CN102249190B - Method for purifying hydroiodic acid - Google Patents
Method for purifying hydroiodic acid Download PDFInfo
- Publication number
- CN102249190B CN102249190B CN 201110208319 CN201110208319A CN102249190B CN 102249190 B CN102249190 B CN 102249190B CN 201110208319 CN201110208319 CN 201110208319 CN 201110208319 A CN201110208319 A CN 201110208319A CN 102249190 B CN102249190 B CN 102249190B
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- CN
- China
- Prior art keywords
- hydroiodic acid
- copper powder
- purifying
- tube container
- sorbent material
- Prior art date
- 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 45
- 229940071870 hydroiodic acid Drugs 0.000 title claims abstract description 39
- 238000000034 method Methods 0.000 title claims abstract description 18
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims abstract description 26
- 229910004298 SiO 2 Inorganic materials 0.000 claims description 11
- 239000002594 sorbent Substances 0.000 claims description 11
- 238000000746 purification Methods 0.000 claims description 7
- 238000001179 sorption measurement Methods 0.000 claims description 7
- KCXVZYZYPLLWCC-UHFFFAOYSA-N EDTA Chemical compound OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC(O)=O KCXVZYZYPLLWCC-UHFFFAOYSA-N 0.000 claims description 6
- 239000002253 acid Substances 0.000 claims description 5
- 229910052739 hydrogen Inorganic materials 0.000 claims description 4
- 239000001257 hydrogen Substances 0.000 claims description 4
- 125000004435 hydrogen atom Chemical class [H]* 0.000 claims description 4
- 239000002245 particle Substances 0.000 claims description 2
- 239000011148 porous material Substances 0.000 claims description 2
- ZCYVEMRRCGMTRW-UHFFFAOYSA-N 7553-56-2 Chemical compound [I] ZCYVEMRRCGMTRW-UHFFFAOYSA-N 0.000 abstract description 13
- 229910052740 iodine Inorganic materials 0.000 abstract description 13
- 239000011630 iodine Substances 0.000 abstract description 13
- 239000002184 metal Substances 0.000 abstract description 7
- 229910052751 metal Inorganic materials 0.000 abstract description 7
- 239000003463 adsorbent Substances 0.000 abstract description 6
- JPVYNHNXODAKFH-UHFFFAOYSA-N Cu2+ Chemical compound [Cu+2] JPVYNHNXODAKFH-UHFFFAOYSA-N 0.000 abstract description 5
- 229910001431 copper ion Inorganic materials 0.000 abstract description 5
- 239000002994 raw material Substances 0.000 abstract description 4
- 229910052802 copper Inorganic materials 0.000 abstract description 3
- 239000010949 copper Substances 0.000 abstract description 3
- 238000005265 energy consumption Methods 0.000 abstract description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical group O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 abstract 3
- 239000000463 material Substances 0.000 abstract 2
- 229910052814 silicon oxide Inorganic materials 0.000 abstract 2
- 238000010521 absorption reaction Methods 0.000 abstract 1
- 238000010924 continuous production Methods 0.000 abstract 1
- 235000000396 iron Nutrition 0.000 abstract 1
- 239000002210 silicon-based material Substances 0.000 description 4
- 238000004458 analytical method Methods 0.000 description 3
- 238000004821 distillation Methods 0.000 description 3
- 238000005070 sampling Methods 0.000 description 3
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 229910021645 metal ion Inorganic materials 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 229910000043 hydrogen iodide Inorganic materials 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- PNDPGZBMCMUPRI-UHFFFAOYSA-N iodine Chemical compound II PNDPGZBMCMUPRI-UHFFFAOYSA-N 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000013335 mesoporous material Substances 0.000 description 1
- 239000012229 microporous material Substances 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 239000012450 pharmaceutical intermediate Substances 0.000 description 1
- 230000002829 reductive effect Effects 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- ISIJQEHRDSCQIU-UHFFFAOYSA-N tert-butyl 2,7-diazaspiro[4.5]decane-7-carboxylate Chemical compound C1N(C(=O)OC(C)(C)C)CCCC11CNCC1 ISIJQEHRDSCQIU-UHFFFAOYSA-N 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 229910001868 water Inorganic materials 0.000 description 1
Landscapes
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
Abstract
The invention discloses a method for purifying hydroiodic acid. The method comprises the following steps of: introducing industrial hydroiodic acid into a sand core tube container with metal copper powder at flow rate of 5 to 10ml/min under the condition of light shading at the temperature of between 20 and 30 DEG C and performing decoloration, removing elementary iodine from a raw material, and removing metal copper ions by using an absorption column with a silicon oxide material mesoporous adsorbent to obtain the purified hydroiodic acid. The elementary iodine content of the hydroiodic acid which is obtained by the method for purifying the hydroiodic acid is less than 0.1ppm, and the content of metal copper irons is less than 1.0ppm. The silicon oxide material mesoporous adsorbent can be recycled and repeatedly used, and is low in cost; and the method can be operated safely and easily, the energy consumption is low, the quality of a product is stable and the method is suitable for continuous production.
Description
Technical field
The present invention relates to a kind of purification process of hydroiodic acid HI, be specifically related to a kind of iodine in the technical grade hydroiodic acid HI, purification process of raising hydroiodic acid HI quality removed.
Background technology
Hydroiodic acid HI claims again the iodine hydracid, hydrogen iodide solution.Hydroiodic acid HI is a kind of mineral acid of tool severe corrosive, is mainly used in common reagent, analytical reagent and reductive agent, and the preparation of organic iodide can be used as pharmaceutical intermediate, the raw material of sterilant.
In the prior art, the preparation method of hydroiodic acid HI adopts red phosphorus, iodine and water reaction, prepares through distillation.Because hydroiodic acid HI is unstable, in storage, meet under the effect of light and air, can dissociate iodine and become yellow, brown even brown affect the quality of hydroiodic acid HI, and need carry out purifying to hydroiodic acid HI during use.Classical purification process is an amount of phosphorous acid to be added in the hydroiodic acid HI heat, and with the iodine in the method removal hydroiodic acid HI of distillation, reach the purpose of purifying, but the method distillation temperature is high, complex operation, easy contaminate environment, poor stability, energy consumption is large, and cost is high, lacks practicality.
Summary of the invention
Technical problem to be solved by this invention is to provide a kind of purification process of technical grade hydroiodic acid HI, overcoming complex operation in the art methods, and easy contaminate environment, energy consumption is large, the deficiency that cost is high.
Technical conceive of the present invention is such: take the technical grade hydroiodic acid HI as raw material, the core tube container that passes into copper powder decolours, remove the iodine in the raw material, then remove metal copper ion through the adsorption column with the earth silicon material mesoporous adsorbent, namely obtain the hydroiodic acid HI of purifying.
The purification process of hydroiodic acid HI of the present invention specifically may further comprise the steps:
With the technical grade hydroiodic acid HI under the temperature of lucifuge, 20-30 ℃, with the flow velocity of 5-10ml/min by the core tube container with copper powder, same condition, with adsorbing by the adsorption column with the mesoporous SiO 2 sorbent material under the flow velocity, namely obtain the hydroiodic acid HI of purifying.
According to the method described above, described core tube container with copper powder, identical at two diameters, with adding copper powder in the middle of the core plate of filter pore, be fixed on the ducted ring support by air pressure, namely be combined into the tube container with the copper powder core, its structure as shown in Figure 1.Wherein leak to prevent copper powder less than the particle diameter of copper powder in the aperture of core plate.
Described mesoporous SiO 2 sorbent material refers to the mesoporous SiO 2 sorbent material take EDTA as finishing.
The copper powder that the present invention uses is analytical pure, and the mass ratio of feed hydrogen acid iodide and copper powder is 1: 0.05-0.1, and g/g, the mass ratio of feed hydrogen acid iodide and mesoporous SiO 2 sorbent material is 1: 1-20, g/g.
Hydroiodic acid HI behind the purifying that obtains with the inventive method is analyzed: wherein iodine content is less than 0.1ppm, and metal copper ion content is less than 1.0ppm.
Earth silicon material mesoporous adsorbent take EDTA as finishing of the present invention can be according to document Microporous and Mesoporous Material, and the method for 2007,103:316-324 report prepares.
The present invention's beneficial effect compared with prior art:
The present invention utilizes copper powder and the iodine effect in the hydroiodic acid HI in the copper powder core can effectively remove iodine, again through the Adsorption metal copper ion of earth silicon material mesoporous adsorbent, has improved the quality of hydroiodic acid HI purifying; Employed earth silicon material mesoporous adsorbent can reclaiming, reuses, and is with low cost; Method simple and safe operation of the present invention, Energy Intensity Reduction, constant product quality is suitable for serialization production.
Figure of description
Fig. 1 is the structural representation of the core tube container with copper powder of the present invention, and wherein 1 is ring support, and 2 is the core plate, and 3 is copper powder.
Embodiment
Below in conjunction with specific embodiment technical scheme of the present invention is described in further detail, but described embodiment does not limit protection scope of the present invention.
Embodiment 1
With 100g technical grade hydroiodic acid HI under lucifuge, 20 ℃ of temperature, with the 5.0ml/min flow velocity successively by the core tube container of 5g copper powder is housed, it is the adsorption column of the mesoporous SiO 2 sorbent material of finishing that 100g EDTA is housed, and obtains at last the hydroiodic acid HI 96.1g of purifying.
With this hydroiodic acid HI sampling analysis: iodine content is 0.83ppm, and metal copper ion concentration is 0.53ppm.
Embodiment 2
With 100g technical grade hydroiodic acid HI under lucifuge, 25 ℃ of temperature, with the 7.0ml/min flow velocity successively by the core tube container of 7g copper powder is housed, it is the adsorption column of the mesoporous SiO 2 sorbent material of finishing that 1000g EDTA is housed, and obtains at last the hydroiodic acid HI 94.6g of purifying.
With this hydroiodic acid HI sampling analysis: iodine content is 0.69ppm, and the metallic copper concentration of metal ions is 0.74ppm.
Embodiment 3
With 100g technical grade hydroiodic acid HI under lucifuge, 30 ℃ of temperature, with the 10.0ml/min flow velocity successively by the core tube container of 10g copper powder is housed, it is the adsorption column of the mesoporous SiO 2 sorbent material of finishing that 2000g EDTA is housed, and obtains at last the hydroiodic acid HI 95.6g of purifying.
With this hydroiodic acid HI sampling analysis: iodine content is 0.66ppm, and the metallic copper concentration of metal ions is 0.80ppm.
Should be noted that, above embodiment is only unrestricted in order to technical scheme of the present invention to be described, although with reference to preferred embodiment the present invention is had been described in detail, those of ordinary skill in the art is to be understood that, can make amendment or be equal to replacement the technical scheme of invention, and not breaking away from the spirit and scope of technical solution of the present invention, it all should be encompassed in the claim scope of the present invention.
Claims (6)
1. the purification process of a hydroiodic acid HI is characterized in that, comprises the steps:
With the technical grade hydroiodic acid HI under the temperature of lucifuge, 20-30 ℃, with the flow velocity of 5-10ml/min by the core tube container with copper powder, same condition, with adsorbing by the adsorption column with the mesoporous SiO 2 sorbent material under the flow velocity, namely obtain the hydroiodic acid HI of purifying.
2. method according to claim 1, it is characterized in that, described core tube container with copper powder, identical at two diameters, with adding copper powder in the middle of the core plate of filter pore, be fixed on the ducted ring support by air pressure, namely be combined into the tube container with the copper powder core.
3. method according to claim 2 is characterized in that, the aperture of described core plate is less than the particle diameter of copper powder.
4. method according to claim 1 is characterized in that, described mesoporous SiO 2 sorbent material refers to the mesoporous SiO 2 sorbent material take EDTA as finishing.
5. method according to claim 1 is characterized in that, the mass ratio of described feed hydrogen acid iodide and copper powder is 1: 0.05-0.1, g/g.
6. method according to claim 1 is characterized in that, the mass ratio of described feed hydrogen acid iodide and mesoporous SiO 2 sorbent material is 1: 1-20, g/g.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201110208319 CN102249190B (en) | 2011-07-25 | 2011-07-25 | Method for purifying hydroiodic acid |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201110208319 CN102249190B (en) | 2011-07-25 | 2011-07-25 | Method for purifying hydroiodic acid |
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| Publication Number | Publication Date |
|---|---|
| CN102249190A CN102249190A (en) | 2011-11-23 |
| CN102249190B true CN102249190B (en) | 2013-03-13 |
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| CN 201110208319 Active CN102249190B (en) | 2011-07-25 | 2011-07-25 | Method for purifying hydroiodic acid |
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Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108435137A (en) * | 2018-03-16 | 2018-08-24 | 三峡大学 | The support type reagent and preparation method of a kind of decoloration of hydrochloric acid and the removing of hydrochloric acid metal ion |
| CN108658044A (en) * | 2018-08-10 | 2018-10-16 | 太仓沪试试剂有限公司 | A kind of purification process of hydroiodic acid |
| CN113753859A (en) * | 2021-10-15 | 2021-12-07 | 太仓沪试试剂有限公司 | Method for purifying high-purity iodide |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0535605A2 (en) * | 1991-09-30 | 1993-04-07 | Union Carbide Chemicals & Plastics Technology Corporation | Iodide removal process |
| CN1302792A (en) * | 1999-12-29 | 2001-07-11 | 赫多特普索化工设备公司 | Method of reducing iodide in industrial product stream |
-
2011
- 2011-07-25 CN CN 201110208319 patent/CN102249190B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0535605A2 (en) * | 1991-09-30 | 1993-04-07 | Union Carbide Chemicals & Plastics Technology Corporation | Iodide removal process |
| US5561168A (en) * | 1991-09-30 | 1996-10-01 | Union Carbide Chemicals & Plastics Technology Corporation | Iodide removal process |
| CN1302792A (en) * | 1999-12-29 | 2001-07-11 | 赫多特普索化工设备公司 | Method of reducing iodide in industrial product stream |
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|---|---|
| CN102249190A (en) | 2011-11-23 |
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| C53 | Correction of patent for invention or patent application | ||
| CB02 | Change of applicant information |
Address after: 200072 Zhabei District, Shanghai, Shanghai Road, No. 1, building 801, No. Applicant after: Sinopharm Chemical Reagent Co., Ltd. Address before: 200002 No. 52, Ningbo Road, Shanghai, Huangpu District Applicant before: Sinopharm Chemical Reagent Co., Ltd. |
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