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Synthetic method of sodium polydithio-dipropyl sulfonate

A technology of sodium polydithiodipropane sulfonate and sodium thiopropane sulfonate, which is applied in the field of synthesis of polydithiodipropane sodium sulfonate, can solve the problems of complex process lines and high production costs, and achieve less side reactions in synthesis , the effect of small environmental impact

Active Publication Date: 2012-12-26
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

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] In a 1000mL flask equipped with electric stirring, constant pressure dropper, thermometer, and reflux condenser, put 200mL of water and 28g of sodium hydrosulfide into it, dissolve it at 50-60°C, cool it at 15-35°C, and add 62.5g of 1,3- After adding PS, raise the temperature to 50-60°C for 1 hour, cool down, and filter to obtain MPS liquid.

[0032] Add 75 grams of tert-butyl hydroperoxide to the above MPS solution, react to the end, heat up, keep warm at 50-60°C for 4 hours, keep warm at 70-80°C for 2 hours, decolorize, dehydrate and nearly dry, add methanol to disperse, filter, and dry 80.5 g SPS was obtained, the yield was 96%.

[0033] Add solvent, recover and apply mechanically.

Embodiment 2

[0035] Put 200kg of water and 28kg of sodium hydrosulfide into a 500L reactor, heat up to 50-60°C to dissolve, cool down to 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.

[0036] Add 75kg of oxidant tert-butyl hydroperoxide to the above MPS liquid, react to the end point, raise the temperature to 50-60°C, and keep it warm for 4 hours; heat up, keep it at 70-80°C for 2 hours, use activated carbon to decolorize, dehydrate under reduced pressure, and dry it. Add methanol to disperse, filter, and dry to obtain 81kg SPS.

[0037] The added solvent was recovered and used mechanically.

Embodiment 3

[0039] In a 1000mL flask equipped with electric stirring, constant pressure dropper, thermometer, and reflux condenser, put 200mL of water and 28g of sodium hydrosulfide into it, dissolve it at 50-60°C, cool it at 15-35°C, and add 62.5g of 1,3- After adding PS, raise the temperature to 50-60°C for 1 hour, cool down, and filter to obtain MPS liquid.

[0040] Add 50 grams of hydrogen peroxide to the above MPS solution, react to the end, heat up, keep warm at 50-60°C for 4 hours, keep warm at 70-80°C for 2 hours, decolorize, dehydrate and nearly dry, add methanol to disperse, filter, and dry to obtain 75.5g SPS , yield 90%.

[0041] The added solvent was recovered and used mechanically.

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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 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 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 (the SPS content is more than or equal to 99 percent).

Description

technical field [0001] The invention belongs to a chemical synthesis method of a brightener for copper plating, in particular to a synthesis method of sodium polydisulfide dipropane sulfonate. Background technique [0002] Sodium polydisulfide dipropane sulfonate (SPS) is a widely used copper plating brightener in printed circuit board copper plating and acid copper plating. It is used in electroplating as long as it is related to copper plating. At present, there are few manufacturers of sodium polydithiodipropanesulfonate (SPS) in the world, and the foreign manufacturer is Rashing Company of Germany; there is domestic production, but the technology is backward, the scale of production is small, and the quality is poor. Good-quality, high-grade copper-plating baths all use imported SPS, and only domestic SPS is used in low-grade copper-plating baths. [0003] At present, there are very few reports on the synthetic production of this product at home and abroad. Generally sp...

Claims

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Application Information

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Patent Type & Authority Patents(China)
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