CN1861528A - Process for preparing nano NiO by ammonia water single phase precipitation - Google Patents
Process for preparing nano NiO by ammonia water single phase precipitation Download PDFInfo
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- CN1861528A CN1861528A CN 200510018697 CN200510018697A CN1861528A CN 1861528 A CN1861528 A CN 1861528A CN 200510018697 CN200510018697 CN 200510018697 CN 200510018697 A CN200510018697 A CN 200510018697A CN 1861528 A CN1861528 A CN 1861528A
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Abstract
A process for preparing nano-NiO from inorganic Ni salt and ammonia water by single-phase deposition in ammonia water includes such steps as preparing precursor by single-phase deposition, hydrothermal modifying at 105-150 deg.C under 0.02-0.3 MPa, filtering, washing and calcining at 300-800 deg.C for 1-5 hr.
Description
(1) technical field: the invention belongs to field of inorganic chemical engineering, be specifically related to the method that a kind of ammonia water single phase precipitation prepares nanometer Nio.
(2) background technology: nanometer powder is meant that particle size is the powdered material of 1-100nm.The special construction level of nano material makes it have surface effects, volume effect, quantum size effect and macro quanta tunnel effect etc., thereby have a series of novel physical, chemical property, comprising in the various fields of chemical industry having great application value.A large amount of interfaces is for example arranged in nano material, and these interfaces provide the short-range diffusion approach for atom, so nano material has higher activity and diffusivity, and performances such as chemical reaction, creep, superplasticity are had remarkable influence.The nanometer material for making clothes is made catalyzer because surfactivity is many, can improve speed of reaction greatly; In rubber, add nano material and can improve its wear resistance and dielectric characteristics; In plastics, add nano material and can improve its intensity and toughness.The nano-powder structured material can carry out sintering, doping, miscible at a lower temperature, forms advanced composite material.
Up to now the preparation method of the nanometer Nio that is reported has the preparation and the optical absorption spectra of the nano-nickel oxide micro mist that Wang Guozhong etc. delivers, Acta PhySico-Chimica Sinica, 1997,13 (5): 455-448, the preparation of nano level Nio and sign in the mixed solvent that Li Yadong etc. are delivered, SCI, 1997,18 (12): 1921-923; The homogeneous precipitation method that Tan Binyuan etc. deliver is produced the nano level nickel oxide, Qingtao Chemical Engineering College's journal, 1998,19 (2): 194-195; The homogeneous precipitation method that Gao Rongjie etc. deliver prepares Ni (OH)
2Nanocrystalline with Nio, Qingdao Marine University's journal (supplementary issue), but these methods or complicated operation, tooling cost are higher, otherwise raw material is more expensive, and difficult quality guarantee all is not easy to realize suitability for industrialized production.
(3) summary of the invention: it is simple, easy to operate, with low cost that purpose of the present invention just provides a kind of technology, is easy to realize that the ammonia water single phase precipitation of large-scale commercial production prepares the method for nanometer Nio.
Processing method of the present invention comprises the steps:
A. in 5-20% (W/V) ammonia soln, add the water soluble dispersing agent solution of 1-5% (W/V), stir evenly; Add 5-20% (W/V) inorganic nickel solution again, stirring reaction 1-5 hour; Make suspension; Wherein the volume ratio of ammonia soln and water soluble dispersing agent and inorganic nickel solution was respectively 1: 0.5: 1;
B. with reaction 1-4 hour in autoclave under 105-150 ℃, the condition of 0.02-0.3Mpa of prepared suspension in the above-mentioned steps, cold filtration; After filter cake washing, place 105 ℃ dry 4 hours down, again with dry thing at 300-800 ℃ of following roasting 1-5 hour, promptly get the Nio that particle diameter is 5-13mm.
Above-mentioned water soluble dispersing agent can be selected CH for use
3CH
2OH, (NaPO
3)
6Or AL
2(SO
4)
3In any.Inorganic nickel can be selected NiSO for use
4, NiCL
2Or Ni (NO
3)
2In any; The adding speed that inorganic nickel solution joins in ammoniacal liquor and the water soluble dispersing agent mixed solution is best with 5-20ml/min.
This technology compared with prior art has following characteristics:
1. be raw material with the inorganic nickel, ammoniacal liquor is precipitation agent, and normal temperature carries out precipitin reaction under the water soluble dispersing agent existence condition, promptly adopts liquid phase to disperse---hydrothermal modification---technologies such as medium temperature roast to guarantee the granularity and the polymolecularity of Nio product;
2. raw material of the present invention is all cheap and easy to get, and required equipment also mostly is conventional chemical industry standard equipment, and technology is simple, and is easy to operate, is easy to suitability for industrialized production.
(4) description of drawings:
Fig. 1 is a process flow diagram of the present invention;
Fig. 2 is that the obtained particle diameter of technology of the present invention is the transmission electron microscope shape appearance figure of 8-11nm Nio;
Fig. 3 is that the obtained particle diameter of technology of the present invention is the transmission electron microscope shape appearance figure of 6-10nm Nio.
(5) embodiment:
Embodiment 1, adds (the NaPO of 1% (W/V) in the ammonia soln 100ml of 5% (W/V)
3)
6Solution 50ml, the limit edged stirs, general (NaPO
3)
6The adding rate-controlling of solution is about 10ml/min; The NiCL that adds 5% (W/V) then while stirring
2Solution 100ml adds rate-controlling about 5ml/min; After adding finishes, continued stirring reaction 2 hours; Prepared suspension is carried out hydrothermal modification handled cold filtration 2 hours under 150 ℃, the condition of 0.3Mpa in autoclave; Respectively with deionized water and 95% washing with alcohol filter cake 3 times, under air atmosphere,, drier thing is placed in the retort furnace 800 ℃ of following roastings 1 hour in 105 ℃ of dryings 4 hours, promptly obtain the Nio that particle diameter is 8-13nm.
Embodiment 2, add the CH of 5% (W/V) in the ammonia soln 100ml of 10% (W/V)
3CH
2OH solution 50ml, the limit edged stirs, general CH
3CH
2The adding rate-controlling of OH solution is about 10ml/min; Ni (the NO that adds 20% (W/V) then while stirring
3)
2Solution 100ml adds rate-controlling about 20ml/min; After adding finishes, continued stirring reaction 1 hour; Prepared suspension is carried out hydrothermal modification handled cold filtration 1 hour under 105 ℃, the condition of 0.02Mpa (gauge pressure) in autoclave; Respectively with deionized water and 5% washing with alcohol filter cake 3 times, under air atmosphere,, drier thing is placed in the retort furnace 400 ℃ of following roastings 2 hours in 105 ℃ of dryings 4 hours, promptly obtain the Nio that particle diameter is 5-9nm.
Embodiment 3, add the AL of 3% (W/V) in the ammonia soln 100ml of 20% (W/V)
2(SO
4)
3Solution 50ml, the limit edged stirs, general AL
2(SO
4)
3The adding rate-controlling of solution is about 10ml/min; The NiSO that adds 10% (W/V) then while stirring
4Solution 100ml adds rate-controlling about 10ml/min; After adding finishes, continued stirring reaction 5 hours; Prepared suspension is carried out hydrothermal modification handled cold filtration 4 hours under 120 ℃, the condition of 0.09Mpa (gauge pressure) in autoclave; Respectively with deionized water and 95% washing with alcohol filter cake 3 times, under air atmosphere,, drier thing is placed in the retort furnace 300 ℃ of following roastings 5 hours in 105 ℃ of dryings 4 hours, promptly obtain the Nio that particle diameter is 6-10nm.
Claims (4)
1. ammonia water single phase precipitation prepares the method for nanometer Nio, it is characterized in that comprising the steps:
A. in 5-20% (W/V) ammonia soln, add the water soluble dispersing agent solution of 1-5% (W/V), stir evenly; Add 5-20% (W/V) inorganic nickel solution again, stirring reaction 1-5 hour; Make suspension; Wherein the volume ratio of ammonia soln and water soluble dispersing agent and inorganic nickel solution was respectively 1: 0.5: 1;
B. with reaction 1-4 hour in autoclave under 105-150 ℃, the condition of 0.02-0.3Mpa of prepared suspension in the above-mentioned steps, cold filtration; After filter cake washing, place 105 ℃ dry 4 hours down, again with dry thing at 300-800 ℃ of following roasting 1-5 hour, promptly get the Nio that particle diameter is 5-13mm.
2. ammonia water single phase precipitation according to claim 1 prepares the method for nanometer Nio, it is characterized in that: described water soluble dispersing agent can be selected CH for use
3CH
2OH, (NaPO
3)
6Or AL
2(SO
4)
3In any.
3. ammonia water single phase precipitation according to claim 1 and 2 prepares the method for nanometer Nio, it is characterized in that: described inorganic nickel can be selected NiSO for use
4, NiCL
2Or Ni (NO
3)
2In any.
4. ammonia water single phase precipitation according to claim 1 prepares the method for nanometer Nio, it is characterized in that: the speed that inorganic nickel solution joins in ammoniacal liquor and the water soluble dispersing agent mixed solution preferably is controlled at 5-20ml/min.
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|---|---|---|---|
| CNB2005100186976A CN100532277C (en) | 2005-05-13 | 2005-05-13 | Process for preparing nano NiO by ammonia water single phase precipitation |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2005100186976A CN100532277C (en) | 2005-05-13 | 2005-05-13 | Process for preparing nano NiO by ammonia water single phase precipitation |
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|---|---|
| CN1861528A true CN1861528A (en) | 2006-11-15 |
| CN100532277C CN100532277C (en) | 2009-08-26 |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101428348B (en) * | 2008-07-29 | 2010-09-08 | 张建玲 | Process for producing spherical submicron metal with hydro-thermal treatment |
| CN102020321A (en) * | 2011-01-13 | 2011-04-20 | 中南大学 | Method for preparing nickel protoxide powder with self-assembled nano structure |
| CN106865628A (en) * | 2017-03-10 | 2017-06-20 | 长春理工大学 | One kind is used for room temperature H2S gas sensing materials nickel oxide and preparation method thereof |
| CN106882844A (en) * | 2015-12-15 | 2017-06-23 | 中国科学院大连化学物理研究所 | Core shell structure NiO/Ni3The preparation method of N materials |
-
2005
- 2005-05-13 CN CNB2005100186976A patent/CN100532277C/en not_active Expired - Fee Related
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101428348B (en) * | 2008-07-29 | 2010-09-08 | 张建玲 | Process for producing spherical submicron metal with hydro-thermal treatment |
| CN102020321A (en) * | 2011-01-13 | 2011-04-20 | 中南大学 | Method for preparing nickel protoxide powder with self-assembled nano structure |
| CN102020321B (en) * | 2011-01-13 | 2012-05-30 | 中南大学 | Method for preparing nickel protoxide powder with self-assembled nano structure |
| CN106882844A (en) * | 2015-12-15 | 2017-06-23 | 中国科学院大连化学物理研究所 | Core shell structure NiO/Ni3The preparation method of N materials |
| CN106882844B (en) * | 2015-12-15 | 2018-06-19 | 中国科学院大连化学物理研究所 | Nucleocapsid NiO/Ni3The preparation method of N materials |
| CN106865628A (en) * | 2017-03-10 | 2017-06-20 | 长春理工大学 | One kind is used for room temperature H2S gas sensing materials nickel oxide and preparation method thereof |
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| Publication number | Publication date |
|---|---|
| CN100532277C (en) | 2009-08-26 |
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Assignee: Saifu Friction Material Co., Ltd., Huangshi Assignor: Huangshi Institute of Technology Contract record no.: 2011420000051 Denomination of invention: Process for preparing nano NiO by ammonia water single phase precipitation Granted publication date: 20090826 License type: Exclusive License Open date: 20061115 Record date: 20110412 |
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Granted publication date: 20090826 Termination date: 20110513 |