CN103130185A - 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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- CN103130185A CN103130185A CN2013100909166A CN201310090916A CN103130185A CN 103130185 A CN103130185 A CN 103130185A CN 2013100909166 A CN2013100909166 A CN 2013100909166A CN 201310090916 A CN201310090916 A CN 201310090916A CN 103130185 A CN103130185 A CN 103130185A
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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 the sea-tangle annual production is 800,000 tons of left and right, and the iodine in sea-tangle is one of important iodine resource of China, is also a kind of strategic material of preciousness simultaneously, is applied to many industries.The carry iodine resource of China take 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, bright sea-tangle blanching waste water, amount of iodine is about 300-600ppm.Present 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.Yet traditional oxygenant generally has the defective in use, can cause environmental pollution simultaneously, demands further improvement urgently.
The oxygenant that adopts 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 the NO toxic gas with Sodium Nitrite as oxygenant, affect the field personnel healthy, the exhaust emission ambient atmosphere, and because the needs excessive oxidant guarantees that oxidation is complete, therefore inevitably produce oxygenant residual, cause carry iodine after discharge of wastewater pollute; Hypochlorous sodium as oxygenant due to its be alkalescence, in use consume more hydrochloric acid, and cause the fluctuation of pH value, use inconvenient and be easy to use the excessive peroxidation sound productive rate that causes, therefore in use generally adopt the method for first replenishing with Sodium Nitrite again with hypochlorite oxidation, 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 with the I in solution
-Be oxidized to I
2Simple substance, but in actual applications due to hydrogen peroxide at I
-And I
2Unstable and accelerate decomposition in situation about existing, thus cause at I
-Can't make the I complete oxidation in the higher solution of concentration is elemental iodine, has limited its application in marine alga water extraction iodine is produced.
The hydrogen peroxide oxidation method is cooperated to carry out phosphorus ore in China Guizhou University and urn good fortune Group Co.,Ltd and is applied in proposing iodine production, and application or the multinomial patent of obtaining the authorization, as: " extracting the method for iodine from contain the iodine phosphate ore production in the dilute phosphoric acid that produces " (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 needs 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, solved the pollution problem that technique of extracting iodine causes due to oxygenant, and technological operation is convenient, production cost is low, and is practical.
For solving the problems of the technologies described above, the technical solution used in the present invention is:
A kind of environmental-protecting process of carrying iodine from sea-tangle water comprises the following steps: (1), quantitative stock liquid adjusting pH value; (2), according to amount of iodine in feed liquid, quantitatively add oxygenant in this part feed liquid; (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 the pH value, with the abundant hybrid reaction of feed liquid after above-mentioned oxidation; (5), the iodine that utilizes the Air blowing method will mix in rear feed liquid blows 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 is regulated the pH value: quantitative sea-tangle water raw material, adding concentration in the raw material is the technical hydrochloric acid of 30-36%, and its pH value is adjusted to 0.5-2.5;
(2), according to amount of iodine in feed liquid, quantitatively add oxygenant in this part feed liquid: add oxygenant in the sea-tangle water of regulating after the pH value, make wherein most of I
-Be converted into I
2, the oxygenant that adds is NaNO
2, NaClO or coupling both, the addition of oxygenant is regulated according to total amount of iodine in raw material, guarantees that total iodo quantity 80% is oxidized, does not need the capacity oxidation;
(3), add again hydrogen peroxide in the feed liquid and make I
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 namely peroxidation is complete, the addition of hydrogen peroxide is regulated according to total amount of iodine in raw material, and the iodine in needs assurance feed liquid is all by peroxidation;
(4), separately get 5-6 doubly to the stock liquid of above-mentioned amount, regulate the pH value, and 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 the pH value to 1.5-2.5, the abundant hybrid reaction of liquid with in step (3) makes IO
3 -With I
-Fully reaction generates I
2Simple substance;
(5), the iodine that utilizes the Air blowing method will mix in rear feed liquid blows out: according to raw material condition, the iodine that produces after utilizing air with the sea-tangle water oxygen blows out, stripping tower's temperature should remain on 40-60 ℃, and the volume ratio of blow out air and liquid is 300-1000: 1;
(6), regulate carry iodine after waste water ph to neutral: react and add Ca (OH) after complete
2Or CaCO
3Regulate waste water ph to 5.5-6.5;
(7), solution absorbs the iodine in blow out air: working concentration is NaOH or the Na of 1-10%
2SO
3Solution is as the molecular iodine in absorption liquid absorption blow out air;
(8), the iodine in absorption liquid is resolved: absorption liquid is carried out 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 the 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, improved greatly the dioxygen water use efficiency, reduced production cost, the application for hydrogen peroxide on technique of extracting iodine provides a practicable method.
3, the present invention adopts the method for quantitative oxidizing reaction, guaranteeing 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, for China's sea-tangle water extraction iodine production provides a practicable environmental-protecting process.
Embodiment
Embodiment 1
Dried kelp soaking water 1m
3, wherein amount of iodine is at 150ppm, 15 ℃ of water temperatures.Adding concentration is that 30% technical hydrochloric acid is regulated sea-tangle water pH value to 0.5; Add NaNO in the sea-tangle water of regulating after the pH value
20.1Kg solution becomes redness; Add while stirring again the 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 is regulated pH value to 1.5, with the abundant hybrid reaction of feed liquid after above-mentioned oxidation; With the feed liquid input air stripping tower after the acidifying oxidation, the temperature of stripping tower is 40 ℃, and direct input adds warm air the molecular iodine that oxidation produces 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 fully, the volume ratio of blow out air and liquid is 300: 1; React and add Ca (OH) after complete
2Regulate waste water ph to 5.5; Use waste gas absorption tower to process air after blowing out, absorption liquid is that concentration is 1% NaOH solution 15L, contains molecular iodine in iodine gas after circulation absorbs and blows out; After absorption was completed, in absorption liquid, iodine content reached 10.2%, first added hydrochloric acid to be adjusted to neutrality in absorption liquid, then added the vitriol oil to regulate pH value to 1.2, and divided 3 days on average with 0.6Kg oxygenant KClO
3Add iodine is slowly separated out, more namely obtain the thick iodine 1.3Kg of finished product through the centrifuging separation, iodine purity is 95.0%.
Embodiment 2
Bright sea-tangle blanching water 1m
3, wherein amount of iodine is at 720ppm, 75 ℃ of water temperatures.Adding concentration is that 36% technical hydrochloric acid is regulated sea-tangle water pH value to 2.5; Add NaNO20.7Kg in the sea-tangle water of regulating after the pH value, solution becomes redness; Add while stirring again the 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 is regulated pH value to 2.5, with the abundant hybrid reaction of feed liquid after above-mentioned oxidation; With the feed liquid input air stripping tower after the acidifying oxidation, the temperature of stripping tower is 60 ℃, and direct input adds in a large number warm air the molecular iodine that oxidation produces 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 fully, the volume ratio of blow out air and liquid is 1000: 1; React and add CaCO after complete
3Regulate waste water ph to 6.5; Use the air after the waste gas absorption tower processing blows out, absorption liquid is that concentration is 10% Na
2SO
3Solution 15L contains molecular iodine in iodine gas after circulation absorbs and to blow out; After absorption was completed, in absorption liquid, iodine content reached 11.3%, added the vitriol oil to regulate pH value to 1.2 in absorption liquid, and divided 3 days on average with 0.7Kg oxygenant KClO
3Add iodine is slowly separated out, more namely obtain the thick iodine 1.42Kg of finished product through the centrifuging separation, iodine purity is 96.0%.
Embodiment 3
Dried kelp soaking water 1m
3, wherein amount of iodine is at 150ppm, 15 ℃ of water temperatures.Adding concentration is that 30% technical hydrochloric acid is regulated sea-tangle water pH value to 1; Add NaClO0.1Kg in the sea-tangle water of regulating after the pH value, solution becomes redness; Add while stirring again the 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 is regulated pH value to 2, with the abundant hybrid reaction of feed liquid after above-mentioned oxidation; With the feed liquid input air stripping tower after the acidifying oxidation, the temperature of stripping tower is 50 ℃, and direct input adds warm air the molecular iodine that oxidation produces 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 fully, the volume ratio of blow out air and liquid is 500: 1; React and add Ca (OH) after complete
2Regulate waste water ph to 6; Use the air after the waste gas absorption tower processing blows out, absorption liquid is that concentration is 1% Na
2SO
3Solution 15L contains molecular iodine in iodine gas after circulation absorbs and to blow out; After absorption was completed, in absorption liquid, iodine content reached 10.2%, first added hydrochloric acid to be adjusted to neutrality in absorption liquid, then added the vitriol oil to regulate pH value to 1.2, and divided 3 days on average with 0.65Kg oxygenant KClO
3Add iodine is slowly separated out, more namely obtain the thick iodine 1.4Kg of finished product through the centrifuging separation, iodine purity is 95.0%.
Embodiment 4
Bright sea-tangle blanching water 1m
3, wherein amount of iodine is at 720ppm, 75 ℃ of water temperatures.Adding concentration is that 30% technical hydrochloric acid is regulated sea-tangle water pH value to 2; Add NaClO0.7Kg in the sea-tangle water of regulating after the pH value, solution becomes redness; Add while stirring again the 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 is regulated pH value to 2.5, with the abundant hybrid reaction of feed liquid after above-mentioned oxidation; With the feed liquid input air stripping tower after the acidifying oxidation, the temperature of stripping tower is 60 ℃, and direct input adds in a large number warm air the molecular iodine that oxidation produces 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 fully, the volume ratio of blow out air and liquid is 1000: 1; React and add CaCO after complete
3Regulate waste water ph to 6.5; Use waste gas absorption tower to process air after blowing out, absorption liquid is that concentration is 10% NaOH solution 15L, contains molecular iodine in iodine gas after circulation absorbs and blows out; After absorption was completed, in absorption liquid, iodine content reached 11.3%, added the vitriol oil to regulate pH value to 1.2 in absorption liquid, and divided 3 days on average with 0.7Kg oxygenant KClO
3Add iodine is slowly separated out, more namely obtain the thick iodine 1.35Kg of finished product through the centrifuging separation, 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: (1), quantitative stock liquid adjusting pH value; (2), according to amount of iodine in feed liquid, quantitatively add oxygenant in this part feed liquid; (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 the pH value, with the abundant hybrid reaction of feed liquid after above-mentioned oxidation; (5), the iodine that utilizes the Air blowing method will mix in rear feed liquid blows 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 is regulated the pH value: quantitative sea-tangle water raw material, adding concentration in the raw material is the technical hydrochloric acid of 30-36%, and its pH value is adjusted to 0.5-2.5;
(2), according to amount of iodine in feed liquid, quantitatively add oxygenant in this part feed liquid: add oxygenant in the sea-tangle water of regulating after the pH value, make wherein most of I
-Be converted into I
2, the oxygenant that adds is NaNO
2, NaClO or coupling both, the addition of oxygenant is regulated according to total amount of iodine in stock liquid, guarantees that total iodo quantity 80% is oxidized, does not need the capacity oxidation;
(3), add again hydrogen peroxide in the feed liquid and make I
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 namely peroxidation is complete, the addition of hydrogen peroxide is regulated according to total amount of iodine in stock liquid, and the iodine in needs assurance feed liquid is all by peroxidation;
(4), separately get 5-6 doubly to the stock liquid of above-mentioned amount, regulate the pH value, and 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 the pH value to 1.5-2.5, the abundant hybrid reaction of liquid with in step (3) makes IO
3 -With I
-Fully reaction generates I
2Simple substance;
(5), the iodine that utilizes the Air blowing method will mix in rear feed liquid blows out: according to the stock liquid situation, the iodine that produces after utilizing air with the sea-tangle water oxygen blows out, stripping tower's temperature should remain on 40-60 ℃, and the volume ratio of blow out air and liquid is 300-1000: 1;
(6), regulate carry iodine after waste water ph to neutral: react and add Ca (OH) after complete
2Or CaCO
3Regulate waste water ph to 5.5-6.5;
(7), solution absorbs the iodine in blow out air: working concentration is NaOH or the Na of 1-10%
2SO
3Solution is as the molecular iodine in absorption liquid absorption blow out air;
(8), the iodine in absorption liquid is resolved: absorption liquid is carried out acidifying oxidation or reduction acidifying oxidation, the iodine in absorption liquid is separated out.
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|---|---|---|---|
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| CN103130185B CN103130185B (en) | 2014-09-24 |
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Cited By (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 |
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|---|---|---|---|---|
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| 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 |
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| CN103130185B (en) | 2014-09-24 |
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