CN102617276A - Method for preparing trifluorochloroethylene by halothane - Google Patents
Method for preparing trifluorochloroethylene by halothane Download PDFInfo
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- CN102617276A CN102617276A CN2012100548159A CN201210054815A CN102617276A CN 102617276 A CN102617276 A CN 102617276A CN 2012100548159 A CN2012100548159 A CN 2012100548159A CN 201210054815 A CN201210054815 A CN 201210054815A CN 102617276 A CN102617276 A CN 102617276A
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- trifluorochloroethylene
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Abstract
The invention discloses a method for preparing trifluorochloroethylene by halothane, which includes the step: subjecting the halothane to a reaction with chlorine and hydrogen in a fixed bed reactor respectively, wherein the chlorine is subjected to a reaction at a position of an inlet of the a reactor, the hydrogen is subjected to the reaction at the position 3m away from the inlet of the reactor, the temperature of the catalytic reaction is between 200 DEG C and 300 DEG C, the molar ratio of halothane and the chlorine is 1: (3-5), and the molar ratio of the halothane and the hydrogen is 1: (1-2). According to the method for preparing the trifluorochloroethylene by the halothane, traditional process is abandoned by the whole technological process, the trifluorochloroethylene is prepared by directly subjecting the halothane to respectively reacting with the chlorine and the hydrogen at different positions of the fixed bed reactor, and thereby the method is low in cost and high in yield.
Description
Technical field
The present invention relates to a kind of method for preparing trifluorochloroethylene, particularly a kind of HFC-143a prepares the method for trifluorochloroethylene.
Background technology
Trifluorochloroethylene (CTFE) is the monomer of main fluoro-resin, Fluroplast-4 and viton.Voltalef is widely used in electronic technology and military aviation field.Especially excellent weathering resistance and the erosion resistance of fluoro-containing coating that with the trifluorochloroethylene is main body obtained using widely in bridge and building trade.
YO both at home and abroad is about 10,000 tons at present; Main production route is main raw material with the zellon; Process Sesquichloratum through chlorination, Sesquichloratum is fluoridized the preparation Freon 113, under the effect of zinc powder or hydrogen, removes chlorine by Freon 113 and obtains trifluorochloroethylene.
Because in traditional technology all is that first chlorination is removing chlorine, has obviously increased process step, thereby increase running cost.And when zinc powder removes chlorine, produce a large amount of zinc chloride waste residues, when handling waste residue, increase the production cost of trifluorochloroethylene.
When adopting hydrogen to remove chlorine, adopt expensive rare metal catalyzer, cause production cost higher.Like document US2685606, US2704777, EP0416015, US3333011 etc. are the operational path that removes chlorine after the chlorination of zellon elder generation.The shortcoming of the disclosed operational path of these documents is that the manufacturing cost of trifluorochloroethylene (CTFE) is higher, and the yield of whole process is about 75%, and is obviously on the low side.
Summary of the invention
The purpose of this invention is to provide the method that a kind of HFC-143a prepares trifluorochloroethylene, this method cost is low, yield is high.
In order to reach above-mentioned goal of the invention; Technical scheme of the present invention is: a kind of HFC-143a prepares the method for trifluorochloroethylene; Its by HFC-143a fixed-bed reactor respectively with chlorine, hydrogen reaction; Said chlorine gets into reaction at the Reactor inlet place, said hydrogen is getting into reaction from Reactor inlet 3m place.
Reaction formula is following:
FH
2C-CHF
2+3Cl
2+H
2→ClFC＝CF
2+5HCl
The temperature of catalyzed reaction is 200～300 ℃.Reaction pressure is a normal pressure, and reaction time is 10～15 seconds.Said HFC-143a and chlorine mol ratio 1: 3～5, said HFC-143a and hydrogen mol ratio 1: 1～2.
Said catalyzer is the mixture of aluminum chloride, platinum chloride, Palladous chloride and aluminum oxide; Wherein the weight percent of aluminum chloride is 12～30%; The weight percent of aluminum oxide is 66～85%, and the weight percent of platinum chloride is 1～3%, and the weight percent of Palladous chloride is 0.1～1%.
The whole technological process of the present invention avoids tradition to adopt zellon chlorination system Sesquichloratum; Sesquichloratum is fluoridized the system Freon 113; Freon 113 adopts the zinc powder dechlorination to prepare the process of trifluorochloroethylene; Directly prepare trifluorochloroethylene with chlorine and hydrogen reaction by HFC-143a respectively at the different positions of fixed-bed reactor, this method cost is low, and yield is high.
Embodiment
The testing tool of the product among the following embodiment adopts Agilent 6890N/5937 (GC/MS) gas chromatography appearance.
Embodiment 1
The mixture of filling 3 kilograms of aluminum chloride, platinum chloride, Palladous chloride and aluminum oxide in
stainless steel tubular type reactor drum wherein contains aluminum chloride 900 grams, aluminum oxide 1980 grams, platinum chloride 90 grams, Palladous chloride 30 grams.Reactor drum is warming up to 350 ℃, uses N
2Deactivated catalyst 10 hours is cooled to 230 ℃ then.The feed rate of HFC-143a is 1680 Grams Per Hours, and the feed rate of chlorine is that the feed rate of 4970 Grams Per Hours and hydrogen is 40 Grams Per Hours.After resultant in the reactor drum is directly washed through scale, behind molecular sieve, condensation and collection trifluorochloroethylene and sampling analysis.Obtaining purity is 98.5% trifluorochloroethylene, 2186.8 grams.Wherein yield is 92.45%.
Embodiment 2
The mixture of filling 3 kilograms of aluminum chloride, platinum chloride, Palladous chloride and aluminum oxide in
stainless steel tubular type reactor drum wherein contains aluminum chloride 477 grams, aluminum oxide 2490 grams, platinum chloride 30 grams, Palladous chloride 3 grams.Reactor drum is warming up to 350 ℃, uses N
2Deactivated catalyst 10 hours is cooled to 300 ℃ then.The feed rate of HFC-143a is 1680 Grams Per Hours, and the feed rate of chlorine is that the feed rate of 4259 Grams Per Hours and hydrogen is 55 Grams Per Hours.After resultant in the reactor drum is directly washed through scale, behind molecular sieve, condensation and collection trifluorochloroethylene and sampling analysis.Obtaining purity is 98.7% trifluorochloroethylene, 2185.3 grams.Wherein yield is 92.57%.
Embodiment 3
The mixture of filling 3 kilograms of aluminum chloride, platinum chloride, Palladous chloride and aluminum oxide in
stainless steel tubular type reactor drum wherein contains aluminum chloride 360 grams, aluminum oxide 2550 grams, platinum chloride 60 grams, Palladous chloride 30 grams.Reactor drum is warming up to 350 ℃, uses N
2Deactivated catalyst 10 hours is cooled to 200 ℃ then.The feed rate of HFC-143a is 1680 Grams Per Hours, and the feed rate of chlorine is that the feed rate of 7100 Grams Per Hours and hydrogen is 80 Grams Per Hours.After resultant in the reactor drum is directly washed through scale, behind molecular sieve, condensation and collection trifluorochloroethylene and sampling analysis.Obtaining purity is 98.7% trifluorochloroethylene, 2185.7 grams.Wherein yield is 92.5%.
The foregoing description does not limit the present invention in any way, and every employing is equal to the technical scheme that replacement or the mode of equivalent transformation obtain and all drops in protection scope of the present invention.
Claims (3)
1. a HFC-143a prepares the method for trifluorochloroethylene; It is characterized in that may further comprise the steps: by HFC-143a fixed-bed reactor respectively with chlorine, hydrogen reaction; Said chlorine gets into reaction at the Reactor inlet place, said hydrogen is getting into reaction from Reactor inlet 3m place, and the temperature of catalyzed reaction is 200～300 ℃; Said HFC-143a and chlorine mol ratio 1: 3～5, said HFC-143a and hydrogen mol ratio 1: 1～2.
2. said HFC-143a according to claim 1 prepares the method for trifluorochloroethylene; It is characterized in that: said catalyzer is the mixture of aluminum chloride, platinum chloride, Palladous chloride and aluminum oxide; Wherein the weight percent of aluminum chloride is 12～30%; The weight percent of aluminum oxide is 66～85%, and the weight percent of platinum chloride is 1～3%, and the weight percent of Palladous chloride is 0.1～1%.
3. said HFC-143a according to claim 1 prepares the method for trifluorochloroethylene, it is characterized in that: said reaction pressure is a normal pressure, and reaction time is 10～15 seconds.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201210054815.9A CN102617276B (en) | 2012-03-05 | 2012-03-05 | Method for preparing trifluorochloroethylene by halothane |
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| CN201210054815.9A CN102617276B (en) | 2012-03-05 | 2012-03-05 | Method for preparing trifluorochloroethylene by halothane |
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| CN102617276A true CN102617276A (en) | 2012-08-01 |
| CN102617276B CN102617276B (en) | 2014-04-02 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104140356A (en) * | 2014-07-16 | 2014-11-12 | 常熟三爱富氟化工有限责任公司 | Novel preparation method for green CTFE |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5120883A (en) * | 1991-08-26 | 1992-06-09 | E. I. Du Pont De Nemours And Company | Catalytic process for producing CCl3 CF3 |
| CN1065261A (en) * | 1991-01-25 | 1992-10-14 | 索尔维公司 | The catalyst composition for preparing the method for a chlorotrifluoroethylene and trifluoro-ethylene and be used for this method |
| US5498806A (en) * | 1990-05-31 | 1996-03-12 | Daikin Industries Ltd. | Process for preparing 1-chloro-1,2,2-trifluoroethylene or 1,2,2-trifluoroethylene |
| US7164050B2 (en) * | 2004-05-01 | 2007-01-16 | Honeywell International Inc. | Preparation of halo-olefin |
| CN101386560A (en) * | 2008-11-11 | 2009-03-18 | 常熟三爱富氟化工有限责任公司 | Process for preparing trifluorochloroethylene |
-
2012
- 2012-03-05 CN CN201210054815.9A patent/CN102617276B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5498806A (en) * | 1990-05-31 | 1996-03-12 | Daikin Industries Ltd. | Process for preparing 1-chloro-1,2,2-trifluoroethylene or 1,2,2-trifluoroethylene |
| CN1065261A (en) * | 1991-01-25 | 1992-10-14 | 索尔维公司 | The catalyst composition for preparing the method for a chlorotrifluoroethylene and trifluoro-ethylene and be used for this method |
| US5120883A (en) * | 1991-08-26 | 1992-06-09 | E. I. Du Pont De Nemours And Company | Catalytic process for producing CCl3 CF3 |
| US7164050B2 (en) * | 2004-05-01 | 2007-01-16 | Honeywell International Inc. | Preparation of halo-olefin |
| CN101386560A (en) * | 2008-11-11 | 2009-03-18 | 常熟三爱富氟化工有限责任公司 | Process for preparing trifluorochloroethylene |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104140356A (en) * | 2014-07-16 | 2014-11-12 | 常熟三爱富氟化工有限责任公司 | Novel preparation method for green CTFE |
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| CN102617276B (en) | 2014-04-02 |
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