CN101318623B - Method for extracting iodine from iodine containing underground bittern - Google Patents
Method for extracting iodine from iodine containing underground bittern Download PDFInfo
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- CN101318623B CN101318623B CN2008103023512A CN200810302351A CN101318623B CN 101318623 B CN101318623 B CN 101318623B CN 2008103023512 A CN2008103023512 A CN 2008103023512A CN 200810302351 A CN200810302351 A CN 200810302351A CN 101318623 B CN101318623 B CN 101318623B
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Abstract
The invention discloses a method for extracting iodine from iodine-containing subsurface brine; the content of iodine in the subsurface brine is 20-30mg/L, compound oxidant is added in the subsurface brine as oxidant for oxidation reaction, air is used for blowing molecular iodine out, then SO2 acidic solution is used for absorbing, the pH value of absorption liquid is between 1-6, then hydrogen peroxide is added to separate iodine out and filtration and separation are carried out to obtain finished iodine. The subsurface brine with iodine content of 20-30 mg/L is usually selected as raw material for extracting iodine; the compound oxidant of the invention can improve the efficiency of oxidant; proved by tests, after the hydrogen peroxide is added with vanadic oxide, the dosage of oxidantcan be reduced by 30%. Therefore, the method and the compound oxidant proposed by the applicant after tests can extract the iodine with low content and can expand the select range of the raw materials for extracting iodine.
Description
Technical field: the present invention relates to from contain the iodine subsurface brine, extract the method for iodine, belong to the environmental protection, the chemical technology field that extract iodine.
Background technology: China most of manufacture iodine producer all contains bittern, bittern or the kelp-soaking liquid (iodine content: 200-300mg/L) make raw material production industry iodine of iodide with higher-grade at present, the technology that adopts mostly is ion-exchange-resin process, after being about to bittern, bittern or kelp-soaking liquid that higher-grade contains iodide and being acidified with acid, feed chlorine, iodine is dissociated separate out, adsorb by polystyrene type ion exchange resin again.The method of desorption has two kinds: a kind of is to use the sulfite solution wash-out. with Potcrate iodine is separated out again, and centrifugation, thick iodine is through the sulfuric acid melt refining; Another kind is to use the sodium hydroxide solution wash-out, generates iodide such as NaI, makes the free precipitation of iodine with sulfuric acid acidation in reactor, filters and centrifugation, re-refines.Mainly there is two large problems in this method: the one, and production run cost height, the 2nd, production technique requires high to raw material (bittern, bittern or the kelp-soaking liquid that contain iodide) amount of iodine.
The method that blows out is at first adopted by Japanese Yi Xi chemical industrial company, and this is a kind of superior technical process at present.Clarifying bittern water is acidified to pH 2～3, enters in the stripping tower after logical chlorine mixes, by C1
2The I that displaces
2Make it gasification with air draught, iodine vapor in the air-flow is introduced behind the absorption tower with being dissolved with S0
2A kind of iodine solution absorb.Iodide solution goes out and keeps iodide solution recirculation from tower bottom flow with the concentration of 50～100g/L, and solution logical chlorine in the reactor of glass is handled iodine is separated out then, and then the filtration of the suspended substance of iodine, filtrate turns back in the iodide system and goes.Iodine is as filter cake melt refining in the vitriol oil.The traditional method that blows out technology contains iodine to production stoste and requires more than the 200mg/L.
Summary of the invention
The object of the invention is: a kind of method of extracting iodine from contain the iodine subsurface brine is provided.This method mainly to can not handle with other method low contain the iodine subsurface brine (I:20～30mg/L) carries out effective iodine to be separated, with composite oxidant and sulfurous gas as the raw materials for production additive, so more convenient, safety; Both solve waste discharge, caused environmental pollution problems, a kind of new system iodine raw material was provided again, waste can be turned waste into wealth, and can overcome the technical problem that prior art exists simultaneously.
The present invention constitutes like this: the method for extracting iodine from contain the iodine subsurface brine, the content of iodine is in the subsurface brine: 20～30mg/L, in subsurface brine solution, add composite oxidant as the oxidizing reaction oxygenant, blow out wherein molecular iodine with air, then with containing SO
2Acidic solution absorbs, and the pH value of absorption liquid adds hydrogen peroxide again between 1～6, iodine is separated out, and filters and separates, must finished product iodine.
The above-mentioned method of extracting iodine from contain the iodine subsurface brine, the acidity scope of adjusting subsurface brine solution is: pH value 2-3.
The above-mentioned method of from contain the iodine subsurface brine, extracting iodine, by weight, the proportioning of described composite oxidant is a hydrogen peroxide 27～35%, Vanadium Pentoxide in FLAKES 0.1～0.2%, rest part are water.
The above-mentioned method of from contain the iodine subsurface brine, extracting iodine, concrete way is: the composite oxidant that adds 0.01～0.1 kilogram in 100 kilograms of subsurface brines is as oxygenant, reaction, blow out wherein molecular iodine with 40～80 degrees centigrade of warm airs, the warm air that blows and the volume ratio of liquid are 130～150: 1, and then with containing SO
2When the content of iodine reaches 100～150g/L in the liquid that acidic solution circulation absorbs, obtains, add 0.5～3 kilogram in hydrogen peroxide in per 100 kilograms of liquid that obtain, iodine is separated out, filter and centrifugation, through refining finished product iodine.
The above-mentioned method of extracting iodine from contain the iodine subsurface brine, when blowing out wherein molecular iodine with air, vapour-liquid ratio is: 130～250: 1.
The above-mentioned method of extracting iodine from contain the iodine subsurface brine, the pH value of absorption liquid is between 1～4.
The above-mentioned method of extracting iodine from contain the iodine subsurface brine, used warm air is 60～70 degrees centigrade.
Subsurface brine is mainly derived from underground bittern water, oil-gas field underground water.Generally contain iodine 7～30mg/L, pH value 3-5.The present invention extracts the raw material of iodine, select the content of iodine in the subsurface brine to be generally 20～30mg/L, iodine content is crossed low prior art and can't be handled, and extracts the method for iodine in the prior art, normally adopt the higher raw material of amount of iodine, the amount of iodine of its raw material generally all is more than the 200mg/L.Subsurface brine is because the content of iodine is low, normally as contaminant removal or emit, not only wasted iodine, also pollutes the environment.Method and composite oxidant that the applicant's test draws can extract the iodine of underground bittern low levels.Therefore compare with prior art, the present invention has enlarged the range of choice of extracting the raw material of iodine.Simultaneously, in subsurface brine, contain impurity such as ore slag, metal ion, and the chemical substance of a lot of organism and reductibility, in iodine oxide, above-mentioned substance is also simultaneously oxidized, so oxygenant actual amount height, the oxygenant waste is serious.Composite oxidant disclosed in this invention, make oxygenant consumption still less, production cost is lower.Through applicant's test, produce 1 ton of iodine, need to use 5～10 tons composite oxidant, than only adopting hydrogen peroxide, can save the consumption 20～30% of oxygenant as oxygenant.
Embodiment:
Embodiments of the invention 1: from contain the iodine subsurface brine, extract iodine, wherein iodine content is in the subsurface brine: 20mg/L, pH:5.5 adjusts this subsurface brine pH to 3 adds 0.01 kilogram in 100 kilograms of these subsurface brines composite oxidant, the proportioning of composite oxidant is a hydrogen peroxide 27～35%, Vanadium Pentoxide in FLAKES 0.1～0.2%, rest part is a water, mix and carried out oxidizing reaction in 5 minutes, blow out wherein molecular iodine with 60 degrees centigrade of warm airs then, the warm air that blows and the volume ratio of liquid are 130: 1, then with containing SO
2The acidic solution circulation liquid that absorbs, obtain in the content of iodine when reaching 100g/L, add 0.5 kilogram in hydrogen peroxide in per 100 kilograms of liquid that obtain, iodine is separated out, filter and centrifugation, through refining finished product iodine.
Embodiments of the invention 2: from contain the iodine subsurface brine, extract iodine, wherein iodine content is in the subsurface brine: 30mg/L, pH:5.5 adjusts this subsurface brine pH to 4, the composite oxidant that in 1000 kilograms of these subsurface brines, adds 1 kilogram, the proportioning of composite oxidant is that 1 kilogram of content is the Vanadium Pentoxide in FLAKESs that add 20 grams in 30% the hydrogen peroxide, mix and carried out oxidizing reaction in 10 minutes, blow out wherein molecular iodine with 70 degrees centigrade of warm airs then, the warm air that blows and the volume ratio of liquid are 150: 1, use SO then
2When the content of iodine reaches 100g/L in the liquid that acidic solution circulation absorbs, obtains, add 0.5 kilogram in hydrogen peroxide in per 100 kilograms of liquid that obtain, iodine is separated out, filter and centrifugation, through refining finished product iodine.
Embodiments of the invention 3: extract iodine from contain the iodine subsurface brine, wherein iodine content is in the subsurface brine: 30mg/L, pH:4.5.The composite oxidant that in 100 kilograms of these subsurface brines, adds 0.1 kilogram, the proportioning of composite oxidant is a hydrogen peroxide 35%, Vanadium Pentoxide in FLAKES 0.2%, rest part is a water, mix and carried out oxidizing reaction in 5 minutes, blow out wherein molecular iodine with 65 degrees centigrade of warm airs then, the warm air that blows and the volume ratio of liquid are 250: 1, use SO then
2When the content of iodine reaches 100g/L in the liquid that acidic solution circulation absorbs, obtains, add 0.5 kilogram in hydrogen peroxide in per 100 kilograms of liquid that obtain, iodine is separated out, filter and centrifugation, through refining finished product iodine.
Embodiments of the invention 4: from contain the iodine subsurface brine, extract iodine, wherein iodine content is in the subsurface brine: 25mg/L, pH:5 adds 0.03 kilogram composite oxidant in 100 kilograms of these subsurface brines, the proportioning of composite oxidant is a hydrogen peroxide 27%, Vanadium Pentoxide in FLAKES 0.1%, rest part is a water, mixes and carries out oxidizing reaction in 5 minutes, blows out wherein molecular iodine with 70 degrees centigrade of warm airs then, the warm air that blows and the volume ratio of liquid are 250: 1, use SO then
2When the content of iodine reaches 100g/L in the liquid that acidic solution circulation absorbs, obtains, add 0.5 kilogram in hydrogen peroxide in per 100 kilograms of liquid that obtain, iodine is separated out, filter and centrifugation, through refining finished product iodine.
Claims (5)
1. extract the method for iodine from contain the iodine subsurface brine, it is characterized in that: the content of iodine is in the subsurface brine: 20～30mg/L, in subsurface brine solution, add composite oxidant as the oxidizing reaction oxygenant, and blow out wherein molecular iodine with air, then with containing SO
2Acidic solution absorbs, and the pH value of absorption liquid adds hydrogen peroxide again between 1～6, iodine is separated out, and filters and separates, must finished product iodine; By weight, the proportioning of described composite oxidant is a hydrogen peroxide 27～35%, and Vanadium Pentoxide in FLAKES 0.1～0.2%, rest part are water.
2. according to the described method of extracting iodine from contain the iodine subsurface brine of claim 1, it is characterized in that: the acidity scope of adjusting subsurface brine solution is: pH value 2-3.
3. according to claim 1 or the 2 described methods of from contain the iodine subsurface brine, extracting iodine, it is characterized in that: concrete way is: the composite oxidant that adds 0.01～0.1 kilogram in 100 kilograms of subsurface brines is as oxygenant, reaction, blow out wherein molecular iodine with 40～80 degrees centigrade of warm airs, the warm air that blows and the volume ratio of liquid are 130～150: 1, and then with containing SO
2When the content of iodine reaches 100～150g/L in the liquid that acidic solution circulation absorbs, obtains, add 0.5～3 kilogram in hydrogen peroxide in per 100 kilograms of liquid that obtain, iodine is separated out, filter and centrifugation, through refining finished product iodine.
4. according to the described method of extracting iodine from contain the iodine subsurface brine of claim 3, it is characterized in that: the pH value of absorption liquid is between 1～4.
5. according to the described method of extracting iodine from contain the iodine subsurface brine of claim 3, it is characterized in that: used warm air is 60～70 degrees centigrade.
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| CN2008103023512A CN101318623B (en) | 2008-06-26 | 2008-06-26 | Method for extracting iodine from iodine containing underground bittern |
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| CN2008103023512A CN101318623B (en) | 2008-06-26 | 2008-06-26 | Method for extracting iodine from iodine containing underground bittern |
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| CN101318623B true CN101318623B (en) | 2010-08-11 |
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| 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 |
| CN103007573B (en) * | 2012-11-19 | 2015-06-10 | 山东洁晶集团股份有限公司 | Method for extracting and preparing elementary iodine from industrial seaweed wastewater through gas extraction method |
| CN103130185B (en) * | 2013-03-21 | 2014-09-24 | 中国水产科学研究院黄海水产研究所 | Novel environment-friendly technology for extracting iodine from kelp water |
| CN104192804B (en) * | 2014-08-22 | 2016-06-15 | 清华大学 | A kind of from containing the polyacid catalysis process extracting iodine iodine waste water |
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Owner name: WENGFU (GROUP) CO., LTD. Free format text: FORMER OWNER: GUIZHOU UNIVERSITY Effective date: 20130207 Free format text: FORMER OWNER: WENGFU (GROUP) CO., LTD. Effective date: 20130207 |
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