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Synthetic method of sodium polydithio-dipropyl sulfonate

A technology of sodium polydisulfide dipropane sulfonate and sodium thiopropane sulfonate is applied in the field of synthesis of sodium polydisulfide dipropane sulfonate, can solve the problems of high production cost, complicated process circuit and the like, and achieves synthesis side reactions Less and less impact on the environment

Active Publication Date: 2009-09-02
武汉松石科技股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Through research experiments, the quality of the product is acceptable, but the whole process line is complicated, the total yield is only 20%, and the production cost is very high

Method used

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  • Synthetic method of sodium polydithio-dipropyl sulfonate
  • Synthetic method of sodium polydithio-dipropyl sulfonate
  • Synthetic method of sodium polydithio-dipropyl sulfonate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] In a 1000mL flask with electric stirring, constant pressure dropper, thermometer and reflux condenser, put 200mL water, 28g sodium hydrosulfide, dissolve at a temperature of 50-60°C, cool at 15-35°C, add 62.5g 1,3- After the addition of PS, the temperature was increased to 50-60° C. for 1 hour, the temperature was lowered, and the MPS solution was obtained by filtration.

[0030] Add 75 grams of tert-butyl hydroperoxide to the above-mentioned MPS solution, react to the end point, heat up, keep at 50-60 °C for 4 hours, keep at 70-80 °C for 2 hours, decolorize, dehydrate and nearly dry, add methanol to disperse, filter, and dry 80.5g SPS was obtained, the yield was 96%.

[0031] Add solvent, recycle and apply.

Embodiment 2

[0033] Put 200kg of water and 28kg of sodium hydrosulfide into a 500L reactor, heat up at 50-60°C to dissolve, cool at 10-30°C, add 62.5kg of 1,3-PS, after adding, heat up to 50-60°C for 1 hour, cool down to 10 ℃~40℃, filter to obtain MPS liquid.

[0034] To above-mentioned MPS liquid, add 75kg oxidant tert-butyl hydroperoxide, react to the end point, be warming up to 50-60 ℃, be incubated for 4 hours; Add methanol to disperse, filter, and dry to obtain 81kg SPS.

[0035] The added solvent is recycled and applied.

Embodiment 3

[0037] In a 1000mL flask with electric stirring, constant pressure dropper, thermometer and reflux condenser, put 200mL water, 28g sodium hydrosulfide, dissolve at a temperature of 50-60°C, cool at 15-35°C, add 62.5g 1,3 -PS, after the addition is completed, the temperature is increased to 50-60° C. for 1 hour, the temperature is lowered, and the MPS liquid is obtained by filtration.

[0038] Add 50 grams of hydrogen peroxide to the above-mentioned MPS solution, react to the end point, heat up, keep at 50-60°C for 4 hours, keep at 70-80°C for 2 hours, decolorize, dehydrate and nearly dry, add methanol to disperse, filter, and dry to obtain 75.5g SPS, 90% yield.

[0039] The added solvent is recycled and applied.

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PUM

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Abstract

The invention discloses a synthetic method of sodium polydithio-dipropyl sulfonate. The sodium sulfhydrate reacts with 1,3-PS to obtain MPS firstly, and then the MPS is oxidized to obtain SPS. The quaThe invention discloses a synthetic method of sodium polydithio-dipropyl sulfonate. The sodium sulfhydrate reacts with 1,3-PS to obtain MPS firstly, and then the MPS is oxidized to obtain SPS. The quality of sodium polydithio-dipropyl sulfonate fully reaches the level of the overseas similar products, has the same content analysis, nuclear magnetic resonance analysis, high-pressure liquid phase anlity of sodium polydithio-dipropyl sulfonate fully reaches the level of the overseas similar products, has the same content analysis, nuclear magnetic resonance analysis, high-pressure liquid phase analysis and ultraviolet analysis as the overseas products. Repeated test and demonstration prove that the invention has stable process, high yield (more than or equal to 95 percent) and good quality (talysis and ultraviolet analysis as the overseas products. Repeated test and demonstration prove that the invention has stable process, high yield (more than or equal to 95 percent) and good quality (the SPS content is more than or equal to 99 percent).he SPS content is more than or equal to 99 percent).

Description

technical field [0001] The invention belongs to a chemical synthesis method of a copper-plating brightener, in particular to a synthesis method of sodium polydisulfide dipropane sulfonate. Background technique [0002] Sodium polydithiopropane sulfonate (SPS) is a copper plating brightener widely used in copper plating and acid copper plating of printed circuit boards. It should be used in electroplating as long as it is related to copper plating. At present, there are few manufacturers of sodium polydithiodipropane sulfonate (SPS) in the world. The foreign manufacturer is Rashing Company of Germany. There is domestic production, but the technology is backward, the production scale is small and the quality is poor. The high-quality and high-grade copper-plating electroplating solutions use imported SPS, and only domestic SPS is used in the low-grade copper-plating electroplating solutions. [0003] At present, there are very few reports on the synthetic production of this p...

Claims

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Application Information

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IPC IPC(8): C07C323/66C07C319/24
Inventor 宋朝阳杨磊周列平张忠良王浩鹏刘淑君王娟张秀丽
Owner 武汉松石科技股份有限公司
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