CN102992541B - Method for simultaneously extracting iodine and fucoidin from salted kelp blanching wastewater - Google Patents
Method for simultaneously extracting iodine and fucoidin from salted kelp blanching wastewater Download PDFInfo
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- CN102992541B CN102992541B CN201210485012.9A CN201210485012A CN102992541B CN 102992541 B CN102992541 B CN 102992541B CN 201210485012 A CN201210485012 A CN 201210485012A CN 102992541 B CN102992541 B CN 102992541B
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- 206010033546 Pallor Diseases 0.000 title claims abstract description 78
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- 239000011630 iodine Substances 0.000 title claims abstract description 57
- 229910052740 iodine Inorganic materials 0.000 title claims abstract description 57
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- PNDPGZBMCMUPRI-UHFFFAOYSA-N iodine Chemical compound II PNDPGZBMCMUPRI-UHFFFAOYSA-N 0.000 claims abstract description 12
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- NWUYHJFMYQTDRP-UHFFFAOYSA-N 1,2-bis(ethenyl)benzene;1-ethenyl-2-ethylbenzene;styrene Chemical compound C=CC1=CC=CC=C1.CCC1=CC=CC=C1C=C.C=CC1=CC=CC=C1C=C NWUYHJFMYQTDRP-UHFFFAOYSA-N 0.000 claims abstract description 9
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- 244000005700 microbiome Species 0.000 claims description 6
- 230000015556 catabolic process Effects 0.000 claims description 5
- 238000006731 degradation reaction Methods 0.000 claims description 5
- 230000003647 oxidation Effects 0.000 claims description 5
- 238000007254 oxidation reaction Methods 0.000 claims description 5
- SUKJFIGYRHOWBL-UHFFFAOYSA-N sodium hypochlorite Chemical compound [Na+].Cl[O-] SUKJFIGYRHOWBL-UHFFFAOYSA-N 0.000 claims description 5
- 241000894006 Bacteria Species 0.000 claims description 4
- 230000000694 effects Effects 0.000 claims description 4
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- 238000005189 flocculation Methods 0.000 claims description 4
- 230000016615 flocculation Effects 0.000 claims description 4
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- 238000004313 potentiometry Methods 0.000 claims description 3
- 230000002269 spontaneous effect Effects 0.000 claims description 3
- 241000588986 Alcaligenes Species 0.000 claims description 2
- 241000589516 Pseudomonas Species 0.000 claims description 2
- 239000000126 substance Substances 0.000 abstract description 5
- 239000002699 waste material Substances 0.000 abstract description 2
- -1 iodide ions Chemical class 0.000 abstract 2
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 12
- 238000004519 manufacturing process Methods 0.000 description 9
- 239000011734 sodium Substances 0.000 description 6
- 238000007664 blowing Methods 0.000 description 5
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 3
- 241001466453 Laminaria Species 0.000 description 3
- 150000001720 carbohydrates Chemical class 0.000 description 3
- 229910052799 carbon Inorganic materials 0.000 description 3
- 238000000605 extraction Methods 0.000 description 3
- 238000001179 sorption measurement Methods 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
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- 230000002378 acidificating effect Effects 0.000 description 2
- 230000000274 adsorptive effect Effects 0.000 description 2
- XKMRRTOUMJRJIA-UHFFFAOYSA-N ammonia nh3 Chemical compound N.N XKMRRTOUMJRJIA-UHFFFAOYSA-N 0.000 description 2
- 239000012267 brine Substances 0.000 description 2
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- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
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- HPALAKNZSZLMCH-UHFFFAOYSA-M sodium;chloride;hydrate Chemical compound O.[Na+].[Cl-] HPALAKNZSZLMCH-UHFFFAOYSA-M 0.000 description 2
- MXNRLFUSFKVQSK-UHFFFAOYSA-N 2-Amino-6-(trimethylazaniumyl)hexanoate Chemical compound C[N+](C)(C)CCCCC(N)C([O-])=O MXNRLFUSFKVQSK-UHFFFAOYSA-N 0.000 description 1
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- FBPFZTCFMRRESA-KVTDHHQDSA-N D-Mannitol Chemical compound OC[C@@H](O)[C@@H](O)[C@H](O)[C@H](O)CO FBPFZTCFMRRESA-KVTDHHQDSA-N 0.000 description 1
- 229930195725 Mannitol Natural products 0.000 description 1
- 229910002651 NO3 Inorganic materials 0.000 description 1
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 description 1
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Landscapes
- Separation Of Suspended Particles By Flocculating Agents (AREA)
- Treatment Of Water By Ion Exchange (AREA)
Abstract
The invention provides a method for simultaneously extracting iodine and fucoidin from salted kelp blanching wastewater, belonging to the technical field of environment protection and chemical industry. The method particularly comprises the following steps of: (1) cooling kelp blanching wastewater; (2) degrading nitrate nitrogen and nitrite nitrogen by inherent microbes in kelp blanching wastewater; (3) adding caustic soda into denitrified kelp blanching wastewater, so that the fucoidin is basified, flocculated, and layered in a floating way, filtering, and drying to obtain a fucoidin crude product; (4) pumping the fucoidin-removed kelp blanching wastewater into an acidification tank, adding oxidant, so that iodide ions in solution can be completely oxidized into iodine, and enriching iodine by ion exchange resin; (5) dissolving iodine absorbed in the resin by NA2SO3 solution; and (6) oxidizing iodide ions in desorption solution into the iodine by KClO3 oxidant, crystallizing, separating out, centrifuging, and filtering to obtain crude iodine. According to the method, iodine and fucoidin can be extracted, and the multipurpose utilization rate can be improved, so that the resources waste and the environment pollution can be avoided.
Description
Technical field
The invention belongs to environmental protection and chemical technology field, relate to particularly a kind of method of simultaneously extracting iodine and fucoidin from salt marsh sea-tangle blanching waste water.
Background technology
The processing of salt marsh sea-tangle is the important processing mode in China's laminaria culture producing region, mainly concentrates on the areas such as Rongcheng, Shandong, Dalian, Liaanjiang county, Fujian.According to statistics, within 2010, China's laminaria culture output reaches 88.4 ten thousand tons (with dry weight basis), and the annual production of algae processed goods reaches 94.6 ten thousand tons, and its medium salting sea-tangle annual production is 420,000 tons, and annual value of production is over 1,200,000,000 yuan.By fresh sea-tangle in 80 ~ 90 ℃ of hot water after the of short duration blanching of high temperature, through cooling, draining, mix dehydration of salt and obtain salt marsh sea-tangle.The blanching sea-tangle processing line that spreads all over laminaria culture region produces more than 50 ten thousand tons of blanching waste waters season producing every year.Find after testing, in these waste water, contain the various active materials such as iodine, fucoidin, N.F,USP MANNITOL, laminine, fucoxanthin, wherein iodine content can reach 500 ~ 1000mg/L.In addition, in waste water, also contain the principal pollutant such as a large amount of suspended substance (SS), nitrate nitrogen, nitrite nitrogen, ammonia nitrogen.Not yet these waste water are recycled at present and directly discharge, on the one hand, caused paralic environment to be polluted; Anxious scarce iodine resource and the contour activeconstituents of fucoidin of China runs off in a large number on the other hand, causes the great wasting of resources.
Iodine is the grand strategy goods and materials that involve the interests of the state and the people.China lacks iodine ore resources, and from sea-tangle, carrying iodine is the fruitful way coming into effect from the sixties in last century, but use always is limnetic dry kelp.Since the eighties in last century, salt marsh sea-tangle secondary industry rises gradually, the annual fresh sea-tangle amount consuming accounts for the more than 30% of sea-tangle ultimate production, but the processing of salt marsh sea-tangle belongs to primary agricultural products processing category, processing mode is extensive, make a low multiple use, in sea-tangle blanching waste water, available affluent resources are out in the cold for a long time.
The extractive technique of iodine mainly contains Air blowing method, active carbon adsorption and ion exchange method etc. at present.Air blowing method is mainly applicable to the stock liquid that amount of iodine is relatively high, as extracted iodine the oil from recover petroleum and Sweet natural gas, natural gas well brine and salt lake interstratal brine, but use cost of equipment high, energy source and power consumption has limited greatly the application of Air blowing method, is not suitable for salt marsh sea-tangle processing enterprise and carries iodine from blanching water.Active carbon adsorption has that selectivity is good, adsorptivity is strong, separation efficiency advantages of higher, but because gac is expensive, disposable input cost is high, and large-scale commercial production is also restricted.Ion-exchange-resin process has the advantages such as energy consumption is low, the rate of recovery is high, facility investment is few, and because sea-tangle blanching manufacturer disperses, industrial scale is generally less, in blanching water, iodine content is low etc., is applicable to adopting ion-exchange-resin process to carry out enrichment extraction to iodine.The more important thing is, adopt ion-exchange-resin process when extracting iodine, can also extract fucoidin, and Air blowing method and active carbon adsorption are all difficult to reclaim fucoidin, therefore, ion-exchange-resin process is easier to apply in the relatively concentrated salt marsh sea-tangle main producing region that distributes.
The sea-tangle in vegetative period has stronger adsorptive power to the ammonia nitrogen in environment and nitrate nitrogen.Sea-tangle is after boiling is processed, and a large amount of nitrite nitrogens and nitrate nitrogen dissolve in blanching water.Find after measured, the content of blanching water Nitrite Nitrogen and nitrate nitrogen reaches 120 ~ 180mg/L.Under acidic conditions, it reacts with hydrogen ion and generates NO and NO
2gas gathers in a large number in the process of ion exchange resin absorption iodine, and the toxic gas of the brown color of emerging from exchange column upper end, has affected anionite-exchange resin to the adsorptive power of iodine and safety in production.
Fucoidin is a kind of natural polysaccharide resource that is widely used in the fields such as food and medicine, has the multiple physiologically actives such as anticoagulation, antitumor, antiviral and reducing blood-fat.In salt marsh sea-tangle blanching water, contain a large amount of fucoidins, increased difficulty to the separation and extraction technology of iodine.If adopt Air blowing method, carry iodine, first the pH of blanching water is adjusted to 0.5 ~ 3.0, under strong acidic condition, cannot extracts fucoidin, and directly discharge as waste, cause the serious wasting of resources, be therefore badly in need of the fucoidin in sea-tangle blanching waste water to recycle.
Summary of the invention
The technical problem to be solved in the present invention is to provide a kind of method of simultaneously extracting iodine and fucoidin from salt marsh sea-tangle blanching waste water.
The technical solution used in the present invention:
A method of simultaneously extracting iodine and fucoidin from salt marsh sea-tangle blanching waste water, specifically comprises the following steps: (1) cooling sea-tangle blanching waste water; (2) utilize in sea-tangle blanching waste water autochthonous microorganism by nitrate nitrogen and nitrite nitrogen degradation; (3) in denitrogenation sea-tangle blanching waste water, add caustic soda, regulate pH to 12, temperature is 20 ~ 30 ℃, makes fucoidin alkalization flocculation floating layering, adopts plate-and-frame filter press will float scum filtering, dry, obtains fucoidin crude product; (4) the sea-tangle blanching waste water of removing fucoidin is pumped into souring tank, regulate pH to 1.5 ~ 2, then add NaClO solution, stir, make Biodine be red-brown, the more supplementary NaNO that adds
2solution, makes the iodide ion in solution be completely oxidized to iodine, then spent ion exchange resin enrichment iodine; (5) use Na
2sO
3the iodine adsorbing in solution stripping resin; (6) use KClO
3oxygenant is oxidized to iodine by iodide ion in stripping liquid, crystallization, and centrifuging obtains thick iodine.
In described step (1), cooling sea-tangle blanching waste water is, in sea-tangle blanching waste water storage tank and alkali refining tank, cooling duct is installed, during by blanching sea-tangle, secondary cooling water used pumps in cooling duct, make temperature in storage tank be down to 40 ~ 50 ℃ at more than 90 ℃ sea-tangle blanching waste waters, after secondary cooling water heats up for the fresh sea-tangle of blanching next batch.
In described step (2), utilizing autochthonous microorganism in sea-tangle blanching waste water is to make sea-tangle blanching waste water spontaneous fermentation 12 ~ 18h under denitrifying bacterium effect by nitrate nitrogen and nitrite nitrogen degradation, action condition is pH7.0 ~ 8.0, temperature is 40 ~ 50 ℃, treat the degraded of high nitride completely, in sea-tangle blanching waste water constantly till bubbling.
It is to judge by potentiometry that the middle iodide ion of described step (4) is completely oxidized to iodine, and its oxidizing potential shows that between 550 ~ 650mV oxidation completely.
The concentration that adds NaClO in described step (4) is 30% (m/v), supplements and adds NaNO
2concentration be 5% (m/v).
Na in described step (5)
2sO
3the concentration of stripping liquid is 10% (m/v), and stripping liquid consumption is 8 ~ 10 times of the interior resin volume of post, and desorption time is 8h.
Oxygenant KClO in described step (6)
3add-on be amount of iodine and KClO in stripping liquid
3mass ratio be 2.5 ~ 3.5: 1.
The present invention's beneficial effect compared with prior art:
The present invention adopts heat exchange method that the secondary cooling water using in sea-tangle blanching process is passed in the cooling duct of wastewater storage tank innovatively, to reach the object of cooling blanching water, the fresh sea-tangle of water coolant blanching after simultaneously heating, both guarantee the recycle of blanching hydro-thermal energy, and avoided again the iodine in secondary cooling water to run off in a large number.
It is raw material that salt marsh sea-tangle blanching waste water is take in the present invention, and intrinsic microorganism natural degradation in blanching waste water, removes the nitride of blanching water middle and high concentration, and do not take to utilize the method for chemical reducing agent degraded, thereby reduce production costs, and reduces chemical substance discharge.
When the present invention adopts ion-exchange-resin process to extract iodine, the flocculence of taking to alkalize makes carbohydrate gum form flocks, then by methods such as floating and filter presss, obtain fucoidin crude product, improved and in traditional method, utilized dry sea-tangle only to extract the production technique of iodine.
Embodiment
Below in conjunction with embodiment, describe technical scheme of the present invention in detail:
The method of simultaneously extracting iodine and fucoidin from salt marsh sea-tangle blanching waste water, specifically comprises the following steps:
1) cooling sea-tangle blanching waste water.At fresh sea-tangle results busy season (annual May first arrival mid-July), every day, every production line can the fresh sea-tangle of blanching 160 tons, produced 20 tons of sea-tangle blanching waste waters, and in sea-tangle blanching waste water, iodine average content is about 700mg/L.First in sea-tangle blanching waste water storage tank and alkali refining tank, cooling duct is installed, secondary cooling water is pumped in cooling duct, make temperature in storage tank be down to 45 ℃ at more than 90 ℃ sea-tangle blanching waste waters, the secondary cooling water after intensification is for the fresh sea-tangle of blanching next batch.
2) utilize autochthonous microorganism in sea-tangle blanching waste water that high oxynitride is degraded step by step, nitrate nitrogen and nitrite nitrogen are reduced to nitrogen.
Sea-tangle blanching waste water spontaneous fermentation 12h under the denitrifying bacterium effects such as pseudomonas and Alcaligenes, action condition is pH8.0, and temperature is 45 ℃, treats nitride degraded completely, in sea-tangle blanching waste water, till continuous bubbling, the decreasing ratio of nitrate and nitrite is respectively 82% and 75%.
3) in sea-tangle blanching waste water, add caustic soda, and pass into air, by fucoidin alkalization flocculation, floating layering, adopts plate-and-frame filter press that carbohydrate gum slag is filtered, dry, obtains fucoidin crude product.
It is 10m that denitrogenation sea-tangle blanching waste water is pumped into volume
3alkali refining tank in, adding concentration is 40% caustic soda soln, regulates pH to 12, seawater is pumped in the cooling duct of alkali refining tank, makes sea-tangle blanching waste water temperature be down to rapidly 25 ℃., to input air in alkali refining tank, stir after 30min, standing 8h, makes fucoidin flocculation floating meanwhile, and wherein carbohydrate gum layer volume accounts for the more than 20% of sea-tangle blanching waste water cumulative volume.Xian Jiang lower floor pumps in souring tank containing iodine clear liquid, then the fucoidin condensation product at the bottom of upper strata floating matter and tank is discharged from alkali refining tank, by plate-and-frame filter press, filters, and obtains fucoidin.What filtration is obtained reclaims containing iodine clear liquid simultaneously, can obviously improve the extraction yield of iodine.
4) the sea-tangle blanching waste water of removing fucoidin is pumped in souring tank, add technical hydrochloric acid, regulate pH to 1.5, then adding concentration is the NaClO solution of 30% (m/v), stir, make liquid be red-brown, then supplement that to add concentration be the NaNO of 5% (m/v)
2solution, makes the iodide ion in solution be completely oxidized to iodine, adopts potentiometry to judge whether complete oxidation of iodide ion, its oxidizing potential between 550 ~ 650mV for oxidation completely.The sea-tangle blanching waste water that contains iodine is pumped into strongly basic anion exchange resin, and flow velocity is set in 16mL/min, and frequently collects the liquid flowing out from exchange resin, surveys its amount of iodine, generally lower than 30mg/L, is advisable.
5) use Na
2sO
3the iodine adsorbing in solution stripping resin.Concrete operations are as follows: first add the water that is equivalent to shaft height 2/3, be filled with pneumatic blending, make wherein impurity float and wash out, pass into the Na that concentration is 10% (m/v) when the water surface is down to apart from resin face 5cm place from top
2sO
3solution, more slowly put into oxidation trough from bottom Jiang Shui.When sodium sulfite solution is added to apart from resin face 5cm place, close bottom valve, after immersion 30min, slowly emit, continue to supplement Na
2sO
3solution, until the Na flowing out
2sO
3stripping liquid from red-brown become faint yellow till.Stripping liquid consumption is 10 times of the interior resin of post, and desorption time is 8h.
6) use KClO
3oxygenant is by iodine crystallization from stripping liquid, and centrifuging obtains thick iodine.First add the vitriol oil, regulating the pH value of stripping liquid is 1.2, according to the content of iodine in stripping liquid, adds oxygenant KClO
3iodine is separated out, iodine and KClO
3mass ratio be 2.5: 1, centrifuging obtains thick iodine.
Claims (8)
1. from salt marsh sea-tangle blanching waste water, extract a method for iodine and fucoidin simultaneously, it is characterized in that specifically comprising the following steps: (1) cooling sea-tangle blanching waste water; (2) utilize in sea-tangle blanching waste water autochthonous microorganism by nitrate nitrogen and nitrite nitrogen degradation; (3) in denitrogenation sea-tangle blanching waste water, add caustic soda, regulate pH to 12, temperature is 20～30 ℃, makes fucoidin alkalization flocculation floating layering, adopts plate-and-frame filter press will float scum filtering, dry, obtains fucoidin crude product; (4) the sea-tangle blanching waste water of removing fucoidin is pumped into souring tank, regulate pH to 1.5～2, then add NaClO solution, stir, make Biodine be red-brown, the more supplementary NaNO that adds
2solution, makes the iodide ion in solution be completely oxidized to iodine, then spent ion exchange resin enrichment iodine; (5) use Na
2sO
3the iodine adsorbing in solution stripping resin; (6) use KClO
3oxygenant is oxidized to iodine by iodide ion in stripping liquid, crystallization, and centrifuging obtains thick iodine.
2. a kind of method of simultaneously extracting iodine and fucoidin from salt marsh sea-tangle blanching waste water according to claim 1, it is characterized in that in described step (1), cooling sea-tangle blanching waste water is, in sea-tangle blanching waste water storage tank and alkali refining tank, cooling duct is installed, during by blanching sea-tangle, secondary cooling water used pumps in cooling duct, make temperature in storage tank be down to rapidly 40～50 ℃ at more than 90 ℃ sea-tangle blanching waste waters, after secondary cooling water heats up for the fresh sea-tangle of blanching next batch.
3. a kind of method of simultaneously extracting iodine and fucoidin from salt marsh sea-tangle blanching waste water according to claim 1, it is characterized in that in described step (2), utilizing autochthonous microorganism in sea-tangle blanching waste water is to make sea-tangle blanching waste water spontaneous fermentation 12～18h under denitrifying bacterium effect by nitrate nitrogen and nitrite nitrogen degradation, action condition is pH7.0～8.0, temperature is 40～50 ℃, treat the nitride degraded of high density completely, in sea-tangle blanching waste water constantly till bubbling.
4. a kind of method of simultaneously extracting iodine and fucoidin from salt marsh sea-tangle blanching waste water according to claim 1, it is characterized in that it is to judge by potentiometry that the middle iodide ion of described step (4) is completely oxidized to iodine, its oxidizing potential shows that between 550～650mV oxidation completely.
5. a kind of method of simultaneously extracting iodine and fucoidin from salt marsh sea-tangle blanching waste water according to claim 1, is characterized in that in described step (4), adding the concentration of NaClO solution is 30%m/v, supplements and adds NaNO
2the concentration of solution is 5%m/v.
6. a kind of method of simultaneously extracting iodine and fucoidin from salt marsh sea-tangle blanching waste water according to claim 1, is characterized in that Na in described step (5)
2sO
3the concentration of stripping liquid is 10%m/v, and stripping liquid consumption is 8～10 times of the interior resin volume of post, and desorption time is 8h.
7. a kind of method of simultaneously extracting iodine and fucoidin from salt marsh sea-tangle blanching waste water according to claim 1, is characterized in that oxygenant KClO in described step (6)
3add-on be amount of iodine and KClO in stripping liquid
3mass ratio be 2.5～3.5: 1.
8. a kind of method of simultaneously extracting iodine and fucoidin from salt marsh sea-tangle blanching waste water according to claim 3, is characterized in that described denitrifying bacterium is pseudomonas and Alcaligenes.
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| CN105523664A (en) * | 2015-12-24 | 2016-04-27 | 山东省环保产业股份有限公司 | Algin production wastewater pretreatment method |
| CN106676010B (en) * | 2017-01-19 | 2021-02-19 | 宁波大学 | Method for increasing fucoxanthin content in phaeodactylum tricornutum by using sodium tungstate |
| CN107382666A (en) * | 2017-07-26 | 2017-11-24 | 中国水产科学研究院黄海水产研究所 | The efficient energy-saving extracting method of dissolved organic matter in one main laminaria blanching water |
| CN107382667A (en) * | 2017-07-26 | 2017-11-24 | 中国水产科学研究院黄海水产研究所 | The cycles, economized processing method of dissolved organic matter in one main laminaria blanching water |
| CN107266606B (en) * | 2017-08-23 | 2020-03-27 | 山东大学 | New process for extracting fucosan sulfate from kelp processing waste liquid |
| CN109368594B (en) * | 2018-11-22 | 2020-11-03 | 山东罗欣药业集团股份有限公司 | Method for recovering iodine from cephalosporin medicament waste liquid |
| CN110845032A (en) * | 2019-11-01 | 2020-02-28 | 自然资源部第三海洋研究所 | Method for recycling kelp blanching liquid |
| CN111099770A (en) * | 2020-01-07 | 2020-05-05 | 昆山之奇美材料科技有限公司 | System and method for extracting iodine from waste solution of polaroid manufacturing process |
| CN114807242B (en) * | 2022-05-10 | 2024-04-23 | 中盐工程技术研究院有限公司 | Method for extracting iodine from seaweed |
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