CN101708558B - Liquid phase preparation method of superfine nickel metal powder - Google Patents
Liquid phase preparation method of superfine nickel metal powder Download PDFInfo
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- CN101708558B CN101708558B CN2009102178559A CN200910217855A CN101708558B CN 101708558 B CN101708558 B CN 101708558B CN 2009102178559 A CN2009102178559 A CN 2009102178559A CN 200910217855 A CN200910217855 A CN 200910217855A CN 101708558 B CN101708558 B CN 101708558B
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- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 title claims abstract description 89
- 229910052759 nickel Inorganic materials 0.000 title claims abstract description 40
- 229910052751 metal Inorganic materials 0.000 title claims abstract description 39
- 239000002184 metal Substances 0.000 title claims abstract description 39
- 239000000843 powder Substances 0.000 title claims abstract description 31
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- 239000007791 liquid phase Substances 0.000 title claims abstract description 11
- 238000000034 method Methods 0.000 claims abstract description 27
- 238000006243 chemical reaction Methods 0.000 claims abstract description 25
- 239000002270 dispersing agent Substances 0.000 claims abstract description 17
- 238000003756 stirring Methods 0.000 claims abstract description 10
- 230000035484 reaction time Effects 0.000 claims abstract description 9
- 238000003828 vacuum filtration Methods 0.000 claims abstract description 7
- 238000010438 heat treatment Methods 0.000 claims abstract description 4
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 claims description 20
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 18
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 18
- 239000007789 gas Substances 0.000 claims description 13
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 claims description 12
- 239000012530 fluid Substances 0.000 claims description 11
- USIUVYZYUHIAEV-UHFFFAOYSA-N diphenyl ether Chemical compound C=1C=CC=CC=1OC1=CC=CC=C1 USIUVYZYUHIAEV-UHFFFAOYSA-N 0.000 claims description 10
- IPCSVZSSVZVIGE-UHFFFAOYSA-N hexadecanoic acid Chemical compound CCCCCCCCCCCCCCCC(O)=O IPCSVZSSVZVIGE-UHFFFAOYSA-N 0.000 claims description 10
- 229910052786 argon Inorganic materials 0.000 claims description 9
- 229910052757 nitrogen Inorganic materials 0.000 claims description 9
- 238000005119 centrifugation Methods 0.000 claims description 8
- WRIDQFICGBMAFQ-UHFFFAOYSA-N (E)-8-Octadecenoic acid Natural products CCCCCCCCCC=CCCCCCCC(O)=O WRIDQFICGBMAFQ-UHFFFAOYSA-N 0.000 claims description 6
- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 claims description 6
- QSBYPNXLFMSGKH-UHFFFAOYSA-N 9-Heptadecensaeure Natural products CCCCCCCC=CCCCCCCCC(O)=O QSBYPNXLFMSGKH-UHFFFAOYSA-N 0.000 claims description 6
- ZQPPMHVWECSIRJ-UHFFFAOYSA-N Oleic acid Natural products CCCCCCCCC=CCCCCCCCC(O)=O ZQPPMHVWECSIRJ-UHFFFAOYSA-N 0.000 claims description 6
- 239000005642 Oleic acid Substances 0.000 claims description 6
- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 claims description 6
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 claims description 6
- 235000021314 Palmitic acid Nutrition 0.000 claims description 5
- 235000021355 Stearic acid Nutrition 0.000 claims description 5
- 239000000284 extract Substances 0.000 claims description 5
- WQEPLUUGTLDZJY-UHFFFAOYSA-N n-Pentadecanoic acid Natural products CCCCCCCCCCCCCCC(O)=O WQEPLUUGTLDZJY-UHFFFAOYSA-N 0.000 claims description 5
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 claims description 5
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 claims description 5
- 239000008117 stearic acid Substances 0.000 claims description 5
- 239000011259 mixed solution Substances 0.000 claims description 4
- 239000003960 organic solvent Substances 0.000 claims description 4
- 238000002347 injection Methods 0.000 claims description 3
- 239000007924 injection Substances 0.000 claims description 3
- 125000002915 carbonyl group Chemical group [*:2]C([*:1])=O 0.000 abstract description 13
- 238000004519 manufacturing process Methods 0.000 abstract description 7
- 238000000354 decomposition reaction Methods 0.000 abstract description 4
- 239000007788 liquid Substances 0.000 abstract 1
- 238000002156 mixing Methods 0.000 abstract 1
- 239000000203 mixture Substances 0.000 abstract 1
- 239000012071 phase Substances 0.000 abstract 1
- 230000001681 protective effect Effects 0.000 abstract 1
- 238000000926 separation method Methods 0.000 abstract 1
- 239000002245 particle Substances 0.000 description 13
- 238000005516 engineering process Methods 0.000 description 7
- 235000021313 oleic acid Nutrition 0.000 description 5
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 4
- 229910002091 carbon monoxide Inorganic materials 0.000 description 4
- 150000002739 metals Chemical class 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 230000000694 effects Effects 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 238000005979 thermal decomposition reaction Methods 0.000 description 3
- 238000007704 wet chemistry method Methods 0.000 description 3
- 239000012159 carrier gas Substances 0.000 description 2
- 239000003638 chemical reducing agent Substances 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 239000000428 dust Substances 0.000 description 2
- 238000009434 installation Methods 0.000 description 2
- 150000002815 nickel Chemical class 0.000 description 2
- DOLZKNFSRCEOFV-UHFFFAOYSA-L nickel(2+);oxalate Chemical compound [Ni+2].[O-]C(=O)C([O-])=O DOLZKNFSRCEOFV-UHFFFAOYSA-L 0.000 description 2
- GNRSAWUEBMWBQH-UHFFFAOYSA-N nickel(II) oxide Inorganic materials [Ni]=O GNRSAWUEBMWBQH-UHFFFAOYSA-N 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000004033 diameter control Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 230000002500 effect on skin Effects 0.000 description 1
- 238000005868 electrolysis reaction Methods 0.000 description 1
- 229920002521 macromolecule Polymers 0.000 description 1
- 239000011553 magnetic fluid Substances 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 238000005272 metallurgy Methods 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- 230000001473 noxious effect Effects 0.000 description 1
- 238000002161 passivation Methods 0.000 description 1
- 230000001376 precipitating effect Effects 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 239000011241 protective layer Substances 0.000 description 1
- 238000006722 reduction reaction Methods 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 238000009834 vaporization Methods 0.000 description 1
- 230000008016 vaporization Effects 0.000 description 1
- 229920003169 water-soluble polymer Polymers 0.000 description 1
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- Manufacture Of Metal Powder And Suspensions Thereof (AREA)
- Powder Metallurgy (AREA)
Abstract
The invention relates to a liquid phase preparation method of superfine nickel metal powder, which more particularly comprises the steps of: evenly mixing nickel tetracarbonyl, organic carrier liquid and dispersing agent; injecting the mixture into a container with protective gas and then heating; stirring in the whole process with the reaction temperature of 50-200 DEG C and the reaction time of 0.1-12h; and finally, extracting the superfine nickel metal powder by vacuum filtration or centrifugal separation. Compared with the existing carbonyl metal gas phase decomposition method, the liquid phase preparation method only needs lower reaction temperature and shorter reaction time, is simple in technique and high in production efficiency. More important, the superfine nickel metal powder prepared by the method has high purity, good dispersibility and controllable granularity, and is not easily oxidized.
Description
Technical field
The invention belongs to powder metallurgical technology, particularly a kind of preparation method of superfine nickel metal powder.
Technical background
Generally speaking, superfine powder is meant that particle diameter is less than 1 micron powder.Because particle diameter is less, superfine powder has a series of special effectses, and has many special natures that are different from common powder, becomes the focus of various countries' research in recent years gradually.
Nickel has good processability, corrosion resistance, electrovacuum and electromagnetism control, is widely used in fields such as metallurgy, chemical industry, electronics and new material.Extra-fine nickel powder is owing to have great bulk effect and skin effect, and in chemism, electrical conductance, aspects such as magnetic demonstrate many special natures, thereby have application prospects.At first, extra-fine nickel powder is a kind of good catalyst, and its stereoselectivity is about ten times of common nickel powder; Secondly, the extra-fine nickel powder good conductivity, non-oxidizability is strong, and alternative noble metal powder prepares electronics industry electrocondution slurry commonly used; Extra-fine nickel powder is dispersed in the macromolecule matrix uniformly, can prepares electromagnetic shielding material, be used for anti-electromagnetic interference, reduce electromagnetic pollution; Extra-fine nickel powder is scattered in forms magnetic fluid in the carrier fluid, can be used for rotatory sealing and make electromagnetic damper.
The method for preparing extra-fine nickel powder mainly contains wet chemistry method, metal carbonyl decomposition method, electrolysis, using vaporization condensation process, physical crushing method etc., and wherein wet chemistry method is the most commonly used, and it is best in quality that the metal carbonyl decomposition method makes extra-fine nickel powder.Patent CN100387383C at first makes the nickel oxalate precipitation by soluble nickel salt, under low vacuum nickel oxalate decomposition, passivation is made extra-fine nickel powder then; It is surface dispersant that patent CN100431750C adopts the water soluble polymer monomer, and the liquid phase chemical reduction by soluble nickel salt makes nano-nickel powder.These wet chemistry methods are owing to adopted raw materials such as precipitating reagent, reducing agent to cause product purity to reduce.Patent application open CN1947902, CN1817528, CN1817526 have introduced the method that the nickel carbonyl thermal decomposition prepares different-shape, different grain size ultra-fine (nanometer) nickel powder, the product purity height, but powder bad dispersibility, easily bonding is grown up, and this process is complicated, causes that easily system reveals the diffusion that causes noxious material.If can improve these shortcomings of metal carbonyl thermal decomposition preparation technology, carbonyl legal system superfine powder technology has application prospects more undoubtedly.
Summary of the invention
The objective of the invention is to improve the deficiency in the metal carbonyl thermal decomposition technology of preparing, provide that a kind of technology is simple, production safety, cheap, method that production efficiency is high, thereby the superfine nickel metal powder of preparation not only purity height, good dispersion, difficult bonding is grown up, and particle diameter control is simple.
According to above-mentioned purpose, technical scheme of the present invention is:
The liquid phase preparation process for preparing a kind of superfine nickel metal powder; it is characterized in that; the concrete steps of this method are: with nickel carbonyl; organic carrier fluid and dispersant are even; injection begins heating after being connected with the container of nitrogen or argon shield gas; and in whole process, keep stirring; reaction temperature is 50~200 ℃; reaction time is 0.1~12 hour; extract superfine nickel metal powder by the method for vacuum filtration or centrifugation at last; described organic carrier fluid can be dimethylbenzene; diphenyl ether; the mixed solution of one or several of dimethyl sulfoxide (DMSO) organic solvent; described dispersant is a stearic acid; palmitic acid or oleic acid; its consumption is 1~2 times of nickel carbonyl mole; the protection gas that this method is used can be nitrogen or argon gas; the protection throughput is 50~200 ml/min, and described nickel carbonyl concentration of volume percent is 1%~20%.
The chemical equation of above-mentioned reaction is: Ni (CO)
4→ Ni+4CO ↑
The organic carrier fluid that uses among the present invention can be one or several mixed solution of organic solvents such as dimethylbenzene, diphenyl ether, dimethyl sulfoxide (DMSO); Dispersant is stearic acid, palmitic acid or oleic acid, and the moment that is decomposed into metal simple-substance at metal carbonyl is wrapped up it, forms protective layer; Protection gas can be nitrogen or argon gas, and the protection throughput is controlled at the 50-200 ml/min.
The superfine nickel metal powder of the present invention's preparation can extract by the method for vacuum filtration or centrifugation.
According to above-mentioned purpose and technical scheme, operation principle of the present invention is: (1) nickel carbonyl, dispersant and carrier fluid three can be dissolved each other, and by stirring the uniformity that keeps reaction system; (2) under the uniform temperature condition, nickel carbonyl is decomposed into elemental metals nickel and carbon monoxide; (3) carbon monoxide is insoluble to dispersant or carrier fluid, takes reaction system out of by carrier gas, also impels reaction constantly to carry out towards the direction of decomposing; (4) elemental metals nickel is just wrapped up by dispersant once appearance in system, and is independent mutually each other, grows up even run foul of each other also can not bond; (5) particle diameter of metal dust decision aspect the concentration of metal carbonyl in reaction system, reaction temperature, reaction time three, relation in direct ratio.
Outstanding feature of the present invention is: (1) product extra-fine nickel powder purity height; (2) reaction temperature is low, the time is short, technology is simple, production efficiency is high, operability and repeatable strong; (3) raw material need not to handle, and does not need special installation, and production cost is low; (3) owing to the coating effect of dispersant, improved the dispersiveness of nickel powder, be difficult for oxidation, avoided the bonding of particle to grow up simultaneously; (4) particle diameter of metallic nickel powder can accurately be controlled by metal carbonyl concentration, reaction time and reaction temperature; (5) wide adaptability of the present invention can be used for the preparation of most of metal carbonyl superfine powders, for the preparation submicron metal provides new approach.
The specific embodiment
Below in conjunction with specific embodiment, further set forth the present invention, but embodiment does not limit the present invention, and do not address part and be applicable to prior art in the invention.
The liquid phase preparation process for preparing a kind of superfine nickel metal powder; the concrete steps of this method are: with nickel carbonyl; organic carrier fluid and dispersant are even; injection begins heating after being connected with the container of nitrogen or argon shield gas; and in whole process, keep stirring; reaction temperature is 50~200 ℃; reaction time is 0.1~12 hour; extract superfine nickel metal powder by the method for vacuum filtration or centrifugation at last; described organic carrier fluid can be dimethylbenzene; diphenyl ether; the mixed solution of one or several of dimethyl sulfoxide (DMSO) organic solvent; described dispersant is a stearic acid; palmitic acid or oleic acid; its consumption is 1~2 times of nickel carbonyl mole; the protection gas that this method is used can be nitrogen or argon gas; the protection throughput is 50~200 ml/min, and described nickel carbonyl concentration of volume percent is 1%~20%.
The chemical equation of above-mentioned reaction is: Ni (CO)
4→ Ni+4CO ↑
The superfine nickel metal powder of the present invention's preparation can extract by the method for vacuum filtration or centrifugation.
According to above-mentioned purpose and technical scheme, operation principle of the present invention is: (1) nickel carbonyl, dispersant and carrier fluid three can be dissolved each other, and by stirring the uniformity that keeps reaction system; (2) under the uniform temperature condition, nickel carbonyl is decomposed into elemental metals nickel and carbon monoxide; (3) carbon monoxide is insoluble to dispersant or carrier fluid, takes reaction system out of by carrier gas, also impels reaction constantly to carry out towards the direction of decomposing; (4) elemental metals nickel is just wrapped up by dispersant once appearance in system, and is independent mutually each other, grows up even run foul of each other also can not bond; (5) particle diameter of metal dust decision aspect the concentration of metal carbonyl in reaction system, reaction temperature, reaction time three, relation in direct ratio.
Embodiment 1
Nickel carbonyl 5 milliliters of (being equivalent to 38.6mmol), 50 milliliters of dimethylbenzene, stearic acid 11 grams (being equivalent to 38.6mmol) are miscible evenly, join in the reaction vessel that has air inlet/outlet and agitating device, continue to feed nitrogen, flow-control is in 90~100 ml/min, keep stirring, begin heat temperature raising then, keep 50 ℃, 12 hours.Obtain about 1.35 grams of extra-fine nickel powder by centrifugation at last, particle mean size is 110 nanometers.
Embodiment 2
Nickel carbonyl 5 milliliters of (being equivalent to 38.6mmol), 450 milliliters of dimethylbenzene, oleic acid 20 grams (being equivalent to 70.8mmol) are miscible evenly, join in the reaction vessel that has air inlet/outlet and agitating device, continue to feed nitrogen, flow-control is in 150~160 ml/min, keep stirring, begin heat temperature raising then, keep 90 ℃, 10 hours.Obtain about 1.03 grams of extra-fine nickel powder by centrifugation at last, particle mean size is 60 nanometers.
Embodiment 3
Nickel carbonyl 10 milliliters of (being equivalent to 77.2mmol), 50 milliliters of dimethyl sulfoxide (DMSO)s, oleic acid 35 grams (being equivalent to 123.9mmol) are miscible evenly, join in the reaction vessel that has air inlet/outlet and agitating device, continue to feed argon gas, flow-control is in 180~190 ml/min, keep stirring, begin heat temperature raising then, keep 150 ℃, 8 hours.Obtain about 4.10 grams of extra-fine nickel powder by vacuum filtration at last, particle mean size is 0.8 micron.
Embodiment 4
Nickel carbonyl 10 milliliters of (being equivalent to 77.2mmol), 50 milliliters of diphenyl ether, palmitic acid 20 grams (being equivalent to 78.Ommol) are miscible evenly, join in the reaction vessel that has air inlet/outlet and agitating device, continue to feed argon gas, flow-control is in 60~70 ml/min, keep stirring, begin heat temperature raising then, keep 200 ℃, 0.1 hour.Obtain about 1.22 grams of extra-fine nickel powder by centrifugation at last, particle mean size is 0.5 micron.
Outstanding feature of the present invention is: (1) product extra-fine nickel powder purity height; (2) reaction temperature is low, the time is short, technology is simple, production efficiency is high, operability and repeatable strong; (3) raw material need not to process, and does not need special installation, and production cost is low; (3) owing to the coating function of dispersant, improved the dispersiveness of nickel powder, be difficult for oxidation, avoided simultaneously the bonding of particle to grow up; (4) particle diameter of metallic nickel powder can accurately be controlled by metal carbonyl concentration, reaction time and reaction temperature; (5) wide adaptability of the present invention can be used for the preparation of most of metal carbonyl superfine powders, for the preparation submicron metal provides new approach.
Claims (4)
1. the liquid phase preparation process of a superfine nickel metal powder; it is characterized in that; the concrete steps of this method are: with nickel carbonyl; and dimethylbenzene; diphenyl ether; the organic carrier fluid and the stearic acid of the mixed solution of one or several of dimethyl sulfoxide (DMSO) organic solvent; the dispersant of palmitic acid or oleic acid is even; injection begins heating after being connected with the container of nitrogen or argon shield gas; and in whole process, keep stirring; reaction temperature is 50~200 ℃; reaction time is 0.1~12 hour, extracts superfine nickel metal powder by the method for vacuum filtration or centrifugation at last.
2. the liquid phase preparation process of a kind of superfine nickel metal powder according to claim 1 is characterized in that, described dispersant dosage is 1~2 times of nickel carbonyl mole.
3. the liquid phase preparation process of a kind of superfine nickel metal powder according to claim 1 is characterized in that, the protection gas that this method is used can be nitrogen or argon gas, and the protection throughput is 50~200 ml/min.
4. the liquid phase preparation process of a kind of superfine nickel metal powder according to claim 1 is characterized in that, described nickel carbonyl concentration of volume percent is 1%~20%.
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CN102443702A (en) * | 2011-10-12 | 2012-05-09 | 上海华力微电子有限公司 | Recovery method of nickel |
CN108941604A (en) * | 2018-08-01 | 2018-12-07 | 浙江埃普瑞纳米材料有限公司 | A kind of preparation method of novel simple block nanometer iron powder |
Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN1491762A (en) * | 2002-10-22 | 2004-04-28 | 中南大学 | Process for preparing fibrous nickel powder |
CN1947902A (en) * | 2006-11-24 | 2007-04-18 | 金川集团有限公司 | Method for producing nano-nickel powder by thermal dissociation of carbonyl nickel |
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Patent Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
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CN1491762A (en) * | 2002-10-22 | 2004-04-28 | 中南大学 | Process for preparing fibrous nickel powder |
CN1947902A (en) * | 2006-11-24 | 2007-04-18 | 金川集团有限公司 | Method for producing nano-nickel powder by thermal dissociation of carbonyl nickel |
Non-Patent Citations (1)
Title |
---|
龚春红等.水性体系中超细镍粉的液相还原制备.《化学研究》.2008,第19卷(第4期),93-96. * |
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