A method for preparing superfine flaky zinc powder by adding antimony-containing compound lye electrolysis

The technology of flake zinc powder and antimony compound is applied in the field of preparation of ultra-fine flake zinc powder, which can solve the problems of increasing cell voltage and energy consumption, high process difficulty and high processing cost, and achieves high process current efficiency and high process flow. Simple, anti-corrosion effect

Inactive Publication Date: 2017-01-18
TONGJI UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Among them, the zinc powder prepared by the atomization method and the ball milling method usually has a particle size of more than 10 μm, so it is impossible to prepare ultra-fine zinc powder; the production efficiency of the distillation method is high, but the activity of the prepared ultra-fine zinc powder is low, and at the same time, the purity of raw materials is required. high
[0004] Chinese patent a method for producing high-purity metallic zinc with zinc oxide ore (publication number 1450182, published on October 22, 2003), and the process proposed in the method for producing high-purity metallic zinc from zinc oxide ore (publication number is 1482263, published on March 17, 2004), promoted the large-scale production of the alkaline electrolytic zinc powder process, but the zinc powder produced by this process has a large particle size and uneven distribution, and the subsequent processing costs are high and the process Difficult; Chinese patents a method for electrolytically preparing ultrafine zinc powder by adding aluminum-containing compound lye (publication number CN102776532A, published on November 14, 2012) and a method for preparing ultrafine zinc powder by adding lead-containing compound lye The method (publication number CN103255442A, published on August 21, 2013) is to use the polarization of additives to increase the specific surface area of ​​zinc powder, and the electrolyzed zinc powder has a dendritic shape, which is suitable for displacers in hydrometallurgy And additives produced by some chemical products are not suitable for plating and coating raw materials
A Chinese invention patent, a method for directly electrolytically producing one-dimensional nano-flaky zinc powder from a strong alkali solution (publication number CN102181886A, published on September 14, 2011), has achieved a flaky zinc powder with a thickness of less than 100nm, but the process A large amount of surfactant needs to be added in the process, which increases the cell voltage and energy consumption

Method used

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  • A method for preparing superfine flaky zinc powder by adding antimony-containing compound lye electrolysis
  • A method for preparing superfine flaky zinc powder by adding antimony-containing compound lye electrolysis
  • A method for preparing superfine flaky zinc powder by adding antimony-containing compound lye electrolysis

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Experimental program
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Effect test

Embodiment 1

[0035] (1) Use distilled water and sodium hydroxide to make a strong alkali solution, and the concentration of NaOH in the solution is 250g / L;

[0036] (2) Then add ZnO and oxyantimony potassium tartrate, stir and dissolve to obtain an electrolyte, the zinc content in the electrolyte is 35g / L, and the antimony content is 0.5mg / L;

[0037] (3) Insert the electrode plate into the obtained electrolyte, the 304 stainless steel plate is the anode plate, the magnesium plate is the cathode plate, and the current density is 1500A / m 2 , the pole spacing is 3cm, the whole electrolysis process is carried out in a tank, the electrolyte temperature is 25°C, and the electrolysis time is 15min;

[0038] (4) Immediately after the electrolysis, take out the zinc powder, first rinse the residual sodium hydroxide with water until the washing solution is neutral, then rinse the residual water on the zinc powder with absolute ethanol, and dry the obtained zinc powder in vacuum to obtain metal-cont...

Embodiment 2

[0043] (1) Use distilled water and sodium hydroxide to make a strong alkali solution, and the concentration of NaOH in the solution is 150g / L;

[0044] (2) Then add ZnCO 3 and antimony trioxide, ultrasonically dissolved to obtain an electrolyte, the zinc content in the electrolyte is 20g / L, and the antimony content is 1mg / L;

[0045] (3) Insert the electrode plate into the obtained electrolyte, the 321 stainless steel plate is the anode plate, the magnesium plate is the cathode plate, and the current density is 800A / m 2 , the pole spacing is 6cm, the whole electrolysis process is carried out in a tank, the electrolyte temperature is 50°C, and the electrolysis time is 60min;

[0046] (4) Immediately after the electrolysis, take out the zinc powder, rinse the residual sodium hydroxide with water until the washing solution is neutral, then rinse the residual water on the zinc powder with absolute ethanol, and dry the obtained zinc powder with nitrogen to obtain Ultrafine flaky ...

Embodiment 3

[0051] (1) Use distilled water and sodium hydroxide to make a strong alkali solution, and the concentration of NaOH in the solution is 200g / L;

[0052] (2) Then add ZnCO 3 and a mixture of antimony trioxide and oxyantimony potassium tartrate (1:1), ultrasonically dissolved to obtain an electrolyte, the zinc content in the electrolyte is 50g / L, and the antimony content is 0.1mg / L;

[0053] (3) Insert the electrode plate into the obtained electrolyte, the 316L stainless steel plate is the anode plate, the magnesium plate is the cathode plate, and the current density is 1200A / m 2 , the pole spacing is 10cm, the whole electrolysis process is carried out in a tank, the electrolyte temperature is 35°C, and the electrolysis time is 40min;,

[0054] (4) Immediately after the electrolysis, take out the zinc powder, rinse the residual sodium hydroxide with water until the washing solution is neutral, then rinse the residual water on the zinc powder with absolute ethanol, and dry the ob...

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Abstract

The invention belongs to the field of high-tech production of ultrafine flake zinc powder, and relates to a method for preparing ultrafine flake zinc powder. The method comprises the following steps: (1) preparing a strong alkali solution; (2) adding a zinc compound and an antimony compound to the solution prepared in the step (1), and dissolving to prepare electrolyte; (3) carrying out electrolytic reaction on the electrolyte obtained in the step (2); and (4) taking out a pole plate after stopping electrolysis, scrapping off zinc powder, cleaning and drying to obtain the ultrafine flake zinc powder. The mean diameter of the zinc powder prepared by the method provided by the invention is 5-10mum, and the ultrafine flake zinc powder is free of obvious dendritic crystals, high in density, and applicable to use as zinc powder for a coating; the current efficiency of the method is greater than 90% by controlling the current density and the scrapping frequency and adding a trace of surfactant and the like. The method is simple to control process, and low in energy consumption, and the obtained zinc powder is wide in use, and can be matched with a plurality of subsequent flows to prepare other high added-value products.

Description

technical field [0001] The invention belongs to the field of ultrafine powder high-tech production, and relates to a preparation method of ultrafine flaky zinc powder. Background technique [0002] Ultrafine zinc powder refers to zinc powder with an average length and diameter of less than 10 μm. It is widely used as an important raw material for chemical and pharmaceutical synthesis, battery electrodes, and metal anticorrosion. The zinc powder required by some special industries has long been monopolized by developed countries. At present, the national demand for ultra-fine zinc powder is more than 100,000 tons per year, and it is increasing year by year, and the price is 3-4 times that of ordinary zinc powder. Zinc powder for coatings and coatings requires high flakiness and low dendrite rate to achieve dense and regular coatings. [0003] The preparation methods of zinc powder mainly include distillation method, atomization method, high energy ball milling method, electr...

Claims

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Application Information

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Patent Type & AuthorityPatents(China)
IPC IPC(8): C25C5/02B22F1/00
Inventor赵由才李强柴晓利牛冬杰
OwnerTONGJI UNIV