Etherification reaction device

Abstract

According to the etherification reaction device provided by the invention, the centrifugal machine is arranged to centrifugally separate the reaction liquid after the reaction in the reaction kettle to obtain the filter cake and the mother liquor, and the mother liquor and the washing liquid with the washed filter cake in the washing kettle are mixed and then transferred into the desolventizing kettle for desolventizing treatment; and respectively transferring the solvent obtained by desolventizing and the filtrate obtained by filter pressing after washing the crude product into corresponding storage tanks for recovery. The etherification reaction device for the flumioxazin intermediate, which is provided by the invention, is easy to implement through the matched use of the equipment, and has the advantages that the reaction process is easy to control, the pollution in the treatment process is less, the reaction solvent can be recycled, and resources are saved.

Description

Technical Field

[0001] This application relates to the technical field of organic synthesis, and particularly to an etherification reaction device. Background Art

[0002] Flumioxazin is a broad-spectrum pre-emergence and post-emergence herbicide selective for soybeans. It has rapid burning activity against weeds, a relatively broad herbicidal spectrum, and is suitable for crop fields such as soybeans, peanuts, orchards, etc. Annual broad-leaved weeds and some gramineous weeds such as Portulaca oleracea, Polygonum spp., Commelina communis, Setaria viridis, Chenopodium spp., Eleusine indica, etc. are its main control targets. It has the characteristics of high efficiency, low toxicity, strong selectivity, safety for non-target organisms, and little environmental pollution. Therefore, this herbicide is widely used in agricultural production and has great economic value.

[0003] Its synthetic route mainly uses 2,4-difluoronitrobenzene as the starting material to obtain 2-nitro-5-fluorophenol, and then etherifies it with haloacetic acid ester, followed by iron-acid reduction and cyclization, nitration with mixed acid, condensation with 3-bromopropyne, iron-acid reduction, reaction with 3,4,5,6-tetrahydrophthalic anhydride, and finally obtaining the target product flumioxazin.

[0004] In the above reaction process, the etherification reaction of 2-nitro-5-fluorophenol with haloacetic acid ester is an important step in the whole reaction. Therefore, it is necessary to develop an easy-to-implement etherification device for 2-nitro-5-fluorophenol and haloacetic acid ester. Utility Model Content

[0005] This application provides an etherification reaction device to provide an easy-to-implement etherification device for 2-nitro-5-fluorophenol and haloacetic acid ester.

[0006] This application provides an etherification reaction device, including a reaction kettle, a centrifuge, a filtrate storage tank, a stripping kettle, a condenser, and a first solvent storage tank connected in series in sequence;

[0007] The reaction kettle is also connected to an etherifying agent storage tank;

[0008] The centrifuge is also connected to a washing kettle, and the washing kettle is also connected to the filtrate storage tank;

[0009] The stripping kettle is respectively connected to a fresh water storage tank and a filter press, and the filter press is respectively connected to a second solvent storage tank and a crude product storage tank;

[0010] The condenser is also connected to a vacuum unit.

[0011] Optionally, the first solvent storage tank and the second solvent storage tank are also connected to a distillation column;

[0012] The distillation column is also connected to a receiving tank group.

[0013] Optionally, a moisture detector and a three-way valve are sequentially arranged between the rectification column and the receiving tank group;

[0014] The three-way valve is also connected to the rectification column;

[0015] The three-way valve is also interlocked with the moisture detector.

[0016] Optionally, the rectification column is also connected to an incinerator.

[0017] Optionally, the washing kettle is also connected to an electrolysis device.

[0018] Optionally, the electrolysis device includes a brine preparation tank, a multi-stage membrane filter, and an electrolysis cell connected in series in sequence.

[0019] Optionally, the reaction kettle includes a reaction kettle body;

[0020] A dropping pipe is arranged at the upper part inside the reaction kettle body, and the dropping pipe is connected to an etherifying agent storage tank;

[0021] The dropping pipe includes a plurality of concentrically arranged annular liquid supply pipes, and adjacent liquid supply pipes are connected through pipelines;

[0022] A plurality of spray heads are connected to the lower surface of the liquid supply pipe;

[0023] A liquid baffle cylinder is also concentrically arranged outside the dropping pipe, and the lower part of the liquid baffle cylinder is flared;

[0024] A plurality of drainage sheets are also arranged at the lower edge of the liquid baffle cylinder, and the plurality of drainage sheets are evenly distributed along the circumferential direction of the lower edge of the liquid baffle cylinder.

[0025] The present application provides an etherification reaction device. By arranging a centrifuge, the reaction liquid after the reaction in the reaction kettle is centrifugally separated into a filter cake and mother liquor. The mother liquor and the washing liquid for washing the filter cake in the washing kettle are combined and then transferred into a stripping kettle for stripping treatment. The solvent obtained by stripping and the filtrate obtained by pressure filtration after washing the crude product with water are respectively transferred into corresponding storage tanks for recovery. Through the combined use of the above-mentioned equipment, the device of the present application provides an etherification reaction device for flumioxazin intermediate that is easy to implement, which has the advantages of easy control of the reaction process, less pollution in the treatment process, recyclable reaction solvent, and resource saving. Description of the Drawings

[0026] In order to more clearly illustrate the technical solutions in the embodiments of the present application or the prior art, the following will briefly introduce the drawings required for use in the description of the embodiments or the prior art. Obviously, the drawings in the following description are some embodiments of the present application. For those of ordinary skill in the art, other drawings can be obtained based on these drawings without creative efforts.

[0027] Figure 1Schematic diagram of an etherification reaction device provided by an embodiment of the present application;

[0028] Figure 2 Schematic diagram of an etherification reaction device provided by another embodiment of the present application;

[0029] Figure 3 Schematic diagram of an etherification reaction device provided by still another embodiment of the present application;

[0030] Figure 4 Schematic diagram of an etherification reaction device provided by yet another embodiment of the present application;

[0031] Figure 5 Schematic diagram of an electrolysis device provided by an embodiment of the present application;

[0032] Figure 6 Schematic diagram of the structure of a reaction kettle provided by an embodiment of the present application;

[0033] Figure 7 Schematic diagram of the structure of a dropping tube provided by an embodiment of the present application;

[0034] Figure 8 Schematic diagram of the structure of a liquid baffle cylinder provided by an embodiment of the present application.

[0035] Explanation of reference numerals:

[0036] 1. Reaction kettle; 2. Centrifuge; 3. Filtrate storage tank; 4. Desolventization kettle; 5. Condenser; 6. Washing kettle; 7. Rectification column; 8. Incinerator; 9. Electrolysis device; 10. Etherifying agent storage tank; 11. Reaction kettle body; 12. Dropping tube; 13. Liquid baffle cylinder; 41. Fresh water storage tank; 42. Filter press; 43. Second solvent storage tank; 44. Crude product storage tank; 51. First solvent storage tank; 52. Vacuum unit; 71. Receiving tank group; 72. Moisture detector; 91. Brine preparation tank; 92. Multi-stage membrane filter; 93. Electrolytic cell; 100. Three-way valve; 121. Liquid supply pipe; 122. Sprayer; 131. Drainage piece. Detailed implementation manners

[0037] To make the objectives, technical solutions and advantages of the embodiments of the present application clearer, the technical solutions in the embodiments of the present application will be clearly and completely described below. Apparently, the described embodiments are some, but not all, of the embodiments of the present application. All other embodiments obtained by those of ordinary skill in the art without creative efforts based on the embodiments in the present application also belong to the scope of protection of the present application.

[0038] In the existing etherification reaction, methyl chloroacetate and 2-nitro-5-fluorophenol react under alkaline conditions using acetone as a solvent. In this reaction, acetone has a low boiling point and is volatile, resulting in a large loss of acetone during the reaction, leading to waste of the solvent. Moreover, due to the volatile nature of acetone, the escaped acetone enters the environment, easily causing environmental pollution and deteriorating the factory production environment.

[0039] As Figure 1 shown, the present application provides an etherification reaction device, which includes a reaction kettle 1, a centrifuge 2, a filtrate storage tank 3, a solvent stripping kettle 4, a condenser 5, and a first solvent storage tank 51 connected in series in sequence;

[0040] The reaction kettle 1 is also connected to an etherifying agent storage tank 10;

[0041] The centrifuge 2 is also connected to a washing kettle 6, and the washing kettle 6 is also connected to the filtrate storage tank 3;

[0042] The solvent stripping kettle 4 is respectively connected to a fresh water storage tank 41 and a filter press 42, and the filter press 42 is respectively connected to a second solvent storage tank 43 and a crude product storage tank 44;

[0043] The condenser 5 is also connected to a vacuum unit 52.

[0044] During use, a solvent (N,N-dimethylformamide, i.e., DMF in the present application), a reaction raw material (2-nitro-5-fluorophenol in the present application), an acid-binding agent (potassium carbonate in the present application), and a phase transfer catalyst (tetrabutylammonium bromide in the present application) are sequentially added to the reaction kettle 1. The stirring is started and the temperature is raised to 90 - 100 °C. The etherifying agent (methyl chloroacetate, which is liquid in the present application) in the etherifying agent storage tank 10 is dropped into the reaction kettle 1.

[0045] After the dropping of the etherifying agent is completed, the reaction solution is kept at 90 - 100 °C for heat preservation reaction for 8 - 12 h. During this process, the reaction solution will gradually turn brown. When the reaction ends (detecting that the content of the raw material in the reaction solution is less than 0.3%), the reaction solution is cooled to 0 - 5 °C. At this time, the salt (mainly potassium chloride) generated in the reaction solution will precipitate. Then the reaction solution with precipitated salt is transferred to the centrifuge 2 for centrifugation to separate the salt (i.e., the filter cake) and the filtrate.

[0046] The filter cake is transferred to the washing kettle 6 and washed with a solvent (DMF) until the product content in the salt is less than 0.1% and qualified. The washing liquid for washing the filter cake and the filtrate separated by the centrifuge 2 are combined in the filtrate storage tank 3 and then transferred to the solvent stripping kettle 4 for solvent stripping to remove the solvent.

[0047] During the desolventization process, a vacuum unit 52 is used to evacuate the desolventization kettle 4 through a condenser 5, adjust the pressure in the desolventization kettle 4 to < -0.8 MPa, and control the temperature inside the desolventization kettle 4 at 130 - 150 °C to distill out the solvent, namely DMF. The distilled DMF is condensed into a liquid in the condenser 5 and transferred to the first solvent storage tank 51 for temporary storage. After the desolventization is completed, nitrogen is introduced into the desolventization kettle 4 to break the vacuum. At this time, the crude product in the desolventization kettle 4 (which contains the salts formed during the reaction and a small amount of the solvent DMF that has not been completely removed) is added with a certain amount of clear water from the clear water storage tank 41 into the desolventization kettle 4. The salts and DMF in the crude product are dissolved in the water. After the addition of the clear water is completed, the material system in the desolventization kettle 4 is heated to 60 - 70 °C and kept warm and stirred for 0.5 h so that the salts and the solvent in the crude product can be fully dissolved in the water. (This process is equivalent to extracting the salts and DMF in the crude product with water), and the product is solid and insoluble in water. Then, the mixture of the crude product - water is transferred to a filter press 42 for filtration to obtain the solid crude product, namely the filter cake, and the solid crude product is transferred to the crude product storage tank 44 for temporary storage. The filtrate is transferred to the second solvent storage tank 43 for storage.

[0048] This application provides an etherification reaction device. By setting a centrifuge 2, the reaction liquid after the reaction in the reaction kettle 1 is centrifugally separated into a filter cake and mother liquor. The mother liquor and the washing liquid that has washed the filter cake in the washing kettle 6 are combined and then transferred to the desolventization kettle 4 for desolventization treatment. The solvent obtained by desolventization and the filtrate obtained by filtering the washed crude product are respectively transferred to the corresponding storage tanks for recovery. Through the coordinated use of the above - mentioned equipment, the device of this application provides an etherification reaction device for flumioxazin intermediates that is easy to implement, which has the advantages of easy control of the reaction process, less pollution in the treatment process, recyclable reaction solvent, and resource conservation.

[0049] As Figure 2 shown, optionally, the first solvent storage tank 51 and the second solvent storage tank 43 are also connected to a distillation column 7;

[0050] The distillation column 7 is also connected to a receiving tank group 71.

[0051] The solvents temporarily stored in the first solvent storage tank 51 and the solvents stored in the second solvent storage tank 43 are respectively transferred to the distillation column 7 for distillation. Solvent DMF and water are taken out at the top of the column. The taken - out DMF and water are respectively stored in the corresponding receiving tanks in the receiving tank group 71.

[0052] As Figure 3 shown, optionally, a water content detector 72 and a three - way valve 100 are sequentially arranged between the distillation column 7 and the receiving tank group 71;

[0053] The three - way valve 100 is also connected to the distillation column 7;

[0054] The three-way valve 100 is also interlocked with the moisture detector 72.

[0055] In this application, during use, since the boiling point of water is lower than that of DMF, water is first extracted during the rectification process. When the moisture detector 72 detects that the moisture content in the extracted water is < 80% (i.e., the DMF content in the water is greater than 20%), due to the interlock between the three-way valve 100 and the moisture detector 72, the three-way valve 100 switches to the state of connecting the moisture detector 72 and the rectification column 7 while blocking the receiving tank group 71, and the extracted water is returned to the rectification column 7 for continuous rectification until the DMF content in the extracted water is qualified. When the DMF content in the extracted water is qualified, the three-way valve 100 interlocked with the moisture detector 72 switches the valve to the state of connecting the moisture detector 72 and the receiving tank group 71 while blocking the rectification column 7, and the extracted water is stored in the storage tank in the receiving tank group 71 for receiving water.

[0056] When extracting the solvent DMF, the moisture detector 72 detects the water content in the DMF. When the water content in the DMF is less than 3%, the three-way valve 100 interlocked with the moisture detector 72 switches the valve to the state of connecting the moisture detector 72 and the receiving tank group 71 while blocking the rectification column 7, and the extracted DMF is stored in the storage tank in the receiving tank group 71 for storing DMF. When the water content in the DMF detected by the moisture detector 72 is greater than 3%, the three-way valve 100 interlocked with the moisture detector 72 switches the valve to the state of connecting the moisture detector 72 and the rectification column 7 while blocking the receiving tank group 71, and the extracted DMF is returned to the rectification column 7 for re-rectification until the water content in the extracted DMF is qualified. The extracted water and DMF can both be reused.

[0057] As Figure 4 shown, optionally, the rectification column 7 is also connected to the incinerator 8.

[0058] In this application, the bottom residue after rectification in the rectification column 7 has complex components (mainly reaction by-products such as some polymers formed by the reaction between substrates), and its recovery value is low. The bottom residue can be transferred to the incinerator 8 for incineration for harmless treatment.

[0059] As Figure 4 shown, optionally, the washing kettle 6 is also connected to the electrolysis device 9.

[0060] In this application, by connecting the washing kettle 6 to the electrolysis device 9, the by-product salt (potassium chloride) can be used for electrolysis to produce hydrogen, chlorine, and potassium hydroxide, realizing the resource utilization of the salts in the reaction.

[0061] As Figure 5 shown, optionally, the electrolysis device 9 includes a brine preparation tank 91, a multi-stage membrane filter 92, and an electrolysis cell 93 connected in series in sequence.

[0062] In this application, during use, the salt after washing in the washing kettle 6 is transferred into the brine preparation tank 91 to prepare a brine solution with a preset concentration (i.e., potassium chloride aqueous solution). Since there is a small amount of solvent DMF in these brines, the brine solution in the brine preparation tank 91 is passed through a multi-stage membrane filter 92 to filter out the organic matter in the brine, obtaining a pure potassium chloride aqueous solution, and then the filtered potassium chloride aqueous solution is transferred into the electrolytic cell 93 for electrolysis.

[0063] As Figures 6 to 8 shown, optionally, the reaction kettle 1 includes a reaction kettle body 11;

[0064] An upper part inside the reaction kettle body 11 is provided with a dropping pipe 12, and the dropping pipe 12 is connected to the etherifying agent storage tank 10;

[0065] The dropping pipe 12 includes a plurality of concentrically arranged annular supply pipes 121, and adjacent supply pipes 121 are communicated through pipelines;

[0066] The lower surface of the supply pipe 121 is connected with a plurality of spray heads 122;

[0067] As Figure 8 shown, outside the dropping pipe 12, a liquid blocking cylinder 13 is also concentrically arranged, and the lower part of the liquid blocking cylinder 13 is flared;

[0068] The lower edge of the liquid blocking cylinder 13 is also provided with a plurality of drainage pieces 131, and the plurality of drainage pieces 131 are evenly distributed along the circumferential direction of the lower edge of the liquid blocking cylinder 13.

[0069] During use, the etherifying agent is pumped into the supply pipe 121 in the reaction kettle 1 through a corresponding transfer pump, and then sprayed out through a plurality of spray heads 122 arranged on the lower surface of the supply pipe 121 (the spraying amount of the spray heads 122 can be controlled according to actual conditions), so that the etherifying agent can be evenly added to the bottom liquid in the reaction kettle 1, avoiding the adverse situation of uneven reaction caused by excessive local concentration; and since the etherifying agent is sprayed out, its flow rate per unit time is small, which can avoid the adverse consequence that the reaction liquid temperature rises too fast due to too much etherifying agent added per unit time and affects the reaction. Since the droplets sprayed out by the spray heads 122 will be in a diffused state, a liquid blocking cylinder 13 is also concentrically arranged outside the dropping pipe 12, using the liquid blocking cylinder 13 to intercept the sprayed droplets and limit the sprayed droplets within a certain range, preventing the sprayed etherifying agent from diffusing too much and spraying on the inner wall of the reaction kettle 1, resulting in the adverse consequence of too high a concentration of the etherifying agent near the inner wall of the reaction kettle 1. The droplets intercepted by the liquid blocking cylinder 13 will flow down along the inner wall of the liquid blocking cylinder 13 and then fall into the reaction liquid through the drainage pieces 131.

[0070] An etherification reaction device has the following working process:

[0071] During use, a solvent (N,N-dimethylformamide, i.e., DMF in this application), a reaction raw material (2-nitro-5-fluorophenol in this application), an acid-binding agent (potassium carbonate in this application), and a phase transfer catalyst (tetrabutylammonium bromide in this application) are sequentially added to the reaction kettle 1. Stirring is started and the temperature is raised to 90-100 °C. The etherifying agent in the etherifying agent storage tank 10 (the etherifying agent is methyl chloroacetate and is in a liquid state in this application) is dropped into the reaction kettle 1.

[0072] The etherifying agent is pumped into the liquid supply pipe 121 in the reaction kettle 1 through a corresponding transfer pump, and then sprayed out through a plurality of spray heads 122 arranged on the lower surface of the liquid supply pipe 121 (the spraying amount of the spray heads 122 can be controlled according to the actual situation), so that the etherifying agent can be evenly added to the bottom liquid of the reaction kettle 1, and the adverse situation of uneven reaction caused by too high local concentration can be avoided; and because the etherifying agent is sprayed out, its flow rate per unit time is small, so that the adverse consequence that the reaction solution heats up too fast due to too much etherifying agent added per unit time and affects the reaction can be avoided. Since the liquid droplets sprayed out by the spray heads 122 will be in a diffused state, a liquid blocking cylinder 13 is concentrically arranged outside the drip tube 12. The liquid blocking cylinder 13 is used to intercept the sprayed liquid droplets and limit the sprayed liquid droplets within a certain range, preventing the sprayed etherifying agent from diffusing too much and spraying on the inner wall of the reaction kettle 1, resulting in the adverse consequence of too high etherifying agent concentration near the inner wall of the reaction kettle 1. The liquid droplets intercepted by the liquid blocking cylinder 13 will flow down along the inner wall of the liquid blocking cylinder 13 and then fall into the reaction solution through the drainage piece 131.

[0073] After the addition of the etherifying agent is completed, the reaction solution is kept at 90-100 °C for heat preservation reaction for 8-12 h. During this process, the reaction solution will gradually turn brown. When the reaction is over (the content of the raw material in the reaction solution is detected to be less than 0.3%), the reaction solution is cooled to 0-5 °C. At this time, the salt (mainly potassium chloride) generated in the reaction solution will precipitate. Then the reaction solution with precipitated salt is transferred to the centrifuge 2 for centrifugation to separate the salt (i.e., the filter cake) and the filtrate.

[0074] The filter cake is transferred to the washing kettle 6 and washed with a solvent (DMF) until the product content in the salt is less than 0.1% to be qualified. The washing liquid for washing the filter cake and the filtrate separated by the centrifuge 2 are combined in the filtrate storage tank 3 and then transferred to the solvent stripping kettle 4 for solvent stripping to remove the solvent.

[0075] Transfer the washed salts in the washing kettle 6 into the brine preparation tank 91 to prepare a brine solution (i.e., potassium chloride aqueous solution) with a preset concentration. Since there is a small amount of solvent DMF in these brines, the brine solution in the brine preparation tank 91 is passed through a multi-stage membrane filter 92 to filter out the organic substances in the brine, obtaining a pure potassium chloride aqueous solution. Then, the filtered potassium chloride aqueous solution is transferred into the electrolytic cell 93 for electrolysis to produce hydrogen, chlorine, and potassium hydroxide, realizing the resource utilization of the salts in the reaction.

[0076] During the desolvation process, a vacuum unit 52 is used to evacuate the desolvation kettle 4 through a condenser 5, adjust the pressure in the desolvation kettle 4 to < -0.8 MPa, and control the temperature inside the desolvation kettle 4 at 130 - 150 °C to distill out the solvent, i.e., DMF. The distilled DMF is condensed into a liquid in the condenser 5 and transferred into the first solvent storage tank 51 for temporary storage. After the desolvation is completed, nitrogen is introduced into the desolvation kettle 4 to break the vacuum. At this time, the crude product in the desolvation kettle 4 (which contains the salts generated in the reaction and a small amount of the solvent DMF that has not been completely removed) is added with a certain amount of clear water from the clear water storage tank 41 into the desolvation kettle 4 to dissolve the salts and DMF in the crude product in water. After the addition of clear water is completed, the material system in the desolvation kettle 4 is heated to 60 - 70 °C and kept stirred for 0.5 h to enable the salts and the solvent in the crude product to be fully dissolved in water (this process is equivalent to using water to extract the salts and DMF in the crude product), while the product is solid and insoluble in water. Then, the mixture of the crude product - water is transferred into a filter press 42 for filtration to obtain the solid crude product, i.e., the filter cake, and the solid crude product is transferred into the crude product storage tank 44 for temporary storage. The filtrate is transferred into the second solvent storage tank 43 for storage.

[0077] The solvents temporarily stored in the first solvent storage tank 51 and the solvents stored in the second solvent storage tank 43 are respectively transferred into a distillation column 7 for distillation, and the solvent DMF and water are taken out at the top of the column. Since the boiling point of water is lower than that of DMF, water is taken out first during the distillation process. When the moisture detector 72 detects that the water content in the taken - out water is < 80% (i.e., the DMF content in the water is greater than 20%), due to the interlock between the three - way valve 100 and the moisture detector 72, at this time, the three - way valve 100 switches to the state of connecting the moisture detector 72 and the distillation column 7 and blocking the receiving tank group 71, and the taken - out water is returned to the distillation column 7 for continuous distillation until the DMF content in the taken - out water is qualified. When the DMF content in the taken - out water is qualified, the three - way valve 100 interlocked with the moisture detector 72 switches the valve to the state of connecting the moisture detector 72 and the receiving tank group 71 and blocking the distillation column 7, and the taken - out water is stored in the storage tank in the receiving tank group 71 for receiving water.

[0078] When the solvent DMF is extracted, the moisture detector 72 detects the water content in the DMF. When the water content in the DMF is less than 3%, the three-way valve 100 interlocked with the moisture detector 72 switches the valve to the state of connecting the moisture detector 72 and the receiving tank group 71 while blocking the distillation column 7, and stores the extracted DMF in the receiving tank group 71 in the storage tank for storing DMF. When the water content in the DMF detected by the moisture detector 72 is greater than 3%, the three-way valve 100 interlocked with the moisture detector 72 switches the valve to the state of connecting the moisture detector 72 and the distillation column 7 while blocking the receiving tank group 71, and returns the extracted DMF to the distillation column 7 for re-distillation until the water content in the extracted DMF is qualified. Both the extracted water and DMF can be recycled.

[0079] The bottom residue after distillation in the distillation column 7 has complex components and low recovery value, and the bottom residue can be transferred to the incinerator 8 for incineration for harmless treatment.

[0080] Finally, it should be noted that the above embodiments are only used to illustrate the technical solutions of the present application, and are not intended to limit them; although the present application has been described in detail with reference to the foregoing embodiments, those of ordinary skill in the art should understand that they can still modify the technical solutions described in the foregoing embodiments, or perform equivalent replacements on some or all of the technical features; and these modifications or replacements do not cause the essence of the corresponding technical solutions to deviate from the scope of the technical solutions of the embodiments of the present application.

Claims

1. An etherification reaction device, characterized in that: It comprises a reaction kettle (1), a centrifuge (2), a filtrate storage tank (3), a desolventizing kettle (4), a condenser (5) and a first solvent storage tank (51) which are connected in series in sequence; The reaction kettle (1) is also connected to an etherifying agent storage tank (10); The centrifuge (2) is also connected to a washing kettle (6), and the washing kettle (6) is also connected to the filtrate storage tank (3); The desolventizing kettle (4) is also connected to the clean water storage tank (41) and the filter press (42), respectively, and the filter press (42) is also connected to the second solvent storage tank (43) and the crude product storage tank (44), respectively; The condenser (5) is also connected to a vacuum unit (52).

2. The etherification reaction device according to claim 1, characterized in that: The first solvent storage tank (51) and the second solvent storage tank (43) are also connected to the distillation tower (7); The distillation tower (7) is also connected to a receiving tank group (71).

3. The etherification reaction device according to claim 2, characterized in that: A moisture detector (72) and a three-way valve (100) are also sequentially arranged between the distillation tower (7) and the receiving tank group (71); The three-way valve (100) is also connected to the distillation tower (7); The three-way valve (100) is also interlocked with the moisture detector (72).

4. The etherification reaction device according to claim 2, characterized in that: The distillation tower (7) is also connected to an incinerator (8).

5. The etherification reaction device according to claim 1, characterized in that: The washing tank (6) is also connected to an electrolysis device (9).

6. The etherification reaction device according to claim 5, characterized in that: The electrolysis device (9) comprises a brine preparation tank (91), a multi-stage membrane filter (92) and an electrolysis tank (93) which are connected in series.

7. The etherification reaction device according to any one of claims 1 to 6, characterized in that: The reactor (1) comprises a reactor body (11); A dripping pipe (12) is provided in the upper part of the reactor body (11), and the dripping pipe (12) is connected to the etherifying agent storage tank (10); The drip tube (12) comprises a plurality of concentrically arranged annular liquid supply tubes (121), and adjacent liquid supply tubes (121) are connected via pipelines; The lower surface of the liquid supply pipe (121) is connected to a plurality of spray heads (122); A liquid retaining cylinder (13) is coaxially arranged outside the liquid dripping tube (12), and the lower part of the liquid retaining cylinder (13) is expanded; The lower edge of the liquid retaining cylinder (13) is further provided with a plurality of drainage pieces (131), and the plurality of drainage pieces (131) are evenly distributed along the circumference of the lower edge of the liquid retaining cylinder (13).

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