CN102260160A - Method for simultaneously preparing carbonyl fluoride and trifluoroaceticfluoride - Google Patents
Method for simultaneously preparing carbonyl fluoride and trifluoroaceticfluoride Download PDFInfo
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- CN102260160A CN102260160A CN2010101824180A CN201010182418A CN102260160A CN 102260160 A CN102260160 A CN 102260160A CN 2010101824180 A CN2010101824180 A CN 2010101824180A CN 201010182418 A CN201010182418 A CN 201010182418A CN 102260160 A CN102260160 A CN 102260160A
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Abstract
The invention relates to a method for simultaneously preparing carbonyl fluoride and trifluoroacetyl fluoride, and belongs to the field of chemical synthesis. The method for simultaneously preparing the carbonyl fluoride and the trifluoroacetyl fluoride comprises the following step of: performing contact reaction on oxygen and hexafluoropropylene gas in the presence of a catalyst in a reactor, wherein the catalyst is silver oxide, active carbon supported silver oxide or alumina supported silver oxide. The reaction is easily controlled, reaction conditions are mild, the conversion rate is high, the carbonyl fluoride and the trifluoroacetyl fluoride can be simultaneously prepared by one-step reaction, and the method is suitable for batch preparation of the carbonyl fluoride and the trifluoroacetyl fluoride.
Description
Technical field
The present invention relates to technical field of chemical synthesis, particularly, the present invention relates to a kind of preparation method who prepares carbonyl fluoride and Trifluoroacetyl fluoride simultaneously.
Background technology
Full acyl fluorides such as carbonyl fluoride, Trifluoroacetyl fluoride can be used for electron trade clean-out system, etching reagent, pesticide intermediate, fluorine material monomer etc., is a kind of important fluorochemicals.
PCT/2006/319652 discloses a kind of method that has tetrafluoroethylene and oxygen reaction to prepare carbonyl fluoride; PCT/JP2005/023175 discloses the method for a kind of carbon monoxide and the synthetic carbonyl fluoride of fluorine gas reaction; CN1121064A disclose a kind of under chromium and Mg catalyst catalysis the method for anhydrous HF and trifluoroacetyl chloride prepared in reaction Trifluoroacetyl fluoride; US4374782A discloses a kind of Perfluoroacetone dimer at Ag
2The method that under alkaline metal fluoride cpd catalysis, prepares Trifluoroacetyl fluoride under the oxygenant effects such as O; GB8625575A discloses the method for a kind of tetrafluoroethylene and oxygen synthetic Trifluoroacetyl fluoride under silver suboxide catalysis.More than these methods be single preparation method as carbonyl fluoride or Trifluoroacetyl fluoride, can not be used for preparing simultaneously these two kinds of compounds.
Document V.S.Alzoba, V.G.Vereskunov and V.I.Tupikov, Khim.Vys.Energ.-17 (1983) 448, reported that a kind of R 1216 and oxygen prepare the method for carbonyl fluoride and Trifluoroacetyl fluoride under action of ultraviolet light; Document A.Lenziand A.Mele, Nature 205 (1965) 1104. have reported that R 1216 and oxygen excite the method for preparing carbonyl fluoride and Trifluoroacetyl fluoride down at gamma-rays; Document D.Sianesi, G.Bernardi and G.Moggi, Fr.Pat.1 531 902 (1966). reported that R 1216 and ozone reaction prepare the method for carbonyl fluoride and Trifluoroacetyl fluoride; Document J.POLA, Z.CHVATAL, J.Fluor。Chem。, 37 (1987) 197-213 have reported that R 1216 and oxygen excite the method for preparing carbonyl fluoride and Trifluoroacetyl fluoride down at the infrared laser of SF6 sensitivity.Aforesaid method can prepare carbonyl fluoride and Trifluoroacetyl fluoride simultaneously, yet preparation technology's more complicated is not suitable for industrialization.
Summary of the invention
The purpose of this invention is to provide a kind of method for preparing carbonyl fluoride and Trifluoroacetyl fluoride simultaneously, this easy control of reaction, and mild condition, transformation efficiency height.
The preparation method who prepares carbonyl fluoride and Trifluoroacetyl fluoride simultaneously, with oxygen and R 1216 (HFP) gas under the catalyzer condition in reactor contact reacts, described catalyzer is silver suboxide, activated carbon supported silver suboxide or the silver suboxide of alumina load.
Described temperature of reaction is 150 ℃～500 ℃.
Preferred 200 ℃～450 ℃, more preferably 300 ℃.
The mol ratio of described oxygen and R 1216 (HFP) is (0.2～5): 1.
Preferred 1: 1.
Described oxygen and R 1216 duration of contact in reactor is 0.1 second to 200 seconds,
Be preferably 10 seconds to 100 seconds, most preferably be 50 seconds.Usually, at high temperature adopt short duration of contact, must adopt long duration of contact at low temperatures.
Described reactor is fixed bed, fluidized-bed or moving-burden bed reactor.
The material of described reactor is stainless steel, nickel material or nickel-base alloy.
The present invention finds that oxygen and R 1216 can leniently react, and are suitable for suitability for industrialized production under the effect of the catalyzer such as silver suboxide of silver suboxide, gac or alumina load.
The ratio that carbonyl fluoride and Trifluoroacetyl fluoride generate can be regulated by the duration of contact of mol ratio, oxygen and the R 1216 of temperature of reaction, oxygen and R 1216.Temperature of reaction is high more, and the ratio that generates carbonyl fluoride is big more; The mol ratio of oxygen and R 1216 is big more, and the ratio that generates carbonyl fluoride is big more; The duration of contact of oxygen and R 1216 is long more, helps the generation of carbonyl fluoride more.
Method of the present invention has been found the new catalyzer that is suitable for, and has overcome problems such as complex process of the prior art, just can prepare carbonyl fluoride and Trifluoroacetyl fluoride simultaneously by single step reaction, is suitable for the preparation in enormous quantities of carbonyl fluoride and Trifluoroacetyl fluoride.
Embodiment
Below the invention will be further described for the description by embodiment, but this is not to be limitation of the present invention, those skilled in the art are according to basic thought of the present invention, can make various modifications or improvement, but only otherwise break away from basic thought of the present invention, all within the scope of the present invention.
Embodiment 1
With 50ml/min oxygen with the 50ml/min R 1216 is gas pre-mixed closes, is preheating to 200 ℃, in the nickel reactant pipe by external diameter Φ 19mm, long 300mm, reaction tubes is heated to 250 ℃, filling 40ml silver suboxide in the reaction tubes.The reaction tubes exit gas detects its composition with gas chromatograph.The result lists in the table 1.
Embodiment 2
With 60ml/min oxygen with the 50ml/min R 1216 is gas pre-mixed closes, is preheating to 200 ℃, in the nickel reactant pipe by external diameter Φ 19mm, long 300mm, reaction tubes is heated to 250 ℃, filling 40ml 10%Ag in the reaction tubes
2The O/ gac (be activated carbon supported silver suboxide, silver suboxide account for vehicle weight 10%).The reaction tubes exit gas detects its composition with gas chromatograph.The result lists in the table 1.
Embodiment 3
With 30ml/min oxygen with the 30ml/min R 1216 is gas pre-mixed closes, is preheating to 200 ℃, in the nickel reactant pipe by external diameter Φ 19mm, long 300mm, reaction tubes is heated to 250 ℃, loads 40ml10%Ag in the reaction tubes
2O/Al
2O
3(be the silver suboxide of alumina load, silver suboxide account for vehicle weight 10%).The reaction tubes exit gas detects its composition with gas chromatograph.The result lists in the table 1.
Embodiment 4
With 50ml/min oxygen with the 50ml/min R 1216 is gas pre-mixed closes, is preheating to 300 ℃, in the nickel reactant pipe by external diameter Φ 19mm, long 300mm, reaction tubes is heated to 350 ℃, filling 40ml silver suboxide in the reaction tubes.The reaction tubes exit gas detects its composition with gas chromatograph.The result lists in the table 1.
Table 1
| Numbering | O 2，％ | COF 2，％ | CF 3COF，％ | CF 3CF＝CF 2，％ | Other, % |
| Embodiment 1 | 0.3 | 50.1 | 47.8 | 0.5 | 1.3 |
| Embodiment 2 | 8.5 | 48.8 | 40.8 | 0.3 | 1.6 |
| Embodiment 3 | 0.2 | 52.3 | 45.7 | 0.3 | 1.5 |
| Embodiment 4 | 0.1 | 56.8 | 42.0 | 0.1 | 1.0 |
Claims (10)
1. the preparation method who prepares carbonyl fluoride and Trifluoroacetyl fluoride simultaneously, with oxygen and R 1216 gas under the catalyzer condition in reactor contact reacts, described catalyzer is silver suboxide, activated carbon supported silver suboxide or the silver suboxide of alumina load.
2. preparation method according to claim 1, described temperature of reaction are 150 ℃～500 ℃.
3. preparation method according to claim 2, described temperature of reaction are 200 ℃～450 ℃.
4. preparation method according to claim 3, described temperature of reaction are 300 ℃.
5. preparation method according to claim 1, the mol ratio of described oxygen and R 1216 are (0.2～5): 1.
6. preparation method according to claim 5, the mol ratio of described oxygen and R 1216 are 1: 1.
7. preparation method according to claim 1, the described catalytic time is 0.1 second to 200 seconds.
8. preparation method according to claim 7, the described catalytic time is 10 seconds to 100 seconds.
9. preparation method according to claim 8, the described catalytic time is 50 seconds.
10. preparation method according to claim 1, described reactor is fixed bed, fluidized-bed or moving-burden bed reactor, the material of described reactor is stainless steel, nickel material or nickel-base alloy.
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| Application Number | Priority Date | Filing Date | Title |
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| CN2010101824180A CN102260160A (en) | 2010-05-26 | 2010-05-26 | Method for simultaneously preparing carbonyl fluoride and trifluoroaceticfluoride |
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| CN2010101824180A CN102260160A (en) | 2010-05-26 | 2010-05-26 | Method for simultaneously preparing carbonyl fluoride and trifluoroaceticfluoride |
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Cited By (9)
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| CN104353454A (en) * | 2014-10-14 | 2015-02-18 | 四川大学 | Preparation method of silver oxide as ultraviolet/visible/infrared photocatalyst |
| CN106946669A (en) * | 2017-03-21 | 2017-07-14 | 国家电网公司 | A kind of environmentally friendly insulating gas joint production process and industrial production device |
| CN106986757A (en) * | 2017-04-24 | 2017-07-28 | 国家电网公司 | A kind of environmentally friendly insulating gas production technology and industrial installation |
| CN107311138A (en) * | 2017-07-21 | 2017-11-03 | 淄博飞源化工有限公司 | A kind of method that utilization aromatic isocyanatcs manufacture carbonyl fluoride |
| CN108314614A (en) * | 2018-04-20 | 2018-07-24 | 北京宇极科技发展有限公司 | The method that gas phase prepares pentafluoroethyl group perfluoroisopropyl ketone |
| CN109503423A (en) * | 2018-11-30 | 2019-03-22 | 天津市长芦化工新材料有限公司 | Hexafluoropropylene dimmer prepares the method and perfluor isobutyronitrile and application of perfluor isobutyronitrile |
| CN109607507A (en) * | 2018-12-24 | 2019-04-12 | 天津市长芦化工新材料有限公司 | Perfluorochemical cracking prepares the method and carbonyl fluoride of carbonyl fluoride |
| WO2020098493A1 (en) * | 2018-11-15 | 2020-05-22 | 四川科源精诚新材料科技有限公司 | Perfluoro surfactant and preparation method therefor |
| CN114620705A (en) * | 2022-02-24 | 2022-06-14 | 浙江诺亚氟化工有限公司 | Method for preparing high-purity carbonyl fluoride from hexafluoropropylene oxide |
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2010
- 2010-05-26 CN CN2010101824180A patent/CN102260160A/en active Pending
Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104353454A (en) * | 2014-10-14 | 2015-02-18 | 四川大学 | Preparation method of silver oxide as ultraviolet/visible/infrared photocatalyst |
| CN106946669A (en) * | 2017-03-21 | 2017-07-14 | 国家电网公司 | A kind of environmentally friendly insulating gas joint production process and industrial production device |
| WO2018171305A1 (en) * | 2017-03-21 | 2018-09-27 | 国家电网公司 | Process and industrialized production device for co-production of environmentally friendly insulating gases |
| CN106946669B (en) * | 2017-03-21 | 2020-09-15 | 国家电网公司 | Environment-friendly insulating gas co-production process and industrial production device |
| CN106986757A (en) * | 2017-04-24 | 2017-07-28 | 国家电网公司 | A kind of environmentally friendly insulating gas production technology and industrial installation |
| CN107311138A (en) * | 2017-07-21 | 2017-11-03 | 淄博飞源化工有限公司 | A kind of method that utilization aromatic isocyanatcs manufacture carbonyl fluoride |
| CN107311138B (en) * | 2017-07-21 | 2019-05-21 | 淄博飞源化工有限公司 | A method of carbonyl fluoride is manufactured using aromatic isocyanatcs |
| CN108314614A (en) * | 2018-04-20 | 2018-07-24 | 北京宇极科技发展有限公司 | The method that gas phase prepares pentafluoroethyl group perfluoroisopropyl ketone |
| CN108314614B (en) * | 2018-04-20 | 2021-03-12 | 北京宇极科技发展有限公司 | Method for preparing pentafluoroethyl perfluoroisopropyl ketone in gas phase |
| WO2020098493A1 (en) * | 2018-11-15 | 2020-05-22 | 四川科源精诚新材料科技有限公司 | Perfluoro surfactant and preparation method therefor |
| CN109503423A (en) * | 2018-11-30 | 2019-03-22 | 天津市长芦化工新材料有限公司 | Hexafluoropropylene dimmer prepares the method and perfluor isobutyronitrile and application of perfluor isobutyronitrile |
| CN109607507A (en) * | 2018-12-24 | 2019-04-12 | 天津市长芦化工新材料有限公司 | Perfluorochemical cracking prepares the method and carbonyl fluoride of carbonyl fluoride |
| CN114620705A (en) * | 2022-02-24 | 2022-06-14 | 浙江诺亚氟化工有限公司 | Method for preparing high-purity carbonyl fluoride from hexafluoropropylene oxide |
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Application publication date: 20111130 |