CN103130185B - Novel environment-friendly technology for extracting iodine from kelp water - Google Patents
Novel environment-friendly technology for extracting iodine from kelp water Download PDFInfo
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- CN103130185B CN103130185B CN201310090916.6A CN201310090916A CN103130185B CN 103130185 B CN103130185 B CN 103130185B CN 201310090916 A CN201310090916 A CN 201310090916A CN 103130185 B CN103130185 B CN 103130185B
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Abstract
The invention discloses a novel environment-friendly technology for extracting iodine from kelp water. The novel environment-friendly technology comprises the following steps of: (1) quantifying feed liquid, and adjusting pH value; (2) quantitatively adding an oxidizing agent to a part of feed liquid according to the content of iodine in the feed liquid; (3) continuously adding hydrogen peroxide to the feed liquid; (4) additionally taking 5-6 times of the feed liquid, adjusting pH value, and fully mixing and reacting with the oxidized feed liquid; (5) blowing out iodine in the mixed feed liquid by using an air blowout method; (6) adjusting the pH value of waste water to be neutral after iodine extraction; (7) absorbing blown-out iodine in air by a solution; and (8) analyzing iodine in an absorption liquid. The novel environment-friendly technology solves the problem of hydrogen peroxide decomposition by adopting a two-step oxidization method, greatly improves the utilization efficiency of hydrogen peroxide and is a novel feasible environment-friendly technology for extracting iodine from kelp water.
Description
Technical field
The present invention relates to a kind of environmental-protecting process of carrying iodine from sea-tangle water, belong to environmental protection, chemical technology field.
Background technology
Sea-tangle processing is one of China's aquaculture industry column support type industry, and sea-tangle annual production is 800,000 tons of left and right, and one of iodine resource that Dian Shi China in sea-tangle is important is also a kind of strategic material of preciousness simultaneously, is applied to many industries.The carry iodine resource of China taking sea-tangle as raw material is mainly sea-tangle water at present, and it is divided into again two parts: the one, and seaweed chemical kelp soaking water, amount of iodine is about 150-300ppm, and the 2nd, fresh sea-tangle blanching waste water, amount of iodine is about 300-600ppm.Current iodine extraction process mainly comprises: feed liquid purification, acidifying, oxidation, ion-exchange or Air blowing extraction, absorption liquid parsing, centrifugal purification, obtain thick iodine product.But traditional oxygenant generally has the defect in use, can cause environmental pollution simultaneously, urgently further improve.
The oxygenant adopting in traditional iodine extraction process mainly contains Sodium Nitrite, chlorine, hydrogen peroxide or clorox and Sodium Nitrite mixes use.In use not only can produce NO toxic gas using Sodium Nitrite as oxygenant, affect field personnel's health, exhaust emission ambient atmosphere, and because needs excessive oxidant ensures that oxidation completely, therefore inevitably produce oxygenant residual, cause and carry discharge of wastewater after iodine and pollute; Using clorox as oxygenant due to its be alkalescence, in use consume more hydrochloric acid, and cause the fluctuation of pH value, use inconvenience and be easy to use the excessive peroxidation sound productive rate that causes, therefore general employing first by hypochlorite oxidation again with the supplementary method of Sodium Nitrite in use, the latter has caused again the excessive problem of aforesaid Sodium Nitrite; Chlorine oxidation process is the method that early stage technique of extracting iodine adopts, but because chlorine use procedure toxic is larger, no longer adopts; Hydrogen peroxide is a kind of eco-friendly oxygenant, in theory also can be by the I in solution
-be oxidized to I
2simple substance, but in actual applications because hydrogen peroxide is at I
-and I
2unstable and accelerate decomposition in situation about existing, thus cause at I
-in the higher solution of concentration, cannot make I complete oxidation is elemental iodine, has limited its application in marine alga water extraction iodine is produced.
Hydrogen peroxide oxidation method Guizhou University of China and Wengfu Group Co.,Ltd cooperate to carry out phosphorus ore carry iodine produce in be applied, and application or the multinomial patent of obtaining the authorization, as: " in the dilute phosphoric acid containing producing iodine phosphate ore production, extracting the method for iodine " (application number 2005100030582), " a kind of method that reclaims iodine from the dilute phosphoric acid of Wet-process Phosphoric Acid Production " (application number 200810302681) etc., but oxidizing reaction need be at Vanadium Pentoxide in FLAKES (V
2o
5) carry out under catalysis, Vanadium Pentoxide in FLAKES also can cause certain environmental protection hidden danger as a kind of toxic substance.
Summary of the invention
The technical problem to be solved in the present invention is to provide a kind of environmental-protecting process of carrying iodine from sea-tangle water, this technique has solved hydrogen peroxide labile problem in iodine solution, and do not need to introduce new catalyzer, solve the pollution problem that technique of extracting iodine causes due to oxygenant, and technological operation is convenient, production cost is low, practical.
For solving the problems of the technologies described above, the technical solution used in the present invention is:
From sea-tangle water, carry an environmental-protecting process for iodine, comprise the following steps: that (1), quantitative stock liquid regulate pH value; (2), according to amount of iodine in feed liquid, quantitatively in this part feed liquid, add oxygenant; (3), continue again to add hydrogen peroxide in feed liquid; (4), separately get 5-6 doubly to the stock liquid of above-mentioned amount, regulate pH value, with the abundant hybrid reaction of feed liquid after above-mentioned oxidation; (5), utilize Air blowing method that the iodine in feed liquid after mixing is blown out; (6) after, iodine is carried in adjusting, waste water ph is to neutral; (7), solution absorbs the iodine in blow out air; (8), the iodine in absorption liquid is resolved;
Specifically comprise the following steps:
(1), quantitatively stock liquid regulates pH value: quantitative sea-tangle water raw material is the technical hydrochloric acid of 30-36% to adding concentration in raw material, and its pH value is adjusted to 0.5-2.5;
(2), according to amount of iodine in feed liquid, quantitatively to adding oxygenant in this part feed liquid: add oxygenant in the sea-tangle water regulating after pH value, make wherein most of I
-be converted into I
2, the oxygenant adding is NaNO
2, NaClO or the coupling of the two, the addition of oxygenant regulates according to total amount of iodine in raw material, ensures that total iodo quantity 80% is oxidized, does not need enough oxidations; ;
(3), make I to adding hydrogen peroxide in feed liquid again
2peroxidation forms IO
3 -: in well-beaten situation, feed liquid in step (2) adds hydrogen peroxide to carry out peroxidation, regulate feed liquid just to substantially colourless, drip the constant indigo plant of starch, represent that peroxidation is complete, the addition of hydrogen peroxide regulates according to total amount of iodine in raw material, need to ensure that iodine in feed liquid is all by peroxidation;
(4), separately get 5-6 doubly to the stock liquid of above-mentioned amount, regulate pH value, with the abundant hybrid reaction of above-mentioned part feed liquid: separately get stock liquid, its volume 5-6 is the reduction of feed volume in step (2) doubly, regulate pH value to 1.5-2.5, the abundant hybrid reaction of liquid with step (3), makes IO
3 -with I
-fully reaction generates I
2simple substance;
(5), utilize Air blowing method that the iodine in feed liquid after mixing is blown out: according to raw material condition, utilize air that the iodine producing after sea-tangle water oxygen is blown out, stripping tower's temperature should remain on 40-60 DEG C, and the volume ratio of blow out air and liquid is 300-1000: 1;
(6) after, iodine is carried in adjusting, waste water ph is to neutral: add after completion of the reaction Ca (OH)
2or CaCO
3regulate waste water ph to 5.5-6.5;
(7), solution absorbs the iodine in blow out air: the NaOH that working concentration is 1-10% or Na
2sO
3solution absorbs the molecular iodine in blow out air as absorption liquid;
(8), the iodine in absorption liquid is resolved: absorption liquid is carried out to acidifying oxidation or reduction acidifying oxidation, the iodine in absorption liquid is separated out;
The invention has the beneficial effects as follows:
1, the present invention adopts novel mode of oxidizing environment-friendly type hydrogen peroxide to be applied to the extraction of iodine in sea-tangle water, has greatly reduced the pollution that original mode of oxidizing causes, and has improved the feature of environmental protection of producing.
2, the present invention has adopted two-step anodization to solve the problem of decomposing hydrogen dioxide solution, will be at I
-under concentration higher strip part, unsettled hydrogen peroxide is converted into stable HIO
3, improve greatly the utilising efficiency of hydrogen peroxide, reduce production cost, for the application of hydrogen peroxide on technique of extracting iodine provides a practicable method.
3, the present invention adopts the method for quantitative oxidizing reaction, ensureing the production impregnable while of yield, has fully reduced raw material consumption, has saved production cost.
4, the present invention consumes low, easy handling, practical, produces a practicable environmental-protecting process is provided for China's sea-tangle water extraction iodine.
Embodiment
Embodiment 1
Dry kelp soaking water 1m
3, wherein amount of iodine is at 150ppm, 15 DEG C of water temperatures.Adding concentration is that 30% technical hydrochloric acid regulates sea-tangle water pH value to 0.5; In the sea-tangle water regulating after pH value, add NaNO
20.1Kg, solution becomes redness; Add while stirring again 0.8Kg hydrogen peroxide, disappear to feed liquid is red, drip the constant indigo plant of starch, prove that peroxidation is complete; Separately get 5m
3stock liquid, regulates pH value to 1.5, with the abundant hybrid reaction of feed liquid after above-mentioned oxidation; By the feed liquid input air stripping tower after acidifying oxidation, the temperature of stripping tower is 40 DEG C, and direct input adds warm air the molecular iodine of oxidation generation is blown out, and it is faint yellow blowing to liquid, and sampling, adds a small amount of NaNO
2without colour-change, confirm substantially to blow out completely, the volume ratio of blow out air and liquid is 300: 1; Add after completion of the reaction Ca (OH)
2regulate waste water ph to 5.5; Use the air after waste gas absorption tower processing blows out, absorption liquid is that concentration is 1% NaOH solution 15L, after circulation absorbs and blows out containing the molecular iodine in iodine gas; After absorption completes, in absorption liquid, iodine content reaches 10.2%, in absorption liquid, first adds hydrochloric acid to be adjusted to neutrality, then adds the vitriol oil to regulate pH value to 1.2, and divides 3 days on average by 0.6Kg oxygenant KClO
3add in solution iodine is slowly separated out, then separate and obtain the thick iodine 1.3Kg of finished product through centrifuging, iodine purity is 95.0%.
Embodiment 2
Fresh sea-tangle blanching water 1m
3, wherein amount of iodine is at 720ppm, 75 DEG C of water temperatures.Adding concentration is that 36% technical hydrochloric acid regulates sea-tangle water pH value to 2.5; In the sea-tangle water regulating after pH value, add NaNO20.7Kg, solution becomes redness; Add while stirring again 6.0Kg hydrogen peroxide, disappear to feed liquid is red, drip the constant indigo plant of starch, prove that peroxidation is complete; Separately get 6m
3stock liquid, regulates pH value to 2.5, with the abundant hybrid reaction of feed liquid after above-mentioned oxidation; By the feed liquid input air stripping tower after acidifying oxidation, the temperature of stripping tower is 60 DEG C, and direct input adds in a large number warm air the molecular iodine of oxidation generation is blown out, and it is faint yellow blowing to liquid, adds a small amount of NaNO
2without colour-change, confirm substantially to blow out completely, the volume ratio of blow out air and liquid is 1000: 1; Add after completion of the reaction CaCO
3regulate waste water ph to 6.5; Use the air after waste gas absorption tower processing blows out, absorption liquid is that concentration is 10% Na
2sO
3solution 15L, circulation absorb after blowing out containing the molecular iodine in iodine gas; After absorption completes, in absorption liquid, iodine content reaches 11.3%, adds the vitriol oil to regulate pH value to 1.2, and divide 3 days on average by 0.7Kg oxygenant KClO in absorption liquid
3add in solution iodine is slowly separated out, then separate and obtain the thick iodine 1.42Kg of finished product through centrifuging, iodine purity is 96.0%.
Embodiment 3
Dry kelp soaking water 1m
3, wherein amount of iodine is at 150ppm, 15 DEG C of water temperatures.Adding concentration is that 30% technical hydrochloric acid regulates sea-tangle water pH value to 1; In the sea-tangle water regulating after pH value, add NaClO0.1Kg, solution becomes redness; Add while stirring again 0.8Kg hydrogen peroxide, disappear to feed liquid is red, drip the constant indigo plant of starch, prove that peroxidation is complete; Separately get 5m
3stock liquid, regulates pH value to 2, with the abundant hybrid reaction of feed liquid after above-mentioned oxidation; By the feed liquid input air stripping tower after acidifying oxidation, the temperature of stripping tower is 50 DEG C, and direct input adds warm air the molecular iodine of oxidation generation is blown out, and it is faint yellow blowing to liquid, and sampling, adds a small amount of NaNO
2without colour-change, confirm substantially to blow out completely, the volume ratio of blow out air and liquid is 500: 1; Add after completion of the reaction Ca (OH)
2regulate waste water ph to 6; Use the air after waste gas absorption tower processing blows out, absorption liquid is that concentration is 1% Na
2sO
3solution 15L, circulation absorb after blowing out containing the molecular iodine in iodine gas; After absorption completes, in absorption liquid, iodine content reaches 10.2%, in absorption liquid, first adds hydrochloric acid to be adjusted to neutrality, then adds the vitriol oil to regulate pH value to 1.2, and divides 3 days on average by 0.65Kg oxygenant KClO
3add in solution iodine is slowly separated out, then separate and obtain the thick iodine 1.4Kg of finished product through centrifuging, iodine purity is 95.0%.
Embodiment 4
Fresh sea-tangle blanching water 1m
3, wherein amount of iodine is at 720ppm, 75 DEG C of water temperatures.Adding concentration is that 30% technical hydrochloric acid regulates sea-tangle water pH value to 2; In the sea-tangle water regulating after pH value, add NaClO0.7Kg, solution becomes redness; Add while stirring again 6.0Kg hydrogen peroxide, disappear to feed liquid is red, drip the constant indigo plant of starch, prove that peroxidation is complete; Separately get 6m
3stock liquid, regulates pH value to 2.5, with the abundant hybrid reaction of feed liquid after above-mentioned oxidation; By the feed liquid input air stripping tower after acidifying oxidation, the temperature of stripping tower is 60 DEG C, and direct input adds in a large number warm air the molecular iodine of oxidation generation is blown out, and it is faint yellow blowing to liquid, adds a small amount of NaNO
2without colour-change, confirm substantially to blow out completely, the volume ratio of blow out air and liquid is 1000: 1; Add after completion of the reaction CaCO
3regulate waste water ph to 6.5; Use the air after waste gas absorption tower processing blows out, absorption liquid is that concentration is 10% NaOH solution 15L, after circulation absorbs and blows out containing the molecular iodine in iodine gas; After absorption completes, in absorption liquid, iodine content reaches 11.3%, adds the vitriol oil to regulate pH value to 1.2, and divide 3 days on average by 0.7Kg oxygenant KClO in absorption liquid
3add in solution iodine is slowly separated out, then separate and obtain the thick iodine 1.35Kg of finished product through centrifuging, iodine purity is 96.0%.
Claims (1)
1. an environmental-protecting process of carrying iodine from sea-tangle water, is characterized in that, comprises the following steps: that (1), quantitative stock liquid regulate pH value; (2), according to amount of iodine in feed liquid, quantitatively in this part feed liquid, add oxygenant; (3), continue again to add hydrogen peroxide in feed liquid; (4), separately get 5-6 doubly to the stock liquid of above-mentioned amount, regulate pH value, with the abundant hybrid reaction of feed liquid after above-mentioned oxidation; (5), utilize Air blowing method that the iodine in feed liquid after mixing is blown out; (6) after, iodine is carried in adjusting, waste water ph is to neutral; (7), solution absorbs the iodine in blow out air; (8), the iodine in absorption liquid is resolved;
Specifically comprise the following steps:
(1), quantitatively stock liquid regulates pH value: quantitative sea-tangle water raw material is the technical hydrochloric acid of 30-36% to adding concentration in raw material, and its pH value is adjusted to 0.5-2.5;
(2), according to amount of iodine in feed liquid, quantitatively to adding oxygenant in this part feed liquid: add oxygenant in the sea-tangle water regulating after pH value, make wherein most of I
-be converted into I
2, the oxygenant adding is NaNO
2, NaClO or the coupling of the two, the addition of oxygenant regulates according to total amount of iodine in stock liquid, ensures that total iodo quantity 80% is oxidized, does not need enough oxidations;
(3), make I to adding hydrogen peroxide in feed liquid again
2peroxidation forms IO
3 -: in well-beaten situation, feed liquid in step (2) adds hydrogen peroxide to carry out peroxidation, regulate feed liquid just to substantially colourless, drip the constant indigo plant of starch, represent that peroxidation is complete, the addition of hydrogen peroxide regulates according to total amount of iodine in stock liquid, need to ensure that iodine in feed liquid is all by peroxidation;
(4), separately get 5-6 doubly to the stock liquid of above-mentioned amount, regulate pH value, with the abundant hybrid reaction of above-mentioned part feed liquid: separately get stock liquid, its volume 5-6 is the reduction of feed volume in step (2) doubly, regulate pH value to 1.5-2.5, the abundant hybrid reaction of feed liquid with step (3), makes IO
3 -with I
-fully reaction generates I
2simple substance;
(5), utilize Air blowing method that the iodine in feed liquid after mixing is blown out: according to stock liquid situation, utilize air that the iodine producing after sea-tangle water oxygen is blown out, stripping tower's temperature should remain on 40-60 DEG C, and the volume ratio of blow out air and liquid is 300-1000: 1;
(6) after, iodine is carried in adjusting, waste water ph is to neutral: add after completion of the reaction Ca (OH)
2or CaCO
3regulate waste water ph to 5.5-6.5;
(7), solution absorbs the iodine in blow out air: the NaOH that working concentration is 1-10% or Na
2sO
3solution absorbs the molecular iodine in blow out air as absorption liquid;
(8), the iodine in absorption liquid is resolved: absorption liquid is carried out to acidifying oxidation or reduction acidifying oxidation, the iodine in absorption liquid is separated out.
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|---|---|---|---|
| CN201310090916.6A CN103130185B (en) | 2013-03-21 | 2013-03-21 | Novel environment-friendly technology for extracting iodine from kelp water |
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|---|---|---|---|
| CN201310090916.6A CN103130185B (en) | 2013-03-21 | 2013-03-21 | Novel environment-friendly technology for extracting iodine from kelp water |
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| CN103130185A CN103130185A (en) | 2013-06-05 |
| CN103130185B true CN103130185B (en) | 2014-09-24 |
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Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104528651A (en) * | 2014-12-15 | 2015-04-22 | 中国水产科学研究院黄海水产研究所 | Novel method for blowing off and extracting iodine air from kelp blanching wastewater |
| CN106517252A (en) * | 2016-10-10 | 2017-03-22 | 无锡易水元资源循环科技有限公司 | Analytical pure potassium iodide preparation method using waste liquid containing iodine |
| CN115368910A (en) * | 2022-08-31 | 2022-11-22 | 王乐 | Preparation method of soil conditioner |
Family Cites Families (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5828287A (en) * | 1981-08-06 | 1983-02-19 | シ−タス・コ−ポレ−シヨン | Production of iodine |
| JP2569104B2 (en) * | 1988-02-06 | 1997-01-08 | 三井東圧化学株式会社 | Method for recovering iodine from waste liquid containing organic iodine compound |
| JPH04310502A (en) * | 1991-04-08 | 1992-11-02 | Merck Patent Gmbh | Manufacturing process of element-form iodine |
| RU2194021C1 (en) * | 2001-09-24 | 2002-12-10 | Талановский Владимир Федорович | Method of iodine isolation from natural iodine-containing solution and iodine preparation |
| CN101318623B (en) * | 2008-06-26 | 2010-08-11 | 贵州大学 | Method for extracting iodine from iodine containing underground bittern |
| CN101323434A (en) * | 2008-06-26 | 2008-12-17 | 瓮福（集团）有限责任公司 | A method for reclaiming iodine from concentrated phosphoric acid produced by wet-process phosphoric acid |
| CN101318624B (en) * | 2008-06-26 | 2010-09-15 | 贵州大学 | Method for extracting iodine from circulating water of iodine-containing yellow phosphorus plant |
| CN101318626B (en) * | 2008-07-10 | 2010-06-09 | 贵州大学 | A device for recovering iodine from dilute phosphoric acid produced by wet-process phosphoric acid |
| CN101318625B (en) * | 2008-07-10 | 2010-06-09 | 贵州大学 | A method for recovering iodine from dilute phosphoric acid produced by wet-process phosphoric acid |
| US9994448B2 (en) * | 2009-11-12 | 2018-06-12 | Iofina Chemical, Inc. | Iodine extraction processes |
| 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 |
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