CN103588693A - Preparation method of trifluoroperacetic acid - Google Patents
Preparation method of trifluoroperacetic acid Download PDFInfo
- Publication number
- CN103588693A CN103588693A CN201310476620.8A CN201310476620A CN103588693A CN 103588693 A CN103588693 A CN 103588693A CN 201310476620 A CN201310476620 A CN 201310476620A CN 103588693 A CN103588693 A CN 103588693A
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- CN
- China
- Prior art keywords
- trifluoroacetic acid
- active oxygen
- oxygen loss
- preparation
- hydrogen peroxide
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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- XYPISWUKQGWYGX-UHFFFAOYSA-N 2,2,2-trifluoroethaneperoxoic acid Chemical compound OOC(=O)C(F)(F)F XYPISWUKQGWYGX-UHFFFAOYSA-N 0.000 title claims abstract description 33
- 238000002360 preparation method Methods 0.000 title claims abstract description 10
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims abstract description 36
- 150000008064 anhydrides Chemical class 0.000 claims abstract description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 10
- 150000002148 esters Chemical class 0.000 claims abstract description 7
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical group CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims description 11
- FKRCODPIKNYEAC-UHFFFAOYSA-N ethyl propionate Chemical compound CCOC(=O)CC FKRCODPIKNYEAC-UHFFFAOYSA-N 0.000 claims description 9
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 abstract description 27
- 239000001301 oxygen Substances 0.000 abstract description 27
- 229910052760 oxygen Inorganic materials 0.000 abstract description 27
- 238000000034 method Methods 0.000 abstract description 4
- 239000003054 catalyst Substances 0.000 abstract 1
- 230000002349 favourable effect Effects 0.000 abstract 1
- 238000010992 reflux Methods 0.000 abstract 1
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- YLFIGGHWWPSIEG-UHFFFAOYSA-N aminoxyl Chemical compound [O]N YLFIGGHWWPSIEG-UHFFFAOYSA-N 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000012847 fine chemical Substances 0.000 description 1
- 239000005457 ice water Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 125000000449 nitro group Chemical group [O-][N+](*)=O 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 239000007800 oxidant agent Substances 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 238000004659 sterilization and disinfection Methods 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
Landscapes
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a preparation method of trifluoroperacetic acid, which comprises the following steps: reacting 50% hydrogen peroxide with trifluoacetic anhydride, adding an ester catalyst, pressurizing, refluxing, and performing azeotropic water carrying to obtain the trifluoroperacetic acid. According to the invention, the preparation method of trifluoroperacetic acid is simple in operation process and low in danger coefficient; the active oxygen loss of the obtained trifluoroperacetic acid within 24 hours is 1%, the active oxygen loss within 48 hours is 3%, and the active oxygen loss within 72 hours is 7%; and the trifluoroperacetic acid has favorable heat stability.
Description
Technical field
The preparation method who the present invention relates to a kind of peroxy trifluoroacetic acid, belongs to field of fine chemical.
Background technology
Peroxy trifluoroacetic acid F3CCOOOH, be a kind of oxidation capacity much larger than the strong oxidizer of hydrogen peroxide, be mainly used in the fields such as the synthetic and SYNTHETIC OPTICAL WHITNER production of disinfection, chemical industry; During as oxygenant, can fall amino oxygen and change into nitro, oxidation capacity is extremely strong; But due to the poor heat stability of peroxy trifluoroacetic acid, need the used time now to join.At present, conventional collocation method, for trifluoacetic anhydride is dripped in the mixed solution of 90% hydrogen peroxide and methylene dichloride, stirs and makes in ice-water bath.Although peroxy trifluoroacetic acid Heat stability is good, productive rate that the hydrogen peroxide of 90% hydrogen peroxide ratio 30% makes are high, but 90% hydrogen peroxide treatment is got up with danger to a certain degree, and hydrogen peroxide and the heat release of trifluoacetic anhydride strong reaction, operate and have certain danger.
Summary of the invention
The object of this invention is to provide that a kind of operating process is simple, danger coefficient is low, the preparation method of Heat stability is good, peroxy trifluoroacetic acid that productive rate is high.
The present invention is achieved through the following technical solutions: 50% hydrogen peroxide reacts with trifluoacetic anhydride, adds ester class catalyzer, obtains peroxy trifluoroacetic acid after pressurization, backflow, azeotropic band water.
Further, the mol ratio of described 50% hydrogen peroxide, trifluoacetic anhydride and ester class catalyzer is 1:1:1-3.
Further, described ester class catalyzer is ethyl acetate and/or ethyl propionate.
The preparation method of peroxy trifluoroacetic acid of the present invention, operating process is simple, danger coefficient is low, active oxygen loss 7% in active oxygen loss 3%, 48h in active oxygen loss 1%, 48h in the peroxy trifluoroacetic acid 24h of acquisition, Heat stability is good.
Embodiment
Embodiment mono-: the hydrogen peroxide of 1 mole 50% and 1 mole of trifluoacetic anhydride are added in 1 mole of acetic acid ethyl ester, at 20-25 ℃, react 10-15min, after pressurization, backflow, azeotropic band water, obtain peroxy trifluoroacetic acid, by iodometry, measure active o content in the peroxy trifluoroacetic acid obtaining, result shows, active oxygen loss 11% in active oxygen loss 6%, 72h in active oxygen loss 2%, 48h in 24h.
Embodiment bis-: the hydrogen peroxide of 1 mole 50% and 1 mole of trifluoacetic anhydride are added in 1.5 mole of acetic acid ethyl esters, at 20-25 ℃, react 10-15min, after pressurization, backflow, azeotropic band water, obtain peroxy trifluoroacetic acid, by iodometry, measure active o content in the peroxy trifluoroacetic acid obtaining, result shows, active oxygen loss 10% in active oxygen loss 4%, 72h in active oxygen loss 1%, 48h in 24h.
Embodiment tri-: the hydrogen peroxide of 1 mole 50% and 1 mole of trifluoacetic anhydride are added in 3 mole of acetic acid ethyl esters, at 20-25 ℃, react 10-15min, after pressurization, backflow, azeotropic band water, obtain peroxy trifluoroacetic acid, by iodometry, measure active o content in the peroxy trifluoroacetic acid obtaining, result shows, active oxygen loss 8% in active oxygen loss 3%, 72h in active oxygen loss 1%, 48h in 24h.
Embodiment tetra-: the hydrogen peroxide of 1 mole 50% and 1 mole of trifluoacetic anhydride are added in 1 mole of ethyl propionate, at 20-25 ℃, react 10-15min, after pressurization, backflow, azeotropic band water, obtain peroxy trifluoroacetic acid, by iodometry, measure active o content in the peroxy trifluoroacetic acid obtaining, result shows, active oxygen loss 9% in active oxygen loss 4.4%, 72h in active oxygen loss 1.2%, 48h in 24h.
Embodiment five: the hydrogen peroxide of 1 mole 50% and 1 mole of trifluoacetic anhydride are added in 1.5 moles of ethyl propionates, at 20-25 ℃, react 10-15min, after pressurization, backflow, azeotropic band water, obtain peroxy trifluoroacetic acid, by iodometry, measure active o content in the peroxy trifluoroacetic acid obtaining, result shows, active oxygen loss 13% in active oxygen loss 7%, 72h in active oxygen loss 3%, 48h in 24h.
Embodiment six: the hydrogen peroxide of 1 mole 50% and 1 mole of trifluoacetic anhydride are added in 3 moles of ethyl propionates, at 20-25 ℃, react 10-15min, after pressurization, backflow, azeotropic band water, obtain peroxy trifluoroacetic acid, by iodometry, measure active o content in the peroxy trifluoroacetic acid obtaining, result shows, active oxygen loss 11% in active oxygen loss 3%, 72h in active oxygen loss 1%, 48h in 24h.
Embodiment seven: the hydrogen peroxide of 1 mole 50% and 1 mole of trifluoacetic anhydride are added in 1.5 mole of acetic acid ethyl esters and 1.5 moles of ethyl propionates, at 20-25 ℃, react 10-15min, after pressurization, backflow, azeotropic band water, obtain peroxy trifluoroacetic acid, by iodometry, measure active o content in the peroxy trifluoroacetic acid obtaining, result shows, active oxygen loss 10% in active oxygen loss 7%, 72h in active oxygen loss 4%, 48h in 24h.
Above-mentioned example just, for explanation technical conceive of the present invention and technical characterstic, can not limit the scope of the invention with this.Equivalent transformation or modification that all essence according to the present invention is done, within all should being encompassed in protection scope of the present invention.
Claims (3)
1. a preparation method for peroxy trifluoroacetic acid, is characterized in that, 50% hydrogen peroxide reacts with trifluoacetic anhydride, adds ester class catalyzer, obtains peroxy trifluoroacetic acid after pressurization, backflow, azeotropic band water.
2. the preparation method of peroxy trifluoroacetic acid according to claim 1, is characterized in that, the mol ratio of described 50% hydrogen peroxide, trifluoacetic anhydride and ester class catalyzer is 1:1:1-3.
3. the preparation method of peroxy trifluoroacetic acid according to claim 1, is characterized in that, described ester class catalyzer is ethyl acetate and/or ethyl propionate.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310476620.8A CN103588693A (en) | 2013-10-14 | 2013-10-14 | Preparation method of trifluoroperacetic acid |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310476620.8A CN103588693A (en) | 2013-10-14 | 2013-10-14 | Preparation method of trifluoroperacetic acid |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN103588693A true CN103588693A (en) | 2014-02-19 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201310476620.8A Pending CN103588693A (en) | 2013-10-14 | 2013-10-14 | Preparation method of trifluoroperacetic acid |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN103588693A (en) |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS62207281A (en) * | 1986-03-06 | 1987-09-11 | Shizuoka Univ | Production of alpha,beta-epoxyphosphine derivative |
| CN1299821A (en) * | 2000-12-22 | 2001-06-20 | 中国科学院上海有机化学研究所 | Lactone compound and its synthesis and use |
| JP2001213847A (en) * | 2000-01-27 | 2001-08-07 | Central Glass Co Ltd | Method for producing optically active 4,4,4-trifluoro-3- hydroxybutanoic acid ester derivative |
-
2013
- 2013-10-14 CN CN201310476620.8A patent/CN103588693A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS62207281A (en) * | 1986-03-06 | 1987-09-11 | Shizuoka Univ | Production of alpha,beta-epoxyphosphine derivative |
| JP2001213847A (en) * | 2000-01-27 | 2001-08-07 | Central Glass Co Ltd | Method for producing optically active 4,4,4-trifluoro-3- hydroxybutanoic acid ester derivative |
| CN1299821A (en) * | 2000-12-22 | 2001-06-20 | 中国科学院上海有机化学研究所 | Lactone compound and its synthesis and use |
Non-Patent Citations (1)
| Title |
|---|
| 吴姗姗: "《过氧三氟乙酸的制备》", 9 February 2015, article "过氧三氟乙酸的制备" * |
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| C02 | Deemed withdrawal of patent application after publication (patent law 2001) | ||
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Application publication date: 20140219 |