CN1699143A - Method of recovering iodine from palygorskite ore - Google Patents
Method of recovering iodine from palygorskite ore Download PDFInfo
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- CN1699143A CN1699143A CN 200510049774 CN200510049774A CN1699143A CN 1699143 A CN1699143 A CN 1699143A CN 200510049774 CN200510049774 CN 200510049774 CN 200510049774 A CN200510049774 A CN 200510049774A CN 1699143 A CN1699143 A CN 1699143A
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- palygorskite
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- 239000011630 iodine Substances 0.000 title claims abstract description 49
- 229910052740 iodine Inorganic materials 0.000 title claims abstract description 49
- ZCYVEMRRCGMTRW-UHFFFAOYSA-N 7553-56-2 Chemical compound [I] ZCYVEMRRCGMTRW-UHFFFAOYSA-N 0.000 title claims abstract description 48
- 229910052625 palygorskite Inorganic materials 0.000 title claims abstract description 43
- 238000000034 method Methods 0.000 title claims abstract description 12
- 239000002253 acid Substances 0.000 claims abstract description 42
- 239000011347 resin Substances 0.000 claims abstract description 37
- 229920005989 resin Polymers 0.000 claims abstract description 37
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 30
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims abstract description 27
- 239000003480 eluent Substances 0.000 claims abstract description 22
- 238000003756 stirring Methods 0.000 claims abstract description 22
- 150000001450 anions Chemical class 0.000 claims abstract description 13
- 239000011780 sodium chloride Substances 0.000 claims abstract description 13
- 239000003638 chemical reducing agent Substances 0.000 claims abstract description 9
- 238000001914 filtration Methods 0.000 claims abstract description 8
- 238000002156 mixing Methods 0.000 claims abstract description 8
- 238000010438 heat treatment Methods 0.000 claims abstract description 7
- PNDPGZBMCMUPRI-UHFFFAOYSA-N iodine Chemical compound II PNDPGZBMCMUPRI-UHFFFAOYSA-N 0.000 claims abstract description 7
- 238000000859 sublimation Methods 0.000 claims abstract description 6
- 230000008022 sublimation Effects 0.000 claims abstract description 6
- 239000003957 anion exchange resin Substances 0.000 claims description 15
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 10
- 229910052500 inorganic mineral Inorganic materials 0.000 claims description 10
- 239000011707 mineral Substances 0.000 claims description 10
- 235000010755 mineral Nutrition 0.000 claims description 9
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 8
- LPXPTNMVRIOKMN-UHFFFAOYSA-M sodium nitrite Chemical compound [Na+].[O-]N=O LPXPTNMVRIOKMN-UHFFFAOYSA-M 0.000 claims description 8
- GEHJYWRUCIMESM-UHFFFAOYSA-L sodium sulfite Chemical compound [Na+].[Na+].[O-]S([O-])=O GEHJYWRUCIMESM-UHFFFAOYSA-L 0.000 claims description 8
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 claims description 6
- 239000000047 product Substances 0.000 claims description 6
- 230000008859 change Effects 0.000 claims description 5
- 239000002244 precipitate Substances 0.000 claims description 5
- 239000004593 Epoxy Substances 0.000 claims description 4
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 4
- 229910017604 nitric acid Inorganic materials 0.000 claims description 4
- SUKJFIGYRHOWBL-UHFFFAOYSA-N sodium hypochlorite Chemical compound [Na+].Cl[O-] SUKJFIGYRHOWBL-UHFFFAOYSA-N 0.000 claims description 4
- 235000010288 sodium nitrite Nutrition 0.000 claims description 4
- 235000010265 sodium sulphite Nutrition 0.000 claims description 4
- AKHNMLFCWUSKQB-UHFFFAOYSA-L sodium thiosulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=S AKHNMLFCWUSKQB-UHFFFAOYSA-L 0.000 claims description 4
- 235000019345 sodium thiosulphate Nutrition 0.000 claims description 4
- NIXOWILDQLNWCW-UHFFFAOYSA-N acrylic acid group Chemical group C(C=C)(=O)O NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims description 3
- 229910001870 ammonium persulfate Inorganic materials 0.000 claims description 3
- 239000011777 magnesium Substances 0.000 claims description 3
- HCWCAKKEBCNQJP-UHFFFAOYSA-N magnesium orthosilicate Chemical compound [Mg+2].[Mg+2].[O-][Si]([O-])([O-])[O-] HCWCAKKEBCNQJP-UHFFFAOYSA-N 0.000 claims description 3
- 239000000391 magnesium silicate Substances 0.000 claims description 3
- 229910052919 magnesium silicate Inorganic materials 0.000 claims description 3
- 235000019792 magnesium silicate Nutrition 0.000 claims description 3
- 239000004927 clay Substances 0.000 claims description 2
- 238000001556 precipitation Methods 0.000 claims description 2
- 239000004133 Sodium thiosulphate Substances 0.000 claims 1
- 238000001179 sorption measurement Methods 0.000 abstract description 6
- 239000007800 oxidant agent Substances 0.000 abstract description 4
- 229940027989 antiseptic and disinfectant iodine product Drugs 0.000 abstract description 3
- 238000000151 deposition Methods 0.000 abstract 1
- 238000005201 scrubbing Methods 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 66
- 238000006243 chemical reaction Methods 0.000 description 7
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 description 6
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 4
- 230000008901 benefit Effects 0.000 description 4
- -1 filters Substances 0.000 description 4
- 238000002360 preparation method Methods 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- 239000007832 Na2SO4 Substances 0.000 description 3
- 239000003054 catalyst Substances 0.000 description 3
- 239000013078 crystal Substances 0.000 description 3
- 238000000605 extraction Methods 0.000 description 3
- 235000013305 food Nutrition 0.000 description 3
- 150000002500 ions Chemical class 0.000 description 3
- 239000002086 nanomaterial Substances 0.000 description 3
- 108090000623 proteins and genes Proteins 0.000 description 3
- 238000011084 recovery Methods 0.000 description 3
- 238000000926 separation method Methods 0.000 description 3
- 229910052938 sodium sulfate Inorganic materials 0.000 description 3
- 238000005303 weighing Methods 0.000 description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 2
- 239000000654 additive Substances 0.000 description 2
- 239000003513 alkali Substances 0.000 description 2
- 239000002781 deodorant agent Substances 0.000 description 2
- 238000004090 dissolution Methods 0.000 description 2
- 239000003814 drug Substances 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 230000001590 oxidative effect Effects 0.000 description 2
- 230000008635 plant growth Effects 0.000 description 2
- KMUONIBRACKNSN-UHFFFAOYSA-N potassium dichromate Chemical compound [K+].[K+].[O-][Cr](=O)(=O)O[Cr]([O-])(=O)=O KMUONIBRACKNSN-UHFFFAOYSA-N 0.000 description 2
- 102000004169 proteins and genes Human genes 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 239000012266 salt solution Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- LCPVQAHEFVXVKT-UHFFFAOYSA-N 2-(2,4-difluorophenoxy)pyridin-3-amine Chemical compound NC1=CC=CN=C1OC1=CC=C(F)C=C1F LCPVQAHEFVXVKT-UHFFFAOYSA-N 0.000 description 1
- NIXOWILDQLNWCW-UHFFFAOYSA-M Acrylate Chemical group [O-]C(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-M 0.000 description 1
- 241000224489 Amoeba Species 0.000 description 1
- 241000894006 Bacteria Species 0.000 description 1
- 241000233866 Fungi Species 0.000 description 1
- 229910019092 Mg-O Inorganic materials 0.000 description 1
- 229910019395 Mg—O Inorganic materials 0.000 description 1
- 229910018557 Si O Inorganic materials 0.000 description 1
- 239000005708 Sodium hypochlorite Substances 0.000 description 1
- 241000700605 Viruses Species 0.000 description 1
- 241000607479 Yersinia pestis Species 0.000 description 1
- AEEAZFQPYUMBPY-UHFFFAOYSA-N [I].[W] Chemical compound [I].[W] AEEAZFQPYUMBPY-UHFFFAOYSA-N 0.000 description 1
- WQHONKDTTOGZPR-UHFFFAOYSA-N [O-2].[O-2].[Mn+2].[Fe+2] Chemical class [O-2].[O-2].[Mn+2].[Fe+2] WQHONKDTTOGZPR-UHFFFAOYSA-N 0.000 description 1
- 238000010306 acid treatment Methods 0.000 description 1
- 238000001994 activation Methods 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 239000003463 adsorbent Substances 0.000 description 1
- 239000003905 agrochemical Substances 0.000 description 1
- 125000003277 amino group Chemical group 0.000 description 1
- 230000001580 bacterial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 150000004649 carbonic acid derivatives Chemical class 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- 239000002734 clay mineral Substances 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 230000001086 cytosolic effect Effects 0.000 description 1
- 230000007123 defense Effects 0.000 description 1
- 239000002274 desiccant Substances 0.000 description 1
- 239000000645 desinfectant Substances 0.000 description 1
- 238000003795 desorption Methods 0.000 description 1
- 201000010099 disease Diseases 0.000 description 1
- 208000037265 diseases, disorders, signs and symptoms Diseases 0.000 description 1
- 239000000975 dye Substances 0.000 description 1
- 235000013399 edible fruits Nutrition 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000010828 elution Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- XMBWDFGMSWQBCA-UHFFFAOYSA-N hydrogen iodide Chemical compound I XMBWDFGMSWQBCA-UHFFFAOYSA-N 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 1
- 238000002386 leaching Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 230000021332 multicellular organism growth Effects 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 150000002894 organic compounds Chemical class 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- JLKDVMWYMMLWTI-UHFFFAOYSA-M potassium iodate Chemical compound [K+].[O-]I(=O)=O JLKDVMWYMMLWTI-UHFFFAOYSA-M 0.000 description 1
- 239000001230 potassium iodate Substances 0.000 description 1
- 235000006666 potassium iodate Nutrition 0.000 description 1
- 229940093930 potassium iodate Drugs 0.000 description 1
- 230000001376 precipitating effect Effects 0.000 description 1
- 239000003755 preservative agent Substances 0.000 description 1
- 230000002335 preservative effect Effects 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- LIVNPJMFVYWSIS-UHFFFAOYSA-N silicon monoxide Inorganic materials [Si-]#[O+] LIVNPJMFVYWSIS-UHFFFAOYSA-N 0.000 description 1
- CHQMHPLRPQMAMX-UHFFFAOYSA-L sodium persulfate Substances [Na+].[Na+].[O-]S(=O)(=O)OOS([O-])(=O)=O CHQMHPLRPQMAMX-UHFFFAOYSA-L 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000007790 solid phase Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 229940125725 tranquilizer Drugs 0.000 description 1
- 239000003204 tranquilizing agent Substances 0.000 description 1
- 230000002936 tranquilizing effect Effects 0.000 description 1
- 235000013311 vegetables Nutrition 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
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- Manufacture And Refinement Of Metals (AREA)
Abstract
The invention discloses a method of recovering iodine from palygorskite ore which comprises slacking paligorskite ores, mixing with acid solution, stirring and reacting, carrying out centrifugal filtration, isolating paligorskite from acid solution, slowly charging oxidizer solution into acid solution while mixing, leading in anion resin column adsorption, scrubbing the resin with NaOH solution and NaCl solution, dropping acid solution into eluent, making solution pH<2.0, then dropping reducing agent solution, stewing and depositing, filtering or centrifuging to obtain crude iodine, storing the crude iodine in air-tight container, heating for sublimation, condensing to obtain the pure iodine products.
Description
Technical Field
The invention relates to a method for recovering iodine from palygorskite ore.
Background
Iodine is called vital element, wisdom element. Is an indispensable element for human body and plant growth, is a raw material for preparing inorganic or organic iodide, and is also a catalyst with good chemical reaction. Iodine products are widely applied to various industries such as food, medicine, industry, agriculture, national defense advanced technology and the like. In medicine, iodine is the most commonly used disinfectant preservative, which oxidizes the active genes of bacterial cytoplasmic proteins and binds to the amino groups of the proteins, denaturing them, thereby killing bacteria, fungi, viruses and amoeba. It can also be used for preparing deodorant, tranquilizer, etc. In agriculture, iodine is used as raw material for preparing agricultural chemicals, and is sprayed with iodine solution to prevent and cure diseases and pests of vegetables, fruits and crops, and can promote plant growth and increase yield. In the food industry, potassium iodate is the main additive of iodized salt, and can also improve the quality of cooked wheaten food. In industry, iodine is a major component in the synthesis of organic dyes. In the metallurgical industry, iodine is used to refine high purity metals. In the lighting industry, the iodine-tungsten lamp has strong luminosity and saves electric energy. In the sophisticated industry, organic compounds of iodine are additives for the manufacture of rocket fuels.
Iodine is therefore a very important element for us, and iodine products have a wide market prospect in daily life and many industrial fields. Palygorskite ores in western regions of China often contain iodine in different quantities from tens ppm to hundreds ppm, and the separation and extraction of iodine from palygorskite can greatly improve the added value of natural resources and bring considerable economic benefits.
Disclosure of Invention
The invention aims to provide a method for recovering iodine from palygorskite ore.
The method comprises the following steps:
1) mixing the palygorskite ore crushed to be less than 200 meshes with an acid solution with the weight 5-20 times that of the palygorskite ore, uniformly stirring, reacting for 5-50 hours, continuously stirring, and centrifuging or filtering to separate the palygorskite from the acid solution;
2) slowly adding 10-30 wt% NaClO or H into the acid solution while stirring2O2The solution or the ammonium persulfate solution with the weight concentration of 10-20% is added when the color of the solution is observed to change from light yellow to brownish red;
3) leading the brownish red acid solution into an anion resin exchange column, gradually deepening the resin color along with the flowing of the acid solution, and replacing the resin column when the resin color is changed into black red;
4) introducing a NaOH solution with the weight concentration of 5-10% into a black-red anion resin exchange column, collecting alkaline eluent flowing out of the exchange column, stopping adding the NaOH solution after the resin is basically faded, adding NaCl solution with the same concentration and volume into the exchange column, and collecting sodium chloride eluent flowing out of the exchange column by using another container;
5) and (3) dropwise adding an acid solution into the eluent while slowly stirring to enable the pH value of the solution to be less than 2.0, dropwise adding a reducing agent solution with the weight concentration of 5-15% until brown precipitate is separated out, standing for precipitation, filtering or centrifuging to obtain crude iodine, placing the crude iodine into a closed container for heating and sublimation, and condensing to obtain a pure iodine product.
The palygorskite is a magnesium silicate mineral with a layer chain structure, and the molecular formula is as follows:
Mg5Si8O20(OH)2(OH2)4·4H2O
the output form of the mineral is clay, mudstone, shale or blocky ore in nature.
The acid solution is hydrochloric acid, nitric acid or sulfuric acid with the concentration of 1-5 mol, the anion resin is one of strongly basic styrene anion exchange resin, weakly basic acrylic anion exchange resin and weakly basic epoxy anion exchange resin, and the reducing agent is one of sodium nitrite, sodium sulfite or sodium thiosulfate.
The invention realizes the recycling of trace iodine element in the palygorskite ore without damaging the crystalline structure of the palygorskite and influencing the physical and chemical properties of the palygorskite, and improves the comprehensive utilization value of the natural resource. The iodine recovered from palygorskite ore has the advantages of wide source and low cost.
Detailed Description
Palygorskite is a natural magnesium silicate mineral with a chain-layered structure. The shape of the nano-material is fibrous, the diameter is 10-100 nanometers, the length is several micrometers to dozens of micrometers, and the nano-material conforms to the definition of a nano-material in terms of single crystal size and belongs to typical natural one-dimensional nano-minerals.
The molecular formula of the palygorskite is as follows:
Mg5Si8O20(OH)2(OH2)4·4H2o in the crystal structure, a Mg-O (OH) octahedral layer is sandwiched between every two Si-O tetrahedral layers in the palygorskite to form basic structural units, the basic structural units are arranged in a staggered mode to form tunnel holes parallel to the lattice direction, and the cross section of each tunnel hole is 0.37 multiplied by 0.64 nanometers. The nano-sized intra-crystalline tunnel pores enable the palygorskite to have huge specific surface area and adsorption-catalytic activity. These characteristics make palygorskite have a wide range of uses in many industrial fields, such as adsorbents, desiccants, deodorants, filters, catalysts and catalyst supports.
In western areas of China, the geological reserves of palygorskite reach billions of tons, the ores often contain various amounts of iodine, the content is from tens of ppm to hundreds of ppm, and the separation and extraction of iodine from palygorskite can greatly improve the added value of natural resources and bring considerable economic benefits.
The first step in the recovery of iodine from palygorskite ore is the separation of iodine from the carrier mineral palygorskite by an acid activation process. Hydrochloric acid, nitric acid or sulfuric acid may be used, and is recommended for environmental and cost reasons. The impurity minerals remaining in the ore can be dissolved by acid, such as carbonates, partial clay minerals, iron manganese oxides and hydroxide minerals. In actual operation, the concentration and dosage of acid should be adjusted according to ore components, and ore with high content of acid-soluble impurities can increase the concentration of acid or increase the dosage of acid. During the acid treatment, iodine adsorbed by palygorskite in ionic form tends to be selectively dissolved into solution. Heating the system during acid dissolution accelerates the reaction process, but also increases the likelihood that the iodine will be vaporized. After acid dissolution, the solution can be separated from the solid ore by filtration or centrifugation, and the solid phase is leached by dilute acid to improve the iodine recovery.
The second step of the preparation process is the oxidation of iodide ions due to the anion exchange resin to polyiodide I3 -Or I5 -The exchange adsorption capacity of the ions is far greater than that of the ions I-The amount of ion adsorption. The oxidant recommended by the invention is sodium hypochlorite, hydrogen peroxide or sodium persulfate, and other oxidants such as potassium dichromate and the like can also be used. The reaction of the oxidant with the iodide ions in the solution is:
the third step of the preparation method is to adsorb the polyiodion in the solution by using anion resin. The type of anion resin has little difference on the adsorption performance of multi-iodide ions, and can be selected from strongly basic styrene anion exchange resin, weakly basic acrylic acid anion exchange resin and weakly basic epoxy anion exchange resin. Attention is paid to the selection of large-aperture resin as much as possible to improve the elution rate after adsorption. The height of the anion exchange resin column should be greater than 20 cm. The adsorption reaction can be expressed as:
The fourth step of the preparation method is desorption reaction, namely, iodine adsorbed by the anion resin is transferred into eluent by leaching of alkali liquor and salt solution. If a weakly basic anion exchange resin is being sampled,can use Na2SO4The solution replaced the NaOH solution. The difference between the pH value of the alkaline eluent and the sodium chloride eluent and the concentration of iodine is large, and the alkaline eluent and the sodium chloride eluent are stored separately and are treated respectively. The exchange column washed by alkali liquor and salt solution can be reused. The reaction between the solution and the resin upon washing was:
The fifth step of the preparation method is that under the acid condition, the multi-iodine ions in the solution are reduced into simple substance iodine by a reducing agent, crude iodine is obtained after standing, precipitating, filtering or centrifuging treatment, the crude iodine is placed in a closed container to be heated and sublimated, and a pure iodine product is obtained after condensation. The reducing agent recommended by the invention is sodium nitrite, sodium sulfite or sodium thiosulfate, other inorganic reducing agents can be used, and organic reducing agents are avoided.
The method for recovering iodine from palygorskite ore has the advantages of wide sources and low cost. Meanwhile, the crystal structure of the palygorskite is not damaged in the extraction and recovery processes of iodine, so that the use performance of the palygorskite in various industrial fields is not influenced, the comprehensive utilization of palygorskite resources and iodine resources is realized, and the added value of natural mineral resources is improved.
The invention is further illustrated below with reference to specific examples.
Example 1:
1) weighing 100 kg of palygorskite ore crushed to be less than 200 meshes, adding 500 kg of hydrochloric acid solution with the concentration of 5 mol, mixing, uniformly stirring, reacting for 5 hours, continuously stirring, and then centrifuging to separate the palygorskite from the acid solution;
2) slowly adding a NaClO solution with the weight concentration of 20% into the acid solution while stirring, observing the color change of the solution, and stopping adding when the acid solution is changed from light yellow to brownish red;
3) introducing the brownish red acid solution into an exchange column filled with strongly basic styrene anion exchange resin, gradually deepening the resin color along with the flowing of the acid solution, and replacing the resin column when the resin color is changed into black red;
4) introducing a NaOH solution with the weight concentration of 10% into the anion resin exchange column which is turned into black red, collecting the alkaline eluent flowing out of the exchange column, stopping adding the NaOH solution after the resin is basically faded, and then collecting the alkaline eluent with the volume of 3.6 liters; adding 3.6 liters of NaCl solution with the concentration of 10 percent into the exchange column, and collecting the sodium chloride eluent flowing out of the exchange column by using another container;
5) slowly stirring, dripping a hydrochloric acid solution with the concentration of 2 mol into the eluent to ensure that the pH value of the solution is less than 2.0, dripping a sodium nitrite solution with the weight concentration of 5% until brown precipitate is separated out, obtaining crude iodine after centrifugal treatment, placing the crude iodine into a closed container, heating for sublimation, and condensing to obtain a pure iodine product.
Example 2:
1) weighing 10 kg of palygorskite ore crushed to be less than 200 meshes, adding 200 kg of sulfuric acid solution with the concentration of 1 mol, mixing, uniformly stirring, reacting for 50 hours, continuously stirring, and then centrifuging to separate the palygorskite from the acid solution;
2) slowly adding 30% hydrogen peroxide into the acid solution while stirring, observing the color change of the solution, and stopping adding when the acid solution is changed from light yellow to brownish red;
3) introducing the brownish red acid solution into an exchange column filled with weakly basic acrylic anion exchange resin, gradually deepening the color of the resin along with the flowing of the acid solution, and replacing the resin column when the color of the resin is changed into black red;
4) adding 10% by weight of Na2SO4Introducing the solution into black-red anion resin exchange column, collecting alkaline eluate flowing out of the exchange column until the resin is substantially fadedAfter color, stop adding Na2SO4The volume of the solution, the basic eluent collected at this point, was 2.4liters; adding 2.4 liters of NaCl solution with the weight concentration of 10 percent into the exchange column, and collecting the sodium chloride eluent flowing out of the exchange column by using another container;
5) while slowly stirring, dropwise adding H with the concentration of 2 mol into the eluent2SO4And (3) dissolving the solution until the pH value of the solution is less than 2.0, dropwise adding a sodium sulfite solution with the weight concentration of 10% until brown precipitate is separated out, centrifuging to obtain crude iodine, heating the crude iodine in a closed container for sublimation, and condensing to obtain a pure iodine product.
Example 3:
1) weighing 20 kg of palygorskite ore crushed to be less than 200 meshes, adding 200 kg of nitric acid solution with the concentration of 2 mol, mixing, uniformly stirring, reacting for 10 hours, continuously stirring, and then performing centrifugal treatment to separate the palygorskite from the acid solution;
2) slowly adding 10 wt% ammonium persulfate solution into the acid solution while stirring, and observing the color change of the solution until the acid solution changes from light yellow to brownish red;
3) introducing a brownish red acid solution into an exchange column filled with a weakly basic epoxy anion exchange resin, gradually deepening the color of the resin along with the flowing of the acid solution, and replacing the resin column when the color of the resin is changed into black red;
4) introducing a NaOH solution with the weight concentration of 5% into the anion resin exchange column which is turned into black red, collecting the alkaline eluent flowing out of the exchange column, stopping adding the NaOH solution after the resin is basically faded, and keeping the volume of the collected alkaline eluent at 2.8 liters; adding 2.8 liters of NaCl solution with the weight concentration of 5 percent into the exchange column, and collecting the sodium chloride eluent flowing out of the exchange column by using another container;
5) while slowly stirring, 6 mol H was added dropwise to the eluate2SO4Making the pH value of the solution be less than 2.0, then dripping sodium thiosulfate solution whose weight concentration is 5% until brown precipitate is separated out, centrifuging to obtain crude iodine, mixing the crude iodine with water, adding water, stirring, coolingPlacing iodine in a closed container, heating for sublimation, and condensing to obtain pure iodine product.
Claims (5)
1. A method for recovering iodine from palygorskite ore is characterized by comprising the following steps:
1) mixing the palygorskite ore crushed to be less than 200 meshes with an acid solution with the weight 5-20 times that of the palygorskite ore, uniformly stirring, reacting for 5-50 hours, continuously stirring, and centrifuging or filtering to separate the palygorskite from the acid solution;
2) slowly adding 10-30 wt% NaClO or H into the acid solution while stirring2O2The solution or the ammonium persulfate solution with the weight concentration of 10-20% is added when the color of the solution is observed to change from light yellow to brownish red;
3) leading the brownish red acid solution into an anion resin exchange column, gradually deepening the resin color along with the flowing of the acid solution, and replacing the resin column when the resin color is changed into black red;
4) introducing a NaOH solution with the weight concentration of 5-10% into a black-red anion resinexchange column, collecting alkaline eluent flowing out of the exchange column, stopping adding the NaOH solution after the resin is basically faded, adding NaCl solution with the same concentration and volume into the exchange column, and collecting sodium chloride eluent flowing out of the exchange column by using another container;
5) and (3) dropwise adding an acid solution into the eluent while slowly stirring to enable the pH value of the solution to be less than 2.0, dropwise adding a reducing agent solution with the weight concentration of 5-15% until brown precipitate is separated out, standing for precipitation, filtering or centrifuging to obtain crude iodine, placing the crude iodine into a closed container for heating and sublimation, and condensing to obtain a pure iodine product.
2. A method for recovering iodine from palygorskite ore according to claim 1, wherein the palygorskite is a magnesium silicate mineral with a lamellar chain structure of the formula:
Mg5Si8O20(OH)2(OH2)4·4H2O
the output form of the mineral is clay, mudstone, shale or blocky ore in nature.
3. The method for recovering iodine from palygorskite ore according to claim 1, wherein the acid solution is hydrochloric acid, nitric acid or sulfuric acid with a concentration of 1-5 mol.
4. The method of claim 1, wherein said anion resin is one of strongly basic styrenic anion exchange resin, weakly basic acrylic anion exchange resin, and weakly basic epoxy anion exchange resin.
5. A process for recovering iodine from palygorskite ore according to claim 1, characterised in that the reductant is one of sodium nitrite, sodium sulphite or sodium thiosulphate.
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| CNB2005100497744A CN1331733C (en) | 2005-05-09 | 2005-05-09 | Method of recovering iodine from palygorskite ore |
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| CNB2005100497744A CN1331733C (en) | 2005-05-09 | 2005-05-09 | Method of recovering iodine from palygorskite ore |
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| CN1331733C CN1331733C (en) | 2007-08-15 |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102502501A (en) * | 2011-10-27 | 2012-06-20 | 瓮福（集团）有限责任公司 | Method for extracting iodine from wet-process phosphoric acid produced from iodine-containing phosphorous ore by semi-water and bi-water method |
| CN102616959A (en) * | 2012-04-01 | 2012-08-01 | 江苏焕鑫高新材料科技有限公司 | Method for recycling iodine and phenolic compounds from waste alkaline water containing phenol ions and iodine ions and realizing pollution-free emission |
| CN117654423A (en) * | 2024-02-01 | 2024-03-08 | 中国科学院地球环境研究所 | System and method for extracting iodine in different occurrence forms in sediment |
Family Cites Families (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4131645A (en) * | 1974-11-21 | 1978-12-26 | Ethyl Corporation | Iodine recovery process |
| JPS6046042B2 (en) * | 1977-07-19 | 1985-10-14 | 日本天然瓦斯興業株式会社 | Method for producing iodine from natural can water |
| JPS5571601A (en) * | 1978-11-21 | 1980-05-29 | Ethyl Corp | Method of taking iodine from salt water |
| JPH06157008A (en) * | 1992-11-13 | 1994-06-03 | Godo Shigen Sangyo Kk | Method for recovering iodine from waste liquor containing iodine and/or inorganic iodine compound |
| US6863905B1 (en) * | 2002-05-21 | 2005-03-08 | Shanbrom Technologies, Llc | Enhanced iodine treatment of drinking water |
-
2005
- 2005-05-09 CN CNB2005100497744A patent/CN1331733C/en not_active Expired - Fee Related
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102502501A (en) * | 2011-10-27 | 2012-06-20 | 瓮福（集团）有限责任公司 | Method for extracting iodine from wet-process phosphoric acid produced from iodine-containing phosphorous ore by semi-water and bi-water method |
| CN102616959A (en) * | 2012-04-01 | 2012-08-01 | 江苏焕鑫高新材料科技有限公司 | Method for recycling iodine and phenolic compounds from waste alkaline water containing phenol ions and iodine ions and realizing pollution-free emission |
| CN102616959B (en) * | 2012-04-01 | 2013-11-06 | 江苏焕鑫高新材料科技有限公司 | Method for recycling iodine and phenolic compounds from waste alkaline water containing phenol ions and iodine ions and realizing pollution-free emission |
| CN117654423A (en) * | 2024-02-01 | 2024-03-08 | 中国科学院地球环境研究所 | System and method for extracting iodine in different occurrence forms in sediment |
| CN117654423B (en) * | 2024-02-01 | 2024-04-26 | 中国科学院地球环境研究所 | System and method for extracting iodine in different occurrence forms in sediment |
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| CN1331733C (en) | 2007-08-15 |
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