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
- Authority
- 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.)
- Active
Links
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 |
Publications (2)
Publication Number | Publication Date |
---|---|
CN102249190A CN102249190A (en) | 2011-11-23 |
CN102249190B true CN102249190B (en) | 2013-03-13 |
Family
ID=44976830
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
CN 201110208319 Active CN102249190B (en) | 2011-07-25 | 2011-07-25 | Method for purifying hydroiodic acid |
Country Status (1)
Country | Link |
---|---|
CN (1) | CN102249190B (en) |
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 |
Also Published As
Publication number | Publication date |
---|---|
CN102249190A (en) | 2011-11-23 |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
CN106698352A (en) | Method and device for preparing high-purity fluorine gas or high-purity fluorine-containing mixed gas | |
CN102249190B (en) | Method for purifying hydroiodic acid | |
CN105238933B (en) | It is a kind of from the method containing removing and reclaiming element mercury in sulfur dioxide flue gas | |
CN101804969A (en) | Low-carbon environment friendly production method for extra high-purity H2O2 | |
CN103432986A (en) | Magnetic kieselgur based adsorbent, and preparation method and application thereof | |
CN102994748A (en) | Fixed-bed adsorption method for removing boron from salt lake magnesium chloride brine | |
CN1332918C (en) | Method for preparing ultra high-purity alcohol compound | |
CN109637686B (en) | Purification treatment method for uranium tetrafluoride fluorinated tail gas leacheate | |
Li et al. | The enrichment of rare earth from magnesium salt leaching solution of ion-adsorbed type deposit: A waste-free process for removing impurities | |
CN106710659B (en) | A kind of method using silicon dioxide composite material absorption Uranium in Waste Water acyl | |
CN102372264A (en) | Phosphorus pentafluoride purifying method | |
CN100384798C (en) | Prepn process of high purity alcohol reagent | |
CN207943871U (en) | A kind of fluosilicic acid produces the production system of anhydrous hydrogen chloride | |
TWI585035B (en) | A waste acid recycling process | |
CN102502499B (en) | Preparation process for super-clean high-purity hydrochloric acid | |
CN110252269A (en) | A kind of resin regeneration method for handling containing high-boiling components waste water | |
CN102875355B (en) | Purification method of cobalt acetate | |
CN103935963B (en) | The method of purifying industrial aqueous hydrogen peroxide solution | |
CN103497265A (en) | Method for preparing resin adsorbent for refining electronic grade phosphoric acid | |
CN105060249B (en) | A kind of method that tail gas hydrogen chloride produced using production monoxone prepares refined hydrochloric acid | |
CN103058819A (en) | Method for removing ferric trichloride from chlorination reaction liquid with styrene type macroporous anion exchange resin | |
CN103011172A (en) | Purification method of impurity iodine in silicon tetrafluoride gas | |
CN102718191A (en) | Method for purifying sulfur | |
CN102502501A (en) | Method for extracting iodine from wet-process phosphoric acid produced from iodine-containing phosphorous ore by semi-water and bi-water method | |
CN109046238B (en) | Preparation method and regeneration method of compound ammonia nitrogen adsorbent |
Legal Events
Date | Code | Title | Description |
---|---|---|---|
C06 | Publication | ||
PB01 | Publication | ||
C10 | Entry into substantive examination | ||
SE01 | Entry into force of request for substantive examination | ||
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. |
|
C14 | Grant of patent or utility model | ||
GR01 | Patent grant |