CN115724710A - Octafluoropropane production method and production line applying same - Google Patents
Octafluoropropane production method and production line applying same Download PDFInfo
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Abstract
The invention discloses an octafluoropropane production method and a production line applying the same, wherein the method comprises the following steps: electrolyzing to obtain fluorine gas: adding a certain amount of hydrogen fluoride liquid into an electrolytic cell, and electrolyzing the hydrogen fluoride liquid to obtain fluorine gas containing impurities; fluorine gas purification: carrying out pressurization, multistage condensation purification and multistage adsorption treatment on the fluorine gas containing impurities to obtain purified fluorine gas; preparing octafluoropropane: adding nitrogen, purified fluorine gas, hexafluoropropylene and a fluorinated liquid into a fluorocarbon reactor, and reacting the purified fluorine gas with the hexafluoropropylene to obtain mixed process gas containing octafluoropropane so as to obtain crude mixed process gas containing octafluoropropane; purifying octafluoropropane: carrying out multi-stage adsorption treatment, pressurization and condensation treatment on the crude mixed process gas containing the octafluoropropane to obtain purified octafluoropropane; the invention aims to provide an octafluoropropane production method and a production line using the same, which are safe in production process and high in production efficiency by reacting fluorine gas and hexafluoropropylene to prepare octafluoropropane.
Description
Technical Field
The invention relates to the technical field of octafluoropropane preparation, in particular to an octafluoropropane production method and a production line applying the same.
Background
Octafluoropropane, an organic compound, is a product of propane in which eight hydrogen atoms are replaced with fluorine atoms, and is a colorless gas which is hardly soluble in water. In the microelectronics industry, the method is used for plasma etching and device surface cleaning, and is also used for low-temperature refrigeration, medical gas and gas insulation and the like.
The existing synthesis methods of octafluoropropane mainly comprise the following two methods: one is prepared by the catalytic addition of hexafluoropropane, and a catalyst is required to be added to prepare octafluoropropane; the other is prepared by extracting and separating a hexafluoropropylene byproduct. The two methods have complicated processes, the reaction degree of octafluoropropane prepared by adding the catalyst is difficult to control, certain potential safety hazards exist, and the hexafluoropropylene byproduct is adopted for extraction and separation, so that the extraction process is complicated, multiple times of extraction and separation are needed, and the yield is relatively small.
Disclosure of Invention
The invention aims to provide an octafluoropropane production method and a production line applying the same, which are safe in production process and high in production efficiency by reacting fluorine gas and hexafluoropropylene to prepare octafluoropropane.
In order to achieve the purpose, the invention adopts the following technical scheme: an octafluoropropane production method comprising the steps of:
electrolyzing to obtain fluorine gas: adding a certain amount of hydrogen fluoride liquid into an electrolytic cell, and electrolyzing the hydrogen fluoride liquid to obtain impurity-containing fluorine gas;
fluorine gas purification: carrying out pressurization, multistage condensation purification and multistage adsorption treatment on the fluorine gas containing impurities to obtain purified fluorine gas;
preparing octafluoropropane: adding nitrogen, purified fluorine gas, hexafluoropropylene and a fluorinated liquid into a fluorocarbon reactor, and reacting the purified fluorine gas and the hexafluoropropylene to obtain mixed process gas containing octafluoropropane so as to obtain crude mixed process gas containing octafluoropropane;
octafluoropropane purification: and carrying out multistage adsorption treatment, pressurization and condensation treatment on the crude mixed process gas containing the octafluoropropane to obtain the purified octafluoropropane.
Preferably, in the multi-stage condensation purification process, the fluorine gas containing impurities is sequentially introduced into the environment with the condensation environment temperature of-20 ℃ to-10 ℃ and the condensation environment temperature of-70 ℃ to-20 ℃ for condensation.
Preferably, the nitrogen gas and the purified fluorine gas are mixed in a ratio of 4 to 5; a fluorine gas and a hexafluoropropylene gas in a ratio of 19:150-600 to prepare the mixed process gas.
Preferably, in the step of preparing octafluoropropane, the temperature of the fluorocarbon reactor is-15 to 50 ℃, and the working pressure of the fluorocarbon reactor is 0 to 0.6MPa.
Preferably, when the nitrogen, the purified fluorine and the hexafluoropropylene are added into the fluorocarbon reactor, a fluorocarbon solvent tank is added, the solvent in the fluorocarbon solvent tank is circulated between the fluorocarbon reactor and the fluorocarbon solvent tank, and the solvent is used for reducing the temperature of the fluorine and the hexafluoropropylene and reducing the side reaction and the generation of side products.
An octafluoropropane production line comprises an electrolytic cell, a pressurizing unit, a condensing and purifying unit, an adsorption treatment unit, a fluorocarbon reaction unit, a fluorocarbon adsorption unit and a storage unit;
the electrolytic cell is connected with the pressurizing unit and is used for electrolyzing hydrogen fluoride to prepare fluorine gas;
the pressurization unit is connected with the condensation purification unit and is used for pressurizing fluorine gas;
the condensation purification unit is connected with the adsorption treatment unit and is used for condensing hydrogen fluoride impurities in the fluorine gas and improving the purity of the fluorine gas;
the adsorption treatment unit is connected with the fluorocarbon reaction unit and is used for adsorbing hydrogen fluoride in the fluorine gas and improving the purity of the fluorine gas;
the fluorocarbon reaction unit is connected with the fluorocarbon adsorption unit and is used for providing reaction sites for fluorine gas and hexafluoropropylene to prepare octafluoropropane;
the fluorocarbon adsorption unit is connected with the storage unit and used for adsorbing excessive gas in the octafluoropropane and improving the purity of the octafluoropropane.
Preferably, the condensation purification unit comprises a first air inlet pipeline, a first-stage condensation purifier, a connecting pipeline, a return pipeline, a second-stage condensation purifier, a fluorine gas outlet pipeline, a collection pipeline and a hydrogen fluoride collection tank; the first gas inlet pipeline is connected with the pressurization unit, the first gas inlet pipeline is connected with the lower input end of the primary condensation purifier, one end of the connecting pipeline is connected with the upper output end of the primary condensation purifier, the other end of the connecting pipeline is connected with the lower input end of the secondary condensation purifier, and the fluorine gas outlet pipeline is connected with the adsorption treatment unit; the lower output end of the secondary condensation purifier is connected with one end of the return pipeline, the other end of the return pipeline is connected with the upper input end of the primary condensation purifier, and the lower output end of the primary condensation purifier is connected with the hydrogen fluoride collecting tank through the collecting pipeline; the condensation temperature of the second-stage condensation purifier is lower than that of the first-stage condensation purifier.
Preferably, the fluorocarbon reaction unit comprises a second air inlet pipeline, a nitrogen inlet pipeline, a first input pipeline, a hexafluoropropylene inlet pipeline, a second input pipeline, a fluorocarbon reactor, a solvent return pipeline, a fluorocarbon solvent tank, a solvent circulation pipeline, a circulation pump and an output pipeline;
the second air inlet pipeline and the nitrogen inlet pipeline are both communicated with the first input pipeline, the first input pipeline is communicated with one end of an internal pipeline of the fluorocarbon reactor, the other end of the internal pipeline of the fluorocarbon reactor is communicated with one end of the solvent return pipeline, the other end of the solvent return pipeline is communicated with the fluorocarbon solvent tank, and the output pipeline is communicated with the upper end of the fluorocarbon solvent tank;
one end of the solvent circulation pipeline is communicated with the fluorocarbon solvent tank, the other end of the solvent circulation pipeline is communicated with the second input pipeline, the circulating pump is arranged on the solvent circulation pipeline, the hexafluoropropylene air inlet pipeline is communicated with the second input pipeline, and the second input pipeline is communicated with one end of the inner pipeline of the fluorocarbon reactor.
Preferably, the fluorocarbon adsorption unit comprises an adsorber, a buffer tank, a booster pump, a liquid nitrogen tank, a condensation collector and a discharge pipeline;
the input end of the adsorber is connected with the output end of the previous process equipment, the output end of the adsorber is connected with the input end of the buffer tank, the output end of the buffer tank is connected with the input end of the booster pump, the output end of the booster pump is connected with the lower end of the condensation collector, and the upper end of the condensation collector is connected with the discharge pipeline; the condensation collector is connected with the storage unit; the condensation collector further comprises a condensation input end and a condensation return end, the liquid nitrogen tank is connected with the condensation input end of the condensation collector, and the condensation return end of the condensation collector is connected with an external buffer tank.
The technical scheme of the invention has the beneficial effects that: firstly, fluorine gas is purified, and OF2, HF and other harmful impurities in the fluorine gas are removed, so that side reactions are avoided. Since hydrogen fluoride is easy to volatilize in the electrolysis process, in order to reduce the content of HF and the corrosion pressure of subsequent equipment, multi-stage condensation purification treatment is needed, and the condensation temperature of fluorine gas and the condensation temperature of hydrogen fluoride are different, so that the hydrogen fluoride is condensed but the fluorine gas is not condensed, the hydrogen fluoride mixed in the fluorine gas is removed, and the purity of the fluorine gas is improved.
Fluorine gas and nitrogen gas are mixed, hexafluoropropylene and a fluorinating agent are mixed, conversion is carried out at low temperature and low pressure, the conversion rate is high, a few byproducts are generated, the fluorinating agent is recycled, the boiling point difference between the byproducts and octafluoropropane is large, the byproducts and the octafluoropropane can be completely separated, a high-purity product is easily obtained, and the reaction process is safe and controllable.
By utilizing the strong oxidizing property of the fluorine gas, hexafluoropropylene and the fluorine gas are added into the fluorocarbon reactor for mixing reaction to prepare octafluoropropane, the production process is safe, and the production efficiency is high; the fluorine gas and the nitrogen gas are mixed, so that the reaction degree of hexafluoropropylene and the fluorine gas is reduced, the severe reaction of the hexafluoropropylene and the fluorine gas is avoided, the purpose of safety and controllability is realized, the safety problem is avoided, no catalyst is required to be added in the reaction, and the production cost is reduced.
Drawings
FIG. 1 is a schematic block diagram of one embodiment of the present invention;
FIG. 2 is a schematic diagram of a condensing and purifying unit according to an embodiment of the present invention;
FIG. 3 is a schematic structural diagram of a fluorocarbon reaction unit according to an embodiment of the present invention;
fig. 4 is a schematic structural diagram of a fluorocarbon adsorption unit according to an embodiment of the present invention.
Wherein: an electrolytic cell 1 and a pressurizing unit 2;
the condensation purification unit 3, a first air inlet pipeline 31, a first-stage condensation purifier 32, a connecting pipeline 33, a return pipeline 34, a second-stage condensation purifier 35, a fluorine gas outlet pipeline 36, a collecting pipeline 37 and a hydrogen fluoride collecting tank 38;
the system comprises an adsorption treatment unit 4, a fluorocarbon reaction unit 5, a second air inlet pipeline 51, a nitrogen inlet pipeline 52, a first input pipeline 53, a hexafluoropropylene inlet pipeline 54, a second input pipeline 55, a fluorocarbon reactor 56, a solvent return pipeline 57, a fluorocarbon solvent tank 58, a solvent circulation pipeline 59, a circulation pump 510 and an output pipeline 511;
the system comprises a fluorocarbon adsorption unit 6, an adsorber 61, a buffer tank 62, a booster pump 63, a liquid nitrogen tank 64, a condensation collector 65 and a discharge pipeline 66; and a storage unit 7.
Detailed Description
The technical scheme of the invention is further explained by the specific implementation mode in combination with the attached drawings.
Reference will now be made in detail to embodiments of the present invention, examples of which are illustrated in the accompanying drawings, wherein like reference numerals refer to the same or similar elements or elements having the same or similar functions throughout. The embodiments described below with reference to the accompanying drawings are illustrative only for the purpose of explaining the present invention, and are not to be construed as limiting the present invention.
In the description of the present invention, it is to be understood that the terms "longitudinal", "lateral", "up", "down", "front", "back", "left", "right", "vertical", "horizontal", "top", "bottom", "inner", "outer", and the like, indicate orientations or positional relationships based on those shown in the drawings, and are used merely for convenience of description and for simplicity of description, and do not indicate or imply that the referenced devices or elements must have a particular orientation, be constructed in a particular orientation, and be operated, and thus, are not to be construed as limiting the present invention. Furthermore, features defined as "first" and "second" may explicitly or implicitly include one or more of the features for distinguishing between descriptive features, non-sequential, non-trivial and non-trivial.
In the description of the present invention, "a plurality" means two or more unless otherwise specified.
In the description of the present invention, it should be noted that, unless otherwise explicitly specified or limited, the terms "mounted," "connected," and "connected" are to be construed broadly and may be, for example, fixedly connected, detachably connected, or integrally connected; can be mechanically or electrically connected; they may be connected directly or indirectly through intervening media, or they may be interconnected between two elements. The specific meanings of the above terms in the present invention can be understood in specific cases to those skilled in the art.
Referring to fig. 1 to 4, a method for producing octafluoropropane includes the steps of:
electrolyzing to obtain fluorine gas: adding a certain amount of hydrogen fluoride liquid into an electrolytic cell, and electrolyzing the hydrogen fluoride liquid to obtain impurity-containing fluorine gas;
fluorine gas purification: carrying out pressurization, multistage condensation purification and multistage adsorption treatment on the fluorine gas containing impurities to obtain purified fluorine gas;
preparing octafluoropropane: adding nitrogen, purified fluorine gas, hexafluoropropylene and a fluorinated liquid into a fluorocarbon reactor, and reacting the purified fluorine gas with the hexafluoropropylene to obtain mixed process gas containing octafluoropropane so as to obtain crude mixed process gas containing octafluoropropane;
purifying octafluoropropane: and carrying out multistage adsorption treatment, pressurization and condensation treatment on the crude mixed process gas containing the octafluoropropane to obtain the purified octafluoropropane.
Octafluoropropane, an organic compound, is a product of propane in which eight hydrogen atoms are replaced with fluorine atoms, and is a colorless gas which is hardly soluble in water. In the microelectronics industry, the method is used for plasma etching and device surface cleaning, and is also used for low-temperature refrigeration, medical gas and gas insulation and the like.
The existing synthesis methods of octafluoropropane mainly comprise the following two methods: one is prepared by the catalytic addition of hexafluoropropane, and a catalyst is required to be added to prepare octafluoropropane; the other is prepared by extracting and separating a hexafluoropropylene byproduct. The two methods have complicated processes, the reaction degree of octafluoropropane prepared by adding the catalyst is difficult to control, certain potential safety hazards exist, and the hexafluoropropylene byproduct is adopted for extraction and separation, so that the extraction process is complicated, multiple times of extraction and separation are needed, and the yield is relatively small.
Firstly, the fluorine gas is purified to remove the harmful impurities OF OF2, HF and the like contained in the fluorine gas, thereby avoiding side reaction. Since hydrogen fluoride is easy to volatilize in the electrolysis process, in order to reduce the content of HF and the corrosion pressure of subsequent equipment, multi-stage condensation purification treatment is needed, and the condensation temperature of fluorine gas and hydrogen fluoride is different, so that the hydrogen fluoride is condensed, the fluorine gas is not condensed, the mixed hydrogen fluoride in the fluorine gas is removed, and the purity of the fluorine gas is improved.
Fluorine gas and nitrogen are mixed, hexafluoropropylene and a fluorinating agent are mixed, conversion is carried out at low temperature and low pressure, the conversion rate is high, a few by-products are generated, the fluorinating agent is recycled, the difference between the boiling points of the by-products and octafluoropropane is large, the by-products and the octafluoropropane can be completely separated, high-purity products can be easily obtained, and the reaction process is safe and controllable.
By utilizing the strong oxidizing property of the fluorine gas, hexafluoropropylene and the fluorine gas are added into the fluorocarbon reactor for mixing reaction to prepare octafluoropropane, the production process is safe, and the production efficiency is high; fluorine gas and nitrogen gas are mixed, so that the reaction degree of hexafluoropropylene and fluorine gas is reduced, severe reaction of hexafluoropropylene and fluorine gas is avoided, the purpose of safety and controllability is realized, and safety problems are avoided.
Specifically, in the multi-stage condensation purification process, the fluorine gas containing impurities is sequentially introduced into the environment with the condensation environment temperature of minus 20 ℃ to minus 10 ℃ and the condensation environment temperature of minus 70 ℃ to minus 20 ℃ for condensation.
According to the invention, by utilizing the difference of the boiling points between hydrogen fluoride and fluorine gas, fluorine gas containing hydrogen fluoride generated by electrolysis sequentially passes through low-temperature and lower-temperature condensation environments to condense and liquefy hydrogen fluoride and is separated from the fluorine gas, low-temperature refrigeration can be realized through a refrigerating unit, lower-temperature refrigeration is realized through a liquid nitrogen refrigeration mode, the condensation temperature is gradually reduced, and the condensation effect of the hydrogen fluoride is ensured.
In the present application, the nitrogen gas and the purified fluorine gas are mixed at a ratio of 4 to 5 to obtain a diluted fluorine gas; a fluorine gas and a hexafluoropropylene gas in a ratio of 19: mixing at a ratio of 150-600 to prepare mixed process gas.
The nitrogen does not participate in the reaction between the fluorine and the hexafluoropropylene, the concentration of the fluorine is reduced by mixing the nitrogen and the fluorine, the reaction intensity between the fluorine and the hexafluoropropylene is reduced, the purpose of controlling the reaction speed is realized, the fluorine and the hexafluoropropylene are fully mixed and reacted, the hexafluoropropylene can completely participate in the reaction, and the subsequent generated octafluoropropane does not contain heteropentafluoropropene and only needs to filter the fluorine and the nitrogen, so that the octafluoropropane with high purity can be obtained.
Specifically, in the step of preparing octafluoropropane, the temperature of the fluorocarbon reactor is-15-50 ℃, and the working pressure of the fluorocarbon reactor is 0-0.6MPa.
As the reaction between the fluorine gas and the hexafluoropropylene is an exothermic process, the reaction between the fluorine gas and the hexafluoropropylene is more and more violent along with the rise of the temperature, in order to avoid accidents caused by overhigh temperature, the temperature of the fluorocarbon reactor is adjusted, the fluorocarbon reactor is kept in a low-temperature state, the fluorocarbon reactor absorbs the generated heat, the fluorine gas and the hexafluoropropylene are kept at a stable reaction speed, and the purpose of safety and controllability is realized.
Preferably, when the nitrogen, the purified fluorine gas and the hexafluoropropylene are added into the fluorocarbon reactor, a fluorocarbon solvent tank is added, the solvent in the fluorocarbon solvent tank forms a circulation between the fluorocarbon reactor and the fluorocarbon solvent tank, and the solvent is used for reducing the temperature of the fluorine gas and the hexafluoropropylene and reducing side reactions and the generation of byproducts.
The solvent does not react with the fluorine gas or the hexafluoropropylene, and the hexafluoropropylene and the fluorine gas can flow between the fluorocarbon reactor and the fluorocarbon solvent tank more easily under the drive of the solvent, so that the hexafluoropropylene and the fluorine gas can be fully contacted and can completely react. Meanwhile, the solvent can reduce the temperature of the fluorine gas and the hexafluoropropylene, and the temperature of the solvent is reduced by cooling the solvent, so that the heat generated by the reaction of the fluorine gas and the hexafluoropropylene can be absorbed, and the generation of side reactions and byproducts can be reduced.
An octafluoropropane production line comprises an electrolytic cell, a pressurizing unit, a condensing and purifying unit, an adsorption treatment unit, a fluorocarbon reaction unit, a fluorocarbon adsorption unit and a storage unit;
the electrolytic cell is connected with the pressurizing unit and is used for electrolyzing hydrogen fluoride to prepare fluorine gas;
the pressurization unit is connected with the condensation purification unit and is used for pressurizing fluorine gas;
the condensation purification unit is connected with the adsorption treatment unit and is used for condensing hydrogen fluoride impurities in the fluorine gas and improving the purity of the fluorine gas;
the adsorption treatment unit is connected with the fluorocarbon reaction unit and is used for adsorbing hydrogen fluoride in the fluorine gas and improving the purity of the fluorine gas;
the fluorocarbon reaction unit is connected with the fluorocarbon adsorption unit and is used for providing reaction sites for fluorine gas and hexafluoropropylene to prepare octafluoropropane;
the fluorocarbon adsorption unit is connected with the storage unit and used for adsorbing excessive gas in the octafluoropropane and improving the purity of the octafluoropropane.
The electrolytic cell is used for electrolyzing hydrogen fluoride to prepare fluorine gas, and simultaneously, the electrolyzed product hydrogen can be discharged after adsorption treatment. The gas generated by electrolysis is pressurized and treated at low temperature by utilizing the difference of the condensation temperature of the hydrogen fluoride and the fluorine gas, so that the hydrogen fluoride in the fluorine gas can be liquefied, and the aim of filtering the hydrogen fluoride is fulfilled. After condensation treatment, a small amount of doped hydrogen fluoride is physically adsorbed by the adsorption treatment unit, and the concentration of the hydrogen fluoride is reduced to the minimum and can be ignored. The octafluoropropane is prepared by mixing hexafluoropropylene and fluorine gas, the production process is safe, the production efficiency is high, the fluorine gas and nitrogen gas are mixed, the reaction speed of hexafluoropropylene and fluorine gas is reduced, and the problem of safety caused by violent reaction of hexafluoropropylene and fluorine gas is avoided.
Specifically, the condensation purification unit comprises a first air inlet pipeline, a primary condensation purifier, a connecting pipeline, a return pipeline, a secondary condensation purifier, a fluorine gas outlet pipeline, a collection pipeline and a hydrogen fluoride collection tank; the first gas inlet pipeline is connected with the pressurization unit, the first gas inlet pipeline is connected with the lower input end of the primary condensation purifier, one end of the connecting pipeline is connected with the upper output end of the primary condensation purifier, the other end of the connecting pipeline is connected with the lower input end of the secondary condensation purifier, and the fluorine gas outlet pipeline is connected with the adsorption treatment unit; the lower output end of the secondary condensation purifier is connected with one end of the return pipeline, the other end of the return pipeline is connected with the upper input end of the primary condensation purifier, and the lower output end of the primary condensation purifier is connected with the hydrogen fluoride collecting tank through the collecting pipeline; the condensation temperature of the second-stage condensation purifier is lower than that of the first-stage condensation purifier.
The invention utilizes the difference of the boiling points between the hydrogen fluoride and the fluorine gas, and the condensation treatment of the primary condensation purifier and the secondary condensation purifier is adopted, so that the hydrogen fluoride is condensed and liquefied in the condensation process, and the fluorine gas is basically not liquefied, thereby realizing the purpose of filtering the hydrogen fluoride. Liquefied hydrogen fluoride flows into the primary condensation purifier from the secondary condensation purifier through the return line, finally enters the hydrogen fluoride collection tank through the collection line, and fluorine gas enters the adsorption treatment unit through the connecting line and the fluorine gas outlet line to be subjected to adsorption treatment, so that a small amount of residual hydrogen fluoride is physically adsorbed. Because the condensation temperature of the secondary condensation purifier is lower than that of the primary condensation purifier, the condensation effect of the secondary condensation purifier on the hydrogen fluoride is better than that of the primary condensation purifier, the further condensation effect is achieved, the hydrogen fluoride mixed in the fluorine gas is removed, and the content of the hydrogen fluoride can be reduced to be within three percent.
Preferably, the fluorocarbon reaction unit comprises a second air inlet pipeline, a nitrogen inlet pipeline, a first input pipeline, a hexafluoropropylene inlet pipeline, a second input pipeline, a fluorocarbon reactor, a solvent return pipeline, a fluorocarbon solvent tank, a solvent circulation pipeline, a circulation pump and an output pipeline;
the second air inlet pipeline and the nitrogen inlet pipeline are both communicated with the first input pipeline, the first input pipeline is communicated with one end of an internal pipeline of the fluorocarbon reactor, the other end of the internal pipeline of the fluorocarbon reactor is communicated with one end of the solvent return pipeline, the other end of the solvent return pipeline is communicated with the fluorocarbon solvent tank, and the output pipeline is communicated with the upper end of the fluorocarbon solvent tank;
one end of the solvent circulation pipeline is communicated with the fluorocarbon solvent tank, the other end of the solvent circulation pipeline is communicated with the second input pipeline, the circulating pump is arranged on the solvent circulation pipeline, the hexafluoropropylene air inlet pipeline is communicated with the second input pipeline, and the second input pipeline is communicated with one end of the inner pipeline of the fluorocarbon reactor.
The method utilizes the strong oxidizing property of the fluorine gas to prepare the octafluoropropane by mixing the hexafluoropropylene and the fluorine gas, has safe production process and high production efficiency, mixes the fluorine gas and the nitrogen gas, reduces the reaction degree of the hexafluoropropylene and the fluorine gas, avoids the severe reaction of the hexafluoropropylene and the fluorine gas to generate safety problems, provides a solvent for pushing the gas to flow by the fluorocarbon solvent tank, does not react with the fluorine gas or the hexafluoropropylene, and ensures that the hexafluoropropylene and the fluorine gas can fully contact and completely react with each other under the driving of the solvent.
Preferably, the fluorocarbon adsorption unit comprises an adsorber, a buffer tank, a booster pump, a liquid nitrogen tank, a condensation collector and a discharge pipeline;
the input end of the adsorber is connected with the output end of the previous process equipment, the output end of the adsorber is connected with the input end of the buffer tank, the output end of the buffer tank is connected with the input end of the booster pump, the output end of the booster pump is connected with the lower end of the condensation collector, and the upper end of the condensation collector is connected with the discharge pipeline; the condensation collector is connected with the storage unit; the condensation collector further comprises a condensation input end and a condensation reflux end, the liquid nitrogen tank is connected with the condensation input end of the condensation collector, and the condensation reflux end of the condensation collector is connected with an external buffer tank.
The fluorine gas in the octafluoropropane is adsorbed and removed through the adsorber, the remaining octafluoropropane contains the nitrogen gas, the characteristic that the octafluoropropane is easy to liquefy and the nitrogen gas is difficult to liquefy is utilized, the gas subjected to adsorption treatment is added into the condensation collector, the liquid nitrogen tank provides the condensation temperature for the condensation collector, the octafluoropropane is liquefied and collected, and the nitrogen gas serving as harmless gas can be directly discharged through the discharge pipeline.
In the description herein, references to the description of "an embodiment," "an example" or the like are intended to mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. In this specification, the schematic representations of the terms used above do not necessarily refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.
The technical principle of the present invention is described above in connection with specific embodiments. The description is made for the purpose of illustrating the principles of the invention and should not be taken in any way as limiting the scope of the invention. Based on the explanations herein, those skilled in the art will be able to conceive of other embodiments of the present invention without inventive step, and these embodiments will fall within the scope of the present invention.
Claims (9)
1. A production method of octafluoropropane is characterized by comprising the following steps:
electrolyzing to obtain fluorine gas: adding a certain amount of hydrogen fluoride liquid into an electrolytic cell, and electrolyzing the hydrogen fluoride liquid to obtain fluorine gas containing impurities;
fluorine gas purification: carrying out pressurization, multistage condensation purification and multistage adsorption treatment on the fluorine gas containing impurities to obtain purified fluorine gas;
preparing octafluoropropane: adding nitrogen, purified fluorine gas, hexafluoropropylene and a fluorinated liquid into a fluorocarbon reactor, and reacting the purified fluorine gas with the hexafluoropropylene to obtain mixed process gas containing octafluoropropane so as to obtain crude mixed process gas containing octafluoropropane;
purifying octafluoropropane: and carrying out multistage adsorption treatment, pressurization and condensation treatment on the crude mixed process gas containing the octafluoropropane to obtain the purified octafluoropropane.
2. The process according to claim 1, wherein in the multistage condensation purification process, the impurity-containing fluorine gas is condensed by being sequentially introduced into an environment having a condensing environment temperature of-20 ℃ to-10 ℃ and a condensing environment temperature of-70 ℃ to-20 ℃.
3. An octafluoropropane production method according to claim 2, wherein said nitrogen gas and said purified fluorine gas are mixed at a ratio of 4 to 5; a fluorine gas and a hexafluoropropylene gas in a ratio of 19: mixing at a ratio of 150-600 to prepare mixed process gas.
4. The octafluoropropane production method according to claim 3, wherein in said step of producing octafluoropropane, the temperature of the fluorocarbon reactor is-15 to 50 ℃ and the operating pressure of the fluorocarbon reactor is 0 to 0.6MPa.
5. The process of claim 1, wherein a fluorocarbon solvent tank is added to the reactor for introducing nitrogen, purified fluorine and hexafluoropropene to the reactor, and a solvent is circulated between the reactor and the tank for reducing the temperature of fluorine and hexafluoropropene to reduce side reactions and by-products.
6. An octafluoropropane production line using the octafluoropropane production method according to any one of claims 1 to 5, characterized by comprising an electrolytic cell, a pressurizing unit, a condensing and purifying unit, an adsorption treatment unit, a fluorocarbon reaction unit, a fluorocarbon adsorption unit and a storage unit;
the electrolytic cell is connected with the pressurizing unit and is used for electrolyzing hydrogen fluoride to prepare fluorine gas;
the pressurization unit is connected with the condensation purification unit and is used for pressurizing fluorine gas;
the condensation purification unit is connected with the adsorption treatment unit and is used for condensing hydrogen fluoride impurities in the fluorine gas and improving the purity of the fluorine gas;
the adsorption treatment unit is connected with the fluorocarbon reaction unit and is used for adsorbing hydrogen fluoride in the fluorine gas and improving the purity of the fluorine gas;
the fluorocarbon reaction unit is connected with the fluorocarbon adsorption unit and is used for providing reaction sites for fluorine gas and hexafluoropropylene to prepare octafluoropropane;
the fluorocarbon adsorption unit is connected with the storage unit and used for adsorbing excessive gas in the octafluoropropane and improving the purity of the octafluoropropane.
7. The octafluoropropane production line according to claim 6, wherein said condensation purification unit comprises a first gas inlet line, a primary condensation purifier, a connecting line, a return line, a secondary condensation purifier, a fluorine gas outlet line, a collecting line and a hydrogen fluoride collecting tank; the first gas inlet pipeline is connected with the pressurization unit, the first gas inlet pipeline is connected with the lower input end of the primary condensation purifier, one end of the connecting pipeline is connected with the upper output end of the primary condensation purifier, the other end of the connecting pipeline is connected with the lower input end of the secondary condensation purifier, and the fluorine gas outlet pipeline is connected with the adsorption treatment unit; the lower output end of the secondary condensation purifier is connected with one end of the return pipeline, the other end of the return pipeline is connected with the upper input end of the primary condensation purifier, and the lower output end of the primary condensation purifier is connected with the hydrogen fluoride collecting tank through the collecting pipeline; the condensation temperature of the second-stage condensation purifier is lower than that of the first-stage condensation purifier.
8. The octafluoropropane production line according to claim 6, wherein the fluorocarbon reaction unit comprises a second air inlet pipeline, a nitrogen inlet pipeline, a first input pipeline, a hexafluoropropylene inlet pipeline, a second input pipeline, a fluorocarbon reactor, a solvent return pipeline, a fluorocarbon solvent tank, a solvent circulation pipeline, a circulation pump and an output pipeline;
the second air inlet pipeline and the nitrogen inlet pipeline are both communicated with the first input pipeline, the first input pipeline is communicated with one end of an internal pipeline of the fluorocarbon reactor, the other end of the internal pipeline of the fluorocarbon reactor is communicated with one end of the solvent return pipeline, the other end of the solvent return pipeline is communicated with the fluorocarbon solvent tank, and the output pipeline is communicated with the upper end of the fluorocarbon solvent tank;
one end of the solvent circulation pipeline is communicated with the fluorocarbon solvent tank, the other end of the solvent circulation pipeline is communicated with the second input pipeline, the circulating pump is arranged on the solvent circulation pipeline, the hexafluoropropylene air inlet pipeline is communicated with the second input pipeline, and the second input pipeline is communicated with one end of the inner pipeline of the fluorocarbon reactor.
9. The octafluoropropane production line according to claim 6, wherein the fluorocarbon adsorption unit comprises an adsorber, a buffer tank, a booster pump, a liquid nitrogen tank, a condensation collector and a discharge pipeline;
the input end of the adsorber is connected with the output end of the previous process equipment, the output end of the adsorber is connected with the input end of the buffer tank, the output end of the buffer tank is connected with the input end of the booster pump, the output end of the booster pump is connected with the lower end of the condensation collector, and the upper end of the condensation collector is connected with the discharge pipeline; the condensation collector is connected with the storage unit; the condensation collector further comprises a condensation input end and a condensation return end, the liquid nitrogen tank is connected with the condensation input end of the condensation collector, and the condensation return end of the condensation collector is connected with an external buffer tank.
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