CN203768475U - High-purity aluminum powder preparation equipment - Google Patents

High-purity aluminum powder preparation equipment Download PDF

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CN203768475U
CN203768475U CN201420147887.2U CN201420147887U CN203768475U CN 203768475 U CN203768475 U CN 203768475U CN 201420147887 U CN201420147887 U CN 201420147887U CN 203768475 U CN203768475 U CN 203768475U
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kettle
deposition
circulation
work
discharging
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郭昭华
东青
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Abstract

The utility model discloses high-purity aluminum powder preparation equipment. The high-purity aluminum powder preparation equipment comprises a charging system, a working kettle body system, an inert gas input system, a detection system, a heating heat preservation system, a stirring system, a power supply system, a deposition circuit, an online detection system, a control system, a product discharging system and a waste liquid drainage system which are connected to one another, wherein the working kettle body system comprises a working kettle body (filled with a working solution and circulation liquid), a deposition working electrode and a deposition anode, the power supply system is used for supplying power to all parts and all systems, the charging system comprises a charging bin, the detection system is provided with a spectrum detection head, a liquid level sensor, a pressure sensor and a temperature sensor and is arranged in the working kettle body, and an ion generator is arranged in the working kettle body which comprises at least one reaction kettle body. The high-purity aluminum powder preparation equipment disclosed by the utility model can be used for directly extracting high-purity aluminum powder at low cost, is capable of detecting change of components of the circulation liquid and the working solution in real time, and is energy-saving, environmental-friendly, pollution-free and high in yield.

Description

High-purity aluminium powder preparation apparatus
Technical field
The utility model relates to aluminium powder preparation apparatus, particularly relates to high-purity aluminium powder preparation apparatus.
Background technology
POWDER METALLURGY ALUMINIUM ALLOYS material has low density, high than features such as strong, high abrasion, stretch-proof, corrosion-resistant and anti-fatigue performance are good, in fields such as aerospace, automobile and engines, has extensive use.Metallic aluminium powder is the basic material of POWDER METALLURGY ALUMINIUM ALLOYS, and the method for producing at present mainly contains two kinds, i.e. ball milling powder process method and powder by atomization method.Ball mill production flakey aluminium powder under protection of inert gas for ball milling powder process method, is also referred to as " dry production ", and this method production efficiency is low, and production process dust is many, and quality is wayward.Powder by atomization method is to utilize the atomizing medium with certain speed directly to smash liquid aluminium technology or alloy and the method that makes powder, applies comparatively extensive.Wherein atomization refers to the high pressure, the high-speed gas that by atomizer nozzle, are penetrated, interacts with fused solution metal or alloy, and liquid metal or alloy are smashed into small droplets, and small droplets is cooled and solidified in flight course, thereby obtains the method for powder.Atomization comprises that (rate of cooling is 10 to air atomizing method 2～10 3k/s) and water atomization (rate of cooling is 10 2～10 4k/s), the existing spherical irregular shape that also has of product, is also referred to as " wet production ".
The activity of Al liquid is very high, when rapid solidification flour, inevitably can form layer oxide film, causes the phase mutual diffusion of densification process interalloy element to be hindered, and is difficult to form metallurgical bond.
Therefore in producing, need to adopt some special densification processes to overcome these difficulties, as hot extrusion method, high velocity compacted etc.
Above-mentioned two kinds of traditional metal aluminium powder form preparation methods, the deficiency such as ubiquity that reparation technology route is long, cost is high, purity and the bad control of the quality of production.
Along with scientific and technical development, laser spectrum tech can have been used among the preparation apparatus of powder production process, the variation tendency of chemical reaction component in can on-line monitoring system, the depositing crystalline effect of quantitative analysis raw material consumption and principal element aluminum metal, the generation of on-line monitoring intermediate product, impurity and impurity-eliminating effect, for the automatic control system of powder preparation apparatus provides the support data of science decision, set up production models and method that laboratory and industry are amplified, to shorten research and development and industrial cycle.The utility model is for rafifinal powder production provides a kind of novel appts and method, make production process more sanitary safe, do not pollute, level of automation is higher, technological line is short and production cost is cheaper, can effectively improve efficiency and quality that aluminium powder form is produced.
Summary of the invention
The utility model completes in order to solve above-mentioned deficiency of the prior art, the purpose of this utility model is to provide can directly extract rafifinal powder, cost is low, produce in process and can detect in real time circulation fluid and working fluid change of component, some work liquid can be recycled, save the energy, reduce or do not consume deposition anode material, environmental protection, there is no environmental pollution, high-purity aluminium powder preparation apparatus that the rate of output is high.
High-purity aluminium powder preparation apparatus of the present utility model, comprises charging system, work kettle system, rare gas element input system, heating and thermal insulation system, stirring system, power supply system, deposition circuit, on-line detecting system, Controlling System, product is discharged system and discharging of waste liquid system, described work kettle system respectively with charging system, rare gas element input system, power supply system, deposition circuit, on-line detecting system, Controlling System, the product system of discharging is connected with discharging of waste liquid system, and described stirring system lower part is arranged in described work kettle system, and described heating and thermal insulation system is arranged on described work kettle system outside, described Controlling System respectively with charging system, work kettle system, rare gas element input system, detection system, heating and thermal insulation system, stirring system, power supply system, deposition circuit, on-line detecting system, product is discharged system and is connected with discharging of waste liquid system, and described work pot systems turnkey is drawn together work kettle, deposition working electrode and deposition anode, described deposition working electrode and deposition anode are all electrically connected to described deposition circuit, in described work kettle, have working fluid and circulation fluid, and described power supply system is given the charging system being attached thereto by power supply netting twine, work kettle system, rare gas element input system, detection system, heating and thermal insulation system, stirring system, deposition circuit, on-line detecting system, Controlling System, product is discharged system and discharging of waste liquid system power supply, and described feeding device comprises at least two feeding chambers, and described feeding chamber is communicated with described work kettle by charge pump, and organic generation halogen is housed respectively in described feeding chamber, aluminum chloride raw material and toluene, described on-line detecting system comprises spectrographic detection head, liquid level sensor, pressure transmitter and temperature sensor, described detection system is all arranged in described work kettle, in described work kettle, be provided with ion generator, described product discharge system comprises ultrasonic vibration head and is arranged on the product offtake of described work autoclave body bottom, described discharging of waste liquid system is the end liquid discharging tube that comprises tapping pump and be arranged on described work autoclave body bottom, and described work kettle at least comprises a reaction kettle body.
High-purity aluminium powder preparation apparatus of the present utility model can also be:
Described work kettle comprises circulation kettle and the deposition kettle can break-make being communicated with, between described circulation kettle and described deposition kettle, by cocycle system and the lower recycle system, be communicated with, described ion generator is arranged in described cocycle system, described circulation kettle is connected with described charging system, in described circulation kettle, there is circulating liquid, in described deposition kettle, be provided with working fluid, deposition working electrode and deposition anode, in described circulation kettle and described deposition kettle, be provided with stirring system, temperature inductor, pressure inductor, spectrographic detection head and liquid level sensor, described circulation kettle and described deposition kettle outside are provided with heating and thermal insulation system, described circulation kettle is all communicated with and is all connected with power supply system with Controlling System with rare gas element input system with described deposition kettle top, described discharging of waste liquid system is arranged at described circulation autoclave body bottom, described product discharge system is arranged at described deposition autoclave body bottom.
Described cocycle system is provided with pumping installation and under meter, and the described lower recycle system is provided with pumping installation and switch electromagnetic valve.
Described work kettle comprises still lower body and the kettle cover covering, and described still lower body and the described kettle cover place of covering are provided with tightness system.
Described stirring system comprises stirrer, agitator arm and agitating vane, and described agitator arm is connected with described stirrer, and described agitating vane is positioned at the bottom of described agitator arm, and described agitating vane is positioned at described work kettle middle part with upper/lower positions.
Between described charging system and described work kettle, between described discharging of waste liquid system and described work kettle, between described rare gas element input system and described work kettle, be provided with pumping installation and under meter.
In described feeding chamber, be provided with a material sensor, described work autoclave body bottom is provided with switch electromagnetic valve.
High-purity aluminium powder preparation apparatus of the present utility model, it comprises charging system, work kettle system, rare gas element input system, heating and thermal insulation system, stirring system, power supply system, deposition circuit, on-line detecting system, Controlling System, product is discharged system and discharging of waste liquid system, described work kettle system respectively with charging system, rare gas element input system, power supply system, deposition circuit, on-line detecting system, Controlling System, the product system of discharging is connected with discharging of waste liquid system, and described stirring system lower part is arranged in described work kettle system, and described heating and thermal insulation system is arranged on described work kettle system outside, described Controlling System respectively with charging system, work kettle system, rare gas element input system, detection system, heating and thermal insulation system, stirring system, power supply system, deposition circuit, on-line detecting system, product is discharged system and is connected with discharging of waste liquid system, and described work pot systems turnkey is drawn together work kettle, deposition working electrode and deposition anode, described deposition working electrode and deposition anode are all electrically connected to described deposition circuit, in described work kettle, have working fluid and circulation fluid, and described power supply system is given the charging system being attached thereto by power supply netting twine, work kettle system, rare gas element input system, detection system, heating and thermal insulation system, stirring system, deposition circuit, on-line detecting system, Controlling System, product is discharged system and discharging of waste liquid system power supply, and described feeding device comprises at least two feeding chambers, and described feeding chamber is communicated with described work kettle by charge pump, and organic generation halogen is housed respectively in described feeding chamber, aluminum chloride raw material and toluene, described on-line detecting system comprises spectrographic detection head, liquid level sensor, pressure transmitter and temperature sensor, described detection system is all arranged in described work kettle, in described work kettle, be provided with ion generator, described product discharge system comprises ultrasonic vibration head and is arranged on the product offtake of described work autoclave body bottom, described discharging of waste liquid system is the end liquid discharging tube that comprises tapping pump and be arranged on described work autoclave body bottom, and described work kettle at least comprises a reaction kettle body.Like this, charging system for adding needed raw material and preparing burden and dosing in work kettle in work kettle system, work kettle is under the effect of Controlling System or as recirculating still or as deposition kettle, can also be the circulation kettle can break-make connecting and the deposition kettle that work kettle itself comprises connection, when work kettle is circulation kettle, after discharging bin discharging, in circulation kettle, be configured as circulation fluid, for looping depositing treatment process after liquid mixing after the deposition with depositing in kettle, and work kettle is while depositing kettle, on-line detecting system detects the temperature of this deposition kettle, pressure, the component of liquid level and the interior deposit fluid of deposition kettle is also transmitted above-mentioned detected value to Controlling System, after Controlling System is compared the detection data that receive and predetermined value scope, when if indices does not reach the standard that starts deposition, Controlling System heating and heat-insulating device is started working and work kettle is heated to preset temperature and starts insulation so, Controlling System startup rare gas element input system starts to input inert gas warranty work kettle internal pressure in work kettle and reaches predetermined range value, can start ion generator and supplement ionic concn simultaneously, or Controlling System starts to start charging system and in work kettle, adds wherein a kind of material or two kinds of materials according to the flow after calculating, so that being controlled at, the component of the interior liquid of work kettle is suitable for deposition, when if indices all reaches the standard that starts deposition, Controlling System is controlled deposition circuit start so, deposition working electrode and deposition anode are started working, aluminium powder through deposition reaction is deposited in deposition anode, aluminium powder in deposition anode reaches certain thickness, starting ultrasonic vibration head that product discharges system departs from aluminium powder drop down onto work autoclave body bottom from deposition anode, opening product offtake discharges high-purity aluminium powder of producing, repeatedly after cyclic deposition reaction, if each ion ratio in working fluid drops to, working fluid is lost activity, so or be to open discharging of waste liquid system waste liquid is discharged to (single kettle), Controlling System is controlled each parts and is again fed in raw material afterwards, batching and deposition procedures, and circulation repeatedly.Be exactly that the communicating passage of opening between work kettle is delivered to (two kettle) in cycle operation kettle by the liquid after deposition reaction, carry out configuration and the mixing of circulation fluid, make working fluid activity recovery and the working fluid of activity recovery inputed to again in the work kettle of deposition again to carry out deposition reaction, until after circulation repeatedly, when after the circulation in cycle operation kettle, ion recovery effects is bad, starting discharging of waste liquid system goes out discharging of waste liquid, and from weighing, batching and dress liquid, deposition, cyclic deposition and discharging of waste liquid move in circles again, constantly prepare high-purity aluminium powder.Certainly in all processes on-line detecting system detect in real time every data and by this data transmission to Controlling System, facilitate Controlling System to control each system works high purity aluminium powder can be realized.The preparation apparatus of high-purity aluminium powder like this with respect to the advantage of prior art is: (1) can directly extract rafifinal powder from aluminum chloride, and technical matters route is short, and cost is low; (2) preparation apparatus on-line monitoring system can detect circulation fluid and working fluid change of component in real time; (3) the working fluid reusable edible that preparation apparatus is used, can utilize inactivation working liquid as the energy storage material of the energy capable of circulation; (4) in electrodeposition process, utilize the number of ions kept in balance of metallic cation number that online measuring technique adds and negative electrode absorption, can consume less or consumable anode material not substantially; (5) whole aluminium powder form production process environmental protection, there is no environmental pollution, low cost and reduce power consumption; (6) preparation apparatus is totally-enclosed, quality product is high, have full automatic control function.
Accompanying drawing explanation
The schematic diagram of one of the high-purity aluminium powder preparation apparatus of Fig. 1 the utility model embodiment.
The high-purity aluminium powder preparation apparatus of Fig. 2 the utility model embodiment Controlling System control flow block diagram.
The high-purity aluminium powder preparation apparatus of Fig. 3 the utility model embodiment manually deposits FB(flow block).
The high-purity aluminium powder preparation apparatus of Fig. 4 the utility model embodiment autodeposition FB(flow block).
Figure number explanation
1, circulation spectrum detecting head, 2, circulation fluid level sensor, 3, circulation kettle, 4, circulating-heating warmer, 5, charging opening 1,6, rate of flow meter 1,7, charge pump 1,8, feeding chamber, 9, material level sensing 2,10, charge pump 2,11, rate of flow meter 2,12, charging opening 2,13, recirculating still wear ring/nitrogen outlet, 14, circulation kettle cover, 15, circulating pressure sensor, 16, circulation magnetic force stirrer, 17, circulation stirring bar, 18, nitrogen pressurization mouth 1,19, upper cycling mouth, 20, rate of flow meter 3,21, circulating temperature sensor, 22, deposition ion generator, 23, cocycle pump, 24, deposition pressure sensor, 25, deposition stirrer, 26, deposition agitator arm, 27, sedimentary deposit tank upper cover, 28, nitrogen pressurization mouth 2,29, sedimentary deposit tank wear ring/nitrogen outlet, 30, nitrogen force (forcing) pump, 31, nitrogengas cylinder, 32, deposition circuit, 33, deposition controller, 34, deposition spectrographic detection head, 35, deposit fluid level sensor, 36, Online Monitoring Control device, 37, power supply netting twine, 38, industrial power, 39, depositing temperature sensor, 40, on-line monitoring system, 41, deposition working electrode, 42, deposition agitating vane, 43, deposition working fluid, 44, deposition tank body, 45, products export, 46, discharging switch electromagnetic valve, 47, ultrasonic vibration head, 48, deposition anode, 49, deposition heating warmer, 50, lower circulation port, 51, cycling switch magnetic valve, 52, lower circulation tube, 53, lower recycle pump, 54, circulation stirring blade, 55, deposition cycle liquid, 56, end liquid discharging tube, 57, rate of flow meter 4,58, tapping pump, 59, tap hole, 60, monitoring/control interface, 61, automatic control system, 62, two-position controller.
Embodiment
Fig. 1 to Fig. 4 below in conjunction with accompanying drawing is described in further detail high-purity aluminium powder preparation apparatus of the present utility model.
High-purity aluminium powder preparation apparatus of the present utility model, please refer to Fig. 1 to Fig. 4, comprises charging system, work kettle system, rare gas element input system, heating and thermal insulation system, stirring system, power supply system, deposition circuit, on-line detecting system, Controlling System, product is discharged system and discharging of waste liquid system, described work kettle system respectively with charging system, rare gas element input system, power supply system, deposition circuit 32, on-line detecting system, Controlling System, the product system of discharging is connected with discharging of waste liquid system, and described stirring system lower part is arranged in described work kettle system, and described heating and thermal insulation system is arranged on described work kettle system outside, described Controlling System respectively with charging system, work kettle system, rare gas element input system, detection system, heating and thermal insulation system, stirring system, power supply system, deposition circuit, on-line detecting system, product is discharged system and is connected with discharging of waste liquid system, and described work pot systems turnkey is drawn together work kettle, deposition working electrode 41 and deposition anode 48, described deposition working electrode 41 and deposition anode 48 are all electrically connected to described deposition circuit 32, in described work kettle, have working fluid 43 and circulation fluid 55, described power supply system gives by power supply netting twine 37 charging system being attached thereto, work kettle system, rare gas element input system, detection system, heating and thermal insulation system, stirring system, deposition circuit 32, on-line detecting system, Controlling System, product is discharged system and discharging of waste liquid system power supply, and described feeding device comprises at least two feeding chambers 8, and described feeding chamber 8 is communicated with described work kettle by charge pump 7 and 9, and organic generation halogen is housed respectively in described feeding chamber, aluminum chloride raw material and toluene, described on-line detecting system comprises spectrographic detection head, liquid level sensor, pressure transmitter and temperature sensor, described detection system is all arranged in described work kettle, in described work kettle, be provided with ion generator 22, described product discharge system comprises ultrasonic vibration 47 and is arranged on the product offtake 45 of described work autoclave body bottom, described discharging of waste liquid system is the end liquid discharging tube 56 that comprises tapping pump 58 and be arranged on described work autoclave body bottom, and described work kettle at least comprises a reaction kettle body.Like this, charging system for adding needed raw material and preparing burden and dosing in work kettle in work kettle system, work kettle is under the effect of Controlling System or as recirculating still or as deposition kettle, can also be the circulation kettle 3 can break-make connecting and the deposition kettle 44 that work kettle itself comprises connection, when work kettle is circulation kettle 3, after discharging bin 8 dischargings, in circulation kettle 3, be configured as circulation fluid 55, for looping depositing treatment process after liquid mixing after the deposition with depositing in kettle 44, and work kettle is while depositing kettle 44, on-line detecting system detects the temperature of this deposition kettle 44, pressure, the component of liquid level and the interior deposit fluid of deposition kettle is also transmitted above-mentioned detected value to Controlling System, after Controlling System is compared the detection data that receive and predetermined value scope, when if indices does not reach the standard that starts deposition, Controlling System heating and heat-insulating device is started working and work kettle is heated to preset temperature and starts insulation so, Controlling System startup rare gas element input system starts to input inert gas warranty work kettle internal pressure in work kettle and reaches predetermined range value, can start ion generator 22 and supplement ionic concn simultaneously, or Controlling System starts to start charging system and in work kettle, adds wherein a kind of material or two kinds of materials according to the flow after calculating, so that being controlled at, the component of the interior liquid of work kettle is suitable for deposition, when if indices all reaches the standard that starts deposition, Controlling System is controlled 32 startups of deposition circuit so, deposition working electrode 41 and deposition anode 48 are started working, aluminium powder through deposition reaction is deposited in deposition anode 48, aluminium powder in deposition anode 48 reaches certain thickness, starting ultrasonic vibration 47 that product discharges system departs from aluminium powder drop down onto work autoclave body bottom from deposition anode 48, opening product offtake 45 discharges high-purity aluminium powder of producing, repeatedly after cyclic deposition reaction, if each ion ratio in working fluid 43 drops to, working fluid 43 is lost activity, so or be to open discharging of waste liquid system waste liquid is discharged, to stop deposition entering the activity (single kettle) that circulating process adds supplementary material and stirs the liquid 43 of resuming work, Controlling System is controlled and is again carried out deposition procedures afterwards, and circulation repeatedly.Be exactly that the communicating passage of opening between work kettle is delivered to the liquid after deposition reaction in cycle operation kettle 3 (two kettle), carry out configuration and the mixing of circulation fluid 55, make working fluid 43 activity recoveries and the working fluid of activity recovery 43 inputed to again in the work kettle 44 of deposition again to carry out deposition reaction, until after circulation repeatedly, when after the circulation in cycle operation kettle 3, ion recovery effects is bad, starting discharging of waste liquid system goes out discharging of waste liquid, and from weighing, batching and dress liquid, deposition, circulation, deposition and discharging of waste liquid move in circles again, constantly prepare high-purity aluminium powder.Certainly in all processes on-line detecting system detect in real time every data and by this data transmission to Controlling System, facilitate Controlling System to control each system works high purity aluminium powder can be realized.The preparation apparatus of high-purity aluminium powder like this with respect to the advantage of prior art is: (1) can directly extract rafifinal powder from aluminum chloride, and technical matters route is short, and cost is low; (2) preparation apparatus on-line monitoring system can detect circulation fluid and working fluid change of component in real time; (3) the working fluid reusable edible that preparation apparatus is used, can utilize inactivation working liquid as the energy storage material of the energy capable of circulation; (4) in electrodeposition process, utilize the number of ions kept in balance of metallic cation number that online measuring technique adds and negative electrode absorption, can consume less or consumable anode material not substantially; (5) whole aluminium powder form production process environmental protection, there is no environmental pollution, low cost and reduce power consumption; (6) preparation apparatus is totally-enclosed, quality product is high, have full automatic control function, has manual single step execution pattern simultaneously, can manually control and carry out which single operation.In addition, aluminium technical powder metallurgy and unicircuit industry be it is generally acknowledged: elementary aluminium powder form: aluminium content 99.00-99.85%, refined aluminium powder: aluminium content 99.95-99.995% (3N-4N), high-purity aluminium powder: aluminium content 99.999-99.9999% (5N-6N), ultra-pure aluminium powder: more than aluminium content 99.99999%>6N, by equipment of the present utility model and method, can on material purity basis, improve 1-2 the order of magnitude, if 99.0%, obtaining powder-product purity, material purity reaches 99.9-99.99% to I haven't seen you for ages.
High-purity aluminium powder preparation apparatus of the present utility model, please refer to Fig. 1 to Fig. 4, on the basis of previous technique scheme, can be specifically that described work kettle comprises circulation kettle 3 and the deposition kettle 44 can break-make being communicated with, between described circulation kettle 3 and described deposition kettle 44, by cocycle system and the lower recycle system, be communicated with, described ion generator 22 is arranged in described cocycle system, described circulation kettle 3 is connected with described charging system, in described circulation kettle 3, there is circulating liquid 55, in described deposition kettle 44, be provided with working fluid 43, deposition working electrode 41 and deposition anode 48, in described circulation kettle 3 and described deposition kettle 44, be provided with stirring system, temperature inductor, pressure inductor, spectrographic detection head and liquid level sensor, described circulation kettle 3 and described deposition kettle 44 outsides are provided with heating and thermal insulation system, described circulation kettle 3 is all communicated with and is all connected with power supply system with Controlling System with rare gas element input system with described deposition kettle 44 tops, described discharging of waste liquid system is arranged at described recirculating still 3 body bottoms, described product discharge system is arranged at described deposition kettle 44 bottoms.In the technical program, work kettle is two, is respectively circulation kettle 3 and deposition kettle 44, and the kettle 3 that wherein circulates is for configuration cycles liquid 55, and deposition kettle 44 is produced aluminium powder for deposition.Two work kettlies configuration, two cover on-line detecting system and stirring systems, circulate simultaneously and can break-make connect between kettle 3 and deposition kettle 44, by cocycle system, can break-make be connected with the lower recycle system between the two, when when needs, both are communicated with, in circulation kettle, 3 circulation fluid 55 constantly enters in deposition kettle 44 and carries out deposition reaction, constantly in deposition anode 48, deposit high-purity aluminium powder, liquid level in liquid level sensor and spectrographic detection head detect recirculating still and deposition still declines, after component ionic concn drops to below preset value, automatic or manual operation control system is carried out charging process or is carried out discharging of waste liquid operation.When needs carry out discharging of waste liquid operation, under opening circulation kettle 3 and depositing between kettle 44, between the recycle system, be communicated with, circulation fluid 55 and working fluid 43 are all disposed to this device external by the discharging of waste liquid system of circulation kettle 3 bottoms.High-purity aluminium powder of producing falls to reaction kettle body 44 bottoms outside by product discharger device for transferring under the effect of ultrasonic vibration 47.The high purity aluminium powder incessantly that can circulate successively like this, the single work kettle of efficiency ratio of producing of high-purity aluminium powder exceeds more than at least one times.Further preferred technical scheme is that described cocycle system is provided with pumping installation and under meter, and the described lower recycle system is provided with pumping installation and discharging switch electromagnetic valve 46.Like this, the pumping installation of cocycle system is pumped to the circulation fluid in circulation kettle 3 55 in deposition kettle 44 and carries out deposition reaction, under meter is for detection of the amount that pumps into the circulation fluid 55 in deposition kettle 44, pumping installation in the lower recycle system by the working fluid 43 of the deposition interior generation of kettle 44 complete deposition reaction pump in circulation kettle 3 with circulation kettle in circulation fluid 3 and the mixing of materials that newly adds improve ionic concn and after the effect of ion generator 22, be again pumped to deposit in kettle 44 after stirring and carry out deposition reaction, so high-purity aluminium powder is prepared in circulation.And the discharging switch electromagnetic valve 46 carrying out in the recycle system at present when deposition reaction can be in closing condition, cut off circulation kettle 3 and deposit being communicated with of kettle 44 lower parts, guarantee that interior working liquid 43 deposition reactions of deposition kettle 44 are complete, can certainly not cut off, make to deposit kettle 44 and carry out deposition reaction simultaneously and deposition working fluid 43 after reaction is delivered to the interior activity recovery of circulation kettle 3.
High-purity aluminium powder preparation apparatus of the present utility model, please refer to Fig. 1 to Fig. 4, on the basis of foregoing technical scheme, can also be that work kettle comprises still lower body and kettle cover 14 and 27 that cover, described still lower body and the described kettle cover place of covering are provided with tightness system 13 and 29.Ectocine is avoided in temperature, pressure and reaction in the still lower body covering like this and kettle cover assurance circulation fluid 55 and/or working fluid 43.And the advantage of tightness system be pressure in assurance work kettle in basicly stable state, avoid outside air to enter and blast etc. dangerous.Can be that described stirring system comprises stirrer 16 and 25, agitator arm 17 and 26 and agitating vane 54 and 42, described agitator arm is connected with described stirrer, described agitating vane is positioned at the bottom of described agitator arm, and described agitating vane is positioned at described work kettle middle part with upper/lower positions.The advantage that stirring system is set is while having fed in raw material rear and deposition reaction, the abundant agitation cycle liquid 55 of difference and working fluid 43, each ion is distributed in circulation fluid and working fluid more even, and then reach better dosing effect and better deposition reaction effect, improve the production efficiency of high-purity aluminium powder.Can also be between described charging system and described work kettle, between described discharging of waste liquid system and described work kettle, between described rare gas element input system and described work kettle, be provided with pumping installation and under meter.So not only improved reinforced efficiency, discharging of waste liquid efficiency and pressurization efficiency, can detect the amount that adds material simultaneously, the amount of discharging of waste liquid amount and the rare gas element adding, wherein rare gas element can be nitrogen.Can also be in described feeding chamber 8, to be provided with a material sensor 9, described work autoclave body bottom be provided with switch electromagnetic valve.When a position material sensor 9 detects at the interior material of feeding chamber 8 lower than preset value time, the acoustooptic alarm system being attached thereto starts to report to the police like this, until user's response, when material adds after feeding chamber 8, feeding chamber 8 again starts and works on.And the switch electromagnetic valve that work autoclave body bottom arranges is for discard solution discharge port 59 and/or the product discharge outlet 45 of opening and closing work autoclave body bottom, be convenient to the discharge of discharging of waste liquid and/or high-purity aluminium powder.
The method of utilizing aforesaid high-purity aluminium powder preparation apparatus high purity aluminium powder of the present utility model, please refer to Fig. 1 to Fig. 4, comprises the following steps:
A. starting outfit, starts Controlling System, starts automatic control mode or single step execution pattern;
B. select automatic control mode: the position that detects material in feed bin, when wherein any one is lower than initial setting alarming value, prompting supplements material, when both are during all over initial setting alarming value, discharging bin is prepared discharging, circulation fluid in spectrographic detection head testing kettle in on-line detecting system and the chemical composition of working fluid, by temperature in temperature sensor testing kettle, with the pressure in pressure transmitter testing kettle, liquid level with liquid level sensor testing kettle internal recycle liquid and working fluid, determine feed bin by mass transport to work kettle preparing burden successively under Controlling System is controlled, dosing and dress liquid operation, the stirring system of Controlling System control afterwards starts to stir, ion generator work supplements ionic concn, after reaching predetermined reaction conditions, working fluid deposits in work kettle, deposition circuit drives deposition working electrode and deposition anode effect, and in deposition anode, deposit high-purity aluminium powder, and high-purity aluminium powder of producing by the discharge of product discharge system, working fluid after use is circulated in work kettle and circulates, feeding device stirs after supplementing and adding material, working fluid is replied after activity to be entered in work kettle again and deposits, the working fluid in kettle of so working after circulation at least 6 times discharges by discharging of waste liquid system as waste liquid, in this process, if pressure transmitter detects work kettle, internal pressure is less than normal, Controlling System is inputted the pressure in rare gas element increase work kettle by controlling rare gas element input system in work kettle, the component of liquid in spectrographic detection head detects work kettle, and Controlling System all starts toward reinforced in work kettle according to one of them or both in this compositional selecting discharging bin,
C. selected single step execution pattern: detect the position of material in feed bin, when wherein any one is lower than initial setting alarming value, prompting supplements material, carries out merely charging process, when both are during all over initial setting alarming value, discharging bin preparation discharging, circulation fluid in spectrographic detection head testing kettle in on-line detecting system and the chemical composition of working fluid, by temperature in temperature sensor testing kettle, with the pressure in pressure transmitter testing kettle, liquid level with liquid level sensor testing kettle internal recycle liquid and working fluid, determine feed bin by mass transport to work kettle preparing burden separately under Controlling System is controlled, dosing and dress liquid operation, Controlling System is controlled separately stirring system and is started to stir afterwards, control separately ion generator work and supplement ionic concn, after reaching predetermined reaction conditions, Controlling System is controlled separately working fluid and carry out deposition procedures in work kettle, deposition circuit drives deposition working electrode and deposition anode effect, and in deposition anode, deposit high-purity aluminium powder, Controlling System starts separately product discharge system and carries out product discharge operation afterwards, after deposition, deactivated deposition working fluid enters the recycle system again, automatic controlling system charging system starts to feed in raw material, make working fluid activity recovery, in work kettle, carry out deposition reaction more afterwards, so the circulation working fluid in kettle of working afterwards at least 6 times discharges by the discharging of waste liquid system of independent startup as waste liquid, during the course, if pressure transmitter detects work kettle, internal pressure is less than normal, manually control rare gas element input system and input the pressure in rare gas element increase work kettle in work kettle, the component of liquid in spectrographic detection head detects work kettle, and according to this component, manually select one of them or both in feed bin and all start toward reinforced in work kettle.
Through above-mentioned steps, can directly extract rafifinal powder, cost is low, produce in process and can detect in real time circulation fluid and working fluid change of component, some work liquid can be recycled, save the energy, reduce or do not consume deposition anode material, environmental protection, there is no environmental pollution, high-purity aluminium powder rate of output is high.That prior art is produced the long energy consumption of aluminium powder form technical matters route is high, needs through bauxite-> Baeyer alkaline process-> Yangization Lv – > electricity Xie Lv – > ball milling powder process method or powder by atomization Fa – > aluminium powder form; And equipment provided by the utility model and method and technology route are short: flyash or bauxite-> Suan Fa – > Lvization Lv – > electricity Chen Ji – > aluminium powder form.Only from producing per kilogram energy consumption used, just can find out the utility model and traditional method comparison, efficiency improves at least 15%, and cost ratio will be over 15%, and concrete data refer to table 5.
The method of utilizing aforesaid high-purity aluminium powder preparation apparatus high purity aluminium powder of the present utility model, please refer to Fig. 1 to Fig. 4, on the basis of previous technique scheme, can also be the former proportioning of expecting: aluminum chloride and halogenated organic salt form according to weight percent 1.5-2.5:1 configuration, described cycle stock: aluminum chloride and halogenated organic salt form according to weight percent 0.08-0.16:1 configuration, initial liquid: toluene forms according to weight percent 0.036:1 configuration with just expecting; Circulation fluid: toluene and cycle stock form according to weight percent 0.1-0.3:1 configuration, toluene can add in work kettle from the later stage from one of them feeding chamber, also can set up separately in addition a feeding chamber and charge pump, charging opening, facilitates toluene to add in work kettle again.Toluene can be at halogenated organic salt and aluminum chloride mix and blend after one and a half hours, and the charging opening by feeding chamber adds under the effect of charge pump, and add-on is controlled by weight percentage and referred to table 1, and after toluene adds initial liquid, remix stirs half an hour.Experiment shows to add the electrolyte prescription after toluene, can effectively reduce the viscosity of electrolytic solution, improves electric conductivity, reduces the granularity of metal-powder, thereby has improved the quality of powder-product.
Certainly in the time of can also being described deposition reaction, bath voltage is 2.1-3V, and reference voltage is-2.1-3.0V that constant current environment is 200-600A/m 2, in work kettle, depositing temperature is 70-90 ℃, and work kettle internal pressure is 0.5Mpa, and the deactivated condition of working fluid is ALCL 7 -: ALCL 4 -ionic group ratio is less than 0.3-1; Circulation fluid activity recovery condition is ALCL 7 -: ALCL 4 -ionic group ratio is greater than 1-1.5.ALCL 7 -ionic group is active electrolytic solution groundwork group, and ALCL4-radical ion figure is the basic condition of electrolytic solution generation electrochemical reaction, on-line monitoring equipment can calculate the activity value of these two groups qualitative or quantitatively, from both ratios, can intuitively reflect the activity of deposition working fluid, for circulating or depositing, provide decision data foundation.
Concrete enforcement one
High-purity aluminium powder preparation apparatus of the present utility model comprises
Two feeding chambers 8, for depositing halogenated organic salt and aluminum chloride raw material, each feed bin is provided with a material sensor 9;
Two charge pumps (7 and 10), for the raw material of feeding chamber is pumped in circulation kettle 3, when preparation circulation fluid 55 or circulation fluid 55 recycle, the order of response automatic control system 61, selection or one of them charge pump of single selection quantitatively, add production desired raw material by two charging openings (5 and 12) to circulation kettle 3 simultaneously;
Four rate of flow meter (6,11,20 and 57), calculate for the flow measurement of each system, are respectively used to the metering of halogenated organic salt, aluminum chloride, deposition working fluid flow and inactivation discharging of waste liquid;
Two spectrographic detection heads (being respectively circulation spectrum detecting head 1 and deposition spectrographic detection head 34), wherein circulate spectrum detecting head 1 for detecting in real time the change of component of circulation kettle 3 circulation fluids 55, and deposition spectrographic detection head 34 is for detecting in real time the change of component of deposition kettle 44 working fluids 43;
Two liquid level sensors (circulation fluid level sensor 2 and deposit fluid level sensor 35), for the liquid position height in detection equipment still, circulation fluid level sensor 2 is for detecting in real time the liquid level change of circulation kettle 3 circulation fluids 55, and deposit fluid level sensor 35 is for detecting in real time the liquid level change of deposition kettle 44 working fluids 43;
Two kettlies (circulation kettle 3 and deposition kettle 44), for storing the liquid material of production process, circulation kettle 3 is for depositing circulation fluid 55, and deposition kettle 44 is for depositing working fluid 43;
Two heating warmers (circular heating warmer 4 and deposition heating, temperature keeping device 49), heating and insulation for equipment, circular heating warmer 4 is for the heating and thermal insulation of the kettle 3 that circulates, deposition heating, temperature keeping device 49 is for depositing the heating and thermal insulation of kettle 44, and heating warmer is wrapped in respectively on circulation kettle 2 and deposition kettle 44 outer walls;
Two kettle cover wear rings (circulation kettle cover wear ring 13 and deposition kettle cover wear ring 29), sealing for work kettle, circulation kettle cover wear ring 13 is for the nitrogen-sealed of the kettle 3 that circulates, deposition kettle cover wear ring 29 is for depositing the inert gas seal (being nitrogen-sealed) of kettle 44, prevent nitrogen leakage, also embed two nitrogen discharge mouths, the discharge of non-purity nitrogen mixed gas when working kettle initial start;
Two kettle covers (circulation kettle cover 14 and deposition kettle cover 27), for the capping sealing of the kettle of working, to form sealing, clean and high-purity production atmosphere, circulation kettle cover 14 adds a cover to circulation kettle 3, and deposition kettle cover 27 is for depositing kettle 44;
Two pressure transmitters (circulating pressure sensor 15 and deposition pressure sensor 24), for the nitrogen pressure in detection equipment, circulating pressure sensor 15 is for the pressure detection of the kettle 3 that circulates, and deposition pressure sensor 24 is for depositing the pressure detection of kettle 44;
Two magnetic stirrers (circulation magnetic force stirrer 16 and deposition magnetic stirrer 25) (can certainly adopt other stirring system), stirring for material in work kettle, to accelerate chemical reaction velocity, increase reaction homogeneity, circulation magnetic force stirrer 16 is for the circulation fluid 55 of agitation cycle kettle 3, deposition magnetic stirrer 25 is for depositing the stirring of the working fluid 43 of kettle 44, with magnetic stirrer supporting also have two agitator arms (circulation stirring bar 17 and deposition agitator arm 26) and two agitating vanes (circulation stirring blade 42 and deposit agitating vane 54);
Two nitrogen pressurization mouthful (circulating nitrogen gas pressurization mouthfuls 18 and the pressurization of deposition nitrogen mouthful 28), for pass into inert protective gas (being nitrogen in the present embodiment) to two work kettlies, the oxidation source that in isolated production process, material contacts with air, circulating nitrogen gas pressurization mouth 18 is for giving circulation kettle 3 logical pressurized nitrogen, and deposition nitrogen pressurization mouth 28 is for giving deposition kettle 44 logical pressurized nitrogen;
Two recycle pumps (cocycle pump 23 and lower recycle pump 53), circulation for material between work kettle, the initialization liquid configuring or circulation fluid 55 by cocycle pump 23, be driven in deposition kettle 44 by upper cycling mouth 19 and upper circular tube, also can be sent back to used deposition working fluid 43 in circulation kettle 3 by lower recycle pump 53, lower circulation port 50, lower circulation tube 52;
Ion generator 22, for depositing the activation of working fluid 43 metal ions, improves ionic concn;
A nitrogen force (forcing) pump 30, for providing inert protective gas (being nitrogen in the present embodiment) to organizing altogether kettle, it is pressed into the nitrogen of nitrogengas cylinder 31 in circulation kettle 3 and deposition kettle 44, prevents that the oxidation of working fluid 43 in deposition process and impurity from entering;
Deposition circuit 32, for providing of the deposition process electrical parameter of work kettle, under the control of deposition controller 33, provide suitable working current, deposition voltage and reference voltage and (refer to follow-up table 1, table 2 and table 3, deposition working fluid 43 is under terminal voltage effect, deposition working electrode 41 and deposition anode 48 are by deposition working fluid 43 generation currents, the interior generation electrochemical reaction of working fluid 43 in deposition kettle 44, thus can namely deposit the depositing crystalline that obtains high pure metal aluminium powder form on working electrode 41 at negative electrode;
Industrial power 38, for providing power supply to equipment components and system, by power supply netting twine 37, give circulation kettle 3, deposition kettle 44, temperature sensor (21 and 39), the parts power supplies such as pressure transmitter (15 and 24) sensor, spectrum probe (1 and 34), on-line monitoring system 40 and automatic control system 61.
Further, this preparation apparatus also comprises:
On-line monitoring system 40, online detection for physical/chemical amount in equipment, in Fig. 1, dot, it includes circulation kettle 3 and the interior rate of flow meter (6 of deposition kettle 44, 11, 20 and 57), level sensor (2 and 35), temperature inductor (21 and 39), pressure inductor (15 and 24) and spectrographic detection head (1 and 34), can detect all above-mentioned data item by real-time online, these data of Online Monitoring Control device 36 acquisition process, by monitoring/controlling network interface 60 can carry out network communication and data sharing with automatic control system 61, detected result is sent to automatic control system 61, reinforced start/stop is provided to the automatic control system 61 of preparation apparatus, circulation kettle 3 is heated/is incubated, circulation stirring start/stop, recycle pump is worked/is stopped, nitrogen pressurization/pressurize/stop, deposition stirs start/stop, deposition start/stop, circulation start/stop, ultrasonic vibration start/stop, the decision data of the action such as tapping start/stop.
Further, this preparation apparatus also comprises:
Automatic control system 61, automatic control for equipment, in Fig. 1, with two-dot chain line, represent, the equipment unit of institute's control linkage comprises charge pump (7 and 10), stirrer (16 and 25), upper and lower recycle pump (23 and 53), nitrogen force (forcing) pump 30 and tapping pump 58, receive after the status data of on-line monitoring system, under the control of two-position controller 62, complete reinforced start/stop, recirculating still is heated/is incubated, circulation stirring start/stop, recycle pump is worked/is stopped, nitrogen pressurization/pressurize/stop, deposition stirs start/stop, deposition start/stop, circulation start/stop, ultrasonic vibration start/stop, the action directive of the switching nodes such as tapping start/stop.
Described preparation apparatus further comprises:
Cycling switch magnetic valve 51, for the outer discharge pipe of equipment opening/closing deposition kettle liquid, when needing circulation time, working fluid 43 opens this valve, interpolation along with new working fluid 43, deposition working fluid 43 is recycle pump 53 under action of gravity or under using, lower circulation port 50 and lower circulation tube 52 will be driven in circulation kettle 3 with the working fluid 43 of crossing, at this, add new aluminum chloride raw material stirring reaction, to recover the activity of circulation fluid 55, under the control of Controlling System 61 flow processs, when need of production, by cocycle pump 23, return the circulation that deposition kettle 44 is realized working fluid 43 again, certainly all working liquid in deposition kettle 44 all can be pressurizeed to input in circulation kettle 3 and circulate, also can deposit kettle 44 and carry out deposition reaction on one side, the working fluid that after reaction, activity reduces sinks down into the Lower Half office of deposition kettle 44 under action of gravity, the lower recycle pump of this place's startup is evacuated to circulation kettle 3 by this some work liquid and carries out activation recovering, working fluid after recovery is again entered in deposition kettle 44 and is deposited by cocycle system, deposit and circulate and can carry out simultaneously,
Ultrasonic vibration 47, for dropping to products export 45 by the aluminium powder form vibration being deposited on deposition working electrode 41;
Discharging switch electromagnetic valve 46, emits rafifinal powder-product for opening products export 45;
Tapping pump 58, discharges the inactivation circulation fluid 55 repeatedly recycled for the kettle of working, this pump work when maintenance of equipment maybe needs to empty in equipment liquid, and waste material is discharged through tap hole 59 by end liquid discharging tube 56.
Described on-line monitoring system 40 also further comprises:
The online detection of working fluid 43 and circulation fluid 55 chemical composition spectrum, qualitative and quantitative analysis for detection of material chemical composition variation tendency and principal element aluminum metal in work kettle, in the still that spectrographic detection head (circulation spectrum detecting head 1 and deposition spectrographic detection head 34) is collected, material spectrum change real time data is sent into online detection controller 36, according to the characteristic spectrum of liquid element and Quantitative Analysis Model, calculate the concentration of principal element aluminium, the variation tendency of circulation fluid 55 and working fluid 43, the calculation result of on-line monitoring system 40 can be by detection/control interface 60 and automatic control system 61 data sharings, each system of instruction control and parts that Controlling System 61 is sent response according to above-mentioned data start or close.
Concrete automatic control system 61 control strategies comprise, deposit in kettle 44 and the activation of the interior liquid ions functional group of circulation kettle 3 and supplementary, make deposition consumes metal ion and supplementary ion kept in balance, few consumption or consumable anode material not substantially, and reach the object of directly producing of metallic aluminium powder, while allowing circulation fluid 55 activity recovery in circulation kettle 3, it is the characteristic peak projection reach the process of maximum boundary value gradually of this liquid, these data are eigenvalue of maximum of finished product working fluid, concrete active group ratio refers to table 3, in the interior deposition process of deposition kettle 44, follow aluminum ion in the deposition of negative electrode, deposit fluid 43 or the acidity that is referred to as free state working fluid 43 decline gradually, the characteristic peak that shows as working liquid is flat gradually, when principal character peak low during to minimum work threshold value, the working liquid 43 of deposition kettle 44 can be put in circulation kettle 3 and recycle processing, also can make deposition and supplementary new liquid make active ion concentration remain in rational working range simultaneously, at this moment aluminum ion in deposition the depositing crystalline reach certain thickness progressively of the deposition working electrode 41 in still 44, rafifinal powder-product drops from deposition working electrode 41 by ultrasonic vibration 47 vibration or physical method, and finally from products export 45, obtain and discharge.
Or further, described automatic control system 61 also comprises: automatic control system 61 servers and watch-dog, in the database of equipment, recorded the historic records of each component working state of preparation apparatus and online detected result, can display equipment state and operation steps on watch-dog, under demonstration information indicating, can easily complete the operation to preparation apparatus, watch-dog can show the operating parameter of preparation apparatus, the on off state of historic records and equipment, each switch comprises charge pump (7 and 10), upper and lower recycle pump (23 and 53), nitrogen pump 30, tapping pump 58, stirrer (16 and 25), ion generator 22, discharging switch electromagnetic valve 46 and cycling switch magnetic valve 51, the material position of display equipment, comprise discharging bin material level 9, circulation fluid level sensor and deposition sensor (2 and 35), in circulation kettle 3, in circulation fluid 55 and deposition kettle 44, the chemical group of working fluid 43 is graded.
As Fig. 2, the utility model provides the method for utilizing above-mentioned rafifinal powder preparation apparatus high purity aluminium powder form, and wherein the proportion scale of working fluid 43, circulation fluid 55 is in Table 1, and in deposition reaction process, physical parameter is in Table 2, electrolytic solution inactivation and circulation activity recovery parameter are in Table 3
The utility model provides the method for utilizing above-mentioned rafifinal powder preparation apparatus high purity aluminium powder form, comprises the steps:
A. starting outfit Controlling System, starts integral device, and power supply system starts comprehensive power supply;
B, automatic control system 61 start automatic control mode or manual single step execution pattern as required;
C, if select to start automatic control mode, automatic control system 61 is called level sensing transducer 9 automatically and continuously, rate of flow meter, circulation kettle 3, deposition kettle 44, temperature sensor, pressure transmitter, spectrographic detection head, liquid level sensor, each pump housing, cocycle system and the lower recycle system, product is discharged system, deposition circuit, rare gas element input system, discharging of waste liquid system, heating and thermal insulation system, stirring system and work kettle system start or close, and then complete, reinforced, batching, dress liquid, deposition, circulation, the operations such as product discharge and discharging of waste liquid, automatically complete from being weighed to and discharge a plurality of continuous production stages of rafifinal powder-product, and be cycled to repeat and carry out, realize producing of rafifinal powder,
If D. select manual one-step control pattern, manually boot the button of concrete single step operation, can Controlling System 61 each parts and the systems of controlling high-purity aluminium powder preparation apparatus of the present utility model start or stop, single stage ground is realized and is surveyed material level, batching, dosing, dress liquid, deposition, circulates, goes out product, discharging of waste liquid operation separately;
E. be finished after automatic control mode or manual one-step control pattern, whether system, in standby treated state, is waited for and is continued to loop or closing device.
Or further, automatic control mode comprises following operation: as Fig. 4,
Autodeposition starts order to be carried out: survey material level calling data; After after → no problem, stocking process starts, dress is just expected for the first time, automatic mounting cycle stock for the second time; → dosing operation starts, joins for the first time after initial liquid, automatically joins for the second time circulation fluid; → dress liquid operation starts, fills for the first time after initial liquid, for the second time automatic mounting circulation fluid; → deposition procedures starts, automatically enters cyclic deposition reaction process; → discharge opeing operation starts, automatically enters pressurization discharge opeing process, passes into nitrogen radioactive waste liquid side by side; → go out product sequence start, automatically enter ultrasonic vibration operation by metallic aluminium powder be vibrated to deposition kettle 44 bottoms; → tapping operation starts, cyclic deposition starts discharging of waste liquid operation 6 times afterwards automatically; After → tapping, metallic aluminium powder is discharged from deposition kettle 44 bottoms.
Or further, manually one-step control pattern comprises: as shown in Figure 3, and after manually deposition starts; Manually boot as required single operation, the real-time detector data that automatic control system is collected according to on-line detecting system, control the kettle 3 that respectively circulates, deposition kettle 44, temperature sensor, pressure transmitter, spectrographic detection head, liquid level sensor, each pump housing, cocycle system and the lower recycle system, product and discharge system, deposition circuit, rare gas element input system, discharging of waste liquid system, heating and thermal insulation system, stirring system and work kettle system start or close, and then realize the operation of selected one step.Concrete analysis: survey material level operation if select, survey two feeding chamber 8 material levels; If there is one to start acoustooptic alarm system lower than equipment initial set value alarming value in two bin levels, integral device is in holding state; If selection charging process, first surveys feeding chamber material level; Selection equipment is that dress is just expected or cycle stock now, having filled just expects also do not carry out tapping operation automatic control system automatically control feeding chamber dress cycle stock, otherwise dress is just expected; Dress is just expected, by Alcl 3: the ratio of halogenated organic salt=1.5, the first composition of expecting of preparation; Dress cycle stock, by Alcl 3: the ratio of halogenated organic salt=0.08, preparation cycle stock composition, wherein halogenated organic salt comprises ionic liquid EMIC, ionic liquid BPC, ionic liquid Et3NHCl, ionic liquid TMPAC, halogenated organic salt is liquid EMIC in the present embodiment.If select dosing operation, if dress is just to expect to join initial liquid, the magnetic force circulation stirring machine 16 that starts circulation kettle 3 stirs 2 hours; If dress is that cycle stock is joined circulation fluid, the magnetic force circulation stirring machine 16 that starts circulation kettle 3 stirs after 20 minutes and stops.If what select is dress liquid operation, if dress is initial liquid, till automatic control system 61 startup cocycle pumps 23 install to the deposition interior formulation of kettle 44 position by initial liquid; If dress is circulation fluid 55, start ion generator 22 and upper and lower recycle pump (23 and 53), according to deposition still 44, interior concentration of metal ions adjustment supplements working fluid 43 speed and completes dress liquid.If selection deposition procedures, temperature, pressure, liquid level and the chemical group first detecting according to the on-line detecting system data of grading, sedimentary environment is adjusted, make envrionment temperature, pressure and deposition ionic concn all meet mode of deposition, do not meet and can start respectively heating warmer (4 and 49), nitrogen pump 30, upper and lower recycle pump (23 and 53) and ion generator 22, depositing temperature is controlled to 80 degree, nitrogen pressure and is controlled at 0.5Mpa and controls and deposit ionic concn and meet setting range value.If selected, be independent deposition procedures, automatic control system has deposited rear device standby by the interior active metallic ion of current deposition kettle 44; If selected, be cyclic deposition (default circulation 6 times or setting depositing time), when active A l concentration of metal ions does not meet the demands, start upper and lower recycle pump (23 and 53) and open the supplementary active ion of ion generator 22, cyclic deposition occurs with supplementary new working fluid 43 simultaneously; In deposition process: Controlling System 61 is connected deposition circuit 32, and the electrical parameter that provides refers to table 2, during institute deposit gage, per minute is got primary depositing spectroscopic data, and active A l concentration of metal ions (referring to table 3) meets the demands and continues to deposit; Otherwise deposition end-of-job.If select discharge opeing circulating process, if select gravity discharge opeing to open lower recycle valve 51; If choosing pressurization discharge opeing is closed lower recycle valve 51 and opened lower recycle pump 53 simultaneously, pass into nitrogen pressurization, until liquid is all discharged simultaneously; If select to discharge product sequence, if choose work physical method, all power supplys of closing device, carry out physics row aluminium mode; If select ultrasonic vibration mode, automatic control system 61 is opened ultrasonic vibrations 47 and is obtained high-purity aluminium powder product from products export 45.If select discharging of waste liquid operation, open circulation kettle 3 tapping pumps 58, waste liquid is discharged until circulation kettle 3 is emptying from tap hole 59.
Specific embodiment two
Embodiment bis-is another kind of embodiments of the present utility model, as shown in Figure 1, when circulation fluid 55 and the shared reaction kettle body of deposit fluid (being working fluid 43), powder preparation apparatus can be simplified to single kettle structure by two kettlies, although equipment operating efficiency does not have two kettlies high, single kettle powder preparation apparatus cost simple in structure is low;
Rafifinal powder preparation apparatus, comprising:
Two feeding chambers 8, for depositing halogenated organic salt and aluminum chloride raw material, each feed bin is provided with a material sensor 9;
Two charge pumps (7 and 10), for the raw material of feeding chamber is pumped in circulation kettle 3, when preparation working fluid 43 or circulation fluid 55 recycle, the order of response automatic control equipment, select two or one of them pump of single selection quantitatively simultaneously, by two charging openings (5 and 12), add and produce desired raw material (identical with specific embodiment one herein, feeding chamber is at least two, can be three, the 3rd for adding toluene);
Three rate of flow meter (6,11 and 57), calculate for the flow measurement of equipment, are respectively used to the metering that halogenated organic salt, aluminum chloride and inactivation waste liquid are discharged;
A spectrographic detection head 1, the real-time detection of the working fluid using for the kettle of working or circulation fluid chemistry component;
A liquid level sensor 2, for the liquid position height in detection operations kettle;
A work kettle 3, for the liquid material of device storage production process;
A heating warmer 4, for heating and the insulation of equipment;
A kettle cover wear ring 13, for the sealing of equipment, prevents nitrogen leakage, has also embedded a nitrogen discharge mouth, the discharge of non-purity nitrogen mixed gas during for equipment initial start;
A kettle cover 14 (the deposition circuit on kettle cover 27 is moved on on 14), for the capping sealing of equipment and the installation of deposition circuit, to form sealing, clean and high-purity production atmosphere;
A pressure transmitter 15, for the nitrogen pressure in detection operations kettle;
A magnetic stirrer 16, for the stirring of material in the kettle of working, increases reaction homogeneity to accelerate chemical reaction velocity, with this magnetic stirrer 16 supporting also have agitator arm 17 and agitating vane 54;
A nitrogen pressurization mouth 18, passes into inert protective gas for giving in work kettle, the oxidation source that in isolated production process, material contacts with air;
A nitrogen force (forcing) pump 30, for providing inert protective gas to equipment, it is pressed into the nitrogen of nitrogengas cylinder 31 in equipment still 3, prevents that the oxidation of working fluid in deposition process and impurity from entering;
Deposition circuit 32 (moving on to circulation kettle cover 14 from the deposition kettle cover 27 of Fig. 1), for providing of the deposition process electrical parameter of equipment, under the control of deposition controller 33, provide suitable working current, deposition voltage and reference voltage, deposition working fluid 43 is under terminal voltage effect, deposition working electrode 41 and deposition anode 48 are by deposition working fluid 43 generation currents, in working fluid in equipment kettle 3, there is electrochemical reaction, thereby can namely deposit the depositing crystalline that obtains high pure metal aluminium powder form on working electrode 41 at negative electrode;
Industrial power 38, for providing power supply to apparatus assembly, gives the assembly power supplies such as sensor, spectrographic detection head 1, on-line monitoring system 40 and automatic control system 61 such as work kettle 3, temperature sensor 21, pressure transmitter 15 by power supply netting twine 37.
Further, this is produced system and also comprises: on-line monitoring system 40, and the online detection for physical/chemical amount in equipment, dots in Fig. 1, and connected device has the liquid flow rate (6 in work kettle 3, 11 and 57), liquid level sensor 2, temperature sensor 21, pressure transmitter 15 and working fluid spectrographic detection head 1, obtain the real-time detection of response data item, especially for the interior flow of work kettle 3, liquid level, temperature, the real-time detection of pressure and working fluid component spectra data, these data of Online Monitoring Control device 36 acquisition process, by monitoring/controlling network interface 60 can carry out network communication and data sharing with automatic control equipment 61, detected result is sent to automatic control equipment 61, reinforced start/stop is provided to the automatic control equipment 61 of preparation apparatus, recirculating still is heated/is incubated, circulation stirring start/stop, recycle pump is worked/is stopped, nitrogen pressurization/pressurize/stop, deposition stirs start/stop, deposition start/stop, circulation start/stop, ultrasonic vibration start/stop, the decision data of the action such as tapping start/stop.
This preparation apparatus also comprises: automatic control equipment 61, automatic control for equipment, in Fig. 1, with two-dot chain line, represent, the apparatus assembly of institute's control linkage comprises charge pump (7 and 10), stirrer 16, nitrogen force (forcing) pump 30 and tapping pump 58, receive after the status data of on-line monitoring equipment, under the control of two-position controller 62, complete reinforced start/stop, work kettle 3 is heated/is incubated, circulation stirring start/stop, nitrogen pressurization/pressurize/stop, deposition stirs start/stop, deposition start/stop, circulation start/stop, ultrasonic vibration start/stop, the action control of the switching nodes such as tapping start/stop.
Described preparation apparatus further comprises: ultrasonic vibration 47 (moving on in the deposition kettle by it from Fig. 1 in circulation kettle 3), for the aluminium powder form vibration being deposited on working electrode is dropped to products export; Tapping pump 58, for equipment, discharge the inactivation working fluid 55 repeatedly recycling, this pump work when maintenance of equipment maybe needs to empty in equipment liquid, waste material is discharged through tap hole 59 by end liquid discharging tube 56, also can be used for opening products export powder-product is emitted.
Described on-line monitoring equipment 40 also further comprises: the online detection of working fluid or circulation fluid 55 chemical composition spectrum, qualitative and quantitative analysis for detection of material chemical composition variation tendency in equipment and principal element aluminum metal, in the still that spectrographic detection head 1 is collected, material spectrum change real time data is sent into online detection controller 36, according to the characteristic spectrum of liquid element and Quantitative Analysis Model, calculate the concentration of principal element aluminium, the variation tendency of cycle working fluid 55 or deposition working fluid 43, the calculation result of on-line monitoring equipment 40 can be by detection/control interface 60 and automatic control equipment 61 data sharings.
Described automatic control equipment 61 also further comprises: automatic control equipment 61 control strategies comprise, the activation of the interior liquid ions functional group of equipment still 3 and supplementary, make deposition consumes metal ion and supplementary ion kept in balance, few consumption or consumable anode material not substantially, and reach the object of directly producing of metallic aluminium powder, while allowing circulation fluid activity recovery in recirculating still 3, it is the characteristic peak projection reach the process of maximum boundary value gradually of working fluid, these data are eigenvalue of maximum of finished product working liquid, concrete active group ratio refers to table 3, in deposition still in 3 deposition process, follow aluminum ion in the deposition of negative electrode, deposition working liquid 55 or the acidity that is referred to as free state working fluid decline gradually, the characteristic peak that shows as working liquid is flat gradually, when principal character peak low during to minimum work threshold value, after can increasing aluminum chloride in equipment still, recycle processing, at this moment aluminum ion in deposition the depositing crystalline reach certain thickness progressively of the working electrode 41 in still 44, rafifinal powder-product can obtain from products export 59 by ultrasonic vibration 47 (moving on in equipment still 3) vibration or physical method.
Or further, described automatic control equipment 61 also comprises:
Automatic control equipment 61 servers, watch-dog, in the database of equipment, recorded the historic records of each component working state of preparation apparatus and online detected result, can display equipment state and operation steps on watch-dog, under demonstration information indicating, can easily complete the operation to preparation apparatus, watch-dog can show the operating parameter of preparation apparatus, the on off state of historic records and equipment, switch assembly comprises charge pump (7 and 10), nitrogen pump 30, tapping pump 58, stirrer 16, the material position of display equipment, comprise bin-level (8 and 9), the chemical group of the interior liquid level 2 of circulation kettle 3 and circulation kettle 3 internal recycle or working fluid 55 is graded.
As Fig. 2, the method that the rafifinal powder that the utility model provides is produced, wherein the proportion scale of working fluid, circulation fluid is in Table 1, and deposition physical parameter is in Table 2, and electrolytic solution inactivation and loop parameter, in Table 3, comprise the steps:
Comprise the steps:
A. starting outfit Controlling System, starts integral device, and power supply system starts comprehensive power supply;
B, automatic control system 61 start automatic control mode or manual single step execution pattern as required;
C, if select to start automatic control mode, automatic control system 61 is called level sensing transducer 9 automatically and continuously, rate of flow meter, circulation kettle 3, temperature sensor 21, pressure transmitter 15, spectrographic detection head 1, liquid level sensor 2, each pump housing, product is discharged system, deposition circuit 32, rare gas element input system, discharging of waste liquid system, heating and thermal insulation system 4, stirring system and work kettle system start or close, and then complete, reinforced, batching, dress liquid, circulation, deposition, the operations such as product discharge and discharging of waste liquid, automatically complete from being weighed to and discharge a plurality of continuous production stages of rafifinal powder-product, and be cycled to repeat and carry out, realize producing of rafifinal powder, comparing specific embodiment one difference is to circulate simultaneously and to deposit, working fluid loses activity needs circulation time, stop depositing → adding and supplement material and stir simultaneously → wait for after working fluid activity recovery → start again deposition → 6 times and so forth, then carry out product discharge and discharging of waste liquid.
If D. select manual one-step control pattern, manually boot the button of concrete single step operation, can Controlling System 61 each parts and the systems of controlling high-purity aluminium powder preparation apparatus of the present utility model start or stop, single stage ground is realized and is surveyed material level, batching, dosing, dress liquid, circulation, deposits, goes out product, discharging of waste liquid operation separately;
E. be finished after automatic control mode or manual one-step control pattern, whether system, in standby treated state, is waited for and is continued to loop or closing device.
Or further, automatic control mode comprises following operation: as Fig. 4,
Autodeposition starts order to be carried out: survey material level calling data; After after → no problem, stocking process starts, dress is just expected for the first time, automatic mounting cycle stock for the second time; → dosing operation starts, joins for the first time after initial liquid, automatically joins for the second time circulation fluid; → dress liquid operation starts, fills for the first time after initial liquid, for the second time automatic mounting circulation fluid; → deposition procedures starts, automatically enters cyclic deposition reaction process; → after having deposited, repeat to start circulating process, add and supplement material and stir, make working fluid activity recovery; → again enter deposition procedures; After deposition procedures, again enter circulating process; → go out product sequence start, automatically enter ultrasonic vibration operation by metallic aluminium powder be vibrated to deposition kettle 44 bottoms; → tapping operation starts, cyclic deposition starts discharging of waste liquid operation 6 times afterwards automatically; After → tapping, metallic aluminium powder is discharged from deposition kettle 44 bottoms.
Or further, in this specific embodiment, for the circulation kettle in specific embodiment one and deposition kettle unite two into one, manually one-step control pattern comprises: as shown in Figure 3, and after manually deposition starts; Manually boot as required single operation, the real-time detector data that automatic control system is collected according to on-line detecting system, control the kettle 3 that respectively circulates, deposition kettle 44, temperature sensor, pressure transmitter, spectrographic detection head, liquid level sensor, each pump housing, product discharge system, deposition circuit, rare gas element input system, discharging of waste liquid system, heating and thermal insulation system, stirring system and work kettle system start or close, and then realize the operation of selected one step.Concrete analysis: survey material level operation if select, survey two feeding chamber 8 material levels; If there is one in two feeding chamber material levels, lower than equipment initial set value alarming value, start acoustooptic alarm system, integral device is in holding state; If selection charging process, first surveys feeding chamber material level; Selection equipment is that dress is just expected or cycle stock now, having filled just expects also do not carry out tapping operation automatic control system automatically control feeding chamber dress cycle stock, otherwise dress is just expected; Dress is just expected, by Alcl 3: the ratio of halogenated organic salt=1.5, the first composition of expecting of preparation; Dress cycle stock, by Alcl 3: the ratio of halogenated organic salt=0.08, preparation cycle stock composition, in the present embodiment, halogenated organic salt comprises ionic liquid EMIC, ionic liquid BPC, ionic liquid Et3NHCl, ionic liquid TMPAC, halogenated organic salt is ionic liquid EMIC in the present embodiment.If select dosing operation, if dress is just to expect to join initial liquid, the magnetic force circulation stirring machine 16 that starts circulation kettle 3 stirs 2 hours; If dress is that cycle stock is joined circulation fluid, the magnetic force circulation stirring machine 16 that starts circulation kettle 3 stirs after 20 minutes and stops.If what select is dress liquid operation, if dress is initial liquid, after stirring, complete dress liquid operation; If dress is circulation fluid 55, after stirring, complete dress liquid operation, according to concentration of metal ions adjustment in work kettle, supplement working fluid 43 speed and complete dress liquid.If selection deposition procedures, temperature, pressure, liquid level and the chemical group first detecting according to the on-line detecting system data of grading, sedimentary environment is adjusted, make envrionment temperature, pressure and deposition ionic concn all meet mode of deposition, do not meet and can start respectively heating warmer 4, nitrogen pump 30, ion generator 22, by depositing temperature be controlled at 80 degree, nitrogen pressure is controlled at 0.5Mpa and controls deposition ionic concn and meets setting range value.If selected, be independent deposition procedures, automatic control system has deposited rear device standby by active metallic ion in work at present kettle; If selected, be cyclic deposition (default circulation 6 times or setting depositing time, when active A l concentration of metal ions does not meet the demands, starting charging system feeds in raw material, ion generator 22 starts and starts to supplement active ion simultaneously, and what be equivalent to carry out is the circulating process of deposition working fluid activity recovery; In deposition process: Controlling System 61 is connected deposition circuit 32, and the electrical parameter that provides refers to table 2, during institute deposit gage, per minute is got primary depositing spectroscopic data, and active A l concentration of metal ions (referring to table 3) meets the demands and continues to deposit; Otherwise deposition end-of-job.If select to discharge product sequence, if choose work physical method, all power supplys of closing device, carry out physics row aluminium mode; If select ultrasonic vibration mode, automatic control system 61 is opened ultrasonic vibrations 47 and is obtained high-purity aluminium powder product from products export 45.If select discharging of waste liquid operation, open circulation kettle 3 tapping pumps 58, waste liquid is discharged until circulation kettle 3 is emptying from tap hole 59.
Table 1, deposition process proportioning materials ratio
Sequence number Title Composition 1 Composition 2 Composition 3 Ratio (weight percent)
1 Just expect Alcl 3 Halogenated organic salt * ? 1.5～2.5:1
2 Cycle stock Alcl 3 Halogenated organic salt * ? 0.08～0.16:1
3 Initial liquid Just expect ? Toluene 1：0.36
4 Circulation fluid Cycle stock ? Toluene 1：0.1～0.3
5 Working fluid Cycle stock ? Toluene 1：0.1～0.3
* note: halogenated organic salt comprises: ionic liquid EMIC/BPC/Et3NHCl/TMPAC
Table 2, deposition physical parameter
Sequence number Title Parameter
1 Bath voltage 2.1～3.0V
2 Reference voltage -2.1～-3.0V
3 Constant current environment 200～600A/m 2
4 Temperature in the kettle 70～90 ℃
5 Nitrogen pressure 0.5Mpa
Table 3, electrolytic solution inactivation and resurrection parameter
The preparation parameter data form of table 4, eight examples
Table 5, organic molten salt galvanic deposit and the contrast of high temperature fused salt electrolysis aluminum technology index
Sequence number Parameter name Galvanic deposit Electrolytic aluminum
1 Bath voltage (Vdc) 2.0 5.0-6.0
2 Energy consumption (kW.Kg -1) 2.5–3.6 15-18
3 Current density (mA.cm -2) 30 ---
4 Interpole gap (mm) 20 100
5 Temperature (℃) 70–90 850-1000
6 CO discharges (kg.t -1.Al -1) Nothing 340
7 CF4 discharges (kg.t -1.Al -1) Nothing 1.5–2.5
In sum, high-purity aluminium powder preparation apparatus of the present utility model, cost is low, efficiency is high and the aluminium powder of production is high-purity aluminium powder, environmental sound.
Above-mentionedly only several specific embodiments in the utility model are illustrated; but can not be as whole protection domains of the present utility model; every equivalence variation of having done according to the design spirit in the utility model or modification or equal proportion zoom in or out etc., all should think and fall into protection domain of the present utility model.

Claims (7)

1. high-purity aluminium powder preparation apparatus, is characterized in that: comprise charging system, work kettle system, rare gas element input system, heating and thermal insulation system, stirring system, power supply system, deposition circuit, on-line detecting system, Controlling System, product is discharged system and discharging of waste liquid system, described work kettle system respectively with charging system, rare gas element input system, power supply system, deposition circuit, on-line detecting system, Controlling System, the product system of discharging is connected with discharging of waste liquid system, and described stirring system lower part is arranged in described work kettle system, and described heating and thermal insulation system is arranged on described work kettle system outside, described Controlling System respectively with charging system, work kettle system, rare gas element input system, detection system, heating and thermal insulation system, stirring system, power supply system, deposition circuit, on-line detecting system, product is discharged system and is connected with discharging of waste liquid system, and described work pot systems turnkey is drawn together work kettle, deposition working electrode and deposition anode, described deposition working electrode and deposition anode are all electrically connected to described deposition circuit, in described work kettle, have working fluid and circulation fluid, and described power supply system is given the charging system being attached thereto by power supply netting twine, work kettle system, rare gas element input system, detection system, heating and thermal insulation system, stirring system, deposition circuit, on-line detecting system, Controlling System, product is discharged system and discharging of waste liquid system power supply, and described feeding device comprises at least two feeding chambers, and described feeding chamber is communicated with described work kettle by charge pump, and organic generation halogen is housed respectively in described feeding chamber, aluminum chloride raw material and toluene, described on-line detecting system comprises spectrographic detection head, liquid level sensor, pressure transmitter and temperature sensor, described detection system is all arranged in described work kettle, in described work kettle, be provided with ion generator, described product discharge system comprises ultrasonic vibration head and is arranged on the product offtake of described work autoclave body bottom, described discharging of waste liquid system is the end liquid discharging tube that comprises tapping pump and be arranged on described work autoclave body bottom, and described work kettle at least comprises a reaction kettle body.
2. high-purity aluminium powder preparation apparatus according to claim 1, it is characterized in that: described work kettle comprises circulation kettle and the deposition kettle can break-make being communicated with, between described circulation kettle and described deposition kettle, by cocycle system and the lower recycle system, be communicated with, described ion generator is arranged in described cocycle system, described circulation kettle is connected with described charging system, in described circulation kettle, there is circulating liquid, in described deposition kettle, be provided with working fluid, deposition working electrode and deposition anode, in described circulation kettle and described deposition kettle, be provided with stirring system, temperature inductor, pressure inductor, spectrographic detection head and liquid level sensor, described circulation kettle and described deposition kettle outside are provided with heating and thermal insulation system, described circulation kettle is all communicated with and is all connected with power supply system with Controlling System with rare gas element input system with described deposition kettle top, described discharging of waste liquid system is arranged at described circulation autoclave body bottom, described product discharge system is arranged at described deposition autoclave body bottom.
3. high-purity aluminium powder preparation apparatus according to claim 2, is characterized in that: described cocycle system is provided with pumping installation and under meter, and the described lower recycle system is provided with pumping installation and switch electromagnetic valve.
4. according to the high-purity aluminium powder preparation apparatus described in claim 1 or 2 or 3, it is characterized in that: described work kettle comprises still lower body and the kettle cover covering, described still lower body and the described kettle cover place of covering are provided with tightness system.
5. according to the high-purity aluminium powder preparation apparatus described in claim 1 or 2 or 3, it is characterized in that: described stirring system comprises stirrer, agitator arm and agitating vane, described agitator arm is connected with described stirrer, described agitating vane is positioned at the bottom of described agitator arm, and described agitating vane is positioned at described work kettle middle part with upper/lower positions.
6. according to the high-purity aluminium powder preparation apparatus described in claim 1 or 2 or 3, it is characterized in that: between described charging system and described work kettle, between described discharging of waste liquid system and described work kettle, between described rare gas element input system and described work kettle, be provided with pumping installation and under meter.
7. according to the high-purity aluminium powder preparation apparatus described in claim 1 or 2 or 3, it is characterized in that: in described feeding chamber, be provided with a material sensor, described work autoclave body bottom is provided with switch electromagnetic valve.
CN201420147887.2U 2014-03-28 2014-03-28 High-purity aluminum powder preparation equipment Withdrawn - After Issue CN203768475U (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103966631A (en) * 2014-03-28 2014-08-06 郭昭华 High-purity aluminum powder preparation equipment and method for preparing high-purity aluminum powder by same
CN104357881B (en) * 2014-11-21 2017-11-28 刘晓鹏 A kind of electrolysis system based on hermetically sealed selective powder electrolysis unit

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103966631A (en) * 2014-03-28 2014-08-06 郭昭华 High-purity aluminum powder preparation equipment and method for preparing high-purity aluminum powder by same
CN103966631B (en) * 2014-03-28 2016-09-07 郭昭华 High-purity aluminium powder producing equipment and the method utilizing its high purity aluminium powder
CN104357881B (en) * 2014-11-21 2017-11-28 刘晓鹏 A kind of electrolysis system based on hermetically sealed selective powder electrolysis unit

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