CN117466257A - Production device and production method for preparing 6N high-purity tellurium by horizontal vacuum distillation - Google Patents
Production device and production method for preparing 6N high-purity tellurium by horizontal vacuum distillation Download PDFInfo
- Publication number
- CN117466257A CN117466257A CN202311480523.6A CN202311480523A CN117466257A CN 117466257 A CN117466257 A CN 117466257A CN 202311480523 A CN202311480523 A CN 202311480523A CN 117466257 A CN117466257 A CN 117466257A
- Authority
- CN
- China
- Prior art keywords
- tellurium
- horizontal
- air inlet
- pipe
- heater
- 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.)
- Pending
Links
- PORWMNRCUJJQNO-UHFFFAOYSA-N tellurium atom Chemical compound [Te] PORWMNRCUJJQNO-UHFFFAOYSA-N 0.000 title claims abstract description 153
- 229910052714 tellurium Inorganic materials 0.000 title claims abstract description 152
- 238000005292 vacuum distillation Methods 0.000 title claims abstract description 49
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 45
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 88
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 88
- 239000010439 graphite Substances 0.000 claims abstract description 88
- 238000010438 heat treatment Methods 0.000 claims abstract description 55
- 239000012535 impurity Substances 0.000 claims abstract description 51
- 238000004321 preservation Methods 0.000 claims abstract description 23
- 239000000463 material Substances 0.000 claims abstract description 22
- 238000004821 distillation Methods 0.000 claims description 62
- 238000009833 condensation Methods 0.000 claims description 44
- 230000005494 condensation Effects 0.000 claims description 44
- 238000007789 sealing Methods 0.000 claims description 34
- 239000007789 gas Substances 0.000 claims description 18
- 239000011261 inert gas Substances 0.000 claims description 18
- 238000005086 pumping Methods 0.000 claims description 12
- 230000007704 transition Effects 0.000 claims description 12
- 238000011068 loading method Methods 0.000 claims description 8
- 238000005070 sampling Methods 0.000 claims description 8
- 238000005303 weighing Methods 0.000 claims description 6
- 238000000034 method Methods 0.000 abstract description 20
- 229910052751 metal Inorganic materials 0.000 abstract description 15
- 239000002184 metal Substances 0.000 abstract description 15
- 230000008569 process Effects 0.000 abstract description 10
- 230000005484 gravity Effects 0.000 abstract description 8
- 238000000926 separation method Methods 0.000 abstract description 8
- 238000009835 boiling Methods 0.000 abstract description 7
- 238000002360 preparation method Methods 0.000 abstract description 4
- 238000012360 testing method Methods 0.000 abstract description 4
- 230000009471 action Effects 0.000 abstract description 3
- 239000000126 substance Substances 0.000 description 13
- 239000002994 raw material Substances 0.000 description 12
- 229910052711 selenium Inorganic materials 0.000 description 8
- 239000011669 selenium Substances 0.000 description 8
- 229920006395 saturated elastomer Polymers 0.000 description 6
- 230000000694 effects Effects 0.000 description 5
- 229910052717 sulfur Inorganic materials 0.000 description 5
- 229910002975 Cd Pb Inorganic materials 0.000 description 4
- 229910017518 Cu Zn Inorganic materials 0.000 description 4
- 238000004458 analytical method Methods 0.000 description 4
- 238000001514 detection method Methods 0.000 description 4
- 238000001036 glow-discharge mass spectrometry Methods 0.000 description 4
- BUGBHKTXTAQXES-UHFFFAOYSA-N Selenium Chemical compound [Se] BUGBHKTXTAQXES-UHFFFAOYSA-N 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 230000005012 migration Effects 0.000 description 3
- 238000013508 migration Methods 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- 238000000746 purification Methods 0.000 description 3
- 229920000742 Cotton Polymers 0.000 description 2
- 229910052785 arsenic Inorganic materials 0.000 description 2
- 238000005266 casting Methods 0.000 description 2
- 238000005868 electrolysis reaction Methods 0.000 description 2
- 150000002739 metals Chemical class 0.000 description 2
- 239000010453 quartz Substances 0.000 description 2
- 238000007670 refining Methods 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 229910001220 stainless steel Inorganic materials 0.000 description 2
- 239000010935 stainless steel Substances 0.000 description 2
- YLZOPXRUQYQQID-UHFFFAOYSA-N 3-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)-1-[4-[2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidin-5-yl]piperazin-1-yl]propan-1-one Chemical compound N1N=NC=2CN(CCC=21)CCC(=O)N1CCN(CC1)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F YLZOPXRUQYQQID-UHFFFAOYSA-N 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 229910000661 Mercury cadmium telluride Inorganic materials 0.000 description 1
- 229910002665 PbTe Inorganic materials 0.000 description 1
- 238000003723 Smelting Methods 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- JAWMENYCRQKKJY-UHFFFAOYSA-N [3-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-ylmethyl)-1-oxa-2,8-diazaspiro[4.5]dec-2-en-8-yl]-[2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidin-5-yl]methanone Chemical compound N1N=NC=2CN(CCC=21)CC1=NOC2(C1)CCN(CC2)C(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F JAWMENYCRQKKJY-UHFFFAOYSA-N 0.000 description 1
- 238000003915 air pollution Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000004070 electrodeposition Methods 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 238000004134 energy conservation Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 238000005984 hydrogenation reaction Methods 0.000 description 1
- 239000012774 insulation material Substances 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 238000000053 physical method Methods 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000005057 refrigeration Methods 0.000 description 1
- 238000005204 segregation Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- OCGWQDWYSQAFTO-UHFFFAOYSA-N tellanylidenelead Chemical compound [Pb]=[Te] OCGWQDWYSQAFTO-UHFFFAOYSA-N 0.000 description 1
- LAJZODKXOMJMPK-UHFFFAOYSA-N tellurium dioxide Chemical compound O=[Te]=O LAJZODKXOMJMPK-UHFFFAOYSA-N 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 239000002912 waste gas Substances 0.000 description 1
- 238000004857 zone melting 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
- C01B19/02—Elemental selenium or tellurium
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Manufacture And Refinement Of Metals (AREA)
Abstract
A production device and a production method for preparing 6N high-purity tellurium by horizontal vacuum distillation, wherein the production device comprises a horizontal pipe; the first heater, the second heater and the heat preservation cover are arranged outside the horizontal pipe and correspond to the first heating area, the second heating area and the heat preservation area respectively; a graphite sleeve, a primary condensing pipe and a secondary condensing pipe are sequentially arranged in the horizontal pipe; the graphite boat is positioned in the first heating area; tellurium materials are filled in a graphite boat. The invention also includes a production method. The method realizes the high-efficiency separation of the metal tellurium and the low-boiling impurity and the high-boiling impurity element, and realizes the preparation of 6N high-purity tellurium; the horizontal vacuum distillation is adopted to prepare high-purity tellurium, the driving force is small under the action of gravity cancellation, the influence of a gravity field is weakened, the flow is short, and the impurity removal efficiency is high; the test process is convenient to sample and sample, and convenient to operate.
Description
Technical Field
The invention relates to a production device and a production method for preparing high-purity tellurium by vacuum distillation, in particular to a production device and a production method for preparing high-purity tellurium by horizontal vacuum distillation.
Background
Tellurium is typical scattered metal, the content of tellurium in the crust is only 0.001-0.005G/t, the reserve is rare, and the tellurium is widely applied to the fields of infrared detection, solar technology, semiconductors, 5G communication, military industry and the like. For example: cdTe is an important solar cell material, bi 2 Te 3 And PbTe are good refrigeration function materials, and HgCdTe, znCdTe, pbSnTe is mainly applied to the field of infrared detection and military industry. The trace impurities in tellurium can directly influence the material performance, for example, in the aspects of infrared detection and guidance of military weapons, the detection precision can be reduced due to the existence of the impurities, so that the operational radius of the pointed weapon is shortened, and the striking precision of the pointed weapon is reduced. Therefore, high purification of tellurium is of great importance.
Tellurium purification techniques include chemical methods including extraction, precipitation, electrolysis, etc., and physical methods including vacuum distillation, zone melting, straight-pull purification, etc. Chemical methods generally purify tellurium only to a value of 4N. Tellurium belongs to low-melting-point high-saturation vapor pressure metal, and most impurities in tellurium can be effectively removed by vacuum distillation, so that distilled tellurium with higher purity is obtained. Tellurium has a melting point of about 452 c and a boiling point of about 1390 c, and under vacuum conditions, 400 c begins to volatilize, and the saturated vapor pressures of impurities in tellurium at various temperatures are shown in table 1 below.
TABLE 1 saturated vapor pressure of tellurium and impurities at various temperatures
When the temperature is 500 ℃, the saturated vapor pressure difference between tellurium and impurities is larger, and at the moment, metal tellurium and impurities are easier to separate in the vacuum distillation process, so that the actual experiment and the production process are generally controlled to be about 500 ℃. However, as is clear from the above table, the saturated vapor pressure of impurities such as Se, S, as, mg and tellurium is relatively close to that of the impurities at about 500 ℃, and the impurities are difficult to remove by a conventional vacuum distillation method. The existing vertical vacuum distillation technology mostly takes 2N-4N metal as a raw material, 5N high-purity tellurium is prepared through multiple times of distillation, 5N tellurium is difficult to further purify to 6N, and the preparation process is long, the production efficiency is low, and the impurity removal rate is low.
The traditional vacuum distillation technology is mainly a vertical vacuum furnace, in the distillation process, the migration of impurities in tellurium is affected by gravity, so that the separation efficiency of the impurities and main metals is reduced, and the sample loading and sampling processes in the test and production processes are complicated, so that the operation is inconvenient.
CN101892496a discloses a method for preparing 5N high-purity tellurium by using 3N crude tellurium as raw material, the method firstly uses 3N crude tellurium to prepare crude tellurium anode, then uses tellurium dioxide to prepare electrolyte, uses titanium plate as cathode in alkaline electrolytic tank, and makes electrolytic refining for 3-5 days to obtain 5N tellurium. The high-purity tellurium is prepared through electrolysis, the process is long, the operation is complicated, the consumption of reagents is large, the pollution risk in the operation process is high, and the current efficiency is low.
CN107313063a discloses a 5N high purity tellurium smelting method, which combines electrolytic refining and vacuum distillation, firstly uses low current density electro-deposition method to prepare 4N tellurium, and then carries out low temperature vacuum distillation on 4N tellurium ingot to produce distilled tellurium; finally, the distilled tellurium is crushed into small particles, and the ingot casting is heated under the action of hydrogen flow to obtain 5N high-purity tellurium, so that the process is long and the operation is complicated.
CN107585745a discloses a 5N tellurium production process, which comprises the steps of obviously reducing the content of partial impurities in the raw materials through pretreatment, obviously reducing the content of impurities which are difficult to separate in the raw materials, and then carrying out vacuum distillation, hydrogenation for selenium reduction and intermediate frequency ingot casting to obtain 5N high-purity tellurium.
Disclosure of Invention
The invention aims to solve the technical problems and overcome the defects in the prior art, and provides a production device and a production method for horizontal vacuum distillation capable of preparing 6N high-purity tellurium.
The technical scheme adopted for solving the technical problems is as follows: a production device for preparing 6N high-purity tellurium by horizontal vacuum distillation comprises a horizontal pipe; one end of the horizontal pipe is closed, the other end of the horizontal pipe is sealed through a sealing valve, and an air outlet is formed in one end of the sealing valve; the horizontal pipe is connected with the vacuumizing system through the air outlet;
the first heater, the second heater and the heat preservation cover are sequentially arranged outside the horizontal pipe from the closed end to the sealed valve end, and correspond to the first heating area, the second heating area and the heat preservation area respectively;
a graphite sleeve, a primary condensing pipe and a secondary condensing pipe are sequentially arranged in the horizontal pipe from the closed end to the sealing valve end; the graphite sleeve is positioned in the first heating area, the secondary condensation pipe is positioned in the heat preservation area, and the primary condensation pipe extends from the first heating area to the heat preservation area;
the graphite boat is positioned in the first heating area; tellurium materials are filled in a graphite boat.
By adopting the technical scheme, the metal tellurium can be separated from low-boiling impurities and high-boiling impurity elements efficiently by multi-stage independent temperature control and sectional condensation.
Preferably, a gap within 20mm is formed between the first heater and the second heater, and the gap corresponds to a transition zone between the first heating zone and the second heating zone; the primary condensing tubes extend from the first heating zone to the soak zone, or from the transition zone to the soak zone.
The invention is provided with two heaters, wherein a graphite boat is arranged in a first heating area corresponding to a first heater, and the first heater mainly plays a role in controlling the temperature of a distillation area; the first condenser pipe is arranged in the second heating area corresponding to the second heater, and the second heater mainly plays a role in controlling the condensing effect of the first condenser pipe.
The heat insulation materials can be arranged around the first heater 1-1 and the second heater 1-2 and corresponding to the first heating area and the second heating area in a conventional manner, so that energy conservation is facilitated.
Preferably, the horizontal pipe is further provided with an air inlet, and the horizontal pipe is connected with an air inlet system for providing inert atmosphere through the air inlet; an air inlet valve is arranged between the air inlet and the air inlet system, and an air outlet valve is arranged between the air outlet and the vacuumizing system.
By adopting the technical scheme, the air can be discharged, and the sample can be prevented from being polluted by the air.
Preferably, a gap of 5-10 mm is arranged between the first heater and the second heater; the graphite sleeve is 50-100 mm longer than the graphite boat; the length of the primary condensation pipe is 700-800 mm.
By adopting the technical scheme, the distillation device has a good distillation effect.
Preferably, the length of the secondary condensation pipe is 700-800 mm; the length of the graphite boat is 500-600 mm.
By adopting the technical scheme, the distillation device has a good distillation effect.
The tellurium product is condensed in the first-stage condensing pipe, and the second-stage condensing pipe mainly plays a role in collecting low-boiling-point substances.
Preferably, the vacuum pumping system is connected with an exhaust gas treatment system. The tail gas treatment system is mainly used for treating the waste gas containing tellurium and impurities. The tail gas treatment system can be provided with filter cotton for removing gas particles such as selenium, tellurium and the like which volatilize.
Preferably, the impurity content of the graphite boat and the graphite sleeve is below 5 ppm.
By adopting the technical scheme, the high-purity tellurium can be obtained.
Preferably, the inert gas provided by the gas inlet system has a purity of above 6N.
By adopting the technical scheme, the high-purity tellurium can be obtained.
The invention relates to a production method for preparing 6N high-purity tellurium by using the horizontal vacuum distillation of a production device for preparing 6N high-purity tellurium by using the horizontal vacuum distillation, which is characterized by comprising the following steps of:
before starting the vacuum distillation, the vacuum degree in the horizontal tube was controlled to 10 -2 Pa or less;
two-stage distillation was employed: the temperature of a first heater in the first section of distillation is 400-450 ℃, and the temperature of a second heater is 350-400 ℃; the first distillation time is 1-2 h; the temperature of the first heater is 480-530 ℃ during the second-stage distillation, and the temperature of the second heater is 300-350 ℃; the second distillation time is 2-4 h.
Because the impurities Se, S, as and the like in tellurium are relatively volatile, the saturated vapor pressure of the tellurium is relatively close to that of metal tellurium, and effective segregation is difficult in the distillation process, a first section of lower-temperature distillation is firstly arranged, so that the impurities Se, S and As in tellurium are primarily volatilized, gaseous tellurium containing more impurities Se, S and As passes through a first-stage condensation pipe and is condensed in a second-stage condensation pipe, and the metal tellurium in the high-purity graphite boat is primarily separated from the impurities; the temperature of the first heater is raised to 480-530 ℃ by the second section of distillation, and the temperature of the second heater is unchanged or properly reduced, so that the metal tellurium is fully volatilized and fully condensed in the first-stage condenser tube. Finally, the high-purity tellurium is fully condensed in the first-stage condensing pipe, the low-boiling-point substances are condensed in the second-stage condensing pipe, and the high-boiling-point substances remain in the high-purity graphite boat, so that the tellurium and impurity elements are effectively separated.
Preferably, the method comprises the following steps:
(S1) charging: weighing tellurium materials, loading the tellurium materials into a graphite boat, and placing the graphite boat into a graphite sleeve; closing the sealing valve;
(S2) vacuumizing: inert gas is introduced into the horizontal pipe through the air inlet system to replace air in the horizontal pipe; closing the air inlet valve, opening the air outlet valve, and controlling the vacuum degree in the horizontal pipe to be 10 through the vacuumizing system -2 Pa or less;
(S3) distillation: performing the two-stage distillation;
(S4) sampling; and after the distillation is finished, the heating power supply is turned off, and after the temperature is reduced to the room temperature, the crystalline tellurium in the primary condensation pipe is obtained.
By adopting the technical scheme, the distillation device has a good distillation effect.
More preferably, in step (S2), flow (a) and flow (b) are alternated to achieve replacement of the air in the horizontal tube with an inert gas:
(a) Closing the air outlet valve and the vacuumizing system, and opening the air inlet valve and the air inlet system;
(b) Closing the air inlet valve and the air inlet system, and opening the air outlet valve and the vacuumizing system.
By adopting the technical scheme, the air-removing device has a good air-removing effect. Air pollution to the sample can be prevented.
More preferably, in step (S4), after the heating power is turned off, the vacuum pumping system is turned off, and the air inlet system and the air inlet valve are opened to form a micro-positive pressure inert atmosphere in the horizontal pipe after the temperature is reduced to below 200 ℃.
By adopting the technical scheme, the high-purity tellurium can be obtained. Air can be prevented from entering to avoid polluting the sample.
The traditional vertical vacuum distillation can only purify the metal tellurium to 5N, and has the advantages of long process flow, low recovery rate and unstable product quality. One side of the horizontal vacuum distillation device is communicated with the vacuumizing system, so that a driving force is provided for tellurium and impurity migration; the gravity field is vertical downwards, the driving force is not counteracted by gravity, compared with vertical distillation, the influence of the gravity field is weakened, the metal vapor migration speed is improved, the mass transfer process in the distillation process is enhanced, the separation efficiency of impurities and main metals is improved, and the metal tellurium can be purified to 6N. And the sample loading and sampling are convenient in the test process.
According to the invention, two heaters and two sections of condensing pipes are adopted to realize multi-section independent temperature control and sectional condensation, impurities such as Se, S, as, mg and the like can be separated to be relatively close to saturated vapor pressure of tellurium, and the preparation of 6N high-purity tellurium is realized through impurities which are difficult to remove by a conventional vacuum distillation method.
Compared with the prior art, the invention has the beneficial effects that:
(1) Realizing the high-efficiency separation of metal tellurium, low-boiling impurities and high-boiling impurity elements and the preparation of 6N high-purity tellurium;
(2) The horizontal vacuum distillation is adopted to prepare high-purity tellurium, the driving force is small under the action of gravity cancellation, the influence of a gravity field is weakened, the flow is short, and the impurity removal efficiency is high;
(3) The test process is convenient to sample and sample, and convenient to operate.
Drawings
FIG. 1 is a schematic structural diagram of a production apparatus for preparing 6N high purity tellurium by horizontal vacuum distillation in example 1.
Reference numerals illustrate:
1-1: a first heater; 1-2: a second heater; 2: tellurium material; 3: a graphite boat; 4: a graphite sleeve; 5: a horizontal tube; 6: a first-stage condenser tube; 7: a secondary condenser tube; 8-2: an air inlet valve; 8-3: an air outlet valve; 9: an air intake system; 10: sealing the valve; 12: an air inlet; 13: an air outlet; 16: a vacuum pumping system; 17: a tail gas treatment system; 18: a furnace body; 19: and a heat preservation cover.
Detailed Description
The invention is further described below with reference to examples and figures.
The starting materials used in the examples of the present invention were all obtained by conventional commercial means.
The following is a preferred embodiment only, and the invention may be embodied in a number of different forms, which are defined and covered by the claims.
Example 1
Reference is made to fig. 1. The production device for preparing 6N high-purity tellurium by horizontal vacuum distillation in the embodiment comprises a horizontal pipe 5; one end of the horizontal pipe 5 is closed, the other end of the horizontal pipe is sealed through a sealing valve 10, and one end of the sealing valve 10 is provided with an air outlet 13; the horizontal pipe 5 is connected with a vacuum pumping system 16 through the air outlet 13;
the first heater 1-1, the second heater 1-2 and the heat preservation cover 19 are sequentially arranged outside the horizontal pipe 5 from the closed end to the end of the sealing valve 10, and correspond to the first heating zone, the second heating zone and the heat preservation zone respectively;
a graphite sleeve 4, a primary condensation pipe 6 and a secondary condensation pipe 7 are sequentially arranged in the horizontal pipe 5 from the closed end to the end of the sealing valve 10; the graphite sleeve 4 is positioned in the first heating area, and the secondary condensing pipe 7 is positioned in the heat preservation area;
in the embodiment, the first heater 1-1 and the second heater 1-2 are positioned in the same furnace body 18, and the interval between the two heaters is 10mm, and the two heaters are correspondingly a transition zone between the first heating zone and the second heating zone; the primary condenser tube 6 extends from the transition zone to the holding zone.
The graphite boat 3 is positioned in the first heating area; tellurium material 2 is loaded in a graphite boat 3. The graphite boat 3 is 500mm long, the graphite sleeve 4 is 550mm long, the primary condensation pipe 6 is 700mm long, and the secondary condensation pipe 7 is 700mm long.
The horizontal pipe 5 is also provided with an air inlet 12, and the horizontal pipe 5 is connected with an air inlet system 9 for providing inert atmosphere through the air inlet 12; an air inlet valve 8-2 is arranged between the air inlet 12 and the air inlet system 9, and an air outlet valve 8-3 is arranged between the air outlet 13 and the vacuumizing system 16.
The vacuum pumping system 16 is connected with the tail gas treatment system 17. The tail gas treatment system 17 is provided with filter cotton for removing gas particles such as selenium, tellurium and the like which volatilize.
The impurity content of the graphite boat 3 and the graphite sleeve 4 is below 5 ppm.
The inert gas provided by the gas inlet system 9 has a purity of more than 6N.
The horizontal tube 5 of this embodiment is made of stainless steel.
The production method for preparing the 6N high-purity tellurium by using the horizontal vacuum distillation of the production device for preparing the 6N high-purity tellurium by using the horizontal vacuum distillation comprises the following steps:
(S1) charging: weighing 3.5kg of 5N tellurium material, loading the 5N tellurium material into a graphite boat 3, and placing the graphite boat 3 into a graphite sleeve 4; closing the sealing valve 10;
(S2) vacuumizing: inert gas is introduced into the horizontal pipe 5 through the air inlet system 9 to replace air in the horizontal pipe 5; closing the air inlet valve 8-2, opening the air outlet valve 8-3, and controlling the vacuum degree in the horizontal pipe 5 to be 10 through the vacuumizing system 16 -2 Pa or less;
(S3) distillation: two-stage distillation was performed: the temperature of a first heater in the first section of distillation is 400 ℃, and the temperature of a second heater is 350 ℃; the first distillation time is 1.5h; the temperature of the first heater in the second stage distillation is 480 ℃, and the temperature of the second heater is 300 ℃; the second distillation time is 3.5h; through distillation, tellurium in the graphite boat 3 is fully volatilized, tellurium is fully condensed in the first-stage condensation pipe 6, low-boiling-point substances are condensed in the second-stage condensation pipe 7, and high-boiling-point substances remain in the graphite boat 3, so that effective separation of tellurium and impurity elements is realized;
(S4) sampling; after the distillation is finished, the heating power supply is turned off; when the temperature is reduced to below 200 ℃, the vacuumizing system is closed, and the air inlet system 9 and the air inlet valve 8-2 are opened to form micro-positive pressure inert atmosphere in the horizontal pipe 5; after the temperature is reduced to room temperature, closing an air inlet system 9, an air inlet valve 8-2 and an air outlet valve 8-3, opening a sealing valve 10, and taking out the secondary condensation pipe 7, the primary condensation pipe 6 and the graphite sleeve 4 in sequence; the crystallized tellurium is positioned in the first-stage condensing tube 6, and high-purity tellurium is obtained.
In step (S2), the flow (a) and the flow (b) are alternately performed 3 times to achieve replacement of the air in the horizontal tube 5 with an inert gas; that is, the steps (a) - (b) - (a) - (b) - (a) - (b) are performed sequentially; wherein:
(a) Closing the air outlet valve 8-3 and the vacuumizing system 16, opening the air inlet valve 8-2 and the air inlet system 9, and ventilating for 10min;
(b) Closing the air inlet valve 8-2 and the air inlet system 9, opening the air outlet valve 8-3 and the vacuumizing system 16, and vacuumizing to the air pressure below 100Pa in the horizontal pipe 5.
The GDMS analysis results of the tellurium product obtained in this example are shown in Table 2, and it can be seen that the impurity contents of the tellurium product obtained in this example are greatly reduced as compared with the raw materials, and reach the 6N level. The units in Table 2 are ppbw.
TABLE 2 statistical Table of impurity content of high purity tellurium (unit: ppbw) obtained in example 1
| Element(s) | Mg | Al | Ca | Fe | Ni | Cu | Zn | Se | Ag | Cd | Pb | As | S |
| Tellurium raw material | 68 | 72 | 65 | 102 | 40 | 91 | 40 | 163 | 31 | 32 | 35 | 46 | 38 |
| Standard of | <50 | <50 | <100 | <50 | <50 | <10 | <100 | <100 | <10 | <50 | <50 | / | / |
| Example 1 | 8 | <5 | 12 | <0.5 | <0.5 | <1 | 7.1 | 58 | <1 | <5 | <5 | 3.3 | 4 |
Example 2
The production device for preparing 6N high-purity tellurium by horizontal vacuum distillation in the embodiment comprises a horizontal pipe 5; one end of the horizontal pipe 5 is closed, the other end of the horizontal pipe is sealed through a sealing valve 10, and one end of the sealing valve 10 is provided with an air outlet 13; the horizontal pipe 5 is connected with a vacuum pumping system 16 through the air outlet 13;
the first heater 1-1, the second heater 1-2 and the heat preservation cover 19 are sequentially arranged outside the horizontal pipe 5 from the closed end to the end of the sealing valve 10, and correspond to the first heating zone, the second heating zone and the heat preservation zone respectively;
a graphite sleeve 4, a primary condensation pipe 6 and a secondary condensation pipe 7 are sequentially arranged in the horizontal pipe 5 from the closed end to the end of the sealing valve 10; the graphite sleeve 4 is positioned in the first heating area, and the secondary condensing pipe 7 is positioned in the heat preservation area;
in the embodiment, the first heater 1-1 and the second heater 1-2 are spaced by 5mm, and the transition zone between the first heating zone and the second heating zone is correspondingly formed; the primary condenser tube 6 extends from the transition zone to the holding zone.
The graphite boat 3 is positioned in the first heating area; tellurium material 2 is loaded in a graphite boat 3. The graphite boat 3 is 600mm long, the graphite sleeve 4 is 700mm long, the primary condensation pipe 6 is 800mm long, and the secondary condensation pipe 7 is 800mm long.
The horizontal pipe 5 is also provided with an air inlet 12, and the horizontal pipe 5 is connected with an air inlet system 9 for providing inert atmosphere through the air inlet 12; an air inlet valve 8-2 is arranged between the air inlet 12 and the air inlet system 9, and an air outlet valve 8-3 is arranged between the air outlet 13 and the vacuumizing system 16.
The vacuum pumping system 16 is connected with the tail gas treatment system 17.
The impurity content of the graphite boat 3 and the graphite sleeve 4 is below 5 ppm.
The inert gas provided by the gas inlet system 9 has a purity of more than 6N.
The horizontal tube 5 of the present embodiment is a quartz tube.
The production method for preparing the 6N high-purity tellurium by using the horizontal vacuum distillation of the production device for preparing the 6N high-purity tellurium by using the horizontal vacuum distillation comprises the following steps:
(S1) charging: weighing 3.8kg of 5N tellurium material, loading the 5N tellurium material into a graphite boat 3, and placing the graphite boat 3 into a graphite sleeve 4; closing the sealing valve 10;
(S2) vacuumizing: inert gas is introduced into the horizontal pipe 5 through the air inlet system 9 to replace air in the horizontal pipe 5; closing the air inlet valve 8-2, opening the air outlet valve 8-3, and controlling the vacuum degree in the horizontal pipe 5 to be 10 through the vacuumizing system 16 -2 Pa or less;
(S3) distillation: two-stage distillation was performed: the temperature of a first heater in the first section of distillation is 400 ℃, and the temperature of a second heater is 400 ℃; the first distillation time is 1.5h; the temperature of the first heater in the second stage of distillation is 500 ℃, and the temperature of the second heater is 300 ℃; the second distillation time is 2.5h; through distillation, tellurium in the graphite boat 3 is fully volatilized, tellurium is fully condensed in the first-stage condensation pipe 6, low-boiling-point substances are condensed in the second-stage condensation pipe 7, and high-boiling-point substances remain in the graphite boat 3, so that effective separation of tellurium and impurity elements is realized;
(S4) sampling; after the distillation is finished, the heating power supply is turned off; when the temperature is reduced to below 200 ℃, the vacuumizing system is closed, and the air inlet system 9 and the air inlet valve 8-2 are opened to form micro-positive pressure inert atmosphere in the horizontal pipe 5; after the temperature is reduced to room temperature, closing an air inlet system 9, an air inlet valve 8-2 and an air outlet valve 8-3, opening a sealing valve 10, and taking out the secondary condensation pipe 7, the primary condensation pipe 6 and the graphite sleeve 4 in sequence; the crystallized tellurium is positioned in the first-stage condensing tube 6, and high-purity tellurium is obtained.
In step (S2), the flow (a) and the flow (b) are alternately performed 3 times to achieve replacement of the air in the horizontal tube 5 with an inert gas; that is, the steps (a) - (b) - (a) - (b) - (a) - (b) are performed sequentially; wherein:
(a) Closing the air outlet valve 8-3 and the vacuumizing system 16, opening the air inlet valve 8-2 and the air inlet system 9, and ventilating for 8min;
(b) Closing the air inlet valve 8-2 and the air inlet system 9, opening the air outlet valve 8-3 and the vacuumizing system 16, and vacuumizing to the air pressure below 100Pa in the horizontal pipe 5.
The GDMS analysis results of the tellurium product obtained in this example are shown in Table 3, and it can be seen that the impurity contents of the tellurium product obtained in this example are greatly reduced as compared with the raw materials, and reach the 6N level. The unit in Table 3 is ppbw.
TABLE 3 statistical Table of impurity content of high purity tellurium (unit: ppbw) obtained in example 2
| Element(s) | Mg | Al | Ca | Fe | Ni | Cu | Zn | Se | Ag | Cd | Pb | As | S |
| Tellurium raw material | 51 | 82 | 61 | 113 | 36 | 131 | 28 | 283 | 31 | 20 | 55 | 54 | 43 |
| Standard of | <50 | <50 | <100 | <50 | <50 | <10 | <100 | <100 | <10 | <50 | <50 | / | / |
| Example 2 | 2 | <5 | 10 | <0.5 | <0.5 | <1 | 1.1 | 79 | <1 | <5 | <5 | 5 | 4.6 |
Example 3
The production device for preparing 6N high-purity tellurium by horizontal vacuum distillation in the embodiment comprises a horizontal pipe 5; one end of the horizontal pipe 5 is closed, the other end of the horizontal pipe is sealed through a sealing valve 10, and one end of the sealing valve 10 is provided with an air outlet 13; the horizontal pipe 5 is connected with a vacuum pumping system 16 through the air outlet 13;
the first heater 1-1, the second heater 1-2 and the heat preservation cover 19 are sequentially arranged outside the horizontal pipe 5 from the closed end to the end of the sealing valve 10, and correspond to the first heating zone, the second heating zone and the heat preservation zone respectively;
a graphite sleeve 4, a primary condensation pipe 6 and a secondary condensation pipe 7 are sequentially arranged in the horizontal pipe 5 from the closed end to the end of the sealing valve 10; the graphite sleeve 4 is positioned in the first heating area, and the secondary condensing pipe 7 is positioned in the heat preservation area;
in the embodiment, the first heater 1-1 and the second heater 1-2 are spaced 15mm apart, and correspond to a transition zone between the first heating zone and the second heating zone; the primary condenser tube 6 extends from the transition zone to the holding zone.
The graphite boat 3 is positioned in the first heating area; tellurium material 2 is loaded in a graphite boat 3. The graphite boat 3 is 600mm long, the graphite sleeve 4 is 700mm long, the primary condensation pipe 6 is 700mm long, and the secondary condensation pipe 7 is 700mm long.
The horizontal pipe 5 is also provided with an air inlet 12, and the horizontal pipe 5 is connected with an air inlet system 9 for providing inert atmosphere through the air inlet 12; an air inlet valve 8-2 is arranged between the air inlet 12 and the air inlet system 9, and an air outlet valve 8-3 is arranged between the air outlet 13 and the vacuumizing system 16.
The vacuum pumping system 16 is connected with the tail gas treatment system 17.
The impurity content of the graphite boat 3 and the graphite sleeve 4 is below 5 ppm.
The inert gas provided by the gas inlet system 9 has a purity of more than 6N.
The horizontal tube 5 of the present embodiment is a quartz tube.
The production method for preparing the 6N high-purity tellurium by using the horizontal vacuum distillation of the production device for preparing the 6N high-purity tellurium by using the horizontal vacuum distillation comprises the following steps:
(S1) charging: weighing 4.2kg of 5N tellurium material, loading the 5N tellurium material into a graphite boat 3, and placing the graphite boat 3 into a graphite sleeve 4; closing the sealing valve 10;
(S2) vacuumizing: inert gas is introduced into the horizontal pipe 5 through the air inlet system 9 to replace air in the horizontal pipe 5; closing the air inlet valve 8-2, opening the air outlet valve 8-3, and controlling the vacuum degree in the horizontal pipe 5 to be 10 through the vacuumizing system 16 -2 Pa or less;
(S3) distillation: two-stage distillation was performed: the temperature of a first heater in the first stage of distillation is 450 ℃, and the temperature of a second heater is 350 ℃; the first distillation time is 1.2h; the temperature of the first heater in the second stage distillation is 530 ℃ and the temperature of the second heater is 300 ℃; the second distillation time is 3h; through distillation, tellurium in the graphite boat 3 is fully volatilized, tellurium is fully condensed in the first-stage condensation pipe 6, low-boiling-point substances are condensed in the second-stage condensation pipe 7, and high-boiling-point substances remain in the graphite boat 3, so that effective separation of tellurium and impurity elements is realized;
(S4) sampling; after the distillation is finished, the heating power supply is turned off; when the temperature is reduced to below 200 ℃, the vacuumizing system is closed, and the air inlet system 9 and the air inlet valve 8-2 are opened to form micro-positive pressure inert atmosphere in the horizontal pipe 5; after the temperature is reduced to room temperature, closing an air inlet system 9, an air inlet valve 8-2 and an air outlet valve 8-3, opening a sealing valve 10, and taking out the secondary condensation pipe 7, the primary condensation pipe 6 and the graphite sleeve 4 in sequence; the crystallized tellurium is positioned in the first-stage condensing tube 6, and high-purity tellurium is obtained.
In step (S2), the flow (a) and the flow (b) are alternately performed 2 times to achieve replacement of the air in the horizontal tube 5 with an inert gas; that is, the steps (a) - (b) - (a) - (b) are performed sequentially; wherein:
(a) Closing the air outlet valve 8-3 and the vacuumizing system 16, opening the air inlet valve 8-2 and the air inlet system 9, and ventilating for 5min;
(b) Closing the air inlet valve 8-2 and the air inlet system 9, opening the air outlet valve 8-3 and the vacuumizing system 16, and vacuumizing to the air pressure below 100Pa in the horizontal pipe 5.
The GDMS analysis results of the tellurium product obtained in this example are shown in Table 4, and it can be seen that the impurity contents of the tellurium product obtained in this example are greatly reduced as compared with the raw materials, and reach the 6N level. The units in Table 4 are ppbw.
TABLE 4 statistical Table of impurity content of high purity tellurium (unit: ppbw) obtained in example 3
| Element(s) | Mg | Al | Ca | Fe | Ni | Cu | Zn | Se | Ag | Cd | Pb | As | S |
| Tellurium raw material | 57 | 96 | 72 | 107 | 28 | 125 | 38 | 179 | 36 | 34 | 53 | 37 | 45 |
| Standard of | <50 | <50 | <100 | <50 | <50 | <10 | <100 | <100 | <10 | <50 | <50 | / | / |
| Example 3 | <1 | <5 | 6 | <0.5 | <0.5 | <1 | 2.6 | 56 | <1 | <5 | <5 | <1 | 4.5 |
Example 4
The production device for preparing 6N high-purity tellurium by horizontal vacuum distillation in the embodiment comprises a horizontal pipe 5; one end of the horizontal pipe 5 is closed, the other end of the horizontal pipe is sealed through a sealing valve 10, and one end of the sealing valve 10 is provided with an air outlet 13; the horizontal pipe 5 is connected with a vacuum pumping system 16 through the air outlet 13;
the first heater 1-1, the second heater 1-2 and the heat preservation cover 19 are sequentially arranged outside the horizontal pipe 5 from the closed end to the end of the sealing valve 10, and correspond to the first heating zone, the second heating zone and the heat preservation zone respectively;
a graphite sleeve 4, a primary condensation pipe 6 and a secondary condensation pipe 7 are sequentially arranged in the horizontal pipe 5 from the closed end to the end of the sealing valve 10; the graphite sleeve 4 is positioned in the first heating area, and the secondary condensing pipe 7 is positioned in the heat preservation area;
in the embodiment, the first heater 1-1 and the second heater 1-2 are spaced by 10mm, and the transition zone between the first heating zone and the second heating zone is correspondingly formed; the primary condenser tube 6 extends from the transition zone to the holding zone.
The graphite boat 3 is positioned in the first heating area; tellurium material 2 is loaded in a graphite boat 3. The graphite boat 3 is 550mm long, the graphite sleeve 4 is 650mm long, the primary condensation pipe 6 is 750mm long, and the secondary condensation pipe 7 is 800mm long.
The horizontal pipe 5 is also provided with an air inlet 12, and the horizontal pipe 5 is connected with an air inlet system 9 for providing inert atmosphere through the air inlet 12; an air inlet valve 8-2 is arranged between the air inlet 12 and the air inlet system 9, and an air outlet valve 8-3 is arranged between the air outlet 13 and the vacuumizing system 16.
The vacuum pumping system 16 is connected with the tail gas treatment system 17.
The impurity content of the graphite boat 3 and the graphite sleeve 4 is below 5 ppm.
The inert gas provided by the gas inlet system 9 has a purity of more than 6N.
The horizontal tube 5 of this embodiment is made of stainless steel.
The production method for preparing the 6N high-purity tellurium by using the horizontal vacuum distillation of the production device for preparing the 6N high-purity tellurium by using the horizontal vacuum distillation comprises the following steps:
(S1) charging: weighing 5.0kg of 5N tellurium material, loading the 5N tellurium material into a graphite boat 3, and placing the graphite boat 3 into a graphite sleeve 4; closing the sealing valve 10;
(S2) vacuumizing: inert gas is introduced into the horizontal pipe 5 through the air inlet system 9 to replace air in the horizontal pipe 5; closing the air inlet valve 8-2, opening the air outlet valve 8-3, and vacuumizing the horizontal tube 5 by the vacuumizing system 16Controlled to 10 -2 Pa or less;
(S3) distillation: two-stage distillation was performed: the temperature of a first heater in the first stage of distillation is 430 ℃, and the temperature of a second heater is 350 ℃; the first distillation time is 2h; the temperature of the first heater in the second stage distillation is 520 ℃, and the temperature of the second heater is 350 ℃; the second distillation time is 3.5h; through distillation, tellurium in the graphite boat 3 is fully volatilized, tellurium is fully condensed in the first-stage condensation pipe 6, low-boiling-point substances are condensed in the second-stage condensation pipe 7, and high-boiling-point substances remain in the graphite boat 3, so that effective separation of tellurium and impurity elements is realized;
(S4) sampling; after the distillation is finished, the heating power supply is turned off; when the temperature is reduced to below 200 ℃, the vacuumizing system is closed, and the air inlet system 9 and the air inlet valve 8-2 are opened to form micro-positive pressure inert atmosphere in the horizontal pipe 5; after the temperature is reduced to room temperature, closing an air inlet system 9, an air inlet valve 8-2 and an air outlet valve 8-3, opening a sealing valve 10, and taking out the secondary condensation pipe 7, the primary condensation pipe 6 and the graphite sleeve 4 in sequence; the crystallized tellurium is positioned in the first-stage condensing tube 6, and high-purity tellurium is obtained.
In step (S2), the flow (a) and the flow (b) are alternately performed 2 times to achieve replacement of the air in the horizontal tube 5 with an inert gas; that is, the steps (a) - (b) - (a) - (b) are performed sequentially; wherein:
(a) Closing the air outlet valve 8-3 and the vacuumizing system 16, opening the air inlet valve 8-2 and the air inlet system 9, and ventilating for 10min;
(b) Closing the air inlet valve 8-2 and the air inlet system 9, opening the air outlet valve 8-3 and the vacuumizing system 16, and vacuumizing to the air pressure below 100Pa in the horizontal pipe 5.
The GDMS analysis results of the tellurium product obtained in this example are shown in Table 5, and it can be seen that the impurity contents of the tellurium product obtained in this example are greatly reduced as compared with the raw materials, and reach the 6N level. The units in Table 5 are ppbw.
TABLE 5 statistical Table of impurity content of high purity tellurium (unit: ppbw) obtained in example 4
| Element(s) | Mg | Al | Ca | Fe | Ni | Cu | Zn | Se | Ag | Cd | Pb | As | S |
| Tellurium raw material | 62 | 91 | 65 | 109 | 38 | 118 | 29 | 191 | 28 | 36 | 48 | 38 | 36 |
| Standard of | <50 | <50 | <100 | <50 | <50 | <10 | <100 | <100 | <10 | <50 | <50 | / | / |
| Example 4 | 5 | <5 | 9 | <0.5 | <0.5 | 4 | <1 | 68 | <1 | <5 | <5 | <1 | 2.8 |
Claims (10)
1. The production device for preparing 6N high-purity tellurium by horizontal vacuum distillation is characterized by comprising a horizontal pipe (5); one end of the horizontal pipe (5) is closed, the other end of the horizontal pipe is sealed through a sealing valve (10), and an air outlet (13) is formed in one end of the sealing valve (10); the horizontal pipe (5) is connected with the vacuumizing system (16) through the air outlet (13);
the first heater (1-1), the second heater (1-2) and the heat preservation cover (19) are sequentially arranged outside the horizontal pipe (5) from the closed end to the end of the sealing valve (10), and correspond to the first heating zone, the second heating zone and the heat preservation zone respectively;
a graphite sleeve (4), a primary condensing pipe (6) and a secondary condensing pipe (7) are sequentially arranged in the horizontal pipe (5) from the closed end to the end of the sealing valve (10); the graphite sleeve (4) is positioned in the first heating zone, the secondary condensing pipe (7) is positioned in the heat preservation zone, and the primary condensing pipe (6) extends from the first heating zone to the heat preservation zone;
the graphite boat (3) is positioned in the first heating area; tellurium (2) is arranged in the graphite boat (3).
2. The production device for preparing 6N high-purity tellurium by horizontal vacuum distillation according to claim 1, wherein a gap of 20mm or less is formed between the first heater (1-1) and the second heater (1-2), which corresponds to a transition zone between the first heating zone and the second heating zone; the primary condensing tube (6) extends from the first heating zone to the holding zone, or from the transition zone to the holding zone.
3. The production device for preparing 6N high purity tellurium by horizontal vacuum distillation according to claim 1 or 2, wherein the horizontal tube (5) is further provided with an air inlet (12), and the horizontal tube (5) is connected with an air inlet system (9) for providing inert atmosphere through the air inlet (12); an air inlet valve (8-2) is arranged between the air inlet (12) and the air inlet system (9), and an air outlet valve (8-3) is arranged between the air outlet (13) and the vacuumizing system (16).
4. A production device for preparing 6N high purity tellurium by horizontal vacuum distillation according to any of claims 1-3, wherein a gap of 5-10 mm is provided between the first heater (1-1) and the second heater (1-2); the graphite sleeve (4) is 50-100 mm longer than the graphite boat (3); the length of the primary condensation pipe (6) is 700-800 mm.
5. The production device for preparing 6N high-purity tellurium by horizontal vacuum distillation according to claim 4, wherein the length of the secondary condensation pipe (7) is 700-800 mm; the length of the graphite boat (3) is 500-600 mm.
6. The production device for preparing 6N high-purity tellurium by horizontal vacuum distillation according to any one of claims 1-5, wherein the vacuumizing system (16) is connected with the tail gas treatment system (17); the impurity content of the graphite boat (3) and the graphite sleeve (4) is below 5 ppm; the inert gas provided by the gas inlet system (9) has the purity of more than 6N.
7. A production method for producing 6N high purity tellurium by horizontal vacuum distillation using the production apparatus for producing 6N high purity tellurium by horizontal vacuum distillation as claimed in any one of claims 1 to 6, characterized by:
before starting the vacuum distillation, the vacuum degree in the horizontal tube (5) is controlled to be 10 -2 Pa or less;
two-stage distillation was employed: the temperature of a first heater in the first section of distillation is 400-450 ℃, and the temperature of a second heater is 350-400 ℃; the first-stage distillation time is 1-2 h; the temperature of the first heater in the second section of distillation is 480-530 ℃, and the temperature of the second heater is 300-350 ℃; the second-stage distillation time is 2-4 h.
8. The method for producing 6N high purity tellurium by horizontal vacuum distillation as claimed in claim 7, comprising the steps of:
(S1) charging: weighing tellurium materials, loading the tellurium materials into a graphite boat (3), and putting the graphite boat (3) into a graphite sleeve (4); closing the sealing valve (10);
(S2) vacuumizing: inert gas is introduced into the horizontal pipe (5) through the air inlet system (9) to replace air in the horizontal pipe (5); closing the air inlet valve (8-2), opening the air outlet valve (8-3), and controlling the vacuum degree in the horizontal pipe (5) to be 10 through the vacuumizing system (16) -2 Pa or less;
(S3) distillation: performing the two-stage distillation;
(S4) sampling; and after the distillation is finished, the heating power supply is turned off, and after the temperature is reduced to the room temperature, the crystalline tellurium in the primary condensation pipe (6) is obtained.
9. The production method for producing 6N high purity tellurium by horizontal vacuum distillation according to claim 8, wherein in step (S2), the flow (a) and the flow (b) are alternately performed to realize replacement of air in the horizontal tube (5) with an inert gas:
(a) Closing the air outlet valve (8-3) and the vacuumizing system (16), and opening the air inlet valve (8-2) and the air inlet system (9);
(b) Closing the air inlet valve (8-2) and the air inlet system (9), and opening the air outlet valve (8-3) and the vacuumizing system (16).
10. The method for producing 6N high purity tellurium by horizontal vacuum distillation according to claim 8 or 9, wherein in step (S4), after the heating power is turned off, the vacuum pumping system is turned off and the air intake system (9) and the air intake valve (8-2) are opened to form a micro positive pressure inert atmosphere in the horizontal tube (5) when the temperature is lowered to 200 ℃.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202311480523.6A CN117466257A (en) | 2023-11-08 | 2023-11-08 | Production device and production method for preparing 6N high-purity tellurium by horizontal vacuum distillation |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202311480523.6A CN117466257A (en) | 2023-11-08 | 2023-11-08 | Production device and production method for preparing 6N high-purity tellurium by horizontal vacuum distillation |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN117466257A true CN117466257A (en) | 2024-01-30 |
Family
ID=89630923
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202311480523.6A Pending CN117466257A (en) | 2023-11-08 | 2023-11-08 | Production device and production method for preparing 6N high-purity tellurium by horizontal vacuum distillation |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN117466257A (en) |
-
2023
- 2023-11-08 CN CN202311480523.6A patent/CN117466257A/en active Pending
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101665253B (en) | Polysilicon purification method and crucible and purification device used for polysilicon purification | |
| CN1317405C (en) | High vacuum in-situ two-step refining process for high purity material | |
| US6805833B2 (en) | Apparatus for enhanced purification of high-purity metals | |
| US20080257109A1 (en) | High Vacuum In-Situ Refining Method for High-Purity Materials and an Apparatus Thereof | |
| CN102465209B (en) | Method and vacuum distillation device for preparing high-purity neodymium | |
| CN110316705B (en) | Method for preparing high-purity selenium from crude selenium product | |
| CN107326199B (en) | The continuous producing method of impurity zinc-mercury in a kind of removing gallium | |
| CN117466257A (en) | Production device and production method for preparing 6N high-purity tellurium by horizontal vacuum distillation | |
| US6932852B2 (en) | Method and apparatus for enhanced purification of high-purity metals | |
| CN113387336B (en) | Method for removing selenium from tellurium ingot | |
| CN204058569U (en) | A kind of system of vacuum distilling separating-purifying bismuth | |
| CN218097186U (en) | Device for treating low-vanadium titanium aluminum waste and preparing high-quality aluminum | |
| CN111646454B (en) | System and method for separating carbon and electrolyte in aluminum electrolysis carbon slag | |
| CN212357345U (en) | Purification device for purifying indium from ITO waste target | |
| CN101941698B (en) | Method and device for efficiently removing phosphorus impurities in silicon by electron beam melting | |
| CN107164786A (en) | A kind of method of copper electrolyte precipitation to remove impurities | |
| CN204417566U (en) | A kind of device processing antimony arsenic material | |
| CN112795796A (en) | Method for distilling and purifying crude indium by using intermediate frequency furnace | |
| CN217236439U (en) | Recovery plant of nickel cadmium battery waste material | |
| CN116328674A (en) | Production device and production method for preparing 5N high-purity tellurium from 2N crude tellurium | |
| CN114807620B (en) | Equipment and method for vacuum gasification-directional condensation separation of ternary alloy of lead, antimony and arsenic | |
| CN111041228A (en) | Method and equipment for integrated refining of crude zinc | |
| CN117776117A (en) | Tellurium purification method for efficiently removing oxygen, sulfur and selenium | |
| CN110482495B (en) | Device and method for purifying crude selenium through oxidation-evaporation-carbothermic reduction | |
| CN104561605B (en) | A kind of device processing antimony arsenic material |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination |