CN117443322A - Device and method for continuously synthesizing tetrafluoroethane-beta-sultone - Google Patents
Device and method for continuously synthesizing tetrafluoroethane-beta-sultone Download PDFInfo
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- CN117443322A CN117443322A CN202311443826.0A CN202311443826A CN117443322A CN 117443322 A CN117443322 A CN 117443322A CN 202311443826 A CN202311443826 A CN 202311443826A CN 117443322 A CN117443322 A CN 117443322A
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- tetrafluoroethylene
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- sulfur trioxide
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- ZMSRCMWBEGLBAI-UHFFFAOYSA-N 3,3,4,4-tetrafluorooxathietane 2,2-dioxide Chemical compound FC1(F)OS(=O)(=O)C1(F)F ZMSRCMWBEGLBAI-UHFFFAOYSA-N 0.000 title claims abstract description 49
- 238000000034 method Methods 0.000 title claims abstract description 47
- 230000002194 synthesizing effect Effects 0.000 title abstract description 14
- AKEJUJNQAAGONA-UHFFFAOYSA-N sulfur trioxide Chemical compound O=S(=O)=O AKEJUJNQAAGONA-UHFFFAOYSA-N 0.000 claims abstract description 92
- BFKJFAAPBSQJPD-UHFFFAOYSA-N tetrafluoroethene Chemical group FC(F)=C(F)F BFKJFAAPBSQJPD-UHFFFAOYSA-N 0.000 claims abstract description 71
- 239000000463 material Substances 0.000 claims abstract description 24
- 239000007788 liquid Substances 0.000 claims abstract description 17
- 238000003786 synthesis reaction Methods 0.000 claims abstract description 11
- 239000000839 emulsion Substances 0.000 claims abstract description 8
- 238000006243 chemical reaction Methods 0.000 claims description 38
- 238000003756 stirring Methods 0.000 claims description 17
- 230000015572 biosynthetic process Effects 0.000 claims description 9
- 238000004821 distillation Methods 0.000 claims description 6
- 239000002994 raw material Substances 0.000 abstract description 8
- 238000007086 side reaction Methods 0.000 abstract description 3
- 230000001276 controlling effect Effects 0.000 description 14
- 239000000047 product Substances 0.000 description 14
- 230000001105 regulatory effect Effects 0.000 description 5
- 238000001308 synthesis method Methods 0.000 description 5
- 238000002156 mixing Methods 0.000 description 4
- 238000000926 separation method Methods 0.000 description 4
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 3
- 229910052731 fluorine Inorganic materials 0.000 description 3
- 239000011737 fluorine Substances 0.000 description 3
- 238000007259 addition reaction Methods 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 238000010924 continuous production Methods 0.000 description 2
- 238000007599 discharging Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000006116 polymerization reaction Methods 0.000 description 2
- QYKIQEUNHZKYBP-UHFFFAOYSA-N Vinyl ether Chemical compound C=COC=C QYKIQEUNHZKYBP-UHFFFAOYSA-N 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- 150000001336 alkenes Chemical class 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000002360 explosive Substances 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 125000000623 heterocyclic group Chemical group 0.000 description 1
- 239000012038 nucleophile Substances 0.000 description 1
- 235000014593 oils and fats Nutrition 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- OBTWBSRJZRCYQV-UHFFFAOYSA-N sulfuryl difluoride Chemical compound FS(F)(=O)=O OBTWBSRJZRCYQV-UHFFFAOYSA-N 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/18—Stationary reactors having moving elements inside
- B01J19/1868—Stationary reactors having moving elements inside resulting in a loop-type movement
- B01J19/1881—Stationary reactors having moving elements inside resulting in a loop-type movement externally, i.e. the mixture leaving the vessel and subsequently re-entering it
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D327/00—Heterocyclic compounds containing rings having oxygen and sulfur atoms as the only ring hetero atoms
- C07D327/02—Heterocyclic compounds containing rings having oxygen and sulfur atoms as the only ring hetero atoms one oxygen atom and one sulfur atom
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention relates to the technical field of organic synthesis, and discloses a device and a method for continuously synthesizing tetrafluoroethane-beta-sultone. The device comprises: the reactor comprises a kettle-type reactor (1) and a micro-interface device (2) arranged in the kettle-type reactor (1), wherein the kettle-type reactor (1) is provided with an outer circulation pipeline (3), a tetrafluoroethylene feeding pipeline (4) and a sulfur trioxide feeding pipeline (5), materials in the kettle-type reactor are circulated back through the outer circulation pipeline and enter the micro-interface device after being mixed with tetrafluoroethylene input through the tetrafluoroethylene feeding pipeline, and gas-liquid emulsion is formed in the kettle-type reactor through the micro-interface device and sulfur trioxide gas input through the sulfur trioxide feeding pipeline. According to the technical scheme of the invention, the kettle type continuous device and the micro-interface device are combined, so that the utilization rate of raw materials and the purity of products are improved, the occurrence of side reactions is inhibited, and the process safety performance is greatly improved.
Description
Technical Field
The invention relates to the technical field of organic synthesis, in particular to a device and a method for continuously synthesizing tetrafluoroethane-beta-sultone.
Background
Tetrafluoroethane-beta-sultone is a colorless transparent strongly acidic liquid with strong pungent odor, which is extremely easy to hydrolyze and volatilize, and has a very strong corrosiveness. Because of its special heterocyclic structure, it can react with various olefins, naphthenes, nucleophiles, etc., to synthesize fluorine-containing compounds of various structures, such as perfluorosulfonyl fluoride vinyl ether (PSVE), fluorine-containing surfactants, fluorine-containing oils and fats, etc.
Currently, tetrafluoroethane- β -sultone is mainly prepared by an addition reaction of sulfur trioxide and tetrafluoroethylene. Sulfur trioxide and tetrafluoroethylene are subjected to addition reaction to prepare tetrafluoroethane-beta-sultone, and the main reaction formula is as follows:
the preparation process of tetrafluoroethane-beta-sultone is an intermittent process, the operation is complex, the process and technical danger that the raw materials adopt explosive and strong corrosive materials and the reaction process releases heat strongly exist, great difficulty and danger exist in the actual operation and the production process, the device is difficult to stably operate, and the production efficiency and the product purity are difficult to be considered.
Patent application CN111072627a discloses a synthesis method of tetrafluoroethane-beta-sultone, sulfur trioxide and tetrafluoroethylene are metered by metering pumps respectively and then continuously enter a micromixer for mixing, and then enter a microreactor for continuous reaction. The tetrafluoroethane-beta-sultone synthesized by the method has higher purity. However, the synthesis method does not solve the problem that tetrafluoroethylene is easy to self-polymerize, so that the reaction efficiency is low. Patent application CN115433158A discloses a process for producing tetrafluoroethane- β -sultone, comprising the steps of: mixing tetrafluoroethane-beta-sultone and sulfur trioxide to obtain a premix; continuously introducing the premix into a tubular reactor set, and simultaneously continuously introducing tetrafluoroethylene into the tubular reactor set; the two react to obtain a reaction product. The method has high reaction pressure, part of tetrafluoroethylene which does not participate in the reaction cannot be separated and recovered later, the tetrafluoroethylene consumption is high, and the reaction efficiency is low.
Aiming at the problems of high raw material consumption, low reaction efficiency, low product purity and the like, a device and a method for continuously synthesizing tetrafluoroethane-beta-sultone are developed.
Disclosure of Invention
The invention aims to solve the problems of low raw material utilization rate, low reaction efficiency, low product purity, local hot spots, self-polymerization of tetrafluoroethylene and the like of the traditional device and method for synthesizing tetrafluoroethane-beta-sultone, and provides a novel device and method for continuously synthesizing tetrafluoroethane-beta-sultone. The invention provides the synthesis device and the synthesis method with high reaction efficiency, high raw material utilization rate and high product purity by combining the kettle type continuous device and the micro-interface device, and the synthesis device and the synthesis method have higher process safety and easier control of the reaction process and the process conditions, thereby realizing continuous production and stable operation of the device.
In order to achieve the above object, the present invention provides an apparatus for continuously synthesizing tetrafluoroethane- β -sultone, comprising: the reactor comprises a kettle-type reactor and a micro-interface device arranged in the kettle-type reactor, wherein the kettle-type reactor is provided with an external circulation pipeline, a tetrafluoroethylene feeding pipeline and a sulfur trioxide feeding pipeline, materials in the kettle-type reactor are circulated back through the external circulation pipeline and enter the micro-interface device after being mixed with tetrafluoroethylene input through the tetrafluoroethylene feeding pipeline, and gas-liquid emulsion is formed in the kettle-type reactor through the micro-interface device and sulfur trioxide gas input through the sulfur trioxide feeding pipeline.
Preferably, the external circulation pipeline is provided with a heat exchange system.
Preferably, a discharge hole is arranged at the bottom of the kettle-type reactor.
In a second aspect the present invention provides a process for the continuous synthesis of tetrafluoroethane- β -sultone, the process being carried out in an apparatus as claimed in any one of claims 1 to 3, the process comprising: and tetrafluoroethylene is input into the kettle-type reactor through a tetrafluoroethylene feed line, sulfur trioxide is input into the kettle-type reactor through a sulfur trioxide feed line, and the reaction is carried out under stirring, wherein the materials in the kettle-type reactor are circulated back through an external circulation pipeline and enter the micro-interface device after being mixed with the tetrafluoroethylene input through the tetrafluoroethylene feed line.
Preferably, the temperature of the circulating material in the external circulation pipeline is controlled within the range of 30-50 ℃ through a heat exchange system.
Preferably, the outer circulation pipeline is provided with a circulation pump, and the volume ratio of the flow rate of the circulation pump to the kettle-type reactor is controlled to be 0.5-10h -1 。
Preferably, the reaction conditions in the tank reactor include: the temperature is 30-50 ℃, the pressure is 0.01-0.2MPa, and the stirring speed is 100-400rpm.
Preferably, the liquid level in the kettle reactor is controlled to be 50-90%.
Preferably, the space velocity of the sulfur trioxide is 0.05 to 0.4h -1 。
Preferably, the product after reaction is discharged from a discharge hole at the bottom of the kettle-type reactor, and the tetrafluoroethane-beta-sultone with the purity of more than 99.7% is obtained after distillation and separation.
According to the device for continuously synthesizing tetrafluoroethane-beta-sultone, the kettle type continuous device and the micro-interface device are combined, so that the operation for controlling the reaction process and the process condition is simpler, and continuous production and stable operation of the device can be realized. By adopting the synthesis method of the device, the mass transfer area of the sulfur trioxide and the tetrafluoroethylene between the kettle reactors is improved, the reaction efficiency between the sulfur trioxide and the tetrafluoroethylene is enhanced within a preset pressure range, and the generation of side reactions is effectively inhibited. Therefore, the reaction can be completed even under mild reaction conditions, and the utilization rate of raw materials and the purity of products are improved; in addition, the problems of local hot spots, tetrafluoroethylene self-aggregation and the like are avoided, and the process safety performance is greatly improved.
Drawings
FIG. 1 is a schematic diagram of a continuous synthesis of tetrafluoroethane- β -sultone.
Description of the reference numerals
1. A tank reactor; 2. a micro interface device; 3. an external circulation pipeline; 4. tetrafluoroethylene feed line; 5. sulfur trioxide feed line.
Detailed Description
The following describes specific embodiments of the present invention in detail. It should be understood that the detailed description and specific examples, while indicating and illustrating the invention, are not intended to limit the invention.
The endpoints and any values of the ranges disclosed herein are not limited to the precise range or value, and are understood to encompass values approaching those ranges or values. For numerical ranges, one or more new numerical ranges may be found between the endpoints of each range, between the endpoint of each range and the individual point value, and between the individual point value, in combination with each other, and are to be considered as specifically disclosed herein.
The device for continuously synthesizing tetrafluoroethane-beta-sultone is shown in fig. 1, and comprises: the reactor comprises a kettle reactor 1 and a micro-interface device 2 arranged in the kettle reactor 1, wherein the kettle reactor 1 is provided with an external circulation pipeline 3, a tetrafluoroethylene feeding pipeline 4 and a sulfur trioxide feeding pipeline 5, and materials in the kettle reactor are circulated back through the external circulation pipeline and enter the micro-interface device after being mixed with tetrafluoroethylene input through the tetrafluoroethylene feeding pipeline, and a gas-liquid emulsion is formed in the kettle reactor through the micro-interface device and sulfur trioxide gas input through the sulfur trioxide feeding pipeline. According to the device provided by the invention, the micro-interface device can convert the kinetic energy of liquid and/or the pressure energy of gas into the surface energy of bubbles and transmit the surface energy of bubbles to tetrafluoroethylene, so that the tetrafluoroethylene is crushed to form micro-bubbles with the diameter of 1 mu m-1mm, and materials and the micro-bubbles are mixed to form a gas-liquid emulsion after crushing, so that the mass transfer area of sulfur trioxide and tetrafluoroethylene in a kettle reactor is greatly increased, the reaction efficiency between the sulfur trioxide and the tetrafluoroethylene is enhanced within a preset pressure range, the generation of side reaction is effectively inhibited, the purity of the product is further improved, the problems of local hot spots, self-polymerization of the tetrafluoroethylene and the like are avoided, and the process safety is greatly improved.
In the apparatus according to the present invention, the external circulation line 3 is preferably provided with a heat exchange system in order to ensure that the temperature of the material in the external circulation line is maintained between 30 and 50 c, thereby improving the reaction efficiency.
In the device according to the invention, the external circulation line 3 is preferably provided with a circulation pump.
In the device according to the invention, the tetrafluoroethylene feed line 4 may be provided with a mass flow meter and a regulating valve.
In the apparatus according to the invention, the sulfur trioxide feed line 5 may be provided with a metering pump and a mass flow meter.
In the apparatus of the present invention, the tank reactor 5 is preferably provided with a stirring device in order to improve the reaction efficiency and the raw material utilization rate.
In the device of the invention, the bottom of the kettle-type reactor can be provided with a discharge port.
In some embodiments, the apparatus for continuously synthesizing tetrafluoroethane- β -sultone comprises: the reactor comprises a kettle-type reactor 1, a micro-interface device 2 and a stirring device, wherein the micro-interface device 2 and the stirring device are arranged in the kettle-type reactor 1, the kettle-type reactor 1 is provided with an outer circulation pipeline 3, a tetrafluoroethylene feeding pipeline 4 and a sulfur trioxide feeding pipeline 5, materials in the kettle-type reactor are circulated back through the outer circulation pipeline and enter the micro-interface device after being mixed with tetrafluoroethylene input through the tetrafluoroethylene feeding pipeline, and a gas-liquid emulsion is formed in the kettle-type reactor through the micro-interface device and sulfur trioxide gas input through the sulfur trioxide feeding pipeline. Wherein, the external circulation pipeline 3 is provided with a circulation pump and a heat exchange system; the tetrafluoroethylene feeding pipeline 4 is provided with a mass flowmeter and a regulating valve; the sulfur trioxide feed line 5 is provided with a metering pump and a mass flow meter.
The present invention also provides a process for the continuous synthesis of tetrafluoroethane- β -sultone, which process is carried out in the apparatus described above, which process comprises: tetrafluoroethylene is input into the kettle-type reactor 1 through a tetrafluoroethylene feeding pipeline 4, sulfur trioxide is input into the kettle-type reactor 1 through a sulfur trioxide feeding pipeline 5, and the reaction is carried out under stirring, wherein the materials in the kettle-type reactor are circulated back through an external circulation pipeline and enter the micro-interface device after being mixed with the tetrafluoroethylene input through the tetrafluoroethylene feeding pipeline. The method is favorable for breaking tetrafluoroethylene to form micro-bubbles with the diameter of 1 mu m-1mm, and the material is mixed with the micro-bubbles to form a gas-liquid emulsion after breaking, so that the gas-liquid emulsion fully reacts with sulfur trioxide, and the reaction efficiency and the raw material utilization rate are improved.
In the process of the present invention, the material in the tank reactor may be tetrafluoroethane- β -sultone.
In the method according to the invention, the temperature of the circulating material in the external circulation line can be controlled in the range of 30-50 ℃, preferably 35-40 ℃, by means of a heat exchange system.
In the method of the invention, the external circulation pipeline can be provided with a circulation pump, and the volume ratio of the flow rate of the circulation pump to the kettle-type reactor 1 can be controlled to be 0.5-10h -1 Preferably 2 to 10 hours -1 。
In the method of the present invention, the reaction conditions in the tank reactor 1 may include: the temperature is 30-50deg.C, preferably 35-40deg.C; the pressure is 0.01-0.2MPa, preferably 0.05-0.15MPa; the stirring speed is 100 to 400rpm, preferably 100 to 300rpm. Herein, pressure refers to gauge pressure.
In the process according to the invention, the liquid level in the tank reactor 1 can be controlled between 50 and 90%, preferably between 50 and 80%.
In the process according to the invention, the space velocity of the sulfur trioxide can be from 0.05 to 0.4h -1 Preferably 0.1-0.4h -1 。
In the method, the reacted product is discharged from a discharge hole at the bottom of the kettle-type reactor 1, and the tetrafluoroethane-beta-sultone with the purity of more than 99.7% is obtained after distillation and separation.
In some embodiments, a method of continuously synthesizing tetrafluoroethane- β -sultone is performed in the apparatus described above, the method comprising: through sulfur trioxide feed line 5 into the tank reactor 1 at a space velocity of 0.05 to 0.4h -1 Sulfur trioxide is input, tetrafluoroethylene is input into the kettle-type reactor 1 through a tetrafluoroethylene feeding pipeline 4, the pressure of the kettle-type reactor is regulated to be 0.01-0.2MPa, the reaction is carried out at the stirring speed of 100-400rpm, the reaction temperature is 30-50 ℃, tetrafluoroethane-beta-sultone in the kettle-type reactor is circulated and returned through an external circulation pipeline, and the ratio of the flow of a circulating pump to the volume of the kettle-type reactor is controlled to be 0.5-10h -1 Controlling the temperature of the materials to be 30-50 ℃, mixing with tetrafluoroethylene input through the tetrafluoroethylene feeding pipeline, and entering the micro-interface device. And after the device runs stably, discharging the reacted product from a discharge port at the bottom of the kettle-type reactor 1, and obtaining tetrafluoroethane-beta-sultone with purity of more than 99.7% after distillation and separation.
In other embodiments, a process for the continuous synthesis of tetrafluoroethane- β -sultone is carried out in the apparatus described above, the process comprising: through the sulfur trioxide feeding line 5 into the kettle reactor 1 at a space velocity of 0.1 to 0.4h -1 Sulfur trioxide is input, tetrafluoroethylene is input into the kettle-type reactor 1 through a tetrafluoroethylene feeding pipeline 4, the pressure of the kettle-type reactor is regulated to be 0.05-0.15MPa, the reaction is carried out at the stirring speed of 100-300rpm, the reaction temperature is 35-40 ℃, tetrafluoroethane-beta-sultone in the kettle-type reactor is circulated and returned through an external circulation pipeline, and the ratio of the flow of a circulation pump to the volume of the kettle-type reactor is controlled to be 2-10h -1 Controlling the temperature of the materials to be 35-40 ℃, mixing with tetrafluoroethylene input through a tetrafluoroethylene feeding pipeline, and entering the micro-interface device. And after the device runs stably, discharging the reacted product from a discharge port at the bottom of the kettle-type reactor 1, and obtaining tetrafluoroethane-beta-sultone with purity of more than 99.7% after distillation and separation.
The apparatus and method for continuously synthesizing tetrafluoroethane-beta-sultone according to the present invention will be further described by way of examples. The embodiment is implemented on the premise of the technical scheme of the invention, and detailed implementation modes and specific operation processes are given, but the protection scope of the invention is not limited to the following embodiment.
The experimental methods in the following examples, unless otherwise specified, are all conventional in the art. The experimental materials used in the examples described below are commercially available unless otherwise specified.
The continuous synthesis of tetrafluoroethane- β -sultone in the following examples was carried out in an apparatus shown in fig. 1, specifically comprising: a kettle-type reactor 1, a micro-interface device 2 and a stirring device, wherein the micro-interface device 2 and the stirring device are arranged in the kettle-type reactor 1, the kettle-type reactor 1 is provided with an outer circulation pipeline 3, a tetrafluoroethylene feeding pipeline 4 and a sulfur trioxide feeding pipeline 5, and the outer circulation pipeline 3 is provided with a circulation pump and a heat exchange system; the tetrafluoroethylene feed line 4 comprises a mass flowmeter and a regulating valve; the sulfur trioxide feed line 5 comprises a metering pump and a mass flow meter.
Example 1
Adding tetrafluoroethane-beta-sultone into a kettle type reactor, starting a circulating pump, and controlling the ratio of the flow of the circulating pump to the volume of the kettle type reactor to be 2h -1 Controlling the pressure of the kettle reactor to be 0.1MPa and the stirring speed to be 200rpm by adjusting the flow of tetrafluoroethylene; the tetrafluoroethane-beta-sultone of the external circulation pipeline is mixed with tetrafluoroethylene input by a tetrafluoroethylene feeding pipeline and then enters the micro-interface device; controlling the space velocity of sulfur trioxide to be 0.1h -1 After the reaction starts, the reaction temperature is controlled to be 35 ℃, the temperature of materials in an external circulation pipeline is controlled to be 40 ℃, and the liquid level of the kettle type reactor is controlled to be 70%. After the device was stably operated and the product continuously obtained from the bottom of the tank reactor was distilled and separated, the purity of tetrafluoroethane-beta-sultone was calculated, and the calculated data are shown in table 1.
Example 2
Adding tetrafluoroethane-beta-sultone into a kettle type reactor, starting a circulating pump, and controlling the ratio of the flow of the circulating pump to the volume of the kettle type reactor to be 5h -1 By adjusting the flow of tetrafluoroethylene, the control is realizedThe pressure of the kettle reactor is 0.05MPa, and the stirring speed is 300rpm; the tetrafluoroethane-beta-sultone of the external circulation pipeline is mixed with tetrafluoroethylene input by a tetrafluoroethylene feeding pipeline and then enters the micro-interface device; controlling the space velocity of sulfur trioxide to be 0.3h -1 After the reaction starts, the reaction temperature is controlled to be 40 ℃, the material temperature in the external circulation pipeline is controlled to be 40 ℃, and the liquid level of the kettle type reactor is controlled to be 80%. After the device was stably operated and the product continuously obtained from the bottom of the tank reactor was distilled and separated, the purity of tetrafluoroethane-beta-sultone was calculated, and the calculated data are shown in table 1.
Example 3
Adding tetrafluoroethane-beta-sultone into a kettle type reactor, starting a circulating pump, and controlling the ratio of the flow of the circulating pump to the volume of the kettle type reactor to be 8h -1 Controlling the pressure of the kettle reactor to be 0.15MPa and the stirring speed to be 300rpm by adjusting the flow of tetrafluoroethylene; the tetrafluoroethane-beta-sultone of the external circulation pipeline is mixed with tetrafluoroethylene input by a tetrafluoroethylene feeding pipeline and then enters the micro-interface device; controlling the space velocity of sulfur trioxide to be 0.1h -1 After the reaction starts, the reaction temperature is controlled to be 40 ℃, the temperature of materials in an external circulation pipeline is controlled to be 35 ℃, and the liquid level of the kettle type reactor is controlled to be 50%. After the device was stably operated and the product continuously obtained from the bottom of the tank reactor was distilled and separated, the purity of tetrafluoroethane-beta-sultone was calculated, and the calculated data are shown in table 1.
Example 4
Adding tetrafluoroethane-beta-sultone into a kettle type reactor, starting a circulating pump, and controlling the ratio of the flow of the circulating pump to the volume of the kettle type reactor to be 10h -1 Controlling the pressure of the kettle reactor to be 0.1MPa and the stirring speed to be 100rpm by adjusting the flow of tetrafluoroethylene; the tetrafluoroethane-beta-sultone of the external circulation pipeline is mixed with tetrafluoroethylene input by a tetrafluoroethylene feeding pipeline and then enters the micro-interface device; controlling the space velocity of sulfur trioxide to be 0.1h -1 After the reaction starts, the reaction temperature is controlled to be 35 ℃, the material temperature in the external circulation pipeline is controlled to be 40 ℃, and the liquid level of the kettle type reactor is controlled to be 80%. After the device runs stably, the catalyst is obtained continuously from the bottom of the kettle type reactorThe purity of tetrafluoroethane-beta-sultone was calculated after the obtained product was separated by distillation, and the calculated data are shown in table 1.
Comparative example 1
In the apparatus used in this comparative example, no micro-interface device was provided in the tank reactor 1, and the other operations were the same as in example 1.
The procedure of example 1 was followed except that tetrafluoroethylene was fed directly into the tank reactor via tetrafluoroethylene feed line and the material in the external circulation line without passing through the micro-interface device.
TABLE 1
As can be seen from the results of Table 1, the apparatus and method for continuously synthesizing tetrafluoroethane-beta-sultone according to the present invention have a purity of not less than 99.7%.
The preferred embodiments of the present invention have been described in detail above, but the present invention is not limited thereto. Within the scope of the technical idea of the invention, a number of simple variants of the technical solution of the invention are possible, including combinations of the individual technical features in any other suitable way, which simple variants and combinations should likewise be regarded as being disclosed by the invention, all falling within the scope of protection of the invention.
Claims (10)
1. An apparatus for continuous synthesis of tetrafluoroethane- β -sultone, comprising: the reactor comprises a kettle-type reactor (1) and a micro-interface device (2) arranged in the kettle-type reactor (1), wherein the kettle-type reactor (1) is provided with an outer circulation pipeline (3), a tetrafluoroethylene feeding pipeline (4) and a sulfur trioxide feeding pipeline (5), materials in the kettle-type reactor are circulated back through the outer circulation pipeline and enter the micro-interface device after being mixed with tetrafluoroethylene input through the tetrafluoroethylene feeding pipeline, and gas-liquid emulsion is formed in the kettle-type reactor through the micro-interface device and sulfur trioxide gas input through the sulfur trioxide feeding pipeline.
2. The device according to claim 1, characterized in that the external circulation line (3) is provided with a heat exchange system.
3. The apparatus according to claim 1 or 2, wherein the bottom of the tank reactor is provided with a discharge port.
4. A process for the continuous synthesis of tetrafluoroethane- β -sultone, characterized in that it is carried out in a device according to any one of claims 1 to 3, comprising: tetrafluoroethylene is input into the kettle-type reactor (1) through a tetrafluoroethylene feeding pipeline (4), sulfur trioxide is input into the kettle-type reactor (1) through a sulfur trioxide feeding pipeline (5), and the reaction is carried out under stirring, wherein materials in the kettle-type reactor are circulated back through an external circulation pipeline and enter the micro-interface device after being mixed with the tetrafluoroethylene input through the tetrafluoroethylene feeding pipeline.
5. The method according to claim 4, wherein the temperature of the circulating material in the external circulation line is controlled in the range of 30-50 ℃ by a heat exchange system.
6. The method according to claim 4 or 5, characterized in that the external circulation pipeline is provided with a circulation pump, and the volume ratio of the flow rate of the circulation pump to the kettle-type reactor (1) is controlled to be 0.5-10h -1 。
7. The method according to any one of claims 4 to 6, characterized in that the reaction conditions in the tank reactor (1) comprise: the temperature is 30-50 ℃, the pressure is 0.01-0.2MPa, and the stirring speed is 100-400rpm.
8. A method according to any of claims 4-6, characterized in that the liquid level in the tank reactor (1) is controlled to 50-90%.
9. The process according to any one of claims 4 to 8, wherein the space velocity of sulfur trioxide is from 0.05 to 0.4h -1 。
10. The method according to any one of claims 4 to 9, wherein the reacted product is discharged from a discharge port at the bottom of the tank reactor (1) and is separated by distillation to obtain tetrafluoroethane- β -sultone having a purity of 99.7% or more.
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| CN202311443826.0A CN117443322A (en) | 2023-10-31 | 2023-10-31 | Device and method for continuously synthesizing tetrafluoroethane-beta-sultone |
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| CN202311443826.0A CN117443322A (en) | 2023-10-31 | 2023-10-31 | Device and method for continuously synthesizing tetrafluoroethane-beta-sultone |
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