阅读说明：本技术 一种微米级氧化亚镍的制备方法 (Preparation method of micron-sized nickel protoxide ) 是由 衣淑立 陈大林 刘世和 丁勇 刘爱春 李芬霞 陈兴纲 马婷 于 2021-08-25 设计创作，主要内容包括：一种微米级氧化亚镍的制备方法,包括以下步骤,步骤1：称取一定量的羰基镍粉置于方形刚玉匣钵,放入箱式保护气氛电阻炉中；步骤2：打开空压机电源,然后把压缩气体通入箱式保护气氛电阻内；步骤3：打开箱式保护气氛电阻炉电源；步骤4：在步骤3焙烧完毕后,箱式保护气氛电阻炉的炉温自然冷却下降到100℃以下,打开炉门取出刚玉匣钵,制备得到氧化亚镍；步骤5：将步骤4制备的氧化亚镍放置于球磨罐中,采用氧化锆研磨球铺满球磨罐底部,球磨后即得到微米级氧化亚镍。该方法以羰基镍粉为原料,采用焙烧制备得到氧化亚镍,在通过球磨处理将氧化亚镍破碎成微米颗粒,其具有工艺简单、过程可控、环境友好、无温室气体排放的优点。(A preparation method of micron-sized nickel protoxide comprises the following steps of 1: weighing a certain amount of carbonyl nickel powder, placing the carbonyl nickel powder in a square corundum sagger, and placing the sagger in a box-type protective atmosphere resistance furnace; step 2: turning on a power supply of an air compressor, and introducing compressed gas into the box type protective atmosphere resistor; and step 3: opening a power supply of the box type protective atmosphere resistance furnace; and 4, step 4: after the roasting in the step 3 is finished, naturally cooling the furnace temperature of the box type protective atmosphere resistance furnace to be lower than 100 ℃, opening the furnace door and taking out the corundum sagger to prepare nickel protoxide; and 5: and (4) placing the nickel protoxide prepared in the step (4) into a ball milling tank, adopting zirconia grinding balls to fully cover the bottom of the ball milling tank, and carrying out ball milling to obtain the micron-sized nickel protoxide. The method takes carbonyl nickel powder as a raw material, the nickel protoxide is prepared by roasting, and the nickel protoxide is crushed into micron particles by ball milling treatment, so that the method has the advantages of simple process, controllable process, environmental friendliness and no greenhouse gas emission.)

1. A preparation method of micron-sized nickel protoxide is characterized by comprising the following steps:

step 1: weighing a certain amount of carbonyl nickel powder, placing the carbonyl nickel powder in a square corundum sagger, placing the square corundum sagger in a box type protective atmosphere resistance furnace, and closing a furnace door;

step 2: turning on a power supply of an air compressor, setting the flow of compressed gas to be 10-50L/min, and then introducing the compressed gas into a box-type protective atmosphere resistor;

and step 3: opening a power supply of the box type protective atmosphere resistance furnace, setting the roasting temperature to be 1000-1200 ℃, and keeping the roasting temperature for 1-3 h;

and 4, step 4: after the roasting in the step 3 is finished, naturally cooling the furnace temperature of the box type protective atmosphere resistance furnace to be lower than 100 ℃, opening the furnace door and taking out the corundum sagger to prepare nickel protoxide;

and 5: and (4) placing the nickel protoxide prepared in the step (4) into a ball milling tank, paving zirconium oxide grinding balls at the bottom of the ball milling tank, wherein the ball milling time is 1-3 hours, the frequency of the ball milling tank is 20-25 Hz, and obtaining the micron-sized nickel protoxide after ball milling.

2. The method for preparing micron-sized nickel protoxide according to claim 1, wherein: in step 2, the flow rate of the compressed gas was set to 40L/min.

3. The method for preparing micron-sized nickel protoxide according to claim 1, wherein: in the step 3, the roasting temperature is set to be 1100 ℃, and the roasting heat preservation time is 2 hours.

4. The method for preparing micron-sized nickel protoxide according to claim 1, wherein: the ball milling time of the step 5 is 2 hours, and the frequency of the ball mill is 22 Hz.

5. The method for preparing micron-sized nickel protoxide according to claim 1, wherein: and 5, grinding balls in the ball milling treatment process in the step 5 are zirconia grinding balls, and the zirconia grinding balls respectively have three diameters of 1cm, 0.8cm and 0.5 cm.

Technical Field

The invention belongs to the technical field of inorganic functional materials, and particularly relates to a preparation method of micron-sized nickel protoxide.

Background

Nickel protoxide (NiO) is an important inorganic functional material, widely used in the fields of catalysts, battery cathodes, gas sensors, electrochromic films, magnetic materials and the like, and is also a raw material for manufacturing nickel salts and nickel catalysts. Heating nickel protoxide at low temperature to obtain nickel oxide (Ni) by absorbing oxygen in air₂O₃) Heating the nickel oxide to 400-500 deg.C to decompose and produce nickel (Ni) oxide₃O₄) And the nickel oxide is decomposed by raising the temperature by one step. If the nickel powder is directly oxidized and roasted, nickel protoxide can also be prepared, but the nickel powder is generally piled up, most of the nickel powder cannot be contacted with oxygen in the oxidizing and roasting process, only a thin layer on the surface of the nickel powder can be contacted with the oxygen and reacts, and the method is not suitable for production with more demand. Filtering, washing and drying the precipitated nickel carbonate, and then feeding the nickel carbonate into a calcining furnace for calcining to obtain a target product nickel protoxide; however, in the calcination process, greenhouse gases such as carbon dioxide are emitted, which poses a serious threat to the ecological environment in which human beings depend for survival.

Disclosure of Invention

The invention aims to solve the technical problem of providing a preparation method of micron-sized nickel protoxide, which has the advantages of simple process, controllable process, environmental protection and no emission of greenhouse gases.

In order to solve the problems, the preparation method of micron-sized nickel protoxide is characterized by comprising the following steps of:

step 1: weighing a certain amount of carbonyl nickel powder, placing the carbonyl nickel powder in a square corundum sagger, placing the square corundum sagger in a box type protective atmosphere resistance furnace, and closing a furnace door;

step 2: turning on a power supply of an air compressor, setting the flow of compressed gas to be 10-50L/min, and then introducing the compressed gas into a box-type protective atmosphere resistor;

and step 3: opening a power supply of the box type protective atmosphere resistance furnace, setting the roasting temperature to be 1000-1200 ℃, and keeping the roasting temperature for 1-3 h;

and 4, step 4: after the roasting in the step 3 is finished, naturally cooling the furnace temperature of the box type protective atmosphere resistance furnace to be lower than 100 ℃, opening the furnace door and taking out the corundum sagger to prepare nickel protoxide;

and 5: and (4) placing the nickel protoxide prepared in the step (4) into a ball milling tank, paving zirconium oxide grinding balls at the bottom of the ball milling tank, wherein the ball milling time is 1-3 hours, the frequency of the ball milling tank is 20-25 Hz, and obtaining the micron-sized nickel protoxide after ball milling.

The further technical scheme is as follows: in step 2, the flow rate of the compressed gas was set to 40L/min.

The further technical scheme is as follows: in the step 3, the roasting temperature is set to be 1100 ℃, and the roasting heat preservation time is 2 hours.

The further technical scheme is as follows: the ball milling time of the step 5 is 2 hours, and the frequency of the ball mill is 22 Hz.

The further technical scheme is as follows: and 5, grinding balls in the ball milling treatment process in the step 5 are zirconia grinding balls, and the zirconia grinding balls respectively have three diameters of 1cm, 0.8cm and 0.5 cm.

In summary, due to the adoption of the technical scheme, the invention has the beneficial effects that: the method takes carbonyl nickel powder as a raw material, the nickel protoxide is prepared by roasting, and the nickel protoxide is crushed into micron particles by ball milling treatment, so that the method has the advantages of simple process, controllable process, environmental friendliness and no greenhouse gas emission. The invention solves the problem that most of nickel powder can not contact with oxygen and only a thin layer on the surface of the nickel powder can contact with the oxygen and react in the oxidizing roasting process, thereby being suitable for large-scale production.

Detailed Description

A preparation method of micron-sized nickel protoxide comprises the following steps: step 1: weighing a certain amount of carbonyl nickel powder, placing the carbonyl nickel powder in a square corundum sagger, placing the square corundum sagger in a box type protective atmosphere resistance furnace, and closing a furnace door; step 2: turning on a power supply of an air compressor, setting the flow of compressed gas to be 10-50L/min, and then introducing the compressed gas into a box-type protective atmosphere resistor; and step 3: opening a power supply of the box type protective atmosphere resistance furnace, setting the roasting temperature to be 1000-1200 ℃, and keeping the roasting temperature for 1-3 h; and 4, step 4: after the roasting in the step 3 is finished, naturally cooling the furnace temperature of the box type protective atmosphere resistance furnace to be lower than 100 ℃, opening the furnace door and taking out the corundum sagger to prepare nickel protoxide; and 5: and (4) placing the nickel protoxide prepared in the step (4) into a ball milling tank, paving zirconium oxide grinding balls at the bottom of the ball milling tank, wherein the ball milling time is 1-3 hours, the frequency of the ball milling tank is 20-25 Hz, and obtaining the micron-sized nickel protoxide after ball milling. The micron-sized nickel protoxide particles prepared by the method have the particle size of 0.3-50 μm, good particle size uniformity and high crystallinity; the nickel carbonyl powder was sprayed on the magnetic carrier by compressed air. Can ensure that the carbonyl nickel powder is uniformly adsorbed on the magnetic carrier, and can separate some nonmetallic impurities because the impurities can not be adsorbed by the magnetic carrier. The compressed gas is compressed air or compressed oxygen

In step 2, the flow rate of the compressed gas was set to 40L/min. In the step 3, the roasting temperature is set to be 1100 ℃, and the roasting heat preservation time is 2 hours. The ball milling time of the step 5 is 2 hours, and the frequency of the ball mill is 22 Hz. And 5, grinding balls in the ball milling treatment process in the step 5 are zirconia grinding balls, and the zirconia grinding balls respectively have three diameters of 1cm, 0.8cm and 0.5 cm. The carbonyl nickel powder is subjected to ball milling treatment, and can be further crushed, so that the particle diameter of the carbonyl nickel powder is smaller, and the carbonyl nickel powder can react with oxygen more easily; the carbonyl nickel powder is uniformly adsorbed on the magnetic carrier, and the material receiving box is arranged below the magnetic carrier, so that the carbonyl nickel powder can be uniformly distributed; the invention solves the problem that most of nickel powder can not contact with oxygen and only a thin layer on the surface of the nickel powder can contact with the oxygen and react in the oxidizing roasting process, thereby being suitable for large-scale production.