Equipment for producing high-purity methyl ethyl ether

Abstract

The utility model discloses equipment for producing high-purity methyl ethyl ether, which relates to the field of synthesis of chemical compounds and comprises a reaction device, a heating component, a cold bath tank, a crude product receiving tank, a heavy component removal tower, a light component removal tower, a first reboiler, a second reboiler, a first condenser, a second condenser, a recovery tank, a product receiving tank and a controller, raw materials including sodium methoxide and halogenated ethane directly react under the anhydrous condition, a catalyst is not needed, crude methyl ethyl ether is produced, then the crude methyl ethyl ether enters a heavy component removal tower, crude methyl ethyl ether gas with heavy components removed enters a light component removal tower from the top of the light component removal tower after being detected to be qualified through a first online analysis and detection component, light component removal rectification is conducted, and methyl ethyl ether is obtained. Gas-phase impurities at the top of the light component removal tower are analyzed through the second online analysis and detection part, when the gas-phase impurities are detected to be qualified, the methyl ethyl ether product enters the product receiving tank, and then the high-purity methyl ethyl ether product is produced through continuous rectification, so that the product purity is high, the reaction temperature is low, the energy consumption is reduced, the reaction yield is high, and the production cost is low.

Description

Technical Field

[0001] The utility model relates to the field of chemical compound synthesis, in particular to a device for producing high-purity methyl ethyl ether. Background Art

[0002] Methyl ether is an organic compound with the chemical formula C 3 H 8 O, a colorless gas with a medicinal smell at room temperature and pressure, soluble in water, miscible in ethanol and ether, and mainly used as an anesthetic. The synthesis of symmetrical ethers such as methyl ether and ethyl ether can be easily achieved by using the corresponding alcohol catalytic dehydration, and the yield is also very high, but asymmetrical ethers are also called mixed ethers. The synthesis of such products uses the corresponding mixed alcohol dehydration, and the yield is low.

[0003] Among them, one method is to use "solid phosphoric acid" catalyst, methanol and ethanol mixed alcohol as raw materials to synthesize methyl ethyl ether, and the equimolar mixture of methanol and ethanol is reacted on solid phosphoric acid at 336° and 60 atmospheres for 1.33 hours. The reaction formula is: CH 3 OH+C 2 H 5 OH→CH 3 OC 2 H 5 The composition of the final product is shown in Table 1. The by-products include ethylene, methyl ether and ethyl ether.

[0004] Table 1. Experimental results of synthesizing methyl ethyl ether from mixed alcohols

[0005] Compound Name weight Methyl ether 18.4 g Methyl ethyl ether 22.4 g Ether 5.6 g the remaining 1.6 g Non-condensable gas 11.8L (22°C, 750mmHg)

[0006] The advantage of this method is that the raw materials are easily available, only methanol and ethanol, and the raw materials are cheap. However, the disadvantages are that the reaction temperature and pressure are very high, the yield is low, and the product components are many, which increases the difficulty and cost of purification.

[0007] Another method is to form methyl ethyl ether by mixed ether exchange of methyl ether and ethyl ether. Equimolar ethyl ether and methyl ether are heated in an autoclave at 150°C for 6 hours under the action of a catalyst to obtain methyl ethyl ether. The reaction formula is: CH 3 OCH 3 +C 2 H 5 OC 2 H 5 →CH 3 OC 2 H 5 The composition of the reactants is shown in Table 2 below.

[0008] Table 2. Experimental results of simple ether synthesis of methyl ethyl ether

[0009] Compound Name weight Number of moles Ethylene 1.8 g 0.06 Methyl ether 18.7 g 0.41 Ether 27.5 g 0.25 Methyl ethyl ether 15g 0.37

[0010] The above two methods of synthesizing methyl ethyl ether have very low yields and are not suitable for large-scale production. Utility Model Content

[0011] In order to solve the above technical problems, the utility model provides a device for producing high-purity methyl ethyl ether, which has high product purity, low reaction temperature, reduced energy consumption, high reaction yield and low production cost.

[0012] To achieve the above purpose, the utility model provides the following solutions:

[0013] The utility model provides an apparatus for producing high-purity methyl ethyl ether, comprising a reaction device, a heating component, a cold bath tank, a crude product receiving tank, a de-weighting tower, a de-lightening tower, a first reboiler, a second reboiler, a first condenser, a second condenser, a recovery tank, a product receiving tank and a controller, wherein the crude product receiving tank is arranged in the cold bath tank, the heating component is arranged in the crude product receiving tank, the reaction device is connected with the crude product receiving tank through a first pipeline; the crude product receiving tank is connected with one side of the lower part of the de-weighting tower through a second pipeline, a first regulating valve is arranged on the second pipeline, the first reboiler is arranged on the other side of the lower part of the de-weighting tower, the top of the de-weighting tower is connected with a first inlet of the first condenser through a third pipeline, the reflux port of the first condenser is connected with one side of the upper part of the de-weighting tower through the first reflux pipeline, the first outlet of the first condenser is connected with one side of the de-lightening tower through a fourth pipeline, and a first online Analysis and detection components and a second regulating valve, the first online analysis and detection component is arranged at one end close to the first outlet of the first condenser; the second reboiler is arranged on one side of the lower part of the light removal tower, the top of the light removal tower is connected to the first inlet of the second condenser through the fifth pipeline, the reflux port of the second condenser is connected to one side of the upper part of the light removal tower through the second reflux pipeline, the first outlet of the second condenser is connected to the recovery tank through the sixth pipeline, the second online analysis and detection component and the third regulating valve are arranged on the sixth pipeline, the second online analysis and detection component is arranged at one end close to the light removal tower, the bottom of the light removal tower is connected to the product receiving tank through the seventh pipeline, and the fourth regulating valve is arranged on the seventh pipeline; the first regulating valve, the second regulating valve, the third regulating valve, the fourth regulating valve, the first online analysis and detection component and the second online analysis and detection component are all connected to the controller.

[0014] Preferably, the reaction device includes a reactor, a stirring paddle, a motor and an elevated tank, the outside of the reactor is provided with a heating jacket, the stirring paddle is provided in the reactor, the motor is provided outside the top of the reactor, the power output shaft of the motor is connected to the stirring paddle, the elevated tank is provided on one side outside the top of the reactor, the elevated tank is connected to one side of the top of the reactor through a connecting pipeline, the other side of the top of the reactor is connected to the top of the crude product receiving tank through the first pipeline, and the motor is connected to the controller.

[0015] Preferably, a first flow meter is provided on the second pipeline, a second flow meter is provided on the fourth pipeline, a third flow meter is provided on the sixth pipeline, a fourth flow meter is provided on the seventh pipeline, a fifth flow meter is provided on the first return pipeline, and a sixth flow meter is provided on the second return pipeline, and the first flow meter, the second flow meter, the third flow meter, the fourth flow meter, the fifth flow meter and the sixth flow meter are all connected to the controller.

[0016] Preferably, a first pressure sensor is provided at the top of the deweighting tower, the second inlet of the first condenser is connected to the first refrigerant inlet pipe, a first refrigerant regulating valve is provided on the first refrigerant inlet pipe, and the first pressure sensor and the first refrigerant regulating valve are both connected to the controller.

[0017] Preferably, it also includes a first heater and a first hot agent regulating valve, the inlet of the lower end of the first reboiler is connected to the bottom of the deweighting tower through a first connecting pipe, the outlet of the upper end of the first reboiler is connected to one side of the lower part of the deweighting tower through a second connecting pipe, a third pressure sensor is arranged at the bottom of the deweighting tower, the hot agent inlet and the hot agent outlet of the first reboiler are connected through a first intermediate pipe, the first heater and the first hot agent regulating valve are arranged on the first intermediate pipe, the first hot agent regulating valve is arranged between the hot agent inlet of the first reboiler and the first heater, and the first heater, the first hot agent regulating valve and the third pressure sensor are all connected to the controller.

[0018] Preferably, a second pressure sensor is provided at the top of the light removal tower, the second inlet of the second condenser is connected to the second refrigerant inlet pipe, a second refrigerant regulating valve is provided on the second refrigerant inlet pipe, and the second pressure sensor and the second refrigerant regulating valve are both connected to the controller.

[0019] Preferably, it also includes a second heater and a second heat agent regulating valve, the inlet of the lower end of the second reboiler is connected to the bottom of the light-removing tower through a third connecting pipe, the outlet of the upper end of the second reboiler is connected to one side of the lower part of the light-removing tower through a fourth connecting pipe, a fourth pressure sensor is arranged at the bottom of the light-removing tower, the heat agent inlet and the heat agent outlet of the second reboiler are connected through a second intermediate pipe, the second heater and the second heat agent regulating valve are arranged on the second intermediate pipe, the second heat agent regulating valve is arranged between the heat agent inlet of the second reboiler and the second heater, and the second heater, the second heat agent regulating valve and the fourth pressure sensor are all connected to the controller.

[0020] Preferably, it also includes a refrigeration circulation tank, a first cooling jacket, a third refrigerant inlet pipe and a third condenser, the first cooling jacket is arranged on the outside of the recovery tank, the third condenser is arranged on the top of the recovery tank, the two ends of the third refrigerant inlet pipe are respectively connected to the refrigeration circulation tank and the bottom of the first cooling jacket, the top of the first cooling jacket is connected to the inlet of the lower end of the third condenser, the outlet of the upper end of the third condenser is connected to the refrigeration circulation tank through the first outlet pipe, the third refrigerant inlet pipe is provided with a third refrigerant regulating valve, and the third refrigerant regulating valve is connected to the controller.

[0021] Preferably, it also includes a second cooling jacket, a fourth refrigerant inlet pipe and a fourth condenser, the second cooling jacket is arranged on the outside of the product receiving tank, the fourth condenser is arranged on the top of the product receiving tank, the two ends of the fourth refrigerant inlet pipe are respectively connected to the refrigeration cycle tank and the bottom of the second cooling jacket, the top of the second cooling jacket is connected to the inlet of the lower end of the fourth condenser, the outlet of the upper end of the fourth condenser is connected to the refrigeration cycle tank through the second outlet pipe, the fourth refrigerant inlet pipe is provided with a fourth refrigerant regulating valve, and the fourth refrigerant regulating valve is connected to the controller.

[0022] Compared with the prior art, the utility model has achieved the following technical effects:

[0023] The utility model of the equipment for producing high-purity methyl ethyl ether makes the raw material sodium methoxide and ethyl halide react directly under anhydrous conditions without the need for a catalyst to produce crude methyl ethyl ether, and then the crude methyl ethyl ether enters a de-heavy tower, and the crude methyl ethyl ether gas from which the heavy components are removed enters a de-light tower from the top of the de-light tower after being tested and qualified by a first online analysis and detection component, and is subjected to de-light distillation, and the gas phase impurities at the top of the de-light tower are analyzed by a second online analysis and detection component, and when the test is qualified, the methyl ethyl ether product enters a product receiving tank, and then a high-purity methyl ethyl ether product is produced through continuous distillation. The utility model has the advantages of high product purity, low reaction temperature, reduced energy consumption, high reaction yield, and low production cost. BRIEF DESCRIPTION OF THE DRAWINGS

[0024] In order to more clearly illustrate the embodiments of the utility model or the technical solutions in the prior art, the drawings required for use in the embodiments will be briefly introduced below. Obviously, the drawings described below are only some embodiments of the utility model. For ordinary technicians in this field, other drawings can be obtained based on these drawings without paying creative work.

[0025] Figure 1 The utility model provides a schematic diagram of the structure of the equipment for producing high-purity methyl ethyl ether.

[0026] Description of the accompanying drawings: 100, equipment for producing high-purity methyl ethyl ether; 1, reactor; 2, heating jacket; 3, motor; 4, stirring paddle; 5, high-level tank; 6, connecting pipeline; 7, first pipeline; 8, crude product receiving tank; 9, cold bath tank; 10, heating component; 11, second pipeline; 12, first regulating valve; 13, first flow meter; 14, deweighting tower; 15, third pipeline; 16, first condenser; 17, first reflux pipeline; 18, first pressure sensor; 19, first refrigerant regulating valve; 20, first reboiler; 21, first connecting pipe; 22, second connecting pipe; 23, first intermediate pipe; 24, first heater; 25, first hot agent regulating valve; 26, third pressure sensor; 27, fourth pipeline; 28, first online analysis and detection component; 29, second flow meter; 3 0. Second regulating valve; 31. Light removal tower; 32. Fifth pipeline; 33. Second condenser; 34. Second reflux pipeline; 35. Second pressure sensor; 36. Second refrigerant regulating valve; 37. Sixth pipeline; 38. Second online analysis and detection component; 39. Third flow meter; 40. Third regulating valve; 41. Recovery tank; 42. First cooling jacket; 43. Third condenser; 44. Seventh pipeline; 45. Fourth flow meter; 46. Fourth regulating valve; 47. Product receiving tank; 48. Second cooling jacket; 49. Fourth condenser; 50. Second reboiler; 51. Third connecting pipe; 52. Fourth connecting pipe; 53. Second intermediate pipe; 54. Second heater; 55. Second hot agent regulating valve; 56. Fourth pressure sensor; 57. Fifth flow meter; 58. Sixth flow meter. DETAILED DESCRIPTION

[0027] The following will be combined with the drawings in the embodiments of the utility model to clearly and completely describe the technical solutions in the embodiments of the utility model. Obviously, the described embodiments are only part of the embodiments of the utility model, not all of the embodiments. Based on the embodiments in the utility model, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the utility model.

[0028] The utility model aims to provide a device for producing high-purity methyl ethyl ether, which has high product purity, low reaction temperature, reduced energy consumption, high reaction yield and low production cost.

[0029] In order to make the above-mentioned purposes, features and advantages of the present invention more obvious and easy to understand, the present invention is further described in detail below in conjunction with the accompanying drawings and specific implementation methods.

[0030] like Figure 1 As shown, this embodiment provides an apparatus 100 for producing high-purity methyl ethyl ether, including a reaction device, a heating component 10, a cold bath tank 9, a crude product receiving tank 8, a de-weighting tower 14, a de-lightening tower 31, a first reboiler 20, a second reboiler 50, a first condenser 16, a second condenser 33, a recovery tank 41, a product receiving tank 47 and a controller. The crude product receiving tank 8 is arranged in the cold bath tank 9, the heating component 10 is arranged in the crude product receiving tank 8, the reaction device is connected to the crude product receiving tank 8 through a first pipeline 7, the cold bath tank 9 is used to place a refrigerant, and the heating component 10 is used to increase the liquid temperature in the crude product receiving tank 8, increase the pressure in the crude product receiving tank 8, and transport the crude methyl ethyl ether to the de-weighting tower 14 by pressure difference.

[0031] The crude product receiving tank 8 is connected to one side of the lower part of the deweighting tower 14 through the second pipeline 11. The deweighting tower 14 is used to remove heavy components in the crude methyl ethyl ether. The second pipeline 11 is provided with a first regulating valve 12. The other side of the lower part of the deweighting tower 14 is provided with a first reboiler 20. The first reboiler 20 is used to heat the bottom of the deweighting tower 14. The top of the deweighting tower 14 is connected to the first inlet of the first condenser 16 through the third pipeline 15. The reflux port of the first condenser 16 is connected to one side of the upper part of the deweighting tower 14 through the first reflux pipeline 17. The first outlet of the first condenser 16 is connected to one side of the lightness removing tower 31 through the fourth pipeline 27. The fourth pipeline 27 is provided with a first online analysis and detection component 28 and a second regulating valve 30. The first online analysis and detection component 28 is arranged at one end close to the first outlet of the first condenser 16.

[0032] The light-removing tower 31 is used to remove light components from the crude methyl ethyl ether. A second reboiler 50 is provided on one side of the lower part of the light-removing tower 31. The second reboiler 50 is used to heat the bottom of the light-removing tower 31. The top of the light-removing tower 31 is connected to the first inlet of the second condenser 33 through the fifth pipeline 32. The reflux port of the second condenser 33 is connected to one side of the upper part of the light-removing tower 31 through the second reflux pipeline 34. The first outlet of the second condenser 33 is connected to the recovery tank 41 through the sixth pipeline 37. The recovery tank 41 is used to recover the gas discharged from the top of the second condenser 33. The sixth pipeline 37 is provided with a second online analysis and detection component 38 and a third regulating valve 40. The second online analysis and detection component 38 is arranged at one end close to the light removal tower 31. The bottom of the light removal tower 31 is connected to the product receiving tank 47 through the seventh pipeline 44. The product receiving tank 47 is used to receive the methyl ethyl ether product. The seventh pipeline 44 is provided with a fourth regulating valve 46; the first regulating valve 12, the second regulating valve 30, the third regulating valve 40, the fourth regulating valve 46, the first online analysis and detection component 28 and the second online analysis and detection component 38 are all connected to the controller.

[0033] Specifically, the reaction device includes a reactor 1, a stirring paddle 4, a motor 3 and an elevated tank 5. A heating jacket 2 is provided on the outside of the reactor 1. The reactor 1 in this embodiment is a glass reactor 1 with a heating jacket 2. The heating jacket 2 is used to pass warm water to heat the liquid in the reactor 1. The stirring paddle 4 is arranged in the reactor 1. The motor 3 is arranged on the outside of the top of the reactor 1. The power output shaft of the motor 3 is connected to the stirring paddle 4. The elevated tank 5 is arranged on one side of the outside of the top of the reactor 1. The elevated tank 5 is connected to one side of the top of the reactor 1 through a connecting pipeline 6. The elevated tank 5 is used to add ethane halide. The other side of the top of the reactor 1 is connected to the top of a crude product receiving tank 8 through a first pipeline 7. The bottom of the crude product receiving tank 8 is connected to one side of the lower part of a deweighting tower 14 through a second pipeline 11. The motor 3 is connected to a controller. When the reaction is carried out, the controller controls the motor 3 to turn on so that the stirring paddle 4 performs stirring to improve the reaction efficiency.

[0034] In order to monitor the flow rate intuitively, a first flow meter 13 is provided on the second pipeline 11, a second flow meter 29 is provided on the fourth pipeline 27, a third flow meter 39 is provided on the sixth pipeline 37, a fourth flow meter 45 is provided on the seventh pipeline 44, a fifth flow meter 57 is provided on the first return pipeline 17, and a sixth flow meter 58 is provided on the second return pipeline 34. The first flow meter 13, the second flow meter 29, the third flow meter 39, the fourth flow meter 45, the fifth flow meter 57 and the sixth flow meter 58 are all connected to the controller.

[0035] During operation, the first flowmeter 13 is used to monitor the production flow rate of crude methyl ethyl ether gas, and cooperates with the first regulating valve 12 to adjust the production flow rate of crude methyl ethyl ether; the second flowmeter 29 is used to monitor the production flow rate of crude methyl ethyl ether gas after removing heavy components, and cooperates with the second regulating valve 30 to adjust the production flow rate of crude methyl ethyl ether gas after removing heavy components; the third flowmeter 39 is used to monitor the flow rate of the recovered product containing light components produced from the top of the light removal tower 31, and cooperates with the third regulating valve 40 to adjust the flow rate of the recovered product containing light components produced; the fourth flowmeter 45 is used to monitor the production flow rate of the methyl ethyl ether product, and cooperates with the fourth regulating valve 46 to adjust the production flow rate of the methyl ethyl ether product; the fifth flowmeter 57 is used to monitor the reflux flow rate of the heavy removal tower 14; the sixth flowmeter 58 is used to monitor the reflux flow rate of the light removal tower 31.

[0036] A first pressure sensor 18 is provided at the top of the deweighting tower 14, a second inlet of the first condenser 16 is connected to a first refrigerant inlet pipe, a first refrigerant regulating valve 19 is provided on the first refrigerant inlet pipe, the second inlet and the second outlet of the first condenser 16 are used for the inflow and outflow of the brine, respectively, and the first pressure sensor 18 and the first refrigerant regulating valve 19 are both connected to the controller. The first pressure sensor 18 and the first refrigerant regulating valve 19 cooperate to adjust the tower top operating pressure of the deweighting tower 14.

[0037] In this embodiment, the first heater 24 and the first heat agent regulating valve 25 are also included. The inlet at the lower end of the first reboiler 20 is connected to the bottom of the de-weighting tower 14 through the first connecting pipe 21, and the outlet at the upper end of the first reboiler 20 is connected to one side of the lower part of the de-weighting tower 14 through the second connecting pipe 22. The bottom of the de-weighting tower 14 is provided with a third pressure sensor 26. The heat agent inlet and the heat agent outlet of the first reboiler 20 are connected through the first intermediate pipe 23. The first heater 24 and the first heat agent regulating valve 25 are provided on the first intermediate pipe 23. The first heat agent regulating valve 25 is provided between the heat agent inlet of the first reboiler 20 and the first heater 24. The first heater 24, the first heat agent regulating valve 25 and the third pressure sensor 26 are all connected to the controller. The first heater 24, the first heat agent regulating valve 25 and the third pressure sensor 26 cooperate to adjust the tower bottom operating pressure of the de-weighting tower 14.

[0038] A second pressure sensor 35 is provided at the top of the light-removing tower 31, a second inlet of the second condenser 33 is connected to a second refrigerant inlet pipe, a second refrigerant regulating valve 36 is provided on the second refrigerant inlet pipe, a second inlet and a second outlet of the second condenser 33 are used for the inflow and outflow of the refrigerant, respectively, and the second pressure sensor 35 and the second refrigerant regulating valve 36 are both connected to the controller. The second pressure sensor 35 and the second refrigerant regulating valve 36 cooperate to adjust the tower top operating pressure of the light-removing tower 31.

[0039] In this embodiment, a second heater 54 and a second heat agent regulating valve 55 are also included. The inlet at the lower end of the second reboiler 50 is connected to the bottom of the light-removing tower 31 through a third connecting pipe 51, and the outlet at the upper end of the second reboiler 50 is connected to one side of the lower part of the light-removing tower 31 through a fourth connecting pipe 52. A fourth pressure sensor 56 is provided at the bottom of the light-removing tower 31. The heat agent inlet and the heat agent outlet of the second reboiler 50 are connected through a second intermediate pipe 53. The second intermediate pipe 53 is provided with a second heater 54 and a second heat agent regulating valve 55. The second heat agent regulating valve 55 is provided between the heat agent inlet of the second reboiler 50 and the second heater 54. The second heater 54, the second heat agent regulating valve 55 and the fourth pressure sensor 56 are all connected to the controller. The second heater 54, the second heat agent regulating valve 55 and the fourth pressure sensor 56 cooperate to adjust the operating pressure of the bottom of the light-removing tower 31.

[0040] In this specific embodiment, the tower bottom volume of the de-weighting tower 14 is 60L, the tower diameter is 108mm, the wall thickness is 6mm, the tower height is 14m, the packing height is 11.5m, and 316L stainless steel random packing is used. The tower bottom volume of the de-lightness tower 31 is 48L, the tower diameter is 89mm, the wall thickness is 5mm, the tower height is 12m, the packing height is 10m, and 316L stainless steel random packing is used.

[0041] In this specific embodiment, the first online analysis and detection component 28 and the second online analysis and detection component 38 are both online gas chromatographs.

[0042] In this specific embodiment, the first regulating valve 12, the second regulating valve 30, the third regulating valve 40 and the fourth regulating valve 46 are all pneumatic regulating valves. In order to facilitate manual control of the production of crude methyl ethyl ether, a manual valve is provided on the second pipeline 11 in this embodiment.

[0043] The present embodiment also includes a refrigeration cycle tank, a first cooling jacket 42, a third refrigerant inlet pipe and a third condenser 43, wherein the first cooling jacket 42 is arranged outside the recovery tank 41, the third condenser 43 is arranged at the top of the recovery tank 41, the two ends of the third refrigerant inlet pipe are respectively connected to the bottom of the refrigeration cycle tank and the first cooling jacket 42, the top of the first cooling jacket 42 is connected to the inlet of the lower end of the third condenser 43, the outlet of the upper end of the third condenser 43 is connected to the refrigeration cycle tank through the first outlet pipe, and the third refrigerant inlet pipe is provided with a third refrigerant regulating valve, which is connected to the controller. The flow of the refrigerant entering the third cooling jacket is adjusted by adjusting the third refrigerant regulating valve, so as to adjust the temperature and pressure of the recovery tank 41.

[0044] The present embodiment also includes a second cooling jacket 48, a fourth refrigerant inlet pipe and a fourth condenser 49. The second cooling jacket 48 is arranged outside the product receiving tank 47, the fourth condenser 49 is arranged at the top of the product receiving tank 47, the two ends of the fourth refrigerant inlet pipe are respectively connected to the refrigeration cycle tank and the bottom of the second cooling jacket 48, the top of the second cooling jacket 48 is connected to the inlet of the lower end of the fourth condenser 49, the outlet of the upper end of the fourth condenser 49 is connected to the refrigeration cycle tank through the second outlet pipe, and the fourth refrigerant inlet pipe is provided with a fourth refrigerant regulating valve, which is connected to the controller. The flow of the refrigerant entering the fourth cooling jacket is adjusted by adjusting the fourth refrigerant regulating valve, so as to adjust the temperature and pressure of the product receiving tank 47.

[0045] Specifically, the cold source of the refrigeration cycle tank, the first condenser 16 and the second condenser 33 is realized by a complete set of refrigeration units, the temperature is controllable, the operating temperature is 0°C ~ 20°C, and the coolant is ethylene glycol aqueous solution, that is, the cold source equipment in this embodiment is simple to operate and the temperature control is stable.

[0046] This embodiment also provides a process based on the device 100 for producing high-purity methyl ethyl ether, comprising the following steps:

[0047] Step 1: Sodium methoxide is put into the reaction device under nitrogen protection, and then methanol solvent is added and heated to make the solution temperature in the reaction device 28°C-32°C, and ethyl halide is added under stirring; that is, in this embodiment, sodium methoxide and ethyl halide are used as raw materials to synthesize methyl ethyl ether product, and the solvent is methanol. In this embodiment, water at 32°C-35°C is passed into the heating jacket 2 to heat the raw materials in the reactor 1.

[0048] Specifically, the molar ratio of sodium methoxide to ethane halide is 1:1.2-1.3. From the perspective of product yield, this molar ratio can obtain the highest yield under the condition of the lowest raw material cost.

[0049] Since the material temperature is lower than 28° C., the reaction is very slow, and the temperature is higher than 32° C., the byproduct ethylene increases and the yield decreases. Therefore, in this embodiment, the reaction temperature of sodium methoxide and ethyl halide is controlled at 28° C. to 32° C., preferably 29° C. to 30° C. The ethyl halide can be ethyl bromide and ethyl chloride, preferably ethyl bromide.

[0050] Step 2: The gas generated by the reaction enters the crude product receiving tank 8, and a refrigerant is added to the cold bath tank 9 for cooling, so that the crude methyl ethyl ether gas is liquefied. Specifically, in order for the reaction to proceed smoothly, the crude methyl ethyl ether gas generated by the reaction must be quickly liquefied after entering the crude product receiving tank 8, and the pressure in the crude product receiving tank 8 is maintained at a slightly positive pressure, and dry ice is usually added to the cold bath tank 9. When the crude methyl ethyl ether in the crude product receiving tank 8 is full, the reaction is stopped, and the crude methyl ethyl ether is transferred to the deweighting tower 14 for low-temperature distillation, and the dry ice needs to be removed at this time.

[0051] Specifically, sodium methoxide is put into a reactor 1 under nitrogen protection, and then methanol is added. The raw materials in the reactor 1 are stirred by a stirring paddle 4 at a rotation speed of 4r / min to 5r / min, and ethyl bromide is slowly added under stirring. When the concentration of ethyl bromide in the sodium methoxide solution of methanol reaches a certain level, the reaction begins, and gas slowly comes out, and the crude ethyl methyl ether gas enters a crude product receiving tank 8. Dry ice is added to a cold bath tank 9 outside the crude product receiving tank 8 for refrigeration, and the crude ethyl methyl ether gas is liquefied in the crude product receiving tank 8 to obtain crude ethyl methyl ether.

[0052] In this specific embodiment, the 100L reactor 1 is purged with nitrogen to ensure that the reactor 1 is in an anhydrous state. Under nitrogen protection, 60KG of 50% (Wt%) sodium methoxide methanol solution is added, and then 30L of dehydrated methanol is added. The heating jacket 2 is heated by warm water circulation, and the water temperature is controlled at 32°C to 35°C to maintain the temperature of the sodium methoxide solution at 28°C to 32°C. After constant temperature, stirring is turned on and 73.2KG of ethyl bromide (20% excess) is slowly added dropwise. Ethyl bromide is added to the high-level tank 5 and added by pressure difference. The reaction continuously produces methyl ethyl ether gas.

[0053] When the raw materials in the reactor 1 are exhausted and no more gas is produced, the collection is stopped. The experimental results show that 20.5 kg of methyl ethyl ether is obtained in each reactor, with a yield of 71%. This is carried out three times in a row, and the crude product receiving tank is 8 to 61.5 kg before the next step of distillation. After sampling and analysis, the composition of the crude methyl ethyl ether is 0.1% ethylene, 2.58% ethyl bromide, 1.35% methanol, and 95.95% methyl ethyl ether.

[0054] Step 3: After the crude product receiving tank 8 has been collected for a period of time, the refrigerant in the cold bath tank 9 is removed, the first regulating valve 12 is opened, and the heating component 10 is opened to increase the temperature and pressure, so that the pressure in the crude product receiving tank 8 reaches 0.3 MPa, and the crude methyl ethyl ether is pressed into the deweighting tower 14 by the pressure difference, and the first reboiler 20 on the lower side of the deweighting tower 14 starts to work to perform deweighting distillation, which mainly removes the heavy components of ethyl bromide and methanol impurities; the second regulating valve 30 is opened to remove the heavy components of the crude methyl ethyl ether. The ether gas enters the first condenser 16 from the top of the de-weighting tower 14, and the liquid phase material formed after cooling in the first condenser 16 is refluxed to the upper part of the de-weighting tower 14 through the first reflux pipeline 17. The crude methyl ethyl ether gas remaining after cooling and removing the heavy components enters the de-weighting tower 31 from the top of the de-weighting tower 31 after being tested and qualified by the first online analysis and detection component 28, and the second reboiler 50 on the lower side of the de-weighting tower 31 starts to work to perform de-weighting distillation, and the de-weighting distillation mainly removes ethylene and air component N 2 , O 2 , CO 2 , CO, CH 4 Specifically, the first online analysis and detection component 28 analyzes the gas-phase impurities at the top of the de-heavy tower 14, and when the impurities ethyl bromide and methanol are qualified, they are continuously extracted and enter the de-light tower 31, and the reflux ratio is controlled at 15-20:1.

[0055] In this embodiment, the heating component 10 in the crude product receiving tank 8 is a heating coil, which is used to pass a hot agent with a temperature of 40°C to 45°C, thereby increasing the liquid temperature and pressure in the crude product receiving tank 8, so as to facilitate the crude methyl ethyl ether to be pressed into the deweighting tower 14 for distillation and purification.

[0056] It should be noted that the crude product receiving tank 8 can be provided in two sets. When the first set is full, the other set can be activated, which is more conducive to operation.

[0057] Specifically, the heating temperature of the first reboiler 20 is 45°C to 60°C by controlling the first heater 24, the third pressure sensor 26 is used to monitor the operating pressure of the bottom of the de-weighting tower 14, and the operating pressure of the bottom of the de-weighting tower 14 can be controlled by controlling the first hot agent regulating valve 25. The first condenser 16 uses an aqueous solution of ethylene glycol as a refrigerant, the temperature is controlled at 0°C to 20°C, and the reflux ratio is controlled at 15 to 20:1. The first pressure sensor 18 is used to monitor the top operating pressure of the de-weighting tower 14, and the top operating pressure of the de-weighting tower 14 can be controlled by controlling the first refrigerant regulating valve 19. In this embodiment, the top temperature of the de-weighting tower 14 is 25°C to 30°C, the bottom operating pressure of the de-weighting tower 14 is controlled at 0.3MPa to 0.35MPa, and the top operating pressure is within 0.03MPa lower than the bottom operating pressure.

[0058] Specifically, the heating temperature of the second reboiler 50 is 45°C to 60°C by controlling the second heater 54, the fourth pressure sensor 56 is used to monitor the tower bottom operating pressure of the lightness removal tower 31, and the tower bottom operating pressure of the lightness removal tower 31 can be controlled by controlling the second hot agent regulating valve 55. The second condenser 33 uses an aqueous solution of ethylene glycol as a coolant, the temperature is controlled at 0°C to 20°C, and the reflux ratio is controlled at 15 to 20:1. The second pressure sensor 35 is used to monitor the tower top operating pressure of the lightness removal tower 31, and the tower top operating pressure of the lightness removal tower 31 can be controlled by controlling the second refrigerant regulating valve 36. In this embodiment, the tower top temperature of the lightness removal tower 31 is 20°C to 25°C, the tower bottom operating pressure of the lightness removal tower 31 is controlled at 0.2MPa to 0.25MPa, and the tower top operating pressure is within 0.03MPa lower than the tower bottom operating pressure.

[0059] In this specific embodiment, the pressure difference between the bottom operating pressure of the heavy removal tower 14 and the bottom operating pressure of the light removal tower 31 is about 0.1 MPa.

[0060] Step 4, open the third regulating valve 40, the recovery product containing light components extracted from the top of the light removal tower 31 enters the second condenser 33, the liquid phase material formed after cooling in the second condenser 33 flows back to the upper part of the light removal tower 31 through the second reflux pipeline 34, and the recovery product containing light components remaining after cooling enters the recovery tank 41, and the recovery product containing light components can be subjected to secondary distillation. The gas phase impurities at the top of the light removal tower 31 are analyzed by the second online analysis and detection component 38. When the detection is qualified, that is, when the impurity ethylene and the air component N 2 , O 2 , CO 2 , CO, CH 4 After passing the test, the fourth regulating valve 46 is opened and the third regulating valve 40 is closed, so that the methyl ethyl ether product enters the product receiving tank 47. The purity of the obtained methyl ethyl ether product is 99.95% to 99.99%. Specifically, the composition of the methyl ethyl ether product is: methanol <50ppm, ethyl bromide <30ppm, N 2 <3ppm,O 2 <0.5ppm, CO 2 <0.5ppm、CO<0.5ppm、CH 4 <0.5ppm, methyl ethyl ether>99.99%.

[0061] In this specific embodiment, the pressure difference between the lightness removal tower 31 and the recovery tank 41 and the product receiving tank 47 is 0.03MPa to 0.05MPa, thereby ensuring the continuity of the entire process.

[0062] In this embodiment, the raw material sodium methoxide and ethyl halide react directly under anhydrous conditions without a catalyst to produce crude methyl ethyl ether, and then the crude methyl ethyl ether enters the de-heaving tower 14, and the crude methyl ethyl ether gas from which the heavy components are removed enters the de-lightening tower 31 from the top of the de-lightening tower 31 after being detected as qualified by the first online analysis and detection component 28, and is subjected to de-lightening rectification, and the gas phase impurities at the top of the de-lightening tower 31 are analyzed by the second online analysis and detection component 38, and when the detection is qualified, the methyl ethyl ether product enters the product receiving tank 47, and then a high-purity methyl ethyl ether product is produced by continuous rectification, so that the product purity is high, the reaction temperature is low, the energy consumption is reduced, the reaction yield is high, and the production cost is low. It can be seen that in this embodiment, low-toxic and low-corrosive raw materials are selected, and a high-yield final product methyl ethyl ether is obtained by Williamson reaction, the synthesis conditions are mild, the method is simple and easy, and it is conducive to the large-scale production of methyl ethyl ether.

[0063] This specification uses specific examples to illustrate the principles and implementation methods of the utility model. The above examples are only used to help understand the method and core idea of ​​the utility model. At the same time, for those skilled in the art, according to the idea of ​​the utility model, there will be changes in the specific implementation methods and application scope. In summary, the content of this specification should not be understood as limiting the utility model.

Claims

1. A device for producing high-purity methyl ethyl ether, characterized in that: The invention comprises a reaction device, a heating component, a cold bath, a crude product receiving tank, a de-weighting tower, a de-lighting tower, a first reboiler, a second reboiler, a first condenser, a second condenser, a recovery tank, a product receiving tank and a controller, wherein the crude product receiving tank is arranged in the cold bath, the heating component is arranged in the crude product receiving tank, the reaction device is connected to the crude product receiving tank through a first pipeline; the crude product receiving tank is connected to one side of the lower part of the de-weighting tower through a second pipeline, a first regulating valve is arranged on the second pipeline, the first reboiler is arranged on the other side of the lower part of the de-weighting tower, the top of the de-weighting tower is connected to the first inlet of the first condenser through a third pipeline, the reflux port of the first condenser is connected to one side of the upper part of the de-weighting tower through the first reflux pipeline, the first outlet of the first condenser is connected to one side of the de-lighting tower through a fourth pipeline, and a first online analysis and detection component and a second regulating valve are arranged on the fourth pipeline. throttle valve, the first online analysis and detection component is arranged at one end close to the first outlet of the first condenser; the second reboiler is arranged on one side of the lower part of the light removal tower, the top of the light removal tower is connected to the first inlet of the second condenser through the fifth pipeline, the reflux port of the second condenser is connected to one side of the upper part of the light removal tower through the second reflux pipeline, the first outlet of the second condenser is connected to the recovery tank through the sixth pipeline, the second online analysis and detection component and the third regulating valve are arranged on the sixth pipeline, the second online analysis and detection component is arranged at one end close to the light removal tower, the bottom of the light removal tower is connected to the product receiving tank through the seventh pipeline, and the fourth regulating valve is arranged on the seventh pipeline; the first regulating valve, the second regulating valve, the third regulating valve, the fourth regulating valve, the first online analysis and detection component and the second online analysis and detection component are all connected to the controller.

2. The device for producing high-purity methyl ethyl ether according to claim 1, characterized in that: The reaction device includes a reactor, a stirring paddle, a motor and an elevated tank. A heating jacket is arranged outside the reactor. The stirring paddle is arranged in the reactor. The motor is arranged outside the top of the reactor. The power output shaft of the motor is connected to the stirring paddle. The elevated tank is arranged on one side outside the top of the reactor. The elevated tank is connected to one side of the top of the reactor through a connecting pipeline. The other side of the top of the reactor is connected to the top of the crude product receiving tank through the first pipeline. The motor is connected to the controller.

3. The device for producing high-purity methyl ethyl ether according to claim 1, characterized in that: A first flow meter is arranged on the second pipeline, a second flow meter is arranged on the fourth pipeline, a third flow meter is arranged on the sixth pipeline, a fourth flow meter is arranged on the seventh pipeline, a fifth flow meter is arranged on the first return pipeline, and a sixth flow meter is arranged on the second return pipeline. The first flow meter, the second flow meter, the third flow meter, the fourth flow meter, the fifth flow meter and the sixth flow meter are all connected to the controller.

4. The device for producing high-purity methyl ethyl ether according to claim 1, characterized in that: A first pressure sensor is arranged on the top of the deweighting tower, a second inlet of the first condenser is connected to a first refrigerant inlet pipe, a first refrigerant regulating valve is arranged on the first refrigerant inlet pipe, and both the first pressure sensor and the first refrigerant regulating valve are connected to the controller.

5. The device for producing high-purity methyl ethyl ether according to claim 1, characterized in that: It also includes a first heater and a first hot agent regulating valve. The inlet of the lower end of the first reboiler is connected to the bottom of the deweighting tower through a first connecting pipe, and the outlet of the upper end of the first reboiler is connected to one side of the lower part of the deweighting tower through a second connecting pipe. A third pressure sensor is arranged at the bottom of the deweighting tower. The hot agent inlet and the hot agent outlet of the first reboiler are connected through a first intermediate pipe. The first heater and the first hot agent regulating valve are arranged on the first intermediate pipe. The first hot agent regulating valve is arranged between the hot agent inlet of the first reboiler and the first heater. The first heater, the first hot agent regulating valve and the third pressure sensor are all connected to the controller.

6. The equipment for producing high-purity methyl ethyl ether according to claim 1, characterized in that: A second pressure sensor is arranged at the top of the light removal tower, a second inlet of the second condenser is connected to a second refrigerant inlet pipe, a second refrigerant regulating valve is arranged on the second refrigerant inlet pipe, and both the second pressure sensor and the second refrigerant regulating valve are connected to the controller.

7. The device for producing high-purity methyl ethyl ether according to claim 1, characterized in that: It also includes a second heater and a second hot agent regulating valve. The inlet at the lower end of the second reboiler is connected to the bottom of the light-removing tower through a third connecting pipe, and the outlet at the upper end of the second reboiler is connected to one side of the lower part of the light-removing tower through a fourth connecting pipe. A fourth pressure sensor is arranged at the bottom of the light-removing tower. The hot agent inlet and the hot agent outlet of the second reboiler are connected through a second intermediate pipe. The second heater and the second hot agent regulating valve are arranged on the second intermediate pipe. The second hot agent regulating valve is arranged between the hot agent inlet of the second reboiler and the second heater. The second heater, the second hot agent regulating valve and the fourth pressure sensor are all connected to the controller.

8. The device for producing high-purity methyl ethyl ether according to claim 1, characterized in that: It also includes a refrigeration circulation tank, a first cooling jacket, a third refrigerant inlet pipe and a third condenser, wherein the first cooling jacket is arranged on the outside of the recovery tank, the third condenser is arranged on the top of the recovery tank, the two ends of the third refrigerant inlet pipe are respectively connected to the bottom of the refrigeration circulation tank and the first cooling jacket, the top of the first cooling jacket is connected to the inlet of the lower end of the third condenser, the outlet of the upper end of the third condenser is connected to the refrigeration circulation tank through the first outlet pipe, the third refrigerant inlet pipe is provided with a third refrigerant regulating valve, and the third refrigerant regulating valve is connected to the controller.

9. The device for producing high-purity methyl ethyl ether according to claim 8, characterized in that: It also includes a second cooling jacket, a fourth refrigerant inlet pipe and a fourth condenser, the second cooling jacket is arranged on the outside of the product receiving tank, the fourth condenser is arranged on the top of the product receiving tank, the two ends of the fourth refrigerant inlet pipe are respectively connected to the refrigeration cycle tank and the bottom of the second cooling jacket, the top of the second cooling jacket is connected to the inlet of the lower end of the fourth condenser, the outlet of the upper end of the fourth condenser is connected to the refrigeration cycle tank through the second outlet pipe, the fourth refrigerant inlet pipe is provided with a fourth refrigerant regulating valve, and the fourth refrigerant regulating valve is connected to the controller.

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