CN101613086A - Utilize the chloride-calcium type oil-field water to extract the method for iodine - Google Patents
Utilize the chloride-calcium type oil-field water to extract the method for iodine Download PDFInfo
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- CN101613086A CN101613086A CN200910117363A CN200910117363A CN101613086A CN 101613086 A CN101613086 A CN 101613086A CN 200910117363 A CN200910117363 A CN 200910117363A CN 200910117363 A CN200910117363 A CN 200910117363A CN 101613086 A CN101613086 A CN 101613086A
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Abstract
The invention provides a kind of air that adopts and blow out method is extracted iodine from the chloride-calcium type oil-field water method, this method earlier with in the chloride-calcium type oil-field water through acidifying, oxide treatment, make iodide ion wherein change into iodine, adopt air to blow out method again and blow out iodine, and contain the airborne iodine of iodine with the alkali lye absorption; The acidified processing of absorption liquid obtains the wet thick product of iodine; The wet thick product of iodine washs after filtration, after the drying, obtains high-quality iodine product.Technology of the present invention is simple relatively, and is easy to operate; Energy consumption is low, and cost is low, has realized the industrialization that oil-field water extracts iodine.
Description
Technical field
The invention belongs to the chemical industry of inorganic salt technical field, relate to a kind of method of utilizing the chloride-calcium type oil-field water to extract iodine, relate in particular to a kind of air that adopts and blow out the method that method is extracted iodine in the chloride-calcium type oil-field water.
Background technology
Iodine is the basic raw material of synthesis of organic substance and inorganic iodide, and the abundance of iodine accounts for 47 in each element, the iodine that occurring in nature does not exist with simple substance form, but exist with iodate, iodide or other chemical combination attitude form.The resource that is rich in iodine is a natural bittern, as China Sichuan from Gongjing halogen (black halogen contain iodine 15.1mg/L), some subsurface brine in Oklahoma, United States An Nadake basin (containing iodine) up to 1.4g/L, Sweet natural gas salt water of Chiba, Japan (contain iodine and reach 2000 times of seawater) etc.Iodine is 0.05ppm in seawater, but some thalassophyte can absorb the iodine in the seawater and build up in vivo.Contain iodide 1.4～1.8% as the ashes after the sea-tangle burning.
At present, divided by outside sodium nitrate and the marine alga system iodine, mainly from bittern, extract iodine abroad.The method of carrying iodine from bittern mainly contains ion-exchange-resin process.Ion-exchange-resin process is because the rate of recovery is not too high, and therefore the content of iodine be not suitable for from the bittern of low levels and extract iodine up to 50ppm in the effluent liquid of absorption back.
The Caidamu Basin, China Zang Bei plateau salt lake resources is abundant, and wherein the iodine reserves are huge, and only the potential resources of Cha Er sweat salt lake iodine just has 0.8 ten thousand tons.The Caidamu Basin also has very huge oil-gas field bittern, contains a large amount of iodine resources, and according to geological survey memoir, the iodine reserves reach 79.56 ten thousand tons.Particularly the Nan Yi mountain oil-field water in the Caidamu Basin is typical chloride-calcium type bittern, carries out the extraction of iodine after concentrating through the natural Exposure to Sunlight in salt pan.The concentration of iodine is 300～335mg/L in the bittern at this moment, and calcium chloride content reaches 30.8～43.0%, and its content and reserves have commercial mining and are worth.
Summary of the invention
The purpose of this invention is to provide and a kind ofly blow out method is extracted iodine from the chloride-calcium type oil-field water method with air.
The present invention utilizes the chloride-calcium type oil-field water to extract the method for iodine, be earlier with in the chloride-calcium type oil-field water through acidifying, oxide treatment, make iodide ion wherein change into iodine; Adopt air to blow out method again and blow out iodine, and absorb with alkali lye; The acidified processing of absorption liquid obtains containing the thick product of iodine of moisture, and the thick product of iodine washs after filtration, after the drying, obtains high-quality iodine product.
Concrete preparation technology is as follows:
(1) acidification: after the chloride-calcium type oil-field water concentrated through the natural Exposure to Sunlight in salt pan, calcium chloride content was 30.8～43.0%, and iodine content is 300～435mg/L.Add concentrated hydrochloric acid in the chloride-calcium type oil-field water after Exposure to Sunlight concentrates, under room temperature, be acidified to PH=1.22～4.23.Its reaction formula is as follows:
IO
-+2H
+→I
-+H
2O
The add-on of concentrated hydrochloric acid is to add industrial concentrated hydrochloric acid 1.50～3.0L in the chloride-calcium type oil-field water after every liter of Exposure to Sunlight concentrates.
(2) oxide treatment: add clorox in the chloride-calcium type oil-field water after acidifying and carry out oxidation, make the iodide ion in the chloride-calcium type oil-field water be converted into elemental iodine.Its reaction formula is as follows:
IO
-+2H
+→I
-+H
2O
The add-on of clorox is: the clorox that adds 2.0～3.0mL in every liter of chloride-calcium type oil-field water; Available chlorine in the clorox 〉=10%.
Because the oxidizing potential of iodine is lower, in oxidising process, be difficult to its current potential of control and by peroxidation.Therefore, for fear of the peroxidation of iodine, oxidizing potential should be strict controlled in 522～535mv.For the ease of the controlled oxidation current potential, can the brine of oil field after the acidifying be oxidizing to oxidizing potential earlier is 833～1023mv, again with unoxidized acidifying after oil-field water mix with 5: 1～2: 1 volume ratio, can obtain the oxidizing potential that needs: 522～535mv.Oxidation ratio reaches 93.7～97.0%.
(3) air blows out iodine: will send into air stripping tower through the chloride-calcium type oil-field water of acidifying, oxide treatment, the temperature in the control air stripping tower is at 40～50 ℃, and air velocity is 0.6～1.5m
3/ h blows out free iodine in the chloride-calcium type oil-field water.The rate that blows out of iodine is 98.2～99.7%.Mother liquor is used to extract bromine.
(4) alkali lye absorbs: that adopts that the NaOH solution absorption air stripping tower of mass concentration 10～15% blows out contains the airborne iodine of iodine.The iodine specific absorption is 92.3～98.9%.
(5) acidification of absorption liquid: the above-mentioned absorption liquid that has absorbed iodine is acidified to PH=1.60～2.5 with concentrated hydrochloric acid, obtains containing the wet thick product of iodine of simple substance of moisture.The eduction rate of iodine is 95.3～98.9%, and the iodine purity in the wet iodine is 79.1～93%, and the iodine yield is 92.3～95.9%.
(6) iodine is refining: will wet the thick product of iodine after filtration, washing after the drying, obtains high-quality iodine product.The purity of iodine is 96.5～99.1%; The yield of iodine is 90～96%.
The present invention compared with prior art has the following advantages:
1, the present invention is a raw material with the chloride-calcium type oil-field water, makes the iodine complete oxidation under acidic conditions that wherein is rich in, and the iodide ion in the oil field is converted into elemental iodine; Adopt air to blow out method and blow out wherein iodine, the yield height of iodine.
2, technology of the present invention is simple relatively, and is easy to operate, and energy consumption is low, and cost is low, realized the industrialization that oil-field water extracts iodine.
Description of drawings
Fig. 1 extracts the process flow sheet of iodine for the present invention
Embodiment
Further specify with air below by specific embodiment and to blow out method is extracted iodine from the chloride-calcium type oil-field water method.
Embodiment 1
(1) acidification: after the chloride-calcium type oil-field water concentrated through the natural Exposure to Sunlight in salt pan, calcium chloride content was 30.8%, and iodine content is 300mg/L.Add concentrated hydrochloric acid in the chloride-calcium type oil-field water after Exposure to Sunlight concentrates, under room temperature, be acidified to PH=1.22.
The add-on of concentrated hydrochloric acid is to add industrial concentrated hydrochloric acid 3.0L in the chloride-calcium type oil-field water after every liter of Exposure to Sunlight concentrates.
(2) oxide treatment: (available chlorine in the clorox 〉=10% adds 2.0～3.0mL) in every liter of chloride-calcium type oil-field water and carries out oxidation to add clorox in the chloride-calcium type oil-field water after acidifying.Free iodide ion oxidation conversion under mild acid conditions is an elemental iodine in the chloride-calcium type oil-field water.
Oxidizing potential should be strict controlled in 522～535mv during oxidation.For the ease of the controlled oxidation current potential, earlier the brine of oil field behind the partial acidification being oxidizing to oxidizing potential is 965mv, and the brine of oil field that adds again after the unoxidized acidifying mixes: add 4.60 liters of unoxidized acidifying oil-field waters in per 10 liters of oxidation liquid.Mixing the rear oxidation current potential is 530mv.The oxidation ratio of iodine is 97.0%.
(3) air blows out iodine: will send into air stripping tower through the chloride-calcium type oil-field water of acidifying, oxide treatment, the temperature in the control air stripping tower is at 40 ℃, and air velocity is 0.6m
3/ h blows out free iodine in the chloride-calcium type oil-field water.The rate that blows out of iodine is 99.7%.Mother liquor is used to extract bromine.
(4) alkali lye absorbs: that adopts that the NaOH solution absorption air stripping tower of mass concentration 10% blows out contains the airborne iodine of iodine.The iodine specific absorption is 98.9%.
(5) acidification of absorption liquid: the above-mentioned absorption liquid that has absorbed iodine is acidified to PH=1.60 with concentrated hydrochloric acid, obtains containing the thick product of iodine of moisture.The eduction rate of iodine is 98.9%, and the iodine purity in the wet iodine is 93.0%, and the iodine yield is 95.9%.
(6) iodine is refining: with the thick product of iodine after filtration, vitriol oil drying is used in washing, and cooling obtains high-quality iodine product.The yield of iodine is more than 96.5%; The purity of iodine is 90%.
Embodiment 2
(1) acidification: after the chloride-calcium type oil-field water concentrated through the natural Exposure to Sunlight in salt pan, calcium chloride content was 40.0%, and iodine content is 320mg/L.Add concentrated hydrochloric acid in the chloride-calcium type oil-field water after Exposure to Sunlight concentrates, under room temperature, be acidified to PH=2.20.
The add-on of concentrated hydrochloric acid is to add industrial concentrated hydrochloric acid 2.20L in the chloride-calcium type oil-field water after every liter of Exposure to Sunlight concentrates.
(2) oxide treatment: (available chlorine in the clorox 〉=10% adds 2.0～3.0mL) in every liter of chloride-calcium type oil-field water and carries out oxidation to add clorox in the chloride-calcium type oil-field water after acidifying.Free iodide ion oxidation conversion under mild acid conditions is an elemental iodine in the chloride-calcium type oil-field water.
Oxidizing potential should be strict controlled in 522～535mv during oxidation.For the ease of the controlled oxidation current potential, earlier the brine of oil field behind the partial acidification being oxidizing to oxidizing potential is 900mv, adds unoxidized acidifying oil-field water again and mixes: add 4 liters of unoxidized acidifying oil-field waters in per 8 liters of oxidation liquid.Mixing the rear oxidation current potential is 522mv.The oxidation ratio of iodine is 93.9%.
(3) air blows out iodine: will send into air stripping tower through the chloride-calcium type oil-field water of acidifying, oxide treatment, the temperature in the control air stripping tower is at 45 ℃, and air velocity is 1.5m
3/ h blows out free iodine in the chloride-calcium type oil-field water.The rate that blows out of iodine is 98.8%.Mother liquor is used to extract bromine.
(4) alkali lye absorbs: that adopts that the NaOH solution absorption air stripping tower of mass concentration 15% blows out contains the airborne iodine of iodine.The iodine specific absorption is 97.8%.
(5) acidification of absorption liquid: the above-mentioned absorption liquid that has absorbed iodine is acidified to PH=2.0 with concentrated hydrochloric acid, obtains containing the thick product of iodine of moisture.The eduction rate of iodine is 96.2%, and the iodine purity in the wet iodine is 82.3%, and the iodine yield is 93.0%.
(6) iodine is refining: with the thick product of iodine after filtration, vitriol oil drying is used in washing, and cooling obtains high-quality iodine product.The yield of iodine is more than 98.3%; The purity of iodine is 94.3%.
Embodiment 3
(1) acidification: after the chloride-calcium type oil-field water concentrated through the natural Exposure to Sunlight in salt pan, calcium chloride content was 43.0%, and iodine content is 335mg/L.Add concentrated hydrochloric acid in the chloride-calcium type oil-field water after Exposure to Sunlight concentrates, under room temperature, be acidified to PH=4.23.
The add-on of concentrated hydrochloric acid is to add industrial concentrated hydrochloric acid 1.50L in the chloride-calcium type oil-field water after every liter of Exposure to Sunlight concentrates.
(2) oxide treatment: (available chlorine in the clorox 〉=10% adds 2.0～3.0mL) in every liter of chloride-calcium type oil-field water and carries out oxidation to add clorox in the chloride-calcium type oil-field water after acidifying.Free iodide ion oxidation conversion under mild acid conditions is an elemental iodine in the chloride-calcium type oil-field water.
Oxidizing potential should be strict controlled in 522～535mv during oxidation.For the ease of the controlled oxidation current potential, earlier the brine of oil field behind the partial acidification being oxidizing to oxidizing potential is 1023mv, adds unoxidized acidifying oil-field water again and mixes: add 0.12 liter of unoxidized acidifying oil-field water in per 0.5 liter of oxidation liquid.Mixing the rear oxidation current potential is 525mv.The oxidation ratio of iodine is 95.0%.
(3) air blows out iodine: will send into air stripping tower through the chloride-calcium type oil-field water of acidifying, oxide treatment, the temperature in the control air stripping tower is at 50 ℃, and air velocity is 1.0m
3/ h blows out free iodine in the chloride-calcium type oil-field water.The rate that blows out of iodine is 98.2%.Mother liquor is used to extract bromine.
(4) alkali lye absorbs: that adopts that the NaOH solution absorption air stripping tower of mass concentration 13% blows out contains the airborne iodine of iodine.The iodine specific absorption is 92.3%.
(5) acidification of absorption liquid: the above-mentioned absorption liquid that has absorbed iodine is acidified to PH=2.5 with concentrated hydrochloric acid, obtains containing the thick product of iodine of moisture.The eduction rate of iodine is 95.3%, and the iodine purity in the wet iodine is 79.1%, and the iodine yield is 92.3%.
(6) iodine is refining: with the thick product of iodine after filtration, vitriol oil drying is used in washing, and cooling obtains high-quality iodine product.The yield of iodine is 99.1%; The purity of iodine is 96.0%.
Claims (8)
1, utilize the chloride-calcium type oil-field water to extract the method for iodine, be earlier with in the chloride-calcium type oil-field water through acidifying, oxide treatment, make iodide ion wherein change into iodine, adopt air to blow out method again and blow out iodine, and absorb with alkali lye; The acidified processing of absorption liquid obtains containing the thick product of iodine of moisture; Thick product washs again after filtration, after the drying, obtains high-quality iodine product.
2, utilize the chloride-calcium type oil-field water to extract the method for iodine according to claim 1, it is characterized in that: the acidification technology of described chloride-calcium type oil-field water is: after the chloride-calcium type oil-field water is concentrated through the natural Exposure to Sunlight in salt pan, add concentrated hydrochloric acid, under room temperature, be acidified to PH=1.22～4.23; The add-on of concentrated hydrochloric acid is: add industrial concentrated hydrochloric acid 1.50～3.0L in the chloride-calcium type oil-field water after every liter of Exposure to Sunlight concentrates.
3, utilize the chloride-calcium type oil-field water to extract the method for iodine according to claim 1, it is characterized in that: described oxidation processing technique is: add clorox in the chloride-calcium type oil-field water after acidifying and carry out oxidation, make the iodide ion in the chloride-calcium type oil-field water be converted into elemental iodine; The controlled oxidation current potential is at 522～535mv.
4, as described in claim 3, utilize the chloride-calcium type oil-field water to extract the method for iodine, it is characterized in that: the available chlorine in the described clorox 〉=10%; The add-on of clorox is: the clorox that adds 2.0～3.0mL in every liter of chloride-calcium type oil-field water.
5, as described in claim 3, utilize the chloride-calcium type oil-field water to extract the method for iodine, it is characterized in that: the control of described oxidizing potential, be that earlier the oil-field water after the acidifying to be oxidizing to oxidizing potential be 833～1023mv, again with unoxidized acidifying after oil-field water mix with 5: 1～2: 1 volume ratio, make oxidizing potential be controlled at 522～535mv.
6, utilize the chloride-calcium type oil-field water to extract the method for iodine according to claim 1, it is characterized in that: described air blows out the technology that method blows out iodine and is: will send into air stripping tower through the chloride-calcium type oil-field water of acidifying, oxide treatment, temperature in the control air stripping tower is at 40～50 ℃, and air velocity is 0.6～1.5m
3/ h blows out free iodine in the chloride-calcium type oil-field water.
7, utilize the chloride-calcium type oil-field water to extract the method for iodine according to claim 1, it is characterized in that: described soda liquor absorption technique is: adopt the NaOH solution absorption of mass concentration 10～15% to contain the airborne iodine of iodine.
8, utilize the chloride-calcium type oil-field water to extract the method for iodine according to claim 1, it is characterized in that: the acidification technology of described absorption liquid is: with concentrated hydrochloric acid absorption liquid is acidified to PH=1.60～2.5, obtains containing the thick product of iodine of moisture.
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|---|---|---|---|
| CN2009101173632A CN101613086B (en) | 2009-07-15 | 2009-07-15 | Method for extracting iodine from chloride-calcium type oil field water |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2009101173632A CN101613086B (en) | 2009-07-15 | 2009-07-15 | Method for extracting iodine from chloride-calcium type oil field water |
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| CN101613086A true CN101613086A (en) | 2009-12-30 |
| CN101613086B CN101613086B (en) | 2011-03-02 |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103950893A (en) * | 2014-05-19 | 2014-07-30 | 山东中氟化工科技有限公司 | Method of recovering and purifying iodine |
| CN108862199A (en) * | 2018-06-28 | 2018-11-23 | 广东先导稀材股份有限公司 | The method of iodine is recycled in the waste liquid of trimethyl gallium containing iodine |
| CN109179329A (en) * | 2018-09-06 | 2019-01-11 | 福建瓮福蓝天氟化工有限公司 | A kind of de- iodine method of phosphoric acid fluosilicic acid as byproduct production anhydrous hydrogen fluoride |
| CN112194204A (en) * | 2020-09-10 | 2021-01-08 | 昆明铂锐金属材料有限公司 | Preparation method of high-purity rhodium triiodide |
-
2009
- 2009-07-15 CN CN2009101173632A patent/CN101613086B/en not_active Expired - Fee Related
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103950893A (en) * | 2014-05-19 | 2014-07-30 | 山东中氟化工科技有限公司 | Method of recovering and purifying iodine |
| CN103950893B (en) * | 2014-05-19 | 2016-05-25 | 山东中氟化工科技有限公司 | A kind of method that reclaims purification iodine |
| CN108862199A (en) * | 2018-06-28 | 2018-11-23 | 广东先导稀材股份有限公司 | The method of iodine is recycled in the waste liquid of trimethyl gallium containing iodine |
| CN109179329A (en) * | 2018-09-06 | 2019-01-11 | 福建瓮福蓝天氟化工有限公司 | A kind of de- iodine method of phosphoric acid fluosilicic acid as byproduct production anhydrous hydrogen fluoride |
| CN109179329B (en) * | 2018-09-06 | 2023-04-07 | 福建瓮福蓝天氟化工有限公司 | Deiodination method for producing anhydrous hydrogen fluoride from phosphoric acid by-product fluosilicic acid |
| CN112194204A (en) * | 2020-09-10 | 2021-01-08 | 昆明铂锐金属材料有限公司 | Preparation method of high-purity rhodium triiodide |
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