CN108033429A - A kind of method that iodine deep purifying is recycled in phosphoric acid by wet process and fluosilicic acid - Google Patents
A kind of method that iodine deep purifying is recycled in phosphoric acid by wet process and fluosilicic acid Download PDFInfo
- Publication number
- CN108033429A CN108033429A CN201711144902.2A CN201711144902A CN108033429A CN 108033429 A CN108033429 A CN 108033429A CN 201711144902 A CN201711144902 A CN 201711144902A CN 108033429 A CN108033429 A CN 108033429A
- Authority
- CN
- China
- Prior art keywords
- iodine
- phosphoric acid
- acid
- recycled
- wet process
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B7/00—Halogens; Halogen acids
- C01B7/13—Iodine; Hydrogen iodide
- C01B7/14—Iodine
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
- C01P2006/82—Compositional purity water content
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
Abstract
The invention discloses a kind of method that iodine deep purifying is recycled in phosphoric acid by wet process and fluosilicic acid, with H2O2As oxidant, iodide ion in phosphoric acid by wet process and fluosilicic acid is oxidized to iodine molecule, air extraction is used to blow away iodine molecule with gas phase, iodine molecule is again through reducing agent circulation washing absorption enrichment in gas phase, iodine purification is carried out after iodide ion concentration reaches 10 50g/L in absorbing liquid, deep purifying, which is included in absorbing liquid, adds calcium carbonate, carry out first order purification, aluminium salt is added, carries out secondary purification, adds hydrogen peroxide, iodine is separated out by oxidation, filtering, is purified again with the concentrated sulfuric acid, filters and fine work iodine is made.The method of the present invention makes iodine resource fully be recycled, and avoids the wasting of resources, and obtained iodine has purity high, and impurity is few, has good economic benefit.
Description
Technical field
The invention belongs to iodine Recovery Purifying field, and in particular to iodine deep purifying is recycled in a kind of phosphoric acid by wet process and fluosilicic acid
Method.
Background technology
Iodine is known as biological element, wisdom element, is plant and the indispensable element of growth in humans, be manufacture it is inorganic or
The primary raw material of organic iodide, and the good catalyst of many chemical reactions.Iodate chemical product is widely used in food, doctor
All conglomeraties such as medicine, dyestuff, metallurgy, synthetic rubber, agricultural, national defence hard-core technology.The demand of global iodine is increasingly powerful.Iodine is dilute
Resource is lacked, iodine ore resources in the world mainly have sodium nitrate, seaweed and subsurface brine.The iodine ore resources utilized with easily exploiting
Increasingly depleted, the price of iodine are constantly soaring.Currently, the production capacity of global iodine is about 20kt/a, and the main place of production concentrates on Japan, Chile
And the U.S..The materials in short supply that iodine has price but no buyers in the international market.The downstream product of iodine is mostly high value added product.Acid iodide
The profit of other iodine products such as potassium, iodoform, iodate rhodium, povidone iodine and high poly- iodine is high.The production capacity of China's iodine is about 800t/a,
The consumption of iodine is about 3000t/a, and with annual 5% speed increase.China is iodine deficiency state, relies primarily on and iodine is carried in seawater
With import iodine.
Currently, the production method of iodine mainly has ion-exchange, active carbon adsorption, solvent signal suppression, the precipitation method (copper method
With silver-colored method), organic solvent extractionprocess, special catalytic oxidation and air extraction etc..Traditional iodine production method is to raw material
Amount of iodine is more demanding, and economic benefit is poor.Currently, in addition to Chile carries iodine from ore containing iodine, external most countries are equal
Rely primarily on seawater and carry iodine.The research of phosphorus ore association iodine resource reclaim technology rarely has play-by-play.The ground such as river Hubei Province, China Yunnan-Guizhou
The oxide of iodine, iodine rich reserves are associated with rock phosphate in powder.Guizhou Province's phosphate rock resource ranks first in the whole country, proven reserve 27
Hundred million tons, prospective reserves over ten billion ton, the oxide of iodine is associated with rock phosphate in powder, average amount of iodine is in 19-76mg/kg.Wherein phosphorus
The reserves of ore association iodine utilize reserves to be temporarily difficult in block rock.Open the average grade of ore association iodine in phosphorylcholine group rock phosphate in powder only about in Guizhou
40mg/kg, belongs to ultralow grade iodine resource, and recovery technology difficulty is larger.
By handling phosphoric acid workshop phosphoric acid,diluted containing iodine and fluosilicic acid containing iodine, the ultralow grade of phosphorus ore association is effectively recycled
Iodine resource, avoids the unordered discharge of iodine, while achievees the purpose that exhaust gas, waste water comprehensive management of environmental protection.But iodine recycling skill before this
Art is only limitted to produce thick iodine, and impurity content is higher in product, cannot be used directly for the medical production of intermediate containing iodine of food.At present,
Thick iodine deep purifying need to be by sublimed method, fusion method etc., and complex production process, cost are higher, and iodine loss is larger.
The content of the invention
The present invention is directed to problems of the prior art, is recycled in phosphoric acid by wet process and fluosilicic acid in iodine containing a large amount of fluorinations
The impurity such as thing, phosphate and ardealite, cannot be used directly for the medical production of intermediate containing iodine of food, directly restrict iodine product effect
Benefit.Before this, thick iodine deep purifying need to be by sublimed method, fusion method etc., and complex production process, cost are higher, and iodine loss is larger.
The present invention provides a kind of method of thick iodine deep purifying, iodine resource is fully recycled, avoid the wasting of resources, have extensive
And positive economic benefit and social benefit.
The method that iodine deep purifying is recycled in a kind of phosphoric acid by wet process and fluosilicic acid that the present invention uses, with H2O2As oxidation
Agent, iodine molecule is oxidized to by iodide ion in phosphoric acid by wet process, then uses air extraction to blow out iodine molecule with gas phase, then by gas phase
Middle iodine molecule through reducing agent circulation washing absorption enrichment, carries out iodine depth after iodide ion concentration reaches 10-50g/L in absorbing liquid again
Degree purification obtains iodine product, and deep purifying comprises the following steps：
(1) calcium carbonate is added in absorbing liquid, is stirred, carries out first order purification；
(2) aluminium salt is added in the clear liquid of first class purification, be stirred, carry out secondary purification；
(3) hydrogen peroxide is added in the clear liquid of secondary purification, when the oxidizing potential of solution reaches 540mV, iodine is analysed by oxidation
Go out, filter；
(4) iodine made from filtering is purified again with the concentrated sulfuric acid, filters and fine work iodine is made.
Calcium carbonate addition is the 110% of theoretical addition amount in step (1), and reaction temperature is 35 DEG C, and the reaction time is
30min。
In step (2)：Aluminium salt is alum, the one or more in aluminium chloride, aluminum sulfate, aluminium polychloride.
Aluminium salt addition is the 105% of theoretical addition amount in step (2), and reaction temperature is 35 DEG C, and the reaction time is
50min。
The temperature that iodine is purified again with the concentrated sulfuric acid in step (4) is 150 DEG C.
The upper clear supernate after the turbid standing of bottom after first class purification and secondary purification, and iodine is by the filter after oxidation precipitation
Liquid, can add in absorbing liquid and recycle.
The technical principle and technique effect of present invention in-depth purification：For fluorine-containing higher iodine absorbing liquid, fluorine is mainly with F-
Form exists, and calcium salt is added into iodine absorbing liquid and utilizes F-With Ca2+The CaF of reaction generation indissoluble2Precipitate and reach the mesh of fluorine removal
's.Its reaction is as follows：
Ca2++2F-=CaF2↓
But CaF2Solubility at 18 DEG C in water is 16.3mg/L, is 7.9mg/L by fluorine ionometer, simultaneously as
The CaF of generation2It is a kind of very trickle crystal, CaF is formed after being 10-20mg/L when the residual quantity of fluorine2The speed of sediment is just
It can slow down, therefore, fluoride is difficult up to standard in iodine absorbing liquid after being handled under room temperature, needs further depth defluorinate processing.
On the basis of calcium salt defluorinate, the addition of aluminium salt can make Al3+With F-Complexing generation hydroxyl fluorination aluminium compound and
Aluminium salt hydrolyzes intermediate product, in addition Al3+Al (OH) can also be generated3Flco is to F-Carry out ligand exchange, the effect of catching of absorption, net and
Remove the fluorine in iodine solution.Its reaction is as follows：
Al3+→Al2(OH)2 4+→Al7(OH)16 5+→Al13O4(OH)24 7+。
Al13O4(OH)24 7++XF-=Al13O4(OH)24-XXF7++XOH-
Al(OH)3+XF-=Al (OH)3-XXF+XOH-
The larger Al (OH) of the surface area that generates during aluminium salt flocculation defluorinate3Flco produces Hydrogen Binding Adsorption to fluorine ion,
Because fluorine ion radius is small and electronegativity is strong, adsorption process is easier to occur, Al3+The various hydroxyl complex ions mainly generated with hydrolysis,
The form of especially positively charged low polymerization degree or the hydroxyl aluminium complex ion of high polymerization degree exists, these networks with positive charge from
Son can not only adsorb F-, moreover it is possible to the tiny CaF of adsorption particle2, produce co-precipitation.On the other hand, due to fluorine ion with it is hydroxy
Radius and electric charge are all very close, during aluminium salt flocculation defluorinate, the Al of generation13O4(OH)24 7+With Al (OH)3Flco, it is therein
OH-Also can be with F-Exchange；F-Can also be with Al3+Formed from AlF2+, AlF2 +, AlF3To AlF6 3-Deng totally 6 kinds of complex compounds, these
Aluminium fluorine complex ion can form aluminium fluoro complex AlF in flocculation processx(OH)(3-x)Or it is mixed in the Al (OH) newly formed3Wadding
Settle down in body.
Further, since being added in high fluorine iodine absorbing liquid after aluminium defluorinating agent, alkalescence is integrally presented in solution, this also causes iodine
Pb, Hg are deposited separation with hydroxide, oxide form respectively in liquid, the arsenates of As generation indissolubles by sedimentation separation, from
And further reduce the impurity content after defluorinate aoxidizes in solid iodine.Its reaction is as follows：
Pb2++2OH-=Pb (OH)2↓
Hg2++2OH-=HgO ↓+H2O
As2O3+Ca(OH)2=Ca (AsO2)2↓+H2O
Iodine absorbing liquid is after the purified treatments such as defluorinate, using H2O2Iodide ion in absorbing liquid is oxidized to iodine molecule precipitation,
And iodine crystal precipitation is placed in the concentrated sulfuric acid, 150 DEG C are warming up to, under the temperature conditionss, iodine is for liquid and because density ratio sulfuric acid is big
And natural subsidence, after the moisture content in crystallization iodine is absorbed by the concentrated sulfuric acid, high-purity iodine product can be made.
The beneficial effect that the present invention reaches compared with prior art：Before and after the purification of iodine product, fluoride is by 10-100mg/kg
0-1mg/kg is reduced to, silica gel is reduced to 0-5mg/kg by 10-70mg/kg, and moisture is reduced to ＜ 0.5% by 1-2%, solves wet
Recycled in method phosphoric acid and fluosilicic acid and contain the impurity deep purifying problems such as a large amount of fluorides, phosphate and ardealite in iodine, directly
Realize that iodine retracting device produces high-purity iodine, while it is higher to solve thick iodine deep purifying complex production process, cost, and iodine loss compared with
Hang-up.
Brief description of the drawings
Fig. 1：Iodine purification process flow chart is recycled in phosphoric acid by wet process of the present invention.
Wherein 1：First class purification groove；2：Secondary purification groove；3：Turbid groove；4：Oxidation analysis iodine groove；5：Absorbing liquid circulating slot；6：
Surge tank；7：Iodine filter；8：Filtrate receiver；9：Smart Iod R kettle；10：Concentrated sulfuric acid storage tank；11：Hydrogen peroxide storage tank；12：Analyse iodine meter
Amount pump；13：Smart iodine separating tank.
Embodiment
Embodiment 1
Iodine purification technique is recycled in phosphoric acid by wet process：Open phosphorylcholine group phosphoric acid workshop and use ore association iodine resource in rock phosphate in powder
About 60% enters in phosphoric acid,diluted, the about 40mg/kg containing iodine in phosphoric acid,diluted, with H2O2As oxidant, by iodide ion oxygen in phosphoric acid by wet process
Iodine molecule is turned to, then uses air extraction to blow away iodine molecule with gas phase, iodine molecule is followed through reducing agent again in gas phase afterwards
Ring washing absorption is enriched with, and is carried out iodine purification after iodide ion concentration reaches 50g/L in absorbing liquid and is obtained iodine product.
It is as shown in Figure 1 that iodine purification technological process is recycled in phosphoric acid by wet process.Pass through iodine absorbing liquid circulating pump self-priming in future
The absorbing liquid that receipts liquid circulating slot 5 includes 50g/L iodide ions enters first class purification groove 1 from top, adds calcium carbonate, starts stirring
Slurry, carries out first class purification, and wherein calcium carbonate addition is the 110% of theoretical addition amount, and reaction temperature is 35 DEG C, and the reaction time is
30min.Clear liquid after first class purification is put into secondary purification groove 2 from bypass, and bottom turbid is put into turbid groove 3.In secondary purification groove 2
Alum is added, starts stirring slurry, carries out secondary purification, wherein alum addition is the 105% of theoretical addition amount, and reaction temperature is
35 DEG C, reaction time 50min.Purified clear liquid is put into oxidation analysis iodine groove 4 from bypass, and bottom turbid is put into turbid groove 3.Open
Iodine groove stirring slurry is analysed in dynamic oxidation, and the hydrogen peroxide in hydrogen peroxide storage tank 11 is added in oxidation analysis iodine groove 4 by analysing iodine metering pump 12,
Iodide ion oxidation in absorbing liquid is generated iodine molecule by hydrogen peroxide, and iodine molecule crystal is constantly grown up, when solution in analysis iodine groove
When oxidizing potential reaches 540mV, more than 95% iodine is separated out by oxidation.Iodine is released from oxidation analysis iodine trench bottom and passes through iodine filter
7 filterings.8 filtrate of filtrate receiver enters absorbing liquid circulating slot 5, and the iodine crystallization that filtering trolley filters out passes through man-handling of materials to smart Iod R
Kettle 9 is purified.3 upper clear supernate of turbid groove puts back to absorbing liquid circulating slot 5 from bypass, and bottom turbid returns phosphoric acid by Pulp pump
Workshop extraction tank.The concentrated sulfuric acid to smart Iod R kettle 9, smart 9 dense shell side of Iod R kettle, which is introduced, from concentrated sulfuric acid storage tank 10 is passed through steam liter
Temperature is to 150 DEG C, under the temperature conditionss, iodine for liquid and because density ratio sulfuric acid is big and natural subsidence, pass through the concentrated sulfuric acid and absorb crystallization
After moisture content in iodine, purity can be made by smart iodine separating tank 13 and be more than 98.5% iodine product, wherein, the fluoride in iodine product
0-1mg/kg is reduced to by 10-100mg/kg, silica gel is reduced to 0-5mg/kg by 10-70mg/kg, and moisture is reduced to by 1-2%
＜ 0.5%.
Embodiment 2
Iodine purification technique is recycled in phosphoric acid by wet process：Open phosphorylcholine group phosphoric acid workshop and use ore association iodine resource in rock phosphate in powder
About 60% enters in phosphoric acid,diluted, the about 40mg/kg containing iodine in phosphoric acid,diluted, with H2O2As oxidant, by iodide ion oxygen in phosphoric acid by wet process
Iodine molecule is turned to, then uses air extraction to blow away iodine molecule with gas phase, iodine molecule is followed through reducing agent again in gas phase afterwards
Ring washing absorption is enriched with, and is carried out iodine purification after iodide ion concentration reaches 40g/L in absorbing liquid and is obtained iodine product.
It is as shown in Figure 1 that iodine purification technological process is recycled in phosphoric acid by wet process.Pass through iodine absorbing liquid circulating pump self-priming in future
The absorbing liquid that receipts liquid circulating slot 5 includes 40g/L iodide ions enters first class purification groove 1 from top, adds calcium carbonate, starts stirring
Slurry, carries out first class purification, and wherein calcium carbonate addition is the 110% of theoretical addition amount, and reaction temperature is 35 DEG C, and the reaction time is
30min.Clear liquid after first class purification is put into secondary purification groove 2 from bypass, and bottom turbid is put into turbid groove 3.In secondary purification groove 2
Aluminium polychloride is added, starts stirring slurry, carries out secondary purification, wherein aluminium polychloride addition is theoretical addition amount
105%, reaction temperature is 35 DEG C, reaction time 50min.Purified clear liquid is put into oxidation analysis iodine groove 4 from bypass, and bottom is turbid
Liquid is put into turbid groove 3.Start oxidation analysis iodine groove stirring slurry, the hydrogen peroxide in hydrogen peroxide storage tank 11 is added by analysing iodine metering pump 12
Entering in oxidation analysis iodine groove 4, hydrogen peroxide constantly grows up the iodide ion oxidation generation iodine molecule in absorbing liquid, iodine molecule crystal,
When the oxidizing potential for analysing solution in iodine groove reaches 540mV, more than 95% iodine is separated out by oxidation.Released from oxidation analysis iodine trench bottom
Iodine is simultaneously filtered by iodine filter 7.8 filtrate of filtrate receiver enters absorbing liquid circulating slot 5, and the iodine crystallization that filtering trolley filters out passes through people
Work is transported to smart Iod R kettle 9 and is purified.3 upper clear supernate of turbid groove puts back to absorbing liquid circulating slot 5 from bypass, and bottom turbid is led to
Cross Pulp pump and return phosphoric acid workshop extraction tank.The concentrated sulfuric acid is introduced to smart Iod R kettle 9, smart Iod R kettle 9 from concentrated sulfuric acid storage tank 10
Dense shell side is passed through steam and is warming up to 150 DEG C, and under the temperature conditionss, iodine leads to for liquid and because of density ratio sulfuric acid natural subsidence greatly
After moisture content in overrich sulfuric acid absorption crystallization iodine, purity can be made by smart iodine separating tank 13 and be more than 98.5% iodine product, wherein,
Fluoride in iodine product is reduced to 0-1mg/kg by 10-100mg/kg, and silica gel is reduced to 0-5mg/kg, water by 10-70mg/kg
Divide and ＜ 0.5% is reduced to by 1-2%.
Embodiment 3
Iodine purification technique is recycled in phosphoric acid by wet process：Open phosphorylcholine group phosphoric acid workshop and use ore association iodine resource in rock phosphate in powder
About 60% enters in phosphoric acid,diluted, the about 40mg/kg containing iodine in phosphoric acid,diluted, with H2O2As oxidant, by iodide ion oxygen in phosphoric acid by wet process
Iodine molecule is turned to, then uses air extraction to blow away iodine molecule with gas phase, iodine molecule is followed through reducing agent again in gas phase afterwards
Ring washing absorption is enriched with, and is carried out iodine purification after iodide ion concentration reaches 10g/L in absorbing liquid and is obtained iodine product.
It is as shown in Figure 1 that iodine purification technological process is recycled in phosphoric acid by wet process.Pass through iodine absorbing liquid circulating pump self-priming in future
The absorbing liquid that receipts liquid circulating slot 5 includes 10g/L iodide ions enters first class purification groove 1 from top, adds calcium carbonate, starts stirring
Slurry, carries out first class purification, and wherein calcium carbonate addition is the 110% of theoretical addition amount, and reaction temperature is 35 DEG C, and the reaction time is
30min.Clear liquid after first class purification is put into secondary purification groove 2 from bypass, and bottom turbid is put into turbid groove 3.In secondary purification groove 2
Aluminium chloride is added, starts stirring slurry, carries out secondary purification, wherein aluminium chloride addition is the 105% of theoretical addition amount, reaction temperature
Spend for 35 DEG C, reaction time 50min.Purified clear liquid is put into oxidation analysis iodine groove 4 from bypass, and bottom turbid is put into turbid groove
3.Start oxidation analysis iodine groove stirring slurry, the hydrogen peroxide in hydrogen peroxide storage tank 11 is added into oxidation analysis iodine by analysing iodine metering pump 12
In groove 4, the iodide ion oxidation in absorbing liquid is generated iodine molecule by hydrogen peroxide, and iodine molecule crystal is constantly grown up, when in analysis iodine groove
When the oxidizing potential of solution reaches 540mV, more than 95% iodine is separated out by oxidation.Iodine is released from oxidation analysis iodine trench bottom and passes through iodine
Filter 7 filters.8 filtrate of filtrate receiver enters absorbing liquid circulating slot 5, and the iodine crystallization that filtering trolley filters out passes through man-handling of materials to essence
Iod R kettle 9 is purified.3 upper clear supernate of turbid groove puts back to absorbing liquid circulating slot 5 from bypass, and bottom turbid is beaten by Pulp pump
Rephosphorization acid workshop extraction tank.The concentrated sulfuric acid to smart Iod R kettle 9, smart 9 dense shell side of Iod R kettle is introduced from concentrated sulfuric acid storage tank 10 to be passed through
Steam is warming up to 150 DEG C, and under the temperature conditionss, iodine is inhaled for liquid and because of density ratio sulfuric acid natural subsidence greatly by the concentrated sulfuric acid
After receiving the moisture content in crystallization iodine, purity can be made by smart iodine separating tank 13 and be more than 98.5% iodine product, wherein, in iodine product
Fluoride is reduced to 0-1mg/kg by 10-100mg/kg, and silica gel is reduced to 0-5mg/kg by 10-70mg/kg, and moisture is by 1-2%
It is reduced to ＜ 0.5%.
Claims (6)
1. the method for iodine deep purifying is recycled in a kind of phosphoric acid by wet process and fluosilicic acid, with H2O2As oxidant, by phosphoric acid by wet process or
Iodide ion is oxidized to iodine molecule in fluosilicic acid, then uses air extraction to blow out iodine molecule with gas phase, then iodine in gas phase is divided
Son is again through reducing agent circulation washing absorption enrichment, it is characterised in that：When to reach 10-50g/L laggard for iodide ion concentration in absorbing liquid
Row iodine deep purifying obtains iodine product, and deep purifying comprises the following steps：
(1) calcium carbonate is added in absorbing liquid, is stirred, carries out first order purification；
(2) aluminium salt is added in the clear liquid of first class purification, be stirred, carry out secondary purification；
(3) hydrogen peroxide is added in the clear liquid of secondary purification, when the oxidizing potential of solution reaches 540mV, iodine is separated out by oxidation, mistake
Filter；
(4) iodine made from filtering is purified again with the concentrated sulfuric acid, filters and fine work iodine is made.
2. the method for iodine deep purifying is recycled in a kind of phosphoric acid by wet process and fluosilicic acid as claimed in claim 1, it is characterised in that：
Calcium carbonate addition is the 110% of theoretical addition amount in step (1), and reaction temperature is 35 DEG C, reaction time 30min.
3. the method for iodine deep purifying is recycled in a kind of phosphoric acid by wet process and fluosilicic acid as claimed in claim 1, it is characterised in that：
In step (2)：Aluminium salt is alum, the one or more in aluminium chloride, aluminum sulfate, aluminium polychloride.
4. the method for iodine deep purifying is recycled in a kind of phosphoric acid by wet process and fluosilicic acid as claimed in claim 3, it is characterised in that：
Aluminium salt addition is the 105% of theoretical addition amount in step (2), and reaction temperature is 35 DEG C, reaction time 50min.
5. the method for iodine deep purifying is recycled in a kind of phosphoric acid by wet process and fluosilicic acid as claimed in claim 1, it is characterised in that：
The temperature purified in step (4) with the concentrated sulfuric acid is 150 DEG C.
6. the method for iodine deep purifying is recycled in a kind of phosphoric acid by wet process and fluosilicic acid as claimed in claim 1, it is characterised in that：
Bottom turbid after first class purification and secondary purification stand after upper clear supernate, and iodine separated out by oxidation after filtrate, can be with
Add in absorbing liquid and recycle.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711144902.2A CN108033429A (en) | 2017-11-17 | 2017-11-17 | A kind of method that iodine deep purifying is recycled in phosphoric acid by wet process and fluosilicic acid |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711144902.2A CN108033429A (en) | 2017-11-17 | 2017-11-17 | A kind of method that iodine deep purifying is recycled in phosphoric acid by wet process and fluosilicic acid |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN108033429A true CN108033429A (en) | 2018-05-15 |
Family
ID=62093125
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201711144902.2A Pending CN108033429A (en) | 2017-11-17 | 2017-11-17 | A kind of method that iodine deep purifying is recycled in phosphoric acid by wet process and fluosilicic acid |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN108033429A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110540179A (en) * | 2019-09-03 | 2019-12-06 | 贵州开磷集团矿肥有限责任公司 | Method and equipment for removing harmful elements in wet-process phosphoric acid and derivative products thereof |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2677687B2 (en) * | 1989-11-28 | 1997-11-17 | 三井東圧化学株式会社 | Method for producing 3,5-diiodosalicylic acid |
| CN101323434A (en) * | 2008-06-26 | 2008-12-17 | 瓮福（集团）有限责任公司 | Method for reclaiming iodine from concentrated phosphoric acid from wet method phosphoric acid production |
| 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 |
| CN103395747A (en) * | 2013-08-05 | 2013-11-20 | 贵州开磷（集团）有限责任公司 | Method for simultaneously recovering iodine in iodine-containing fluosilicic acid and iodine-containing dilute phosphoric acid |
| 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 |
-
2017
- 2017-11-17 CN CN201711144902.2A patent/CN108033429A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2677687B2 (en) * | 1989-11-28 | 1997-11-17 | 三井東圧化学株式会社 | Method for producing 3,5-diiodosalicylic acid |
| CN101323434A (en) * | 2008-06-26 | 2008-12-17 | 瓮福（集团）有限责任公司 | Method for reclaiming iodine from concentrated phosphoric acid from wet method phosphoric acid production |
| 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 |
| CN103395747A (en) * | 2013-08-05 | 2013-11-20 | 贵州开磷（集团）有限责任公司 | Method for simultaneously recovering iodine in iodine-containing fluosilicic acid and iodine-containing dilute phosphoric acid |
| 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 |
Non-Patent Citations (1)
| Title |
|---|
| 彭宝林等: "磷矿伴生超低品位碘资源回收工业化技术研究", 《现代化工》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110540179A (en) * | 2019-09-03 | 2019-12-06 | 贵州开磷集团矿肥有限责任公司 | Method and equipment for removing harmful elements in wet-process phosphoric acid and derivative products thereof |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN104745823B (en) | Method for recycling lithium from waste lithium ion battery | |
| CN105060579B (en) | A kind of method of advanced treating fluoride waste | |
| CN101774556B (en) | Method for preparing industrial grade and food grade phosphoric acid by decomposing low grade phosphate rocks with hydrochloric acid | |
| CN101532096B (en) | A recovery method of tin in tin-stripping waste liquid | |
| CN105540619A (en) | Method for directly preparing battery grade lithium carbonate from salt lake brine with high magnesium-to-lithium ratio | |
| CN207375760U (en) | A kind of device that lithium is carried from salt lake brine with high magnesium-lithium ratio | |
| CN102732731B (en) | Method for extracting valuable metals and refining zinc sulphate monohydrate from zinc-containing waste material | |
| CN105126742B (en) | A kind of method using modified kaolin sorbent treatment fluoride waste | |
| CN103805781A (en) | Method for inhibiting organic phosphorus and COD in wastewater discharged from rare earth extraction separation enterprises | |
| CN113277489A (en) | Method for preparing high-purity iron phosphate by using ferrophosphorus waste | |
| CN101126124A (en) | Method for preparing high-purity electrolyte for vanadium battery from stone-like coal | |
| CN105098279A (en) | Technique for recycling lithium from scrapped lithium battery | |
| CN105417770A (en) | Treatment method of waste liquor containing lithium hexafluorophosphate | |
| CN104438287A (en) | Arsenic sulfide waste residue recycling treatment method and device thereof | |
| CN103950950B (en) | The preparation method of high abundance boron-11 acid | |
| CN102838097A (en) | Method for removing magnesium oxide in phosphate concentrate through phosphatic fertilizer and phosphorus chemical industry acid wastewater | |
| CN108033429A (en) | A kind of method that iodine deep purifying is recycled in phosphoric acid by wet process and fluosilicic acid | |
| CN102925899A (en) | Method for refining copper chloride etching waste liquor | |
| CN101824542A (en) | Comprehensive utilization method of titanium dioxide waste acid by sulfuric acid process | |
| CN100400687C (en) | Method of extracting radioactive uranium in phosphate | |
| CN103103351A (en) | Method for preparing high-purity calcium carbonate for saponifying rare earth extraction agent | |
| CN105084608B (en) | A kind of preprocess method of acrylic ester wastewater biochemical treatment | |
| CN108411110B (en) | A kind of rare-earth liquid impurity removal process | |
| Han et al. | Recycling of lithium and fluoride from LiF wastewater from LiF synthesis industry by solvent extraction | |
| CN102337405B (en) | Method for applying baotite mixed carbonate-rare earth precipitation wastewater in precipitation of europium (II) sulfate |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20180515 |