CN107235474B - Method and device for purifying crude iodine - Google Patents
Method and device for purifying crude iodine Download PDFInfo
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- CN107235474B CN107235474B CN201710633711.6A CN201710633711A CN107235474B CN 107235474 B CN107235474 B CN 107235474B CN 201710633711 A CN201710633711 A CN 201710633711A CN 107235474 B CN107235474 B CN 107235474B
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- 239000011630 iodine Substances 0.000 title claims abstract description 223
- 229910052740 iodine Inorganic materials 0.000 title claims abstract description 223
- ZCYVEMRRCGMTRW-UHFFFAOYSA-N 7553-56-2 Chemical compound [I] ZCYVEMRRCGMTRW-UHFFFAOYSA-N 0.000 title claims abstract description 221
- 238000000034 method 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 69
- 238000002844 melting Methods 0.000 claims abstract description 37
- 230000008018 melting Effects 0.000 claims abstract description 37
- PNDPGZBMCMUPRI-UHFFFAOYSA-N iodine Chemical compound II PNDPGZBMCMUPRI-UHFFFAOYSA-N 0.000 claims abstract description 29
- 238000007670 refining Methods 0.000 claims abstract description 25
- 230000008016 vaporization Effects 0.000 claims abstract description 21
- 238000009834 vaporization Methods 0.000 claims abstract description 13
- 238000000746 purification Methods 0.000 claims abstract description 11
- 238000007689 inspection Methods 0.000 claims abstract description 5
- 230000008023 solidification Effects 0.000 claims abstract 4
- 238000007711 solidification Methods 0.000 claims abstract 4
- 239000007788 liquid Substances 0.000 claims description 94
- 230000005496 eutectics Effects 0.000 claims description 8
- 238000007599 discharging Methods 0.000 claims description 3
- 238000005243 fluidization Methods 0.000 claims 1
- 238000002360 preparation method Methods 0.000 abstract description 19
- 239000011362 coarse particle Substances 0.000 abstract description 2
- 239000000126 substance Substances 0.000 abstract description 2
- 230000000052 comparative effect Effects 0.000 description 20
- 239000000047 product Substances 0.000 description 17
- 238000001816 cooling Methods 0.000 description 12
- 238000001514 detection method Methods 0.000 description 10
- 238000005406 washing Methods 0.000 description 7
- 238000006243 chemical reaction Methods 0.000 description 6
- 238000010438 heat treatment Methods 0.000 description 6
- 238000002309 gasification Methods 0.000 description 5
- 238000002156 mixing Methods 0.000 description 5
- 238000000926 separation method Methods 0.000 description 5
- 238000000859 sublimation Methods 0.000 description 5
- 230000008022 sublimation Effects 0.000 description 5
- 230000009967 tasteless effect Effects 0.000 description 5
- 206010018498 Goitre Diseases 0.000 description 4
- 238000003723 Smelting Methods 0.000 description 4
- 201000003872 goiter Diseases 0.000 description 4
- 238000003860 storage Methods 0.000 description 4
- 239000002253 acid Substances 0.000 description 3
- 239000000919 ceramic Substances 0.000 description 3
- 230000018044 dehydration Effects 0.000 description 3
- 238000006297 dehydration reaction Methods 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 238000004806 packaging method and process Methods 0.000 description 3
- 210000001685 thyroid gland Anatomy 0.000 description 3
- 229910021612 Silver iodide Inorganic materials 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 238000009833 condensation Methods 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 239000000645 desinfectant Substances 0.000 description 2
- 239000003814 drug Substances 0.000 description 2
- 229940079593 drug Drugs 0.000 description 2
- 239000000975 dye Substances 0.000 description 2
- 235000013305 food Nutrition 0.000 description 2
- 150000004694 iodide salts Chemical class 0.000 description 2
- OKJPEAGHQZHRQV-UHFFFAOYSA-N iodoform Chemical compound IC(I)I OKJPEAGHQZHRQV-UHFFFAOYSA-N 0.000 description 2
- 239000007791 liquid phase Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000012544 monitoring process Methods 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 239000003755 preservative agent Substances 0.000 description 2
- 238000005086 pumping Methods 0.000 description 2
- PNDPGZBMCMUPRI-HVTJNCQCSA-N 10043-66-0 Chemical compound [131I][131I] PNDPGZBMCMUPRI-HVTJNCQCSA-N 0.000 description 1
- 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
- 241000512259 Ascophyllum nodosum Species 0.000 description 1
- 102100037328 Chitotriosidase-1 Human genes 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 101000879661 Homo sapiens Chitotriosidase-1 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
- 208000024770 Thyroid neoplasm Diseases 0.000 description 1
- 150000001413 amino acids Chemical class 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000007664 blowing Methods 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 238000013399 early diagnosis Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 235000013373 food additive Nutrition 0.000 description 1
- 239000002778 food additive Substances 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
- 235000006479 iodine deficiency Nutrition 0.000 description 1
- 230000004060 metabolic process Effects 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
- 230000002335 preservative effect Effects 0.000 description 1
- 230000002285 radioactive effect Effects 0.000 description 1
- 238000001959 radiotherapy Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 229920006395 saturated elastomer Polymers 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
- 230000009897 systematic effect Effects 0.000 description 1
- 208000013076 thyroid tumor Diseases 0.000 description 1
- 239000011573 trace mineral Substances 0.000 description 1
- 235000013619 trace mineral Nutrition 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 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 invention relates to the field of chemical product refining, in particular to a method and a device for purifying crude iodine; the invention relates to a method for purifying crude iodine, which comprises the following steps: liquefying, quality inspection, vaporization treatment, secondary liquefying and solidification; the invention relates to a device for purifying crude iodine, which comprises a sulfuric acid regenerator (1), an iodine melting furnace (3), a refining tower (4), a cooler (5) and a condenser (6); the refined iodine prepared by the method and the device has regular appearance, coarse particles and purity up to 99.90-99.99%, and the loss rate of iodine is reduced to 1.45-1.78% in the whole preparation process, so that the purification rate of the crude iodine is effectively improved.
Description
Technical Field
The invention relates to the field of chemical product refining, in particular to a method and a device for purifying crude iodine.
Background
Iodine is one of the essential trace elements of the human body, known as "intellectual elements", iodine is extremely important for life of animals and plants, iodides and iodate in sea water enter metabolism of most marine organisms, iodine is concentrated in thyroid glands in the form of iodinated amino acids, in advanced mammals, iodine deficiency causes goiter, about 2/3 of iodine and compounds are used for preparing preservatives, disinfectants and medicines, such as iodine tincture and iodic CHI3, sodium iodate supplements the insufficient intake of iodine as food additives, radioisotope iodine-131 is used for radiotherapy and radioactive tracing technology, iodine can also be used for manufacturing dyes and photographic films, iodine and related compounds thereof are mainly used for medicines, photographs and dyes, and can also be used as tracers for systematic monitoring, such as geothermal system monitoring. Silver iodide (AgI) can be used as a sensitizer for photographic negative, and also as seed crystal for cloud formation during artificial rainfall. Alcohol solutions of I2 and KI, i.e., iodine, are commonly used disinfectants; the iodized imitation (CHI 3) is used as a preservative, iodine is closely related to human health, the adult contains 20-50mg of iodine, the iodine is an element necessary for maintaining normal functions of thyroid gland of human body, when the human body lacks iodine, the human body suffers from goiter, so that the iodine can prevent and treat goiter, and the iodine-rich foods such as kelp and sea fish are eaten much, the iodine-rich foods are also effective for preventing and treating goiter, the radioisotope 131I of iodine can be used for early diagnosis and treatment of thyroid tumor, and the total amount of iodine in the healthy adult is about 30mg (20-50 mg), wherein 70% -80% of the iodine exists in thyroid gland.
The method is characterized in that the traditional method for purifying crude iodine and the device thereof are used, such as application number 200810068752.6 'a method for refining industrial crude iodine', discloses a method for refining industrial crude iodine, which adopts industrial crude iodine with the content of 70-95% as a raw material, and adds the industrial crude iodine into a sublimator provided with concentrated sulfuric acid, a temperature measuring device and a gas blowing device, the environment temperature of a crystallization device is controlled to 20 ℃, the sublimator is firstly heated to 60-90 ℃, the sublimator is enabled to flow into a crystallizer by using gas with the flow rate of 8-15L/MIN, the sublimator is heated to 160-200 ℃ after the MIN is kept at 40-60 MIN, the gas flow rate is adjusted to 1-1.5L/MIN, and the rest iodine is continuously collected; as another example, application number 201320419837.0, "a crude iodine purification apparatus", discloses a crude iodine purification apparatus comprising a reaction section, a desublimation section, and a washing section; the reaction part consists of a ceramic reaction kettle (2), wherein the ceramic reaction kettle (2) is connected with an air compressor (4), and a jacket type heating device is arranged outside the ceramic reaction kettle (2); the desublimation part consists of a desublimation device (1), and a product storage tank (6) is arranged at the bottom of the desublimation device (1); the washing part consists of a washing tank (3), a washing liquid preparation tank (5) and a washing liquid storage tank (7); the washing tank (3) is provided with a pipeline connected to the outlet of the desublimation device (1), the gas outlet of the washing tank (3) is connected with a fan (9), the characteristics of easy sublimation of iodine and easy desublimation after sublimation are utilized in the existing purification method and the device, the thought of sublimation and desublimation of crude iodine is utilized, but in the actual production process, the sublimation and desublimation rate and efficiency of the crude iodine are difficult to meet the industrial production requirement, meanwhile, the obtained iodine product is mostly in powder or small particle form, the specific surface area is large, the solution sublimates again in the packaging and storage processes, the loss is caused, meanwhile, great difficulties exist in feeding, discharging, packaging and the like, especially the discharging and packaging of desublimation refined iodine are utilized in the existing device, the sublimated iodine is brought into the desublimation device by adopting air, the external components of the air, hidden danger exists in the quality reliability of the finished refined iodine, and the defects of the existing crude iodine is more or less and more or less improved in the existing purification method and the device are still present.
Disclosure of Invention
The invention provides a method and a device for purifying crude iodine to solve the technical problems.
The method is realized by the following technical scheme:
mixing crude iodine and concentrated sulfuric acid in a mass ratio of 1:0-2 in an iodine melting furnace, performing eutectic liquefaction at 100-140 ℃, keeping the liquid level of liquid iodine to be 5-30 times of the pipe diameter of a liquid iodine discharge port, detecting the taste of the melted liquid iodine to be more than or equal to 98%, heating to 190-210 ℃, vaporizing the liquid iodine, cooling and liquefying the vaporized iodine steam at 100-120 ℃ until the iodine steam is completely liquefied, and cooling, condensing and solidifying to obtain refined iodine; the detected liquid iodine has the taste less than 98 percent, the liquid iodine and concentrated sulfuric acid in the iodine melting furnace are returned to the sulfuric acid regenerator, and the liquid iodine and the concentrated sulfuric acid are circulated to the iodine melting furnace for repeated operation, thus obtaining the refined iodine.
The method of the invention is further illustrated by the following device flow:
the device for purifying the crude iodine comprises a sulfuric acid regenerator (1), an iodine melting furnace (3), a refining tower (4), a cooler (5) and a condenser (6), wherein the sulfuric acid regenerator (1) is connected with the iodine melting furnace (3) through an acid inlet pump (2); three outlets are formed in the bottom end of the iodine melting furnace (3), the iodine melting furnace (3) is connected with the upper portion of the refining tower (4) through a stop valve (9), and the bottom of the cooler (5) is connected with the upper portion of the condenser (6) through a stop valve (10).
The iodine melting furnace (3) is characterized in that one end of the iodine melting furnace is connected with the sulfuric acid regenerator (1) through a stop valve (7) to convey liquid iodine, and the other end of the iodine melting furnace is connected with the sulfuric acid regenerator (1) through a stop valve (8) to convey concentrated sulfuric acid.
The refining tower (4) is provided with a sieve plate (11) below the feed inlet, and a fluidized bed furnace (12) is arranged at the bottom.
In summary, the beneficial effects of the invention are as follows: the refined iodine prepared by the method and the device thereof has regular appearance, coarse particles, the purity can reach 99.90% -99.99%, the loss rate of iodine is reduced to 1.45% -1.78% in the whole preparation process, the purification rate of the crude iodine is effectively improved, the sublimation-condensation one-step in-place method adopted in the traditional crude iodine purification is avoided, the defect that the reaction rate and the efficiency are difficult to industrialize in the sublimation-condensation process is overcome, the specific surface area of the refined iodine is increased by the method and the device thereof, the package is convenient, and the resource waste caused by direct sublimation of small particles or powdery refined iodine prepared in the traditional process during storage is avoided.
Drawings
Fig. 1: is a flow diagram of the invention;
a 1-sulfuric acid regenerator; 2-acid feeding pump; 3-iodine smelter; 4-a refining tower; a 5-cooler; 6-a condenser; 7-10-stop valves; 11-sieve plates; 12-boiling furnace;
fig. 2: schematic diagram of connection of iodine smelter:
3-iodine smelter; 7-9-stop valve.
Fig. 3: is a structural schematic diagram of the refining tower;
4-a refining tower; 11-sieve plates; 12-fluidized bed furnace.
Detailed Description
The invention will be described in detail below with reference to the drawings and examples.
Fig. 1: the device comprises a sulfuric acid regenerator (1), an iodine melting furnace (3), a refining tower (4), a cooler (5) and a condenser (6), wherein the sulfuric acid regenerator (1) is connected with the iodine melting furnace (3) through an acid inlet pump (2); the utility model provides a three export is offered to iodine smelting pot (3) bottom, iodine smelting pot (3) are connected through stop valve (9) with the upper portion of refinement tower (4), iodine smelting pot (3) are connected through stop valve (7) with sulfuric acid regenerator (1) and carry liquid iodine, iodine smelting pot (3) are connected through stop valve (8) with sulfuric acid regenerator (1) and carry concentrated sulfuric acid, refinement tower (4), below the feed inlet, set up sieve (11), set up fluidized bed furnace (12) in the bottom, cooler (5) bottom be connected with condenser (6) upper portion through stop valve (10).
The method for purifying the crude iodine by adopting the device comprises the following steps:
mixing crude iodine and concentrated sulfuric acid in a mass ratio of 1:1.2-2 in an iodine melting furnace, performing eutectic liquefaction at 100-140 ℃, keeping the liquid level of liquid iodine to be 5-30 times of the pipe diameter of a liquid iodine discharge port, detecting the liquefied liquid iodine, detecting that the liquid iodine after melting is more than or equal to 98 percent in taste, heating to 190-210 ℃, vaporizing the liquid iodine, cooling and liquefying iodine steam generated after vaporization at 100-120 ℃ until the iodine steam is totally liquefied, and cooling, condensing and solidifying to obtain refined iodine; the detected liquid iodine has the taste less than 98 percent, the liquid iodine and concentrated sulfuric acid in the iodine melting furnace are returned to the sulfuric acid regenerator, and the liquid iodine and the concentrated sulfuric acid are circulated to the iodine melting furnace for repeated operation, thus obtaining the refined iodine.
The invention is illustrated by the following examples.
Example 1
Mixing crude iodine and concentrated sulfuric acid in a mass ratio of 1:1.2 in an iodine melting furnace, performing eutectic liquefaction at 100 ℃, keeping the liquid level of liquid iodine to be 5 times of the pipe diameter of a liquid iodine discharge port, detecting the taste of the liquefied liquid iodine, detecting that the taste of the liquefied liquid iodine is more than or equal to 98%, heating to 190 ℃, vaporizing the liquid iodine, cooling and liquefying iodine steam generated after vaporization at the temperature of 100 ℃, cooling, condensing and solidifying to obtain refined iodine after all the iodine steam is liquefied; the detected liquid iodine has the taste less than 98 percent, the liquid iodine and concentrated sulfuric acid in the iodine melting furnace are returned to the sulfuric acid regenerator, and the liquid iodine and the concentrated sulfuric acid are circulated to the iodine melting furnace for repeated operation, thus obtaining the refined iodine.
The purity of the finished product of refined iodine obtained by detection is 99.90 percent, and the iodine loss rate in the whole preparation process is 1.73 percent.
Example 2
Mixing crude iodine and concentrated sulfuric acid in a mass ratio of 1:2 in an iodine melting furnace, performing eutectic liquefaction at 140 ℃, keeping the liquid level of liquid iodine to be 30 times of the pipe diameter of a liquid iodine discharge port, detecting the taste of the liquefied liquid iodine, detecting that the taste of the melted liquid iodine is more than or equal to 98%, heating to 210 ℃, vaporizing the liquid iodine, cooling and liquefying iodine steam generated after vaporization at 120 ℃, cooling and solidifying the cooled and liquefied liquid iodine steam until the liquefied liquid iodine steam is completely liquefied, and obtaining refined iodine; the detected liquid iodine has the taste less than 98 percent, the liquid iodine and concentrated sulfuric acid in the iodine melting furnace are returned to the sulfuric acid regenerator, and the liquid iodine and the concentrated sulfuric acid are circulated to the iodine melting furnace for repeated operation, thus obtaining the refined iodine.
The purity of the finished product of refined iodine obtained by detection is 99.95 percent, and the iodine loss rate in the whole preparation process is 1.78 percent.
Example 3
Mixing crude iodine and concentrated sulfuric acid in a mass ratio of 1:1.6 in an iodine melting furnace, performing eutectic liquefaction at 120 ℃, keeping the liquid level of liquid iodine to be 18 times of the pipe diameter of a liquid iodine discharge port, detecting the taste of the liquefied liquid iodine, detecting that the taste of the liquefied liquid iodine is more than or equal to 98%, heating to 200 ℃, vaporizing the liquid iodine, cooling and liquefying iodine steam generated after vaporization at 110 ℃, cooling and solidifying to obtain refined iodine after all the iodine steam is liquefied; the detected liquid iodine has the taste less than 98 percent, the liquid iodine and concentrated sulfuric acid in the iodine melting furnace are returned to the sulfuric acid regenerator, and the liquid iodine and the concentrated sulfuric acid are circulated to the iodine melting furnace for repeated operation, thus obtaining the refined iodine.
The purity of the finished product of refined iodine obtained by detection is 99.99 percent, and the iodine loss rate in the whole preparation process is 1.45 percent.
Example 4
The method comprises the steps of (1) carrying out eutectic liquefaction on crude iodine at 100 ℃ in an iodine melting furnace, pumping liquefied liquid iodine into a refining tower by using a booster pump, increasing the temperature to 240 ℃ at the lower part of the refining tower, realizing gasification of the liquid iodine, arranging a liquid iodine liquid separation baffle and a liquid outlet in the upper part of the refining tower, realizing gasification of the liquid iodine by high temperature at the lower part of the refining tower, allowing gaseous iodine to rise into the expansion section, carrying out liquid phase collection on the liquefied liquid iodine through a space formed by the liquid separation baffle and the wall of the expansion section, and obtaining secondary liquefied refined iodine, wherein the secondary liquefied liquid iodine is discharged from the liquid outlet of the refining tower and enters a cooling shaper to obtain finished product refined iodine;
the purity of the finished product of refined iodine obtained by detection is 99.96 percent, and the iodine loss rate in the whole preparation process is 1.68 percent.
Example 5
The method comprises the steps of (1) carrying out eutectic liquefaction on crude iodine at 120 ℃ in an iodine melting furnace, pumping liquefied liquid iodine into a refining tower by using a booster pump, increasing the temperature to 220 ℃ at the lower part of the refining tower, realizing gasification of the liquid iodine, arranging a liquid iodine liquid separation baffle and a liquid outlet in the upper part of the refining tower, realizing gasification of the liquid iodine by high temperature at the lower part of the refining tower, allowing gaseous iodine to rise into the expansion section, carrying out liquid phase collection on the liquefied liquid iodine through a space formed by the liquid separation baffle and the wall of the expansion section, and obtaining secondary liquefied refined iodine, wherein the secondary liquefied liquid iodine is discharged from the liquid outlet of the refining tower and enters a cooling shaper to obtain finished product refined iodine;
the purity of the finished product of refined iodine obtained by detection is 99.94 percent, and the iodine loss rate in the whole preparation process is 1.77 percent.
Comparative example 1
In examples 1 to 3, the screen plate at the lower part of the inlet of the purifying column was 2 layers, and in this comparative example, the screen plate at the lower part of the inlet of the purifying column was 3 layers.
The purity of the finished product of refined iodine obtained by detection is 99.98 percent, and the iodine loss rate in the whole preparation process is 1.82 percent.
Comparative example 2
In examples 1 to 3, the screen plate at the lower part of the inlet of the purifying column was 2 layers, and in this comparative example, the screen plate at the lower part of the inlet of the purifying column was 5 layers.
The purity of the finished product of refined iodine obtained by detection is 99.99 percent, and the iodine loss rate in the whole preparation process is 1.95 percent.
Comparative example 3
In examples 1 to 3, the method of purifying crude iodine was performed according to the process steps of liquefying crude iodine, vaporizing, secondarily liquefying and solidifying to obtain a finished product, and in this comparative example, the method of purifying crude iodine was adjusted according to the process steps of liquefying crude iodine, vaporizing, secondarily liquefying, secondarily vaporizing, secondarily liquefying and solidifying to obtain a finished product.
The purity of the finished product of refined iodine obtained by detection is 99.99 percent, and the iodine loss rate in the whole preparation process is 2.12 percent.
Comparative example 4
In examples 1 to 3, the liquefied liquid iodine in the iodine melting furnace was detected to have a taste of 98% or more, that is, the liquefied liquid iodine was sent to the refinement tower for vaporization, and if the liquid iodine has a taste of 98%, concentrated sulfuric acid and liquid iodine were sent to the sulfuric acid regenerator for repeated operations, and in this comparative example, when the liquefied iodine in the iodine melting furnace was detected to have a taste of 98.3% or more, the liquid iodine was sent to the refinement tower for vaporization.
The purity of the finished product of refined iodine obtained by detection is 99.95 percent, and the iodine loss rate in the whole preparation process is 1.88 percent.
Comparative example 5
In examples 1 to 3, the liquefied liquid iodine in the iodine melting furnace was detected to have a taste of 98% or more, that is, the liquefied liquid iodine was sent to the purification column for vaporization, and if the liquid iodine has a taste of 98%, concentrated sulfuric acid and liquid iodine were sent to the sulfuric acid regenerator for repeated operations, and in this comparative example, when the liquefied iodine in the iodine melting furnace was detected to have a taste of 98.5% or more, the liquid iodine was sent to the purification column for vaporization.
The purity of the finished product of refined iodine obtained by detection is 99.99 percent, and the iodine loss rate in the whole preparation process is 2.05 percent.
The results show that table 1 shows the purity of the refined iodides prepared in examples 1 to 5 and comparative examples 1 to 5 and the loss rate of iodine during the whole preparation process.
TABLE 1
| Project | Purity% | Iodine loss rate% |
| Example 1 | 99.90 | 1.73 |
| Example 2 | 99.95 | 1.78 |
| Example 3 | 99.99 | 1.45 |
| Example 4 | 99.96 | 1.68 |
| Example 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 in examples 1 to 3, concentrated sulfuric acid and crude iodine are added for purification treatment, the concentrated sulfuric acid is added to effectively prevent gasification loss of iodine, and the concentrated sulfuric acid has a density lower than that of liquid iodine, and can be used as a closed solution to reduce loss of iodine, and in examples 1 to 3, concentrated sulfuric acid is added for dehydration by utilizing dehydration property of concentrated sulfuric acid, but after the concentrated sulfuric acid is reacted for a period of time, the concentrated sulfuric acid is diluted to a certain concentration and loses dehydration property, and at this time, sulfuric acid needs to be replaced or concentrated and regenerated again; therefore, the quality of the iodine after exiting the melting furnace needs to be analyzed, and the purity of the iodine is further improved; in examples 4 to 5, concentrated sulfuric acid is not added, separation is performed by utilizing the principle that the saturated vapor pressure of iodine and water vapor are different, and the liquid iodine discharged from a melting furnace does not need quality inspection at the corresponding temperature, so that the required purity can be achieved; from the standpoint of purity of refined iodine prepared and loss rate of iodine in the whole preparation process, examples 1 to 5 are preferred, comparative examples 1 to 2 are that the number of layers of sieve plates at the lower part of the feed of the refining tower is adjusted based on example 1, while purity of refined iodine is improved, but loss rate of iodine in the whole preparation process is increased, resources are wasted, cost is also increased, comparative example 3 is that on the basis of example 1, liquefaction times and vaporization times of iodine are adjusted, while purity is improved, but loss rate of iodine in the whole preparation process is increased, resources are wasted, cost is also increased, and comparative examples 4 to 5 are that on the basis of example 1, discharge taste of liquid iodine in an iodine smelter is adjusted, purity is also effectively improved, but loss rate of iodine in the whole preparation process is increased, resources are wasted, cost is also increased, and it is seen that purity of comparative examples 1 to 5 is effectively improved, but loss rate of iodine in the whole preparation process is increased, and cost is also increased.
Claims (1)
1. A method for purifying crude iodine, which is characterized by comprising the following steps: liquefying, quality inspection, vaporization treatment, secondary liquefying and solidification;
the liquefaction is that crude iodine and concentrated sulfuric acid are mixed according to the mass ratio of 1:1.2-2 in an iodine melting furnace, and eutectic liquefaction is carried out at 100-140 ℃;
the liquid level of the liquid iodine in the iodine melting furnace is 5-30 times of the pipe diameter of the liquid iodine outlet, and when sulfuric acid is added for liquefaction, the liquid level of the sulfuric acid is 1.2-2 times of the liquid iodine level;
the quality inspection is applied to liquefying operation by adding concentrated sulfuric acid, specifically, the quality inspection of the melted liquid iodine is more than or equal to 98 percent, the next procedure can be carried out, and if the quality of the detected liquid iodine is less than 98 percent, the liquid iodine returns to an iodine melting furnace for continuous purification;
the vaporization treatment is to send the liquid iodine from the upper middle part of the refining tower and heat the liquid iodine to 190-210 ℃ to realize the vaporization of the liquid iodine;
and (3) performing secondary fluidization and solidification, discharging the vaporized iodine vapor from the top of the refining tower, entering a cooler, adjusting the temperature of the cooler to 100-120 ℃, and sending the cooled iodine vapor into a condenser after the iodine vapor is completely liquefied, so as to obtain refined iodine by solidification.
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