CN216404266U

CN216404266U - Fluorinated polyether carboxylic acid microchannel preparation device for fluorinated ethylene propylene

Info

Publication number: CN216404266U
Application number: CN202122081475.6U
Authority: CN
Inventors: 景宏伟; 徐�明; 钱厚琴; 孙生勤
Original assignee: Taixing Meilan New Material Co ltd
Current assignee: Taixing Meilan New Material Co ltd
Priority date: 2021-08-31
Filing date: 2021-08-31
Publication date: 2022-04-29
Anticipated expiration: 2031-08-31

Abstract

The utility model discloses a microchannel preparation device of fluoropolyether carboxylic acid for polyperfluorinated ethylene propylene, wherein an olefin metering tank I (1) is communicated with a metering pump I (4), an olefin metering tank II (2) is communicated with a metering pump II (6), an oxygen metering tank (3) is communicated with a gas delivery pump (7), a pipeline I (12) is respectively communicated with the metering pump I (4) and a cooling device, the metering pump II (6) and the gas delivery pump (7) are both communicated with an inlet of a static mixer (8), a pipeline II (13) is respectively communicated with an outlet of the static mixer (8) and the cooling device, an outlet of the cooling device is communicated with an inlet of a gas-liquid separator (9), a liquid outlet (15) of the gas-liquid separator (9) positioned at the bottom is communicated with an inlet of a vaporizer (10), and an outlet of the vaporizer (10) is communicated with a hydrolysis kettle (11) through a pipeline III (17). The utility model solves the problem of recovering a large amount of olefin after the preparation of the fluorine-containing polyether carboxylic acid is finished.

Description

Fluorinated polyether carboxylic acid microchannel preparation device for fluorinated ethylene propylene

Technical Field

The utility model belongs to the technical field of fluorine-containing surfactants and preparation methods thereof, and particularly relates to a microchannel preparation device of fluorine-containing polyether carboxylic acid for fluorinated ethylene propylene.

Background

The quality difference of the fluorinated ethylene propylene resin is caused by the difference of the particle size, the particle size distribution and the particle shape, and the particle size of the dispersed tetrafluoro resin produced by emulsion polymerization is small, the particle size distribution is reasonable, the particle shape is controllable, so the processing performance and the product performance are good.

Ammonium Perfluorooctanoate (PFOA) is the most commonly used emulsifier in the polymerization of perfluoroethylene propylene, but is also one of the most difficult organic pollutants known to degrade, with high bioaccumulation and various toxicities, defined by the chemical commission as a substance that persists in the environment, is bioaccumulative and is harmful to humans. Under such a large background, a global substitution of perfluorooctanoic acid is imperative.

Disclosure of Invention

The utility model provides a microchannel preparation device of fluoropolyether carboxylic acid for polyperfluoroethylene propylene, which can recover a large amount of olefin after the preparation of fluoropolyether carboxylic acid is finished, simultaneously ensures the stable quality of products, can control the reaction time according to the target yield, is convenient and quick and greatly reduces the cost.

The utility model adopts the following technical scheme: the microchannel preparation device of the fluoropolyether carboxylic acid for the fluorinated ethylene propylene comprises an olefin metering tank I, an olefin metering tank II, an oxygen metering tank, a metering pump I, a metering pump II, a gas delivery pump, a static mixer, a cooling device, a gas-liquid separator, a vaporizer and a hydrolysis kettle, wherein a discharge port of the olefin metering tank I is communicated with a pump inlet of the metering pump I, a discharge port of the olefin metering tank II is communicated with a pump inlet of the metering pump II, a discharge port of the oxygen metering tank is communicated with a pump inlet of the gas delivery pump, an outlet of the metering pump I is connected with a pipeline I, one end of the pipeline I is communicated with an outlet of the metering pump I, the other end of the pipeline I extends into the cooling device, an outlet of the metering pump II and an outlet of the gas delivery pump are communicated with an inlet of the static mixer, an outlet of the static mixer is connected with a pipeline II, one end of the pipeline II is communicated with an outlet of the static mixer, the other end of the pipeline II extends into the cooling device, an outlet of the cooling device is communicated with an inlet of the gas-liquid separator, a gas outlet of the gas-liquid separator is positioned at the top, a liquid outlet of the gas-liquid separator, which is positioned at the bottom, is communicated with an inlet of the vaporizer, a recycling port of the vaporizer is positioned at the top, and an outlet of the vaporizer is communicated with the hydrolysis kettle through a pipeline III.

Pump export department of measuring pump I be equipped with one-way check valve I, one-way check valve I is located between the pump export and the cooling device of measuring pump I, the pump export department of measuring pump II is equipped with one-way check valve II, one-way check valve II is located between the pump export of measuring pump II and the import of static mixer, the pump export department of gas transfer pump is equipped with one-way check valve III, one-way check valve III is located between the pump export of gas transfer pump and the import of static mixer.

The gas delivery pump is set as a vacuum pump. And the olefin metering tank I and the olefin metering tank II are both set to be vacuum metering tanks, and the static mixer is set to be a tubular static mixer.

The cooling device is set as a low-temperature cold trap, a refrigerant is placed in the low-temperature cold trap, and an ultraviolet lamp is inserted in the low-temperature cold trap. The pipeline I and the pipeline II are both set to be F46 pipes.

The utility model has the following beneficial effects: by adopting the technical scheme, the method can recover a large amount of olefin after the preparation of the fluoropolyether carboxylic acid is finished, simultaneously ensures the stable product quality, can control the reaction time according to the target yield, is convenient and quick, and greatly reduces the cost. The utility model can effectively adjust the feeding speed by putting the raw material I into the olefin metering tank I, putting the raw material II into the olefin metering tank II and putting the oxygen into the oxygen metering tank, thereby achieving the continuous production process. The low-temperature cold trap increases the photocatalytic reaction area during polymerization reaction, improves the retention time, ensures the stable product quality, can control the reaction time according to the target yield, is convenient and quick, greatly reduces the cost, and has less gas amount in a mixed explosion space, safety and reliability compared with a large kettle type reactor.

Drawings

FIG. 1 is a schematic structural diagram of the present invention.

Detailed Description

In figure 1, the utility model provides a microchannel preparation device of fluoropolyether carboxylic acid for polyperfluorinated ethylene propylene, which comprises an olefin metering tank I1, an olefin metering tank II 2, an oxygen metering tank 3, a metering pump I4, a metering pump II 6, a gas delivery pump 7, a static mixer 8, a cooling device, a gas-liquid separator 9, a vaporizer 10 and a hydrolysis kettle 11, wherein the olefin metering tank I1 and the olefin metering tank II 2 are both set as vacuum metering tanks, the olefin metering tank I1 and the olefin metering tank II 2 are both vacuumized by adding nitrogen with gauge pressure of 0.1Mpa, the temperature during storage is 25 ℃, the vacuumizing is generally carried out for three times, the gas delivery pump 7 is set as a vacuum pump, the static mixer 8 is set as a tubular static mixer, a discharge port of the olefin metering tank I1 is communicated with a pump inlet of the metering pump I4, a discharge port of the olefin metering tank II 2 is communicated with a pump inlet of the metering pump II 6, the discharge hole of the oxygen metering tank 3 is communicated with the pump inlet of the gas delivery pump 7, the pump outlet of the metering pump I4 is connected with a pipeline I12, the pipelines I12 are all set to be F46 pipes, one end of the pipeline I12 is communicated with the pump outlet of the metering pump I4, the other end of the pipeline I12 extends into the cooling device, the pump outlet of the metering pump II 6 and the pump outlet of the gas delivery pump 7 are both communicated with the inlet of the static mixer 8, the outlet of the static mixer 8 is connected with a pipeline II 13, the pipeline II 13 is set to be an F46 pipe, one end of the pipeline II 13 is communicated with the outlet of the static mixer 8, the other end of the pipeline II 13 extends into the cooling device, the outlet of the cooling device is communicated with the inlet of the gas-liquid separator 9, the cooling device is set to be a low-temperature cold trap 5, a refrigerant 21 is placed in the low-temperature cold trap 5, an ultraviolet lamp 22 is inserted in the low-temperature cold trap 5, and the gas outlet 14 of the gas-liquid separator 9 is positioned at the top, the liquid outlet 15 that vapour and liquid separator 9 is located the bottom is linked together with the import of vaporizer 10, and recovery mouth 16 of vaporizer 10 is located the top, and the export of vaporizer 10 is linked together through pipeline III 17 and hydrolysis kettle 11, the pump export department of measuring pump I4 be equipped with one-way check valve I18, one-way check valve I18 is located between the pump export of measuring pump I4 and cooling device, the pump export department of measuring pump II 6 is equipped with one-way check valve II 19, one-way check valve II 19 is located between the pump export of measuring pump II 6 and static mixer 8's the import, the pump export department of gas delivery pump 7 is equipped with one-way check valve III 20, one-way check valve III 20 is located between the pump export of gas delivery pump 7 and static mixer 8's the import.

The use method of the utility model comprises the following steps: firstly, preparing a raw material I, a raw material II and oxygen, wherein the raw material I is placed into an olefin metering tank I1, the raw material II is placed into an olefin metering tank II 2, the oxygen is placed into an oxygen metering tank 3, the raw material I is olefin, the raw material II is olefin, and the water content of the raw material I and the water content of the raw material II are less than or equal to 30 ppm; pumping a raw material I into a low-temperature cold trap 5 through a metering pump I4, pumping a raw material II and oxygen into a static mixer 8 through a metering pump II 6 and a gas delivery pump 7 respectively, mixing, and then introducing into the low-temperature cold trap 5, wherein the mixture of the raw material II and the oxygen and the raw material I are subjected to low-temperature polymerization reaction in the low-temperature cold trap 5 by photocatalysis generated by an ultraviolet lamp to obtain a fluorine-containing polyether carboxylic acid solution mixed with olefin, wherein the initial temperature of the low-temperature polymerization reaction is-40 ℃, the temperature in the polymerization reaction process is kept at-30 ℃, and the pressure of the polymerization reaction is 0.12-0.15 MPa; after the low-temperature polymerization reaction is finished, introducing the fluorine-containing polyether carboxylic acid solution mixed with olefin into a gas-liquid separator 9, separating the mixed oxygen and then discharging; step four, introducing the fluorine-containing polyether carboxylic acid solution mixed with olefin after oxygen separation into a vaporizer 10 to vaporize the mixed olefin and discharge the vaporized olefin, and recovering the vaporized olefin; the fluoropolyether carboxylic acid solution from which the olefin has been removed is introduced into the hydrolysis reactor 11.

Claims

1. The microchannel preparation device of the fluoropolyether carboxylic acid for the fluorinated ethylene propylene is characterized by comprising an olefin metering tank I (1), an olefin metering tank II (2), an oxygen metering tank (3), a metering pump I (4), a metering pump II (6), a gas delivery pump (7), a static mixer (8), a cooling device, a gas-liquid separator (9), a vaporizer (10) and a hydrolysis kettle (11), wherein a discharge port of the olefin metering tank I (1) is communicated with a pump inlet of the metering pump I (4), a discharge port of the olefin metering tank II (2) is communicated with a pump inlet of the metering pump II (6), a discharge port of the oxygen metering tank (3) is communicated with a pump inlet of the gas delivery pump (7), an outlet of the metering pump I (4) is connected with a pipeline I (12), one end of the pipeline I (12) is communicated with an outlet of the metering pump I (4), and the other end of the pipeline I (12) extends into the cooling device, the pump outlet of the metering pump II (6) and the pump outlet of the gas conveying pump (7) are communicated with the inlet of the static mixer (8), the outlet of the static mixer (8) is connected with a pipeline II (13), one end of the pipeline II (13) is communicated with the outlet of the static mixer (8), the other end of the pipeline II (13) extends into the cooling device, the outlet of the cooling device is communicated with the inlet of the gas-liquid separator (9), the gas outlet (14) of the gas-liquid separator (9) is positioned at the top, the liquid outlet (15) of the gas-liquid separator (9) positioned at the bottom is communicated with the inlet of the vaporizer (10), the recovery port (16) of the vaporizer (10) is positioned at the top, and the outlet of the vaporizer (10) is communicated with the hydrolysis kettle (11) through a pipeline III (17).

2. The apparatus for preparing a fluoropolyether carboxylic acid microchannel for polyperfluoroethylene propylene as claimed in claim 1, wherein a one-way check valve I (18) is disposed at the pump outlet of the metering pump I (4), and the one-way check valve I (18) is disposed between the pump outlet of the metering pump I (4) and the cooling device.

3. The apparatus for preparing a fluoropolyether carboxylic acid microchannel for poly (perfluoroethylene propylene) according to claim 1, wherein the pump outlet of the metering pump II (6) is provided with a one-way check valve II (19), and the one-way check valve II (19) is positioned between the pump outlet of the metering pump II (6) and the inlet of the static mixer (8).

4. The apparatus for preparing fluoropolyether carboxylic acid for poly (perfluoroethylene propylene) according to claim 1, wherein said gas delivery pump (7) is provided at the outlet thereof with a one-way check valve III (20), said one-way check valve III (20) being disposed between the outlet of said gas delivery pump (7) and the inlet of said static mixer (8).

5. The apparatus for producing a fluoropolyether carboxylic acid for polyperfluoroethylene propylene as claimed in claim 1 or 2, wherein said gas-conveying pump (7) is provided as a vacuum pump.

6. The apparatus for producing a fluoropolyether carboxylic acid for polyperfluoroethylene propylene as claimed in claim 1, wherein said olefin metering tank I (1) and said olefin metering tank II (2) are both vacuum metering tanks.

7. The apparatus for producing a fluoropolyether carboxylic acid for polyperfluoroethylene propylene as claimed in claim 1, wherein said static mixer (8) is provided as a tubular static mixer.

8. The apparatus for producing a fluoropolyether carboxylic acid having a microchannel as claimed in claim 1 or 2, wherein the cooling apparatus is a cryotrap (5), a refrigerant (21) is placed in the cryotrap (5), and an ultraviolet lamp (22) is inserted into the cryotrap (5).

9. The apparatus for producing a fluoropolyether carboxylic acid for perfluoroethylene propylene according to claim 1, wherein said line I (12) and said line II (13) are each an F46 pipe.