Method for reducing tetravalent tin content in stannous sulfate

A technology of stannous sulfate and tetravalent tin, which is applied in the direction of electrolytic components and electrolytic processes, can solve the problems of affecting the storage validity period and product appearance, not being suitable for large-scale continuous production, and difficult and precise control of current density, so as to improve the international Competitiveness, low cost, and the effect of improving quality

Active Publication Date: 2019-02-26
FINE CHEM GRP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Therefore, the tetravalent tin content seriously affects its storage validity period and product appearance
[0004] Domestic scholar Wei Qing (Journal of Wuyi University, 2000, 14, 55-59) once reported that the current density needs to be controlled to suppress tetravalent tin when preparing stannous sulfate in the laboratory, but this method is obtained by intermittent electrolysis under laboratory conditions. In the process of large-scale industrial production, the anode area is constantly changing, and the current density is difficult to accurately control, which is not suitable for large-scale continuous production; The impact of oxidation into tetravalent tin, but the paper does not consider the impact of dissolved oxygen in the electrolyte on the generation of tetravalent tin; Chinese patent 201410846701.7 describes the method of adding organic antioxidants to prolong the shelf life of stannous sulfate products, but this method is added to the product Adding foreign matter affects product quality; Du Jianzhong (Food Science: 2005, 26, 397-399) introduced the test method of tetravalent tin

Method used

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  • Method for reducing tetravalent tin content in stannous sulfate
  • Method for reducing tetravalent tin content in stannous sulfate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] Embodiment 1, a kind of method that reduces tetravalent tin content in stannous sulfate production process comprises the steps:

[0041] 1), at the bottom of the stannous sulfate electrolytic cell, laying a layer of tin particle layer (particle size D) with a thickness of 2cm 50 is 2 μm);

[0042] 2), add acetone oxime as oxygen scavenger in dilute sulfuric acid, obtain the dilute sulfuric acid after treatment; The consumption ratio of dilute sulfuric acid and oxygen scavenger is 100ml / 0.05g;

[0043] Described dilute sulfuric acid is the sulfuric acid solution that concentration is 1mol / L;

[0044] 3) Add treated dilute sulfuric acid to the stannous sulfate electrolytic cell until the liquid level of the treated dilute sulfuric acid is below the cathode by 2 to 4 cm, and control the voltage of the electrolytic cell to 1.9V;

[0045] 4) When the tin ion content in the electrolyte at the bottom of the stannous sulfate electrolytic cell is ≥ 85g / L, discharge the electro...

Embodiment 2

[0049] Embodiment 2, a kind of method that reduces tetravalent tin content in stannous sulfate production process:

[0050] The particle size of tin particles D 50 10μm;

[0051] Add acetone oxime as oxygen scavenger in dilute sulfuric acid to obtain dilute sulfuric acid after treatment; the consumption ratio of dilute sulfuric acid and oxygen scavenger is 100ml / 0.08g;

[0052] Control the electrolyzer voltage to 2.0V;

[0053] Use acetone as a rinse agent;

[0054] The rest are equal to Example 1.

[0055] The content of tetravalent tin in the obtained stannous sulfate is 0.04%.

Embodiment 3

[0056] Embodiment 3, a kind of method that reduces tetravalent tin content in stannous sulfate production process:

[0057] The particle size of tin particles D 50 1 μm;

[0058] Add hydrazine as oxygen scavenger in dilute sulfuric acid to obtain dilute sulfuric acid after treatment; the consumption ratio of dilute sulfuric acid and oxygen scavenger is 100ml / 0.08g;

[0059] Control the electrolyzer voltage to 1.8V;

[0060] Use methyl ethyl ketone as eluent;

[0061] The rest are equal to Example 1.

[0062] The content of tetravalent tin in the obtained stannous sulfate is 0.07%.

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Abstract

The invention discloses a method for reducing the content of tetravalent stannum in stannous mono-sulphate. The method for reducing the content of the tetravalent stannum in the stannous mono-sulphate comprises the following steps that a stannum granular layer is laid in the bottom of a stannous mono-sulphate electrolytic tank; a deoxidant is added into a dilute sulphuric acid, and the treated dilute sulphuric acid is obtained; the treated dilute sulphuric acid is added into the stannous mono-sulphate electrolytic tank till the liquid level of the treated dilute sulphuric acid is higher than a cathode by 2-4 cm, and the voltage of the electrolytic tank is controlled to be lower than 2.4 V; when the content of stannum ions in an electrolyte at the bottom of the stannous mono-sulphate electrolytic tank is greater than or equal to 85 g / L, the electrolyte is discharged out of the tank from an outlet, and the treated dilute sulphuric acid is supplement into the tank to maintain the liquid level of tank liquid to be an original height while the electrolyte is discharged; when the content of the stannum ions in the electrolyte at the bottom of the stannous mono-sulphate electrolytic tank is decreased to 80 g / L, discharging of the electrolyte and supplementing of the treated dilute sulphuric acid are stopped; and the electrolyte is subjected to condensation crystallization, obtained crystals are eluted by using an eluting agent and then dried, and the stannous mono-sulphate is obtained.

Description

technical field [0001] The invention belongs to the field of stannous sulfate preparation, and in particular relates to a method for reducing the content of tetravalent tin in stannous sulfate. Background technique [0002] Stannous sulfate is a white or light yellow crystalline powder, which can be dissolved in water and dilute sulfuric acid. The aqueous solution decomposes rapidly, and it will slowly oxidize in the air, turning slightly yellow. It is an important fine chemical product, and stannous sulfate is commonly used It is widely used in many industries such as acid plating of metal, alloy and non-metallic materials, electrolytic oxidation coloring of aluminum alloy, hydrogen peroxide remover and mixed with nickel salt as sealing agent, printed circuit board and many other industries. [0003] The bivalent tin in stannous sulfate has poor stability and is easily oxidized to tetravalent tin by oxygen in the air. The presence of tetravalent tin will make the tin protos...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C25B15/02C25B1/00
CPCC25B1/00C25B15/02
Inventor 王宙晖江军王兴赵金浩上官鹏鹏
Owner FINE CHEM GRP
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