CN103253703A - Preparation method and equipment of high-purity arsenic oxide - Google Patents
Preparation method and equipment of high-purity arsenic oxide Download PDFInfo
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- CN103253703A CN103253703A CN2013102224587A CN201310222458A CN103253703A CN 103253703 A CN103253703 A CN 103253703A CN 2013102224587 A CN2013102224587 A CN 2013102224587A CN 201310222458 A CN201310222458 A CN 201310222458A CN 103253703 A CN103253703 A CN 103253703A
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Abstract
The invention discloses a preparation method and equipment of a high-purity arsenic oxide, and particularly discloses a method and equipment for obtaining a high-purity arsenic oxide through normal-pressure distillation and purification of arsenic oxide based on a principle of removing high-boiling point oxides according to the difference in steam pressures of the oxides. The equipment comprises a distillation box, a distillation framework, a framework flange, a sealing door, a channel and a material box, wherein the distillation box is a rectangular box body and is embedded in the distillation framework; the distillation framework is a vertically-placed rectangular framework, and a framework flange is arranged at the outer edge; the sealing door is fixed behind the framework flange; a hole is formed in the sealing door in a position corresponding to the distillation box at the top layer and is welded together with the channel; the channel is in an L-shaped tubular structure; and another place opens downward and is connected with the material box. The equipment disclosed by the invention is simple and convenient to use and easy to operate, has a short preparation flow, can be used for quickly and effectively preparing high-purity arsenic, and creates a new way of producing high-purity simple-substance arsenic while ensuring stable quality and high safety and avoiding environmental pollution.
Description
Technical field
The present invention relates to a kind of difference according to the oxide compound vapour pressure and remove processing method and the equipment of high boiling point oxide compound, be specifically related to the arsenic oxide arsenoxide air distillation and purify and obtain processing method and the equipment of high-purity mangesium oxide arsenic.
Background technology
The purification of arsenic oxide arsenoxide generally is to purify by vacuum distilling, its deficiency has two aspects, on the one hand because the vapour pressure of each impurity composition of oxide compound and the size of vacuum tightness have direct relation, trim point between vacuum tightness and the temperature is difficult to remain balance in practice, thereby cause the arsenic oxide arsenoxide purity instability that obtains, the vacuum tank volume of second aspect vacuum distilling is all smaller, a charging capacity is about 100kg, it is frequent to take on the material number of times, labour intensity is big, produces product quality in batches and is difficult to control; In the classical technology chlorination of high purity elemental arsenic rectifying reducing process, owing to use chlorine, in rectifying, produce a large amount of still liquid, in the arsenic trichloride reduction, produce hydrochloric acid gas, safety in production and environmental protection are difficult to be effectively controlled in the production; Arsenical lead nitrogen atmosphere sublimation process, plumbous purity determines the purity of final elemental arsenic quality, it is harmful to produce plumbous steam simultaneously in synthetic, quality is difficult to be effectively controlled, and developing a kind of high-purity mangesium oxide arsenic production process route and equipment safe, pollution-free, stay in grade is purpose of the present invention.
Summary of the invention
Technical problem solved by the invention is to provide a kind of preparation technology and equipment of high-purity mangesium oxide arsenic, to solve the shortcoming in the above-mentioned background technology.
Technical problem solved by the invention realizes by the following technical solutions:
The preparation equipment of high-purity mangesium oxide arsenic, comprise the arsenic oxide arsenoxide distilling furnace, described arsenic oxide arsenoxide distilling furnace comprises the distillation case, the distillation framework, the framework flange, hermatic door, passage and hopper, described distillation case is rectangular box, every distilling furnace is provided with 4 ~ 10 layers of distillation case, horizontal positioned is vertically arranged, evenly be entrenched on the distillation framework, described distillation framework is the rectangular frame of vertically placing, outer rim is provided with the framework flange, fixedly there is hermatic door the back of described framework flange, and the hermatic door size is consistent with framework flange outer rim size, distills the corresponding position of case with the superiors and offer mouth on described hermatic door, with channel welds together, described passage is L type structure, and Open Side Down at another place, is connected with hopper.
Described distillation case is long 1500 ~ 5000mm, wide 300 ~ 1000mm, and the rectangular box of high 50 ~ 200mm, an end of distillation case is done plug with the plate of long 300 ~ 1000mm, wide 50 ~ 200mm, at the ventpipe of diameter a 10 ~ 16mm of plug welding.
Described distillation framework is long 1400 ~ 3200mm, wide 300 ~ 1000mm, the rectangle frame of high 100 ~ 300mm, select long 1400 ~ 3200mm, arbitrary of wide 300 ~ 1000mm is with long 100 ~ 200mm, wide 300 ~ 1000 plate, 5 ~ 8 be evenly distributed on above, and make the long 300 ~ 1000mm of section of the vacancy space that stays and rectangular parallelepiped, wide 50 ~ 200mm unanimity.
Described framework flange is the rectangular frame structure, and interior rectangle is consistent with distillation framework outer rim size, and the size of outer rectangle is than the long 150 ~ 350mm of each length of side of interior rectangle.
The opening part of described distillation case is welded on the place, vacancy space of distillation framework, a distillation of each vacancy space welding case, it is parallel and vertical with the distillation framework up and down that each distills case, is welded with some pillar stiffeners in the both sides of distillation case, and the relative position of assurance distillation case maintains static and shakes.
In described distillation case, be placed with long 280 ~ 980mm, wide 300 ~ 600mm, the charging tray of high 40 ~ 160mm is put 4 ~ 8 charging trays in every layer of distillation case.
Described hopper is circular or square, and its volume size is relevant with the number of plies of distillation case, and perhaps according to distiller charging capacity decision at full capacity, namely the charging capacity of distilling furnace is 300 ~ 3000kg, and the size of hopper is 0.3 ~ 2 cubic metre.
Be provided with hot-plate between described adjacent layers distillation case, the length of described hot-plate is wide consistent with the distillation case, hot-plate wide for distilling 1/15 ~ 1/6 of case length, the fused salt pipe that to be evenly distributed 5 ~ 8 diameters on every layer of hot-plate be 40 ~ 100mm.
Described fused salt pipe coupling volume is 6 ~ 20m
3The fused salt groove, the fused salt groove is connected with the fused salt heating boiler by pump for liquid salts, the fused salt that pumps from the fused salt groove flows in the fused salt pipe of distilling furnace interlayer after the heating boiler heating, the fused salt of distilling furnace follows down the principle that outes, fused salt enters from orlop, flow out from the superiors, the fused salt that the superiors flow out is back to the fused salt groove, the fused salt that reaches the technological temperature requirement is flowed in the fused salt Guan Licheng of distilling furnace interlayer S type, height size according to distiller, select supporting pump for use, guarantee that into the salt temperature is controlled in 1 ~ 2 ℃ of scope with the difference that goes out the salt temperature; Each fused salt groove is joined 2 ~ 4 pump for liquid salts, and every pump is joined the fused salt heating boiler of 50 ~ 300kw power, and each boiler makes the fused salt flow that flows to each arsenic oxide arsenoxide distilling furnace even for 1 ~ 3 arsenic oxide arsenoxide distilling furnace with valve.
In the present invention, described high-purity mangesium oxide arsenic distilling furnace each several part all adopts titanium or aluminum to form fully.
Based on the high-purity mangesium oxide arsenic distilling furnace of said structure, the production technique of high-purity mangesium oxide arsenic realizes by following steps:
(1) according to the charging tray quantity of every distilling furnace, through no sulphuring treatment and through the charging tray of packing into except the arsenic oxide arsenoxide evenly distribute behind selenium, the boron;
(2) charged charging tray is put into the casing of every layer of distilling furnace of distilling furnace, dish with coil between together adjacent, until the interlayer distilling furnace casing of all charging trays all being put into distilling furnace;
(3) put anti-200 ~ 600 ℃ elevated-temperature seal pad in framework flange edge, as alumina high temperature fibre packing etc.; Shut hermatic door, tighten the bolt between framework flange and the hermatic door;
(4) aerating oxygen is stopped leakage in the roof, and the jar bubble smoothness that oxygen flow 1 ~ 3L tail gas connects is the intensification of normally can switching on;
(5) hot-plate of heating heats up, and design temperature is certain temperature value between 140 ~ 650 ℃, and before the heating hot-plate heated up, the temperature of molten salt of fused salt groove was warming up to 200 ~ 400 ℃ in advance, when temperature of heating plate is raised to design temperature, and equilibrium temperature 1 ~ 10 hour;
(6) after hot-plate is warmed up to design temperature and temperature equilibrium time and arrives, open the pump for liquid salts of this arsenic oxide arsenoxide distilling furnace correspondence, make fused salt flow to fused salt pipe in the arsenic oxide arsenoxide distilling furnace, set the temperature of fused salt heating boiler simultaneously at 300 ~ 650 ℃;
(7) after pump for liquid salts is started working, go out the salt temperature head between each distilling furnace of every pump for liquid salts correspondence of 1 ~ 2 hour observed and recorded in every interval, that regulates each distilling furnace correspondence advances salt and salt-supplying valve, makes each corresponding arsenic oxide arsenoxide distilling furnace temperature uniformity of every pump for liquid salts (perhaps every fused salt boiler); Then need not to adjust salt and salt-supplying valve as the corresponding arsenic oxide arsenoxide distilling furnace of pump for liquid salts, only need advancing salt and salt-supplying valve maximum the getting final product of performing fighting;
(8) after the temperature of molten salt of fused salt boiler arrives and sets technological temperature, continuously insulation remaining amount of material in distilling furnace accounts for 10% of the total amount that feeds intake ~ 40% o'clock, close fused salt boiler power supply earlier after 10 ~ 60 minutes, close the pump for liquid salts power supply again, the salt valve that advances of an arsenic oxide arsenoxide distilling furnace correspondence is reached maximum, the interior ducted fused salt of fused salt of arsenic oxide arsenoxide distilling furnace is back in the fused salt groove;
(9) occur leaking as occurring fused salt valve, pump for liquid salts, fused salt heating boiler in the work, damage need repairing, during situation such as replacing, temperature of heating plate is set at the temperature than low 5 ~ 20 ℃ of fused salt heating boiler technological temperature, continue to keep the arsenic oxide arsenoxide distilling furnace to be in normal operating conditions, do not influence the work of arsenic oxide arsenoxide distilling furnace because of maintenance, replacing fused salt valve, pump for liquid salts, fused salt heating boiler etc.;
When (10) arsenic oxide arsenoxide distilling furnace internal temperature is down to normal temperature, the material that takes out in the hopper is the arsenic oxide arsenoxide distillage, according to the requirement of producing different quality products, the i.e. requirement of reduction back 5N-7N different purity elemental arsenic product, determine the number of times of arsenic oxide arsenoxide distillation, general distillation 1 ~ 4 time, namely the product that takes out in the last distillation hopper is as the raw material that distills next time, obtain highly purified arsenic oxide arsenoxide through distillation repeatedly, this highly purified arsenic oxide arsenoxide obtains the elemental arsenic that purity is 5N-7N after with hydrogen reducing;
(11) open hermatic door, take out charging tray, the arsenic oxide arsenoxide of charging tray bottom glass shape is taken out, and concentrated the storage, when focusing on some amount, the material that the single flash charging tray takes out carrying out distilling remaining 10 ~ 15% the not recyclable tailing of frit conduct in the charging tray of distillation back under 600 ℃ of temperature condition in the distilling furnace; The glassy arsenic oxide arsenoxide that takes out in the second distillation charging tray returns as single distilled raw material, distills through no sulphuring treatment with except the material behind selenium, the boron with new; In like manner, the material in three distillation back charging trays is as the raw material of second distillation, and the material in four distillation charging trays is as the raw material of three distillations.
Beneficial effect: present device is simple in structure, easy to use, operation easily, preparation flow is short, can prepare the raw material high-purity mangesium oxide arsenic that obtains 6N-7N high purity elemental arsenic behind hydrogen reducing fast and effectively, preparation quality is stable, safe, the new approaches of non-environmental-pollution for the production of high purity elemental arsenic is opened up.
Description of drawings
Fig. 1 is the structural representation of high-purity mangesium oxide arsenic distilling furnace of the present invention.
Among the figure: distillation case 1, distillation framework 2, framework flange 3, hermatic door 4, passage 5, hopper 6, hot-plate 7.
Embodiment
For technique means, creation characteristic that the present invention is realized, reach purpose and effect is easy to understand, below in conjunction with concrete diagram, further set forth the present invention.
Production unit referring to a kind of high-purity mangesium oxide arsenic of Fig. 1, comprise the arsenic oxide arsenoxide distilling furnace, described arsenic oxide arsenoxide distilling furnace comprises distillation case 1, distillation framework 2, framework flange 3, hermatic door 4, passage 5 and hopper 6, described distillation case 1 is rectangular box, every distilling furnace is provided with 4 ~ 10 layers of distillation case 1, horizontal positioned is vertically arranged, evenly be entrenched on the distillation framework 2, described distillation framework 2 is the rectangular frame of vertically placing, outer rim is provided with framework flange 3, fixedly there is hermatic door 4 back of described framework flange 3, and hermatic door 4 size is consistent with framework flange 3 outer rims size, distills the corresponding position of case 1 with the superiors and offer mouth on described hermatic door 4, weld together with passage 5, described passage 5 is L type tubular structure, and Open Side Down at another place, is connected with hopper 6.
Between described adjacent layers distillation case 1, be provided with hot-plate 7, the fused salt pipe that to be evenly distributed 5 ~ 8 diameters on every layer of hot-plate be 40 ~ 100mm.
Based on the production unit of the high-purity mangesium oxide arsenic of said structure, the present invention further sets forth the present invention in conjunction with specific examples.
Embodiment 1: optional distilling furnace distillation purification 1000kg is through no sulphuring treatment with except the arsenic oxide arsenoxide behind selenium, the boron, and every distilling furnace hypothesis charging tray adds up to 20 charging trays, puts into the 50kg arsenic oxide arsenoxide in each charging tray; Put into the material of charging tray and spread out uniformly, make the arsenic oxide arsenoxide thickness in the charging tray even; The charging tray of putting arsenic oxide arsenoxide well is put into every layer of distillation of distilling furnace case, make every layer of charging tray in the distillation case together adjacent; Put the gasket of wide 50 ~ 100mm well in framework flange edge; Shut hermatic door, connect the exhaust pipe of hopper; Feed the oxygen jar bubble smoothness of 2 ~ 4L/min, it is normal then to be tightly connected; Rose behind temperature of heating plate to 100 ~ 200 ℃ constant temperature 3 ~ 10 hours, and made the moisture oven dry that contains in the material; The valve of opening charging basket bottom is emitted the water in the charging basket; Constant temperature was 140 ~ 190 hours after hot-plate was warming up to 350 ~ 600 ℃ then; Close distilling furnace hot-plate power supply behind the constant temperature, take out the material in the charging basket when temperature is down to normal temperature, the material in the charging basket with hydrogen reducing after the gained elemental arsenic detect through GDMS, its quality is between 6N-7N; Take out the glassy tailing of charging tray bottom, continue to repeat the discharging that feeds intake according to above-mentioned, thereby obtain the high high-purity arsenic oxide arsenoxide of steady quality output.
Embodiment 2: one group of corresponding 2 ~ 3 distilling furnace of an optional pump for liquid salts (or heating boiler), every distilling furnace on average feeds intake 1500kg through no sulphuring treatment with except the arsenic oxide arsenoxide behind selenium, the boron, every distilling furnace hypothesis charging tray adds up to 30 charging trays, on average puts into the 50kg arsenic oxide arsenoxide in each charging tray; Put into the material of charging tray and spread out uniformly, make the arsenic oxide arsenoxide thickness in the charging tray even; The charging tray of putting arsenic oxide arsenoxide well is put into every layer of distillation of distilling furnace case, make every layer of charging tray in the distillation case together adjacent; Put the gasket of wide 50 ~ 100mm well in framework flange edge; Shut hermatic door, connect the exhaust pipe of hopper; Every distilling furnace all feeds the oxygen jar bubble smoothness of 2 ~ 4L/min, and it is normal then to be tightly connected; Rose behind temperature of heating plate to 100 ~ 200 ℃ constant temperature 5 ~ 30 hours, and made the moisture oven dry that contains in the material; The valve of opening every distilling furnace charging basket bottom is emitted the water in the charging basket; Every distilling furnace hot-plate is warming up to 200 ~ 600 ℃ then, and the distilling furnace interior conduit is melted fully from getting fused salt; Open earlier pump for liquid salts, make fused salt in distilling furnace internal recycle half an hour; Open fused salt heating boiler power supply, set the fused salt heating boiler at 300 ~ 600 ℃; The fused salt heating boiler is closed the hot-plate power supply after arriving technological temperature, gives the heat supply of arsenic oxide arsenoxide distilling furnace by fused salt fully, fused salt heating boiler constant temperature is after 190 ~ 240 hours, close fused salt heating boiler power supply earlier, close the pump for liquid salts power supply after half an hour, stop the fused salt circulation; The salt valve that advances of each distilling furnace is opened fully, the fused salt that makes fused salt pipeline in the distilling furnace as far as possible total reflux in the fused salt groove; In each charging basket, in bucket, get the sample 20g at five positions when temperature is down to normal temperature in the distilling furnace respectively arbitrarily, five 20g test portions of each charging basket are mixed, get the 20g sample after mixing again respectively, sample detects through the key element Sb of ICP-MS, Zn, Pb, elements such as Bi, Mn, arsenic oxide arsenoxide product after 2 ~ 3 distilling furnace distillations of each fused salt heating boiler correspondence of detected result, its impurity concentration is fully in a concentration range; Taking out every material in the distilling furnace charging basket respectively puts together as same batch, get the 10kg arsenic oxide arsenoxide behind hydrogen reducing, the elemental arsenic that reduction obtains detects through GDMS, total impurities concentration in the elemental arsenic is between 500-1000PPb, and the glassy tailing of taking-up charging tray F bottom is put in the tailing storage barrel and stored; The charging tray repetition said process that continues to feed intake continue to be produced.
Material in the above-mentioned single flash product charging basket weighed divide equally, put in the distilling furnace charging tray that is exclusively used in second distillation; Perhaps continue to use former single flash stove, the charging basket that changes the special-purpose charging basket of second distillation or use with the clean single flash of pure water rinsing, charging tray is replaced by the charging tray of second distillation special use; Charging tray is put well behind single distilled product, charging tray is all put in every layer of distillation case of distilling furnace; Repeat single distilled all technological processs until the blowing out cooling discharge; Respectively take out 5kg second distillation product in each second distillation furnace charge bucket of same batch, each 5kg material of taking-up is put and is mixed together evenly; The material that mixes is got the 20g sample and is detected with ICP-MS, the arsenic oxide arsenoxide product of detected result second distillation reaches the specification of quality of 6N-7N, through hydrogen reducing, the elemental arsenic that reduction obtains is crossed once logical hydrogen distillation at quartz tubular sublimation pipe back warp to the high-purity mangesium oxide arsenic that distills more than the secondary that obtains with this technology again as the raw material of reduction; The elemental arsenic that finally obtains detects through GDMS, and the total impurities concentration in the elemental arsenic is between 80-200PPb.
More than show and described ultimate principle of the present invention and principal character and advantage of the present invention.The technician of the industry should understand; the present invention is not restricted to the described embodiments; that describes in above-described embodiment and the specification sheets just illustrates principle of the present invention; without departing from the spirit and scope of the present invention; the present invention also has various changes and modifications, and these changes and improvements all fall in the claimed scope of the invention.The claimed scope of the present invention is defined by appending claims and equivalent thereof.
Claims (10)
1. the preparation equipment of high-purity mangesium oxide arsenic, it is characterized in that, comprise the arsenic oxide arsenoxide distilling furnace, described arsenic oxide arsenoxide distilling furnace comprises the distillation case, the distillation framework, the framework flange, hermatic door, passage and hopper, described distillation case is rectangular box, every distilling furnace is provided with 4 ~ 10 layers of distillation case, horizontal positioned is vertically arranged, evenly be entrenched on the distillation framework, described distillation framework is the rectangular frame of vertically placing, and outer rim is provided with the framework flange, and fixedly there is hermatic door the back of described framework flange, the hermatic door size is consistent with framework flange outer rim size, position corresponding with the superiors distillations case on described hermatic door offers mouth, with channel welds together, described passage is L type structure, Open Side Down at another place, is connected with hopper.
2. the preparation equipment of high-purity mangesium oxide arsenic according to claim 1, it is characterized in that, described distillation case is long 1500 ~ 5000mm, wide 300 ~ 1000mm, the rectangular box of high 50 ~ 200mm, one end of distillation case is done plug with the plate of long 300 ~ 1000mm, wide 50 ~ 200mm, at the ventpipe of diameter a 10 ~ 16mm of plug welding.
3. the preparation equipment of high-purity mangesium oxide arsenic according to claim 1, it is characterized in that described distillation framework is long 1400 ~ 3200mm, wide 300 ~ 1000mm, the rectangle frame of high 100 ~ 300mm, select long 1400 ~ 3200mm, arbitrary of wide 300 ~ 1000mm is with long 100 ~ 200mm, wide 300 ~ 1000 plate, 5 ~ 8 be evenly distributed on above, and make the long 300 ~ 1000mm of section of the vacancy space that stays and rectangular parallelepiped, wide 50 ~ 200mm unanimity.
4. the preparation equipment of high-purity mangesium oxide arsenic according to claim 1 is characterized in that, described framework flange is the rectangular frame structure, and interior rectangle is consistent with distillation framework outer rim size, and the size of outer rectangle is than the long 150 ~ 350mm of each length of side of interior rectangle.
5. the preparation equipment of high-purity mangesium oxide arsenic according to claim 1, it is characterized in that, the opening part of described distillation case is welded on the place, vacancy space of distillation framework, a distillation of each vacancy space welding case, it is parallel and vertical with the distillation framework up and down that each distills case, is welded with some pillar stiffeners in the both sides of distillation case.
6. the preparation equipment of high-purity mangesium oxide arsenic according to claim 1 is characterized in that, is placed with long 280 ~ 980mm in described distillation case, wide 300 ~ 600mm, and the charging tray of high 40 ~ 160mm is put 4 ~ 8 charging trays in every layer of distillation case.
7. the preparation equipment of high-purity mangesium oxide arsenic according to claim 1 is characterized in that, described hopper is circular or square, and its volume size is relevant with the number of plies of distillation case, perhaps according to distiller charging capacity decision at full capacity.
8. the preparation equipment of high-purity mangesium oxide arsenic according to claim 1, it is characterized in that, between described adjacent layers distillation case, be provided with hot-plate, the length of described hot-plate is wide consistent with the distillation case, hot-plate wide is 1/15 ~ 1/6 of distillation case length, the fused salt pipe that to be evenly distributed 5 ~ 8 diameters on every layer of hot-plate be 40 ~ 100mm.
9. the preparation equipment of high-purity mangesium oxide arsenic according to claim 1 is characterized in that, described high-purity mangesium oxide arsenic distilling furnace each several part all adopts titanium or aluminum to form fully.
10. preparation technology's method of high-purity mangesium oxide arsenic is characterized in that, its concrete processing step is as follows:
(1) according to the charging tray quantity of every distilling furnace, through no sulphuring treatment and through the charging tray of packing into except the arsenic oxide arsenoxide evenly distribute behind selenium, the boron;
(2) charged charging tray is put into the casing of every layer of distilling furnace of distilling furnace, dish with coil between together adjacent, until the interlayer distilling furnace casing of all charging trays all being put into distilling furnace;
(3) put anti-200 ~ 600 ℃ elevated-temperature seal pad in framework flange edge, as alumina high temperature fibre packing etc.; Shut hermatic door, tighten the bolt between framework flange and the hermatic door;
(4) aerating oxygen is stopped leakage in the roof, and the jar bubble smoothness that oxygen flow 1 ~ 3L tail gas connects is the intensification of normally can switching on;
(5) hot-plate of heating heats up, and design temperature is certain temperature value between 140 ~ 650 ℃, and before the heating hot-plate heated up, the temperature of molten salt of fused salt groove was warming up to 200 ~ 400 ℃ in advance, when temperature of heating plate is raised to design temperature, and equilibrium temperature 1 ~ 10 hour;
(6) after hot-plate is warmed up to design temperature and temperature equilibrium time and arrives, open the pump for liquid salts of this arsenic oxide arsenoxide distilling furnace correspondence, make fused salt flow to fused salt pipe in the arsenic oxide arsenoxide distilling furnace, set the temperature of fused salt heating boiler simultaneously at 300 ~ 650 ℃;
(7) after pump for liquid salts is started working, go out the salt temperature head between each distilling furnace of every pump for liquid salts correspondence of 1 ~ 2 hour observed and recorded in every interval, that regulates each distilling furnace correspondence advances salt and salt-supplying valve, makes each corresponding arsenic oxide arsenoxide distilling furnace temperature uniformity of every pump for liquid salts (perhaps every fused salt boiler); Then need not to adjust salt and salt-supplying valve as the corresponding arsenic oxide arsenoxide distilling furnace of pump for liquid salts, only need advancing salt and salt-supplying valve maximum the getting final product of performing fighting;
(8) after the temperature of molten salt of fused salt boiler arrives and sets technological temperature, continuously insulation remaining amount of material in distilling furnace accounts for 10% of the total amount that feeds intake ~ 40% o'clock, close fused salt boiler power supply earlier after 10 ~ 60 minutes, close the pump for liquid salts power supply again, the salt valve that advances of an arsenic oxide arsenoxide distilling furnace correspondence is reached maximum, the interior ducted fused salt of fused salt of arsenic oxide arsenoxide distilling furnace is back in the fused salt groove;
(9) occur leaking as occurring fused salt valve, pump for liquid salts, fused salt heating boiler in the work, damage need repairing, during situation such as replacing, temperature of heating plate is set at the temperature than low 5 ~ 20 ℃ of fused salt heating boiler technological temperature, continue to keep the arsenic oxide arsenoxide distilling furnace to be in normal operating conditions, do not influence the work of arsenic oxide arsenoxide distilling furnace because of maintenance, replacing fused salt valve, pump for liquid salts, fused salt heating boiler etc.;
When (10) arsenic oxide arsenoxide distilling furnace internal temperature is down to normal temperature, the material that takes out in the hopper is the arsenic oxide arsenoxide distillage, according to the requirement of producing different quality products, the i.e. requirement of reduction back 5N-7N different purity elemental arsenic product, determine the number of times of arsenic oxide arsenoxide distillation, general distillation 1 ~ 4 time, namely the product that takes out in the last distillation hopper is as the raw material that distills next time, obtain highly purified arsenic oxide arsenoxide through distillation repeatedly, this highly purified arsenic oxide arsenoxide obtains the elemental arsenic that purity is 5N-7N after with hydrogen reducing;
(11) open hermatic door, take out charging tray, the arsenic oxide arsenoxide of charging tray bottom glass shape is taken out, and concentrated the storage, when focusing on some amount, the material that the single flash charging tray takes out carrying out distilling remaining 10 ~ 15% the not recyclable tailing of frit conduct in the charging tray of distillation back under 600 ℃ of temperature condition in the distilling furnace; The glassy arsenic oxide arsenoxide that takes out in the second distillation charging tray returns as single distilled raw material, distills through no sulphuring treatment with except the material behind selenium, the boron with new; In like manner, the material in three distillation back charging trays is as the raw material of second distillation, and the material in four distillation charging trays is as the raw material of three distillations.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105195129A (en) * | 2014-05-30 | 2015-12-30 | 东北大学 | Columbate-loaded diatomite ball visible-light-driven photocatalyst and preparation method thereof |
| CN107058752A (en) * | 2017-03-15 | 2017-08-18 | 西安建筑科技大学 | A kind of method of rhenium in use vacuum distillation furnace enrichment method calcining molybdenum ore concentrate flue dust |
| CN111265906A (en) * | 2020-02-17 | 2020-06-12 | 峨嵋半导体材料研究所 | Method for preparing 6N high-purity sulfur |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN2225006Y (en) * | 1994-11-24 | 1996-04-17 | 云南锡业公司研究所 | Vacuum distillating furnace for treating alloy with high lead content and low tin content |
| CN101386919A (en) * | 2008-10-24 | 2009-03-18 | 贵阳铝镁设计研究院 | High-pure magnesium preparation method and apparatus |
| CN101570831A (en) * | 2009-06-09 | 2009-11-04 | 扬州高能新材料有限公司 | Large-sized distillation furnace for producing high purity arsenic |
-
2013
- 2013-06-06 CN CN2013102224587A patent/CN103253703A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN2225006Y (en) * | 1994-11-24 | 1996-04-17 | 云南锡业公司研究所 | Vacuum distillating furnace for treating alloy with high lead content and low tin content |
| CN101386919A (en) * | 2008-10-24 | 2009-03-18 | 贵阳铝镁设计研究院 | High-pure magnesium preparation method and apparatus |
| CN101570831A (en) * | 2009-06-09 | 2009-11-04 | 扬州高能新材料有限公司 | Large-sized distillation furnace for producing high purity arsenic |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105195129A (en) * | 2014-05-30 | 2015-12-30 | 东北大学 | Columbate-loaded diatomite ball visible-light-driven photocatalyst and preparation method thereof |
| CN107058752A (en) * | 2017-03-15 | 2017-08-18 | 西安建筑科技大学 | A kind of method of rhenium in use vacuum distillation furnace enrichment method calcining molybdenum ore concentrate flue dust |
| CN111265906A (en) * | 2020-02-17 | 2020-06-12 | 峨嵋半导体材料研究所 | Method for preparing 6N high-purity sulfur |
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Application publication date: 20130821 |