CN210994236U - Preparation device of perfluoroisobutyryl fluoride - Google Patents
Preparation device of perfluoroisobutyryl fluoride Download PDFInfo
- Publication number
- CN210994236U CN210994236U CN201921004685.1U CN201921004685U CN210994236U CN 210994236 U CN210994236 U CN 210994236U CN 201921004685 U CN201921004685 U CN 201921004685U CN 210994236 U CN210994236 U CN 210994236U
- Authority
- CN
- China
- Prior art keywords
- shell
- exhaust port
- feed inlet
- gas
- reaction
- 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
Images
Landscapes
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The utility model belongs to the field of fluorine chemistry, in particular to a device for preparing perfluoro isobutyryl fluoride, which comprises a reaction kettle and a cooling reflux device; the reaction kettle comprises a kettle body, a gas feed inlet, a liquid feed inlet, an exhaust port and a waste discharge port, wherein the gas feed inlet, the liquid feed inlet and the exhaust port are arranged at the top of the kettle body; the exhaust port is communicated with the cooling reflux device through a valve; the cooling reflux device comprises a shell, a snakelike condensing pipe arranged in the shell, a raw material gas inlet arranged on one side of the shell and connected with an exhaust port, a raw material gas outlet arranged on the other side of the shell and a product outlet arranged at the bottom of the shell. The utility model provides a preparation facilities of perfluor isobutyryl fluoride utilizes the kinetic equilibrium of reaction, with continuous shifting out of result to make keeping higher concentration always of raw materials, and the product keeps lower concentration, the reaction goes on to the positive direction, thereby improves the productivity of product, the device design is simple, does benefit to the industrialization.
Description
Technical Field
The utility model belongs to the fluorine chemistry field, concretely relates to preparation facilities of perfluor isobutyryl fluoride.
Background
The perfluoro isobutyryl fluoride is an important fluorine-containing compound, has wide application, and can be used for cleaning agents, etching agents, pesticide intermediates, fluorine-containing material monomers and the like in the electronic industry.
There are many methods for preparing perfluorobutyryl fluoride, such as an electrochemical method or a chemical synthesis method, among which, a reaction kettle liquid phase method is a commonly used chemical synthesis method, which has the advantage of simple operation, but tends to have a low yield due to the one-pot method of feeding for reaction. Aiming at the defects of low yield, complex separation process, difficult industrialization and the like when the perfluoro isobutyryl fluoride is prepared by one-pot reaction, a simple and convenient preparation device of the perfluoro isobutyryl fluoride is urgently needed.
SUMMERY OF THE UTILITY MODEL
The utility model aims to provide a preparation facilities of perfluor isobutyryl fluoride.
The utility model discloses a realize above-mentioned purpose, adopt following technical scheme:
a preparation device of perfluoro isobutyryl fluoride comprises a reaction kettle and a cooling reflux device; the reaction kettle comprises a kettle body, a gas feed inlet, a liquid feed inlet, an exhaust port and a waste discharge port, wherein the gas feed inlet, the liquid feed inlet and the exhaust port are arranged at the top of the kettle body; the exhaust port is communicated with the cooling reflux device through a valve; the cooling reflux device comprises a shell, a serpentine condenser pipe arranged in the shell, a feed gas inlet arranged on one side of the shell and connected with the exhaust port, a feed gas outlet arranged on the other side of the shell and a product outlet arranged at the bottom of the shell.
And a refrigerant inlet and a refrigerant outlet are respectively arranged at two ends of the snakelike condensation pipe.
The raw material gas outlet is communicated with the gas feed inlet or the raw material gas storage tank through a pipeline.
The gas raw materials in the reaction kettle are hexafluoropropylene and carbonyl fluoride, the liquid solvent is DMF, and the catalyst is alkaline fluoride; the reaction temperature is 75-85 ℃.
The initial feeding molar ratio of the hexafluoropropylene to the carbonyl fluoride is 1:1-2, and the concentration of the basic fluoride in DMF is 0.05-0.1 mol/L.
The alkaline fluoride is NaF, KF or CsF.
Compared with the prior art, the beneficial effects of the utility model are that:
the utility model provides a preparation facilities of perfluor isobutyryl fluoride utilizes the kinetic equilibrium of reaction, with continuous shifting out of result to make keeping higher concentration always of raw materials, and the product keeps lower concentration, the reaction goes on to the positive direction, thereby improves the productivity of product, the device design is simple, does benefit to the industrialization.
Drawings
FIG. 1 is a schematic view of the overall structure of the apparatus for producing perfluoroisobutyryl fluoride according to 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.
FIG. 1 shows a perfluoroisobutyryl fluoride preparation apparatus, which comprises a reaction kettle 1 and a cooling reflux apparatus 2; the reaction kettle comprises a kettle body 11, a gas feed inlet 12, a liquid feed inlet 13, an exhaust port 14 and a waste discharge port 15, wherein the gas feed inlet 12, the liquid feed inlet 13 and the exhaust port are arranged at the top of the kettle body; the exhaust port is communicated with the cooling reflux device through a valve; the cooling reflux device comprises a shell 21, a serpentine condenser pipe 22 arranged in the shell, a raw material gas inlet 23 arranged on one side of the shell and connected with the exhaust port, a raw material gas outlet 24 arranged on the other side of the shell and a product outlet 25 arranged at the bottom of the shell. And a refrigerant inlet and a refrigerant outlet are respectively arranged at two ends of the snakelike condensation pipe. The raw material gas outlet is communicated with the gas feed inlet or the raw material gas storage tank 3 through a pipeline.
Example 1 gaseous raw materials hexafluoropropylene and carbonyl fluoride are fed into a reaction kettle according to component quantity at a gas feed inlet, the molar ratio is 1:1.5, a small amount of carbonyl fluoride is added to facilitate the reaction, a liquid solvent mixed with a catalyst is DMF at a liquid feed inlet, the catalyst is KF, the reaction temperature of the reaction kettle is set to be 75-85 ℃, the concentration of the alkaline fluoride in DMF is 0.08 mol/L, the perfluoroisobutyryl fluoride is prepared by using the preparation device, the yield of the product perfluoroisobutyryl fluoride reaches more than 96% after continuous reaction for 12 h.
Example 2 is the same as example 1 except that the initial feed molar concentration of the feed gas was 1:1 the catalyst was CsF and the molar concentration was 0.05 mol/L.
Example 3 is the same as example 1 except that the initial feed molar concentration of the feed gas was 1:2 the catalyst was NaF and the molar concentration was 0.1 mol/L.
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 (3)
1. A preparation device of perfluoroisobutyryl fluoride is characterized by comprising a reaction kettle and a cooling reflux device; the reaction kettle comprises a kettle body, a gas feed inlet, a liquid feed inlet, an exhaust port and a waste discharge port, wherein the gas feed inlet, the liquid feed inlet and the exhaust port are arranged at the top of the kettle body; the exhaust port is communicated with the cooling reflux device through a valve; the cooling reflux device comprises a shell, a serpentine condenser pipe arranged in the shell, a feed gas inlet arranged on one side of the shell and connected with the exhaust port, a feed gas outlet arranged on the other side of the shell and a product outlet arranged at the bottom of the shell.
2. The apparatus according to claim 1, wherein the two ends of the serpentine condenser tube are respectively provided with a coolant inlet and a coolant outlet.
3. The apparatus according to claim 1, wherein the feed gas outlet is connected to the gas feed port or the feed gas storage tank via a pipeline.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201921004685.1U CN210994236U (en) | 2019-06-30 | 2019-06-30 | Preparation device of perfluoroisobutyryl fluoride |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201921004685.1U CN210994236U (en) | 2019-06-30 | 2019-06-30 | Preparation device of perfluoroisobutyryl fluoride |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN210994236U true CN210994236U (en) | 2020-07-14 |
Family
ID=71484622
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201921004685.1U Active CN210994236U (en) | 2019-06-30 | 2019-06-30 | Preparation device of perfluoroisobutyryl fluoride |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN210994236U (en) |
-
2019
- 2019-06-30 CN CN201921004685.1U patent/CN210994236U/en active Active
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102675093B (en) | A kind of process of n-butyl acetate synthesis | |
| CN105363321A (en) | Hydrogen chloride gas absorption device | |
| CN210448119U (en) | Continuous enrichment facility of quaternary ammonium alkaline aqueous solution | |
| CN210994236U (en) | Preparation device of perfluoroisobutyryl fluoride | |
| CN203687669U (en) | Acid gas condenser | |
| CN111530472A (en) | Titanium-based heterogeneous amination composite catalyst and application thereof in production of N-methylpyrrolidone for liquid crystal panel | |
| CN112552149B (en) | Reaction system and method for preparing perfluoroalkyl vinyl ether | |
| CN107434253B (en) | Continuous production process and production system of high-quality cyanide solution | |
| CN208525866U (en) | A kind of bead tube, rectifying column and rectifying plate | |
| CN110433743A (en) | The preparation facilities of perfluor isobutyl acyl fluorides | |
| CN209481173U (en) | A kind of electronic grade hydrochloric acid purification system | |
| CN210993045U (en) | Baffle distillation column purification reaction system | |
| CN104084042B (en) | Complete-cycle double-way-feeding energy-saving system for producing stable isotope 15N | |
| CN214916135U (en) | Device for preparing hydrofluoroether in gas phase | |
| CN111185070A (en) | NF removal using low temperature HF3System and method for removing impurities from electrolysis gas | |
| CN218853499U (en) | FNO 2 Rectification and purification device | |
| CN1193977C (en) | Process for preparing granular patassium formate and its pelletizing equipment | |
| CN2934207Y (en) | Hydrochloric acid purification device | |
| CN220176837U (en) | Device for preparing fluorobenzene by micro-reflection continuous flow | |
| CN217313345U (en) | Aliphatic nitrile production system | |
| CN112500285B (en) | Continuous preparation method of trifluoroacetyl fluoride | |
| CN218810377U (en) | Production system for improving quality of sodium nitrate | |
| CN218642657U (en) | Phase separation system for 1, 2-tetrafluoroethane | |
| CN214032306U (en) | Device for preparing perfluoroalkyl vinyl ether by liquid continuous tubular decarboxylation | |
| CN115849409B (en) | Synthesis process of liquid lithium hexafluorophosphate |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| GR01 | Patent grant | ||
| GR01 | Patent grant |