CN103523753A - Method of preparing high-purity hydroiodic acid from iodine-containing solution - Google Patents
Method of preparing high-purity hydroiodic acid from iodine-containing solution Download PDFInfo
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- CN103523753A CN103523753A CN201310497800.4A CN201310497800A CN103523753A CN 103523753 A CN103523753 A CN 103523753A CN 201310497800 A CN201310497800 A CN 201310497800A CN 103523753 A CN103523753 A CN 103523753A
- Authority
- CN
- China
- Prior art keywords
- reaction
- biodine
- purity
- iodine
- hydroiodic acid
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- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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- XMBWDFGMSWQBCA-UHFFFAOYSA-N hydrogen iodide Chemical compound I XMBWDFGMSWQBCA-UHFFFAOYSA-N 0.000 title claims abstract description 31
- 229910052740 iodine Inorganic materials 0.000 title claims abstract description 25
- 239000011630 iodine Substances 0.000 title claims abstract description 25
- ZCYVEMRRCGMTRW-UHFFFAOYSA-N 7553-56-2 Chemical compound [I] ZCYVEMRRCGMTRW-UHFFFAOYSA-N 0.000 title claims abstract description 24
- 229940071870 hydroiodic acid Drugs 0.000 title claims abstract description 22
- 238000000034 method Methods 0.000 title claims abstract description 22
- 238000006477 desulfuration reaction Methods 0.000 claims abstract description 8
- 230000023556 desulfurization Effects 0.000 claims abstract description 8
- 239000000126 substance Substances 0.000 claims abstract description 8
- 238000006243 chemical reaction Methods 0.000 claims description 38
- 239000000706 filtrate Substances 0.000 claims description 19
- 238000003756 stirring Methods 0.000 claims description 19
- AYJRCSIUFZENHW-UHFFFAOYSA-L barium carbonate Chemical compound [Ba+2].[O-]C([O-])=O AYJRCSIUFZENHW-UHFFFAOYSA-L 0.000 claims description 16
- 235000019353 potassium silicate Nutrition 0.000 claims description 8
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 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
- 239000002253 acid Substances 0.000 claims description 6
- 229910052739 hydrogen Inorganic materials 0.000 claims description 6
- 239000001257 hydrogen Substances 0.000 claims description 6
- 125000004435 hydrogen atom Chemical class [H]* 0.000 claims description 6
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 claims description 2
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims description 2
- 239000004411 aluminium Substances 0.000 claims description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 2
- 229910052782 aluminium Inorganic materials 0.000 claims description 2
- 229910052791 calcium Inorganic materials 0.000 claims description 2
- 239000011575 calcium Substances 0.000 claims description 2
- XMBWDFGMSWQBCA-UHFFFAOYSA-M iodide Chemical compound [I-] XMBWDFGMSWQBCA-UHFFFAOYSA-M 0.000 claims description 2
- 229940006461 iodide ion Drugs 0.000 claims description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 2
- 229910052742 iron Inorganic materials 0.000 claims description 2
- -1 iron ion Chemical class 0.000 claims description 2
- 229910052749 magnesium Inorganic materials 0.000 claims description 2
- 239000011777 magnesium Substances 0.000 claims description 2
- 230000008719 thickening Effects 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 abstract description 7
- 239000002994 raw material Substances 0.000 abstract description 6
- 238000010924 continuous production Methods 0.000 abstract 1
- 238000006115 defluorination reaction Methods 0.000 abstract 1
- 238000004321 preservation Methods 0.000 abstract 1
- 238000006722 reduction reaction Methods 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 17
- 239000000047 product Substances 0.000 description 16
- 230000035484 reaction time Effects 0.000 description 12
- 238000001914 filtration Methods 0.000 description 5
- RWSOTUBLDIXVET-UHFFFAOYSA-N Dihydrogen sulfide Chemical compound S RWSOTUBLDIXVET-UHFFFAOYSA-N 0.000 description 4
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 4
- 229910000037 hydrogen sulfide Inorganic materials 0.000 description 4
- 238000002360 preparation method Methods 0.000 description 4
- 239000007864 aqueous solution Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 229910000043 hydrogen iodide Inorganic materials 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 238000013019 agitation Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- DNJIEGIFACGWOD-UHFFFAOYSA-N ethanethiol Chemical group CCS DNJIEGIFACGWOD-UHFFFAOYSA-N 0.000 description 1
- 238000010304 firing Methods 0.000 description 1
- 239000000796 flavoring agent Substances 0.000 description 1
- 235000019634 flavors Nutrition 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 230000002829 reductive effect Effects 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 235000012976 tarts Nutrition 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Landscapes
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
Abstract
The invention discloses a method of preparing high-purity hydroiodic acid from an iodine-containing solution. The method comprises the steps: with the iodine-containing solution as a raw material, preparing the high-purity hydroiodic acid by the steps of elemental iodine reduction, desulfurization, defluorination, concentration and the like. According to the method, the high-purity hydroiodic acid product has the purity at above 98 percent, is suitable for preparing iodine chemical downstream products with high added value, overcomes the safety hidden dangers of the traditional process in the production process, is high in the product purity, is low in the production cost, is stable in the product quality, and can be stored for a long time by virtue of a correct preservation method. The method is suitable for industrial large-scale continuous production.
Description
Technical field
The present invention relates to hydrogen iodide, specifically a kind of preparation method of high-purity hydrogen acid iodide.
Background technology
Hydroiodic acid HI is the aqueous solution of hydrogen iodide, has the tart flavour of intense stimulus, easily oxidized and separate out free-iodine in air.Be mainly used in the preparation of raw material and the organic iodide of analytical reagent and reductive agent, medicine intermediate, sterilant.The method of preparing at present hydroiodic acid HI both at home and abroad mainly contains two kinds:
1, iodine and red phosphorus chemical synthesis: it is raw material that this method is utilized iodine and red phosphorus, the first product of synthetic hydroiodic acid HI in the aqueous solution, then obtain through distillation.Building-up reactions has two steps: 2P+3I
3→ 2PI
3; PI
3+ 3H
20 → H
3pO
3+ 3HI; Adopt this legal system need control temperature of reaction for hydroiodic acid HI and be no more than 80 ℃, otherwise the easy volatilization loss of iodine should fully stir during operation, allow iodine and phosphorus be submerged in completely in water, during filtration, need pay special attention to filter clean red phosphorus, otherwise security incident may occur.
2, hydrogen sulfide reduction iodine preparation method: this method elemental iodine is raw material, utilizes hydrogen sulfide reduction elemental iodine to prepare hydroiodic acid HI.Chemical equation is: H
2s+I
2→ 2HI+S, gets a certain amount of elemental iodine and is dissolved in a certain amount of pure water, under agitation passes into hydrogen sulfide, when solution becomes colorless, filters, and filtrate is distilled and obtained hydroiodic acid HI.Utilize this legal system high for hydroiodic acid HI purity, but hydrogen sulfide is stench, hypertoxic gas, and in air easy firing, during operation, should be noted and prevent security incident.
Summary of the invention
The object of the present invention is to provide a kind of method of utilizing Biodine to prepare high-purity hydrogen acid iodide; utilize this legal system for hydroiodic acid HI, to overcome the potential safety hazard existing in traditional technology production process; and the product purity of preparation is high, production cost is low, constant product quality, be applicable to industrial mass-producing, serialization production.
Technical scheme of the present invention is: a kind of method of utilizing Biodine to prepare high-purity hydrogen acid iodide, and the method comprises 4 processing steps:
1. elemental iodine reduction: get 500ml Biodine, add S-WAT and react 10 ~ 60min;
2. desulfurization: filter in backward filtrate and add barium carbonate to react 40 ~ 120min;
3. defluorinate: after reaction, solution left standstill filters half an hour, adds water glass in filtrate, reacts 5 ~ 60min;
4. concentrated: reaction finishes rear solution filters again, gets filtrate vacuum concentration, prepares the hydroiodic acid HI solution of different concns.
Above-mentioned steps 1. in, described Biodine, its principal element content consists of: elemental iodine is the about 30000 ~ 50000ppm of 100 ~ 1500ppm iodide ion approximately; Sulfate radical is 35000 ~ 60000ppm approximately; The about 400-1500ppm of fluorion; Calcium, magnesium, aluminium, iron ion are total to approximately 50 ~ 200ppm.
Above-mentioned steps 1. in, control temperature of reaction: 25 ~ 60 ℃; In S-WAT and Biodine, the amount of substance of elemental iodine than (mol ratio) is: 1 ~ 1.4:1; Stirring velocity during reaction is: 50 ~ 300rpm.
Above-mentioned steps 2. in, control temperature of reaction: 25 ~ 60 ℃; Stir
Speed is: 50 ~ 300rpm; Add the amount of substance of sulfate radical in barium carbonate and Biodine than (mol ratio) to be: 1 ~ 1.4:1.
Above-mentioned steps 3. in, in water glass add-on and Biodine, the amount of substance of fluorion than (mol ratio) is: 0.17 ~ 0.23:1; Temperature of reaction is: 25 ~ 60 ℃; Stirring velocity is: 50 ~ 400rpm.
Above-mentioned steps 4. in, concentrated vacuum tightness is-0.1 ~ 0MPa; Thickening temperature is 30 ~ 65 ℃.
The present invention utilizes Biodine for raw material, and through the reduction of elemental iodine in solution, desulfurization, defluorinate, concentratedly prepare high-purity hydrogen acid iodide, product purity can reach more than 98%.Whole production process is simple, with short production cycle, utilization rate of raw materials is high, and waste is few, is a kind of environmental type technique.
Embodiment
embodiment 1
Get 500ml Biodine, add the elemental iodine in 0.4644g S-WAT reduction Biodine, 40 ℃ of temperature of reaction of control, stirring velocity are that 150rpm, reaction times are 30min.Reaction finishes rear filtration, to the barium carbonate desulfurization that adds 36.2873g in filtrate, controls 45 ℃ of temperature of reaction, stirring velocity is that 220rpm, reaction times are 60min.After reaction, solution left standstill half an hour filters, and to the water glass that adds 0.8554g in filtrate, temperature of reaction is that 45 ℃, stirring velocity are 250rpm, reaction times to be: 30min.Reaction finishes rear solution filters again, and filtrate is product hydroiodic acid HI, and analyzing and recording product purity is 98.4%.Product can be prepared the hydroiodic acid HI solution of different mass concentration (0-45%) through vacuum concentration.
embodiment 2
Get 500ml Biodine, add the elemental iodine in 0.6414g S-WAT reduction Biodine, 40 ℃ of temperature of reaction of control, stirring velocity are that 100rpm, reaction times are 20min.Reaction finishes rear filtration, to the barium carbonate desulfurization that adds 38.2873g in filtrate, controls 45 ℃ of temperature of reaction, stirring velocity is that 220rpm, reaction times are 40min.After reaction, solution left standstill half an hour filters, and to the water glass that adds 0.8854g in filtrate, temperature of reaction is that 45 ℃, stirring velocity are 250rpm, reaction times to be: 30min.Reaction finishes rear solution filters again, and filtrate is product hydroiodic acid HI, and analyzing and recording product purity is 97.7%.Product can be prepared the hydroiodic acid HI solution of different mass concentration (0-45%) through vacuum concentration.
embodiment 3
Get 500ml Biodine, add the elemental iodine in 0.5142g S-WAT reduction Biodine, 30 ℃ of temperature of reaction of control, stirring velocity are that 200rpm, reaction times are 60min.Reaction finishes rear filtration, to the barium carbonate desulfurization that adds 36.2873g in filtrate, controls 45 ℃ of temperature of reaction, stirring velocity is that 300rpm, reaction times are 60min.After reaction, solution left standstill half an hour filters, and to the water glass that adds 0.9114g in filtrate, temperature of reaction is that 45 ℃, stirring velocity are 250rpm, reaction times to be: 30min.Reaction finishes rear solution filters again, and filtrate is product hydroiodic acid HI, and analyzing and recording product purity is 96.9%.Product can be prepared the hydroiodic acid HI solution of different mass concentration (0-45%) through vacuum concentration.
embodiment 4
Get 500ml Biodine, add the elemental iodine in 0.6111g S-WAT reduction Biodine, 40 ℃ of temperature of reaction of control, stirring velocity are that 120rpm, reaction times are 40min.Reaction finishes rear filtration, to the barium carbonate desulfurization that adds 37.7823g in filtrate, controls 45 ℃ of temperature of reaction, stirring velocity is that 220rpm, reaction times are 60min.After reaction, solution left standstill half an hour filters, and to the water glass that adds 0.8933g in filtrate, temperature of reaction is that 45 ℃, stirring velocity are 300rpm, reaction times to be: 30min.Reaction finishes rear solution filters again, and filtrate is product hydroiodic acid HI, and analyzing and recording product purity is 98.1%.Product can be prepared the hydroiodic acid HI solution of different mass concentration (0-45%) through vacuum concentration.
Claims (6)
1. utilize Biodine to prepare a method for high-purity hydrogen acid iodide, its feature the method comprises 4 processing steps:
1. elemental iodine reduction: get 500ml Biodine, add S-WAT and react 10 ~ 60min;
2. desulfurization: filter in backward filtrate and add barium carbonate to react 40 ~ 120min;
3. defluorinate: after reaction, solution left standstill filters half an hour, adds water glass in filtrate, reacts 5 ~ 60min;
4. concentrated: reaction finishes rear solution filters again, gets filtrate vacuum concentration, prepares the hydroiodic acid HI solution of different concns.
2. in accordance with the method for claim 1, it is characterized in that: step 1. in, control temperature of reaction: 25 ~ 60 ℃; In S-WAT and Biodine, the amount of substance ratio of elemental iodine is: 1 ~ 1.4:1; Stirring velocity during reaction is: 50 ~ 300rpm.
3. in accordance with the method for claim 1, it is characterized in that: step 2. in, control temperature of reaction: 25 ~ 60 ℃; Stirring velocity is: 50 ~ 300rpm; Add the amount of substance ratio of sulfate radical in barium carbonate and Biodine to be: 1 ~ 1.4:1.
4. in accordance with the method for claim 1, it is characterized in that: step 3. in, in water glass add-on and Biodine, the amount of substance ratio of fluorion is: 0.17 ~ 0.23:1; Temperature of reaction is: 25 ~ 60 ℃; Stirring velocity is: 50 ~ 400rpm.
5. in accordance with the method for claim 1, it is characterized in that: step 4. in, concentrated vacuum tightness is-0.1 ~ 0MPa; Thickening temperature is 30 ~ 65 ℃.
6. according to the method described in claim 1-5, it is characterized in that: the Biodine of step described in 1., its principal element content consists of: elemental iodine is the about 30000 ~ 50000ppm of 100 ~ 1500ppm iodide ion approximately; Sulfate radical is 35000 ~ 60000ppm approximately; The about 400-1500ppm of fluorion; Calcium, magnesium, aluminium, iron ion are total to approximately 50 ~ 200ppm.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310497800.4A CN103523753A (en) | 2013-10-22 | 2013-10-22 | Method of preparing high-purity hydroiodic acid from iodine-containing solution |
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|---|---|---|---|
| CN201310497800.4A CN103523753A (en) | 2013-10-22 | 2013-10-22 | Method of preparing high-purity hydroiodic acid from iodine-containing solution |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104085857A (en) * | 2014-06-26 | 2014-10-08 | 周海军 | New method for preparing high-purity hydroiodic acid |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102502504A (en) * | 2011-10-26 | 2012-06-20 | 瓮福（集团）有限责任公司 | Method for preparing iodized salt from iodine-contained absorption solution |
-
2013
- 2013-10-22 CN CN201310497800.4A patent/CN103523753A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102502504A (en) * | 2011-10-26 | 2012-06-20 | 瓮福（集团）有限责任公司 | Method for preparing iodized salt from iodine-contained absorption solution |
Non-Patent Citations (1)
| Title |
|---|
| 何之华 等: "工业磷酸用氯化钠、硅酸钠脱氟的实验研究", 《磷肥与复肥》, vol. 24, 31 March 2009 (2009-03-31), pages 21 - 23 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104085857A (en) * | 2014-06-26 | 2014-10-08 | 周海军 | New method for preparing high-purity hydroiodic acid |
| CN104085857B (en) * | 2014-06-26 | 2015-12-30 | 周海军 | A kind of novel method preparing high-purity hydrogen acid iodide |
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| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
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| C02 | Deemed withdrawal of patent application after publication (patent law 2001) | ||
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Application publication date: 20140122 |