Perfluoro-n-propyl vinyl ether dimer preparation device

Abstract

The utility model discloses a perfluoro-n-propyl vinyl ether dimer preparation device, which comprises an oil bath pan, a three-necked flask is arranged in the oil bath pan, the three-necked flask comprises three bottle mouths, a thermometer, a stirrer and a condensation reflux pipe are respectively arranged on the three bottle mouths, the thermometer, the stirrer and the condensation reflux pipe are fixed through a support frame, and the support frame is fixed on the oil bath pan. A water avoiding mechanism is arranged at the upper port of the condensation return pipe which is connected with a collecting bottle through a three-way pipe. The condensation return pipe comprises a cooling cavity and a spiral pipe arranged in the cooling cavity, condensate flows in the spiral pipe to cool a product in the cooling cavity, product steam is liquefied when meeting the low-temperature condensate, and the liquefied product steam flows back into the three-necked flask through the three-way pipe to carry out the next reaction; the water avoiding mechanism can discharge gas generated in the reaction process out of the three-necked flask, balance internal and external pressure and prevent the three-necked flask from bursting due to increase of air pressure, and can isolate external water molecules to keep the whole reaction to be carried out under a water-free condition.

Description

Technical Field

[0001] The utility model relates to the field of chemistry, and particularly to a preparation device for perfluoropropyl vinyl ether dimer. Background Art

[0002] Fluoroolefin compounds have certain chemical activities and can undergo addition or polymerization reactions to derive various fluorinated organic compounds. In addition, fluoroolefins have low surface tension, good electrochemical properties and environmental compatibility, and are widely used in the fields of surfactants, pharmaceutical intermediates, heat transfer media, etc.

[0003] The preparation of perfluoropropyl vinyl ether dimer requires the synthesis of hexafluoropropylene oxide dimer and sodium carbonate in a DG solvent (the salt-forming reaction temperature is 50 °C) to form perfluoropropyl vinyl ether (boiling point 35 °C) (after salting, the decarboxylation reaction temperature is 120 °C), and the generated perfluoropropyl vinyl ether is then cooled and refluxed into the reaction system to form perfluoropropyl vinyl ether dimer.

[0004] The preparation of perfluoropropyl vinyl ether dimer is carried out under anhydrous conditions, and gases will be generated during the reaction process, and exhaust is required to avoid danger caused by excessive pressure in the container. Therefore, a reaction preparation device that can isolate moisture and exhaust gas is needed. Summary of the Utility Model

[0005] In order to solve the above problems, the utility model provides a preparation device for perfluoropropyl vinyl ether dimer, which includes an oil bath pot, and a three-necked flask is arranged in the oil bath pot. The three-necked flask includes three bottle mouths, and a thermometer, a stirrer and a condensation reflux pipe are respectively installed on the three bottle mouths. The thermometer, the stirrer and the condensation reflux pipe are fixed by a support frame. A water-proof mechanism is arranged at the upper port of the condensation reflux pipe, and the condensation reflux pipe is connected to a collection bottle through a three-way pipe.

[0006] Furthermore, the support frame includes a vertical rod and three cross rods connected to the vertical rod. The three cross rods are respectively used to fix the thermometer, the stirrer and the condensation reflux pipe.

[0007] Furthermore, the thermometer is connected to the three-necked flask through a sealing plug, and the thermometer penetrates through the sealing plug and extends into the interior of the three-necked flask.

[0008] Furthermore, the stirrer includes a motor, a stirring shaft and a stirring paddle. The motor is fixedly connected to the support frame, the output shaft of the motor is fixedly connected to the stirring shaft, the end of the stirring shaft is connected to the stirring paddle, and the stirring shaft penetrates through the sealing plug and extends into the interior of the three-necked flask.

[0009] Further, the three-necked flask is connected to a condensation reflux tube through a connecting tube 1 which is inclined. The condensation reflux tube includes a cooling chamber and a spiral tube built inside the cooling chamber. The lower end of the cooling chamber is connected to the three-necked flask through the connecting tube 1, and the upper end is connected to a water-proofing mechanism. The lower port of the spiral tube is set as the liquid inlet, and the upper port of the spiral tube is set as the liquid outlet.

[0010] Further, the three-way pipe includes a vertical pipe and a connecting tube 2 which is inclined. The upper port of the vertical pipe is connected to the cooling chamber and forms a fork with the connecting tube 1. The lower port of the vertical pipe is connected to a collecting bottle. A three-way valve is provided at the junction of the vertical pipe and the connecting tube 2. The end of the connecting tube 2 is connected to the three-necked flask.

[0011] Further, the water-proofing mechanism includes a housing. The bottom of the housing is open to form a receiving chamber. The cavity of the receiving chamber is narrower at the bottom and wider at the top. An absorbent is provided in the receiving chamber for isolating and absorbing external moisture. A ventilation hole is opened at the top of the housing, and the ventilation hole communicates with the receiving chamber for balancing the air pressure inside and outside the three-necked flask.

[0012] Further, a partition layer is provided below the absorbent to prevent the absorbent from falling.

[0013] The beneficial effects of the present utility model are as follows:

[0014] In the preparation device for perfluoropropyl vinyl ether dimer of the present utility model, the condensation reflux tube includes a cooling chamber and a spiral tube built inside the cooling chamber. The condensate flows in the spiral tube to cool the product in the cooling chamber. The product vapor liquefies when it meets the low-temperature condensate and flows back into the three-necked flask through the three-way pipe for the next reaction. The water-proofing mechanism includes a housing. The bottom of the housing is open to form a receiving chamber. An absorbent is provided in the receiving chamber. The water-proofing mechanism can not only discharge the gas generated during the reaction from the three-necked flask to balance the internal and external pressures and prevent the three-necked flask from bursting due to increased air pressure, but also isolate external water molecules to keep the whole reaction under anhydrous conditions. BRIEF DESCRIPTION OF THE DRAWINGS

[0015] Figure 1 is a schematic structural diagram of the present utility model.

[0016] Figure 2 is a three-dimensional schematic diagram of the water-proofing mechanism.

[0017] Figure 3 is a sectional view of the water-proofing mechanism.

[0018] Reference numerals: 1. oil bath pot, 2. stirrer, 201. motor, 202. stirring shaft, 3. thermometer, 4. three-necked flask, 5. condensation reflux tube, 501. cooling chamber, 502. spiral tube, 503. liquid inlet, 504. liquid outlet, 6. support frame, 601. vertical rod, 602. cross bar, 7. sealing plug, 8. connecting pipe I, 9. three-way pipe, 901. vertical pipe, 902. connecting pipe II, 903. three-way valve, 10. collection bottle, 11. water avoidance mechanism, 1101. housing, 1102. accommodation chamber, 1103. water absorbent, 1104. partition layer, 1105. ventilation hole. Detailed implementation manners

[0019] The embodiments of the present invention will be described in detail below. The examples of the embodiments are shown in the accompanying drawings. The embodiments described below by referring to the accompanying drawings are exemplary and are intended to explain the present invention, and should not be construed as a limitation to the present invention.

[0020] The present invention provides a preparation device for perfluoropropyl vinyl ether dimer, comprising: an oil bath pot 1, a three-necked flask 4 is arranged in the oil bath pot 1. The three-necked flask 4 has three mouths, and a thermometer 3, a stirrer 2 and a condensation reflux tube 5 are respectively installed on the three mouths. The thermometer 3, the stirrer 2 and the condensation reflux tube 5 are fixed by a support frame 6. A water avoidance mechanism 11 is arranged at the upper port of the condensation reflux tube 5, and the condensation reflux tube 5 is connected to a collection bottle 10 through a three-way pipe 9. The oil bath pot 1 is a prior art and has functions of constant temperature heating and magnetic rotor stirring, which will not be elaborated here.

[0021] The support frame 6 includes a vertical rod 601 and three cross bars 602 connected to the vertical rod 601. The three cross bars 602 are respectively used to fix the thermometer 3, the stirrer 2 and the condensation reflux tube 5. The support frame 6 is a prior art and will not be elaborated here.

[0022] The thermometer 3 is connected to the three-necked flask 4 through a sealing plug 7, and the thermometer 3 penetrates through the sealing plug 7 and extends into the interior of the three-necked flask 4. The mouth of the three-necked flask 4 where the thermometer 3 is located is provided with a short bottleneck to reduce the amount of product gas at the mouth where the thermometer 3 is located. The temperature measuring end of the thermometer 3 is located below the liquid level of the reactants to monitor the temperature of the reactants in real time.

[0023] The stirrer 2 includes a motor 201, a stirring shaft 202 and a stirring paddle. The motor 201 is fixedly connected to the cross bar 602. The output shaft of the motor 201 is fixedly connected to the stirring shaft 202. The end of the stirring shaft 202 is connected to the stirring paddle. The stirring shaft 202 penetrates through the sealing plug 7 and extends into the interior of the three-necked flask 4. The stirrer 2 is installed on the middle mouth of the three-necked flask 4. The stirring shaft 202 is vertically inserted into the three-necked flask 4, and the stirring paddle is located in the lower middle part of the three-necked flask 4. The motor 201 is connected to a power supply to drive the stirring paddle to stir the reactants in the three-necked flask 4.

[0024] The three-necked flask 4 is connected to the condensation reflux tube 5 through a connecting tube 8 arranged obliquely. The condensation reflux tube 5 includes a cooling chamber 501 and a spiral tube 502 built in the cooling chamber 501. The lower end of the cooling chamber 501 is communicated with the three-necked flask 4 through the connecting tube 8, and the upper end is communicated with the water-proof mechanism 11. The lower port of the spiral tube 502 is set as the liquid inlet 503, and the upper port of the spiral tube 502 is set as the liquid outlet 504.

[0025] The three-way pipe 9 includes a vertical pipe 901 and an obliquely arranged connecting tube 902. The upper port of the vertical pipe 901 is connected to the cooling chamber 501 and forms a fork with the connecting tube 8. The lower port of the vertical pipe 901 is connected to the collection bottle 10. A three-way valve 903 is provided at the intersection of the vertical pipe 901 and the connecting tube 902, and the end of the connecting tube 902 is connected to the three-necked flask 4.

[0026] The product generated by the three-necked flask 4 rises in the form of steam, passes through the connecting tube 8 and enters the cooling chamber 501 of the condensation reflux tube 5. Under the cooling effect of the coolant in the spiral tube 502, it liquefies to form a liquid. The product in the form of liquid flows down along the inner wall of the cooling chamber 501 and enters the vertical pipe 901 of the three-way pipe 9 at the fork; when the three-way valve 903 is closed, the upper part of the vertical pipe 901 is communicated with the connecting tube 902, and the upper part of the vertical pipe 901 is not communicated with the lower part of the vertical pipe 901. At this time, the liquid product flows back into the three-necked flask 4 through the upper part of the vertical pipe 901 and the connecting tube 902 for further reaction; when the three-way valve 903 is rotated 90°, the upper part of the vertical pipe 901 is not communicated with the connecting tube 902, and the upper part of the vertical pipe 901 is communicated with the lower part of the vertical pipe 901. At this time, the liquid product flows into the collection bottle 10 through the upper part of the vertical pipe 901 and the lower part of the vertical pipe 901.

[0027] The water-proof mechanism 11 includes a housing 1101. The housing 1101 is fixedly connected to the condensation reflux tube 5. The bottom of the housing 1101 is opened to form a receiving cavity 1102. The cavity of the receiving cavity 1102 is narrow at the bottom and wide at the top. An absorbent 1103 is provided in the receiving cavity 1102 for isolating and absorbing external moisture. A ventilation hole 1105 is opened at the top of the housing 1101, and the ventilation hole 1105 is communicated with the receiving cavity 1102 for balancing the air pressure inside and outside the three-necked flask 4. A partition layer 1104 is arranged below the absorbent 1103 to prevent the absorbent 1103 from falling. The absorbent 1103 can be resin particles, and the partition layer 1104 prevents the absorbent 1103 from falling into the condensation reflux tube 5; the absorbent 1103 is silica gel. The silica gel is located in the upper part of the receiving cavity 1102. The silica gel is water-absorbing silica gel. The silica gel does not fill the receiving cavity 1102, and the lower part of the receiving cavity 1102 is narrow to limit the silica gel from falling.

[0028] Working principle: This device is used for synthesizing perfluoropropyl vinyl ether from hexafluoropropylene oxide dimer. The perfluoropropyl vinyl ether dimer is prepared through a reflux reaction device. The hexafluoropropylene oxide dimer and sodium carbonate are synthesized in a DG solvent (the salt-forming reaction temperature is 50 °C) to form perfluoropropyl vinyl ether (the boiling point is 35 °C) through a decarboxylation reaction at 120 °C after salt formation. The generated perfluoropropyl vinyl ether is then cooled and refluxed into the reaction system to form perfluoropropyl vinyl ether dimer. Start the oil bath 1, place the reactants in the three-necked flask 4, and use the magnetic rotor to stir the dimethyl silicone oil in the oil bath 1; the thermometer 3 is fixed by the support frame 6, and the temperature measuring end extends into the three-necked flask 4 and is hermetically connected to the three-necked flask 4; the motor 201 of the stirrer 2 is fixed on the support frame 6, and the stirring paddle extends into the three-necked flask 4 to stir the reactants; the condenser reflux tube 5 is held in position by the support frame 6. The three-necked flask 4, the condenser reflux tube 5, and the water-proof mechanism 11 are connected. The vapor of the product condenses into a liquid in the condenser reflux tube 5 and flows back into the three-necked flask 4 along the cooling cavity 501. The gas generated by the reaction enters the outside through the vent hole 1105 of the water-proof mechanism 11; the water molecules in the outside air will be adsorbed on the water absorbent 1103 and cannot enter the condenser reflux tube 5.

[0029] Although the above embodiments have been shown and described, it can be understood that the above embodiments are exemplary and should not be construed as limitations on the present invention. Any changes, modifications, substitutions, and variations made by those of ordinary skill in the art to the above embodiments are within the protection scope of the present invention.

Claims

1. A device for preparing perfluoro n-propyl vinyl ether dimer, characterized in that: include: An oil bath pot is provided with a three-necked flask in the oil bath pot. The three-necked flask comprises three bottle openings, on which a thermometer, an agitator and a condensation reflux pipe are respectively installed. The thermometer, the agitator and the condensation reflux pipe are fixed by a supporting frame. A water-avoiding mechanism is provided at the upper port of the condensation reflux pipe, and the condensation reflux pipe is connected to a collecting bottle by a three-way pipe.

2. The device for preparing perfluoro n-propyl vinyl ether dimer according to claim 1, characterized in that: The support frame comprises a vertical pole and three horizontal poles connected to the vertical pole, and the three horizontal poles are used to fix a thermometer, a stirrer and a condensation reflux pipe respectively.

3. The device for preparing perfluoro n-propyl vinyl ether dimer according to claim 1, characterized in that: The thermometer is connected to the three-necked flask through a sealing plug, and the thermometer penetrates the sealing plug and extends into the interior of the three-necked flask.

4. The device for preparing perfluoro n-propyl vinyl ether dimer according to claim 1, characterized in that: The stirrer comprises a motor, a stirring shaft and a stirring paddle. The motor is fixedly connected to the support frame, the motor output shaft is fixedly connected to the stirring shaft, the end of the stirring shaft is connected to the stirring paddle, and the stirring shaft passes through the sealing plug and extends into the interior of the three-necked flask.

5. The device for preparing perfluoro n-propyl vinyl ether dimer according to claim 1, characterized in that: The three-necked flask is connected to a condensation reflux pipe through an inclined connecting pipe. The condensation reflux pipe includes a cooling chamber and a spiral tube built in the cooling chamber. The lower end of the cooling chamber is connected to the three-necked flask through a connecting pipe, and the upper end is connected to a water-avoiding mechanism. The lower end of the spiral tube is set as a liquid inlet, and the upper end of the spiral tube is set as a liquid outlet.

6. The device for preparing perfluoro n-propyl vinyl ether dimer according to claim 5, characterized in that: The three-way pipe includes a vertical pipe and an inclined connecting pipe 2, the upper end of the vertical pipe is connected to the cooling chamber and forms a fork with the connecting pipe 1, the lower end of the vertical pipe is connected to the collecting bottle, a three-way valve is provided at the intersection of the vertical pipe and the connecting pipe 2, and the end of the connecting pipe 2 is connected to the three-necked flask.

7. The device for preparing perfluoro n-propyl vinyl ether dimer according to claim 1, characterized in that: The water-avoiding mechanism comprises a shell, the bottom opening of the shell forms a containing cavity, the containing cavity is narrow at the bottom and wide at the top, a water absorbent is arranged in the containing cavity for isolating and absorbing external moisture, a vent hole is arranged at the top of the shell, the vent hole is connected to the containing cavity, and is used for balancing the air pressure inside and outside the three-necked flask.

8. The device for preparing perfluoro n-propyl vinyl ether dimer according to claim 7, characterized in that: A partition is arranged below the water absorbing agent to prevent the water absorbing agent from falling in.

Images