Preparing process of nano zinc oxide

A technology of nano-zinc oxide and sub-zinc oxide, which is applied in the fields of nanostructure manufacturing, zinc oxide/zinc hydroxide, nanotechnology, etc., can solve the problem that the final product zinc oxide particle size is difficult to control, the particle size increases, and the basic zinc carbonate crystal particle size unevenness etc.

Inactive Publication Date: 2007-06-27
CHINA NAT OFFSHORE OIL CORP +1
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Problems solved by technology

Since a large amount of water was added during hydrolysis, in order to promote the decomposition reaction to complete, the operation of heating the hydrolyzate requires a longer process, and the newly generated basic zinc carbonate will grow on the surface of the original crystal nucleus after heating and decomposition. Prompting the crystals produced in the previous hydrolysis process to continue to grow, it is easy to cause uneven or enlarged particle size of basic zinc carbonate crystals, making it difficult to control the particle size of the final product zinc oxide

Method used

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  • Preparing process of nano zinc oxide

Examples

Experimental program
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Effect test

Embodiment 1

[0024] A mixed solution of zinc oxide with a content of 80% in terms of ZnO, ammonia and ammonium bicarbonate, the ratio of which is Zn:NH 3 :CO 2 =1:4:0.9 (molar ratio), stirred and reacted at room temperature for 2 hours, filtered to remove insoluble impurities, and removed metal impurities such as iron, manganese and lead through redox to obtain a purified zinc ammonia complex solution. Pump the zinc ammonia complex solution and 98°C hot water continuously into the tubular reactor at the same time, control the flow rate ratio of hot water and zinc ammonia complex solution to 8, and continuously separate the alkali from the decomposition solution Formula zinc carbonate precipitates, and the mother liquor is heated to 98°C and circulated to the reactor. The isolated basic zinc carbonate was dried and calcined at 600° C. for 2 hours to obtain a zinc oxide product with a narrow particle size distribution. As determined by transmission electron microscope and XRD line broadeni...

Embodiment 2

[0026] The zinc ammonia complex solution was obtained in the same manner as in Example 1. Pump the zinc ammonia complex solution and 90°C hot water continuously into the tubular reactor at the same time, control the flow rate ratio of hot water and zinc ammonia complex solution to 20, and continuously separate the alkali from the decomposition solution Formula zinc carbonate precipitates, and the mother liquor is heated to 90°C and circulated to the reactor. The isolated basic zinc carbonate was dried and calcined at 600° C. for 2 hours to obtain a zinc oxide product with a narrow particle size distribution. As determined by transmission electron microscope and XRD line broadening method, the average particle size of zinc oxide is 10nm, and the BET specific surface area is 62m 2 / g.

Embodiment 3

[0028] A mixed solution of zinc calcine with a content of 72% in terms of ZnO, ammonia and ammonium bicarbonate, the ratio of which is Zn:NH 3 :CO 2 =1:4.5:1 (molar ratio), stirred and reacted at room temperature for 3 hours, filtered to remove insoluble impurities, and removed metal impurities such as iron, manganese and lead through redox to obtain a purified zinc ammonia complex solution. Pump the zinc-ammonia complex solution and 95°C hot water continuously into the tubular reactor at the same time, control the flow rate ratio of the hot water and the zinc-ammonia complex solution to 5, and continuously separate the alkali from the decomposition solution Formula zinc carbonate precipitates, and the mother liquor is heated to 95°C and circulated to the reactor. The isolated basic zinc carbonate was dried and calcined at 600° C. for 2 hours to obtain a zinc oxide product with a narrow particle size distribution. As determined by transmission electron microscope and XRD lin...

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Abstract

The process of preparing nanometer zinc oxide with low grade zinc oxide containing material includes the following steps: leaching the material with the mixed solution of ammonium bicarbonate and ammonia, separating to eliminate insoluble impurity, redox to eliminate Fe, Mn, Pb and other metal impurity to obtain zinc-ammonia complex solution; heating the zinc-ammonia complex solution to 90-100 deg.c through continuous mixing with hot circular mother liquid or hot water for fast continuous decomposition of zinc-ammonia complex; controlling the flow rate ratio between the circular mother liquid and the zinc-ammonia complex solution in 2-20, separating the basic zinc carbonate crystal continuously from the decomposed solution; drying and roasting at 400-600 deg.c for 1-4 hr to obtain the nanometer zinc oxide product of homogeneous size 10-50 nm.

Description

technical field [0001] The invention belongs to the field of inorganic functional materials. It relates to the preparation technology of inorganic nanomaterials, especially a preparation method of nano zinc oxide: a preparation method for producing nano zinc oxide based on the continuous preparation process of precursor basic zinc carbonate. Background technique [0002] There are two main processes for wet production of zinc oxide: acid leaching and ammonia compounding. Compared with the acid leaching method, the ammonia compounding method has the advantages of less anti-corrosion requirements for equipment, and can recycle ammonia and carbon dioxide, so it has become one of the main methods for producing zinc oxide. The traditional ammonia complexing process is mainly composed of leaching, purification, pyrolysis, ammonia absorption, drying and roasting. Since the traditional pyrolysis operation generally puts the purified zinc ammonia complex solution into a container, ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G9/02B82B3/00
Inventor 董广前王洁寇丽华安峰王继杨秀英
Owner CHINA NAT OFFSHORE OIL CORP
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