Continuous production system for synthesis of 1-chloro-1, 1, 4, 4, 4-pentafluoro-2-butene and E-1, 1, 1, 4, 4, 4-hexafluoro-2-butene
By employing hypergravity process enhancement technology and azeotropic separation, combined with single-trans synthesis and double-trans synthesis systems, the problems of low yield and severe pollution of 1-chloro-1,1,4,4,4-pentafluoro-2-butene and E-1,1,1,4,4,4-hexafluoro-2-butene in existing technologies have been solved, achieving efficient and environmentally friendly continuous production.
Patent Information
- Application Number
- CN202510851637.X
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-06-24
- Publication Date
- 2025-11-11
AI Technical Summary
Existing methods for preparing 1-chloro-1,1,4,4,4-pentafluoro-2-butene and E-1,1,1,4,4,4-hexafluoro-2-butene suffer from problems such as low yield, poor selectivity, strong catalyst corrosivity, and serious pollution from waste.
By employing the concepts of supergravity process enhancement technology, azeotropic separation, and reaction separation unit coupling, HF is separated using azeotropic characteristics through the connection of a primary reaction synthesis system and a secondary reaction synthesis system. Combined with a high-efficiency catalyst and a precision heat exchange system, continuous production is achieved.
It improves reaction conversion rate and selectivity, reduces resource waste and energy consumption, and lowers wastewater, waste gas and solid waste emissions, meeting the requirements of green chemistry processes.
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Figure CN120919929A_ABST
Abstract
Description
Technical Field
[0001] This invention relates to the field of chemical process technology, and in particular to a continuous production system for the synthesis of 1-chloro-1,1,4,4,4-pentafluoro-2-butene and E-1,1,1,4,4,4-hexafluoro-2-butene. Background Technology
[0002] 1-Chloro-1,1,4,4,4-pentafluoro-2-butene and E-1,1,1,4,4,4-hexafluoro-2-butene are typical representatives of fluorinated olefins, with excellent properties and important industrial value.
[0003] 1-Chloro-1,1,4,4,4-pentafluoro-2-butene can be used as a refrigerant, cleaning agent, foaming agent, fire extinguishing agent, and diluent. For example, in the cleaning field, cleaning agents produced using 1-chloro-1,1,4,4,4-pentafluoro-2-butene exhibit better cleaning performance than some commercially available hydrofluoroether products. E-1,1,1,4,4,4-hexafluoro-2-butene is widely used in refrigerants, high-temperature heat pumps, organic Rankine cycles, and foaming agents. It is also an important intermediate in the synthesis of Z-1,1,1,4,4,4-hexafluoro-2-butene. Therefore, the industrial value of 1-chloro-1,1,4,4,4-pentafluoro-2-butene and E-1,1,1,4,4,4-hexafluoro-2-butene is evident.
[0004] Currently, almost all existing methods for producing 1-chloro-1,1,4,4,4-pentafluoro-2-butene use 1-chloro-1,1,4,4,4-pentafluoro-2-butene as a byproduct, resulting in low yields.
[0005] However, methods for preparing E-1,1,1,4,4,4-hexafluoro-2-butene suffer from problems such as low product yield, poor selectivity, strong catalyst corrosion, and pollution from waste, etc. The prior art with publication number WO2009117458A2 points out a method for reacting copper powder with HCFC-123 to generate E-1,1,1,4,4,4-hexafluoro-2-butene. This method has poor trans selectivity and causes serious pollution. The prior art disclosed in CN103172489B describes a method for obtaining E-1,1,1,4,4,4-hexafluoro-2-butene by fluorination reaction. This method has a low conversion rate, produces a lot of by-products, and has excessively high waste liquid treatment costs.
[0006] The prior art disclosed in CN111065616A points out that a method for producing E-1,1,1,4,4,4-hexafluoro-2-butene by reacting CF3CHClCH2CCl3 with HF using a highly corrosive catalyst (such as SbF5) is problematic due to its corrosiveness, thus requiring high-quality equipment.
[0007] It is evident that the existing processes for preparing 1-chloro-1,1,4,4,4-pentafluoro-2-butene and / or E-1,1,1,4,4,4-hexafluoro-2-butene have many shortcomings, and therefore, improvements are needed. Summary of the Invention
[0008] To address the shortcomings of existing technologies, the present invention aims to provide a continuous production system and a fully continuous process for the synthesis of 1-chloro-1,1,4,4,4-pentafluoro-2-butene and E-1,1,1,4,4,4-hexafluoro-2-butene. This system fills the gaps in existing processes by employing hypergravity process enhancement technology, azeotropic separation, the concept of reaction separation unit coupling, and a comprehensive energy utilization scheme for the entire system.
[0009] The technical solution of the present invention is implemented as follows: a continuous production system for synthesizing 1-chloro-1,1,4,4,4-pentafluoro-2-butene and E-1,1,1,4,4,4-hexafluoro-2-butene, comprising a first-pass synthesis system for producing 1-chloro-1,1,4,4,4-pentafluoro-2-butene and a second-pass synthesis system for producing E-1,1,1,4,4,4-hexafluoro-2-butene; In this process, at least one connecting branch is constructed between the primary and secondary synthesis systems to allow materials to enter the secondary synthesis system from the primary synthesis system. Hydrogen fluoride and / or 1-chloro-1,1,4,4,4-pentafluoro-2-butene generated from the primary synthesis system can enter the secondary synthesis system through the connecting branch.
[0010] Preferably, the connecting branch includes a first branch supplying hydrogen fluoride from the first reaction synthesis system to the second reaction synthesis system and a second branch supplying 1-chloro-1,1,4,4,4-pentafluoro-2-butene from the first reaction synthesis system to the second reaction synthesis system.
[0011] Preferably, the first-stage synthesis system includes a first-stage reaction system, a first-stage separation system, and a first-stage product system; The second reaction synthesis system includes a second reaction system, a second reaction separation system, and a second reaction product system; Among them, at least one third branch is constructed between the first-stage reaction separation system and the second-stage reaction separation system to allow HCL to enter the second-stage reaction separation system from the first-stage reaction separation system.
[0012] Preferably, the primary reaction system includes a primary reaction vaporizer, a high-gravity reactor, a reaction separation tower, a primary reaction discharge condenser, a primary reaction preheater, a reaction circulation vessel, a reaction circulation pump, and a circulation heater; This also includes: The hydrogen fluoride branch is used to transport hydrogen fluoride through the first vaporizer and into the hypergravity reactor. The primary reactor feedstock branch is used to transport the primary reactor feedstock sequentially through the primary reactor preheater, reaction circulation vessel, reaction circulation pump, circulation heater, and into the hypergravity reactor. The first return feed branch connects the reaction separation tower and the reaction circulation vessel; The second return feed branch connects the centrifugal reactor and the reaction circulation vessel; The first discharge branch is used to transport materials from the supergravity reactor and after passing through the reaction separation tower and the first reaction discharge condenser, they are discharged from the first reaction system.
[0013] Preferably, the primary reaction separation system includes a primary reaction discharge separator, a primary reaction high gravity separator, a primary reaction heavy phase buffer tank, a primary reaction light phase buffer tank, a primary reaction light phase circulating pump, and a primary reaction light phase removal tower; Among them, the first reverse discharge separation tank can receive the material discharged from the first discharge branch, and after separating the material into gas and liquid phases, send the liquid phase material into the first reverse gravity separator, and send the gas phase material into the second reverse separation system. Also includes: The first reaction light phase branch can send the first reaction light phase material separated from the first reaction ultragravity separator into the first reaction light phase buffer tank, and then the first reaction light phase circulation pump will transport the first reaction light phase material to the first reaction vaporizer and / or the second reaction system. The first reverse heavy phase branch can transport the first reverse heavy phase material separated from the first reverse ultragravity separator through the first reverse heavy phase buffer tank and the first reverse light phase removal tower in sequence.
[0014] Preferably, the primary reaction finished product system includes a primary reaction finished product tower, a primary reaction finished product tower outlet, and a primary reaction high-boiling circulating pump; The primary reactor product tower receives the material discharged from the primary reactor light removal tower and collects 1-chloro-1,1,4,4,4-pentafluoro-2-butene at the top of the primary reactor product tower before discharging it from the outlet of the primary reactor product tower; the material in the bottom of the primary reactor product tower is sent back to the reaction circulation vessel through the third return feed branch.
[0015] Preferably, the second reaction system includes a second reaction vaporizer, a second reaction heat exchanger, a second reaction heater, a second reaction reactor, and a second reaction cooler; the second reaction vaporizer is connected to the first reaction light phase branch and the first reaction light phase removal tower; This also includes: The secondary reactor feedstock branch is used to transport the secondary reactor feedstock from the secondary reactor vaporizer through the tube side of the secondary reactor heat exchanger, the secondary reactor heater, the secondary reactor reactor, the shell side of the secondary reactor heat exchanger, and the secondary reactor cooler before sending it into the secondary reactor separation system.
[0016] Preferably, the second-phase separation system includes an HCl separation tower, an HCl tower bottom cooler, a second-phase high-gravity separator, a second-phase heavy phase buffer tank, a second-phase heavy phase discharge pump, a second-phase light phase buffer tank, a second-phase light phase discharge pump, an HF recovery tower, a second-phase preheater, and a second-phase light phase removal tower. The HCl separation tower is connected to the feed branch of the second reactor and the discharge separator of the first reactor. The HCl separation tower has an HCl gas outlet and separates and purifies the HCl in the material before sending the mixture into the high gravity separator of the second reactor. Also includes: The second-phase light phase branch can transport the second-phase light phase material separated from the second-phase ultragravity separator through the second-phase light phase buffer tank and the HF recovery tower in sequence. The second-phase heavy phase branch can transport the second-phase heavy phase material separated from the second-phase ultragravity separator through the second-phase heavy phase buffer tank, the second-phase preheater and the second-phase light phase removal tower in sequence. The third return feed branch connects the HF recovery tower and the second reactor vaporizer; The fourth return feed branch connects the HF recovery tower and the second-stage gravity separator.
[0017] Preferably, the secondary reaction finished product system includes a secondary reaction finished product tower, a secondary reaction finished product outlet, and a secondary reaction high-boiling circulating pump; The product tower of the second reactor is connected to the light product removal tower of the second reactor, and also includes a fifth return feed branch, which can transport the intermediate product in the product tower of the second reactor to the vaporizer of the second reactor.
[0018] Preferably, the secondary desulfurization tower is equipped with an intermittent discharge outlet for light component impurities.
[0019] The reaction equations involved in the above-mentioned continuous production system used in this invention are as follows: In a one-reaction synthetic system (one-reaction reaction): In a two-trans synthesis system (two-trans reaction): The present invention has at least the following beneficial effects: 1. The reaction process of the present invention is divided into two main stages. When the first stage is used alone, it can be used to prepare 1-chloro-1,1,4,4,4-pentafluoro-2-butene. When the first stage and the second stage are used, 1-chloro-1,1,4,4,4-pentafluoro-2-butene and E-1,1,1,4,4,4-hexafluoro-2-butene can be produced simultaneously. Moreover, the 1-chloro-1,1,4,4,4-pentafluoro-2-butene produced is far superior to that of the prior art. Therefore, the present invention not only has a production process that can use 1-chloro-1,1,4,4,4-pentafluoro-2-butene as the main product, but can also simultaneously produce two products: 1-chloro-1,1,4,4,4-pentafluoro-2-butene and E-1,1,1,4,4,4-hexafluoro-2-butene.
[0020] The two main stages of this invention are as follows: First stage (synthesis of 1-chloro-1,1,4,4,4-pentafluoro-2-butene): In the first stage, 1,1,1,3-tetrachloro-4,4,4-trifluorobutane reacts with hydrogen fluoride in a hypergravity reactor to produce 1-chloro-1,1,4,4,4-pentafluoro-2-butene. Through the efficient hypergravity reactor design, the reaction can achieve high conversion rate and high selectivity in a short time.
[0021] Second stage (synthesis of E-1,1,1,4,4,4-hexafluoro-2-butene): In the second stage, 1-chloro-1,1,4,4,4-pentafluoro-2-butene and hydrogen fluoride react with a second-stage catalyst in a fixed-bed reactor to produce E-1,1,1,4,4,4-hexafluoro-2-butene. This process employs a highly efficient heat exchange system to ensure stable reaction temperature and improve reaction efficiency.
[0022] 2. In the separation process after the reaction, the present invention employs the single-reaction separation system and the double-reaction separation system of this application, which can significantly improve the utilization rate of reactants and the purity of products, as can be manifested in: High gravity separator and HF separation: In the first-stage reaction synthesis system, after condensation and separation, the reactants are subjected to phase separation using a high-gravity separator, effectively separating 1-chloro-1,1,4,4,4-pentafluoro-2-butene from HF. The separated HF is then reused, maximizing the utilization rate of the raw materials and reducing resource waste.
[0023] In the two-phase reaction synthesis system, after heat exchange and condensation, E-1,1,1,4,4,4-hexafluoro-2-butene and HF undergo HCl removal treatment. Next, the mixture enters a high-gravity separator for phase separation. The lighter phase (HF) is separated and returned to the reaction system, ensuring the continuity of the reaction process. Furthermore, the extractant is recycled, further improving the system's efficiency.
[0024] Azeotropic properties are utilized for the complete removal of HF: Azeotropic properties of HF with 1-chloro-1,1,4,4,4-pentafluoro-2-butene: By utilizing the azeotropic properties of HF and 1-chloro-1,1,4,4,4-pentafluoro-2-butene, HF is completely removed and effectively recovered. This process avoids traditional water washing and alkaline washing steps, improving the recovery rate and reducing waste emissions, thus meeting green environmental protection requirements.
[0025] Azeotropic properties of HF with E-1,1,1,4,4,4-hexafluoro-2-butene: Similarly, through the azeotropic properties of HF and E-1,1,1,4,4,4-hexafluoro-2-butene, HF is completely removed and recycled into the system, avoiding the traditional water washing and alkaline washing processes. This not only improves the yield but also reduces the generation of waste, achieving high efficiency and environmental protection in the process.
[0026] 3. Environmental Protection and Energy Conservation: The process flow of this invention significantly reduces the emission of wastewater, waste gas, and solid waste through efficient separation, recovery, and comprehensive energy utilization. It avoids high-pollution steps commonly found in traditional processes, such as water washing and alkaline washing, ensuring not only the full recovery of reactants and solvents but also achieving efficient energy utilization through a sophisticated heat exchange system. Through continuous production and optimized separation steps, this invention reduces resource waste and energy consumption while maintaining high yields, meeting the requirements of modern green chemical processes.
[0027] In summary, the process of the present invention has at least the following advantages: Improved reaction efficiency: By utilizing the synergistic effect of the supergravity reactor and the high-efficiency catalyst, the conversion rate and selectivity of the reaction are improved, avoiding the inefficiency problems of traditional processes.
[0028] Efficient resource utilization: By recovering HF and other reactants multiple times, the maximum utilization of raw materials is ensured, and the cost of raw materials is reduced.
[0029] Environmentally friendly and energy-saving: It avoids the traditional water washing and alkaline washing processes, reducing wastewater discharge, and effectively reduces energy consumption through a precision heat exchange system.
[0030] Wide applicability: The process of this invention is not only applicable to the synthesis of 1-chloro-1,1,4,4,4-pentafluoro-2-butene and E-1,1,1,4,4,4-hexafluoro-2-butene, but can also be extended to the production of other fluorinated olefins (such as the preparation of 1,2-dichloro-3,3,4,4,5,5-hexafluorocyclopentene and 1-chloro-2,3,3,4,4,5,5-heptafluorocyclopentene from hexachlorocyclopentadiene and hydrogen fluoride).
[0031] It is worth mentioning that, unless otherwise specified, the meanings of the substances described in this invention can be found in the table below: 1,1,1,3-Tetrachloro-4,4,4-trifluorobutane 1-Chloro-1,1,4,4,4-pentafluoro-2-butene E-1,1,1,4,4,4-hexafluoro-2-butene Furthermore, the specific use of the continuous production system of the present invention will be shown in the embodiments section of the present invention, thereby making the beneficial effects of the present invention even more significant. Attached Figure Description
[0032] To more clearly illustrate the technical solutions in the embodiments of the present invention or the prior art, the drawings used in the description of the embodiments or the prior art will be briefly introduced below. Obviously, the drawings described below are only some embodiments of the present invention. For those skilled in the art, other drawings can be obtained based on these drawings without creative effort.
[0033] Figure 1 This is a system block diagram illustrating a specific embodiment of the present invention; Figure 2 This is a schematic diagram of the structure of the hypergravity reactor in a specific embodiment of the present invention; Figure 3 This is a schematic diagram of the structure of the supergravity separator in a specific embodiment of the present invention. Detailed Implementation
[0034] The technical solutions of the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of the present invention.
[0035] like Figures 1-3 As shown, this embodiment provides a continuous production system for synthesizing 1-chloro-1,1,4,4,4-pentafluoro-2-butene and E-1,1,1,4,4,4-hexafluoro-2-butene, including a single-reaction synthesis system for producing 1-chloro-1,1,4,4,4-pentafluoro-2-butene and a double-reaction synthesis system for producing E-1,1,1,4,4,4-hexafluoro-2-butene, as described above. Figure 1 , Figure 1The upper half of the region is the inverse synthesis system of this embodiment. Figure 1 The lower half of the text is the two-inverse synthesis system of this embodiment.
[0036] In this embodiment, a connecting branch is constructed between the primary and secondary synthesis systems to allow materials to enter the secondary synthesis system from the primary synthesis system. Hydrogen fluoride and / or 1-chloro-1,1,4,4,4-pentafluoro-2-butene generated from the primary synthesis system can enter the secondary synthesis system through the connecting branch. The connecting branch in this embodiment includes a first branch for supplying hydrogen fluoride from the primary synthesis system to the secondary synthesis system and a second branch for supplying 1-chloro-1,1,4,4,4-pentafluoro-2-butene from the primary synthesis system to the secondary synthesis system. The first branch in this embodiment is a pipeline connecting the primary light phase circulation pump 56 in the primary synthesis system and the secondary vaporizer 34 in the secondary synthesis system. The second branch is a pipeline connecting the primary light phase removal tower feed pump 29 and the secondary vaporizer 34 in the secondary synthesis system.
[0037] In this embodiment: the first-stage synthesis system includes a first-stage reaction system, a first-stage separation system, and a first-stage product system; the second-stage synthesis system includes a second-stage reaction system, a second-stage separation system, and a second-stage product system. Among them, a third branch is constructed between the primary reaction separation system and the secondary reaction separation system to allow HCl to enter the secondary reaction separation system from the primary reaction separation system. The third branch is a pipeline connecting the primary reaction discharge separator 19 in the primary reaction synthesis system and the HCl separation tower 20 in the secondary reaction synthesis system.
[0038] The inverse synthesis system of this embodiment is as follows: The primary reaction system of this embodiment includes a primary reaction vaporizer 11, a high-gravity reactor 14, a reaction separation tower 15, a primary reaction discharge condenser 18, a primary reaction preheater 12, a reaction circulation vessel 13, a reaction circulation pump 16, and a circulation heater 17. This primary reaction system has a hydrogen fluoride inlet 01 and a feed inlet 02, with 1,1,1,3-tetrachloro-4,4,4-trifluorobutane entering through the feed inlet 02. It also includes: The hydrogen fluoride branch is used to transport hydrogen fluoride through the first vaporizer 11 and into the hypergravity reactor 14. Hydrogen fluoride enters the hydrogen fluoride branch from the hydrogen fluoride inlet 01, and enters the hypergravity reactor 14 after passing through the first vaporizer 11. The primary reactor feedstock branch is used to transport the primary reactor feedstock (1,1,1,3-tetrachloro-4,4,4-trifluorobutane) sequentially through the primary reactor preheater 12, the reaction circulation vessel 13, the reaction circulation pump 16, the circulation heater 17, and into the hypergravity reactor 14. The first return feed branch is connected between the reaction separation tower 15 and the reaction circulation vessel 13; The second return feed branch is connected between the supergravity reactor 14 and the reaction circulation vessel 13; The first discharge branch is used to transport materials from the supergravity reactor 14 to the reaction separation tower 15 and the first reaction discharge condenser 18 before being discharged from the first reaction system.
[0039] The primary reactor separation system in this embodiment includes a primary reactor discharge separator 19, a primary reactor gravity separator 23, a primary reactor heavy phase buffer tank 24, a primary reactor light phase buffer tank 25, a primary reactor light phase circulation pump 56, and a primary reactor light phase removal tower 26. Among them, the first reverse discharge separation tank 19 can receive the material discharged from the first discharge branch, and after separating the material into gas and liquid phases, send the liquid phase material into the first reverse gravity separator 23, and send the gas phase material into the second reverse separation system. It also includes: a light phase branch, which can send the light phase material separated from the first reaction supergravity separator 23 into the light phase buffer tank 25, and then the light phase circulation pump 56 transports the light phase material to the first reaction vaporizer 11 or the second reaction system. In this embodiment, the light phase branch is also provided with a hydrogen fluoride recycling outlet 06. The first reverse heavy phase branch can transport the first reverse heavy phase material separated from the first reverse ultragravity separator 23 through the first reverse heavy phase buffer tank 24 and the first reverse light phase removal tower 26 in sequence. The first reverse light phase removal tower 26 has a first reverse light phase removal tower reboiler 27, a first reverse light phase removal tower condenser 28 and a first reverse light phase removal tower top discharge pump 29.
[0040] The primary reactor finished product system in this embodiment includes a primary reactor finished product tower 30, a primary reactor finished product tower outlet 04, and a primary reactor high-boiling circulating pump 33. The primary reactor finished product tower 30 in this embodiment also has a primary reactor finished product tower reboiler 31 and a primary reactor finished product tower condenser 32. The primary reactor product tower 30 can receive the material discharged from the primary reactor light removal tower 26 and collect 1-chloro-1,1,4,4,4-pentafluoro-2-butene at the top of the primary reactor product tower before discharging it from the primary reactor product tower outlet 04; the material in the bottom of the primary reactor product tower is sent back to the reaction circulation vessel through the third return branch, which is connected between the primary reactor high-boiling circulation pump 33 and the reaction circulation vessel.
[0041] The two-in-one synthesis system of this embodiment is as follows: The second reaction system in this embodiment includes a second reaction vaporizer 34, a second reaction heat exchanger 35, a second reaction heater 36, a second reaction reactor 37, and a second reaction cooler 38; the second reaction vaporizer 34 is connected to the first reaction light phase branch and the first reaction light phase removal tower, and the first reaction light phase branch located between the first reaction light phase circulation pump 56 and the second reaction vaporizer is the first branch in this embodiment; It also includes: a secondary reactor feedstock branch, used to transport secondary reactor feedstock from the secondary reactor vaporizer 34 through the tube side of the secondary reactor heat exchanger 35, the secondary reactor heater 36, the secondary reactor reactor 37, the shell side of the secondary reactor heat exchanger 35, and the secondary reactor cooler 38 before sending it into the secondary reactor separation system.
[0042] The second-phase separation system in this embodiment includes an HCl separation tower 20, an HCl tower bottom cooler 55, a second-phase gravity separator 39, a second-phase heavy phase buffer tank 40, a second-phase heavy phase discharge pump 41, a second-phase light phase buffer tank 42, a second-phase light phase discharge pump 43, an HF recovery tower 44, a second-phase preheater 47, and a second-phase light phase removal tower 48. The HCl separation tower also includes an HCl separation tower reboiler 21 and an HCl separation tower condenser 22. The HF recovery tower 44 includes an HF recovery tower reboiler 45 and an HF recovery tower condenser 46. The second-phase light phase removal tower 48 includes a second-phase light phase removal tower reboiler 49 and a second-phase light phase removal tower condenser 50. The HCl separation tower 20 is connected to the feed branch of the second reactor and the discharge separation tank 19 of the first reactor. The HCl separation tower 20 has an HCl gas outlet 03. After separating and purifying the HCl in the material, the HCl separation tower 20 sends the mixture to the second reactor gravity separator 39. Also includes: The second-phase light phase branch can transport the second-phase light phase material separated from the second-phase ultragravity separator 39 through the second-phase light phase buffer tank 42 and the HF recovery tower 44 in sequence. The second-phase heavy phase branch can transport the second-phase heavy phase material separated from the second-phase ultragravity separator 39 through the second-phase heavy phase buffer tank 40, the second-phase preheater 47 and the second-phase light phase removal tower 48 in sequence. The third return feed branch is connected between the HF recovery tower 44 and the second vaporizer 34; The fourth return branch connects the HF recovery tower 44 and the second-stage gravity separator 39.
[0043] Second-stage reaction finished product system: The second-stage reaction finished product system in this embodiment includes a second-stage reaction finished product tower 51, a second-stage reaction finished product outlet 08, and a second-stage reaction high-boiling circulation pump 54. The second-stage reaction finished product tower 51 also has a second-stage reaction finished product tower reboiler 52 and a second-stage reaction finished product tower condenser 53. The product tower 51 of the second reactor is connected to the light product removal tower 58 of the second reactor, and also includes a fifth return branch, which can transport the intermediate product in the product tower 51 of the second reactor to the vaporizer 34 of the second reactor.
[0044] In this embodiment: the secondary desulfurization tower is provided with an intermittent discharge port 07 for light component impurities.
[0045] like Figure 2As shown, the hypergravity reactor in this embodiment includes a gas phase inlet 14-1, a liquid phase inlet 14-2, a gas phase outlet 14-3, a liquid phase outlet 14-4, a motor 14-5, a frame 14-6, a rotating shaft 14-7, a liquid distributor 14-8, a gas guide hood 14-9, a rotating packing disc 14-10, an outer shell 14-11, and a jacket. The rotating packing disc 14-10 is fixed to the rotating shaft 14-7 and rotates together with it under the drive of the motor. The gas guide hood 14-9 is fixed to the outer shell, and a circumferential gas flow channel is opened at the position between the bottom plate of the rotating packing disc and the bottom plate of the outer shell of the hypergravity reactor.
[0046] like Figure 3 As shown, the supergravity separator of this embodiment (the structure of the first-stage supergravity separator and the second-stage supergravity separator is the same) has a feed inlet a, a recycling inlet b, a heavy phase outlet c, and a light phase outlet d.
[0047] To elaborate further: The connection sequence of the primary reaction synthesis system is as follows: the hydrogen fluoride inlet 01 and the primary reaction hydrogen fluoride recycling outlet 06 are combined and enter the primary reaction vaporizer 11, and then enter the gas phase inlet 14-1 of the hypergravity reactor 14; the feed inlet 02 is connected to the inlet of the primary reaction preheater 12, the outlet of the primary reaction preheater 12 is connected to one inlet of the reaction circulation vessel 13, the liquid phase outlet 14-4 of the hypergravity reactor is connected to the other inlet of the reaction circulation vessel 13, and the bottom outlet of the reaction circulation vessel 13 is connected to the inlet of the reaction circulation pump 16. The outlet of the reaction circulation pump 16 is connected to the inlet of the circulation heater 17, and the outlet of the circulation heater 17 is connected to the liquid phase inlet 14-2 of the hypergravity reactor. The gas phase outlet 14-3 of the hypergravity reactor is connected in sequence to the inlet of the first reactor discharge condenser 18 and the first reactor discharge separator 19. The gas phase outlet of the first reactor discharge separator 19 is connected to the inlet of the HCl separation tower 20. The liquid phase outlet of the first reactor discharge separator 19 is connected to the inlet a of the first reactor hypergravity separator. The light phase outlet d of the first reactor hypergravity separator is connected to the light phase outlet d of the first reactor. The inlet of buffer tank 25 is connected to the first reactor light phase buffer tank 25, and the outlet of the first reactor light phase circulation pump 56 is connected to the inlet of the first reactor light phase circulation pump 56. The first reactor light phase circulation pump 56 is equipped with a first reactor hydrogen fluoride recycling outlet 06 and a second reactor hydrogen fluoride outlet 05. The heavy phase outlet c of the first reactor ultragravity separator is connected to the inlet of the first reactor light phase removal tower 26. The first reactor light phase removal tower 26 is equipped with a first reactor light phase removal tower reboiler 27 and a first reactor light phase removal tower condenser 28. The liquid phase collection pipeline at the top of the first reactor light phase removal tower 26 is connected to the inlet of the first reactor light phase removal tower top discharge pump 29. The outlet of the top discharge pump 29 is connected to the inlet of the second reactor vaporizer 34; the liquid phase collection pipeline of the bottom of the first reactor light removal tower 26 is connected to the inlet of the first reactor product tower 30; the first reactor product tower 30 is equipped with a first reactor product tower reboiler 31 and a first reactor product tower condenser 32; the top of the first reactor product tower 30 is equipped with a liquid phase product collection pipeline (including the first reactor product outlet); the liquid phase collection pipeline of the bottom of the first reactor product tower 30 is connected to the inlet of the first reactor high boiling circulation pump 33; the outlet of the first reactor high boiling circulation pump 33 is connected to another inlet of the reaction circulation vessel 13.
[0048] The connection sequence of the second-stage reaction synthesis system is as follows: the hydrogen fluoride outlet 05 of the first-stage reaction and the outlet of the top discharge pump 29 of the first-stage reaction light phase removal tower are connected to the inlet of the second-stage reaction vaporizer 34. The outlet of the second-stage reaction vaporizer 34 is connected sequentially to the second-stage reaction heat exchanger 35 (tube side), the second-stage reaction heater 36, the second-stage reaction reactor 37, the second-stage reaction heat exchanger 35 (shell side), the second-stage reaction cooler 38, and the other inlet of the HCl separation tower 20. The HCl separation tower 20 is equipped with an HCl separation tower reboiler 21 and an HCl separation tower condenser 22. The top of the HCl separation tower is equipped with a gas phase outlet (HCl gas outlet 03). The liquid phase outlet of the HCl separation tower bottom 20 is connected to the inlet of the HCl tower bottom discharge condenser 55. The outlet of the HCl tower bottom discharge condenser 55 is connected to the inlet a of the second-stage reaction high gravity separator. The light phase outlet d of the second-stage reaction high gravity separator is connected sequentially to the second-stage reaction light phase buffer tank 42, the second-stage reaction light phase discharge pump 43, and the inlet of the HF recovery tower 44. The HF recovery tower 44 is equipped with an HF recovery tower reboiler 45 and an HF recovery tower reboiler 45. The condenser 46 of the recovery tower has its top vapor phase outlet connected to the inlet of the second reactor vaporizer 34. The liquid phase outlet of the HF recovery tower 44 is connected to the reuse port b of the second reactor ultragravity separator. The heavy phase outlet c of the second reactor ultragravity separator is sequentially connected to the heavy phase buffer tank 40, the heavy phase discharge pump 41, the feed preheater 47 of the second reactor light removal tower, and the inlet of the second reactor light removal tower 48. The second reactor light removal tower 48 is equipped with a reboiler 49 and a condenser 50. The vapor phase outlet at the top of tower 51 is connected to the inlet of the vaporizer 34 of the second reactor. The liquid phase outlet at the bottom of tower 48, which is used for removing light pollutants, is connected to the inlet of the product tower 51. The product tower 51 is equipped with a reboiler 52 and a condenser 53. The liquid phase outlet at the bottom of the product tower 51 is connected to the inlet of the high-boiling circulation pump 54 of the second reactor. The outlet of the high-boiling circulation pump 54 is connected to the inlet of the vaporizer 34 of the second reactor. The top of the product tower 51 is equipped with a liquid phase outlet (product outlet 08).
[0049] Referring to the continuous production system of this embodiment, the production steps of this embodiment (i.e., a fully continuous production process for synthesizing 1-chloro-1,1,4,4,4-pentafluoro-2-butene and E-1,1,1,4,4,4-hexafluoro-2-butene) include: (1) Add a first reaction catalyst and a first reaction co-catalyst, as well as hydrogen fluoride to the reaction circulation vessel 13, turn on the stirring and the reaction circulation pump 16 to circulate the mixture in the reaction circulation vessel 13, and turn on the circulation heater 17 to heat it. After heating, the material enters from the liquid phase inlet 14-2, passes through the supergravity reactor 14, and the liquid phase material flows into the reaction circulation vessel 13. The reaction system establishes circulation, and the system temperature and pressure increase. (2) Hydrogen fluoride is introduced into the hydrogen fluoride inlet 01, and 1,1,1,3-tetrachloro-4,4,4-trifluorobutane is introduced into the raw material inlet 02. After being vaporized by the first reactor vaporizer 11, the hydrogen fluoride enters the gas phase inlet 14-1 of the supergravity reactor 14. After entering the reaction circulation vessel 13, it is mixed with liquid hydrogen fluoride, the first reactor catalyst and the first reactor co-catalyst in the reaction circulation vessel 13. After passing through the circulation heater 17, the partially vaporized hydrogen fluoride enters the supergravity reactor from the gas phase inlet 14-1, and the liquid material enters from the liquid phase inlet 14-1. 4-2 Enters the hypergravity reactor, where a gas-liquid contact reaction occurs. The hydrogen chloride gas, 1-chloro-1,1,4,4,4-pentafluoro-2-butene, and some hydrogen fluoride produced by the reaction are collected from the gas outlet 14-3 of the hypergravity reactor and enter the reaction separation tower 15. In the reaction separation tower, the azeotrope of HCl gas, 1-chloro-1,1,4,4,4-pentafluoro-2-butene, and hydrogen fluoride is collected from the top of the tower in gas phase and enters the first-stage discharge condenser 18. Some hydrogen fluoride is returned from the bottom of the tower to the reaction circulation vessel 13. (3) After passing through the first reactor discharge condenser 18, the product enters the first reactor discharge separator 19. In the separator, 1-chloro-1,1,4,4,4-pentafluoro-2-butene and hydrogen fluoride are in the liquid phase (liquid phase material), while HCl remains in the gas phase (gas phase material). Gas-liquid separation occurs, with the HCl gas phase entering the HCl separation tower 20 and the liquid phase entering the first reactor supergravity separator 23. After passing through the first reactor supergravity separator, the hydrogen fluoride light phase (first reactor light phase material) enters the first reactor light phase buffer tank 25, and then returns to the first reactor vaporizer 11 via the first reactor light phase circulation pump 56 to participate in the reaction again. It can also be sent to the second reactor vaporizer 34. Hydrogen fluoride is added; the heavy phase (heavy phase material from the first reaction) flows into the heavy phase buffer tank 24 of the first reaction, and then enters the light phase removal tower 26 of the first reaction. Hydrogen fluoride and 1-chloro-1,1,4,4,4-pentafluoro-2-butene are separated in this tower and collected from the top of the tower and enter the vaporizer 34 of the second reaction. The bottom material of the tower, mainly 1-chloro-1,1,4,4,4-pentafluoro-2-butene and a small amount of high-boiling substances, enters the product tower 30 of the first reaction. The top of the product tower 30 of the first reaction collects the 1-chloro-1,1,4,4,4-pentafluoro-2-butene product, and the bottom material of the product tower of the first reaction is returned to the reaction recycling tank 13 to participate in the reaction again. (4) A solid particulate catalyst (chromium-based catalyst, i.e., the catalyst of the present invention) is added to the second reactor 37. The reactor is a fixed bed reactor; an extractant (such as concentrated sulfuric acid) is added to the second reactor gravity separator 39. (5) The material vaporized after entering the second reactor vaporizer 34 passes through the second reactor heat exchanger 35 (tube side), the second reactor heater 36, the second reactor reactor 37, the second reactor heat exchanger 35 (shell side), and the second reactor cooler 38. In the second reactor reactor 37, 1-chloro-1,1,4,4,4-pentafluoro-2-butene undergoes a fluorine-chlorine substitution reaction with hydrogen fluoride to generate E-1,1,1,4,4,4-hexafluoro-2-butene and HCl. E-1,1,1,4,4,4-hexafluoro-2-butene, HCl, and excess hydrogen fluoride are partially liquefied in the second-stage reactor cooler 38 and enter the HCl separation tower. This tower separates and purifies the HCl produced by the first and second-stage reactor synthesis systems, and high-purity HCl gas is collected from the top of the HCl separation tower. This gas can be used to produce hydrochloric acid or calcium chloride. The bottom of the HCl separation tower, containing a mixture mainly composed of E-1,1,1,4,4,4-hexafluoro-2-butene and hydrogen fluoride, after being completely dehydrated, enters the second-stage reactor high-gravity separator 39. The lighter phase (second-stage reactor light phase material), mainly composed of hydrogen fluoride and extractant, then enters the second-stage reactor light phase buffer tank. 42. The light phase feed pump 43 of the second reactor enters the HF recovery tower 44. The hydrogen fluoride collected from the top of the HF recovery tower is returned to the vaporizer 34 of the second reactor. The extractant in the bottom of the HF recovery tower is returned to the recycling port of the second reactor supergravity separator for reuse. The heavy phase (heavy phase material of the second reactor) flows into the heavy phase buffer tank 40 of the second reactor. After being preheated by the heavy phase feed pump 41 of the second reactor, it enters the light phase removal tower 48 of the second reactor. The liquid phase collected from the top of the light phase removal tower 48 contains hydrogen fluoride and an azeotrope of E-1,1,1,4,4,4-hexafluoro-2-butene, which is returned to the supergravity separator 39 of the second reactor. The gaseous light components enriched at the top of the tower can be intermittently discharged from the second reactor synthesis system through the light component impurity intermittent discharge port. (6) The material in the bottom of the second reaction light removal tower 48 enters the second reaction product tower 51. E-1,1,1,4,4,4-hexafluoro-2-butene product is collected at the top of the second reaction product tower. The heavy component in the bottom of the second reaction product tower (i.e., the unreacted material, also known as the intermediate) is returned to the second reaction vaporizer 34 to participate in the reaction again.
[0050] It should be noted that: the raw material 1,1,1,3-tetrachloro-4,4,4-trifluorobutane forms a liquid phase system with the recycled primary and secondary catalysts, the primary and secondary co-catalysts, and excess and liquefied hydrogen fluoride. This system, along with fresh hydrogen fluoride and the phase-separated recovered hydrogen fluoride gas phase, undergoes a high-efficiency counter-current contact reaction in a hypergravity reactor, resulting in extremely high conversion and selectivity. The product 1-chloro-1,1,4,4,4-pentafluoro-2-butene, an azeotrope with HF, a small amount of HF, and HCl leave the hypergravity reactor in gaseous form. In the first-phase synthesis system, the HCl product is initially separated from other liquid products by liquid separation. The HCl gas after initial separation enters the HCl separation tower (second-phase synthesis system) for purification. The small amount of HCl in the liquid products can be stored in the light phase buffer tank and heavy phase buffer tank of the first-phase synthesis system, and then enter the supergravity reactor and the second-phase reactor.
[0051] In the primary reaction synthesis system, the products are separated from the liquid phase by the primary reaction outlet separator, where HCl gas is separated from other liquid products. The liquid products then enter a high-gravity separator for phase separation. The light phase, mainly composed of hydrogen fluoride, can be used in both the primary and secondary reactions. The heavy phase, mainly composed of organic matter, enters the primary reaction light phase removal tower. In the primary reaction light phase removal tower, HCl, HF, and the azeotrope of 1-chloro-1,1,4,4,4-pentafluoro-2-butene are removed, as well as 1-chloro-1,1,4,4,4-pentafluoro-2-butene, which was increased to meet the feed rate requirements of the secondary reaction. The feed consists of 1,4,4,4-pentafluoro-2-butene and other light components generated during the reaction. This feed is collected from the top of the first reaction light component removal tower and enters the second reaction system. The feed mainly consists of 1-chloro-1,1,4,4,4-pentafluoro-2-butene and a small amount of HF. This design ensures that the light components of 1-chloro-1,1,4,4,4-pentafluoro-2-butene are completely removed, and is cleverly used as feed for the second reaction. The introduced components do not have any adverse effects on the second reaction.
[0052] In the second reaction, 1-chloro-1,1,4,4,4-pentafluoro-2-butene collected from the top of the first reaction's light phase removal tower and hydrogen fluoride pumped from the first reaction's light phase pass sequentially through the second reaction vaporizer, second reaction heat exchanger, second reaction heater, fixed-bed reactor (second reaction reactor), second reaction heat exchanger, second reaction condenser, and HCl separation tower. In the fixed-bed reactor, under the action of the second reaction catalyst, 1-chloro-1,1,4,4,4-pentafluoro-2-butene reacts with excess HF to produce E-1,1,1,4,4,4-hexafluoro-2-butene and HCl. This reaction exhibits extremely high conversion and selectivity. After HCl removal in the HCl separation tower, other reaction products are collected from the bottom liquid phase of the HCl separation tower, cooled, and then fed into the second reaction's high-gravity separator. With the aid of the extractant, the light and heavy phases are rapidly separated. Hydrogen fluoride and the extractant constitute the light phase, while the organic matter constitutes the heavy phase. The light phase enters the HF recovery tower, where the HF, after removing the extractant, is collected from the top and returned to the reaction system. The extractant is returned to the second-stage ultragravity separator to participate in the reaction again. The heavy phase material, mainly composed of E-1,1,1,4,4,4-hexafluoro-2-butene, enters the second-stage light phase removal tower. Utilizing the azeotropic properties, the azeotrope of HF and E-1,1,1,4,4,4-hexafluoro-2-butene is separated from the top of the tower and returned to the second-stage ultragravity separator to participate in the reaction again, while also carrying away trace amounts of light component impurities. As these impurities accumulate and affect the quality of the finished product, they can be intermittently discharged from the top of the second-stage light phase removal tower to ensure that the content of light component impurities in the finished product meets the requirements.
[0053] Preparation Example 1: The reaction was prepared using the continuous production process described in the above embodiments. The primary reactor catalyst in the primary reactor synthesis system was barium chloride, and the co-catalyst was tri-n-propylamine. The molar ratio of 1,1,1,3-tetrachloro-4,4,4-trifluorobutane, anhydrous hydrogen fluoride, primary reactor catalyst, and primary reactor co-catalyst was 1:10-60:0.02-0.3:0.05-3. The reaction temperature was 100-140℃, and the reaction system pressure was maintained at 1.2-3.5 MPa. The primary reactor discharge separator was maintained at ≤50℃ and 1.2 MPa. The pressure at the top of the primary reactor light removal tower was 0.15-0.4 MPa, and the bottom temperature was 90-120℃. The pressure at the top of the primary reactor product tower was 0-100 kPa, and the top temperature was 35-60℃. The total conversion rate was measured to be 99.99%, the product 1-chloro-1,1,4,4,4-pentafluoro-2-butene contained 99.6 wt%, and the yield was 96%.
[0054] Preparation Example 2: The process employs a continuous production flow to prepare the product. The second-stage reaction synthesis system uses a chromium-based catalyst and concentrated sulfuric acid as the extractant. The molar ratio of 1-chloro-1,1,4,4,4-pentafluoro-2-butene to hydrogen fluoride is 1:3-15. The reaction pressure is 0-1.2 MPa, the reaction temperature is 200-350℃, and the contact time is 20-80 seconds. The single-pass conversion rate is 97%, and the overall conversion rate is 99.99%. The HCl tower top pressure is 0.8-1.0 MPa, -35 to -28℃, with a byproduct HCl content >99.99%; the HF recovery tower top pressure is 0.2-1.4 MPa, 47-90℃; the second-stage reaction light component removal tower top pressure is 0.5-0.8 MPa, 40-57℃; and the second-stage reaction product tower top pressure is 0.4-0.6 MPa, 69-80℃. E-1,1,1,4,4,4-hexafluoro-2-butene product composition ≥99.9wt%, yield 99%.
[0055] It is worth mentioning that: In other preparation examples, the range of first-stage catalysts that can be used includes, but is not limited to, one or more of the chlorides or fluorides of metal M, where metal M is any one of Ti, Ba, Sn, Al, Co, Ni, and Fe; the range of first-stage co-catalysts that can be used includes, but is not limited to, at least one of trimethylamine, tetramethylethylenediamine, diethylamine, triethylamine, propylamine, butylamine, and triethanolamine; and the range of second-stage catalysts that can be used includes, but is not limited to, aluminum fluoride and chromium oxide.
[0056] The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention. Any modifications, equivalent substitutions, improvements, etc., made within the spirit and principles of the present invention should be included within the protection scope of the present invention.
Claims
1. A continuous production system for synthesizing 1-chloro-1,1,4,4,4-pentafluoro-2-butene and E-1,1,1,4,4,4-hexafluoro-2-butene, characterized in that: This includes a single-trans synthesis system for producing 1-chloro-1,1,4,4,4-pentafluoro-2-butene and a two-trans synthesis system for producing E-1,1,1,4,4,4-hexafluoro-2-butene; In this process, at least one connecting branch is constructed between the primary and secondary synthesis systems to allow materials to enter the secondary synthesis system from the primary synthesis system. Hydrogen fluoride and / or 1-chloro-1,1,4,4,4-pentafluoro-2-butene generated from the primary synthesis system can enter the secondary synthesis system through the connecting branch.
2. The continuous production system for synthesizing 1-chloro-1,1,4,4,4-pentafluoro-2-butene and E-1,1,1,4,4,4-hexafluoro-2-butene according to claim 1, characterized in that: The connecting branches include a first branch supplying hydrogen fluoride from the first reaction synthesis system to the second reaction synthesis system, and a second branch supplying 1-chloro-1,1,4,4,4-pentafluoro-2-butene from the first reaction synthesis system to the second reaction synthesis system.
3. A continuous production system for synthesizing 1-chloro-1,1,4,4,4-pentafluoro-2-butene and E-1,1,1,4,4,4-hexafluoro-2-butene according to claim 1 or 2, characterized in that: The first-reaction synthesis system includes a first-reaction reaction system, a first-reaction separation system, and a first-reaction product system; The second reaction synthesis system includes a second reaction system, a second reaction separation system, and a second reaction product system; Among them, at least one third branch is constructed between the first-stage reaction separation system and the second-stage reaction separation system to allow HCL to enter the second-stage reaction separation system from the first-stage reaction separation system.
4. The continuous production system for synthesizing 1-chloro-1,1,4,4,4-pentafluoro-2-butene and E-1,1,1,4,4,4-hexafluoro-2-butene according to claim 3, characterized in that: The primary reaction system includes a primary reaction vaporizer (11), a supergravity reactor (14), a reaction separation tower (15), a primary reaction discharge condenser (18), a primary reaction preheater (12), a reaction circulation vessel (13), a reaction circulation pump (16), and a circulation heater (17). This also includes: The hydrogen fluoride branch is used to transport hydrogen fluoride through the first vaporizer (11) and into the supergravity reactor (14). The primary reactor feedstock branch is used to transport the primary reactor feedstock through the primary reactor preheater (12), the reaction circulation vessel (13), the reaction circulation pump (16), the circulation heater (17) and into the supergravity reactor (15). The first return feed branch is connected between the reaction separation tower (15) and the reaction circulation vessel (13); The second return feed branch is connected between the supergravity reactor (14) and the reaction circulation vessel (13); The first discharge branch is used to transport materials from the supergravity reactor (14) and after passing through the reaction separation tower (15) and the first-reaction discharge condenser (18), they are discharged from the first-reaction system.
5. The continuous production system for synthesizing 1-chloro-1,1,4,4,4-pentafluoro-2-butene and E-1,1,1,4,4,4-hexafluoro-2-butene according to claim 4, characterized in that: The first reactor separation system includes a first reactor discharge separator (19), a first reactor gravity separator (23), a first reactor heavy phase buffer tank (24), a first reactor light phase buffer tank (25), a first reactor light phase circulation pump (56), and a first reactor light phase removal tower (26). Among them, the first reverse discharge separator (19) can receive the material discharged from the first discharge branch, and after separating the material into gas and liquid phases, send the liquid phase material into the first reverse gravity separator (23) and the gas phase material into the second reverse separation system. Also includes: The first reaction light phase branch can send the first reaction light phase material separated from the first reaction supergravity separator (23) into the first reaction light phase buffer tank (25), and then the first reaction light phase circulation pump (56) will transport the first reaction light phase material to the first reaction vaporizer (11) and / or the second reaction system. The first reverse heavy phase branch can transport the first reverse heavy phase material separated from the first reverse ultragravity separator (23) through the first reverse heavy phase buffer tank (24) and the first reverse light phase removal tower (26) in sequence.
6. The continuous production system for synthesizing 1-chloro-1,1,4,4,4-pentafluoro-2-butene and E-1,1,1,4,4,4-hexafluoro-2-butene according to claim 5, characterized in that: The primary reaction finished product system includes a primary reaction finished product tower (30), a primary reaction finished product tower outlet, and a primary reaction high boiling circulating pump (33). The primary reaction product tower (30) can receive the material discharged from the primary reaction light removal tower (26) and collect 1-chloro-1,1,4,4,4-pentafluoro-2-butene at the top of the primary reaction product tower (30) before discharging it from the outlet of the primary reaction product tower; the material in the bottom of the primary reaction product tower (30) is sent back to the reaction circulation vessel (13) through the third return branch.
7. A continuous production system for synthesizing 1-chloro-1,1,4,4,4-pentafluoro-2-butene and E-1,1,1,4,4,4-hexafluoro-2-butene according to claim 5 or 6, characterized in that: The second reaction system includes a second reaction vaporizer (34), a second reaction heat exchanger (35), a second reaction heater (37), a second reaction reactor (37), and a second reaction cooler (38); the second reaction vaporizer (34) is connected to the first reaction light phase branch and the first reaction light phase removal tower (26); This also includes: The secondary reactor feedstock branch is used to transport the secondary reactor feedstock from the secondary reactor vaporizer (34) through the tube side of the secondary reactor heat exchanger (35), the secondary reactor heater (36), the secondary reactor reactor (37), the shell side of the secondary reactor heat exchanger (35), and the secondary reactor cooler (38) before sending it into the secondary reactor separation system.
8. The continuous production system for synthesizing 1-chloro-1,1,4,4,4-pentafluoro-2-butene and E-1,1,1,4,4,4-hexafluoro-2-butene according to claim 7, characterized in that: The second reaction separation system includes an HCl separation tower (20), an HCl tower bottom cooler (55), a second reaction high gravity separator (39), a second reaction heavy phase buffer tank (40), a second reaction heavy phase discharge pump (41), a second reaction light phase buffer tank (42), a second reaction light phase discharge pump (43), an HF recovery tower (44), a second reaction preheater (47), and a second reaction light phase removal tower (48). The HCl separation tower (20) is connected to the feed branch of the second reactor and the discharge separator (19) of the first reactor. The HCl separation tower (20) has an HCl gas outlet. After separating and purifying the HCl in the material, the HCl separation tower (20) sends the mixture to the second reactor gravity separator (39). Also includes: The secondary light phase branch can transport the secondary light phase material separated from the secondary high gravity separator (39) through the secondary light phase buffer tank (42) and the HF recovery tower (44) in sequence. The second-phase heavy phase branch can transport the second-phase heavy phase material separated from the second-phase supergravity separator (39) through the second-phase heavy phase buffer tank (40), the second-phase preheater (47), and the second-phase light phase removal tower (48) in sequence. The third return feed branch is connected between the HF recovery tower (44) and the second vaporizer (34); The fourth return branch connects the HF recovery tower (44) and the second-stage gravity separator (39).
9. A continuous production system for synthesizing 1-chloro-1,1,4,4,4-pentafluoro-2-butene and E-1,1,1,4,4,4-hexafluoro-2-butene according to claim 8, characterized in that: The secondary reaction finished product system includes a secondary reaction finished product tower (51), a secondary reaction finished product outlet, and a secondary reaction high-boiling circulating pump (54). The secondary reactor finished product tower (51) is connected to the secondary reactor light removal tower (48), and also includes a fifth return branch, which can transport the intermediate product in the secondary reactor finished product tower (51) to the secondary reactor vaporizer (34).
10. A continuous production system for synthesizing 1-chloro-1,1,4,4,4-pentafluoro-2-butene and E-1,1,1,4,4,4-hexafluoro-2-butene according to claim 8 or 9, characterized in that: The second-stage desulfurization tower (48) is equipped with an intermittent discharge port for light component impurities.
Citation Information
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