CN101274748B - Method for refining industrial coarse iodine - Google Patents
Method for refining industrial coarse iodine Download PDFInfo
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- CN101274748B CN101274748B CN2008100687526A CN200810068752A CN101274748B CN 101274748 B CN101274748 B CN 101274748B CN 2008100687526 A CN2008100687526 A CN 2008100687526A CN 200810068752 A CN200810068752 A CN 200810068752A CN 101274748 B CN101274748 B CN 101274748B
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Abstract
The invention relates to a method for refining industrial crude iodine. The method comprises the steps that the industrial crude iodine with the iodine content accounting for 70 to 95 percent is adopted as material to be added into a sublimator which is provided with concentrated sulfuric acid, a temperature measurement device and a gas blowing-out device; the ambient temperature of a crystallization device is controlled to be 20 DEG C, the sublimator is first heated to 60 to 90 DEG C and the sublimated iodine is caused to flow into a crystallizer by using the gas with the flow rate of 8 to 15L/min; after being maintained for 40 to 60 min, the temperature of the sublimator is heated to 160 to 200 DEG C and the gas-flow rate is adjusted to 1 to 1.5L/min so as to continue to collect the remaining iodine. By adopting the refining method, the content of volatile impurities in iodine products can be effectively reduced; multi-level crystallization devices are adopted to be connected in series to prevent the loss of the iodine and improve the working efficiency of the iodine sublimator. The obtained refined iodine products have neat appearance, large particle size and low impurity content. In addition, the refining method of the invention has the advantages of easy industrialization, low investment, high recovery rate and cleanness without pollution, etc., and can also increase the added value of the iodine products as well as generate relatively high economic and social benefits.
Description
Technical field
Patent of the present invention relates to the process for purification of iodine, and particularly a kind of is the method that raw material is produced smart iodine with the industrial coarse iodine.
Background technology
Iodine is the basic raw material of preparation iodide, and iodine is the requisite nutritive element of human body and plant, at aspects such as medicine, agricultural, dyestuff, metallurgy, synthetic rubber, national defence and sophisticated technologies purposes is widely arranged.Iodine is carried in comparatively common having at present from seawater, but seawater amount of iodine 0.05mg/L only.Industrial mainly is to utilize when producing algin and kelp food in the solution that soaks, cleans sea-tangle to contain iodine as byproduct system iodine.Continuous development along with science and technology, system iodine industry by original be the iodine suitability for industrialized production of raw material with the sea-food, direction to the thick iodine of plurality of raw materials manufacture develops, and the relevant patent of having announced has: " a kind of method of extracting active iodine from sea-tangle ", " a kind of method of extracting iodine from sea-tangle ", " reclaiming the method for iodine from palygorskite ore ", " extracting the method for iodine from contain the waste that produces when the iodine Rock Phosphate (72Min BPL) is produced phosphorus product ".
But because it is more and more higher to the purity requirement of iodine to relate to the iodine product, the demand of smart iodine increases day by day.And the resulting product of above patent can not satisfy the growing demand to the higher smart iodine of purity nothing but the higher slightly industrial coarse iodine product of index.And the process for purification of traditional thick iodine, the old backwardness of technology be difficult for to form suitability for industrialized production, efficient is lower, and the rate of recovery is low, and foreign matter content is higher in the gained iodine product.Present method is raw material with the industrial coarse iodine, and its technological process is improved and optimizated, and adopts measures such as gas blow-out and fractional crystallization, produces smart iodine, has improved the rate of recovery of production efficiency and iodine product, has effectively reduced the foreign matter content in the iodine product.Have very high using value and very wide application prospect.
Summary of the invention
The objective of the invention is to overcome the shortcoming in the process for purification of conventional iodine, provide a kind of easy industrialization, production cost low, production efficiency height, rate of recovery height, purity height and cleanliness without any pollution be the method that raw material is produced smart iodine with the industrial coarse iodine.
A kind of method of refining industrial coarse iodine iodine, it is characterized in that getting content and be 70%～95% industrial coarse iodine is raw material, join the vitriol oil is housed, in the sublimer of temperature measuring equipment and gas blowing out device, the amount of the adding vitriol oil is 3: 1～6: 1 with the ratio of processed industrial coarse iodine amount, crystallization control device context temperature to 20 ℃, sublimer is heated to 60 ℃～90 ℃ earlier, open gas blow-out device switch, the adjustments of gas flow is opened sublimer pneumatic outlet valve to 8L～14L/min, collects the iodine product, keep 40min～60min, sublimer is heated to 160 ℃～200 ℃ then, and the adjustments of gas flow continues to collect remaining iodine to 1L～1.5L/min.
The method of above-mentioned a kind of refining industrial coarse iodine iodine, the gas that is blown into by the gas blow-out device is dry air or N
2Gas.
The method of above-mentioned a kind of refining industrial coarse iodine iodine, the industrial coarse iodine raw material in its method refers to from natural bittern, or sodium nitrate, or marine alga, or the industrial coarse iodine produced by chemical process of Rock Phosphate (72Min BPL).
The method of above-mentioned a kind of refining industrial coarse iodine iodine, used crystallization apparatus are to adopt the plural serial stage crystallization apparatus, with the rate of recovery of raising product and the throughput of equipment.
The present invention compared with prior art, by such scheme as can be known, employing is with by various natural bitterns, sodium nitrate, the industrial coarse iodine that marine alga or Rock Phosphate (72Min BPL) etc. produces by chemical process is a raw material, with itself and vitriol oil azeotropic, the amount of the adding vitriol oil is 3: 1～6: 1 with the ratio of processed industrial coarse iodine, control simultaneously is blown into the envrionment temperature of the flow and the crystallization apparatus of gas, so that the distillation of iodine is better carried out, effectively reduces the easy volatile foreign matter content in the iodine product more.Adopt the series connection of multistage crystallization device, prevent the loss of iodine, improve the working efficiency of iodine sublimer.The smart iodine product appearance of gained is regular, particle is thick, foreign matter content is low.Have advantages such as easy industrialization, less investment, rate of recovery height, cleanliness without any pollution.Improve the added value of product of iodine, had high economic benefit and social benefit.
Description of drawings
Fig. 1 is the schema of refining industrial coarse iodine method.
1. gas bomb, 2. gas meter, 3. sublimer heating unit, 4. sublimer, 5. crystallizer, 6. crystallizer temperature control unit, 7. plural serial stage crystallization apparatus.
Embodiment
Embodiment 1
Get iodine content and be 70.18% thick iodine 300.21kg join the gas blow-out device is housed and added in the vitriol oil jacketed type sublimer of 50L98%, regulate crystallization apparatus envrionment temperature to 20 ℃, open the hydronics switch, the feeding circulation adds hot glycerine makes sublimer be heated to 60 ℃, the adjustments of gas under meter, gas distributor bottom sublimer feeds the dry air of 8.00L/mi n, makes iodine begin distillation and enters crystallizer, keeps 60min.Regulate hydronics, be warming up to 160 ℃, the adjustments of gas under meter makes gas flow rate be passed in the sublimer with 1.20L/min, after maintenance 40min collects surplus iodine, closes gas switch and hydronics valve.The smart iodine of gained is 204.08kg in the crystallizer.
After testing, the content of elemental iodine is 99.98% in the smart iodine.The rate of recovery is 96.84%, and overall treatment time is 110min.
Getting iodine content and be 95.28% thick iodine 250.19kg joins in the jacketed type sublimer that the vitriol oil gas blow-out device and that added 50L98% is housed, regulate crystallization apparatus envrionment temperature to 20 ℃, open the hydronics switch, the feeding circulation adds hot glycerine makes sublimer be heated to 90 ℃, the adjustments of gas under meter, the gas distributor bottom sublimer feeds the dry N of 10.00L/min
2, make iodine begin distillation and enter crystallizer, keep 40min, regulate hydronics, be warming up to 200 ℃, the adjustments of gas under meter, gas flow rate is passed in the sublimer with 1.10L/min, keeps 50min to collect surplus iodine, close gas switch and hydronics valve.The smart iodine of gained is 235.52kg in the crystallizer.
After testing, the content of elemental iodine is 99.99% in the smart iodine.The rate of recovery is 98.79%, and the treatment time is 100min.
Embodiment 3
Getting iodine content and be 82.41% thick iodine 200.38kg joins in the jacketed type sublimer of the vitriol oil that the gas blow-out device is housed and has added 50L98%, regulate crystallization apparatus envrionment temperature to 20 ℃, open the hydronics switch, the feeding circulation adds hot glycerine makes sublimer be heated to 100 ℃, the adjustments of gas under meter, gas distributor bottom sublimer feeds the dry air of 14.00L/min, makes iodine begin distillation and enters crystallizer, keeps 80min.Regulate hydronics, be warming up to 190 ℃, the adjustments of gas under meter makes gas flow rate be passed in the sublimer with 1.00L/min, keeps 60min to collect surplus iodine, closes gas switch and hydronics valve.The smart iodine of gained is 163.94kg in the crystallizer.
After testing, the content of elemental iodine is 99.99% in the smart iodine.The rate of recovery is 99.27%, and the treatment time is 150min.
Embodiment 4
Getting iodine content and be 74.83% thick iodine 150.38kg joins in the jacketed type sublimer of the vitriol oil that the gas blow-out device is housed and has added 50L98%, regulate crystallization apparatus envrionment temperature to 20 ℃, open the hydronics switch, the feeding circulation adds hot glycerine makes sublimer be heated to 90 ℃, the adjustments of gas under meter, gas distributor bottom sublimer feeds the dry air of 15.00L/min, makes iodine begin distillation and enters crystallizer, keeps 60min.Regulate hydronics, be warming up to 180 ℃, the adjustments of gas under meter makes gas flow rate be passed in the sublimer with 1.50L/min, keeps 60min to collect surplus iodine, closes gas switch and hydronics valve.The smart iodine of gained is 109.87kg in the crystallizer.
After testing, the content of elemental iodine is 99.97% in the smart iodine.The rate of recovery is 97.61%, and the treatment time is 150min.
Claims (4)
1. the method for a refining industrial coarse iodine iodine, it is characterized in that getting content and be 70%～95% industrial coarse iodine is raw material, join in the sublimer that the vitriol oil, temperature measuring equipment and gas blowing out device are housed, the amount of the adding vitriol oil is 3: 1～6: 1 with the ratio of processed industrial coarse iodine amount; Crystallization control device context temperature to 20 ℃, sublimer is heated to 60 ℃～90 ℃ earlier, open gas blow-out device switch, adjustments of gas flow to 8～15L/min is opened sublimer pneumatic outlet valve, begins to collect the iodine product, keep 40min～60min, then sublimer is heated to 160 ℃～200 ℃, the adjustments of gas flow continues to collect remaining iodine to 1L～1.5L/min.
2. the method for a kind of refining industrial coarse iodine iodine according to claim 1 is characterized in that the gas that is blown into by the gas blow-out device is dry air, or nitrogen.
3. the method for a kind of refining industrial coarse iodine iodine according to claim 1 is characterized in that the industrial coarse iodine raw material in the method refers to from natural bittern, or sodium nitrate, or marine alga, or the industrial coarse iodine produced by chemical process of Rock Phosphate (72Min BPL).
4. the method for a kind of refining industrial coarse iodine iodine according to claim 1 is characterized in that crystallization apparatus used in the method is to adopt the plural serial stage crystallization apparatus.
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| Application Number | Priority Date | Filing Date | Title |
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| CN2008100687526A CN101274748B (en) | 2008-05-21 | 2008-05-21 | Method for refining industrial coarse iodine |
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| CN2008100687526A CN101274748B (en) | 2008-05-21 | 2008-05-21 | Method for refining industrial coarse iodine |
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| CN101274748B true CN101274748B (en) | 2010-08-18 |
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Families Citing this family (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102020247A (en) * | 2010-12-31 | 2011-04-20 | 瓮福（集团）有限责任公司 | Preparation method of high-purity iodine |
| CN102583249B (en) * | 2012-01-20 | 2013-08-21 | 河南科技大学 | Method for recovering iodine from industrial byproduct containing KI |
| CN103342343A (en) * | 2013-07-16 | 2013-10-09 | 瓮福（集团）有限责任公司 | Ultra-high-purity iodine production device |
| CN103332653A (en) * | 2013-07-16 | 2013-10-02 | 瓮福（集团）有限责任公司 | Crude iodine purification device |
| CN103332654A (en) * | 2013-07-16 | 2013-10-02 | 瓮福（集团）有限责任公司 | High-purity iodine production device |
| CN103342344A (en) * | 2013-07-16 | 2013-10-09 | 瓮福（集团）有限责任公司 | Crude iodine purifying process |
| CN104671209A (en) * | 2013-11-27 | 2015-06-03 | 天津市艾碘科技有限公司 | Method for sublimating industrial crude iodine |
| CN109336054A (en) * | 2018-12-20 | 2019-02-15 | 四川久大蓬莱盐化有限公司 | A method of recycling iodine from salt-making mother liquor |
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