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Preparation method of zinc oxide normal-temperature desulfurizing agent

A technology of zinc oxide and desulfurizer, which is applied in chemical instruments and methods, separation methods, and dispersed particle separation, etc., can solve problems such as insufficient mixing, cumbersome steps, and large particle size of nanoparticles.

Active Publication Date: 2015-01-28
SHENYANG SANJUKAITE CATALYST +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Although the desulfurizer has a high sulfur capacity and can achieve high-precision desulfurization at a relatively low temperature, the above-mentioned prior art still has the disadvantages that the breakthrough sulfur capacity of the desulfurizer at 200-250°C is greater than 24wt%. However, the breakthrough sulfur capacity at 30°C is only 15.5wt%, which still cannot meet the demand, which may be due to the uneven mixing of the active components nano-zinc oxide and copper oxide in the preparation process of kneading molding.
But the above-mentioned process steps are loaded down with trivial details, all have very high requirement to the control of condition and the operation of equipment, once operation is unstable, will cause crystallinity difference, make the particle diameter of nano-particle larger than normal, therefore, the coprecipitation of prior art The process is not yet suitable for mass production

Method used

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  • Preparation method of zinc oxide normal-temperature desulfurizing agent

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Embodiment 1

[0032] The preparation method of zinc oxide normal temperature desulfurizer described in this embodiment comprises the following steps:

[0033] (1) adding an aqueous solution of sodium carbonate to an aqueous solution of zinc nitrate, the molar ratio of the zinc nitrate to the sodium carbonate is 1:0.5, stirring and reacting at 60°C for 0.5 hours to obtain the first slurry;

[0034] (2) Add an aqueous solution of sodium carbonate to the aqueous solution of copper nitrate, and stir and react at 60° C. for 0.5 hour to obtain a second slurry; wherein, the molar ratio of the copper nitrate to the zinc nitrate is 1:18, so The mol ratio of described copper nitrate and described sodium carbonate is 1: 0.5;

[0035] (3) In the double-cone rotary vacuum reactor, mix the first slurry and the second slurry, and add an aqueous solution of sodium hydroxide under a vacuum condition of -0.08MPa, and stir at 60°C for reaction 1 hour to obtain a precursor slurry, wherein the molar ratio of t...

Embodiment 2

[0039] The preparation method of zinc oxide normal temperature desulfurizer described in this embodiment comprises the following steps:

[0040] (1) Add potassium carbonate to the aqueous solution of zinc chloride, the molar ratio of the zinc chloride to the potassium carbonate is 1:0.8, stir and react at 55° C. for 40 minutes to obtain the first slurry;

[0041] (2) Add potassium carbonate to the aqueous solution of cupric chloride, stir and react at 60° C. for 40 minutes to obtain the second slurry; wherein, the molar ratio of the cupric chloride to the zinc chloride is 1:16, so The mol ratio of described cupric chloride and described potassium carbonate is 1: 0.6;

[0042] (3) In a double-cone rotary vacuum reactor, mix the first slurry and the second slurry, and add an aqueous solution of potassium hydroxide under a vacuum condition of -0.07MPa, and stir at 70°C for reaction 1 hour to obtain a precursor slurry, wherein the molar ratio of the potassium hydroxide to the zin...

Embodiment 3

[0046] The preparation method of zinc oxide normal temperature desulfurizer described in this embodiment comprises the following steps:

[0047] (1) Adding an aqueous solution of sodium carbonate to an aqueous solution of zinc sulfate, the molar ratio of the zinc sulfate to the sodium carbonate is 1:0.65, stirring and reacting at 55° C. for 20 minutes to obtain the first slurry;

[0048] (2) Add an aqueous solution of sodium carbonate to an aqueous solution of copper sulfate, and stir and react for 20 minutes at 55° C. to obtain a second slurry; wherein, the molar ratio of the copper sulfate to the zinc sulfate is 1:16, and the The mol ratio of cupric sulfate and described sodium carbonate is 1: 0.8;

[0049] (3) In a double-cone rotary vacuum reactor, mix the first slurry and the second slurry, add sodium hydroxide under a vacuum condition of -0.09MPa, and stir at 65°C for 1 hour , to obtain a precursor slurry, wherein the molar ratio of the sodium hydroxide to the zinc sulf...

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Abstract

The invention provides a preparation method of zinc oxide normal-temperature desulfurizing agent. The method comprises the following steps: firstly forming respective unstable precipitate of partial zinc salt and copper salt; and then completely translating residual zinc salt and copper salt not participating the precipitation in a bipyramid rotary vacuum reaction kettle and above unstable precipitates into stable zinc hydroxide and copper hydroxide, roasting to obtain compound powder of zinc oxide and copper oxide, and then preparing the zinc oxide normal temperature desulfurizing agent. The preparation method of the zinc oxide normal temperature desulfurizing agent provided by the invention has a simple process step, and less requirements on condition control and equipment operation, and the sulfur capacity of the prepared zinc oxide normal temperature desulfurizing agent at normal temperature reaches up to 20.3% and more; and therefore, the preparation method provided by the invention is suitable for large-scale production, and has high actual application value.

Description

technical field [0001] The invention relates to a preparation method of a desulfurizer, in particular to a preparation method of a zinc oxide normal temperature desulfurizer, and belongs to the technical field of desulfurizers. technical background [0002] According to the application temperature, desulfurizers can be divided into high temperature desulfurizers, medium and low temperature desulfurizers and normal temperature desulfurizers. In recent years, from the perspective of rational use of heat energy, energy saving and consumption reduction, both at home and abroad are committed to the development and research of low temperature and normal temperature desulfurizers . However, since it is difficult for the reactants to break through the energy barrier at room temperature, only substances with special physical and chemical properties can achieve the purpose of desulfurization at room temperature, and the desulfurization agents currently developed for medium and high te...

Claims

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Application Information

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IPC IPC(8): B01D53/48
Inventor 赵素云
Owner SHENYANG SANJUKAITE CATALYST
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