CN108658044A - A kind of purification process of hydroiodic acid - Google Patents
A kind of purification process of hydroiodic acid Download PDFInfo
- Publication number
- CN108658044A CN108658044A CN201810910944.0A CN201810910944A CN108658044A CN 108658044 A CN108658044 A CN 108658044A CN 201810910944 A CN201810910944 A CN 201810910944A CN 108658044 A CN108658044 A CN 108658044A
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- CN
- China
- Prior art keywords
- hydroiodic acid
- purification process
- frame structure
- structure material
- zeolite imidazole
- 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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-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B7/00—Halogens; Halogen acids
- C01B7/13—Iodine; Hydrogen iodide
- C01B7/135—Hydrogen iodide
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D15/00—Separating processes involving the treatment of liquids with solid sorbents; Apparatus therefor
- B01D15/08—Selective adsorption, e.g. chromatography
- B01D15/10—Selective adsorption, e.g. chromatography characterised by constructional or operational features
- B01D15/20—Selective adsorption, e.g. chromatography characterised by constructional or operational features relating to the conditioning of the sorbent material
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Analytical Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Inorganic Chemistry (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
Abstract
The invention discloses a kind of purification process of hydroiodic acid.The purification process is that pending hydroiodic acid crude product is made to pass through the adsorption column for being filled with zeolite imidazole ester frame structure material (ZIFs) with 10~20mL/min flow velocitys.Elemental iodine is adsorbed using zeolite imidazole ester frame structure material (ZIFs) in the purification process of the present invention, elemental iodine can be preferably removed, reduce the content of elemental iodine impurity.This purification process is easy to operate, and the product of purifying has preferable purity and high income.
Description
Technical field
The present invention relates to the technical field of hydroiodic acid purification more particularly to a kind of purification process of hydroiodic acid.
Background technology
Hydroiodic acid is aqueous azeotrope, contains 55~57% hydrogen iodide.The liquid of colourless to light yellow irritant stink
Body, in air strong smoke.122.5~126.5 DEG C of boiling point, (0.936~0. 99g/ containing HI of relative density d=1. 07
ML), -50.8 DEG C of fusing point (sterling).In addition a concentration of 45% and 67% hydroiodic acid, 67% hydroiodic acid are added 0.03%
Hypophosphorous acid can be more stable.Place several big if bottleneck opened, hydroiodic acid solution can go bad, and should be sealed and before sealing
It is filled with nitrogen.As reducing agent, it is also used for synthesis iodine alkane and other iodine body compounds.
It is elemental iodine that content is higher in hydroiodic acid impurity, if elemental iodine can be effectively removed directly about the good of purifying
It is bad.Chinese patent CN201010285002.1 discloses a kind of preparation method of hydroiodic acid, and this method is:Using red phosphorus method, according to
It is secondary that deionized water is added into consersion unit in reaction step including reaction step, filtration step and distilation steps, it adds
After red phosphorus and iodine, the proportion of reaction material liquid is measured, controls its proportion 1.2~1.4, hydroiodic acid steam is absorbed with water spray pump, mistake
Filter step is to filter twice, most obtains hydroiodic acid through distillation afterwards.This method is relatively low to the removal rate of elemental iodine impurity, removes this, step
Rapid cumbersome, the time is long, and energy consumption is big, of high cost.
Invention content
In view of this, the present invention provides a kind of purification process of hydroiodic acid easy to operate, obtained through the purification process
Purified product purity is higher and yield is larger.
The purification process of the hydroiodic acid of the present invention, makes pending hydroiodic acid crude product pass through dress with 10~20mL/min flow velocitys
It is filled with the adsorption column of zeolite imidazole ester frame structure material (ZIFs).
Here, zeolite imidazole ester frame structure material (ZIFs) is a kind of metal that Yaghi research groups of the U.S. are developed
Organic framework material MOFs.ZIFs has preferable suction-operated to elemental iodine in the present invention.The preparation of ZIFs can be used known
Method carry out, can refer to periodical literature, " progress of U.S.'s zeolite imidazole ester frame structure material, Liu Man etc. are modern
Chemical industry the 6th phase of volume 28 ".
Preferably, the dosage of the zeolite imidazole ester frame structure material is 3~15, with the quality of hydroiodic acid crude product for 1
Meter.
Preferably, the zeolite imidazole ester frame structure material is ZIF1~100.Here, ZIF1~100 are ground for Yashi
Study carefully a series of ZIFs synthesized by group.
Preferably, it is 20~40 DEG C by the temperature of adsorption column.
As used herein, above-mentioned term：
"one", "an" and " described " be used interchangeably and refer to one or more.
"and/or" is used to indicate that one of illustrated situation or both may to occur, for example, A and/or B includes (A
And B) and (A or B).
In addition, the range stated herein by endpoint includes all numerical value for being included within the scope of this（For example, 1 to 10 packet
Include 1.4,1.9,2.33,5.75,9.98 etc.）.
In addition, the statement of "at least one" herein includes one or more all numbers（For example, at least two, at least
4, at least six, at least eight, at least ten, at least 25, at least 50, at least 100 etc.）.
Elemental iodine is adsorbed using zeolite imidazole ester frame structure material (ZIFs) in the purification process of the present invention, energy
Enough preferable removing elemental iodines, reduce the content of elemental iodine impurity.This purification process is easy to operate, the product of purifying have compared with
Good purity and high income.
Specific implementation mode
The technical solution further illustrated the present invention with reference to embodiment.
Embodiment 1
By technical grade hydroiodic acid with 15mL/min flow velocitys at a temperature of 25 DEG C by being filled with zeolite imidazole ester frame structure material
(ZIFs) adsorption column, the wherein dosage of zeolite imidazole ester frame structure material are 10, are in terms of 1 by the quality of hydroiodic acid crude product.
The sampled analysis of this example hydroiodic acid, iodine impurity content are 0.35ppm, product yield 97.2%.
Embodiment 2
By technical grade hydroiodic acid with 20mL/min flow velocitys at a temperature of 40 DEG C by being filled with zeolite imidazole ester frame structure material
(ZIFs) adsorption column, the wherein dosage of zeolite imidazole ester frame structure material are 15, are in terms of 1 by the quality of hydroiodic acid crude product.
The sampled analysis of this example hydroiodic acid, iodine impurity content are 0.39ppm, product yield 97.0%.
Embodiment 3
By technical grade hydroiodic acid with 20mL/min flow velocitys at a temperature of 20 DEG C by being filled with zeolite imidazole ester frame structure material
(ZIFs) adsorption column, the wherein dosage of zeolite imidazole ester frame structure material are 12, are in terms of 1 by the quality of hydroiodic acid crude product.
The sampled analysis of this example hydroiodic acid, iodine impurity content are 0.43ppm, product yield 96.5%.
Embodiment 4
By technical grade hydroiodic acid with 20mL/min flow velocitys at a temperature of 40 DEG C by being filled with zeolite imidazole ester frame structure material
(ZIFs) adsorption column, the wherein dosage of zeolite imidazole ester frame structure material are 3, are in terms of 1 by the quality of hydroiodic acid crude product.This
The example sampled analysis of hydroiodic acid, iodine impurity content are 0.35ppm, product yield 96.1%.
Comparative example
Hydroiodic acid crude product is purified with reference to the method for patent CN102249190.The yield that this example is collected into hydroiodic acid is
96.8%, its elemental iodine impurity content is 0.75ppm after tested.
Since the numberical range of each technological parameter involved in the present invention can not possibly all embody in the above-described embodiments,
As long as but those skilled in the art's envisioned any numerical value fallen into the above-mentioned numberical range completely can implement this
Invention also includes the arbitrary combination of occurrence in several numberical ranges certainly.Herein, for length the considerations of, be omitted to
Go out the embodiment of occurrence in certain one or more numberical range, this disclosure for being not to be construed as technical scheme of the present invention is not filled
Point.
Applicant states that the present invention illustrates detailed process equipment and the technological process of the present invention by above-described embodiment,
But the invention is not limited in above-mentioned detailed process equipment and technological processes, that is, it is above-mentioned detailed not mean that the present invention has to rely on
Process equipment and technological process could be implemented.Person of ordinary skill in the field it will be clearly understood that any improvement in the present invention,
The addition of equivalence replacement and auxiliary element to each raw material of product of the present invention, the selection etc. of concrete mode all fall within the present invention's
Within protection domain and the open scope.
Claims (4)
1. a kind of purification process of hydroiodic acid, which is characterized in that make pending hydroiodic acid crude product with 10~20mL/min flow velocitys
By the adsorption column for being filled with zeolite imidazole ester frame structure material (ZIFs).
2. purification process according to claim 1, which is characterized in that the dosage of the zeolite imidazole ester frame structure material
It is 3~15, is in terms of 1 by the quality of hydroiodic acid crude product.
3. purification process according to claim 1, which is characterized in that the zeolite imidazole ester frame structure material is ZIF1
~100.
4. purification process according to claim 1, which is characterized in that the temperature by adsorption column is 20~40 DEG C.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810910944.0A CN108658044A (en) | 2018-08-10 | 2018-08-10 | A kind of purification process of hydroiodic acid |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810910944.0A CN108658044A (en) | 2018-08-10 | 2018-08-10 | A kind of purification process of hydroiodic acid |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN108658044A true CN108658044A (en) | 2018-10-16 |
Family
ID=63788950
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201810910944.0A Pending CN108658044A (en) | 2018-08-10 | 2018-08-10 | A kind of purification process of hydroiodic acid |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN108658044A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101830443A (en) * | 2010-04-14 | 2010-09-15 | 清华大学 | Process for purifying sulfuric acid phase and hydriodic acid phase in iodine-sulfur cycle |
| US20100308261A1 (en) * | 2008-01-31 | 2010-12-09 | Nippoh Chemicals Co., Ltd | System and method for producing iodine compound |
| CN102249190A (en) * | 2011-07-25 | 2011-11-23 | 国药集团化学试剂有限公司 | Method for purifying hydroiodic acid |
| CN102847334A (en) * | 2012-09-14 | 2013-01-02 | 清华大学 | Method and apparatus for rectifying iodine-containing hydriodic acid liquid |
| CN107792831A (en) * | 2016-08-31 | 2018-03-13 | 天津市科密欧化学试剂有限公司 | A kind of preparation method of SILVER REAGENT hydroiodic acid |
| CN108163811A (en) * | 2018-01-23 | 2018-06-15 | 江苏索普（集团）有限公司 | A kind of preparation method of hydroiodic acid |
-
2018
- 2018-08-10 CN CN201810910944.0A patent/CN108658044A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20100308261A1 (en) * | 2008-01-31 | 2010-12-09 | Nippoh Chemicals Co., Ltd | System and method for producing iodine compound |
| CN101830443A (en) * | 2010-04-14 | 2010-09-15 | 清华大学 | Process for purifying sulfuric acid phase and hydriodic acid phase in iodine-sulfur cycle |
| CN102249190A (en) * | 2011-07-25 | 2011-11-23 | 国药集团化学试剂有限公司 | Method for purifying hydroiodic acid |
| CN102847334A (en) * | 2012-09-14 | 2013-01-02 | 清华大学 | Method and apparatus for rectifying iodine-containing hydriodic acid liquid |
| CN107792831A (en) * | 2016-08-31 | 2018-03-13 | 天津市科密欧化学试剂有限公司 | A kind of preparation method of SILVER REAGENT hydroiodic acid |
| CN108163811A (en) * | 2018-01-23 | 2018-06-15 | 江苏索普（集团）有限公司 | A kind of preparation method of hydroiodic acid |
Non-Patent Citations (1)
| Title |
|---|
| THOMAS D. BENNETT ET AL: "Ball-Milling-Induced Amorphization of Zeolitic Imidazolate Frameworks (ZIFs) for the Irreversible Trapping of Iodine", 《CHEM. EUR. J.》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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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Application publication date: 20181016 |