CN101284775A - Process for reclaiming 2-keto-L-gulonate by salting out method - Google Patents
Process for reclaiming 2-keto-L-gulonate by salting out method Download PDFInfo
- Publication number
- CN101284775A CN101284775A CNA2008100499813A CN200810049981A CN101284775A CN 101284775 A CN101284775 A CN 101284775A CN A2008100499813 A CNA2008100499813 A CN A2008100499813A CN 200810049981 A CN200810049981 A CN 200810049981A CN 101284775 A CN101284775 A CN 101284775A
- Authority
- CN
- China
- Prior art keywords
- keto
- gulonate
- mother liquor
- sodium
- gulonic
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- 238000000034 method Methods 0.000 title claims abstract description 30
- 238000005185 salting out Methods 0.000 title claims abstract description 11
- VBUYCZFBVCCYFD-NUNKFHFFSA-N 2-dehydro-L-idonic acid Chemical compound OC[C@H](O)[C@@H](O)[C@H](O)C(=O)C(O)=O VBUYCZFBVCCYFD-NUNKFHFFSA-N 0.000 title claims description 46
- 239000012452 mother liquor Substances 0.000 claims abstract description 36
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims abstract description 15
- 239000011734 sodium Substances 0.000 claims abstract description 15
- 229910052708 sodium Inorganic materials 0.000 claims abstract description 15
- 239000002253 acid Substances 0.000 claims description 12
- 239000013078 crystal Substances 0.000 claims description 10
- 238000000605 extraction Methods 0.000 claims description 9
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 8
- 238000003756 stirring Methods 0.000 claims description 8
- DPDMMXDBJGCCQC-UHFFFAOYSA-N [Na].[Cl] Chemical group [Na].[Cl] DPDMMXDBJGCCQC-UHFFFAOYSA-N 0.000 claims description 7
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 claims description 6
- 229910052938 sodium sulfate Inorganic materials 0.000 claims description 6
- 235000011152 sodium sulphate Nutrition 0.000 claims description 6
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 4
- 235000017550 sodium carbonate Nutrition 0.000 claims description 4
- 239000002244 precipitate Substances 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 claims description 2
- 230000001105 regulatory effect Effects 0.000 claims description 2
- 239000002699 waste material Substances 0.000 abstract description 5
- 238000011084 recovery Methods 0.000 abstract description 3
- 159000000000 sodium salts Chemical class 0.000 abstract 1
- 239000000126 substance Substances 0.000 abstract 1
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 6
- 238000001914 filtration Methods 0.000 description 5
- 239000007788 liquid Substances 0.000 description 5
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 4
- 235000019154 vitamin C Nutrition 0.000 description 4
- 239000011718 vitamin C Substances 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- 238000007599 discharging Methods 0.000 description 3
- 238000001291 vacuum drying Methods 0.000 description 3
- 238000005406 washing Methods 0.000 description 3
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 238000013019 agitation Methods 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 238000004042 decolorization Methods 0.000 description 2
- 230000032050 esterification Effects 0.000 description 2
- 238000005886 esterification reaction Methods 0.000 description 2
- 238000000855 fermentation Methods 0.000 description 2
- 230000004151 fermentation Effects 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- MEIRRNXMZYDVDW-MQQKCMAXSA-N (2E,4E)-2,4-hexadien-1-ol Chemical compound C\C=C\C=C\CO MEIRRNXMZYDVDW-MQQKCMAXSA-N 0.000 description 1
- FRXSZNDVFUDTIR-UHFFFAOYSA-N 6-methoxy-1,2,3,4-tetrahydroquinoline Chemical compound N1CCCC2=CC(OC)=CC=C21 FRXSZNDVFUDTIR-UHFFFAOYSA-N 0.000 description 1
- LKDRXBCSQODPBY-AMVSKUEXSA-N L-(-)-Sorbose Chemical compound OCC1(O)OC[C@H](O)[C@@H](O)[C@@H]1O LKDRXBCSQODPBY-AMVSKUEXSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000003610 charcoal Substances 0.000 description 1
- 230000008030 elimination Effects 0.000 description 1
- 238000003379 elimination reaction Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 239000000284 extract Substances 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- -1 sodium-chlor Chemical compound 0.000 description 1
Landscapes
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention relates to a method for reclaiming 2-Keto-L-gulonic sodium by a salting out method. The crystallized mother liquor of 2-Keto-L-gulonic sodium or the extracted mother liquor of 2-Keto-L-gulonic sodium is heated to 30 to 40 DEG C, then inorganic sodium salt is added into the mother liquor while being stirred, then the temperature of the mother liquor is reduced to 10 to 15 DEG C, the temperature is kept for 2 to 10 h until 2-Keto-L-gulonic sodium is no longer separated out, and the separated educt is 2-Keto-L-gulonic sodium, wherein the pH value of the crystallized mother liquor of 2-Keto-L-gulonic sodium is adjusted to 5-7 before being heated. The method reclaims 2-Keto-L-gulonic sodium in discharged waste liquor, and has the advantages that the method is simple, the operation is convenient, the recovery rate is more than 70 percent, and simultaneously the pollution of organic substances in the discharged waste liquor is reduced.
Description
(1) technical field
The present invention relates to the method that a kind of salting-out process reclaims the 2-keto-L-gulonate.
(2) background technology
The 2-keto-L-gulonate is the intermediate that generates in synthesise vitamins C process, and industrial main employing two-step fermenting is produced: generate sorbose by sorbyl alcohol through one-step fermentation, generate the 2-keto-L-gulonate through two stage fermentation again.Thereafter 2-keto-L-gulonate fermented liquid is after removing impurity such as thalline, albumen, and concentration extraction 2-ketone group after Zeo-karb takes off sodium-L-Gu is imperial sour, and is sour through esterification, conversion synthesise vitamins C sodium with the ancient dragon of 2-ketone group-L-again; Also can be with direct concentration extraction 2-keto-L-gulonate after the fermented liquid removal of impurities of 2-keto-L-gulonate, again in methyl alcohol with 2-keto-L-gulonate sulfuric acid acidation, remove sodium sulfate after esterification, conversion synthesise vitamins C sodium.In the process of ancient imperial acid of 2-ketone group-L-or 2-keto-L-gulonate concentration extraction, there is a certain amount of mother liquor to reclaim, as the mother liquor behind the ancient imperial acid crystal of 2-ketone group-L-, and the mother liquor after the extraction of 2-keto-L-gulonate, industrial generally as discharging of waste liquid, but this processing mode had both increased environmental pollution, can influence product yield again.
(3) summary of the invention
The object of the present invention is to provide a kind of salting-out process to reclaim the method for 2-keto-L-gulonate, mother liquor behind the ancient imperial acid crystal of the 2-ketone group-L-that produces in the vitamins C building-up process or the mother liquor after the extraction of 2-keto-L-gulonate are utilized, reclaim 2-keto-L-gulonate wherein, reduce the pollution of discharge environment.
The technical solution used in the present invention is as follows:
A kind of salting-out process reclaims the method for 2-keto-L-gulonate, mother liquor behind the ancient imperial acid crystal of 2-ketone group-L-or the mother liquor after the extraction of 2-keto-L-gulonate are heated to 30-40 ℃, stir then and add inorganic sodium down, fully be cooled to 10-15 ℃ after the dissolving, keep 2-10h to 2-keto-L-gulonate no longer to separate out, separate precipitate and be the 2-keto-L-gulonate; Wherein be 5-7 for regulating its pH value before the mother liquor heating behind the ancient imperial acid crystal of 2-ketone group-L-.
Present method is to utilize common-ion effcet that the 2-keto-L-gulonate is separated out from solution, the pH value by adjusting solution and the difference of the solubleness of solute when utilizing differing temps, the 2-keto-L-gulonate is farthest separated out from mother liquor, improve its rate of recovery, reduce organic content in the mother liquor, reduce and pollute.
Further, the preferred sodium-chlor of described inorganic sodium, yellow soda ash or sodium sulfate, the amount of adding and the weight ratio of mother liquor are 1: 5-20.
Further again, the mother liquor after the mother liquor behind the ancient imperial acid crystal of 2-ketone group-L-or 2-keto-L-gulonate extracted decolours and handles the back reheat.Specifically can use activated carbon decolorizing, the amount of adding is the 0.5-2% of mother liquor quality.
Concrete, described salting-out process reclaims the method for the 2-keto-L-gulonate in the mother liquor to carry out according to the following steps:
With sodium hydroxide or yellow soda ash adjust behind the ancient imperial acid crystal of 2-ketone group-L-mother liquor to pH be 5-7, add the activated carbon decolorizing of mother liquor quality 0.5-2% then, filter.Mother liquor after the 2-keto-L-gulonate extracts in this way, directly decolorization filtering.
Mother liquor behind the decolorization filtering is heated to 30-40 ℃, stir the inorganic sodium such as sodium-chlor, yellow soda ash or the sodium sulfate that add mother liquor quality 5-20% down then, fully be cooled to 10-15 ℃ after the dissolving, keep 2-10h to 2-keto-L-gulonate no longer to separate out, separate precipitate and be the 2-keto-L-gulonate with a small amount of frozen water washing.
The present invention has following advantage with respect to prior art:
Present method reclaims the 2-keto-L-gulonate in the discharging waste liquid, and method is simple, and is easy to operate, and the rate of recovery has alleviated organic pollution in the discharging waste liquid simultaneously up to more than 70%.
(4) embodiment:
Below with specific embodiment technical scheme of the present invention is described, but protection scope of the present invention is not limited thereto:
Embodiment 1
Getting mother liquor 500mL behind the ancient imperial acid crystal of 2-ketone group-L-, to place volume be the beaker of 1000ml, the ancient imperial acid content 185g/L (counting 223g/L) of 2-ketone group-L-wherein with 2-keto-L-gulonate content, stirring down and being neutralized to the pH value with 40% sodium hydroxide is 6; Maintain under 40 ℃ of conditions, stir and add 70 gram sodium-chlor, continue stirring sodium-chlor is dissolved fully, be cooled to 10 ℃ then, kept 4 hours, with the 2-keto-L-gulonate filtering separation of separating out, and with the washing of a small amount of frozen water, vacuum-drying gets 2-keto-L-gulonate 84.1g, and content is 93.2%, pure is 78.4g, and yield is 70.3%.
Embodiment 2
Getting mother liquor after the 500ml 2-keto-L-gulonate concentration extraction, to place volume be the beaker of 1000ml, and wherein 2-keto-L-gulonate content is 161.3g/L; Mother liquor is heated to 35 ℃, under agitation add 80 gram sodium-chlor, continue stirring sodium-chlor is dissolved fully, be cooled to 12 ℃ then, and kept 5 hours, with the 2-keto-L-gulonate filtering separation of separating out, and with the washing of a small amount of frozen water, vacuum-drying gets 2-keto-L-gulonate 60.5g, and content is 88.2%, pure is 53.3g, and yield is 66.1%.
Embodiment 3
Getting mother liquor after the 500ml 2-keto-L-gulonate concentration extraction, to place volume be the beaker of 1000ml, and wherein 2-keto-L-gulonate content is 161.3g/L; Mother liquor is added charcoal absorption decolouring, elimination gac then; Solution is heated to 40 ℃, under agitation adds 80 gram sodium sulfate, continue stirring sodium sulfate is dissolved fully, be cooled to 15 ℃ then, and kept 3 hours, the 2-keto-L-gulonate of separating out was stirred 1 hour, then be cooled to 10 ℃, left standstill 2.5 hours, and separated the 2-keto-L-gulonate after filtration, and wash with a small amount of frozen water, vacuum-drying gets 2-keto-L-gulonate 58.9g, content is 87.6%, and pure is 51.6g, and yield is 64%.
Claims (4)
1. a salting-out process reclaims the method for 2-keto-L-gulonate, it is characterized in that mother liquor behind the ancient imperial acid crystal of 2-ketone group-L-or the mother liquor after the extraction of 2-keto-L-gulonate are heated to 30-40 ℃, stir then and add inorganic sodium down, fully be cooled to 10-15 ℃ after the dissolving, keep 2-10h to 2-keto-L-gulonate no longer to separate out, separate precipitate and be the 2-keto-L-gulonate; Wherein be 5-7 for regulating its pH value before the mother liquor heating behind the ancient imperial acid crystal of 2-ketone group-L-.
2. salting-out process as claimed in claim 1 reclaims the method for 2-keto-L-gulonate, it is characterized in that the amount of inorganic sodium adding and the weight ratio of mother liquor are 1: 5-20.
3. salting-out process as claimed in claim 2 reclaims the method for 2-keto-L-gulonate, it is characterized in that described inorganic sodium is sodium-chlor, yellow soda ash or sodium sulfate.
4. reclaim the method for 2-keto-L-gulonate as the described salting-out process of one of claim 1-3, the mother liquor after it is characterized in that the mother liquor behind the ancient imperial acid crystal of 2-ketone group-L-or 2-keto-L-gulonate extracted decolours and handles the back reheat.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2008100499813A CN101284775B (en) | 2008-06-06 | 2008-06-06 | Process for reclaiming 2-keto-L-gulonate by salting out method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2008100499813A CN101284775B (en) | 2008-06-06 | 2008-06-06 | Process for reclaiming 2-keto-L-gulonate by salting out method |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN101284775A true CN101284775A (en) | 2008-10-15 |
| CN101284775B CN101284775B (en) | 2011-05-11 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2008100499813A Active CN101284775B (en) | 2008-06-06 | 2008-06-06 | Process for reclaiming 2-keto-L-gulonate by salting out method |
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| Country | Link |
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| CN (1) | CN101284775B (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102267962A (en) * | 2010-06-01 | 2011-12-07 | 河北维尔康制药有限公司 | Method for recovering vitamin C from vitamin C secondary mother liquor |
| CN103073601A (en) * | 2013-02-01 | 2013-05-01 | 东北制药集团股份有限公司 | Controllable concentration and crystallization method for adding seed crystals to 2-keto-L-gulonic acid solution |
| CN108774125A (en) * | 2018-05-28 | 2018-11-09 | 苏州澄江环境科技有限公司 | A kind of technique recycling raw material from gulonic acid mother solution |
-
2008
- 2008-06-06 CN CN2008100499813A patent/CN101284775B/en active Active
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102267962A (en) * | 2010-06-01 | 2011-12-07 | 河北维尔康制药有限公司 | Method for recovering vitamin C from vitamin C secondary mother liquor |
| CN103073601A (en) * | 2013-02-01 | 2013-05-01 | 东北制药集团股份有限公司 | Controllable concentration and crystallization method for adding seed crystals to 2-keto-L-gulonic acid solution |
| CN108774125A (en) * | 2018-05-28 | 2018-11-09 | 苏州澄江环境科技有限公司 | A kind of technique recycling raw material from gulonic acid mother solution |
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| Publication number | Publication date |
|---|---|
| CN101284775B (en) | 2011-05-11 |
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Effective date of registration: 20231017 Address after: 458000 No.9 Muping Road, Shancheng District, Hebi City, Henan Province Patentee after: Xintuoyang Bioengineering Co.,Ltd. Address before: 450002 No. 76 science Avenue, Henan, Zhengzhou Patentee before: ZHENGZHOU TUOYANG INDUSTRIAL CO.,LTD. |
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