CN210993045U - Baffle distillation column purification reaction system - Google Patents
Baffle distillation column purification reaction system Download PDFInfo
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- CN210993045U CN210993045U CN201921012751.XU CN201921012751U CN210993045U CN 210993045 U CN210993045 U CN 210993045U CN 201921012751 U CN201921012751 U CN 201921012751U CN 210993045 U CN210993045 U CN 210993045U
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Abstract
The utility model belongs to the field of fluorine chemistry, in particular to a baffle distillation tower purification reaction system, which comprises a reaction kettle, a condenser and a baffle tower; the reaction kettle comprises a kettle body, a feed inlet and a connector which are arranged at the top of the kettle body, and a discharge outlet which is arranged at the bottom of the kettle body; the interface is communicated with the condenser through a connecting piece; the condenser is communicated with the clapboard tower through a pipeline; the clapboard tower comprises a tower body and a clapboard arranged along the height direction of the tower; the tower bottom of the clapboard tower is provided with a heating jacket, and the tower top is provided with a condensing pipe; the left side end of the distillation tower is provided with a pre-separation product inlet, and the right side end of the distillation tower is provided with a separation product outlet; a control valve is arranged on the pipeline. The utility model provides a baffle distillation column purification reaction system utilizes the setting of tower body baffle, can realize once the rectification and get rid of low boiling and high boiling impurity simultaneously, and the purity of purification back perfluor isobutyryl fluoride > 99.9% even higher.
Description
Technical Field
The utility model belongs to the fluorine chemistry field, concretely relates to baffle distillation column purification reaction system.
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. And when hexafluoropropylene and carbonyl fluoride are used as raw materials to prepare the perfluoroisobutyryl fluoride, a byproduct of perfluoroheptacarbon ketone exists, although the perfluoroheptacarbon ketone and the perfluorobutyryl fluoride can be separated by conventional reduced pressure distillation, the conventional method is difficult to completely separate the perfluoroheptacarbon ketone, so that the quality of the perfluoroisobutyryl fluoride is influenced. Aiming at the defects of low yield, difficult separation of perfluoro-heptacarbon ketone and the like when the perfluoro-isobutyryl fluoride is prepared by a one-pot reaction, a simple and convenient device for preparing and purifying the perfluoro-isobutyryl fluoride is urgently needed.
SUMMERY OF THE UTILITY MODEL
An object of the utility model is to provide a baffle distillation column purification reaction system.
The utility model discloses a realize above-mentioned purpose, adopt following technical scheme:
a partition distillation tower purification reaction system comprises a reaction kettle, a condenser and a partition tower; the reaction kettle comprises a kettle body, a feed inlet and a connector which are arranged at the top of the kettle body, and a discharge outlet which is arranged at the bottom of the kettle body; the interface is communicated with the condenser through a connecting piece; the condenser is communicated with the clapboard tower through a pipeline; the clapboard tower comprises a tower body and a clapboard arranged along the height direction of the tower; the tower bottom of the clapboard tower is provided with a heating jacket, and the tower top is provided with a condensing pipe; the left side end of the distillation tower is provided with a pre-separation product inlet, and the right side end of the distillation tower is provided with a separation product outlet; the area between the upper end of the clapboard and the tower top is a liquid distribution section; the area between the lower end of the clapboard and the bottom of the tower is a gas distribution section; the pipeline is provided with a control valve.
Snakelike condensation pipelines are arranged in the condenser and the condensation pipe; and a refrigerant inlet and a refrigerant outlet are respectively arranged at two ends of the snake-shaped condensation pipeline.
A reflux port and an exhaust port are respectively arranged at two ends of the condenser; the reflux port is communicated with the interface of the kettle body; the exhaust port is communicated with a pre-separation product inlet of the clapboard tower.
One end of the condensing pipe is provided with a liquid reflux port; the liquid reflux port is communicated with the top of the tower body.
The reaction kettle is used for synthesizing perfluoro isobutyryl fluoride; the clapboard tower is used for separating perfluor hepta-carbon ketone; the reaction kettle is internally provided with raw materials of hexafluoropropylene and carbonyl fluoride, a catalyst of 2-perfluoroalkyl benzothiazole compounds, and a solvent of acetonitrile.
The mol ratio of the hexafluoropropylene to the carbonyl fluoride to the 2-perfluoroalkyl benzothiazole compound is as follows: 1:1-2:0.05-0.1.
The 2-perfluoroalkyl benzothiazole compound is a 2-perfluoropropyl benzothiazole compound, a 2-perfluorobutane benzothiazole compound or a 2-perfluoropentane benzothiazole compound.
The preparation method in the reaction kettle specifically comprises the following steps: putting hexafluoropropylene and carbonyl fluoride as raw materials, 2-perfluorobutane benzothiazole and a solvent into a reaction kettle, heating to 75-85 ℃ for reaction for 2-5 hours.
Compared with the prior art, the beneficial effects of the utility model are that:
the utility model provides a baffle distillation column purification reaction system utilizes the setting of tower body baffle, can realize once the rectification and get rid of low boiling and high boiling impurity simultaneously, and the purity of purification back perfluor isobutyryl fluoride > 99.9% even higher. Meanwhile, the 2-perfluoroalkyl benzothiazole compound is adopted as a catalyst in the application, can be dissolved in an acetonitrile solvent and uniformly wraps around raw material hexafluoropropylene, and has electron donor acceptor performance capable of tightly combining carbonyl fluoride free radicals, hexafluoropropylene free radicals and isobutyryl fluoride free radicals generated under an alkaline condition, so that the reaction time is favorably shortened, and the yield is improved.
Drawings
FIG. 1 is a schematic diagram of the overall structure of a baffle distillation column purification reaction system 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.
Fig. 1 shows a baffle distillation column purification reaction system comprising a reaction vessel 1, a condenser 2, and a baffle column 3; the reaction kettle comprises a kettle body 11, a feed inlet 12 and a connector 13 which are arranged at the top of the kettle body, and a discharge outlet 14 which is arranged at the bottom of the kettle body; the interface is communicated with the condenser through a connecting piece; the condenser is communicated with the clapboard tower through a pipeline; the clapboard tower comprises a tower body 31 and a clapboard 32 arranged along the height direction of the tower; the tower bottom of the clapboard tower is provided with a heating jacket 33, and the tower top is provided with a condensing pipe 34; the left side end of the distillation tower is provided with a pre-separation product inlet 35, and the right side end of the distillation tower is provided with a separation product outlet 36; the area between the upper end of the clapboard and the tower top is a liquid distribution section; the area between the lower end of the clapboard and the bottom of the tower is a gas distribution section; the pipeline is provided with a control valve. Snakelike condensation pipelines are arranged in the condenser and the condensation pipe; and a refrigerant inlet and a refrigerant outlet are respectively arranged at two ends of the snake-shaped condensation pipeline. A return port 21 and an exhaust port 22 are respectively arranged at two ends of the condenser; the reflux port is communicated with the interface of the kettle body; the exhaust port is communicated with a pre-separation product inlet of the clapboard tower. One end of the condensation pipe is provided with a liquid return port 341; the liquid reflux port is communicated with the top of the tower body.
Example 1: a method for preparing perfluoroisobutyryl fluoride by using the device comprises the following steps: 1mol of hexafluoropropylene and 1.5mol of carbonyl fluoride are used as raw materials, 0.08mol of 2-perfluorobutyl benzothiazole is used as a catalyst, the raw materials are added into 100ml of acetonitrile solution, the heating is carried out at 85 ℃, and the content of the target product is detected within 2h, 3h, 4h, 5h and 6h respectively. See table 1 below, respectively. And after the reaction is finished, opening the control valve, allowing the product to flow into the partition distillation tower for distillation, and detecting the obtained product by GC-MS (gas chromatography-Mass spectrometer), wherein the product does not contain perfluoroheptacarbon ketone.
TABLE 1
| Reaction time | Yield of |
| 2h | 92％ |
| 3h | 93.5％ |
| 4h | 93.2％ |
| 5h | 91.6％ |
| 6h | 91.25％ |
Example 2: example 2 differs from the example only in that the catalyst used is 2-perfluoropentylbenzothiazole, which has a reaction law similar to that of 2-perfluorobutanebenzothiazole in 2-6h, but the yield is lower than that of 2-perfluorobutanebenzothiazole in example 1, and thus the description is omitted.
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 partition distillation tower purification reaction system is characterized by comprising a reaction kettle, a condenser and a partition tower; the reaction kettle comprises a kettle body, a feed inlet and a connector which are arranged at the top of the kettle body, and a discharge outlet which is arranged at the bottom of the kettle body; the interface is communicated with the condenser through a connecting piece; the condenser is communicated with the clapboard tower through a pipeline; the clapboard tower comprises a tower body and a clapboard arranged along the height direction of the tower; the tower bottom of the clapboard tower is provided with a heating jacket, and the tower top is provided with a condensing pipe; the left side end of the distillation tower is provided with a pre-separation product inlet, and the right side end of the distillation tower is provided with a separation product outlet; the area between the upper end of the clapboard and the tower top is a liquid distribution section; the area between the lower end of the clapboard and the bottom of the tower is a gas distribution section; the pipeline is provided with a control valve.
2. The barrier distillation column purification reaction system as recited in claim 1 wherein said condenser and said condenser tube have serpentine condensation lines; and a refrigerant inlet and a refrigerant outlet are respectively arranged at two ends of the snake-shaped condensation pipeline.
3. The barrier distillation column purification reaction system according to claim 1, wherein a reflux port and an exhaust port are provided at both ends of the condenser, respectively; the reflux port is communicated with the interface of the kettle body; the exhaust port is communicated with a pre-separation product inlet of the clapboard tower.
4. The barrier distillation column purification reaction system as claimed in claim 1, wherein a liquid reflux port is provided at one end of the condensation pipe; the liquid reflux port is communicated with the top of the tower body.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201921012751.XU CN210993045U (en) | 2019-06-30 | 2019-06-30 | Baffle distillation column purification reaction system |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201921012751.XU CN210993045U (en) | 2019-06-30 | 2019-06-30 | Baffle distillation column purification reaction system |
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| Publication Number | Publication Date |
|---|---|
| CN210993045U true CN210993045U (en) | 2020-07-14 |
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| CN201921012751.XU Active CN210993045U (en) | 2019-06-30 | 2019-06-30 | Baffle distillation column purification reaction system |
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| CN (1) | CN210993045U (en) |
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- 2019-06-30 CN CN201921012751.XU patent/CN210993045U/en active Active
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