CN112500285B - Continuous preparation method of trifluoroacetyl fluoride - Google Patents
Continuous preparation method of trifluoroacetyl fluoride Download PDFInfo
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- CN112500285B CN112500285B CN202011328073.5A CN202011328073A CN112500285B CN 112500285 B CN112500285 B CN 112500285B CN 202011328073 A CN202011328073 A CN 202011328073A CN 112500285 B CN112500285 B CN 112500285B
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- DCEPGADSNJKOJK-UHFFFAOYSA-N 2,2,2-trifluoroacetyl fluoride Chemical compound FC(=O)C(F)(F)F DCEPGADSNJKOJK-UHFFFAOYSA-N 0.000 title claims abstract description 40
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 239000003054 catalyst Substances 0.000 claims abstract description 45
- 238000006243 chemical reaction Methods 0.000 claims abstract description 34
- 239000007789 gas Substances 0.000 claims abstract description 31
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims abstract description 26
- 229910000040 hydrogen fluoride Inorganic materials 0.000 claims abstract description 24
- 239000003153 chemical reaction reagent Substances 0.000 claims abstract description 22
- 230000000694 effects Effects 0.000 claims abstract description 14
- -1 trifluoroethyl compound Chemical class 0.000 claims abstract description 8
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 7
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 7
- OBAJXDYVZBHCGT-UHFFFAOYSA-N tris(pentafluorophenyl)borane Chemical compound FC1=C(F)C(F)=C(F)C(F)=C1B(C=1C(=C(F)C(F)=C(F)C=1F)F)C1=C(F)C(F)=C(F)C(F)=C1F OBAJXDYVZBHCGT-UHFFFAOYSA-N 0.000 claims abstract description 6
- 238000010574 gas phase reaction Methods 0.000 claims abstract description 5
- 238000001816 cooling Methods 0.000 claims abstract description 3
- BPKXQSLAVGBZEM-UHFFFAOYSA-N tris[3,5-bis(trifluoromethyl)phenyl]borane Chemical compound FC(F)(F)C1=CC(C(F)(F)F)=CC(B(C=2C=C(C=C(C=2)C(F)(F)F)C(F)(F)F)C=2C=C(C=C(C=2)C(F)(F)F)C(F)(F)F)=C1 BPKXQSLAVGBZEM-UHFFFAOYSA-N 0.000 claims abstract description 3
- DTQVDTLACAAQTR-UHFFFAOYSA-N Trifluoroacetic acid Chemical compound OC(=O)C(F)(F)F DTQVDTLACAAQTR-UHFFFAOYSA-N 0.000 claims description 44
- QAEDZJGFFMLHHQ-UHFFFAOYSA-N trifluoroacetic anhydride Chemical compound FC(F)(F)C(=O)OC(=O)C(F)(F)F QAEDZJGFFMLHHQ-UHFFFAOYSA-N 0.000 claims description 8
- 238000003682 fluorination reaction Methods 0.000 claims description 5
- 239000002994 raw material Substances 0.000 claims description 5
- 239000012025 fluorinating agent Substances 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 4
- 238000010924 continuous production Methods 0.000 claims description 3
- 238000009834 vaporization Methods 0.000 claims 1
- 230000008016 vaporization Effects 0.000 claims 1
- 238000011084 recovery Methods 0.000 abstract description 9
- 239000000126 substance Substances 0.000 abstract description 9
- 239000002904 solvent Substances 0.000 abstract description 6
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 abstract description 5
- 239000011737 fluorine Substances 0.000 abstract description 5
- 229910052731 fluorine Inorganic materials 0.000 abstract description 5
- 239000007788 liquid Substances 0.000 abstract description 2
- 239000002699 waste material Substances 0.000 abstract description 2
- 238000002309 gasification Methods 0.000 description 23
- 238000003860 storage Methods 0.000 description 11
- 238000000926 separation method Methods 0.000 description 10
- 239000012043 crude product Substances 0.000 description 7
- 238000005868 electrolysis reaction Methods 0.000 description 5
- 239000005457 ice water Substances 0.000 description 4
- 239000000047 product Substances 0.000 description 4
- 238000003756 stirring Methods 0.000 description 4
- WFDIJRYMOXRFFG-UHFFFAOYSA-N Acetic anhydride Chemical compound CC(=O)OC(C)=O WFDIJRYMOXRFFG-UHFFFAOYSA-N 0.000 description 3
- 150000003973 alkyl amines Chemical class 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 150000001875 compounds Chemical class 0.000 description 3
- 238000001704 evaporation Methods 0.000 description 3
- 230000008020 evaporation Effects 0.000 description 3
- 239000000945 filler Substances 0.000 description 3
- 238000000034 method Methods 0.000 description 3
- 230000007704 transition Effects 0.000 description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000005034 decoration Methods 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 238000012856 packing Methods 0.000 description 2
- NROKBHXJSPEDAR-UHFFFAOYSA-M potassium fluoride Chemical compound [F-].[K+] NROKBHXJSPEDAR-UHFFFAOYSA-M 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- PNQBEPDZQUOCNY-UHFFFAOYSA-N trifluoroacetyl chloride Chemical group FC(F)(F)C(Cl)=O PNQBEPDZQUOCNY-UHFFFAOYSA-N 0.000 description 2
- LRMSQVBRUNSOJL-UHFFFAOYSA-N 2,2,3,3,3-pentafluoropropanoic acid Chemical compound OC(=O)C(F)(F)C(F)(F)F LRMSQVBRUNSOJL-UHFFFAOYSA-N 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- IDWDYJLTAISHRH-UHFFFAOYSA-N [3,5-bis(trifluoromethyl)phenyl]borane Chemical compound BC1=CC(=CC(=C1)C(F)(F)F)C(F)(F)F IDWDYJLTAISHRH-UHFFFAOYSA-N 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000005886 esterification reaction Methods 0.000 description 1
- 229920002313 fluoropolymer Polymers 0.000 description 1
- 239000004811 fluoropolymer Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 235000003270 potassium fluoride Nutrition 0.000 description 1
- 239000011698 potassium fluoride Substances 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 239000007787 solid Chemical class 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000001308 synthesis method Methods 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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Classifications
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/58—Preparation of carboxylic acid halides
- C07C51/60—Preparation of carboxylic acid halides by conversion of carboxylic acids or their anhydrides or esters, lactones, salts into halides with the same carboxylic acid part
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/58—Preparation of carboxylic acid halides
- C07C51/64—Separation; Purification; Stabilisation; Use of additives
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention belongs to the field of fluorine chemical industry, and particularly relates to a continuous preparation method of trifluoroacetyl fluoride, which comprises the following steps: 1) After being gasified, the trifluoroethyl compound and the fluorinating reagent are mixed with anhydrous hydrogen fluoride and then are introduced into a packed column filled with a high-activity catalyst for gas phase reaction; 2) Cooling and rectifying the gas obtained after the reaction to obtain trifluoroacetyl fluoride with the purity of more than 99.9 percent; wherein the high-activity catalyst is a supported catalyst which takes active carbon as a carrier and contains catalyst active components; the active component of the catalyst is one of tris (pentafluorophenyl) borane or tris [3,5-bis (trifluoromethyl) phenyl ] borane. The preparation process of the invention is a gas phase reaction, which avoids the recovery treatment of solvent and the pollution of waste liquid, and generates high-value chemical intermediate trifluoroacetyl fluoride under the action of catalyst, and the invention has the advantages of high product yield, mild reaction conditions, continuous reaction, simple operation of reaction process and high efficiency.
Description
Technical Field
The invention belongs to the field of fluorine chemical industry, and particularly relates to a continuous preparation method of trifluoroacetyl fluoride.
Background
Perfluoroacetyl fluoride, also known as trifluoroacetyl fluoride, has the formula: CF3COF, boiling point: colorless gas at the normal temperature of-59 ℃, is a compound containing-COF functional groups, and is not easy to store and transport; has high activity, is easy to generate esterification reaction with alcohol, generates HF gas and perfluoropropionic acid when meeting water, and can be used for preparing various compounds.
Perfluoroacetyl fluoride is an important compound which is paid much attention to as an intermediate for chemically synthesizing a perfluoroalkylated product, such as a polymerization monomer necessary for preparing a high-purity fluoropolymer, and derivatives thereof are widely applied to various fields. The prior preparation method of perfluoroacetyl fluoride mainly comprises a trifluoroacetyl chloride substitution method, a trifluoroacetic acid conversion method, an acetic anhydride electrolysis method and the like. US5672748 trifluoroacetyl chloride substituted for trifluoroacetyl fluoride requires the use of hydrofluoric acid and the apparatus is complex; the electrolysis synthesis method of US2717871 is cheap in raw materials, but has low electrolysis efficiency, is difficult to avoid low product purity caused by electrolysis impurities, is expensive in manufacturing cost of an electrolysis polar plate, and is not beneficial to industrial implementation due to high equipment cost.
Disclosure of Invention
The invention aims to overcome the defects in the prior art and provide a continuous preparation method of trifluoroacetyl fluoride.
In order to achieve the purpose, the invention adopts the technical scheme that:
a continuous preparation method of trifluoroacetyl fluoride comprises the following steps:
1) After being gasified, the trifluoroethyl compound and the fluorinating reagent are mixed with anhydrous hydrogen fluoride and then are introduced into a packed column filled with a high-activity catalyst for gas phase reaction; the introduction rate of the vaporized trifluoroethyl compound, the fluorinated reagent and the anhydrous hydrogen fluoride is 1;
2) Cooling and rectifying the gas obtained after the reaction to obtain trifluoroacetyl fluoride with the purity of more than 99.9 percent;
wherein the high-activity catalyst is a supported catalyst which takes active carbon as a carrier and contains catalyst active components; the active component of the catalyst is one of tris (pentafluorophenyl) borane or tris [3,5-bis (trifluoromethyl) phenyl ] borane.
Preferably, the gas in the step 2) is cooled and passes through double cold traps, the first cold trap is used for recovering the raw material trifluoroethyl compound, the fluorinating agent and anhydrous hydrogen fluoride, and the second cold trap is used for collecting crude trifluoroacetyl fluoride.
The temperature of the packed column is 30-100 ℃.
The trifluoroethyl compound is one of trifluoroacetic acid and trifluoroacetic anhydride.
The fluorinating agent is FCHFCF 2 N(CH 3 ) 2 、FCHFCF 2 N(C 2 H 5 ) 2 、ClCHFCF 2 N(CH 3 ) 2 、ClCHFCF 2 N(C 2 H 5 ) 2 、CF 3 OCHFCF 2 N(C 2 H 5 ) 2 Or a mixture thereof.
The gasification temperature of the fluorinating reagent is 50-100 ℃.
Compared with the prior art, the invention has the beneficial effects that:
the preparation process of the invention is firstly a gas phase reaction, which avoids the recovery treatment of solvent and the pollution of waste liquid, and generates high-value chemical intermediate trifluoroacetyl fluoride under the action of catalyst, the product yield is high, the reaction condition is mild, and meanwhile, the reaction process is a continuous reaction, the operation is simple, and the efficiency is high; the final purification process is simple, the product purity is more than 99 percent, the large-scale industrial production is easy, and the storage and transportation probability of trifluoroacetyl fluoride can be effectively reduced.
Description of the drawings:
FIG. 1 is an overall schematic view of a continuous production apparatus;
FIG. 2 is an overall schematic of a rectification column unit.
Detailed Description
In order to make the technical solutions of the present invention better understood by those skilled in the art, the present invention will be further described in detail with reference to the accompanying drawings and preferred embodiments.
Example 1: the temperature of an anhydrous hydrogen fluoride gasification chamber is 25 ℃, the temperature of a trifluoroacetic acid gasification chamber is 75 ℃, and a fluorinating reagent ClCHFCF 2 N(C 2 H 5 ) 2 The temperature of the gasification chamber is 40 ℃, after the anhydrous hydrogen fluoride, the trifluoroacetic acid and the fluorinating reagent are gasified, the gas quality controller is used for controlling the ratio of the amount of the gas substances: 1, feeding the mixed gas into a mixed gas transition chamber, wherein the obtained mixed gas slowly passes through a catalyst filler column from bottom to top, and the column temperature is 80 ℃; the packed column is filled with a high-activity catalyst, wherein the high-activity catalyst is a supported catalyst which takes active carbon as a carrier and contains catalyst active components; the active component of the catalyst is tris (pentafluorophenyl) borane. And (3) removing trifluoroacetic acid, a fluorinating reagent and hydrogen fluoride from the gas obtained from the upper end outlet of the catalyst packed column by a first cold trap, wherein the first cold trap is ice water bath at 0 ℃, the first cold trap is a cold trap at-75 ℃, crude perfluoroacetyl fluoride is collected by a second cold trap, the obtained perfluoroacetyl fluoride is subjected to low-temperature rectification to obtain perfluoroacetyl fluoride with the purity of more than 99.9%, and the comprehensive yield of the reaction reaches 82.3%.
Wherein, the adopted continuous preparation device is shown in figure 1 and comprises a raw material tank unit, a gasification unit, a reaction unit, a recovery unit and a rectification unit which are communicated in sequence; the raw material tank unit comprises a trifluoroacetic acid storage tank 1, a fluorine-containing alkylamine fluorination reagent storage tank 2 and an anhydrous hydrogen fluoride storage tank 3; the gasification unit comprises a trifluoroacetic acid gasification chamber 4, a fluorine-containing alkylamine fluorination reagent gasification chamber 5 and an anhydrous hydrogen fluoride gasification chamber 6 which are respectively communicated with a trifluoroacetic acid storage tank 1, a fluorine-containing alkylamine fluorination reagent storage tank 2 and an anhydrous hydrogen fluoride storage tank 3; a mixed gasification chamber 7 is arranged between the gasification unit and the reaction unit; the reaction unit comprises a reaction tube 8 loaded with a catalyst and a heating jacket 9 arranged outside the reaction tube;
the recovery unit comprises a first cold trap 10 and a second cold trap 12 which are communicated in sequence, and a recovery gasification chamber 11 connected with the first cold trap; the recovery gasification chamber 11 is communicated with the mixing gasification chamber 7.
The second cold trap is connected with the rectifying tower unit 13; the rectifying tower unit comprises a separation chamber 132, a heavy component recovery chamber 131 which is arranged at the lower end of the separation chamber and communicated with the separation chamber, and a rectifying tower 134 which is arranged at the upper end of the separation chamber and communicated with the separation chamber; a crude product inlet is formed in one side of the separation chamber, and an evaporation plate is arranged on the other side, corresponding to the crude product inlet, of the separation chamber; the crude product inlet is communicated with the second cold trap; the evaporation plate is connected with a temperature control element 136; a pressurizing nozzle 133 is arranged at the crude product inlet; the crude product enters a separation chamber through a pressurizing nozzle to realize primary separation, the temperature of an evaporation plate is controlled to be-55-0 ℃, light components in the crude product enter a rectifying tower, a heavy component fluorination reagent, HF and trifluoroacetic acid enter a heavy component recovery chamber to realize primary separation of the crude product, the temperature of the heavy component recovery chamber is set to be 0 ℃, and the top end of the rectifying tower is communicated with a cold trap 14 through a pipeline. The following examples were carried out using the same apparatus as in the present example.
Example 2: the temperature of an anhydrous hydrogen fluoride gasification chamber is 25 ℃, the temperature of a trifluoroacetic acid gasification chamber is 75 ℃, and a fluorinating reagent ClCHFCF 2 N(C 2 H 5 ) 2 The temperature of the gasification chamber is 40 ℃, after the anhydrous hydrogen fluoride, the trifluoroacetic acid and the fluorinating reagent are gasified, the gas quality controller is used for controlling the ratio of the amount of the gas substances: 1, 1The obtained mixed gas slowly passes through a catalyst packing column from bottom to top, and the column temperature is 80 ℃; the packed column is filled with a high-activity catalyst, wherein the high-activity catalyst is a supported catalyst which takes active carbon as a carrier and contains catalyst active components; the active component of the catalyst is tri [3,5-bis (trifluoromethyl) phenyl]Borane. And (3) removing trifluoroacetic acid, a fluorinating reagent and hydrogen fluoride from the gas obtained from the upper end outlet of the catalyst packed column by a first cold trap, collecting crude perfluoroacetyl fluoride by a second cold trap after the first cold trap is in a 0-DEG ice-water bath, and rectifying the obtained perfluoroacetyl fluoride at low temperature to obtain the perfluoroacetyl fluoride with the purity of more than 99.9%, wherein the comprehensive yield of the reaction reaches 80.3%.
Example 3: the temperature of an anhydrous hydrogen fluoride gasification chamber is 25 ℃, the temperature of a trifluoroacetic acid gasification chamber is 75 ℃, and a fluorinating reagent ClCHFCF 2 N(C 2 H 5 ) 2 The temperature of a gasification chamber is 40 ℃, and after the anhydrous hydrogen fluoride, the trifluoroacetic acid and the fluorinating reagent are gasified, the gas quality controller is used for controlling the ratio of the amount of the gas substances: 1, feeding the mixed gas into a mixed gas transition chamber, wherein the obtained mixed gas slowly passes through a catalyst filler column from bottom to top, and the column temperature is 80 ℃; the packed column is filled with a high-activity catalyst, wherein the high-activity catalyst is a supported catalyst which takes active carbon as a carrier and contains catalyst active components; the active component of the catalyst is alumina. And (3) removing trifluoroacetic acid, a fluorinating reagent and hydrogen fluoride from the gas obtained from the upper end outlet of the catalyst packed column by a first cold trap, collecting crude perfluoroacetyl fluoride by a second cold trap after the first cold trap is in a 0-DEG ice-water bath, and rectifying the obtained perfluoroacetyl fluoride at low temperature to obtain the perfluoroacetyl fluoride with the purity of more than 99.9%, wherein the comprehensive yield of the reaction reaches 62.5%.
Example 4: the temperature of the anhydrous hydrogen fluoride gasification chamber is 25 ℃, the temperature of the trifluoroacetic anhydride gasification chamber is 65 ℃, and the fluorinating reagent ClCHFCF 2 N(C 2 H 5 ) 2 The temperature of the gasification chamber is 40 ℃, after the anhydrous hydrogen fluoride, the trifluoroacetic anhydride and the fluorinating reagent are gasified, the gas quality controller is used for controlling the ratio of the amount of the gas substances: 1, feeding the mixed gas into a mixed gas transition chamber, wherein the obtained mixed gas slowly passes through a catalyst filler column from bottom to top, and the column temperature is 80 ℃; the packing column is internally provided with a heightThe high-activity catalyst is a supported catalyst which takes active carbon as a carrier and contains a catalyst active component; the active component of the catalyst is tris (pentafluorophenyl) borane. And (3) removing trifluoroacetic acid, a fluorinating reagent and hydrogen fluoride from the gas obtained from the upper end outlet of the catalyst packed column by a first cold trap, collecting crude perfluoroacetyl fluoride by a second cold trap after the first cold trap is in a 0-DEG ice-water bath, and rectifying the obtained perfluoroacetyl fluoride at low temperature to obtain the perfluoroacetyl fluoride with the purity of more than 99.9%, wherein the comprehensive yield of the reaction reaches 71.2%.
Comparative example 1 anhydrous hydrogen fluoride, trifluoroacetic acid, clCHFCF2N (C2H 5) 2 in quantitative ratios of substances: 1, slowly adding the mixture into a pressure-resistant reaction kettle, controlling the reaction temperature to be between 0 and 15 ℃, adding a solvent and tris (pentafluorophenyl) borane, starting stirring until the pressure in the kettle is constant, continuing stirring for 3 hours to finish the reaction, opening an exhaust valve, transferring gas in the reaction kettle to a low-temperature pressure-resistant storage tank, controlling the temperature of the storage tank to be-70 ℃, carrying out low-temperature rectification to obtain perfluoroacetyl fluoride with the purity of more than 99.9%, controlling the comprehensive yield of the reaction to be 76.2%, and mixing unreacted trifluoroacetic acid, hydrogen fluoride and the solvent in the reaction kettle.
Comparative example 2: anhydrous hydrogen fluoride, trifluoroacetic acid and potassium fluoride in the mass ratio: 1, slowly adding the mixture into a pressure-resistant reaction kettle, controlling the reaction temperature to be between 0 and 15 ℃, adding a solvent, starting stirring until the pressure in the kettle is constant, continuing stirring for 3 hours to finish the reaction, opening an exhaust valve, transferring gas in the reaction kettle to a low-temperature pressure-resistant storage tank, wherein the temperature of the storage tank is-70 ℃, carrying out low-temperature rectification to obtain perfluoroacetyl fluoride with the purity of more than 99.9 percent, the comprehensive yield of the reaction is 45.8 percent, and unreacted trifluoroacetic acid, solid salt and the solvent are mixed and exist in the reaction kettle.
Comparative example 3: in US2717871, the highest yield of trifluoroacetyl fluoride obtained by electrolyzing trifluoroacetic acid at a given current density is 45% by using an iron plate with a certain surface area as a cathode and a nickel plate as an anode.
Compared with the traditional reaction in solution, the technical scheme provided by the invention has higher conversion rate and equipment utilization rate and extremely high industrial application prospect. In addition, the technical scheme has higher conversion rate and yield than that of the disclosed electrolytic method for preparing trifluoroacetyl fluoride US 2717871.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (4)
1. A continuous preparation method of trifluoroacetyl fluoride is characterized by comprising the following steps:
1) After being gasified, the trifluoroethyl compound and the fluorinating reagent are mixed with anhydrous hydrogen fluoride and then are introduced into a packed column filled with a high-activity catalyst for gas phase reaction;
2) Cooling and rectifying the gas obtained after the reaction to obtain trifluoroacetyl fluoride with the purity of more than 99.9 percent;
wherein the high-activity catalyst is a supported catalyst which takes active carbon as a carrier and contains catalyst active components;
the active component of the catalyst is one of tris (pentafluorophenyl) borane or tris [3,5-bis (trifluoromethyl) phenyl ] borane;
the trifluoroethyl compound is one of trifluoroacetic acid and trifluoroacetic anhydride;
the fluorinating agent is FCHFCF 2 N(CH 3 ) 2 、FCHFCF 2 N(C 2 H 5 ) 2 、ClCHFCF 2 N(CH 3 ) 2 、ClCHFCF 2 N(C 2 H 5 ) 2 、CF 3 OCHFCF 2 N(C 2 H 5 ) 2 One or a mixture thereof.
2. The continuous process for the preparation of trifluoroacetyl fluoride according to claim 1, wherein the packed column temperature is in the range of 30 to 100 ℃.
3. The continuous process for the preparation of trifluoroacetyl fluoride according to claim 1, wherein the fluorination reagent has a temperature of from 50 to 100 ℃ of vaporization.
4. The continuous preparation method of trifluoroacetyl fluoride according to claim 1, characterized in that the gas in step 2) is cooled and passed through double cold traps, the first cold trap is used for recovering the raw material trifluoroethyl compound, the fluorinating agent and anhydrous hydrogen fluoride, and the second cold trap is used for collecting crude trifluoroacetyl fluoride.
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| DE4423386A1 (en) * | 1994-07-04 | 1996-01-18 | Hoechst Ag | Process for the preparation of trifluoroacetyl fluoride |
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| CN105198719B (en) * | 2015-09-06 | 2017-08-01 | 浙江工业大学 | A kind of preparation method of the pentanone of 2 methyl of perfluor 3 |
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