CN113880978A - Method and device for preparing microchannel of fluoropolyether carboxylic acid for fluorinated ethylene propylene - Google Patents
Method and device for preparing microchannel of fluoropolyether carboxylic acid for fluorinated ethylene propylene Download PDFInfo
- Publication number
- CN113880978A CN113880978A CN202111016674.7A CN202111016674A CN113880978A CN 113880978 A CN113880978 A CN 113880978A CN 202111016674 A CN202111016674 A CN 202111016674A CN 113880978 A CN113880978 A CN 113880978A
- Authority
- CN
- China
- Prior art keywords
- pump
- olefin
- raw material
- metering
- carboxylic acid
- 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.)
- Pending
Links
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F214/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen
- C08F214/18—Monomers containing fluorine
- C08F214/182—Monomers containing fluorine not covered by the groups C08F214/20 - C08F214/28
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F2/00—Processes of polymerisation
- C08F2/01—Processes of polymerisation characterised by special features of the polymerisation apparatus used
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F214/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen
- C08F214/02—Monomers containing chlorine
- C08F214/04—Monomers containing two carbon atoms
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F214/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen
- C08F214/18—Monomers containing fluorine
- C08F214/24—Trifluorochloroethene
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F214/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen
- C08F214/18—Monomers containing fluorine
- C08F214/26—Tetrafluoroethene
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F214/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen
- C08F214/18—Monomers containing fluorine
- C08F214/28—Hexyfluoropropene
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F232/00—Copolymers of cyclic compounds containing no unsaturated aliphatic radicals in a side chain, and having one or more carbon-to-carbon double bonds in a carbocyclic ring system
- C08F232/02—Copolymers of cyclic compounds containing no unsaturated aliphatic radicals in a side chain, and having one or more carbon-to-carbon double bonds in a carbocyclic ring system having no condensed rings
- C08F232/04—Copolymers of cyclic compounds containing no unsaturated aliphatic radicals in a side chain, and having one or more carbon-to-carbon double bonds in a carbocyclic ring system having no condensed rings having one carbon-to-carbon double bond
Landscapes
- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a microchannel preparation device of fluoropolyether carboxylic acid for polyfluorinated ethylene propylene, which comprises 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). The invention also provides a preparation method, which comprises the steps of pumping the raw material I, the raw material II and oxygen into a static mixer (8), mixing, introducing into a low-temperature cold trap (5), carrying out low-temperature polymerization reaction on the mixture of the raw material II and the oxygen and the raw material I in the low-temperature cold trap (5) by adopting photocatalysis generated by an ultraviolet lamp to obtain a fluorine-containing polyether carboxylic acid solution mixed with olefin, and discharging the mixed oxygen after separation; recovering the vaporized olefin; the fluoropolyether carboxylic acid solution from which the olefin has been removed is introduced into a hydrolysis reactor (11).
Description
Technical Field
The invention belongs to the technical field of fluorine-containing surfactants and preparation methods thereof, and particularly relates to a preparation method and a device of a microchannel 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 invention provides a method and a device for preparing a microchannel of fluoropolyether carboxylic acid for polyfluorinated ethylene propylene, which can recover a large amount of olefin after the preparation of the fluoropolyether carboxylic acid is finished, ensure the stable quality of products, control the reaction time according to the target yield, be convenient and quick and greatly reduce the cost.
The invention 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 preparation method of the microchannel of the fluoropolyether carboxylic acid for the fluorinated ethylene propylene 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 I, the raw material II is placed into an olefin metering tank II, the oxygen is placed into the oxygen metering tank, 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 the raw material I into a low-temperature cold trap through a metering pump I, pumping the raw material II and oxygen into a static mixer through a metering pump II and a gas delivery pump respectively, mixing, and then introducing into the low-temperature cold trap, 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 by adopting photocatalysis generated by an ultraviolet lamp to obtain a fluorine-containing polyether carboxylic acid solution mixed with olefin; step three, introducing the fluorine-containing polyether carboxylic acid solution mixed with olefin into a gas-liquid separator after the low-temperature polymerization reaction is finished, separating the mixed oxygen and then discharging the oxygen; step four, introducing the fluorine-containing polyether carboxylic acid solution mixed with the olefin after oxygen separation into a vaporizer to vaporize the mixed olefin and discharge the vaporized olefin, and recovering the vaporized olefin; and step five, introducing the fluorine-containing polyether carboxylic acid solution with the olefin removed into a hydrolysis kettle.
The raw material I is one or a combination of more of octafluoro-2-butene, octafluoro-1-butene, hexafluoropropylene, perfluoroisobutylene, tetrafluoroethylene, hexafluorocyclobutene, chlorotrifluoroethylene, tetrafluoropropene, 1 chloro-2-fluoroethylene and trichloroethylene. The raw material II is one or a combination of more of octafluoro-2-butene, octafluoro-1-butene, hexafluoropropylene, perfluoroisobutylene, tetrafluoroethylene, hexafluorocyclobutene, chlorotrifluoroethylene, tetrafluoropropene, 1 chloro-2-fluoroethylene and trichloroethylene.
In the second step of the invention, 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.
The invention 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 invention 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 invention 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 invention provides a preparation method of a microchannel of fluoropolyether carboxylic acid for polyperfluoroethylene propylene, which 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 in the step II 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; step three, 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 the oxygen; 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;
and step five, introducing the fluorine-containing polyether carboxylic acid solution with the olefin removed into the hydrolysis kettle 11.
The raw material I is one or a combination of more of octafluoro-2-butene, octafluoro-1-butene, hexafluoropropylene, perfluoroisobutylene, tetrafluoroethylene, hexafluorocyclobutene, chlorotrifluoroethylene, tetrafluoropropene, 1 chloro-2-fluoroethylene and trichloroethylene. The raw material II is one or a combination of more of octafluoro-2-butene, octafluoro-1-butene, hexafluoropropylene, perfluoroisobutylene, tetrafluoroethylene, hexafluorocyclobutene, chlorotrifluoroethylene, tetrafluoropropene, 1 chloro-2-fluoroethylene and trichloroethylene.
The following examples further illustrate the preparation of the present invention and are intended to enable one of ordinary skill in the art to understand and practice the present invention. It is to be noted, however, that the present invention is not limited to the preferred embodiments disclosed, and that any obvious modifications or equivalents thereof, based on the teachings of the present invention, should also be considered as falling within the scope of the present invention.
The invention provides a method for preparing a microchannel of fluoropolyether carboxylic acid for polyperfluoroethylene propylene, which comprises the following steps: firstly, preparing a raw material I, a raw material II and oxygen, wherein the raw material I is octafluoro-2-butene, the raw material II is hexafluorocyclobutene, the octafluoro-2-butene is placed into an olefin metering tank I1, the hexafluorocyclobutene is placed into an olefin metering tank II 2, the oxygen is placed into an oxygen metering tank 3, and the water content of the octafluoro-2-butene and the hexafluorocyclobutene is less than or equal to 30 ppm; pumping octafluoro-2-butene into a low-temperature cold trap 5 through a metering pump I4, pumping hexafluorocyclobutene 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 pumped gas and liquid can only flow in a single direction due to the arrangement of a one-way check valve I18, a one-way check valve II 19 and a one-way check valve III 20, the mixture of hexafluorocyclobutene and oxygen and the octafluoro-2-butene are subjected to low-temperature polymerization reaction in the low-temperature cold trap 5 by photocatalysis generated by an ultraviolet lamp to obtain a fluoropolyether carboxylic acid solution mixed with olefin, wherein the initial temperature of the low-temperature polymerization reaction in the second step is-40 ℃, the temperature in the polymerization reaction process is kept at-30 ℃, the pressure of the polymerization reaction is 0.12MPa, and the constant-pressure reaction is carried out; step three, 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 the oxygen; 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;
and step five, introducing the fluorine-containing polyether carboxylic acid solution with the olefin removed into the hydrolysis kettle 11.
In a second embodiment, the present invention provides a method for preparing fluoropolyether carboxylic acid for polyperfluoroethylene propylene, comprising the steps of: firstly, preparing a raw material I, a raw material II and oxygen, wherein the raw material I is octafluoro-1-butene, the raw material II is chlorotrifluoroethylene, the octafluoro-1-butene is placed into an olefin metering tank I1, the chlorotrifluoroethylene is placed into an olefin metering tank II 2, the oxygen is placed into an oxygen metering tank 3, and the water content of the octafluoro-1-butene and the chlorotrifluoroethylene is less than or equal to 30 ppm; pumping octafluoro-1-butene into a low-temperature cold trap 5 through a metering pump I4, pumping chlorotrifluoroethylene 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 pumped gas and liquid can only flow in a single direction due to the arrangement of a one-way check valve I18, a one-way check valve II 19 and a one-way check valve III 20, the mixture of the chlorotrifluoroethylene and the oxygen and the octafluoro-1-butene 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 in the second step is-40 ℃, the temperature in the polymerization reaction process is kept at-30 ℃, and the pressure of the polymerization reaction is 0.15MPa, and the constant-pressure reaction is carried out; step three, 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 the oxygen; 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;
and step five, introducing the fluorine-containing polyether carboxylic acid solution with the olefin removed into the hydrolysis kettle 11.
Claims (10)
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 microchannel of fluoropolyether carboxylic acid for polyperfluoroethylene propylene as claimed in claim 1, wherein said pump outlet of said metering pump I (4) is provided with a one-way check valve I (18), said one-way check valve I (18) is positioned between the pump outlet of said metering pump I (4) and said cooling device, said pump outlet of said metering pump II (6) is provided with a one-way check valve II (19), said one-way check valve II (19) is positioned between the pump outlet of said metering pump II (6) and the inlet of said static mixer (8), said pump outlet of said gas delivery pump (7) is provided with a one-way check valve III (20), said one-way check valve III (20) is positioned between the pump outlet of said gas delivery pump (7) and the inlet of said static mixer (8).
3. 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.
4. 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, and said static mixer (8) is a tubular static mixer.
5. 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).
6. 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.
7. The preparation method of the microchannel of the fluoropolyether carboxylic acid for the fluorinated ethylene propylene is characterized by comprising 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 I (1), 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 the raw material I into a low-temperature cold trap (5) through a metering pump I (4), respectively pumping the raw material II and oxygen into a static mixer (8) through a metering pump II (6) and a gas delivery pump (7) for mixing, then introducing into the low-temperature cold trap (5), and carrying out low-temperature polymerization reaction on the mixture of the raw material II and the oxygen and the raw material I in the low-temperature cold trap (5) by adopting photocatalysis generated by an ultraviolet lamp to obtain a fluorine-containing polyether carboxylic acid solution mixed with olefin;
step three, 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;
and step five, introducing the fluorine-containing polyether carboxylic acid solution with the olefin removed into a hydrolysis kettle (11).
8. The process of claim 7, wherein the raw material I is one or more selected from octafluoro-2-butene, octafluoro-1-butene, hexafluoropropylene, perfluoroisobutylene, tetrafluoroethylene, hexafluorocyclobutene, chlorotrifluoroethylene, tetrafluoropropene, 1 chloro 2-fluoroethylene, and trichloroethylene.
9. The process of claim 7, wherein the raw material II is one or more selected from octafluoro-2-butene, octafluoro-1-butene, hexafluoropropylene, perfluoroisobutylene, tetrafluoroethylene, hexafluorocyclobutene, chlorotrifluoroethylene, tetrafluoropropene, 1 chloro 2-fluoroethylene, and trichloroethylene.
10. The method of claim 7, wherein the initial temperature of the low temperature polymerization reaction in the second step is-40 ℃, the temperature during the polymerization reaction is maintained at-30 ℃, and the pressure of the polymerization reaction is 0.12 to 0.15 MPa.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202111016674.7A CN113880978A (en) | 2021-08-31 | 2021-08-31 | Method and device for preparing microchannel of fluoropolyether carboxylic acid for fluorinated ethylene propylene |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202111016674.7A CN113880978A (en) | 2021-08-31 | 2021-08-31 | Method and device for preparing microchannel of fluoropolyether carboxylic acid for fluorinated ethylene propylene |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN113880978A true CN113880978A (en) | 2022-01-04 |
Family
ID=79011559
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202111016674.7A Pending CN113880978A (en) | 2021-08-31 | 2021-08-31 | Method and device for preparing microchannel of fluoropolyether carboxylic acid for fluorinated ethylene propylene |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN113880978A (en) |
Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20110207880A1 (en) * | 2008-08-15 | 2011-08-25 | Nova-Duet Technologies, Pty. Ltd. | Peroxidic fluoropolyether and its use in emulsion polymerization of fluorin-containing monomer |
| CN103554318A (en) * | 2013-10-21 | 2014-02-05 | 应悦 | Method and device for preparing fluorine-containing polymer under micro-emulsion form |
| CN104530291A (en) * | 2014-12-17 | 2015-04-22 | 中昊晨光化工研究院有限公司 | Chlorotrifluoroethylene modified fluorinated ethylene propylene resin and preparation method thereof |
| CN105344289A (en) * | 2015-09-30 | 2016-02-24 | 成都晨光博达橡塑有限公司 | Fluorine-containing surfactant free of perfluorooctanoic acid and salts thereof |
| CN106076195A (en) * | 2016-07-28 | 2016-11-09 | 浙江赞宇科技股份有限公司 | The technique of a kind of continuous preparation alkyl ether carboxylic acid's salt surfactant and device |
| CN109851470A (en) * | 2019-03-19 | 2019-06-07 | 浙江巨化技术中心有限公司 | A method of the chloro- 1,1,1,4,4,4- hexafluoro -2- butylene of 2- is prepared using micro passage reaction |
| CN112028803A (en) * | 2020-08-21 | 2020-12-04 | 青岛中科荣达新材料有限公司 | Method for synthesizing liquid sodium dimethyl dithiocarbamate by using microchannel reactor |
| CN216404266U (en) * | 2021-08-31 | 2022-04-29 | 泰兴梅兰新材料有限公司 | Fluorinated polyether carboxylic acid microchannel preparation device for fluorinated ethylene propylene |
-
2021
- 2021-08-31 CN CN202111016674.7A patent/CN113880978A/en active Pending
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20110207880A1 (en) * | 2008-08-15 | 2011-08-25 | Nova-Duet Technologies, Pty. Ltd. | Peroxidic fluoropolyether and its use in emulsion polymerization of fluorin-containing monomer |
| CN103554318A (en) * | 2013-10-21 | 2014-02-05 | 应悦 | Method and device for preparing fluorine-containing polymer under micro-emulsion form |
| CN104530291A (en) * | 2014-12-17 | 2015-04-22 | 中昊晨光化工研究院有限公司 | Chlorotrifluoroethylene modified fluorinated ethylene propylene resin and preparation method thereof |
| CN105344289A (en) * | 2015-09-30 | 2016-02-24 | 成都晨光博达橡塑有限公司 | Fluorine-containing surfactant free of perfluorooctanoic acid and salts thereof |
| CN106076195A (en) * | 2016-07-28 | 2016-11-09 | 浙江赞宇科技股份有限公司 | The technique of a kind of continuous preparation alkyl ether carboxylic acid's salt surfactant and device |
| CN109851470A (en) * | 2019-03-19 | 2019-06-07 | 浙江巨化技术中心有限公司 | A method of the chloro- 1,1,1,4,4,4- hexafluoro -2- butylene of 2- is prepared using micro passage reaction |
| CN112028803A (en) * | 2020-08-21 | 2020-12-04 | 青岛中科荣达新材料有限公司 | Method for synthesizing liquid sodium dimethyl dithiocarbamate by using microchannel reactor |
| CN216404266U (en) * | 2021-08-31 | 2022-04-29 | 泰兴梅兰新材料有限公司 | Fluorinated polyether carboxylic acid microchannel preparation device for fluorinated ethylene propylene |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CA2888298C (en) | Efficient, high-yield conversion of monosaccharides to 5-(chloromethyl)-2-furaldehyde | |
| CN216404266U (en) | Fluorinated polyether carboxylic acid microchannel preparation device for fluorinated ethylene propylene | |
| CN111918839B (en) | Method and apparatus for producing molybdenum hexafluoride | |
| CN105084369B (en) | A kind of recycling and processing device of chlorine-containing silane waste gas | |
| CN111643917B (en) | Continuous production device and method for 1,1, 3-trichloropropene | |
| CN113880978A (en) | Method and device for preparing microchannel of fluoropolyether carboxylic acid for fluorinated ethylene propylene | |
| CN105367379B (en) | A kind of method that utilization circular response prepares perfluoroethane | |
| CN102531827A (en) | Method for preparing dichloroethane through direct chlorination by using dry gas | |
| EP4268950A1 (en) | Continuous preparation system and method for vinylidene chloride | |
| CN115490215B (en) | Device and method for preparing nitrogen trifluoride | |
| CN103318842A (en) | HCL gas recycling process and HCL gas recycling device in gaseous phase chlorination reaction | |
| CN108569739B (en) | System and method for recovering OP-10 in polytetrafluoroethylene concentrated dispersion liquid waste liquid | |
| CN107902627B (en) | High-purity chlorine dioxide generator | |
| CN101723454A (en) | Method for preparing antimony pentafluoride | |
| US20030111429A1 (en) | Cavitation method and apparatus for deaeration | |
| CN107998679B (en) | Device and method for improving vacuum degree of acyl chloride vacuum rectification | |
| US10787412B2 (en) | Recovery and use of wood acetylation fluid | |
| CN211800863U (en) | Chlorohydrination reaction device for chlorohydrination process of epoxide | |
| CN105152134B (en) | A kind of method and device for preparing hydrogen fluoride | |
| CN107663144A (en) | A kind of method of methanol in removal hexafluoropropene | |
| CN107857695B (en) | Device and method for improving yield of 2-propoxyl chloroethane | |
| JP5320684B2 (en) | Method for producing dichlorobutene | |
| CN105111093A (en) | Production process of ethanolamine | |
| CN212998463U (en) | Tetrafluoroethylene polymerization inhibitor recovery system | |
| CN220276989U (en) | Aromatic amine alkylation device |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination |