CN1840469A - Process for extracting iodine from kelp - Google Patents
Process for extracting iodine from kelp Download PDFInfo
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- CN1840469A CN1840469A CN 200510044408 CN200510044408A CN1840469A CN 1840469 A CN1840469 A CN 1840469A CN 200510044408 CN200510044408 CN 200510044408 CN 200510044408 A CN200510044408 A CN 200510044408A CN 1840469 A CN1840469 A CN 1840469A
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Abstract
The disclosed method to extract I2 from kelp comprises: with fresh kelp as material, cutting up, adding 200wt% water to dip for 30-50min; putting soak into pond, adjusting pH value with alkali, while filling gas to stir and then filter to obtain the clear liquid with I2 and mannitol; acidifying and oxidizing to obtain dissociative I2 and then adsorb with basic anion exchange resin; desorbing the I2 on resin with Na2S2O3; adding strong H2SO4 and KClO3 to separate out coarse I2; cleaning, and refining with 25wt% strong H2SO4 at 140Deg to obtain the refined iodine. This invention reduces cost and source.
Description
Technical field
The present invention relates to the seaweed chemical technology, especially a kind of method of from sea-tangle, extracting iodine.
Background technology
Iodine belongs to a kind of element in the halogen family, and very big to the mankind and animals and plants existence influence, it is mainly used in medical aspect, this external agricultural, chemical industry, the also widespread use of national defence sophisticated technology aspect.Traditional method of from sea-tangle, extracting iodine, the raw material that is adopted is the dried sea-tangle through the system of shining, and through following technology: in dried sea-tangle, add 4-16 tap water doubly, soaked 24 hours, must contain iodine, the sea-tangle water soak solution of N.F,USP MANNITOL, adding caustic soda adjusting pH value in sea-tangle water soak solution is about 12, retrogradation 8 hours, obtaining purifies waste water adds hydrochloric acid again to regulate pH value is 2, adds clorox again and evenly stirs and make it to be red-brown, restock adds 5% Sodium Nitrite during near oxidation, make it complete oxidation, make iodine free, iodine is adsorbed by anionite-exchange resin, feed the reductive agent desorb again, iodine is analysed, and promptly gets medical iodine after making with extra care." a kind of method of extracting active iodine from sea-tangle " for example also disclosed in the CN1102067C Chinese invention patent specification sheets that on February 26th, 2003 was announced, it is through 120 ℃ of high temperature high pressure process 30-60 minutes with drying sea-tangle, the 55-60 ℃ of immersion of water control temperature of getting 10 times of weight of dried sea-tangle obtained soak solution in 10-24 hour, after soak solution is filtered, filter step by step with hyperfiltration membrane assembly again, keeping molecular weight cut-off is the liquid of 1000-400, adjust its pH value, successively with sun, the anionite-exchange resin exchange, to exchange liquid concentrates, absorption, behind the wash-out, enriched material is promptly got the sea-tangle active iodine 180-240 ℃ of following spraying drying.But, no matter be in the traditional method of from sea-tangle, extracting iodine or the above-mentioned patent specification disclosed " a kind of method of from sea-tangle, extracting active iodine ", its raw material all adopts drying sea-tangle, and to adopt a large amount of water to soak the sea-tangle raw material for a long time and obtain soak solution, thereby exist the consume of water big, the deficiency that the time is long; In addition, labor force and the threshing ground of the dried sea-tangle of solarization system lacks factors such as (the sea-tangle system of shining need take a large amount of soils), also can make from the production cost of sea-tangle extraction iodine and rise significantly.
Summary of the invention
Obtain the used long-time and a large amount of fresh water of need of sea-tangle water soak solution in the prior art in order to solve, shine the deficiency that factors such as system required labor force of dried sea-tangle and threshing ground cause production cost to improve, and a kind of method of extracting iodine from sea-tangle is provided, this method is extracted the used sea-tangle raw material of iodine need not shine system, reduce production cost, and need not adopt a large amount of water to soak raw material for a long time.
The technical scheme that technical solution problem of the present invention is adopted is: a kind of method of from sea-tangle, extracting iodine, and it is characterized in that: the bright sea-tangle of selecting new harvesting for use is a raw material, weighing is accurately after following treatment process:
(A), soak: with the bright accurately sea-tangle chopping of above-mentioned weighing, be transported to fermentation vat and soaked 30～50 minutes, amount of water is 2 times of bright sea-tangle weight;
(B), purify: above-mentioned kelp-soaking liquid is placed in the floating pond, adding alkali adjustment soak solution pH value is between 12～13, sends into air with recycle pump simultaneously, carries out air agitation 20～30 minutes, after static floating 4～6 hours, filter the clear liquid that proposes to contain iodine and N.F,USP MANNITOL;
(C), acidifying oxidation: add hydrochloric acid in the above-mentioned clear liquid that contains iodine and N.F,USP MANNITOL, adjusting pH value is between 1.5～2, adds chlorine oxidation again, and oxidizing potential remains between 550～650 millivolts, with the I in the soak solution
-Be oxidized to I
2
(D), iodine absorption: the soak solution that contains free-iodine after the above-mentioned oxidation is passed through basic anion exchange resin, and free-iodine is by resin absorption;
(E), desorb: be adsorbed in iodine on the resin with 10% S-WAT desorb with above-mentioned, amount of iodine is 16～20% in the control stripping liquid;
(F), iodine analyses: add the vitriol oil again and reach 2mol/L to stripping liquid acidity in stripping liquid, add Potcrate again, the Potcrate add-on is 0.16 times of amount of iodine in the stripping liquid, can separate out thick iodine crystallization;
(G), refining: thick iodine crystallization that will be above-mentioned is washed, and it is refining to use the vitriol oil of thick iodine weight 1/4th to melt altogether at 140 ℃ again, promptly gets smart iodine;
The present invention be directly with bright sea-tangle as extracting the iodine raw materials for production, need not adopt a large amount of fresh water to soak raw material for a long time, and save the solarization system process of sea-tangle, reduced production cost, technological process of the present invention is simple and feasible, the saving energy and production time.
Embodiment
The present invention is further described below in conjunction with embodiment.
Embodiment 1:
Selecting the fresh sea-tangle of marine harvesting for use is raw material, after 100 kilograms of the weighings, through following treatment process:
(A), soak: 100 kilograms bright sea-tangle chopping with above-mentioned weighing adds water with pump delivery to fermentation vat and soaked 30 minutes for 200 kilograms; Immersion process adopts cover bubble method twice, soaks with carrying out the first time with two times water jackets that soak for the second time, improves the iodine, the mannitol content that soak water;
(B), purify: above-mentioned kelp-soaking liquid is placed in the floating pond, and the pH value that adds liquid caustic soda adjustment soak solution is 12, makes organic colloid impurity cohesions such as carbohydrate gum, pump into air with recycle pump simultaneously, mixed gas 20 minutes, and, can emit clear liquid at static floating 4 o'clock from the bottom in floating pond;
(C), acidifying oxidation: add technical hydrochloric acid in the above-mentioned clear liquid of obtaining that contains iodine, N.F,USP MANNITOL, adjusting pH value is 1.6, adds chlorine oxidation again, regulates the chlorine valve and makes oxidizing potential remain on 550 millivolts, and the I in the soak solution is oxidized to I
2, free iodine produces;
(D), iodine absorption: the soak solution that will contain free-iodine through peroxidation is by 717 type strongly basic anion exchange resins, and free-iodine is promptly adsorbed by exchange resin;
(E), desorb: will be adsorbed in iodine on the exchange resin with 10% S-WAT desorb, amount of iodine is 17% in the control stripping liquid;
(F), iodine analyses: add the vitriol oil again and reach 2mol/L to stripping liquid acidity in stripping liquid, add Potcrate again, the Potcrate add-on is 0.16 times of amount of iodine in the stripping liquid, separates out thick iodine crystallization;
(G): refining: with thick iodine crystallization for several times, use centrifuge dewatering, the thicker iodine and the vitriol oil that is equivalent to its weight 1/4th are added in the enamel reaction still with distilled water wash, with 140 ℃ of temperature heating, make iodine be in molten state, leave standstill crystallisation by cooling after stirring, promptly get smart iodine.
Embodiment 2:
Selecting the fresh sea-tangle of marine harvesting for use is raw material, after 500 kilograms of the weighings, through following treatment process:
(A), soak: 500 kilograms bright sea-tangle chopping with above-mentioned weighing adds water with pump delivery to fermentation vat and soaked 50 minutes for 1000 kilograms; Immersion process adopts cover bubble method twice, soaks with carrying out the first time with two times water jackets that soak for the second time, improves the iodine, the mannitol content that soak water;
(B), purify: above-mentioned kelp-soaking liquid is placed in the floating pond, and the pH value that adds liquid caustic soda adjustment soak solution is 12, makes organic colloid impurity cohesions such as carbohydrate gum; Pump into air with recycle pump simultaneously, mixed gas 30 minutes, static floating 6 hours, can emit clear liquid from bottom, floating pond;
(C), acidifying oxidation: add technical hydrochloric acid in the above-mentioned clear liquid of obtaining that contains iodine, N.F,USP MANNITOL, adjusting pH value is 2, adds chlorine oxidation again, regulates the chlorine valve and makes oxidizing potential remain on 650 millivolts, with the I in the soak solution
-Be oxidized to I
2, free iodine produces;
(D), iodine absorption: the soak solution that will contain free-iodine through peroxidation is by 717 type strongly basic anion exchange resins, and free-iodine is promptly adsorbed by exchange resin;
(E), desorb: will be adsorbed in iodine on the exchange resin with 10% S-WAT desorb, amount of iodine is 20% in the control stripping liquid;
(F), iodine analyses: add the vitriol oil again and reach 2mol/L to stripping liquid acidity in stripping liquid, add Potcrate again, the Potcrate add-on is 0.16 times of amount of iodine in the stripping liquid, separates out thick iodine crystallization;
(G): refining: with thick iodine crystallization for several times, use centrifuge dewatering, the thicker iodine and the vitriol oil that is equivalent to its weight 1/4th are added in the enamel reaction still with distilled water wash, with 140 ℃ of steam heating, make iodine be in molten state, leave standstill crystallisation by cooling after stirring, promptly get smart iodine.
Claims (1)
1, a kind of method of from sea-tangle, extracting iodine, it is characterized in that: the bright sea-tangle of selecting new harvesting for use is a raw material, weighing is accurately after following treatment process:
(A), soak: with the bright accurately sea-tangle chopping of above-mentioned weighing, be transported to fermentation vat and soaked 30～50 minutes, amount of water is 2 times of bright sea-tangle weight;
(B), purify: above-mentioned kelp-soaking liquid is placed in the floating pond, adding alkali adjustment soak solution pH value is between 12～13, sends into air with recycle pump simultaneously, carries out air agitation 20～30 minutes, after static floating 4～6 hours, filter the clear liquid that proposes to contain iodine and N.F,USP MANNITOL;
(C), acidifying oxidation: add hydrochloric acid in the above-mentioned clear liquid that contains iodine and N.F,USP MANNITOL, adjusting pH value is between 1.5～2, adds chlorine oxidation again, and oxidizing potential remains between 550～650 millivolts, with the I in the soak solution
-Be oxidized to I
2
(D), iodine absorption: the soak solution that contains free-iodine after the above-mentioned oxidation is passed through basic anion exchange resin, and free-iodine is by resin absorption;
(E), desorb: be adsorbed in iodine on the resin with 10% S-WAT desorb with above-mentioned, amount of iodine is 16～20% in the control stripping liquid;
(F), iodine analyses: add the vitriol oil again and reach 2mol/L to stripping liquid acidity in stripping liquid, add Potcrate again, the Potcrate add-on is 0.16 times of amount of iodine in the stripping liquid, can separate out thick iodine crystallization;
(G), refining: thick iodine crystallization that will be above-mentioned is washed, and it is refining to use the vitriol oil of thick iodine weight 1/4th to melt altogether at 140 ℃ again, promptly gets smart iodine.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB200510044408XA CN100425526C (en) | 2005-08-18 | 2005-08-18 | Process for extracting iodine from kelp |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB200510044408XA CN100425526C (en) | 2005-08-18 | 2005-08-18 | Process for extracting iodine from kelp |
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|---|---|
| CN1840469A true CN1840469A (en) | 2006-10-04 |
| CN100425526C CN100425526C (en) | 2008-10-15 |
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|---|---|---|---|
| CNB200510044408XA Expired - Fee Related CN100425526C (en) | 2005-08-18 | 2005-08-18 | Process for extracting iodine from kelp |
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Cited By (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101107985B (en) * | 2007-08-21 | 2010-09-29 | 浙江大学 | Method of salting and processing preserved szechuan pickle containing natural iodine |
| CN101774545B (en) * | 2008-12-30 | 2012-03-07 | 刘树军 | Algae iodate and method for extracting algae iodate from algae |
| CN102390811A (en) * | 2011-08-23 | 2012-03-28 | 山东成武天元海藻工业有限公司 | Extraction method of iodine |
| CN102515106A (en) * | 2011-12-28 | 2012-06-27 | 中国水产科学研究院黄海水产研究所 | Method for extracting iodine from blanching waste water of fresh kelp |
| CN101643430B (en) * | 2009-08-14 | 2012-07-18 | 迟逸仙 | Method for extracting seaweed organic iodine from seaweed or seaweed root |
| WO2012146863A1 (en) | 2011-04-27 | 2012-11-01 | Algues Et Mer | Edible brown algae extract with a low iodine content |
| CN103072947A (en) * | 2012-12-20 | 2013-05-01 | 青岛明月海藻集团有限公司 | Method for extracting iodine from kelp |
| CN103193897A (en) * | 2013-04-22 | 2013-07-10 | 青岛贝尔特生物科技有限公司 | Method for coproduction of sodium alginate, mannitol and iodine by enzymolysis approach |
| CN104387232A (en) * | 2014-11-11 | 2015-03-04 | 常州大学 | Method for extracting mannose from sea vegetable |
| CN107916258A (en) * | 2016-10-11 | 2018-04-17 | 北京工商大学 | For extracting the enzyme preparation of seaweed iodine solution and the method for extraction seaweed iodine solution |
| CN109336054A (en) * | 2018-12-20 | 2019-02-15 | 四川久大蓬莱盐化有限公司 | A method of recycling iodine from salt-making mother liquor |
| CN111961639A (en) * | 2020-08-25 | 2020-11-20 | 山东东方海洋科技股份有限公司 | Method for quickly sterilizing kelp gametophyte in conventional culture process |
| CN113880692A (en) * | 2021-11-18 | 2022-01-04 | 湖南蓝之碘生物科技有限公司 | Method for extracting iodine and mannitol from kelp |
| CN115368910A (en) * | 2022-08-31 | 2022-11-22 | 王乐 | Preparation method of soil conditioner |
Family Cites Families (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB450210A (en) * | 1934-01-11 | 1936-07-13 | Victor Charles Emile Le Gloahe | Improvements in or relating to the recovery of iodine from seaweed |
| SU507519A1 (en) * | 1974-05-31 | 1976-03-25 | Лаборатория Института Общей И Неорганической Химии Ан Украинской Сср | The method of obtaining iodine |
| CN1102067C (en) * | 2000-09-26 | 2003-02-26 | 烟台长岛经济开发有限公司 | Process for extracting active iodine from kelp |
-
2005
- 2005-08-18 CN CNB200510044408XA patent/CN100425526C/en not_active Expired - Fee Related
Cited By (18)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101107985B (en) * | 2007-08-21 | 2010-09-29 | 浙江大学 | Method of salting and processing preserved szechuan pickle containing natural iodine |
| CN101774545B (en) * | 2008-12-30 | 2012-03-07 | 刘树军 | Algae iodate and method for extracting algae iodate from algae |
| CN101643430B (en) * | 2009-08-14 | 2012-07-18 | 迟逸仙 | Method for extracting seaweed organic iodine from seaweed or seaweed root |
| US20140199410A1 (en) * | 2011-04-27 | 2014-07-17 | Algues Et Mer | Edible brown algae extract with a low iodine content |
| WO2012146863A1 (en) | 2011-04-27 | 2012-11-01 | Algues Et Mer | Edible brown algae extract with a low iodine content |
| CN102390811A (en) * | 2011-08-23 | 2012-03-28 | 山东成武天元海藻工业有限公司 | Extraction method of iodine |
| CN102390811B (en) * | 2011-08-23 | 2012-10-17 | 山东成武天元海藻工业有限公司 | Extraction method of iodine |
| CN102515106A (en) * | 2011-12-28 | 2012-06-27 | 中国水产科学研究院黄海水产研究所 | Method for extracting iodine from blanching waste water of fresh kelp |
| CN103072947A (en) * | 2012-12-20 | 2013-05-01 | 青岛明月海藻集团有限公司 | Method for extracting iodine from kelp |
| CN103193897A (en) * | 2013-04-22 | 2013-07-10 | 青岛贝尔特生物科技有限公司 | Method for coproduction of sodium alginate, mannitol and iodine by enzymolysis approach |
| CN103193897B (en) * | 2013-04-22 | 2015-04-22 | 青岛贝尔特生物科技有限公司 | Method for coproduction of sodium alginate, mannitol and iodine by enzymolysis approach |
| CN104387232A (en) * | 2014-11-11 | 2015-03-04 | 常州大学 | Method for extracting mannose from sea vegetable |
| CN107916258A (en) * | 2016-10-11 | 2018-04-17 | 北京工商大学 | For extracting the enzyme preparation of seaweed iodine solution and the method for extraction seaweed iodine solution |
| CN109336054A (en) * | 2018-12-20 | 2019-02-15 | 四川久大蓬莱盐化有限公司 | A method of recycling iodine from salt-making mother liquor |
| CN111961639A (en) * | 2020-08-25 | 2020-11-20 | 山东东方海洋科技股份有限公司 | Method for quickly sterilizing kelp gametophyte in conventional culture process |
| CN111961639B (en) * | 2020-08-25 | 2022-06-24 | 山东东方海洋科技股份有限公司 | Rapid sterilization method in routine culture process of kelp gametophyte clone |
| CN113880692A (en) * | 2021-11-18 | 2022-01-04 | 湖南蓝之碘生物科技有限公司 | Method for extracting iodine and mannitol from kelp |
| CN115368910A (en) * | 2022-08-31 | 2022-11-22 | 王乐 | Preparation method of soil conditioner |
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|---|---|
| CN100425526C (en) | 2008-10-15 |
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Owner name: WEIHAI CHANGQING MARINE SCIENCE AND TECHNOLOGY CO. Free format text: FORMER OWNER: SHANDONG XUNSHAN AQUATIC PRODUCT GROUP CO., LTD. Effective date: 20120815 |
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Effective date of registration: 20120815 Address after: 264316 No. 590, Xun Shan Road, Rongcheng Economic Development Zone, Shandong Patentee after: Weihai Changqing Marine Science and Technology Co., Ltd. Address before: 264316 Shandong city of Rongcheng Province town cliffs herring Beach Village Patentee before: Shandong Xunshan Aquatic Product Group Co., Ltd. Patentee before: Wang Qingyin |
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