CN1903430A - Method for preparing nickel nanometer catalyst - Google Patents
Method for preparing nickel nanometer catalyst Download PDFInfo
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- CN1903430A CN1903430A CN 200610109613 CN200610109613A CN1903430A CN 1903430 A CN1903430 A CN 1903430A CN 200610109613 CN200610109613 CN 200610109613 CN 200610109613 A CN200610109613 A CN 200610109613A CN 1903430 A CN1903430 A CN 1903430A
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- exchange resin
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Abstract
A nano-Ni catalyst features that the Ni nanoparticles are adsorbed onto the ion exchange resin. Its preparing process includes reaction between ion exchange resins or the high-molecular material with the function of ion exchange resin and nickel chloride or lithium nickelate and reducing by sodium borohydride.
Description
Affiliated technical field
The present invention relates to prepare a kind of method of heterogeneous nickel nanometer catalyst, belong to the material field with lithium nickelate or nickel chloride and ion exchange resin or macromolecular material reaction with ion exchanging function.
Background technology
Raney nickel is because price is low, and process controllability is strong, and the reactivity height is widely used in hydrogenation, coupling, and oxidation is in the various organic reactions such as disproportionation.Adopt Raney-Ni as catalyst now in the industrial production mostly.Raney-Ni is the Raney nickel that utilizes the fusion method preparation, and its major defect is that reaction selectivity is low, and than being easier to inactivation, poor heat resistance has limited production capacity and life of catalyst.Therefore develop high activity, low cost, the low pollution, novel Raney nickel has crucial meaning.
Nanometer nickel is because size is little, and specific area is big, and the surface atom number is more to cause its surface-active site to be increased with coordination unsaturation surface atom, has very high catalytic activity, has caused catalysis circle researcher's very big attention in recent years.The synthetic method of nanometer nickel has at present: vapor phase method, liquid phase method and solid phase method.Vapor phase method comprises the inert gases agglomeration method, gas chemistry reducing process etc.Liquid phase method comprises: liquid phase chemical reduction method, sol-gel process, reverse microemulsion process.Solid phase method comprises mechanical alloying method and phase oxidative reducing process.Wherein, the product purity height of inert gases agglomeration method, crystalline structure is good, the particle cleaning, rare reunion is the main method for preparing nanometer nickel at present, but technical equipment requires height, the energy consumption height, and the particle diameter wider distribution, the easy oxidation of particle is difficult for industrialization.And solid phase method production nanometer nickel output height, technology is simple, but size of microcrystal is bigger than normal and distribute widely, and product purity is not high.
Different with the method that prepared nanometer nickel in the past, the present invention adopts NiCl
2Or LiNiO
2With cation or anion exchange resin reaction, make Ni
+Or NiO
2 -Ion is attracted on the ion exchange resin, uses NaBH then
4Deng the reducing agent reduction, make it to be converted into Ni (0) also equably attached on the ion exchange resin.The method is simple to operate, and the nanometer nickel shot footpath that obtains is even, the purity height, and catalytic activity is strong, and it is convenient to reclaim, and can reuse repeatedly, has good industrial prospect.
Summary of the invention
Use LiNiO
2With anion exchange resin or macromolecular material reaction, make NiO with anion exchange function
2 -On anion exchange resin, use NaBH
4The reduction, obtain Ni (0), then with watery hydrochloric acid or sodium-chloride water solution wash product.Synthetic route is as follows:
Concrete synthetic method is: anion exchange resin is added LiNiO
2The aqueous solution in, jolting 1hr filters, with the washing of 100ml deionized water.Resin after the washing is added NaBH
4In the aqueous solution, jolting is simultaneously filtered till no gas is emitted, spend the 100ml deionised water,, filter obtaining 1hr among the HCl that resin is soaked in 2mol/L, be washed till pH=6 with deionized water, wash vacuum drying then with 100ml methyl alcohol at last and got product in two days.
Use NiCl
2With cationic ion-exchange resin or have the macromolecular material effect of cation exchange effect, make Ni
2+Get product attached to cationic ion-exchange resin, use NaBH
4Reduction is adsorbed with Ni
2+Cationic ion-exchange resin get product.Synthetic route is as follows:
Concrete synthetic method is: cationic ion-exchange resin is added LiCl
2The aqueous solution in, jolting 1hr filters, with the washing of 100ml deionized water.Resin after the washing is added NaBH
4In the aqueous solution, jolting is simultaneously filtered till no gas is emitted, spend the 100ml deionised water,, filter obtaining 2hr in the NaCl solution that resin is soaked in 2mol/L, be washed till pH=6 with deionized water, wash vacuum drying then with 100ml methyl alcohol at last and got product in two days.
The invention has the advantages that easy and simple to handlely, obtain the nano particle diameter narrowly distributing, the catalytic activity height is easy to reclaim.
Embodiment
Specify the present invention below by embodiment, but the present invention has more than and is limited to following Example.
Embodiment 1
With 0.293g (3mmol) LiNiO
2Be dissolved in the 100ml deionized water, add 30g strong base quaternary ammonium I type anion exchange resin (201*4 type), jolting 1hr filters, with the washing of 100ml deionized water, 1.07g NaBH
4Be dissolved in the 150ml deionized water, jolting simultaneously produces up to no gas in the adding resin.Filter, with the washing of 100ml deionized water, then resin is dissolved in the hydrochloric acid (2mol/L) of 100ml, jolting 1hr filters, and is washed to pH=6, uses the 100ml methanol wash, and vacuum drying got product in 2 days.
Embodiment 2
With 0.713g (3mmol) NiCl
26H
2O is dissolved in the 100ml deionized water, adds 30g sulfonic acid ion exchange resin (TS-92 type), and jolting 1hr filters, with the washing of 100ml deionized water.1.07g NaBH
4Be dissolved in the 150ml deionized water, jolting simultaneously produces until no gas in the adding resin, filters, with the washing of 100ml deionized water, then resin is dissolved in the NaCl solution of 2mol/L, jolting 2hr filters, be washed to pH=6, wash with 100ml methyl alcohol, vacuum drying got product in two days.
Claims (1)
1. synthetic method that is adsorbed in nanometer nickel on the ion exchange resin is characterized in that: spent ion exchange resin or have macromolecular material and the nickel chloride or the lithium nickelate reaction of ion exchange resin, get product with sodium borohydride reduction then, and concrete route is as follows:
Wherein anion exchange resin comprises alkalescent, strong-base anion-exchange resin, the anion exchange resin of transition and corresponding with it various external anion exchange resin, the macromolecular material with anion exchange function; As strong base quaternary ammonium I type anion exchange resin (201*4 type, the 201*7 type), macropore strong base quaternary ammonium I type anion exchange resin (D201 type) macropore strong base quaternary ammonium type П anion exchange resin (D202 type), macroreticular weakly base styrene series anion exchange resin various anion exchange resin such as (D301 types); Cationic ion-exchange resin comprises strong-acid type, middle strong-acid type and weak-acid cation-exchange resin, the cationic ion-exchange resin of transition and corresponding with it various external anion exchange resin, the macromolecular material with anion exchange function; As 001*4 (734) strongly acidic styrene type cation exchange resin, the TS-90 storng-acid cation exchange resin that punches, the equal hole of JT008 strongly acidic styrene type cation exchange resin etc.; NiX
2Comprise NiCl
2, Ni (NO
2)
2, NiSO
4Divalence and trivalent salt etc. various nickel.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2006101096134A CN100406119C (en) | 2006-08-10 | 2006-08-10 | Method for preparing nickel nanometer catalyst |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2006101096134A CN100406119C (en) | 2006-08-10 | 2006-08-10 | Method for preparing nickel nanometer catalyst |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1903430A true CN1903430A (en) | 2007-01-31 |
| CN100406119C CN100406119C (en) | 2008-07-30 |
Family
ID=37672883
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB2006101096134A Expired - Fee Related CN100406119C (en) | 2006-08-10 | 2006-08-10 | Method for preparing nickel nanometer catalyst |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN100406119C (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101862686B (en) * | 2009-04-17 | 2014-04-16 | 财团法人工业技术研究院 | Method for preparing catalysts for catalyzing hydrogen discharge reaction |
| US20150082946A1 (en) * | 2013-09-23 | 2015-03-26 | Soonchunhyang University Incustry Academy Cooperation Foundation | Method of manufacturing nanoparticles using ion exchange resin and liquid reducing process |
Family Cites Families (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1022545C (en) * | 1989-01-30 | 1993-10-27 | 天津大学 | Resin-carried nickel boride catalyst and preparation thereof |
| DE19907861B4 (en) * | 1999-02-24 | 2006-04-13 | Basf Coatings Ag | Polyaddition resins, preparable by heterogeneous catalysis, process and use |
| US6977314B2 (en) * | 2001-12-19 | 2005-12-20 | Rohm And Haas Company | Metal-doped sulfonated ion exchange resin catalysts |
-
2006
- 2006-08-10 CN CNB2006101096134A patent/CN100406119C/en not_active Expired - Fee Related
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101862686B (en) * | 2009-04-17 | 2014-04-16 | 财团法人工业技术研究院 | Method for preparing catalysts for catalyzing hydrogen discharge reaction |
| US20150082946A1 (en) * | 2013-09-23 | 2015-03-26 | Soonchunhyang University Incustry Academy Cooperation Foundation | Method of manufacturing nanoparticles using ion exchange resin and liquid reducing process |
| US9089897B2 (en) * | 2013-09-23 | 2015-07-28 | Soonchunyang University Industry Academy Cooperation Foundation | Method of manufacturing nanoparticles using ion exchange resin and liquid reducing process |
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| Publication number | Publication date |
|---|---|
| CN100406119C (en) | 2008-07-30 |
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| C06 | Publication | ||
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| C14 | Grant of patent or utility model | ||
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| EE01 | Entry into force of recordation of patent licensing contract |
Assignee: Beijing Mediking Pharmaceutical Group Co., Ltd. Assignor: BEIJING INSTITUTE OF TECHNOLOGY Contract fulfillment period: 2009.11.2 to 2014.11.2 Contract record no.: 2009990001264 Denomination of invention: Method for preparing nickel nanometer catalyst Granted publication date: 20080730 License type: Exclusive license Record date: 20091113 |
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| LIC | Patent licence contract for exploitation submitted for record |
Free format text: EXCLUSIVE LICENSE; TIME LIMIT OF IMPLEMENTING CONTACT: 2009.11.2 TO 2014.11.2; CHANGE OF CONTRACT Name of requester: BEIJING MEDIKING BIOPHARM CO.,LTD. Effective date: 20091113 |
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Granted publication date: 20080730 Termination date: 20110810 |