CN114195105A - Preparation method of high-purity tellurium dioxide - Google Patents
Preparation method of high-purity tellurium dioxide Download PDFInfo
- Publication number
- CN114195105A CN114195105A CN202111531055.1A CN202111531055A CN114195105A CN 114195105 A CN114195105 A CN 114195105A CN 202111531055 A CN202111531055 A CN 202111531055A CN 114195105 A CN114195105 A CN 114195105A
- Authority
- CN
- China
- Prior art keywords
- tellurium
- purity
- tetrachloride
- dioxide
- tellurium dioxide
- 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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- LAJZODKXOMJMPK-UHFFFAOYSA-N tellurium dioxide Chemical compound O=[Te]=O LAJZODKXOMJMPK-UHFFFAOYSA-N 0.000 title claims abstract description 32
- 238000002360 preparation method Methods 0.000 title claims abstract description 10
- OFDISMSWWNOGFW-UHFFFAOYSA-N 1-(4-ethoxy-3-fluorophenyl)ethanamine Chemical compound CCOC1=CC=C(C(C)N)C=C1F OFDISMSWWNOGFW-UHFFFAOYSA-N 0.000 claims abstract description 47
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims abstract description 33
- PORWMNRCUJJQNO-UHFFFAOYSA-N tellurium atom Chemical compound [Te] PORWMNRCUJJQNO-UHFFFAOYSA-N 0.000 claims abstract description 28
- 229910052714 tellurium Inorganic materials 0.000 claims abstract description 26
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 claims abstract description 15
- 239000000460 chlorine Substances 0.000 claims abstract description 15
- 229910052801 chlorine Inorganic materials 0.000 claims abstract description 15
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 11
- 229910021642 ultra pure water Inorganic materials 0.000 claims abstract description 10
- 239000012498 ultrapure water Substances 0.000 claims abstract description 10
- 239000003960 organic solvent Substances 0.000 claims abstract description 9
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000007788 liquid Substances 0.000 claims abstract description 8
- 238000000926 separation method Methods 0.000 claims abstract description 8
- 238000001035 drying Methods 0.000 claims abstract description 7
- 230000003301 hydrolyzing effect Effects 0.000 claims abstract description 6
- 238000001704 evaporation Methods 0.000 claims abstract description 5
- 230000007062 hydrolysis Effects 0.000 claims abstract description 4
- 238000006460 hydrolysis reaction Methods 0.000 claims abstract description 4
- 239000007791 liquid phase Substances 0.000 claims abstract description 3
- 239000000126 substance Substances 0.000 claims abstract 2
- 238000001914 filtration Methods 0.000 claims description 9
- 238000000034 method Methods 0.000 claims description 9
- 238000006243 chemical reaction Methods 0.000 claims description 2
- 238000004140 cleaning Methods 0.000 claims 1
- 239000012535 impurity Substances 0.000 abstract description 12
- 239000007795 chemical reaction product Substances 0.000 abstract description 8
- 238000001953 recrystallisation Methods 0.000 abstract description 2
- 230000008020 evaporation Effects 0.000 abstract 1
- 238000001095 inductively coupled plasma mass spectrometry Methods 0.000 description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 1
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 235000011114 ammonium hydroxide Nutrition 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- 239000013064 chemical raw material Substances 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 239000003755 preservative agent Substances 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B19/00—Selenium; Tellurium; Compounds thereof
- C01B19/004—Oxides; Hydroxides
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The invention discloses a preparation method of high-purity tellurium dioxide, which comprises the steps of reacting single tellurium with dry chlorine to obtain tellurium tetrachloride, dissolving the tellurium tetrachloride in an organic solvent, carrying out first solid-liquid separation, carrying out evaporation and recrystallization on the obtained liquid phase to obtain the high-purity tellurium tetrachloride, putting the high-purity tellurium tetrachloride into ultrapure water, introducing ammonia gas, controlling the pH value of the solution to be 6.5-7.5, hydrolyzing the tellurium tetrachloride, carrying out second solid-liquid separation, and drying to obtain the high-purity tellurium dioxide. According to the invention, the tellurium tetrachloride is obtained by reacting the simple substance tellurium with the dry chlorine, the characteristic that the reaction product of the tellurium and the chlorine can be dissolved in methanol and absolute ethanol, and the reaction product of impurities in the tellurium and the chlorine is insoluble in the methanol and the absolute ethanol is utilized, so that the tellurium is separated from the impurities, the purity of the tellurium tetrachloride is further improved after the tellurium tetrachloride is recrystallized, and the tellurium tetrachloride is put into ultrapure water for hydrolysis.
Description
Technical Field
The invention belongs to the technical field of preparation of high-purity oxide materials, and particularly relates to a preparation method of high-purity tellurium dioxide.
Background
Tellurium dioxide is an important chemical raw material and is mainly used for preparing tellurium dioxide single crystals, infrared devices, acousto-optic devices, infrared window materials, electronic element materials, preservatives and the like.
Most of the existing methods for preparing tellurium dioxide are prepared by oxidizing elemental tellurium by nitric acid or hydrogen peroxide, the condition of incomplete oxidation of the elemental tellurium generally exists, the prepared tellurium dioxide is usually wrapped by the elemental tellurium, new impurity elements are introduced due to the oxidation of the elemental tellurium and the use of a large amount of acid, alkali and other reagents in subsequent processes, the purity of the prepared tellurium dioxide is generally 3N and 4N (99.9-99.99%), a product with higher purity is difficult to prepare, and strong acid and strong base are seriously corroded on equipment and have larger pollution on the environment.
Disclosure of Invention
In view of the problems of the prior art, the invention aims to provide a preparation method of high-purity tellurium dioxide with the purity of more than 5N.
In order to achieve the purpose, the invention provides the following technical scheme:
the invention relates to a preparation method of high-purity tellurium dioxide, which comprises the following steps: reacting elemental tellurium with dry chlorine to obtain tellurium tetrachloride, dissolving the tellurium tetrachloride in an organic solvent, carrying out solid-liquid separation for the first time, evaporating and recrystallizing the obtained liquid phase to obtain high-purity tellurium tetrachloride, putting the high-purity tellurium tetrachloride into ultrapure water, introducing ammonia gas, controlling the pH value of the solution to be 6.5-7.5, hydrolyzing the tellurium tetrachloride, carrying out solid-liquid separation for the second time, and drying to obtain the high-purity tellurium dioxide.
According to the invention, the tellurium tetrachloride is obtained by reacting elemental tellurium with dry chlorine, the characteristic that the reaction product of tellurium and chlorine can be dissolved in an organic solvent, and the reaction product of impurities in tellurium and chlorine is insoluble in the organic solvent is utilized, so that tellurium is separated from impurities, the purity of tellurium tetrachloride is further improved after recrystallization, the tellurium tetrachloride is put into ultrapure water, and the pH value is controlled to be 6.5-7.5 by introducing ammonia gas, so that the tellurium tetrachloride is hydrolyzed.
In a preferred embodiment, the purity of the elemental tellurium is 4N.
In a preferable scheme, the reaction temperature is 400-600 ℃.
In a preferred embodiment, the organic solvent is at least one selected from methanol and absolute ethanol.
Dissolving tellurium tetrachloride in the organic solvent, and filtering out impurities which are insoluble in the organic solvent to obtain the tellurium tetrachloride solution.
The inventor finds that the purity of the finally obtained high-purity tellurium dioxide can reach more than 5N by dissolving tellurium tetrachloride in methanol and/or absolute ethyl alcohol.
In a preferred embodiment, the first solid-liquid separation is filtration.
In a preferred embodiment, the purity of the ammonia water is 5N.
According to the preferable scheme, after the hydrolysis is finished, the high-purity tellurium dioxide is obtained after the washing, the filtering and the drying by ultrapure water.
Principles and advantages
The preparation method of the high-purity tellurium dioxide utilizes the characteristic that a reaction product of tellurium and chlorine can be dissolved in methanol and absolute ethyl alcohol, and a reaction product of impurities in tellurium and chlorine is insoluble in methanol and absolute ethyl alcohol, so that tellurium is separated from impurities of tellurium, the purity of tellurium is further improved after the tellurium tetrachloride is recrystallized, then the tellurium tetrachloride is put into ultrapure water, and the pH value is controlled to be 6.5-7.5 by introducing ammonia gas, so that the tellurium tetrachloride is completely hydrolyzed.
Detailed Description
A preparation method of tellurium dioxide utilizes the characteristic that reaction products of tellurium and chlorine can be dissolved in methanol and absolute ethanol, and reaction products of impurities in tellurium and chlorine are not dissolved in methanol and absolute ethanol, so that tellurium is separated from impurities of tellurium, the purity of tellurium tetrachloride is further improved after the tellurium tetrachloride is recrystallized, and the high-purity tellurium dioxide is obtained by hydrolyzing the tellurium tetrachloride.
Example 1
Reacting the 4N tellurium powder with dry chlorine at 450 ℃ to obtain tellurium tetrachloride. Dissolving tellurium tetrachloride in methanol, filtering, removing impurities insoluble in methanol to obtain a tellurium tetrachloride solution, evaporating and recrystallizing the tellurium tetrachloride solution to obtain high-purity tellurium tetrachloride, pouring the tellurium tetrachloride into ultrapure water, introducing high-purity ammonia gas, controlling the pH value of the solution to be 6.8, completely hydrolyzing the tellurium tetrachloride, filtering, drying to obtain tellurium dioxide, and detecting by ICP-MS (inductively coupled plasma-mass spectrometry) to obtain the tellurium dioxide with the purity of 99.9994% which reaches above 5N standard.
Example 2
Reacting 4N tellurium powder with dry chlorine at 500 ℃ to obtain tellurium tetrachloride. Dissolving tellurium tetrachloride in absolute ethyl alcohol, filtering, removing impurities insoluble in absolute ethyl alcohol to obtain a tellurium tetrachloride solution, evaporating and recrystallizing the tellurium tetrachloride solution to obtain high-purity tellurium tetrachloride, pouring the tellurium tetrachloride into ultrapure water, introducing high-purity ammonia gas, controlling the pH value of the solution to be 7.0, completely hydrolyzing the tellurium tetrachloride, filtering, drying to obtain tellurium dioxide, and detecting by ICP-MS (inductively coupled plasma Mass Spectrometry), wherein the purity of the tellurium dioxide is 99.9996 percent and reaches above 5N standard.
Comparative example 1
The other conditions are the same as the example 1, except that the high-purity tellurium tetrachloride is put into the NaOH solution for hydrolysis, filtered and dried to obtain the tellurium dioxide with the Na content of up to 5ppm, which obviously does not reach the 5N standard.
For the convenience of the reader, the above description has focused on a representative sample of all possible embodiments, a sample that is illustrative of the principles of the invention, and the best mode contemplated for carrying out the invention. The description is not intended to be exhaustive of all possible variations. Other variations or modifications not described are possible.
Claims (7)
1. A preparation method of high-purity tellurium dioxide is characterized by comprising the following steps: the method comprises the following steps:
reacting elemental tellurium with dry chlorine to obtain tellurium tetrachloride, dissolving the tellurium tetrachloride in an organic solvent, carrying out solid-liquid separation for the first time, evaporating and recrystallizing the obtained liquid phase to obtain high-purity tellurium tetrachloride, putting the high-purity tellurium tetrachloride into ultrapure water, introducing ammonia gas, controlling the pH value of the solution to be 6.5-7.5, hydrolyzing the tellurium tetrachloride, carrying out solid-liquid separation for the second time, and drying to obtain the high-purity tellurium dioxide.
2. The method for preparing high-purity tellurium dioxide as claimed in claim 1, wherein: the purity of the simple substance tellurium is 4N.
3. The method for preparing high-purity tellurium dioxide as claimed in claim 1, wherein: the reaction temperature is 400-600 ℃.
4. The method for preparing high-purity tellurium dioxide as claimed in claim 1, wherein: the organic solvent is at least one of methanol and absolute ethyl alcohol.
5. The method for preparing high-purity tellurium dioxide as claimed in claim 1, wherein: the first solid-liquid separation mode is filtration.
6. The method for preparing high-purity tellurium dioxide as claimed in claim 1, wherein: the purity of the ammonia gas is 5N.
7. The method for preparing high-purity tellurium dioxide as claimed in claim 1, wherein: and after the hydrolysis is finished, cleaning with ultrapure water, filtering and drying to obtain the high-purity tellurium dioxide.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202111531055.1A CN114195105A (en) | 2021-12-15 | 2021-12-15 | Preparation method of high-purity tellurium dioxide |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202111531055.1A CN114195105A (en) | 2021-12-15 | 2021-12-15 | Preparation method of high-purity tellurium dioxide |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN114195105A true CN114195105A (en) | 2022-03-18 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202111531055.1A Pending CN114195105A (en) | 2021-12-15 | 2021-12-15 | Preparation method of high-purity tellurium dioxide |
Country Status (1)
| Country | Link |
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| CN (1) | CN114195105A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115128044A (en) * | 2022-06-28 | 2022-09-30 | 成都欣科医药有限公司 | Used for preparing iodine 131 I]Quality standard of tellurium dioxide as raw material of sodium chloride solution |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102923678A (en) * | 2012-11-22 | 2013-02-13 | 浏阳市亚光高新材料有限公司 | Method for preparing anhydrous tellurium tetrachloride by using tellurium dioxide as raw material |
| CN103303879A (en) * | 2013-06-28 | 2013-09-18 | 上海应用技术学院 | Preparation method of high-purity tellurium dioxide powder |
-
2021
- 2021-12-15 CN CN202111531055.1A patent/CN114195105A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102923678A (en) * | 2012-11-22 | 2013-02-13 | 浏阳市亚光高新材料有限公司 | Method for preparing anhydrous tellurium tetrachloride by using tellurium dioxide as raw material |
| CN103303879A (en) * | 2013-06-28 | 2013-09-18 | 上海应用技术学院 | Preparation method of high-purity tellurium dioxide powder |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115128044A (en) * | 2022-06-28 | 2022-09-30 | 成都欣科医药有限公司 | Used for preparing iodine 131 I]Quality standard of tellurium dioxide as raw material of sodium chloride solution |
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| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication | ||
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Application publication date: 20220318 |