CN115976340A - Device and method for separating antimony from crude arsenic by vacuum distillation - Google Patents
Device and method for separating antimony from crude arsenic by vacuum distillation Download PDFInfo
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- CN115976340A CN115976340A CN202211451262.0A CN202211451262A CN115976340A CN 115976340 A CN115976340 A CN 115976340A CN 202211451262 A CN202211451262 A CN 202211451262A CN 115976340 A CN115976340 A CN 115976340A
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- 229910052787 antimony Inorganic materials 0.000 title claims abstract description 44
- WATWJIUSRGPENY-UHFFFAOYSA-N antimony atom Chemical compound [Sb] WATWJIUSRGPENY-UHFFFAOYSA-N 0.000 title claims abstract description 44
- 238000000034 method Methods 0.000 title claims abstract description 30
- GOLCXWYRSKYTSP-UHFFFAOYSA-N Arsenious Acid Chemical compound O1[As]2O[As]1O2 GOLCXWYRSKYTSP-UHFFFAOYSA-N 0.000 title claims abstract description 26
- 238000005292 vacuum distillation Methods 0.000 title claims abstract description 16
- 229910052785 arsenic Inorganic materials 0.000 claims abstract description 65
- RQNWIZPPADIBDY-UHFFFAOYSA-N arsenic atom Chemical compound [As] RQNWIZPPADIBDY-UHFFFAOYSA-N 0.000 claims abstract description 64
- 238000009833 condensation Methods 0.000 claims abstract description 50
- 230000005494 condensation Effects 0.000 claims abstract description 50
- 238000010438 heat treatment Methods 0.000 claims abstract description 33
- 238000001816 cooling Methods 0.000 claims abstract description 14
- 239000012535 impurity Substances 0.000 claims description 11
- 239000002994 raw material Substances 0.000 claims description 9
- 238000004821 distillation Methods 0.000 claims description 6
- 238000007789 sealing Methods 0.000 claims description 3
- 238000000746 purification Methods 0.000 abstract description 10
- 239000000126 substance Substances 0.000 abstract description 9
- 238000000926 separation method Methods 0.000 abstract description 6
- 229920006395 saturated elastomer Polymers 0.000 abstract description 4
- 238000004519 manufacturing process Methods 0.000 description 11
- 239000000463 material Substances 0.000 description 11
- 239000000203 mixture Substances 0.000 description 8
- 230000001276 controlling effect Effects 0.000 description 7
- 239000000498 cooling water Substances 0.000 description 6
- 229910052751 metal Inorganic materials 0.000 description 6
- 239000002184 metal Substances 0.000 description 6
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 description 5
- 239000007789 gas Substances 0.000 description 5
- 230000000694 effects Effects 0.000 description 4
- 238000011084 recovery Methods 0.000 description 4
- 239000004065 semiconductor Substances 0.000 description 4
- 229910000978 Pb alloy Inorganic materials 0.000 description 3
- HUEBVZADHUOMHL-UHFFFAOYSA-N [As].[Pb] Chemical compound [As].[Pb] HUEBVZADHUOMHL-UHFFFAOYSA-N 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
- 239000007859 condensation product Substances 0.000 description 3
- 238000011161 development Methods 0.000 description 3
- 238000009616 inductively coupled plasma Methods 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- 229910000881 Cu alloy Inorganic materials 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 2
- 239000000956 alloy Substances 0.000 description 2
- JEMGLEPMXOIVNS-UHFFFAOYSA-N arsenic copper Chemical compound [Cu].[As] JEMGLEPMXOIVNS-UHFFFAOYSA-N 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 230000001105 regulatory effect Effects 0.000 description 2
- JBRZTFJDHDCESZ-UHFFFAOYSA-N AsGa Chemical compound [As]#[Ga] JBRZTFJDHDCESZ-UHFFFAOYSA-N 0.000 description 1
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 229910001218 Gallium arsenide Inorganic materials 0.000 description 1
- 229910000530 Gallium indium arsenide Inorganic materials 0.000 description 1
- 238000012356 Product development Methods 0.000 description 1
- 238000003723 Smelting Methods 0.000 description 1
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 230000001093 anti-cancer Effects 0.000 description 1
- FAWGZAFXDJGWBB-UHFFFAOYSA-N antimony(3+) Chemical compound [Sb+3] FAWGZAFXDJGWBB-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 238000005660 chlorination reaction Methods 0.000 description 1
- 239000000460 chlorine Substances 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
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- 229910052732 germanium Inorganic materials 0.000 description 1
- GNPVGFCGXDBREM-UHFFFAOYSA-N germanium atom Chemical compound [Ge] GNPVGFCGXDBREM-UHFFFAOYSA-N 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 239000004009 herbicide Substances 0.000 description 1
- RPQDHPTXJYYUPQ-UHFFFAOYSA-N indium arsenide Chemical compound [In]#[As] RPQDHPTXJYYUPQ-UHFFFAOYSA-N 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 239000002917 insecticide Substances 0.000 description 1
- 239000011133 lead Substances 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 238000005272 metallurgy Methods 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 238000012856 packing Methods 0.000 description 1
- 239000000049 pigment Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 239000003755 preservative agent Substances 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 239000011819 refractory material Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 239000002893 slag Substances 0.000 description 1
- 239000000779 smoke Substances 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- XPDICGYEJXYUDW-UHFFFAOYSA-N tetraarsenic tetrasulfide Chemical compound S1[As]2S[As]3[As]1S[As]2S3 XPDICGYEJXYUDW-UHFFFAOYSA-N 0.000 description 1
- 239000011135 tin Substances 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 239000002912 waste gas Substances 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
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- 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
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Abstract
The invention discloses a device and a method for separating antimony from crude arsenic by vacuum distillation, and belongs to the technical field of crude arsenic purification. The device provided by the invention comprises a reactor cover, a temperature measuring device, a cooling device, a condensing tower, a heating device, a connecting flange, a vacuum tank body, a charging crucible, a vacuumizing device and a control system. The invention also provides a method for separating antimony from crude arsenic by vacuum distillation by using the device, which adopts a technical route of realizing vacuum distillation fractional condensation by using an adjustable multistage condensation tower, wherein the inter-stage distance can be adjusted by changing the position of a nut, the volatilized antimony vapor and part of arsenic vapor are condensed on a condensing sheet with higher temperature by utilizing the difference between the saturated vapor pressure and the condensation temperature of arsenic, antimony vapor and other low-boiling-point substances and the position of a condensing sheet is adjusted, the low-boiling-point substances are condensed on a collecting device at the upper part of a furnace body, and arsenic with lower antimony content is collected by the condensing sheet in a medium-low temperature region, so that the efficient separation of the arsenic and the antimony is realized.
Description
Technical Field
The invention relates to the technical field of crude arsenic purification; in particular to a device and a method for separating antimony from crude arsenic by vacuum distillation.
Background
Arsenic has excellent physical and chemical properties, and can improve the properties of metal materials when used as a metal additive; arsenic can be combined with a series of metals to form alloy materials, such as arsenic-lead alloy and arsenic-copper alloy, wherein the arsenic-lead alloy is mainly applied to the production of lead storage batteries and military lead bombs, and the arsenic-copper alloy is mainly applied to the production of supporting screw rods of train combustion chambers and parts in high-temperature reducing atmosphere. The semiconductor material is one of the most important applications of arsenic, is mainly applied to synthesis of gallium arsenide, indium arsenide and the like, and can be used as a doping element of germanium and silicon of the semiconductor material, and the conductivity of the semiconductor is greatly improved after the arsenic is doped. As a core material of the second generation semiconductor, arsenic has become a key material for supporting high-tech development and new product development. Arsenic also has medical value, and researches prove that arsenic plays an important role in the anticancer neighborhood. Arsenic is also an important raw material for preparing materials such as herbicides, insecticides, preservatives, pigments and the like. With the development of the arsenic industry, arsenic plays an increasingly important role in the fields of metallurgy, materials, chemical industry, medical treatment and the like.
Most of arsenic is associated in non-ferrous metal ores such as tin, lead, zinc, copper, gold and the like, an independent arsenic deposit is few, the recovery amount of mineral resources in China far exceeds the current arsenic demand, so the independent arsenic ore is not mined at present, arsenic is mainly extracted and utilized from high-arsenic smoke dust and arsenic sulfide slag containing high arsenic in non-ferrous smelting secondary resources, and the produced industrial arsenic is low in grade and difficult to sell and low in price due to the fact that raw material components are complex, particularly the arsenic enters a finished product together with antimony which is a main group impurity in the production process. The high-grade arsenic is short in supply and demand and high in price, and the effective equipment and method for separating antimony from crude arsenic are developed, so that the development of harmless and recycling treatment technologies of arsenic-containing materials is promoted, and good social and economic benefits are created for producing high-grade arsenic.
The existing methods for purifying arsenic and separating antimony mainly comprise a chemical purification method and a physical purification method. The chemical purification method comprises the steps of chloridizing, rectifying and purifying arsenic, and then reducing by hydrogen to obtain high-grade arsenic. CN103184354A discloses a preparation method of high-purity arsenic, which comprises the steps of vacuum distillation, chlorine chlorination, rectification and purification and hydrogen reduction of crude arsenic to obtain the high-purity arsenic. The method is the mainstream method for preparing high-grade arsenic, but has the disadvantages of long process, high requirement on equipment, safety risk in the production process, high production cost and unstable product quality. The physical purification method is a method for generating a compound difficult to volatilize by adding alloy and impurity elements according to the difference of saturated vapor pressure of each element in crude arsenic at different temperatures, wherein the arsenic element with high saturated vapor pressure is preferentially volatilized and condensed under the conditions of certain temperature and system pressure, so that the arsenic element is separated from other impurity elements. CN101054168A discloses a production method of high-purity arsenic, which comprises the steps of firstly heating arsenic and lead in a crucible according to the proportion of 1.5-4 to prepare arsenic-lead alloy, placing the crucible in a vacuum tank, connecting the crucible with a conical condenser, vacuumizing and heating, condensing arsenic on the condenser, and keeping impurity elements in residues to realize separation to obtain high-grade arsenic. The method has stable quality and low cost, but the labor intensity in the production process is high. CN112226633A discloses a device capable of reducing antimony content in industrial arsenic and a production method thereof, wherein the device comprises a heating furnace, a vacuum tank body, a charging crucible, a refractory material layer, a conical condenser, a condensation diversion sieve plate and a vacuum system; the device structure is comparatively simple, and the processing procedure is shorter, but the process is more difficult to control, and is required to the raw materials higher.
Disclosure of Invention
Aiming at the existing problems of crude arsenic purification, the invention provides a device for separating antimony from crude arsenic by vacuum distillation; a certain temperature gradient is formed in the device, and according to the difference between the saturated vapor pressure and the condensation temperature, arsenic and antimony vapors are condensed at different positions through fractional condensation, so that high-efficiency separation is realized; the invention is realized by the following technical scheme:
a device for separating antimony from crude arsenic by vacuum distillation comprises a reactor cover 1, a temperature measuring device 2, a cooling device 3, a condensing tower 4, a heating device 5, a connecting flange 6, a vacuum tank body 7, a charging crucible 8, a vacuumizing device 9 and a control system 10; the feeding crucible 8 and the heating device 5 are arranged at the bottom of the vacuum tank body 7, the heating device 5 heats the periphery of the feeding crucible 8, the multistage condensation tower 4 is arranged above the feeding crucible 8 and the heating device 5, a plurality of condensation sheets and a central screw rod are arranged in the multistage condensation tower 4, the condensation sheets are fixed on the central screw rod through nuts, the positions of the condensation sheets are adjusted through adjusting nuts, airflow holes are formed in the condensation sheets, the airflow holes in two adjacent condensation sheets are oppositely arranged, and the fixed temperature measuring device 2 is arranged on the condensation sheets; a reactor cover 1 is arranged above the condensing tower 4, the reactor cover 1 is connected with a vacuumizing device 9, the vacuumizing device 9 is connected with a vacuum tank body through a flange, a cooling device 3 is arranged on the reactor cover 1, and low-boiling-point impurities and tail gas are collected on the reactor cover; the entire apparatus is connected to the control system 10.
The condensing tower 4 is cylindrical, and the condensing sheet is fixed through a gasket.
The condensing tower 4 realizes multi-stage condensation by changing the number of condensing sheets, thereby achieving the purpose of controllable and adjustable condensing stage; the positions of nuts and washers for fixing the condensing sheet are changed, so that the stage spacing is accurately controllable, and the aim of relatively accurately regulating and controlling the stage spacing according to the desired experimental effect is fulfilled; through changing the position of nut and packing ring, make the condensation piece remove on the screw rod, realize that the condensation piece relative heating surface height at different levels is accurate controllable, reach the purpose that the experiment effect that the condensation temperature zone can reach as will carries out accurate regulation and control relatively.
Preferably, the vacuum tank 7 and the heating device 5 on one side of the charging crucible 8 are provided with sealing doors to facilitate taking out and putting in the charging crucible 8.
Preferably, the height of the condensation tower 4 is 26.0cm, the thickness of the condensation sheet is 5mm, the thickness of the nut is 10.5mm, and the thickness of the gasket is 2.5mm.
Preferably, the raw materials are added into a charging crucible 8 in a vacuum tank body 7, a vacuumizing device 9 and a cooling device 3 are started, vapor is condensed in a condensing tower 4, the condensing temperature zone is fully covered from the set temperature to 80 ℃, volatilized antimony vapor and part of arsenic vapor are condensed on a condensing disc with higher temperature by changing the stage number, the position and the distance of condensing sheets, and low-boiling-point impurities and tail gas are collected on a reactor cover at the upper part of a furnace body; arsenic with low antimony content is collected in a condensing disc in a medium-low temperature zone.
Preferably, the raw material of the invention is crude arsenic with 0.5-2% of antimony and 96-98% of purity;
preferably, the pressure in the vacuum tank 7 is 1-10000 Pa, the distillation temperature is 400-650 ℃, and the distillation time is 1-7 h.
The invention has the beneficial effects that:
(1) The production process of the method does not generate any arsenic-containing waste gas and waste water, and is safe and pollution-free; the furnace has reasonable structure, the charging crucible and the heating device of the device are arranged in the vacuum tank, the heat transfer efficiency is high, the crude arsenic is melted quickly, the production efficiency is greatly improved, and the production cost is reduced; meanwhile, the external heating mode of the traditional vacuum furnace is changed, and only the periphery of the charging crucible is heated, so that the heating efficiency is improved, and the internal space is sufficient.
(2) The device can directly take out the charging crucible, and solves the problem that the traditional vacuum furnace is difficult to take and discharge materials; the top is provided with a cooling device 3, the temperature of the reactor cover can be controlled to be lower than 80 ℃, and impurities with low boiling point and tail gas are collected on the reactor cover.
(3) The condensation area of the device is a multi-stage condensation tower, and multi-stage condensation can be realized by adjusting the number of condensation sheets; the accurate control of the inter-stage distance can be realized by adjusting the distance between the condensing sheets; the position of the condensing sheet on the central screw rod can be adjusted to realize the control of a condensing temperature zone; the three components are cooperatively regulated, so that the requirements of different stages, different strokes and different temperature areas of the mixed steam in the vacuum distillation process are met, and the fine regulation and control of the separation effect are easy to realize; the condensing tower is cylindrical, condensing steam cannot volatilize to the vacuum furnace wall, and cleaning is convenient.
(4) The top of the device is provided with the vacuumizing device, so that double control of air pressure and temperature in the vacuum furnace is realized, and the control of condensation conditions is better realized.
(5) The method has the advantages of short process flow, high product quality, good separation effect of impurity antimony element, simple required equipment, low purification cost, high recovery rate and safe and friendly operation environment, and crude arsenic is subjected to vacuum distillation, fractional condensation and vacuum gasification, separation and purification to obtain arsenic with antimony content of not more than 0.04%.
(6) The method has wide raw material adaptability and wide operable conditions, and can find the raw materials with different arsenic and antimony contents and the optimal condensation temperature areas under different conditions.
Drawings
FIG. 1 is a schematic view of the apparatus of the present invention.
Fig. 2 is a schematic structural view of the condensation plate according to the present invention.
Fig. 3 is a schematic connection diagram of the condensation plate according to the present invention.
In the figure: 1-a reactor cover, 2-a temperature measuring device, 3-a cooling device, 4-a condensing tower, 5-a heating device, 6-a connecting flange, 7-a vacuum tank body, 8-a charging crucible and 9-a vacuumizing device; 10-control system.
Detailed Description
The invention will be further described with reference to the drawings and the following detailed description, without limiting the scope of the invention thereto.
Example 1
A device for separating antimony from crude arsenic by vacuum distillation comprises a reactor cover 1, a temperature measuring device 2, a cooling device 3, a condensing tower 4, a heating device 5, a connecting flange 6, a vacuum tank body 7, a charging crucible 8, a vacuumizing device 9 and a control system 10; the charging crucible 8 and the heating device 5 are arranged at the bottom of the vacuum tank body 7, and the heating device 5 heats the periphery of the charging crucible 8, so that the heating efficiency is improved, and the phenomenon that the traditional equipment heats the whole furnace body to cause more heat loss is avoided; a condensing tower 4 is arranged above a charging crucible 8 and a heating device 5, the condensing tower 4 is cylindrical and has the height of 26.0cm, a central screw rod is arranged in the condensing tower 4, condensing sheets are sleeved on the central screw rod, two sides of the condensing sheets are fixed by nuts or gaskets, airflow holes are formed in the condensing sheets, the airflow holes of two adjacent condensing sheets are oppositely arranged, and a fixed temperature measuring device 2 is arranged outside the condensing tower 4; the travel of the mixed steam in the condensation area is determined by the number of the condensation sheets, and the temperature and the distance of each stage of condensation area are determined by the positions of the condensation sheets and are fixed by nuts and gaskets. The mixed vapor is condensed in the condensing tower, the coverage of a condensing temperature zone is wide, the condensing temperature gradient is obvious, the condensing area is flexible and controllable, and the collected materials can more truly reflect the condensing conditions corresponding to the composition of a condensing phase at the position; a reactor cover 1 is arranged above the condensing tower 4, the reactor cover 1 is connected with a vacuumizing device 9, the vacuumizing device 9 is connected with a vacuum tank body through a flange, a cooling device 3 is arranged on the reactor cover 1, and low-boiling-point impurities and tail gas are collected on the reactor cover; the whole device is connected with a control system 10; and sealing doors are arranged on the vacuum tank body 7 and the heating device 5 on one side of the charging crucible 8, so that the charging crucible 8 can be conveniently taken out and put in.
Example 2
Treating 300g of massive crude arsenic containing 96.88% of arsenic and 0.32% of antimony to be in a small block shape with the diameter of less than 1cm, placing the massive crude arsenic into a charging crucible 8, placing the charging crucible 8 into a vacuum tank body 7 with a heating device 5, placing a condensing tower 4 on the upper part of the charging crucible 8, arranging a condensing sheet in the condensing tower every 4.7cm and fixing the condensing sheet to form 5 equidistant condensing sections, installing a reactor cover 1 after the condensing tower 4 is installed, connecting a vacuumizing device 9, controlling the pressure to be 1Pa, controlling the distillation temperature to be 420-470 ℃, distilling for 3 hours, raising the temperature after the pressure is stable, and simultaneously opening a cooling water switch, wherein the temperature raising rate is 10 ℃/min.
In the heating process, arsenic and antimony in the charging crucible 8 are evaporated to form steam, the steam passes through the condensing tower 4, the volatilized antimony steam and part of arsenic steam are condensed on a condensing sheet with higher temperature, low-boiling-point substances are condensed on a collecting device at the upper part of the furnace body, arsenic with lower antimony content is obtained by collecting on a condensing sheet in a medium-low temperature region, and a condensation product is mainly concentrated between 170-80 ℃; and (3) cooling to below 100 ℃ after the reaction is finished, closing the cooling water, stopping the pump, and collecting the materials. In the experimental process, the condensation temperature zones are 352.8 ℃ in the I zone, 318.7 ℃ in the II zone, 220 ℃ in the III zone, 169.9 ℃ in the IV zone and 134.4 ℃ in the V zone.
51.2g of the first zone, 11.4g of the second zone, 19.4g of the third zone, 135.7g of the fourth zone, 53.3g of the fifth zone, 23.7g of the reactor cover and 0.9g of the crucible are collected, the volatility reaches 98.23 percent, and the recovery rate reaches 69.43 percent; the obtained arsenic is detected by an inductively coupled plasma mass spectrometer (ICP-MS) according to the national non-ferrous metal industry standard TS/T68-2014, and the arsenic purity is more than 99 percent and the antimony content is 0.19 percent.
Example 3
Treating 300g of massive crude arsenic containing 96.72 percent of arsenic and 0.81 percent of antimony to be in a small block shape with the diameter of less than 1cm, putting the small block into a charging crucible 8, putting the charging crucible 8 into a vacuum tank body 7 with a heating device 5, putting a condensing tower 4 on the upper part of the charging crucible 8, arranging a condensing sheet in the condensing tower every 4.7cm and fixing the condensing sheet to form 5 equidistant condensing areas which just correspond to temperature measuring points, installing a reactor cover 1 after the condensing tower 4 is installed, connecting a vacuumizing device 9, controlling the pressure to be 5000Pa, controlling the distillation temperature to be 480-520 ℃, distilling for 6h, heating after the pressure is stable, wherein the heating rate is 10 ℃/min, and simultaneously opening a cooling water switch.
In the heating process, the arsenic and antimony in the charging crucible 8 are evaporated to form steam, the steam passes through the condensing tower 4, the volatilized antimony steam and part of arsenic steam are condensed on a condensing sheet with higher temperature, low-boiling-point substances are condensed on a collecting device on the upper part of the furnace body, arsenic with lower antimony content is collected by the condensing sheet in a middle-low temperature region, and a condensation product is mainly concentrated between 230 ℃ and 80 ℃; and (3) cooling to below 100 ℃ after the reaction is finished, closing the cooling water, stopping the pump, and collecting the materials. In the experimental process, the condensation temperature zone corresponding to each condensation sheet is 432.9 ℃ in the I zone, 391.0 ℃ in the II zone, 278.2 ℃ in the III zone, 229.5 ℃ in the IV zone and 174.1 ℃ in the V zone.
Collecting 0.7g in a region I, 5.7g in a region II, 17g in a region III, 71.2g in a region IV, 130.3g in a region V, 66.5g in a reactor cover and 0.5g in a crucible, wherein the volatility reaches 97.13 percent, and the yield reaches 72.83 percent; the obtained arsenic is detected by an inductively coupled plasma mass spectrometer (ICP-MS) according to the national non-ferrous metal industry standard TS/T68-2014, and the arsenic purity is more than 99 percent and the antimony content is 0.04 percent.
Example 4
Treating 300g of massive crude arsenic containing 96.12% of arsenic and 1.81% of antimony to form small blocks with the diameter of less than 1cm, placing the small blocks into a charging crucible 8, placing the charging crucible 8 into a vacuum tank body 7 with a heating device 5, placing a condensing tower 4 on the upper part of the charging crucible 8, arranging a condensing sheet in the condensing tower every 4.7cm and fixing to form 5 equidistant condensing areas, corresponding to a temperature measuring point, installing a reactor cover 1 after the condensing tower 4 is installed, connecting a vacuumizing device 9, introducing CO gas, controlling the pressure to be 10000Pa, controlling the distillation temperature to be 580-620 ℃, distilling for 7h, raising the temperature after the pressure is stable, wherein the temperature raising rate is 10 ℃/min, and simultaneously opening a cooling water switch.
In the heating process, the arsenic and antimony in the charging crucible 8 are evaporated to form steam, the steam passes through the condensing tower 4, the volatilized antimony steam and part of arsenic steam are condensed on a condensing sheet with higher temperature, low-boiling-point substances are condensed on a collecting device on the upper part of the furnace body, arsenic with lower antimony content is obtained by collecting on a condensing sheet in a medium-low temperature region, and a condensation product is mainly concentrated between 480-310 ℃ temperature regions; cooling to below 100 ℃ after the reaction is finished, closing the cooling water, stopping the pump, and collecting the materials; in the experimental process, the condensation temperature zone corresponding to each condensation sheet is 484.8 ℃ in the I zone, 436.7 ℃ in the II zone, 314.6 ℃ in the III zone, 236.1 ℃ in the IV zone and 173.6 ℃ in the V zone.
32.8g of the mixture is collected in a region I, 184.8g of the mixture is collected in a region II, 22.5g of the mixture is collected in a region III, 1.2g of the mixture is collected in a region IV, 0.9g of the mixture is collected in a region V, 35.4g of the mixture is collected in a reactor cover, 1.6g of the mixture is collected in a crucible, the volatility reaches 99.47 percent, and the recovery rate is 70.10 percent; the obtained arsenic is detected by an inductively coupled plasma mass spectrometer (ICP-MS) according to the national non-ferrous metal industry standard TS/T68-2014, and the arsenic purity is more than 99 percent and the antimony content is 0.14 percent.
Claims (7)
1. An apparatus for separating antimony from crude arsenic by vacuum distillation, which is characterized in that: the device comprises a reactor cover (1), a temperature measuring device (2), a cooling device (3), a condensing tower (4), a heating device (5), a connecting flange (6), a vacuum tank body (7), a charging crucible (8), a vacuumizing device (9) and a control system (10);
the feeding crucible (8) and the heating device (5) are arranged at the bottom of the vacuum tank body (7), the heating device (5) heats the feeding crucible (8) all around, a multi-stage condensation tower (4) is arranged above the feeding crucible (8) and the heating device (5), a plurality of condensation sheets and a central screw rod are arranged in the multi-stage condensation tower (4), the condensation sheets are fixed on the central screw rod through nuts, the positions of the condensation sheets are adjusted through adjusting nuts, airflow holes are formed in the condensation sheets, the airflow holes in two adjacent condensation sheets are arranged oppositely, and a fixed temperature measuring device (2) is arranged on each condensation sheet;
a reactor cover (1) is arranged above the condenser tower (4), the reactor cover (1) is connected with a vacuumizing device (9), the vacuumizing device (9) is connected with a vacuum tank body through a flange, a cooling device (3) is arranged on the reactor cover (1), and low-boiling-point impurities and tail gas are collected on the reactor cover; the whole device is connected with a control system (10).
2. The apparatus for separating antimony from crude arsenic by vacuum distillation according to claim 1, wherein: and sealing doors are arranged on the vacuum tank body (7) and the heating device (5) on one side of the charging crucible (8) so as to be convenient for taking out and putting in the charging crucible (8).
3. The apparatus for separating antimony from crude arsenic by vacuum distillation according to claim 1, wherein: the multistage condensation tower (4) is cylindrical, the condensation sheets are fixed through gaskets, and the distance between the condensation sheets is increased by increasing the number of the gaskets.
4. A method for separating antimony from crude arsenic by vacuum distillation using the apparatus of claims 1 to 3, wherein: adding raw materials into a charging crucible (8) in a vacuum tank body (7), starting a vacuumizing device (9) and a cooling device (3), condensing generated steam in a condensing tower (4), controlling the number and the positions of condensing sheets, the inter-stage distance and the condensing temperature region from a set temperature to 80 ℃, condensing volatilized antimony steam and part of arsenic steam on the condensing sheets with higher temperature, and collecting low-boiling-point impurities and tail gas on a reactor cover at the upper part of a furnace body; arsenic with low antimony content is obtained by collecting in a medium-low temperature zone condensation sheet.
5. The method of claim 4, wherein: the raw material is crude arsenic with the antimony content of 0.5-2% and the purity of 96-98%.
6. The method of claim 4, further comprising: the internal pressure of the vacuum tank body (7) is 1 to 10000Pa, the distillation temperature is 400 to 650 ℃, and the time is 1 to 7h.
7. The method of claim 4, further comprising: the temperature of the reactor cover (1) is lower than 80 ℃.
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| US20060005665A1 (en) * | 2002-10-17 | 2006-01-12 | Beijing Goldtech Co., Ltd. | Process for extracting gold in arsenic-containing concentrate of gold and the equipment thereof |
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| US20060005665A1 (en) * | 2002-10-17 | 2006-01-12 | Beijing Goldtech Co., Ltd. | Process for extracting gold in arsenic-containing concentrate of gold and the equipment thereof |
| US20190284658A1 (en) * | 2018-03-13 | 2019-09-19 | Kunming University Of Science And Technology | Device for fractional condensation of arsenic lead vapor mixture and application method thereof |
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