CN109336054A - A method of recycling iodine from salt-making mother liquor - Google Patents
A method of recycling iodine from salt-making mother liquor Download PDFInfo
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- CN109336054A CN109336054A CN201811563205.5A CN201811563205A CN109336054A CN 109336054 A CN109336054 A CN 109336054A CN 201811563205 A CN201811563205 A CN 201811563205A CN 109336054 A CN109336054 A CN 109336054A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
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- C01B7/00—Halogens; Halogen acids
- C01B7/13—Iodine; Hydrogen iodide
- C01B7/14—Iodine
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Abstract
The present invention provides a kind of method that iodine is recycled from salt-making mother liquor, belongs to iodine technical field processed.It include: 1) to stand salt-making mother liquor to clarify, acid adding adjusts acidification, and chlorine water oxidation is passed through after preheated;2) oxidized liquid enters stripping tower, and the iodine in liquid enters gas phase and enters absorption tower from blowout column overhead blowout, and the iodine in absorption tower in gas phase enters absorbing liquid and is absorbed reduction;3) oxidant secondary oxidation is added into absorbing liquid, crystallization iodine is precipitated, and crystallization iodine is separated by filtration with waste liquid;4) filtered crystallization iodine is washed, the concentrated sulfuric acid is added into the crystallization iodine after washing and melts purification at high temperature, cooling crush obtains finished product iodine.Stripping tower, absorption tower and mist eliminating of the present invention constitute air closed cycle and propose iodine system, oxidized feed liquid mentions in iodine system through air closed cycle to be blown out, absorbs, gas-liquid contacts in filler surface and carries out mass exchange, two phase compositions reduce the discharge and environmental pollution of tail gas along tower height consecutive variations.
Description
Technical field
The invention belongs to iodine technical field processed, specially a kind of method that iodine is recycled from salt-making mother liquor.
Background technique
China is the more poor country of iodine resource, and reserves are about 4000 tons, and iodine product annual production capacity is at 600-700 tons
Left and right, accounts for 2.14% or so of global total output.Demand of the China to iodine product increases year by year, and imbalance between supply and demand is prominent, and 2015
About 6000 tons of the demand of iodine, about 90% needs from the national import such as Chile, Japan, Turkmenistan.It is long-term main before Chinese
By iodine is extracted from marine algae plant, manufacturer focuses primarily upon coastal area, wherein Shandong District occupy 80% with
On.Representing enterprise has: 90 tons of Shandong Jie Jing group, 30 tons of Qingdao Rising seaweed, 20 tons of Qingdao Nan Yang seaweed, Qingdao, which are contained, foreignizes work
20 tons, 10 tons of Qingdao bright moon seaweed, 10 tons of Qingdao Hai Yuan seaweed.Other production paths of iodine in addition to using brine as raw material other than, also
There is the iodine in recycling phosphate fertilizer plant's exhaust gas, the country is concentrated mainly on Guizhou, Yunnan, Hubei, Hunan, Sichuan, these save phosphorus ore master
China's phosphorus ore 80% accounted for based on sedimentary rock phosphorus ore, represent Guizhou Wengfu group of enterprise, company official website produces 250 tons of iodine number per year.
2010, as Chinese Wengfu group recycles improving for iodine technology and building up for device from the phosphoric acid that sulfuric acid decomposition phosphorus ore produces
It goes into operation, huge variation has occurred in the production method of Chinese iodine.Nevertheless, including from the iodine recycled in various waste liquids,
The annual output of Chinese iodine is also only 600 tons or so, and annual requirement has reached 4000 tons or more, there are also 85% need from foreign countries into
Mouthful.
Summary of the invention
It is an object of the invention to the problems too low for existing domestic iodine yield, provide one kind and recycle from salt-making mother liquor
The method of iodine had not only been able to achieve the recycling of iodine in salt-making mother liquor, but also can produce despumation for subsequent product.
The object of the invention is achieved through the following technical solutions:
A method of recycling iodine from salt-making mother liquor, the following steps are included:
1) salt-making mother liquor is stood and is clarified, acid adding adjusts acidification, and chlorine water oxidation is passed through after preheated;
2) oxidized liquid enters stripping tower, and the iodine in liquid enters gas phase and enters absorption from blowout column overhead blowout
Tower, the iodine in absorption tower in gas phase enter absorbing liquid and are absorbed reduction;
3) oxidant secondary oxidation is added into absorbing liquid, crystallization iodine is precipitated, and crystallization iodine is separated by filtration with waste liquid;
4) filtered crystallization iodine is washed, into the crystallization iodine after washing, the addition concentrated sulfuric acid melts at high temperature mentions
Pure purification, cooling crush obtain finished product iodine.
Further, it be that hydrochloric acid is added to be acidified to pH is 3~4 that the acid adding, which adjusts acidification, the chlorine water be iodine waste liquid processed and
The chlorine water of chlorine preparation.
Further, the preheating temperature is 40~50 DEG C, and the preheating is heated using bromine extraction waste brine.
Further, stripping tower is returned after liquid of the absorbing tower bottom discharge gas phase through carrying secretly in mist eliminating removal gas phase.
Further, the main component of the absorbing liquid is sulfur dioxide and water.
Further, the absorbing liquid for absorbing Gas-phase iodine is recycled in absorption tower in HI concentration unsaturation, in HI concentration
Oxidant secondary oxidation is added in extraction when saturation.
Further, the HI saturated concentration is 18~20.Be.
Further, the oxidant is sodium chlorate saturated solution or chlorine.
Further, the washing is using steam condensate after ion exchange column removes removing calcium and magnesium chlorine and sulfate radical zwitterion
Obtained pure water.
Further, the melting purification carries out under the conditions of high-temperature steam.
Compared with prior art, the invention has the following advantages:
The present invention provide it is a kind of from salt-making mother liquor recycle iodine method, salt-making mother liquor is acidified, preheat, aoxidize it is laggard
Enter stripping tower and absorption tower, the absorbing liquid for absorbing iodine in absorption tower washed after secondary oxidation, filter after obtain crystallization iodine, knot
Brilliant iodine obtains finished product iodine after the concentrated sulfuric acid melts purification under the conditions of high-temperature steam.In the present invention, stripping tower, absorption tower with
And mist eliminating constitutes an air closed cycle and proposes iodine system, oxidized feed liquid mentions in iodine system through air closed cycle blows
Out, it absorbs, during blowing/inhaling, gas-liquid contacts in filler surface and carries out mass exchange, and the composition of two-phase continuously becomes along tower height
Change, closed cycle blows out the more former open circuit blowout technology of technique, eliminates the discharge of tail gas, reduces environmental pollution.The present invention from
The yield that iodine is recycled in salt-making mother liquor can achieve 80%, and the purity purity of iodine can achieve 99.7%.
Detailed description of the invention
Fig. 1 is a kind of process flow chart that iodine is recycled from salt-making mother liquor of the present invention.
Specific embodiment
In order to make the objectives, technical solutions, and advantages of the present invention clearer, with reference to embodiments, to the present invention
It is further elaborated.It should be appreciated that the specific embodiments described herein are merely illustrative of the present invention, it is not used to
Limit the present invention.
It is carried out specifically below with reference to specific steps and the principle method for recycling iodine from salt-making mother liquor a kind of to the present invention
It is bright, present invention process process as shown in Figure 1, specifically includes the following steps:
1, salt-making mother liquor is stood and is clarified, acid adding adjusts acidification, and chlorine water oxidation is passed through after preheated.
Specifically, by salt-making mother liquor stand clarify, be added hydrochloric acid be acidified to pH be 3~4, it is preheated to feed liquid temperature be 40
~50 DEG C, it is passed through chlorine water oxidation.
The purpose of acidification is to improve product recovery rate to inhibit iodine to hydrolyze.For iodine in PH ﹥ 6, hydrolysis is more bright
Aobvious, hydrolysate is hydrogen iodide (HI) and acid iodide (HIO3), product recovery rate is not only reduced in this way, but also increases supplies consumption.
The purpose of preheating is to increase the activity of iodine molecule, improves the volatility of iodine, iodine molecule is enable to be easier to parse from salt-making mother liquor
Out, the rate of recovery of iodine is improved.Oxidation is to make the iodine in salt-making mother liquor be converted into molecularity from the compound of ionic condition
The iodine of state.It is substantially the mixed liquor for including the substances such as bromine, excessive free chlorine with mentioning iodine waste liquid to be passed through the chlorine water of chlorine preparation
Body, since the content of iodine is very low, chlorine water is liquid, is convenient for accurate control additional amount in operation.Its reaction equation is as follows:
Chlorine water is prepared: 2Br-+Cl2→Br2+2Cl-
Chlorine water oxidation: Br2+2I-→I2+2Br- Cl2+2I-→I2+2Cl-
In this step, the additional amount of chlorine water determines that those skilled in the art can according to the content of iodide ion in iodine mother liquor processed
To be adjusted according to additional amount of the iodide ion content to chlorine water.
Further, in order to preferably be recycled to resource, preheating is heated using bromine extraction waste brine, and chlorine water is preferably made
The chlorine water of iodine waste liquid and chlorine preparation.Iodine waste liquid processed and chlorine preparation chlorine water use the ordinary skill in the art, certainly, chlorine
Water can also be preferably the chlorine water that other way is prepared or fresh chlorine water.
2, oxidized liquid enters stripping tower, and the iodine in liquid enters gas phase and enters absorption from blowout column overhead blowout
Tower, the iodine in absorption tower in gas phase enter absorbing liquid and are absorbed reduction.
Specifically, oxidized liquid enters stripping tower, iodine under the action of stripping tower in liquid enter gas phase from
Blow out column overhead blowout, and enter absorption tower from absorbing tower jacking, the iodine in absorption tower in gas phase enter absorbing liquid (mainly at
It is divided into water and sulfur dioxide, absorbing liquid also enters from absorbing tower jacking) it is absorbed reduction, gas phase is discharged through mist eliminating in absorbing tower bottom
From return stripping tower after the liquid carried secretly in removal gas phase.Absorbing tower bottom discharge gas phase, which returns to stripping tower, may be implemented to gas phase
The recycling again of middle iodine, increases the rate of recovery of iodine.The reactive chemistry equation between iodine and absorbing liquid in gas phase:
I2+SO2+2H2O→H2SO4+2HI
In the present invention, stripping tower, absorption tower and mist eliminating constitute an air closed cycle and propose iodine system, oxidized
Feed liquid mentions in iodine system through air closed cycle to be blown out, absorbs, and during blowing/inhaling, gas-liquid contacts in filler surface and carries out object
Mass transter, along tower height consecutive variations, closed cycle blows out the more former open circuit blowout technology of technique, eliminates tail gas the composition of two-phase
Discharge, reduces environmental pollution.
In this step, absorbing liquid is that sulfur dioxide is dissolved in made of water, is mainly existed in water with sulfur dioxide molecule,
Those skilled in the art can be adjusted the additional amount of sulfur dioxide according to the content for entering iodine in absorption tower.Preferably,
The additional amount of sulfur dioxide is into 25~35% of the quality of iodine in absorption tower in absorbing liquid.
The reason of present invention is using iodine is prepared after stripping tower and absorption tower and secondary oxidation are as follows: iodine in salt-making mother liquor
Content is very low, only the about 0.2kg containing iodine in about 0.2g/L, i.e., 0.015%, that is, every cubic metre of salt-making mother liquor, and salt-making mother liquor
In calcium sulphate content it is also higher than iodine, there are also other impurity such as sodium chloride, magnesium chloride, if directly filtering after chlorine water once oxidation
It is almost impossible to obtain product, it is necessary to be enriched with and be purified by blowing out to absorb.The iodine of stripping tower's blowout is with gas
There is the air capacity 5200m in blow out air in phase state3/ h, iodine vapor account for 0.034% in blow out air, do not have directly
The condition of simple substance product is obtained, needs to be enriched with again secondary oxidation by cyclic absorption and obtains product.
The specific work process on stripping tower and absorption tower is as follows:
In stripping tower, the feed liquid after preprocessed oxidation is uniformly distributed in packing layer through tower top spray equipment, by weight
Power effect along filler surface flow through packing layer from top to bottom after from tower bottom be discharged;Gas then passes through packing layer under pressure difference promotion
Gap, tower top is flowed to by tower bottom, the iodine in liquid phase enters in gas phase to be blown out by air.In absorption tower, absorbing liquid is through tower top
Spray equipment is uniformly distributed in packing layer, and with gas phase containing iodine from tower top through packing layer fair current to tower bottom, the iodine in gas phase enters liquid
It is absorbed in phase, tower bottom gas phase returns to stripping tower after the liquid through carrying secretly in mist eliminating removal gas phase.
Further, the absorbing liquid for absorbing Gas-phase iodine is recycled in absorption tower in HI concentration unsaturation, in HI concentration
Oxidant secondary oxidation is added in extraction when saturation.Further, the HI saturated concentration is 18~20.Be.By unsaturated suction
It receives liquid to recycle, cost absorption can be reduced.With the concentration of HI to determine whether saturation is inhaled because as HI concentration increases
It receives motive force to be gradually reduced, absorptivity gradually decreases.
3, oxidant secondary oxidation is added into absorbing liquid, crystallization iodine is precipitated, and crystallization iodine is separated by filtration with waste liquid.
Specifically, when absorbing liquid concentration containing HI, which reaches 18~20.Be, to be saturated, oxidant (chlorine is added in extraction absorbing liquid
Crystallization iodine is precipitated in sour sodium saturated solution or chlorine oxidation, by the absorbing liquid of the iodine containing crystallization be emitted into vacuum filter will crystallize iodine with
Waste liquid separation.Reactive chemistry equation between absorbing liquid and oxidant:
6HI+NaClO3→3I2+NaCl+3H2O
The additional amount of secondary oxidation agent sodium chlorate saturated solution or chlorine is according to I in absorbing liquid-What content was adjusted,
The additional amount of sodium chlorate is 10~20% of iodine quality in absorbing liquid in secondary oxidation agent, and the additional amount of chlorine is iodine in absorbing liquid
The 25~35% of quality.
4, filtered crystallization iodine is washed, into the crystallization iodine after washing, the addition concentrated sulfuric acid melts at high temperature mentions
Pure purification, cooling crush obtain finished product iodine.
Specifically, addition is prepared after ion exchange column removes the zwitterions such as removing calcium and magnesium chlorine and sulfate radical with steam condensate
Pure water filtered crystallization iodine is washed, then with vacuum pump by crystallize iodine drain, will crystallization iodine and the concentrated sulfuric acid be added
Melting purification, last cooling crush are finished product iodine under the conditions of high-temperature steam in reaction kettle.
The concentration of the concentrated sulfuric acid is 92.5% or more, and the addition mass ratio of the concentrated sulfuric acid and crystallization iodine is 1:2~1:3.
Be primarily due to using melt refining iodine under concentrated sulfuric acid layer: 1. sulfuric acid and iodine are immiscible, and sulfuric acid and molten condition
Iodine has apparent interface, can realize separation well;2. the concentrated sulfuric acid has strong absorptive, the moisture in thick iodine can be inhaled
It receives;3. the concentrated sulfuric acid has strong oxidizing property, organic impurities and reducing substances oxidation in thick iodine can be made;4. sulfuric acid boiling with higher
Point, during iodinating and refining, even if iodine has boiled, sulfuric acid forms fluid-tight on liquid iodine, does not cause iodine evolution (because iodine easily rises
China).
The method that iodine is recycled from salt-making mother liquor a kind of to the present invention carries out further detailed combined with specific embodiments below
Explanation.
Embodiment 1
The concrete technology flow process that the present embodiment recycles iodine from salt-making mother liquor is as described in Figure 1, and process is as follows:
Salt-making mother liquor (content of iodine about 0.2g/L) from salt manufacturing workshop section adds hydrochloric acid to adjust PH to 3 after standing clarification, through one
Grade preheater heats feed liquid temperature to 45 DEG C with bromine extraction waste brine, is passed through in venturi distributor by iodine waste liquid processed and chlorine preparation
Chlorine water (mass concentration 0.4%, additional amount about 26L/m3Salt-making mother liquor), then the system after mentioning iodine static mixer and preheating acidification
Iodine mother liquor and chlorine water are sufficiently mixed oxidation, and into stripping tower, iodine under the action of stripping tower in liquid enters gas phase from blowout
Column overhead blowout enters absorption tower, and the iodine in absorption tower in gas phase enters with water and sulfur dioxide absorbing liquid as main component
It is absorbed reduction, absorbing tower bottom returns to stripping tower after liquid of the gas phase through carrying secretly in mist eliminating removal gas phase is discharged.Wherein, it absorbs
The additional amount of sulfur dioxide about enters 30% of gas phase iodine quality in absorption tower in liquid.
It is recycled in absorption tower when absorbing liquid unsaturation, when absorbing liquid concentration containing HI reaches 18.Be, extracts absorbing liquid out
Sodium chlorate saturated solution (additional amount of sodium chlorate is 15% of iodine quality in absorbing liquid) oxidation is added, crystallization iodine is precipitated.Containing crystallization
The absorbing liquid of iodine is emitted into vacuum filter and separates crystallization iodine with waste liquid, and addition is removed with steam condensate through ion exchange column
The pure water prepared after the zwitterions such as calcium and magnesium chlorine and sulfate radical carries out 3 washings, then is drained with vacuum pump by iodine is crystallized, and will tie
Brilliant iodine and the concentrated sulfuric acid (mass ratio of concentration 98%, additional amount and crystallization iodine is 1:2) are added in reaction kettle in high-temperature steam item
Melting purification under part, last cooling crush are packaged as finished product iodine.
The yield that iodine is recycled in the present embodiment salt-making mother liquor is 80%, purity 99.7%.
Embodiment 2
The concrete technology flow process that the present embodiment recycles iodine from salt-making mother liquor is as described in Figure 1, and process is as follows:
Salt-making mother liquor (content of iodine about 0.2g/L) from salt manufacturing workshop section adds hydrochloric acid to adjust PH to 4 after standing clarification, through one
Grade preheater heats feed liquid temperature to 50 DEG C with bromine extraction waste brine, and being passed through chlorine water in venturi distributor, (mass concentration 0.4%, adds
Enter amount about 26L/m3Salt-making mother liquor), then mentioned the iodine mother liquor processed that iodine static mixer is acidified after preheating and be sufficiently mixed oxygen with chlorine water
Change, into stripping tower, iodine under the action of stripping tower in liquid enters gas phase and enters absorption tower from blowout column overhead blowout,
Iodine in absorption tower in gas phase, which enters, is absorbed reduction, absorbing tower bottom row with water and sulfur dioxide absorbing liquid as main component
Stripping tower is returned after liquid of the gas phase through carrying secretly in mist eliminating removal gas phase out.Wherein, the additional amount of sulfur dioxide is about in absorbing liquid
It is 25% of gas phase iodine quality in entrance absorption tower.
It is recycled in absorption tower when absorbing liquid unsaturation, when absorbing liquid concentration containing HI reaches 20.Be, extracts absorbing liquid out
Chlorine (additional amount is 30% of iodine quality in absorbing liquid) oxidation is added, crystallization iodine is precipitated.The absorbing liquid of the iodine containing crystallization is emitted into very
Air filter will crystallize iodine and separate with waste liquid, and addition removes the yin such as removing calcium and magnesium chlorine and sulfate radical through ion exchange column with steam condensate
The pure water prepared after cation carries out 4 washings, then is drained with vacuum pump by iodine is crystallized, by crystallization iodine and the concentrated sulfuric acid (concentration
It is 98%, the mass ratio of additional amount and crystallization iodine is 1:3) melting purification under the conditions of high-temperature steam is added in reaction kettle,
Last cooling crush is packaged as finished product iodine.
The yield that iodine is recycled in the present embodiment salt-making mother liquor is 77%, purity 99.7%.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all in essence of the invention
Made any modifications, equivalent replacements, and improvements etc., should all be included in the protection scope of the present invention within mind and principle.
Claims (10)
1. a kind of method for recycling iodine from salt-making mother liquor, which comprises the following steps:
1) salt-making mother liquor is stood and is clarified, acid adding adjusts acidification, and chlorine water oxidation is passed through after preheated;
2) oxidized liquid enters stripping tower, and the iodine in liquid enters gas phase and enters absorption tower from blowout column overhead blowout,
Iodine in absorption tower in gas phase enters absorbing liquid and is absorbed reduction;
3) oxidant secondary oxidation is added into absorbing liquid, crystallization iodine is precipitated, and crystallization iodine is separated by filtration with waste liquid;
4) filtered crystallization iodine is washed, the concentrated sulfuric acid is added into the crystallization iodine after washing and melts purification essence at high temperature
System, cooling crush obtain finished product iodine.
2. a kind of method for recycling iodine from salt-making mother liquor as described in claim 1, which is characterized in that the acid adding adjusts acidification
It is 3~4 for hydrochloric acid is added to be acidified to pH, the chlorine water is the chlorine water of iodine waste liquid processed and chlorine preparation.
3. a kind of method for recycling iodine from salt-making mother liquor as described in claim 1, which is characterized in that the preheating temperature is 40
~50 DEG C, the preheating is heated using bromine extraction waste brine.
4. a kind of method for recycling iodine from salt-making mother liquor as described in claim 1, which is characterized in that the absorbing tower bottom row
Stripping tower is returned after liquid of the gas phase through carrying secretly in mist eliminating removal gas phase out.
5. as described in claim 1 it is a kind of from salt-making mother liquor recycle iodine method, which is characterized in that the absorbing liquid it is main
Ingredient is sulfur dioxide and water.
6. a kind of method for recycling iodine from salt-making mother liquor as described in claim 1, which is characterized in that absorb the absorption of Gas-phase iodine
Liquid is recycled in absorption tower in HI concentration unsaturation, and in HI concentration saturation, oxidant secondary oxidation is added in extraction.
7. a kind of method for recycling iodine from salt-making mother liquor as claimed in claim 6, which is characterized in that the HI saturated concentration is
18~20.Be.
8. a kind of method for recycling iodine from salt-making mother liquor as claimed in claim 1 or 6, which is characterized in that the oxidant is
Sodium chlorate saturated solution or chlorine.
9. a kind of method for recycling iodine from salt-making mother liquor as described in claim 1, which is characterized in that the washing uses steam
The pure water that condensed water obtains after ion exchange column removes removing calcium and magnesium chlorine and sulfate radical zwitterion.
10. a kind of method for recycling iodine from salt-making mother liquor as described in claim 1, which is characterized in that the melting purification essence
System carries out under the conditions of high-temperature steam.
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Cited By (3)
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CN112028020A (en) * | 2020-09-02 | 2020-12-04 | 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 |
CN115948799A (en) * | 2023-03-14 | 2023-04-11 | 四川科宏达集团有限责任公司 | Method for preparing iodine single crystal from crude iodine at low temperature and iodine single crystal |
CN116873867A (en) * | 2023-09-08 | 2023-10-13 | 珙县华洁危险废物治理有限责任公司成都分公司 | Harmless treatment method and system for high-purity bromine |
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