CN1927701A - Producing device of high-purity selenium and producing process - Google Patents
Producing device of high-purity selenium and producing process Download PDFInfo
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- CN1927701A CN1927701A CN 200610122508 CN200610122508A CN1927701A CN 1927701 A CN1927701 A CN 1927701A CN 200610122508 CN200610122508 CN 200610122508 CN 200610122508 A CN200610122508 A CN 200610122508A CN 1927701 A CN1927701 A CN 1927701A
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- 239000011669 selenium Substances 0.000 title claims abstract description 107
- BUGBHKTXTAQXES-UHFFFAOYSA-N Selenium Chemical compound [Se] BUGBHKTXTAQXES-UHFFFAOYSA-N 0.000 title claims abstract description 101
- 229910052711 selenium Inorganic materials 0.000 title claims abstract description 101
- 238000000034 method Methods 0.000 title claims abstract description 52
- 239000000463 material Substances 0.000 claims abstract description 54
- 210000004907 gland Anatomy 0.000 claims abstract description 3
- 238000004519 manufacturing process Methods 0.000 claims description 62
- 239000002994 raw material Substances 0.000 claims description 44
- 230000002950 deficient Effects 0.000 claims description 18
- 238000004821 distillation Methods 0.000 claims description 6
- 230000015572 biosynthetic process Effects 0.000 claims description 5
- 238000001816 cooling Methods 0.000 claims description 5
- 238000013467 fragmentation Methods 0.000 claims description 4
- 238000006062 fragmentation reaction Methods 0.000 claims description 4
- 238000013022 venting Methods 0.000 claims description 3
- 238000009826 distribution Methods 0.000 claims description 2
- 238000009413 insulation Methods 0.000 claims 1
- 239000012535 impurity Substances 0.000 abstract description 11
- 238000000926 separation method Methods 0.000 abstract description 4
- 238000009792 diffusion process Methods 0.000 abstract 1
- 230000002349 favourable effect Effects 0.000 abstract 1
- 239000000047 product Substances 0.000 description 48
- 239000004065 semiconductor Substances 0.000 description 15
- 238000005516 engineering process Methods 0.000 description 11
- 238000010438 heat treatment Methods 0.000 description 8
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 7
- 238000004134 energy conservation Methods 0.000 description 5
- 150000001875 compounds Chemical class 0.000 description 4
- 238000011161 development Methods 0.000 description 4
- 230000007613 environmental effect Effects 0.000 description 4
- 239000011133 lead Substances 0.000 description 4
- 239000010453 quartz Substances 0.000 description 4
- 238000009835 boiling Methods 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
- 238000009833 condensation Methods 0.000 description 3
- 230000005494 condensation Effects 0.000 description 3
- 238000003698 laser cutting Methods 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 238000000746 purification Methods 0.000 description 3
- SBIBMFFZSBJNJF-UHFFFAOYSA-N selenium;zinc Chemical compound [Se]=[Zn] SBIBMFFZSBJNJF-UHFFFAOYSA-N 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- 230000001276 controlling effect Effects 0.000 description 2
- UIPVMGDJUWUZEI-UHFFFAOYSA-N copper;selanylideneindium Chemical compound [Cu].[In]=[Se] UIPVMGDJUWUZEI-UHFFFAOYSA-N 0.000 description 2
- 239000008358 core component Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000005265 energy consumption Methods 0.000 description 2
- 235000021050 feed intake Nutrition 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 238000005057 refrigeration Methods 0.000 description 2
- 230000003252 repetitive effect Effects 0.000 description 2
- 229940065287 selenium compound Drugs 0.000 description 2
- 150000003343 selenium compounds Chemical class 0.000 description 2
- 239000010409 thin film Substances 0.000 description 2
- YBNMDCCMCLUHBL-UHFFFAOYSA-N (2,5-dioxopyrrolidin-1-yl) 4-pyren-1-ylbutanoate Chemical compound C=1C=C(C2=C34)C=CC3=CC=CC4=CC=C2C=1CCCC(=O)ON1C(=O)CCC1=O YBNMDCCMCLUHBL-UHFFFAOYSA-N 0.000 description 1
- 206010070834 Sensitisation Diseases 0.000 description 1
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 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
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- 229910052798 chalcogen Inorganic materials 0.000 description 1
- 150000001787 chalcogens Chemical class 0.000 description 1
- 229910017052 cobalt Inorganic materials 0.000 description 1
- 239000010941 cobalt Substances 0.000 description 1
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 1
- 239000000306 component Substances 0.000 description 1
- 239000002826 coolant Substances 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
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- 238000009776 industrial production Methods 0.000 description 1
- 238000003331 infrared imaging Methods 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 238000009434 installation Methods 0.000 description 1
- 238000005342 ion exchange Methods 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 description 1
- 229910052753 mercury Inorganic materials 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 238000006386 neutralization reaction Methods 0.000 description 1
- 229910001120 nichrome Inorganic materials 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 230000000737 periodic effect Effects 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000003672 processing method Methods 0.000 description 1
- 238000011027 product recovery Methods 0.000 description 1
- 239000012264 purified product Substances 0.000 description 1
- 238000012797 qualification Methods 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 238000006722 reduction reaction Methods 0.000 description 1
- 238000010992 reflux Methods 0.000 description 1
- 229910000058 selane Inorganic materials 0.000 description 1
- 230000008313 sensitization Effects 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 238000013083 solar photovoltaic technology Methods 0.000 description 1
- 238000000638 solvent extraction Methods 0.000 description 1
- 239000004575 stone Substances 0.000 description 1
- 229910052569 sulfide mineral Inorganic materials 0.000 description 1
- LSNNMFCWUKXFEE-UHFFFAOYSA-L sulfite Chemical compound [O-]S([O-])=O LSNNMFCWUKXFEE-UHFFFAOYSA-L 0.000 description 1
- 238000005979 thermal decomposition reaction Methods 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 231100000167 toxic agent Toxicity 0.000 description 1
- 239000003440 toxic substance Substances 0.000 description 1
- 239000002912 waste gas Substances 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
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Abstract
High purity selenium producing apparatus and process are disclosed. The producing apparatus includes one rectifying unit coated with heat insulating layer, one temperature controlling system and one vacuum system comprising one mechanical pump and one diffusion pump. The rectifying unit with vacuum gland in the upper part is divided into one material layer and one product layer communicated mutually. The material layer includes one conical condenser, one umbrella shaped material accepter and one connecting pipe vertically distributed successively; and the product layer is provided with one product kettle connected through the connecting pipe to the material accepter. The rectifying unit in inside multilayer structure is favorable to the separation of selenium from other impurity elements, and has high yield and high product purity.
Description
Technical field
The present invention relates to a kind of production unit and production technique of high-purity selenium.
Background technology
Some compound of metallic selenium and selenium is the semi-conductor of knowing, and has excellent physics-chem characteristic, and extensive and special purposes, selenium are arranged is in the periodic table of elements in the VIA family (chalcogen), and the abundance of selenium in the earth's crust is 9 * 10
-6% exists in the many forms with compound of occurring in nature, is distributed widely in the sulfide mineral, as berzelianite, eukairite etc.High-purity selenium is meant that the content of selenium in the selenium product is 99.999%5N and two kinds of specifications of 99.9999%6N, promptly contain in the product innovation other impurity element always less than 10PPM and 1PPM (10
-6PPM).
In recent years along with the continuous development of light-guide material technology, semiconductor laser technique, semiconductor refrigerating technology, semiconductor light emitting technology, solar-photovoltaic technology, infrared detection technique, functional glass technology, high-purity (5N represents 99.999%, 6N represent 99.9999%) Application Areas of selenium is wide day by day.The world market to demand every year of (5N, 6N) high-purity selenium with the speed increment more than 20%.Along with the continuous development of the national defence top science, the Application Areas of (5N, 6N) high-purity selenium will constantly enlarge thereupon, and the world market imbalance between supply and demand is further aggravation thereupon also, so the high-purity selenium production project has vast market prospect.
High-purity (5N, 6N) selenium is as one of main production raw material of compound semiconductor, and its Application Areas mainly contains:
(1), it is the main raw material of synthetic toner cartridge Photoactive compounds light-guide material, is the core component of making high speed copier, the critical material of duplicating machine sensitization toner cartridge.Synthetic light-guide material is one of main application fields of high-purity selenium.
(2), it is the main raw material of synthetic high power semiconductor lasers spare material (ZnSe).High power semiconductor lasers spare can be used as semiconductor laser cutting Laser Devices, is the core component of semiconductor laser cutting facility.The semiconductor laser cutting technique, energy-conservation with it, the working accuracy height, volume is little, and convenient carrying has become the developing direction of cutting technique.
(3), it can be used as semiconductor refrigeration material Bi2 (Tel-xSb x), semiconductor refrigerating technology has become the main direction of Refrigeration Technique development with its environmental protection, energy-conservation advantage.
(4), it is to be used for one of main raw that synthesizes the solar energy photovoltaic material selenium indium copper (CuInSe2) that has development prospect.The solar-energy photo-voltaic cell of being made by this material belongs to the direct band gap thin film solar, because its material belongs to direct band gap, so it makes the photoelectric conversion rate height (20%) of the solar cell of system; Simultaneously because the solar cell of its making belongs to thin-film solar cells, so the materials consumption of its making solar cell seldom.Film photovoltaic cell has become the main developing direction of solar cell.Because this material is unique material that does not have the light decay effect in all photovoltaic materials, its long service life is so selenium indium copper solar cell is being represented the main developing direction of photovoltaic solar cell material simultaneously.
(5), it is to be used to make infrared optics lens material (as: ZnSe), also available material of infrared window.PbSe, PbSeTe are mainly used in infrared imaging, infrared acquisition, infrared tracking.
(6), it is to make partly to lead luminescent material (as: ZnSe) semiconductor lighting material, the main raw of semi-conductor white light emitting material LED.Semiconductor lighting is energy-conservation, efficient with it, the advantage of long life, environmental protection, has become the developing direction of illumination of future generation.
(7), it can be used as functional glass such as As-Te-Se.Its Application Areas is extensive, and market outlook are wide.
Selenium belongs to dissipated metal, and it is the association component of other non-ferrous metal deposit; Therefore selenium generally is the comprehensive product that reclaims in the non-ferrous metal mineral smelting process.
The method of purification of selenium mainly contains following four kinds at present:
(1) chemical method (or claiming ion exchange method), chemical method is that selenium compound is dissolved in HNO
3In, pass through SO again
2This selenium compound is reduced into simple substance selenium, oxidation, neutralization precipitation and the solvent extraction technology logotype in the lump of the general and selenium of this production technique, will inevitably produce a large amount of waste gas waste water in process of production, thereby cause environmental pollution, and it is little to have production capacity, and quality product is difficult to control, the defective that production cost is high, because the purity of finished product is not high, also must work in coordination with other production technology and just can produce high-purity selenium.
(2) the distillation subliming method generally is used to extract thick selenium, with the condensation under 593K immediately after distillation under the 923K of thick selenium, obtains high-purity selenium and SeO after the repetitive operation
2, again with SeO
2With NH
4OH obtains high-purity selenium through reduction reaction.This production technique need be passed through repetitive operation, and the product after production cost height, normal pressure distill down directly contacts with air, often makes quality product be difficult to guarantee, oxidizing reaction takes place easily once more, must combine with other technology and just can produce high-purity selenium.
(3) Selenium hydride thermal decomposition method is with Se and H
2Be heated to 823-923K and generate H
2Se is by putting in the silica tube that temperature is 1273K H after the purification utensil removal of impurity
2Se resolves into H
2And Se, thereby reach the purpose of purification Se.In this production process, can produce H
2Se, H
2Se is a highly toxic substance, pollutes the environment in case leak, and human body is produced harm, and there is the little shortcoming of production capacity equally in this production technique.
(4) sulphite circulation method, the production process of this production technique is slow, and the rate of recovery is not high.
General existing high-purity selenium purifying technique has long flow path, complex manufacturing, unfavorable factor such as product recovery rate is low, and production capacity is little.Along with the continuous growth of world market to the high-purity selenium demand, the production technology and the technology of high-purity selenium relatively lag behind at present, far can not satisfy the demand of market to high-purity selenium.
Therefore, demand urgently a kind of efficient, environmental protection, the low input, the rectifying production technique of energy-conservation high-purity selenium is to overcome the defective of existing production technique.
Summary of the invention
Based on the deficiencies in the prior art, the object of the invention is to provide the rectifying production technique of a kind of efficient, energy-conservation, safety, environmental protection, the low high-purity selenium that drops into.
Another object of the present invention is the rectifying device that provides simple in structure and be applicable to the large-scale industrial production of high-purity selenium.
In order to achieve the above object, the invention provides a kind of production unit of high-purity selenium, comprise rectifying device, temperature control system and vacuum system, temperature control system is wrapped in outside the rectifying device, and vacuum system is located at the upper strata of rectifying device.Rectifying device is divided into raw material layer and the gas producing formation that is interconnected, and raw material layer comprises condenser, material receiver, raw material still and the pipe connecting that is erect-type distribution in regular turn, and gas producing formation is provided with the product still, and described product still is connected with material receiver by pipe connecting.
In a preferred embodiment of the invention, condenser is tapered, and material receiver is umbrella shape, and raw material layer further comprises the defective material discharge port that communicates with the raw material still.Further be provided with vacuum system on the raw material layer.Rectification process equipment adopts quartz to make.
The present invention also further provides a kind of rectification process of high-purity selenium, and it may further comprise the steps:
Step (1) is broken into raw material selenium less than 10mm earlier;
Step (2) is with the raw material selenium heat fused after the fragmentation;
Step (3) is poured into the raw material selenium after the fusing in the raw material still of rectifying device, adds a cover vacuum cover on rectifying device, the unlatching vacuum system vacuumizes, control product still layer temperature is 250-400 ℃, and raw material still layer temperature is 150-300 ℃, distills production under vacuum state;
Step (4), cooling stops vacuum system, and distillation system venting emptying is taken out product and defective material by outlet for product and defective material discharge port respectively.
Wherein, in described step (3), vacuum degree control is 9 * 10
-2-1 * 10
-3Pa; In step (2), raw material selenium is placed in and carries out heat fused in the quartz crucible.
Compared with prior art, rectifying device of the present invention and production technique have the following advantages:
(1) high yield: adopt erect-type arrangement and tower inside multilayer architecture to combine, easier collection selenium flores helps selenium and other separation of foreign elements, and productive rate and product percent of pass are higher.
(2) high purity: under the enclosed vacuum environment, carry out rectifying on the one hand, avoided surrounding environment to contact, thereby guaranteed the high purity of selenium product with product; This rectification process adopts the type of heating of two sections temperature on the other hand, and adopts two sections accurate temperature controllings, has fundamentally solved raw material section and product section and has heated the lower-boiling impurity that causes after the match in same temperature and be difficult to an isolating difficult problem, thereby guaranteed the purity of product.
(3) energy-conserving and environment-protective: the defective material that produces in the production process can also feed intake through reclaiming again, and defective material is discharged after repeatedly purifying repeatedly again, has guaranteed making full use of of material, has improved the output of selenium greatly.This production technique per-unit production energy consumption only is the 1/2-1/3 of other production technique.
For making the present invention easier to understand, further set forth the specific embodiment of the rectifying production technique of a kind of high-purity selenium of the present invention below in conjunction with accompanying drawing.
Description of drawings
Fig. 1 is the structural representation of the production unit of high-purity selenium of the present invention;
Fig. 2 is the workflow diagram of the rectifying production technique of high-purity selenium of the present invention.
Embodiment
The invention provides a kind of production unit of high-purity selenium, with reference to shown in Figure 1, it comprises rectifying device 100, temperature control system 200 and vacuum system 300, temperature control system 200 is wrapped in outside the rectifying device 100, vacuum system 300 is located at the upper strata of rectifying device 100, makes the temperature in the rectifying device 100 keep accurately constant in process of production by temperature control system 200.
Rectifying device 100 is divided into two-part, and the upper strata is used for the splendid attire raw material, and lower floor is provided with product still 20, is used to collect product.Wherein, the upper strata comprises raw material still 10 and is built in wherein condenser 12, material receiver 14, pipe connecting 16 and defective material discharge port 18, the upper end open of raw material still 10 is sealed by a vacuum gland 101, form vacuum system 300, make whole rectifying device 100 keep vacuum state in working order down by vacuumizing.Condenser 12 is tapered, is placed on the material receiver 14 with standing upside down, and the width of its taper bottom surface equals the internal diameter of raw material still 10.Material receiver 14 is umbrella, back-off is on pipe connecting 16, the product still 20 that connects material receiver 14 and rectifying device 100 lower ends by pipe connecting 16, the product that obtains is derived by the outlet for product 201 of product still 20, defective material discharge port 18 is drawn downwards along the sidewall of raw material still 10, communicate with the external world, defective material is discharged by defective material discharge port 18.
Described temperature control system 200 is divided into heating zone and cooling section, and heating zone comprises last heating zone 221 and the following heating zone 222 that does not wait the temperature field, and upper strata raw material still and lower floor's product still in the corresponding control rectification process process keep certain temperature head.Cooling section 224 is located at the perisporium upper strata of rectifying device 100, is made of the pipeline that is communicated with, and is used to feed water coolant.
Next with reference to shown in Figure 2, set forth the rectification process of high-purity selenium of the present invention:
Step (1) is broken into raw material selenium less than 10mm earlier;
Step (2), then, with the raw material selenium heat fused after the fragmentation;
Step (3) then, is poured into the raw material selenium after the fusing in the raw material still 10 of rectifying device, adds a cover vacuum cover on rectifying device, vacuumizes vacuum tightness: 9 * 10
-2-1 * 10
-3Pa; Control upper strata temperature is 250-400 ℃, and lower floor's temperature is 150-300 ℃, distills under vacuum state;
Step (4), cooling stops vacuum system, and distillation system venting emptying is taken out product and defective material by outlet for product and defective material discharge port respectively.
Wherein, in step (1), raw material selenium can be milled to the particulate state of certain specification with it by agate stone;
In step (2), the raw material selenium after the fragmentation can be put in the quartz crucible and carry out heat fused by electric furnace, in quartz crucible, heat, guaranteed that selenium can not stain by other materials under the condition of high temperature.
In step (3), heating installation can adopt nichrome resistance stove silk, and the pumpdown time is 20-30 minute, 10-20 hour rectifying time.
The rectifying production cycle of the present invention is shorter, is generally 10-20 hour.
The principle of work of the rectification process of high-purity selenium of the present invention is as follows:
The raw material selenium of upper strata raw material still is evaporated to the taper tower head of condenser through after heating under vacuum state, flow in the material receiver of umbrella shape after the selenium steam condensation immediately after the distillation, flow in the product still of lower floor again.Under the condition of the technical parameter of high vacuum and this production technique, according to the difference of the vapour pressure of the vapour pressure of selenium and other element, thereby reached, thereby obtained highly purified selenium product the purpose of selenium with other separation of foreign elements.
The production unit of high-purity selenium of the present invention and production technique are mainly used in the selenium product that production purity is 5N or 6N, it is the selenium of 3N and 4N that raw material can adopt purity, certainly do not limit raw material and degree of purity of production at this yet, based on above-mentioned processing method, can control under given conditions, preparation can obtain required high purity selenium product through multiple cycles, if need to obtain the selenium product of 5N, can adopt the selenium raw material of 3N or 4N to carry out the rectifying preparation, further improve the selenium degree of purity of production as needs, can be invested in the 5N product that generates raw material in the rectifying device once more as next process, thereby obtaining purity is the selenium product of 6N, certainly, for obtaining more highly purified product, generally need multiple cycles production, impurity is subjected to processing parameter control and fewer and feweri, therefore, can produce the selenium product that should need, particularly high-purity selenium product according to demand, break through the technical bottleneck that former high-purity selenium production is confined to 4N selenium, reduced the production cost of high-purity selenium significantly.
Below, embody the superiority of the rectification process of the more traditional high-purity selenium of the present invention by various parameter comparison.One: required energy consumption only is the 1/2-1/3 of other selenium rectifying production technique; Its two: the qualification rate of product reaches more than 95%, and the product percent of pass of other production technique generally has only 60-70%; Its three: particularly for hazardness troublesome impurities such as reducing iron, nickel, lead, cobalt, mercury, zinc, titanium, silver extraordinary effect is arranged, the actual detected data are all less than 0.05ppm in the production, and other production technique can only reach 0.5-1ppm to this class impurity.
Oneself reaches the product innovation specification of quality of our company high-purity 5N that this invention is produced and 6N selenium product innovation.This product uses through users at home and abroad, and reaction is good, all reaches the specification of quality of users at home and abroad.It below is the quality standard of high-purity 5N of our company and 6N selenium product.
5N quality standard unit of our company (ppm)
| Impurity | Cu | Ag | Mg | Sb | Ni | Bi | Hg | In | Fe | Cd | Te | Ga | Al | Ti | Pb |
| Content | 0.2 | 0.2 | 0.5 | 0.5 | 0.2 | 0.5 | 1 | 0.5 | 0.2 | 0.2 | 0.5 | 0.5 | 0.5 | 0.5 | 0.5 |
6N quality standard unit of our company (ppm)
| Impurity | Cu | Ag | Mg | Ni | Bi | In | Fe | Cd | Te | Al | Ti | Pb |
| Content | 0.05 | 0.05 | 0.1 | 0.05 | 0.05 | 0.05 | 0.1 | 0.05 | 0.1 | 0.05 | 0.05 | 0.05 |
Rectifying device of the present invention adopts erect-type arrangement, with respect to the easier collection selenium of horizontal type structure flores, helps selenium and other separation of foreign elements, and productive rate and product percent of pass are higher; In addition, rectifying device adopts tower inside multilayer architecture, condenser be shaped as umbrella shape, the condensation that helps selenium flores in the rectifying is collected and is separated lower-boiling impurity, can adjust and stablize the reflux ratio of controlling in the rectifying more accurately; Material receiver be shaped as taper, the selenium product that helps collecting is drained by outlet for product.
Rectification process of the present invention is operated under the enclosed vacuum environment, has avoided surrounding environment to contact with product, thereby has guaranteed the high purity of selenium product in process of production.The defective material that produces in the production process can also feed intake through reclaiming again, and defective material is discharged after repeatedly extracting repeatedly again, has guaranteed making full use of of material, has improved the output of selenium greatly.In addition, this rectification process adopts the type of heating of two sections temperature, has fundamentally solved raw material section and product section and has heated the lower-boiling impurity that causes after the match in same temperature and be difficult to an isolating difficult problem, thereby guaranteed the purity of product.
Above disclosedly only be the preferred embodiment of the production unit of high-purity selenium of the present invention and production technique, certainly can not limit the present invention's interest field with this, therefore the equivalent variations of being done according to the present patent application claim still belongs to the scope that the present invention is contained.
Claims (10)
1, a kind of production unit of high-purity selenium is characterized in that: comprise rectifying device, temperature control system and vacuum system, thermal insulation layer is wrapped in outside the rectifying device, and the vacuum gland is located at the upper strata of rectifying device.
2. the production unit of a kind of high-purity selenium as claimed in claim 1, it is characterized in that: rectifying device is divided into raw material layer and the gas producing formation that is interconnected.
3. the production unit of a kind of high-purity selenium as claimed in claim 2, it is characterized in that: raw material layer comprises condenser, material receiver, raw material still, pipe connecting and the defective material discharge port that is erect-type distribution in regular turn.
4. the production unit of a kind of high-purity selenium as claimed in claim 3, it is characterized in that: gas producing formation is provided with the product still, and described product still is connected with material receiver by pipe connecting.
5. the production unit of a kind of high-purity selenium as claimed in claim 2, it is characterized in that: temperature control system is divided into two-layer, and raw material layer and gas producing formation in the corresponding control rectifying keep certain temperature head.
6. the production unit of a kind of high-purity selenium as claimed in claim 3, it is characterized in that: described condenser is tapered.
7. the production unit of a kind of high-purity selenium as claimed in claim 3, it is characterized in that: described material receiver is umbrella shape.
8. the production unit of a kind of high-purity selenium as claimed in claim 1 is characterized in that: adopt quartzy as rectification process equipment.
9. the rectification process of a high-purity selenium is characterized in that may further comprise the steps:
Step (1) is broken into raw material selenium less than 10mm earlier;
Step (2) is with the raw material selenium heat fused after the fragmentation;
Step (3) is poured into the raw material selenium after the fusing in the raw material still of rectifying device, adds a cover vacuum cover on rectifying device, the unlatching vacuum system vacuumizes, control product still layer temperature is 250-400 ℃, and raw material still layer temperature is 150-300 ℃, distills under vacuum state;
Step (4), cooling stops vacuum system, and distillation system venting emptying is taken out product and defective material by outlet for product and defective material discharge port respectively.
10. the rectification process of a kind of high-purity selenium as claimed in claim 9, it is characterized in that: in described step (3), vacuum degree control is 9 * 10
-2-1 * 10
-3Pa.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2006101225084A CN100411975C (en) | 2006-09-29 | 2006-09-29 | Producing device of high-purity selenium and producing process |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2006101225084A CN100411975C (en) | 2006-09-29 | 2006-09-29 | Producing device of high-purity selenium and producing process |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1927701A true CN1927701A (en) | 2007-03-14 |
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| CN102706144A (en) * | 2012-05-25 | 2012-10-03 | 吉首大学 | Fractional condensation vacuum furnace |
| CN103172038A (en) * | 2011-12-23 | 2013-06-26 | 广东先导稀材股份有限公司 | Preparation device and method for high purity selenium |
| CN104964941A (en) * | 2015-06-29 | 2015-10-07 | 浙江大学 | Method and separating and collecting device for detecting elemental selenium quickly and quantitatively |
| CN105967152A (en) * | 2016-05-17 | 2016-09-28 | 广东省稀有金属研究所 | Method and device for preparing high-purity oxygen-free selenium granules |
| CN106032270A (en) * | 2015-03-09 | 2016-10-19 | 广东先导稀材股份有限公司 | Preparation method of selenium powder |
| CN106946233A (en) * | 2017-04-18 | 2017-07-14 | 昆明鼎邦科技股份有限公司 | A kind of method of impure selenium material vacuum Refining |
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| CN110482495A (en) * | 2019-07-08 | 2019-11-22 | 昆明理工大学 | A kind of device and method of oxidation-evaporation-carbon thermal reduction purification impure selenium |
| CN110894065A (en) * | 2019-12-18 | 2020-03-20 | 中南大学 | Equipment and method for preparing high-purity tellurium |
| CN111979432A (en) * | 2020-09-03 | 2020-11-24 | 武汉拓材科技有限公司 | Novel process for preparing ultra-high-purity indium by tower plate rectification |
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| US4548800A (en) * | 1982-08-02 | 1985-10-22 | Xerox Corporation | Process for selenium purification |
| CN2755530Y (en) * | 2004-12-03 | 2006-02-01 | 云南铜业技术中心 | Semi-continuous metallurgical furnace with three chamber |
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| CN105967152A (en) * | 2016-05-17 | 2016-09-28 | 广东省稀有金属研究所 | Method and device for preparing high-purity oxygen-free selenium granules |
| CN107032309B (en) * | 2017-04-18 | 2019-03-15 | 昆明鼎邦科技股份有限公司 | A kind of selenium vacuum smelting equipment Special discharging device |
| CN106946233A (en) * | 2017-04-18 | 2017-07-14 | 昆明鼎邦科技股份有限公司 | A kind of method of impure selenium material vacuum Refining |
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| CN110894065A (en) * | 2019-12-18 | 2020-03-20 | 中南大学 | Equipment and method for preparing high-purity tellurium |
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| CN111979432A (en) * | 2020-09-03 | 2020-11-24 | 武汉拓材科技有限公司 | Novel process for preparing ultra-high-purity indium by tower plate rectification |
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