5 times of D293 anionite-exchange resin volumes was washed 12～14 hours earlier, after bleeding off deionized water, the sodium-chlor mass concentration that adds 2～5 times of D293 anionite-exchange resin volumes again is 10% sodium chloride solution, bubble was washed 2～5 hours, bleed off sodium chloride solution, and then it is washed till clean sodium-chlor with deionized water, carry out the alkali cleaning of alkali cleaning-pickling-again activation D293 anionite-exchange resin at last, just prepare the D293 anion-exchange resin column, be used for next step and carry out ion-exchange.Wherein alkali cleaning is to be 4% sodium hydroxide solution flushing 30min with the sodium hydroxide mass concentration, again with distilled water flushing till the neutrality; Pickling is to be 4% hydrochloric acid soln flushing 30min with the hydrochloric acid mass concentration, again with distilled water flushing till the neutrality.
2. anionresin
(3)-1. the step finish after, in the D293 anionite-exchange resin that the oxydasis liquid pump people who crosses post that (2)-2. step was collected prepared in (3)-1. step, carry out anionresin, its pump into speed be 7～9 times of D293 anionite-exchange resin volumes/hour, till in effusive anionresin liquid, gluconic acid occurring, collect the D293 anion-exchange resin column that effusive anionresin liquid and exchange have gluconic acid respectively.To effusive anionresin liquid, concentrate and crystallization make wood sugar; For the exchange of collecting the D293 anion-exchange resin column of gluconic acid is arranged, being used for down, the step wash-out prepares Sunmorl N 60S.
(4) preparation Sunmorl N 60S
(3) step finish after, the exchange of collecting to (3)-2. step earlier has in the D293 anion-exchange resin column of gluconic acid, pump into the distilled water of 2～3 times of D293 anionite-exchange resin volumes, clean, in order to clean pectinose, semi-lactosi and wood sugar in the D293 anionite-exchange resin, collect effluent liquid; Pumping into the sodium hydroxide mass concentration to it again is that 7% sodium hydroxide solution carries out wash-out, its pump into speed be 3～4 times D293 anionite-exchange resin volume/hour, in elutriant till the no Sunmorl N 60S, collect the D293 anionite-exchange resin behind elutriant and the wash-out respectively.To the effluent liquid of collecting, because of containing pectinose, semi-lactosi and wood sugar, carry out vacuum concentration after, be used to prepare wood sugar etc., do not discharge; To the D293 anionite-exchange resin behind the wash-out of collecting, after cleaning-regenerating, reuse; To the elutriant of collecting (being sodium gluconate solution), pump in the rotatory evaporator earlier, under 80～100 ℃ of temperature, heat that to be concentrated into the Sunmorl N 60S mass concentration be 50～55% Sunmorl N 60S concentrated solution, till back adding dehydrated alcohol to gluconic acid sodium crystal is separated out, collect gluconic acid sodium crystal and surplus liquid respectively.Surplus liquid is used to reclaim ethanol, does not discharge.For the gluconic acid sodium crystal is that 85% ethanolic soln cleans 2～4 times with the ethanol mass concentration earlier, and to remove surface impurity, gluconic acid sodium crystal and filtrate are collected in filtration respectively then.For filtrate, after being rotated evaporation and reclaiming ethanol and utilize, Yu Shui reclaims, and is used further to (1) step dilution xylose crystallization mother liquor; To the gluconic acid sodium crystal, be positioned in the constant pressure and dry case, under 50～60 ℃ of temperature, carry out drying, just prepare the Sunmorl N 60S mass content and be 96～98% Sunmorl N 60S crystal product.
After the present invention adopts technique scheme, mainly contain following effect:
1, the present invention is a raw material with the xylose crystallization mother liquor industrial effluent, prepare purity up to byproducts such as 96%～98% Sunmorl N 60S product and caramel colorants, can turn waste into wealth, production cost is low, and has opened up new way for the resource reutilization of the xylose crystallization mother liquor industrial waste of preparation behind the Xylitol.
2, the present invention adopts the oxidation of immobilized glucose oxidase resin column to prepare the technology of gluconic acid, and mild condition, selectivity is good, by product is few, equipment is simple and practical, immobilized enzyme column can reuse, and reduces production costs;
3, the present invention adopts the technology of anionite-exchange resin D293 exchange separating glucose acid, disturbs less, adsorptive capacity is big, good separating effect, and exchange resin can reuse, and further reduces production costs;
4, the inventive method is simple, and equipment used is simple, realizes cleaner production in process of production, does not have " three wastes " discharging, environmental friendliness, comprehensive utilization of resources rate height, the target of realization energy-saving and emission-reduction.
The product that adopts invention to prepare can be widely used in doing in the foodstuffs industry accessory substance, solidifying agent, buffer reagent etc.; Be used for aspects such as the agent of industrial sector acid base equilibrium, water quality stabilizer, surface cleaning agent, cement blending agent etc.In industries such as chemical industry, medicine, light industrys purposes is widely arranged also.
Four, embodiment
Below in conjunction with embodiment, further specify the present invention.
Embodiment 1
A kind of method that from xylose crystallization mother liquor, prepares Sunmorl N 60S, concrete steps are as follows:
(1) dilution, nanofiltration
With the xylose crystallization mother liquor industrial effluent is raw material, and according to xylose crystallization mother liquor: the volume ratio of pure water is 1: 1 a ratio, adds pure water, agitation and dilution in xylose crystallization mother liquor.Then the xylose crystallization mother liquor diluent being pumped in the nanofiltration device, is that the nanofiltration membrane of 1000Da is carried out nanofiltration and handled with molecular weight cut-off, collects filtered solution and trapped fluid respectively.Filtered solution is the saccharide solution that contains wood sugar, glucose, semi-lactosi, pectinose etc.; Trapped fluid is the solution that contains macromolecule solutes such as pigment, pumps in the thermostat water bath, is concentrated into pulpous state under 80 ℃ of temperature, prepares caramel colorant.
(2) oxydasis
1. prepare the immobilized glucose oxidase resin column
(1) step was a carrier with cross-linked chitosan-Methionin resin after finishing, and by cross-linked chitosan-Methionin resin carrier amino: glucose oxidase: the mol ratio of glutaraldehyde is 1: 1.0 * 10
-4: 0.4 ratio, in cross-linked chitosan-Methionin resin carrier, add glucose oxidase and glutaraldehyde, regulating its pH value with Sodium phosphate dibasic-citrate buffer solution again is 3.0, adsorbs crosslinked 2 hours, just makes immobilized glucose oxidase (IGOD) resin.Then immobilized glucose oxidase (IGOD) resin that makes is placed in the constant temperature interlayer resin post, just makes the immobilized glucose oxidase resin column of constant temperature interlayer, be used for next step and carry out oxydasis.
2. oxydasis
(2)-1. the step finish after, (1) filtered solution that goes on foot collection is pumped into (2)-1. to be gone on foot in the immobilized glucose oxidase resin column of the constant temperature interlayer that makes, be under 35 ℃ the constant temperature in temperature, carry out oxydasis, the speed that pumps into of filtered liquid be 2 times of immobilized glucose oxidase resin volumes/hour, till no gluconic acid flows out in the oxydasis liquid of crossing post, collected the oxydasis liquid of post and the immobilized glucose oxidase resin behind the oxydasis respectively.Oxydasis liquid for collecting is used for next step and carries out ion-exchange; For the immobilized glucose oxidase resin of collecting, after cleaning with pure water, reusable.
(3) anionresin
1. prepare anion-exchange resin column
(2) step finish after, with D293 anionite-exchange resin, be filled in the ion exchange column, the deionization bubble that adds 3 times of D293 anionite-exchange resin volumes was washed 12 hours earlier, after bleeding off deionized water, the sodium-chlor mass concentration that adds 2 times of D293 anionite-exchange resin volumes again is 10% sodium chloride solution, bubble was washed 2 hours, bleed off sodium chloride solution, and then it is washed till clean sodium-chlor with deionized water, through alkali cleaning-pickling-alkali cleaning activates D293 anionite-exchange resin again, just prepares the D293 anion-exchange resin column, be used for next step and carry out ion-exchange at last.Wherein alkali cleaning is to be 4% sodium hydroxide solution flushing 30min with the sodium hydroxide mass concentration, again with distilled water flushing till the neutrality; Pickling is to be 4% hydrochloric acid soln flushing 30min with mass concentration, again with distilled water flushing till the neutrality.
2. anionresin
(3)-1. the step finish after, in the D293 anionite-exchange resin that the oxydasis liquid pump people who crosses post that (2)-2. step was collected prepared in (3)-1. step, carry out anionresin, its pump into speed be 7 times of D293 anionite-exchange resin volumes/hour, till in effusive anionresin liquid, gluconic acid occurring, collect the D293 anion-exchange resin column that effusive anionresin liquid and exchange have gluconic acid respectively.To the anionresin liquid of collecting, make wood sugar through concentrated and crystallization; The exchange of collecting is had the D293 anion-exchange resin column of gluconic acid, and being used for down, the step wash-out prepares Sunmorl N 60S.
(4) preparation Sunmorl N 60S
(3) step finish after, the exchange of collecting to (3)-2. step earlier has the distilled water that pumps into 2 times of D293 anionite-exchange resin volumes in the D293 anion-exchange resin column of gluconic acid, clean, in order to clean pectinose, semi-lactosi and wood sugar in the D293 anionite-exchange resin, collect effluent liquid; Pumping into the sodium hydroxide mass concentration to it again is that 7% sodium hydroxide solution carries out wash-out, its pump into speed be 3 times D293 anionite-exchange resin volume/hour, in elutriant till the no Sunmorl N 60S, collect the D293 anionite-exchange resin behind elutriant and the wash-out respectively.Effluent liquid to collecting because of containing pectinose, semi-lactosi and wood sugar, behind vacuum concentration, is used to prepare wood sugar etc., does not discharge; To the D293 anionite-exchange resin behind the wash-out of collecting,, reuse through after the cleaning-regeneration; For elutriant (being sodium gluconate solution), pump in the rotatory evaporator earlier, under 80 ℃ of temperature, heat that to be concentrated into the Sunmorl N 60S mass concentration be 50% Sunmorl N 60S concentrated solution, till back adding dehydrated alcohol to gluconic acid sodium crystal is separated out, collect gluconic acid sodium crystal and surplus liquid respectively.Surplus liquid is used to reclaim ethanol, does not discharge.To the gluconic acid sodium crystal is that 85% ethanolic soln cleans 2 times with the ethanol mass concentration earlier, and to remove surface impurity, gluconic acid sodium crystal and filtrate are collected in filtration respectively then.For filtrate, after rotary evaporation recovery ethanol utilized again, Yu Shui reclaimed, and was used for (1) step dilution xylose crystallization mother liquor; To the gluconic acid sodium crystal, be positioned in the constant pressure and dry case, under 50 ℃ of temperature, carry out drying, just prepare the Sunmorl N 60S mass content and be 96 product.
Embodiment 2
A kind of method that from xylose crystallization mother liquor, prepares Sunmorl N 60S, concrete steps are as follows:
(1) dilution, nanofiltration
With embodiment 1, wherein: xylose crystallization mother liquor: the volume ratio of pure water is 1: 2.5, and the molecular weight cut-off of nanofiltration membrane is 3000Da; The water bath with thermostatic control temperature that concentrates trapped fluid is 90 ℃.
(2) oxydasis
1. prepare the immobilized glucose oxidase resin column
With embodiment 1, wherein: cross-linked chitosan-Methionin resin carrier amino: glucose oxidase: the mol ratio of glutaraldehyde is 1: 1.35 * 10
-4: 0.55, regulating its pH value with Sodium phosphate dibasic-citrate buffer solution is 4.0, adsorbs crosslinked 3 hours.
2. oxydasis
With embodiment 1, wherein: the temperature of carrying out oxydasis is 40 ℃, the speed that filtered liquid pumps into be 4 times of immobilized glucose oxidase resin volumes/hour.
(3) anionresin
1. prepare anion-exchange resin column
With embodiment 1, wherein: the deionization bubble that adds 4 times of D293 anionite-exchange resin volumes was washed 13 hours, and the sodium-chlor mass concentration that adds 3 times of D293 anionite-exchange resin volumes again is 10% sodium chloride solution, and bubble was washed 3 hours.
2. anionresin
With embodiment 1, wherein: the oxydasis liquid pump go into speed be 8 times of D293 anionite-exchange resin volumes/hour.
(4) preparation Sunmorl N 60S
With embodiment 1, wherein: the distilled water that is used to clean is 2.5 times of D293 anionite-exchange resin volumes, the speed that 7% sodium hydroxide solution pumps into be 3.5 times D293 anionite-exchange resin volume/hour, elutriant in the rotatory evaporator, under 90 ℃ of temperature, it is 53% Sunmorl N 60S concentrated solution that heating is concentrated into the Sunmorl N 60S mass concentration, is that 85% ethanolic soln cleans 3 times to the gluconic acid sodium crystal after the crystallization with the ethanol mass concentration, to the gluconic acid sodium crystal after cleaning, under 55 ℃ of temperature, carry out drying, make the Sunmorl N 60S mass content and be 97% gluconic acid sodium crystal.
Embodiment 3
A kind of method that from xylose crystallization mother liquor, prepares Sunmorl N 60S, concrete steps are as follows:
(1) dilution, nanofiltration
With embodiment 1, wherein: xylose crystallization mother liquor: the volume ratio of pure water is 1: 5, and the molecular weight cut-off of nanofiltration membrane is 6000Da; The water bath with thermostatic control temperature that concentrates trapped fluid is 100 ℃.
(2) oxydasis
1. prepare the immobilized glucose oxidase resin column
With embodiment 1, wherein: cross-linked chitosan-Methionin resin carrier amino: glucose oxidase: the mol ratio of glutaraldehyde is 1: 2.0 * 10
-4: 0.6, regulating its pH value with Sodium phosphate dibasic-citrate buffer solution is 5.0, adsorbs crosslinked 4 hours.
2. oxydasis
With embodiment 1, wherein: the temperature of carrying out oxydasis is 45 ℃, the speed that filtered liquid pumps into be 6 times of immobilized glucose oxidase resin volumes/hour.
(3) anionresin
1. prepare anion-exchange resin column
With embodiment 1, wherein: the deionization bubble that adds 5 times of D293 anionite-exchange resin volumes was washed 14 hours, and the sodium-chlor mass concentration that adds 5 times of D293 anionite-exchange resin volumes again is 10% sodium chloride solution, and bubble was washed 5 hours.
2. anionresin
With embodiment 1, wherein: the oxydasis liquid pump go into speed be 9 times of D293 anionite-exchange resin volumes/hour.
(4) preparation Sunmorl N 60S
With embodiment 1, wherein: the distilled water that is used to clean is 3 times of D293 anionite-exchange resin volumes, the speed that 7% sodium hydroxide solution pumps into be 4 times D293 anionite-exchange resin volume/hour, elutriant in the rotatory evaporator, under 100 ℃ of temperature, it is 55% Sunmorl N 60S concentrated solution that heating is concentrated into the Sunmorl N 60S mass concentration, is that 85% ethanolic soln cleans 4 times to the gluconic acid sodium crystal after the crystallization with the ethanol mass concentration, to the gluconic acid sodium crystal after cleaning, under 60 ℃ of temperature, carry out drying, make product.
Claims (4)
1. method for preparing Sunmorl N 60S from xylose crystallization mother liquor is characterized in that concrete method steps is as follows:
(1) dilution, nanofiltration
With the xylose crystallization mother liquor industrial effluent is raw material, according to xylose crystallization mother liquor: the volume ratio of pure water is 1: 1～5 ratio, in xylose crystallization mother liquor, add pure water, agitation and dilution, then the xylose crystallization mother liquor diluent being pumped in the nanofiltration device, is that the nanofiltration membrane of 1000～6000Da is carried out nanofiltration and handled with molecular weight cut-off, collects filtered solution and trapped fluid respectively, trapped fluid pumps in the thermostat water bath, is concentrated into pulpous state under 80～100 ℃ of temperature;
(2) oxydasis
1. prepare the immobilized glucose oxidase resin column
(1) step was a carrier with cross-linked chitosan-Methionin resin after finishing, and by cross-linked chitosan-Methionin resin carrier amino: glucose oxidase: the mol ratio of glutaraldehyde is 1: (1.0 * 10
-4～2.0 * 10
-4): the ratio of (0.4～0.6), in cross-linked chitosan-Methionin resin carrier, add glucose oxidase and glutaraldehyde, regulating its pH value with Sodium phosphate dibasic-citrate buffer solution again is 3.0～5.0, adsorbed crosslinked 2～4 hours, and then the immobilized glucose oxidase resin that makes was placed in the constant temperature interlayer resin post;
2. oxydasis
(2)-1. the step finish after, (1) filtered solution that goes on foot collection is pumped into (2)-1. to be gone on foot in the immobilized glucose oxidase resin column of the constant temperature interlayer that makes, be under 35～45 ℃ the constant temperature in temperature, carry out oxydasis, the speed that pumps into of filtered liquid be 2～6 times of immobilized glucose oxidase resin volumes/hour, in the oxydasis liquid of crossing post till the no Sunmorl N 60S, collected the oxydasis liquid of post and the immobilized glucose oxidase resin behind the oxydasis respectively, immobilized glucose oxidase resin for absorbing cleans with pure water;
(3) anionresin
1. prepare anion-exchange resin column
(2) step finish after, with D293 anionite-exchange resin, be filled in the ion exchange column, earlier the deionization bubble that adds 3～5 times of D293 anionite-exchange resin volumes was washed 12～14 hours, bleed off deionized water after, the sodium-chlor mass concentration that adds 2～5 times of D293 anionite-exchange resin volumes again is 10% sodium chloride solution, bubble was washed 2～5 hours, bleed off sodium chloride solution, with deionized water it is washed then, carry out alkali cleaning-pickling-alkali cleaning more at last;
2. anionresin
(3)-1. the step finish after, in the D293 anionite-exchange resin that the oxydasis liquid pump people who crosses post that (2)-2. step was collected prepared in (3)-1. step, its pump into speed be 7～9 times of D293 anionite-exchange resin volumes/hour, collect effusive anionresin liquid, to effusive anionresin liquid, concentrate and crystallization;
(4) preparation Sunmorl N 60S
(3) step finish after, the exchange of collecting to (3)-2. step earlier has in the D293 anion-exchange resin column of gluconic acid, pump into the distilled water of 2～3 times of D293 anionite-exchange resin volumes, clean, collect effluent liquid, pumping into the sodium hydroxide mass concentration to it again is that 7% sodium hydroxide solution carries out wash-out, its pump into speed be 3～4 times D293 anionite-exchange resin volume/hour, in elutriant till the no Sunmorl N 60S, collect the D293 anionite-exchange resin behind elutriant and the wash-out respectively, for effluent liquid, carry out vacuum concentration, the D293 anionite-exchange resin to behind the wash-out of collecting cleans, for elutriant, pump into earlier in the rotatory evaporator, under 80～100 ℃ of temperature, heat that to be concentrated into the Sunmorl N 60S mass concentration be 50～55% Sunmorl N 60S concentrated solution, the back adds dehydrated alcohol, collects gluconic acid sodium crystal and surplus liquid respectively; To the gluconic acid sodium crystal is 85% ethanolic soln cleaning 2～4 times with the ethanol mass concentration earlier, filter then, collect gluconic acid sodium crystal and filtrate respectively, for filtrate, be rotated evaporation, Yu Shui reclaims, to the gluconic acid sodium crystal, be positioned in the constant pressure and dry case, under 50～60 ℃ of temperature, carry out drying, just prepare the Sunmorl N 60S mass content and be 96～98% gluconic acid sodium crystal.
2. according to the described method that from xylose crystallization mother liquor, prepares Sunmorl N 60S of claim 1, it is characterized in that concrete step is as follows:
In (1) step, xylose crystallization mother liquor: the volume ratio of pure water is 1: 1, and the molecular weight cut-off of nanofiltration membrane is 1000Da, and the water bath with thermostatic control temperature that concentrates trapped fluid is 80 ℃;
In (2)-1. step, cross-linked chitosan-Methionin resin carrier amino: glucose oxidase: the mol ratio of glutaraldehyde is 1: 1.0 * 10
-4: 0.4, regulating its pH value with Sodium phosphate dibasic-citrate buffer solution is 3.0, adsorbs crosslinked 2 hours;
In (2)-2., the temperature of carrying out oxydasis is 35 ℃, the speed that filtered liquid pumps into be 2 times of immobilized glucose oxidase resin volumes/hour;
In (3)-1. step, the deionization bubble that adds 3 times of D293 anionite-exchange resin volumes was washed 12 hours, and the sodium-chlor mass concentration that adds 2 times of D293 anionite-exchange resin volumes again is 10% sodium chloride solution, and bubble was washed 2 hours;
(3)-2. the step in, the oxydasis liquid pump go into speed be 7 times of D293 anionite-exchange resin volumes/hour;
In (4) step, the distilled water that is used to clean is 2 times of D293 anionite-exchange resin volumes, the speed that 7% sodium hydroxide solution pumps into be 3 times D293 anionite-exchange resin volume/hour, elutriant in the rotatory evaporator, under 80 ℃ of temperature, it is 50% Sunmorl N 60S concentrated solution that heating is concentrated into the Sunmorl N 60S mass concentration, is that 85% ethanolic soln cleans 2 times to the gluconic acid sodium crystal after the crystallization with the ethanol mass concentration, to the gluconic acid sodium crystal after cleaning, under 50 ℃ of temperature, carry out drying, make the Sunmorl N 60S mass content and be 96% gluconic acid sodium crystal.
3. according to the described method that from xylose crystallization mother liquor, prepares Sunmorl N 60S of claim 1, it is characterized in that concrete step is as follows:
In (1) step, xylose crystallization mother liquor: the volume ratio of pure water is 1: 2.5, and the molecular weight cut-off of nanofiltration membrane is 3000Da, and the water bath with thermostatic control temperature that concentrates trapped fluid is 90 ℃;
In (2)-1. step, cross-linked chitosan-Methionin resin carrier amino: glucose oxidase: the mol ratio of glutaraldehyde is 1: 1.35 * 10
-4: 0.55, regulating its pH value with Sodium phosphate dibasic-citrate buffer solution is 4.0, adsorbs crosslinked 3 hours;
In (2)-2., the temperature of carrying out oxydasis is 40 ℃, the speed that filtered liquid pumps into be 4 times of immobilized glucose oxidase resin volumes/hour;
In (3)-1. step, the deionization bubble that adds 4 times of D293 anionite-exchange resin volumes was washed 13 hours, and the sodium-chlor mass concentration that adds 3 times of D293 anionite-exchange resin volumes again is 10% sodium chloride solution, and bubble was washed 3 hours;
(3)-2. the step in, the oxydasis liquid pump go into speed be 8 times of D293 anionite-exchange resin volumes/hour;
In (4) step, the distilled water that is used to clean is 2.5 times of D293 anionite-exchange resin volumes, the speed that 7% sodium hydroxide solution pumps into be 3.5 times D293 anionite-exchange resin volume/hour, elutriant in the rotatory evaporator, under 90 ℃ of temperature, it is 53% Sunmorl N 60S concentrated solution that heating is concentrated into the Sunmorl N 60S mass concentration, is that 85% ethanolic soln cleans 3 times to the gluconic acid sodium crystal after the crystallization with the ethanol mass concentration, to the gluconic acid sodium crystal after cleaning, under 55 ℃ of temperature, carry out drying, make the Sunmorl N 60S mass content and be 97% gluconic acid sodium crystal.
4. according to the described method that from xylose crystallization mother liquor, prepares Sunmorl N 60S of claim 1, it is characterized in that concrete step is as follows:
In (1) step, xylose crystallization mother liquor: the volume ratio of pure water is 1: 5, and the molecular weight cut-off of nanofiltration membrane is 6000Da, and the water bath with thermostatic control temperature that concentrates trapped fluid is 100 ℃;
In (2)-1. step, cross-linked chitosan-Methionin resin carrier amino: glucose oxidase: the mol ratio of glutaraldehyde is 1: 2.0 * 10
-4: 0.6, regulating its pH value with Sodium phosphate dibasic-citrate buffer solution is 5.0, adsorbs crosslinked 4 hours;
In (2)-2., the temperature of carrying out oxydasis is 45 ℃, the speed that filtered liquid pumps into be 6 times of immobilized glucose oxidase resin volumes/hour;
In (3)-1. step, the deionization bubble that adds 5 times of D293 anionite-exchange resin volumes was washed 14 hours, and the sodium-chlor mass concentration that adds 5 times of D293 anionite-exchange resin volumes again is 10% sodium chloride solution, and bubble was washed 5 hours;
(3)-2. the step in, the oxydasis liquid pump go into speed be 9 times of D293 anionite-exchange resin volumes/hour;
In (4) step, the distilled water that is used to clean is 3 times of D293 anionite-exchange resin volumes, the speed that 7% sodium hydroxide solution pumps into be 4 times D293 anionite-exchange resin volume/hour, elutriant in the rotatory evaporator, under 100 ℃ of temperature, it is 55% Sunmorl N 60S concentrated solution that heating is concentrated into the Sunmorl N 60S mass concentration, is that 85% ethanolic soln cleans 4 times to the gluconic acid sodium crystal after the crystallization with the ethanol mass concentration, to the gluconic acid sodium crystal after cleaning, under 60 ℃ of temperature, carry out drying, make the Sunmorl N 60S mass content and be 98% gluconic acid sodium crystal.
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| CN102701951A (en) * | 2012-05-22 | 2012-10-03 | 华东理工大学 | Method for producing sodium gluconate from sodium gluconate fermentation liquid |
| CN103409315A (en) * | 2013-07-15 | 2013-11-27 | 重庆大学 | Reaction separating and coupling apparatus, and technology for preparation of gluconic acid from xylitol crystallization mother liquor |
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| CN102701951A (en) * | 2012-05-22 | 2012-10-03 | 华东理工大学 | Method for producing sodium gluconate from sodium gluconate fermentation liquid |
| CN102701951B (en) * | 2012-05-22 | 2014-07-30 | 华东理工大学 | Method for producing sodium gluconate from sodium gluconate fermentation liquid |
| CN103409315A (en) * | 2013-07-15 | 2013-11-27 | 重庆大学 | Reaction separating and coupling apparatus, and technology for preparation of gluconic acid from xylitol crystallization mother liquor |
| CN103980110A (en) * | 2014-05-07 | 2014-08-13 | 内蒙古玉王生物科技开发有限公司 | Combined separation, purification and extraction process for sodium gluconate mother liquor |
| CN103980110B (en) * | 2014-05-07 | 2015-11-25 | 内蒙古玉王生物科技开发有限公司 | Gluconic acid mother liquid of sodium combination isolation of purified extraction process |
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