CN1234491C - Method for preparing high performance nickel powder using shearing and breaking process - Google Patents
Method for preparing high performance nickel powder using shearing and breaking process Download PDFInfo
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- CN1234491C CN1234491C CN 200410046726 CN200410046726A CN1234491C CN 1234491 C CN1234491 C CN 1234491C CN 200410046726 CN200410046726 CN 200410046726 CN 200410046726 A CN200410046726 A CN 200410046726A CN 1234491 C CN1234491 C CN 1234491C
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Abstract
The present invention relates to a method for preparing high-performance nickel powder using a shearing and breaking process. After foam metal nickel raw materials are dynamically rotated and oxidized, oxidation products with a brittle nickel oxide surface layer coating metal nickel are obtained. The oxidation products are sheared and crushed by adopting a multi-level shearing breaker; the breaking level adopts from 1 to 5 levels; then, the crushed powder is re-oxidized to obtain nickel oxide powder with tiny granules. The nickel oxide powder is reduced by decomposeing aminoacylation in grading to produce high-quality metal nickel powder with high purity, tiny granules and small loosening ratio. The process can be widely used in all the processes adopting an oxidation reduction method to prepare the metal nickel powder. The present invention has the advantages that the intermediate oxidation products are sheared and crushed, re-oxidized and then treated with the reduction process in grading to prepare the high-quality metal nickel powder with the tiny granules. The produced metal nickel powder can be widely used in powder metallurgy products (hard alloys, diamond tools, ferronickel alloy products, nickel base products, etc.), stainless steel products, batteries, chemical products, etc. The method of the present invention without any pollution drainage, is favorable for environment protection, shortens process procedure, and lowers production cost.
Description
Technical field:
The present invention relates to a kind of method for preparing nickel powder, especially a kind of refinement technology of low-cost and pollution-less prepares the method for nickel powder.
Background technology:
Metal nickel powder is widely used in sintered metal product (carbide alloy, diamond tool, dilval goods, Ni-based product etc.), stainless steel products, battery and chemical industry series products etc.At present, the production method that is used to prepare metal nickel powder mainly contains oxidation-reduction method, electrolysis, atomization and carbonyl process etc.Wherein, the nickel powder pattern of electrolysis preparation is dendroid, and there is bigger internal stress in powder particle itself, and powder compaction is relatively poor; The nickel powder oxygen content of atomization preparation is higher; The nickel powder powder particle of carbonyl process preparation is tiny, but produces poisonous inorganic matter in the preparation process, causes serious environmental to pollute.The common powder combination property of nickel powder of oxidation-reduction method preparation is better, and oxygen content in power is lower, and in preparation process non-environmental-pollution.Along with the increasingly extensive commercial Application of nickel powder, each industry is increasing to the demand of fine grained or ultra-fine grain nickel powder, and the common powder particle of nickel powder of traditional oxidation-reduction method preparation is thicker, and particle is thicker, and difficulty satisfies this vast market demand.
Summary of the invention:
The object of the invention is to provide a kind of method that adopts shearing-crushing method refinement nickel powder particle, to overcome the thicker deficiency of nickel powder powder particle of traditional oxidation-reduction method preparation.This method can be prepared fine grained and even ultra-fine grain nickel powder, and no any environmental pollution in whole process flow, and is simple for process, with low cost.
Technical solution of the present invention is to adopt shearing-crushing technology to prepare the method for high-performance nickel powder, is a kind of method of significantly refinement nickel powder particle.Adopt the oxidation technology of the foam metal nickel raw material of purifying one loose metallization processes preparation, and shearing-crushing technology subsequently, secondary oxidation technology and reducing process, the tiny high-performance metal nickel powder of preparation particle.Its technological process is: foam metal nickel raw material → oxidation → shearing-crushing → secondary oxidation → nickel oxide powder → stage reduction → metal nickel powder.At first the foam metal nickel raw material is carried out dynamic continuous oxidation and handle, device therefor is the dynamic rotation oxidation furnace, and oxidizing temperature is 850～1000 ℃, and oxidization time is 10～30min, and the oxidation furnace rotative speed is 20～80rpm.After the first oxidation, adopt multistage shear breaker that oxidation product is carried out fragmentation.Shearing-crushing blade material therefor is that strain-induced martensite is strengthened steel Mn13 in the shear breaker.The broken time is 20～40min, and crushing steps is 1～5 grade.Subsequently, the product behind the shearing-crushing is carried out secondary oxidation, device therefor is the dynamic rotation oxidation furnace, and oxidizing temperature is 850～900 ℃, and oxidization time is 10～20min, and the oxidation furnace rotative speed is 30～80rpm.Nickel oxide powder after adopting horizontal continuous reduction furnace to this secondary oxidation carries out three stage reduction to be handled, and three stage reduction temperatures are respectively 400～500 ℃, and 450～600 ℃, 500～650 ℃, each recovery time in stage is 15～30min.The principle that the technical program adopted is: traditional once oxidation reducing process is generally: foam metal nickel raw material → once oxidation → impact grinding → reduction → metal nickel powder.At the initial stage that the foam metal nickel raw material is carried out oxidation, generate the fine and close protective layer of one deck nickel oxide on the metallic nickel surface, oxygen element is played stronger inhibition to the further diffusion of nickel core portion, so often cause the oxidation of foam metal nickel raw material not saturating.In impact grinding process subsequently, on the one hand, the existence of center toughness metallic nickel makes that the shattering process of this form is difficult to well carry out; On the other hand, the unsalted surface of the metallic nickel that broken back forms has very high activity, very easily causes the reunion of powder particle.Reduction process subsequently can not be eliminated this agglomeration basically, causes the thick of metal nickel powder particle in the reduction process like this.The technical program is the improvement of traditional handicraft: adopt shearing-crushing to replace impact grinding, the oxidation foam metal nickel is carried out abundant fragmentation, secondary oxidation is carried out to oxidation product in broken back.Compare with the impulsive force of impact grinding, shearing force can the first oxidation product of more efficiently fragmentation, causes the unsalted surface of more metallic nickel, in secondary oxidation process subsequently, these unsalted surfaces are easy to oxidized, thereby play good elimination powder particle aggregation phenomenon.After through interim reduction, obtain the tiny metal nickel powder of particle.
Compare with existing method, the present invention has the following advantages:
1. adopt the shearing-crushing legal system to be equipped with nickel powder, the crushing efficiency height, prepared nickel powder particle is tiny, has polymolecularity.Foam metal nickel is after first oxidation, because oxidation is not saturating, forming heart portion is ductile metal nickel, and the surface is the structure of the fine and close protective layer of one deck nickel oxide.Traditional impact grinding technology is difficult to this oxidation product is carried out good fragmentation, adopts shearing-crushing to replace impact grinding, compares with impulsive force, and shearing force can more efficiently broken oxidation product, obtains more fine grained nickel oxide powder.Final through the metal nickel powder that particle is tiny, have polymolecularity that is easy to get behind the reducing process.
2. combining of shearing-crushing technology and subsequently secondary oxidation technology provides a kind of low cost, high efficiency to prepare the process of high-performance fine grained nickel powder.Shearing-crushing technology can the first oxidation product of more efficiently fragmentation, causes the unsalted surface of more metallic nickel, and in secondary oxidation process subsequently, these unsalted surfaces are easy to oxidized, thereby play good elimination powder particle aggregation phenomenon.After through interim reduction, obtain high-performance fine grained nickel powder.
3. adopt the shearing-crushing legal system to be equipped with nickel powder, simple for process, with low cost, can realize producing in enormous quantities, and not need to add any additives in the preparation process, no discharge any pollutant helps environmental protection.
Description of drawings
Fig. 1 is a shear breaker shearing blade organigram of the present invention.
Fig. 2 is three grades of shearing-crushing structural representations of shear breaker of the present invention.
Fig. 3 is a process chart of the present invention.
Among the figure, 1. shearing blade, 2. impeller clearance, 3. vane machine wall gap, 4. shear breaker main shaft, 5. charging aperture,
6. elementary shearing blade, 7. secondary shear blade, 8. three grades of shearing blades, 9. discharging openings.
The specific embodiment
The present invention further specifies as follows referring to accompanying drawing in conjunction with specific embodiments:
Referring to Fig. 1,2, oxidation product is entered in the multistage shear breaker by charging aperture 5, is sheared under the high speed rotation by shear breaker main shaft 4 drive shearing blades 1 and is broken into powder.Oxidation product at first carries out primary breakup by elementary shearing blade 6, and the powder after the fragmentation flows to secondary shear blade 7 by impeller clearance 2 and vane machine wall gap 3, and by further broken.Can be generally 1～5 grade according to the progression of the multistage shear breaker of actual process condition setting.In the present embodiment, oxidation product is flowed out by discharging opening 9 in the broken back through three grades of shearing blades 8, thereby obtains the nickel oxide powder of fine grained and even ultra-fine grain.
Embodiment 1
Adopt the dynamic rotation oxidation furnace that the foam metal nickel raw material is carried out continuous oxidation processes, oxidizing temperature is 860 ℃, and oxidization time is 15min, and the oxidation furnace rotative speed is 25rpm.After the first oxidation, adopt multistage shear breaker that oxidation product is carried out fragmentation, strengthen steel Mn13 as shearing-crushing blade material in the shear breaker with strain-induced martensite.The broken time is 20min, and crushing steps is 2 grades.Subsequently, the product behind the shearing-crushing is carried out secondary oxidation, device therefor is the dynamic rotation oxidation furnace, and oxidizing temperature is 860 ℃, and oxidization time is 10min, and the oxidation furnace rotative speed is 35rpm.Nickel oxide powder after adopting horizontal continuous reduction furnace to this secondary oxidation carries out three stage reduction to be handled, and three stage reduction temperatures are respectively 420 ℃, and 470 ℃, 530 ℃, each recovery time in stage is 15min.Finally obtain the metal nickel powder of 2 kinds of different grain size scopes: purity is 99.3%, and particle diameter is-325 orders, and pine is than being 1.7g/cm
3Metal nickel powder (accounting for 96%); And purity is 98.9%, and particle diameter is-200～+ 325 orders, and pine is than being 1.8g/cm
3Metal nickel powder (accounting for 4%).
Adopt the dynamic rotation oxidation furnace that the foam metal nickel raw material is carried out continuous oxidation processes, oxidizing temperature is 900 ℃, and oxidization time is 20min, and the oxidation furnace rotative speed is 45rpm.After the first oxidation, adopt multistage shear breaker that oxidation product is carried out fragmentation, shearing-crushing blade material therefor is that strain-induced martensite is strengthened steel Mn13 in the shear breaker.The broken time is 30min, and crushing steps is 3 grades.Subsequently, the product behind the shearing-crushing is carried out secondary oxidation, device therefor is the dynamic rotation oxidation furnace, and oxidizing temperature is 870 ℃, and oxidization time is 15min, and the oxidation furnace rotative speed is 55rpm.Nickel oxide powder after adopting horizontal continuous reduction furnace to this secondary oxidation carries out three stage reduction to be handled, and three stage reduction temperatures are respectively 460 ℃, and 560 ℃, 600 ℃, each recovery time in stage is 25min.Finally obtaining purity is 99.1%, and particle diameter is-325 orders, and pine is than being 1.7g/cm
3Metal nickel powder.
Adopt the dynamic rotation oxidation furnace that the foam metal nickel raw material is carried out continuous oxidation processes, oxidizing temperature is 950 ℃, and oxidization time is 30min, and the oxidation furnace rotative speed is 65rpm.After the first oxidation, adopt multistage shear breaker that oxidation product is carried out fragmentation, shearing-crushing blade material therefor is that strain-induced martensite is strengthened steel Mn13 in the shear breaker.The broken time is 40min, and crushing steps is 4 grades.Subsequently, the product behind the shearing-crushing is carried out secondary oxidation, device therefor is the dynamic rotation oxidation furnace, and oxidizing temperature is 880 ℃, and oxidization time is 20min, and the oxidation furnace rotative speed is 70rpm.Nickel oxide powder after adopting horizontal continuous reduction furnace to this secondary oxidation carries out three stage reduction to be handled, and three stage reduction temperatures are respectively 480 ℃, and 590 ℃, 630 ℃, each recovery time in stage is 25min.Finally obtaining purity is 99.5%, and particle diameter is-325 orders, and pine is than being 1.6g/cm
3Metal nickel powder.
Claims (2)
1. adopt shearing-crushing technology to prepare the method for nickel powder, its method is: adopt the foam metal nickel raw material, after oxidation, break process, obtain the oxide of fragility nickel oxide surfaces layer coated metal nickel; Obtain metal nickel powder through the reduction treatment process again, it is characterized in that: the foam metal nickel crushing process is to adopt multistage shear breaker that this oxidation product is carried out repeatedly shearing-crushing, broken technological parameter is: the broken time is 20～40min, and crushing steps is 2～5 grades; Subsequently the powder after this fragmentation is carried out oxidation processes, obtain nickel oxide powder, the nickel oxide powder after adopting cracked ammonium to fragmentation then reduces processing stage by stage, obtains metal nickel powder.
2. employing shearing-crushing technology according to claim 1 prepares the method for nickel powder, it is characterized in that: it is to adopt the dynamic rotation oxidation furnace that foam metal nickel is carried out dynamic continuous oxidation to handle that the oxidation processing of foam metal nickel is handled: oxidizing temperature is 850～1000 ℃, oxidization time is 10～30min, the oxidation furnace rotative speed is 20～80rpm, with the raw material of this oxidation product as shearing-crushing technology.
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| CN 200410046726 CN1234491C (en) | 2004-09-06 | 2004-09-06 | Method for preparing high performance nickel powder using shearing and breaking process |
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| CN 200410046726 CN1234491C (en) | 2004-09-06 | 2004-09-06 | Method for preparing high performance nickel powder using shearing and breaking process |
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| CN1603035A CN1603035A (en) | 2005-04-06 |
| CN1234491C true CN1234491C (en) | 2006-01-04 |
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