CN115814737A - Device and method for continuously preparing tetrafluoroethane-beta-sultone - Google Patents
Device and method for continuously preparing tetrafluoroethane-beta-sultone Download PDFInfo
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Abstract
The invention discloses a device and a method for continuously preparing tetrafluoroethane-beta-sultone. The invention has the advantages of simple structure, safety, controllability, high reaction efficiency and good product selectivity.
Description
Technical Field
The invention relates to the field of organic synthesis, in particular to a device and a method for continuously preparing tetrafluoroethane-beta-sultone.
Background
Tetrafluoroethane-beta-sultone is a volatile, highly irritating, colorless, transparent liquid, CAS no: 697-18-7, molecular formula C2F4SO3, molecular weight: 180.08, boiling point: 41 ℃ (101.3 KPa), liquid density: 1.6g/ml (25 ℃), is easily soluble in ether solvents. The chemical structural formula of tetrafluoroethane-beta-sultone is as follows:
the perfluoroalkyl sultone is an important fluorine-containing intermediate, and can be used for preparing functional compounds containing sulfonic groups, wherein tetrafluoroethane-beta-sultone is a widely-applied perfluoroalkyl sultone. The perfluoroalkyl sultone can react with various olefins, cycloparaffins, nucleophiles and the like to synthesize fluorine-containing compounds with various structures because of having special structures, and the fluorine-containing compounds are mainly used for synthesizing functional polymer materials and fine chemicals, such as PSVE, fluorine-containing surfactants, fluorine grease and the like. Tetrafluoroethane-beta-sultone mainly composed of sulfur trioxide (SO) 3 ) And Tetrafluoroethylene (TFE) by the following main reaction formula:
at present, the synthesis of tetrafluoroethane-beta-sultone usually adopts intermittent kettle type reaction, the reaction has large heat release, the corrosivity of raw materials and products is extremely strong, and the method also has explosive risk, and has great safety risk in actual production. In response to this problem, some modifications have been made to the reaction apparatus by researchers.
For example, CN111072627A discloses a method for synthesizing tetrafluoroethane- β -sultone, in which sulfur trioxide and perfluoroolefin are continuously introduced into a micro mixer to be mixed, and then enter a microchannel reactor to react. The method improves the safety of the process, but the reactor is easy to generate the phenomenon of blockage because of the self-polymerization of TFE.
Also, for example, CN114950320A discloses a kettle type continuous reaction apparatus, which comprises two kettle type reactors connected in series, wherein the material of the first reaction kettle overflows to the second reaction kettle through an overflow port of the reaction kettle. The process gives high product yields but also risks in terms of safety at scale-up.
Disclosure of Invention
The invention aims to solve the problems in the prior art and provides a device and a method for continuously preparing tetrafluoroethane-beta-sultone, which have the advantages of simple structure, safety, controllability, high reaction efficiency and good product selectivity.
In order to achieve the above object, the present invention is realized by the following technical solutions: the utility model provides a device of serialization preparation tetrafluoroethane-beta-sultone, is including the mixing tank, measuring pump, reactor, condenser and the crude collecting vat that connect gradually, the discharge gate of mixing tank with the access connection of measuring pump, the condensate export of condenser with the access connection of crude collecting vat, the reactor comprises one-level tubular reactor, secondary tubular reactor and tertiary tubular reactor of establishing ties, the export of measuring pump with the feed inlet of one-level tubular reactor links to each other, the discharge gate of one-level tubular reactor with the feed inlet of secondary tubular reactor is connected, the discharge gate of secondary tubular reactor with the feed inlet of tertiary tubular reactor is connected, the discharge gate of tertiary tubular reactor with the gaseous phase import of condenser links to each other, one-level tubular reactor in be provided with the first gas distributor that is used for first way tetrafluoroethylene to get into, secondary tubular reactor in be provided with the second gas distributor that is used for the second way tetrafluoroethylene to get into, tertiary tubular reactor in be provided with the third gas distributor that is used for third way tetrafluoroethylene to get into.
In a preferred embodiment of the present invention, the first gas distributor, the second gas distributor and the third gas distributor are tubular, and the first gas distributor, the second gas distributor and the third gas distributor are provided with 5 to 15 layers of feed gas distribution holes with a pore size of 300 to 600um uniformly distributed along the axial direction.
The method for continuously preparing the tetrafluoroethane-beta-sultone by using the device comprises the following steps:
(1) Respectively and continuously pumping sulfur trioxide and tetrafluoroethane-beta-sultone mother liquor into a mixing tank to be uniformly mixed, then continuously feeding the mixed material of the sulfur trioxide and the tetrafluoroethane-beta-sultone mother liquor into a primary tubular reactor from the mixing tank through a metering pump, and simultaneously continuously feeding a first path of tetrafluoroethylene into the primary tubular reactor through a first gas distributor to react to obtain primary reaction liquid;
(2) Continuously feeding the first-stage reaction liquid into a secondary tubular reactor, and simultaneously continuously feeding a second path of tetrafluoroethylene into the secondary tubular reactor through a second gas distributor for reaction to obtain a second-stage reaction liquid;
(3) Continuously feeding the second-stage reaction liquid into a third-stage tubular reactor, and simultaneously continuously feeding a third path of tetrafluoroethylene into the third-stage tubular reactor through a third gas distributor for reaction to obtain a third-stage reaction liquid;
(4) And continuously feeding the tertiary reaction liquid into a condenser, collecting the obtained tetrafluoroethane-beta-sultone crude product into a crude product collecting tank, and carrying out additional rectification to obtain the tetrafluoroethane-beta-sultone product.
As a preferred embodiment of the invention, the molar ratio of the first path of tetrafluoroethylene entering the first-stage tubular reactor, the second path of tetrafluoroethylene entering the second-stage tubular reactor and the third path of tetrafluoroethylene entering the third-stage tubular reactor is 1: 0.75-1.3: 0.5-1.3.
As a preferable embodiment of the invention, the temperature of the primary tubular reactor, the temperature of the secondary tubular reactor and the temperature of the tertiary tubular reactor are all 30-60 ℃, and the pressure is all 0.05-0.2 MPa.
As a preferred embodiment of the invention, the feeding molar ratio of the sulfur trioxide and the tetrafluoroethane-beta-sultone mother liquor entering the primary tubular reactor is 1: 2.5-5.
As a preferred embodiment of the present invention, the total feed molar ratio of sulfur trioxide to tetrafluoroethylene is 1: 1 to 1.5.
The device for continuously preparing the tetrafluoroethane-beta-sultone adopts three-stage series-connected tubular reactors, TFE is divided into three paths to respectively enter each stage of tubular reactor, sulfur trioxide and tetrafluoroethane-beta-sultone mother liquor are firstly mixed in a mixing tank, then a mixed material is injected into a first-stage tubular reactor by a metering pump to react, the reacted mixture continuously enters a second-stage tubular reactor and a third-stage tubular reactor to continuously react, materials discharged from the third-stage tubular reactor are condensed by a condenser and collected into a crude product collecting tank, and the crude product is subjected to conventional rectification and purification in the field to obtain a pure product with the purity of more than 99.5%. The method has the advantages of safe and controllable reaction process, high reaction efficiency, less self-polymerization of the TFE raw material and good product selectivity.
Compared with the prior art, the invention has the following advantages:
1. the method has the advantages of simple structure and high reaction efficiency, realizes the continuous addition reaction of sulfur trioxide and tetrafluoroethylene to prepare tetrafluoroethane-beta-sultone by adopting the three-stage tubular reactor and optimizing process parameters, simplifies the operation process, shortens the reaction time, obviously simplifies the production process, improves the reaction efficiency, and ensures that the product selectivity is over 96.6 percent.
2. The tubular reactor is safe and controllable, and the heat generated by the reaction can be removed in time by utilizing the efficient mass transfer and heat transfer characteristics of the tubular reactor, so that the self-polymerization of the tetrafluoroethylene and the generation of byproducts are reduced; the gas distributor is arranged in each stage of tubular reactor, tetrafluoroethylene enters the reactor in three paths, and the fed tetrafluoroethylene is uniformly dispersed into the reactor through the feeding gas distribution holes arranged on the gas distributor, so that the materials are stable in proportion and can be effectively contacted, the temperature distribution is uniform in the reaction process, and the stable control capability of the reaction is obviously enhanced; the sulfur trioxide and the tetrafluoroethane-beta-sultone mother liquor are mixed and fed, so that the heat transfer efficiency of the reaction is enhanced, and the safety of the reaction is improved.
3. The invention is suitable for industrialization, has large operation flexibility, can increase or reduce the number of tubular reactors according to the actual production condition, can accurately control the feeding proportion of materials by adopting a metering pump and a regulating valve to control raw materials, realizes continuous production, has small device volume and small occupied area, and is easy for industrialized production.
Drawings
Fig. 1 is a schematic diagram of an apparatus for continuously preparing tetrafluoroethane-beta-sultone according to the present invention.
In the figure: the device comprises a mixing tank 1, a metering pump 2, a primary tubular reactor 3, a secondary tubular reactor 4, a tertiary tubular reactor 5, a condenser 6, a crude product collecting tank 7, a first gas distributor 3-1, a second gas distributor 4-1 and a third gas distributor 5-1.
Detailed Description
As shown in the attached drawing, the device for continuously preparing tetrafluoroethane-beta-sultone comprises a mixing tank 1, a metering pump 2, a reactor, a condenser 6 and a crude product collecting tank 7 which are sequentially connected, wherein a discharge port of the mixing tank 1 is connected with an inlet of the metering pump 2, a condensate outlet of the condenser 6 is connected with an inlet of the crude product collecting tank 7, the reactor consists of a primary tubular reactor 3, a secondary tubular reactor 4 and a tertiary tubular reactor 5 which are connected in series, an outlet of the metering pump 2 is connected with a feed port of the primary tubular reactor 3, a discharge port of the primary tubular reactor 3 is connected with a feed port of the secondary tubular reactor 4, a discharge port of the secondary tubular reactor 4 is connected with a feed port of the tertiary tubular reactor 5, a discharge port of the tertiary tubular reactor 5 is connected with a gas phase inlet of the condenser 6, a first gas distributor 3-1 for feeding a first path of tetrafluoroethylene is arranged in the primary tubular reactor 3, a second gas distributor 4-1 for feeding a second path of tetrafluoroethylene is arranged in the secondary tubular reactor 4, a third gas distributor 5-1 for feeding a third path of tetrafluoroethylene is arranged in the tertiary tubular reactor 5, and a third gas distributor 5-1 and a third gas distributor 5 are respectively arranged in the third gas distributor 5.
The process flow for continuously preparing the tetrafluoroethane-beta-sultone by using the device is as follows:
(1) Respectively and continuously introducing sulfur trioxide and tetrafluoroethane-beta-sultone mother liquor into a mixing tank 1 to be uniformly mixed, continuously feeding a mixed material of the sulfur trioxide and the tetrafluoroethane-beta-sultone mother liquor into a primary tubular reactor 3 from the mixing tank 1 through a metering pump 2, continuously and uniformly spraying a first path of tetrafluoroethylene into the primary tubular reactor 3 through a first gas distributor 3-1 at a stable flow rate, dissolving the sulfur trioxide and the tetrafluoroethylene into the tetrafluoroethane-beta-sultone mother liquor to be fully contacted for reaction, and obtaining a primary reaction liquid;
(2) Continuously feeding the first-stage reaction liquid into a secondary tubular reactor 4, continuously and uniformly spraying a second path of tetrafluoroethylene into the secondary tubular reactor 4 through a second gas distributor 4-1 at a stable flow rate, uniformly distributing the tetrafluoroethylene in the reactor, and enabling reaction materials to be in stable proportion and fully contact for reaction to obtain a secondary reaction liquid;
(3) Continuously feeding the second-stage reaction liquid into a third-stage tubular reactor 5, simultaneously continuously and uniformly spraying a third path of tetrafluoroethylene into the third-stage tubular reactor 5 through a third gas distributor 5-1 at a stable flow rate, wherein the tetrafluoroethylene is uniformly distributed in the reactor, so that the reaction materials are stably proportioned and fully contacted for reaction to obtain a third-stage reaction liquid;
(4) And continuously feeding the tertiary reaction liquid into a condenser 6, collecting the obtained tetrafluoroethane-beta-sultone crude product into a crude product collecting tank 7, and carrying out additional rectification to obtain a tetrafluoroethane-beta-sultone product.
The present invention is described in further detail below by way of examples, and it is to be understood that the examples described herein are for purposes of illustration and explanation only and are not intended to limit the present invention.
Example 1
A device for continuously preparing tetrafluoroethane-beta-sultone, which comprises a mixing tank 1, a metering pump 2 and a primary tubular reactor 3 (material 316L,
) A two-stage tubular reactor 4 (material 316L,
) And a three-stage tubular reactor 5 (material 316L,
) Condenser 6 and crude product collecting vat 7, the discharge gate of mixing tank 1 and the access connection of measuring pump 2, the export of measuring pump 2 links to each other with one-level tubular reactor 3's feed inlet, one-level tubular reactor 3's discharge gate and second tubular reactor 4's feed inlet are connected, second tubular reactor 4's discharge gate and third tubular reactor 5's feed inlet are connected, third tubular reactor 5's play of third tubular reactor 5 is connectedThe material inlet is connected with a gas phase inlet of a condenser 6, a condensate outlet of the condenser 6 is connected with an inlet of a crude product collecting tank 7, a first tubular gas distributor 3-1 for a first path of tetrafluoroethylene to enter is arranged in the first-stage tubular reactor 3, a second tubular gas distributor 4-1 for a second path of tetrafluoroethylene to enter is arranged in the second-stage tubular reactor 4, a third tubular gas distributor 5-1 for a third path of tetrafluoroethylene to enter is arranged in the third-stage tubular reactor 5, and eight layers of feeding gas distribution holes (the hole diameter is 300 mu m) are respectively and uniformly distributed on the first gas distributor 3-1, the second gas distributor 4-1 and the third gas distributor 5-1 along the axial direction.
The device has the following technological parameters when being used for continuously preparing tetrafluoroethane-beta-sultone:
the reaction temperature of the first-stage tubular reactor, the reaction temperature of the second-stage tubular reactor and the reaction temperature of the third-stage tubular reactor are all 40 ℃, and the pressure is all 0.1MPa;
the sulfur trioxide feeding flow is 5.6mol/h;
the feed flow of the tetrafluoroethane-beta-sultone mother liquor is 16.8mol/h;
the TFE feeding flow of the first-stage tubular reactor is 2.69mol/h;
the TFE feeding flow of the secondary tubular reactor is 2.02mol/h;
the TFE feed rate to the three-stage tubular reactor was 2.02mol/h.
As a result: the reaction process is safe and controllable, and the crude product is rectified and purified to obtain the tetrafluoroethane-beta-sultone with the purity of 99.8 percent and the selectivity of the tetrafluoroethane-beta-sultone is 96.7 percent.
Example 2
A device for continuously preparing tetrafluoroethane-beta-sultone, which comprises a mixing tank 1, a metering pump 2 and a primary tubular reactor 3 (material 316L,
) A two-stage tubular reactor 4 (material 316L,
) And a three-stage tubular reactor 5 (material 316L,
) The system comprises a condenser 6 and a crude product collecting tank 7, wherein a discharge port of a mixing tank 1 is connected with an inlet of a metering pump 2, an outlet of the metering pump 2 is connected with a feed inlet of a first-stage tubular reactor 3, a discharge port of the first-stage tubular reactor 3 is connected with a feed inlet of a second-stage tubular reactor 4, a discharge port of the second-stage tubular reactor 4 is connected with a feed inlet of a third-stage tubular reactor 5, a discharge port of the third-stage tubular reactor 5 is connected with a gas-phase inlet of the condenser 6, a condensate outlet of the condenser 6 is connected with an inlet of the crude product collecting tank 7, a first tubular gas distributor 3-1 for a first path of tetrafluoroethylene to enter is arranged in the first-stage tubular reactor 3, a second tubular gas distributor 4-1 for a second path of tetrafluoroethylene to enter is arranged in the second-stage tubular reactor 4, a third tubular gas distributor 5-1 for a third path of tetrafluoroethylene to enter is arranged in the third-stage tubular reactor 5, and ten layers of feeding gas are respectively arranged on the first gas distributor 3-1, the second gas distributor 4-1 and the third gas distributor 5-1 along the axial direction (the uniform distribution holes are 400 um).
The device has the following technological parameters when being used for continuously preparing tetrafluoroethane-beta-sultone:
the reaction temperature of the first-stage tubular reactor, the reaction temperature of the second-stage tubular reactor and the reaction temperature of the third-stage tubular reactor are all 35 ℃, and the reaction pressure is all 0.15MPa;
the sulfur trioxide feeding flow is 5.6mol/h;
the feed flow rate of the tetrafluoroethane-beta-sultone mother liquor is 14mol/h;
the TFE feeding flow of the first-stage tubular reactor is 2.18mol/h;
the TFE feeding flow of the secondary tubular reactor is 2.91mol/h;
the TFE feed rate to the three-stage tubular reactor was 2.18mol/h.
As a result: the reaction process is safe and controllable, and the crude product is rectified and purified to obtain the tetrafluoroethane-beta-sultone with the purity of 99.7 percent and the selectivity of the tetrafluoroethane-beta-sultone is 96.7 percent.
Example 3
Continuous preparation of tetrafluoroethane-beta-sulfoleneThe ester device comprises a mixing tank 1, a metering pump 2 and a primary tubular reactor 3 (material 316L,
) A two-stage tubular reactor 4 (material 316L,
) And a three-stage tubular reactor 5 (material 316L,
) The system comprises a condenser 6 and a crude product collecting tank 7, wherein a discharge port of a mixing tank 1 is connected with an inlet of a metering pump 2, an outlet of the metering pump 2 is connected with a feed inlet of a first-stage tubular reactor 3, a discharge port of the first-stage tubular reactor 3 is connected with a feed inlet of a second-stage tubular reactor 4, a discharge port of the second-stage tubular reactor 4 is connected with a feed inlet of a third-stage tubular reactor 5, a discharge port of the third-stage tubular reactor 5 is connected with a gas-phase inlet of the condenser 6, a condensate outlet of the condenser 6 is connected with an inlet of the crude product collecting tank 7, a first tubular gas distributor 3-1 for a first path of tetrafluoroethylene to enter is arranged in the first-stage tubular reactor 3, a second tubular gas distributor 4-1 for a second path of tetrafluoroethylene to enter is arranged in the second-stage tubular reactor 4, a third tubular gas distributor 5-1 for a third path of tetrafluoroethylene to enter is arranged in the third-stage tubular reactor 5, and twelve layers of feeding gas distribution holes (the uniform distribution holes are uniformly distributed along the axial direction) are respectively arranged on the first gas distributor 3-1, the second gas distributor 4-1 and the third gas distributor 5-1.
The device has the following technological parameters when being used for continuously preparing tetrafluoroethane-beta-sultone:
the reaction temperature of the first-stage tubular reactor, the reaction temperature of the second-stage tubular reactor and the reaction temperature of the third-stage tubular reactor are all 45 ℃, and the pressure is all 0.05MPa;
the sulfur trioxide feeding flow is 5.6mol/h;
the feed flow of the tetrafluoroethane-beta-sultone mother liquor is 19.6mol/h;
the TFE feeding flow of the first-stage tubular reactor is 2.35mol/h;
the TFE feeding flow of the secondary tubular reactor is 2.35mol/h;
the TFE feed rate to the three-stage tubular reactor was 3.14mol/h.
As a result: the reaction process is safe and controllable, and the crude product is rectified and purified to obtain the tetrafluoroethane-beta-sultone with the purity of 99.6 percent, and the selectivity of the tetrafluoroethane-beta-sultone is 96.6 percent.
Example 4
A device for continuously preparing tetrafluoroethane-beta-sultone, which comprises a mixing tank 1, a metering pump 2 and a primary tubular reactor 3 (material 316L,
) A two-stage tubular reactor 4 (material 316L,
) And a three-stage tubular reactor 5 (material 316L,
) The system comprises a condenser 6 and a crude product collecting tank 7, wherein a discharge port of a mixing tank 1 is connected with an inlet of a metering pump 2, an outlet of the metering pump 2 is connected with a feed inlet of a first-stage tubular reactor 3, a discharge port of the first-stage tubular reactor 3 is connected with a feed inlet of a second-stage tubular reactor 4, a discharge port of the second-stage tubular reactor 4 is connected with a feed inlet of a third-stage tubular reactor 5, a discharge port of the third-stage tubular reactor 5 is connected with a gas-phase inlet of the condenser 6, a condensate outlet of the condenser 6 is connected with an inlet of the crude product collecting tank 7, a first tubular gas distributor 3-1 for a first path of tetrafluoroethylene to enter is arranged in the first-stage tubular reactor 3, a second tubular gas distributor 4-1 for a second path of tetrafluoroethylene to enter is arranged in the second-stage tubular reactor 4, a third tubular gas distributor 5-1 for a third path of tetrafluoroethylene to enter is arranged in the third-stage tubular reactor 5, and fourteen layers of feeding gas distribution holes (the apertures of 300um uniformly distributed along the axial direction) are respectively arranged on the first gas distributor 3-1, the second gas distributor 4-1 and the third gas distributor 5-1.
The device has the following technological parameters when being used for continuously preparing tetrafluoroethane-beta-sultone:
the reaction temperature of the first-stage tubular reactor, the reaction temperature of the second-stage tubular reactor and the reaction temperature of the third-stage tubular reactor are all 40 ℃, and the pressure is all 0.05MPa;
the sulfur trioxide feeding flow is 5.6mol/h;
the feed flow of the tetrafluoroethane-beta-sultone mother liquor is 19.6mol/h;
the TFE feeding flow of the first-stage tubular reactor is 2.91mol/h;
the TFE feeding flow of the secondary tubular reactor is 2.91mol/h;
the TFE feed rate to the three-stage tubular reactor was 1.46mol/h.
As a result: the reaction process is safe and controllable, and the crude product is rectified and purified to obtain the tetrafluoroethane-beta-sultone with the purity of 99.8 percent and the selectivity of the tetrafluoroethane-beta-sultone is 96.8 percent.
Example 5
A device for continuously preparing tetrafluoroethane-beta-sultone, which comprises a mixing tank 1, a metering pump 2 and a primary tubular reactor 3 (material 316L,
) A two-stage tubular reactor 4 (material 316L,
) And a three-stage tubular reactor 5 (material 316L,
) Condenser 6 and crude collecting vat 7, the discharge gate of mixing tank 1 and the access connection of measuring pump 2, the export of measuring pump 2 links to each other with one-level tubular reactor 3's feed inlet, one-level tubular reactor 3's discharge gate and second tubular reactor 4's feed inlet are connected, second tubular reactor 4's discharge gate and tertiary tubular reactor 5's feed inlet are connected, tertiary tubular reactor 5's discharge gate links to each other with condenser 6's gaseous phase import, condenser 6's condensate export and crude collecting vat 7's access connection, be provided with the first gas distribution who is used for the first tubular of a kind of tetrafluoroethylene entering in one-level tubular reactor 3The reactor comprises a reactor 3-1, a second tubular gas distributor 4-1 for a second path of tetrafluoroethylene to enter is arranged in the secondary tubular reactor 4, a third tubular gas distributor 5-1 for a third path of tetrafluoroethylene to enter is arranged in the tertiary tubular reactor 5, and fifteen layers of feeding gas distribution holes (with the aperture of 300 mu m) are uniformly distributed on the first gas distributor 3-1, the second gas distributor 4-1 and the third gas distributor 5-1 along the axial direction respectively.
The device has the following technological parameters when being used for continuously preparing tetrafluoroethane-beta-sultone:
the reaction temperature of the first-stage tubular reactor, the reaction temperature of the second-stage tubular reactor and the reaction temperature of the third-stage tubular reactor are all 35 ℃, and the reaction pressure is all 0.1MPa;
the sulfur trioxide feeding flow is 5.6mol/h;
the feed flow of the tetrafluoroethane-beta-sultone mother liquor is 16.8mol/h;
the TFE feeding flow of the first-stage tubular reactor is 2.46mol/h;
the TFE feed flow rate of the secondary tubular reactor is 2.46mol/h;
the TFE feed rate to the three-stage tubular reactor was 1.23mol/h.
As a result: the reaction process is safe and controllable, and the crude product is rectified and purified to obtain the tetrafluoroethane-beta-sultone with the purity of 99.5 percent and the selectivity of the tetrafluoroethane-beta-sultone is 96.6 percent.
Claims (7)
1. The utility model provides a device of serialization preparation tetrafluoroethane-beta-sultone, is including the mixing tank, measuring pump, reactor, condenser and the crude collecting vat that connect gradually, the discharge gate of mixing tank with the access connection of measuring pump, the condensate outlet of condenser with the access connection of crude collecting vat, its characterized in that, the reactor comprises one-level tubular reactor, second grade tubular reactor and tertiary tubular reactor of establishing ties, the export of measuring pump with the feed inlet of one-level tubular reactor links to each other, the discharge gate of one-level tubular reactor with the feed inlet of second grade tubular reactor is connected, the discharge gate of second grade tubular reactor with the feed inlet of tertiary tubular reactor is connected, the discharge gate of tertiary tubular reactor with the gaseous phase import of condenser links to each other, be provided with the first gas distributor that is used for first way tetrafluoroethylene to get into in the one-level tubular reactor, be provided with the second gas distributor that is used for second way tetrafluoroethylene to get into in the second grade tubular reactor, be provided with the third gas distributor that is used for third way tetrafluoroethylene to get into in the tertiary tubular reactor.
2. The device for continuously preparing tetrafluoroethane-beta-sultone according to claim 1, wherein the first gas distributor, the second gas distributor and the third gas distributor are in a circular tube shape, and 5-15 layers of feeding gas distribution holes with the aperture of 300-600 um are uniformly distributed on the first gas distributor, the second gas distributor and the third gas distributor along the axial direction.
3. The method for continuously preparing tetrafluoroethane-beta-sultone by using the device of claim 1, which is characterized by comprising the following steps of:
(1) Respectively and continuously pumping sulfur trioxide and tetrafluoroethane-beta-sultone mother liquor into a mixing tank to be uniformly mixed, continuously feeding the mixed material of the sulfur trioxide and the tetrafluoroethane-beta-sultone mother liquor into a primary tubular reactor from the mixing tank through a metering pump, and simultaneously continuously feeding a first path of tetrafluoroethylene into the primary tubular reactor through a first gas distributor to perform reaction to obtain primary reaction liquid;
(2) Continuously feeding the first-stage reaction liquid into a secondary tubular reactor, and simultaneously continuously feeding a second path of tetrafluoroethylene into the secondary tubular reactor through a second gas distributor for reaction to obtain a second-stage reaction liquid;
(3) Continuously feeding the second-stage reaction liquid into a third-stage tubular reactor, and simultaneously continuously feeding a third path of tetrafluoroethylene into the third-stage tubular reactor through a third gas distributor for reaction to obtain a third-stage reaction liquid;
(4) And continuously feeding the tertiary reaction liquid into a condenser, collecting the obtained tetrafluoroethane-beta-sultone crude product into a crude product collecting tank, and carrying out additional rectification to obtain the tetrafluoroethane-beta-sultone product.
4. The continuous preparation method of tetrafluoroethane-beta-sultone as claimed in claim 3, wherein the molar ratio of the first path of tetrafluoroethylene entering the first tubular reactor, the second path of tetrafluoroethylene entering the second tubular reactor and the third path of tetrafluoroethylene entering the third tubular reactor is 1: 0.75-1.3: 0.5-1.3.
5. The continuous preparation method of tetrafluoroethane-beta-sultone as claimed in claim 3, wherein the temperature of the primary tubular reactor, the temperature of the secondary tubular reactor and the temperature of the tertiary tubular reactor are all 30-60 ℃, and the pressure of the primary tubular reactor, the secondary tubular reactor and the tertiary tubular reactor is all 0.05-0.2 MPa.
6. The continuous preparation method of tetrafluoroethane-beta-sultone as claimed in claim 3, wherein the feeding molar ratio of the sulfur trioxide to the tetrafluoroethane-beta-sultone mother liquor entering the primary tubular reactor is 1: 2.5-5.
7. The continuous process for preparing tetrafluoroethane- β -sultone as recited in claim 3, wherein the total feed molar ratio of sulfur trioxide to tetrafluoroethylene is 1: 1 to 1.5.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115433158A (en) * | 2022-10-20 | 2022-12-06 | 衢州学院 | Production method of tetrafluoroethane-beta-sultone |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115433158A (en) * | 2022-10-20 | 2022-12-06 | 衢州学院 | Production method of tetrafluoroethane-beta-sultone |
| CN115433158B (en) * | 2022-10-20 | 2023-07-21 | 衢州学院 | Process for producing tetrafluoroethane-beta-sultone |
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