CN103966631B - High-purity aluminium powder producing equipment and the method utilizing its high purity aluminium powder - Google Patents

High-purity aluminium powder producing equipment and the method utilizing its high purity aluminium powder Download PDF

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Publication number
CN103966631B
CN103966631B CN201410122332.7A CN201410122332A CN103966631B CN 103966631 B CN103966631 B CN 103966631B CN 201410122332 A CN201410122332 A CN 201410122332A CN 103966631 B CN103966631 B CN 103966631B
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kettle
deposition
work
aluminium powder
liquid
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CN103966631A (en
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郭昭华
东青
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Abstract

The present invention discloses high-purity aluminium powder producing equipment and the method utilizing its high purity aluminium powder, high-purity aluminium powder producing equipment includes interconnective charging system, work kettle system, inert gas input system, detection system, heating and thermal insulation system, stirring system, electric power system, deposition circuit, on-line detecting system, control system, product discharges system and discharging of waste liquid system, work kettle system has the work kettle of working solution and circulation fluid in including, deposition working electrode and deposition anode, electric power system gives each parts and system power supply, feeding device contains feeding chamber, detection system has spectrographic detection head, liquid level, pressure and temperature sensor, detection system is arranged in work kettle, ion generator is had in work kettle, work kettle is containing at least one reaction kettle body.The present invention high-purity aluminium powder high-purity aluminium powder of producing equipment extracting directly, low cost, in real time detection circulation fluid and working solution change of component, save the energy, environmental protection, non-environmental-pollution, the rate of output is high.

Description

High-purity aluminium powder producing equipment and the method utilizing its high purity aluminium powder
Technical field
The present invention relates to aluminium powder producing equipment, particularly relate to high-purity aluminium powder producing equipment.
The invention still further relates to produce the method for aluminium powder, particularly to utilizing above-mentioned high-purity aluminium powder producing equipment high purity aluminium The method of powder.
Background technology
POWDER METALLURGY ALUMINIUM ALLOYS material has low-density, Gao Biqiang, high abrasion, stretch-proof, corrosion-resistant and anti-fatigue performance The feature such as good, has extensive use in fields such as Aero-Space, automobile and engines.Metallic aluminium powder is POWDER METALLURGY ALUMINIUM ALLOYS Basic material, the method produced at present mainly has two kinds, i.e. ball milling powder process method and powder by atomization method.Ball milling powder process method ball Grinding machine produces flakey aluminium powder under inert gas shielding, is also referred to as " dry production ", and this method production efficiency is low, produces Cheng Fenchen is many, and quality is wayward.Powder by atomization method is to utilize the atomizing medium with certain speed directly to smash liquid aluminium skill Art or alloy and the method for preparing powder, apply relatively broad.Wherein atomization refers to high pressure, the high speed gas penetrated by atomizer nozzle Body, interacts with fused solution metal or alloy, liquid metal or alloy is smashed into droplet, and droplet is at flight course Middle cooled and solidified, thus the method obtaining powder.Atomization includes that (cooldown rate is 10 to air atomizing method2～103And water smoke K/s) (cooldown rate is 10 to change method2～104K/s), product is existing spherical also has non-regular shape, also referred to as " wet production ".
The activity of Al liquid is the highest, inevitably forms layer oxide film when rapid solidification flour, causes densified During the phase counterdiffusion of alloying element hindered, it is difficult to form metallurgical bond.
Therefore need in producing to use some special densification processes to overcome these difficulties, such as hot extrusion method, at a high speed Compacting etc..
Above two conventional metals aluminium powder preparation method, generally also exist that reparation technology route length, cost be high, purity and The deficiencies such as the bad control of the quality of production.
Along with science and technology development, laser spectrum tech available to the producing equipment of powder manufacturing process among, can The variation tendency of chemical reaction component in on-line monitoring system, quantitative analysis consumption of raw materials and the depositing crystalline of host element aluminum metal Effect, on-line monitoring intermediate product, the generation of impurity and impurity-eliminating effect, for the automatic control system offer section of powder extraction equipment Learn the support data of decision-making, set up production model and method that laboratory is amplified with industry, to shorten research and development with industrial Cycle.The present invention provides a kind of novel device and method for rafifinal powder production, makes production process more sanitary safe, does not has dirt Contaminate, automaticity is higher, technology path is short and production cost is less expensive, can be effectively improved efficiency and matter that aluminium powder produces Amount.
Summary of the invention
The present invention completes to solve above-mentioned deficiency of the prior art, and it is an object of the invention to provide can be straight Connect extraction rafifinal powder, low cost, producing process can detect circulation fluid and working solution change of component, part working solution in real time Can be recycled, save the energy, reduce or do not consume deposition anode material, environmental protection, not having environmental pollution, the rate of output is high High-purity aluminium powder producing equipment.
High-purity aluminium powder producing equipment of the present invention, including charging system, work kettle system, inert gas input system, Heating and thermal insulation system, stirring system, electric power system, deposition circuit, on-line detecting system, control system, product discharge system and Discharging of waste liquid system, described work kettle system respectively with charging system, inert gas input system, electric power system, deposition electricity Road, on-line detecting system, control system, product discharge system and the connection of discharging of waste liquid system, described stirring system the latter half Being arranged in described work kettle system, described heating and thermal insulation system is arranged on described work kettle its exterior, described control System with charging system, work kettle system, inert gas input system, detection system, heating and thermal insulation system, stirring is respectively System, electric power system, deposition circuit, on-line detecting system, product discharge system and discharging of waste liquid system connects, described work kettle System includes work kettle, deposition working electrode and deposition anode, and described deposition working electrode and deposition anode are all heavy with described Long-pending circuit electrical connection, has working solution and circulation fluid in described work kettle, described electric power system is connected therewith by power supply netting twine The charging system that connects, work kettle system, inert gas input system, detection system, heating and thermal insulation system, stirring system, heavy Long-pending circuit, on-line detecting system, control system, product discharge system and discharging of waste liquid system power supply, and described feeding device includes At least two feeding chamber, described feeding chamber is connected with described work kettle by charge pump, has been respectively provided with in described feeding chamber Machine includes spectrographic detection head, liquid level sensor, pressure sensing for halogen, aluminium chloride raw material and toluene, described on-line detecting system Device and temperature sensor, described detection system is arranged in described work kettle, is provided with ion and sends out in described work kettle Raw device, described product is discharged system and is included ultrasonic vibration head and be arranged on the product offtake of described work autoclave body bottom, described Discharging of waste liquid system is to include tapping pump and be arranged on the end liquid discharging tube of described work autoclave body bottom, and described work kettle at least wraps Containing a reaction kettle body.
High-purity aluminium powder producing equipment of the present invention it may also is that
Described work kettle includes can the circulation kettle of break-make connection and deposition kettle, described circulation kettle and described deposition Being connected with the lower circulatory system by the upper circulatory system between kettle, described ion generator is arranged in the described upper circulatory system, Described circulation kettle is connected with described charging system, has circulating liquid, be provided with work in described deposition kettle in described recirculating still body It is provided with stirring system, temperature in making liquid, deposition working electrode and deposition anode, described circulation kettle and described deposition kettle It is respectively provided with outside inductor, pressure inductor, spectrographic detection head and liquid level sensor, described circulation kettle and described deposition kettle Have heating and thermal insulation system, described circulation kettle all connect with inert gas input system with described deposition kettle top and all with control System processed and electric power system connect, and described discharging of waste liquid system is arranged at described circulation autoclave body bottom, and described product discharges system It is arranged at described deposition autoclave body bottom.
The described upper circulatory system is provided with pumping installations and flowmeter, and the described lower circulatory system is provided with pumping installations and opens Close magnetic valve.
Described work kettle includes still lower body and the kettle cover covered, and described still lower body is provided with close with the described kettle cover place of covering Seal apparatus.
Described stirring system includes that mixer, puddler and stirring vane, described puddler are connected with described mixer, institute Stating stirring vane and be positioned at the bottom of described puddler, described stirring vane is positioned at following position in the middle part of described work kettle.
Between described charging system and described work kettle, between described discharging of waste liquid system and described work kettle, institute State and be provided with pumping installations and flowmeter between inert gas input system and described work kettle.
Being provided with position material sensor in described feeding chamber, described work autoclave body bottom is provided with switch electromagnetic valve.
High-purity aluminium powder producing equipment of the present invention, it includes that charging system, work kettle system, inert gas input are System, heating and thermal insulation system, stirring system, electric power system, deposition circuit, on-line detecting system, control system, product discharge system With discharging of waste liquid system, described work kettle system respectively with charging system, inert gas input system, electric power system, deposition Circuit, on-line detecting system, control system, product discharge system and discharging of waste liquid system connects, described stirring system lower half Dividing and be arranged in described work kettle system, described heating and thermal insulation system is arranged on described work kettle its exterior, described control System processed is respectively with charging system, work kettle system, inert gas input system, detection system, heating and thermal insulation system, stirring System, electric power system, deposition circuit, on-line detecting system, product discharge system and discharging of waste liquid system connects, described work still System system includes work kettle, deposition working electrode and deposition anode, and described deposition working electrode and deposition anode are all with described Deposition circuit electrical connection, has working solution and circulation fluid in described work kettle, described electric power system is given therewith by power supply netting twine Connect charging system, work kettle system, inert gas input system, detection system, heating and thermal insulation system, stirring system, Deposition circuit, on-line detecting system, control system, product discharge system and discharging of waste liquid system power supply, described feeding device bag Including at least two feeding chamber, described feeding chamber is connected with described work kettle by charge pump, is respectively provided with in described feeding chamber Organic generation halogen, aluminium chloride raw material and toluene, described on-line detecting system includes that spectrographic detection head, liquid level sensor, pressure pass Sensor and temperature sensor, described detection system is arranged in described work kettle, is provided with ion in described work kettle Generator, described product is discharged system and is included ultrasonic vibration head and be arranged on the product offtake of described work autoclave body bottom, institute Stating discharging of waste liquid system is to include tapping pump and be arranged on the end liquid discharging tube of described work autoclave body bottom, and described work kettle is at least Comprise a reaction kettle body.So, charging system is for adding required raw material and at work still in work kettle system Internal carry out dispensing and dosing, work kettle then under the effect of control system or as recirculating still or as heavy Long-pending kettle, it is also possible to be work kettle itself comprise connection can the circulation kettle that connects of break-make and deposition kettle, when work still When body is for circulation kettle, in recirculating still body, after discharging bin discharging, it is configured as circulation fluid, is used for and the deposition in deposition kettle Can circulate after the mixing of rear liquid and carry out deposition process, and when the kettle that works is deposition kettle, on-line detecting system detects The temperature of this deposition kettle, pressure, liquid level and the component of deposition still internal deposition liquid also transmit above-mentioned detected value to control system, After control system is by the detection data received and predetermined value scope comparison, if indices not up to starts deposition During standard, then control system heating and heat-insulating device is started working and work kettle is heated to predetermined temperature and starts insulation, control System processed starts pressure in inert gas input system starts to input inert gas warranty work kettle in work kettle and reaches Predetermined range value, can start ion generator simultaneously and supplement ion concentration, or control system start to start charging system by In work kettle, it is added thereto a kind of material or two kinds of materials according to the flow after calculating, so that the group of liquid in work kettle Sub-control system is being suitable for deposition, if indices all reaches the standard starting deposition, then control system controls deposition electricity Road starts, and deposition working electrode and deposition anode are started working, and the aluminium powder through deposition reaction is deposited in deposition anode, when heavy Aluminium powder on long-pending anode reaches certain thickness, and startup product is discharged the ultrasonic vibration head of system and departed from also from deposition anode by aluminium powder Drop down onto work autoclave body bottom, open product offtake and the high-purity aluminium powder produced is discharged, repeatedly after cyclic deposition reaction, if work Make each ion ratio in liquid to drop to make working solution lose activity, then otherwise being on discharging of waste liquid system discharges waste liquid (one-pot body), afterwards control system control each parts again carry out feeding, dispensing and deposition procedures, and circulate repeatedly.Just Liquid after deposition reaction is delivered to circulate in work kettle (double kettle) by the communicating passage being between work kettle, enters The configuration of row circulation fluid and mixing so that working solution activity recovery the work working solution of activity recovery inputted again to deposition Deposition reaction is again carried out in making kettle, until after circulation repeatedly, ion recovery effects after the circulation in circulation work kettle Time bad, start discharging of waste liquid system and discharging of waste liquid is gone out, and from weighing, dispensing and dress liquid, deposition, cyclic deposition and waste liquid Discharge moves in circles again, constantly prepares high-purity aluminium powder.Certainly during all, on-line detecting system detects every in real time These data are also transmitted to control system by data, facilitate control system to control the work of each system and make the high purity aluminium powder can be real Existing.The producing equipment of such high-purity aluminium powder relative to the advantage of prior art is: (1) can from aluminium chloride extracting directly high-purity Aluminium powder, technical matters route is short, low cost；(2) producing equipment on-line monitoring system can detect circulation fluid and working solution in real time Change of component；(3) the working solution reusable edible that producing equipment is used, available inactivation hydraulic fluid is as the energy capable of circulation Energy storage material；(4) in electrodeposition process, the ion that the metal cation number utilizing online measuring technique to add absorbs with negative electrode Number kept in balance, can consume or the most not consumable anode material less；(5) whole aluminium powder production process green ring Protect, there is no environmental pollution, low cost and low-power consumption；(6) producing equipment is totally-enclosed, product quality is high, have Automatic Control merit Energy.
It is a further object of the present invention to provide utilize above-mentioned can be with extracting directly rafifinal powder, low cost, producing process In can detect circulation fluid and working solution change of component in real time, part working solution can be recycled, save the energy, reduce or do not consume Deposition anode material, environmental protection, there is no environmental pollution, the side of high-purity aluminium powder producing equipment high purity aluminium powder that the rate of output is high Method.
The method utilizing high-purity aluminium powder producing equipment high purity aluminium powder of the present invention, comprises the following steps:
A. starting device, starts control system, starts automatic control mode or single step performs pattern；
B. automatic control mode is selected: detect the position of material in feed bin, when wherein any one sets less than initial During alarming value, prompting supplements material, and when both of which exceedes initial setting alarming value, discharging bin prepares discharging, at on-line checking Circulation fluid in intrasystem spectrographic detection head detection work kettle and the chemical constituent of working solution, detect work with temperature sensor Make still body temperature, with the pressure in pressure sensor detection work kettle, with liquid level sensor detection work still body-internal-circulation Liquid and the liquid level of working solution, determine that material is delivered to work kettle and joins successively under control system control by feed bin Material, dosing and dress liquid operation, the stirring system of control system control afterwards proceeds by stirring, and ion generator work supplements ion Concentration, after reaching predetermined reaction condition, working solution deposits in work kettle, deposition circuit drives deposition work electricity Pole and deposition anode effect, and in deposition anode, deposit high-purity aluminium powder, and discharge, by product, the height that system discharge is produced Pure aluminium powder, the working solution after using is circulated in being recycled to work kettle, and feeding device supplements after adding material and stirs so that Working solution deposits in entering back into work kettle after replying activity, and in the kettle that works after so circulating at least 6 times, working solution is made Discharged by discharging of waste liquid system for waste liquid, in the process, if pressure is less than normal in pressure sensor detects work kettle, Then control system inputs the pressure in inert gas increase work kettle by controlling inert gas input system in work kettle Power, the component of liquid in spectrographic detection head detects work kettle, and control system are according in this compositional selecting discharging bin Either or both of which all starts charging in work kettle；
C. select single step and perform pattern: detect the position of material in feed bin, when wherein any one sets less than initial During alarming value, prompting supplements material, performs merely charging process, and when both of which exceedes initial setting alarming value, discharging bin is accurate Standby discharging；The circulation fluid in spectrographic detection head detection work kettle in on-line detecting system and the chemical constituent of working solution, use Temperature sensor detection work still body temperature, with the pressure in pressure sensor detection work kettle, examines with liquid level sensor Survey circulation fluid and the liquid level of working solution in work kettle, determine that material is delivered to work kettle and in control system control by feed bin Individually carrying out dispensing, dosing and dress liquid operation under system, control system individually controls stirring system and proceeds by stirring, individually afterwards Controlling ion generator work and supplement ion concentration, after reaching predetermined reaction condition, control system individually controls working solution Carrying out deposition procedures in work kettle, deposition circuit drives deposits working electrode and deposition anode effect, and in deposition anode On deposit high-purity aluminium powder, control system is activated individually product and discharges system and carry out product and discharge operation afterwards, loses after deposition The deposition working solution of activity is again introduced into the circulatory system, and automatic controlling system charging system starts charging so that working solution Activity recovery, carries out deposition reaction the most again in work kettle, working solution conduct in the kettle that works after so circulating at least 6 times Waste liquid is discharged, during the course, if pressure sensor detects work kettle internal pressure by the discharging of waste liquid system being activated individually Power is less than normal, then Non-follow control inert gas input system inputs the pressure in inert gas increase work kettle in work kettle Power, the component of liquid in spectrographic detection head detects work kettle, and manually select in discharging bin wherein according to this component One or both of all start toward work kettle in charging.
The method utilizing high-purity aluminium powder producing equipment high purity aluminium powder of the present invention, owing to have employed above-mentioned steps, because of This, can detect circulation fluid and working solution change of component in real time with extracting directly rafifinal powder in low cost, producing process, Part working solution can be recycled, and saves the energy, reduces or does not consume deposition anode material, environmental protection, not having environmental pollution, High-purity aluminium powder rate of output is high.
Accompanying drawing explanation
The schematic diagram of one of Fig. 1 present invention high-purity aluminium powder producing equipment embodiment.
Fig. 2 present invention high-purity aluminium powder producing equipment embodiment control system control flow block diagram.
Fig. 3 present invention high-purity aluminium powder producing equipment embodiment manually deposits FB(flow block).
Fig. 4 present invention high-purity aluminium powder producing equipment 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 Mouthful 1,6, flowmeter 1,7, charge pump 1,8, feed bin 1/ weigh 1/ material position sensing 1,9, feed bin 2/ weigh 2/ material position sensing 2,10, add Material pump 2,11, flowmeter 2,12, charge door 2,13, recirculating still sealing ring/nitrogen outlet, 14, circulation kettle cover, 15, circulating pressure Sensor, 16, circulation magnetic force mixer, 17, circulation stirring bar, 18, nitrogen pressurization mouth 1,19, upper cycling mouth, 20, flowmeter 3, 21, circulating temperature sensor, 22, depositing ions generator, 23, upper circulating pump, 24, deposition pressure sensor, 25, deposition stirring Machine, 26, deposition puddler, 27, sedimentary deposit tank upper cover, 28, nitrogen pressurization mouth 2,29, sedimentary deposit tank sealing ring/nitrogen outlet, 30, nitrogen Gas force (forcing) pump, 31, nitrogen cylinder, 32, deposition circuit, 33, Deposition Controller, 34, deposition spectrographic detection head, 35, deposition liquid level passes 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 stirring vane, 43, deposition working solution, 44, deposition tank body, 45, products export, 46, discharging switch electromagnetic valve, 47, ultrasonic vibration head, 48, deposition anode, 49, deposition hot warmer, 50, lower circulation port, 51, Cycling switch magnetic valve, 52, lower circulation pipe, 53, lower circulating pump, 54, circulation stirring blade, 55, deposition cycle liquid, 56, the end puts Liquid pipe, 57, flowmeter 4,58, tapping pump, 59, tap hole, 60, monitoring/control interface, 61, automatic control system, 62, automatically Controller.
Detailed description of the invention
Fig. 1 to Fig. 4 below in conjunction with the accompanying drawings is to high-purity aluminium powder producing equipment of the present invention and utilizes its high purity aluminium powder Method be described in further detail.
High-purity aluminium powder producing equipment of the present invention, refer to Fig. 1 to Fig. 4, including charging system, work kettle system, lazy Property gas feeding system, heating and thermal insulation system, stirring system, electric power system, deposition circuit, on-line detecting system, control system, Product discharges system and discharging of waste liquid system, described work kettle system respectively with charging system, inert gas input system, confession Electricity system, deposition circuit 32, on-line detecting system, control system, product are discharged system and discharging of waste liquid system and are connected, described in stir The system the latter half of mixing is arranged in described work kettle system, and described heating and thermal insulation system is arranged on described work kettle system Outside, described control system is protected with charging system, work kettle system, inert gas input system, detection system, heating respectively Temperature system, stirring system, electric power system, deposition circuit, on-line detecting system, product discharge system and discharging of waste liquid system connects Connecing, described work kettle system includes work kettle, deposition working electrode 41 and deposition anode 48, described deposition working electrode 41 All electrically connect with described deposition circuit 32 with deposition anode 48, in described work kettle, have working solution 43 and circulation fluid 55, described Electric power system gives charging system, work kettle system, inert gas input system, the detection being attached thereto by power supply netting twine 37 System, heating and thermal insulation system, stirring system, deposition circuit 32, on-line detecting system, control system, product are discharged system and give up Liquid exhaust system is powered, and described feeding device includes at least two feeding chamber 8, and described feeding chamber 8 is by charge pump 7 and 9 and institute State the connection of work kettle, in described feeding chamber, be respectively provided with organic generation halogen, aluminium chloride raw material and toluene, described on-line checking system System includes that spectrographic detection head, liquid level sensor, pressure sensor and temperature sensor, described detection system are arranged at described work Making in kettle, be provided with ion generator 22 in described work kettle, described product is discharged system and is included ultrasonic vibration 47 He Being arranged on the product offtake 45 of described work autoclave body bottom, described discharging of waste liquid system is for including tapping pump 58 and being arranged on institute Stating the end liquid discharging tube 56 of work autoclave body bottom, described work kettle includes at least a reaction kettle body.So, charging system is used for Adding required raw material in work kettle system and carry out dispensing and dosing in work kettle, the kettle that works is then in control Under the effect of system processed or as recirculating still or as deposition kettle, it is also possible to be that work kettle itself comprises connection Can the circulation kettle 3 that connects of break-make and deposition kettle 44, when the kettle that works is for circulation kettle 3, following after discharging bin 8 discharging It is configured as circulation fluid 55 in ring kettle 3, can circulate after mixing with liquid after the deposition in deposition kettle 44 and sink Long-pending processing procedure, and the kettle that works for deposition kettle 44 time, on-line detecting system detect the temperature of this deposition kettle 44, pressure, Liquid level and deposition still internal deposition liquid component and to control system transmit above-mentioned detected value, when the inspection that control system will receive After surveying data and predetermined value scope comparison, if indices not up to starts the standard of deposition, then control system adds Hot attemperator is started working and work kettle is heated to predetermined temperature and starts insulation, and control system starts inert gas input In system starts to input inert gas warranty work kettle in work kettle, pressure reaches predetermined range value, can start simultaneously Ion generator 22 supplements ion concentration, or control system starts to start charging system according to the flow after calculating to work still Internal it is added thereto a kind of material or two kinds of materials, so that the component of liquid controls be suitable for deposition in work kettle, as When really indices all reaches the standard starting deposition, then control system controls deposition circuit 32 and starts, and deposits working electrode 41 and deposition anode 48 start working, the aluminium powder through deposition reaction is deposited in deposition anode 48, when in deposition anode 48 Aluminium powder reaches certain thickness, and startup product is discharged the ultrasonic vibration 47 of system and departed from from deposition anode 48 by aluminium powder and drop down onto work Make autoclave body bottom, open product offtake 45 and the high-purity aluminium powder produced is discharged, repeatedly after cyclic deposition reaction, if working solution Each ion ratio in 43 drops to make working solution 43 lose activity, then otherwise being on discharging of waste liquid system arranges waste liquid Go out, or being off being deposited into circulating process adds and supplement material and stirring is resumed work the activity (one-pot body) of liquid 43, it Rear control system controls again to carry out deposition procedures, and circulates repeatedly.Just it is on the communicating passage between work kettle It is delivered to the liquid after deposition reaction circulate in work kettle 3 (double kettle), is circulated configuration and the mixing of liquid 55 so that Working solution 43 activity recovery and the working solution 43 of activity recovery is inputted again to deposition work kettle 44 in again sink Long-pending reaction, until after circulation repeatedly, when ion recovery effects is bad after the circulation circulated in work kettle 3, starting waste liquid row Discharging of waste liquid is gone out by place system, and from weighing, dispensing and dress liquid, deposit, circulate, deposit and discharging of waste liquid circulates past again Multiple, constantly prepare high-purity aluminium powder.Certainly during all, on-line detecting system detects each item data and in real time by these data Transmission, to control system, facilitates control system to control the work of each system and high purity aluminium powder is capable of.Such high-purity The producing equipment of aluminium powder relative to the advantage of prior art is: (1) can from aluminium chloride extracting directly rafifinal powder, technical staff Skill route is short, low cost；(2) producing equipment on-line monitoring system can detect circulation fluid and working solution change of component in real time；(3) system The working solution reusable edible that taking equipment is used, available inactivation hydraulic fluid is as the energy storage material of the energy capable of circulation；(4) In electrodeposition process, the number of ions utilizing metal cation number that online measuring technique adds and negative electrode to absorb keeps flat substantially Weighing apparatus, can consume or the most not consumable anode material less；(5) whole aluminium powder production process environmental protection, do not have environment dirty Dye, low cost and low-power consumption；(6) producing equipment is totally-enclosed, product quality is high, have Automatic Control function, has hand simultaneously Dynamic single step performs pattern, can carry out which single operation with Non-follow control.It addition, aluminum i ndustry powder metallurgy and integrated circuit industry It is generally acknowledged: primary aluminium powder: aluminium content 99.00-99.85%, refined aluminium powder: aluminium content 99.95-99.995% (3N-4N), high Pure aluminium powder: aluminium content 99.999-99.9999% (5N-6N), ultra-pure aluminium powder: aluminium content 99.99999% > more than 6N, with this Equipment and the method for invention can improve 1-2 the order of magnitude on the basis of material purity, if material purity is 99.0%, obtain powder End product purity reaches 99.9-99.99% to I haven't seen you for ages.
High-purity aluminium powder producing equipment of the present invention, refer to Fig. 1 to Fig. 4, specifically may be used on the basis of previous technique scheme Being that described work kettle includes can the circulation kettle 3 of break-make connection and deposition kettle 44, described circulation kettle 3 and described deposition Being connected with the lower circulatory system by the upper circulatory system between kettle 44, described ion generator 22 is arranged at the described upper circulatory system In, described circulation kettle 3 is connected with described charging system, has circulating liquid 55, described deposition kettle 44 in described circulation kettle 3 It is all provided with in being inside provided with working solution 43, deposition working electrode 41 and deposition anode 48, described circulation kettle 3 and described deposition kettle 44 It is equipped with stirring system, temperature inductor, pressure inductor, spectrographic detection head and liquid level sensor, described circulation kettle 3 and described Deposition kettle 44 is outside is provided with heating and thermal insulation system, described circulation kettle 3 and described deposition kettle 44 top all and inertia Gas feeding system connects and is all connected with control system and electric power system, and described discharging of waste liquid system is arranged at described recirculating still Bottom 3 bodies, described product is discharged system and is arranged at bottom described deposition kettle 44.In the technical program, work kettle is two Individual, it is respectively circulation kettle 3 and deposition kettle 44, wherein circulation kettle 3 is used for configuring circulation fluid 55, deposits kettle 44 and then uses Aluminium powder is produced in deposition.Two work kettle configuration two set on-line detecting system and stirring systems, circulation kettle 3 and deposition simultaneously Break-make can connect between kettle 44, can break-make be connected, when needs two by the upper circulatory system and the lower circulatory system the most between the two When person connects, in recirculating still body, the circulation fluid 55 of 3 carries out deposition reaction in constantly entering deposition kettle 44, constantly in deposition High-purity aluminium powder is deposited, under the liquid level in liquid level sensor and spectrographic detection head detect recirculating still and deposition still on anode 48 After fall, component ion concentration drop to below predetermined value, automatic or manual operation control system carries out charging process or gives up Liquid discharge operation.When needs carry out discharging of waste liquid operation, then open the lower circulatory system between circulation kettle 3 and deposition kettle 44 Between connect, circulation fluid 55 and working solution 43 all by circulation kettle 3 bottom discharging of waste liquid system be emitted into this device external. The high-purity aluminium powder produced then falls to discharge dress bottom reaction kettle body 44 and by product under the effect of ultrasonic vibration 47 Put outside device for transferring.So can circulate high purity aluminium powder incessantly successively, high-purity aluminium powder to produce efficiency ratio single Work kettle exceeds more than at least one times.Further preferred technical scheme be the described upper circulatory system be provided with pumping installations and Flowmeter, the described lower circulatory system is provided with pumping installations and discharging switch electromagnetic valve 46.So, the pumping dress of the upper circulatory system Putting in being pumped to deposit kettle 44 by the circulation fluid 55 in circulation kettle 3 and carry out deposition reaction, flowmeter is then for detecting Pumping into the amount of the circulation fluid 55 deposited in kettle 44, the pumping installations in the lower circulatory system will occur deposition in deposition kettle 44 The working solution 43 of reaction pumps in circulation kettle 3 and carries with after the circulation fluid 3 in recirculating still body and the material mix and blend that is newly added High ion concentration also is pumped to deposit in kettle 44 carry out deposition reaction after the effect of ion generator 22 again, so follows Ring prepares high-purity aluminium powder.And the discharging switch electromagnetic valve 46 in deposition reaction carries out the circulatory system at present may be at closing shape State, cuts off the connection of circulation kettle 3 and deposition kettle 44 the latter half, it is ensured that hydraulic fluid 43 deposition reaction in deposition kettle 44 Completely, naturally it is also possible to do not cut off so that after deposition kettle 44 carries out deposition reaction simultaneously and will react, deposition working solution 43 is defeated Deliver to circulate activity recovery in kettle 3.
High-purity aluminium powder producing equipment of the present invention, refer to Fig. 1 to Fig. 4, on the basis of foregoing technical scheme, Can also is that still lower body and kettle cover 14 and 27 that work kettle includes covering, described still lower body is provided with the described kettle cover place of covering Sealing device 13 and 29.The still lower body so covered and kettle cover ensure the temperature in circulation fluid 55 and/or working solution 43, pressure and Reaction is from ectocine.And the pressure that the advantage of sealing device is to ensure that in work kettle is in basicly stable state, it is to avoid Outside air enters and the danger such as blast occurs.Can be that described stirring system includes mixer 16 and 25, puddler 17 and 26 With stirring vane 54 and 42, described puddler is connected with described mixer, and described stirring vane is positioned at the bottom of described puddler, Described stirring vane is positioned at following position in the middle part of described work kettle.The advantage arranging stirring system is the rear and deposition that fed During reaction, it is sufficiently stirred for circulation fluid 55 and working solution 43 respectively so that each ion is distributed more equal in circulation fluid and working solution Even, and then reach more preferable dosing effect and more preferable deposition reaction effect, improve the production efficiency of high-purity aluminium powder.Can also is that Between described charging system and described work kettle, between described discharging of waste liquid system and described work kettle, described indifferent gas It is provided with pumping installations and flowmeter between body input system and described work kettle.This not only increases charging efficiency, Discharging of waste liquid efficiency and pumping efficiency, can detect the amount adding material simultaneously, the inert gas of discharging of waste liquid amount and addition Amount, wherein inert gas can be nitrogen.Position material sensor 9, described work still it is provided with in can also is that described feeding chamber 8 Switch electromagnetic valve it is provided with bottom body.So when position material sensor 9 detects that material is less than predetermined value in feeding chamber 8 Waiting, the acoustooptic alarm system being attached thereto starts to report to the police, until user responds, after material adds feeding chamber 8, and feeding chamber 8 are again started up working on.And the switch electromagnetic valve that the autoclave body bottom that works is arranged is for opening and closing work autoclave body bottom Discard solution discharge port 59 and/or product floss hole 45, it is simple to discharging of waste liquid and/or the discharge of high-purity aluminium powder.
The method utilizing aforesaid high-purity aluminium powder producing equipment high purity aluminium powder of the present invention, refer to Fig. 1 to Fig. 4, Comprise the following steps:
A. starting device, starts control system, starts automatic control mode or single step performs pattern；
B. automatic control mode is selected: detect the position of material in feed bin, when wherein any one sets less than initial During alarming value, prompting supplements material, and when both of which exceedes initial setting alarming value, discharging bin prepares discharging, at on-line checking Circulation fluid in intrasystem spectrographic detection head detection work kettle and the chemical constituent of working solution, detect work with temperature sensor Make still body temperature, with the pressure in pressure sensor detection work kettle, with liquid level sensor detection work still body-internal-circulation Liquid and the liquid level of working solution, determine that material is delivered to work kettle and joins successively under control system control by feed bin Material, dosing and dress liquid operation, the stirring system of control system control afterwards proceeds by stirring, and ion generator work supplements ion Concentration, after reaching predetermined reaction condition, working solution deposits in work kettle, deposition circuit drives deposition work electricity Pole and deposition anode effect, and in deposition anode, deposit high-purity aluminium powder, and discharge, by product, the height that system discharge is produced Pure aluminium powder, the working solution after using is circulated in being recycled to work kettle, and feeding device supplements after adding material and stirs so that Working solution deposits in entering back into work kettle after replying activity, and in the kettle that works after so circulating at least 6 times, working solution is made Discharged by discharging of waste liquid system for waste liquid, in the process, if pressure is less than normal in pressure sensor detects work kettle, Then control system inputs the pressure in inert gas increase work kettle by controlling inert gas input system in work kettle Power, the component of liquid in spectrographic detection head detects work kettle, and control system are according in this compositional selecting discharging bin Either or both of which all starts charging in work kettle；
C. select single step and perform pattern: detect the position of material in feed bin, when wherein any one sets less than initial During alarming value, prompting supplements material, performs merely charging process, and when both of which exceedes initial setting alarming value, discharging bin is accurate Standby discharging；The circulation fluid in spectrographic detection head detection work kettle in on-line detecting system and the chemical constituent of working solution, use Temperature sensor detection work still body temperature, with the pressure in pressure sensor detection work kettle, examines with liquid level sensor Survey circulation fluid and the liquid level of working solution in work kettle, determine that material is delivered to work kettle and in control system control by feed bin Individually carrying out dispensing, dosing and dress liquid operation under system, control system individually controls stirring system and proceeds by stirring, individually afterwards Controlling ion generator work and supplement ion concentration, after reaching predetermined reaction condition, control system individually controls working solution Carrying out deposition procedures in work kettle, deposition circuit drives deposits working electrode and deposition anode effect, and in deposition anode On deposit high-purity aluminium powder, control system is activated individually product and discharges system and carry out product and discharge operation afterwards, loses after deposition The deposition working solution of activity is again introduced into the circulatory system, and automatic controlling system charging system starts charging so that working solution Activity recovery, carries out deposition reaction the most again in work kettle, working solution conduct in the kettle that works after so circulating at least 6 times Waste liquid is discharged, during the course, if pressure sensor detects work kettle internal pressure by the discharging of waste liquid system being activated individually Power is less than normal, then Non-follow control inert gas input system inputs the pressure in inert gas increase work kettle in work kettle Power, the component of liquid in spectrographic detection head detects work kettle, and manually select in discharging bin wherein according to this component One or both of all start toward work kettle in charging.
Through above-mentioned steps, with extracting directly rafifinal powder, low cost, producing process can detect circulation fluid in real time With working solution change of component, part working solution can be recycled, and saves the energy, reduces or does not consume deposition anode material, green Environmental protection, does not has environmental pollution, and high-purity aluminium powder rate of output is high.It is high that prior art produces the aluminium powder long energy consumption of technical matters route, needs Pass through: bauxite ＞ Baeyer alkaline process ＞ alumina G T.GT.GT electrolytic aluminium ＞ ball milling powder process method or powder by atomization method ＞ aluminium powder；And Equipment provided by the present invention and method and technology route are short: flyash or bauxite ＞ acid system ＞ aluminium chloride ＞ electro-deposition ＞ aluminium Powder.Only just can be seen that the present invention compares with conventional method from energy consumption used by production per kilogram, efficiency improves at least 15%, cost Reduction ratio will be more than 15%, and concrete data refer to table 5.
The method utilizing aforesaid high-purity aluminium powder producing equipment high purity aluminium powder of the present invention, refer to Fig. 1 to Fig. 4, Original material proportioning is can also is that: aluminium chloride and halogenated organic salt are according to percentage by weight 1.5-on the basis of previous technique scheme 2.5:1 configuration forms, described cycle stock: aluminium chloride forms according to percentage by weight 0.08-0.16:1 configuration with halogenated organic salt, Initial liquid: toluene forms according to percentage by weight 0.036:1 configuration with just expecting；Circulation fluid: toluene and cycle stock are according to weight Percentage 0.1-0.3:1 configuration forms, and toluene can be within later stage from which a feeding chamber addition work kettle, it is also possible to another Individually set up a feeding chamber and charge pump, charge door again, in facilitating toluene addition work kettle outward.Toluene can be at halogenated organic Salt and aluminium chloride mix and blend, after one and a half hours, are added under the effect of charge pump by the charge door of feeding chamber, addition Controlling to refer to table 1 by weight percentage, toluene remixes after adding initial liquid and stirs half an hour.After experiment shows to add toluene Electrolyte prescription, can effectively reduce the viscosity of electrolyte, improves conductance, reduces the granularity of metal dust, thus improves The quality of powder-product.
When certainly can also is that described deposition reaction, tank voltage is 2.1-3V, and reference voltage is-2.1-3.0V, constant current ring Border is 200-600A/m2, in work kettle, depositing temperature is 70-90 DEG C, and in work kettle, pressure is 0.5Mpa, and working solution loses The condition of activity is ALCL7 -: ALCL4 -Ionic group ratio is less than 0.3-1；Circulation fluid activity recovery condition is ALCL7 -: ALCL4 - Ionic group ratio is more than 1-1.5.ALCL7 -Ionic group is active electrolyte groundwork group, and ALCL4-ion radical figure Being the basic condition of electrolyte generation electrochemical reaction, on-line monitoring equipment can qualitatively or quantitatively calculate the two group Activity value, can intuitively reflect the activity of deposition working solution from both ratios, provides decision data foundation for circulation or deposition.
It is embodied as one
High-purity aluminium powder producing equipment of the present invention includes
Two feeding chambers 8, are used for depositing halogenated organic salt and aluminium chloride raw material, and each feed bin is provided with position material sensor 9；
Two charge pumps (7 and 10), for pumping in circulation kettle 3, when preparation circulation fluid by the raw material in feeding chamber 55 or circulation fluid 55 when recycling, the order of response automatic control system 61, select simultaneously or single selection one of them add Material pump quantitatively, adds production needed raw material by two charge doors (5 and 12) to circulation kettle 3；
Four flowmeters (6,11,20 and 57), for each system flow measurement calculate, be respectively used to halogenated organic salt, Aluminium chloride, deposition working solution flow and the metering of inactivation discharging of waste liquid；
Two spectrographic detection heads (respectively circulation spectrum detecting head 1 and deposition spectrographic detection head 34), wherein circulate spectrum Detecting head 1 is the change of component of circulation fluid 55 in the kettle 3 of detection circulation in real time, and deposition spectrographic detection head 34 is for detection in real time The change of component of working solution 43 in deposition kettle 44；
Two liquid level sensors (circulation fluid level sensor 2 and deposition liquid level sensor 35), in detecting devices still Liquid position height, circulation fluid level sensor 2 is the liquid level change of circulation fluid 55 in the kettle 3 of detection circulation in real time, deposits liquid Level sensor 35 is the liquid level change of working solution 43 in the kettle 44 of detection deposition in real time；
Two kettlies (circulation kettle 3 and deposition kettle 44), for storing the liquid material in production process, circulate kettle 3 are used for depositing circulation fluid 55, and deposition kettle 44 is used for depositing working solution 43；
Two heating warmers (circular heating warmer 4 and deposition heating, temperature keeping device 49), for heating and the guarantor of equipment Temperature, circular heating warmer 4 is for circulating the heating and thermal insulation of kettle 3, and deposition heating, temperature keeping device 49 is for depositing adding of kettle 44 Heat insulation, heating warmer is wrapped on circulation kettle 2 and deposition kettle 44 outer wall respectively；
Two kettle cover sealing rings (circulation kettle cover sealing ring 13 and deposition kettle cover sealing ring 29), close for work kettle Envelope, circulation kettle cover sealing ring 13 is for circulating the nitrogen-sealed of kettle 3, and deposition kettle cover sealing ring 29 is for depositing the lazy of kettle 44 Property air seal (i.e. nitrogen-sealed), prevent smooth base, also embed two nitrogen discharge mouths, for work kettle initial start Time non-purity nitrogen mixed gas discharge；
Two kettle covers (circulation kettle cover 14 and deposition kettle cover 27), for the lidstock of work kettle, with formed seal, clean Clean and high-purity production atmosphere, circulation kettle cover 14 is added a cover to circulation kettle 3, is deposited kettle cover 27 and be used for depositing kettle 44；
Two pressure sensors (circulating pressure sensor 15 and deposition pressure sensor 24), the nitrogen in detecting devices Atmospheric pressure, circulating pressure sensor 15 is for circulating the pressure detecting of kettle 3, and deposition pressure sensor 24 is used for depositing kettle 44 Pressure detecting；
Two magnetic stirrers (circulation magnetic force mixer 16 and deposition magnetic stirrer 25) (can certainly use other Stirring system), the stirring of material in work kettle, with accelerate chemical reaction velocity increase reaction uniformity, circulate magnetic Power mixer 16 is for the circulation fluid 55 of agitation cycle kettle 3, and deposition magnetic stirrer 25 is for depositing the working solution of kettle 44 The stirring of 43, supporting with magnetic stirrer also have two puddlers (circulation stirring bar 17 and deposit puddler 26) and two stir Mix blade (circulation stirring blade 42 and deposition stirring vane 54)；
Two nitrogen pressurization mouths (circulating nitrogen gas pressurization mouth 18 and deposition nitrogen pressurization mouth 28), for two work kettlies Being passed through inert protective gas (in the present embodiment for nitrogen), in isolation production process, material and the oxidation source of air contact, follow Ring nitrogen pressurization mouth 18 is for leading to pressurized nitrogen to circulation kettle 3, and for giving, deposition kettle 44 is logical to be added deposition nitrogen pressurization mouth 28 Pressure nitrogen；
Two circulating pumps (upper circulating pump 23 and lower circulating pump 53), the circulation of material between work kettle, will configuration Good initialization liquid or circulation fluid 55 are by upper circulating pump 23, be driven into deposition kettle by upper cycling mouth 19 and upper circular tube In 44, also used deposition working solution 43 can be sent back to circulation by lower circulating pump 53, lower circulation port 50, lower circulation pipe 52 In kettle 3；
Ion generator 22, for depositing the activation of metal ion in working solution 43, improves ion concentration；
One nitrogen force (forcing) pump 30, for providing inert protective gas (being nitrogen in the present embodiment) to group kettle altogether, The nitrogen of nitrogen cylinder 31 is pressed in circulation kettle 3 and deposition kettle 44 by it, prevents the oxidation of working solution 43 in deposition process Enter with impurity；
Deposition circuit 32, the offer of electrical quantity in the deposition process of work kettle, in the control of Deposition Controller 33 Under, provide suitable operating current, deposition voltage and reference voltage and (refer to follow-up table 1, table 2 and table 3, deposit working solution 43 Under terminal voltage effect, deposition working electrode 41 and deposition anode 48 produce electric current by deposition working solution 43, at deposition kettle There is electrochemical reaction in working solution 43 in 44, thus can namely deposit at negative electrode and obtain high pure metal on working electrode 41 The depositing crystalline of aluminium powder；
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), pressure sensor (15 and 24) sensor, spectroscopic probe head (1 and 34), supervise online The parts such as examining system 40 and automatic control system 61 are powered.
Further, this producing equipment also includes:
On-line monitoring system 40, in equipment, the on-line checking of physical/chemical amount, is represented by dashed line in Fig. 1, and it includes There is flowmeter (6,11,20 and 57), level sensor (2 and 35), temperature inductor (21 in circulation kettle 3 and deposition kettle 44 With 39), pressure inductor (15 and 24) and spectrographic detection head (1 and 34), all above-mentioned data item can be detected with real-time online, Line monitor controller 36 these data of acquisition process, can carry out net with automatic control system 61 by monitoring/Controling network interface 60 Network communication and data sharing, be sent to automatic control system 61 by testing result, carries to the automatic control system 61 of producing equipment Start for charging/stop, kettle 3 is heated/is incubated, circulation stirring starts/stops in circulation, circulating pump works/stops, nitrogen adds Pressure/pressurize/stop, depositing that stirring starts/stops, deposition starts/stops, circulation starts/stops, ultrasonic vibration starts/stops, Tapping starts/decision data of the action such as stopping.
Further, this producing equipment also includes:
Automatic control system 61, automatically controlling for equipment, Fig. 1 represents with two-dot chain line, is controlled setting of connection Standby parts include charge pump (7 and 10), mixer (16 and 25), upper and lower circulating pump (23 and 53), nitrogen force (forcing) pump 30 and tapping Pump 58, after receiving the status data of on-line monitoring system, complete under the control of automatic controller 62 charging start/stop, Recirculating still is heated/is incubated, circulation stirring starts/stops, circulating pump work/stopping, nitrogen pressurization/pressurize/stop, depositing stirring Start/stop, deposition starts/stops, circulation starts/stops, ultrasonic vibration starts/stops, tapping starts the/joint such as stopping The action directive of point.
Described producing equipment farther includes:
Cycling switch magnetic valve 51, beats the opening/closing outer discharge pipe of deposition kettle liquid for equipment, when working solution 43 needs Open this valve during circulation, along with the interpolation of new working solution 43, deposition working solution 43 under gravity or use lower circulating pump 53, Used working solution 43 is driven in circulation kettle 3 by lower circulation port 50 and lower circulation pipe 52, adds new aluminium chloride at this former Expect and stir reaction, to recover the activity of circulation fluid 55, under the control of control system 61 flow process, passing through again when production needs Upper circulating pump 23 is returned deposition kettle 44 and is realized the circulation of working solution 43, it is of course possible to by all working in deposition kettle 44 Liquid all pressurizes in input extremely circulates kettle 3 and is circulated, it is also possible to deposition kettle 44 carries out deposition reaction, lives after reaction Property the working solution that reduces sink down into the office, lower half of deposition kettle 44 under gravity, start lower circulating pump at this by this portion Dividing working solution to be evacuated to circulate kettle 3 and carry out activation recovering, the working solution after recovery enters deposition still again by the upper circulatory system Deposit in body 44, i.e. deposit and circulate and can carry out simultaneously；
Ultrasonic vibration 47, for dropping to products export 45 by the aluminium powder being deposited on deposition working electrode 41 vibration；
Discharging switch electromagnetic valve 46, is used for opening products export 45 and is released by rafifinal powder-product；
Tapping pump 58, discharges the inactivation circulation fluid 55 being recycled for multiple times for work kettle, when maintenance of equipment or need This pump work during liquid in equipment to be emptied, waste material is discharged through tap hole 59 by end liquid discharging tube 56.
Described on-line monitoring system 40 may further comprise:
Working solution 43 and the on-line checking of circulation fluid 55 chemical constituent spectrum, be used for detecting material chemical group in work kettle Divide variation tendency and the qualitative and quantitative analysis of host element aluminum metal, by spectrographic detection head (circulation spectrum detecting head 1 and deposition spectrum Detecting head 34) material spectrum change real time data sends into on-line checking controller 36, according to liquid element in the still that collects Characteristic spectrum and Quantitative Analysis Model calculate the concentration of host element aluminium, circulation fluid 55 and the variation tendency of working solution 43, online The result of calculation of monitoring system 40 can be by detection/control interface 60 and automatic control system 61 data sharing, control system 61 The instruction sending response according to above-mentioned data controls each system and parts startup or closes.
Concrete automatic control system 61 control strategy includes, with liquid ions merit in circulation kettle 3 in deposition kettle 44 Can the activation of group and supplementing, make deposition consume metal ion and supplementary ion kept in balance, few consume or do not disappear Consumption anode material, and reach the purpose directly produced of metallic aluminium powder；Circulation fluid 55 activity recovery is allowed in circulation kettle 3 Time, it is that the characteristic peak of this liquid is gradually protruding and reach the process of maximum boundary value, these data are the maximums of finished product working solution Characteristic value, concrete active group ratio refers to table 3, in deposition kettle 44 in deposition process, with aluminium ion sinking at negative electrode Long-pending, the acidity of deposition liquid 43 or referred to as free state working solution 43 is gradually reduced, and the characteristic peak showing as hydraulic fluid is the most flat Flat, when principal character peak low to minimum work threshold time, the hydraulic fluid 43 of deposition kettle 44 can be put into circulation kettle 3 In be circulated use and process, it is possible to make deposition and supplement new liquid and make active ion concentration be maintained at reasonably work simultaneously In the range of, at this moment aluminium ion deposition working electrode 41 progressively depositing crystalline in deposition still 44 reach certain thickness is high Fine aluminium powder-product is vibrated by ultrasonic vibration 47 or physical method drops from deposition working electrode 41, and finally goes out from product Mouth 45 obtains and discharges.
Or further, described automatic control system 61 also includes: automatic control system 61 server and supervision Device, have recorded producing equipment each component working state and the historical record of on-line checking result, monitor in the database of equipment On can display device state and operating procedure, display information alert under can be easily accomplished the operation to producing equipment, monitor The on off state of the operational factor of producing equipment, historical record and equipment can be shown, each switch include charge pump (7 and 10), on Lower circulating pump (23 and 53), nitrogen pump 30, tapping pump 58, mixer (16 and 25), ion generator 22, discharging switch electromagnetic valve 46 and cycling switch magnetic valve 51, the material position of display device, including discharging bin material position 9, circulation fluid level sensor and deposition Sensor (2 and 35), in circulation kettle 3, circulation fluid 55 grades with the chemical group of working solution 43 in deposition kettle 44.
Such as Fig. 2, the present invention provides the method utilizing above-mentioned rafifinal powder extraction equipment high purity aluminium powder, Qi Zhonggong Make liquid 43, the proportion scale of circulation fluid 55 is shown in Table 1, and during deposition reaction, physical parameter is shown in Table 2, and electrolyte inactivates and circulates extensive Active parameter is shown in Table 3,
The present invention provides the method utilizing above-mentioned rafifinal powder extraction equipment high purity aluminium powder, including walking as follows Rapid:
A. starting device control system, starts integral device, and electric power system starts to power comprehensively；
B, automatic control system 61 start automatic control mode as required or manual single step performs pattern；
If C selects to start automatic control mode, automatic control system 61 calls level sensor 9, stream automatically and continuously Scale, circulation kettle 3, deposition kettle 44, temperature sensor, pressure sensor, spectrographic detection head, liquid level sensor, each pump housing, The upper circulatory system and the lower circulatory system, product discharge system, deposition circuit, inert gas input system, discharging of waste liquid system, add Hot heat-insulation system, stirring system and work kettle system start or close, and then complete, and charging, dispensing, dress liquid, deposit, follow The operations such as the discharge of ring, product and discharging of waste liquid, are automatically performed from being weighed to the multiple continuous production step of discharge rafifinal powder-product Suddenly, and circulate repeat, it is achieved producing of rafifinal powder；
If D. selecting manual one-step control pattern, then manually boot the button of concrete one step process, can be with control system 61 The each parts and the system that control high-purity aluminium powder producing equipment of the present invention start or stop, realization survey material position, independent single stage ground, Dispensing, dosing, dress liquid, deposit, circulate, go out product, discharging of waste liquid operation；
E. being finished after automatic control mode or manual one-step control pattern, system is in standby process state, etc. Treat whether to continue cycling through and carry out or close hull closure.
Or further, automatic control mode includes following operation: such as Fig. 4,
Autodeposition starts order and performs: surveys material position and calls data；After → no problem, stocking process starts, first time fills After just expecting, second time fills cycle stock automatically；→ dosing operation starts, join initial liquid for the first time after, second time joins circulation automatically Liquid；→ dress liquid operation starts, for the first time fill initial liquid after, second time fills circulation fluid automatically；→ deposition procedures starts, automatically into Cyclic deposition course of reaction；→ discharge opeing operation starts, automatically into pressurization discharge opeing process, be passed through nitrogen radioactive waste liquid side by side；→ go out Product sequence starts, is vibrated to deposit bottom kettle 44 by metallic aluminium powder automatically into ultrasonic vibration operation；→ tapping operation Start, automatically start discharging of waste liquid operation after cyclic deposition 6 times；After → tapping, metallic aluminium powder is arranged bottom deposition kettle 44 Go out.
Or further, manual one-step control pattern includes: as it is shown on figure 3, after manually deposition starts；As required Manually boot single operation, the real-time detector data that automatic control system is collected according to on-line detecting system, control each recirculating still Body 3, deposition kettle 44, temperature sensor, pressure sensor, spectrographic detection head, liquid level sensor, each pump housing, the upper circulatory system System, deposition circuit, inert gas input system, discharging of waste liquid system, heating and thermal insulation system is discharged with the lower circulatory system, product System, stirring system and work kettle system start or close, and then realize the operation of the one step selected.Concrete analysis: If selecting to survey material position operation, survey two feeding chamber 8 material positions；If two bin levels there being one report to the police less than equipment initial set value Value, then start acoustooptic alarm system, and integral device is in holding state；If selection charging process, the most first survey feeding chamber material position；Choosing Equipment of selecting is that dress is just expected or cycle stock now, and having filled just expects also does not has execution tapping operation then automatic control system automatic Controlling feeding chamber dress cycle stock, otherwise dress is just expected；Dress is just expected, by Alcl3: the ratio of halogenated organic salt=1.5, at the beginning of preparation Expect composition；Dress cycle stock, by Alcl3: the ratio of halogenated organic salt=0.08, prepare cycle stock composition, wherein halogenated organic Salt includes ionic liquid EMIC, ionic liquid BPC, ionic liquid Et3NHCl, ionic liquid TMPAC, the most organic Halogeno salt is liquid EMIC.If selecting dosing operation, if dress is just to expect, joining initial liquid, starting the magnetic of circulation kettle 3 Power circulation stirring machine 16 stirs 2 hours；If dress is cycle stock, join circulation fluid, start the magnetic force circulation stirring of circulation kettle 3 Machine 16 stops after stirring 20 points.If select is dress liquid operation, if dress is initial liquid, then in automatic control system 61 startup Till circulating pump 23 formulates position in installing to initial liquid deposit kettle 44；If dress is circulation fluid 55, then starts ion and send out Raw device 22 and upper and lower circulating pump (23 and 53), adjust supplementary working solution 43 speed according to concentration of metal ions in deposition still 44 and complete Dress liquid.If selection deposition procedures, temperature, pressure, liquid level and the chemical group first detected according to on-line detecting system grade data, Depositional environment is adjusted so that environment temperature, pressure and depositing ions concentration are satisfied by sedimentary condition, are unsatisfactory for, and can divide Do not start heating warmer (4 and 49), nitrogen pump 30, upper and lower circulating pump (23 and 53) and ion generator 22, by depositing temperature Control 80 degree, nitrogen pressure controls at 0.5Mpa and controls depositing ions concentration and meet setting range value.If selected is single Solely deposition procedures, then active metallic ion in current deposition kettle 44 has been deposited rear device standby by automatic control system；If institute Choosing is cyclic deposition (default circulation 6 times or setting sedimentation time), then when activity Al concentration of metal ions is unsatisfactory for requiring Starting upper and lower circulating pump (23 and 53) unlatching ion generator 22 and supplement active ion, cyclic deposition is same with supplementary new working solution 43 Shi Fasheng；In deposition process: control system 61 connects deposition circuit 32, and provided electrical quantity refers to table 2, opens during institute's deposit gage Beginning, the primary depositing spectroscopic data that takes per minute, activity Al concentration of metal ions (referring to table 3) meets requirement and then continues deposition；No Then deposit end-of-job.If selecting discharge opeing circulating process, if selecting gravity drainage, open lower circulating valve 51；If choosing pressurization discharge opeing Then close lower circulating valve 51 and open lower circulating pump 53 simultaneously, be passed through nitrogen pressurization, until liquid is all discharged simultaneously；If selected Discharge product sequence, if choosing work physical method, then close all power supplys of hull closure, carry out physical rank aluminium mode；If selecting Under Ultrasonic Vibration Flowing mode, then automatic control system 61 is opened ultrasonic vibration 47 and obtains high-purity aluminium powder product from products export 45.If choosing Selecting discharging of waste liquid operation, open circulation kettle 3 tapping pump 58, waste liquid is discharged from tap hole 59 until circulation kettle 3 empties.
Specific embodiment two
Embodiment two is another embodiment of the invention, as it is shown in figure 1, when circulation fluid 55 and deposition liquid (i.e. work Liquid 43) share a reaction kettle body time, powder extraction equipment can be simplified to single kettle structure by double kettlies, although equipment run effect Rate does not has double kettle high, but the one-pot body simple low cost of powder extraction device structure；
Rafifinal powder extraction equipment, including:
Two feeding chambers 8, are used for depositing halogenated organic salt and aluminium chloride raw material, and each feed bin is provided with position material sensor 9；
Two charge pumps (7 and 10), for pumping in circulation kettle 3, when preparation working solution by the raw material in feeding chamber 43 or circulation fluid 55 when recycling, the order of response automatic control equipment, select simultaneously two or single selection one of them Pump quantitatively, by two charge doors (5 and 12) add produce needed raw material (identical with specific embodiment one herein, feeding chamber At least two, can be three, and the 3rd is used for adding toluene)；
Three flowmeters (6,11 and 57), the flow measurement for equipment calculates, and is respectively used to halogenated organic salt, aluminium chloride The metering discharged with inactivation waste liquid；
One spectrographic detection head 1, the working solution used for work kettle or the real-time detection of circulation fluid chemical constituent；
One liquid level sensor 2, the liquid position height in detection operations kettle；
One work kettle 3, the liquid material in equipment storage production process；
One heating warmer 4, for heating and the insulation of equipment；
One kettle cover sealing ring 13, for the sealing of equipment, prevents smooth base, also embedded in a nitrogen discharge mouth, The discharge of non-purity nitrogen mixed gas when equipment initial start；
One kettle cover 14 (being moved on on 14 by the deposition circuit on kettle cover 27), for lidstock and the deposition circuit of equipment Installation, with formed seal, clean and high-purity production atmosphere；
One pressure sensor 15, the nitrogen pressure in detection operations kettle；
One magnetic stirrer 16, the stirring of material in work kettle, to accelerate chemical reaction velocity increase reaction Uniformity, supporting with this magnetic stirrer 16 also has puddler 17 and stirring vane 54；
One nitrogen pressurization mouth 18, for being passed through inert protective gas in work kettle, completely cuts off material in production process Oxidation source with air contact；
One nitrogen force (forcing) pump 30, for providing inert protective gas to equipment, the nitrogen of nitrogen cylinder 31 is pressed into by it In equipment still 3, prevent the oxidation of working solution in deposition process and impurity from entering；
Deposition circuit 32 (moving on to circulate kettle cover 14 from the deposition kettle cover 27 of Fig. 1), electricity in the deposition process of equipment The offer of parameter, under the control of Deposition Controller 33, provides suitable operating current, deposition voltage and reference voltage, deposition Working solution 43 is under terminal voltage effect, and deposition working electrode 41 and deposition anode 48 produce electric current by deposition working solution 43, There is electrochemical reaction in working solution in equipment kettle 3, thus can namely deposit at negative electrode and obtain height on working electrode 41 The depositing crystalline of pure metallic aluminum powder；
Industrial power 38, for providing power supply to apparatus assembly, gives work kettle 3, TEMP by power supply netting twine 37 The assemblies such as the sensors such as device 21, pressure sensor 15, spectrographic detection head 1, on-line monitoring system 40 and automatic control system 61 supply Electricity.
Further, this preparation system also includes: on-line monitoring system 40, and in equipment, physical/chemical amount is online Detection, be represented by dashed line in Fig. 1, connected device have the fluid flow (6,11 and 57) in work kettle 3, liquid level sensor 2, Temperature sensor 21, pressure sensor 15 and working solution spectrographic detection head 1, it is thus achieved that the real-time detection of response data item, particularly The real-time detection of flow, liquid level, temperature, pressure and working solution component spectra data, Online Monitoring Control in the kettle 3 that works Device 36 these data of acquisition process, can carry out network communication sum with automatic control equipment 61 by monitoring/Controling network interface 60 According to share, testing result is sent to automatic control equipment 61, to the automatic control equipment 61 of producing equipment provide charging start/ Stop, recirculating still is heated/is incubated, circulation stirring starts/stops, circulating pump work/stopping, nitrogen pressurization/pressurize/stop, sink Long-pending stirring starts/stops, deposition starts/stops, circulation starts/stops, ultrasonic vibration starts/stops, tapping starts/stopping etc. The decision data of action.
This producing equipment also includes: automatic control equipment 61, and automatically controlling for equipment uses two-dot chain line table in Fig. 1 Showing, the apparatus assembly being controlled to connect includes charge pump (7 and 10), mixer 16, nitrogen force (forcing) pump 30 and tapping pump 58, receives After the status data of on-line monitoring equipment, complete under the control of automatic controller 62 charging start/stop, work kettle 3 Heat/be incubated, circulation stirring starts/stops, nitrogen pressurization/pressurize/stop, depositing stirring start/stop, deposition start/stop Only, circulation starts/stops, ultrasonic vibration starts/stops, tapping starts the/action control of the switching node such as stopping.
Described producing equipment farther includes: ultrasonic vibration 47 (will move on to circulation in its deposition kettle from Fig. 1 In kettle 3), for the aluminium powder vibration deposited on the working electrode (s is dropped to products export；Tapping pump 58, discharges for equipment The inactivation working solution 55 being recycled for multiple times, this pump work when maintenance of equipment or liquid in needing the equipment that empties, waste material leads to Cross end liquid discharging tube 56 to discharge it can also be used to open products export and released by powder-product through tap hole 59.
Described on-line monitoring equipment 40 may further comprise: the online inspection of working solution or circulation fluid 55 chemical constituent spectrum Survey, for detecting material chemical constituent variation tendency and the qualitative and quantitative analysis of host element aluminum metal in equipment, by spectrographic detection In 1 still collected, material spectrum change real time data sends into on-line checking controller 36, according to the characteristic light of liquid element Spectrum and Quantitative Analysis Model calculate the concentration of host element aluminium, cycle working fluid 55 or the variation tendency of deposition working solution 43, The result of calculation of line monitoring device 40 can be by detection/control interface 60 and automatic control equipment 61 data sharing.
Described automatic control equipment 61 may further comprise: that automatic control equipment 61 control strategy includes, in equipment still 3 The activation of liquid ions functional group and supplementing, makes deposition consume metal ion and supplementary ion kept in balance, few consumes Or the most not consumable anode material, and reach the purpose directly produced of metallic aluminium powder；Circulation fluid is allowed to recover in recirculating still 3 During activity, being that the characteristic peak of working solution is gradually protruding and reach the process of maximum boundary value, these data are finished product hydraulic fluids Eigenvalue of maximum, concrete active group ratio refers to table 3, in deposition still in 3 deposition process, with aluminium ion at negative electrode Deposition, the acidity of deposition hydraulic fluid 55 or referred to as free state working solution is gradually reduced, and shows as the characteristic peak of hydraulic fluid The most flat, when principal character peak low to minimum work threshold time, can be circulated after increasing aluminium chloride in equipment still Use processes, at this moment aluminium ion working electrode 41 progressively depositing crystalline in deposition still 44 reach certain thickness, high-purity Aluminium powder product can be vibrated by ultrasonic vibration 47 (moving on in equipment still 3) or physical method obtains from products export 59.
Or further, described automatic control equipment 61 also includes:
Automatic control equipment 61 server, monitor, have recorded producing equipment each component working shape in the database of equipment State and the historical record of on-line checking result, on monitor can display device state and operating procedure, display information alert under Can be easily accomplished the operation to producing equipment, monitor can show opening of the operational factor of producing equipment, historical record and equipment Off status, switch module includes charge pump (7 and 10), nitrogen pump 30, tapping pump 58, mixer 16, the material level of display device Put, including circulation or the chemical constituent of working solution 55 in liquid level 2 in bin-level (8 and 9), circulation kettle 3 and circulation kettle 3 Deng.
Such as Fig. 2, the method for the rafifinal powder extraction that the present invention provides, wherein working solution, the proportion scale of circulation fluid are shown in Table 1, deposition physical parameter is shown in Table 2, and electrolyte inactivation and loop parameter are shown in Table 3, comprise the steps:
Comprise the steps:
A. starting device control system, starts integral device, and electric power system starts to power comprehensively；
B, automatic control system 61 start automatic control mode as required or manual single step performs pattern；
If C selects to start automatic control mode, automatic control system 61 calls level sensor 9, stream automatically and continuously Scale, circulation kettle 3, temperature sensor 21, pressure sensor 15, spectrographic detection head 1, liquid level sensor 2, each pump housing, product Discharge system, deposition circuit 32, inert gas input system, discharging of waste liquid system, heating and thermal insulation system 4, stirring system and work Make kettle system start or close, and then complete, charging, dispensing, dress liquid, circulate, deposit, the work such as product discharge and discharging of waste liquid Sequence, is automatically performed from being weighed to discharge the multiple continuous production stage of rafifinal powder-product, and circulation repeats, it is achieved be high-purity Producing of aluminium powder；For comparing specific embodiment one, difference is can not be circulated simultaneously and deposit, and working solution loses When deactivation needs circulation, after stopping deposition → supplementary material of addition stirs simultaneously → waits working solution activity recovery → start again to sink Long-pending → 6 times and so forth, then carry out product discharge and discharging of waste liquid.
If D. selecting manual one-step control pattern, then manually boot the button of concrete one step process, can be with control system 61 The each parts and the system that control high-purity aluminium powder producing equipment of the present invention start or stop, realization survey material position, independent single stage ground, Dispensing, dosing, dress liquid, circulate, deposit, go out product, discharging of waste liquid operation；
E. being finished after automatic control mode or manual one-step control pattern, system is in standby process state, etc. Treat whether to continue cycling through and carry out or close hull closure.
Or further, automatic control mode includes following operation: such as Fig. 4,
Autodeposition starts order and performs: surveys material position and calls data；After → no problem, stocking process starts, first time fills After just expecting, second time fills cycle stock automatically；→ dosing operation starts, join initial liquid for the first time after, second time joins circulation automatically Liquid；→ dress liquid operation starts, for the first time fill initial liquid after, second time fills circulation fluid automatically；→ deposition procedures starts, automatically into Cyclic deposition course of reaction；→ deposited after repeat to start the cycle over operation, add and supplement material and also stir so that working solution is extensive Active；→ it is again introduced into deposition procedures；Circulating process it is again introduced into after deposition procedures；→ go out product sequence and start, automatically enter Enter ultrasonic vibration operation to be vibrated to metallic aluminium powder deposit bottom kettle 44；→ tapping operation starts, after cyclic deposition 6 times from Dynamic startup discharging of waste liquid operation；After → tapping, metallic aluminium powder is discharged bottom deposition kettle 44.
Or further, in this specific embodiment, for the circulation kettle in specific embodiment one and deposition kettle Uniting two into one, manual one-step control pattern includes: as it is shown on figure 3, after manually deposition starts；Manually boot single work as required Sequence, the real-time detector data that automatic control system is collected according to on-line detecting system, control each circulation kettle 3, deposition kettle 44, Temperature sensor, pressure sensor, spectrographic detection head, liquid level sensor, each pump housing, product discharge system, deposition circuit, inertia Gas feeding 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 the one step selected.Concrete analysis: if selecting to survey material position operation, survey two feeding chamber 8 material positions；If two Having one then to start acoustooptic alarm system less than equipment initial set value alarming value in feeding chamber material position, integral device is in be treated Machine state；If selection charging process, the most first survey feeding chamber material position；Selection equipment is that dress is just expected or cycle stock now, fills Crossing just expects also does not has execution tapping operation then automatic control system to automatically control feeding chamber dress cycle stock, and otherwise dress is just expected；Dress Just expect, by Alcl3: the ratio of halogenated organic salt=1.5, the first composition of expecting of preparation；Dress cycle stock, by Alcl3: halogenated organic The ratio of salt=0.08, prepares cycle stock composition, and in the present embodiment, halogenated organic salt includes ionic liquid EMIC, ionic liquid BPC, ionic liquid Et3NHCl, ionic liquid TMPAC, halogenated organic salt is ionic liquid EMIC in the present embodiment.If choosing Selecting dosing operation, if dress is just to expect, join initial liquid, the magnetic force circulation stirring machine 16 starting circulation kettle 3 stirs 2 hours； If dress is cycle stock, joining circulation fluid, the magnetic force circulation stirring machine 16 of startup circulation kettle 3 stops after stirring 20 points.If choosing Select is dress liquid operation, if dress is initial liquid, then completes after stirring to fill liquid operation；If dress is circulation fluid 55, then after stirring Complete to fill liquid operation, adjust supplementary working solution 43 speed according to concentration of metal ions in work kettle and complete to fill liquid.If it is heavy to select Long-pending operation, temperature, pressure, liquid level and the chemical group first detected according to on-line detecting system is graded data, enters depositional environment Row sum-equal matrix so that environment temperature, pressure and depositing ions concentration are satisfied by sedimentary condition, are unsatisfactory for, can be respectively started heating and protect Temperature device 4, nitrogen pump 30, ion generator 22, depositing temperature is controlled 80 degree, nitrogen pressure control 0.5Mpa and control sink Long-pending ion concentration meets setting range value.If selected is independent deposition procedures, then automatic control system is by work at present kettle Interior active metallic ion has deposited rear device standby；If selected is cyclic deposition (default circulation 6 times or set sedimentation time, Then starting charging system when activity Al concentration of metal ions is unsatisfactory for requiring to feed, ion generator 22 startup simultaneously is opened Beginning to supplement active ion, be equivalent to carry out is the circulating process of deposition working solution activity recovery；In deposition process: control system System 61 connection deposition circuit 32, provided electrical quantity refers to table 2, during institute's deposit gage, per minute takes primary depositing spectrum number According to, activity Al concentration of metal ions (referring to table 3) meets requirement and then continues deposition；Otherwise deposit end-of-job.If the row of selection Go out product sequence, if choosing work physical method, then close all power supplys of hull closure, carry out physical rank aluminium mode；If selecting ultrasonic vibration Mode, then automatic control system 61 is opened ultrasonic vibration 47 and obtains high-purity aluminium powder product from products export 45.If selected Discharging of waste liquid operation, opens circulation kettle 3 tapping pump 58, and waste liquid is discharged from tap hole 59 until circulation kettle 3 empties.
Table 1, deposition process proportioning materials ratio
Sequence number Title Composition 1 Composition 2 Composition 3 Ratio (percentage by weight)
1 Just expect Alcl3 Halogenated organic salt* 1.5～2.5:1
2 Cycle stock Alcl3 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 solution Cycle stock Toluene 1:0.1～0.3
* note: halogenated organic salt includes: ionic liquid EMIC/BPC/Et3NHCl/TMPAC
Table 2, deposition physical parameter
Sequence number Title Parameter
1 Tank voltage 2.1～3.0V
2 Reference voltage -2.1～-3.0V
3 Constant current environment 200～600A/m2
4 Temperature in the kettle 70～90℃
5 Nitrogen pressure 0.5Mpa
Table 3, electrolyte inactivation and resurrection parameter
The preparation parameter data form of 4, eight examples of table
Table 5, organic molten salt electro-deposition contrast with high temperature fused salt electrolysis aluminum technology index
Sequence number Parameter name Electro-deposition Electrolytic aluminium
1 Tank 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 Die opening (mm) 20 100
5 Temperature (DEG C) 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 producing equipment of the present invention and preparation method, low cost, efficiency is high and the aluminium that produces Powder is high-purity aluminium powder, environmental sound.
Above-mentioned only several specific embodiments in the present invention are illustrated, but can not be as whole protections of the present invention Scope, every zooms in or out, all according to the equivalence change done by the design spirit in the present invention or modification or equal proportion It is deemed to fall protection scope of the present invention.

Claims (9)

  1. The most high-purity aluminium powder producing equipment, it is characterised in that: include charging system, work kettle system, inert gas input system, Heating and thermal insulation system, stirring system, electric power system, deposition circuit, on-line detecting system, control system, product discharge system and Discharging of waste liquid system, described work kettle system respectively with charging system, inert gas input system, electric power system, deposition electricity Road, on-line detecting system, control system, product discharge system and the connection of discharging of waste liquid system, described stirring system the latter half Being arranged in described work kettle system, described heating and thermal insulation system is arranged on described work kettle its exterior, described control System with charging system, work kettle system, inert gas input system, detection system, heating and thermal insulation system, stirring is respectively System, electric power system, deposition circuit, on-line detecting system, product discharge system and discharging of waste liquid system connects, described work kettle System includes work kettle, deposition working electrode and deposition anode, and described deposition working electrode and deposition anode are all heavy with described Long-pending circuit electrical connection, has working solution and circulation fluid in described work kettle, described electric power system is connected therewith by power supply netting twine The charging system that connects, work kettle system, inert gas input system, detection system, heating and thermal insulation system, stirring system, heavy Long-pending circuit, on-line detecting system, control system, product discharge system and discharging of waste liquid system power supply, and described charging system includes At least two feeding chamber, described feeding chamber is connected with described work kettle by charge pump, has been respectively provided with in described feeding chamber Machine includes spectrographic detection head, liquid level sensor, pressure sensing for halogen, aluminium chloride raw material and toluene, described on-line detecting system Device and temperature sensor, described detection system is arranged in described work kettle, is provided with ion and sends out in described work kettle Raw device, described product is discharged system and is included ultrasonic vibration head and be arranged on the product offtake of described work autoclave body bottom, described Discharging of waste liquid system is to include tapping pump and be arranged on the end liquid discharging tube of described work autoclave body bottom, and described work kettle at least wraps Containing a reaction kettle body.
  2. High-purity aluminium powder producing equipment the most according to claim 1, it is characterised in that: described work kettle includes break-make connecting Logical circulation kettle and deposition kettle, by the upper circulatory system and lower cyclic system between described circulation kettle and described deposition kettle System connection, described ion generator is arranged in the described upper circulatory system, and described circulation kettle is connected with described charging system, institute Have circulating liquid in stating recirculating still body, in described deposition kettle, be provided with working solution, deposition working electrode and deposition anode, described in follow It is provided with stirring system, temperature inductor, pressure inductor, spectrographic detection head and liquid level in ring kettle and described deposition kettle Heating and thermal insulation system it is provided with, described circulation kettle and described outside sensor, described circulation kettle and described deposition kettle Deposition kettle top all connects with inert gas input system and is all connected with control system and electric power system, described discharging of waste liquid System is arranged at described circulation autoclave body bottom, and described product is discharged system and is arranged at described deposition autoclave body bottom.
  3. High-purity aluminium powder producing equipment the most according to claim 2, it is characterised in that: the described upper circulatory system is provided with pumping Device and flowmeter, the described lower circulatory system is provided with pumping installations and switch electromagnetic valve.
  4. 4. according to the high-purity aluminium powder producing equipment described in claim 1 or 2 or 3, it is characterised in that: described work kettle includes lid The still lower body closed and kettle cover, described still lower body and the described kettle cover place of covering are provided with sealing device.
  5. 5. according to the high-purity aluminium powder producing equipment described in claim 1 or 2 or 3, it is characterised in that: described stirring system includes stirring Mixing machine, puddler and stirring vane, described puddler is connected with described mixer, and described stirring vane is positioned at described puddler Bottom, described stirring vane is positioned at following position in the middle part of described work kettle.
  6. 6. according to the high-purity aluminium powder producing equipment described in claim 1 or 2 or 3, it is characterised in that: described charging system is with described Between work kettle, between described discharging of waste liquid system and described work kettle, described inert gas input system and described work Make between kettle, to be provided with pumping installations and flowmeter.
  7. 7. according to the high-purity aluminium powder producing equipment described in claim 1 or 2 or 3, it is characterised in that: it is respectively provided with in described feeding chamber Having position to expect sensor, described work autoclave body bottom is provided with switch electromagnetic valve.
  8. 8. the method utilizing high-purity aluminium powder producing equipment high purity aluminium powder described in claim 1 or 2 or 3, it is characterised in that: Comprise the following steps:
    A. starting device, starts control system, starts automatic control mode or single step performs pattern；
    B. select automatic control mode: detect the position of material in feed bin, when wherein any one less than initially setting warning During value, prompting supplements material, and when both of which exceedes initial setting alarming value, discharging bin prepares discharging, at on-line detecting system The interior circulation fluid in spectrographic detection head detection work kettle and the chemical constituent of working solution, with temperature sensor detection work still Body temperature, with the pressure in pressure sensor detection work kettle, with circulation fluid in liquid level sensor detection work kettle and The liquid level of working solution, determines that material is delivered to work kettle and carries out dispensing under control system control successively, joins by feed bin Liquid and dress liquid operation, the stirring system of control system control afterwards proceeds by stirring, and ion generator work supplements ion concentration, After reaching predetermined reaction condition, working solution work kettle in deposit, deposition circuit drives deposition working electrode and Deposition anode effect, and in deposition anode, deposit high-purity aluminium powder, and discharge, by product, the rafifinal that system discharge is produced Powder, the working solution after using is circulated in being recycled to work kettle, and feeding device supplements after adding material and stirs so that work Liquid deposits in entering back into work kettle after replying activity, and in the kettle that works after so circulating at least 6 times, working solution is as useless Liquid is discharged by discharging of waste liquid system, in the process, if pressure is less than normal in pressure sensor detects work kettle, then controls System processed inputs the pressure in inert gas increase work kettle by controlling inert gas input system in work kettle, when Spectrographic detection head detects the component of liquid in work kettle, and control system according in this compositional selecting discharging bin wherein it One or both of which start toward work kettle in charging；
    C. select single step and perform pattern: detect the position of material in feed bin, when wherein any one less than initially setting warning During value, prompting supplements material, performs merely charging process, and when both of which exceedes initial setting alarming value, discharging bin prepares Material；The circulation fluid in spectrographic detection head detection work kettle in on-line detecting system and the chemical constituent of working solution, use temperature Sensor detecting work still body temperature, with the pressure in pressure sensor detection work kettle, detects work with liquid level sensor Make circulation fluid and the liquid level of working solution in kettle, determine that material is delivered to work kettle and under control system control by feed bin Individually carrying out dispensing, dosing and dress liquid operation, control system individually controls stirring system and proceeds by stirring afterwards, individually controls Ion generator work supplements ion concentration, and after reaching predetermined reaction condition, control system individually controls working solution in work Carry out deposition procedures, deposition circuit drives deposition working electrode and deposition anode effect in making kettle, and sink in deposition anode Amassing out high-purity aluminium powder, control system is activated individually product and discharges system and carry out product and discharge operation afterwards, loses activity after deposition Deposition working solution be again introduced into the circulatory system, automatic controlling system charging system start charging so that working solution recover Activity, carries out deposition reaction the most again in work kettle, and in the kettle that works after so circulating at least 6 times, working solution is as waste liquid Discharged, during the course, if pressure is inclined in pressure sensor detects work kettle by the discharging of waste liquid system being activated individually Little, then Non-follow control inert gas input system inputs the pressure in inert gas increase work kettle in work kettle, when Spectrographic detection head detects the component of liquid in work kettle, and according to this component manually select one of them in discharging bin or Both of which starts charging in work kettle.
  9. The method utilizing high-purity aluminium powder producing equipment high purity aluminium powder the most according to claim 8, it is characterised in that: former Expect proportioning: aluminium chloride and halogenated organic salt form according to percentage by weight 1.5-2.5:1 configuration, cycle stock: aluminium chloride with have Machine halogeno salt according to percentage by weight 0.08-0.16:1 configuration form, initial liquid: toluene with just expect according to percentage by weight 0.036:1 configuration forms；Circulation fluid: toluene forms according to percentage by weight 0.1-0.3:1 configuration with cycle stock.
CN201410122332.7A 2014-03-28 2014-03-28 High-purity aluminium powder producing equipment and the method utilizing its high purity aluminium powder Expired - Fee Related CN103966631B (en)

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CN202081156U (en) * 2011-05-19 2011-12-21 江苏森美铝颜料有限公司 Ball mill for aluminum paste production
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