Nanometer zinc oxide, preparation method thereof and desulfurizing agent

A nano-zinc oxide and desulfurizer technology, applied in the direction of zinc oxide/zinc hydroxide, nanotechnology, etc., can solve the problems of little active zinc oxide, wide product particle size distribution, and reduced specific surface area, so as to reduce the calcination temperature , Improve the purity and reduce the dosage

Pending Publication Date: 2020-06-26
JIYUAN LUTAI NANO MATERIAL CO LTD
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] At present, the active zinc oxide used in the zinc oxide desulfurizer is prepared by a wet process. For example, the existing preparation method of nano-zinc oxide directly precipitated in a reaction tank has serious agglomeration among precursor particles. After calcination, the particle size distribution of the product is wide, easy to agglomerate, and the specific surface area is reduced
However, the active nano-zinc oxide products on the market at this stage, regardless of whether the zinc oxide content is more than 95% or more than 99%, have a specific surface area of ​​40-65m. 2 / g, rarely break through 65m 2 / g of active zinc oxide, and when it is used in zinc oxide desulfurizers, it can only meet the basic standard requirements of HG / T 2508-2012 zinc oxide desulfurizer standard of 20% of the breakthrough sulfur capacity at 220°C, and cannot Make a greater breakthrough in its penetration sulfur capacity, and some products are even difficult to make the penetration sulfur capacity of zinc oxide desulfurizer reach the requirement of 20%.

Method used

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  • Nanometer zinc oxide, preparation method thereof and desulfurizing agent
  • Nanometer zinc oxide, preparation method thereof and desulfurizing agent
  • Nanometer zinc oxide, preparation method thereof and desulfurizing agent

Examples

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preparation example Construction

[0049] For details, please refer to figure 1 , a preparation method of nano-zinc oxide, which comprises:

[0050] S1. Obtain zinc sulfate solution and soda ash solution.

[0051] Among them, the zinc sulfate solution includes allowed impurities, and the impurities mainly include Fe 2+ 、Cu 2+ , Mn 2+ and Cd 2+ , and when [Zn 2 + ]=100g / L, [Fe 2+ ]2+ ]≤2mg / L, [Cu 2+ ]2+ ]<2mg / L.

[0052] When the impurity includes in addition to protecting Fe 2+ 、Cu 2+ , Mn 2+ and Cd 2+ In addition, it also includes Al 3+ , when the zinc sulfate solution [Zn 2+ ]=100g / L, [Al 3+ ]<10mg / L.

[0053] Zinc sulfate solution can be prepared by yourself or purchased, as long as it meets the above requirements.

[0054] Alternatively, the zinc sulfate solution is prepared by:

[0055] (1) obtain zinc sulfate crude liquid

[0056] Optionally, the crude zinc sulfate solution is put into water by sub-zinc oxide for leaching and slurrying, until the leachate pH=5 and [Zn 2 + ]=60-105g / L,...

Embodiment 1

[0092] Zinc sulfate solution is prepared by the following method:

[0093] A. Put 1 part by weight of zinc oxide into 4-8 parts by weight of water for leaching until pH=5 and [Zn 2+]=100g / L, filter, obtain zinc sulfate thick liquid.

[0094] B. Detect the iron content in the crude zinc sulfate solution. After calculation, add quantitative hydrogen peroxide and continue stirring for 10 minutes. Then according to the amount of hydrogen peroxide added, drop into calcium carbonate in proportion to carry out hydrolysis iron removal, adjust pH value=5, stir 10min, get filtrate detection, [Fe 2+ ] < 2mg / L, the material enters the plate and frame filter press for filtration to obtain the zinc sulfate crude liquid after iron removal.

[0095] C. Check the aluminum content in the crude zinc sulfate solution after iron removal, raise the temperature to 60-70°C, add the quantitative flocculant obtained after calculation, stir for 20 minutes and then let it settle for 3 hours, then the m...

Embodiment 2

[0100] A kind of nano zinc oxide, it is made by following preparation method:

[0101] Zn in the supernatant that embodiment 1 obtains 2+ The concentration was adjusted to 100g / L as the zinc sulfate solution used in this embodiment.

[0102] Get 1 volume part of zinc sulfate solution and 0.65 volume parts of concentration and be 20wt% soda ash solution, at 50 ℃, press the feed total amount of zinc sulfate solution and soda ash solution to be 18m 3 / h and the flow rate ratio of zinc sulfate solution to soda ash solution is 1:0.65 into the hypergravity reactor for neutralization reaction to generate precursor slurry.

[0103] Put the precursor slurry obtained after the reaction into the reaction tank, stir, adjust the pH value to 7, raise the temperature to 80°C, stir for 30 minutes, let it stand and age for 3 hours, then wash with water, press filter to obtain a water content of 50±1% precursors. The washed water is reclaimed, and sodium sulfate is reclaimed according to rel...

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Abstract

The invention discloses nano-zinc oxide, a preparation method thereof and a desulfurizing agent, and relates to the field of nano-zinc oxide preparation. The preparation method of the nano-zinc oxidecomprises the following steps: carrying out neutralization reaction on a zinc sulfate solution and a sodium carbonate solution in a supergravity reactor to generate precursor slurry; adjusting the precursor slurry to be neutral, standing and aging for at least 2.5 hours, washing and carrying out filter pressing to obtain a precursor; calcining the precursor; carrying out direct precipitation reaction by adopting a supergravity reactor; the generated basic zinc carbonate precursor is quickly nucleated in a supergravity reactor; the method comprises the following steps: calcining nano-zinc oxide, then aging, nucleating uniformly and finely, mainly condensing and growing among nuclei, so that the particle size of the nano-zinc oxide after subsequent calcination is uniform and fine, the specific surface area of the nano-zinc oxide after calcination is effectively increased compared with that of a direct precipitation method, and the penetration sulfur capacity of the desulfurizing agent can be up to 25% when the prepared nano-zinc oxide is applied to the desulfurizing agent.

Description

technical field [0001] The application relates to the field of nano-zinc oxide preparation, in particular, to a nano-zinc oxide, a preparation method thereof, and a desulfurizer. Background technique [0002] At present, active nano zinc oxide is widely used in desulfurizer, rubber, ceramics, medical treatment, photocatalysis, cosmetics, feed and other industries. Active nano-zinc oxide prepared by wet method has excellent surface activity and has become the main raw material of zinc oxide desulfurizer. [0003] At present, the active zinc oxide used in the zinc oxide desulfurizer is prepared by a wet process. For example, the existing preparation method of nano-zinc oxide directly precipitated in a reaction tank has serious agglomeration among precursor particles. After calcination, the particle size distribution of the product is wide, easy to agglomerate, and the specific surface area is reduced. However, the active nano-zinc oxide products on the market at this stage, ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G9/02B82Y40/00
CPCC01G9/02B82Y40/00C01P2006/80C01P2006/12
Inventor 齐磊王东石磊
Owner JIYUAN LUTAI NANO MATERIAL CO LTD
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