CN104961100B - A kind of method that iodine is extracted from Biodine - Google Patents
A kind of method that iodine is extracted from Biodine Download PDFInfo
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Abstract
The present invention discloses a kind of method that iodine is extracted from Biodine, including adjusting the pH of Biodine, adding into Biodine oxidizing certain time, extractant is added to the solution after oxidation, heat and stirs certain time, organic phase washing process after back washing agent back extraction, back extraction is added into load organic phases, aqueous phase acidifying separates out thick iodine after back extraction.The present invention uses oxidation-extraction method, with extraction yield is high, equipment is simple, consume energy low advantage.The extraction yield of iodine reaches more than 93%, and extractant can be with Reusability.
Description
Technical field
The present invention relates to the environmental protective chemical industry technical field for extracting iodine.Extracted more particularly, to one kind from Biodine
The method of iodine.
Background technology
Iodine is important strategic materials, is widely used in terms of national defence, industrial or agricultural, health care.With economical fast
Speed development, China greatly increases to the demand of iodine, and due to being limited by iodine resource and recovery technology, China's iodine total output is relatively low,
And production cost is higher, it is required for every year from a large amount of iodine of external import.Iodine is distributed all over the world, but developable iodine is provided
Source is seldom.The gross reserves of iodine is very big in ocean, up to 70,000,000,000 tons.The main source that China's industry carries iodine has sea-tangle blanching solution, sea
Band leaching liquid, subsurface brine, phosphorus ore factory water containing iodine etc., putting forward the main technique of iodine has Air blowing method and ion-exchange-resin process.
The A of CN 102515106 disclose " method that iodine is extracted from the fresh sea-tangle blanching waste water " method and first use technical hydrochloric acid
The pH of blanching waste water is adjusted to 0.5~3.0, excessive oxidant natrium nitrosum or sodium hypochlorite is then added, by iodide ion
Free-iodine is oxidized to, then uses gas-liquid volume ratio to be 300~100 at room temperature:1 Air blowing iodine, with sodium hydroxide or Asia
Sodium sulphate absorbs the iodine of blowout, then to absorbing liquid acidification, separates out iodine, the extraction rate reached of iodine to 80%.The method it is excellent
Point be using fresh sea-tangle blanching waste water temperature it is high the characteristics of solve conventional air blow out method heating problems, reduce technique into
This.But iodide ion peroxide can be melted into iodate ion by the oxidizing agent sodium hypochlorite that the method is used, so as to reduce yield；Air
Some other impurity can be also carried secretly during blowout iodine, made troubles to subsequent technique；Requirement of the Air blowing method to equipment
The use of height, such as desorber and maintenance.
The A of CN 103072947 disclose a kind of " method from the Extracting Iodine from Kelp " method using kelp-soaking liquid as raw material,
First pass around three air-flotation process and obtain clear liquid, then add sulfuric acid adjust clear liquid pH to 1~2, add oxidant iodine from
Son is oxidized to free-iodine, is then adsorbed by basic anionic resin, and sodium sulfite solution desorption, stripping liquid acidifying separates out iodine.
The advantage of the method is that after three air-flotation process and resin adsorption, obtained iodine is impure less.But the method complex steps, tree
Fat is vulnerable to other impurities interference.
The A of CN 101318623 disclose " method that iodine is extracted from subsurface brine containing the iodine " method first by subsurface brine
PH adjust to 2~3, iodide ion is oxidized to free-iodine by composite oxidant, blows out free-iodine with 60~70 DEG C of hot-airs, so
Sulfur dioxide acid solution cyclic absorption is used afterwards, is added 0.5~3kg/100kg hydrogen peroxide, is separated out iodine.The advantage of the hair is
Using composite oxidant, the consumption of oxidant is reduced.But the method blows out iodine using hot-air, energy expenditure is larger.
The A of CN 101638220 disclose " method that iodine is extracted from rock phosphate in powder containing the iodine " method directly in phosphoric acid delivery pipe
Oxidant is added on line, and extracting gas uses angential admission mode, diluted acid is produced eddy flow, selects bubble type sieve plate, makes extraction
Gas and diluted acid are fully contacted.The advantage of the method is that oxidant is directly added on diluted acid feed-line, reduces oxidization time；Use
Extracting gas bubble type is extracted, and contact is abundant.But the sieve plate that the method is used easily is blocked by impurity, the parallel-adder settle-out time of extraction tower compared with
It is short.
The content of the invention
It is an object of the present invention to provide a kind of method that iodine is extracted from Biodine, this method has technique letter
Single, energy consumption is low, and the rate of recovery is high and is adapted to industrial mass production.
To reach above-mentioned purpose, the present invention uses following technical proposals：
A kind of method that iodine is extracted from Biodine, this method comprises the following steps：
1) Biodine is acidified, then aoxidized；
2) to step 1) oxidation after mixed liquor carry out extracting operation；
3) to step 2) obtain containing iodine extraction organic phase carry out back extraction extract operation；
4) by step 3) acidifying of obtained strip liquor separates out iodine, and suction filtration obtains thick iodine.
It is above-mentioned from Biodine extract iodine method, step 1) Biodine include sea-tangle blanching solution, sea-tangle extract
Take liquid, subsurface brine containing iodine or phosphorus ore factory water containing iodine；Content of iodine in the Biodine is 60-2000mg/L.
The above-mentioned method that iodine is extracted from Biodine, step 1) pH value of Biodine is is adjusted to 1- by the acidifying
5；Acid used in the acidifying is sulfuric acid or hydrochloric acid.
The above-mentioned method that iodine is extracted from Biodine, step 1) described in the oxidant of oxidation be selected from natrium nitrosum, double
Oxygen water or sodium chlorate；The consumption of the Biodine Sodium Nitrite is 0.05-5.0g/L, and the consumption of hydrogen peroxide is 0.15-
20ml/L, the consumption of sodium chlorate is 0.018-2.3g/L；The mass percent concentration of the hydrogen peroxide is 3.0-40%.
It is above-mentioned from Biodine extract iodine method, step 2) extracting operation extractant be selected from mineral oil, coal
One or more in oil, carbon tetrachloride, n-octyl alcohol, isooctanol and ten carbon alcohol.
It is above-mentioned from Biodine extract iodine method, step 2) described in extracting operation by organic phase compared with aqueous phase
【Heretofore described compares the volume ratio for each meaning organic phase and aqueous phase, no longer indicates one by one】For 1:10-10:1 ratio
Add extractant.
The above-mentioned method that iodine is extracted from Biodine, step 2) described in extracting operation include counter-current extraction or cross-flow and extract
Take；The temperature of the counter-current extraction operation is 10-90 DEG C, and rotating speed is that 50-1000 turns/min, and mixing time is 0-120min.
It is above-mentioned from Biodine extract iodine method, step 3) described in back extraction extract operation strippant be hydroxide
Sodium solution, the mass percent concentration of the sodium hydroxide solution is 1.5-40%；It is stripped to the purplish red decoloration of organic phase.
It is above-mentioned from Biodine extract iodine method, step 3) described in back extraction extract operation temperature be 10-90 DEG C, instead
What is extracted is in a ratio of 200:1-1:200, the back extraction takes mode, the cross-flow back extraction using cross-flow back extraction or countercurrent reextraction
The number of times taken is 5-10 times, and the mixing speed of cross-flow back extraction turns/min for 50-1000, and the time of cross-flow back extraction is 0-
120min.The mixing speed that countercurrent reextraction takes is that 50-1000 turns/min, and the time that countercurrent reextraction takes is 0-120min, back extraction
Series is 1 grade to 10 grades.
The above-mentioned method that iodine is extracted from Biodine, in step 4) also include organic phase regeneration step afterwards：Regeneration has
Machine is with compared to 10:1-1:10, after 1-10 grades are washed, the pH value of the aqueous solution is 7, and organic phase is reusable.
Beneficial effects of the present invention are as follows：
The present invention uses oxidation-extraction technique, and free-iodine is extracted to organic phase from aqueous phase using organic extractant, richness is reached
The purpose of collection, extraction process only has a small amount of impurity entrainment；And this process equipment is simple, energy consumption is low, the iodine rate of recovery high, fit
Close industrial mass production.The extraction yield of the iodine of described extracting operation is 93-98%
Embodiment
In order to illustrate more clearly of the present invention, with reference to preferred embodiment, the present invention is described further.Ability
Field technique personnel should be appreciated that following specifically described content is illustrative and be not restrictive, and this should not be limited with this
The protection domain of invention.
Embodiment 1【Heretofore described compares the volume ratio for each meaning organic phase and aqueous phase, no longer indicates one by one】
A kind of method that iodine is extracted from Biodine, the Biodine is iodine in sea-tangle blanching solution, sea-tangle blanching solution
Content is 704mg/L；Its pH is adjusted with 30wt% technical hydrochloric acid to 1.0,1L sea-tangle blanching solutions is taken, 0.45g is added thereto
Natrium nitrosum, is aoxidized 4 hours；Then press and compare 2:1 adds 2L mineral oil into reaction solution, is heated to 30 DEG C, mixing speed is
400 turns/min, extraction time 30min, one-level extraction yield is 89.5% after testing；With compared to 200:1 contains iodine extraction to what is obtained
Liquid adds 15wt% sodium hydroxide solutions, then carries out back extraction behaviour under conditions of 30 DEG C, mixing speed are 400 turns/min
Make, be stripped 20min, back extraction mode is stripped for cross-flow, back extraction number of times is 5 times, be stripped to the purplish red decoloration of organic phase；After back extraction
Organic phase at normal temperatures with 10:1 is compared, and organic phase can be reused after 2 grades are washed, the analysis of strip liquor acidification
Go out iodine, suction filtration obtains thick iodine 598.58mg, and the total recovery of iodine is 85%.
Embodiment 2
A kind of method that iodine is extracted from Biodine, the Biodine is content of iodine in sea-tangle blanching solution, the solution
For 704mg/L, its pH is adjusted with 30wt% technical hydrochloric acid to 1.0, the 1L solution is taken, 0.48g natrium nitrosums are added thereto,
Oxidation 3 hours；Then press and compare 1:1 adds 1L mineral oil into reaction solution, is heated to 40 DEG C, mixing speed is 500 turns/min,
Extraction time 30min, one-level extraction yield is 86.1% after testing；With compared to 200:1 adds to obtained extract containing iodine
18wt% sodium hydroxide solutions, then carry out back extraction extract operation, back extraction under conditions of 40 DEG C, mixing speed are 300 turns/min
15min, back extraction mode is countercurrent reextraction, and back extraction series is 8 times, is stripped to the purplish red decoloration of organic phase；It is organic after back extraction
Mutually at normal temperatures with 12:1 is compared, and organic phase can be reused after 3 grades are washed, and strip liquor acidification separates out iodine,
Suction filtration obtains thick iodine 594.0mg, and the total recovery of iodine is 84.37%.
Embodiment 3
A kind of method that iodine is extracted from Biodine, the Biodine is content of iodine in sea-tangle blanching solution, the solution
For 704mg/L, its pH is adjusted with 40wt% technical hydrochloric acid to 1.5, the 1L solution is taken, 0.48g natrium nitrosums are added thereto,
Oxidation 4 hours；Then press and compare 1:3 add 333mL mineral oil into reaction solution, are heated to 45 DEG C, and mixing speed is 300 turns/
Min, extraction time 40min, the extraction yield of six stage countercurrents extraction is 98.4%；With compared to 22.2:1 to obtained extract containing iodine
Middle addition 18wt% sodium hydroxide solutions, then carry out back extraction behaviour under conditions of 45 DEG C, mixing speed are 500 turns/min
Make, be stripped 15min, back extraction mode is stripped for cross-flow, back extraction number of times is 5 times, be stripped to the purplish red decoloration of organic phase；After back extraction
Organic phase at normal temperatures with 13:1 is compared, and organic phase can be reused after 3 grades are washed, the analysis of strip liquor acidification
Go out iodine, suction filtration obtains thick iodine 678.88mg, and the total recovery of iodine is 96.4%.
Embodiment 4
A kind of method that iodine is extracted from Biodine, the Biodine is sea-tangle blanching solution, the material liquid amount of iodine
For 704mg/L, its pH is adjusted with 40wt% technical hydrochloric acid to 2.0, the 1L material liquids are taken, and adds 30wt% dioxygens thereto
Water 2.0mL, is aoxidized 4 hours；Then press and compare 1:1 adds 1L mineral oil into reaction solution, is heated to 35 DEG C, mixing speed is
350 turns/min, extraction time 20min, one-level extraction yield is 89.6% after testing；With compared to 67:1 to obtained extract containing iodine
Middle addition 15wt% sodium hydroxide solutions, then carry out back extraction extract operation in 40 DEG C, mixing speed for 350 turns/min condition,
20min is stripped, back extraction mode is stripped for cross-flow, back extraction number of times is 10 times, be stripped to the purplish red decoloration of organic phase；After back extraction
Organic phase is at normal temperatures with 15:1 is compared, and organic phase can be reused after 4 grades are washed, and strip liquor acidification is separated out
Iodine, suction filtration obtains thick iodine 618.2mg, and the total recovery of iodine is 87.8%.
Embodiment 5
A kind of method that iodine is extracted from Biodine, the Biodine is sea-tangle blanching solution, the material liquid amount of iodine
For 704mg/L, its pH is adjusted with 40wt% industrial sulphuric acid to 2.5, the 1L material liquids are taken, and adds 0.2g chloric acid thereto
Sodium, is aoxidized 5 hours；Then press and compare 1:4 add 250mL mineral oil into reaction solution, are heated to 45 DEG C, mixing speed is 250
Turn/min, extraction time 40min, the extraction yield of six grades of cross current solvent extractions is 95.4%；With compared to 25:1 contains iodine extraction to what is obtained
20wt% sodium hydroxide solutions are added in liquid, then back extraction behaviour are carried out under conditions of 45 DEG C, mixing speed are 500 turns/min
Make, be stripped 15min, back extraction mode is stripped for cross-flow, back extraction number of times is 8 times, be stripped to the purplish red decoloration of organic phase；After back extraction
Organic phase at normal temperatures with 15:1 is compared, and organic phase can be reused after 3 grades are washed, the analysis of strip liquor acidification
Go out iodine, suction filtration obtains thick iodine 658.2mg, and the total recovery of iodine is 93.45%.
Embodiment 6
A kind of method that iodine is extracted from Biodine, the Biodine is sea-tangle blanching solution, the material liquid amount of iodine
For 704mg/L, its pH is adjusted with 30wt% technical hydrochloric acid to 2.0, the 1L material liquids are taken, and adds 0.5g nitrous acid thereto
Sodium, is aoxidized 4 hours；Then press and compare 1:1 adds 1L kerosene into reaction solution, is heated to 50 DEG C, and mixing speed is 300 turns/
Min, extraction time 40min, one-level extraction yield is 85.7% after testing；With compared to 67:1 adds into obtained extract containing iodine
15wt% sodium hydroxide solutions, then carry out back extraction operation, back extraction under conditions of 50 DEG C, mixing speed are 450 turns/min
25min, back extraction mode is stripped for cross-flow, and back extraction number of times is 5 times, is stripped to the purplish red decoloration of organic phase；It is organic after back extraction
Mutually at normal temperatures with 13:1 is compared, and organic phase can be reused after 3 grades are washed, and strip liquor acidification separates out iodine,
Suction filtration obtains thick iodine 591.3mg, and the total recovery of iodine is 84.0%.
Embodiment 7
A kind of method that iodine is extracted from Biodine, the Biodine is sea-tangle blanching solution, the material liquid amount of iodine
For 704mg/L, its pH is adjusted with 40wt% technical hydrochloric acid to 2.5, the 1L material liquids are taken, and adds 30wt% dioxygens thereto
Water 2.0mL, is aoxidized 4 hours；Then press and compare 1:2 add 500mL kerosene into reaction solution, are heated to 45 DEG C, mixing speed is
450 turns/min, extraction time 30min, one-level extraction yield is 81.6% after testing；With compared to 50:1 to obtained extract containing iodine
Middle addition 20wt% sodium hydroxide solutions, then carry out back extraction operation under conditions of 45 DEG C, mixing speed are 550 turns/min,
30min is stripped, back extraction mode is stripped for cross-flow, back extraction number of times is 5 times, be stripped to the purplish red decoloration of organic phase；After back extraction
Organic phase is at normal temperatures with 13:1 is compared, and organic phase can be reused after 2 grades are washed, and strip liquor acidification is separated out
Iodine, suction filtration obtains thick iodine 563.0mg, and the total recovery of iodine is 80.0%.
Embodiment 8
A kind of method that iodine is extracted from Biodine, the Biodine is sea-tangle leaching liquid, the material liquid amount of iodine
For 704mg/L, its pH is adjusted with 30wt% technical hydrochloric acid to 3.0, the 1L material liquids are taken, and adds 0.45g nitrous thereto
Sour sodium, is aoxidized 4 hours；Then press and compare 1:1 adds 1L carbon tetrachloride into reaction solution, is heated to 45 DEG C, mixing speed is 500
Turn/min, extraction time 30min, one-level extraction yield is 87.5% after testing；With compared to 67:1 into obtained extract containing iodine
15wt% sodium hydroxide solutions are added, then back extraction operation are carried out under conditions of 45 DEG C, mixing speed are 500 turns/min, instead
Extract 20min, back extraction mode is stripped for cross-flow, back extraction number of times is 8 times, be stripped to the purplish red decoloration of organic phase；Having after back extraction
Machine is mutually at normal temperatures with 15:1 is compared, and organic phase can be reused after 3 grades are washed, and strip liquor acidification is separated out
Iodine, suction filtration obtains thick iodine, 603.68mg, the total recovery 85.8% of iodine.
Embodiment 9
A kind of method that iodine is extracted from Biodine, the Biodine is subsurface brine containing iodine, and the material liquid contains iodine
Measure as 704mg/L, its pH is adjusted with 30wt% industrial sulphuric acid to 3.5, take the 1L material liquids, and add 0.23g chlorine thereto
Sour sodium, is aoxidized 4 hours；Then press and compare 1:2 add 500mL n-octyl alcohols, are heated to 40 DEG C, mixing speed is 500 turns/min, extraction
Time 30min is taken, one-level extraction yield is 83.7% after testing；18wt% sodium hydroxides are added into obtained extract containing iodine molten
Liquid, is in a ratio of 50 to 1, then carries out back extraction extract operation, back extraction under conditions of 40 DEG C, mixing speed are 600 turns/min
18min, back extraction mode is stripped for cross-flow, and back extraction number of times is 10 times, is stripped to the purplish red decoloration of organic phase；It is organic after back extraction
Mutually at normal temperatures with 12:1 is compared, and organic phase can be reused after 3 grades are washed, and strip liquor acidification separates out iodine,
Suction filtration obtains thick iodine, 577.46mg, the total recovery 82% of iodine.
Embodiment 10
A kind of method that iodine is extracted from Biodine, the Biodine is sea-tangle blanching solution, the material liquid amount of iodine
For 704mg/L, its pH is adjusted with 30wt% industrial sulphuric acid to 2.0, the 1L material liquids are taken, and adds 0.5g nitrous acid thereto
Sodium, is aoxidized 4 hours；Then press and compare 1:1 adds 1L isooctanol, is heated to 45 DEG C, mixing speed is 600 turns/min, during extraction
Between 40min, after testing one-level extraction yield be 86.6%；15wt% sodium hydroxide solutions are added into obtained extract containing iodine,
100 to 1 are in a ratio of, then back extraction extract operation is carried out under conditions of 45 DEG C, mixing speed are 350 turns/min, is stripped 10min,
Back extraction mode is stripped for cross-flow, and back extraction number of times is 5 times, is stripped to the purplish red decoloration of organic phase；Organic phase after back extraction is normal
With 12 under temperature:1 is compared, and organic phase can be reused after 2 grades are washed, and strip liquor acidification separates out iodine, and suction filtration is obtained
To thick iodine 597.5mg, the total recovery 85% of iodine.
Embodiment 11
A kind of method that iodine is extracted from Biodine, the Biodine is sea-tangle blanching solution, the material liquid amount of iodine
For 704mg/L, its pH is adjusted with 40wt% industrial sulphuric acid to 2.0, the 1L material liquids are taken, and adds 0.5g nitrous acid thereto
Sodium, is aoxidized 4 hours；Then press and compare 1:2 add the carbon alcohol of 500mL ten into reaction solution, are heated to 45 DEG C, mixing speed is 480
Turn/min, extraction time 40min, one-level extraction yield is 82.4% after testing；15wt% is added into obtained extract containing iodine
Sodium hydroxide solution, is in a ratio of 50 to 1, then carries out back extraction behaviour under conditions of 45 DEG C, mixing speed are 400 turns/min
Make, be stripped 25min, back extraction mode is stripped for cross-flow, back extraction number of times is 5 times, be stripped to the purplish red decoloration of organic phase；After back extraction
Organic phase at normal temperatures with 12:1 is compared, and organic phase can be reused after 2 grades are washed, the analysis of strip liquor acidification
Go out iodine, suction filtration obtains thick iodine 568.5mg, and the total recovery of iodine is 81%.
Embodiment 12
A kind of method that iodine is extracted from Biodine, the Biodine is sea-tangle blanching solution, the material liquid amount of iodine
For 704mg/L, its pH is adjusted with 30wt% industrial sulphuric acid to 3.5, the 1L material liquids are taken, and adds 0.23g chloric acid thereto
Sodium, is aoxidized 4 hours；Then press and compare 1:1 adds mixture (mineral oil and the n-octyl alcohol volume ratio 2 of 1L mineral oil and n-octyl alcohol:
1) 40 DEG C, are heated to, mixing speed is 500 turns/min, extraction time 30min, and one-level extraction yield is 93.7% after testing；With phase
Than 50:1 into obtained extract containing iodine add 18wt% sodium hydroxide solutions, then 40 DEG C, mixing speed be 600 turns/
Back extraction extract operation is carried out under conditions of min, 18min is stripped, back extraction mode is stripped for cross-flow, back extraction number of times is 10 times, and back extraction is extremely
The purplish red decoloration of organic phase；Organic phase after back extraction is at normal temperatures with 12:1 compares, and organic phase can be with after 3 grades wash
Recycling, strip liquor acidification separates out iodine, and suction filtration obtains thick iodine 598.4mg, and the total recovery of iodine is 85%.
Embodiment 13
A kind of method that iodine is extracted from Biodine, the Biodine is sea-tangle blanching solution, the material liquid amount of iodine
For 704mg/L, its pH is adjusted with 30wt% industrial sulphuric acid to 2.0, the 1L material liquids are taken, and adds 0.5g nitrous acid thereto
Sodium, is aoxidized 4 hours；Then press and compare 1:1 mixture for adding 1L mineral oil, n-octyl alcohol and isooctanol (mineral oil, n-octyl alcohol and
Isooctanol volume ratio 1.5:1:1) 45 DEG C, are heated to, mixing speed is 600 turns/min, extraction time 40min, after testing one-level
Extraction yield is 90.6%；With compared to 100:1 adds 15wt% sodium hydroxide solutions into obtained extract containing iodine, then 45
DEG C, mixing speed be 350 turns/min under conditions of carry out back extraction extract operation, be stripped 10min, back extraction mode be cross-flow back extraction, instead
It is 5 times to extract number of times, is stripped to the purplish red decoloration of organic phase；Organic phase after back extraction is at normal temperatures with 12:1 compares, by 2
Organic phase can be reused after level washing, and strip liquor acidification separates out iodine, and suction filtration obtains thick iodine 640.64mg, total receipts of iodine
Rate is 91%.
Obviously, the above embodiment of the present invention is only intended to clearly illustrate example of the present invention, and is not pair
The restriction of embodiments of the present invention, for those of ordinary skill in the field, may be used also on the basis of the above description
To make other changes in different forms, all embodiments can not be exhaustive here, it is every to belong to this hair
Row of the obvious changes or variations that bright technical scheme is extended out still in protection scope of the present invention.
Claims (4)
1. a kind of method that iodine is extracted from Biodine, it is characterised in that this method comprises the following steps：
1) Biodine is acidified, then aoxidized；The Biodine includes sea-tangle blanching solution, sea-tangle extract, underground containing iodine
Bittern or phosphorus ore factory water containing iodine；Content of iodine in the Biodine is 60-2000mg/L；
2) to step 1) mixed liquor after oxidation carries out extracting operation, and the extractant of the extracting operation is mineral oil and n-octyl alcohol
Mixture, the volume ratio of mixture mineral oil in fluid and n-octyl alcohol is 2:1；Described extracting operation presses the phase of organic phase and aqueous phase
Than for 1:10-10:1 ratio adds extractant；Described extracting operation includes counter-current extraction or cross current solvent extraction；The adverse current extraction
The temperature of extract operation is 10-90 DEG C, and rotating speed is that 50-1000 turns/min, and mixing time is 0-120min；
3) to step 2) obtain containing iodine extraction organic phase carry out back extraction extract operation；The strippant of described back extraction extract operation is
Sodium hydroxide solution, the mass percent concentration of the sodium hydroxide solution is 1.5-40%；It is stripped to the aubergine of organic phase
Disappear；The temperature of described back extraction extract operation is 10-90 DEG C, and back extraction is in a ratio of 200:1-1:200, the back extraction is used
Cross-flow back extraction or countercurrent reextraction take mode, and the number of times of the cross-flow back extraction is 5-10 times, the mixing speed of cross-flow back extraction
For 50-1000 turn/min, cross-flow back extraction time be 0-120min, the mixing speed that countercurrent reextraction takes be 50-1000 turn/
Min, the time that countercurrent reextraction takes is 0-120min, and back extraction series is 1 grade to 10 grades；
4) by step 3) acidifying of obtained strip liquor separates out iodine, and suction filtration obtains thick iodine.
2. according to the method described in claim 1, it is characterised in that：Step 1) acidifying is to adjust the pH value of Biodine
For 1-5；Acid used in the acidifying is sulfuric acid or hydrochloric acid.
3. according to the method described in claim 1, it is characterised in that：Step 1) described in oxidation oxidant be selected from nitrous acid
Sodium, hydrogen peroxide or sodium chlorate；The consumption of the Biodine Sodium Nitrite is 0.05-5.0g/L, and the consumption of hydrogen peroxide is
0.15-20ml/L, the consumption of sodium chlorate is 0.018-2.3g/L；The mass percent concentration of the hydrogen peroxide is 3.0-40%.
4. according to the method described in claim 1, it is characterised in that：In step 4) also include organic phase regeneration step afterwards：Again
Raw organic phase is with compared to 10:1-1:10, after 1-10 grades are washed, the pH value of the aqueous solution is 7, and organic phase is reusable.
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| CN112028020B (en) * | 2020-09-02 | 2021-06-22 | 山东博苑医药化学股份有限公司 | Process for recovering iodine from iodine bromide-containing medical organic waste liquid |
| CN114715848B (en) * | 2021-01-04 | 2023-09-12 | 中国科学院江西稀土研究院 | Method for recovering iodine from iodine-containing solution |
| CN113865947B (en) * | 2021-08-20 | 2024-05-14 | 中国原子能科学研究院 | Online sampling device and method for low-concentration molecular iodine in gas circulation loop |
| CN115724403A (en) * | 2022-11-22 | 2023-03-03 | 浙江巨化技术中心有限公司 | Method for recovering iodine from iodine-containing flue gas absorption liquid |
| CN115676778A (en) * | 2022-11-24 | 2023-02-03 | 中船(邯郸)派瑞特种气体股份有限公司 | Method for preparing iodine chloride by using iodine waste liquid |
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| 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 |
| CN103508420A (en) * | 2013-09-29 | 2014-01-15 | 辽宁师范大学 | Method for recovering iodine from iodine-contained waste liquid in laboratory |
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