Preparation method and device of high-purity hydrofluoroether HFE374

Abstract

The invention relates to the technical field of preparation of hydrofluoroether, in particular to a preparation method and device of high-purity hydrofluoroether HFE374. The preparation method comprises the following steps: carrying out a reaction on ethanol and TFE at 50-60 DEG C under 0.1-0.2 MPa, and then rectifying to obtain the high-purity hydrofluoroether HFE374. The high-purity hydrofluoroether HFE374 is prepared through the reaction of ethanol and TFE, washing is not needed, the amount of waste water is reduced, and the reaction is simple in process, high in conversion rate and low in reaction temperature, and has outstanding advantages in energy consumption, cost, yield, economical efficiency and environmental protection property.

Description

TECHNICAL FIELD

[0001] The present application relates to the technical field of preparation of hydrofluoroether, in particular to a preparation method and device of high-purity hydrofluoroether HFE374. BACKGROUND

[0002] The high-purity hydrofluoroether HFE374 (chemical name: 1,1,2,2-tetrafluoroethyl ethyl ether) belongs to the hydrofluoroether compound, and has ether bond and fluorine atom in the molecular structure, which endows it with the following core characteristics: 1. environmental friendliness: the ozone depletion potential is 0, the global warming potential is low, and the atmospheric residence time is short, which is an ideal substitute for chlorofluorocarbon; 2. physical and chemical properties: no flash point (non-flammable), low toxicity, low surface tension, and good solubility to polar / non-polar substances; 3. industrial application: widely used in anti-fingerprint agent diluent (such as electronic touch screen coating), precision cleaning agent, refrigerant and lithium battery electrolyte cosolvent.

[0003] The mainstream synthesis route of the hydrofluoroether at present is shown in the Chinese patent for invention with publication number CN105906489A, which is prepared by addition reaction of fluorine-containing alcohol and fluorine-containing olefin, but the production technology means of the process condition is too traditional, the operation condition is very harsh, a large amount of waste salt is generated after the reaction of the solid catalyst, and complex water washing separation is needed, which leads to high cost and environmental pressure, and the boiling point of the solvent is close to the boiling point of the product, which leads to sharp increase of the energy consumption of the rectification and great difficulty in separation. The production technology of the high-purity hydrofluoroether is limited in the prior art, and a relatively perfect preparation method and refining device have not been established for the development of the high-purity hydrofluoroether, which limits the industrialization to some extent, so it is of important practical significance to carry out research on the process preparation method and device of the high-purity hydrofluoroether with simple process. SUMMARY

[0004] The technical problem to be solved by the present application is to provide a preparation method and device of high-purity hydrofluoroether HFE374 with simple process.

[0005] In order to solve the above technical problems, the technical scheme adopted by the present application is as follows: a preparation method of high-purity hydrofluoroether HFE374, comprising the following steps: reacting ethanol and TFE (tetrafluoroethylene) at 50-60℃ and 0.1-0.2MPa, and then rectifying to obtain high-purity hydrofluoroether HFE374.

[0006] Another technical scheme adopted by the present application is a device applied to the preparation method of high-purity hydrofluoroether HFE374, comprising a finished product collecting system, a reaction system, and a monomer collecting system and a rectification system connected with the reaction system respectively, the rectification system is connected with the finished product collecting system, and the monomer collecting system and the reaction system both comprise a blast relief device.

[0007] The application has the beneficial effect that: the application prepares high-purity hydrofluoroether HFE374 by the reaction of ethanol and TFE, without water washing, reducing the amount of waste water, and the reaction process is simple, the conversion rate is high, the reaction temperature is low, and the energy consumption, cost, yield, economy and environmental protection are all outstanding advantages. BRIEF DESCRIPTION OF DRAWINGS

[0008] Figure 1 The structure schematic diagram of the device for preparing high-purity hydrofluoroether HFE37 in the embodiment of the application is shown in the figure. Figure 2 The structure schematic diagram of the reaction system in the embodiment of the application is shown in the figure. Figure 3 The structure schematic diagram of the alcohol feeding system in the embodiment of the application is shown in the figure. Figure 4 The structure schematic diagram of the monomer collecting system in the embodiment of the application is shown in the figure. Figure 5 The structure schematic diagram of the distillation system in the embodiment of the application is shown in the figure. Figure 6 The structure schematic diagram of the finished product collecting system in the embodiment of the application is shown in the figure. Label explanation: 1, reaction system; 11, reaction kettle; 12, second remote pressure transmitter; 13, reaction kettle evacuation cut-off valve; 14, first thermal resistance; 15, reaction kettle steam regulating valve; 16, reaction kettle circulating water regulating valve; 17, remote flow meter; 18, reaction kettle TFE inlet regulating valve; 19, reaction kettle TFE inlet cut-off valve; 2, alcohol feeding system; 21, ethanol metering tank; 22, first remote weighing controller; 23, air breather; 24, ethanol metering tank alcohol inlet cut-off valve; 3, monomer collecting system; 31, TFE buffer tank; 32, first remote pressure transmitter; 33, TFE buffer tank TFE inlet cut-off valve; 4, distillation system; 41, distillation kettle; 42, reflux column; 43, reflux condenser; 44, second thermal resistance; 45, distillation kettle steam regulating valve; 46, third thermal resistance; 47, first cold brine regulating valve; 5, finished product collecting system; 51, finished product tank; 52, second remote weighing controller; 53, fourth thermal resistance; 54, finished product tank feed cut-off valve; 55, second cold brine regulating valve; 6, explosion venting device; 61, explosion state operation display; 62, bursting disc; 63, flame arrester. DETAILED DESCRIPTION

[0009] The technical content, purposes and effects of the application are described in detail below in combination with the embodiments and the drawings.

[0010] The application discloses a preparation method of high-purity hydrogen fluoride ether HFE374, and the method comprises the following steps: reacting ethanol and TFE at 50-60 DEG C and 0.1-0.2 MPa, and then rectifying to obtain high-purity hydrogen fluoride ether HFE374.

[0011] As can be seen from the above description, the preparation method reduces the conventional water washing process, avoids the risk of high COD of water body caused by the raw material ethanol being brought into waste water after water washing in traditional industrial production, and is green and environmentally friendly. The preparation method has the advantages of simple process, high conversion rate, low reaction temperature, and comprehensive advantages in energy consumption, cost, yield, economy and environmental protection.

[0012] Further, the mass ratio of ethanol and TFE is 1:1.8-2.2.

[0013] Further, the rectification temperature is 60-70 DEG C.

[0014] Please refer to Figure 1 Another technical solution adopted by the application is a device applied to the preparation method of high-purity hydrogen fluoride ether HFE374, comprising a finished product collecting system, a reaction system, and a monomer collecting system and a rectification system connected with the reaction system respectively, the rectification system is connected with the finished product collecting system, and the monomer collecting system and the reaction system both comprise a pressure relief device.

[0015] As can be seen from the above description, the preparation of HFE374 product involves tetrafluoroethylene monomer, which is a flammable and explosive material, therefore, the pressure relief device is arranged in the monomer collecting system and the reaction system to further improve the safety in the production process of HFE374. When the pressure of the monomer collecting system and the reaction system reaches the upper limit of the blasting pressure, the blasting state runs in green and makes a sound report to remind the operator to pay attention to the control pressure and immediately respond to the adjustment.

[0016] Please refer to Figure 3 Further, the alcohol feeding system comprises an ethanol metering tank, and a first weighing module, a first remote weighing controller and an ethanol metering tank alcohol feeding cut-off valve which are arranged on the ethanol metering tank in sequence, and an air breather arranged on the ethanol metering tank.

[0017] Further, the control ends of the first weighing module, the first remote weighing controller and the ethanol metering tank alcohol feeding cut-off valve are connected in sequence. The first weighing module transmits the gravity information to the first remote weighing controller, when the first remote weighing controller senses the expected gravity, the signal is transmitted to the control end of the ethanol metering tank alcohol feeding cut-off valve, so that the ethanol metering tank alcohol feeding cut-off valve is opened or closed.

[0018] Further, the first weighing module is arranged at the middle of the bottom of the ethanol metering tank.

[0019] Further, the number of the first weighing module is at least one.

[0020] Further, the ethanol metering tank is provided with an ethanol metering tank feed pipe, and an ethanol metering tank feed cut-off valve is arranged on the ethanol metering tank feed pipe.

[0021] From the above description, it can be known that the ethanol metering tank is arranged in the device, the air breather is arranged on the ethanol metering tank, when the ethanol metering tank is in the alcohol feeding state, the ethanol metering tank alcohol feeding cut-off valve can be opened, after the weight of the ethanol metering tank reaches the expected value, the ethanol metering tank alcohol feeding cut-off valve is automatically closed, the weight of the ethanol metering tank and the alcohol feeding cut-off valve are interlocked to realize automatic control of the weight of ethanol in the ethanol metering tank, at the same time, the weight of the ethanol metering tank is set to be high limit alarm, when the weight of the ethanol metering tank reaches the high limit value, the automatic control system makes corresponding sound indication, reminding the operator that the weight of ethanol has approached the carrying capacity of the ethanol metering tank, to prevent the overflow phenomenon from occurring. Ethanol is a flammable and explosive product, the above device not only ensures safety, but also effectively solves the accurate measurement of the ethanol metering tank.

[0022] Please refer to Figure 4 , further, the monomer collecting system comprises a TFE buffer tank, a first remote pressure transmitter arranged on the TFE buffer tank and a TFE buffer tank TFE cut-off valve, and the first remote pressure transmitter is connected with the control end of the TFE buffer tank TFE cut-off valve. When the first remote pressure transmitter senses the expected pressure, a signal is transmitted to the control end of the TFE buffer tank TFE cut-off valve, so that the TFE cut-off valve is opened or closed.

[0023] Further, the TFE buffer tank is provided with a TFE buffer tank through pipe opening, and the first remote pressure transmitter and the TFE buffer tank through pipe opening are connected by a pressure guide pipe.

[0024] Further, the TFE buffer tank through pipe opening is arranged at the top of the TFE buffer tank.

[0025] From the above description, it can be known that when the TFE buffer tank meets the monomer feeding condition, the TFE buffer tank TFE regulating valve can be opened to supply monomers to the TFE buffer tank, after the monomer pressure in the TFE buffer tank reaches the expected value, the opening degree of the TFE buffer tank TFE regulating valve is automatically adjusted, so that the monomer pressure in the TFE buffer tank is maintained within a certain range, the monomer pressure in the TFE buffer tank and the TFE buffer tank TFE regulating valve are interlocked to realize automatic control of the monomer pressure, so that the monomer pressure in the TFE buffer tank is always maintained within a relatively stable pressure range, the overpressure condition of the monomers in the TFE buffer tank is avoided, on the one hand, the safety of the equipment and personnel is ensured, and on the other hand, raw material guarantee is provided for the subsequent reaction kettle to continuously supply monomers.

[0026] Further, the TFE buffer tank is provided with an explosion relief device on the top.

[0027] Please refer to Figure 2 Further, the reaction system comprises a reaction kettle, a second remote pressure transmitter and a reaction kettle evacuation cut-off valve arranged on the reaction kettle, and the second remote pressure transmitter is connected with the control end of the reaction kettle evacuation cut-off valve. When the second remote pressure transmitter senses the expected pressure, a signal is transmitted to the control end of the reaction kettle evacuation cut-off valve, so that the reaction kettle evacuation cut-off valve is opened or closed.

[0028] Further, the number of the second remote pressure transmitter is two, one of which is connected with the reaction kettle evacuation cut-off valve, and the other is connected with the first remote pressure transmitter.

[0029] Further, a second reaction kettle through port is arranged on the reaction kettle, and the second remote pressure transmitter is connected with the second reaction kettle through port through a pressure guide pipe.

[0030] Further, the second reaction kettle through port is arranged on the top of the reaction kettle.

[0031] From the above description, it can be known that when the reaction kettle reaches the initial temperature and is in the monomer feeding state, the reaction kettle steam regulating valve is closed, the reaction kettle evacuation cut-off valve is opened, and after the pressure in the reaction kettle reaches the expected pressure, the reaction kettle evacuation cut-off valve is automatically closed. The reaction kettle pressure and the reaction kettle evacuation cut-off valve are interlocked to realize the automatic control of the evacuation pressure of the reaction kettle, and the evacuation interlocking avoids the phenomenon of evacuation material running and poor oxygen removal effect of the reaction kettle.

[0032] Further, a first thermal resistance is arranged on the reaction kettle, a reaction kettle jacket is arranged on the outside of the reaction kettle, a steam inlet pipe and a steam outlet pipe are arranged on the reaction kettle jacket, a reaction kettle steam regulating valve is arranged on the steam inlet pipe, and the first thermal resistance is connected with the control end of the reaction kettle steam regulating valve. When the first thermal resistance senses the expected temperature, a signal is transmitted to the control end of the reaction kettle steam regulating valve, so that the opening degree of the reaction kettle steam regulating valve is adjusted.

[0033] Further, a first reaction kettle through port is arranged on the reaction kettle, and the first thermal resistance is connected with the first reaction kettle through port.

[0034] Further, the first reaction kettle through port is arranged on the bottom of the reaction kettle.

[0035] From the above description, when the reaction kettle is heated, the reaction kettle steam regulating valve can be opened to supply steam to the reaction kettle. After the initial temperature in the reaction kettle reaches the expected value, the opening size of the reaction kettle steam regulating valve is automatically adjusted to maintain the initial temperature of the reaction kettle at a certain temperature to meet the monomer feeding conditions. The reaction kettle temperature and the reaction kettle steam regulating valve are interlocked to realize automatic control of the reaction kettle temperature, which greatly solves the temperature hysteresis problem caused by manual operation, avoids the situation that the reaction cannot be triggered due to low initial temperature, and avoids the generation of safety hazards caused by excessive reaction due to high initial temperature.

[0036] Further, the reaction kettle jacket is also provided with a circulating water inlet pipe and a circulating water outlet pipe. The circulating water inlet pipe is provided with a reaction kettle circulating water regulating valve. The first thermal resistance is connected with the control end of the reaction kettle circulating water regulating valve. When the first thermal resistance senses the expected temperature, a signal is transmitted to the control end of the reaction kettle circulating water regulating valve to adjust the opening of the reaction kettle circulating water regulating valve.

[0037] Further, the number of first thermal resistances is two, one of which is connected with the control end of the reaction kettle steam regulating valve, and the other is connected with the control end of the reaction kettle circulating water regulating valve.

[0038] From the above description, when the reaction kettle is supplied with TFE monomer, the temperature of the reaction kettle can be observed to slowly rise at the beginning of the reaction to determine that the reaction has started. The reaction kettle circulating water regulating valve can be opened to supply circulating water to the reaction kettle. After the temperature in the reaction kettle stabilizes, the opening size of the reaction kettle circulating water regulating valve is automatically adjusted to maintain the temperature of the reaction kettle at a certain temperature, continuously supply TFE monomer for reaction, and realize automatic control of the temperature of the reaction kettle through interlocking of the reaction kettle temperature and the reaction kettle circulating water regulating valve. The use of circulating water temperature control can solve the disadvantages of manual temperature control during the reaction. On the one hand, delayed opening can cause the reaction kettle to overheat and overpressure, bringing uncontrollable safety hazards. On the other hand, delayed closing can cause the reaction kettle to overcool, thereby causing abnormal phenomena such as premature termination of the reaction.

[0039] Further, the reaction kettle is also provided with a reaction kettle evacuation pipe, and the reaction kettle evacuation pipe is provided with a reaction kettle evacuation shut-off valve.

[0040] Further, the reaction kettle is also provided with a reaction kettle feed pipe connected with the monomer collecting system; a remote flow meter, a reaction kettle TFE inlet adjusting valve and a reaction kettle TFE inlet cut-off valve are arranged on the reaction kettle feed pipe, and the remote flow meter is connected with the control end of the reaction kettle TFE inlet adjusting valve and the control end of the reaction kettle TFE inlet cut-off valve. When the remote flow meter senses a predicted pressure, a signal is transmitted to the control end of the reaction kettle TFE inlet adjusting valve to control the opening degree of the reaction kettle TFE inlet adjusting valve; when the remote flow meter senses another predicted pressure, a signal is transmitted to the control end of the reaction kettle TFE inlet cut-off valve to control the opening or closing of the reaction kettle TFE inlet cut-off valve.

[0041] As can be known from the above description, the reaction kettle TFE inlet adjusting valve is opened to start supplying monomers to the reaction kettle, and after the monomer pressure in the reaction kettle reaches the predicted pressure, the opening degree of the reaction kettle TFE inlet adjusting valve is automatically adjusted to maintain the monomer pressure in the reaction kettle within a certain range. The reaction kettle pressure and the reaction kettle TFE inlet adjusting valve are interlocked to realize automatic control of the reaction kettle TFE inlet pressure. The TFE interlocking solves the problem of manual pressure deviation, reduces the labor intensity, ensures the timeliness of the reaction kettle monomer supply and the stability of the reaction kettle pressure, avoids affecting the product quality, and reminds the operator when the reaction kettle TFE inlet pressure reaches the upper limit value to prevent overpressure and other abnormal phenomena from causing certain degree of safety hazards. The differential pressure interlocking between the TFE buffer tank pressure and the reaction kettle pressure can always ensure that the TFE buffer tank pressure is higher than the reaction kettle pressure within a certain range, prevent the material in the reaction kettle from flowing back to the TFE buffer tank to cause danger, and further ensure the safety of the equipment and personnel.

[0042] In the later stage of the reaction, the reaction kettle TFE inlet cut-off valve is automatically closed when the cumulative value of the reaction kettle TFE inlet flow meter reaches a certain amount, the reaction kettle TFE inlet flow and the reaction kettle TFE inlet cut-off valve are interlocked to realize automatic control of the reaction kettle TFE inlet cumulative value, the time of reaction termination can be predicted in advance, the consumption of raw materials caused by excessive TFE monomers in the later stage is avoided, and the production cost is effectively reduced.

[0043] Further, the top of the reaction kettle is provided with a pressure relief device.

[0044] Further, the pressure relief device comprises a bursting process pipeline, and a bursting state operation display, a bursting disc and a flame arrester arranged in the bursting process pipeline from bottom to top.

[0045] Further, the bursting state operation display is detachably connected with the bursting process pipeline, the bursting disc is connected with the bursting process pipeline by a clamp holder, and the flame arrester is connected with the bursting process pipeline by a flange; From the above description, the explosion vent device is arranged at the top of the TFE buffer tank and the reaction kettle, when the pressure of the TFE buffer tank and the reaction kettle reaches the upper limit of the burst pressure, the rupture disc breaks, and the pressure in the TFE buffer tank and the reaction kettle is released, thereby fundamentally avoiding the overpressure abnormal phenomenon of the TFE buffer tank and the reaction kettle.

[0046] Please refer to Figure 5 Further, the rectification system comprises a rectification kettle and a second thermal resistance arranged on the rectification kettle; a rectification kettle jacket is arranged outside the rectification kettle, the rectification kettle jacket is provided with a steam inlet pipe and a steam outlet pipe, a rectification kettle steam regulating valve is arranged on the steam inlet pipe, and the second thermal resistance is connected with the control end of the rectification kettle steam regulating valve. When the second thermal resistance senses the expected temperature, a signal is transmitted to the control end of the rectification kettle steam regulating valve, so that the opening degree of the rectification kettle steam regulating valve is adjusted.

[0047] Further, a rectification kettle through pipe opening is arranged on the rectification kettle, and the second thermal resistance is connected with the rectification kettle through pipe opening.

[0048] Further, the rectification kettle through pipe opening is arranged at the kettle bottom of the rectification kettle.

[0049] From the above description, after the reaction is completed and the rectification kettle meets the rectification product conditions, the reaction liquid in the reaction kettle is completely discharged into the rectification kettle, the cold brine regulating valve of the reflux condenser is opened to supply cold brine to the reflux condenser, the rectification kettle steam regulating valve is opened to supply steam to the rectification kettle, the opening degree of the rectification kettle steam regulating valve is automatically adjusted after the temperature of the material in the rectification kettle reaches the expected value, so that the temperature of the rectification kettle is maintained within a certain temperature range, the temperature of the rectification kettle and the rectification kettle steam regulating valve are interlocked to realize automatic control of the temperature of the rectification kettle, and the overhigh kettle temperature is prevented from causing ethanol to be evaporated and introduced into the next process, so that a water washing process needs to be additionally arranged, an environmental protection problem of overhigh COD of the water washing liquid is caused, and the water washing process greatly increases fuel consumption and labor cost.

[0050] Further, the rectification system further comprises a reflux condenser, a third thermal resistance, a first cold brine inlet pipe and a first cold brine outlet pipe are arranged on the reflux condenser, a first cold brine regulating valve is arranged on the first cold brine inlet pipe, and the third thermal resistance is connected with the control end of the first cold brine regulating valve. When the third thermal resistance senses the expected temperature, a signal is transmitted to the control end of the first cold brine regulating valve, so that the opening degree of the first cold brine regulating valve is controlled.

[0051] Further, a reflux condenser through pipe opening is arranged on the reflux condenser, and the third thermal resistance is connected with the reflux condenser through pipe opening.

[0052] From the above description, after the outlet temperature of the reflux condenser reaches the expected value, the opening size of the cold salt water regulating valve of the reflux condenser is automatically adjusted, so that the high-purity hydrofluoroether HFE374 is completely condensed and collected, thereby realizing the rectification separation; the outlet temperature of the reflux condenser is interlocked with the cold salt water regulating valve of the reflux condenser, so as to realize the automatic control of the outlet temperature of the reflux condenser; the cold salt water is interlocked and controlled, and since the high-purity hydrofluoroether HFE374 is a highly volatile product, the control of the amount of cold salt water can prevent the volatilization loss of the product HFE374, thereby effectively improving the yield of the product high-purity hydrofluoroether HFE374.

[0053] Further, the rectification system further comprises a reflux tower, and the rectification kettle, the reflux tower and the reflux condenser are sequentially connected.

[0054] Please refer to Figure 6 Further, the product collection system comprises a product tank, and a second weighing module, a second remote weighing controller and a product tank feed cut-off valve are sequentially connected on the product tank.

[0055] The control ends of the second weighing module, the second remote weighing controller and the product tank feed cut-off valve are sequentially connected. The second weighing module transmits the gravity information to the second remote weighing controller, and when the second remote weighing controller senses the expected gravity, a signal is transmitted to the control end of the product tank feed cut-off valve, so that the product tank feed cut-off valve is opened or closed.

[0056] From the above description, the product tank feed cut-off valve is opened, and the continuous collection of the high-purity hydrofluoroether HFE374 into the product tank is started. After the weight of the product tank reaches the expected value, the product tank feed cut-off valve is automatically closed. The weight of the product tank is interlocked with the product tank feed cut-off valve, so as to realize the automatic control of the weight of the product tank. The HFE374 product in the product tank is filled, the product tank feed cut-off valve is continuously opened, and after the sight glass does not collect any material, it is considered that the rectification is completed, and the remaining HFE374 product in the product tank is filled.

[0057] Further, the second weighing module is arranged at the middle of the bottom of the product tank.

[0058] Further, the number of the second weighing module is at least one.

[0059] Further, a product tank feed pipe is arranged on the product tank, the product tank feed pipe is communicated with the rectification system, and the product tank feed cut-off valve is arranged on the product tank feed pipe.

[0060] Further, a product tank jacket is arranged on the outside of the product tank, a second cold salt water inlet pipe and a second cold salt water outlet pipe are arranged on the product tank jacket, and a second cold salt water regulating valve is arranged on the second cold salt water inlet pipe.

[0061] Further, a fourth thermal resistance is arranged on the product tank, and the control end of the second cold brine regulating valve is connected with the fourth thermal resistance.

[0062] Further, a product tank through port is arranged on the product tank, and the fourth thermal resistance is connected with the product tank through port.

[0063] From the above description, it can be seen that the product tank is in a material receiving state, the product tank jacket cold brine regulating valve can be opened to supply cold brine to the product tank, and after the temperature in the product tank reaches the expected temperature, the opening degree of the product tank cold brine regulating valve is automatically adjusted, so that the temperature in the product tank is maintained within a certain range, and the product tank temperature and the product tank cold brine regulating valve are interlocked to realize automatic control of the product tank temperature. The addition of the product tank cold brine can realize secondary condensation of the product in the production process, avoid process loss caused by volatilization of the product, and prevent the phenomenon of yield loss and increased product unit consumption caused by excessive material receiving of the product tank.

[0064] Embodiment one of the present application is a preparation method of high-purity hydrofluoroether HFE374, which comprises the following steps: reacting ethanol and TFE with a mass ratio of 1:2 at 50-60 DEG C and 0.1-0.2 MPa, and then performing rectification at 60-70 DEG C to obtain high-purity hydrofluoroether HFE374.

[0065] Please refer to Figures 1-6 Embodiment two of the present application is a device applied to preparation of high-purity hydrofluoroether HFE374, which comprises a reaction system 1, and a alcohol feeding system 2, a monomer collecting system 3 and a rectification system 4 connected with the reaction system 1 respectively, and the rectification system 4 is connected with a product collecting system 5.

[0066] The alcohol feeding system 2 comprises an ethanol metering tank 21, and a first weighing module, a first remote weighing controller 22, an air respirator 23 and an ethanol metering tank feeding pipe arranged on the ethanol metering tank 21; the first weighing module is arranged in the middle of the bottom of the ethanol metering tank 21, and the number of the first weighing modules is four; an ethanol metering tank alcohol feeding cut-off valve 24 is arranged on the ethanol metering tank feeding pipe, and the control ends of the first weighing module, the first remote weighing controller 22 and the ethanol metering tank alcohol feeding cut-off valve 24 are connected in sequence.

[0067] The monomer collecting system 3 comprises a TFE buffer tank 31, a first remote pressure transmitter 32 and a TFE buffer tank inlet TFE cut-off valve 33 arranged on the TFE buffer tank 31, the first remote pressure transmitter 32 being connected with the control end of the TFE buffer tank inlet TFE cut-off valve 33; a TFE buffer tank venting port is arranged on the top of the TFE buffer tank 31, and the first remote pressure transmitter 32 is connected with the TFE buffer tank venting port through a pressure guide pipe.

[0068] The reaction system 1 comprises a reaction kettle 11, two second remote pressure transmitters 12, a reaction kettle evacuation cut-off valve 13, two first thermal resistors 14, a reaction kettle evacuation pipe and a reaction kettle feeding pipe arranged on the reaction kettle 11, the reaction kettle feeding pipe being communicated with the alcohol feeding system 2 and the monomer collecting system 3, one of the second remote pressure transmitters 12 being connected with the reaction kettle evacuation cut-off valve 13, and the other second remote pressure transmitter 12 being connected with the first remote pressure transmitter 32; a second reaction kettle venting port is arranged on the top of the reaction kettle 11, and a first reaction kettle venting port is arranged on the bottom of the reaction kettle 11, the first thermal resistor 14 being threadedly connected with the first reaction kettle venting port, and the second remote pressure transmitter 12 being connected with the second reaction kettle venting port through a pressure guide pipe. A reaction kettle jacket is arranged outside the reaction kettle 11, and a steam inlet pipe, a steam outlet pipe, a circulating water inlet pipe and a circulating water outlet pipe are arranged on the reaction kettle jacket, the steam inlet pipe being provided with a reaction kettle steam regulating valve 15, one of the first thermal resistors 14 being connected with the control end of the reaction kettle steam regulating valve 15, the circulating water inlet pipe being provided with a reaction kettle circulating water regulating valve 16, the other first thermal resistor 14 being connected with the control end of the reaction kettle circulating water regulating valve 16, and the reaction kettle evacuation cut-off valve 13 being arranged on the reaction kettle evacuation pipe; the reaction kettle feeding pipe is connected with the monomer collecting system 3, and a remote flow meter 17, a reaction kettle inlet TFE regulating valve 18 and a reaction kettle inlet TFE cut-off valve 19 are arranged on the reaction kettle feeding pipe, the remote flow meter 17 being connected with the control ends of the reaction kettle inlet TFE regulating valve 18 and the reaction kettle inlet TFE cut-off valve 19, and the reaction kettle feeding pipe being flange-connected with the remote flow meter 17.

[0069] The rectification system 4 comprises a rectification kettle 41, a reflux tower 42 and a reflux condenser 43 which are sequentially communicated, and a second thermal resistor 44 arranged on the rectification kettle 41; a kettle bottom of the rectification kettle 41 is provided with a rectification kettle through pipe, and the second thermal resistor 44 is threadedly connected with the rectification kettle through pipe; a rectification kettle jacket is arranged outside the rectification kettle 41, the rectification kettle jacket is provided with a steam inlet pipe and a steam outlet pipe, a rectification kettle steam adjusting valve 45 is arranged on the steam inlet pipe, and the second thermal resistor 44 is connected with a control end of the rectification kettle steam adjusting valve 45; the reflux condenser 43 is provided with a third thermal resistor 46, a first cold salt water inlet pipe and a first cold salt water outlet pipe, a first cold salt water adjusting valve 47 is arranged on the first cold salt water inlet pipe, and the third thermal resistor 46 is connected with a control end of the first cold salt water adjusting valve 47; the reflux condenser 43 is provided with a reflux condenser through pipe, and the third thermal resistor 46 is threadedly connected with the reflux condenser through pipe.

[0070] The finished product collecting system 5 comprises a finished product tank 51, and a finished product tank feed pipe, a second weighing module, a second remote weighing controller 52 and a fourth thermal resistor 53 which are arranged on the finished product tank 51; the second weighing module is arranged at the middle of the bottom of the finished product tank 51, and the number of the second weighing module is four; the finished product tank feed pipe is communicated with the rectification system 4, a finished product tank feed cut-off valve 54 is arranged on the finished product tank feed pipe, and the second weighing module, the second remote weighing controller 52 and the control end of the finished product tank feed cut-off valve 54 are sequentially connected. The finished product tank 51 is provided with a finished product tank jacket outside, the finished product tank jacket is provided with a second cold salt water inlet pipe and a second cold salt water outlet pipe, a second cold salt water adjusting valve 55 is arranged on the second cold salt water inlet pipe, the fourth thermal resistor 53 is connected with a control end of the second cold salt water adjusting valve 55; the finished product tank 51 is provided with a finished product tank through pipe, and the fourth thermal resistor 53 is threadedly connected with the finished product tank through pipe.

[0071] The top of the TFE buffer tank 31 and the top of the reaction kettle 11 are both provided with a blast device 6, the blast device 6 comprises a blast process pipeline, and a blast state operation display 61, a burst disc 62 and a flame arrester 63 which are sequentially arranged from bottom to top in the blast process pipeline; the blast state operation display 61 is threadedly connected with the blast process pipeline, the burst disc 62 is connected with the blast process pipeline by using a clamp holder, and the flame arrester 63 is connected with the blast process pipeline by using a flange; Embodiment three of the present application is that the device of embodiment two is used to prepare high-purity hydrofluoroether HFE374, and the steps are as follows: S1: open the ethanol metering tank 21 in the alcohol state, open the ethanol metering tank alcohol inlet cut-off valve 24, after the ethanol metering tank 21 weight reaches 1500Kg, the ethanol metering tank alcohol inlet cut-off valve 24 is automatically closed, the ethanol metering tank 21 weight and the alcohol inlet cut-off valve interlock to realize the automatic control of the ethanol weight in the ethanol metering tank 21, and the high limit alarm is set for the ethanol metering tank 21 weight, when the ethanol metering tank 21 weight reaches the high limit value, the automatic control system gives corresponding sound indication to remind the operator that the ethanol weight has approached the carrying capacity of the ethanol metering tank 21, to prevent the overflow phenomenon.

[0072] Open the TFE buffer tank 31 TFE regulating valve, supply monomer to the TFE buffer tank 31, after the monomer pressure in the TFE buffer tank 31 reaches 0.6MPa, automatically adjust the opening size of the TFE buffer tank 31 TFE regulating valve, so that the monomer pressure in the TFE buffer tank 31 is maintained at 0.6~0.7MPa, the monomer pressure in the TFE buffer tank 31 and the TFE buffer tank 31 TFE regulating valve interlock to realize the automatic control of the monomer pressure, to ensure that the monomer pressure in the TFE buffer tank 31 is always maintained in a relatively stable pressure range.

[0073] Open the reaction kettle steam regulating valve 15, supply steam to the reaction kettle 11, after the initial temperature in the reaction kettle 11 reaches 40℃, automatically adjust the opening size of the reaction kettle steam regulating valve 15, so that the initial temperature of the reaction kettle 11 is maintained at 40~50℃, to meet the monomer feeding conditions.

[0074] S2: after the reaction kettle 11 reaches the initial temperature, close the reaction kettle steam regulating valve 15, and open the reaction kettle evacuation cut-off valve 13, after the pressure in the reaction kettle 11 reaches-0.090MPa, automatically close the reaction kettle evacuation cut-off valve 13.

[0075] S3: open the reaction kettle TFE regulating valve 18, start to supply monomer to the reaction kettle 11, after the monomer pressure in the reaction kettle 11 reaches 0.1MPa, automatically adjust the opening size of the reaction kettle TFE regulating valve 18, so that the monomer pressure in the reaction kettle 11 is maintained at 0.1~0.2MPa; After the reaction kettle 11 is connected with TFE monomer, observe the slow temperature rise of the reaction kettle 11 to determine that the reaction phenomenon begins, open the reaction kettle circulating water regulating valve 16 to supply circulating water to the reaction kettle 11, after the temperature in the reaction kettle 11 stabilizes, automatically adjust the opening size of the reaction kettle circulating water regulating valve 16, so that the temperature of the reaction kettle 11 is maintained at 50~60℃, and the TFE monomer is continuously and automatically supplied for reaction; When the cumulative value of the reaction kettle 11 TFE flow meter reaches 3000Kg, the reaction kettle TFE cut-off valve 19 is automatically closed; The explosion relief device 6 is arranged on the top of the TFE buffer tank 31 and the reaction kettle 11, when the pressure of the TFE buffer tank 31 and the reaction kettle 11 reaches the upper limit of the explosion pressure, the rupture disc 62 breaks, and the pressure in the TFE buffer tank 31 and the reaction kettle 11 is released, so that the overpressure abnormality of the TFE buffer tank 31 and the reaction kettle 11 is fundamentally avoided.

[0076] S4: After the reaction is completed, the reaction liquid in the reaction kettle 11 is discharged into the rectification kettle 41, the cold salt water adjusting valve of the reflux condenser 43 is opened, -15 DEG C cold salt water is supplied to the reflux condenser 43, the rectification kettle steam adjusting valve 45 is opened, steam is supplied to the rectification kettle 41, and after the temperature of the material in the rectification kettle 41 reaches 60 DEG C, the opening degree of the rectification kettle steam adjusting valve 45 is automatically adjusted, so that the temperature of the rectification kettle 41 is maintained at 60-70 DEG C. After the temperature of the outlet of the reflux condenser 43 reaches 40 DEG C, the opening degree of the cold salt water adjusting valve of the reflux condenser 43 is automatically adjusted, so that the high-purity hydrofluoroether HFE374 is completely condensed and collected, and the rectification separation is realized.

[0077] S5: The product tank feed cut-off valve 54 is opened, and the high-purity hydrofluoroether HFE374 is continuously collected into the product tank 51. After the weight of the product tank 51 reaches 2500 Kg, the product tank feed cut-off valve 54 is automatically closed. The weight of the product tank 51 is interlocked with the product tank feed cut-off valve 54 to realize automatic control of the weight of the product tank 51. The HFE374 product in the product tank 51 is filled. The product tank feed cut-off valve 54 is continuously opened. After the sight glass does not collect material, it is considered that the rectification is completed, and the remaining HFE374 product in the product tank 51 is filled. The product tank 51 is in a material collecting state, the product tank jacket cold salt water adjusting valve is opened, -15 DEG C cold salt water is supplied to the product tank 51, after the temperature of the product tank 51 reaches 10 DEG C, the opening degree of the product tank 51 cold salt water adjusting valve is automatically adjusted, so that the temperature of the product tank 51 is maintained at 10-20 DEG C, and the temperature of the product tank 51 is interlocked with the product tank 51 cold salt water adjusting valve to realize automatic control of the temperature of the product tank 51.

[0078] In summary, the preparation method and device of the high-purity hydrofluoroether HFE374 have the following advantages: (1) The preparation method and application device reduce the water washing process, and the process route is green and environmentally friendly.

[0079] (2) The preparation method has simple process, high conversion rate, low reaction temperature and low cost.

[0080] (3) The device is provided with two sets of explosion relief devices, which can improve the safety in the production process of HFE374.

[0081] (4) The device of the present application is provided with automatic alcohol feeding cut-off interlocking, single body material collecting regulation interlocking, initial temperature rising regulation interlocking, reaction evacuation cut-off interlocking, reaction feed regulation interlocking, reaction temperature control regulation interlocking, reaction termination cut-off interlocking, rectification temperature rising regulation interlocking, rectification condensation regulation interlocking, collection cold preservation regulation interlocking, product tapping cut-off interlocking, which can further improve the safety in the production process of HFE374, reduce the volatile loss of HFE374 product, and improve the conversion rate and yield of raw materials.

[0082] The above description is only an embodiment of the present application, and does not limit the patent scope of the present application, and any equivalent transformation or direct or indirect application in the related technical field by using the content of the present application specification and drawings is also included in the patent protection scope of the present application.

Claims

1. A method for producing high purity hydrofluoroether HFE 374, characterized by, The method comprises the following steps: reacting ethanol and TFE at 50-60 DEG C and 0.1-0.2 MPa, and then rectifying to obtain high-purity HFE374.

2. The method of producing high purity hydrofluoroether HFE 374 according to claim 1, characterized by, The mass ratio of the ethanol and TFE is 1:1.8-2.

2.

3. The method for preparing high-purity hydrofluoroether HFE374 according to claim 1, characterized in that, The rectifying temperature is 60-70 DEG C.

4. An apparatus for use in the process for the production of high purity hydrofluoroether HFE 374 according to any one of claims 1 to 3, characterized in that The system comprises a product collection system, a reaction system, an alcohol feeding system connected with the reaction system, a monomer collection system and a rectifying system connected with the reaction system, wherein the rectifying system is connected with the product collection system, and the monomer collection system and the reaction system each comprises an explosion relief device.

5. The apparatus of claim 4, wherein, The alcohol feeding system comprises an ethanol metering tank, a first weighing module, a first remote weighing controller and an ethanol metering tank alcohol feeding cut-off valve connected in sequence on the ethanol metering tank, and an air breather arranged on the ethanol metering tank.

6. The apparatus of claim 4, wherein, The monomer collection system comprises a TFE buffer tank, a first remote pressure transmitter and a TFE buffer tank TFE feeding cut-off valve arranged on the TFE buffer tank, wherein the first remote pressure transmitter is connected with the control end of the TFE buffer tank TFE feeding cut-off valve.

7. The apparatus of claim 4, wherein, The reaction system comprises a reaction kettle, a second remote pressure transmitter and a reaction kettle evacuation cut-off valve arranged on the reaction kettle, wherein the second remote pressure transmitter is connected with the control end of the reaction kettle evacuation cut-off valve.

8. The apparatus of claim 7, wherein, The reaction kettle is further provided with a reaction kettle feeding pipe connected with the monomer collection system, and a remote flow meter, a reaction kettle TFE feeding regulating valve and a reaction kettle TFE feeding cut-off valve arranged on the reaction kettle feeding pipe, wherein the remote flow meter is connected with the control end of the reaction kettle TFE feeding regulating valve and the control end of the reaction kettle TFE feeding cut-off valve.

9. The apparatus of claim 7, wherein, The reaction kettle is provided with a first thermal resistor, and the reaction kettle is provided with a reaction kettle jacket outside, a steam inlet pipe and a steam outlet pipe arranged on the reaction kettle jacket, and a reaction kettle steam regulating valve arranged on the steam inlet pipe, wherein the first thermal resistor is connected with the control end of the reaction kettle steam regulating valve.

10. The apparatus of claim 4, wherein, The rectifying system comprises a rectifying kettle and a second thermal resistor arranged on the rectifying kettle, and the rectifying kettle is provided with a rectifying kettle jacket outside, a steam inlet pipe and a steam outlet pipe arranged on the rectifying kettle jacket, and a rectifying kettle steam regulating valve arranged on the steam inlet pipe, wherein the second thermal resistor is connected with the control end of the rectifying kettle steam regulating valve.

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