CN101508496B - Method for purification of macromolecule chromophoric matter in water from Vc fermentation wastewater by biochemical treatment - Google Patents
Method for purification of macromolecule chromophoric matter in water from Vc fermentation wastewater by biochemical treatment Download PDFInfo
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- CN101508496B CN101508496B CN2009100260436A CN200910026043A CN101508496B CN 101508496 B CN101508496 B CN 101508496B CN 2009100260436 A CN2009100260436 A CN 2009100260436A CN 200910026043 A CN200910026043 A CN 200910026043A CN 101508496 B CN101508496 B CN 101508496B
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- water
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- fermentation
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 57
- 238000000034 method Methods 0.000 title claims abstract description 26
- 238000000855 fermentation Methods 0.000 title claims abstract description 13
- 230000004151 fermentation Effects 0.000 title claims abstract description 13
- 239000002351 wastewater Substances 0.000 title claims abstract description 11
- 238000000746 purification Methods 0.000 title claims description 16
- 229920002521 macromolecule Polymers 0.000 title description 2
- 239000012530 fluid Substances 0.000 claims abstract description 40
- 238000000108 ultra-filtration Methods 0.000 claims abstract description 39
- 239000012528 membrane Substances 0.000 claims abstract description 23
- 230000000149 penetrating effect Effects 0.000 claims abstract description 18
- 238000001914 filtration Methods 0.000 claims abstract description 8
- 238000009826 distribution Methods 0.000 claims abstract description 6
- 238000001641 gel filtration chromatography Methods 0.000 claims abstract description 6
- 229910021642 ultra pure water Inorganic materials 0.000 claims abstract description 5
- 239000012498 ultrapure water Substances 0.000 claims abstract description 5
- 239000007787 solid Substances 0.000 claims abstract description 3
- 239000000463 material Substances 0.000 claims description 37
- 239000002921 fermentation waste Substances 0.000 claims description 17
- 229910017053 inorganic salt Inorganic materials 0.000 claims description 8
- 229920002307 Dextran Polymers 0.000 claims description 6
- 239000004627 regenerated cellulose Substances 0.000 claims description 6
- 238000000926 separation method Methods 0.000 claims description 6
- 238000000703 high-speed centrifugation Methods 0.000 claims description 5
- 239000012982 microporous membrane Substances 0.000 claims description 5
- 239000000126 substance Substances 0.000 claims description 5
- 238000005119 centrifugation Methods 0.000 claims description 4
- 238000002242 deionisation method Methods 0.000 claims description 4
- JEGUKCSWCFPDGT-UHFFFAOYSA-N h2o hydrate Chemical compound O.O JEGUKCSWCFPDGT-UHFFFAOYSA-N 0.000 claims 1
- 238000004519 manufacturing process Methods 0.000 abstract description 4
- 239000002245 particle Substances 0.000 abstract 1
- 150000003839 salts Chemical class 0.000 abstract 1
- 150000002500 ions Chemical class 0.000 description 12
- 229910052500 inorganic mineral Inorganic materials 0.000 description 10
- 239000011707 mineral Substances 0.000 description 10
- 238000004458 analytical method Methods 0.000 description 5
- 235000019154 vitamin C Nutrition 0.000 description 4
- 239000011718 vitamin C Substances 0.000 description 4
- 230000015556 catabolic process Effects 0.000 description 3
- 238000006731 degradation reaction Methods 0.000 description 3
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 description 2
- 238000011088 calibration curve Methods 0.000 description 2
- 239000000284 extract Substances 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 238000005304 joining Methods 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 239000003643 water by type Substances 0.000 description 2
- BHPQYMZQTOCNFJ-UHFFFAOYSA-N Calcium cation Chemical compound [Ca+2] BHPQYMZQTOCNFJ-UHFFFAOYSA-N 0.000 description 1
- FBPFZTCFMRRESA-FSIIMWSLSA-N D-Glucitol Natural products OC[C@H](O)[C@H](O)[C@@H](O)[C@H](O)CO FBPFZTCFMRRESA-FSIIMWSLSA-N 0.000 description 1
- ZZZCUOFIHGPKAK-UHFFFAOYSA-N D-erythro-ascorbic acid Natural products OCC1OC(=O)C(O)=C1O ZZZCUOFIHGPKAK-UHFFFAOYSA-N 0.000 description 1
- FBPFZTCFMRRESA-JGWLITMVSA-N D-glucitol Chemical compound OC[C@H](O)[C@@H](O)[C@H](O)[C@H](O)CO FBPFZTCFMRRESA-JGWLITMVSA-N 0.000 description 1
- JLVVSXFLKOJNIY-UHFFFAOYSA-N Magnesium ion Chemical compound [Mg+2] JLVVSXFLKOJNIY-UHFFFAOYSA-N 0.000 description 1
- 229910019142 PO4 Inorganic materials 0.000 description 1
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 1
- 229930003268 Vitamin C Natural products 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910001424 calcium ion Inorganic materials 0.000 description 1
- 150000001768 cations Chemical class 0.000 description 1
- 238000004587 chromatography analysis Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000010790 dilution Methods 0.000 description 1
- 239000012895 dilution Substances 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000000921 elemental analysis Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 229910001425 magnesium ion Inorganic materials 0.000 description 1
- 239000010452 phosphate Substances 0.000 description 1
- -1 phosphate anion Chemical class 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 229910001415 sodium ion Inorganic materials 0.000 description 1
- 229960002920 sorbitol Drugs 0.000 description 1
Landscapes
- Separation Using Semi-Permeable Membranes (AREA)
Abstract
The invention relates to a method for separating and purifying the macromolecular color development matters in the outputted water of the Vc fermentation wastewater biochemical treatment. The Vc fermentation wastewater is the wastewater produced by the two-step fermentation method for producing Vc. The method comprises the following steps: (1) centrifugating the outputted water at a high speed, and filtering the outputted water through a microporous filter membrane so as to remove the suspended matters and solid particles in the outputted water; (2) determining the molecular weight distribution of the water sample through a gel filtration chromatography so as to determine the parameters of the intercepted molecular weight of an ultrafiltration membrane in the step (3); (3) according to the result of the step (2), selecting an ultrafiltration membrane with a proper intercepted molecular weight so as to carry out the ultrafiltration to obtain a penetrating fluid containing inorganic salts and micromolecular organisms and a trapped fluid containing the macromolecular color development matters; (4) adding deionized ultra pure water into the trapped fluid, and repeating the step (3); and (5) repeating the step (3) and step (4).
Description
The present invention relates to the separating and purifying method of macromole chromonic material in the Vc fermentation waste water biochemical treatment water outlet, specifically, be to adopt ultra-filtration membrane to separating purification with inorganic salt with the macromole chromonic material of small organic molecule coexistence in the Vc fermentation waste water biochemical treatment water outlet.
Technical background
At present, industrial production vitamins C adopts two-step fermentation, and this method was found out by Chinese Academy of Sciences's Shanghai biotechnology research in 1975, belongs to China's initiative.Two-step fermentation is produced vitamins C can be divided into fermentation, extracts and transform three big steps.Promptly, extract the ancient dragon acid of vitamin C precursor 2-ketone group-L-, be converted into vitamins C with chemical method more earlier from the D-sorbitol fermentation.The fermentation waste water that emits in the Vc production process belongs to salinity height, high concentrated organic wastewater that colourity is high, and through after the biochemical treatment, wherein most of organism is by biological degradation, but because chromonic material has bio-refractory, so effluent color dilution is still higher.The wastewater discharge standard increasingly stringent of China, and colourity is related with COD and deposit, therefore chromonic material being carried out feature, to resolve and then set up high-efficient decolorizing method be that Vc industry adapts to countries and regions and carries mark and reduce discharging the key that requires.Prior art is not noted this, has influence on the subsequent disposal efficient to this water yet.
The prerequisite that adopts various modern analysis means that organism is analyzed is that this organism must have higher degree.The method that separating organic matters is purified in the solution has extraction, chromatography, post separation etc., mainly be to utilize that target compound is different with impurity polarity to separate purification, and impurity component is too much unsuitable.The Vc fermentation waste water after biochemical treatment, contain in the water outlet more not by biodegradable macromole chromonic material, solubleness height in water, polarity is strong; Simultaneously also contain a large amount of small organic molecules that form after multiple mineral ion and the biochemical treatment in the water outlet, complicated component, and in water the solubleness height, polarity is strong.Therefore, adopting aforesaid method the macromole chromonic material can't be separated purifies.
Summary of the invention
The present invention seeks to: the deficiency that overcomes above-mentioned purification technique, a kind of method of separating macromole chromonic material in the purification Vc fermentation waste water biochemical treatment water outlet is provided, propose a kind of simply, efficiently fast with macromole chromonic material and mineral ion, the isolating novel method of small organic molecule.
For solving the problems of the technologies described above, technical solution of the present invention is: the method for separating macromole chromonic material in the purification Vc fermentation waste water biochemical treatment water outlet, it is characterized in that described Vc fermentation waste water is that two-step fermentation is produced the waste water that produces in the Vc process, described biochemical treatment is that anaerobism adds aerobic associating biochemical treatment, and described macromole chromonic material is not by the biodegradable larger molecular organics that contains chromophoric group after biochemical treatment.Vc fermentation waste water complicated component contains large amount of organic and mineral ion, and in described biochemical treatment, most of organism has been formed small organic molecule by biological degradation, and the macromole chromonic material is not by biological degradation.Small organic molecule and mineral ion cause obstacle to the analysis of macromole chromonic material, must separate purification to the macromole chromonic material.Described separating and purifying method comprises
(1) waste water that will adopt two-step fermentation to produce to produce in the Vc process to the water outlet high speed centrifugation, and use filtering with microporous membrane, removal suspended substance and solid particulate wherein after anaerobism adds aerobic associating biochemical treatment;
(2) molecular weight distribution of this water sample of employing gel filtration chromatography is with the molecular weight cut-off of ultra-filtration membrane in the determining step (3);
(3) according to the result of step (2), the ultra-filtration membrane of selected suitable molecular weight cut-off carries out ultrafiltration to this water sample, obtains penetrating fluid and trapped fluid, and described macromole chromonic material is included in the trapped fluid, and inorganic salt and small organic molecule are included in the penetrating fluid;
(4) in trapped fluid, add deionization ultrapure water, repeating step (3);
(5) repeating step (3) and (4).So far inorganic salt and small organic molecule have all entered penetrating fluid, and chromonic material has entered trapped fluid.
The effect that the present invention uses the ultra-filtration membrane of suitable molecular weight cut-off can obtain to want, and the mode of the form of hyperfiltration membrane assembly and ultrafiltration does not have influence substantially; The macromole chromonic material is the solubleness height in water.Mineral ion in the described Vc fermentation waste water biochemical treatment water outlet is the inorganic salt that add in the Vc production process, and secondly Na ion concentration maximum in the positively charged ion is calcium ion, and other contains other small cations such as potassium, magnesium ion; Negatively charged ion is carbanion and phosphate anion.Organism (not comprising chromonic material) in the described Vc fermentation waste water biochemical treatment water outlet is the small molecular weight organism, solubleness height in water.
Ultracentrifugal rotating speed is 8000rpm-12000rpm, and centrifugation time is 10 ± 5min minute, and the aperture of millipore filtration is 0.22 μ m.Described ultra-filtration membrane places centrifugal ultrafiltration pipe, and ultrafiltration is finished by centrifugal, and centrifugal speed is 2000rpm-6000rpm, and the centrifugation time of each ultrafiltration is 10-20 minute.Described ultra-filtration membrane has with respect to the dextran meter, and scope is the molecular weight cut-off of 1000-10000, and mould material is a regenerated cellulose.
Adopt two-step fermentation to produce the waste water that produces in Vc (be international advanced and be unique production technique of the domestic Vc almost) process, wherein contain tawny chromonic material, multiple organism and mineral ion; Adopt present method can be simple and easy to do, efficiently apace the macromole chromonic material is separated with mineral ion and small organic molecule, be beneficial to adopt various analysis means that the macromole chromonic material is carried out feature and resolve.
Embodiment
Below among all embodiment all the water outlet of Vc fermentation waste water after anaerobism+aerobic biochemical is handled with pharmaceutical factory be objective for implementation.With water sample high speed centrifugation 10min under the 10000rpm rotating speed, use the filtering with microporous membrane of 0.22 μ m more earlier; With the molecular weight distribution of water sample after the centrifuging of gel filtration chromatography mensuration, molecular weight accounts for 98.95% less than 3000 small organic molecule, and the larger molecular organics of molecular weight in the 3000-9900 scope accounts for 1.05%.With ultra-filtration membrane water sample is separated, the macromolecule organism enters trapped fluid, and small molecular weight organism and mineral ion enter penetrating fluid.The penetrating fluid color is very light, and the more former water sample of trapped fluid color is denseer, therefore judges that chromonic material is a larger molecular organics.In following table 1, cited embodiment explanation is used to separate the ultra-filtration membrane of purification.In following table 2, enumerated and carried out the forward and backward analytical results of ultra-filtration membrane separation purification.
Embodiment 1
With water sample high speed centrifugation 15min under the 8000rpm rotating speed, use the filtering with microporous membrane of 0.22 μ m more earlier; Adopt the molecular weight distribution of this water sample of gel filtration chromatography then, analysis condition is as follows:
Adopt Waters 600 high performance liquid chromatographs (joining 2410 differential refraction detectors and Empower workstation), chromatographic column is Ultrahydrogel Linear 300mm * 7.8mmid * 2, and moving phase is the NaNO of 0.1M
3, flow rate of mobile phase is 0.9ml/min, and column temperature is 45 ℃, and the used standard substance of molecular weight calibration curve are MW2000000, MW133800, MW41100, MW21400, MW4600, MW180.
Get this water sample of 15mL and carry out ultrafiltration, wherein the molecular weight cut-off of ultra-filtration membrane is counted 3000Dalton by dextran, mould material is a regenerated cellulose, ultra-filtration membrane is placed centrifugal ultrafiltration pipe, centrifugal 10min finishes ultrafiltration under the 6000rpm rotating speed, obtain penetrating fluid and trapped fluid, described macromole chromonic material is included in the trapped fluid, inorganic salt and small organic molecule are included in the penetrating fluid;
Remove penetrating fluid, and add the deionization ultrapure water to 15mL in trapped fluid, the recentrifuge ultrafiltration repeats above-mentioned steps 6 times;
Measure the mineral ion concentration in trapped fluid and the penetrating fluid, the results are shown in following table 2.Collect trapped fluid, wherein contain the macromole chromonic material of having purified, use for follow-up various analyzing and testing.
Embodiment 2
With water sample high speed centrifugation 10min under the 10000rpm rotating speed, use the filtering with microporous membrane of 0.22 μ m more earlier; Adopt the molecular weight distribution of this water sample of gel filtration chromatography then, analysis condition is as follows:
Adopt Waters 600 high performance liquid chromatographs (joining 2410 differential refraction detectors and Empower workstation), chromatographic column is Ultrahydrogel Linear 300mm * 7.8mmid * 2, and moving phase is the NaNO of 0.1M
3, flow rate of mobile phase is 0.9ml/min, and column temperature is 45 ℃, and the used standard substance of molecular weight calibration curve are MW2000000, MW133800, MW41100, MW21400, MW4600, MW180.
Get this water sample of 15mL and carry out ultrafiltration, wherein the molecular weight cut-off of ultra-filtration membrane is counted 5000Dalton by dextran, mould material is a regenerated cellulose, ultra-filtration membrane is placed centrifugal ultrafiltration pipe, centrifugal 15min finishes ultrafiltration under the 4000rpm rotating speed, obtain penetrating fluid and trapped fluid, described macromole chromonic material is included in the trapped fluid, inorganic salt and small organic molecule are included in the penetrating fluid;
Remove penetrating fluid, and add the deionization ultrapure water to 15mL in trapped fluid, the recentrifuge ultrafiltration repeats above-mentioned steps 6 times;
Measure the mineral ion concentration in trapped fluid and the penetrating fluid, the results are shown in following table 2.Collect trapped fluid, wherein contain the macromole chromonic material of having purified, use for follow-up various analyzing and testing.
The results of elemental analyses of Vc chromonic material is as follows: C: H: O: N=5: 11: 2: 1.
Table 1 is used to separate the ultra-filtration membrane of purification
| Embodiment | Ultra-filtration membrane | Specification |
| 1 | Regenerated cellulose | 3000 molecular weight cut-offs are by dextran |
| 2 | Regenerated cellulose | 5000 molecular weight cut-offs are by dextran |
Table 2 analytical results (mg/L)
ND: expression does not detect.
Claims (4)
1. method of separating macromole chromonic material in the purification Vc fermentation waste water biochemical treatment water outlet, described Vc fermentation waste water is that two-step fermentation is produced the waste water that produces in the Vc process, described biochemical treatment is that anaerobism adds aerobic associating biochemical treatment, it is characterized in that described separation purification step is as follows:
(1) will adopt two-step fermentation to produce the waste water water outlet after anaerobism adds aerobic associating biochemical treatment that produces in the Vc process and carry out high speed centrifugation, and use filtering with microporous membrane, remove wherein suspended substance and solid particulate;
(2) adopt the molecular weight distribution of this water sample of gel filtration chromatography, with the parameter of the molecular weight cut-off of ultra-filtration membrane in the determining step (3);
(3) according to the result of step (2), the ultra-filtration membrane of selected suitable molecular weight cut-off carries out ultrafiltration to this water sample and obtains penetrating fluid and trapped fluid, and described macromole chromonic material is included in the trapped fluid, and inorganic salt and small organic molecule are included in the penetrating fluid;
(4) in trapped fluid, add deionization ultrapure water, repeating step (3);
(5) repeating step (3) and (4);
So far inorganic salt and small organic molecule have all entered penetrating fluid, and chromonic material has entered trapped fluid.
2. according to the method for macromole chromonic material in the described separation purification of the claim 1 Vc fermentation waste water biochemical treatment water outlet, it is characterized in that ultracentrifugal rotating speed is 8000rpm-12000rpm, centrifugation time is 10 ± 5min minute, and the aperture of millipore filtration is 0.22 μ m.
3. according to the method for macromole chromonic material in the described separation purification of the claim 1 Vc fermentation waste water biochemical treatment water outlet, it is characterized in that described ultra-filtration membrane places centrifugal ultrafiltration pipe, ultrafiltration is finished by centrifugal, centrifugal speed is 2000rpm-6000rpm, and the centrifugation time of each ultrafiltration is 10-20 minute; Described ultra-filtration membrane has with respect to the dextran meter, and scope is the molecular weight cut-off of 1000-10000, and mould material is a regenerated cellulose.
4. according to the method for macromole chromonic material in the described separation purification of the claim 1 Vc fermentation waste water biochemical treatment water outlet, it is characterized in that described method monitors by the ionic strength of measuring described penetrating fluid, when detecting, ionic strength do not stop.
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| CN2009100260436A CN101508496B (en) | 2009-03-12 | 2009-03-12 | Method for purification of macromolecule chromophoric matter in water from Vc fermentation wastewater by biochemical treatment |
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101298445A (en) * | 2008-06-17 | 2008-11-05 | 徐昌洪 | Method for directly preparing vitamin C with sodium gulonate |
| CN101353337A (en) * | 2008-09-08 | 2009-01-28 | 陈星� | Vitamin C clean production method |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101298445A (en) * | 2008-06-17 | 2008-11-05 | 徐昌洪 | Method for directly preparing vitamin C with sodium gulonate |
| CN101353337A (en) * | 2008-09-08 | 2009-01-28 | 陈星� | Vitamin C clean production method |
Non-Patent Citations (1)
| Title |
|---|
| 王强等.VC制药废水处理进展.《河北化工》.2007,第30卷(第9期),75-77. * |
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