CN1117943A - Industrial method for preparation of pure iodic acid solution and its salts - Google Patents
Industrial method for preparation of pure iodic acid solution and its salts Download PDFInfo
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- CN1117943A CN1117943A CN 94111445 CN94111445A CN1117943A CN 1117943 A CN1117943 A CN 1117943A CN 94111445 CN94111445 CN 94111445 CN 94111445 A CN94111445 A CN 94111445A CN 1117943 A CN1117943 A CN 1117943A
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- iodic acid
- iodate
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- QFWPJPIVLCBXFJ-UHFFFAOYSA-N glymidine Chemical compound N1=CC(OCCOC)=CN=C1NS(=O)(=O)C1=CC=CC=C1 QFWPJPIVLCBXFJ-UHFFFAOYSA-N 0.000 title claims abstract description 37
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 15
- 150000003839 salts Chemical class 0.000 title claims abstract description 9
- 238000002360 preparation method Methods 0.000 title claims description 8
- ZCYVEMRRCGMTRW-UHFFFAOYSA-N 7553-56-2 Chemical compound [I] ZCYVEMRRCGMTRW-UHFFFAOYSA-N 0.000 claims abstract description 37
- 239000011630 iodine Substances 0.000 claims abstract description 37
- 229910052740 iodine Inorganic materials 0.000 claims abstract description 37
- 238000000034 method Methods 0.000 claims abstract description 33
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims abstract description 30
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims abstract description 18
- 239000002253 acid Substances 0.000 claims abstract description 18
- 229910017604 nitric acid Inorganic materials 0.000 claims abstract description 18
- 238000007254 oxidation reaction Methods 0.000 claims abstract description 16
- ICIWUVCWSCSTAQ-UHFFFAOYSA-M iodate Chemical compound [O-]I(=O)=O ICIWUVCWSCSTAQ-UHFFFAOYSA-M 0.000 claims abstract description 13
- 230000003647 oxidation Effects 0.000 claims abstract description 13
- 229910052736 halogen Inorganic materials 0.000 claims abstract description 7
- 150000002367 halogens Chemical class 0.000 claims abstract description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 claims abstract description 7
- 238000006243 chemical reaction Methods 0.000 claims description 14
- 239000003054 catalyst Substances 0.000 claims description 5
- ICIWUVCWSCSTAQ-UHFFFAOYSA-N iodic acid Chemical class OI(=O)=O ICIWUVCWSCSTAQ-UHFFFAOYSA-N 0.000 claims description 5
- XTEGARKTQYYJKE-UHFFFAOYSA-N chloric acid Chemical compound OCl(=O)=O XTEGARKTQYYJKE-UHFFFAOYSA-N 0.000 claims description 4
- 229940005991 chloric acid Drugs 0.000 claims description 4
- 238000006386 neutralization reaction Methods 0.000 claims description 3
- 229910000288 alkali metal carbonate Inorganic materials 0.000 claims description 2
- 150000008041 alkali metal carbonates Chemical class 0.000 claims description 2
- SXDBWCPKPHAZSM-UHFFFAOYSA-N bromic acid Chemical compound OBr(=O)=O SXDBWCPKPHAZSM-UHFFFAOYSA-N 0.000 claims description 2
- XMBWDFGMSWQBCA-UHFFFAOYSA-N hydrogen iodide Chemical compound I XMBWDFGMSWQBCA-UHFFFAOYSA-N 0.000 claims description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 13
- 239000013078 crystal Substances 0.000 abstract description 11
- 229910052783 alkali metal Inorganic materials 0.000 abstract description 7
- 150000001340 alkali metals Chemical class 0.000 abstract description 5
- PNDPGZBMCMUPRI-UHFFFAOYSA-N iodine Chemical compound II PNDPGZBMCMUPRI-UHFFFAOYSA-N 0.000 abstract description 5
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 abstract description 4
- 239000001301 oxygen Substances 0.000 abstract description 4
- 229910052760 oxygen Inorganic materials 0.000 abstract description 4
- 229960002163 hydrogen peroxide Drugs 0.000 description 14
- JLKDVMWYMMLWTI-UHFFFAOYSA-M potassium iodate Chemical compound [K+].[O-]I(=O)=O JLKDVMWYMMLWTI-UHFFFAOYSA-M 0.000 description 11
- 239000001230 potassium iodate Substances 0.000 description 11
- 235000006666 potassium iodate Nutrition 0.000 description 11
- 229940093930 potassium iodate Drugs 0.000 description 11
- 239000000047 product Substances 0.000 description 9
- TYJJADVDDVDEDZ-UHFFFAOYSA-M potassium hydrogencarbonate Chemical compound [K+].OC([O-])=O TYJJADVDDVDEDZ-UHFFFAOYSA-M 0.000 description 7
- 239000000126 substance Substances 0.000 description 7
- 235000002639 sodium chloride Nutrition 0.000 description 6
- 239000004151 Calcium iodate Substances 0.000 description 5
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 description 5
- UHWJJLGTKIWIJO-UHFFFAOYSA-L calcium iodate Chemical compound [Ca+2].[O-]I(=O)=O.[O-]I(=O)=O UHWJJLGTKIWIJO-UHFFFAOYSA-L 0.000 description 5
- 235000019390 calcium iodate Nutrition 0.000 description 5
- 238000001035 drying Methods 0.000 description 5
- 238000001704 evaporation Methods 0.000 description 5
- 239000012535 impurity Substances 0.000 description 5
- 238000000926 separation method Methods 0.000 description 5
- 239000012153 distilled water Substances 0.000 description 4
- 238000001914 filtration Methods 0.000 description 4
- 238000005406 washing Methods 0.000 description 4
- KZBUYRJDOAKODT-UHFFFAOYSA-N Chlorine Chemical compound ClCl KZBUYRJDOAKODT-UHFFFAOYSA-N 0.000 description 3
- -1 alkali metal iodate Chemical class 0.000 description 3
- 239000006227 byproduct Substances 0.000 description 3
- 230000003197 catalytic effect Effects 0.000 description 3
- 239000008367 deionised water Substances 0.000 description 3
- 229910021641 deionized water Inorganic materials 0.000 description 3
- 235000013305 food Nutrition 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 239000012452 mother liquor Substances 0.000 description 3
- VKJKEPKFPUWCAS-UHFFFAOYSA-M potassium chlorate Chemical compound [K+].[O-]Cl(=O)=O VKJKEPKFPUWCAS-UHFFFAOYSA-M 0.000 description 3
- 235000008733 Citrus aurantifolia Nutrition 0.000 description 2
- 229910002651 NO3 Inorganic materials 0.000 description 2
- 235000011941 Tilia x europaea Nutrition 0.000 description 2
- 150000007513 acids Chemical class 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- ZCCIPPOKBCJFDN-UHFFFAOYSA-N calcium nitrate Chemical compound [Ca+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O ZCCIPPOKBCJFDN-UHFFFAOYSA-N 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 238000002425 crystallisation Methods 0.000 description 2
- 230000008025 crystallization Effects 0.000 description 2
- 238000007323 disproportionation reaction Methods 0.000 description 2
- 238000005868 electrolysis reaction Methods 0.000 description 2
- 230000008020 evaporation Effects 0.000 description 2
- 238000009776 industrial production Methods 0.000 description 2
- 239000004571 lime Substances 0.000 description 2
- 239000008267 milk Substances 0.000 description 2
- 210000004080 milk Anatomy 0.000 description 2
- 235000013336 milk Nutrition 0.000 description 2
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Chemical compound [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 description 2
- 238000007086 side reaction Methods 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- 239000013589 supplement Substances 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 description 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 description 1
- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 description 1
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 1
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 150000008044 alkali metal hydroxides Chemical class 0.000 description 1
- 229910052784 alkaline earth metal Inorganic materials 0.000 description 1
- 150000001342 alkaline earth metals Chemical class 0.000 description 1
- 239000003674 animal food additive Substances 0.000 description 1
- 150000001552 barium Chemical class 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- 239000001110 calcium chloride Substances 0.000 description 1
- 229910001628 calcium chloride Inorganic materials 0.000 description 1
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 description 1
- 239000000920 calcium hydroxide Substances 0.000 description 1
- 229910001861 calcium hydroxide Inorganic materials 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 238000003889 chemical engineering Methods 0.000 description 1
- 239000012295 chemical reaction liquid Substances 0.000 description 1
- 239000000460 chlorine Substances 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000012847 fine chemical Substances 0.000 description 1
- 239000002778 food additive Substances 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 229940071870 hydroiodic acid Drugs 0.000 description 1
- 150000004715 keto acids Chemical class 0.000 description 1
- 238000002386 leaching 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
- 230000007935 neutral effect Effects 0.000 description 1
- 239000007800 oxidant agent Substances 0.000 description 1
- 150000002926 oxygen Chemical class 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- 229910000027 potassium carbonate Inorganic materials 0.000 description 1
- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Inorganic materials [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 description 1
- 238000011112 process operation Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000012066 reaction slurry Substances 0.000 description 1
- 238000001953 recrystallisation Methods 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 239000011780 sodium chloride Substances 0.000 description 1
- 239000011697 sodium iodate Substances 0.000 description 1
- 235000015281 sodium iodate Nutrition 0.000 description 1
- 229940032753 sodium iodate Drugs 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- 239000002341 toxic gas Substances 0.000 description 1
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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The present invention relates to an industrial method for preparing pure iodic acid and its salts. It adopts refined iodine, uses the hydrogen dioxide solution oxidation process and adds a small quantity of nitric acid or halogen oxyacid or non-oxygen acid to prepare the pure iodic acid solution, whose yield (by iodine) can be up to 98%. Besides, said invention uses hydroxide or (arbonate of alkali metal to neutralize the iodic acid solution and makes its pH value equal to 7, so that the pure iodate crystal can be made up, and then said crystal is washed with water and dried and made into the invented finished product. its iodate purity is up to 99.0%, and its yield (by iodic acid) is up to 85-95%.
Description
The present invention relates to a production method of pure iodine acid and its salts.
Iodic acid is one of oxyacids of iodine and has a molecular formula of HIO3And is industrially used as an intermediate for pharmaceutical synthesis, a catalyst and a chemical reagent. The iodates are commonly used as alkali metal (e.g., sodium, potassium) and alkaline earth metal (e.g., calcium, barium) salts, where potassium iodate is used as a reference reagent in chemical analysis and as an iodine supplement, such as salt and iodine. And calcium iodate is used as an additive for food and feed. These products are in ChinaAll the production is carried out.
The preparation method of the iodic acid and the salts thereof which are disclosed at home and abroad at present is introduced as follows:
the preparation method of the (I) iodic acid comprises the following steps:
(1) chlorine gas oxidation method〔1〕：
(2) Concentrated nitric acid oxidation process〔1、2〕：
(3) Oxydol and concentrated nitric acid oxidation method〔3〕：
Concentrated HNO3
The addition amount of the concentrated nitric acid is 1.5 times of the amount of the added fine iodine.
(4) Chloric acid oxidation method〔1、2〕：
(5) And an ozone oxidation method.
Among the above methods, the products obtained by the methods 1, 2 and 3 are actually mixed acids, and the process for preparing pure iodic acid solution from the mixed acids is complicated and the yield is low. In addition, in the methods 2 and 4, harmful and toxic gases can also escape in the reaction, so that the treatment is difficult and the operation is complicated. The method 5 has high requirements on equipment and low yield. Therefore, no industrial reports are found in methods 1, 2, 4 and 5. In the method 3, a large amount of concentrated nitric acid is required to be added, so that the obtained product is still mixed acid, the process requirement for preparing the iodic acid is high, and the separation process is complex.
The preparation method of the (di) iodate comprises the following steps:
the iodate is commonly used as potassium iodate, sodium iodate and calcium iodate, and is commonly used for chemical analysis, iodine supplement, food and feed additives.
(1) The production method of the potassium iodate comprises the following steps:
① Oxidation of potassium chlorate(4)：
② disproportionation method:
③ electrolytic method:
electrolysis
At present, potassium chlorate oxidation method is used for industrial production at home and abroad. The disproportionation method and the electrolysis method have no industrial reports due to low yield and complex separation. Potassium chlorate oxidation method because of more by-products (KCl, Cl)2、KNO3And the like), particularly toxic chlorine gas needs to be recovered, so that the method has the defects of complex separation process, long flow, high energy consumption, low product quality, high cost and the like,and is not beneficial to popularization in enterprises.
The industrial production method for directly preparing potassium iodate by using iodic acid by adopting a neutralization method has not been reported so far.
(2) The production method of domestic calcium iodate comprises the following steps:
① chlorine gas is introduced into boiling solution of iodine-dissolved calcium hydroxide and its main reaction formula is
② the iodic acid solution (containing nitric acid) is prepared by oxidation of iodine, hydrogen peroxide and concentrated nitric acid, and then neutralized by lime milk, the main reaction is
Concentrated nitric acid
Calcium iodate is extremely soluble and can be separated from calcium chloride and calcium nitrate as by-products relatively easily.
The same process is adopted to produce the alkali metal iodate with higher solubility, the separation work of the byproduct is complicated, the quality of the product is difficult to improve, and the production cost is correspondingly improved.
In view of the current national requirement for the general iodization of common salt, the domestic demand for pharmaceutical grade and food grade iodates will increase greatly, and due to the wide range of the iodates, people generally require the improvement of the process for preparing the iodate, thereby reducing the cost and improving the quality.
The invention aims to provide an industrial method for producing iodic acid and salts thereof at low cost under the condition of simplifying the process.
The invention is implemented as follows:
the invention selects catalytic hydrogen peroxide oxidation method to prepare pure iodine acid solution, then the pure iodine acid solution reacts with hydroxide or alkali carbonate to prepare corresponding pure iodic acid salt.
In the (one) (3) oxydol and concentrated nitric acid oxidation method of the iodic acid preparation method, concentrated nitric acid and oxydol are used as composite oxidants to oxidize iodine to prepare iodic acid, wherein the dosage of the concentrated nitric acid is 1.5 times of the dosage of iodine, so that a large amount of nitrate ions exist in iodic acid solution, and the mixed acid cannot be used for reacting with hydroxide or carbonate of alkali metal to prepare pure iodate. Because the impurity separation work of the preparation method is too complicated and the quality is not high.
The invention uses nitric acid with the dosage of 1-10% of the iodine dosage to react with hydrogen peroxide with the corresponding dosage to directly prepare pure iodine acid solution. The pure iodine acid solution reacts with hydroxide or carbonate of alkali metal to directly prepare the required iodate solution, and the trace nitrate in the solution is easy to separate, so that the iodate with good quality can be prepared under the condition of low cost.
Meanwhile, the invention discovers that oxygen-containing acid and non-oxygen-containing acid of a smallamount of chloric acid, bromic acid, iodic acid, hydroiodic acid and other halogen elements have catalytic action in the hydrogen peroxide oxidation reaction of iodine. The addition amount is 0.5-50% of the iodine amount.
The key point of the invention is that the catalyst is selected in the oxidation reaction of iodine by hydrogen peroxide, and iodine can be oxidized into iodic acid at the temperature of 50-100 ℃.
Oxo or non-oxo acids of halogens
The reaction liquid generated by the reaction can directly react with hydroxide or carbonate of alkali metal without separating impurities, and the reaction can also not generate impurities, and pure high-quality iodate can be prepared by simple steps of evaporation, crystallization, water washing, drying and the like. The method of the present invention has no inevitable impurity separating process and harmful gas recovering process, and thus has greatly shortened technological steps, less investment in apparatus, low power consumption, low production cost and high product quality. The method has more obvious superiority and advancement in preparing alkali metal iodate with higher solubility.
By adopting the production process of iodic acid and iodate thereof, if medicinal potassium iodate or food-grade calcium iodate is to be prepared, industrial high-grade potassium carbonate or lime milk can be reacted with refined iodine and industrial high-grade hydrogen peroxide under the specified conditions, and then a pure product with the yield of 89-91% can be obtained.
The catalyst selected by the invention has the characteristics of small dosage, obvious catalytic effect, simple process operation, no impurities in the system and the like. A typical example of the invention is as follows:
adding a certain amount of refined iodine at the temperature of 50-100 ℃, adding a proper amount of water, a certain amount of hydrogen peroxide and a small amount of nitric acid or oxyacid or non-oxyacid of halogen, stirring for 2-8 hours under the condition of keeping the temperature to obtain a pure iodine acid solution with the content of about 18-23 percent, wherein the conversion rate of the iodic acid is about 90-99 percent (taking the input amount of the pure iodine as a calculation reference); then adding proper quantity of alkali metal hydroxide or carbonate solution into said pure iodine acid solution to make pH of said solution be 7, evaporating said neutral solution, crystallizing, filtering, washing and drying so as to obtain iodate whose content is higher than 99%, and its yield can be up to 85-95% calculated by starting iodine-adding quantity
References to the invention:
(1) the book of inorganic chemistry, second edition, inorganic chemistry research and development room edition of Beijing university of teachers, university of China, university of teachers in Nanjing; advanced education press, 2 months 1986;
(2) "handbook of inorganic chemical Synthesis", edited by the society of chemical Japan, published by the chemical industry Press, 10 months in 1983;
(3) (inorganic preparation chemical handbook), (de) George Bolaer eds, published by chemical industry Press 7 months 1959;
(4) and the handbook of Fine chemical engineering in the world, the institute of science and technology and information of Ministry of chemical industry, published in 5 months in 1986.
The present invention will be described in detail with reference to the following flowchart and examples.
FIG. 1 is a process flow diagram of iodic acid and iodate in accordance with the present invention.
Reference is made to the following examples with reference to fig. 1.
The raw materials and specifications used by the method are as follows:
superior grade of refined iodine industry
Superior grade of hydrogen peroxide industry
Industrial grade superior hydroxide
Industrial super grade of alkali metal carbonate
Industrial grade of oxygen-containing or non-oxygen acids of halogen
Distilled or deionized water
Example 1:
100 kg of distilled water, 50 kg of hydrogen peroxide (calculated by 100%), 2 l of nitric acid (98%) and 40 kg of refined iodine are added into a 500-liter reaction kettle, the mixture is continuously stirred, the temperature is controlled within the range of 50-90 ℃, and the reaction is carried out for 2-4 hours, so that 300 kg of iodic acid solution with the content of 18% can be prepared, and the yield of the iodic acid is 98% (based on the amount of iodine added). Then, the mixture was stirred continuously at a temperature ranging from 20 ℃ to 50 ℃ and a 40% strength potassium carbonate solution was slowly added so that the pH of the reaction solution became 7 and the total amount of the added potassium carbonate solution became 61 kg. Filtering the separated crystal by a filter, returning the mother liquor to the reaction kettle for evaporation and recrystallization, washing the crystal by using distilled shower water, and finally drying the washed crystal at 70-110 ℃ until the water content is less than 0.5 percent to obtain 60 kilograms of finished potassium iodate (the content is not less than 99.0 percent), wherein the yield is 91 percent calculated by iodic acid
Example 2:
20 kg of deionized water, 40 kg of refined iodine, 60 kg of hydrogen peroxide (calculated by 100%) and 20 kg of chloric acid (with the concentration of 10%) are added into a 500-liter reaction kettle, and the mixture is reacted for 8 hours under continuous stirring at the temperature of 50-90 ℃ to obtain 235 kg of 23% iodic acid solution, wherein the yield of iodic acid is 98% (calculated by iodine). After the temperature of the iodic acid solution was lowered to 20 c, 64 kg of potassium carbonate solution was added until the PH of the potassium carbonate solution was equal to 7 by slowly adding 40% potassium carbonate solution. Filtering the separated crystal in a filter, evaporating the mother liquor for crystallization to recover potassium iodate, washing the filtered potassium iodate crystal with deionized water, taking out the crystal, and drying at 75 ℃ until the water content is less than 0.5%, thus obtaining 64 kg of finished product potassium iodate with the content not less than 99.0%. The yield was 90% calculated as iodine.
Example 3:
40 kg of refined iodine, 52 kg of hydrogen peroxide (calculated by 100 percent), 100 kg of distilled water and 20 kg of 10 percent iodic acid solution are added into a 500-liter reaction kettle, and continuously stirred at 90 ℃ and reacted for 6 hours to obtain 281 kg of 20 percent iodic acid solution, wherein the yield of the iodic acid is 98 percent calculated by iodine. Cooling the temperature of the iodic acid solution to 30 ℃, slowly adding 40% potassium carbonate solution until the pH value of the solution is equal to 7, adding 56 kg of the potassium carbonate solution, filtering the reaction slurry with separated crystals, evaporating the mother liquor to recover potassium iodate, leaching the filtered crystals with distilled water, taking out the crystals, and drying at 95 ℃ until the free moisture is lower than 0.5%, thus obtaining 61 kg of finished product potassium iodate (the content is not lower than 99.0%). The yield thereof was 89% based on iodic acid.
Claims (3)
1. An industrial method for preparing pure iodine acid solution and its salts, it is a method for adopting refined iodine to oxidize by hydrogen peroxide to prepare iodic acid, characterized by that in the reaction of adopting hydrogen peroxide to oxidize refined iodine to prepare pure iodic acid, add a small amount of nitric acid or a small amount of oxyacid of halogen, oxyacid not as catalyst of oxidation reaction, the addition amount of nitric acid used is 1-10% of the amount of refined iodine charged, the addition amount of oxyacid, oxyacid not using halogen is 0.5-50% of the amount of refined iodine charged; the reaction temperature is within the range of 50 ℃ to 100 ℃; the yield of pure iodic acid is 90-99% (calculated by iodine).
2. An industrial method for preparing pure iodine acid solution and its salts is characterized by that its iodate salt preparation is a method using pure iodine acid solution to directly neutralize with hydroxide or alkali metal carbonate solution; wherein the temperature of the neutralization reaction is controlled in the range of 20 ℃ to 50 ℃ and the pH of the neutralization is equal to 7; the purity of the finished iodate is 99%, and the yield is 85-95% calculated by iodic acid.
3. An oxidation catalyst according to claim 1, characterized in that, in addition to nitric acid, mainly chloric acid, bromic acid, iodic acid, hydriodic acid are used.
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| CN94111445A CN1034410C (en) | 1994-09-03 | 1994-09-03 | Industrial method for preparation of pure iodic acid solution and its salts |
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| CN94111445A CN1034410C (en) | 1994-09-03 | 1994-09-03 | Industrial method for preparation of pure iodic acid solution and its salts |
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| CN1034410C CN1034410C (en) | 1997-04-02 |
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Cited By (7)
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|---|---|---|---|---|
| CN1298616C (en) * | 2004-06-21 | 2007-02-07 | 汕头西陇化工有限公司 | Preparation of potassium iodate |
| CN101397126B (en) * | 2007-09-28 | 2012-01-25 | 天津市化学试剂研究所 | Method for preparing primary standard reagent potash iodate |
| CN105174220A (en) * | 2015-07-21 | 2015-12-23 | 安徽六国化工股份有限公司 | Method for preparing iodate by recovering high-valence iodine associated with phosphate rock in wet-process phosphoric acid production |
| CN106276805A (en) * | 2015-06-05 | 2017-01-04 | 颜笑天 | A kind of preparation method of iodate |
| CN107934917A (en) * | 2017-12-13 | 2018-04-20 | 西陇科学股份有限公司 | A kind of production method of high yield Potassiumiodate |
| CN108083232A (en) * | 2016-11-21 | 2018-05-29 | 国药集团化学试剂有限公司 | A kind of preparation method of Potassiumiodate |
| CN109250689A (en) * | 2018-11-29 | 2019-01-22 | 河北远大中正生物科技有限公司 | It is a kind of rinsed using secondary zinc oxide after the salt water technique for preparing calcium iodate as raw material |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE3207884A1 (en) * | 1982-03-05 | 1983-09-15 | Riedel-De Haen Ag, 3016 Seelze | Process for the preparation of crystalline calcium iodate |
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1994
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1298616C (en) * | 2004-06-21 | 2007-02-07 | 汕头西陇化工有限公司 | Preparation of potassium iodate |
| CN101397126B (en) * | 2007-09-28 | 2012-01-25 | 天津市化学试剂研究所 | Method for preparing primary standard reagent potash iodate |
| CN106276805A (en) * | 2015-06-05 | 2017-01-04 | 颜笑天 | A kind of preparation method of iodate |
| CN105174220A (en) * | 2015-07-21 | 2015-12-23 | 安徽六国化工股份有限公司 | Method for preparing iodate by recovering high-valence iodine associated with phosphate rock in wet-process phosphoric acid production |
| CN105174220B (en) * | 2015-07-21 | 2017-05-17 | 安徽六国化工股份有限公司 | Method for preparing iodate by recovering phosphorite associated high-valence iodine in wet-process phosphoric acid production |
| CN108083232A (en) * | 2016-11-21 | 2018-05-29 | 国药集团化学试剂有限公司 | A kind of preparation method of Potassiumiodate |
| CN107934917A (en) * | 2017-12-13 | 2018-04-20 | 西陇科学股份有限公司 | A kind of production method of high yield Potassiumiodate |
| CN109250689A (en) * | 2018-11-29 | 2019-01-22 | 河北远大中正生物科技有限公司 | It is a kind of rinsed using secondary zinc oxide after the salt water technique for preparing calcium iodate as raw material |
| CN109250689B (en) * | 2018-11-29 | 2020-06-05 | 河北远大中正生物科技有限公司 | Process for preparing calcium iodate by taking saline water obtained after rinsing secondary zinc oxide as raw material |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1034410C (en) | 1997-04-02 |
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