Detailed description of the invention
Be described below in detail embodiment of the present utility model, the example of described embodiment is shown in the drawings, and wherein same or similar label represents same or similar element or has element that is identical or similar functions from start to finish.Be exemplary below by the embodiment be described with reference to the drawings, be intended to for explaining the utility model, and can not be interpreted as restriction of the present utility model.
In description of the present utility model, it will be appreciated that, term " " center ", " longitudinal direction ", " transverse direction ", " length ", " width ", " thickness ", " on ", D score, " front ", " afterwards ", " left side ", " right side ", " vertically ", " level ", " top ", " end ", " interior ", " outward ", " clockwise ", " counterclockwise ", " axis ", " radial direction ", orientation or the position relationship of the instruction such as " circumference " are based on orientation shown in the drawings or position relationship, only the utility model and simplified characterization for convenience of description, instead of indicate or imply that the device of indication or element must have specific orientation, with specific azimuth configuration and operation, therefore can not be interpreted as restriction of the present utility model.
In addition, term " first ", " second " only for describing object, and can not be interpreted as instruction or hint relative importance or imply the quantity indicating indicated technical characteristic.Thus, be limited with " first ", the feature of " second " can express or impliedly comprise at least one this feature.In description of the present utility model, the implication of " multiple " is at least two, such as two, three etc., unless otherwise expressly limited specifically.
In the utility model, unless otherwise clearly defined and limited, the term such as term " installation ", " being connected ", " connection ", " fixing " should be interpreted broadly, and such as, can be fixedly connected with, also can be removably connect, or integral; Can be mechanical connection, also can be electrical connection; Can be directly be connected, also indirectly can be connected by intermediary, can be the connection of two element internals or the interaction relationship of two elements, unless otherwise clear and definite restriction.For the ordinary skill in the art, the concrete meaning of above-mentioned term in the utility model can be understood as the case may be.
In the utility model, unless otherwise clearly defined and limited, fisrt feature second feature " on " or D score can be that the first and second features directly contact, or the first and second features are by intermediary mediate contact.And, fisrt feature second feature " on ", " top " and " above " but fisrt feature directly over second feature or oblique upper, or only represent that fisrt feature level height is higher than second feature.Fisrt feature second feature " under ", " below " and " below " can be fisrt feature immediately below second feature or tiltedly below, or only represent that fisrt feature level height is less than second feature.
In one of the present utility model, the utility model proposes a kind of system utilizing dilval to prepare carbonyl nickel powder.According to embodiment of the present utility model, this system comprises: melting appartus, described melting appartus has dilval entrance, sulfur-bearing solid compounds entrance and ferronickel melt outlet, and be suitable for carrying out melt processed, to obtain ferronickel melt by after described dilval and the mixing of sulfur-bearing solid compounds; Atomization granulation device, described atomization granulation device has ferronickel melt inlet and dilval particle outlet, described ferronickel melt inlet is connected with described ferronickel melt outlet, and is suitable for described ferronickel melt being carried out atomization pelletization treatment, to obtain dilval particle; Carbonylation synthesis device, described carbonylation synthesis device has carbon monoxide inlet, dilval particle entrance, gaseous mixture outlet and iron powder outlet, described dilval particle entrance is connected with described dilval particle outlet, and be suitable for described dilval particle being contacted with carbon monoxide, so that the gaseous mixture obtained containing carbonyl nickel, carbonyl iron and carbon monoxide and iron powder; Condensing unit, described condensing unit has gaseous mixture entrance, liquefied mixture outlet and the outlet of the first carbon monoxide, described gaseous mixture entrance exports with described gaseous mixture and is connected, and be suitable for the described gaseous mixture containing carbonyl nickel, carbonyl iron and carbon monoxide to carry out condensation process, so that the liquefied mixture obtained containing carbonyl nickel and carbonyl iron and the first carbon monoxide; Rectifier unit, described rectifier unit has liquefied mixture entrance and the outlet of gaseous state carbonyl nickel, described liquefied mixture entrance exports with described liquefied mixture and is connected, and is suitable for the described liquefied mixture containing carbonyl nickel and carbonyl iron to carry out rectification process, to obtain gaseous state carbonyl nickel; And decomposer, described decomposer has gaseous state carbonyl nickel entrance, carbonyl nickel powder outlet and the outlet of the second carbon monoxide, described gaseous state carbonyl nickel entrance is connected with described gaseous state carbonyl nickel outlet, and be suitable for described gaseous state carbonyl nickel to carry out resolution process, to obtain carbonyl nickel powder and the second carbon monoxide respectively.Inventor finds, by carrying out melt processed by after dilval and the mixing of sulfur-bearing solid compounds, the sulphur in sulfur-bearing solid compounds can be made to enter activated ni in ferronickel melt, namely highly active ferronickel melt is obtained, granulate by carrying out atomization to gained ferronickel melt simultaneously, the contact area of itself and carbon monoxide can be significantly improved, thus itself and carbon monoxide are directly contacted can react generation carbonyls, and carbonyls synthetic ratio is higher, compared with prior art, the utility model does not need to add catalyst in carbonyls building-up process, thus shorten technological process, secondly adopt dilval as the raw material preparing carbonyl nickel powder, the more existing raw copper nickel alloy preparing carbonyl nickel powder is compared, dilval has lower cost, thus while improving dilval value, reduce the production cost of carbonyl nickel powder, and directly apply to STEELMAKING PRODUCTION compared to by dilval, dilval is had higher economic benefit for the preparation of carbonyl nickel powder by the utility model, this entire system technique is simple in addition, convenient operation, large-scale production can be realized.
The system utilizing dilval to prepare carbonyl nickel powder below with reference to Fig. 1-3 pairs of the utility model embodiments is described in detail.According to embodiment of the present utility model, this system comprises:
Melting appartus 100: according to embodiment of the present utility model, melting appartus 100 has dilval entrance 101, sulfur-bearing solid compounds entrance 102 and ferronickel melt outlet 103, and be suitable for carrying out melt processed by after dilval and the mixing of sulfur-bearing solid compounds, thus ferronickel melt can be obtained.Inventor finds, the sulphur in sulfur-bearing solid compounds can be made to enter activated ni in ferronickel melt by melt processed, namely highly active ferronickel melt is obtained, thus significantly improve carbonyls reaction rate, and carbonyls synthetic ratio is higher, compared with prior art, the utility model does not need to add catalyst in carbonyls building-up process, thus shortens technological process.
According to an embodiment of the present utility model, in dilval nickel and iron concrete content and be not particularly limited, those skilled in the art can select according to actual needs, according to specific embodiment of the utility model, dilval nickel content can be 10 ~ 45wt%, and iron content can be 60 ~ 80wt%.Inventor finds, in order to obtain highly purified carbonyl nickel powder in existing preparation technology, usually the copper nickel adopting nickel content higher is needed, cause raw material production cost higher, not easily purchase, and the utility model is lower to nickel grade requirement threshold in raw material, although the grade of nickel is lower in dilval, but adopt method of the present utility model still can prepare highly purified carbonyl nickel powder (nickel content is higher than more than 99%), thus reduce the production cost of carbonyl nickel powder while widening raw material sources.
According to another embodiment of the present utility model, sulfur content in ferronickel melt is also not particularly limited, those skilled in the art can select according to actual needs, and according to specific embodiment of the utility model, in ferronickel melt, sulfur content can account for 0.5 ~ 3% of ferronickel melt gross mass.Inventor finds, in ferronickel melt, sulfur content is higher, make gained dilval seed activity higher, thus be more conducive to carrying out fast of carbonyl nickel synthetic reaction, and carbonyl nickel synthetic ratio is also higher, comparatively prior art adds gaseous state sulfur-bearing thing and compares as catalyst in carbonyl nickel synthesis step, the utility model does not need additionally to add catalyst, thus shorten preparation technology's flow process, but sulfur content is too high in ferronickel melt, improve not obvious to dilval seed activity, and the concentration adding nickel in membership dilution ferronickel melt of excessive sulfur-bearing solid compounds, also can cause sulfur-bearing wastage of material simultaneously, improve production cost.
According to another embodiment of the present utility model, the condition of melt processed is also not particularly limited, and those skilled in the art can select according to actual needs, and according to specific embodiment of the utility model, melt processed can be carried out at 1400 ~ 1600 DEG C.Thus, can make the sulphur in sulfur-bearing solid compounds dispersed to ferronickel melt activated ni, namely obtain highly active ferronickel melt, thus further improve follow-up carbonyls synthetic ratio.
According to another embodiment of the present utility model, the concrete kind of sulfur-bearing solid compounds is also not particularly limited, those skilled in the art can select according to actual needs, and according to specific embodiment of the utility model, sulfur-bearing solid compounds can be sulphur iron.Thus, can effective activation ferronickel melt, thus improve follow-up carbonyls synthetic ratio further, and sulphur iron material cost is lower.
According to another embodiment of the present utility model, dilval can obtain by reducing-melt divisional processing to lateritic nickel ore.Concrete, first just lateritic nickel ore, coal and additive carry out mixed pelletizing, obtain mixing pelletizing, then this mixing pelletizing is carried out reduction treatment in rotary kiln or rotary hearth furnace, obtain metallized pellet, then divide stove to carry out molten divisional processing in electric arc furnaces, mineral hot furnace or non-electric smelting this metallized pellet, obtain dilval and tailings.Inventor finds, adopt lateritic nickel ore as the raw material preparing dilval, although the grade of nickel is lower in lateritic nickel ore, but adopt method of the present utility model still can prepare highly purified carbonyl nickel powder (nickel content is higher than more than 99%), thus reduce the production cost of carbonyl nickel powder while widening raw material sources.
Atomization granulation device 200: according to embodiment of the present utility model, atomization granulation device 200 has ferronickel melt inlet 201 and dilval particle outlet 202, ferronickel melt inlet 201 is connected with ferronickel melt outlet 103, and be suitable for ferronickel melt to carry out atomization pelletization treatment, thus dilval particle can be obtained.Inventor finds; granulate by carrying out atomization to gained ferronickel melt; the contact area of itself and carbon monoxide can be significantly improved; and gained dilval seed activity is higher; thus itself and carbon monoxide are directly contacted can react generation carbonyls, and carbonyls synthetic ratio is higher.In this step, concrete, atomization pelletization utilizes High-Pressure Water or inert gas to be smashed by ferronickel melt in atomizer to become fine droplet, the dilval particle meeting dimensional requirement is obtained again after cooling, oven dry, screening, atomization mechanism is when High-Pressure Water or inert gas impact ferronickel melt, by the surface energy that kinetic transformation is ferronickel melt, form numerous fine particle.
According to an embodiment of the present utility model, dilval grain diameter is also not particularly limited, and those skilled in the art can select according to actual needs, and according to specific embodiment of the utility model, the particle diameter of dilval particle is not more than 0.5 millimeter.Inventor finds, the dilval seed activity of this particle size range is higher, and comparatively large with carbon monoxide contact area in carbonyl nickel synthetic process, thus can significantly improve the synthetic ratio of carbonyl nickel.
Carbonylation synthesis device 300: according to embodiment of the present utility model, carbonylation synthesis device 300 has carbon monoxide inlet 301, dilval particle entrance 302, gaseous mixture outlet 303 and iron powder outlet 304, dilval particle entrance 302 is connected with dilval particle outlet 202, and be suitable for above-mentioned gained dilval particle to contact with carbon monoxide, thus the gaseous mixture that can obtain containing carbonyl nickel, carbonyl iron and carbon monoxide and iron powder.Inventor finds, adopt highly active dilval particle directly to contact with carbon monoxide and can react generation carbonyls, and carbonyls synthetic ratio is higher, compared with prior art, the utility model does not need to add catalyst in carbonyls building-up process, thus shortens technological process.
According to an embodiment of the present utility model, dilval particle and reaction of carbon monoxide condition are also not particularly limited, those skilled in the art can select according to actual needs, according to specific embodiment of the utility model, dilval particle contacts with carbon monoxide and can carry out 24 ~ 48 hours under the condition of 100 ~ 200 degrees Celsius and 5 ~ 15MPa.Thus, adopt this condition can significantly improve the synthetic ratio of carbonyl nickel, and the synthetic ratio of gained carbonyl nickel is up to more than 95%.
According to another embodiment of the present utility model, dilval particle to contact with carbon monoxide thing and can carry out in carbonylation synthesis device, and the volume content of carbon monoxide is not less than 90% of carbonylation synthesis device cumulative volume.Inventor finds, generating the reaction of carbonyls is reversible reaction, and adds the chemical balance that excessive carbon monoxide makes to react and move to the direction generating carbonyls, thus improves carbonyls synthetic ratio further.
Condensing unit 400: according to embodiment of the present utility model, condensing unit 400 has gaseous mixture entrance 401, liquefied mixture outlet 402 and the first carbon monoxide outlet 403, gaseous mixture entrance 401 and gaseous mixture export 303 and are connected, and be suitable for the gaseous mixture containing carbonyl nickel, carbonyl iron and carbon monoxide obtained above to carry out condensation process, thus the liquefied mixture that can obtain containing carbonyl nickel and carbonyl iron and the first carbon monoxide.Thus, the carbonyl nickel in the gaseous mixture containing carbonyl nickel, carbonyl iron and carbon monoxide and carbonyl iron condensation can be made to become liquid by condensation process, carbon monoxide wherein then exists in gaseous form, thus realizes the separation of carbon monoxide.It should be noted that, those skilled in the art can select the condition of condensation process according to actual needs.
Rectifier unit 500: according to embodiment of the present utility model, rectifier unit 500 has liquefied mixture entrance 501 and gaseous state carbonyl nickel outlet 502, liquefied mixture entrance 501 and liquefied mixture export 402 and are connected, and be suitable for the liquefied mixture containing carbonyl nickel and carbonyl iron obtained above to carry out rectification process, thus gaseous state carbonyl nickel can be obtained.Thus, being separated both realizing according to carbonyl nickel and carbonyl iron boiling point difference, and separating obtained gaseous state carbonyl nickel has higher purity.It should be noted that, those skilled in the art can select the actual conditions of rectifying according to actual needs.
Decomposer 600: according to embodiment of the present utility model, decomposer 600 has gaseous state carbonyl nickel entrance 601, carbonyl nickel powder outlet 602 and the second carbon monoxide outlet 603, gaseous state carbonyl nickel entrance 601 is connected with gaseous state carbonyl nickel outlet 502, and be suitable for gaseous state carbonyl nickel to carry out resolution process, thus carbonyl nickel powder and the second carbon monoxide can be obtained respectively.Concrete, carbonyl nickel is unstable, can be decomposed into rapidly carbonyl nickel powder and carbon monoxide, thus can obtain highly purified carbonyl nickel powder (nickel content is higher than 99wt%) when heating.
According to an embodiment of the present utility model, the condition of resolution process is also not particularly limited, those skilled in the art can select according to actual needs, according to specific embodiment of the utility model, resolution process can be carried out under the condition of 230 ~ 300 degrees Celsius and 0.01 ~ 0.05MPa.Inventor finds, this decomposition condition significantly can be better than the decomposition efficiency that other improve carbonyl nickel, thus can obtain highly purified carbonyl nickel powder.
The dilval that utilizes according to the utility model embodiment prepares the system of carbonyl nickel powder by carrying out melt processed by after dilval and the mixing of sulfur-bearing solid compounds, the sulphur in sulfur-bearing solid compounds can be made to enter activated ni in ferronickel melt, namely highly active ferronickel melt is obtained, granulate by carrying out atomization to gained ferronickel melt simultaneously, the contact area of itself and carbon monoxide can be significantly improved, thus itself and carbon monoxide are directly contacted can react generation carbonyls, and carbonyls synthetic ratio is higher, compared with prior art, the utility model does not need to add catalyst in carbonyls building-up process, thus shorten technological process, secondly adopt dilval as the raw material preparing carbonyl nickel powder, the more existing raw copper nickel alloy preparing carbonyl nickel powder is compared, dilval has lower cost, thus while improving dilval value, reduce the production cost of carbonyl nickel powder, and directly apply to STEELMAKING PRODUCTION compared to by dilval, dilval is had higher economic benefit for the preparation of carbonyl nickel powder by the utility model, this entire system technique is simple in addition, convenient operation, large-scale production can be realized.
With reference to figure 2, according to an embodiment of the present utility model, first carbon monoxide outlet 403 is connected with carbon monoxide inlet 301, and be suitable for condensing unit gained first carbon monoxide being back to carbonylation synthesis device 300 and dilval particle contacts, thus carbon monoxide cycle utilization rate can be significantly improved.
With reference to figure 3, according to another embodiment of the present utility model, second carbon monoxide outlet 603 is connected with carbon monoxide inlet 301, and be suitable for decomposer gained second carbon monoxide being back to carbonylation synthesis device 300 and dilval particle contacts, thus carbon monoxide cycle utilization rate can be significantly improved.
In one of the present utility model, the utility model proposes a kind of method utilizing dilval to prepare carbonyl nickel powder.According to embodiment of the present utility model, the method comprises: (1) carries out melt processed, to obtain ferronickel melt by after described dilval and the mixing of sulfur-bearing solid compounds; (2) described ferronickel melt is carried out atomization pelletization treatment, to obtain dilval particle; (3) described dilval particle is contacted with carbon monoxide, so that the gaseous mixture obtained containing carbonyl nickel, carbonyl iron and carbon monoxide and iron powder; (4) the described gaseous mixture containing carbonyl nickel, carbonyl iron and carbon monoxide is carried out condensation process, so that the liquefied mixture obtained containing carbonyl nickel and carbonyl iron and the first carbon monoxide; (5) the described liquefied mixture containing carbonyl nickel and carbonyl iron is carried out rectification process, to obtain gaseous state carbonyl nickel; And described gaseous state carbonyl nickel is carried out resolution process by (6), to obtain carbonyl nickel powder and the second carbon monoxide respectively.Inventor finds, by carrying out melt processed by after dilval and the mixing of sulfur-bearing solid compounds, the sulphur in sulfur-bearing solid compounds can be made to enter activated ni in ferronickel melt, namely highly active ferronickel melt is obtained, granulate by carrying out atomization to gained ferronickel melt simultaneously, the contact area of itself and carbon monoxide can be significantly improved, thus itself and carbon monoxide are directly contacted can react generation carbonyls, and carbonyls synthetic ratio is higher, compared with prior art, the utility model does not need to add catalyst in carbonyls building-up process, thus shorten technological process, secondly adopt dilval as the raw material preparing carbonyl nickel powder, the more existing raw copper nickel alloy preparing carbonyl nickel powder is compared, dilval has lower cost, thus while improving dilval value, reduce the production cost of carbonyl nickel powder, and directly apply to STEELMAKING PRODUCTION compared to by dilval, dilval is had higher economic benefit for the preparation of carbonyl nickel powder by the utility model, the method integrated artistic is simple in addition, convenient operation, large-scale production can be realized.
Conveniently understand, below with reference to Fig. 4-6, the method adopting the System Implementation utilizing dilval to prepare carbonyl nickel powder of the utility model embodiment to utilize dilval to prepare carbonyl nickel powder is described in detail.According to embodiment of the present utility model, the method comprises:
S100: carry out melt processed by after dilval and the mixing of sulfur-bearing solid compounds
According to embodiment of the present utility model, carry out melt processed by after dilval and the mixing of sulfur-bearing solid compounds, thus ferronickel melt can be obtained.Inventor finds, the sulphur in sulfur-bearing solid compounds can be made to enter activated ni in ferronickel melt by melt processed, namely highly active ferronickel melt is obtained, thus significantly improve carbonyls reaction rate, and carbonyls synthetic ratio is higher, compared with prior art, the utility model does not need to add catalyst in carbonyls building-up process, thus shortens technological process.
According to an embodiment of the present utility model, in dilval nickel and iron concrete content and be not particularly limited, those skilled in the art can select according to actual needs, according to specific embodiment of the utility model, dilval nickel content can be 10 ~ 45wt%, and iron content can be 60 ~ 80wt%.Inventor finds, in order to obtain highly purified carbonyl nickel powder in existing preparation technology, usually the copper nickel adopting nickel content higher is needed, cause raw material production cost higher, not easily purchase, and the utility model is lower to nickel grade requirement threshold in raw material, although the grade of nickel is lower in dilval, but adopt method of the present utility model still can prepare highly purified carbonyl nickel powder (nickel content is higher than more than 99%), thus reduce the production cost of carbonyl nickel powder while widening raw material sources.
According to another embodiment of the present utility model, sulfur content in ferronickel melt is also not particularly limited, those skilled in the art can select according to actual needs, and according to specific embodiment of the utility model, in ferronickel melt, sulfur content can account for 0.5 ~ 3% of ferronickel melt gross mass.Inventor finds, in ferronickel melt, sulfur content is higher, make gained dilval seed activity higher, thus be more conducive to carrying out fast of carbonyl nickel synthetic reaction, and carbonyl nickel synthetic ratio is also higher, comparatively prior art adds gaseous state sulfur-bearing thing and compares as catalyst in carbonyl nickel synthesis step, the utility model does not need additionally to add catalyst, thus shorten preparation technology's flow process, but sulfur content is too high in ferronickel melt, improve not obvious to dilval seed activity, and the concentration adding nickel in membership dilution ferronickel melt of excessive sulfur-bearing solid compounds, also can cause sulfur-bearing wastage of material simultaneously, improve production cost.
According to another embodiment of the present utility model, the condition of melt processed is also not particularly limited, and those skilled in the art can select according to actual needs, and according to specific embodiment of the utility model, melt processed can be carried out at 1400 ~ 1600 DEG C.Thus, can make the sulphur in sulfur-bearing solid compounds dispersed to ferronickel melt activated ni, namely obtain highly active ferronickel melt, thus further improve follow-up carbonyls synthetic ratio.
According to another embodiment of the present utility model, the concrete kind of sulfur-bearing solid compounds is also not particularly limited, those skilled in the art can select according to actual needs, and according to specific embodiment of the utility model, sulfur-bearing solid compounds can be sulphur iron.Thus, can effective activation ferronickel melt, thus improve follow-up carbonyls synthetic ratio further, and sulphur iron material cost is lower.
According to another embodiment of the present utility model, dilval can obtain by reducing-melt divisional processing to lateritic nickel ore.Concrete, first just lateritic nickel ore, coal and additive carry out mixed pelletizing, obtain mixing pelletizing, then this mixing pelletizing is carried out reduction treatment in rotary kiln or rotary hearth furnace, obtain metallized pellet, then divide stove to carry out molten divisional processing in electric arc furnaces, mineral hot furnace or non-electric smelting this metallized pellet, obtain dilval and tailings.Inventor finds, adopt lateritic nickel ore as the raw material preparing dilval, although the grade of nickel is lower in lateritic nickel ore, but adopt method of the present utility model still can prepare highly purified carbonyl nickel powder (nickel content is higher than more than 99%), thus reduce the production cost of carbonyl nickel powder while widening raw material sources.
S200: ferronickel melt is carried out atomization pelletization treatment
According to embodiment of the present utility model, ferronickel melt is carried out atomization pelletization treatment, thus dilval particle can be obtained.Inventor finds; granulate by carrying out atomization to gained ferronickel melt; the contact area of itself and carbon monoxide can be significantly improved; and gained dilval seed activity is higher; thus itself and carbon monoxide are directly contacted can react generation carbonyls, and carbonyls synthetic ratio is higher.In this step, concrete, atomization pelletization utilizes High-Pressure Water or inert gas to be smashed by ferronickel melt in atomizer to become fine droplet, the dilval particle meeting dimensional requirement is obtained again after cooling, oven dry, screening, atomization mechanism is when High-Pressure Water or inert gas impact ferronickel melt, by the surface energy that kinetic transformation is ferronickel melt, form numerous fine particle.
According to an embodiment of the present utility model, dilval grain diameter is also not particularly limited, and those skilled in the art can select according to actual needs, and according to specific embodiment of the utility model, the particle diameter of dilval particle is not more than 0.5 millimeter.Inventor finds, the dilval seed activity of this particle size range is higher, and comparatively large with carbon monoxide contact area in carbonyl nickel synthetic process, thus can significantly improve the synthetic ratio of carbonyl nickel.
S300: dilval particle is contacted with carbon monoxide
According to embodiment of the present utility model, above-mentioned gained dilval particle is contacted with carbon monoxide, thus the gaseous mixture that can obtain containing carbonyl nickel, carbonyl iron and carbon monoxide and iron powder.Inventor finds, adopt highly active dilval particle directly to contact with carbon monoxide and can react generation carbonyls, and carbonyls synthetic ratio is higher, compared with prior art, the utility model does not need to add catalyst in carbonyls building-up process, thus shortens technological process.
According to an embodiment of the present utility model, dilval particle and reaction of carbon monoxide condition are also not particularly limited, those skilled in the art can select according to actual needs, according to specific embodiment of the utility model, dilval particle contacts with carbon monoxide and can carry out 24 ~ 48 hours under the condition of 100 ~ 200 degrees Celsius and 5 ~ 15MPa.Thus, adopt this condition can significantly improve the synthetic ratio of carbonyl nickel, and the synthetic ratio of gained carbonyl nickel is up to more than 95%.
According to another embodiment of the present utility model, dilval particle to contact with carbon monoxide thing and can carry out in carbonylation synthesis device, and the volume content of carbon monoxide is not less than 90% of carbonylation synthesis device cumulative volume.Inventor finds, generating the reaction of carbonyls is reversible reaction, and adds the chemical balance that excessive carbon monoxide makes to react and move to the direction generating carbonyls, thus improves carbonyls synthetic ratio further.
S400: the gaseous mixture containing carbonyl nickel, carbonyl iron and carbon monoxide is carried out condensation process
According to embodiment of the present utility model, the gaseous mixture containing carbonyl nickel, carbonyl iron and carbon monoxide obtained above is carried out condensation process, thus the liquefied mixture that can obtain containing carbonyl nickel and carbonyl iron and the first carbon monoxide.Thus, the carbonyl nickel in the gaseous mixture containing carbonyl nickel, carbonyl iron and carbon monoxide and carbonyl iron condensation can be made to become liquid by condensation process, carbon monoxide wherein then exists in gaseous form, thus realizes the separation of carbon monoxide.It should be noted that, those skilled in the art can select the condition of condensation process according to actual needs.
S500: the liquefied mixture containing carbonyl nickel and carbonyl iron is carried out rectification process
According to embodiment of the present utility model, the liquefied mixture containing carbonyl nickel and carbonyl iron obtained above is carried out rectification process, thus gaseous state carbonyl nickel can be obtained.Thus, being separated both realizing according to carbonyl nickel and carbonyl iron boiling point difference, and separating obtained gaseous state carbonyl nickel has higher purity.It should be noted that, those skilled in the art can select the actual conditions of rectifying according to actual needs.
S600: gaseous state carbonyl nickel is carried out resolution process
According to embodiment of the present utility model, gaseous state carbonyl nickel is carried out resolution process, thus carbonyl nickel powder and the second carbon monoxide can be obtained respectively.Concrete, carbonyl nickel is unstable, can be decomposed into rapidly carbonyl nickel powder and carbon monoxide, thus can obtain highly purified carbonyl nickel powder (nickel content is higher than 99wt%) when heating.
According to an embodiment of the present utility model, the condition of resolution process is also not particularly limited, those skilled in the art can select according to actual needs, according to specific embodiment of the utility model, resolution process can be carried out under the condition of 230 ~ 300 degrees Celsius and 0.01 ~ 0.05MPa.Inventor finds, this decomposition condition significantly can be better than the decomposition efficiency that other improve carbonyl nickel, thus can obtain highly purified carbonyl nickel powder.
Dilval is utilized to prepare the method for carbonyl nickel powder by carrying out melt processed by after dilval and the mixing of sulfur-bearing solid compounds according to the System Implementation utilizing dilval to prepare carbonyl nickel powder of the utility model embodiment, the sulphur in sulfur-bearing solid compounds can be made to enter activated ni in ferronickel melt, namely highly active ferronickel melt is obtained, granulate by carrying out atomization to gained ferronickel melt simultaneously, the contact area of itself and carbon monoxide can be significantly improved, thus itself and carbon monoxide are directly contacted can react generation carbonyls, and carbonyls synthetic ratio is higher, compared with prior art, the utility model does not need to add catalyst in carbonyls building-up process, thus shorten technological process, secondly adopt dilval as the raw material preparing carbonyl nickel powder, the more existing raw copper nickel alloy preparing carbonyl nickel powder is compared, dilval has lower cost, thus while improving dilval value, reduce the production cost of carbonyl nickel powder, and directly apply to STEELMAKING PRODUCTION compared to by dilval, dilval is had higher economic benefit for the preparation of carbonyl nickel powder by the utility model, the method integrated artistic is simple in addition, convenient operation, large-scale production can be realized.
With reference to figure 5, comprise further according to the method that the System Implementation utilizing dilval to prepare carbonyl nickel powder of the utility model embodiment utilizes dilval to prepare carbonyl nickel powder:
S700: the first carbon monoxide is returned S300 and dilval particle contacts.
According to embodiment of the present utility model, condensation process gained first carbon monoxide is back to S300 and dilval particle contacts, thus carbon monoxide cycle utilization rate can be significantly improved.
With reference to figure 6, comprise further according to the method that the System Implementation utilizing dilval to prepare carbonyl nickel powder of the utility model embodiment utilizes dilval to prepare carbonyl nickel powder:
S800: the second carbon monoxide is returned S300 and dilval particle contacts
According to embodiment of the present utility model, resolution process gained second carbon monoxide is back to S300 and dilval particle contacts, thus improves carbon monoxide cycle utilization rate further.
Below with reference to specific embodiment, be described the utility model, it should be noted that, these embodiments are only descriptive, and limit the utility model never in any form.
Embodiment 1
Melt processed is carried out after getting the dilval of table 1 composition and the mixing of sulphur iron, obtain ferronickel melt (in ferronickel melt, sulfur content is 0.5wt%), then gained ferronickel melt is carried out atomization pelletization treatment, obtain the dilval particle of average grain diameter 0.2 millimeter, then dilval particle and CO counter current contacting generation oxonation are generated containing carbonyl nickel, the gaseous mixture of carbonyl iron and carbon monoxide, carbonylation conditions is: pressure 7.5MPa, temperature 185 DEG C, time 35h, CO gas concentration 90.5%, then will containing carbonyl nickel, the gaseous mixture of carbonyl iron and carbon monoxide is delivered to condensation process in condenser, obtain the liquefied mixture containing carbonyl nickel and carbonyl iron and carbon monoxide, carbon monoxide is returned carbonylation synthesis device to continue to use, and the liquefied mixture containing carbonyl nickel and carbonyl iron obtained is sent into rectifying column again and carry out rectifying and obtain high-purity gaseous state carbonyl nickel, finally gaseous state carbonyl nickel is sent into decomposer to carry out decomposing and obtain high purity nickel (major impurity is C and Fe) that nickel grade is 99.82wt% and carbon monoxide, wherein carbon monoxide returns carbonylation synthesis device continuation use.
Embodiment 2
Melt processed is carried out after getting the dilval of table 1 composition and the mixing of sulphur iron, obtain ferronickel melt (in ferronickel melt, sulfur content is 1.5wt%), then gained ferronickel melt is carried out atomization pelletization treatment, obtain the dilval particle of average grain diameter 0.5 millimeter, then dilval particle and CO counter current contacting generation oxonation are generated containing carbonyl nickel, the gaseous mixture of carbonyl iron and carbon monoxide, carbonylation conditions is: pressure 12.5MPa, temperature 135 DEG C, time 46h, CO gas concentration 92%, then will containing carbonyl nickel, the gaseous mixture of carbonyl iron and carbon monoxide is delivered to condensation process in condenser, obtain the liquefied mixture containing carbonyl nickel and carbonyl iron and carbon monoxide, gained carbon monoxide is returned carbonylation synthesis device to continue to use, and the liquefied mixture containing carbonyl nickel and carbonyl iron obtained is sent into rectifying column again and carry out rectifying and obtain high-purity gaseous state carbonyl nickel, finally gaseous state carbonyl nickel is sent into decomposer to carry out decomposing and obtain high purity nickel (major impurity is C and Fe) that nickel grade is 99.54wt% and carbon monoxide, wherein carbon monoxide returns carbonylation synthesis device continuation use.
Embodiment 3
Melt processed is carried out after getting the dilval of table 1 composition and the mixing of sulphur iron, obtain ferronickel melt (in ferronickel melt, sulfur content is 3wt%), then gained ferronickel melt is carried out atomization pelletization treatment, obtain the dilval particle of average grain diameter 0.35 millimeter, then dilval particle and CO counter current contacting generation oxonation are generated containing carbonyl nickel, the gaseous mixture of carbonyl iron and carbon monoxide, carbonylation conditions is: pressure 15MPa, temperature 155 DEG C, time 29h, CO gas concentration 90%, then will containing carbonyl nickel, the gaseous mixture of carbonyl iron and carbon monoxide is delivered to condensation process in condenser, obtain the liquefied mixture containing carbonyl nickel and carbonyl iron and carbon monoxide, carbon monoxide is returned carbonylation synthesis device to continue to use, and the liquefied mixture containing carbonyl nickel and carbonyl iron obtained is sent into rectifying column again and carry out rectifying and obtain high-purity gaseous state carbonyl nickel, finally gaseous state carbonyl nickel is sent into decomposer to carry out decomposing and obtain high purity nickel (major impurity is C and Fe) that nickel grade is 99.82wt% and carbon monoxide, wherein carbon monoxide returns carbonylation synthesis device continuation use.
Table 1 embodiment 1 ~ 3 dilval main component, wt.%
Embodiment |
TFe |
Ni |
Co |
S |
Si |
Cr |
Mn |
P |
C |
1 |
85.99 |
12.57 |
0.93 |
0.17 |
0.01 |
0.06 |
0.01 |
0.05 |
0.04 |
2 |
78.19 |
20.28 |
0.63 |
0.14 |
0.35 |
0.08 |
0.01 |
0.04 |
0.11 |
3 |
53.15 |
44.19 |
0.60 |
0.10 |
0.19 |
0.09 |
0.037 |
0.03 |
0.08 |
In the description of this description, specific features, structure, material or feature that the description of reference term " embodiment ", " some embodiments ", " example ", " concrete example " or " some examples " etc. means to describe in conjunction with this embodiment or example are contained at least one embodiment of the present utility model or example.In this manual, to the schematic representation of above-mentioned term not must for be identical embodiment or example.And the specific features of description, structure, material or feature can combine in one or more embodiment in office or example in an appropriate manner.In addition, when not conflicting, the feature of the different embodiment described in this description or example and different embodiment or example can carry out combining and combining by those skilled in the art.
Although illustrate and described embodiment of the present utility model above, be understandable that, above-described embodiment is exemplary, can not be interpreted as restriction of the present utility model, those of ordinary skill in the art can change above-described embodiment, revises, replace and modification in scope of the present utility model.