CN107235474A - The method and its device of a kind of thick iodine purification - Google Patents
The method and its device of a kind of thick iodine purification Download PDFInfo
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- CN107235474A CN107235474A CN201710633711.6A CN201710633711A CN107235474A CN 107235474 A CN107235474 A CN 107235474A CN 201710633711 A CN201710633711 A CN 201710633711A CN 107235474 A CN107235474 A CN 107235474A
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- 229910052740 iodine Inorganic materials 0.000 title claims abstract description 182
- 239000011630 iodine Substances 0.000 title claims abstract description 182
- ZCYVEMRRCGMTRW-UHFFFAOYSA-N 7553-56-2 Chemical compound [I] ZCYVEMRRCGMTRW-UHFFFAOYSA-N 0.000 title claims abstract description 180
- 238000000034 method Methods 0.000 title claims abstract description 31
- 238000000746 purification Methods 0.000 title claims abstract description 30
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 77
- 238000003723 Smelting Methods 0.000 claims abstract description 45
- 238000007670 refining Methods 0.000 claims abstract description 30
- 230000008929 regeneration Effects 0.000 claims abstract description 20
- 238000011069 regeneration method Methods 0.000 claims abstract description 20
- 238000009834 vaporization Methods 0.000 claims abstract description 14
- 230000008016 vaporization Effects 0.000 claims abstract description 13
- 238000007689 inspection Methods 0.000 claims abstract description 6
- 238000007711 solidification Methods 0.000 claims abstract description 6
- 230000008023 solidification Effects 0.000 claims abstract description 6
- 239000007788 liquid Substances 0.000 claims description 85
- 238000001514 detection method Methods 0.000 claims description 19
- 230000008018 melting Effects 0.000 claims description 9
- 238000002844 melting Methods 0.000 claims description 9
- 238000002156 mixing Methods 0.000 claims description 6
- NIDNOXCRFUCAKQ-UMRXKNAASA-N (1s,2r,3s,4r)-bicyclo[2.2.1]hept-5-ene-2,3-dicarboxylic acid Chemical compound C1[C@H]2C=C[C@@H]1[C@H](C(=O)O)[C@@H]2C(O)=O NIDNOXCRFUCAKQ-UMRXKNAASA-N 0.000 claims 1
- 238000002360 preparation method Methods 0.000 abstract description 19
- 239000002245 particle Substances 0.000 abstract description 3
- 239000000126 substance Substances 0.000 abstract description 2
- 230000000052 comparative effect Effects 0.000 description 18
- 239000000047 product Substances 0.000 description 18
- PNDPGZBMCMUPRI-UHFFFAOYSA-N iodine Chemical compound II PNDPGZBMCMUPRI-UHFFFAOYSA-N 0.000 description 15
- OKJPEAGHQZHRQV-UHFFFAOYSA-N iodoform Chemical compound IC(I)I OKJPEAGHQZHRQV-UHFFFAOYSA-N 0.000 description 8
- 238000004821 distillation Methods 0.000 description 6
- 239000000110 cooling liquid Substances 0.000 description 5
- 238000005406 washing Methods 0.000 description 5
- 238000001816 cooling Methods 0.000 description 4
- 239000012530 fluid Substances 0.000 description 4
- 210000001685 thyroid gland Anatomy 0.000 description 4
- 239000002699 waste material Substances 0.000 description 4
- 239000000919 ceramic Substances 0.000 description 3
- 238000009833 condensation Methods 0.000 description 3
- 230000005494 condensation Effects 0.000 description 3
- 238000002309 gasification Methods 0.000 description 3
- 238000004806 packaging method and process Methods 0.000 description 3
- 230000000737 periodic effect Effects 0.000 description 3
- 238000003860 storage Methods 0.000 description 3
- 102100037328 Chitotriosidase-1 Human genes 0.000 description 2
- 206010018498 Goitre Diseases 0.000 description 2
- 101000879661 Homo sapiens Chitotriosidase-1 Proteins 0.000 description 2
- 229910021612 Silver iodide Inorganic materials 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 210000002421 cell wall Anatomy 0.000 description 2
- 238000004140 cleaning Methods 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 230000018044 dehydration Effects 0.000 description 2
- 238000006297 dehydration reaction Methods 0.000 description 2
- 239000000645 desinfectant Substances 0.000 description 2
- 238000007599 discharging Methods 0.000 description 2
- 239000003814 drug Substances 0.000 description 2
- 239000000975 dye Substances 0.000 description 2
- 201000003872 goiter Diseases 0.000 description 2
- XMBWDFGMSWQBCA-UHFFFAOYSA-N hydrogen iodide Chemical compound I XMBWDFGMSWQBCA-UHFFFAOYSA-N 0.000 description 2
- 239000007791 liquid phase Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000003755 preservative agent Substances 0.000 description 2
- 230000002335 preservative effect Effects 0.000 description 2
- 239000000700 radioactive tracer Substances 0.000 description 2
- 238000007493 shaping process Methods 0.000 description 2
- 229940098465 tincture Drugs 0.000 description 2
- JKFYKCYQEWQPTM-UHFFFAOYSA-N 2-azaniumyl-2-(4-fluorophenyl)acetate Chemical compound OC(=O)C(N)C1=CC=C(F)C=C1 JKFYKCYQEWQPTM-UHFFFAOYSA-N 0.000 description 1
- 241000251468 Actinopterygii Species 0.000 description 1
- 101000800133 Homo sapiens Thyroglobulin Proteins 0.000 description 1
- 206010067997 Iodine deficiency Diseases 0.000 description 1
- 241000124008 Mammalia Species 0.000 description 1
- 241001465754 Metazoa Species 0.000 description 1
- 230000001476 alcoholic effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000007664 blowing Methods 0.000 description 1
- 229910052729 chemical element Inorganic materials 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 230000006835 compression Effects 0.000 description 1
- 238000007906 compression Methods 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000013399 early diagnosis Methods 0.000 description 1
- 239000000839 emulsion Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000005496 eutectics Effects 0.000 description 1
- 235000013373 food additive Nutrition 0.000 description 1
- 239000002778 food additive Substances 0.000 description 1
- 239000003292 glue Substances 0.000 description 1
- 230000012010 growth Effects 0.000 description 1
- 229910052736 halogen Inorganic materials 0.000 description 1
- 150000002367 halogens Chemical class 0.000 description 1
- 102000047688 human TG Human genes 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- ICIWUVCWSCSTAQ-UHFFFAOYSA-M iodate Chemical compound [O-]I(=O)=O ICIWUVCWSCSTAQ-UHFFFAOYSA-M 0.000 description 1
- 230000002083 iodinating effect Effects 0.000 description 1
- 235000006479 iodine deficiency Nutrition 0.000 description 1
- 230000004060 metabolic process Effects 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- NALMPLUMOWIVJC-UHFFFAOYSA-N n,n,4-trimethylbenzeneamine oxide Chemical compound CC1=CC=C([N+](C)(C)[O-])C=C1 NALMPLUMOWIVJC-UHFFFAOYSA-N 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000001172 regenerating effect Effects 0.000 description 1
- 239000013535 sea water Substances 0.000 description 1
- 229940045105 silver iodide Drugs 0.000 description 1
- 229940032753 sodium iodate Drugs 0.000 description 1
- 235000015281 sodium iodate Nutrition 0.000 description 1
- 239000011697 sodium iodate Substances 0.000 description 1
- 239000013589 supplement Substances 0.000 description 1
- 238000002560 therapeutic procedure Methods 0.000 description 1
- 239000011573 trace mineral Substances 0.000 description 1
- 235000013619 trace mineral Nutrition 0.000 description 1
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
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (AREA)
- Manufacture And Refinement Of Metals (AREA)
Abstract
The present invention relates to chemical products field of refinement, the method and its device of more particularly to a kind of thick iodine purification；A kind of method of thick iodine purification in the present invention, comprises the following steps：Liquefaction, taste quality inspection, vaporization process, secondary liquefaction and its solidification；A kind of device of thick iodine purification in the present invention, including regeneration of sulfuric acid device (1), iodine smelting furnace (3), tower of refining (4), cooler (5) and condenser (6)；The smart iodine prepared by the inventive method and its device, outward appearance is regular, and particle is thick, and purity can reach 99.90%~99.99%, in whole preparation process, and the loss late of iodine is reduced to 1.45%~1.78%, effectively raises the purification rate of thick iodine.
Description
Technical field
The present invention relates to chemical products field of refinement, the method and its device of more particularly to a kind of thick iodine purification.
Background technology
Iodine is one of essential trace element of human body, the title for having " intelligence element ", and iodine is extremely heavy to the life of animals and plants
Want, the iodide and iodate in seawater enter most of marine growths metabolism in, in higher mammals, iodine with
Amino-acid iodide form is concentrated in thyroid gland, and Thyroid Gland Swell can be caused by lacking iodine, and about 2/3 iodine and compound are used for making
Standby preservative, disinfectant and medicine, such as tincture of iodine and iodoform CHI3, sodium iodate supplement Iodine intake deficiency as food additives,
Iodine radioisotope -131 is used for radiation treatment and Radioactive tracer techniques, and iodine can be additionally used in manufacture dyestuff and glue of photographing
Piece, iodine and its related compound are mainly used in medicine, photograph and dyestuff, and it is alternatively arranged as tracer, carries out the monitoring of system, example
Such as it is used to geothermal system monitor.Silver iodide (AgI) can be made to make cloud during rain making in addition to the emulsion as photographic negative, also
Crystal seed.I2 and KI alcoholic solution is the tincture of iodine, is conventional disinfectant；Iodoform (CHI3) is used as preservative, and iodine and the mankind's is strong
Health is closely bound up, the iodine containing 20-50mg in adult human body, and iodine is to maintain element necessary to human thyroglobulin normal function,
Goitre will be suffered from when human body iodine deficiency, therefore iodide can prevent and treat Thyroid Gland Swell, eat sea-tangle, ocean fish etc. more
The food enriched containing iodine, also very effective for preventing and treating Thyroid Gland Swell, the radio isotope 131I of iodine can be used for goitre
The total amount of iodine in the early diagnosis and therapy of knurl, health adult's body is about 30mg (20~50mg), wherein 70%~80% deposits
In Thyreoidine.
Because the utilization of iodine is more and more extensive, requirement to the purity of iodine also more and more higher, the demand of smart iodine increasingly increases
Greatly, iodine is No. 53 elements of the periodic table of elements, and it is one of halogen that the A races of 5 periodic system VII are located in the periodic table of chemical element, single
Matter iodine is in atropurpureus crystal, easily distillation, is easily sublimated after distillation, so being used in terms of the method and its device of traditional thick iodine purification
Be exactly iodine this characteristic, such as application number 200810068752.6《A kind of method of refining industrial coarse iodine》Disclose a kind of work
The method of the thick iodinating and refining of industry, it is raw material for 70%~95% industrial coarse iodine to use content, is added to equipped with the concentrated sulfuric acid, thermometric dress
Put in the sublimator with gas blowing out device, control crystallization apparatus environment temperature is to 20 DEG C, and sublimator is first heated to 60 DEG C~90
DEG C, flowed into flow velocity for the iodine that 8~15L/MIN gas goes out distillation in crystallizer, keeping will distillation after 40MIN~60MIN
Device is heated to 160 DEG C~200 DEG C, and adjusting gas flow to 1~1.5L/MIN continues to collect remaining iodine；And for example application number
201320419837.0《A kind of crude iodine purification device》A kind of crude iodine purification device is disclosed, it includes reactive moieties, sublimate portion
Divide and washing part；Wherein reactive moieties are made up of ceramic reactor (2), and the ceramic reactor (2) is connected with air compression
Machine (4), the outside of the ceramic reactor (2) is provided with jacket type heater；The part of sublimating is made up of device of sublimating (1),
The bottom of the device of sublimating (1) is provided with product storage tank (6)；It is described washing part by washing tank (3), cleaning solution make-up tank (5) and
Cleaning solution storage tank (7) is constituted；The washing tank (3) has pipeline to be connected to the outlet of device of sublimating (1), the gas of the washing tank (3)
Body outlet is connected with blower fan (9), it is seen that current method of purification and its device are all the easy distillations using iodine, are easily sublimated after distillation
The characteristics of, be all by first allowing after thick iodine distils, then purification of sublimating thinking, but among actual production process, thick iodine liter
Speed and efficiency magnificent and sublimate are to be difficult to meet industrial production demand, meanwhile, the iodine product mostly powder for acquisition of sublimating
Shape is short grained, and specific surface area is big, and solution distils again in packaging and storing process, causes loss, meanwhile, charging,
There is great difficulty in discharging, packaging etc., the discharging for smart iodine of especially sublimating and packaging, and air is used in existing apparatus by sublimed iodine
Bring device of sublimating into sublimate, wherein being mingled with the ektogenic of air so that the reliability of finished product essence iodine has hidden danger, can
See, also there are more or less shortcoming in the method and its device of current thick iodine purification has much room for improvement.
The content of the invention
The present invention is in order to solve the above technical problems, there is provided the method and its device of a kind of thick iodine purification.
Realized particular by following technical scheme：
A kind of method of thick iodine purification, is by 1 in iodine smelting furnace by thick iodine and the concentrated sulfuric acid:0~2 mass ratio mixing,
Congruent melting is liquefied at 100~140 DEG C, and the liquid level for keeping liquid iodophor is 5~30 times of liquid iodophor outlet caliber, the inspection sampled
Survey, taste >=98% of the liquid iodophor after detection fusing is heated to 190~210 DEG C, liquid iodophor is vaporized, vapour
The iodine steam produced after change cooling liquid at a temperature of 100~120 DEG C, to iodine vapor all liquefaction, then the cooling solidification that cools
Change obtains smart iodine；The taste ＜ 98% of liquid iodophor after detection, regeneration of sulfuric acid is returned by the liquid iodophor in iodine smelting furnace and the concentrated sulfuric acid
Device, is recycled in iodine smelting furnace, operates repeatedly, obtains smart iodine.
The method of the present invention is further illustrated by following device flow：
A kind of device of thick iodine purification, including regeneration of sulfuric acid device (1), iodine smelting furnace (3), tower of refining (4), cooler (5) with
And condenser (6), described regeneration of sulfuric acid device (1) is connected by entering sour pump (2) with iodine smelting furnace (3)；Described iodine smelting furnace (3)
Bottom opens up three outlets, and iodine smelting furnace (3) is connected with the top of tower of refining (4) by stop valve (9), described cooler
(5) bottom is connected by stop valve (10) with condenser (6) top.
Described iodine smelting furnace (3), one end and regeneration of sulfuric acid device (1) are connected conveying liquid iodophor by stop valve (7), another
End is connected the conveying concentrated sulfuric acid with regeneration of sulfuric acid device (1) by stop valve (8).
Described tower of refining (4), below charging aperture, there is provided sieve plate (11), in bottom there is provided fluidized bed furnace (12).
In summary, the beneficial effects of the present invention are：The smart iodine prepared by the inventive method and its device, outward appearance rule
Whole, particle is thick, and purity can reach 99.90%~99.99%, in whole preparation process, and the loss late of iodine is reduced to
1.45%~1.78%, effectively raise the purification rate of thick iodine, it is to avoid distillation-solidifyingization one that traditional thick iodine purification is used
The way of step in place, solves reaction rate and efficiency in distillation-solidifyingization and is difficult to industrialized defect, this method and its device
The specific surface area of smart iodine is increased, it is instant packed, it is to avoid the little particle of traditional preparation or powdered smart iodine are direct in storage
Distil the wasting of resources caused.
Brief description of the drawings
Fig. 1：For the schematic flow sheet of the present invention；
1- regeneration of sulfuric acid devices；2- enters sour pump；3- iodine smelting furnaces；4- refines tower；5- coolers；6- condensers；7~10- ends
Valve；11- sieve plates；12- fluidized bed furnaces；
Fig. 2：For the connection diagram of iodine smelting furnace：
3- iodine smelting furnaces；7~9- stop valves.
Fig. 3：For the structural representation for tower of refining；
4- refines tower；11- sieve plates；12- fluidized bed furnaces.
Embodiment
Describe the present invention in detail with reference to the accompanying drawings and examples.
Fig. 1：For the present invention schematic flow sheet, the device include regeneration of sulfuric acid device (1), iodine smelting furnace (3), tower of refining (4),
Cooler (5) and condenser (6), described regeneration of sulfuric acid device (1) are connected by entering sour pump (2) with iodine smelting furnace (3)；It is described
Iodine smelting furnace (3) bottom open up three outlets, iodine smelting furnace (3) is connected with the top of tower of refining (4) by stop valve (9), iodine
Smelting furnace (3) and regeneration of sulfuric acid device (1) are connected conveying liquid iodophor, iodine smelting furnace (3) and regeneration of sulfuric acid device (1) by stop valve (7)
It is connected the conveying concentrated sulfuric acid by stop valve (8), described tower of refining (4), below charging aperture, there is provided sieve plate (11),
Bottom is provided with fluidized bed furnace (12), and described cooler (5) bottom is connected by stop valve (10) with condenser (6) top.
The method and step purified using said apparatus to thick iodine is as follows：
Thick iodine and the concentrated sulfuric acid are pressed 1 in iodine smelting furnace:1.2~2 mass ratio mixing, the eutectic liquids at 100~140 DEG C
Change, the liquid level for keeping liquid iodophor is 5~30 times of liquid iodophor outlet caliber, the inspection sampled to the liquid iodophor after liquefaction
Survey, taste >=98% of the liquid iodophor after detection fusing is heated to 190~210 DEG C, liquid iodophor is vaporized, vapour
The iodine steam produced after change cooling liquid at a temperature of 100~120 DEG C, to iodine vapor all liquefaction, then the cooling solidification that cools
Change obtains smart iodine；The taste ＜ 98% of liquid iodophor after detection, regeneration of sulfuric acid is returned by the liquid iodophor in iodine smelting furnace and the concentrated sulfuric acid
Device, is recycled in iodine smelting furnace, operates repeatedly, obtains smart iodine.
Specific description is done to the present invention below by several specific embodiments.
Embodiment 1
Thick iodine and the concentrated sulfuric acid are pressed 1 in iodine smelting furnace:1.2 mass ratio mixing, congruent melting is liquefied at 100 DEG C, keeps liquid
The liquid level of state iodine is 5 times of liquid iodophor outlet caliber, the detection sampled to the liquid iodophor after liquefaction, after detection fusing
Taste >=98% of liquid iodophor, is heated to 190 DEG C, liquid iodophor is vaporized, and the iodine steam produced after vaporization is 100
Cooling liquid at a temperature of DEG C, to iodine vapor all liquefaction, then the condensation cured that cools obtains smart iodine；Liquid iodophor after detection
＜ 98% is sampled, the liquid iodophor in iodine smelting furnace and the concentrated sulfuric acid are returned into regeneration of sulfuric acid device, is recycled in iodine smelting furnace, operates repeatedly,
Obtain smart iodine.
The purity of obtained smart iodine finished product is that the iodine loss rate in 99.90%, whole preparation process is 1.73% after testing.
Embodiment 2
Thick iodine and the concentrated sulfuric acid are pressed 1 in iodine smelting furnace:2 mass ratio mixing, congruent melting is liquefied at 140 DEG C, keeps liquid
The liquid level of iodine is 30 times of liquid iodophor outlet caliber, the detection sampled to the liquid iodophor after liquefaction, after detection fusing
Taste >=98% of liquid iodophor, is heated to 210 DEG C, liquid iodophor is vaporized, and the iodine steam produced after vaporization is 120
Cooling liquid at a temperature of DEG C, to iodine vapor all liquefaction, then the condensation cured that cools obtains smart iodine；Liquid iodophor after detection
＜ 98% is sampled, the liquid iodophor in iodine smelting furnace and the concentrated sulfuric acid are returned into regeneration of sulfuric acid device, is recycled in iodine smelting furnace, operates repeatedly,
Obtain smart iodine.
The purity of obtained smart iodine finished product is that the iodine loss rate in 99.95%, whole preparation process is 1.78% after testing.
Embodiment 3
Thick iodine and the concentrated sulfuric acid are pressed 1 in iodine smelting furnace:1.6 mass ratio mixing, congruent melting is liquefied at 120 DEG C, keeps liquid
The liquid level of state iodine is 18 times of liquid iodophor outlet caliber, the detection sampled to the liquid iodophor after liquefaction, after detection fusing
Liquid iodophor taste >=98%, be heated to 200 DEG C, liquid iodophor be vaporized, the iodine steam produced after vaporization exists
Cooling liquid at a temperature of 110 DEG C, to iodine vapor all liquefaction, then the condensation cured that cools obtains smart iodine；Liquid after detection
The taste ＜ 98% of iodine, returns to regeneration of sulfuric acid device by the liquid iodophor in iodine smelting furnace and the concentrated sulfuric acid, is recycled in iodine smelting furnace, grasps repeatedly
Make, obtain smart iodine.
The purity of obtained smart iodine finished product is that the iodine loss rate in 99.99%, whole preparation process is 1.45% after testing.
Embodiment 4
By thick iodine, congruent melting is liquefied at 100 DEG C in iodine smelting furnace, and the liquid iodophor after liquefaction is squeezed into using force (forcing) pump and refined
Tower, it is 240 DEG C to improve temperature in tower bottom of refining, and realizes the gasification of liquid iodophor, tower top of refining is provided with expanding reach, is set in it
Liquid iodophor is put every liquid baffle plate and leakage fluid dram, liquid iodophor is realized by the high temperature for tower bottom of refining to gasify, and gaseous iodine ascends into expansion
Big section, by carrying out liquid-phase collection every the space of liquid baffle plate and the formation of expanding reach cell wall after liquefaction, obtains secondary liquefied smart iodine,
Secondary liquefied liquid iodophor escapes and enter cooling and shaping device by tower leakage fluid dram of refining and obtains the smart iodine of finished product；
The purity of obtained smart iodine finished product is that the iodine loss rate in 99.96%, whole preparation process is 1.68% after testing.
Embodiment 5
By thick iodine, congruent melting is liquefied at 120 DEG C in iodine smelting furnace, and the liquid iodophor after liquefaction is squeezed into using force (forcing) pump and refined
Tower, it is 220 DEG C to improve temperature in tower bottom of refining, and realizes the gasification of liquid iodophor, tower top of refining is provided with expanding reach, is set in it
Liquid iodophor is put every liquid baffle plate and leakage fluid dram, liquid iodophor is realized by the high temperature for tower bottom of refining to gasify, and gaseous iodine ascends into expansion
Big section, by carrying out liquid-phase collection every the space of liquid baffle plate and the formation of expanding reach cell wall after liquefaction, obtains secondary liquefied smart iodine,
Secondary liquefied liquid iodophor escapes and enter cooling and shaping device by tower leakage fluid dram of refining and obtains the smart iodine of finished product；
The purity of obtained smart iodine finished product is that the iodine loss rate in 99.94%, whole preparation process is 1.77% after testing.
Comparative example 1
The sieve plate of the bottom of the charging aperture of tower of refining in embodiment 1~3 is 2 layers, right at this by taking embodiment 1 as an example
In ratio, the sieve plate of the bottom of the charging aperture for tower of refining is set to 3 layers.
The purity of obtained smart iodine finished product is that the iodine loss rate in 99.98%, whole preparation process is 1.82% after testing.
Comparative example 2
The sieve plate of the bottom of the charging aperture of tower of refining in embodiment 1~3 is 2 layers, right at this by taking embodiment 1 as an example
In ratio, the sieve plate of the bottom of the charging aperture for tower of refining is set to 5 layers.
The purity of obtained smart iodine finished product is that the iodine loss rate in 99.99%, whole preparation process is 1.95% after testing.
Comparative example 3
In embodiment 1~3, the method for thick iodine purification is that-secondary liquefaction-solidifies to obtain finished product according to thick iodine solution-vaporization
Processing step carry out, by taking embodiment 1 as an example, the method that the purification of thick iodine is adjusted in this comparative example is according to thick iodine solution-vapour
Change-secondary liquefaction-- three liquefaction of secondary vaporizing-solidify the processing step of finished product is carried out.
The purity of obtained smart iodine finished product is that the iodine loss rate in 99.99%, whole preparation process is 2.12% after testing.
Comparative example 4
The detection sampled in embodiment 1~3 to the liquid iodophor after liquefaction in iodine smelting furnace, the liquid after detection fusing
Taste >=98% of iodine, i.e., deliver to liquid iodophor tower vaporization of refining, if the taste ＜ 98% of liquid iodophor, by the concentrated sulfuric acid and liquid
Iodine is delivered to be repeated in regeneration of sulfuric acid device, by taking embodiment 1 as an example, in this comparative example, when the liquid iodophor for detecting iodine smelting furnace
Taste >=98.3%, could deliver to liquid iodophor tower vaporization of refining.
The purity of obtained smart iodine finished product is that the iodine loss rate in 99.95%, whole preparation process is 1.88% after testing.
Comparative example 5
The detection sampled in embodiment 1~3 to the liquid iodophor after liquefaction in iodine smelting furnace, the liquid after detection fusing
Taste >=98% of iodine, i.e., deliver to liquid iodophor tower vaporization of refining, if the taste ＜ 98% of liquid iodophor, by the concentrated sulfuric acid and liquid
Iodine is delivered to be repeated in regeneration of sulfuric acid device, by taking embodiment 1 as an example, in this comparative example, when the liquid iodophor for detecting iodine smelting furnace
Taste >=98.5%, could deliver to liquid iodophor tower vaporization of refining.
The purity of obtained smart iodine finished product is that the iodine loss rate in 99.99%, whole preparation process is 2.05% after testing.
As a result illustrate, table 1 is the purity of smart iodine prepared by embodiment 1~5 and comparative example 1~5 and entirely prepared
The loss late of iodine in journey.
Table 1
| Project | Purity % | Iodine loss rate % |
| Embodiment 1 | 99.90 | 1.73 |
| Embodiment 2 | 99.95 | 1.78 |
| Embodiment 3 | 99.99 | 1.45 |
| Embodiment 4 | 99.96 | 1.68 |
| Embodiment 5 | 99.94 | 1.77 |
| Comparative example 1 | 99.98 | 1.82 |
| Comparative example 2 | 99.99 | 1.95 |
| Comparative example 3 | 99.99 | 2.12 |
| Comparative example 4 | 99.95 | 1.88 |
| Comparative example 5 | 99.99 | 2.05 |
It can be seen that, embodiment 1~3 is to the addition of the concentrated sulfuric acid to carry out purification processes with thick iodine, and the addition concentrated sulfuric acid can be effective
The gasification loss of iodine is prevented and treated, and concentrated sulfuric acid density is less than liquid iodophor, as closed solution, can reduce the loss of iodine, this
Embodiment 1~3 is the addition concentrated sulfuric acid, is dehydrated using the dehydration property of the concentrated sulfuric acid, but after a period of time is reacted, the concentrated sulfuric acid
Its dehydration property will be lost by being diluted to after finite concentration, now be needed to change sulfuric acid or be carried out the concentrating regenerative again of sulfuric acid；
So it is accomplished by analyzing the quality for the iodine after melting furnace, further the purity of lifting iodine；Embodiment 4~5 does not add
Enriching sulfuric acid, using be that the iodine principle different from steam-laden vapour pressure is separated, at the corresponding temperature, go out melting furnace
Liquid iodophor without quality inspection, required purity can be reached；From the purity and whole preparation process of the smart iodine of preparation
In iodine loss rate from the point of view of, embodiment 1~5 is preferably to choose, and comparative example 1~2 is on the basis of embodiment 1, to have adjusted
Refine tower charging lower screen deck the number of plies, although the purity of smart iodine has been lifted, but is increased in whole preparation process
Iodine loss late, waste resource, also increase cost, comparative example 3 is the liquid that iodine is have adjusted on the basis of embodiment 1
Change number of times and vaporization number of times, although purity has been lifted, but increases the loss late of the iodine in whole preparation process, waste
Resource, also increases cost, comparative example 4~5 is that the discharge of liquid iodophor in iodine smelting furnace is have adjusted on the basis of embodiment 1
Taste, equally also effectively improves purity, but increases the loss late of the iodine in whole preparation process, wastes money
Source, also increases cost, it is seen that though comparative example 1~5 effectively improves purity, but increase in whole preparation process
The loss late of iodine, wastes resource, also increases cost.
Claims (9)
1. a kind of method of thick iodine purification, it is characterised in that this method is divided into following steps：Liquefaction, taste quality inspection, at vaporization
Reason, secondary liquefaction and its solidification.
2. the method for thick iodine purification as claimed in claim 1, it is characterised in that described liquefaction, being will be thick in iodine smelting furnace
Iodine and the concentrated sulfuric acid press 1:0~2 mass ratio mixing, congruent melting is liquefied at 100~140 DEG C.
3. the method for thick iodine purification as claimed in claim 1, it is characterised in that described taste quality inspection, dense applied to adding
Taste >=98% of liquid iodophor after the Operation for liquefaction that sulfuric acid is carried out, specifically detection fusing, you can enter next step process, if
The taste ＜ 98% of liquid iodophor after detection, that is, return to iodine smelting furnace and continue to purify.
4. the method for thick iodine purification as claimed in claim 2, it is characterised in that the liquid of described iodine smelting furnace, wherein liquid iodophor
Position is 5~30 times of liquid iodophor outlet caliber, when addition sulfuric acid is liquefied, and sulfuric acid liquid level is the 1.2~2 of liquid iodophor liquid level
Times.
5. the method for iodine purification as claimed in claim 1 thick, it is characterised in that described vaporization process, be by liquid iodophor by
Refine tower middle and upper part feeding, be heated to 190~210 DEG C, realize the vaporization of liquid iodophor.
6. the method for thick iodine purification as claimed in claim 1, it is characterised in that described secondary liquefaction and its solidification, vaporization
The iodine steam produced afterwards is discharged into cooler by top of tower of refining, and regulation chiller temperature is 100~120 DEG C, to iodine vapor
All after liquefaction, in feeding condenser, solidification obtains smart iodine.
7. a kind of device of thick iodine purification, it is characterised in that including regeneration of sulfuric acid device (1), iodine smelting furnace (3), tower of refining (4), cold
But device (5) and condenser (6), described regeneration of sulfuric acid device (1) are connected by entering sour pump (2) with iodine smelting furnace (3)；Described
Iodine smelting furnace (3) bottom opens up three outlets, and iodine smelting furnace (3) is connected with the top of tower of refining (4) by stop valve (9), described
Cooler (5) bottom be connected by stop valve (10) with condenser (6) top.
8. the device of thick iodine purification as claimed in claim 7, it is characterised in that described iodine smelting furnace (3), one end and sulfuric acid are again
Raw device (1) is connected conveying liquid iodophor by stop valve (7), and the other end is connected with regeneration of sulfuric acid device (1) by stop valve (8)
Convey the concentrated sulfuric acid.
9. the device of iodine purification as claimed in claim 7 thick, it is characterised in that described tower of refining (4), charging aperture with
Under, there is provided sieve plate (11), in bottom there is provided fluidized bed furnace (12).
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110954529A (en) * | 2019-11-04 | 2020-04-03 | 厦门市集美区乐安中学 | Iodine vapor fingerprint detection device |
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