CN107585745A - A kind of 5N telluriums production technology - Google Patents
A kind of 5N telluriums production technology Download PDFInfo
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- CN107585745A CN107585745A CN201710643803.2A CN201710643803A CN107585745A CN 107585745 A CN107585745 A CN 107585745A CN 201710643803 A CN201710643803 A CN 201710643803A CN 107585745 A CN107585745 A CN 107585745A
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Abstract
The present invention relates to a kind of the method for 5N high purity telluriums is obtained using 4N telluriums as raw material by the way that purification is evaporated in vacuo, the characteristics of this method is, in the process of screening or the preparation of raw material, by screening or pre-processing the obvious content for reducing partial impurities in raw material, the impurity content for making to be difficult to separate in raw material substantially reduces, vacuum distillation purification is carried out again, obtains the satisfactory high-purity 5N telluriums of every impurity content.
Description
Technical field
The present invention relates to a kind of preparation method of 5N telluriums, belongs to metal metallurgy smelting purification field.
Background technology
High purity tellurium is the basic material of prepare compound semi-conducting material, such as cadmium telluride can be used for manufacturing light-emitting diodes
Pipe, radiation detector and solar cell；Tellurium mercury cadmium alloy is the optimal material of infrared emitter and detector；Tellurium bismuth, selenium, stibium closes
Gold is a kind of important temperature-difference thermoelectric material, can be used for generating electricity and refrigeration, such as water dispenser, refrigerator, the civilian production of air-conditioning
The refrigeration of product, can also use universe dynamical system, Aero-Space, upper-level weather recording apparatus, military radar cooler and
In submarine air-conditioning device.However, the purity of the metallic tellurium for preparing tellurium bismuth, selenium, stibium alloy material must reach more than 4N ability
Meet ingredient requirement, otherwise directly influence device performance and effect.
At present, preparing the method for high purity tellurium has zone-melting process, electrolysis and vacuum distillation method etc., and zone-melting process is using impure
Amorphous material fusing after when recrystallizing, impurity concentration in the solid and uncrystallized liquid of crystallization is different methods；Electricity
Solution purifying method is that the tellurium dioxide by purification is dissolved in into sodium hydroxide solution to be configured to electrolyte, and free alkalinity control exists
100g/L, under certain electric current, temperature and time, product tellurium is obtained on minus plate；The vacuum distillation method of thick tellurium be according to
There is high vapour pressure according to tellurium, and the principle of bigger difference is pressed with the steam of other impurities metal, higher than tellurium fusing point
At a temperature of distilled, it is strict to control condensation temperature to realize segmentation condensation, obtain high purity tellurium.
Thick tellurium using purity as 4N is the method that raw material prepares that purity is 5N telluriums, up to the present, most commonly vacuum
The way of distillation, most technique are by separation or removal of the condensation temperature realization for impurity in control flow, due to tellurium
Contain a variety of different impurity in material, the saturated vapor pressure of the saturated vapor pressure ratio tellurium of partial impurities such as sodium, selenium is high, is steamed in vacuum
It can be evaporated during evaporating prior to tellurium into gas phase, have a strong impact on the purity of tellurium.Therefore, in order to improve the purity of tellurium, big portion
The technique divided is by the condensation temperature in control flow, is condensed by being segmented, allows tellurium from sodium, selenium element respectively in different temperature
Degree condenses out in region, so as to reach the purpose of separation.But it is difficult to above by segmentation condensation by tellurium and sodium, selenium member
The impurity elements such as element being completely separated or quickly reducing, so as to be difficult to obtain satisfactory high-purity 5N telluriums.
The content of the invention
For drawbacks described above, the present invention is intended to provide a kind of, using 4N telluriums as raw material, by the way that purification is evaporated in vacuo, to obtain 5N high-purity
The method of tellurium, it is the characteristics of this method, in the process of screening or the preparation of raw material, by screening or pre-processing obvious reduction
The content of partial impurities in raw material, the impurity content for making to be difficult to separate in raw material substantially reduce, and in follow-up technical process, lead to
Crossing segmentation condensation further reduces its content, obtains the satisfactory high-purity 5N telluriums of every impurity content.
The purpose of the present invention is realized by following technical measures, and a kind of production technology of 5N telluriums, the technique includes following step
Suddenly：
4N tellurium raw materials are fitted into crucible, before heating system vacuumize when reaching required vacuum,
Start to warm up to required temperature, evaporate tellurium, evaporant is condensed and collected, evaporation product is cast in protective atmosphere
Ingot is molded, and obtains high-purity 5N telluriums.
Preferably, all smart telluriums for meeting 4N- tellurium national standard quality index can serve as preparing the original of high-purity 5N- telluriums
Material.
Preferably, when the raw material meets 4N tellurium national standard quality index but Se content ＞ 3ppm, selenium drops by hydrogenating
Pretreatment makes Se ＜ 3ppm.
Preferably, when the raw material meets 4N tellurium national standard quality index but sodium content ＞ 0.8ppm, dropped by slag making
Sodium pretreatment makes Na ＜ 0.8ppm.
Preferably, 470 ± 10 DEG C, time 3.0--4.5h of the temperature of vacuum distillation, vacuum 2~8 × 10-3pa。
Preferably, obtained product will be evaporated in vacuo in protective atmosphere ingot casting shaping, obtain high-purity 5N telluriums ingot.
Preferably, obtained undesirable product will be distilled, returns to vacuum distillation process.
Preferably, by distillation obtain selenium beyond quality control requirement and other impurities element meets product quality indicator, lead to
After over hydrogenation drop selenium processing, it is set to be collected after becoming qualified products.
Preferably, defective material distillation obtained carries out the defective material that secondary vacuum distills to obtain, and is prepared into content as 99.9%
Tellurium ball.
Preferably, the defective material that distillation obtains is obtained into secondary vacuum distillage by second distillation, returns to vacuum steaming
Process is evaporated to be distilled again.
The present invention is described in detail below：
The purpose of the present invention is realized by following technical measures, a kind of production technology of high-purity 5N telluriums, the technique include with
Lower step：
4N tellurium raw materials are fitted into crucible, before heating system vacuumize when reaching required vacuum,
Start to warm up to required temperature, evaporate tellurium, evaporant is condensed and collected, evaporation product is cast in protective atmosphere
Ingot is molded, and obtains high-purity 5N telluriums.
The screening and preparation of raw material：
1), all smart telluriums for meeting 4N- tellurium national standard quality index can serve as preparing the qualified original of high-purity 5N- telluriums
Material, the raw material voluntarily can be bought or produce, and table 1 below is the national standard of 4N telluriums.
The 4N- tellurium national standards of table 1
2) it is, every after being once evaporated in vacuo, the tellurium raw material of qualified 5N- telluriums product can be obtained, can serve as making
The raw material of standby high-purity 5N- telluriums.
3) when, the raw material meets 4N tellurium national standard quality index but Se content ＞ 3ppm, located in advance by hydrogenating drop selenium
Reason makes Se ＜ 3ppm.
4) when, the raw material meets 4N tellurium national standard quality index but sodium content ＞ 0.8ppm, it is pre- that sodium is dropped by slag making
Processing makes Na ＜ 0.8ppm.
Vacuum distillation technique：
4N tellurium raw materials are fitted into crucible, when be evacuated to required vacuum to system before heating, started
Be warming up to required temperature, evaporate tellurium, evaporant is condensed and collected, by evaporation product protective atmosphere ingot casting into
Type, obtain high-purity 5N telluriums.
Technological parameter：Distilling period：470 ± 10 DEG C of actual temperature claimed range
Soaking zone：260 ± 10 DEG C of actual temperature
Being incubated condensable product head material should the appropriate distance away from crucible upper end：15~25mm
Distillation time：3.0--4.5h；
Crucible defective material amount：20~25%
Vacuum：2~8 × 10-3pa。
About 488 DEG C of tellurium fusing point, lower 400 DEG C of vacuum condition start to volatilize, and general control is 470 ± 10 in actual production process
DEG C, table 2 is the saturated vapour pressure of various impurity elements under different temperatures：
The saturated vapor pressure (Pa) of impurity element in the tellurium of table 2
As can be seen from Table 2, when vapo(u)rizing temperature is 550 DEG C, the saturated vapor pressure of tetra- kinds of impurity elements of Cu, Al, Fe, Si
Respectively 3.3 × 10-10Pa、4.2×10-9Pa、5.5×10-13Pa、7.3×10-15Pa, these four impurity elements saturated vapor
Press the saturated vapor pressure (3.3 × 10 than tellurium-10Pa) more than low 11 orders of magnitude, what they can be more in still-process is residual
Stay in the liquid phase, without evaporating；The saturated vapor pressure of two kinds of impurity elements of Pb, Bi is respectively 1.3 × 10-2Pa、1.5×
10-2Pa, the saturated vapor than tellurium force down 4 orders of magnitude, and they can be than tetra- kinds of impurity elements of Cu, Al, Fe, Si in still-process
It is easy to volatilize；Impurity element Mg saturated vapor pressure value is 4.3 × 101Pa, although the saturated vapor of its saturated vapor pressure ratio tellurium
Press small, but numerical value is fairly close, differs only by 1 order of magnitude, and more Mg elements are had in vacuum distillation process and enter gas phase
In；The saturated vapor pressure of Na, Se impurity element is respectively 1.5 × 103Pa、1.4×104Pa, their saturated vapor pressures than tellurium
Height, it can be evaporated in vacuum distillation process prior to tellurium into gas phase, have a strong impact on the purity of tellurium.Therefore, it is cold by controlling
Solidifying temperature, segmentation condensation is carried out, allows tellurium to be condensed out respectively in different temperature provinces from Na, Se, so as to the condensation reached
Purpose, because (270 DEG C) of condensation temperature (250 DEG C) and the tellurium of selenium is close, extends condensation segment length and be also difficult to reach preferable
Separating effect, simple to be unable to reach purpose of the depth except selenium by distillation, we use the method melted in hydrogen atmosphere, obtain very
Good effect, can drop to Se content below test limit.
The processing of product and defective material is evaporated in vacuo：
1), in distillage, every satisfactory product of impurity content directly carries out intermediate frequency ingot casting, obtains 5N tellurium ingots,
Then packaging and storage.
2), in distillage, selenium exceeds quality control requirement and other impurities element meets product quality indicator, passes through hydrogen
After changing drop selenium processing, it is set to become after qualified products packaging and storage again.
3), in distillage, the impurity element index in addition to selenium exceeds such product of control standard, is returned directly to
Vacuum distillation process is distilled again.
4), the defective material that product is evaporated in vacuo obtains secondary vacuum distillage by second distillation, and secondary vacuum is distilled
Product returns to vacuum distillation process and distilled again as raw material.
5), the defective material that product is evaporated in vacuo obtains defective material by second distillation, and defective material is prepared into content 99.9%
Tellurium ball.
It is evaporated in vacuo it can be seen from the above in obtained distillage, is met the requirements for every impurity content
Distillage directly carry out intermediate frequency ingot casting, obtain 5N tellurium ingots, then packaging and storage, for it is undesirable vacuum distillation produce
Product, continue return vacuum distillation technique and carry out circulation distillation, wherein selenium exceeds quality control requirement and other impurities element meets
Product quality indicator, after hydrogenating drop selenium processing, it is set to become packaging and storage, and entering for defective material again after qualified products
The processing of row second distillation, second distillation product are re-used as raw material, return to vacuum distillation technique and carry out circulation distillation, second distillation is residual
Material prepares the tellurium ball that content is 99.9%, in whole technological process, carries out vacuum distillation processing for raw material, collection meets the requirements
High-purity 5N telluriums, and carry out further distillation processing for undesirable distillage, dropped until by impurity therein
For satisfactory high-purity 5N telluriums product.
It can be seen from the above technical proposal that the present invention has advantages below：
1. the present invention is provided a kind of purified using 4N telluriums as raw material by vacuum distillation and obtains the method for 5N high purity telluriums, the present invention
Passing through the screening or pretreatment for raw material, hence it is evident that reduce the content of partial impurities in raw material, make to be difficult to separate in raw material
Impurity content substantially reduce, in follow-up technical process, further reduce its content by being segmented condensation, obtain every miscellaneous
The satisfactory high-purity 5N telluriums of matter content.
2. technological parameter is evaporated in vacuo by controlling in the present invention, tellurium is set to condense collection, tellurium again after fully volatilizing
About 488 DEG C of fusing point, lower 400 DEG C of vacuum condition start to volatilize, and vacuum distillation temperature requirement is controlled in the present invention at 470 ± 10 DEG C,
Tellurium is volatilized at such a temperature, control vapo(u)rizing temperature and time, obtain high-purity 5N telluriums that every impurity content substantially reduces.
3. the impurity content of product is low, purity is high；In the present invention satisfactory high-purity 5N telluriums are collected by being evaporated in vacuo
Product, it is further processed for the undesirable product after vacuum distillation, such as continues return and be evaporated in vacuo
Cheng Jinhang second distillations, or for the high distillage of Se content therein, then carry out hydrogenation drop selenium and handle to be conformed to
The high-purity 5N telluriums asked, and second distillation processing is carried out for defective material, second distillation product returns again to vacuum distillation process, until
Every impurity meets the requirements, and second distillation defective material is prepared into the tellurium ball that content is 99.9%.
4. whole technical process is carried out in the closed state, can anti-oxidation, and do not produce toxic and harmful gas, environment
Very little is polluted, production is fool proof.
Brief description of the drawings
Fig. 1 is high-purity 5N telluriums production technological process.
Embodiment
Embodiment 1：
1st, the screening and preparation of raw material：
1), all smart telluriums for meeting 4N- tellurium national standard quality index can serve as my company and produce high-purity 5N- telluriums
Acceptable material.Including outsourcing and self-produced smart tellurium.
The 4N- tellurium national standards of table 3
2), every normal process program by my company：After being once evaporated in vacuo, qualified 5N- telluriums product can be obtained
Tellurium raw material, we are defined as meeting the acceptable material of tellurium normal process requirement.
3) when, for meeting above-mentioned 4N telluriums national standard quality index but Se content ＞ 3ppm, such raw material has to pass through
After hydrogenation drop selenium processing, Se ＜ 3ppm, the normal technological process of production of 5N- telluriums could be entered；
4) when, for meeting above-mentioned 4N telluriums national standard quality index but sodium content ＞ 0.8ppm, such raw material must be through
Cross after slag making drop sodium pretreatment, during Na ＜ 0.8ppm, the normal technological process of production of 5N telluriums could be entered.
2nd, preliminary preparation：
The preparation of chloroazotic acid：60% deionized water is first put into the chloroazotic acid groove cleaned up, is then poured slowly into 6 bottles
2500ml hydrochloric acid and 2 bottles of 2500ml nitric acid, stir stand-by.
The processing of quartz member and operation tool：Distill quartz ampoule, condenser pipe, operation tool before the use, first with
Soak more than 6 hours, then take out in the chloroazotic acid made, rinsed repeatedly for more than 3 times to clean with deionized water, dry standby
With.
3rd, vacuum distillation technique：
1) charging is claimed：The raw material after crushing is weighed, is encased in crucible after weighing up, then slowly puts the crucible equipped with material
Enter the bottom to distillery, place into condenser pipe, pay attention to coordinate between crucible and condenser pipe, connect, in order to avoid distillation
When tellurium condense to other places beyond condenser pipe.
2) gland, vacuumize：It is determined that vacuum valve be all turned off in the state of open vacuum mechanical pump, check sealing
Mouth has N/D, takes a small amount of medical absorbent cotton to dip in absolute ethyl alcohol and cleans seal and vacuum gland and seal gasket at same direction
To cleaning, gland rubber cushion is aligned into seal pressure after drying, glass two-way valve is then turned on and takes out low vacuum.Treat low vacuum
When being evacuated to 1 × below 10Pa, cooling water is opened, opens heating diffusion pumps, simultaneously closes off low vacuum valve, high vacuum valve is opened and takes out height
Vacuum.
3) it is evaporated in vacuo:When high vacuum is evacuated to 1 × 10-3During Pa levels, open retort heating power supply and begin to warm up (heating temperature
It is 510 DEG C or so to spend distilling period, and soaking zone is 270 DEG C or so), it is heated to start timing during design temperature, and make a record.Steam
It is 3.0--4.5 hours to evaporate the time.The equipment such as vacuum system, temperature control system, dynamical system must strictly be monitored in the process to be had
It is without exception, timely processing of pinpointing the problems or report, and perform corresponding record.
4) blowing out：After the completion of distillation, retort heating power supply is first closed, then close heating diffusion pumps power supply, glass successively
Two-port valve, high vacuum valve, after opening low vacuum valve takes out low vacuum 30 minutes, turn off mechanical pump and cooling water.Distill simultaneously
Pipe puts forward to be put on brandreth after cooling down in heating furnace 30 minutes to be cooled down.High-temperature-resistant glove must be worn during pipe is carried
Stand and slowly distillation cascade is proposed out of stove on iron stand, avoid security incident！
5) discharge：After pipe to be distilled is cooled to room temperature, opens vent valve and deflate, while remove gland, distillation cascade is taken
On operating desk pipe support, taking out that condenser pipe and crucible sequentially neatly put out of distillation cascade successively (position put will be with equipment stove
It is number corresponding), weigh and record crucible residual quantity, judge whether product meets the requirements according to crucible residual quantity, meeting the requirements
Product carefully tremble and pour out out of condenser pipe in feed box, and remove afterbody (top 10 --- 15cm) and crystallize loose part
In afterbody defective material case, into hydrogenation process；It is residual in head defective material case, entrance to remove head (5 --- 10cm) crystallization compact portion
Expect distillation process；Center section is left as product (certain in the process to pay attention to paying attention to high-purity consciousness, to avoid polluted product).
It the above is only the preferred embodiment of the present invention, it is noted that above-mentioned preferred embodiment is not construed as pair
The limitation of the present invention, protection scope of the present invention should be defined by claim limited range.For the art
For those of ordinary skill, without departing from the spirit and scope of the present invention, some improvements and modifications can also be made, these change
Enter and retouch and also should be regarded as protection scope of the present invention.
Claims (10)
1. a kind of high-purity 5N Te production technology, it is characterised in that this method comprises the following steps：
4N tellurium raw materials are fitted into crucible, before heating system vacuumize when reaching required vacuum, are started
Be warming up to required temperature, evaporate tellurium, evaporant is condensed and collected, by evaporation product in protective atmosphere ingot casting
Shaping, obtains high-purity 5N telluriums.
2. high-purity 5N Te as claimed in claim 1 production technology, it is characterised in that all to meet 4N- tellurium national standard quality
The smart tellurium of index can serve as preparing the raw material of high-purity 5N- telluriums.
3. high-purity 5N Te as claimed in claim 1 production technology, it is characterised in that the raw material meets 4N tellurium national standards
Quality index but during Se content ＞ 3ppm, makes Se ＜ 3ppm by hydrogenating drop selenium pretreatment.
4. high-purity 5N Te as claimed in claim 1 production technology, it is characterised in that the raw material meets 4N tellurium national standards
Quality index but during sodium content ＞ 0.8ppm, dropping sodium pretreatment by slag making makes Na ＜ 0.8ppm.
5. high-purity 5N Te as claimed in claim 1 production technology, it is characterised in that 470 ± 10 DEG C of the temperature of vacuum distillation,
Time 3.0--4.5h, vacuum 2~8 × 10-3pa。
6. high-purity 5N Te as claimed in claim 1 production technology, it is characterised in that protecting the product that vacuum distillation obtains
Shield property atmosphere ingot casting shaping, obtains high-purity 5N telluriums ingot.
7. high-purity 5N Te as claimed in claim 1 production technology, it is characterised in that obtain distillation undesirable
Product, return to vacuum distillation process.
8. high-purity 5N Te as claimed in claim 1 production technology, it is characterised in that distillation is obtained into selenium and exceeds quality control
It is required that and other impurities element meets product quality indicator, by hydrogenate drop selenium processing after, it is become qualified products.
9. high-purity 5N Te as claimed in claim 1 production technology, it is characterised in that the defective material for obtaining distillation carries out secondary
Obtained defective material is evaporated in vacuo, is prepared into the tellurium ball that content is 99.9%.
10. high-purity 5N Te as claimed in claim 1 production technology, it is characterised in that obtained defective material will be distilled by secondary
Distillation obtains secondary vacuum distillage, returns to vacuum distillation process and is distilled again.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112758901A (en) * | 2020-12-30 | 2021-05-07 | 清远先导材料有限公司 | Preparation method of high-purity tellurium |
| CN113460975A (en) * | 2021-08-06 | 2021-10-01 | 江西中晶新材料有限公司 | Production method of 5N selenium |
| CN114132902A (en) * | 2021-12-31 | 2022-03-04 | 峨嵋半导体材料研究所 | Recovery method of cadmium telluride waste material |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112758901A (en) * | 2020-12-30 | 2021-05-07 | 清远先导材料有限公司 | Preparation method of high-purity tellurium |
| CN112758901B (en) * | 2020-12-30 | 2023-08-01 | 清远先导材料有限公司 | Preparation method of high-purity tellurium |
| CN113460975A (en) * | 2021-08-06 | 2021-10-01 | 江西中晶新材料有限公司 | Production method of 5N selenium |
| CN114132902A (en) * | 2021-12-31 | 2022-03-04 | 峨嵋半导体材料研究所 | Recovery method of cadmium telluride waste material |
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Application publication date: 20180116 |