CN101323434A - Method for reclaiming iodine from concentrated phosphoric acid from wet method phosphoric acid production - Google Patents
Method for reclaiming iodine from concentrated phosphoric acid from wet method phosphoric acid production Download PDFInfo
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- CN101323434A CN101323434A CNA2008103023546A CN200810302354A CN101323434A CN 101323434 A CN101323434 A CN 101323434A CN A2008103023546 A CNA2008103023546 A CN A2008103023546A CN 200810302354 A CN200810302354 A CN 200810302354A CN 101323434 A CN101323434 A CN 101323434A
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- phosphoric acid
- iodine
- hydrogen peroxide
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- strong phosphoric
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Abstract
The invention discloses a method for recovering iodine from concentrated phosphoric acid which is produced by wet-process phosphoric acid; the method comprises the following steps of: extracting the iodine from the concentrated phosphoric acid produced in the production process of phosphorous ore which contains iodine, wherein, the concentrated phosphoric acid contains 50 to 110 mg/L of the iodine and 40 percent to 52 percent of P2O5; adding 27 percent to 35 percent of hydrogen peroxide water solution into the phosphoric acid as an oxidizing agent for reaction; using air to blow out the molecular iodine of the phosphoric acid; then absorbing the molecular iodine by acid solution containing liquid SO2 with the PH value of the absorbing solution ranging from 1 to 6; adding hydrogen peroxide and leading the iodine to be precipitated; carrying out filtering and separation and obtaining the finished iodine. The applicant finds that the iodine is extracted from the concentrated phosphoric acid after the diluted phosphoric acid is concentrated into the concentrated phosphoric acid; as the material liquid is concentrated, the concentration of the material iodine is high, the solution impurity is little and the content of the reducible matter and the organic matter is low, therefore, the usage of the oxidizing agent can be reduced; the method of the invention has the advantages of high concentration of the material iodine, little usage of the oxidizing agent, easy extraction, high recovery rate and low production cost.
Description
Technical field:
The present invention relates to a kind of method of extracting iodine from the strong phosphoric acid of Wet-process Phosphoric Acid Production, is P in the raw material production phosphorus product process to contain the iodine Rock Phosphate (72Min BPL) particularly
2O
5Concentration concentration is 40～52% the interior method of extracting iodine of strong phosphoric acid; The field that belongs to environmental protection, chemical industry technology.
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. make iodine separate out, filter with the Potcrate oxidation again, 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, filters with sulfuric acid acidation in reactor, 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 Cl
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 SO
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 the requirement height of iodine technical indicator to production stoste, blows out iodine content in the stoste more than 200mg/L.The inventor applied for that a name was called " method of extracting iodine from contain the iodine phosphate ore production in the dilute phosphoric acid that produces ", the patent No. is: 2005100030582 application for a patent for invention, utilize this method to extract iodine from contain the dilute phosphoric acid that produces when the iodine Rock Phosphate (72Min BPL) is produced phosphorus product; But in industrial test, find, adopt common hydrogen peroxide as oxygenant, actual usage quantity, big more a lot of than theoretical value, prepare 1 ton iodine in the test, only need 600 kilograms in theory, and actual amount has reached 30 tons.Therefore raw materials consumption is big, the production cost height.
Summary of the invention
The object of the invention is: a kind of method that reclaims iodine from the strong phosphoric acid of Wet-process Phosphoric Acid Production is provided; This method is mainly carried out effective iodine separation to the low iodine strong phosphoric acid (about I:50～110mg/L) that contains that can not handle with other method, and uses hydrogen peroxide and sulfurous gas as raw materials for production, 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: reclaim the method for iodine from the strong phosphoric acid of Wet-process Phosphoric Acid Production, extract in the strong phosphoric acid that produces from contain the iodine phosphate ore production, wherein the content of iodine is in the strong phosphoric acid: the P in 50～110mg/L, the strong phosphoric acid
2O
5Concentration is 40～52%, adds 27～35% aqueous hydrogen peroxide solution as oxidant reaction in phosphoric acid, blows out wherein molecular iodine with air, then with containing liquid SO
2Acidic solution absorb, 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.
Above-mentioned a kind of method that reclaims iodine from the strong phosphoric acid of Wet-process Phosphoric Acid Production, the proportioning of oxygenant is: hydrogen peroxide 27～35%, surplus are water.
Above-mentioned a kind of method that reclaims iodine from the strong phosphoric acid of Wet-process Phosphoric Acid Production, the proportioning of oxygenant is: hydrogen peroxide 27～35%, Vanadium Pentoxide in FLAKES 0.1～0.2%, rest part are water.
Above-mentioned a kind of method that reclaims iodine from the strong phosphoric acid of Wet-process Phosphoric Acid Production blows out wherein molecular iodine, vapour-liquid ratio: 100～250: 1 with air.
Above-mentioned a kind of method that from the strong phosphoric acid of Wet-process Phosphoric Acid Production, reclaims iodine, concrete way is: the aqueous hydrogen peroxide solution oxygenant, the reaction that add 0.05～0.1 kilogram in 100 kilograms of these strong phosphoric acid, blow out wherein molecular iodine with air, then with containing liquid SO
2The acidic solution circulation liquid that absorbs, obtain in the content of iodine when reaching 100～150g/L, add 0.5～3 kilogram in common hydrogen peroxide in per 100 kilograms of liquid that obtain, iodine is separated out, filter and centrifugation, through refining finished product iodine.
Above-mentioned a kind of method that reclaims iodine from the strong phosphoric acid of Wet-process Phosphoric Acid Production, adding the time that the aqueous hydrogen peroxide solution oxygenant carries out oxidizing reaction in the strong phosphoric acid is 5～30 minutes.
Above-mentioned a kind of method that reclaims iodine from the strong phosphoric acid of Wet-process Phosphoric Acid Production, the pH value of absorption liquid is between 1～4.
Extract 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.Test discovery through the applicant, the dilute phosphoric acid that Wet-process Phosphoric Acid Production obtains, further prepare strong phosphoric acid after, wherein major ingredient is: P
2O
5: 40～52%; SO
4: 2～5.8%; F:0.7～1.5%; Ca:100～150mg/L; SiO
2: 850～950mg/L; Na:350～750mg/L; K:360～400mg/L; I:50～110mg/L; Therefore, in the strong phosphoric acid of Wet-process Phosphoric Acid Production, the content of iodine is generally 50～110mg/L, than dilute phosphoric acid height, and in the dilute phosphoric acid liquid that produces in the phosphate ore production, wherein contain impurity such as a large amount of ore slags, 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.The applicant has carried out industrialized a series of test and research in phosphatization factory, find that dilute phosphoric acid is condensed into after the strong phosphoric acid, from strong phosphoric acid, extract iodine again, because raw material liq is through concentrating, raw material iodine concentration height, solution impurity are few, reducing substances and organic content are low, therefore can reduce the consumption of oxygenant.Find through the industrial test that the applicant carries out, adopt dilute phosphoric acid, prepare 1000 kilograms iodine in the test, only need 600 kilograms of hydrogen peroxide in theory, and actual amount has reached 30 tons.Adopt strong phosphoric acid, the oxygenant consumption is 10～15 tons, and the raw material treatment capacity also reduces half, has shortened the production time.Compare with prior art, the present invention have raw material iodine concentration height, oxygenant consumption few, extract easily, the rate of recovery is high, production cost is low advantage.
Embodiment
Embodiments of the invention 1: reclaim the method for iodine from the strong phosphoric acid of Wet-process Phosphoric Acid Production, wherein the content of iodine is in the strong phosphoric acid: the P in 50mg/L, the strong phosphoric acid
2O
5Concentration is 52%, adds 0.05 kilogram of 30% aqueous hydrogen peroxide solution oxygenant in 100 kilograms of these strong phosphoric acid.Mix and carried out oxidizing reaction in 5 minutes, blow out wherein molecular iodine with 40 degrees centigrade of warm airs then, the warm air that blows and the volume ratio of liquid are 100: 1, then with containing liquid 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: reclaim the method for iodine from the strong phosphoric acid of Wet-process Phosphoric Acid Production, wherein the content of iodine is in the strong phosphoric acid: the P in 110mg/L, the strong phosphoric acid
2O
5Concentration is 40%, and 27% aqueous hydrogen peroxide solution that adds 0.1 kilogram in 100 kilograms of these strong phosphoric acid is as oxygenant.Mix and carried out oxidizing reaction in 30 minutes, blow out wherein molecular iodine with 40 degrees centigrade of warm airs then, the warm air that blows and the volume ratio of liquid are 130: 1, then with containing liquid SO
2The acidic solution circulation liquid that absorbs, obtain in the content of iodine when reaching 110g/L, add 3 kilograms 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: a kind of method that reclaims iodine from the strong phosphoric acid of Wet-process Phosphoric Acid Production, wherein the content of iodine is in the strong phosphoric acid: the P in 80mg/L, the strong phosphoric acid
2O
5Concentration is 48%, the oxygenant that in 100 kilograms of these strong phosphoric acid, adds 0.05 kilogram, the proportioning of oxygenant is a hydrogen peroxide 27～35%, Vanadium Pentoxide in FLAKES 0.1～0.2%, rest part is a water, mixes and carries out oxidizing reaction in 10～20 minutes, and the time of oxidizing reaction is controlled at and both can guarantees that oxidizing reaction was abundant in 10～20 minutes, can control the production time again, reduce production costs.Blow out wherein molecular iodine with 40 degrees centigrade of warm airs then, the warm air that blows and the volume ratio of liquid are 250: 1, then with containing liquid SO
2The acidic solution circulation liquid that absorbs, obtain in the content of iodine when reaching 150g/L, add 2 kilograms in hydrogen peroxide in per 100 kilograms of liquid that obtain, iodine is separated out, filter and centrifugation, through refining finished product iodine.
Claims (7)
1. method that from the strong phosphoric acid of Wet-process Phosphoric Acid Production, reclaims iodine, it is characterized in that: extract in the strong phosphoric acid that from contain the iodine phosphate ore production, produces, wherein the content of iodine is in the strong phosphoric acid: the P2O5 concentration in 50～110mg/L, the strong phosphoric acid is 40～52%, in phosphoric acid, add 27～35% aqueous hydrogen peroxide solution as oxidant reaction, blow out wherein molecular iodine with air, absorb with the acidic solution that contains liquid SO 2 then, the pH value of absorption liquid is between 1～6, add hydrogen peroxide again, iodine is separated out, filter and separates, must finished product iodine.
2. according to the described a kind of method that reclaims iodine from the strong phosphoric acid of Wet-process Phosphoric Acid Production of claim 1, it is characterized in that: by weight, the proportioning of oxygenant is: hydrogen peroxide 27～35%, surplus are water.
3. according to the described a kind of method that reclaims iodine from the strong phosphoric acid of Wet-process Phosphoric Acid Production of claim 2, it is characterized in that: by weight, the proportioning of oxygenant is: hydrogen peroxide 27～35%, Vanadium Pentoxide in FLAKES 0.1～0.2%, rest part are water.
4. according to the described a kind of method that from the strong phosphoric acid of Wet-process Phosphoric Acid Production, reclaims iodine of claim 1, it is characterized in that: blow out wherein molecular iodine, vapour-liquid ratio: 100～250: 1 with air.
5. according to the described a kind of method that from the strong phosphoric acid of Wet-process Phosphoric Acid Production, reclaims iodine of the arbitrary claim of claim 1～4, it is characterized in that: concrete way is: the aqueous hydrogen peroxide solution oxygenant that adds 0.05～0.1 kilogram in 100 kilograms of these strong phosphoric acid, reaction, blow out wherein molecular iodine with air, absorb with the acidic solution circulation that contains liquid SO 2 then, when the content of iodine reaches 100～150g/L in the liquid that 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.
6. according to the described a kind of method that reclaims iodine from the strong phosphoric acid of Wet-process Phosphoric Acid Production of claim 5, it is characterized in that: adding the time that the aqueous hydrogen peroxide solution oxygenant carries out oxidizing reaction in the strong phosphoric acid is 5～30 minutes.
7. according to the described a kind of method that reclaims iodine from the strong phosphoric acid of Wet-process Phosphoric Acid Production of claim 5, it is characterized in that: the pH value of absorption liquid is between 1～4.
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Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102502501A (en) * | 2011-10-27 | 2012-06-20 | 瓮福（集团）有限责任公司 | Method for extracting iodine from wet-process phosphoric acid produced from iodine-containing phosphorous ore by semi-water and bi-water method |
| CN102583250A (en) * | 2012-03-19 | 2012-07-18 | 瓮福（集团）有限责任公司 | Device for extracting iodine from wet process phosphate acid liquor |
| CN103011084A (en) * | 2012-12-10 | 2013-04-03 | 瓮福（集团）有限责任公司 | Method for extracting iodine from dehydrate wet method diluted phosphoric acid reaction iodic waste gas |
| CN103011085A (en) * | 2012-12-10 | 2013-04-03 | 瓮福（集团）有限责任公司 | Method for extracting iodine from semi-wet method diluted phosphoric acid reaction iodic waste gas |
| CN103130185A (en) * | 2013-03-21 | 2013-06-05 | 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 |
| CN103172026A (en) * | 2013-04-18 | 2013-06-26 | 瓮福（集团）有限责任公司 | Filtering and heating device for extracting iodine from wet process phosphoric acid and operation method thereof |
| CN103435008A (en) * | 2013-08-16 | 2013-12-11 | 甘肃瓮福化工有限责任公司 | Iodine recovering process for improving iodine recovery rate |
| CN103482574A (en) * | 2013-08-05 | 2014-01-01 | 贵州开磷（集团）有限责任公司 | Recovery method for iodine from wet-process phosphoric acid at low gas-liquid ratio |
| CN105110296A (en) * | 2015-07-21 | 2015-12-02 | 安徽六国化工股份有限公司 | Method used for preparing iodine via recovery of phosphorus ore associated high valence iodine in wet phosphoric acid production |
| CN105129820A (en) * | 2015-07-21 | 2015-12-09 | 安徽六国化工股份有限公司 | Method of recycling phosphorite-associated high-valence iodine from wet-method phosphoric acid production to prepare iodized salt |
| CN105439089A (en) * | 2016-01-11 | 2016-03-30 | 浙江海洲制药有限公司 | Method for recovering iodine from wastewater in medicine production |
| CN108033429A (en) * | 2017-11-17 | 2018-05-15 | 贵阳开磷化肥有限公司 | A kind of method that iodine deep purifying is recycled in phosphoric acid by wet process and fluosilicic acid |
| 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 |
-
2008
- 2008-06-26 CN CNA2008103023546A patent/CN101323434A/en active Pending
Cited By (15)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102502501A (en) * | 2011-10-27 | 2012-06-20 | 瓮福（集团）有限责任公司 | Method for extracting iodine from wet-process phosphoric acid produced from iodine-containing phosphorous ore by semi-water and bi-water method |
| CN102583250A (en) * | 2012-03-19 | 2012-07-18 | 瓮福（集团）有限责任公司 | Device for extracting iodine from wet process phosphate acid liquor |
| CN102583250B (en) * | 2012-03-19 | 2013-09-11 | 瓮福（集团）有限责任公司 | Device for extracting iodine from wet process phosphate acid liquor |
| CN103011085A (en) * | 2012-12-10 | 2013-04-03 | 瓮福（集团）有限责任公司 | Method for extracting iodine from semi-wet method diluted phosphoric acid reaction iodic waste gas |
| CN103011084A (en) * | 2012-12-10 | 2013-04-03 | 瓮福（集团）有限责任公司 | Method for extracting iodine from dehydrate wet method diluted phosphoric acid reaction iodic waste gas |
| CN103130185A (en) * | 2013-03-21 | 2013-06-05 | 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 |
| CN103172026A (en) * | 2013-04-18 | 2013-06-26 | 瓮福（集团）有限责任公司 | Filtering and heating device for extracting iodine from wet process phosphoric acid and operation method thereof |
| CN103482574A (en) * | 2013-08-05 | 2014-01-01 | 贵州开磷（集团）有限责任公司 | Recovery method for iodine from wet-process phosphoric acid at low gas-liquid ratio |
| CN103482574B (en) * | 2013-08-05 | 2015-04-01 | 贵州开磷（集团）有限责任公司 | Recovery method for iodine from wet-process phosphoric acid at low gas-liquid ratio |
| CN103435008A (en) * | 2013-08-16 | 2013-12-11 | 甘肃瓮福化工有限责任公司 | Iodine recovering process for improving iodine recovery rate |
| CN105110296A (en) * | 2015-07-21 | 2015-12-02 | 安徽六国化工股份有限公司 | Method used for preparing iodine via recovery of phosphorus ore associated high valence iodine in wet phosphoric acid production |
| CN105129820A (en) * | 2015-07-21 | 2015-12-09 | 安徽六国化工股份有限公司 | Method of recycling phosphorite-associated high-valence iodine from wet-method phosphoric acid production to prepare iodized salt |
| CN105439089A (en) * | 2016-01-11 | 2016-03-30 | 浙江海洲制药有限公司 | Method for recovering iodine from wastewater in medicine production |
| CN108033429A (en) * | 2017-11-17 | 2018-05-15 | 贵阳开磷化肥有限公司 | A kind of method that iodine deep purifying is recycled in phosphoric acid by wet process and fluosilicic acid |
| 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 |
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