CN103276225B - Apparatus and process method for preparing simple substance arsenic by continuously reducing arsenic oxide - Google Patents
Apparatus and process method for preparing simple substance arsenic by continuously reducing arsenic oxide Download PDFInfo
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Abstract
The invention relates to an apparatus and a process method for preparing simple substance arsenic by continuously reducing arsenic oxide. The apparatus comprises an arsenic oxide negative pressure feeding system, a reducing bin, a continuous unloading system, a reducing furnace and a product discharging device. The above systems are connected according to a production flow. The process is a method for preparing the simple substance arsenic by continuously reducing arsenic oxide based on the above apparatus. The apparatus is simple in structure, convenient for use and operations and short in preparation flow, and can prepare a great amount of the simple substance arsenic by continuous reduction rapidly and effectively. The apparatus for continuously reducing high pure arsenic oxide by once heating without cooling effectively overcomes the problems in intermittent arsenic oxide reduction by repeated heating and cooling.
Description
Technical field
The present invention relates to technique and equipment thereof that oxide compound hydrogen reducing prepares simple substance, be specifically related to processing method and equipment that arsenic oxide arsenoxide reduction obtains elemental arsenic.
Background technology
In the preparation of high purity elemental arsenic, be no matter that vacuum distilling is purified the ultrapurity arsenic oxide arsenoxide obtained, or air distillation is purified the high-purity mangesium oxide arsenic obtained, and all needs hydrogen reducing high-purity mangesium oxide arsenic to obtain highly purified elemental arsenic; Arsenic oxide arsenoxide is owing to being pressed powder or vitreous solid particle, not there is mobility, its reduction is all highly purified arsenic oxide arsenoxide is put in the quartz boat of tubulose or titanium boat use, reduce in the crystal reaction tube again boat putting material well being put into tubulose, every boat can only throw in arsenic oxide arsenoxide 8 ~ 20kg, and its shortcoming has following and aspect:
1, because discontinuous reduction once feeds intake 8 ~ 20kg, the boat portion of reduction furnace is difficult to the balance of control temperature and arsenic oxide arsenoxide boil-off rate, during temperature height, arsenic oxide arsenoxide evaporating capacity is large, the hydrogen needed increases suddenly, the backflow of hydrogen supply not enough afterbody water collector hydrogen participates in reaction, form negative pressure suck air in reaction tubes, there is serious potential safety hazard;
2, because the speed of temperature and arsenic oxide arsenoxide vaporization is difficult to balance, the yield of arsenic oxide arsenoxide reduction is unstable, and operator is experienced is that yield can reach 50 ~ 60%, and when operator is unskilled, yield only has 30 ~ 50%, well below theoretic 75%, have a strong impact on reduction efficiency;
3, after the arsenic oxide arsenoxide material in each boat has all been vaporized, just must be down to normal temperature from the furnace temperature of 800 ~ 1000 DEG C to come out of the stove, in boat, from new charging, new one heating, cooling is taken turns again after coming out of the stove, heating, cooling so repeatedly, come out of the stove, shove charge, cause that unstable product quality, labour intensity are large, arsenic oxide arsenoxide on the impact of operating environment and operator very greatly, energy consumption is high;
4, reaction tubes uses the silica tube of tubulose, and the arsenic oxide arsenoxide of melting or arsenic oxide arsenoxide steam have corrodibility to quartz 300 ~ 1000 DEG C time, and crystal reaction tube easily damages; Simultaneously careless also as easy as rolling off a logly in the process taking on stove break silica tube, considerably increase cost.
Summary of the invention
Technical problem solved by the invention is to provide a kind of arsenic oxide arsenoxide to reduce continuously prepares the instrument and supplies method of elemental arsenic, to solve the shortcoming in above-mentioned background technology.
Technical problem solved by the invention realizes by the following technical solutions:
Arsenic oxide arsenoxide reduces the equipment preparing elemental arsenic continuously, and comprise arsenic oxide arsenoxide negative pressure feeding system, reduction feed bin, continuously blanking system, reduction furnace and product discharge device, above-mentioned each system installs connection successively according to Production Flow Chart.
Described arsenic oxide arsenoxide negative pressure feeding system comprises: 2 ~ 10m
2hundred grades of clean workplaces; The clean transport pipe of diameter 60 ~ 120mm, the mouth of pipe of pipeline one end or the mouth of pipe connect suction storehouse, are positioned in clean area, and the other end of pipeline is connected with feed bin; Cubic capacity is 0.3 ~ 1.5m
3inclination angle>=60, bottom ° angle centrum, top is columniform negative pressure stock bin, multiple diameter 60 ~ 150mm is placed in feed bin top cylinder, filtering order number is 100 ~ 2000 object dust filtering bags, the adapter of feed bin one diameter 50 ~ 100mm is connected with clean charging line, and the adapter of another diameter 50 ~ 100mm is connected with air-inlet of vacuum pump; The vacuum pump of 5 ~ 75kw, is connected with the pipeline of 50 ~ 100mm between air-inlet of vacuum pump with feed bin air outlet; Take offence or the air compressor machine of source of the gas for pneumatic vacuum pump provides, and housing, the feed bin of described feeding system is positioned over the top of reduction feed bin, and the convenient fixing feed bin feed supplement for reduction furnace, vacuum pump, housing are placed on side.
Described reducing material storage capacity is 0.3 ~ 1.5m
3, bottom is the centrum at degree angle, inclination angle>=60, and top is cylindrical body; Staving topmost lid is arranged the air inlet tube of a diameter 3 ~ 20mm, the feed supplement adapter of a diameter 40 ~ 200mm, feed supplement adapter has cover plate for sealing; Pneumatic or manually-operated gate is had bottom centrum; Feed bin cone end flange upwards installs bin level indicator and material level alarm in position, 50 ~ 500mm place, and when need feed in raw material, the operated pneumatic valve opened bottom negative pressure loading bin is the feed supplement of reduction feed bin, a feed supplement 10 ~ 500kg.
Described continuous blanking system comprises the cylindrical charging basket of 3 ~ 50L, screw rod is configured bottom charging basket, bottom charging basket, upwards the next and upper two bin level indicators are installed by 50 ~ 500mm place, two bin level indicator signals are connected with the operated pneumatic valve switch signal of reduction feed bin, when the next indicator signal of charging basket material exports, the operated pneumatic valve of reduction bin bottom opens feed barrel feed supplement automatically, and when feed supplement arrives upper telltale, the valve of reduction bin bottom is closed automatically; What as reduced, bin bottom installed is manually-operated gate, when the next indicator light of charging basket material is bright, manually opens the feed supplement of reduction feed bin bottom valve feed barrel, and when the upper pilot lamp of charging basket is bright, manual-lock changes raw material cabin bottom valve and stops feed supplement; Screw rod is connected with adjustable speed motor and controls blanking velocity.
Described reduction furnace comprises reaction tubes, tremie pipe, air diffuser, junction station, product condenser and tail gas and observes jar, described reaction tubes, tremie pipe, air diffuser, junction station, product condenser all adopt nitrate nitroge or quartz to make, described reaction tube diameter is 100 ~ 250mm, length 1500 ~ 4500mm, reaction tubes one end back cover, open the interface of a diameter 40 ~ 120mm perpendicular to reaction tubes from back cover 100 ~ 500mm, reaction tubes opening end is the flange of external diameter 160 ~ 300mm, the flange that internal diameter is consistent with tube inner diameter; Described tremie pipe external diameter and the little 1 ~ 2mm of opening inside diameter perpendicular to reaction tubes, tremie pipe can insert in the opening perpendicular to reaction tubes, gap high-temp glue between tremie pipe with reaction tubes mixes aluminum oxide powder or carborundum powder becomes pasty state to fill gap seasoning sealing, tremie pipe the other end blanking flange that is flanged and continuous blanking system docks, and adds gasket bolt and connects; When described reaction tubes adopts quartz to make, its sealing end is directly welded on reaction tubes perpendicular to the tremie pipe of crystal reaction tube, dock with four fluorine tube Butt sealing good with tremie pipe major diameter fit between the feed opening of tremie pipe and continuously blanking system, reaction tubes the other end PTFE is processed into flange and docks with crystal reaction tube, with clip clamping tetrafluoro flange and silica tube butted part, seal together with making tightly to paste between tetrafluoro with quartz, tetrafluoro flange flange bolt Butt sealing again and between water collector; When described air diffuser silicon carbide makes, the external diameter of air diffuser is determined by tube inner diameter, has 2 ~ 5mm with tube inner diameter gap, the disk of thick 20 ~ 100mm, with the circular hole of disc shaft to parallel uniform 5 ~ 12 diameter 10 ~ 30mm in disk; When described air diffuser quartz makes, with the quartzy plectane of less than tube inner diameter 2 ~ 10 millimeters of two pieces of external diameters, grow the silica tube of 10 ~ 100mm with 4 ~ 12 diameter 10 ~ 30mm uniform and be parallel to each other and be welded between two quartzy plectanes, make two plectanes parallel; When described junction station silicon carbide makes, be designed to external diameter 2 ~ 5mm less of tube inner diameter, thickness is the disk that 20 ~ 100mm is thick, have in the middle part of disk a diameter be 10 ~ 80 circular hole, one side and the plectane dead in line of plectane connect an internal diameter and disk perforate always, the adapter of long 50 ~ 100mm; When described junction station quartz makes, with the quartz wafer of two 2 ~ 5mms less of tube inner diameter, the silica tube of weld diameter 10 ~ 80mm in the middle part of two quartz wafers, make to flow out from the silica tube of diameter 10 ~ 80mm after confluxing in air flow collection, in order to make to seal between junction station and reaction tubes, avoid air-flow to flow out from the gap between junction station and reduction, reach between junction station and reaction tubes with silica wool filling between two quartz wafers and seal; The specification of described condenser is made into external diameter 5 ~ 20mm less of tube inner diameter, and the semicircle tile of long 200 ~ 800mm, is condensate in cylinder according to product and facilitates discharging.
Described product discharge device be metal titanium or, quartz, the internal diameter that the material such as aluminium makes or than tube inner diameter slightly large 5 ~ 20mm consistent with tube inner diameter, long 50 ~ 400mm longer than reaction tubes inner condenser overall length, product discharge device one end connects the internal diameter corrugated tube consistent with tube inner diameter, one end internal diameter is 80 ~ 200mm arm flange port that can free in and out and a diameter is the gas fittings of 4 ~ 20mm, the flange of hand turnover connects the tetrafluoro bag of a long 400 ~ 800mm, the feeding bar of a tightly colligation long band hook on tetrafluoro bag, gas fittings pipeline is connected to bagroom and gathers dust.
Based on aforesaid device, arsenic oxide arsenoxide reduces the processing method preparing elemental arsenic continuously and is:
(1) needing the arsenic oxide arsenoxide material of reduction to be extracted in negative pressure system feed bin by negative pressure system;
(2) feed bin that reduces passes into nitrogen (or argon gas) displaced air, the amount of inert gas passed into is 1 ~ 3 times of feed bin volume, the gas of displacement is by continuous blanking machine, tremie pipe, reaction tubes, reductive water collector, finally observes jar from tail gas and flows out, make air displacement in whole restoring system clean;
(3) open vacuum charging system bin bottom valve, make the material of feeding system feed bin all enter reduction feed bin;
(4) corresponding in reduction furnace material section, conversion zone, product section heat up, material section design temperature 360 ~ 700 DEG C, conversion zone design temperature 600 ~ 1100 DEG C, product section design temperature 280 ~ 550 DEG C;
(5) guarantee to reduce rare gas element passes in whole system volume be not less than reduction high hopper volume 3 times time, switch to the hydrogen passing into flow 5L/min to open the blanking of continuous blanking system power supply after 20 ~ 50 minutes, blanking speed is 30 ~ 300g/min;
(6) observe jar bubble, according to blanking speed adjustment bubble, the bubble adjusting to jar is smooth denumerable;
(7) calculate the elemental arsenic amount restored in condenser according to arsenic oxide arsenoxide discharge quantity, in condenser, elemental arsenic is stop blanking at 10 ~ 20 kilograms, and restoring system switches to and passes into rare gas element, replaces the hydrogen in clean restoring system;
(8) unload the reduction water butt in restoring system, product discharge device corrugated tube flange is docked airtight with reaction tubes corrugated tube flange;
(9) stretch into feeding to be hooked to and to go back in the middle part of original product condenser, catch on the product of condenser, product is drawn in product discharge device together with product condenser;
(10) unload product discharge device and reaction tubes flange bolt, first-class cover plate on condenser corrugated tube flange, on the cover board passes into rare gas element, and product discharge device is shifted onto and slowly made product naturally cooling;
(11) continue in reaction tubes to put into product condenser for subsequent use, connect reductive water water butt, connect offgas duct;
(12) step repeating (6) ~ (11) continues blanking and carries out also original production;
(13) after the product of product discharge device is cooled to normal temperature, the elemental arsenic product taken out in product discharge device is the high purity elemental arsenic of reduction gained, can be used as the raw material continuing next procedure and lead to hydrogen distillation, also can crushing packing.
beneficial effect:
Present device structure is simple, easy to use, easy operation, preparation flow is short, can reduce continuously fast and effectively and prepare a large amount of elemental arsenic products, once heating up the equipment of reduction high-purity mangesium oxide arsenic of not lowering the temperature continuously, effectively solves problem existing in the cooling discontinuous arsenic oxide arsenoxide reduction that repeatedly heats up.
Embodiment
The technique means realized to make the present invention, creation characteristic, reaching object and effect is easy to understand, below in conjunction with specific examples, setting forth the present invention further.
Embodiment 1:50kg arsenic oxide arsenoxide is extracted in vacuum charging system feed bin by vacuum charging system; Restoring system passes into the nitrogen 30 minutes of 8L/min; Material in vacuum feeder feed bin is put into reduction feed bin, removes vacuum charging system, airtight for reduction feed bin opening for feed; Confirm that reduction each section of furnace temperature is warmed up to material section 500 DEG C, conversion zone 850 DEG C, product section 350 DEG C; Open continuous blanking system blanking, blanking rate-controlling is at 50g/min; Observe jar bubble, adjustment hydrogen flowmeter flow, be adjusted to that jar bubble is smooth is denumerablely steady state, or else by adjustment hydrogen flowing quantity and blanking speed until discharging; According to blanking rate calculations discharge quantity, when arsenic oxide arsenoxide blanking arrives 25 kilograms, close continuous blanking system power supply and stop blanking; To stop after blanking 10 ~ 30 minutes, close hydrogen, switch to nitrogen, nitrogen flow 5L/min, the hydrogen in displacement restoring system 20 ~ 40 minutes; Unload reduction water butt; The corrugated tube flange of product discharge device and reaction tubes Flange joint; With the product in the bar of the buckle in product discharge device pull-out reaction tubes and product condenser in product discharge device; Unload product discharge device, build product discharge device with the first-class bolt of flange plate, pass into nitrogen and make elemental arsenic naturally cool to normal temperature; Continue in reaction tubes to put another set of product condenser for subsequent use well; Connect reduction water butt and offgas duct; Then nitrogen is closed, the blanking of blanking system power supply is opened after first opening hydrogen 5L/min10 minute, denumerable to jar bubble smoothness by aforementioned adjustment hydrogen flowmeter flow, continue to produce until remaining 25kg arsenic oxide arsenoxide all terminates to close blanking machine power supply and hydrogen in reduction feed bin, after switching to nitrogen, take out the elemental arsenic product in condenser; Open cover plate after the product of product discharge device is cooled to normal temperature, take out elemental arsenic, twice discharging gained elemental arsenic product amounts to 36 kilograms.
Embodiment 2:300kg arsenic oxide arsenoxide is extracted in vacuum charging system feed bin by vacuum charging system; Restoring system passes into the nitrogen 30 minutes of 8L/min; Material in vacuum feeder feed bin is put into reduction feed bin, removes vacuum charging system, airtight for reduction feed bin opening for feed; Confirm that reduction each section of furnace temperature is warmed up to material section 600 DEG C, conversion zone 1000 DEG C, product section 400 DEG C; Open continuous blanking system blanking, blanking rate-controlling is at 100g/min; Observe jar bubble, adjustment hydrogen flowmeter flow, be adjusted to that jar bubble is smooth is denumerablely steady state, or else by adjustment hydrogen flowing quantity and blanking speed until discharging; According to blanking rate calculations discharge quantity, when arsenic oxide arsenoxide blanking arrives 25 kilograms, close continuous blanking system power supply and stop blanking; To stop after blanking 10 ~ 30 minutes, close hydrogen, switch to nitrogen, nitrogen flow 5L/min, the hydrogen in displacement restoring system 20 ~ 40 minutes; Unload reduction water butt; The corrugated tube flange of product discharge device and reaction tubes Flange joint; With the product in the bar of the buckle in product discharge device pull-out reaction tubes and product condenser in product discharge device; Unload product discharge device, build product discharge device with the first-class bolt of flange plate, pass into nitrogen and make elemental arsenic naturally cool to normal temperature; Continue in reaction tubes to put another set of product condenser for subsequent use well; Connect reduction water butt and offgas duct; Then close nitrogen, after first opening hydrogen 5L/min10 minute, open the blanking of blanking system power supply, denumerable to jar bubble smoothness by aforementioned adjustment hydrogen flowmeter flow, continue to produce until by preceding method discharging when also discharge quantity reaches 25kg arsenic oxide arsenoxide again; So repeatedly, until 300 kilograms of arsenic oxide arsenoxides in feed bin all terminate, discharging obtains elemental arsenic summation 220 kilograms, wherein from reduction water butt, collects 7.2kg powdered elemental arsenic.
More than show and describe 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; what describe in above-described embodiment and 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.Application claims protection domain is defined by appending claims and equivalent thereof.
Claims (2)
1. arsenic oxide arsenoxide reduces the equipment preparing elemental arsenic continuously, it is characterized in that, comprise arsenic oxide arsenoxide negative pressure feeding system, reduction feed bin, continuously blanking system, reduction furnace and product discharge device, above-mentioned each system installs connection successively according to Production Flow Chart, described arsenic oxide arsenoxide negative pressure feeding system comprises: 2 ~ 10m
2hundred grades of clean workplaces, the clean transport pipe of diameter 60 ~ 120mm, the mouth of pipe of pipeline one end or the mouth of pipe connect suction storehouse, are positioned in clean area, and the other end of pipeline is connected with feed bin, cubic capacity is 0.3 ~ 1.5m
3inclination angle>=60, bottom ° angle centrum, top is columniform negative pressure stock bin, multiple diameter 60 ~ 150mm is placed in feed bin top cylinder, filtering order number is 100 ~ 2000 object dust filtering bags, the adapter of feed bin one diameter 50 ~ 100mm is connected with clean charging line, and the adapter of another diameter 50 ~ 100mm is connected with air-inlet of vacuum pump, the vacuum pump of 5 ~ 75kw, is connected with the pipeline of 50 ~ 100mm between air-inlet of vacuum pump with feed bin air outlet, take offence or the air compressor machine of source of the gas for pneumatic vacuum pump provides, and housing, the feed bin of described feeding system is positioned over the top of reduction feed bin, and vacuum pump, housing are placed on side, described reducing material storage capacity is 0.3 ~ 1.5m
3, bottom is the centrum at degree angle, inclination angle>=60, and top is cylindrical body, staving topmost lid is arranged the air inlet tube of a diameter 3 ~ 20mm, the feed supplement adapter of a diameter 40 ~ 200mm, feed supplement adapter has cover plate for sealing, pneumatic or manually-operated gate is had bottom centrum, feed bin cone end flange upwards installs bin level indicator and material level alarm in position, 50 ~ 500mm place, described continuous blanking system comprises the cylindrical charging basket of 3 ~ 50L, configures screw rod bottom charging basket, and bottom charging basket, upwards the next and upper two bin level indicators are installed by 50 ~ 500mm place, and two bin level indicator signals are connected with the operated pneumatic valve switch signal of reduction feed bin, described reduction furnace comprises reaction tubes, tremie pipe, air diffuser, junction station, product condenser and tail gas and observes jar, described reaction tubes, tremie pipe, air diffuser, junction station, product condenser all adopt nitrate nitroge or quartz to make, described reaction tube diameter is 100 ~ 250mm, length 1500 ~ 4500mm, reaction tubes one end back cover, open the interface of a diameter 40 ~ 120mm perpendicular to reaction tubes from back cover 100 ~ 500mm, reaction tubes opening end is the flange of external diameter 160 ~ 300mm, the flange that internal diameter is consistent with tube inner diameter, described tremie pipe external diameter and the little 1 ~ 2mm of opening inside diameter perpendicular to reaction tubes, tremie pipe can insert in the opening perpendicular to reaction tubes, gap high-temp glue between tremie pipe with reaction tubes mixes aluminum oxide powder or carborundum powder becomes pasty state to fill gap seasoning sealing, tremie pipe the other end blanking flange that is flanged and continuous blanking system docks, and adds gasket bolt and connects, when described reaction tubes adopts quartz to make, its sealing end is directly welded on reaction tubes perpendicular to the tremie pipe of crystal reaction tube, dock with four fluorine tube Butt sealing good with tremie pipe major diameter fit between the feed opening of tremie pipe and continuously blanking system, reaction tubes the other end PTFE is processed into flange and docks with crystal reaction tube, with clip clamping tetrafluoro flange and silica tube butted part, seal together with making tightly to paste between tetrafluoro with quartz, tetrafluoro flange flange bolt Butt sealing again and between water collector, when described air diffuser silicon carbide makes, air diffuser is that external diameter is determined by tube inner diameter, and has 2 ~ 5mm with tube inner diameter gap, the disk of thick 20 ~ 100mm, with the circular hole of disc shaft to parallel uniform 5 ~ 12 diameter 10 ~ 30mm in disk, when described air diffuser quartz makes, with the quartzy plectane of less than tube inner diameter 2 ~ 10 millimeters of two pieces of external diameters, uniform and be parallel to each other and be welded between two quartzy plectanes with the silica tube of the long 10 ~ 100mm of 4 ~ 12 diameter 10 ~ 30mm, make two plectanes parallel, when described junction station silicon carbide makes, be designed to external diameter 2 ~ 5mm less of tube inner diameter, thickness is the disk that 20 ~ 100mm is thick, have in the middle part of disk a diameter be 10 ~ 80 circular hole, one side and the plectane dead in line of plectane connect an internal diameter and disk perforate always, the adapter of long 50 ~ 100mm, when described junction station quartz makes, with the quartz wafer of two 2 ~ 5mms less of tube inner diameter, the silica tube of weld diameter 10 ~ 80mm in the middle part of two quartz wafers, reaches between junction station and reaction tubes with silica wool filling between two quartz wafers and seals, the specification of described condenser is made into external diameter 5 ~ 20mm less of tube inner diameter, the semicircle tile of long 200 ~ 800mm, described product discharge device be metal titanium or, quartz, an internal diameter or than the tube inner diameter slightly large 5 ~ 20mm consistent with tube inner diameter that aluminum makes, long 50 ~ 400mm longer than reaction tubes inner condenser overall length, product discharge device one end connects the internal diameter corrugated tube consistent with tube inner diameter, one end internal diameter is 80 ~ 200mm arm flange port that can free in and out and a diameter is the gas fittings of 4 ~ 20mm, the flange of hand turnover connects the tetrafluoro bag of a long 400 ~ 800mm, the feeding bar of a tightly colligation long band hook on tetrafluoro bag, gas fittings pipeline is connected to bagroom.
2. arsenic oxide arsenoxide reduces the processing method preparing elemental arsenic continuously, it is characterized in that, utilizes equipment described in claim 1, and comprise the following steps:
(1) needing the arsenic oxide arsenoxide material of reduction to be extracted in negative pressure system feed bin by negative pressure system;
(2) feed bin that reduces passes into nitrogen or argon replaces air, the amount of inert gas passed into is 1 ~ 3 times of feed bin volume, the gas of displacement is by continuous blanking machine, tremie pipe, reaction tubes, reductive water collector, finally observes jar from tail gas and flows out, until air displacement is clean in whole restoring system;
(3) open vacuum charging system bin bottom valve, make the material of feeding system feed bin all enter reduction feed bin;
(4) corresponding in reduction furnace material section, conversion zone, product section heat up, material section design temperature 360 ~ 700 DEG C, conversion zone design temperature 600 ~ 1100 DEG C, product section design temperature 280 ~ 550 DEG C;
(5) when the volume guaranteeing that in reduction whole system, rare gas element passes into is not less than reduction high hopper volume 3 times, switch to the hydrogen passing into flow 5L/min to open the blanking of continuous blanking system power supply after 20 ~ 50 minutes, blanking speed is 30 ~ 300g/min;
(6) observe jar bubble, according to blanking speed adjustment bubble, the bubble adjusting to jar is smooth denumerable;
(7) calculate the elemental arsenic amount restored in condenser according to arsenic oxide arsenoxide discharge quantity, in condenser, elemental arsenic stops blanking 10 ~ 20 kilograms time, and restoring system switches to and passes into rare gas element, replaces the hydrogen in clean restoring system;
(8) unload the reduction water butt in restoring system, product discharge device corrugated tube flange is docked airtight with reaction tubes corrugated tube flange;
(9) stretch into feeding to be hooked to and to go back in the middle part of original product condenser, catch on the product of condenser, product is drawn in product discharge device together with product condenser;
(10) unload product discharge device and reaction tubes flange bolt, first-class cover plate on condenser corrugated tube flange, on the cover board passes into rare gas element, and product discharge device is shifted onto and slowly made product naturally cooling;
(11) continue in reaction tubes to put into product condenser for subsequent use, connect reductive water water butt, connect offgas duct;
(12) step repeating (6) ~ (11) continues blanking and carries out also original production;
(13) after the product of product discharge device is cooled to normal temperature, the elemental arsenic product taken out in product discharge device is the high purity elemental arsenic of reduction gained, can be used as the raw material continuing next procedure and lead to hydrogen distillation, also can crushing packing.
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| CN104975191B (en) * | 2015-07-17 | 2017-05-31 | 广东先导稀材股份有限公司 | A kind of hydro-reduction device and high purity arsenic preparation method for high purity arsenic production |
| CN107983969B (en) * | 2017-12-29 | 2024-02-23 | 深圳微纳增材技术有限公司 | Device for continuously reducing metal powder and application method thereof |
| CN108913915A (en) * | 2018-07-19 | 2018-11-30 | 湖南腾驰环保科技有限公司 | A kind of arsenic trioxide restores to obtain the technique of elemental arsenic |
| CN109957654A (en) * | 2019-03-12 | 2019-07-02 | 济源市中亿科技有限公司 | A kind of steaming arsenic tank |
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