CN100413973C - Method for producing gluconic acid lactone - Google Patents
Method for producing gluconic acid lactone Download PDFInfo
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- CN100413973C CN100413973C CNB02151254XA CN02151254A CN100413973C CN 100413973 C CN100413973 C CN 100413973C CN B02151254X A CNB02151254X A CN B02151254XA CN 02151254 A CN02151254 A CN 02151254A CN 100413973 C CN100413973 C CN 100413973C
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- crystallization
- gluconolactone
- fermentation
- sugar
- seed culture
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Abstract
The present invention discloses a method for producing glucolactone. In the method, aspergillus niger M290 is used to ferment amylolytic sugar; firstly, the amylolytic sugar is converted into calcium gluconate by the steps of seed cultivation, fermentation, mycelium removal, decolorization, decalcification by ion exchange, concentration, crystallization, drying, etc.; then, the calcium gluconate is converted into gluconic acid by removing calcium ions through ionexchange resin; and finally, glucolactone is generated by concentration and crystallization. The method has the characteristics of simple operating technology and low energy consumption.
Description
Technical field
The present invention relates to a kind of production method of glucolactone, particularly adopt the fermentation of Aspergillus niger amylum hydrolysate of the sugar, generate calglucon earlier, produce the method for Gluconolactone again through the Zeo-karb decalcification.
Background technology
Gluconolactone be glucono delta lactone (abbreviation of Glucono-δ-lactone), outward appearance is white crystal or crystalline powder, is slightly soluble in ethanol, very easily water-soluble, hydrolysis is slow under room temperature or the lesser temps, and along with the rising of temperature, hydrolysis rate is accelerated.Glucono delta lactone is the nontoxic foodstuff additive of generally acknowledging in the world at present, can be used for making the peptizer of bean curd, makes the raising agent of bread, makes the souring agent and the sanitas of cheese class, makes the toner of sausage ham.Also can be used as industrial additive, be used for preparing clean-out system, add toothpaste and help to remove tartar, be used for the generation that milk industry prevents mammary calculus, be used for the generation that brewery industry prevents beer scale, and as the pH depressant etc.
Mainly contain two kinds of methods with glucose for the raw material production Gluconolactone: a kind of is to adopt enzyme process and electrochemical process, with the direct catalyzed oxidation of glucose is Gluconolactone, present method transformation efficiency is low, reaction control difficulty, and the making step of catalyzer is loaded down with trivial details, this method is only limited to the laboratory study stage at present, successfully is not used for suitability for industrialized production.Another kind method is to produce Gluconolactone by gluconate.Present method is divided microbe fermentation method and air catalytic oxidation method again.Catalyst metal palladium source difficulty in the air catalytic oxidation method, method for preparing catalyst requires high, thereby the air catalytic oxidation method is not used widely.Microbe fermentation method, because the transformation efficiency height, production cost is lower, is easy to carry out suitability for industrialized production, thereby microbe fermentation method is mainly adopted in the production of Gluconolactone at present.
Microbe fermentation method is divided into calcium salt method and sodium salt method.In the calcium salt method, earlier glucose is converted into calglucon through the gluconic acid that microbial fermentation generates, crystallization goes out calglucon from fermented liquid through concentrating again, then with calglucon through the acidifying decalcification, calcium ion is removed in ion-exchange, and last condensing crystal is separated out Gluconolactone.In the sodium salt method, earlier gluconic acid is converted into sodium salt, removes sodium ion through ion-exchange again, last condensing crystal is separated out Gluconolactone.
In the above-mentioned calcium salt method, fermented liquid earlier generates calglucon through condensing crystal, acidifying decalcification again, and sulfuric acid is used in the acidifying decalcification, and temperature of reaction is up to 100 ℃, and to the equipment requirements height, and fermented liquid will concentrate through twice, just can obtain Gluconolactone, the energy consumption height.The sodium salt method is low at calglucon solubleness in the calcium salt method, can not carry out the problem of high sugar-fermenting, add the sodium hydroxide of high density during the fermentation, the pH value of control fermented liquid, the fermentation later stage is added glucose, carries out high sugar-fermenting, and this method adopts stream to add fermentation, and the interpolation high-concentration sodium hydroxide is to equipment and operational requirement height, easily microbiological contamination.
Summary of the invention
At the problem that exists in above-mentioned calcium salt method and the sodium salt method, the present invention adopts the fermentation of Aspergillus niger amylum hydrolysate of the sugar, generate calglucon earlier, remove calcium ion through Zeo-karb again, save steps such as calglucon condensing crystal and acidifying decalcification, thereby reach the purpose of simplifying technological operation and cutting down the consumption of energy.
The present invention adopts aspergillus niger M290 fermentation amylum hydrolysate of the sugar, through seed culture, fermentation, remove thalline, decolouring, ion-exchange decalcification, concentrate, crystallization and drying and other steps, with amylum hydrolysate of the sugar, be converted into calglucon earlier, remove calcium ion through ion exchange resin again, be converted into gluconic acid, condensing crystal generates Gluconolactone then.Step of the present invention is as follows:
1. seed liquor is cultivated:
Aspergillus niger M290 slant strains (czapek's solution) is chosen seed culture medium after an articulating is gone into sterilization, and in 30 ℃, 180rpm cultivated 20 hours, seed culture fluid.The composition of seed culture medium (mass percent concentration): glucose 3%, wheat bran 2%, KH
2PO
40.03%, (NH4)
2HPO
40.04%, CaCO
31%, MnSO
46ppm, natural pH value.
2. fermentation
With the inoculum size access fermention medium of seed liquor with 10% weight ratio, cultivated 40～44 hours for 30 ℃, be calglucon with conversion of glucose, the composition of fermention medium (mass percent concentration): amylum hydrolysate of the sugar 20% (with glucose meter), KH
2PO
40.03%, (NH4)
2HPO
40.03%, MgSO
40.02%, CaCO
3(10%-20% of sugar amount), MnSO
48ppm, natural pH value.
3. remove thalline
Put a jar filtration sterilization body.
4. decolouring
Adding weight ratio and be 2% gac boils and decolours the centrifugal again gac of removing.
5. cationic exchange is removed calcium ion
To remove calcium ion through Zeo-karb through the fermented liquid of decolouring.
6. condensing crystal:
To 1/5th of original volume, put into crystallizer adding weight ratio is the crystal seed of 0.1～0.2% Gluconolactone to deionization liquid, 48 ℃～52 ℃ following stirred crystallization at 80 ℃ of following vacuum concentration.
7. the whizzer centrifuge dehydration is put in the gained crystallization, with a small amount of cold water washing three times, in 60 ℃ of oven dry, promptly gets Gluconolactone then.Centrifuge dehydration liquid and three washingss merge, the reconcentration crystallization once, to improve the yield of Gluconolactone.
The present invention is further illustrated below by embodiment, but should be appreciated that these embodiment are only used for illustrating the present invention, rather than limitation of the present invention.Those of ordinary skill in the art replaces the present invention on the basis of specification sheets of the present invention and changes, and all should comprise within the scope of the invention.
Embodiment 1
The 100 milliliters of above-mentioned seed culture mediums of packing in 500 milliliters of triangular flasks insert a ring M290 slant preservation bacterial classification, and in 30 ℃, 180rpm cultivates and made seed liquor in 20 hours.Be respectively charged into 30 milliliters of above-mentioned fermention mediums in 30-37 ℃ in 25 500 milliliters of triangular flasks, 300rpm cultivated 44 hours.Fermented liquid is in 80 ℃ of heating in water bath 15 minutes, suction filtration, and use hot wash, 1100 milliliters of fermented liquids.Filtrate adds the gac boiling decoloring, and suction filtration gets destainer again.Destainer is removed calcium ion by ion exchange resin column (φ 20 * 400), and deionization liquid is dry that Gluconolactone 98 restrains through condensing crystal, and Gluconolactone is 65.33% to the yield of glucose.
Embodiment 2
The 10 liters of fermention mediums of packing in 30 liters of machinery fermentation stirred pots insert the seed liquor of making by seed liquor cultural method of the present invention by 10% inoculum size, stir fermentation 44 hours at 30-37 ℃, and mixing speed is 500～700rpm, and air flow is 1.5～2.0m
3/ m
3Min, fermented liquid is heated to 80 ℃ of insulations and removes by filter thalline with whizzer after 15 minutes, filtrate adds the gac boiling decoloring, destainer removes calcium ion by cationic exchange coloum (φ 60 * 700), deionization liquid is through dry 1.23 kilograms of the Gluconolactones that get of condensing crystal, and Gluconolactone is 62.5% to the yield of glucose.
Embodiment 3
The 20 liters of seed culture mediums of in 30 liters of machinery fermentation stirred pots, packing into, insert the seed liquor of making by seed liquor cultural method of the present invention by 10% inoculum size, 30 ℃ of stir culture 20 hours, make secondary seed solution, secondary seed is inserted 500 liters of mechanical agitator tanks that 200 liters of fermention mediums are housed, mixing speed is 500～700rpm, and the condition of pressing embodiment 2 was fermented 44 hours.Fermented liquid removes calcium ion by cationic exchange coloum (φ 120 * 1500) after removing the thalline decolouring, and deionization liquid is through dry 24.6 kilograms of the Gluconolactones that get of condensing crystal, and Gluconolactone is 61.5% to the yield of glucose.
Claims (5)
1. method of producing Gluconolactone, it is characterized in that adopting aspergillus niger M290 fermentation amylum hydrolysate of the sugar, through seed culture, fermentation, remove thalline, decolouring, the ion-exchange decalcification, concentrate, crystallization and drying step, wherein ferment amylum hydrolysate of the sugar is converted into calglucon, the ion-exchange decalcification is meant through ion exchange resin and removes calcium ion, be converted into gluconic acid, concentrate, crystallization is that condensing crystal generates Gluconolactone, deionization liquid at 80 ℃ of following vacuum concentration to 1/5th of original volume, putting into crystallizer adding weight ratio is the crystal seed of 0.1～0.2% Gluconolactone, 48 ℃～52 ℃ following stirred crystallization;
Wherein, described seed culture is carried out under the following conditions: aspergillus niger M290 slant strains is chosen seed culture medium after an articulating is gone into sterilization, in 30 ℃, 180rpm cultivated 20 hours, seed culture fluid, the composition of seed culture medium is in mass concentration: glucose 3%, wheat bran 2%, KH
2PO
40.03%, (NH4)
2HPO
40.04%, CaCO
31%, and MnSO
46ppm, natural pH value;
Wherein, described fermentation is carried out under the following conditions: seed liquor is inserted fermention medium with 10% inoculum size, cultivated 40～44 hours, and be calglucon with conversion of glucose for 30-37 ℃, the composition of fermention medium is in mass concentration: with the glucose meter amylum hydrolysate of the sugar is 20%, KH
2PO
40.03%, (NH4)
2HPO
40.03%, MgSO
40.02%, CaCO
3Be the 10%-20% of sugar amount, and MnSO
48ppm, natural pH value.
2. the method for claim 1 is characterized in that the described thalline that removes is undertaken by putting a jar filtration.
3. the method for claim 1 is characterized in that described decolouring undertaken by following steps: add weight ratio and be 2% gac and boil and decolour the centrifugal again gac of removing.
4. the method for claim 1 is characterized in that and will remove calcium ion through Zeo-karb through the fermented liquid of decolouring.
5. the method for claim 1 is characterized in that the gained crystallization puts into the whizzer centrifuge dehydration, with a small amount of cold water washing three times, in 60 ℃ of oven dry, promptly gets Gluconolactone then, and centrifuge dehydration liquid and three washingss merge, and the reconcentration crystallization once.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB02151254XA CN100413973C (en) | 2002-12-13 | 2002-12-13 | Method for producing gluconic acid lactone |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB02151254XA CN100413973C (en) | 2002-12-13 | 2002-12-13 | Method for producing gluconic acid lactone |
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|---|---|
| CN1508255A CN1508255A (en) | 2004-06-30 |
| CN100413973C true CN100413973C (en) | 2008-08-27 |
Family
ID=34234351
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB02151254XA Expired - Fee Related CN100413973C (en) | 2002-12-13 | 2002-12-13 | Method for producing gluconic acid lactone |
Country Status (1)
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Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102489027B (en) * | 2011-12-12 | 2014-06-04 | 山东凯翔生物化工有限公司 | Energy-saving concentration method and device for glucono-delta-lactones |
| CN104447653A (en) * | 2014-11-05 | 2015-03-25 | 朱忠良 | Production method of glucono-delta-lactone |
| CN106244647B (en) * | 2016-08-24 | 2020-04-24 | 德州汇洋生物科技有限公司 | Method for simultaneously preparing trehalose and gluconolactone |
| CN115154415B (en) * | 2022-08-04 | 2024-03-08 | 山东新华制药股份有限公司 | Preparation method of calcium gluconate injection |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1155012A (en) * | 1996-10-10 | 1997-07-23 | 中山大学 | Production of lactone gluconate by using black aspergillus to ferment glucose |
-
2002
- 2002-12-13 CN CNB02151254XA patent/CN100413973C/en not_active Expired - Fee Related
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1155012A (en) * | 1996-10-10 | 1997-07-23 | 中山大学 | Production of lactone gluconate by using black aspergillus to ferment glucose |
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| CN1508255A (en) | 2004-06-30 |
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