CN1073482C - Method for producing superfine sphere metallic nickel powder - Google Patents
Method for producing superfine sphere metallic nickel powder Download PDFInfo
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- CN1073482C CN1073482C CN98124035A CN98124035A CN1073482C CN 1073482 C CN1073482 C CN 1073482C CN 98124035 A CN98124035 A CN 98124035A CN 98124035 A CN98124035 A CN 98124035A CN 1073482 C CN1073482 C CN 1073482C
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- nickel powder
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- hydrazine
- metallic nickel
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Abstract
The present invention provides a method for producing superfine sphere metal nickel powder. In the method, an amide type surfactant is added in a bivalent soluble nickel salt solution; under the alkaline condition, hydrazine or hydrazine hydrate is used for direct reduction to produce the high-quality metal nickel spherical powder with the advantages of narrow grain size distribution, low oxidation rate and average grain size of 0.1 to 2.0 mu m. The present invention hugely lowers production cost and reduces environmental pollution. The produced metal nickel powder can be widely used in industries of chemical industry catalysis, powder metallurgy, batteries, magnetic materials, electrons, electric appliances, etc.
Description
What the present invention relates to is a kind of a kind of manufacture method of superfine sphere metallic nickel powder, belongs to the manufacturing technology field of powder body material.
The ultra micro metal nickel powder has very big skin effect and bulk effect, and in magnetic, methods such as interior pressure, thermal resistance, chemism demonstrate many special nature, and its application technology constantly is being penetrated into each scientific domain.
The method of existing manufacturing metal nickel powder is a lot: as mechanical crushing method, and electrolysis, carboxyl thermal dissociation method, vacuum distillation condensation method, pulp High Pressure Hydrogen reducing process and solution reduction method etc.Adopting these the prepared metal nickel powder of method is not that the out-of-shape granularity is big, is exactly that the manufacture method cost is too high, can not push industrial production to.
Liquid phase reduction prepares nickel powder generally all to be finished by two steps.The first step is prepared Ni (OH) at normal temperatures
2Colloid belongs to liquid phase and becomes nuclear reaction; Second step was used hydrazine hydrate reduction Ni (OH) under the uniform temperature condition
2Generate metal nickel powder, belong to oxidation---reduction reaction.The basic chemical reaction in two steps is:
The change of two-step reaction condition all will influence the granularity and the shape of nickel powder, especially the Ni (OH) of first step generation
2The granular size of colloid and shape have direct influence and play a decisive role the size of the nickel powder of final generation and shape.
At Ni (OH)
2In the precipitation process, because Van der Waals force effect between micelle, micelle is incited somebody to action spontaneous rapidly gathering and is grown up.Again because the colloid size that just has been settled out is very little, its cloth youth motion highly significant makes that the gathering between micelle is fine and close more and irreversible simultaneously.Thereby make Ni (OH)
2The nickel powder particle that micelle and final reduction generate is thick and irregular.
The flat 4-74810 of Japan adopts the mixing reducing agent reduction nickel salt contain hydrazine hydrate to prepare nickel powder, and Japanese flat 5-51610 adopts the compound of hydrazine or hydrazine directly to reduce nickel hydroxide, the big and out-of-shape of gained nickel powder particle diameter, and it is serious to reunite.
Shanghai East China University of Science is a reducing agent with the hydrazine hydrate, and silver nitrate is a nucleator, and polyvinylpyrrolidone is that to prepare nickel powder be nickel sulfate solution directly to be added drop-wise to contain Na to protective agent
2CO
3In the mixed liquor of hydrazine hydrate and PVP, add AgNO again
3Nucleation.Though this method can make the thinner nickel powder of particle diameter, very easily produce the very high suitability for industrialized production that is difficult for of sheet nickel and manufacturing cost in the process.
The objective of the invention is to overcome above deficiency, providing a kind of can reduce production costs greatly, the manufacture method of the superfine sphere metallic nickel powder that little, the regular suitability for industrialized of nickel powder particle diameter is produced.
The object of the present invention is achieved like this:
The inventive method is to add amide surfactants in divalence soluble nickel salting liquid, under alkali condition, generate nickel hydroxide precipitate with the alkali metal hydroxide reaction, be 8～13 at pH then, temperature is in 40～90 ℃ of scopes, the hydrate reduction nickel hydroxide that adds hydrazine or hydrazine, make the sphere metal nickel powder that average grain diameter is 0.1～2 μ m, the concentration of amide surfactants is 1%～1 ‰ (percentage by weight), molecular weight 〉=1,000,000.
The concentration of nickel salt is 0.1～3mol/L among the present invention, and used nickel salt can be soluble nickel salt such as nickel chloride, nickelous sulfate.
The hydrate concentration of hydrazine of the present invention or hydrazine is 10～80% (percentage by weights).
Characteristics of the present invention just are to add in advance specific high molecular surfactant in nickel salt solution, utilize the absorption of good sterically hindered effect of surfactant and characteristic, at the Ni of the harsh one-tenth of precipitation reaction (OH)
2The micelle surface forms one deck protection mould, has stoped Ni (OH) effectively
2The gathering of micelle and growing up, thus guaranteed that the second step reduction reaction prepares the high-quality nickel powder of superfine sphere.
The inventive method need not used AgNO
3Cook nucleator and a large amount of organic protective agent Deng precious metal salt, and only use (100,000/to ten thousand/Ni/ additive) amide surfactants of trace, just can produce the high-quality regular spherical metal nickel powder of average grain diameter 0.1～2.0 μ m.Metal nickel powder particle size distribution range narrow (0.1～03 μ m or 1. (0～2.0 μ m) and oxygenation efficiency extremely low (120～140 ℃ of oven dry 6 hours, oxygen content≤0.03%, and put 60 days oxygen content at normal temperatures in the air and do not increase).The inventive method can reduce environmental pollution, and suitability for industrialized production reduces production costs significantly, can be widely used in industries such as chemical industry catalysis, powder metallurgy, battery, magnetic material and electronic apparatus.
Introduce embodiments of the invention below:
Embodiment 1:
At volume is in the enamel reaction still of 2000L, add nickel chloride solution that 1000L concentration is 1.2mol/L and 1L weight percent concentration and be 5 ‰ polyacrylamide solution, under stirring condition, the sodium hydroxide solution that adds concentration and be 5mol/L is to pH value 11.5, be warmed up to 70 ℃ then, the hydrazine hydrate solution 140L that adds 60% (weight percent concentration) again carries out reduction reaction.Reaction time is 30 minutes.Reaction finishes, after filtration, washing, vacuum drying, powder process shape metal nickel powder.
The metal nickel powder that makes by said method is viewed as sphere under Electronic Speculum, flat footpath granularity is 0.2 μ m.
Embodiment 2:
At volume is in the reactor of 2000L, add nickel sulfate solution that 1000L concentration is 0.5mol/L and weight percent concentration and be 1% polyacrylamide solution 0.5L, under stirring condition, adding concentration is the sodium hydroxide solution of 10mol/L, to pH value 9, and then being warmed up to 90 ℃, the hydrazine hydrate solution 50L that adds 80% (percentage by weight) concentration carries out reduction reaction.Reaction time is 20 minutes.Reaction finishes, after filtration, washing, the granulated metal nickel powder is made in vacuum drying.
The metal nickel powder that makes by said method is viewed as sphere under Electronic Speculum, flat footpath particle diameter is 1.0 μ m.
The embodiment hole
At volume is in the reactor of 2000L, adding concentration is that nickel sulfate solution 1000L and (percentage by weight) concentration of 1.0mol/L is 0.5% polyacrylamide solution 1L, adding weight concentration under stirring condition is the sodium hydroxide solution of 8mol/L, to pH value 13, heat up 70 ℃ then, add weight percent concentration and be 40% hydrazine hydrate solution 170L and carry out reduction reaction, the reaction time is 30 minutes.Reaction finishes after filtration, washs dry that average grain diameter is the metal nickel powder of 0.3 μ m.
Embodiment 4:
At volume is in the reactor of 2000L, adding concentration is the polyacrylamide solution 3L of nickel sulfate solution 1000L and 0.1% (percentage by weight) concentration of 1.5 mol/L, under stirring condition, the sodium hydroxide solution that adds concentration and be 10mol/L concentration is to pH value 12, and then be warming up to 75 ℃, add weight percent concentration and be 60% hydrazine hydrate solution 150L and carry out reduction reaction.20 minutes reaction time.Reaction finishes, and after filtration, washing is dry, makes the metal nickel powder that average grain diameter is 0.1 μ m.
Embodiment 5:
At volume is in the reactor of 2000L, adding concentration is the polyacrylamide solution 2L of nickel sulfate solution 1000L and 0.3% (percentage by weight) concentration of 1.2 mol/L, under stirring condition, the sodium hydroxide solution that adds 50mol/L concentration is to pH value 10, be warming up to 80 ℃ then, add weight percent concentration and be 40% hydrazine hydrate solution and carry out reduction reaction.10 minutes reaction time.After filtration, drying makes the metal nickel powder that average grain diameter is 0.2 μ m.
Embodiment 6:
In the reactor of volume 2000L, adding concentration is the nickel sulfate solution 1000L of 1.5mol/L and the polyacrylamide solution 0.5L that weight percent concentration is 1% concentration, under stirring condition, the sodium hydroxide solution that adds concentration and be 10mol/L is to pH value 8, be warming up to 85 ℃ then, add weight percent concentration and be 80% hydrazine hydrate 100L and carry out reduction reaction.40 minutes reaction time.Washing after filtration,, drying make the metal nickel powder of particle mean size 0.2 μ m.
The molecular weight of polyacrylamide all 〉=1,000,000 in the various embodiments described above.
Claims (5)
1, the manufacture method of superfine sphere metallic nickel powder, it is characterized in that described method is to add amide surfactants in divalence soluble nickel salting liquid, under alkali condition, generating nickel hydroxide precipitate with the alkali metal hydroxide reaction, is 8～13 at pH then, and temperature is under 40～90 ℃ of conditions, the hydrate reduction nickel hydroxide that adds hydrazine or hydrazine, make superfine sphere metallic nickel powder, the concentration of amide surfactants is 1%～1 ‰ (percentage by weight), molecular weight 〉=1,000,000.
2, the manufacture method of superfine sphere metallic nickel powder according to claim 1 is characterized in that the soluble nickel concentration of salt solution is 0.1～3mol/L.
3, the manufacture method of superfine sphere metallic nickel powder according to claim 1 and 2, the concentration that it is characterized in that alkali metal hydroxide is 1～10mol/L.
4, the manufacture method of superfine sphere metallic nickel powder according to claim 1 and 2, the hydrate concentration that it is characterized in that hydrazine or hydrazine are 10～80% (percentage by weights).
5, the manufacture method of superfine sphere metallic nickel powder according to claim 3 is characterized in that hydrazine hydrate concentration is 10～80% (percentage by weights).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN98124035A CN1073482C (en) | 1998-12-29 | 1998-12-29 | Method for producing superfine sphere metallic nickel powder |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN98124035A CN1073482C (en) | 1998-12-29 | 1998-12-29 | Method for producing superfine sphere metallic nickel powder |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1223919A CN1223919A (en) | 1999-07-28 |
| CN1073482C true CN1073482C (en) | 2001-10-24 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN98124035A Expired - Fee Related CN1073482C (en) | 1998-12-29 | 1998-12-29 | Method for producing superfine sphere metallic nickel powder |
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Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP3915387B2 (en) * | 2000-08-29 | 2007-05-16 | 昭栄化学工業株式会社 | Conductor paste |
| CN1299863C (en) * | 2005-03-31 | 2007-02-14 | 上海交通大学 | Method for preparing hollow or clad nickel alloy spherical powder |
| CN100448574C (en) * | 2005-09-29 | 2009-01-07 | 江苏大学 | Method for preparing nano nickel |
| CN100389916C (en) * | 2006-04-14 | 2008-05-28 | 北京科技大学 | Method of preparing ultrafine alloy powder by coprecipitation coreduction |
| CN102528073A (en) * | 2012-02-16 | 2012-07-04 | 四川大学 | Non-ferromagnetic nickel powder and preparation method for same |
| CN102962470B (en) * | 2012-11-06 | 2015-04-29 | 昆明舒扬科技有限公司 | Method for preparing spherical ultrafine nickel powder at room temperature |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS551610A (en) * | 1978-06-19 | 1980-01-08 | Hitachi Ltd | Magnetic bubble detector |
| CN1104137A (en) * | 1994-08-31 | 1995-06-28 | 华东理工大学 | Super-fine globular silver-palladium alloy powder production method |
-
1998
- 1998-12-29 CN CN98124035A patent/CN1073482C/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS551610A (en) * | 1978-06-19 | 1980-01-08 | Hitachi Ltd | Magnetic bubble detector |
| CN1104137A (en) * | 1994-08-31 | 1995-06-28 | 华东理工大学 | Super-fine globular silver-palladium alloy powder production method |
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| CN1223919A (en) | 1999-07-28 |
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Granted publication date: 20011024 Termination date: 20101229 |