CN104611733A - Chromium fog inhibitor and preparation method thereof - Google Patents
Chromium fog inhibitor and preparation method thereof Download PDFInfo
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- CN104611733A CN104611733A CN201510032333.7A CN201510032333A CN104611733A CN 104611733 A CN104611733 A CN 104611733A CN 201510032333 A CN201510032333 A CN 201510032333A CN 104611733 A CN104611733 A CN 104611733A
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- fog inhibitor
- chromium fog
- preparation
- sulfonic acid
- chromium
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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
The present invention relates to a kind of preparation method of chromium fog inhibitor.
Background technology
In electroplating technology, for avoiding the generation of chromium mist, chromium fog inhibitor need be added in electroplate liquid.But traditional chromium fog inhibitor is owing to containing PFOS (perfluoro octane sulfonate), serious harm human health and physical environment, use restricted (in May, 2009 " Convention of Stockholm " using PFOS class material as persistence organic pollutant, list in newly-increased POPs, and arrange worldwide time limit and stop using).
Chinese patent CN103130691A discloses a kind of not containing the new chromium fog inhibitor of PFOS, and to containing PFOS class chromium fog inhibitor substitute as traditional, but this chromium fog inhibitor synthetic route of invention is long, and complex process, cost of manufacture is high, applies difficulty.
Summary of the invention:
In order to develop, a kind of cost is lower, easy to make, performance and traditional chromium fog inhibitor quite but not containing the novel chromium fog inhibitor of PFOS, the invention provides the preparation method of a kind of chromium fog inhibitor-perfluor base sulfonic acid tetraethyl-amine.
Technical scheme of the present invention is as follows: a kind of chromium fog inhibitor, and chemical name is perfluor base sulfonic acid tetraethyl-amine.
The present invention also provides the preparation method of above-mentioned chromium fog inhibitor, and concrete steps are:
1) triethylamine, Union carbide A-162 and inert solvent are mixed in the reactor, stir;
2) control temperature of reaction at 0 ~ 40 DEG C, drip perfluor base sulfonic acid fluoride;
3) temperature is kept, stirring reaction 6 hours;
4) obtain chromium fog inhibitor after separating and filtering, chemical name is perfluor base sulfonic acid tetraethyl-amine.
Described inert solvent is chlorobenzene, benzene or isopropyl ether.
In described reaction, the mol ratio of perfluor base sulfonic acid fluoride, triethylamine and Union carbide A-162 is 1:(1 ~ 1.8): (0.6 ~ 1.5).
Chromium fog inhibitor provided by the invention is not containing PFOS, not only surface energy is low, can stable existence in electroplate liquid, suppress chromium mist performance and traditional chromium fog inhibitor close, and due to carbochain be 6, short compared with PFOS carbochain, more easily degrade, little to environmental hazard, be the better substitute of traditional chromium fog inhibitor.
Accompanying drawing illustrates:
Fig. 1 is the perfluor cloudy spectrogram of base sulfonic acid tetraethyl-amine nuclear magnetic spectrogram-19F;
Fig. 2 is perfluor base sulfonic acid tetraethyl-amine nuclear magnetic spectrogram-1H sun spectrogram.
Embodiment:
Further illustrate the present invention by the following examples.
Embodiment 1
By triethylamine (11.0 grams, 0.109mol), Union carbide A-162 (14.1 grams, 0.079mol), 143 grams of chlorobenzenes add in 250ml three-necked bottle, stir, temperature controls 20 DEG C, slowly drip perfluor base sulfonic acid fluoride (30.2 grams, 93%, 0.07mol), then continue stirring reaction 6 hours, leave standstill, filter, filter cake proceeds to rotatory evaporator, in 70 DEG C of decompression dryings, obtain white powder crystal perfluor base sulfonic acid tetraethyl-amine (34.1 grams, 0.064mol) yield be 92%.
Embodiment 2
By triethylamine (12.1 grams, 0.12mol), Union carbide A-162 (17.8 grams, 0.1mol), 180 grams of chlorobenzenes add in 250ml three-necked bottle, stir, temperature controls 25 DEG C, slowly drip perfluor base sulfonic acid fluoride (43.2 grams, 93%, 0.1mol), complete rear continuation stirring reaction 8 hours, leaves standstill, filters, filter cake proceeds to rotatory evaporator, in 60 DEG C of decompression dryings, obtain white powder crystal perfluor base sulfonic acid tetraethyl-amine (47.6 grams, 0.09mol) yield be 90%.
Product fusing point test: 185.5 ~ 187.5 DEG C.
Its molecular weight 529 is determined by product MS figure.
Table 1. chromium fog inhibitor performance
Claims (4)
1. a chromium fog inhibitor, is characterized in that, chemical name is perfluor base sulfonic acid tetraethyl-amine.
2. a preparation method for chromium fog inhibitor, is characterized in that, concrete steps are:
1) triethylamine, Union carbide A-162 and inert solvent are mixed in the reactor, stir;
2) control temperature of reaction at 0 ~ 40 DEG C, drip perfluor base sulfonic acid fluoride;
3) temperature is kept, stirring reaction 6 hours;
4) obtain chromium fog inhibitor after separating and filtering, chemical name is perfluor base sulfonic acid tetraethyl-amine.
3. the preparation method of a kind of chromium fog inhibitor according to claim 1, is characterized in that, described inert solvent is chlorobenzene, benzene or isopropyl ether.
4. the preparation method of a kind of chromium fog inhibitor according to claim 1, it is characterized in that, in described reaction, the mol ratio of perfluor base sulfonic acid fluoride, triethylamine and Union carbide A-162 is 1:(1 ~ 1.8): (0.6 ~ 1.5).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510032333.7A CN104611733A (en) | 2015-01-22 | 2015-01-22 | Chromium fog inhibitor and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510032333.7A CN104611733A (en) | 2015-01-22 | 2015-01-22 | Chromium fog inhibitor and preparation method thereof |
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| Publication Number | Publication Date |
|---|---|
| CN104611733A true CN104611733A (en) | 2015-05-13 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
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| CN201510032333.7A Pending CN104611733A (en) | 2015-01-22 | 2015-01-22 | Chromium fog inhibitor and preparation method thereof |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110055564A (en) * | 2019-05-08 | 2019-07-26 | 天津格林泰格科技有限公司 | A kind of inhibition reagent of electrodeposited chromium mist |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4168277A (en) * | 1976-12-23 | 1979-09-18 | Bayer Aktiengesellschaft | Production of tetraethyl ammonium perfluoroalkyl sulphonate |
| CN104136535A (en) * | 2012-02-29 | 2014-11-05 | 沙特基础创新塑料Ip私人有限责任公司 | Thermoplastic polycarbonate copolymer compositions, methods of their manufacture, and articles thereof |
-
2015
- 2015-01-22 CN CN201510032333.7A patent/CN104611733A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4168277A (en) * | 1976-12-23 | 1979-09-18 | Bayer Aktiengesellschaft | Production of tetraethyl ammonium perfluoroalkyl sulphonate |
| CN104136535A (en) * | 2012-02-29 | 2014-11-05 | 沙特基础创新塑料Ip私人有限责任公司 | Thermoplastic polycarbonate copolymer compositions, methods of their manufacture, and articles thereof |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110055564A (en) * | 2019-05-08 | 2019-07-26 | 天津格林泰格科技有限公司 | A kind of inhibition reagent of electrodeposited chromium mist |
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Application publication date: 20150513 |