CN107892336A - A kind of preparation method of nickel oxide microballoon - Google Patents
A kind of preparation method of nickel oxide microballoon Download PDFInfo
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- CN107892336A CN107892336A CN201711380520.XA CN201711380520A CN107892336A CN 107892336 A CN107892336 A CN 107892336A CN 201711380520 A CN201711380520 A CN 201711380520A CN 107892336 A CN107892336 A CN 107892336A
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- nickel oxide
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- oxide microballoon
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G53/00—Compounds of nickel
- C01G53/04—Oxides; Hydroxides
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/30—Particle morphology extending in three dimensions
- C01P2004/32—Spheres
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
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- Inorganic Chemistry (AREA)
- Manufacturing Of Micro-Capsules (AREA)
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- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The present invention discloses a kind of preparation method of nickel oxide microballoon, comprises the following steps：(1) it is 1.5~2 by mol ratio：1 Nickelous nitrate hexahydrate and Pyromellitic Acid is dissolved in solvent, at room temperature magnetic agitation 30min；(2) step (1) resulting solution is transferred in reactor, 12~24h is reacted at 100~150 DEG C, reaction solution is then cooled to room temperature；(3) powder that obtains reactor bottom is scrubbed, is calcined after vacuum drying, obtains nickel oxide microballoon.The present invention is based on solvent-thermal method, first Pyromellitic Acid is coordinated under the conditions of solvent thermal reaction with Nickelous nitrate hexahydrate, prepare the presoma of microspheroidal metal organic complex, then high temperature thermal decomposition method is passed through again, in Muffle furnace with certain temperature calcination for a period of time, the organic frame in metal organic complex is removed, roasting obtains the nickel oxide of micro-sphere structure later, realizes the simple preparation to NiO micro-sphere structures.
Description
Technical field
The present invention relates to a kind of preparation method of nickel oxide microballoon, belong to technical field of inorganic nanometer material.
Background technology
Nickel oxide (NiO) has stable and wide energy band, and it is considered as a kind of typical transition metal oxide
It is a kind of p-type semiconductor material of great application prospect.Due to NiO show in electricity, magnetics and catalysis etc. it is excellent
Different property, it is widely used in each field such as fuel cell, catalyst, gas sensor, active fibre, electroplated film disk,
It is a kind of very promising inorganic functional material.A however, important influence in the physical and chemical performance of material
Factor is exactly the microscopic appearance of material.In recent years, its physical and chemical performance is lifted always by controlling the microscopic appearance of material
Receive much concern, people have carried out the largely research on synthesizing labyrinth.
At present, the method for the NiO on preparing specific structure emerges in an endless stream, including solid phase method, vapor phase method etc..Wherein, Gu
Phase method has the advantages that cost is low, solvent-free, selectivity is strong, high income, preparation technology are simple, easily-controlled reaction conditions, still
But also there is the shortcomings of energy consumption is big, efficiency is low, product cut size is not fine enough and particle easily aoxidizes deformation；Vapor phase method is prepared and received
Rice nickel oxide powder mainly uses spray heating decomposition, and this method has the advantages that efficiently quick, high income, but droplet is fast
Speed evaporation and the quick release of decomposition gas so that the control to solids structure and morphology is relatively difficult.
The content of the invention
Goal of the invention：The present invention is for problem existing for existing oxidation method for preparing nickel, there is provided a kind of nickel oxide microballoon
Preparation method, this method can simply realize the controllable preparation of nickel oxide material structure.
Technical scheme：A kind of preparation method of nickel oxide microballoon of the present invention, comprises the following steps：
(1) it is 1.5~2 by mol ratio：1 Nickelous nitrate hexahydrate and Pyromellitic Acid is dissolved in solvent, at room temperature magnetic force
Stir 30min；
(2) step (1) resulting solution is transferred in reactor, 12~24h is reacted at 100~150 DEG C, then will be anti-
Liquid is answered to be cooled to room temperature；
(3) powder that obtains reactor bottom is scrubbed, is calcined after vacuum drying, obtains nickel oxide microballoon.
In above-mentioned steps (1), solvent is preferably absolute methanol；It is preferred that in every 50~80ml solvents, the six of 1.274g is added
Nitric hydrate nickel.
In above-mentioned steps (3), the powder for preferably obtaining reactor bottom uses ethanol and distills water washing 2~3 times respectively.
After washing, vacuum drying condition is preferably：Vacuum drying temperature is 60 DEG C, and the vacuum drying time is 12h.
Further, roasting described in step (3) is that the powder after vacuum drying is placed in Muffle furnace, with 1~10
DEG C/min speed makes Muffle furnace be warming up to 400~600 DEG C, 1~5h is calcined at such a temperature, obtains nickel oxide microballoon.
Beneficial effect：Compared with prior art, remarkable advantage of the invention is：The present invention based on solvent-thermal method,
First Pyromellitic Acid is coordinated under the conditions of solvent thermal reaction with Nickelous nitrate hexahydrate, prepares microspheroidal metal organic complex
Presoma, then again by high temperature thermal decomposition method, removing metal has in Muffle furnace with certain temperature calcination for a period of time
Organic frame in machine complex, roasting obtain micro-sphere structure nickel oxide later, and the preparation method is simple and easy, gained nickel oxide
The Nomenclature Composition and Structure of Complexes of microballoon is easy to control, moreover, this method energy consumption is low, it is micro- to realize nickel oxide without special equipment or technological requirement
The simple and controllable preparation of ball.
Brief description of the drawings
Fig. 1 is that Pyromellitic Acid and Nickelous nitrate hexahydrate react obtained metal organic complex before being calcined in embodiment 1
SEM figure；
Fig. 2 is the SEM figures of the NiO microballoons obtained after the metal organic complex in embodiment 1 is calcined；
Fig. 3 is the XRD of the NiO microballoons in Fig. 2.
Embodiment
Technical scheme is described further below in conjunction with the accompanying drawings.
Embodiment 1
(1) 1.274g Nickelous nitrate hexahydrates and 0.620g Pyromellitic Acids are dissolved in 70mL absolute ethyl alcohols, at room temperature magnetic
Power stirs 30min；
(2) step (1) resulting solution is transferred in 100mL ptfe autoclaves, reacts 24h at 150 DEG C；
(3) treat that reaction solution is cooled to room temperature in step (2), the fruit green powder that bottom is obtained uses ethanol and distillation respectively
Water washing 2~3 times, 60 DEG C of vacuum drying 12h, obtained sample structure such as Fig. 1；Gained sample is put into ceramic crucible and is placed in
In Muffle furnace, from being warming up to 400 DEG C at room temperature with 1 DEG C/min heating rates, and 4h is kept at 400 DEG C, it is cold to treat that roasting finishes
But to room temperature, that is, NiO microballoons are obtained, its structure and XRD spectrum such as Fig. 2~3.
Embodiment 2
(1) 1.274g Nickelous nitrate hexahydrates and 0.745g Pyromellitic Acids are dissolved in 50mL absolute ethyl alcohols, at room temperature magnetic
Power stirs 30min；
(2) step (1) resulting solution is transferred in 100mL ptfe autoclaves, reacts 12h at 100 DEG C；
(3) treat that reaction solution is cooled to room temperature in step (2), the fruit green powder that bottom is obtained uses ethanol and distillation respectively
Water washing 2~3 times, 60 DEG C of vacuum drying 12h, gained sample, which is put into ceramic crucible, to be placed in Muffle furnace, from room temperature with 1
DEG C/min heating rates are warming up to 400 DEG C, and keep 2h at 400 DEG C, treat that roasting finishes and be cooled to room temperature, obtain NiO microballoons,
Its appearance structure is close with the NiO microballoons of the gained of embodiment 1.
Embodiment 3
(1) 1.274g Nickelous nitrate hexahydrates and 0.699g Pyromellitic Acids are dissolved in 60mL absolute ethyl alcohols, at room temperature magnetic
Power stirs 30min；
(2) step (1) resulting solution is transferred in 100mL ptfe autoclaves, reacts 12h at 100 DEG C；
(3) treat that reaction solution is cooled to room temperature in step (2), the fruit green powder that bottom is obtained uses ethanol and distillation respectively
Water washing 2~3 times, 60 DEG C of vacuum drying 12h, gained sample, which is put into ceramic crucible, to be placed in Muffle furnace, from room temperature with 2.5
DEG C/min heating rates are warming up to 450 DEG C, and keep 2h at 450 DEG C, treat that roasting finishes and be cooled to room temperature, obtain NiO microballoons,
Its appearance structure is close with the NiO microballoons of the gained of embodiment 1.
Embodiment 4
(1) 1.274g Nickelous nitrate hexahydrates and 0.658g Pyromellitic Acids are dissolved in 65mL absolute ethyl alcohols, at room temperature magnetic
Power stirs 30min；
(2) step (1) resulting solution is transferred in 100mL ptfe autoclaves, reacts 18h at 125 DEG C；
(3) treat that reaction solution is cooled to room temperature in step (2), the fruit green powder that bottom is obtained uses ethanol and distillation respectively
Water washing 2~3 times, 60 DEG C of vacuum drying 12h, gained sample, which is put into ceramic crucible, to be placed in Muffle furnace, from room temperature with 5
DEG C/min heating rates are warming up to 500 DEG C, and keep 3h at 500 DEG C, treat that roasting finishes and be cooled to room temperature, that is, it is micro- to obtain NiO
Ball, its appearance structure are close with the NiO microballoons of the gained of embodiment 1.
Embodiment 5
(1) 1.274g Nickelous nitrate hexahydrates and 0.559g Pyromellitic Acids are dissolved in 80mL absolute ethyl alcohols, at room temperature magnetic
Power stirs 30min；
(2) step (1) resulting solution is transferred in 100mL ptfe autoclaves, reacts 24h at 150 DEG C；
(3) treat that reaction solution is cooled to room temperature in step (2), the fruit green powder that bottom is obtained uses ethanol and distillation respectively
Water washing 2~3 times, 60 DEG C of vacuum drying 12h, gained sample, which is put into ceramic crucible, to be placed in Muffle furnace, from room temperature with 10
DEG C/min heating rates are warming up to 600 DEG C, and keep 5h at 600 DEG C, treat that roasting finishes and be cooled to room temperature, that is, it is micro- to obtain NiO
Ball, its appearance structure are close with the NiO microballoons of the gained of embodiment 1.
Claims (5)
1. a kind of preparation method of nickel oxide microballoon, it is characterised in that comprise the following steps：
(1) by Nickelous nitrate hexahydrate and Pyromellitic Acid with 1.5~2：1 mol ratio is dissolved in solvent, at room temperature magnetic agitation
30min；
(2) step (1) resulting solution is transferred in reactor, 12~24h is reacted at 100~150 DEG C, then by reaction solution
It is cooled to room temperature；
(3) powder that obtains reactor bottom is scrubbed, is calcined after vacuum drying, obtains nickel oxide microballoon.
2. the preparation method of nickel oxide microballoon according to claim 1, it is characterised in that in step (1), the solvent is
Absolute methanol, in every 50~80ml solvents, the quality of the Nickelous nitrate hexahydrate of addition is 1.274mg.
3. the preparation method of nickel oxide microballoon according to claim 1, it is characterised in that in step (3), by reactor bottom
The powder that portion obtains with ethanol and distills water washing 2~3 times respectively.
4. the preparation method of nickel oxide microballoon according to claim 1, it is characterised in that in step (3), the vacuum is done
Dry temperature is 60 DEG C, and the vacuum drying time is 12h.
5. the preparation method of nickel oxide microballoon according to claim 1, it is characterised in that in step (3), the roasting is
Powder after vacuum drying is placed in Muffle furnace, Muffle furnace is warming up to 400~600 DEG C with 1~10 DEG C/min speed,
1~5h is calcined at this temperature, obtains nickel oxide microballoon.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| RU2700047C1 (en) * | 2019-01-10 | 2019-09-12 | Федеральное государственное бюджетное образовательное учреждение высшего образования "Ивановский государственный химико-технологический университет" | Nickel oxide production method |
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| CN101857604A (en) * | 2010-05-17 | 2010-10-13 | 天津师范大学 | Three-dimensional copper coordination polymer with hypoxanthine and pyromellitic benzoic acid mixed ligand and preparation method thereof |
| CN103483394A (en) * | 2013-09-17 | 2014-01-01 | 天津师范大学 | Organic complex with metal zinc as center body, preparation method thereof and application thereof |
| CN104844657A (en) * | 2015-04-09 | 2015-08-19 | 山西大学 | Manganese metal polymer and preparation method and application thereof |
| CN105854911A (en) * | 2016-06-23 | 2016-08-17 | 中国石油大学(华东) | Micron nickel phosphide electro-catalytic material used for hydrogen evolution/oxygen evolution double functions |
-
2017
- 2017-12-20 CN CN201711380520.XA patent/CN107892336A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101857604A (en) * | 2010-05-17 | 2010-10-13 | 天津师范大学 | Three-dimensional copper coordination polymer with hypoxanthine and pyromellitic benzoic acid mixed ligand and preparation method thereof |
| CN103483394A (en) * | 2013-09-17 | 2014-01-01 | 天津师范大学 | Organic complex with metal zinc as center body, preparation method thereof and application thereof |
| CN104844657A (en) * | 2015-04-09 | 2015-08-19 | 山西大学 | Manganese metal polymer and preparation method and application thereof |
| CN105854911A (en) * | 2016-06-23 | 2016-08-17 | 中国石油大学(华东) | Micron nickel phosphide electro-catalytic material used for hydrogen evolution/oxygen evolution double functions |
Non-Patent Citations (3)
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| 王娟: "羧酸类金属配合物的合成、晶体结构及性质", 《中国优秀硕士学位论文全文数据库 工程科技Ⅰ辑》 * |
| 王梦娅: "稀土羧酸配位聚合物复杂纳米结构的合成、表征及其性能研究", 《中国优秀硕士学位论文全文数据库 工程科技Ⅰ辑》 * |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| RU2700047C1 (en) * | 2019-01-10 | 2019-09-12 | Федеральное государственное бюджетное образовательное учреждение высшего образования "Ивановский государственный химико-технологический университет" | Nickel oxide production method |
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