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Method for preparing electronic-grade high-purity stannous methanesulfonate solution

The technology of pure stannous methanesulfonate and stannous methanesulfonate is applied in the field of preparation of electronic-grade high-purity stannous methanesulfonate solution, which can solve the problems of long operation cycle, difficult handling, and difficult product quality requirements. , to achieve the effect of less environmental pollution, low cost and complete crystal form

Inactive Publication Date: 2010-03-17
广东光华化学厂有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the common disadvantages of the first two processes are high energy consumption, long operation cycle, many impurity ions and difficult to handle, and pollute the environment, and the product quality is difficult to meet the quality requirements of the electroplating process in the electronics industry for stannous methanesulfonate S (MS). The quality of the stannous methanesulfonate synthesized by adopting the method described in technique (3) is relatively high, but hydrogen is produced in the process, and the safety requirements of the whole process equipment are high, so that the process flow is tedious and complicated

Method used

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  • Method for preparing electronic-grade high-purity stannous methanesulfonate solution

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] (1) Take methanesulfonic acid (purity 99.9%) and stannous oxide with a molar ratio of 3:1 and place them in a container, heat up to 100°C, and react for 4h under stirring conditions with a rotating speed of 100r / min, and wait for oxidation End reaction after stannous dissolving completely, obtain reaction solution;

[0022] (2) Cool and crystallize the reaction solution, filter to obtain a filter cake; wash the filter cake with anhydrous ether, and vacuum-dry it at 85°C to obtain a white solid stannous methanesulfonate; after testing, the methanesulfonate The purity of stannous acid is 99.9% by mass percentage, and the content of metal impurities Fe, Pb, Zn, Cu, Co, Cd, Mn is all≤5ppm;

[0023] (3) Add stannous methanesulfonate to deionized water to prepare a stannous methanesulfonate solution that is 300 g / L with stannous ion mass volume ratio concentration.

Embodiment 2

[0025] (1) Take methanesulfonic acid (purity 80%) and stannous oxide with a molar ratio of 6:1 and place them in a container, heat up to 130°C, and react for 6h under stirring conditions with a rotating speed of 200r / min, and wait for oxidation End reaction after stannous dissolving completely, obtain reaction solution;

[0026] (2) Cool and crystallize the reaction solution, filter to obtain a filter cake; wash the filter cake with anhydrous ether, and vacuum-dry it at 80°C to obtain a white solid stannous methanesulfonate; after testing, the methanesulfonate The purity of stannous acid is 99.93% by mass percentage, and the content of metal impurities Fe, Pb, Zn, Cu, Co, Cd, Mn is all≤5ppm;

[0027] (3) Add stannous methanesulfonate to deionized water to prepare a stannous methanesulfonate solution that is 300 g / L with stannous ion mass volume ratio concentration.

Embodiment 3

[0029] (1) Take methanesulfonic acid (purity 90%) and stannous oxide with a molar ratio of 4.5:1 and place them in a container, heat up to 120°C, and react for 5h under stirring conditions with a rotating speed of 150r / min, and wait for oxidation End reaction after stannous dissolving completely, obtain reaction solution;

[0030] (2) Cool and crystallize the reaction solution, filter to obtain a filter cake; wash the filter cake with anhydrous ether, and vacuum-dry it at 82°C to obtain a white solid stannous methanesulfonate; after testing, the methanesulfonate The purity of stannous acid is 99.9% by mass percentage, and the content of metal impurities Fe, Pb, Zn, Cu, Co, Cd, Mn is all≤5ppm;

[0031] (3) Add stannous methanesulfonate to deionized water to prepare a stannous methanesulfonate solution that is 300 g / L with stannous ion mass volume ratio concentration.

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Abstract

The invention discloses a method for preparing an electronic-grade high-purity stannous methanesulfonate solution. The method comprises the following steps: (1) placing methanesulfonic acid and stannous oxide with the molar ratio thereof being 3:1-6:1 in a container, and heating up to 100-130 DEG C, reacting for 4-6h while stirring until the stannous oxide completely dissolves, so as to obtain a reaction liquid; (2) crystallizing the reaction liquid by cooling, filtering to obtain a filter cake, and washing and vacuum-drying the filter cake to obtain white stannous methanesulfonate crystals; and (3) adding stannous methanesulfonate to de-ionized water to obtain the stannous methanesulfonate solution. The method provided by the invention for preparing the electronic-grade high-purity stannous methanesulfonate solution has fewer impurity ions; containing only stannous methanesulfonate and water, the prepared product can be easily separated, thereby ensuring the high purity of stannous methanesulfonate solids; and the invention has the advantages of simple process, low cost and less environmental pollution.

Description

technical field [0001] The invention belongs to the field of chemical production, in particular to a method for preparing an electronic-grade high-purity stannous methanesulfonate solution. Background technique [0002] With the rapid development of electroplating and electronics industry, people have higher and higher requirements for electroplating solution. Fluoroborate electroplating solution series and tin-lead alloy electroplating process are often used in traditional industries. This electroplating process containing fluorine and lead is highly corrosive to equipment, seriously endangering the health of operators, seriously polluting the environment, and waste liquid treatment. Also very difficult. At present, developed countries have adopted methanesulfonate series products to change this situation, and my country is also urgently requiring the use of environmentally friendly new processes and new products to replace traditional production processes and products. S...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C25D3/32
Inventor 谭泽黄永润洪朝辉周一朗余军文
Owner 广东光华化学厂有限公司
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