CN101367556A - Method for preparing nickelous oxide with microwave mode - Google Patents
Method for preparing nickelous oxide with microwave mode Download PDFInfo
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- CN101367556A CN101367556A CNA2008100685592A CN200810068559A CN101367556A CN 101367556 A CN101367556 A CN 101367556A CN A2008100685592 A CNA2008100685592 A CN A2008100685592A CN 200810068559 A CN200810068559 A CN 200810068559A CN 101367556 A CN101367556 A CN 101367556A
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Abstract
The invention relates to a method for preparing the nickel oxide in micro-wave way, in particular relates to a method for preparing the nickel oxide, which comprises the following steps: (1) the following raw materials are obtained at the weight rate: 100 nickel hydroxide, and 1 to 10 metal-doped compound; (2) all raw materials in step (1) are uniformly mixed; (3) the mixture in step (2) is arranged inside a corundum crucible, and powdered carbon is taken to be arranged inside a ceramic vessel, and the corundum crucible is arranged inside the ceramic vessel, so that the powdered carbon surrounds the corundum crucible, and the corundum crucible is covered with a cover, and the surface of the cover is attached with powdered carbon; (4) the reaction system of the ceramic vessel is moved into a micro-wave oven, and is reacted for 1 to 10 minutes under the effect of the micro wave, and the frequency of the micro wave is 2450 MHz and the power is 160 W to 800 W; (5) after the reaction is ended, the reaction system is taken out of the ceramic vessel to be kept static and be cooled down to the room temperature, and is ground by an agate mortar and is filtered by a 300-mesh sieve to get the black product of nickel oxide. The method is used for preparing the nickel oxide.
Description
Technical field
The present invention relates to a kind of preparation method of nickel oxide, particularly relate to a kind of method of preparing nickelous oxide with microwave mode.
Background technology
In recent years, along with people's deepening continuously to nano ZnO and related preparation technical study, hyperfine structure with special appearance and function often shows excellent characteristic at aspects such as chemistry, mechanics, optics, electricity and magnetics, these hyperfine structures are expected to be widely used in military and civilian fields such as chemical industry, electronics, metallurgy, aviation, medicine.Particularly nano-nickel oxide has excellent characteristic aspect electrochemical capacitor, is expected to be widely used at the electrochemical capacitor production field.
The method for preparing nickel oxide of prior art adopts high temperature solid-state method mostly, promptly reacts certain hour at a certain temperature and prepare nickel oxide in retort furnace.Adopt high temperature solid-state method to prepare nickel oxide, the major defect of this method is that long reaction time, consumes energy are many, and production efficiency is lower, have pollution, product purity not high to environment, and reaction product does not reach nano level.
Summary of the invention
Technical problem to be solved by this invention is, overcome the long reaction time of the method existence for preparing nickel oxide of prior art, the defective that consumes energy is many, a kind of method of preparing nickelous oxide with microwave mode is provided, with this energy apply of microwave in the preparation of nickel oxide, this method have the reaction times short, production efficiency is high, consumed energy is few, environmentally safe, characteristics that product purity is high, reaction product particle is little, all can reach nano level, can significantly reduce the consumption of reaction times and energy.
The technical solution adopted for the present invention to solve the technical problems is: the method for preparing nickelous oxide with microwave mode is characterized in that comprising following concrete steps:
(1), get following raw materials by weight:
Nickel hydroxide 100;
The compound 1～10 of doping metals;
(2), each raw material in the step (1) is mixed;
(3), the mixture in the step (2) is put into corundum crucible, get carbon dust and put into earthenware porcelain receptacle, corundum crucible is placed earthenware porcelain receptacle, carbon dust is enclosed in around the corundum crucible, cover lid, and the lid surface attached carbon dust that looses;
(4), the reaction system of earthenware porcelain receptacle is moved in the microwave oven, reaction is 1 minute～10 minutes under microwave action, microwave frequency 2450MHz, power 160W～800W;
(5), after reaction finishes, the reaction system of taking out earthenware porcelain receptacle leaves standstill and is cooled to room temperature, grinds 300 mesh sieve with agate mortar, obtains black product nickel oxide.
In technique scheme, the preparation method of nickel hydroxide is a kind of in ball milling solid phase method, homogeneous precipitation method, the hydrothermal synthesis method.
The compound of doping metals is selected from one or more in hydrochloride, nitrate, vitriol or the metal oxide.
Doping metals is selected from one or more in aluminium, cobalt, chromium, iron, tin, vanadium, the tantalum.
The invention has the beneficial effects as follows: the method for preparing nickel oxide with the employing high temperature solid-state method of prior art is compared, the present invention have the reaction times short, production efficiency is high, consumed energy is few, environmentally safe, characteristics that product purity is high, reaction product particle is little, all can reach nano level, especially can significantly reduce the consumption of reaction times and energy; Difference on function is that the high-energy rapid heating of applied microwave, the principle of moment reaction prepare nano-nickel oxide, the nickel oxide better crystallinity degree of preparing, purity height; The nickel oxide that the nano-nickel oxide and the high temperature solid-state method of microwave method preparation are prepared is applied to the electrochemical capacitor aspect, and its volumetric properties and cycle performance be basically identical all; Be that specific storage is respectively 10.96mAh/g and 10.24mAh/g under the condition of 200mA/g in current density, 100 times circulation volume decays to 3.96% and 4.52%.The particle size of the nickel oxide of microwave method preparation is between 40-50nm; Principle of the present invention is that carbon material can absorb microwave, heat-up rate is fast, the corundum crucible that nickel hydroxide is housed is placed on the centre of raw material of wood-charcoal material, intensification by the raw material of wood-charcoal material adds 1 heat to corundum crucible, moment reaches the temperature of reaction of nickel hydroxide, through 2 minutes reaction, obtains the nickel oxide product, thereby shortened the reaction times greatly, reduced the consumption of the energy; The present invention has the free of contamination characteristics of safety and environmental protection.
Embodiment
Embodiment 1, and the method for the described a kind of preparing nickelous oxide with microwave mode of present embodiment is characterized in that comprising following concrete steps:
(1), get following raw materials by weight:
Nickel hydroxide 100;
The compound 5 of doping metals;
(2), each raw material in the step (1) is mixed;
(3), the mixture in the step (2) is put into corundum crucible, get carbon dust and put into earthenware porcelain receptacle, corundum crucible is placed earthenware porcelain receptacle, carbon dust is enclosed in around the corundum crucible, cover lid, and the lid surface attached carbon dust that looses;
(4), the reaction system of earthenware porcelain receptacle is moved in the microwave oven, optimum reacting time is 2 minutes under microwave action, microwave frequency 2450MHz, optimum response power 640W;
(5), after reaction finishes, the reaction system of taking out earthenware porcelain receptacle leaves standstill and is cooled to room temperature, grinds 300 mesh sieve with agate mortar, obtains black product nickel oxide.
In technique scheme, the preparation method of nickel hydroxide is a kind of in ball milling solid phase method, homogeneous precipitation method, the hydrothermal synthesis method, and present embodiment adopts the ball milling solid phase method to prepare nickel hydroxide; The compound of doping metals is selected from one or more in hydrochloride, nitrate, vitriol or the metal oxide, and it is the compound of doping metals that present embodiment adopts hydrochloride; Doping metals is selected from one or more in aluminium, cobalt, chromium, iron, tin, vanadium, the tantalum, and it is doping metals that present embodiment adopts aluminium.Embodiment 1 is a most preferred embodiment.
Embodiment 2, and the method for the described a kind of preparing nickelous oxide with microwave mode of present embodiment is characterized in that comprising following concrete steps:
(1), get following raw materials by weight:
Nickel hydroxide 100;
The compound 10 of doping metals;
(2), each raw material in the step (1) is mixed;
(3), the mixture in the step (2) is put into corundum crucible, get carbon dust and put into earthenware porcelain receptacle, corundum crucible is placed earthenware porcelain receptacle, carbon dust is enclosed in around the corundum crucible, cover lid, and the lid surface attached carbon dust that looses;
(4), the reaction system of earthenware porcelain receptacle is moved in the microwave oven, reaction is 1 minute under microwave action, microwave frequency 2450MHz, power 800W;
(5), after reaction finishes, the reaction system of taking out earthenware porcelain receptacle leaves standstill and is cooled to room temperature, grinds 300 mesh sieve with agate mortar, obtains black product nickel oxide.
In technique scheme, the preparation method of nickel hydroxide is a kind of in ball milling solid phase method, homogeneous precipitation method, the hydrothermal synthesis method, and present embodiment adopts homogeneous precipitation method to prepare nickel hydroxide; The compound of doping metals is selected from one or more in hydrochloride, nitrate, vitriol or the metal oxide, and it is the compound of doping metals that present embodiment adopts nitrate; Doping metals is selected from one or more in aluminium, cobalt, chromium, iron, tin, vanadium, the tantalum, and it is doping metals that present embodiment adopts aluminium and iron.2 reaction times of embodiment are shorter.
Embodiment 3, and the method for the described a kind of preparing nickelous oxide with microwave mode of present embodiment is characterized in that comprising following concrete steps:
(1), get following raw materials by weight:
Nickel hydroxide 100;
The compound 1 of doping metals;
(2), each raw material in the step (1) is mixed;
(3), the mixture in the step (2) is put into corundum crucible, get carbon dust and put into earthenware porcelain receptacle, corundum crucible is placed earthenware porcelain receptacle, carbon dust is enclosed in around the corundum crucible, cover lid, and the lid surface attached carbon dust that looses;
(4), the reaction system of earthenware porcelain receptacle is moved in the microwave oven, reaction is 10 minutes under microwave action, microwave frequency 2450MHz, power 160W;
(5), after reaction finishes, the reaction system of taking out earthenware porcelain receptacle leaves standstill and is cooled to room temperature, grinds 300 mesh sieve with agate mortar, obtains black product nickel oxide.
In technique scheme, the preparation method of nickel hydroxide is a kind of in ball milling solid phase method, homogeneous precipitation method, the hydrothermal synthesis method, and present embodiment adopts hydrothermal synthesis method to prepare nickel hydroxide; The compound of doping metals is selected from one or more in hydrochloride, nitrate, vitriol or the metal oxide, and it is the compound of doping metals that present embodiment adopts vitriol; Doping metals is selected from one or more in aluminium, cobalt, chromium, iron, tin, vanadium, the tantalum, and it is doping metals that present embodiment adopts iron.3 reaction times of embodiment are longer.
The above only is three embodiment of the present invention; should be understood that; for the person of ordinary skill of the art; under the prerequisite that does not break away from principle of the present invention; can also make some improvement to the present invention; so all equivalences of doing according to the described method of patent claim of the present invention, feature and principle change or modify; for example; the umber of the compound of doping metals is 1～10; reaction is 1 minute～10 minutes under microwave action; power 160W～800W etc., these features belong to the scope of patent application protection of the present invention equally.
Claims (5)
1. the method for preparing nickelous oxide with microwave mode is characterized in that comprising following concrete steps:
(1), get following raw materials by weight:
Nickel hydroxide 100;
The compound 1～10 of doping metals;
(2), each raw material in the step (1) is mixed;
(3), the mixture in the step (2) is put into corundum crucible, get carbon dust and put into earthenware porcelain receptacle, corundum crucible is placed earthenware porcelain receptacle, carbon dust is enclosed in around the corundum crucible, cover lid, and the lid surface attached carbon dust that looses;
(4), the reaction system of earthenware porcelain receptacle is moved in the microwave oven, reaction is 1 minute～10 minutes under microwave action, microwave frequency 2450MHz, power 160W～800W;
(5), after reaction finishes, the reaction system of taking out earthenware porcelain receptacle leaves standstill and is cooled to room temperature, grinds 300 mesh sieve with agate mortar, obtains black product nickel oxide.
2. the method for preparing nickelous oxide with microwave mode according to claim 1 is characterized in that the reaction system of earthenware porcelain receptacle is moved in the microwave oven, and optimum reacting time is 2 minutes under microwave action, optimum response power 640W.
3. the method for preparing nickelous oxide with microwave mode according to claim 1, the preparation method who it is characterized in that nickel hydroxide are a kind of in ball milling solid phase method, homogeneous precipitation method, the hydrothermal synthesis method.
4. the method for preparing nickelous oxide with microwave mode according to claim 1, the compound that it is characterized in that doping metals is selected from one or more in hydrochloride, nitrate, vitriol or the metal oxide.
5. the method for preparing nickelous oxide with microwave mode according to claim 4 is characterized in that doping metals is selected from one or more in aluminium, cobalt, chromium, iron, tin, vanadium, the tantalum.
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| Application Number | Priority Date | Filing Date | Title |
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| CNA2008100685592A CN101367556A (en) | 2008-07-18 | 2008-07-18 | Method for preparing nickelous oxide with microwave mode |
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| CNA2008100685592A CN101367556A (en) | 2008-07-18 | 2008-07-18 | Method for preparing nickelous oxide with microwave mode |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115367799A (en) * | 2022-09-14 | 2022-11-22 | 贵州梅岭电源有限公司 | Method for preparing high-performance chromium oxide cathode material by microwave method |
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2008
- 2008-07-18 CN CNA2008100685592A patent/CN101367556A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115367799A (en) * | 2022-09-14 | 2022-11-22 | 贵州梅岭电源有限公司 | Method for preparing high-performance chromium oxide cathode material by microwave method |
| CN115367799B (en) * | 2022-09-14 | 2023-10-31 | 贵州梅岭电源有限公司 | Method for preparing high-performance chromium oxide positive electrode material by microwave method |
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