CN103691931A - Antioxidant method for grading treatment of metal nickel powder by water - Google Patents
Antioxidant method for grading treatment of metal nickel powder by water Download PDFInfo
- Publication number
- CN103691931A CN103691931A CN201310690780.2A CN201310690780A CN103691931A CN 103691931 A CN103691931 A CN 103691931A CN 201310690780 A CN201310690780 A CN 201310690780A CN 103691931 A CN103691931 A CN 103691931A
- Authority
- CN
- China
- Prior art keywords
- nickel powder
- antioxidant
- metal nickel
- slip
- classification
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Abstract
The invention discloses an antioxidant method for grading treatment of metal nickel powder by water. The method comprises the following steps of adding an antioxidant TX-02 into deionized water, stirring until the antioxidant is completely dissolved to prepare corrosion inhibition solution in which the antioxidant TX-02 accounts for 0.1 to 2 mass percent, and controlling that the pH of the corrosion inhibition solution ranges from 7 to 8, wherein the antioxidant TX-02 is prepared by uniformly mixing carbohydrazide and citric acid in a weight ratio of 1-3:1; adding metal nickel powder which is not graded into emulsifying equipment containing the corrosion inhibition solution with the mass concentration of 0.1-2 percent prepared in the step (1) to prepare nickel powder slurry of which the solid content is 10 to 25 percent; starting the emulsifying equipment, emulsifying the nickel powder slurry for 20 to 50 minutes and dispersing metal nickel powder into slurry with uniformly distributed particles; filtering the emulsified nickel powder slurry, and grading in a grading system. The method has the advantage that metal powder is difficulty corroded and oxidized in the water grading process.
Description
Technical field:
The present invention is a kind of metal powder moisture level anti-oxidation tech field, is specifically related to the anti-oxidation method that a kind of moisture level is processed metal nickel powder.
Background technology:
The submicron order metal nickel powder that PVD method is produced, diameter of particle size is inhomogeneous, can not directly be used in MLCC industry, need to process through classification, obtains the powder that particle diameter is evenly distributed.In known submicron order metal nickel powder grading technology, in liquid phase stage division, mainly with alcohols, be medium, conventional solvent medium has the alcohols such as ethanol, propyl alcohol.Such as relative other organic solvents of ethanol, light specific gravity, viscosity is also little, and classification was imitated good, and raw material is easy to get.Classification processing procedure powder surface is long-pending, oxygen content variation is little, stable performance.But ethanol belongs to volatile product, classification process, ethanol, under the high speed machine motion of centrifugal pump impeller, produces a large amount of heat, and the mutual collision of metal nickel powder particle also produces a large amount of heat energy, and ethanol temperature is raise, and has accelerated ethanol evaporation.Because ethanol is expensive, a large amount of ethanol of classification process consumption, increases nickel powder classification cost.By statistics, in nickel powder classification production process, ethanol consumption accounts for the more than 50% of classification cost.
Ethanol is again inflammable thing simultaneously, and classification process, under the mechanical movement of water pump, produce a large amount of heat energy ethanol temperature is raise, ethanol evaporates in a large number, and in working environment, ethanol vapor concentration is too high, easy combustion explosion while approaching the limit, there is great potential safety hazard as nickel powder classification medium in ethanol.
Adopt water instead of ethanol as nickel powder classification medium, be not only economical and but also one of the production method of safety, but what in moisture level method, adopt is industrial deionized water, in classification process, metal-powder soaks for a long time in water, with the dissolved oxygen generation oxidation reaction in water, causes the metal nickel powder oxidized corrosion in surface, form small scraggly surface, metal nickel powder surface area is increased.While detecting specific area calculating nickel powder particle diameter by BET method, poor larger with actual particle size sheet.Nickel powder surface is rough and uneven in surface, and between particle, frictional force is large, causes nickel powder to increase in pulping process viscosity, affects slurrying and produces.Metal-powder soaks in water, and nickel powder is oxidized, and oxygen content increases.Nickel powder also can occur and manufacturing capacitor sintering process generation cracking phenomena, therefore, the problem that solves metal-powder burn into oxidation in liquid phase water stage division is crucial.
Summary of the invention:
The present invention is directed to the above-mentioned deficiency of prior art, the moisture level that provides metal-powder in a kind of water classification process to be difficult for being corroded, being oxidized is processed the anti-oxidation method of metal nickel powder.
In order to solve the problems of the technologies described above, the technical solution used in the present invention is: a kind of moisture level is processed the anti-oxidation method of metal nickel powder, and step comprises:
(1) in deionized water, add antioxidant TX-02, be stirred to antioxidant and dissolve completely, be mixed with the corrosion inhibiting solution that antioxidant TX-02 mass concentration is 0.1-2%, control this corrosion inhibiting solution pH within the scope of 7-8; Above-mentioned antioxidant TX-02 is obtained for (1-3:1) mixes according to weight ratio by carbohydrazide and citric acid;
(2) unassorted metal nickel powder is added in the emulsifying device that fills the corrosion inhibiting solution that mass concentration prepared by step (1) is 0.1-2%, being mixed with solid content is the nickel powder slip of 10-25%;
(3) start emulsifying device, the nickel powder slip 20-50min of emulsifying step (2), the slip that metal nickel powder emulsion dispersion becomes particle to be evenly distributed;
(4) after emulsification, nickel powder slip after filtering, is sent into hierarchy system classification.
The described unassorted metal nickel powder of step of the present invention (2) is the standby submicron particle of PVD legal system.
As preferably, the described corrosion inhibiting solution of step of the present invention (1) is the corrosion inhibiting solution that antioxidant TX-02 mass concentration is 0.2%.
As preferably, the solid content that is mixed with nickel powder slip described in step of the present invention (2) is 20%.
As preferably, the described emulsification nickel powder slip emulsification times of step of the present invention (3) is 30min.
Classification metal nickel powder of the present invention adopts liquid phase wet classification, is specially described hierarchy system by surge tank, centrifugal pump, cyclone hydraulic separators, and receiving vat forms; Classification process is: by step (4) emulsification, sieve after solid content be 10-25% nickel powder slip is delivered to surge tank, by centrifugal pump under 1.0-1.5MPa pressure, squeeze into and in cyclone hydraulic separators, carry out centrifugal classification, remove super large particle, from the overfall of cyclone hydraulic separators, obtain the powder that particle diameter is evenly distributed, the temperature of institute of the present invention classification processing procedure is carried out at normal temperature condition.Above-mentioned hierarchy system classification process is the conventional classification processing procedure of industry.
Advantage of the present invention and beneficial effect:
1. superfine metal nickel powder of the present invention, in moisture level processing procedure, adds composite antioxidant TX-02(carbohydrazide, the citric acid of preparation in classification deionized water used), be mixed with certain proportion corrosion inhibiting solution.This composite antioxidant TX-02 has strong reducing property, with the dissolved oxygen generation redox reaction in the aqueous solution, consumes the oxygen in water, and reaction generates nitrogen and carbon dioxide is discharged, and reduces the dissolved oxygen content in solution; Corrosion inhibiting solution can form passivating film on metal nickel powder surface on the other hand, the oxidation of the dissolved oxygen in isolated solution to metal nickel powder, thus reach the effect that slows down the oxidation of metal nickel powder and play protection metal nickel powder surface.Therefore, method of the present invention has solved industrial deionized water classification nickel powder and has been corroded, and surface is rough and uneven in surface, and it is large that surface area becomes, and between particle, frictional force is large, and pulping process viscosity increases problem; Also solved nickel powder classification process oxidized, oxygen content increases, and nickel powder occurs in the phenomenon of manufacturing capacitor sintering process generation cracking.
2. antioxidant TX-02 raw material of the present invention is easy to get, and safety non-toxic, stage solution is antioxidant TX-02(carbohydrazide, citric acid) corrosion inhibiting solution that is mixed with, adopt deionized water preparation, raw material is easy to get, price is low, and production process is safe, pollution-free; Composite antioxidant TX-02(carbohydrazide used, citric acid) be organic compound, metal ion not, classification processing procedure, can not generate metal salt compound, does not therefore consume metal nickel powder; Composite antioxidant TX-02(carbohydrazide used, citric acid) react with oxygen in water, consume oxygen in water, classification processing procedure, does not produce insoluble precipitate, has deaerating effect good, metallic nickel powder good in oxidation resistance, oxygen content changes little, and metallic nickel powder corrosion resistance is good, and nickel powder surface is round and smooth, surface area changes little, avoids nickel powder in the advantage of manufacturing capacitor sintering process generation cracking phenomena.
3. the present invention carries out nickel powder slurry to carry out classification after emulsification treatment again, and nickel powder is fully uniformly dispersed in slurry, does not reunite, does not unite, and therefore more easily separated in follow-up classification process, grading effect is good; And in the corrosion inhibiting solution that is mixed with at antioxidant TX-02 of abundant scattered nickel powder, make each disperse nickel powder particle all can fully contact with antioxidant TX-02, therefore, antioxidant effect is better.After emulsification, nickel powder slip after filtration, to remove the nickel powder of larger particles, makes follow-up classification process more smooth.
The specific embodiment:
Below in conjunction with example, the present invention is further described.
Embodiment
(1) preparation of corrosion inhibiting solution: adding weight ratio in deionized water is the carbohydrazide of 3:1, the antioxidant TX-02 that citric acid mixture forms, being stirred to antioxidant TX-02 dissolves completely, be mixed with the corrosion inhibiting solution that antioxidant TX-02 mass concentration is 0.2%, control this corrosion inhibiting solution pH within the scope of 7-8;
(2) in the emulsifying device of the corrosion inhibiting solution that the mass concentration of utilizing conveyer to add step (1) to prepare unassorted metal nickel powder is 0.2%, the volume of emulsifying device is 250L, is mixed with solid content and is 25% nickel powder slip;
(3) start emulsifying device, emulsifying device power is 15kw, and rotating speed is 2900rpm, emulsification nickel powder slip 30min, the slip that metal nickel powder emulsion dispersion becomes particle to be evenly distributed;
(4) after emulsification, nickel powder slip filters through 600 order vibratory sieves, removes in former slip and is greater than 30 microns of above agglomerates, foreign matter etc., stops up cyclone hydraulic separators while avoiding classification;
(5) hierarchy system is by surge tank (600L), centrifugal pump (15KW), cyclone hydraulic separators, and receiving vat (100L) forms, and is industry conventional equipment;
(6) emulsification, sieve after solid content be 20% nickel powder slip is delivered to surge tank, by centrifugal pump, under 1.0-1.5MPa pressure, squeeze in cyclone hydraulic separators and carry out centrifugal classification, remove super large particle, from overflow, obtain the powder that particle diameter is evenly distributed.
Nickel powder slip carries out classification in adding the corrosion inhibiting solution of composite antioxidant, and classification process temperature is carried out at normal temperatures.
Nickel powder slip is classified as in hierarchy system the slip that different grain size distributes, and the overflow slurry after classification detects after requirement up to specification mutually through SEM/BET/PSD etc., enters in drying system and is dried.
Table 1:
| Grading technology | BET(m2/g) | Particle diameter (nm) | Oxygen (ppm) | Oxygen rate of change % |
| Nickel powder is not before classification | 2.46 | 274 | 5719 | ? |
| After the classification of nickel powder pure water | 2.49 | 271 | 8131 | 42.1 |
| After the classification of nickel powder oxidation resistance liquid | 2.24 | 301 | 5991 | 4.7 |
By the nickel powder Data Detection to above-mentioned distinct methods, from upper table 1, can find out, after metal nickel powder emulsification, classification, storing process all complete in the corrosion inhibiting solution that adds composite antioxidant TX-02, oxygen content amplification 4.7%, and after using pure water classification, oxygen content increases floating 42.1%.Therefore, foregoing invention metallic nickel powder moisture level anti-oxidation method has effectively reduced the oxide etch effect of oxygen in water to metal nickel powder, compares classification metal nickel powder in pure water, and extent of corrosion is little, and surface area variable quantity is little, and oxygen content amplification is little.
Superfine metal nickel powder moisture level processing procedure antioxygen method of the present invention, classification cost is used ethanol low, production process safety, product oxygen content changes little, and product is stable.
Claims (5)
1. moisture level is processed an anti-oxidation method for metal nickel powder, it is characterized in that: step comprises:
(1) in deionized water, add antioxidant TX-02, be stirred to antioxidant and dissolve completely, be mixed with the corrosion inhibiting solution that antioxidant TX-02 mass concentration is 0.1-2%, control this corrosion inhibiting solution pH within the scope of 7-8; Above-mentioned antioxidant TX-02 is obtained for (1-3:1) mixes according to weight ratio by carbohydrazide and citric acid;
(2) unassorted metal nickel powder is added in the emulsifying device that fills the corrosion inhibiting solution that mass concentration prepared by step (1) is 0.1-2%, being mixed with solid content is the nickel powder slip of 10-25%;
(3) start emulsifying device, emulsification nickel powder slip 20-50min, the slip that metal nickel powder emulsion dispersion becomes particle to be evenly distributed;
(4) after emulsification, nickel powder slip after filtering, is sent into hierarchy system classification.
2. moisture level according to claim 1 is processed the anti-oxidation method of metal nickel powder, it is characterized in that: the described corrosion inhibiting solution of step (1) is the corrosion inhibiting solution that antioxidant TX-02 mass concentration is 0.2%.
3. moisture level according to claim 1 is processed the anti-oxidation method of metal nickel powder, it is characterized in that: the solid content that is mixed with nickel powder slip described in step (2) is 20%.
4. moisture level according to claim 1 is processed the anti-oxidation method of metal nickel powder, it is characterized in that: the described emulsification nickel powder slip emulsification times of step (3) is 30min.
5. moisture level according to claim 1 is processed the anti-oxidation method of metal nickel powder, it is characterized in that: the hierarchy system described in step (4) is by surge tank, centrifugal pump, cyclone hydraulic separators, and receiving vat forms; Classification process is: by step (4) emulsification, sieve after solid content be 10-25% nickel powder slip is delivered to surge tank, by centrifugal pump under 1.0-1.5MPa pressure, squeeze in cyclone hydraulic separators and carry out centrifugal classification, from the overfall of cyclone hydraulic separators, obtain the powder that particle diameter is evenly distributed.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310690780.2A CN103691931B (en) | 2013-12-16 | 2013-12-16 | The anti-oxidation method of moisture level process metal nickel powder |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310690780.2A CN103691931B (en) | 2013-12-16 | 2013-12-16 | The anti-oxidation method of moisture level process metal nickel powder |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN103691931A true CN103691931A (en) | 2014-04-02 |
| CN103691931B CN103691931B (en) | 2015-12-02 |
Family
ID=50353683
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201310690780.2A Active CN103691931B (en) | 2013-12-16 | 2013-12-16 | The anti-oxidation method of moisture level process metal nickel powder |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN103691931B (en) |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103962251A (en) * | 2014-04-18 | 2014-08-06 | 松阳县中奇环境工程有限公司 | Shearing emulsifying smashing device for processing materials containing ferrites |
| CN104399975A (en) * | 2014-12-18 | 2015-03-11 | 江苏博迁新材料有限公司 | Method for fully dispersing nanoscale nickel powder |
| CN104785354A (en) * | 2015-04-07 | 2015-07-22 | 台州市金博超导纳米材料科技有限公司 | Method for grading nano-sized metal powder with low-temperature high purity water as medium |
| CN105127412A (en) * | 2015-09-14 | 2015-12-09 | 宁波广博纳米新材料股份有限公司 | Preparation method of low-oxygen submicron copper and manganese alloy powder |
| CN112893830A (en) * | 2020-12-29 | 2021-06-04 | 宁波广新纳米材料有限公司 | Liquid phase grading method for magnetic metal powder |
Citations (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3945863A (en) * | 1973-09-20 | 1976-03-23 | Martin Marietta Corporation | Process for treating metal powders |
| CN1321113A (en) * | 1999-08-31 | 2001-11-07 | 东邦钛株式会社 | Nickel powder for monolithic ceramic capacitor |
| CN1522296A (en) * | 2001-06-20 | 2004-08-18 | 西屋电气有限责任公司 | Improved scale conditioning agents |
| JP2005146386A (en) * | 2003-11-18 | 2005-06-09 | Mitsui Mining & Smelting Co Ltd | Method of producing metal powder slurry, and nickel powder slurry obtained by the production method |
| CN1648070A (en) * | 2005-01-07 | 2005-08-03 | 清华大学 | Method for preparing controlled release high molecular carbon source material for biological method to treat water |
| CN102120257A (en) * | 2011-01-26 | 2011-07-13 | 宁波广博纳米材料有限公司 | Method for removing impurities on surface of ultrafine nickel powder and lubricating and modifying surface of ultrafine nickel powder |
| CN102151823A (en) * | 2011-01-26 | 2011-08-17 | 宁波广博纳米材料有限公司 | Antioxidation method of nano copper powder |
| JP2011156520A (en) * | 2010-02-04 | 2011-08-18 | Sumitomo Metal Mining Co Ltd | Method of classifying metal fine powder |
| CN102325604A (en) * | 2009-03-18 | 2012-01-18 | 日清工程株式会社 | Method for classifying powder |
| CN102327806A (en) * | 2011-06-20 | 2012-01-25 | 宁波广博纳米新材料股份有限公司 | Method taking organic solvent as medium for grading nano-nickel powder for MLCC (multilayer ceramic capacitor) |
| CN102989576A (en) * | 2012-11-07 | 2013-03-27 | 宁波广博纳米新材料股份有限公司 | Method for grading silver powder for solar battery |
-
2013
- 2013-12-16 CN CN201310690780.2A patent/CN103691931B/en active Active
Patent Citations (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3945863A (en) * | 1973-09-20 | 1976-03-23 | Martin Marietta Corporation | Process for treating metal powders |
| CN1321113A (en) * | 1999-08-31 | 2001-11-07 | 东邦钛株式会社 | Nickel powder for monolithic ceramic capacitor |
| CN1522296A (en) * | 2001-06-20 | 2004-08-18 | 西屋电气有限责任公司 | Improved scale conditioning agents |
| JP2005146386A (en) * | 2003-11-18 | 2005-06-09 | Mitsui Mining & Smelting Co Ltd | Method of producing metal powder slurry, and nickel powder slurry obtained by the production method |
| CN1648070A (en) * | 2005-01-07 | 2005-08-03 | 清华大学 | Method for preparing controlled release high molecular carbon source material for biological method to treat water |
| CN102325604A (en) * | 2009-03-18 | 2012-01-18 | 日清工程株式会社 | Method for classifying powder |
| JP2011156520A (en) * | 2010-02-04 | 2011-08-18 | Sumitomo Metal Mining Co Ltd | Method of classifying metal fine powder |
| CN102120257A (en) * | 2011-01-26 | 2011-07-13 | 宁波广博纳米材料有限公司 | Method for removing impurities on surface of ultrafine nickel powder and lubricating and modifying surface of ultrafine nickel powder |
| CN102151823A (en) * | 2011-01-26 | 2011-08-17 | 宁波广博纳米材料有限公司 | Antioxidation method of nano copper powder |
| CN102327806A (en) * | 2011-06-20 | 2012-01-25 | 宁波广博纳米新材料股份有限公司 | Method taking organic solvent as medium for grading nano-nickel powder for MLCC (multilayer ceramic capacitor) |
| CN102989576A (en) * | 2012-11-07 | 2013-03-27 | 宁波广博纳米新材料股份有限公司 | Method for grading silver powder for solar battery |
Non-Patent Citations (2)
| Title |
|---|
| 李玉磊等: "新型除氧剂的研究与进展", 《工业水处理》 * |
| 王正平等: "新型除氧剂研究", 《应用科技》 * |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103962251A (en) * | 2014-04-18 | 2014-08-06 | 松阳县中奇环境工程有限公司 | Shearing emulsifying smashing device for processing materials containing ferrites |
| CN104399975A (en) * | 2014-12-18 | 2015-03-11 | 江苏博迁新材料有限公司 | Method for fully dispersing nanoscale nickel powder |
| CN104785354A (en) * | 2015-04-07 | 2015-07-22 | 台州市金博超导纳米材料科技有限公司 | Method for grading nano-sized metal powder with low-temperature high purity water as medium |
| CN105127412A (en) * | 2015-09-14 | 2015-12-09 | 宁波广博纳米新材料股份有限公司 | Preparation method of low-oxygen submicron copper and manganese alloy powder |
| CN112893830A (en) * | 2020-12-29 | 2021-06-04 | 宁波广新纳米材料有限公司 | Liquid phase grading method for magnetic metal powder |
Also Published As
| Publication number | Publication date |
|---|---|
| CN103691931B (en) | 2015-12-02 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN103691931B (en) | The anti-oxidation method of moisture level process metal nickel powder | |
| EP3040140B1 (en) | Method of preparing nano-copper powder and nano-copper powder prepared with the same | |
| CN102977224B (en) | Method for preparing calcium alginate | |
| CN103468004B (en) | Wax slurry of loaded with nano Graphene and its production and use | |
| CN102248176A (en) | Preparation method of flake silver powder with low burning loss | |
| CN105579566A (en) | Oil extraction aids in grain processing | |
| CN103351651B (en) | Preparation method of nano molybdenum disulfide organic dispersion liquid | |
| Foo et al. | Preparation of black cumin seed oil Pickering nanoemulsion with enhanced stability and antioxidant potential using nanocrystalline cellulose from oil palm empty fruit bunch | |
| CN103977909A (en) | High-argillization coal washing agent | |
| CN108947580B (en) | Preparation method of layered vermiculite powder | |
| CN106698378B (en) | A kind of preparation method and applications of novel organically-modified porous nanometer material | |
| Guo et al. | One-step synthesis of micro-sized hexagon silver sheets by the ascorbic acid reduction with the presence of H2SO4 | |
| CN102191118A (en) | Oil-based suspended base liquid of nano diamond powder and preparation process thereof | |
| CN103264167A (en) | Surface modification nanometer copper particle and preparation method thereof | |
| CN114181731B (en) | Micelle dispersion type oil slurry settling agent and preparation method thereof | |
| CN115260795B (en) | Method for reducing agglomerated particles in titanium dioxide product | |
| CN115152888B (en) | Cannabin pickering granules and preparation method and application thereof | |
| CN103503862B (en) | Mesotrione oil suspension agent composition | |
| CN105008070B (en) | Silver powder | |
| CN105345013A (en) | Manufacturing method for flaky silver powder with high flake rate and narrow particle size distribution | |
| CN110684206B (en) | Preparation method of asphalt modified emulsified asphalt without sticking wheel rock | |
| CN108940218B (en) | Preparation method of heavy metal adsorbent-lignin microspheres | |
| CN107177229B (en) | Aqueous wax dispersion and preparation method thereof | |
| CN111138717A (en) | Preparation method of nanoscale coated red phosphorus flame retardant | |
| CN112974827A (en) | Preparation method of spherical silver powder with high tap density and surface wrinkles |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| C41 | Transfer of patent application or patent right or utility model | ||
| TR01 | Transfer of patent right |
Effective date of registration: 20161028 Address after: 223801 Suqian province high tech Development Zone, Jiangshan Road, No. 23, No. Patentee after: Jiangsu Bo move new materials Limited by Share Ltd Address before: Yinzhou District Zhejiang city in Ningbo province where 315153 broad industrial park spring news site Patentee before: Ningbo Guangbo New Nanomaterials Stock Co.,Ltd. |