Chromium fog inhibitor and preparation method thereof

A technology of chromium mist inhibitor and inert solvent, which is applied in the field of preparation of chromium mist inhibitor, can solve the problems of high production cost, limited use, complex process, etc., and achieve the effects of small environmental hazards, stable existence, and low surface energy

Inactive Publication Date: 2015-05-13
湖北恒新化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the traditional chromium mist inhibitor contains PFOS (perfluorooctane sulfonate), which seriously endangers human health and the natural environment, and its use is restricted (the "Stockholm Convention" in May 2009 regards PFOS substances as persistent organic pollutants , included in the newly added POPs, and agreed to stop using it within a limited period

Method used

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  • Chromium fog inhibitor and preparation method thereof
  • Chromium fog inhibitor and preparation method thereof
  • Chromium fog inhibitor and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] Add triethylamine (11.0 g, 0.109 mol), methyltriethoxysilane (14.1 g, 0.079 mol), and 143 g of chlorobenzene into a 250 ml three-necked flask, stir, and slowly add all the Fluorohexylsulfonyl fluoride (30.2 g, 93%, 0.07 mol), then continue to stir for 6 hours, stand still, filter, transfer the filter cake to a rotary evaporator, and dry it under reduced pressure at 70 ° C to obtain white powdery crystals The yield of tetraethylamine perfluorohexylsulfonate (34.1 g, 0.064 mol) was 92%.

Embodiment 2

[0020] Add triethylamine (12.1 g, 0.12 mol), methyltriethoxysilane (17.8 g, 0.1 mol), and 180 g of chlorobenzene into a 250 ml three-necked flask, stir, control the temperature at 25°C, and slowly add all Fluorohexylsulfonyl fluoride (43.2 g, 93%, 0.1 mol), continued to stir and react for 8 hours after completion, let stand, filter, transfer the filter cake to a rotary evaporator, and dry it under reduced pressure at 60°C to obtain a white powder The yield of crystalline tetraethylamine perfluorohexylsulfonate (47.6 g, 0.09 mol) was 90%.

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Abstract

The invention discloses a chromium fog inhibitor-tetraethylammonium perflurohexane sulfonate free of PFOS (perfluorooctane sulfonate). The invention further discloses a preparation method for the chromium fog inhibitor, that is to say, perflurohexane sulphonyl fluoride, triethylamine and methyl triethoxysilane react in an inert solvent to obtain tetraethylammonium perflurohexane sulfonate, wherein a proper reaction temperature is 0-40 DEG C, a molar ratio of perflurohexane sulphonyl fluoride, triethylamine and methyl triethoxysilane is 1:(1-1.8):(0.6-1.5), and the proper inert solvent is chlorobenzene, benzene or isopropyl ether. The provided method is simple and convenient in process, and the chromium fog inhibitor is high in yield and good in surface activity.

Description

technical field [0001] The invention relates to a preparation method of a chromium mist inhibitor. Background technique [0002] In the electroplating process, in order to avoid the generation of chromium mist, it is necessary to add a chromium mist inhibitor to the electroplating solution. However, the traditional chromium mist inhibitor contains PFOS (perfluorooctane sulfonate), which seriously endangers human health and the natural environment, and its use is restricted (the "Stockholm Convention" in May 2009 regards PFOS substances as persistent organic pollutants , included in the newly added POPs, and agreed to stop using it within a limited period of time worldwide). [0003] Chinese patent CN103130691A discloses a new chromium mist inhibitor that does not contain PFOS, in order to be used as a substitute for traditional PFOS-containing chromium mist inhibitors, but the invented chromium mist inhibitor has a long synthesis route, complicated process and high producti...

Claims

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Application Information

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IPC IPC(8): C25D3/04C07C303/32C07C309/06C07C209/00C07C211/63
Inventor 杨祥发李书涛高伟
Owner 湖北恒新化工有限公司
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