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Method for preparing tin methanesulfonate through using methanesulfonyl chloride

A technology of methanesulfonyl chloride and tin methanesulfonate, which is applied in the preparation of sulfonate, can solve the problems of not meeting the needs of industrial production, high equipment requirements, and low production efficiency, so as to avoid oxidative discoloration and reduce the preparation process , cost-saving effect

Inactive Publication Date: 2012-06-27
HUBEI XINGHUO CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The production of tin methanesulfonate by electrolysis has high requirements on equipment, and the production efficiency is low, which cannot meet the needs of industrial production.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] (1) Preparation of stannous chloride

[0021] Add 60L of concentrated hydrochloric acid with a content of 31% and 20kg of metal tin powder (average particle size: 400 mesh) into a 100L enamel reaction kettle, start stirring, raise the temperature to 70°C, reflux for 4 hours, and filter while hot to remove unreacted metal tin powder to obtain 51L of colorless and transparent tin protochloride aqueous solution.

[0022] (2) Preparation of tin methanesulfonate aqueous solution

[0023] The temperature of the solution obtained from the above reaction was raised to 70° C., and the stirring was started. 30 L of methanesulfonyl chloride was added dropwise within 1 h. Exhaust gas is absorbed through two-stage falling film. After the hydrolysis is completed, heat up to 90°C, distill under reduced pressure, and further remove chlorine until the chlorine ion 2+ >300g / L. Obtain 50.1 kilograms of colorless transparent tin methanesulfonate solutions containing divalent tin ions 3...

Embodiment 2

[0026] (1) Preparation of stannous chloride

[0027] Add 60L of concentrated hydrochloric acid and 20kg of stannous oxide into a 100L enamel reaction kettle, start stirring, raise the temperature to 80°C, reflux for 4 hours, filter while hot to remove unreacted solids, and obtain a colorless and transparent aqueous solution of stannous chloride.

[0028] (2) Preparation of tin methanesulfonate aqueous solution

[0029] The temperature of the above solution was raised to 80°C, and the stirring was started. Add 30L methanesulfonyl chloride dropwise within 1 hour, and the tail gas is absorbed by two-stage falling film. Raise the temperature to 120°C, distill under reduced pressure, and further remove chlorine until the chlorine ion 2+ >300g / L. Obtain 70.6 kilograms of colorless transparent tin methanesulfonate solution containing 301 g / L of divalent tin ions.

[0030] Embodiment three:

Embodiment 3

[0032] (1) Preparation of stannous chloride

[0033] Add 100L concentrated hydrochloric acid and 20k tin particles into a 200L enamel reaction kettle, start stirring, raise the temperature to 120°C, reflux for 4 hours, filter while hot to remove unreacted solids, and obtain a colorless and transparent aqueous solution of stannous chloride.

[0034] (2) Preparation of tin methanesulfonate aqueous solution

[0035] The temperature of the above solution was raised to 80°C, and the stirring was started. Add 30L methanesulfonyl chloride dropwise within 1 hour, and the tail gas is absorbed by two-stage falling film. Raise the temperature to 100°C, distill under reduced pressure, and further remove chlorine until the chlorine ion 2+ >300g / L. Obtain 56.6 kilograms of colorless transparent tin methanesulfonate solutions containing divalent tin ions 301g / L.

[0036] Embodiment four:

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Abstract

The invention relates to a method for preparing tin methanesulfonate through using methanesulfonyl chloride. The method comprises the following steps: 1, preparing stannous chloride; and 2, preparing an aqueous solution of stannous methanesulfonate. According to the invention, metallic tin or stannous oxide is dissolved by cheap hydrochloric acid to prepare the aqueous solution of stannous chloride, and methanesulfonyl chloride is hydrolyzed in the aqueous solution of stannous chloride to prepare stannous methanesulfonate. All reactions are carried out under low temperature and normal pressure or low pressure or reduced pressure conditions, so the decomposition of methanesulfonic acid and the oxidation color change of stannous ions are avoided; the methanesulfonyl chloride hydrolysis and a displacement reaction of methanesulfonic acid and stannous chloride are simultaneously carried out, so the methanesulfonic acid preparation process is omitted, and the cost is saved; and hydrochloric acid obtained through the hydrolysis and the displacement reaction can be recycled.

Description

technical field [0001] The invention belongs to the technical field of preparation of special chemicals for electroplating, and in particular relates to a preparation method of tin methanesulfonate for electronic electroplating. Background technique [0002] Tin and tin-lead alloy coatings have been widely used in the electronics industry due to their excellent corrosion resistance and solderability. However, in recent years, due to the great restriction of lead, the electroplating tin process will become the main plating type of solderable coating in electronic electroplating. Previous tin plating baths were mainly based on highly polluting fluoroborates, phenol sulfonates, and halides. In recent years, the sulfate tin plating process has greatly improved environmental pollution, but the baths are unstable. Methanesulfonate tin plating can basically solve the above problems and has high industrial application value. Therefore, the tin plating process of tin methanesulfon...

Claims

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Application Information

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IPC IPC(8): C07C309/04C07C303/32
Inventor 曾丹田汪志君
Owner HUBEI XINGHUO CHEM
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