Device and method for producing ethyl methyl carbonate using impinging flow transesterification tubular reactor
By using an impact flow transesterification tube reactor in the preparation process of methyl ethyl carbonate, a high-speed jet impact chamber is used to form a turbulent zone, which solves the problems of low heat transfer and mass transfer efficiency, and achieves high-efficiency and low-energy consumption carbonic acid methyl ethyl ester preparation meets the needs of industrial production and improves product quality and automation.
Patent Information
- Application Number
- CN202211287428.X
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2022-10-20
- Publication Date
- 2024-12-20
- Estimated Expiration
- 2042-10-20
AI Technical Summary
In the existing preparation process of methyl ethyl carbonate, the heat transfer and mass transfer efficiency are low, the reaction cycle is long, and the energy consumption is high, resulting in an increase in costs, making it difficult to meet the needs of industrial production.
Impact flow transesterification tube reactor is used to form a highly turbulent impact zone through the Laval nozzle and the high-speed jet impact chamber, improving the mixing and mass transfer effect in the reactor, and improving the reaction rate and product yield. The device includes a batching tank, impact flow transesterification tube reactor, post-transesterification tower system, delight component tower system and methyl ethyl carbonate distillation tower system, using components such as power fluid pumps, heaters and gas-liquid couplers. , realize transesterification reaction and separation.
It shortens the reaction time, saves energy, improves production efficiency, and the quality of the prepared methyl ethyl carbonate is higher than the industrial standard, has mature processes, advanced equipment, high degree of automation, and is environmentally friendly.
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Figure CN115554720B_ABST
Abstract
Description
Technical Field
[0001] The invention belongs to the technical field of chemical industry, and particularly relates to a device and a method for producing ethyl methyl carbonate by using an impinging flow transesterification tubular reactor. Background Art
[0002] Ethyl methyl carbonate (EMC) is known as a green chemical. Its molecular formula is C 4 H 8 O 3 , unique molecular structure (C 2 H 5 O-CO-OCH 3 ), is an organic carbonate compound with an asymmetric molecular structure. EMC molecules contain multiple active groups at the same time, and their chemical properties are very active, and they have broad application prospects in many fields. Due to its low viscosity, high dielectric constant, and strong solubility in lithium salts, ethyl methyl carbonate is an excellent electrolyte solvent for lithium-ion batteries, which can improve the energy density and discharge capacity of the battery, and can also improve the safety performance and service life of the battery.
[0003] The industrial production method of ethyl methyl carbonate generally adopts phosgene method, carbonyl oxidation method, transesterification method, etc. In the presence of a catalyst, dimethyl carbonate and ethanol or diethyl carbonate undergo transesterification to produce ethyl methyl carbonate. The transesterification method for producing ethyl methyl carbonate has the advantages of low raw material toxicity, low pollution, simple process, and mild reaction conditions. However, the transesterification method for producing ethyl methyl carbonate also has outstanding problems such as large catalyst dosage, low raw material conversion rate, and long reaction time. The reason is that the preparation process of ethyl methyl carbonate generally adopts a mechanically stirred tank reactor or a tower reactor. The disadvantages of these preparation equipments are low heat and mass transfer efficiency, long reaction cycle, high energy consumption, and increased energy consumption leads to rising costs, which is not conducive to industrial production.
[0004] The art is eager to find a low-energy consumption, environmentally friendly process and equipment for preparing ethyl methyl carbonate, which can overcome the above technical problems. Summary of the invention
[0005] The present invention provides an apparatus and method for producing ethyl methyl carbonate using an impinging flow transesterification tubular reactor, aiming to overcome the problems of low heat and mass transfer efficiency, long reaction cycle and high energy consumption in the above-mentioned existing preparation equipment and methods.
[0006] To achieve the above object, the present invention adopts the following technical solutions:
[0007] A device for producing ethyl methyl carbonate using an impinging flow transesterification tubular reactor, the device comprising a batching tank, an impinging flow transesterification tubular reactor, a post-esterification tower system, a light component removal tower system, and an ethyl methyl carbonate distillation tower system connected in sequence; the batching tank is also directly connected to the post-esterification tower system, the light component removal tower system, and the ethyl methyl carbonate distillation tower system;
[0008] The impinging flow transesterification tubular reactor comprises a power fluid pump, a Laval nozzle, a high-speed jet impact chamber, a gas-liquid coupler, a tubular reactor, a heater, and an ethanol vaporizer; the Laval nozzle, the high-speed jet impact chamber, the gas-liquid coupler, and the tubular reactor are all arranged inside the heater; the ends of the two Laval nozzles facing each other are fixedly connected with the gas-liquid coupler, and the pipe mouth of the gas-liquid coupler is connected with the outlet end of the ethanol vaporizer; the two Laval nozzles are arranged opposite to each other and connected, and the cavity formed at the middle connecting part is a mixing chamber, the middle part of the mixing chamber is connected to the high-speed jet impact chamber in the vertical direction, the high-speed jet impact chamber is connected to one end of the tubular reactor, and the other end of the tubular reactor is connected to the liquid inlet in the middle of the rear transesterification tower.
[0009] Furthermore, the batching tank is a tank structure with a heating jacket arranged on the outer circumference and a mechanical agitator arranged inside. A liquid inlet is opened on the top of the batching tank, and the liquid inlet is connected to the methanol-dimethyl ester azeotrope pump of the rear ester exchange tower. The liquid outlet at the bottom of the batching tank is connected to the inlet end of the power fluid pump, and the outlet end of the power fluid pump is connected to the liquid inlet end of the gas-liquid coupler of the impact flow ester exchange tubular reactor.
[0010] Furthermore, the post-ester exchange tower system consists of a post-ester exchange tower, a post-ester exchange tower reboiler, a post-ester exchange tower plate-type tower plate, a post-ester exchange tower white steel structured packing, a post-ester exchange tower condenser, a methanol-dimethyl ester azeotrope receiving tank, a methanol-dimethyl ester azeotrope pump, a post-ester exchange tower bottom pump, and a catalyst filter; the post-ester exchange tower is a tower structure with a post-ester exchange tower plate-type tower plate at the bottom and a post-ester exchange tower white steel structured packing at the top, the tubular reactor is connected to the post-ester exchange tower, and the top of the post-ester exchange tower is connected to the post-ester exchange tower in sequence. The exchange tower condenser, the methanol-dimethyl ester azeotrope receiving tank and the inlet of the methanol-dimethyl ester azeotrope pump, and the outlet of the methanol-dimethyl ester azeotrope pump are respectively connected to the rear ester exchange tower, the feed inlet at the top of the batching tank and the methanol recovery system; the bottom end of the rear ester exchange tower is respectively connected to the inlet ends of the rear ester exchange tower reboiler and the catalyst filter through the rear ester exchange tower bottom pump, the outlet end of the rear ester exchange tower reboiler is connected to the rear ester exchange tower, and the outlet end of the catalyst filter is respectively connected to the light component removal tower and the catalyst recovery system of the light component removal tower system.
[0011] Furthermore, the light component removal tower system is composed of a light component removal tower, a light component removal tower reboiler, a light component removal tower white steel structured packing, a light component removal tower condenser, a light component receiving tank, a light component pump, and a light component removal tower bottom pump; the light component removal tower is provided with a light component removal tower white steel structured packing, the top of the light component removal tower is sequentially connected to the light component removal tower condenser, the light component receiving tank, and the light component pump, and the light component pump outlet end is respectively connected to the light component removal tower and the batching tank; the bottom end of the light component removal tower is connected to the light component removal tower bottom pump, the light component removal tower bottom pump is respectively connected to the light component removal tower reboiler and the methyl ethyl carbonate distillation tower of the methyl ethyl carbonate distillation tower system, and the light component removal tower reboiler is then connected to the light component removal tower.
[0012] Furthermore, the ethyl methyl carbonate distillation tower system consists of an ethyl methyl carbonate distillation tower, a distillation tower reboiler, a distillation tower condenser, an ethyl methyl carbonate receiving tank, an ethyl methyl carbonate pump, an ethyl methyl carbonate storage tank, and a bottom pump of the ethyl methyl carbonate distillation tower; the ethyl methyl carbonate distillation tower is provided with a white steel structured packing of the distillation tower; the top of the ethyl methyl carbonate distillation tower is connected with the distillation tower condenser, the ethyl methyl carbonate receiving tank, and the ethyl methyl carbonate pump in sequence, and the ethyl methyl carbonate pump is respectively connected with the ethyl methyl carbonate distillation tower and the ethyl methyl carbonate storage tank; the bottom end of the ethyl methyl carbonate distillation tower is connected with the bottom pump of the ethyl methyl carbonate distillation tower, and the bottom pump of the ethyl methyl carbonate distillation tower is respectively connected with the distillation tower reboiler and the batching tank, and the distillation tower reboiler is further connected with the ethyl methyl carbonate distillation tower.
[0013] Furthermore, the tubular reactor is a tube with a length-to-diameter ratio greater than 1000, a tube diameter of Φ75 mm or Φ100 mm, and is configured as a reciprocating type or a spring type.
[0014] A method for producing ethyl methyl carbonate using an impinging flow transesterification tubular reactor, comprising the steps of:
[0015] (1) The raw material dimethyl carbonate, catalyst and recycled materials enter the batching tank, and the raw materials are mixed evenly under the action of a mechanical stirrer to obtain a mixed liquid; the mixed liquid reaches the reaction temperature under the heating of a heat medium, and enters the impinging flow transesterification tubular reactor through a power fluid pump;
[0016] (2) The mixed liquid entering the impinging flow transesterification tubular reactor and the ethanol vapor from the ethanol vaporizer enter the opposite Laval nozzles through the gas-liquid coupler. The two high-speed jets ejected from the opposite Laval nozzles collide with each other in the high-speed jet impact chamber and then enter the tubular reactor. The ethanol vapor and dimethyl carbonate undergo an ester exchange reaction in the tubular reactor to obtain an ester exchange liquid, which continuously enters the post-ester exchange tower;
[0017] (3) the ester exchange reaction between ethanol and dimethyl carbonate is continued on the plate-type tower of the post-ester exchange tower, and the methanol-dimethyl carbonate azeotrope is separated out at the same time. The separated methanol-dimethyl carbonate azeotrope gas enters the post-ester exchange tower condenser. The methanol-dimethyl carbonate azeotrope condensed by the post-ester exchange tower condenser enters the methanol-dimethyl carbonate azeotrope receiving tank. The methanol-dimethyl carbonate azeotrope in the methanol-dimethyl carbonate azeotrope receiving tank is pumped by the methanol-dimethyl carbonate azeotrope, part of which enters the post-ester exchange tower as reflux and part of which enters the methanol recovery system. The remaining methanol-dimethyl carbonate azeotrope is returned to the batching tank as a recycled material. The bottom liquid of the post-ester exchange tower is pumped by the bottom pump of the post-ester exchange tower, part of which enters the reboiler of the post-ester exchange tower for heating and then returns to the post-ester exchange tower, and part of which is filtered out of the catalyst through the catalyst filter. The filtrate enters the light component removal tower, and the filtered catalyst enters the catalyst recovery system.
[0018] (4) The dimethyl carbonate vapor separated from the light component removal tower enters the condenser of the light component removal tower, and the dimethyl carbonate condensed by the condenser of the light component removal tower enters the light component receiving tank. The dimethyl carbonate in the light component receiving tank is pumped by the light component, and part of it enters the light component removal tower as reflux, and the remaining dimethyl carbonate is returned to the batching tank as recycled material; the bottom liquid of the light component removal tower is pumped by the bottom pump of the light component removal tower, and part of it enters the reboiler of the light component removal tower for heating and then returns to the light component removal tower, and part of it enters the ethyl methyl carbonate distillation tower;
[0019] (5) The ethyl methyl carbonate vapor distilled from the ethyl methyl carbonate distillation tower enters the condenser of the distillation tower, and the ethyl methyl carbonate condensed in the distillation tower condenser enters the ethyl methyl carbonate receiving tank. The ethyl methyl carbonate in the ethyl methyl carbonate receiving tank is pumped by the ethyl methyl carbonate, part of which enters the ethyl methyl carbonate distillation tower as reflux, and part of which directly enters the ethyl methyl carbonate storage tank; the bottom liquid of the ethyl methyl carbonate distillation tower is pumped by the bottom pump of the ethyl methyl carbonate distillation tower, part of which enters the reboiler of the distillation tower for heating and then returns to the ethyl methyl carbonate distillation tower, and the remaining bottom liquid is returned to the batching tank as recycled material.
[0020] Preferably,
[0021] In step (1), the reaction temperature in the batching tank is 85°C to 90°C, the pressure is 0.22MPa to 0.26MPa, the catalyst is 0.2% to 0.4% of the mass of dimethyl carbonate, and the residence time of the material is 0.5h to 0.75h;
[0022] The molar ratio of ethanol to dimethyl carbonate added in the ethanol vaporizer in step (2) is (1.2-1.4): 1, the temperature in the tubular reactor is 105° C.-110° C., and the pressure is 0.42 MPa-0.48 MPa;
[0023] In step (3), the top temperature of the post-esterification tower is 64°C, the top pressure is atmospheric pressure, the bottom temperature is 90°C to 110°C, the reflux ratio is 1.0 to 1.5, and the residence time of the material is 1.0h to 1.5h;
[0024] In step (4), the top temperature of the light component removal tower is 60°C, the top pressure is 0.035 MPa, the bottom temperature is 75°C to 85°C, and the reflux ratio is 1;
[0025] In step (5), the top temperature of the ethyl methyl carbonate distillation tower is 66°C, the top pressure is 0.026 MPa, the bottom temperature is 80°C to 85°C, and the reflux ratio is 2.
[0026] Compared with the prior art, the device and method for producing ethyl methyl carbonate using an impinging flow transesterification tubular reactor of the present invention have the following beneficial effects:
[0027] 1. The impinging flow transesterification tubular reactor is used for transesterification reaction. Two heterogeneous fluids flow toward each other at high speed, forming a highly turbulent impact zone through impact. The impinging flow effectively improves the mixing and mass transfer effect in the reactor, and increases the reaction rate and product yield.
[0028] 2. Shortened the reaction time, saved energy, improved production efficiency, green and environmentally friendly;
[0029] 3. The quality of the prepared ethyl methyl carbonate is higher than the HG / T 5158-2017 industrial ethyl methyl carbonate standard; the process of the present invention is mature, the equipment is advanced, the operation is continuous, and the degree of automation is high. BRIEF DESCRIPTION OF THE DRAWINGS
[0030] Figure 1 The schematic diagram of the device for producing ethyl methyl carbonate using an impinging flow transesterification tubular reactor of the present invention;
[0031] Figure numerals: 1. batching tank, 1-1. mechanical agitator, 1-2. heating jacket; 2. impinging flow transesterification tubular reactor, 2-1. power fluid pump, 2-2. Laval nozzle, 2-3. high-speed jet impact chamber, 2-4. gas-liquid coupler, 2-5. tubular reactor, 2-6. heater, 2-7. ethanol vaporizer; 3. post-esterification tower, 3-1. post-esterification tower reboiler, 3-2. post-esterification tower plate, 3-3. post-esterification tower white steel structured packing, 3-4. post-esterification tower condenser, 3-5. methanol-dimethyl ester azeotrope receiving tank, 3-6. methanol-dimethyl ester azeotrope , 3-7, bottom pump of post-ester exchange tower, 3-8, catalyst filter; 4, light component removal tower, 4-1, light component removal tower reboiler, 4-2, white steel structured packing of light component removal tower, 4-3, light component removal tower condenser, 4-4, light component receiving tank, 4-5, light component pump, 4-6, bottom pump of light component removal tower; 5, ethyl methyl carbonate distillation tower, 5-1, distillation tower reboiler, 5-2, white steel structured packing of distillation tower, 5-3, distillation tower condenser, 5-4, ethyl methyl carbonate receiving tank, 5-5, ethyl methyl carbonate pump, 5-6, ethyl methyl carbonate storage tank, 5-7 bottom pump of ethyl methyl carbonate distillation tower. DETAILED DESCRIPTION
[0032] In order to make the purpose, technical solution and advantages of the present invention more clearly understood, the present invention is further described in detail below in conjunction with the embodiments. It should be understood that the specific embodiments described herein are only used to explain the present invention and are not used to limit the present invention.
[0033] In view of the above-mentioned engineering problems and market demands, in order to overcome the problems existing in the prior art, the present invention provides a method with mature process, continuous operation, high degree of automation, advanced reactor technology, high reaction efficiency, energy saving and environmental friendliness; an advanced impinging flow transesterification tubular reactor is used for transesterification reaction, which strengthens heat transfer and mass transfer, improves reaction rate and product yield, and the quality of prepared ethyl methyl carbonate is higher than the HG / T 5158-2017 industrial ethyl methyl carbonate standard.
[0034] Example 1
[0035] like Figure 1 As shown, the device for producing ethyl methyl carbonate by using an impinging flow transesterification tubular reactor comprises a batching tank 1, an impinging flow transesterification tubular reactor 2, a post-esterification tower system, a light component removal tower system, and an ethyl methyl carbonate distillation tower system which are connected in sequence; the batching tank 1 is also directly connected to the post-esterification tower system, the light component removal tower system, and the ethyl methyl carbonate distillation tower system.
[0036] The batching tank 1 is a tank structure with a heating jacket 1-2 arranged on the outer circumference and a mechanical stirrer 1-1 arranged inside. A liquid inlet is provided on the top of the batching tank 1, and the liquid inlet is connected to the methanol-dimethyl ester azeotrope pump 3-6 of the rear ester exchange tower 3. The liquid outlet at the bottom of the batching tank 1 is connected to the inlet end of the power fluid pump 2-1, and the outlet end of the power fluid pump 2-1 is connected to the liquid inlet end of the gas-liquid coupler 2-4 of the impinging flow ester exchange tubular reactor 2. The batching tank 1 is used for batching dimethyl carbonate, catalyst, and recycled materials (methanol, dimethyl carbonate, ethyl methyl carbonate, diethyl carbonate). At the same time, dimethyl carbonate, catalyst, and recycled materials are mixed uniformly under the stirring action of the mechanical stirrer 1-1 to obtain a mixed liquid. The mixed liquid reaches the reaction temperature under the heating of the heat medium and enters the impinging flow ester exchange tubular reactor 2 through the power fluid pump 2-1. The heating jacket 1-2 is a structure in which the heat medium flows inside.
[0037] The impinging flow transesterification tubular reactor 2 is used for transesterification reaction between ethanol vapor and dimethyl carbonate; the impinging flow transesterification tubular reactor 2 comprises a power fluid pump 2-1, a Laval nozzle 2-2, a high-speed jet impact chamber 2-3, a gas-liquid coupler 2-4, a tubular reactor 2-5, a heater 2-6, and an ethanol vaporizer 2-7; the Laval nozzle 2-2, the high-speed jet impact chamber 2-3, the gas-liquid coupler 2-4, and the tubular reactor 2-5 are all arranged inside the heater 2-6; two Laval nozzles 2-2 are arranged opposite to each other and connected, and the cavity formed at the middle connecting portion is a mixing cavity, and the middle of the mixing cavity The high-speed jet impact chamber 2-3 is connected in the vertical direction, and the high-speed jet impact chamber 2-3 is connected to one end of the tubular reactor 2-5, and the other end of the tubular reactor 2-5 is connected to the liquid inlet in the middle of the rear ester exchange tower 3; the two Laval nozzles 2-2 are fixed with gas-liquid couplers 2-4 at the opposite ends, and a steam inlet is provided at the mouth of the gas-liquid coupler 2-4, and the steam inlet is connected to the outlet end of the ethanol vaporizer 2-7. The ethanol vaporizer 2-7 is a structure with a heat medium arranged outside. Fresh ethanol is passed into the ethanol vaporizer 2-7, and after vaporization, it enters the gas-liquid coupler 2-4 from the steam inlet to react with the mixed liquid from the batching tank 1. The tubular reactor 2-5 is a tube with a length-to-diameter ratio greater than 1000, which can be Φ75mm or Φ100mm, and can be set to a reciprocating type or a spring type. The heater 2-6 is a closed box structure, and a flowing heat medium structure is arranged inside.
[0038] The two opposite Laval nozzles 2-2 are connected to the batching tank 1 through the first power fluid pump 2-1, and are connected to the outlet end of the ethanol vaporizer 2-7. The mixed liquid in the batching tank 1 is pumped into the gas-liquid coupler 2-4 of the two opposite Laval nozzles 2-2 through the first power fluid pump 2-1. The air inlet of the gas-liquid coupler 2-4 simultaneously inhales the ethanol vapor vaporized at the outlet end of the ethanol vaporizer 2-7. The two high-speed jets (the mixed liquid in the batching tank 1 and the ethanol vapor in the ethanol vaporizer 2-7) ejected from the Laval nozzle 2-2 collide with each other in the high-speed jet impact chamber 2-3 through the mixing chamber, and then enter the tubular reactor 2-5 for ester exchange reaction. The ester exchange liquid continuously enters the post-ester exchange tower 3 of the post-ester exchange tower system.
[0039] Since the mixed liquid is ejected at high speed through the Laval tube, a negative pressure zone will be generated at the gas suction port of the gas-liquid coupler 2-4, causing the gas to be sucked in, and rapidly expand in the negative pressure zone and be beaten into tiny bubbles by the power fluid and enter the mixing chamber; at this time, in the mixing chamber, the gas and liquid are fully mixed in the mixing chamber, and are accelerated to discharge due to energy exchange, and the speed can reach the speed of sound, and then pass through the expansion chamber of the Laval tube to increase the potential energy of the mixed liquid to the maximum, further enhancing the mass transfer and heat transfer effects; two heterogeneous fluids flow towards each other at high speed, and form a highly turbulent collision zone through collision, which greatly enhances the process heat and mass transfer; the strong micro-mixing and pressure fluctuation characteristics of the impact flow can make the chemical reaction proceed quickly and produce effective and uniform supersaturation instantly; and because the chaotic flow state rapidly reduces the mixing scale, the vortices of different scales and the folding collision with each other enhance the turbulence intensity and energy diffusion, prompting the molecules to reach a more effective high-energy level collision when the chemical reaction occurs, and the impact flow effectively improves the mixing and mass transfer effects in the reactor, and increases the reaction rate and product yield.
[0040] The post-esterification tower system is used for continuing the ester exchange reaction between ethanol and dimethyl carbonate, and separating the methanol generated by the reaction. The post-esterification tower system is composed of a post-esterification tower 3, a post-esterification tower reboiler 3-1, a post-esterification tower plate-type tower plate 3-2, a post-esterification tower white steel structured packing 3-3, a post-esterification tower condenser 3-4, a methanol-dimethyl ester azeotrope receiving tank 3-5, a methanol-dimethyl ester azeotrope pump 3-6, a post-esterification tower bottom pump 3-7, and a catalyst filter 3-8; the post-esterification tower 3 is a tower body structure in which a post-esterification tower plate-type tower plate 3-2 is arranged at the bottom of the interior, and a post-esterification tower white steel structured packing 3-3 is arranged above. The tubular reactor 2-5 is connected to the post-ester exchange tower 3, the top of the post-ester exchange tower 3 is connected to the post-ester exchange tower condenser 3-4, the methanol-dimethyl ester azeotrope receiving tank 3-5 and the inlet of the methanol-dimethyl ester azeotrope pump 3-6 in sequence, and the outlet end of the methanol-dimethyl ester azeotrope pump 3-6 is respectively connected to the post-ester exchange tower 3, the feed inlet at the top of the batching tank 1 and the methanol recovery system; the bottom end of the post-ester exchange tower 3 is respectively connected to the inlet ends of the post-ester exchange tower reboiler 3-1 and the catalyst filter 3-8 through the post-ester exchange tower bottom pump 3-7, the outlet end of the post-ester exchange tower reboiler 3-1 is connected to the post-ester exchange tower 3, and the outlet end of the catalyst filter 3-8 is respectively connected to the light component removal tower 4 and the catalyst recovery system of the light component removal tower system.
[0041] The ester exchange reaction of ethanol and dimethyl carbonate is continued on the reaction tower plate in the lower half of the rear ester exchange tower 3, and the methanol-dimethyl carbonate azeotrope is separated in the upper half of the tower. The separated methanol-dimethyl carbonate azeotrope gas enters the rear ester exchange tower condenser 3-4, and the methanol-dimethyl carbonate azeotrope condensed by the rear ester exchange tower condenser 3-4 enters the methanol-dimethyl carbonate azeotrope receiving tank 3-5. The methanol-dimethyl carbonate azeotrope receiving tank 3-5 is used to collect the methanol-dimethyl carbonate azeotrope. The methyl ester azeotrope passes through the methanol-dimethyl carbonate azeotrope pump 3-6, part of which enters the post-ester exchange tower 3 as reflux, part of which enters the methanol recovery system, and part of which is directly returned to the batching tank 1; the bottom liquid of the post-ester exchange tower 3 passes through the post-ester exchange tower bottom pump 3-7, part of which enters the post-ester exchange tower reboiler 3-1 for heating and then returns to the post-ester exchange tower 3, and part of which is filtered out of the catalyst through the catalyst filter 3-8, and the filtrate enters the light component removal tower 4, and the filtered catalyst enters the catalyst recovery system.
[0042] The light component removal tower system is used to remove light components in the filtrate, mainly dimethyl carbonate; the light component removal tower system consists of a light component removal tower 4, a light component removal tower reboiler 4-1, a light component removal tower white steel structured packing 4-2, a light component removal tower condenser 4-3, a light component receiving tank 4-4, a light component pump 4-5, and a light component removal tower bottom pump 4-6; the light component removal tower 4 is provided with a light component removal tower white steel structured packing 4-2. The top of the light component removal tower 4 is connected to the light component removal tower condenser 4-3, the light component receiving tank 4-4, and the light component pump 4-5 in sequence, and the outlet end of the light component pump 4-5 is connected to the light component removal tower 4 and the batching tank 1 respectively; the bottom end of the light component removal tower 4 is connected to the light component removal tower bottom pump 4-6, and the light component removal tower bottom pump 4-6 is connected to the light component removal tower reboiler 4-1 and the methyl ethyl carbonate distillation tower 5 of the methyl ethyl carbonate distillation tower system respectively, and the light component removal tower reboiler 4-1 is connected to the light component removal tower 4.
[0043] The filtrate from the catalyst filter 3-8 enters the light component removal tower 4, the dimethyl carbonate vapor separated in the light component removal tower 4 enters the light component removal tower condenser 4-3, the dimethyl carbonate condensed in the light component removal tower condenser 4-3 enters the dimethyl carbonate light component receiving tank 4-4, the dimethyl carbonate in the light component receiving tank 4-4 passes through the dimethyl carbonate light component pump 4-5, part of which enters the light component removal tower 4 as reflux, and part of which is directly returned to the batching tank 1; the bottom liquid of the light component removal tower 4 passes through the light component removal tower bottom pump 4-6, part of which enters the light component removal tower reboiler 4-1 for heating and then returns to the light component removal tower 4, and part of which enters the methyl ethyl carbonate distillation tower 5 of the methyl ethyl carbonate distillation tower system.
[0044] The ethyl methyl carbonate distillation tower system is used to distill ethyl methyl carbonate from the bottom liquid of the light component removal tower; the ethyl methyl carbonate distillation tower system consists of an ethyl methyl carbonate distillation tower 5, a distillation tower reboiler 5-1, a distillation tower condenser 5-3, an ethyl methyl carbonate receiving tank 5-4, an ethyl methyl carbonate pump 5-5, an ethyl methyl carbonate storage tank 5-6, and an ethyl methyl carbonate distillation tower bottom pump 5-7; and a distillation tower white steel structured packing 5-2 is arranged inside the ethyl methyl carbonate distillation tower 5. The top of the ethyl methyl carbonate distillation tower 5 is connected to the distillation tower condenser 5-3, the ethyl methyl carbonate receiving tank 5-4, and the ethyl methyl carbonate pump 5-5 in sequence, and the ethyl methyl carbonate pump 5-5 is respectively connected to the ethyl methyl carbonate distillation tower 5 and the ethyl methyl carbonate storage tank 5-6; the bottom of the ethyl methyl carbonate distillation tower 5 is connected to the ethyl methyl carbonate distillation tower bottom pump 5-7, and the ethyl methyl carbonate distillation tower bottom pump 5-7 is respectively connected to the distillation tower reboiler 5-1 and the batching tank 1, and the distillation tower reboiler 5-1 is then connected to the ethyl methyl carbonate distillation tower 5.
[0045] The bottom liquid from the light component removal tower enters the ethyl methyl carbonate distillation tower 5, the ethyl methyl carbonate vapor distilled from the ethyl methyl carbonate distillation tower 5 enters the distillation tower condenser 5-3, the ethyl methyl carbonate condensed by the distillation tower condenser 5-3 enters the ethyl methyl carbonate receiving tank 5-4, the ethyl methyl carbonate in the ethyl methyl carbonate receiving tank 5-4 passes through the ethyl methyl carbonate pump 5-5, part of which enters the ethyl methyl carbonate distillation tower 5 as reflux, and part of which directly enters the ethyl methyl carbonate storage tank 5-6; the bottom liquid of the ethyl methyl carbonate distillation tower 5 passes through the ethyl methyl carbonate distillation tower bottom pump 5-7, part of which enters the distillation tower reboiler 5-1 for heating and then returns to the ethyl methyl carbonate distillation tower 5, and part of which directly returns to the batching tank 1.
[0046] The raw materials used in the present invention are industrial dimethyl carbonate (mass content greater than 99.5%), industrial ethanol (mass content greater than 99.5%), catalysts, etc.; the public engineering water vapor used is 0.4 MPa, 290°C superheated water vapor; the public engineering water vapor mainly provides heat source for the heat medium of the batching tank 1, the heat medium of the heater 2-6, the heat medium of the ethanol vaporizer 2-7, the heat medium of the post-ester exchange tower reboiler 3-1, the heat medium of the light component removal tower reboiler 4-1, and the heat medium of the distillation tower reboiler 5-1; the various devices of the device are connected by corresponding pipelines, and the heat medium structure of the tower kettle is the existing reboiler structure. The light component receiving tank 4-4 and the ethyl methyl carbonate receiving tank 5-4 are both connected to the vacuum system. Cooling water is introduced into the post-ester exchange tower condenser 3-4, the light component removal tower condenser 4-3 and the distillation tower condenser 5-3 for condensation, and the attached Figure 1 When the central pipelines cross on the diagram but do not actually intersect, they are drawn according to the principle of vertical breaks but not horizontal breaks.
[0047] The process for producing ethyl methyl carbonate using an impinging flow transesterification tubular reactor specifically comprises the following steps:
[0048] (1) The raw material dimethyl carbonate, catalyst, and recycled materials (methanol, dimethyl carbonate, ethyl methyl carbonate, and diethyl carbonate recycled through the methanol-dimethyl ester azeotrope pump 3-6, the light component pump 4-5, and the methyl ethyl carbonate distillation tower bottom pump 5-7) enter the batching tank 1, and the dimethyl carbonate, catalyst, and recycled materials are mixed uniformly under the stirring action of the mechanical stirrer 1-1 to obtain a mixed liquid; the mixed liquid reaches the reaction temperature under the heating of the heat medium, and enters the impinging flow transesterification tubular reactor 2 through the power fluid pump 2-1;
[0049] The raw material is dimethyl carbonate (mass content greater than 99.9%), the temperature in the batching tank 1 is 85°C to 90°C, the pressure is 0.22MPa to 0.26MPa, the catalyst is 0.2% to 0.4% of the mass of dimethyl carbonate, and the residence time of the material is 0.5h to 0.75h;
[0050] (2) The mixed liquid in the batching tank 1 is pumped into two gas-liquid couplers 2-4 through the power fluid pump 2-1. The gas-liquid couplers 2-4 simultaneously inhale ethanol vapor from the ethanol vaporizer 2-7. The two high-speed jets ejected from the opposite Laval nozzles 2-2 collide with each other in the high-speed jet impact chamber 2-3 and then enter the tubular reactor 2-5. The ethanol vapor and dimethyl carbonate undergo an ester exchange reaction in the tubular reactor to obtain an ester exchange liquid. The ester exchange liquid continuously enters the post-ester exchange tower 3;
[0051] The ethanol (mass content greater than 99.5%) steam from the ethanol vaporizer 2-7, the molar ratio of dimethyl carbonate:ethanol (ethanol fed to the ethanol vaporizer 2-7) is 1:(1.2-1.4), the temperature in the tubular reactor is 105°C-110°C, and the pressure is 0.42MPa-0.48MPa.
[0052] (3) In the post-esterification tower 3, ethanol and dimethyl carbonate continue to undergo ester exchange reaction, and methanol generated by the reaction is separated; in the post-esterification tower plate 3-2 in the lower half of the post-esterification tower 3, ethanol and dimethyl carbonate continue to undergo ester exchange reaction, and methanol-dimethyl carbonate azeotrope is separated in the upper half of the tower, and the separated methanol-dimethyl carbonate azeotrope gas enters the post-esterification tower condenser 3-4, and the methanol-dimethyl carbonate azeotrope condensed by the post-esterification tower condenser 3-4 enters the methanol-dimethyl carbonate azeotrope receiving tank 3-5 The methanol-dimethyl carbonate azeotrope in the methanol-dimethyl carbonate azeotrope receiving tank 3-5 is pumped by the methanol-dimethyl carbonate azeotrope pump 3-6, part of which enters the post-esterification tower 3 as reflux, part of which enters the methanol recovery system, and part of which is directly returned to the batching tank 1; the bottom liquid of the post-esterification tower 3 is pumped by the post-esterification tower bottom pump 3-7, part of which enters the post-esterification tower reboiler 3-1 for heating and then returns to the post-esterification tower 3, and part of which is filtered out of the catalyst through the catalyst filter 3-8, and the filtrate enters the light component removal tower 4, and the filtered catalyst enters the catalyst recovery system;
[0053] The top temperature of the post-esterification tower 3 is 64°C, the top pressure is normal pressure, the bottom temperature is 90°C to 110°C, the reflux ratio is 1.0 to 1.5, and the residence time of the material is 1.0h to 1.5h;
[0054] (4) The filtrate from the catalyst filter enters the light component removal tower 4 to remove the light components in the filtrate, mainly dimethyl carbonate; the dimethyl carbonate vapor separated from the light component removal tower 4 enters the light component removal tower condenser 4-3, and the dimethyl carbonate condensed by the light component removal tower condenser 4-3 enters the light component receiving tank 4-4. The dimethyl carbonate in the light component receiving tank 4-4 is pumped by the light component pump 4-5, part of which enters the light component removal tower 4 as reflux, and part of which is directly returned to the batching tank 1; the bottom liquid of the light component removal tower 4 is pumped by the light component removal tower bottom pump 4-6, part of which enters the light component removal tower reboiler 4-1 for heating and then returns to the light component removal tower 4, and part of which enters the methyl ethyl carbonate distillation tower 5;
[0055] The light component removal tower has a top temperature of 60°C, a top pressure of 0.035 MPa, a bottom temperature of 75°C to 85°C, and a reflux ratio of 1;
[0056] (5) The ethyl methyl carbonate gas distilled from the ethyl methyl carbonate distillation tower 5 enters the distillation tower condenser 5-3, and the ethyl methyl carbonate condensed by the distillation tower condenser 5-3 enters the ethyl methyl carbonate receiving tank 5-4. The ethyl methyl carbonate in the ethyl methyl carbonate receiving tank 5-4 passes through the ethyl methyl carbonate pump 5-5, part of which enters the ethyl methyl carbonate distillation tower 5 as reflux, and part of which directly enters the ethyl methyl carbonate storage tank 5-6; the bottom liquid of the ethyl methyl carbonate distillation tower 5 passes through the ethyl methyl carbonate distillation tower bottom pump 5-7, part of which enters the distillation tower reboiler 5-1 for heating and then returns to the ethyl methyl carbonate distillation tower 5, and part of which directly returns to the batching tank 1.
[0057] The top temperature of the ethyl methyl carbonate distillation tower 5 is 66° C., the top pressure is 0.026 MPa, the bottom temperature is 80° C. to 85° C., and the reflux ratio is 2.
[0058] Example 2
[0059] A method for producing ethyl methyl carbonate based on a device for preparing ethyl methyl carbonate based on an impinging flow transesterification tubular reactor 2 described in Example 1 comprises the following steps:
[0060] In the step (1), 91 kg / h of dimethyl carbonate (mass content greater than 99.9%), 0.364 kg / h of catalyst, and recycled materials (methanol, dimethyl carbonate, ethyl methyl carbonate, diethyl carbonate) are introduced into a batching tank 1, and the dimethyl carbonate, catalyst, and recycled materials are uniformly mixed under stirring; the mixed liquid reaches the reaction temperature under the heating of a heat medium, and enters the impinging flow transesterification tubular reactor 2 through a power fluid pump; the temperature in the batching tank 1 is 85° C., the pressure is 0.22 MPa, the molar ratio of dimethyl carbonate to ethanol (ethanol fed to the ethanol vaporizer) is 1:1.4, the catalyst is 0.4% (mass) of dimethyl carbonate, and the residence time of the materials is 0.75 h;
[0061] (2) The mixed liquid in the batching tank 1 is pumped into two gas-liquid couplers 2-4 through the power fluid pump 2-1. The gas-liquid couplers 2-4 simultaneously inhale ethanol vapor from the ethanol vaporizer 2-7. The two high-speed jets ejected from the opposite Laval nozzles 2-2 collide with each other in the high-speed jet impact chamber 2-3 and then enter the tubular reactor 2-5. The ethanol vapor and dimethyl carbonate undergo an ester exchange reaction in the tubular reactor to obtain an ester exchange liquid. The ester exchange liquid continuously enters the post-ester exchange tower 3. The temperature in the tubular reactor is 105°C and the pressure is 0.42MPa.
[0062] (3) In the post-esterification tower 3, ethanol and dimethyl carbonate continue to undergo ester exchange reaction, and the methanol generated by the reaction is separated; the ester exchange reaction between ethanol and dimethyl carbonate continues on the post-esterification tower plate 3-2 in the lower half of the post-esterification tower 3, and the methanol-dimethyl carbonate azeotrope is separated in the upper half of the tower. The separated methanol-dimethyl carbonate azeotrope vapor enters the post-esterification tower condenser 3-4, and the methanol-dimethyl carbonate azeotrope condensed by the post-esterification tower condenser 3-4 enters the methanol-dimethyl carbonate azeotrope receiving tank 3- 5. The methanol-dimethyl carbonate azeotrope in the methanol-dimethyl carbonate azeotrope receiving tank 3-5 is pumped by the methanol-dimethyl carbonate azeotrope pump 3-6, part of which enters the post-esterification tower 3 as reflux, part of which enters the methanol recovery system, and part of which is directly returned to the batching tank 1; the bottom liquid of the post-esterification tower 3 is pumped by the post-esterification tower bottom pump 3-7, part of which enters the post-esterification tower reboiler 3-1 for heating and then returns to the post-esterification tower 3, and part of which is filtered out of the catalyst through the catalyst filter 3-8, and the filtrate enters the light component removal tower 4, and the filtered catalyst enters the catalyst recovery system;
[0063] The top temperature of the post-esterification tower 3 is 64°C, the top pressure is normal pressure, the bottom temperature is 90°C, the reflux ratio is 1.0, and the residence time of the material is 1.5h;
[0064] (4) The filtrate from the catalyst filter enters the light component removal tower 4 to remove the light components in the filtrate, mainly dimethyl carbonate; the dimethyl carbonate vapor separated from the light component removal tower 4 enters the light component removal tower condenser 4-3, and the dimethyl carbonate condensed by the light component removal tower condenser 4-3 enters the light component receiving tank 4-4. The dimethyl carbonate in the light component receiving tank 4-4 is pumped by the light component pump 4-5, part of which enters the light component removal tower 4 as reflux, and part of which is directly returned to the batching tank 1; the bottom liquid of the light component removal tower 4 is pumped by the light component removal tower bottom pump 4-6, part of which enters the light component removal tower reboiler 4-1 for heating and then returns to the light component removal tower 4, and part of which enters the methyl ethyl carbonate distillation tower 5;
[0065] The light component removal tower has a top temperature of 60°C, a top pressure of 0.035 MPa, a bottom temperature of 75°C, and a reflux ratio of 1;
[0066] (5) The ethyl methyl carbonate gas distilled from the ethyl methyl carbonate distillation tower 5 enters the distillation tower condenser 5-3, and the ethyl methyl carbonate condensed by the distillation tower condenser 5-3 enters the ethyl methyl carbonate receiving tank 5-4. The ethyl methyl carbonate in the ethyl methyl carbonate receiving tank 5-4 passes through the ethyl methyl carbonate pump 5-5, part of which enters the ethyl methyl carbonate distillation tower 5 as reflux, and part of which directly enters the ethyl methyl carbonate storage tank 5-6; the bottom liquid of the ethyl methyl carbonate distillation tower 5 passes through the ethyl methyl carbonate distillation tower bottom pump 5-7, part of which enters the distillation tower reboiler 5-1 for heating and then returns to the ethyl methyl carbonate distillation tower 5, and part of which directly returns to the batching tank 1.
[0067] The top temperature of the ethyl methyl carbonate distillation tower 5 is 66° C., the top pressure is 0.026 MPa, the bottom temperature is 80° C. to 85° C., and the reflux ratio is 2.
[0068] The top temperature of the ethyl methyl carbonate distillation tower 5 is 66° C., the top pressure is 0.026 MPa, the bottom temperature is 80° C., the reflux ratio is 2, the ethyl methyl carbonate production is 102.2 kg / h, and the ethyl methyl carbonate yield is 97.180% (mass content is greater than 99.9%).
[0069] Example 3
[0070] The method for producing ethyl methyl carbonate based on the device for producing ethyl methyl carbonate using the impinging flow transesterification tubular reactor described in Example 1 comprises the following steps:
[0071] In the step (1), 91 kg / h of dimethyl carbonate (mass content greater than 99.9%), 0.182 kg / h of catalyst, and recycled materials (methanol, dimethyl carbonate, ethyl methyl carbonate, diethyl carbonate) are introduced into a batching tank 1, and the dimethyl carbonate, catalyst, and recycled materials are uniformly mixed under stirring; the mixed liquid reaches the reaction temperature under the heating of a heat medium, and enters the impinging flow transesterification tubular reactor 2 through a power fluid pump; the temperature in the batching tank 1 is 90° C., the pressure is 0.26 MPa, the molar ratio of dimethyl carbonate to ethanol (ethanol fed to the ethanol vaporizer) is 1:1.2, the catalyst is 0.2% (mass) of dimethyl carbonate, and the residence time of the materials is 0.5 h;
[0072] (2) The mixed liquid in the batching tank 1 is pumped into two gas-liquid couplers 2-4 through the power fluid pump 2-1. The gas-liquid couplers 2-4 simultaneously inhale ethanol vapor from the ethanol vaporizer 2-7. The two high-speed jets ejected from the opposite Laval nozzles 2-2 collide with each other in the high-speed jet impact chamber 2-3 and then enter the tubular reactor 2-5. The ethanol vapor and dimethyl carbonate undergo an ester exchange reaction in the tubular reactor to obtain an ester exchange liquid. The ester exchange liquid continuously enters the post-ester exchange tower 3. The temperature in the tubular reactor is 110°C and the pressure is 0.48MPa.
[0073] (3) In the post-esterification tower 3, ethanol and dimethyl carbonate continue to undergo ester exchange reaction, and methanol generated by the reaction is separated; the ester exchange reaction between ethanol and dimethyl carbonate continues on the post-esterification tower plate 3-2 in the lower half of the post-esterification tower 3, and methanol-dimethyl carbonate azeotrope is separated in the upper half of the tower, and the separated methanol-dimethyl carbonate azeotrope gas enters the post-esterification tower condenser 3-4, and the methanol-dimethyl carbonate azeotrope condensed by the post-esterification tower condenser 3-4 enters the methanol-dimethyl carbonate azeotrope receiving tank 3-5. The methanol-dimethyl carbonate azeotrope in the methanol-dimethyl carbonate azeotrope receiving tank 3-5 is pumped by the methanol-dimethyl carbonate azeotrope pump 3-6, part of which enters the post-esterification tower (3) as reflux, part of which enters the methanol recovery system, and part of which is directly returned to the batching tank 1; the bottom liquid of the post-esterification tower 3 is pumped by the post-esterification tower bottom pump 3-7, part of which enters the post-esterification tower reboiler 3-1 for heating and then returns to the post-esterification tower 3, and part of which is filtered out of the catalyst through the catalyst filter 3-8, and the filtrate enters the light component removal tower 4, and the filtered catalyst enters the catalyst recovery system;
[0074] The top temperature of the post-esterification tower 3 is 64°C, the top pressure is normal pressure, the bottom temperature is 110°C, the reflux ratio is 1.5, and the residence time of the material is 1.0h;
[0075] (4) The filtrate from the catalyst filter enters the light component removal tower 4 to remove the light components in the filtrate, mainly dimethyl carbonate; the dimethyl carbonate vapor separated from the light component removal tower 4 enters the light component removal tower condenser 4-3, and the dimethyl carbonate condensed by the light component removal tower condenser 4-3 enters the light component receiving tank 4-4. The dimethyl carbonate in the light component receiving tank 4-4 is pumped by the light component pump 4-5, part of which enters the light component removal tower 4 as reflux, and part of which is directly returned to the batching tank 1; the bottom liquid of the light component removal tower 4 is pumped by the light component removal tower bottom pump 4-6, part of which enters the light component removal tower reboiler 4-1 for heating and then returns to the light component removal tower 4, and part of which enters the methyl ethyl carbonate distillation tower 5;
[0076] The light component removal tower has a top temperature of 60°C, a top pressure of 0.035 MPa, a bottom temperature of 85°C, and a reflux ratio of 1;
[0077] (5) The ethyl methyl carbonate gas distilled from the ethyl methyl carbonate distillation tower 5 enters the distillation tower condenser 5-3, and the ethyl methyl carbonate condensed by the distillation tower condenser 5-3 enters the ethyl methyl carbonate receiving tank 5-4. The ethyl methyl carbonate in the ethyl methyl carbonate receiving tank 5-4 passes through the ethyl methyl carbonate pump 5-5, part of which enters the ethyl methyl carbonate distillation tower 5 as reflux, and part of which directly enters the ethyl methyl carbonate storage tank 5-6; the bottom liquid of the ethyl methyl carbonate distillation tower 5 passes through the ethyl methyl carbonate distillation tower bottom pump 5-7, part of which enters the distillation tower reboiler 5-1 for heating and then returns to the ethyl methyl carbonate distillation tower 5, and part of which directly returns to the batching tank 1.
[0078] The top temperature of the ethyl methyl carbonate distillation tower 5 is 66° C., the top pressure is 0.026 MPa, the bottom temperature is 85° C., the reflux ratio is 2, the ethyl methyl carbonate production is 102.4 kg / h, and the ethyl methyl carbonate yield is 97.370% (mass content is greater than 99.9%).
[0079] The present embodiment provides a production method for preparing ethyl methyl carbonate based on an impinging flow transesterification tubular reactor. The quality of the prepared ethyl methyl carbonate is higher than the HG / T 5158-2017 industrial ethyl methyl carbonate standard.
[0080] The above technical scheme explains the technical idea of the present invention, which cannot be used to limit the protection scope of the present invention. Any changes and modifications made to the above technical scheme based on the technical essence of the present invention without departing from the content of the technical scheme of the present invention shall fall within the protection scope of the technical scheme of the present invention.
Claims
1. A device for producing ethyl methyl carbonate using an impinging flow transesterification tubular reactor, characterized in that: The device comprises a batching tank (1), an impinging flow transesterification tubular reactor (2), a post-esterification tower system, a light component removal tower system, and a methyl ethyl carbonate distillation tower system, which are connected in sequence; the batching tank (1) is also directly connected to the post-esterification tower system, the light component removal tower system, and the methyl ethyl carbonate distillation tower system; The impinging flow transesterification tubular reactor (2) comprises a power fluid pump (2-1), a Laval nozzle (2-2), a high-speed jet impingement chamber (2-3), a gas-liquid coupler (2-4), a tubular reactor (2-5), a heater (2-6), and an ethanol vaporizer (2-7); the Laval nozzle (2-2), the high-speed jet impingement chamber (2-3), the gas-liquid coupler (2-4), and the tubular reactor (2-5) are all arranged inside the heater (2-6); two Laval nozzles (2-2) are disposed opposite to each other. The ends are fixedly connected to a gas-liquid coupler (2-4), and the pipe mouth of the gas-liquid coupler (2-4) is connected to the outlet end of the ethanol vaporizer (2-7); the two Laval nozzles (2-2) are arranged opposite to each other and are connected, and the cavity formed at the middle connecting part is a mixing cavity, and the middle of the mixing cavity is connected to a high-speed jet impact cavity (2-3) in the vertical direction, and the high-speed jet impact cavity (2-3) is connected to one end of the tubular reactor (2-5), and the other end of the tubular reactor (2-5) is connected to the liquid inlet in the middle of the rear ester exchange tower (3); The batching tank (1) is a tank structure with a heating jacket (1-2) arranged on the outer circumference and a mechanical stirrer (1-1) arranged inside. A liquid inlet is provided on the top of the batching tank (1), and the liquid inlet is connected to the methanol-dimethyl ester azeotrope pump (3-6) of the rear ester exchange tower (3). The liquid outlet at the bottom of the batching tank (1) is connected to the inlet end of the power fluid pump (2-1), and the outlet end of the power fluid pump (2-1) is connected to the liquid inlet end of the gas-liquid coupler (2-4) of the impinging flow ester exchange tubular reactor (2). The post-ester exchange tower system comprises a post-ester exchange tower (3), a post-ester exchange tower reboiler (3-1), a post-ester exchange tower plate-type tower plate (3-2), a post-ester exchange tower white steel structured packing (3-3), a post-ester exchange tower condenser (3-4), a methanol-dimethyl ester azeotrope receiving tank (3-5), a methanol-dimethyl ester azeotrope pump (3-6), a post-ester exchange tower bottom pump (3-7), and a catalyst filter (3-8); the post-ester exchange tower (3) is a tower structure in which a post-ester exchange tower plate-type tower plate (3-2) is arranged at the bottom and a post-ester exchange tower white steel structured packing (3-3) is arranged at the top; the tubular reactor (2-5) is connected to the post-ester exchange tower (3); and the top of the post-ester exchange tower (3) is connected in sequence to the post-ester exchange tower. The inlet of the ester exchange tower condenser (3-4), the methanol-dimethyl ester azeotrope receiving tank (3-5) and the methanol-dimethyl ester azeotrope pump (3-6), and the outlet of the methanol-dimethyl ester azeotrope pump (3-6) are respectively connected to the post-ester exchange tower (3), the feed inlet at the top of the batching tank (1) and the methanol recovery system; the bottom of the post-ester exchange tower (3) is respectively connected to the inlet of the post-ester exchange tower reboiler (3-1) and the catalyst filter (3-8) through the post-ester exchange tower bottom pump (3-7); the outlet of the post-ester exchange tower reboiler (3-1) is connected to the post-ester exchange tower (3); and the outlet of the catalyst filter (3-8) is respectively connected to the light component removal tower (4) of the light component removal tower system and the catalyst recovery system.
2. The device for producing ethyl methyl carbonate using an impinging flow transesterification tubular reactor according to claim 1, characterized in that: The light component removal tower system comprises a light component removal tower (4), a light component removal tower reboiler (4-1), a light component removal tower white steel structured packing (4-2), a light component removal tower condenser (4-3), a light component receiving tank (4-4), a light component pump (4-5), and a light component removal tower bottom pump (4-6); the light component removal tower (4) is provided with the light component removal tower white steel structured packing (4-2), and the top of the light component removal tower (4) is connected in sequence to the light component removal tower condenser (4-3), A light component receiving tank (4-4) and a light component pump (4-5), the outlet end of the light component pump (4-5) are respectively connected to a light component removal tower (4) and a batching tank (1); the bottom end of the light component removal tower (4) is connected to a light component removal tower bottom pump (4-6), the light component removal tower bottom pump (4-6) is respectively connected to a light component removal tower reboiler (4-1) and an ethyl methyl carbonate distillation tower (5) of the ethyl methyl carbonate distillation tower system, and the light component removal tower reboiler (4-1) is further connected to the light component removal tower (4).
3. The device for producing ethyl methyl carbonate using an impinging flow transesterification tubular reactor according to claim 1, characterized in that: The ethyl methyl carbonate distillation tower system comprises an ethyl methyl carbonate distillation tower (5), a distillation tower reboiler (5-1), a distillation tower condenser (5-3), an ethyl methyl carbonate receiving tank (5-4), an ethyl methyl carbonate pump (5-5), an ethyl methyl carbonate storage tank (5-6), and a ethyl methyl carbonate distillation tower bottom pump (5-7); a distillation tower white steel structured packing (5-2) is arranged inside the ethyl methyl carbonate distillation tower (5), and the top of the ethyl methyl carbonate distillation tower (5) is connected in sequence to the distillation tower condenser (5-3). , an ethyl methyl carbonate receiving tank (5-4), and an ethyl methyl carbonate pump (5-5), the ethyl methyl carbonate pump (5-5) is respectively connected to the ethyl methyl carbonate distillation tower (5) and the ethyl methyl carbonate storage tank (5-6); the bottom end of the ethyl methyl carbonate distillation tower (5) is connected to the ethyl methyl carbonate distillation tower bottom pump (5-7), the ethyl methyl carbonate distillation tower bottom pump (5-7) is respectively connected to the distillation tower reboiler (5-1) and the batching tank (1), and the distillation tower reboiler (5-1) is further connected to the ethyl methyl carbonate distillation tower (5).
4. The device for producing ethyl methyl carbonate using an impinging flow transesterification tubular reactor according to claim 1, characterized in that: The tubular reactor (2-5) is a tube with a length-to-diameter ratio greater than 1000, a tube diameter of Φ75 mm or Φ100 mm, and is configured as a reciprocating type or a spring type.
5. A method for producing ethyl methyl carbonate using an impinging flow transesterification tubular reactor as claimed in claim 1, characterized in that: The steps are: (1), the raw material dimethyl carbonate, the catalyst and the recycled material enter into the batching tank (1), and the raw materials are mixed evenly under the stirring action of the mechanical stirrer (1-1) to obtain a mixed liquid; the mixed liquid reaches the reaction temperature under the heating of the heat medium, and enters into the impinging flow transesterification tubular reactor (2) through the power fluid pump (2-1); (2), the mixed liquid entering the impinging flow transesterification tubular reactor (2) and the ethanol vapor from the ethanol vaporizer (2-7) enter the opposite Laval nozzles (2-2) through the gas-liquid coupler (2-4), and the two high-speed jets ejected from the opposite Laval nozzles (2-2) collide with each other in the high-speed jet impact chamber (2-3), and then enter the tubular reactor (2-5), and the ethanol vapor and dimethyl carbonate undergo an ester exchange reaction in the tubular reactor (2-5) to obtain an ester exchange liquid, and the ester exchange liquid continuously enters the post-ester exchange tower (3); (3) The ester exchange reaction between ethanol and dimethyl carbonate is continued on the post-ester exchange tower plate (3-2) of the post-ester exchange tower (3), and the methanol-dimethyl carbonate azeotrope is separated at the same time. The separated methanol-dimethyl carbonate azeotrope gas enters the post-ester exchange tower condenser (3-4). The methanol-dimethyl carbonate azeotrope condensed by the post-ester exchange tower condenser (3-4) enters the methanol-dimethyl carbonate azeotrope receiving tank (3-5). The methanol-dimethyl carbonate azeotrope in the methanol-dimethyl carbonate azeotrope receiving tank (3-5) is condensed by the methanol. - dimethyl carbonate azeotrope pump (3-6), part of which enters the post-esterification tower (3) as reflux, and part of which enters the methanol recovery system, and the remaining methanol-dimethyl carbonate azeotrope is returned to the batching tank (1) as a recycled material; the bottom liquid of the post-esterification tower (3) is pumped through the post-esterification tower bottom pump (3-7), part of which enters the post-esterification tower reboiler (3-1) for heating and then returns to the post-esterification tower (3), and part of which is filtered out of the catalyst through the catalyst filter (3-8), and the filtrate enters the light component removal tower (4), and the filtered catalyst enters the catalyst recovery system; (4), the dimethyl carbonate vapor separated by the light component removal tower (4) enters the light component removal tower condenser (4-3), and the dimethyl carbonate condensed by the light component removal tower condenser (4-3) enters the light component receiving tank (4-4). The dimethyl carbonate in the light component receiving tank (4-4) passes through the light component pump (4-5), and part of it enters the light component removal tower (4) as reflux, and the remaining dimethyl carbonate is returned to the batching tank (1) as a recycled material; the bottom liquid of the light component removal tower (4) passes through the light component removal tower bottom pump (4-6), and part of it enters the light component removal tower reboiler (4-1) and returns to the light component removal tower (4) after heating, and part of it enters the ethyl methyl carbonate distillation tower (5); (5), the ethyl methyl carbonate vapor distilled from the ethyl methyl carbonate distillation tower (5) enters the distillation tower condenser (5-3), and the ethyl methyl carbonate condensed by the distillation tower condenser (5-3) enters the ethyl methyl carbonate receiving tank (5-4). The ethyl methyl carbonate in the ethyl methyl carbonate receiving tank (5-4) passes through the ethyl methyl carbonate pump (5-5), part of which enters the ethyl methyl carbonate distillation tower (5) as reflux, and part of which directly enters the ethyl methyl carbonate storage tank (5-6); the bottom liquid of the ethyl methyl carbonate distillation tower (5) passes through the ethyl methyl carbonate distillation tower bottom pump (5-7), part of which enters the distillation tower reboiler (5-1) to be heated and then returns to the ethyl methyl carbonate distillation tower (5), and the remaining bottom liquid is returned to the batching tank (1) as a recycled material.
6. The method for producing ethyl methyl carbonate using an impinging flow transesterification tubular reactor according to claim 5, characterized in that: The reaction temperature in the batching tank (1) in step (1) is 85°C to 90°C, the pressure is 0.22MPa to 0.26MPa, the catalyst is 0.2% to 0.4% of the mass of dimethyl carbonate, and the residence time of the material is 0.5h to 0.75h; The molar ratio of ethanol to dimethyl carbonate added in the ethanol vaporizer (2-7) in step (2) is (1.2-1.4): 1, the temperature in the tubular reactor (2-5) is 105°C-110°C, and the pressure is 0.42MPa-0.48MPa; The post-esterification tower (3) in step (3) has a top temperature of 64°C, a top pressure of atmospheric pressure, a bottom temperature of 90°C to 110°C, a reflux ratio of 1.0 to 1.5, and a residence time of the material of 1.0h to 1.5h; The light component removal tower (4) in step (4) has a top temperature of 60°C, a top pressure of 0.035 MPa, a bottom temperature of 75°C to 85°C, and a reflux ratio of 1; The ethyl methyl carbonate distillation tower (5) in step (5) has a top temperature of 66°C, a top pressure of 0.026 MPa, a bottom temperature of 80°C to 85°C, and a reflux ratio of 2.
