CN105033269A - Method and system for preparing carbonyl nickel powder through laterite nickel ore - Google Patents
Method and system for preparing carbonyl nickel powder through laterite nickel ore Download PDFInfo
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- carbon monoxide
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- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 title claims abstract description 635
- 229910052759 nickel Inorganic materials 0.000 title claims abstract description 218
- 238000000034 method Methods 0.000 title claims abstract description 111
- 239000011504 laterite Substances 0.000 title abstract description 5
- 229910001710 laterite Inorganic materials 0.000 title abstract description 5
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 182
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 claims abstract description 144
- 229910002091 carbon monoxide Inorganic materials 0.000 claims abstract description 144
- 239000002245 particle Substances 0.000 claims abstract description 93
- 230000008569 process Effects 0.000 claims abstract description 70
- 229910052742 iron Inorganic materials 0.000 claims abstract description 67
- 238000005453 pelletization Methods 0.000 claims abstract description 64
- 239000003245 coal Substances 0.000 claims abstract description 62
- 239000008246 gaseous mixture Substances 0.000 claims abstract description 44
- 239000011593 sulfur Substances 0.000 claims abstract description 39
- 229910052717 sulfur Inorganic materials 0.000 claims abstract description 39
- 239000000654 additive Substances 0.000 claims abstract description 32
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims description 99
- 239000005864 Sulphur Substances 0.000 claims description 65
- 238000002156 mixing Methods 0.000 claims description 47
- 238000003786 synthesis reaction Methods 0.000 claims description 34
- 230000015572 biosynthetic process Effects 0.000 claims description 32
- 230000000996 additive effect Effects 0.000 claims description 31
- 230000006315 carbonylation Effects 0.000 claims description 28
- 238000005810 carbonylation reaction Methods 0.000 claims description 28
- 238000012545 processing Methods 0.000 claims description 19
- 238000000746 purification Methods 0.000 claims description 10
- 238000005469 granulation Methods 0.000 claims description 8
- 230000003179 granulation Effects 0.000 claims description 8
- 229910052783 alkali metal Inorganic materials 0.000 claims description 4
- 229910000272 alkali metal oxide Inorganic materials 0.000 claims description 4
- -1 alkali metal salt Chemical class 0.000 claims description 4
- 150000001447 alkali salts Chemical class 0.000 claims description 4
- 229910000287 alkaline earth metal oxide Inorganic materials 0.000 claims description 4
- 239000008188 pellet Substances 0.000 abstract description 10
- 229910000640 Fe alloy Inorganic materials 0.000 abstract 2
- 229910000990 Ni alloy Inorganic materials 0.000 abstract 2
- 125000002915 carbonyl group Chemical group [*:2]C([*:1])=O 0.000 description 75
- 239000002994 raw material Substances 0.000 description 29
- 238000004519 manufacturing process Methods 0.000 description 22
- 238000006243 chemical reaction Methods 0.000 description 20
- 238000006722 reduction reaction Methods 0.000 description 19
- 230000009467 reduction Effects 0.000 description 17
- 239000003054 catalyst Substances 0.000 description 16
- 239000000203 mixture Substances 0.000 description 16
- 239000003638 chemical reducing agent Substances 0.000 description 14
- 230000000694 effects Effects 0.000 description 14
- 239000000463 material Substances 0.000 description 13
- 238000009833 condensation Methods 0.000 description 9
- 230000005494 condensation Effects 0.000 description 9
- 238000005516 engineering process Methods 0.000 description 9
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 8
- 238000000354 decomposition reaction Methods 0.000 description 8
- 238000003723 Smelting Methods 0.000 description 7
- 238000010586 diagram Methods 0.000 description 6
- 239000004615 ingredient Substances 0.000 description 6
- 229910052500 inorganic mineral Inorganic materials 0.000 description 6
- 239000011707 mineral Substances 0.000 description 6
- 229910000863 Ferronickel Inorganic materials 0.000 description 5
- 230000007613 environmental effect Effects 0.000 description 5
- 239000007789 gas Substances 0.000 description 5
- 239000007788 liquid Substances 0.000 description 5
- 229910000792 Monel Inorganic materials 0.000 description 4
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 4
- 229910000029 sodium carbonate Inorganic materials 0.000 description 4
- 239000002699 waste material Substances 0.000 description 4
- 229910045601 alloy Inorganic materials 0.000 description 3
- 239000000956 alloy Substances 0.000 description 3
- 229910052799 carbon Inorganic materials 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- 239000012535 impurity Substances 0.000 description 3
- 238000011946 reduction process Methods 0.000 description 3
- 230000002441 reversible effect Effects 0.000 description 3
- 235000019738 Limestone Nutrition 0.000 description 2
- 229910017709 Ni Co Inorganic materials 0.000 description 2
- 238000003916 acid precipitation Methods 0.000 description 2
- 238000000889 atomisation Methods 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 239000003034 coal gas Substances 0.000 description 2
- 239000000567 combustion gas Substances 0.000 description 2
- 125000004122 cyclic group Chemical group 0.000 description 2
- 238000010891 electric arc Methods 0.000 description 2
- 229910052840 fayalite Inorganic materials 0.000 description 2
- 229910052839 forsterite Inorganic materials 0.000 description 2
- 239000000295 fuel oil Substances 0.000 description 2
- 239000006028 limestone Substances 0.000 description 2
- HCWCAKKEBCNQJP-UHFFFAOYSA-N magnesium orthosilicate Chemical compound [Mg+2].[Mg+2].[O-][Si]([O-])([O-])[O-] HCWCAKKEBCNQJP-UHFFFAOYSA-N 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 239000003345 natural gas Substances 0.000 description 2
- 229910000480 nickel oxide Inorganic materials 0.000 description 2
- GNRSAWUEBMWBQH-UHFFFAOYSA-N oxonickel Chemical compound [Ni]=O GNRSAWUEBMWBQH-UHFFFAOYSA-N 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 230000009257 reactivity Effects 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 239000010935 stainless steel Substances 0.000 description 2
- 229910001220 stainless steel Inorganic materials 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000010189 synthetic method Methods 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 229910000881 Cu alloy Inorganic materials 0.000 description 1
- 229910004298 SiO 2 Inorganic materials 0.000 description 1
- FDEJSJBWOCAQAD-UHFFFAOYSA-N [Ni].O=C=[Ni] Chemical compound [Ni].O=C=[Ni] FDEJSJBWOCAQAD-UHFFFAOYSA-N 0.000 description 1
- 238000001994 activation Methods 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 239000002817 coal dust Substances 0.000 description 1
- YOCUPQPZWBBYIX-UHFFFAOYSA-N copper nickel Chemical compound [Ni].[Cu] YOCUPQPZWBBYIX-UHFFFAOYSA-N 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000006870 function Effects 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 238000009434 installation Methods 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N iron oxide Inorganic materials [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- NQNBVCBUOCNRFZ-UHFFFAOYSA-N nickel ferrite Chemical compound [Ni]=O.O=[Fe]O[Fe]=O NQNBVCBUOCNRFZ-UHFFFAOYSA-N 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- WWNBZGLDODTKEM-UHFFFAOYSA-N sulfanylidenenickel Chemical compound [Ni]=S WWNBZGLDODTKEM-UHFFFAOYSA-N 0.000 description 1
Abstract
The invention discloses a method and system for preparing carbonyl nickel powder through laterite nickel ore. The method includes the steps that firstly, the laterite nickel ore, high-sulfur coal and additives are mixed for pelletizing so that mixed pellets can be obtained; secondly, the mixed pellets are reduced, molten and separated so that nickel-containing molten iron and tailings can be obtained; thirdly, the nickel-containing molten iron is pelletized so that nickel and iron alloy particles can be obtained; fourthly, the nickel and iron alloy particles make contact with carbon monoxide so that gaseous mixtures containing carbonyl nickel, carbonyl iron and carbon monoxide and iron powder can be obtained; fifthly, the gaseous mixtures containing carbonyl nickel, carbonyl iron and carbon monoxide are purified so that gaseous carbonyl nickel and first carbon monoxide can be obtained; and sixthly, the gaseous carbonyl nickel is decomposed so that thecarbonyl nickel powder and second carbon monoxide can be obtained. According to the method, the low-price laterite nickel ore can be effectively utilized to prepare the high-purity carbonyl nickel powder, the technological process is simple, and the method is environment-friendly.
Description
Technical field
The invention belongs to metallurgical technology field, specifically, the present invention relates to a kind of method and system utilizing lateritic nickel ore to prepare carbonyl nickel powder.
Background technology
In recent years, along with the exhaustion of high-grade nickel sulfide ore and the fast development of domestic stainless steel industry, low-grade laterite nickel ore has become the primary raw material producing ferro-nickel product.In order to solve the Rational Utilization of lateritic nickel ore, take lateritic nickel ore as raw material, coal dust is reducing agent, adopts direct-reduction process that the iron nickel oxide in ore is reduced into metallic iron and metallic nickel, then through a superfusion point stove, nickel is enriched in dilval.Commercial Application at present to dilval, only rest in the aspect of the raw material that it can be used as smelting stainless steel its research, value-added content of product is not high yet.
Carbonyl nickel is found by Meng De and Lan Ji for 1889, they find that the CO of four molecules can react with the active nickel of a molecule in normal pressure and 40 ~ 100 DEG C and generate colourless gas and carbonyl nickel, and they prove that this reaction is reversible further, heating carbonyl nickel just resolves into nickel and CO to 150 ~ 300 DEG C.Carbonyl process produces simple metal, optionally can not only generate carbonyl products, and can easily be separated Sum decomposition under suitable condition and become highly purified metal.Such as, the carbonyls of nickel and iron differs greatly due to their boiling point, and be respectively 43 DEG C and 103 DEG C, available straightforward procedure is separated.International Nickel company of Canada Ltd. reports, has the corronil of certain sulfur content, after atomization is granulated, can obtain highly active carbonylation synthesis raw material, material composition Ni65 ~ 70%, Cu15%, Fe1%, S4 ~ 5%.
Chinese research carbonylation metallurgical technology also has the history of more than 50 year, but all do not form systematization and industrialization, and raw material is selected from electrolytic nickel, this all causes production carbonyl nickel nickel powder cost and remains high, and utilizes other nickel-containing material to produce carbonyl nickel and is still a technical barrier.
Chinese patent CN1603240A discloses a kind of synthetic method of carbonyl nickel, monel or nickel copper alloy are placed in fixed bed reactors by the method, pass into carbon monoxide and carry out oxonation, at oxonation condition pressure 5 ~ 15MPa, at temperature 150 ~ 250 DEG C, obtain carbonyl nickel product.But the shortcoming of the method is nickel in monel is not activated, the reactivity of nickel is low, and alloy is not also granulated in addition, limited with the contact area of CO, and these will have a strong impact on the synthesis of carbonyl nickel.
Chinese patent CN1775695A discloses a kind of synthetic method of carbonyl nickel, and monel is carried out atomization process in molten state and granulates by the method, carries out carbonylation, carbonylation synthesis condition: CO content >=92% in the autoclave of 10 liters; CO gas circulation rate 8 ~ 12 times/hour in the system of carbonylation synthesis, pressure: 5 ~ 12Mpa; Temperature: 100 ~ 150 DEG C; Generated time: 24 ~ 32 hours.But the shortcoming of the method be nickel in monel not through activation process, the reactivity of nickel is low, is unfavorable for the synthesis of carbonyl nickel.
Therefore, the existing technology preparing nickel is further improved.
Summary of the invention
The present invention is intended to solve one of technical problem in correlation technique at least to a certain extent.For this reason, one object of the present invention is to propose a kind of method and system utilizing lateritic nickel ore to prepare carbonyl nickel powder, and the method can effectively utilize cheap lateritic nickel ore to prepare highly purified carbonyl nickel powder, and technological process is simple, environmental friendliness.
In one aspect of the invention, the present invention proposes a kind of method utilizing lateritic nickel ore to prepare carbonyl nickel powder, according to embodiments of the invention, the method comprises:
(1) lateritic nickel ore, sulphur coal and additive are carried out mixed pelletizing, to obtain mixing pelletizing;
(2) described mixing pelletizing is carried out reduce-melt divisional processing, to obtain nickel-containing molten iron and tailings;
(3) described nickel-containing molten iron is carried out pelletization treatment, to obtain dilval particle;
(4) 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;
(5) the described gaseous mixture containing carbonyl nickel, carbonyl iron and carbon monoxide is carried out purification processes, to obtain gaseous state carbonyl nickel and the first carbon monoxide; And
(6) described gaseous state carbonyl nickel is carried out resolution process, to obtain carbonyl nickel powder and the second carbon monoxide respectively.
Thus, the method utilizing lateritic nickel ore to prepare carbonyl nickel powder according to the embodiment of the present invention can effectively utilize cheap lateritic nickel ore to prepare highly purified carbonyl nickel powder, and technological process is simple, environmental friendliness.
In addition, the method utilizing lateritic nickel ore to prepare carbonyl nickel powder according to the above embodiment of the present invention can also have following additional technical characteristic:
In some embodiments of the invention, in step (1), described high-sulfur sulfur content of coal is higher than 3wt%.Thus, not only can reduce reducing agent cost, and significantly can simplify follow-up carbonylic synthesis technology flow process.
In some embodiments of the invention, in step (1), described additive is be selected from least one in alkali metal oxide, alkali metal salt, alkaline earth oxide and alkali salt.
In another aspect of the present invention, the present invention proposes a kind of system utilizing lateritic nickel ore to prepare carbonyl nickel powder, according to embodiments of the invention, this system comprises:
Mixed pelletizing device, described mixed pelletizing device has lateritic nickel ore entrance, sulphur coal entrance, additive entrance and the outlet of mixing pelletizing, and is suitable for lateritic nickel ore, sulphur coal and additive to carry out mixed pelletizing, to obtain mixing pelletizing;
Reduction-molten separating device, described reduction-molten separating device has mixing pelletizing entrance, nickel-containing molten iron outlet and tailings outlet, described mixing pelletizing entrance is connected with the outlet of described mixing pelletizing, and be suitable for described mixing pelletizing to carry out reducing-melt divisional processing, to obtain nickel-containing molten iron and tailings;
Granulation device, described granulation device has nickel-containing molten iron entrance and dilval particle outlet, and described nickel-containing molten iron entrance exports with described nickel-containing molten iron and is connected, and is suitable for described nickel-containing molten iron to carry out 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;
Purifying plant, described purifying plant has gaseous mixture entrance, the outlet of gaseous state carbonyl nickel and the first carbon monoxide and exports described gaseous mixture entrance and to export with described gaseous mixture and be connected, and be suitable for the described gaseous mixture containing carbonyl nickel, carbonyl iron and carbon monoxide to carry out purification processes, to obtain gaseous state carbonyl nickel and the first carbon monoxide; 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.
Thus, the system utilizing lateritic nickel ore to prepare carbonyl nickel powder according to the embodiment of the present invention can effectively utilize cheap lateritic nickel ore to prepare highly purified carbonyl nickel powder, and technological process is simple, environmental friendliness.
In addition, the system utilizing lateritic nickel ore to prepare carbonyl nickel powder according to the above embodiment of the present invention can also have following additional technical characteristic:
In some embodiments of the invention, described first carbon monoxide outlet is connected with described carbon monoxide inlet, and is suitable for described first carbon monoxide to return described carbonylation synthesis device and described dilval particle contacts.Thus, the cyclic utilization rate of carbon monoxide can be significantly improved.
In some embodiments of the invention, described second carbon monoxide outlet is connected with described carbon monoxide inlet, and is suitable for described second carbon monoxide to return described carbonylation synthesis device and described dilval particle contacts.Thus, the cyclic utilization rate of carbon monoxide can be improved further.
Additional aspect of the present invention and advantage will part provide in the following description, and part will become obvious from the following description, or be recognized by practice of the present invention.
Accompanying drawing explanation
Above-mentioned and/or additional aspect of the present invention and advantage will become obvious and easy understand from accompanying drawing below combining to the description of embodiment, wherein:
Fig. 1 is the method flow schematic diagram utilizing lateritic nickel ore to prepare carbonyl nickel powder according to an embodiment of the invention;
Fig. 2 prepares the method flow schematic diagram of carbonyl nickel powder according to the lateritic nickel ore that utilizes of another embodiment of the present invention;
Fig. 3 prepares the method flow schematic diagram of carbonyl nickel powder according to the lateritic nickel ore that utilizes of another embodiment of the present invention;
Fig. 4 is the system architecture schematic diagram utilizing lateritic nickel ore to prepare carbonyl nickel powder according to an embodiment of the invention;
Fig. 5 prepares the system architecture schematic diagram of carbonyl nickel powder according to the lateritic nickel ore that utilizes of another embodiment of the present invention;
Fig. 6 prepares the system architecture schematic diagram of carbonyl nickel powder according to the lateritic nickel ore that utilizes of another embodiment of the present invention.
Detailed description of the invention
Be described below in detail embodiments of the invention, 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 present invention, and can not limitation of the present invention be interpreted as.
In describing the invention, 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 present invention for convenience of description and simplified characterization, instead of indicate or imply that the device of indication or element must have specific orientation, with specific azimuth configuration and operation, therefore limitation of the present invention can not be interpreted as.
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 describing the invention, the implication of " multiple " is at least two, such as two, three etc., unless otherwise expressly limited specifically.
In the present invention, 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, above-mentioned term concrete meaning in the present invention can be understood as the case may be.
In the present invention, 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 aspect of the invention, the present invention proposes a kind of method utilizing lateritic nickel ore to prepare carbonyl nickel powder.According to embodiments of the invention, the method comprises: lateritic nickel ore, sulphur coal and additive are carried out mixed pelletizing by (1), to obtain mixing pelletizing; (2) described mixing pelletizing is carried out reduce-melt divisional processing, to obtain nickel-containing molten iron and tailings; (3) described nickel-containing molten iron is carried out pelletization treatment, to obtain dilval particle; (4) 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; (5) the described gaseous mixture containing carbonyl nickel, carbonyl iron and carbon monoxide is carried out purification processes, to obtain gaseous state carbonyl nickel and the first carbon monoxide; 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, adopt lateritic nickel ore as the raw material preparing carbonyl nickel powder, although the grade of nickel is lower in lateritic nickel ore, but adopt method of the present invention still can prepare highly purified carbonyl nickel powder, thus while widening raw material sources, reduce the production cost of carbonyl nickel powder, simultaneously by adopting sulphur coal as reducing agent, the nickel that not only can effectively reduce in lateritic nickel ore, ferriferous oxide, and sulphur can be made to enter containing activated ni in ferronickel molten iron by molten divisional processing, namely highly active dilval particle is obtained, thus itself and carbon monoxide are directly contacted can react generation carbonyls, and carbonyls synthetic ratio is higher, compared with prior art, the present invention does not need to add catalyst in carbonyls building-up process, thus shorten technological process, secondly by granulating to gained nickel-containing molten iron, the contact area of itself and carbon monoxide can be significantly improved, thus improve carbonyls synthetic ratio further, adopt cheap sulphur coal as reducing agent in addition, not only effectively can reduce production cost, and sulphur wherein can be made to be applied in carbonyls building-up process as beneficiating ingredient, and in carbonyls building-up process, do not produce gaseous state sulfur-bearing thing, atmosphere pollution can not be caused.
The method utilizing lateritic nickel ore to prepare carbonyl nickel powder below with reference to Fig. 1-3 pairs of embodiment of the present invention is described in detail.According to embodiments of the invention, the method comprises:
S100: lateritic nickel ore, sulphur coal and additive are carried out mixed pelletizing
According to embodiments of the invention, lateritic nickel ore, sulphur coal and additive are carried out mixed pelletizing, thus can obtain mixing pelletizing.Inventor finds, adopt lateritic nickel ore as the raw material preparing carbonyl nickel powder, although the grade of nickel is lower in lateritic nickel ore, but adopt method of the present invention still can prepare highly purified carbonyl nickel powder (nickel content is higher than more than 99%), thus while widening raw material sources, reduce the production cost of carbonyl nickel powder, and iron content is up to 85 ~ 99wt% in gained iron powder, simultaneously by adopting sulphur coal as reducing agent, the nickel that not only can effectively reduce in lateritic nickel ore, ferriferous oxide, and highly active dilval particle can be obtained, thus itself and carbon monoxide are directly contacted can react generation carbonyls, and carbonyls synthetic ratio is higher, compared with prior art, the present invention does not need to add catalyst in carbonyls building-up process, thus shorten technological process, high sulfur coal resource rich reserves in addition, but the environmental problems such as serious sulphur pollution and acid rain can be caused due to it and be difficult to be effectively utilized, and the present invention adopts sulphur coal as reducing agent, not only effectively can reduce production cost, and sulphur coal does not need through desulfur technology process, sulphur wherein can be made on the contrary to be applied in carbonyls building-up process as beneficiating ingredient, and in carbonyls building-up process, do not produce gaseous state sulfur-bearing thing, atmosphere pollution can not be caused.
According to one embodiment of present invention, the mixed proportion of lateritic nickel ore, sulphur coal and additive is also not particularly limited, those skilled in the art can select according to actual needs, according to a particular embodiment of the invention, lateritic nickel ore, sulphur coal and additive can be that 100:5 ~ 25:3 ~ 15 mix according to mass ratio.Inventor finds, if the addition of sulphur coal is too low, then affect the reduction effect of metallized pellet on the one hand, on the other hand, the sulfur content of dilval particle can be caused low and affect its carbonylation activity, be unfavorable for that carbongl group synthesis reaction carries out, if and the addition of sulphur coal is too high, final products technical indicator can not be improved, and high sulfur coal resource can be caused to waste, improve production cost, and the consumption of additive is intended to the reduction of nickel in auxiliary lateritic nickel ore, finds that too high or too low consumption all can reduce the reduction effect of nickel in test.Concrete, before lateritic nickel ore, sulphur coal and additive are mixed, in advance lateritic nickel ore, sulphur coal and additive are pulverized.
According to still a further embodiment, nickel content in lateritic nickel ore is also not particularly limited, and those skilled in the art can select according to actual needs, and according to a particular embodiment of the invention, in lateritic nickel ore, nickel content is 0.5 ~ 3.0wt%.Thus, in order to obtain highly purified carbonyl nickel powder in existing synthesis technique, usually the nickel minerals adopting nickeliferous content higher is needed, cause raw material production cost higher, not easily purchase, and in centering nickel minerals of the present invention, nickel grade requirement threshold is lower, adopts nickel content to be only the lateritic nickel ore of 0.5 ~ 3.0wt% as the raw material preparing carbonyl nickel powder, highly purified carbonyl nickel powder can be prepared, thus significantly reduce cost of material while widening nickel raw material sources.
According to still another embodiment of the invention, the sulfur content in sulphur coal is also not particularly limited, and those skilled in the art can select according to actual needs, and according to a particular embodiment of the invention, high-sulfur sulfur content of coal can higher than 3wt%.Inventor finds, adopt the sulphur coal of the type can prepare highly active dilval particle, thus itself and carbon monoxide are directly contacted can react generation carbonyls, and carbonyls synthetic ratio is higher, compared with prior art, the present invention does not need to add catalyst in carbonyls building-up process, thus shortens technological process.
According to still another embodiment of the invention, the particular type of additive is also not particularly limited, those skilled in the art can select according to actual needs, according to a particular embodiment of the invention, additive can for being selected from least one in alkali metal oxide, alkali metal salt, alkaline earth oxide and alkali salt.Inventor finds, in the reduction process of lateritic nickel ore, such additive can displace NiO from forsterite or fayalite, to improve the activity of NiO, thus significantly reduce reducing and smelting temperature, the reducing condition of lateritic nickel ore is greatly improved, promotes that reduction reaction is carried out.
S200: mixing pelletizing is carried out reducing-melt divisional processing
According to embodiments of the invention, mixing pelletizing is carried out reducing-melt divisional processing, thus nickel-containing molten iron and tailings can be obtained.Inventor finds, sulphur can be made to enter activated ni in nickel-containing molten iron by molten divisional processing, namely highly active dilval particle is obtained, thus itself and carbon monoxide are directly contacted can react generation carbonyls, and carbonyls synthetic ratio is higher, compared with prior art, the present invention does not need to add catalyst in carbonyls building-up process, thus shortens technological process.
According to one embodiment of present invention, the combined apparatus of reduction apparatus and molten separating device can be adopted to carry out the reduction of mixing pelletizing-molten divisional processing, according to a particular embodiment of the invention, reduction apparatus can for being selected from least one in rotary hearth furnace, rotary kiln, car-bottom furnace and tunnel cave, molten separating device can divide stove for electric arc furnaces, mineral hot furnace and non-electric smelting, and such as non-electric smelting divides stove can be the molten point stove of natural gas, the molten point stove of coal gas or the molten point stove of fuel oil.Thus, sulphur can be made to enter activated ni in nickel-containing molten iron, namely obtain highly active dilval particle.It should be noted that, those skilled in the art can select the condition of reduction and molten divisional processing according to actual needs.
According to still a further embodiment, nickel content in nickel-containing molten iron is also not particularly limited, and those skilled in the art can select according to actual needs, and according to a particular embodiment of the invention, in nickel-containing molten iron, nickel content can be 5 ~ 45wt%.Inventor finds, in order to obtain highly purified carbonyl nickel powder in existing carbonyl nickel synthesis technique, usually need to adopt nickel content more than the corronil of 50wt% or high-purity nickel oxide, cause raw material production cost higher, not easily purchase, and the present invention is lower to nickel grade requirement threshold in raw material, nickel content is adopted to be only the synthesis material of dilval particle as carbonyl nickel powder of 5 ~ 45wt%, highly purified carbonyl nickel powder can be prepared, thus significantly reduce cost of material while widening nickel raw material sources.
According to still another embodiment of the invention, sulfur content in dilval particle is also not particularly limited, and those skilled in the art can select according to actual needs, and according to a particular embodiment of the invention, in dilval particle, sulfur content can be 2 ~ 5wt%.Inventor finds, in nickel-containing alloys particle, sulfur content is higher, make nickel activity in gained dilval particle 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 present invention does not need additionally to add catalyst, thus shorten preparation technology's flow process, but dilval particle sulfur content is too high, to nickel activity improve not obvious, in addition, excessive sulfur content can improve coal blending amount accordingly, the content of nickel in dilval can be reduced on the one hand, also the waste of feed coal can be caused on the other hand.
S300: nickel-containing molten iron is carried out pelletization treatment
According to embodiments of the invention, above-mentioned gained nickel-containing molten iron is carried out pelletization treatment, thus obtains dilval particle.Inventor finds, by granulating to gained nickel-containing molten iron, thus can significantly improve the contact area with carbon monoxide, and then improves carbonyls synthetic ratio further.
According to still another embodiment of the invention, dilval grain graininess is also not particularly limited, and those skilled in the art can select according to actual needs, and according to a particular embodiment of the invention, the particle diameter of dilval particle is not more than 0.5 millimeter.Inventor finds, the dilval 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.
S400: dilval particle is contacted with carbon monoxide
According to embodiments of the invention, by dilval particle and carbon monoxide counter current contacting, thus iron powder and the gaseous mixture containing carbonyl nickel, carbonyl iron and carbon monoxide can be obtained.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 present invention does not need to add catalyst in carbonyls building-up process, thus shortens technological process.
According to one embodiment of present invention, 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 a particular embodiment of the invention, 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, the synthetic ratio of carbonyl nickel can be significantly improved.
According to still a further embodiment, dilval particle and reaction of carbon monoxide carry out in carbonylation synthesis device, and according to a particular embodiment of the invention, in carbonylation synthesis device, the volume content of carbon monoxide is not less than 90%.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.
S500: the gaseous mixture containing carbonyl nickel, carbonyl iron and carbon monoxide is carried out purification processes
According to embodiments of the invention, the gaseous mixture containing carbonyl nickel, carbonyl iron and carbon monoxide is carried out purification processes, thus gaseous state carbonyl nickel and the first carbon monoxide can be obtained.Thus, the purity of follow-up gained carbonyl nickel powder can be significantly improved.In this step, concrete, first the gaseous mixture containing carbonyl nickel, carbonyl iron and carbon monoxide is carried out condensation process, the carbonyl nickel in gaseous mixture and carbonyl iron condensation is made to become liquid, carbon monoxide wherein then exists in gaseous form, then rectification process is carried out to the liquefied mixture that gained contains carbonyl nickel and carbonyl iron, thus can be separated and obtain highly purified gaseous state carbonyl nickel.It should be noted that, those skilled in the art can select the concrete operations condition of adopted condensation and rectifying according to actual needs.
S600: gaseous state carbonyl nickel is carried out resolution process
According to embodiments of the invention, 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 when heating.
According to one embodiment of present invention, the condition of resolution process is also not particularly limited, those skilled in the art can select according to actual needs, and according to a particular embodiment of the invention, 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 the purity of carbonyl nickel powder.
The method utilizing lateritic nickel ore to prepare carbonyl nickel powder according to the embodiment of the present invention adopts lateritic nickel ore as the raw material preparing carbonyl nickel powder, although the grade of nickel is lower in lateritic nickel ore, but adopt method of the present invention still can prepare highly purified carbonyl nickel powder, thus while widening raw material sources, reduce the production cost of carbonyl nickel powder, simultaneously by adopting sulphur coal as reducing agent, the nickel that not only can effectively reduce in lateritic nickel ore, ferriferous oxide, and sulphur can be made to enter containing activated ni in ferronickel molten iron by molten divisional processing, namely highly active dilval particle is obtained, thus itself and carbon monoxide are directly contacted can react generation carbonyls, and carbonyls synthetic ratio is higher, compared with prior art, the present invention does not need to add catalyst in carbonyls building-up process, thus shorten technological process, secondly by granulating to gained nickel-containing molten iron, the contact area of itself and carbon monoxide can be significantly improved, thus improve carbonyls synthetic ratio further, adopt cheap sulphur coal as reducing agent in addition, not only effectively can reduce production cost, and sulphur wherein can be made to be applied in carbonyls building-up process as beneficiating ingredient, and in carbonyls building-up process, do not produce gaseous state sulfur-bearing thing, atmosphere pollution can not be caused.
With reference to figure 2, the method utilizing lateritic nickel ore to prepare carbonyl nickel powder according to the embodiment of the present invention comprises further:
S700: the first carbon monoxide is returned S400 and dilval particle contacts.
According to embodiments of the invention, purification processes gained first carbon monoxide is back to S400 and dilval particle contacts, thus carbon monoxide cycle utilization rate can be significantly improved.
With reference to figure 3, the method utilizing lateritic nickel ore to prepare carbonyl nickel powder according to the embodiment of the present invention comprises further:
S800: the second carbon monoxide is returned S400 and dilval particle contacts
According to embodiments of the invention, resolution process gained second carbon monoxide is back to S400 and dilval particle contacts, thus improves carbon monoxide cycle utilization rate further.
In another aspect of the present invention, the present invention proposes a kind of system utilizing lateritic nickel ore to prepare carbonyl nickel powder.According to embodiments of the invention, this system comprises: mixed pelletizing device, described mixed pelletizing device has lateritic nickel ore entrance, sulphur coal entrance, additive entrance and the outlet of mixing pelletizing, and is suitable for lateritic nickel ore, sulphur coal and additive to carry out mixed pelletizing, to obtain mixing pelletizing; Reduction-molten separating device, described reduction-molten separating device has mixing pelletizing entrance, nickel-containing molten iron outlet and tailings outlet, described mixing pelletizing entrance is connected with the outlet of described mixing pelletizing, and be suitable for described mixing pelletizing to carry out reducing-melt divisional processing, to obtain nickel-containing molten iron and tailings; Granulation device, described granulation device has nickel-containing molten iron entrance and dilval particle outlet, and described nickel-containing molten iron entrance exports with described nickel-containing molten iron and is connected, and is suitable for described nickel-containing molten iron to carry out pelletization treatment, to obtain dilval particle; Carbonylation synthesis device, described carbonylation synthesis device has carbon monoxide inlet, dilval particle entrance and gaseous state mixture 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; Purifying plant, described purifying plant has gaseous mixture entrance, the outlet of gaseous state carbonyl nickel and the first carbon monoxide and exports described gaseous mixture entrance and to export with described gaseous mixture and be connected, and be suitable for the described gaseous mixture containing carbonyl nickel, carbonyl iron and carbon monoxide to carry out purification processes, to obtain gaseous state carbonyl nickel and the first carbon monoxide; 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, adopt lateritic nickel ore as the raw material preparing carbonyl nickel powder, although the grade of nickel is lower in lateritic nickel ore, but adopt system of the present invention still can prepare highly purified carbonyl nickel powder, thus while widening raw material sources, reduce the production cost of carbonyl nickel powder, simultaneously by adopting sulphur coal as reducing agent, the nickel that not only can effectively reduce in lateritic nickel ore, ferriferous oxide, and sulphur can be made to enter containing activated ni in ferronickel molten iron by molten divisional processing, namely highly active dilval particle is obtained, thus itself and carbon monoxide are directly contacted can react generation carbonyls, and carbonyls synthetic ratio is higher, compared with prior art, the present invention does not need to add catalyst in carbonyls building-up process, thus shorten technological process, secondly by granulating to gained nickel-containing molten iron, the contact area of itself and carbon monoxide can be significantly improved, thus improve carbonyls synthetic ratio further, adopt cheap sulphur coal as reducing agent in addition, not only effectively can reduce production cost, and sulphur wherein can be made to be applied in carbonyls building-up process as beneficiating ingredient, and in carbonyls building-up process, do not produce gaseous state sulfur-bearing thing, atmosphere pollution can not be caused.
The system utilizing lateritic nickel ore to prepare carbonyl nickel powder below with reference to Fig. 4-6 pairs of embodiment of the present invention is described in detail.According to embodiments of the invention, this system comprises:
Mixed pelletizing device 100: according to embodiments of the invention, mixed pelletizing device 100 has lateritic nickel ore entrance 101, sulphur coal entrance 102, additive entrance 103 and mixing pelletizing outlet 104, and be suitable for lateritic nickel ore, sulphur coal and additive to carry out mixed pelletizing, thus can obtain mixing pelletizing.Inventor finds, adopt lateritic nickel ore as the raw material preparing carbonyl nickel powder, although the grade of nickel is lower in lateritic nickel ore, but adopt system of the present invention still can prepare highly purified carbonyl nickel powder (nickel content is higher than more than 99%), thus while widening raw material sources, reduce the production cost of carbonyl nickel powder, and iron content is up to 85 ~ 99wt% in gained iron powder, simultaneously by adopting sulphur coal as reducing agent, the nickel that not only can effectively reduce in lateritic nickel ore, ferriferous oxide, and highly active dilval particle can be obtained, thus itself and carbon monoxide are directly contacted can react generation carbonyls, and carbonyls synthetic ratio is higher, compared with prior art, the present invention does not need to add catalyst in carbonyls building-up process, thus shorten technological process, high sulfur coal resource rich reserves in addition, but the environmental problems such as serious sulphur pollution and acid rain can be caused due to it and be difficult to be effectively utilized, and the present invention adopts sulphur coal as reducing agent, not only effectively can reduce production cost, and sulphur coal does not need through desulfur technology process, sulphur wherein can be made on the contrary to be applied in carbonyls building-up process as beneficiating ingredient, and in carbonyls building-up process, do not produce gaseous state sulfur-bearing thing, atmosphere pollution can not be caused.Concrete, the mixed pelletizing device adopted in the present invention can be the combined apparatus of mixing arrangement and palletizing device.
According to one embodiment of present invention, the mixed proportion of lateritic nickel ore, sulphur coal and additive is also not particularly limited, those skilled in the art can select according to actual needs, according to a particular embodiment of the invention, lateritic nickel ore, sulphur coal and additive can be that 100:5 ~ 25:3 ~ 15 mix according to mass ratio.Inventor finds, if the addition of sulphur coal is too low, then affect the reduction effect of metallized pellet on the one hand, on the other hand, the sulfur content of dilval particle can be caused low and affect its carbonylation activity, be unfavorable for that carbongl group synthesis reaction carries out, if and the addition of sulphur coal is too high, final products technical indicator can not be improved, and high sulfur coal resource can be caused to waste, improve production cost, and the consumption of additive is intended to the reduction of nickel in auxiliary lateritic nickel ore, finds that too high or too low consumption all can reduce the reduction effect of nickel in test.Concrete, before lateritic nickel ore, sulphur coal and additive are mixed, in advance lateritic nickel ore, sulphur coal and additive are pulverized.
According to still a further embodiment, nickel content in lateritic nickel ore is also not particularly limited, and those skilled in the art can select according to actual needs, and according to a particular embodiment of the invention, in lateritic nickel ore, nickel content is 0.5 ~ 3.0wt%.Thus, in order to obtain highly purified carbonyl nickel powder in existing synthesis technique, usually the nickel minerals adopting nickeliferous content higher is needed, cause raw material production cost higher, not easily purchase, and in centering nickel minerals of the present invention, nickel grade requirement threshold is lower, adopts nickel content to be only the lateritic nickel ore of 0.5 ~ 3.0wt% as the raw material preparing carbonyl nickel powder, highly purified carbonyl nickel powder can be prepared, thus significantly reduce cost of material while widening nickel raw material sources.
According to still another embodiment of the invention, the sulfur content in sulphur coal is also not particularly limited, and those skilled in the art can select according to actual needs, and according to a particular embodiment of the invention, high-sulfur sulfur content of coal can higher than 3wt%.Inventor finds, adopt the sulphur coal of the type can prepare highly active dilval particle, thus itself and carbon monoxide are directly contacted can react generation carbonyls, and carbonyls synthetic ratio is higher, compared with prior art, the present invention does not need to add catalyst in carbonyls building-up process, thus shortens technological process.
According to still another embodiment of the invention, the particular type of additive is also not particularly limited, those skilled in the art can select according to actual needs, according to a particular embodiment of the invention, additive can for being selected from least one in alkali metal oxide, alkali metal salt, alkaline earth oxide and alkali salt.Inventor finds, in the reduction process of lateritic nickel ore, such additive can displace NiO from forsterite or fayalite, to improve the activity of NiO, thus significantly reduce reducing and smelting temperature, the reducing condition of lateritic nickel ore is greatly improved, promotes that reduction reaction is carried out.
Reduction-molten separating device 200: according to embodiments of the invention, reduction-molten separating device 200 has mixing pelletizing entrance 201, nickel-containing molten iron outlet 202 and tailings outlet 203, mixing pelletizing entrance 201 is connected with mixing pelletizing outlet 104, and be suitable for mixing pelletizing to carry out reducing-melt divisional processing, thus nickel-containing molten iron and tailings can be obtained.Inventor finds, sulphur can be made to enter activated ni in nickel-containing molten iron by molten divisional processing, namely highly active dilval particle is obtained, thus itself and carbon monoxide are directly contacted can react generation carbonyls, and carbonyls synthetic ratio is higher, compared with prior art, the present invention does not need to add catalyst in carbonyls building-up process, thus shortens technological process.
According to one embodiment of present invention, the combined apparatus of reduction apparatus and molten separating device can be adopted to carry out the reduction of mixing pelletizing-molten divisional processing, according to a particular embodiment of the invention, reduction apparatus can for being selected from least one in rotary hearth furnace, rotary kiln, car-bottom furnace and tunnel cave, molten separating device can divide stove for electric arc furnaces, mineral hot furnace and non-electric smelting, and such as non-electric smelting divides stove can be the molten point stove of natural gas, the molten point stove of coal gas or the molten point stove of fuel oil.Thus, sulphur can be made to enter activated ni in nickel-containing molten iron, namely obtain highly active dilval particle.It should be noted that, those skilled in the art can select the condition of reduction and molten divisional processing according to actual needs.
According to still a further embodiment, nickel content in nickel-containing molten iron is also not particularly limited, and those skilled in the art can select according to actual needs, and according to a particular embodiment of the invention, in nickel-containing molten iron, nickel content can be 5 ~ 45wt%.Inventor finds, in order to obtain highly purified carbonyl nickel powder in existing carbonyl nickel synthesis technique, usually need to adopt nickel content more than the corronil of 50wt% or high-purity nickel oxide, cause raw material production cost higher, not easily purchase, and the present invention is lower to nickel grade requirement threshold in raw material, nickel content is adopted to be only the synthesis material of dilval particle as carbonyl nickel powder of 5 ~ 45wt%, highly purified carbonyl nickel powder can be prepared, thus significantly reduce cost of material while widening nickel raw material sources.
According to still another embodiment of the invention, sulfur content in dilval particle is also not particularly limited, and those skilled in the art can select according to actual needs, and according to a particular embodiment of the invention, in dilval particle, sulfur content can be 2 ~ 5wt%.Inventor finds, in nickel-containing alloys particle, sulfur content is higher, make nickel activity in gained dilval particle 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 present invention does not need additionally to add catalyst, thus shorten preparation technology's flow process, but dilval particle sulfur content is too high, to nickel activity improve not obvious, in addition, excessive sulfur content can improve coal blending amount accordingly, the content of nickel in dilval can be reduced on the one hand, also the waste of feed coal can be caused on the other hand.
Granulation device 300: according to embodiments of the invention, granulation device 300 has nickel-containing molten iron entrance 301 and dilval particle outlet 302, nickel-containing molten iron entrance 301 and nickel-containing molten iron export 202 and are connected, and be suitable for above-mentioned gained nickel-containing molten iron to carry out pelletization treatment, thus obtain dilval particle.Inventor finds, by granulating to gained nickel-containing molten iron, thus can significantly improve the contact area with carbon monoxide, and then improves carbonyls synthetic ratio further.
According to still another embodiment of the invention, dilval grain graininess is also not particularly limited, and those skilled in the art can select according to actual needs, and according to a particular embodiment of the invention, the particle diameter of dilval particle is not more than 0.5 millimeter.Inventor finds, the dilval 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 400: according to embodiments of the invention, carbonylation synthesis device 400 has carbon monoxide inlet 401, dilval particle entrance 402, gaseous mixture outlet 403 and iron powder outlet 404, dilval particle entrance 402 is connected with dilval particle outlet 302, and be suitable for dilval particle and carbon monoxide counter current contacting, thus iron powder and the gaseous mixture containing carbonyl nickel, carbonyl iron and carbon monoxide can be obtained.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 present invention does not need to add catalyst in carbonyls building-up process, thus shortens technological process.
According to one embodiment of present invention, 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 a particular embodiment of the invention, 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, the synthetic ratio of carbonyl nickel can be significantly improved.
According to still a further embodiment, dilval particle and reaction of carbon monoxide carry out in carbonylation synthesis device, and according to a particular embodiment of the invention, in carbonylation synthesis device, the volume content of carbon monoxide is not less than 90%.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.
Purifying plant 500: according to embodiments of the invention, purifying plant 500 has gaseous mixture entrance 501, gaseous state carbonyl nickel outlet 502 and the first carbon monoxide outlet 503, gaseous mixture entrance 501 and gaseous mixture export 403 and are connected, and be suitable for the gaseous mixture containing carbonyl nickel, carbonyl iron and carbon monoxide to carry out purification processes, thus gaseous state carbonyl nickel and the first carbon monoxide can be obtained.Thus, the purity of follow-up gained carbonyl nickel powder can be significantly improved.In this step, concrete, first the gaseous mixture containing carbonyl nickel, carbonyl iron and carbon monoxide is carried out condensation process, the carbonyl nickel in gaseous mixture and carbonyl iron condensation is made to become liquid, carbon monoxide wherein then exists in gaseous form, then rectification process is carried out to the liquefied mixture that gained contains carbonyl nickel and carbonyl iron, thus can be separated and obtain highly purified gaseous state carbonyl nickel.It should be noted that, those skilled in the art can select the concrete operations condition of adopted condensation and rectifying according to actual needs.
Decomposer 600: according to embodiments of the invention, decomposer 600 has gaseous state carbonyl nickel entrance 601, dilval 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 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 when heating.
According to one embodiment of present invention, the condition of resolution process is also not particularly limited, those skilled in the art can select according to actual needs, and according to a particular embodiment of the invention, 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 the purity of carbonyl nickel powder.
The system utilizing lateritic nickel ore to prepare carbonyl nickel powder according to the embodiment of the present invention adopts lateritic nickel ore as the raw material preparing carbonyl nickel powder, although the grade of nickel is lower in lateritic nickel ore, but adopt system of the present invention still can prepare highly purified carbonyl nickel powder, thus while widening raw material sources, reduce the production cost of carbonyl nickel powder, simultaneously by adopting sulphur coal as reducing agent, the nickel that not only can effectively reduce in lateritic nickel ore, ferriferous oxide, and sulphur can be made to enter containing activated ni in ferronickel molten iron by molten divisional processing, namely highly active dilval particle is obtained, thus itself and carbon monoxide are directly contacted can react generation carbonyls, and carbonyls synthetic ratio is higher, compared with prior art, the present invention does not need to add catalyst in carbonyls building-up process, thus shorten technological process, secondly by granulating to gained nickel-containing molten iron, the contact area of itself and carbon monoxide can be significantly improved, thus improve carbonyls synthetic ratio further, adopt cheap sulphur coal as reducing agent in addition, not only effectively can reduce production cost, and sulphur wherein can be made to be applied in carbonyls building-up process as beneficiating ingredient, and in carbonyls building-up process, do not produce gaseous state sulfur-bearing thing, atmosphere pollution can not be caused.
With reference to figure 5, according to one embodiment of present invention, first carbon monoxide outlet 503 is connected with carbon monoxide inlet 401, and be suitable for purifying plant 500 gained first carbon monoxide being back to carbonylation synthesis device 400 and dilval particle contacts, thus carbon monoxide cycle utilization rate can be significantly improved.
With reference to figure 6, according to still a further embodiment, second carbon monoxide outlet 603 is connected with carbon monoxide inlet 401, and be suitable for decomposer 600 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.
Below with reference to specific embodiment, present invention is described, it should be noted that, these embodiments are only descriptive, and do not limit the present invention in any way.
Embodiment 1
Get the lateritic nickel ore of composition shown in table 1, allocate the sulphur coal that sulfur content is 3.5% into, ball processed after lime stone mixing is also dried, wherein, lateritic nickel ore, the mixing quality ratio of sulphur coal and lime stone is 100:15:10, dried mixing pelletizing is distributed into rotary hearth furnace and reduces, reducing condition 1300 DEG C, time 35min, the direct heat of metallized pellet after reduction delivers to the molten point stove of combustion gas, molten point temperature is 1550 DEG C, obtain nickel-containing molten iron (composition is as shown in table 2), then gained nickel-containing molten iron is made in pellet fabrication device the dilval particle that average grain diameter is 0.25mm, and carry out stored dry as carbonyl material, then in carbonyl reaction device, 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%, will containing carbonyl nickel, the gaseous mixture of carbonyl iron and carbon monoxide is delivered in condenser and carries out condensation process, wherein carbonyl nickel and carbonyl iron are condensed into liquid state, and carbon monoxide exists in a gaseous form, and separating obtained carbon monoxide is returned continuation use in carbonyl reaction device, and liquefied mixture gained being contained carbonyl nickel and carbonyl iron is sent into rectifying column again and is carried 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 carbon monoxide and nickel content is the carbonyl nickel powder of 99.82wt%, wherein in carbonyl nickel powder, major impurity is C and Fe, and decomposition gained carbon monoxide is returned continuation use in carbonyl reaction device.
Embodiment 2
Get the lateritic nickel ore of composition shown in table 1, allocate the sulphur coal that sulfur content is 4.5% into, ball processed after sodium carbonate mixing is also dried, wherein, lateritic nickel ore, the mixing quality ratio of sulphur coal and sodium carbonate is 100:10:15, dried mixing pelletizing is distributed into rotary kiln and reduces, reducing condition 900 DEG C, time 65min, the direct heat of metallized pellet after reduction delivers to molten point of electric furnace, molten point temperature is 1550 DEG C, obtain nickel-containing molten iron (composition is as shown in table 2), then gained nickel-containing molten iron is made in pellet fabrication device the dilval particle that average grain diameter is 0.15mm, and carry out stored dry as carbonyl material, then in carbonyl reaction device, 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%, will containing carbonyl nickel, the gaseous mixture of carbonyl iron and carbon monoxide is delivered in condenser and carries out condensation process, wherein carbonyl nickel and carbonyl iron are condensed into liquid state, and carbon monoxide exists in a gaseous form, and separating obtained carbon monoxide is returned continuation use in carbonyl reaction device, and liquefied mixture gained being contained carbonyl nickel and carbonyl iron is sent into rectifying column again and is carried 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 carbon monoxide and nickel content is the carbonyl nickel powder of 99.54wt%, wherein in carbonyl nickel powder, major impurity is C and Fe, and decomposition gained carbon monoxide is returned continuation use in carbonyl reaction device.
Embodiment 3
Get the lateritic nickel ore of composition shown in table 1, allocate the sulphur coal that sulfur content is 6% into, ball processed after sodium carbonate mixing is also dried, wherein, lateritic nickel ore, the mixing quality ratio of sulphur coal and sodium carbonate is 100:20:5, dried mixing pelletizing is distributed into tunnel cave and reduces, reducing condition 1220 DEG C, time 40min, the direct heat of metallized pellet after reduction delivers to the molten point stove of combustion gas, molten point temperature is 1550 DEG C, obtain nickel-containing molten iron (composition is as shown in table 2), then gained nickel-containing molten iron is made in pellet fabrication device the dilval particle that average grain diameter is 0.05mm, and carry out stored dry as carbonyl material, then in carbonyl reaction device, 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 90.0%, will containing carbonyl nickel, the gaseous mixture of carbonyl iron and carbon monoxide is delivered in condenser and carries out condensation process, wherein carbonyl nickel and carbonyl iron are condensed into liquid state, and carbon monoxide exists in a gaseous form, and separating obtained carbon monoxide is returned continuation use in carbonyl reaction device, and liquefied mixture gained being contained carbonyl nickel and carbonyl iron is sent into rectifying column again and is carried 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 carbon monoxide and nickel content is the carbonyl nickel powder of 99.82wt%, wherein in carbonyl nickel powder, major impurity is C and Fe, and decomposition gained carbon monoxide is returned continuation use in carbonyl reaction device.
Table 1 embodiment 1 ~ 3 lateritic nickel ore main component, wt.%
| Embodiment | TFe | FeO | CaO | MgO | SiO 2 | Al 2O 3 | MnO | Cr 2O 3 | Ni | Co |
| 1 | 16.71 | 0.37 | 0.87 | 20.17 | 36.28 | 3.73 | 1.15 | 1.11 | 1.87 | 0.054 |
| 2 | 19.34 | 0.34 | 3.80 | 9.66 | 35.19 | 6.09 | 0.55 | 1.51 | 1.78 | 0.063 |
| 3 | 13.33 | 0.76 | 0.12 | 25.31 | 38.26 | 2.30 | 0.35 | 1.12 | 1.85 | 0.055 |
Table 2 embodiment 1 ~ 3 nickel-containing molten iron composition main component, wt.%
| Embodiment | TFe | Ni | Co | S | Si | Cr | Mn | P | C |
| 1 | 75.99 | 22.57 | 0.93 | 2.53 | 0.01 | 0.06 | 0.01 | 0.051 | 0.05 |
| 2 | 78.19 | 20.28 | 0.63 | 3.28 | 0.35 | 0.08 | 0.01 | 0.046 | 0.11 |
| 3 | 73.15 | 24.19 | 0.60 | 4.37 | 0.19 | 0.09 | 0.04 | 0.039 | 0.09 |
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 invention 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 describe embodiments of the invention above, be understandable that, above-described embodiment is exemplary, can not be interpreted as limitation of the present invention, and those of ordinary skill in the art can change above-described embodiment within the scope of the invention, revises, replace and modification.
Claims (8)
1. utilize lateritic nickel ore to prepare a method for carbonyl nickel powder, it is characterized in that, comprising:
(1) lateritic nickel ore, sulphur coal and additive are carried out mixed pelletizing, to obtain mixing pelletizing;
(2) described mixing pelletizing is carried out reduce-melt divisional processing, to obtain nickel-containing molten iron and tailings;
(3) described nickel-containing molten iron is carried out pelletization treatment, to obtain dilval particle;
(4) 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;
(5) the described gaseous mixture containing carbonyl nickel, carbonyl iron and carbon monoxide is carried out purification processes, to obtain gaseous state carbonyl nickel and the first carbon monoxide; And
(6) described gaseous state carbonyl nickel is carried out resolution process, to obtain carbonyl nickel powder and the second carbon monoxide respectively.
2. method according to claim 1, is characterized in that, comprises further:
(7) described first carbon monoxide is returned step (4) and described dilval particle contacts.
3. method according to claim 1, is characterized in that, comprises further:
(8) described second carbon monoxide is back to step (4) and described dilval particle contacts.
4. method according to claim 1, is characterized in that, in step (1), described high-sulfur sulfur content of coal is higher than 3wt%.
5. method according to claim 1, is characterized in that, in step (1), described additive is be selected from least one in alkali metal oxide, alkali metal salt, alkaline earth oxide and alkali salt.
6. utilize lateritic nickel ore to prepare a system for carbonyl nickel powder, it is characterized in that, comprising:
Mixed pelletizing device, described mixed pelletizing device has lateritic nickel ore entrance, sulphur coal entrance, additive entrance and the outlet of mixing pelletizing, and is suitable for lateritic nickel ore, sulphur coal and additive to carry out mixed pelletizing, to obtain mixing pelletizing;
Reduction-molten separating device, described reduction-molten separating device has mixing pelletizing entrance, nickel-containing molten iron outlet and tailings outlet, described mixing pelletizing entrance is connected with the outlet of described mixing pelletizing, and be suitable for described mixing pelletizing to carry out reducing-melt divisional processing, to obtain nickel-containing molten iron and tailings;
Granulation device, described granulation device has nickel-containing molten iron entrance and dilval particle outlet, and described nickel-containing molten iron entrance exports with described nickel-containing molten iron and is connected, and is suitable for described nickel-containing molten iron to carry out 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;
Purifying plant, described purifying plant has gaseous mixture entrance, the outlet of gaseous state carbonyl nickel and the first carbon monoxide and exports described gaseous mixture entrance and to export with described gaseous mixture and be connected, and be suitable for the described gaseous mixture containing carbonyl nickel, carbonyl iron and carbon monoxide to carry out purification processes, to obtain gaseous state carbonyl nickel and the first carbon monoxide; 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.
7. system according to claim 6, is characterized in that, described first carbon monoxide outlet is connected with described carbon monoxide inlet, and is suitable for described first carbon monoxide to return described carbonylation synthesis device and described dilval particle contacts.
8. system according to claim 6, is characterized in that, described second carbon monoxide outlet is connected with described carbon monoxide inlet, and is suitable for described second carbon monoxide to return described carbonylation synthesis device and described dilval particle contacts.
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| CN106119573A (en) * | 2016-08-09 | 2016-11-16 | 江苏省冶金设计院有限公司 | A kind of method and system utilizing lateritic nickel ore to extract nickel oxide |
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| CN105907967A (en) * | 2016-06-13 | 2016-08-31 | 江苏省冶金设计院有限公司 | System and method for extracting ferronickel alloy from limonite type lateritic nickel ore |
| CN106086467A (en) * | 2016-08-09 | 2016-11-09 | 江苏省冶金设计院有限公司 | A kind of method and system utilizing lateritic nickel ore to extract nickel oxide |
| CN106119573A (en) * | 2016-08-09 | 2016-11-16 | 江苏省冶金设计院有限公司 | A kind of method and system utilizing lateritic nickel ore to extract nickel oxide |
| CN107190148A (en) * | 2017-06-30 | 2017-09-22 | 中国恩菲工程技术有限公司 | Handle the method and its system of metal alloy |
| CN107190148B (en) * | 2017-06-30 | 2019-03-12 | 中国恩菲工程技术有限公司 | Handle the method and its system of metal alloy |
| CN108163902A (en) * | 2017-12-14 | 2018-06-15 | 金川集团股份有限公司 | A kind of method of lateritic nickel ore intermediate product nickel hydroxide production carbonyl nickel raw material |
| CN108996553A (en) * | 2018-08-06 | 2018-12-14 | 金川集团股份有限公司 | A kind of deep processing treatment system and processing method of the thick ferronickel of laterite pyrometallurgical smelting product |
| CN108996556A (en) * | 2018-08-06 | 2018-12-14 | 金川集团股份有限公司 | A kind of raw material of synthesizing carbonyl nickel |
| CN113735199A (en) * | 2021-08-25 | 2021-12-03 | 广东邦普循环科技有限公司 | Method for preparing nickel sulfate from nickel iron |
| CN113735199B (en) * | 2021-08-25 | 2022-11-15 | 广东邦普循环科技有限公司 | Method for preparing nickel sulfate from nickel iron |
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