CN109311094A - Manufacturing method, the manufacturing device of nickel powder of nickel powder - Google Patents
Manufacturing method, the manufacturing device of nickel powder of nickel powder Download PDFInfo
- Publication number
- CN109311094A CN109311094A CN201780036158.6A CN201780036158A CN109311094A CN 109311094 A CN109311094 A CN 109311094A CN 201780036158 A CN201780036158 A CN 201780036158A CN 109311094 A CN109311094 A CN 109311094A
- Authority
- CN
- China
- Prior art keywords
- nickel powder
- reactive tank
- piping
- nickel
- discharge
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
- B22F9/24—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions
- B22F9/26—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions using gaseous reductors
Abstract
The present invention provides one kind and can prevent that the equipment such as used piping, valve is made to be damaged or be caught in nickel powder during being discharged from reaction under high pressure slot and recycling the slurry containing nickel powder, can continuously run method thereby increasing productivity.The manufacturing method of nickel powder of the invention is to react sulfuric acid nickel ammine solution with hydrogen, the method for obtaining the nickel powder slurry containing nickel powder, it is characterized in that, after the nickel powder slurry be discharged and conveyed via discharge piping from the reactive tank for generating the slurry containing nickel powder, cleaning solution is supplied to discharge piping under defined pressure and is cleaned.
Description
Technical field
The method for carrying out hydrogen reduction the present invention relates to a kind of pair of sulfuric acid nickel ammine solution to obtain nickel powder, it is specific and
Speech, more particularly to a kind of manufacturing method and nickel powder of the nickel powder that steadily the nickel powder slurry generated in reactive tank can be discharged
Manufacturing device.
Background technique
As the method for industrial manufacture nickel powder, can illustrate the dissolution of raw material containing nickel in sulfuric acid solution, and gone
Except the processing comprising impurity in the feed, then, ammonia is added in the solution of obtained nickel sulfate, makes nickel with ammino-complex
Form exist, such as make the nickel sulfate ammonia complexing under 150 DEG C~250 DEG C, the high temperature and pressure of 2.5MPa~3.5MPa or so
Object solution is contacted with hydrogen, to restore the nickel in sulfuric acid nickel ammine solution to manufacture the method (patent document 1) of nickel powder.
Although this method is a kind of method that can effectively obtain high-quality nickel metal with compact equipment, another
Aspect, is reacted due to high-pressure bottle to be used, and industrially there are problems that being difficult to work continuously.
Although working as discharge side always that is, being easy to supply raw material, hydrogen to the reactive tank of high temperature and pressure
When open to extraneous gas, the internal pressure of reactive tank is easy to become identical as extraneous gas, can not carry out the reaction under high pressure again.Cause
This, the balance that needs to keep supplying and be discharged suitably to adjust the pressure inside reactive tank.
In the prior art, as at high temperature under high pressure carry out successive reaction technique, for example, as it is known that have patent document 2
Shown in that high pressure Ore Leaching (HPAL) technique nickel oxide ores are packed into autoclave together with sulfuric acid, are added in the process
Heat to 250 DEG C or so, make in ore it is micro containing the valuable metals such as nickel leached in sulfuric acid solution, recycle the valuable metal.
In HPAL technique, flash chamber (relief groove) and flash valve are arranged by the exhaust end in autoclave (reactive tank)
(dump valve), and carry out such as the control as disclosed in patent document 3 or patent document 4, in the inside for managing reactive tank
Repeat switch flash valve while pressure, to work continuously.
It the use of the method for flash chamber, flash valve is so a kind of good method, the steaming that can will be generated when being depressured
Gas is as energy regenerating and recycles.However, that is worked continuously using the reactive tank of high pressure conditions shown in HPAL technique,
The complexing reducing process for being difficult to carry out hydrogen reduction to sulfuric acid nickel ammine solution suitable for above-mentioned to obtain nickel powder.
The reason is that, being prone to wear and matching when being discharged from reactive tank due to the nickel powder metal superfine and harder that reaction generates
The components such as the valve of the piping are managed or be mounted on, there are problems that needing a large amount of maintenance management expense and the amount of labour.
In particular, passing through the slurry containing nickel powder of flash valve when reactive tank is depressurized to level identical with atmospheric pressure
The flow velocity of material, which reaches, connects near sonic fierce speed, so that frictional force obviously increases, further, in discharge removal process
It can also be collided with flash chamber inner wall and cause to damage.
In addition, in complexing reducing process, due to nickel powder from solution be precipitated during solution sometimes by from reactive tank
Discharge, so the reason of being precipitated on the inner wall of the piping of nickel powder after the exit and become blocking can occur or be discharged in control
The inside of valve be precipitated or be caught in nickel powder and the on-off phenomenon of valve can not be carried out.
Therefore, it is necessary to the maintenance of piping, valve etc. continually be dismantled and cleaned, so being difficult to be connected for a long time
Continuous reaction.In addition, each reaction is all replaced from reactive tank in commodity production also without industrializing the concrete instance worked continuously
The batch-type reaction of liquid is mainstream, and improving productivity becomes main problem.
Existing technical literature
Patent document
Patent document 1: Japanese Unexamined Patent Publication 2015-212411 bulletin
Patent document 2: Japanese Unexamined Patent Publication 2005-350766 bulletin
Patent document 3: Japanese Unexamined Patent Publication 2010-59489 bulletin
Patent document 4: Japanese Unexamined Patent Publication 2014-240524 bulletin.
Summary of the invention
Problem to be solved by the invention
The present invention is to propose in view of the foregoing, it is intended that providing one kind can prevent from reaction under high pressure
Slot, which is discharged and recycles, makes the equipment such as used piping, valve be damaged or be caught in nickel powder in the slurry process containing nickel powder, can connect
Reforwarding turns method thereby increasing productivity.
The technical solution solved the problems, such as
The present inventor passes through further investigation, as a result, it has been found that: by the slurry containing nickel powder obtained in reactive tank via discharge
After piping discharge conveying, supply cleaning solution is piped to the discharge to implement cleaning treatment with defined pressure, is able to solve above-mentioned
Problem so far completes the present invention.
(1) first invention of the invention is a kind of manufacturing method of nickel powder, is to make nickel sulfate ammonia complexing in reactive tank
Object solution is reacted with hydrogen under high pressure, obtains the manufacturing method of the nickel powder of the nickel powder slurry containing nickel powder, wherein contain from generation
The reactive tank of the slurry of nickel powder, by after nickel powder slurry discharge conveying, is matched under defined pressure to the discharge via discharge piping
Pipe supplies cleaning solution to be cleaned.
(2) the second invention of the invention is, in first invention, forced down in than above-mentioned reactive tank 0.2MPa or more and
Under 1.0MPa pressure below, above-mentioned cleaning solution supplying to above-mentioned discharge is piped.
(3) third invention of the present invention is, in first or second invention, carries out solid-liquid point using to the nickel powder slurry of recycling
The filtrate from obtained from is as above-mentioned cleaning solution.
(4) the 4th invention of the invention is a kind of manufacturing device of nickel powder, is to make sulfuric acid nickel ammine solution in height
Pressure is reacted with hydrogen to obtain the nickel powder making device of the nickel powder slurry containing nickel powder, and have: reactive tank makes nickel sulfate ammino
Polymer solution reacts with hydrogen and generates nickel powder；The nickel powder slurry that slot from the reactions above is discharged is depressurized to normal pressure by relief groove；Row
It is piped out, connects above-mentioned reactive tank and relief groove, for above-mentioned nickel powder slurry to be expelled to the relief groove from the reactive tank；With it is clear
Piping is washed, above-mentioned discharge piping is connected to, is piped supply cleaning solution to the discharge.
Invention effect
In accordance with the invention it is possible to prevent from being made during being discharged from reaction under high pressure slot and recycling the slurry containing nickel powder
The equipment such as piping, valve are damaged or are caught in nickel powder.It, can be continuous thereby, it is possible to subtract the reduced-maintenance amount of labour and cost
Operating is thereby increasing productivity.
Detailed description of the invention
Fig. 1 is the flow chart for indicating the manufacturing method of nickel powder, is the figure for indicating solution etc. and flowing to each treatment trough.
Fig. 2 is an exemplary diagram for indicating the manufacturing device structure of nickel powder.
Specific embodiment
Hereinafter, the specific embodiment (hereinafter referred to as " present embodiment ") that the present invention will be described in detail.It needs to illustrate
It is that the present invention is not limited to the following embodiments and the accompanying drawings, various repair can be carried out without departing from the spirit and scope of the invention
Change.In addition, in the present specification, the statement of " X~Y " (X, Y are any numbers) refers to " X or more and Y or less ".
" manufacturing methods of 1. nickel powders "
The manufacturing method of the nickel powder of present embodiment is a kind of by making sulfuric acid nickel ammine solution loading reactive tank
It is contacted with hydrogen under elevated pressure, so that nickel ion is reduced into nickel in the solution, obtains the side of the nickel powder slurry containing nickel powder
Method.
Specifically, in this manufacturing method, by supplying sulfuric acid nickel ammine solution to reactive tank, by the reaction
The internal temperature of slot is maintained at prescribed limit, while adjusting in a manner of continuously supplying hydrogen the pressure in the gas phase portion inside reactive tank
Power, so that the nickel ion in sulfuric acid nickel ammine solution is reduced into nickel under elevated pressure.It, can be with nickel sulfate in reactive tank
Ammino-complex solution adds the nickel powder as crystal seed together, makes hydrogen reduction by supplying the mixed slurry with nickel powder to reactive tank
Reaction occurs, so that the nickel for generating reduction is precipitated on the surface of the nickel powder as crystal seed.
In this way, the nickel powder with high-quality and optimum shape can be effectively manufactured in a manner of working continuously.
(about the hydrogen reduction reaction in reactive tank)
Specifically, Fig. 1 is the flow chart for indicating the manufacturing method of nickel powder, the stream to each treatment trough such as solution is shown
It is dynamic.As shown in Figure 1, in this manufacturing method, firstly, by sulfuric acid nickel ammine solution and as nickel powder (the nickel powder slurry of crystal seed
Material) mixed slurry supply to reactive tank.Then, start to the mixing slurry that sulfuric acid nickel ammine solution and crystal seed nickel powder are housed
The reactive tank of material, the continuous hydrogen for supplying reduction.
Sulfuric acid nickel ammine solution is the solution for containing nickel in the form of ammino-complex, for example, can be by sulfuric acid
Nickel (NiSO4) ammonia or ammonium hydroxide (NH are added in solution4OH it) obtains.
When manufacturing sulfuric acid nickel ammine solution, to the ammonia density of addition, there is no particular limitation, for example, it is preferable to add
Ammonia is so that the molar ratio of itself and the nickel concentration in solution is 1.9 or more.Thereby, it is possible to prevent the nickel in solution from becoming nickel hydroxide
It precipitates and exists not in the form of ammino-complex.
The nickel powder that adds as crystal seed is, it is preferable to use average grain diameter is 0.1 μm or more and 300 μm of nickel powders below, more
It is preferable to use 10 μm or more and 200 μm of nickel powders below.When the partial size of the nickel powder as crystal seed is less than 0.1 μm, nickel powder is too micro-
Carefully, it is possible to the effect as crystal seed can not be played.On the other hand, when the partial size of the nickel powder as crystal seed is greater than 300 μm, by
In excessively coarse, it is unable to get the effect for inhibiting the abrasion of equipment, it is also uneconomical in addition to prepare nickel powder coarse in this way.
Commercially available nickel powder can be used in nickel powder as crystal seed, can also be to the nickel powder being precipitated according to well known method chemistry
It is classified to use.Further, the nickel powder of manufacture can also be reused.In addition, by using mashing pump etc.
Feedway, the nickel powder as crystal seed is continuously supplied into reaction together with the sulfuric acid nickel ammine solution as raw material
Slot.
The internal temperature of reactive tank, the i.e. reaction temperature of hydrogen reduction reaction are set in 150 DEG C or more and 250 DEG C of models below
It encloses.It is preferably set to 150 DEG C or more and 185 DEG C of ranges below.For example, being adjusted using heating such as heating devices and keeping anti-
Answer the internal temperature of solution.When reaction temperature is lower than 150 DEG C, the reduction efficiency drop of the nickel ion in sulfate of ammoniac complex solution
It is low, on the other hand, even if reaction temperature is higher than 250 DEG C, reduction reaction is not also influenced, generates supply instead to reactive tank
The loss of hydrogen, thermal energy.
In this manufacturing method, by the way that the temperature of reactive tank is being maintained at 150 DEG C or more and 250 DEG C of states below
Under, into the reactive tank, the gas phase portion of unfilled solution continuously supplies hydrogen, make the gas phase portion pressure adjust 2.5MPa with
Upper and 3.5MPa range below.Specifically, the gas phase portion that is directly blown into hydrogen such as from gas cylinder in reactive tank or
It is blown into slurry.
About the pressure in gas phase portion, when internal pressure is lower than 2.5MPa, the efficiency of the reduction reaction of nickel ion is reduced.Separately
On the one hand, even if internal pressure is set as the condition of high voltage higher than 3.5MPa, reduction reaction is not also influenced, will increase instead
The loss of the hydrogen of supply.
So, in the manufacturing method of the nickel powder of present embodiment, by sulfuric acid nickel ammine solution and crystal seed
The mixed slurry of nickel powder is blown into hydrogen to be adjusted to defined pressure, thus under elevated pressure by institute in sulfuric acid nickel ammine solution
The nickel ion for including is reduced into nickel.The nickel for restoring generation as a result, is precipitated on the surface of the nickel powder supplied as crystal seed, can obtain
Obtain reduced nickel powder.
(taking-up about nickel powder slurry)
Next, slurry after the reaction generated in reactive tank, the nickel powder slurry that will contain nickel powder are taken out from reactive tank
And it is expelled to relief groove.Nickel powder slurry is the product generated by the reduction reaction under the pressurization in reactive tank, is in extremely high pressure
State.Therefore, such nickel powder slurry is discharged and is delivered in relief groove, then depressurize the relief groove slowly, for example, drop
To level identical with atmospheric pressure.
Reactive tank and relief groove are by piping (discharge is piped) connection for conveying nickel powder slurry, the nickel to spue from reactive tank
Slurry material is discharged to relief groove via discharge piping.
Here, in the manufacturing method of the nickel powder of present embodiment, which is characterized in that the nickel powder that will be generated in reactive tank
After slurry is discharged and conveys via discharge piping, supply cleaning solution is piped to the discharge under defined pressure and is matched to clean discharge
Inside pipe, the valve that the discharge is piped is set.According to this method, it can clean and remove in the discharge process of nickel powder slurry
The nickel powder of precipitation or other precipitates, the nickel powder being caught in valve etc., and the nickel powder etc. due to the precipitation can be effectively prevent
Caused piping or the abrasion of valve, blocking.Thereby, it is possible to effectively reduce the amount of labour of maintenance or cost, and can continuously transport
Turn thereby increasing productivity.
It should be noted that about use cleaning solution discharge piping cleaning, then with the structure of aftermentioned manufacturing device
It elaborates together.
(recycling nickel powder about from nickel powder slurry)
After the pressure to atmospheric pressure of nickel powder slurry in relief groove, then, nickel powder slurry is taken out from the relief groove, and
It is delivered to solid-liquid separation tank.
In solid-liquid separation tank, solid-liquid separation treatment is implemented to nickel powder slurry according to well known method, to be separated into nickel
Powder and filtrate recycle nickel powder.It can be again acted as by isolated filtrate herein and nickel powder slurry is delivered to relief groove from reactive tank
Be discharged piping cleaning solution, behind will be described in detail.
" manufacturing devices of 2. nickel powders "
Next, the manufacturing device to the manufacturing method for implementing nickel powder, carries out more specific description.In present embodiment
In the manufacturing method of nickel powder, the manufacturing device of nickel powder described further below can be used to carry out.
Fig. 2 is an exemplary diagram of the structure for the manufacturing device for indicating nickel powder.The manufacturing device 1 of the nickel powder is under high pressure
React sulfuric acid nickel ammine solution with hydrogen to obtain the manufacturing device of the nickel powder slurry containing nickel powder.
Specifically, the manufacturing device 1 (hreinafter referred to as " manufacturing device 1 ") of nickel powder has: reactive tank 11 makes sulfuric acid
Nickel ammine solution is reacted with hydrogen；The nickel powder slurry generated in reactive tank 11 is depressurized to normal pressure by relief groove 12；And row
It is piped 13 out, connects reactive tank 11 and relief groove 12 to be discharged and convey nickel powder slurry.In addition, being arranged in the manufacturing device 1
There is cleaning to be piped 14, cleaning piping 14 is connected to discharge piping 13 and supplies cleaning solution to discharge piping 13.
As described above, the cleaning piping 14 of discharge piping 13 is connected to by setting one in the manufacturing device 1 of nickel powder,
So as to which to 13 supply cleaning solution of discharge piping, effectively the inside of cleaning discharge piping 13, setting are in discharge piping 13
Valve etc., action failure can be prevented and steadily operation, to improve production efficiency.
[reactive tank]
Reactive tank 11 is the place for reacting sulfuric acid nickel ammine solution with hydrogen.In the reactive tank 11, supplying
Hydrogen under the action of, restore the reaction that the nickel ion and generating in sulfuric acid nickel ammine solution generates nickel powder.For example, logical
Cross and continuously feed hydrogen, by the pressure in the gas phase portion inside reactive tank 11 adjust and be maintained at 2.5MPa or more and 3.5MPa with
Under range, to make hydrogen reduction reaction.
As reactive tank 11, as long as be adjustable and the compressive reaction slot of temperature condition, pressure condition as defined in keeping i.e.
There is no particular limitation.It is, for example, possible to use autoclaves etc..To the material of autoclave, there is no particular limitation, for example, can make
With the autoclave of the austenite stainless steel by SUS316L, SUS304L etc..In addition, about its size, it can be according to as raw material
Sulfuric acid nickel ammine solution and the treating capacity etc. of mixed slurry of the nickel powder as crystal seed suitably set.
In reactive tank 11, at least provided with: loading port 11A is loaded as the sulfuric acid nickel ammine solution of raw material；Hydrogen
Gas supply mouth 11B, supply are used for the hydrogen of hydrogen reduction；With discharge opening 11C, discharge (discharge) is contained by hydrogen reduction reaction is generated
The slurry (nickel powder slurry) of nickel powder.
(loading port)
Loading port 11A is connect with piping (not shown) is packed into, and loading piping is molten with such as sulfuric acid nickel ammine
The reserve tank of liquid connects.In reactive tank 11, by the sulfuric acid nickel ammine solution of loading piping conveying, via loading port
11A is loaded into inside.In addition, can be individual sulfuric acid nickel ammine solution from the raw material that loading port 11A is packed into, it can also
To be the mixed slurry for being pre-mixed crystal seed nickel powder in the complex solution and obtaining.
(hydrogen body supply mouth)
Hydrogen supply mouth 11B is connect with hydrogen supplying tubing 21, and the hydrogen supplying tubing 21 with such as hydrogen cylinder
Hydrogen gas supplying apparatus connection.In reactive tank 11, the hydrogen supplied by the hydrogen supplying tubing 21 is via hydrogen supply mouth
11B is supplied to inside.
Here, being for supplying hydrogen to reactive tank 11 as described above, hydrogen supplying tubing 21 and hydrogen cylinder etc. are connect
Interior piping.It is provided with air supply valve 21a, on the specified position of the hydrogen supplying tubing 21 for controlling the confession of hydrogen
It gives.In addition, air supply valve 21a can be the ON/OFF valve of the supply ON (having supply) of control hydrogen, OFF (no supply), or
Person is also possible to that the controlling valve of hydrogen supply amount can be regulated and controled.
(discharge opening)
Discharge opening 11C is for making to be spued by hydrogen reduction reaction nickel powder slurry generated from reactive tank 11 in reactive tank 11
And the discharge opening being discharged.Discharge opening 11C is connect with aftermentioned discharge piping 13, the nickel powder slurry warp to spue from discharge opening 11C
It is discharged by discharge piping 13 and is delivered to relief groove 12.
[relief groove]
Relief groove 12 is the slot that the nickel powder slurry that will be generated in reactive tank 11 is for example depressurized to normal pressure.The relief groove 12 is by example
As flash tank (flash chamber) is constituted.
In relief groove 12, such as loading port 12A is provided on defined position at the top of it, being used for will be from reactive tank 11
The nickel powder slurry of discharge is packed into internal.Loading port 12A is connect with aftermentioned discharge piping 13, the nickel powder slurry from reactive tank 11
Material is conveyed by discharge piping 13, and the inside of relief groove 12 is loaded into via loading port 12A.
[discharge piping]
13 connection reactive tank 11 of discharge piping and relief groove 12 are the nickel powder slurry discharges for will generate in reactive tank 11
And it is delivered to the piping of relief groove 12.13 nickel powder slurry is discharged and be piped by the discharge from reactive tank 11, remains high pressure
State is flowed into piping 13 with connecing near sonic flow velocity at such high pressures, is loaded into relief groove 12.
It is at least provided with discharge valve 13a near 11 side of reactive tank in discharge piping 13 and to be located at relief groove 12 attached
Close flash valve (flash valve) 13b.
(discharge valve)
Discharge valve 13a is being arranged for controlling from the discharge-amount of the discharge opening 11C of the reactive tank 11 nickel powder slurry to spue
The control valve of the conveying capacity of the nickel powder slurry conveyed in piping 13 out.As discharge valve 13a, the defeated of control nickel powder slurry can be
The ON/OFF valve of ON (having conveying), OFF (no conveying) are sent, alternatively, being also possible to that the regulation of the conveying capacity of nickel powder slurry can be regulated and controled
Valve.
(flash valve)
Flash valve 13b is, when during will be packed into relief groove 12 by the nickel powder slurry conveyed in discharge piping 13
Control this control valve for being packed into operation.The internal pressure of reactive tank 11 is suitably managed on one side, on one side opening by flash valve 13b
It closes and nickel powder slurry is packed into relief groove 12, thus, it is possible to work continuously.Flash valve 13b can be control and fill to relief groove 12
Enter the ON/OFF valve of nickel powder slurry ON (having addition), OFF (no additives), alternatively, being also possible to that nickel powder slurry additive amount can be regulated and controled
Controlling valve.
[cleaning piping]
Cleaning piping 14 is the piping being connected in discharge piping 13, is matching to 13 supply cleaning solution of discharge piping
Pipe.For example, bifurcated, connection cleaning piping 14 is arranged in the predetermined portion (for example, " P " in Fig. 2) in discharge piping 13.Cleaning is matched
Link position of the pipe 14 in discharge piping 13 is not particularly limited, and can be located near discharge valve 13a or flash valve 13b
Near, the middle position of the discharge piping 13 of connection reactive tank 11 and relief groove 12 can also be located at.
Cleaning solution supplying valve 14a is provided in cleaning piping 14.Cleaning liquid bath etc. is arranged in cleaning solution supplying valve 14a
Near, to control the supply of cleaning solution, wherein the storages such as described cleaning liquid bath are piped 13 supplies to discharge by cleaning piping 14
Cleaning solution.Cleaning solution supplying valve 14a can be supply ON (having supply), the OFF of cleaning piping 14 of the control via cleaning solution
The ON/OFF valve of (no supply), alternatively, being also possible to that the controlling valve of the conveying capacity of cleaning solution can be regulated and controled.
As described above, the manufacturing device 1 of the nickel powder of present embodiment has cleaning piping 14, it is connected to for being discharged
The discharge piping 13 of nickel powder slurry from reactive tank 11 supplies cleaning solution to discharge piping 13 via cleaning piping 14, from
And the inside of piping 13, the valve (discharge valve 13a, flash valve 13b) being arranged in discharge piping 1 can be cleaned etc..Thereby, it is possible to
It cleans and removes the nickel powder or other precipitates that are precipitated in discharge piping 13, flash valve 13b etc., so as to for example effectively prevent
Block or be caught in flash valve 13b.
To cleaning solution, there is no particular limitation, and water (ejected wash water) etc. can be used for example.In addition to this, also can be used from
The draining (drain) generated after the vapor recovery heat generated during relief groove is depressurized to normal pressure, can also recycle with public affairs
Filtrate obtained from the method known is separated by solid-liquid separation the nickel powder slurry of recycling.
In addition, being connected on the defined position of cleaning piping 14 for supplying the non-active gas such as nitrogen or argon gas
Non-active gas supplying tubing 22.The non-active gas such as the nitrogen adjust the internal pressure of cleaning piping 14 and discharge piping 13,
And it is used to adjust pressure during from cleaning piping 14 to 13 supply cleaning solution of discharge piping.Non-active gas supply
Piping 22 is connect with the gas bottle of such as nitrogen etc., and the gas for adjusting gas flow is provided on position as defined in it
Body supply valve 22a.The pressure of non-active gas is controlled by air supply valve 22a, via non-active gas supplying tubing
22 are supplied to cleaning piping 14.
In addition, be not limited to control the pressure of cleaning solution using the supply of above-mentioned non-active gas, for example, it is also possible to
Connection infusion pump is in cleaning piping 14 so as to the cleaning solution pressurization in cleaning piping 14.It can also be by above-mentioned nonactive gas
Body supplying tubing 22 is directly connected to the cleaning solution reserve tank connecting with cleaning piping 14, and nonactive gas is supplied into the reserve tank
Body is to supply cleaning solution under defined pressure.
(being piped supply cleaning solution via cleaning)
Here, it is preferred that by than the cleaning for the pressure for forcing down 0.2MPa or more and 1.0MPa range below in reactive tank 11
Liquid is supplied to cleaning piping 14.More preferably it is set as than forcing down 0.5MPa or more and 1.0MPa following range of pressure in reactive tank 11
Power.In addition, as described above, controlling the pressure of cleaning solution using the air supply valve 22a that cleaning piping 14 is arranged in.It is specific and
Speech, since internal pressure by the supply of hydrogen is maintained at 2.5MPa or more and 3.5MPa range below in reactive tank 11, because
This is forced down in than the reactive tank 11 under 0.2MPa or more and 1.0MPa following range of pressure, for example, in 2.0MPa or more and
Under 2.5MPa pressure below, via 14 supply cleaning solution of cleaning piping.
When the difference of the supply pressure of cleaning solution and the internal pressure of reactive tank 11 is less than 0.2Mpa, by flow velocity when cleaning solution supplying
The removal power of generation becomes smaller, and may be unable to reach and fully clean.On the other hand, even if being greater than with the difference of internal pressure of reactive tank 11
1.0Mpa, cleaning effect also and may not be more preferable, instead it is possible that because the nickel powder etc. being removed based on cleaning makes piping, valve wear
Or it is damaged.
Embodiment
Hereinafter, the present invention is illustrated referring to embodiment, but the invention is not limited to the following embodiments.
[embodiment 1]
Nickel powder is manufactured using the device schematically shown in Fig. 2.That is, using capacity be 200 liters SUS316L,
The autoclave of the austenite stainless steel such as SUS304L continuously feeds hydrogen as reactive tank, to sulfuric acid nickel ammine solution
So that hydrogen reduction reaction occurs.In addition, using capacity is 1000 liters of flash tank as relief groove, it is fitted into and is generated in reactive tank
Nickel powder slurry is simultaneously depressurized to atmospheric pressure.In addition, reactive tank and relief groove are piped connection with the discharge that internal diameter is 10mm.In addition,
Discharge valve is set in the discharge opening of reactive tank, and flash valve is set at the top of relief groove, is packed into for controlling into relief groove
Nickel powder slurry carries out loading control by the switch of valve.
In the manufacturing apparatus, bifurcated, connection cleaning piping, to be piped via the cleaning are set in the way of discharge piping
Can by cleaning solution supplying to be discharged piping.In addition, the side setting bifurcated close with reactive tank in discharge piping is clear to connect
Wash piping.In addition, the connection industrial water piping in cleaning piping, under based on the supply of cleaning solution supplying valve control, supply
Industrial water as cleaning solution.Further, connection is used to supply the nitrogen as non-active gas in cleaning piping
Supplying tubing, so as to based on air supply valve supply control under, supply nitrogen.
Using such manufacturing device, by sulfuric acid nickel ammine solution that nickel concentration is 82.5g/L with 1.0L/ minutes
Flow is supplied to reactive tank.And with 0.5L/ minutes flows, by the slurry containing 75 μm of nickel powder 33g/L below supply to
Reactive tank is as crystal seed.
In addition, the internal temperature of reactive tank is maintained at 185 DEG C, hydrogen is blown into reactive tank for internal pressure from gas cylinder
It is adjusted to 2.5MPa~3.5MPa range.In addition, discontinuously switch is mounted on the flash valve at the top of relief groove, match via discharge
Nickel powder slurry is drawn in relief groove by pipe, and the amount of solution in reactive tank is made to be maintained at 90 liters.
After extracting nickel powder out, the discharge valve of reactive tank is successively first closed, flash valve is turned off.Then, setting is opened cleaning
4 liters of cleaning solution (industrial water) supply to discharges are piped via cleaning piping, are then shut off clear by the cleaning supply valve of piping
Washing lotion supply valve.It should be noted that between making 1~2 lift-off of the internal residual that cleaning is piped and discharge is piped.Then, it beats
Air supply valve is opened, cleaning is piped and the internal pressure of discharge piping is adjusted to than forcing down 0.5MPa~1.0Mpa in reactive tank
Range, be adjusted to the range of 2.0MPa~2.5Mpa, at this pressure by cleaning solution supplying to piping is discharged.
Based on the cleaning solution via cleaning piping supply, flash valve is opened to clean discharge piping and flash valve.Cleaning
After, the discharge valve and flash valve of reactive tank are opened, the discharge of the nickel powder slurry from reactive tank to relief groove is repeated.
Above-mentioned operation continue for 6 hours, but absorption or the card of flash valve, the abrasion, the nickel powder that are discharged in piping etc. do not occur
Enter, it being capable of extraction that is accessible and steadily carrying out the nickel powder slurry from reactive tank to relief groove.
[embodiment 2]
Cleaning piping is connected to 350 liters of capacity of cleaning solution reserve tank, is directly connected to nitrogen on the cleaning solution reserve tank
Gas supplying tubing is can supply nitrogen, in addition to this, carried out operation using manufacturing device similarly to Example 1.
Using suction filter, the nickel powder slurry recycled to the operation by embodiment 1 from relief groove is separated by solid-liquid separation, by institute
300 liters of obtained filtrates are used as cleaning solution.It is used in addition, the filtrate is stored in cleaning solution reserve tank as cleaning solution.Separately
Outside, nitrogen is supplied to cleaning solution reserve tank and the internal pressure of cleaning solution reserve tank is adjusted to the model of 2.0MPa~2.5Mpa
It encloses, control purge valve is so that cleaning solution is piped to discharge via cleaning piping each time by 4 liters of discharge and supplies cleaning solution.
It is more than hour to continue for 7 for above-mentioned operation, but the suction of flash valve, the abrasion, the nickel powder that are discharged in piping etc. does not occur
It is attached or be caught in, it being capable of extraction that is accessible and steadily carrying out the nickel powder slurry from reactive tank to relief groove.
[comparative example 1]
Other than not set cleaning piping, operation has been carried out using manufacturing device similarly to Example 1.That is, using
The manufacturing device of the mechanism of supply cleaning solution is piped under pressure as defined in being not disposed on to discharge to carry out operation.
Operation in 6 hours has been carried out under the condition that is similarly to Example 1,1 hour after bringing into operation, has been unable to control flash distillation
The switch of valve causes the nickel powder slurry beyond necessary amount that relief groove is discharged and be delivered to from reactive tank, can not will be in reactive tank
Amount of solution be maintained at 90 liters, operation is cut off.
After out of service, flash valve is observed, as a result, it has been found that, nickel precipitate, small nickel powder are precipitated or are caught in valve.
The explanation of appended drawing reference
1: the manufacturing device of nickel powder
11: reactive tank
11A: loading port
11B: hydrogen supply mouth
11C: discharge opening
12: relief groove
12A: loading port
13: discharge piping
13a: discharge valve
13b: flash valve
14: cleaning piping
14a: cleaning solution supplying valve
21: hydrogen supplying tubing
21a: air supply valve
22: non-active gas supplying tubing
22a: air supply valve.
Claims (4)
1. a kind of manufacturing method of nickel powder is to make sulfuric acid nickel ammine solution and hydrogen anti-in reactive tank under high pressure
It answers, obtains the manufacturing method of the nickel powder of the nickel powder slurry containing nickel powder, wherein
From generating after the nickel powder slurry is discharged and conveyed via discharge piping by the reactive tank of the slurry containing nickel powder, defined
Supply cleaning solution is piped to be cleaned to the discharge under pressure.
2. the manufacturing method of nickel powder as described in claim 1, wherein
It is forced down in than the reactive tank under 0.2MPa or more and 1.0MPa pressure below, by the cleaning solution supplying to institute
State discharge piping.
3. the manufacturing method of nickel powder as claimed in claim 1 or 2, wherein
Using filtrate obtained from being separated by solid-liquid separation to the nickel powder slurry of recycling, as the cleaning solution.
4. a kind of manufacturing device of nickel powder, the manufacturing device of the nickel powder make sulfuric acid nickel ammine solution under high pressure with hydrogen
Reaction is to obtain the nickel powder slurry containing nickel powder, wherein has:
Reactive tank makes sulfuric acid nickel ammine solution react with hydrogen and generate nickel powder；
The nickel powder slurry being discharged from the reactive tank is depressurized to normal pressure by relief groove；
Discharge piping, connects the reactive tank and relief groove, for the nickel powder slurry to be expelled to the decompression from the reactive tank
Slot；With
Cleaning piping, is connected to the discharge piping, is piped supply cleaning solution to the discharge.
Applications Claiming Priority (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2016-122309 | 2016-06-21 | ||
| JP2016122309A JP6819087B2 (en) | 2016-06-21 | 2016-06-21 | Nickel powder manufacturing method, nickel powder manufacturing equipment |
| PCT/JP2017/021980 WO2017221787A1 (en) | 2016-06-21 | 2017-06-14 | Nickel powder production method and nickel powder production device |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN109311094A true CN109311094A (en) | 2019-02-05 |
Family
ID=60783484
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201780036158.6A Pending CN109311094A (en) | 2016-06-21 | 2017-06-14 | Manufacturing method, the manufacturing device of nickel powder of nickel powder |
Country Status (8)
| Country | Link |
|---|---|
| US (1) | US20190308249A1 (en) |
| EP (1) | EP3473362A4 (en) |
| JP (1) | JP6819087B2 (en) |
| CN (1) | CN109311094A (en) |
| AU (1) | AU2017283345B2 (en) |
| CA (1) | CA3027666A1 (en) |
| PH (1) | PH12018502669A1 (en) |
| WO (1) | WO2017221787A1 (en) |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP6931474B2 (en) * | 2016-08-31 | 2021-09-08 | 住友金属鉱山株式会社 | Solids recovery device |
| JP7034439B2 (en) * | 2018-06-19 | 2022-03-14 | 住友金属鉱山株式会社 | Nickel powder recovery method |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103273074A (en) * | 2013-03-27 | 2013-09-04 | 深圳市中金岭南科技有限公司 | Process method of continuously producing ultra-fine nickel powder |
| JP2016033255A (en) * | 2014-03-26 | 2016-03-10 | 国立大学法人高知大学 | Nickel powder production process |
Family Cites Families (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS4829553Y1 (en) * | 1969-03-11 | 1973-09-07 | ||
| US4801432A (en) * | 1986-01-09 | 1989-01-31 | Intevep, S.A. | Apparatus for withdrawing particulate solid from a high pressure vessel |
| JP4525428B2 (en) | 2004-05-13 | 2010-08-18 | 住友金属鉱山株式会社 | Method for hydrometallizing nickel oxide ore |
| JP5332418B2 (en) | 2008-09-04 | 2013-11-06 | 住友金属鉱山株式会社 | Autoclave pressure adjustment method |
| CN104039993B (en) | 2012-01-13 | 2016-03-30 | 住友金属矿山株式会社 | Flasher and method of operation thereof |
| JP6406613B2 (en) | 2014-04-15 | 2018-10-17 | 住友金属鉱山株式会社 | Method for producing nickel powder with reduced concentration of carbon and sulfur |
-
2016
- 2016-06-21 JP JP2016122309A patent/JP6819087B2/en active Active
-
2017
- 2017-06-14 EP EP17815256.7A patent/EP3473362A4/en not_active Withdrawn
- 2017-06-14 US US16/309,209 patent/US20190308249A1/en not_active Abandoned
- 2017-06-14 WO PCT/JP2017/021980 patent/WO2017221787A1/en unknown
- 2017-06-14 CN CN201780036158.6A patent/CN109311094A/en active Pending
- 2017-06-14 AU AU2017283345A patent/AU2017283345B2/en not_active Ceased
- 2017-06-14 CA CA3027666A patent/CA3027666A1/en not_active Abandoned
-
2018
- 2018-12-18 PH PH12018502669A patent/PH12018502669A1/en unknown
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103273074A (en) * | 2013-03-27 | 2013-09-04 | 深圳市中金岭南科技有限公司 | Process method of continuously producing ultra-fine nickel powder |
| JP2016033255A (en) * | 2014-03-26 | 2016-03-10 | 国立大学法人高知大学 | Nickel powder production process |
Also Published As
| Publication number | Publication date |
|---|---|
| EP3473362A1 (en) | 2019-04-24 |
| EP3473362A4 (en) | 2020-01-22 |
| US20190308249A1 (en) | 2019-10-10 |
| AU2017283345B2 (en) | 2020-06-25 |
| PH12018502669A1 (en) | 2019-10-07 |
| JP2017226867A (en) | 2017-12-28 |
| AU2017283345A1 (en) | 2019-01-17 |
| JP6819087B2 (en) | 2021-01-27 |
| CA3027666A1 (en) | 2017-12-28 |
| WO2017221787A1 (en) | 2017-12-28 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN109311094A (en) | Manufacturing method, the manufacturing device of nickel powder of nickel powder | |
| JP6882851B2 (en) | Method for manufacturing crude nickel sulfate solution | |
| JP6388043B2 (en) | Sulfide production method, nickel oxide ore hydrometallurgy method | |
| JP6459879B2 (en) | Nickel powder manufacturing method and reaction facility operation method | |
| CA2897707C (en) | Operation method for dezincification plant | |
| EP3249061B1 (en) | Sulfuric acid adding facility and operation method therefor | |
| JP2016113703A (en) | Neutralization method by wet type refining of nickel oxide ore | |
| JP7277074B2 (en) | Method for removing residual hydrogen sulfide and sulfurization reaction vessel | |
| JP7034439B2 (en) | Nickel powder recovery method | |
| JP7298126B2 (en) | Nickel Oxide Ore Autoclave Equipment | |
| JP2021115559A (en) | Cooling tool and cooling method for autoclave | |
| JP2015038251A (en) | Method of operating dezincification plant | |
| KR101536468B1 (en) | Hydrometallurgical process and equipment | |
| CN216727210U (en) | Ash removal device | |
| JP7279578B2 (en) | Solid-liquid separation method using thickener and nickel oxide ore hydrometallurgical method including the same | |
| JP7310490B2 (en) | Operation method for starting up treatment in the neutralization process | |
| WO2018143121A1 (en) | Sulfurization reaction facility | |
| JP2023043553A (en) | pH MEASUREMENT DEVICE, AND WET REFINING METHOD OF NICKEL OXIDE ORE USING THE SAME | |
| JP2020059909A (en) | Filtration facility for removing zinc sulfide and production method of nickel cobalt mixed sulfide using the same | |
| JP2023031095A (en) | Operational method of filtration unit, dezincification processing method, and purification method of nickel oxide ore | |
| JP2019026868A (en) | Method for removing residual hydrogen sulfide | |
| CN115382353A (en) | Device and method for treating a gas flow leaving the reaction section of a melamine production plant | |
| WO2015092147A1 (en) | An autoclave, a method for draining an autoclave and use of a connection line | |
| KR20160043590A (en) | Storage Tank of Recycling Wastewater and Valuable Metal Hydrometallurgical Facility Comprising the Same |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| WD01 | Invention patent application deemed withdrawn after publication | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20190205 |