CN107313063A - 5N high purity tellurium smelting processes - Google Patents
5N high purity tellurium smelting processes Download PDFInfo
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- CN107313063A CN107313063A CN201710382623.3A CN201710382623A CN107313063A CN 107313063 A CN107313063 A CN 107313063A CN 201710382623 A CN201710382623 A CN 201710382623A CN 107313063 A CN107313063 A CN 107313063A
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- tellurium
- distillation
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B1/00—Electrolytic production of inorganic compounds or non-metals
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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
- C01B19/00—Selenium; Tellurium; Compounds thereof
- C01B19/02—Elemental selenium or tellurium
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- 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
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Abstract
The invention discloses a kind of 5N high purity telluriums smelting process, comprise the following steps：（1）Meet the 4N tellurium ingots of the standards of YS/T222 2010 with low current density electrodeposition method output；（2）4N telluriums ingot progress cryogenic vacuum is really evaporated, output distillation tellurium；（3）Distillation tellurium is broken into little particle, is then placed in pure silica crucible and heats in the hydrogen gas stream, ingot casting obtains 5N high purity tellurium ingots.
Description
Technical field
The present invention relates to a kind of method of purification of tellurium, more particularly to a kind of 5N high purity telluriums smelting process.
Background technology
The purification of tellurium is always a problem for perplexing those skilled in the art.
Current high purity tellurium smelting process typically uses the true distilled 3N of vacuum or 4N telluriums.There is major defect in these methods：The
First, serious such as selenium is remained in the close element of vacuum shape boiling point with tellurium, lead residual is also very serious during temperature drift, influences the pure of tellurium
Degree, makes tellurium be difficult to reach 5N；Secondth, vacuum is relative, and the tellurium total surface distilled has the oxide-film of one layer of black gray expandable same
Sample influences the purity of tellurium.The high purity tellurium that current Traditional high purity tellurium smelting process is produced is than the 4N in YS/T222-2010 standard
Tellurium ingot grade is high, but does not reach 5N telluriums, can only be referred to as distillation high purity tellurium, can not still be referred to as 5N telluriums.
The content of the invention
It is an object of the invention to provide a kind of 5N high purity telluriums smelting process.
In order to solve the above-mentioned technical problem, method of the invention comprises the following steps：
（1）Meet the 4N tellurium ingots of YS/T222-2010 standards with low current density electrodeposition method output；
（2）4N telluriums ingot progress cryogenic vacuum is really evaporated, output distillation tellurium；
（3）Distillation tellurium is broken into little particle, is then placed in pure silica crucible and heats in the hydrogen gas stream, ingot casting obtains 5N high purity telluriums
Ingot.
Step（1）, tellurium dioxide, which is dissolved in sodium hydroxide solution, makes every liter 60-70 grams of tellurium content, and 80-90 DEG C of insulation is stirred
3 hours, plus 1-10 kilograms of akali sulphide are mixed, 10-50 kilograms of calcium oxide is hydrogenated with, is stirred for 1 hour, every liter of lead content of chemical examination is less than
Untill 0.003 gram, press filtration, it is 5-5.5 that filtrate, which is neutralized to pH value with sulfuric acid, then press filtration must refine tellurium dioxide, and gained is refined
Tellurium dioxide be configured to 99% caustic soda every liter of 150-240 containing tellurium grams, every liter containing NaOH50-120 grams of electric effusion, it is close in electric current
Electrodeposition in the range of 30-60 is spent, tellurium is separated out, scrubbed drying ingot casting must meet the 4N tellurium ingots of YS/T222-2010 standards.
Step（2）, gained 4N tellurium ingots are fitted into vacuum distillation furnace, vacuum is below 5 handkerchiefs, and tellurium ingot is in 600 DEG C of constant temperatures
Fusing, is incubated 3-8 hours, and distillation tellurium is condensed in quartz basin produces silver gray acicular crystal distillation tellurium.
Step（3）, gained distillation tellurium is broken into little particle, is put into pure silica crucible and heats in the hydrogen gas stream, quartz
Crucible is heated in quartz pipe, and logical pure hydrogen 5-20 minutes before heating, hydrogen flowing quantity keeps 2-10 liters per minute, tellurium fusing
Afterwards, change logical nitrogen, remove heater, being cooled to normal temperature to tellurium produces 5N high purity telluriums, and gained 5N high purity telluriums ingot is silvery white, table
Face is smooth.
The method of the present invention, the additive in the first step can effectively go removing heavy-metal impurities and silicate, stannous acid group,
Meta-aluminic acid root etc., low current density electrodeposition method has efficiently controlled the content of impurity selenium element, the method selenium can be down to 5PPM with
It is interior（Standard is no more than 20PPM）, it is that subsequent technique lays the first stone, principle is the electrode electricity of the 4 valency cations using selenium and tellurium
Position is different, obtains the ability difference that electronics changes into atom, and the valency plasma selenium of 4 valency tellurium ion ratio 4 is easier acquisition electronics and changed into
Tellurium atom, 4 valency plasma seleniums are more difficult to obtain electronics in negative electrode precipitation selenium atom under low current density state, so as to be effectively reduced
Negative electrode separates out the content of selenium in tellurium.Low temperature in second step（600℃）Be evaporated in vacuo 4N telluriums effectively by impurity lead, aluminium, bismuth,
Iron, the content of sodium are down within 1PPM, and impurity copper, silicon, magnesium, arsenic, the content of sulphur are down within 0.5PPM（If lead therein is not
It is difficult to be down within 1PPM using the method, principle is lead volatilization point temperature under vacuum conditions and tellurium waving under vacuum conditions
Hair point temperature difference very little, the only volatilization point temperature as far as possible close to tellurium could effectively suppress the volatilization of lead, the temperature control point
In 600 degrees centigrades）.3rd step use will be broken into short grained distillation tellurium and be put into pure silica crucible to be added in the hydrogen gas stream
Hot-cast ingot, can be effectively reduced the content of foreign matter selenium within 0.5PPM, principle is that selenium is produced when heating fusing in the hydrogen gas stream
Raw volatile hydrogen selenide is removed, and tellurium surface film oxide is removed, and principle is oxygen element in oxide-film in heating and hydrogen stream
Middle protium reaction produces water volatilization, so as to obtain the smooth 5N tellurium ingots being silvery white in color in surface.
Using the method for the present invention, the first step uses low current density（30-60A/ square metres）Electrodeposition method output YS/
4N tellurium ingots in T222-2010 standards；Second step, which is used, really evaporates 4N telluriums ingot progress cryogenic vacuum, output distillation tellurium；3rd step
Ingot casting is heated in the hydrogen gas stream obtain 5N tellurium ingots, it is ensured that production using that will be broken into short grained distillation tellurium and be put into pure silica crucible
Product are real 5N telluriums, and the smooth No oxided film in surface is bright silvery white as silver ingot, overcomes the various defects of prior art, real
Goal of the invention is showed.
Embodiment
The method to the present invention is described in detail below.
The method of the present invention comprises the following steps：
The first step, the 4N tellurium ingots of YS/T222-2010 standards are met with low current density electrodeposition method output, i.e., tellurium dioxide is molten
Make every liter 60-70 grams of tellurium content in sodium hydroxide solution, be incubated 80-90 DEG C and stir 3 hours, plus 1-10 kilograms of akali sulphide, plus
10-50 kilograms of calcium hydroxide, is stirred for 1 hour, untill every liter of chemical examination lead content is less than 0.003 gram, press filtration, in filtrate sulfuric acid
Be 5-5.5 to pH value, then press filtration must refine tellurium dioxide, gained is refined into tellurium dioxide be configured to every liter with 99% caustic soda and contain
150-240 grams of tellurium, every liter containing NaOH50-120 grams of electric effusion, the electrodeposition in the range of current density 30-60, separate out tellurium, through washing
The 4N tellurium ingots of YS/T222-2010 standards must be met by washing drying ingot casting.
Second step, 4N telluriums ingot progress cryogenic vacuum is really evaporated, output distillation tellurium, will the ingot loading vacuum distillation of gained 4N telluriums
In stove, vacuum is below 5 handkerchiefs, and tellurium ingot melts in 600 DEG C of constant temperatures, is incubated 3-8 hours, and distillation tellurium is condensed in quartz basin to be produced
Silver gray acicular crystal distills tellurium.
3rd step, is broken into little particle by distillation tellurium, is then placed in pure silica crucible and heats in the hydrogen gas stream, ingot casting is obtained
5N high purity tellurium ingots, will gained distillation tellurium be broken into little particle, be put into pure silica crucible and heat in the hydrogen gas stream, silica crucible
Heated in quartz pipe, logical pure hydrogen 5-20 minutes before heating, hydrogen flowing quantity keeps 2-10 liters per minute, after tellurium fusing, changes
Logical nitrogen, removes heater, and being cooled to normal temperature to tellurium produces 5N high purity telluriums, and gained 5N high purity telluriums ingot is silvery white, surface light
It is sliding.
Claims (4)
1. a kind of 5N high purity telluriums smelting process, it is characterised in that comprise the following steps：
（1）Meet the 4N tellurium ingots of YS/T222-2010 standards with low current density electrodeposition method output；
（2）4N telluriums ingot progress cryogenic vacuum is really evaporated, output distillation tellurium；
（3）Distillation tellurium is broken into little particle, is then placed in pure silica crucible and heats in the hydrogen gas stream, ingot casting obtains 5N high purity telluriums
Ingot.
2. method according to claim 1, it is characterised in that：Step（1）, tellurium dioxide, which is dissolved in sodium hydroxide solution, makes tellurium
Every liter 60-70 grams of content, is incubated 80-90 DEG C and stirs 3 hours, plus 1-10 kilograms of akali sulphide, is hydrogenated with 10-50 kilograms of calcium oxide, then
Stirring 1 hour, untill every liter of chemical examination lead content is less than 0.003 gram, press filtration, it is 5-5.5 that filtrate, which is neutralized to pH value with sulfuric acid, then is pressed
Tellurium dioxide must be refined by filtering, and the refined tellurium dioxide of gained is configured into every liter of 150-240 containing tellurium grams, every liter with 99% caustic soda contains
NaOH50-120 grams of electric effusion, the electrodeposition in the range of current density 30-60 separates out tellurium, and scrubbed drying ingot casting must meet YS/
The 4N tellurium ingots of T222-2010 standards.
3. method according to claim 1, it is characterised in that：Step（2）, gained 4N tellurium ingots are fitted into vacuum distillation furnace, very
Reciprocal of duty cycle is below 5 handkerchiefs, and tellurium ingot melts in 600 DEG C of constant temperatures, is incubated 3-8 hours, and distillation tellurium is condensed in quartz basin produces silver gray
Acicular crystal distills tellurium.
4. method according to claim 1, it is characterised in that：Step（3）, gained distillation tellurium is broken into little particle, is put into pure
Heated in the hydrogen gas stream in silica crucible, silica crucible is heated in quartz pipe, logical pure hydrogen 5-20 minutes, hydrogen before heating
Flow keeps 2-10 liters per minute, after tellurium fusing, changes logical nitrogen, removes heater, and being cooled to normal temperature to tellurium, to produce 5N high-purity
Tellurium, gained 5N high purity telluriums ingot is silvery white, surface is smooth.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201710382623.3A CN107313063A (en) | 2017-05-26 | 2017-05-26 | 5N high purity tellurium smelting processes |
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| CN201710382623.3A CN107313063A (en) | 2017-05-26 | 2017-05-26 | 5N high purity tellurium smelting processes |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108950213A (en) * | 2018-07-03 | 2018-12-07 | 昆明理工大学 | A method of recycling tellurium and bismuth from bismuth telluride material |
| CN110775948A (en) * | 2019-12-05 | 2020-02-11 | 成都理工大学 | Method for improving reduction efficiency of tellurium oxide |
| CN110894065A (en) * | 2019-12-18 | 2020-03-20 | 中南大学 | Equipment and method for preparing high-purity tellurium |
| CN113387336A (en) * | 2021-06-15 | 2021-09-14 | 中南大学 | Method for removing selenium from tellurium ingot |
| CN113772634A (en) * | 2021-09-15 | 2021-12-10 | 广东先导稀贵金属材料有限公司 | Preparation method of 5N high-purity selenium granules |
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| US5035874A (en) * | 1987-06-26 | 1991-07-30 | The United Staes Of America As Represented By The Secretary Of The Navy | Diallyl telluride and synthesis of diorgano tellurides |
| CN101892496A (en) * | 2010-06-30 | 2010-11-24 | 四川鑫炬矿业资源开发股份有限公司 | Method for preparing high-purity 5N tellurium from 3N crude tellurium |
| CN105399062A (en) * | 2015-12-01 | 2016-03-16 | 湖南省金润碲业有限公司 | Method for extracting tellurium dioxide from anode slime produced through tellurium electro-deposition |
| CN105776152A (en) * | 2016-05-05 | 2016-07-20 | 郭舒洋 | Preparation method of high-purity tellurium |
| CN106276820A (en) * | 2016-07-28 | 2017-01-04 | 江西铜业集团公司 | A kind of be raw material production high purity tellurium with coarse tellurium powder technique |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108950213A (en) * | 2018-07-03 | 2018-12-07 | 昆明理工大学 | A method of recycling tellurium and bismuth from bismuth telluride material |
| CN110775948A (en) * | 2019-12-05 | 2020-02-11 | 成都理工大学 | Method for improving reduction efficiency of tellurium oxide |
| CN110894065A (en) * | 2019-12-18 | 2020-03-20 | 中南大学 | Equipment and method for preparing high-purity tellurium |
| CN110894065B (en) * | 2019-12-18 | 2023-04-07 | 中南大学 | Equipment and method for preparing high-purity tellurium |
| CN113387336A (en) * | 2021-06-15 | 2021-09-14 | 中南大学 | Method for removing selenium from tellurium ingot |
| CN113387336B (en) * | 2021-06-15 | 2022-05-20 | 中南大学 | Method for removing selenium from tellurium ingot |
| CN113772634A (en) * | 2021-09-15 | 2021-12-10 | 广东先导稀贵金属材料有限公司 | Preparation method of 5N high-purity selenium granules |
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