CN213951046U - Combined preparation device of trifluoroacetyl fluoride - Google Patents
Combined preparation device of trifluoroacetyl fluoride Download PDFInfo
- Publication number
- CN213951046U CN213951046U CN202022661877.9U CN202022661877U CN213951046U CN 213951046 U CN213951046 U CN 213951046U CN 202022661877 U CN202022661877 U CN 202022661877U CN 213951046 U CN213951046 U CN 213951046U
- Authority
- CN
- China
- Prior art keywords
- gasification
- unit
- communicated
- chamber
- cold trap
- 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.)
- Active
Links
- 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 28
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- 238000002309 gasification Methods 0.000 claims abstract description 41
- DTQVDTLACAAQTR-UHFFFAOYSA-N Trifluoroacetic acid Chemical compound OC(=O)C(F)(F)F DTQVDTLACAAQTR-UHFFFAOYSA-N 0.000 claims abstract description 34
- 238000006243 chemical reaction Methods 0.000 claims abstract description 32
- 238000011084 recovery Methods 0.000 claims abstract description 23
- 238000003860 storage Methods 0.000 claims abstract description 21
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000003153 chemical reaction reagent Substances 0.000 claims abstract description 15
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 claims abstract description 14
- 238000003682 fluorination reaction Methods 0.000 claims abstract description 14
- 229910052731 fluorine Inorganic materials 0.000 claims abstract description 14
- 239000011737 fluorine Substances 0.000 claims abstract description 14
- 229910000040 hydrogen fluoride Inorganic materials 0.000 claims abstract description 14
- 150000003973 alkyl amines Chemical class 0.000 claims abstract description 12
- 239000002994 raw material Substances 0.000 claims abstract description 10
- 239000003054 catalyst Substances 0.000 claims abstract description 4
- 238000010438 heat treatment Methods 0.000 claims abstract description 4
- 238000002156 mixing Methods 0.000 claims abstract description 4
- 238000000926 separation method Methods 0.000 claims description 25
- 239000012043 crude product Substances 0.000 claims description 15
- 238000001704 evaporation Methods 0.000 claims description 7
- 230000008020 evaporation Effects 0.000 claims description 7
- 238000004519 manufacturing process Methods 0.000 claims description 3
- 239000000126 substance Substances 0.000 abstract description 5
- 239000002904 solvent Substances 0.000 abstract description 4
- 238000009776 industrial production Methods 0.000 abstract description 2
- 239000007788 liquid Substances 0.000 abstract description 2
- 239000002699 waste material Substances 0.000 abstract description 2
- 239000007792 gaseous phase Substances 0.000 abstract 1
- 239000007789 gas Substances 0.000 description 9
- 239000000047 product Substances 0.000 description 5
- 150000001875 compounds Chemical class 0.000 description 4
- WFDIJRYMOXRFFG-UHFFFAOYSA-N Acetic anhydride Chemical compound CC(=O)OC(C)=O WFDIJRYMOXRFFG-UHFFFAOYSA-N 0.000 description 3
- 238000000034 method Methods 0.000 description 3
- 230000009286 beneficial effect Effects 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
- 238000009835 boiling Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005868 electrolysis reaction Methods 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
- 239000012535 impurity Substances 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000001308 synthesis method Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Images
Landscapes
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The utility model belongs to the field of fluorine chemical preparation, in particular to a combined preparation device of trifluoroacetyl fluoride, a raw material tank unit comprises a trifluoroacetic acid storage tank, a fluorine-containing alkylamine fluorination reagent storage tank and an anhydrous hydrogen fluoride storage tank; the gasification unit comprises a trifluoroacetic acid gasification chamber, a fluorine-containing alkylamine fluorination reagent gasification chamber and an anhydrous hydrogen fluoride gasification chamber; a mixed gasification chamber is arranged between the gasification unit and the reaction unit; the reaction unit comprises a reaction tube loaded with a catalyst and a heating sleeve arranged on the outer side of the reaction tube; the recovery unit comprises a first cold trap and a second cold trap which are sequentially communicated and a recovery gasification chamber connected with the first cold trap; the recovery gasification chamber is communicated with the mixing gasification chamber. The application provides a gaseous phase preparation facilities of trifluoroacetyl fluoride, the device has avoided the recovery processing and the waste liquid pollution of solvent, obtains high value chemical industry midbody trifluoroacetyl fluoride, easily scale industrial production.
Description
Technical Field
The utility model belongs to fluorine chemical preparation field, concretely relates to trifluoroacetyl fluoride's joint preparation facilities.
Background
Perfluoroacetyl fluoride, also known as trifluoroacetyl fluoride, has the formula: CF3COF, boiling point: the compound is colorless gas at the temperature of minus 59 ℃, is a compound containing a-COF functional group, 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 a chemical synthesis intermediate of a perfluoroalkylated product, is a polymerization monomer and the like necessary for preparing a high-purity fluoropolymer and is concerned, 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 electrolytic synthesis method of US2717871 is cheap in raw materials, but has low electrolytic efficiency, is difficult to avoid low product purity caused by electrolytic impurities, is expensive in manufacturing cost of an electrolytic plate, and is not beneficial to industrial implementation due to high equipment cost. Trifluoroacetic acid conversion is usually carried out by a solvent method, which causes a large amount of solvent consumption pollution and complicated post-treatment.
SUMMERY OF THE UTILITY MODEL
The utility model aims to overcome the defects in the prior art and provide a combined preparation device of trifluoroacetyl fluoride.
The utility model discloses a realize above-mentioned purpose, adopt following technical scheme:
a combined preparation device of trifluoroacetyl fluoride 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, a fluorine-containing alkylamine fluorination reagent storage tank and an anhydrous hydrogen fluoride storage tank;
the gasification unit comprises a trifluoroacetic acid gasification chamber, a fluorine-containing alkylamine fluorination reagent gasification chamber and an anhydrous hydrogen fluoride gasification chamber which are respectively communicated with a trifluoroacetic acid storage tank, a fluorine-containing alkylamine fluorination reagent storage tank and an anhydrous hydrogen fluoride storage tank; a mixed gasification chamber is arranged between the gasification unit and the reaction unit;
the reaction unit comprises a reaction tube loaded with a catalyst and a heating jacket arranged outside the reaction tube;
the recovery unit comprises a first cold trap and a second cold trap which are sequentially communicated and a recovery gasification chamber connected with the first cold trap; the recovery gasification chamber is communicated with the mixing gasification chamber.
The second cold trap is connected with the rectifying tower unit; the rectifying tower unit comprises a separation chamber, a heavy component recovery chamber arranged at the lower end of the separation chamber and communicated with the separation chamber, and a rectifying tower 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 the temperature control element; a pressurizing nozzle is arranged at the crude product inlet; the top end of the rectifying tower is communicated with the cold trap through a pipeline.
The reaction units are connected in parallel.
The reaction tube is in a straight tube shape or a spiral coil shape.
Compared with the prior art, the beneficial effects of the utility model are that:
the application provides a gas phase preparation device of trifluoroacetyl fluoride, which avoids the recovery treatment of a solvent and the pollution of waste liquid, can realize the primary separation of products and the recovery of raw materials by arranging two cold traps, wherein the first cold trap is arranged at 0-10 ℃, and can recover most of trifluoroacetic acid, a fluorine-containing alkylamine fluorination reagent and anhydrous hydrogen fluoride; the second cold trap is set to be-65 to-75 ℃, crude trifluoroacetyl fluoride can be obtained, the crude trifluoroacetyl fluoride is added into a rectifying tower unit to realize the purification of trifluoroacetyl fluoride, high-value chemical intermediate trifluoroacetyl fluoride is obtained, the product yield is high, the product purity is more than 99%, meanwhile, raw materials can be recovered, and the large-scale industrial production is easy.
Drawings
FIG. 1 is a schematic view of the overall structure of the apparatus for the combined preparation of trifluoroacetyl fluoride according to the present invention;
fig. 2 is a schematic diagram of the whole structure of the rectifying tower unit of the present invention.
Detailed Description
In order to make those skilled in the art better understand the technical solution of the present invention, the present invention will be further described in detail with reference to the accompanying drawings and preferred embodiments.
FIGS. 1-2 show an integrated trifluoroacetyl fluoride production apparatus comprising, in series, a feed tank unit, a gasification unit, a reaction unit, a recovery unit and a rectification unit; 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-65-0 ℃, 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 reaction units are connected in parallel. The reaction tube is in a straight tube shape or a spiral coil shape.
The utility model discloses a concrete implementation form does: after the anhydrous hydrogen fluoride, the trifluoroacetic acid and the fluorinating reagent are gasified, the gas quality controller is used for controlling the gas quality according to the following ratio of the amount of the gas substances: 1:1:1, feeding the obtained mixed gas into a mixed gasification chamber 7, slowly passing the obtained mixed gas through a reaction tube 8 from bottom to top, sequentially passing the gas obtained from an outlet at the upper end of the reaction tube through a first cold trap, namely a cold trap at 0-10 ℃ to recover hydrogen fluoride, trifluoroacetic acid and a fluorination reagent, collecting crude perfluoroacetyl fluoride in a second cold trap, namely a cold trap at-65 ℃, feeding the raw material in the first cold trap into the reaction tube after gasification for continuous reaction, and carrying out low-temperature rectification on the perfluoroacetyl fluoride obtained in the second cold trap to obtain perfluoroacetyl fluoride with the purity of more than 99.9%.
The above description is only for the preferred embodiment of the present invention, and for those skilled in the art, there are variations on the detailed description and the application scope according to the idea of the present invention, and the content of the description should not be construed as a limitation to the present invention.
Claims (4)
1. A combined preparation device of trifluoroacetyl fluoride is characterized by comprising 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, a fluorine-containing alkylamine fluorination reagent storage tank and an anhydrous hydrogen fluoride storage tank;
the gasification unit comprises a trifluoroacetic acid gasification chamber, a fluorine-containing alkylamine fluorination reagent gasification chamber and an anhydrous hydrogen fluoride gasification chamber which are respectively communicated with a trifluoroacetic acid storage tank, a fluorine-containing alkylamine fluorination reagent storage tank and an anhydrous hydrogen fluoride storage tank; a mixed gasification chamber is arranged between the gasification unit and the reaction unit;
the reaction unit comprises a reaction tube loaded with a catalyst and a heating jacket arranged outside the reaction tube;
the recovery unit comprises a first cold trap and a second cold trap which are sequentially communicated and a recovery gasification chamber connected with the first cold trap; the recovery gasification chamber is communicated with the mixing gasification chamber.
2. The integrated trifluoroacetyl fluoride production apparatus of claim 1, wherein the second cold trap is connected to a rectification column unit; the rectifying tower unit comprises a separation chamber, a heavy component recovery chamber arranged at the lower end of the separation chamber and communicated with the separation chamber, and a rectifying tower 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 the temperature control element; a pressurizing nozzle is arranged at the crude product inlet; the top end of the rectifying tower is communicated with the cold trap through a pipeline.
3. The apparatus for the integrated preparation of trifluoroacetyl fluoride according to claim 1 or claim 2, wherein the reaction units are a plurality of reaction units connected in parallel.
4. The apparatus for the integrated preparation of trifluoroacetyl fluoride according to claim 1 or claim 2, wherein the reaction tube is of a straight tube type or a spiral coil type.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202022661877.9U CN213951046U (en) | 2020-11-17 | 2020-11-17 | Combined preparation device of trifluoroacetyl fluoride |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202022661877.9U CN213951046U (en) | 2020-11-17 | 2020-11-17 | Combined preparation device of trifluoroacetyl fluoride |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN213951046U true CN213951046U (en) | 2021-08-13 |
Family
ID=77209503
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202022661877.9U Active CN213951046U (en) | 2020-11-17 | 2020-11-17 | Combined preparation device of trifluoroacetyl fluoride |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN213951046U (en) |
-
2020
- 2020-11-17 CN CN202022661877.9U patent/CN213951046U/en active Active
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN103342642B (en) | Process for continuously producing dimethyl adipate through reaction-rectification method | |
| CN101362776A (en) | Continuous production method of propyl trialkoxysilane | |
| CN101747176B (en) | Method for preparation of trifluoro acetyl chloride with trifluoroethane chlorinated mixture | |
| CN103864615A (en) | Method for preparing ethyl trifluoroacetate through continuous non-catalytic method | |
| CN213951046U (en) | Combined preparation device of trifluoroacetyl fluoride | |
| CN213951045U (en) | Preparation device of trifluoroacetyl fluoride | |
| CN101306980B (en) | Method for preparing perchloro cyclopentadiene | |
| CN208883750U (en) | A kind of serialization prepare glycine around pipe reaction device | |
| CN106220491B (en) | Production of chloroacetic acid method | |
| CN106431908B (en) | A kind of preparation method of Trifluoroacetic Acid Ethyl Ester | |
| CN214181844U (en) | Cryogenic rectification device for perfluoroacetyl fluoride | |
| CN218392293U (en) | System for preparing trichloroethylene and tetrachloroethylene by azeotropic separation | |
| CN214383703U (en) | Low-concentration impurity-containing dilute hydrochloric acid hydrogen chloride purification device by sulfuric acid method | |
| CN105418439A (en) | Method and device for producing 3-chlorine-4-fluoroaniline | |
| CN112552149B (en) | Reaction system and method for preparing perfluoroalkyl vinyl ether | |
| CN113666805B (en) | Method and system for continuously producing 4-chloro-3, 5-dimethylphenol | |
| CN112500285B (en) | Continuous preparation method of trifluoroacetyl fluoride | |
| CN107973692A (en) | A kind of preparation method of brominated alkanes | |
| CN112341310B (en) | Preparation method of bromo-perfluoroalkane | |
| Van Velzen et al. | Development and design of a continuous laboratory-scale plant for hydrogen production by the Mark-13 cycle | |
| CN103755625A (en) | Method for cleanly preparing high-purity pyridine hydrochloride | |
| CN107434253B (en) | Continuous production process and production system of high-quality cyanide solution | |
| CN214916135U (en) | Device for preparing hydrofluoroether in gas phase | |
| CN113511954B (en) | Continuous flow preparation method of 1,2, 3-trichloropropane | |
| CN218909881U (en) | Tetrafluoro oxygen sulfur apparatus for producing |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| TR01 | Transfer of patent right |
Effective date of registration: 20231113 Address after: No. 60 Cangsheng Street, Economic and Technological Development Zone (Nangang Industrial Zone), Binhai New Area, Tianjin, 300452 Patentee after: TIANJIN CHANGLU CHEMICAL NEW MATERIAL Co.,Ltd. Address before: 300000 Building 9, ligangyuan, Shuanggang Industrial Zone, Shuanggang Town, Jinnan District, Tianjin Patentee before: TIANJIN CHANGLU NEW MATERIAL RESEARCH INSTITUTE CO.,LTD. |
|
| TR01 | Transfer of patent right |