CN102249190A - Method for purifying hydroiodic acid - Google Patents
Method for purifying hydroiodic acid Download PDFInfo
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- CN102249190A CN102249190A CN201110208319XA CN201110208319A CN102249190A CN 102249190 A CN102249190 A CN 102249190A CN 201110208319X A CN201110208319X A CN 201110208319XA CN 201110208319 A CN201110208319 A CN 201110208319A CN 102249190 A CN102249190 A CN 102249190A
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- hydroiodic acid
- copper powder
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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 the iodine hydracid again, 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 the hydroiodic acid HI instability, in storage, meet under the effect of light and air, can dissociate iodine and become yellow, brown even brown influence 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 distillatory method removal hydroiodic acid HI, reaches the purpose of purifying, but this method distillation temperature height, complex operation, easy contaminate environment, poor stability, energy consumption is big, and the cost height 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 big, the deficiency that cost is high.
Technical conceive of the present invention is such: with the technical grade hydroiodic acid HI is raw material, the core tube container that feeding has copper powder decolours, remove the iodine in the raw material, adsorption column through having the mesoporous sorbent material of earth silicon material is removed metal copper ion then, promptly obtains 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 having the core tube container of copper powder, same condition, with adsorbing by the adsorption column that has the mesoporous SiO 2 sorbent material under the flow velocity, promptly obtain the hydroiodic acid HI of purifying.
According to the method described above, the described core tube container that has copper powder, be identical at two diameters, add copper powder in the middle of the core plate of band filter pore, be fixed on the ducted ring support by air pressure, promptly be combined into the tube container that has 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 is meant with EDTA to be the mesoporous SiO 2 sorbent material of 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.
Of the present invention is that the mesoporous sorbent material of earth silicon material of finishing can be according to document Microporous and Mesoporous Material with EDTA, 2007, and the 103:316-324 reported method 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, removes metal copper ion through the absorption of the mesoporous sorbent material of earth silicon material again, has improved the quality of hydroiodic acid HI purifying; The mesoporous sorbent material of employed earth silicon material can reclaiming, reuses, and is with low cost; Method simple and safe operation of the present invention, energy consumption reduces, and constant product quality is suitable for serialization production.
Figure of description
Fig. 1 is the structural representation that has the core tube container of 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 the hydroiodic acid HI 96.1g of purifying at last.
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 the hydroiodic acid HI 94.6g of purifying at last.
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 the hydroiodic acid HI 95.6g of purifying at last.
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 the present invention is had been described in detail with reference to preferred embodiment, 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 having the core tube container of copper powder, same condition, with adsorbing by the adsorption column that has the mesoporous SiO 2 sorbent material under the flow velocity, promptly obtain the hydroiodic acid HI of purifying.
2. method according to claim 1, it is characterized in that, the described core tube container that has copper powder, be identical at two diameters, add copper powder in the middle of the core plate of band filter pore, be fixed on the ducted ring support by air pressure, promptly be combined into the tube container that has 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 is meant with EDTA to be the mesoporous SiO 2 sorbent material of 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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| CN102249190A true CN102249190A (en) | 2011-11-23 |
| CN102249190B CN102249190B (en) | 2013-03-13 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN 201110208319 Active CN102249190B (en) | 2011-07-25 | 2011-07-25 | Method for purifying hydroiodic acid |
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Cited By (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 |
Cited By (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 |
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| Publication number | Publication date |
|---|---|
| CN102249190B (en) | 2013-03-13 |
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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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