Synthesis kettle for producing diethylene glycol dimethyl ether
By using agitator, heating coil, cooling water interlayer and gas distributor in the diethylene glycol dimethyl ether synthesis reactor, the problems of uneven stirring, slow dissolution and more side reactions are solved, and more efficient material mixing, more accurate temperature control and lower side reaction frequency are achieved, and product quality and yield are improved.
Patent Information
- Application Number
- CN202422183193.0
- Authority / Receiving Office
- CN · China
- Patent Type
- Utility models(China)
- Current Assignee / Owner
- Filing Date
- 2024-09-06
- Publication Date
- 2025-06-17
- Estimated Expiration
- 2034-09-06
AI Technical Summary
The existing diethylene glycol dimethyl ether synthesis reactors have uneven stirring, slow and incomplete dissolution rate of sodium hydroxide during the production process, resulting in frequent pipeline blockage and side reactions, affecting product quality and yield.
A synthetic kettle including a stirrer, heating coil, cooling water interlayer and gas distributor was designed. The mixer was used to achieve uniform material mixing, and the gas distributor ensured uniform gas distribution. The heating coil and cooling water interlayer jointly achieved the accuracy of temperature control and reduced side reactions.
It effectively avoids pipeline blockage, improves material dissolution efficiency, reduces the occurrence of side reactions, improves product quality and yield, and improves the degree of automation of the synthetic kettle.
Smart Images
Figure CN222984365U_ABST
Abstract
Description
Technical Field
[0001] The utility model belongs to the technical field of reactor equipment, and particularly relates to a synthesis kettle for producing diethylene glycol dimethyl ether. Background Technique
[0002] Diethylene glycol dimethyl ether, with the molecular formula C6H14O3 and molecular weight 134.17, is a colorless transparent liquid with a boiling point of 162 °C and a relative density of 0.9467. It is a high-boiling aprotic polar solvent with a weak ether odor and can be miscible with water, alcohols, dimethyl ether, and hydrocarbon solvents. Diethylene glycol dimethyl ether can be used in polar organic reactions, as a solvent for anionic polymerization and coordination ionic polymerization reactions, as a solvent for reduction, alkylation, and condensation reactions, etc., and can also be used as a medium for Grignard and similar syntheses, and is also used as a pollution-free cleaning agent, extractant, diluent, pharmaceutical adjuvant, and resin solvent, etc.
[0003] At present, there are various process routes for the synthesis of diethylene glycol dimethyl ether, including the hydrogenolysis of triethylene glycol monomethyl ether, the hydrogenolysis of diglycol ether polyacetal, the dehydration of ethylene glycol monomethyl ether, the etherification reaction of diglycol or its monomethyl ether, the reaction of dimethyl ether with ethylene oxide, etc. Among them, the etherification reaction of diglycol or its monomethyl ether is the most ideal, with simple process, easy operation, and safety.
[0004] Now the most commonly used preparation method of diethylene glycol dimethyl ether is to use diethylene glycol monomethyl ether, chloromethane, and sodium hydroxide as raw materials, react under certain conditions to produce a crude product, and then obtain a pure product through centrifugation and rectification analysis. During the production process, the synthesis reactor for diethylene glycol dimethyl ether is particularly important. In the current synthesis reactor during the production process, the stirring is often uneven, the dissolution rate of sodium hydroxide is slow and incomplete, resulting in frequent blockage of the pipeline during the discharging process; secondly, during the synthesis of diethylene glycol dimethyl ether, heating is required, and the temperature control of the synthesis kettle is not stable enough, prone to side reactions, resulting in a decrease in the yield. In order to improve the current production status of diethylene glycol dimethyl ether, reduce the problems of pipeline blockage and difficult material dissolution, improve the stability of temperature control, reduce the occurrence of side reactions, and improve the yield, it is particularly important to develop a synthesis kettle for producing diethylene glycol dimethyl ether. Content of the Utility Model
[0005] The purpose of the utility model is to overcome the deficiencies of the prior art and provide a synthesis kettle for producing diethylene glycol dimethyl ether with good product quality, anti-pipeline blockage, few side reactions, and high degree of automation.
[0006] The purpose of the present utility model is achieved as follows: A synthesis kettle for producing diethylene glycol dimethyl ether, comprising a kettle body and a kettle cover. The upper end of the kettle cover is provided with a nitrogen pipeline, a caustic soda feed pipeline, a monoether feed pipeline, a safety relief pipeline, a tail gas discharge pipeline, a stirring motor, an on-line thermometer, an on-line pressure gauge, an explosion-proof searchlight, a sight glass and an observation port. One side of the kettle body is provided with an on-line liquid level gauge. The kettle body is provided with a cooling water interlayer, and the outside of the cooling water interlayer is provided with a heat preservation layer. The outside of the heat preservation layer is provided with an aluminum alloy layer. A stirrer is arranged inside the kettle body, and a heating coil is arranged around the outside of the stirrer. A gas distributor is arranged below the stirrer inside the kettle body. The lower end of the kettle body is provided with a discharge pipeline and a chloromethane inlet pipeline communicated with the gas distributor. An on-line flowmeter A and an on-line flowmeter B are respectively installed on the monoether feed pipeline and the discharge pipeline. The detection data of the on-line thermometer, the on-line pressure gauge, the on-line liquid level gauge, the on-line flowmeter A and the on-line flowmeter B are transmitted to a remote control system.
[0007] Preferably, the stirring blades of the stirrer are divided into two layers, one layer on the upper and lower sides respectively, and each layer has three stirring blades. The included angle between the stirring blades and the plane is 30 to 50°.
[0008] Preferably, the gas distributor is in a ring-shaped tubular shape, and a number of gas outlet holes are arranged on the ring-shaped tube. The aperture of the gas outlet holes is 1 to 2 mm.
[0009] Preferably, the upper end of the heating coil extends out of the kettle body and is communicated with a steam inlet, and the lower end of the heating coil extends out of the kettle cover and is communicated with a steam outlet. A steam water discharge port is arranged at the bottom of the heating coil.
[0010] Preferably, control valves are arranged at the positions of the nitrogen pipeline, the caustic soda feed pipeline, the monoether feed pipeline, the safety relief pipeline, the tail gas discharge pipeline close to the kettle cover, the chloromethane inlet pipeline, the discharge pipeline close to the kettle body, the steam inlet, the steam outlet and the steam water discharge port.
[0011] Preferably, the control valves on the caustic soda feed pipeline, the monoether feed pipeline, the tail gas discharge pipeline, the chloromethane inlet pipeline and the discharge pipeline are connected to pneumatic cut-off valves, and the pneumatic cut-off valves are connected to the remote control system.
[0012] Preferably, the stirring motor is a servo variable frequency motor. The servo variable frequency motor is provided with an adjustment switch and is connected to the remote control system. A wire protection net is additionally installed outside the servo variable frequency motor.
[0013] Preferably, the explosion-proof searchlight is installed above the opposite side of the observation port, and the sight glass is below the explosion-proof searchlight.
[0014] Preferably, a rupture disc and a safety valve are installed on the safety relief pipeline.
[0015] Due to the adoption of the above technical solutions, the beneficial effects of the present utility model are as follows: The present utility model adopts a stirrer, a heating coil, a cooling water interlayer and a gas distributor. The stirrer can make the materials mix evenly, with high efficiency in dissolving flake caustic soda, effectively avoiding pipeline blockage. The gas distributor can make the gas distribute evenly, and the reaction is sufficient and thorough. The heating coil and the cooling water interlayer can accurately control the temperature, with fewer side reactions. The three together make the product quality high. The present utility model adopts an explosion-proof searchlight, a sight glass and an observation port, which are convenient for manual direct viewing of the material reaction situation, ensuring the product quality and reaction environment from multiple angles. The present utility model adopts an online thermometer, an online pressure gauge and an online flowmeter to online detect and analyze the reaction environment, improving the automation degree of the synthesis kettle. Generally, the present utility model has the advantages of good product quality, anti-pipeline blockage, fewer side reactions and high automation degree. Description of the Drawings
[0016] Figure 1 is the front view structural schematic diagram of the present utility model.
[0017] Figure 2 is the top view structural schematic diagram of the gas distributor of the present utility model.
[0018] In the figure: 1. Kettle cover; 2. Observation port; 3. Online flowmeter A; 4. Monoether feed pipeline; 5. Tail gas discharge pipeline; 6. Online pressure gauge; 7. Stirring motor; 8. Online thermometer; 9. Rupture disc; 10. Safety valve; 11. Safety relief pipeline; 12. Steam outlet; 13. Flake caustic soda feed pipeline; 14. Nitrogen pipeline; 15. Steam inlet; 16. Explosion-proof searchlight; 17. Sight glass; 18. Online liquid level gauge; 19. Cooling water inlet; 20. Methyl chloride inlet pipeline; 21. Pneumatic cut-off valve; 22. Online flowmeter B; 23. Discharge pipeline; 24. Gas distributor; 241. Air outlet hole; 25. Steam water discharge port; 26. Kettle body; 27. Heating coil; 28. Stirrer; 29. Cooling water outlet; 30. Control valve. Detailed Embodiments
[0019] The technical solutions of the present utility model will be further specifically described below with reference to the drawings.
[0020] As Figure 1 and Figure 2 shown, the present utility model provides a synthesis kettle for producing diethylene glycol dimethyl ether, mainly used to solve the problems of low efficiency in dissolving flake caustic soda materials, easy pipeline blockage, many side reactions and thus affecting product quality during the production of diethylene glycol dimethyl ether.
[0021] The utility model relates to a synthesis kettle for producing and synthesizing diethylene glycol dimethyl ether, which is a device for the reaction of synthesis raw materials. The main body of the device is mainly a synthesis kettle, including a kettle cover 1 and a kettle body 26. The material of the kettle is 304 stainless steel. The connection between the kettle cover 1 and the kettle body 26 is fixed by bolts, and a gasket is added in the middle.
[0022] A stirrer 28 is arranged in the synthesis kettle, and a servo variable-frequency motor (i.e., a stirring motor 7) is installed. The servo variable-frequency motor is provided with an adjustment switch and is connected to a remote control system. The motor speed can be adjusted manually and remotely. A wire protection net is installed outside the servo variable-frequency motor.
[0023] The stirrer 28 of the synthesis kettle is rotatably fixed on the kettle cover 1 of the synthesis kettle. In order to achieve good stirring effect, the stirring blades of the stirrer 28 are divided into two layers, one layer on the upper and lower sides, with three stirring blades on each layer. The angle between the stirring blades and the plane is 30-50°.
[0024] The inside of the synthesis kettle is a heating coil 27. The coil extends to the bottom of the kettle, and a steam water discharge port 25 is arranged at the bottom. The material of the coil is stainless steel 304 or 316, preferably stainless steel 304.
[0025] The kettle body 26 of the synthesis kettle is provided with a cooling water interlayer. The interlayer is provided with cooling water inlets and outlets for installing control valves 30. The cooling water inlet 19 is located at the lower side of one side of the kettle body 26, and the cooling water outlet 29 is located at the upper side of one side of the kettle body 26. There is a heat preservation layer outside the interlayer, and the outside of the heat preservation layer is wrapped by aluminum alloy.
[0026] Above the kettle cover 1 of the synthesis kettle, there are an observation port 2, an explosion-proof searchlight 16, a caustic soda feed port (i.e., the connection between the caustic soda feed pipe 13 and the kettle cover 1), a nitrogen gas inlet (i.e., the connection between the nitrogen gas feed pipe 14 and the kettle cover 1), a monoether feed port (i.e., the connection between the monoether feed pipe 4 and the kettle cover 1), a tail gas discharge port (i.e., the connection between the tail gas discharge pipe 5 and the kettle cover 1), and a safety pressure relief port (i.e., the connection between the safety pressure relief pipe 11 and the kettle cover 1). Control valves 30 are installed at the caustic soda feed port, the monoether feed port, and the tail gas discharge port. The control valves 30 are connected to pneumatic cut-off valves 21 and are connected to a remote control system, and can be operated manually on site and remotely. The safety pressure relief port is connected to a rupture disk 9 and a safety valve 10 to ensure safe production. An on-line flowmeter A3 is installed on the pipe connected to the monoether feed port, and the data of the on-line flowmeter A3 is transmitted to the remote control system. An explosion-proof searchlight 16 is installed above the observation port 2, and a sight glass 17 is arranged below the explosion-proof searchlight 16 for convenient visual inspection. Since nitrogen has stable chemical properties and is non-toxic, it can be used as a protective gas during the synthesis reaction process, such as in the pipeline gas replacement during charging, discharging, and hot work operations.
[0027] An online thermometer 8 and an online pressure gauge 6 are installed on the kettle cover 1 of the described synthesis kettle. An online liquid level gauge 18 is installed on the kettle side to detect the reaction situation inside the kettle, and the analyzed data is transmitted to the remote control system.
[0028] A discharge port (i.e., the connection between the discharge pipeline 23 and the kettle body 26) and a methyl chloride feed port (i.e., the connection between the methyl chloride feed pipeline 20 and the kettle body 26, internally connected to the gas distributor 24) are provided below the kettle body 26. A control valve 30 and an online flowmeter B22 are installed on the discharge pipeline 23. Pneumatic cut-off valves 21 are connected to both the discharge pipeline 23 and the methyl chloride feed pipeline 20, and are connected to the remote control system.
[0029] Methyl chloride enters from the bottom of the synthesis kettle through the methyl chloride inlet pipeline 20. The end of the pipeline is a gas distributor 24. The gas distributor 24 is located below the stirrer 28. The gas distributor 24 is in the shape of an annular tube, made of stainless steel pipe. A number of air inlet holes 241 with a pore diameter of 1 - 2 mm are arranged on the annular tube for the escape of methyl chloride gas.
[0030] After the above installation, the present utility model can be put into use. Raw materials are added from the monoether feed pipeline 4, the flake soda feed pipeline 13, and the methyl chloride inlet pipeline 20. The stirring motor 7 is started, the heating coil 27 is turned on, and the cooling water jacket is turned on. Each raw material reacts fully in the synthesis kettle. After the reaction is completed, the material is discharged from the discharge pipeline 23. During this period, the online thermometer 8, the online pressure gauge 6, the online liquid level gauge 18, the online flowmeter A3, and the online flowmeter B22 detect and analyze the reaction environment inside the kettle under the unified control of the remote control system to ensure the smooth progress of the synthesis reaction. During this period, each control valve 30 and each pneumatic cut-off valve 21 work coordinately under the unified control of the remote control system to ensure the smooth operation of the synthesis kettle.
[0031] In summary, the present utility model can effectively solve problems such as low material dissolution efficiency, easy blockage of pipelines, and many side reactions during the synthesis of diethylene glycol dimethyl ether. At the same time, it reduces on-site manual operation and analysis and determination, is safer in operation, more accurate in analysis, saves labor, has a high degree of automation, and greatly improves the production efficiency of diethylene glycol dimethyl ether.
[0032] The present utility model redesigned the diethylene glycol dimethyl ether synthesis device. The main body of the device is a synthesis kettle, and the main components include a stirrer 28, a heating coil 27, pneumatic cut-off valves 21, an online flowmeter A3, an online flowmeter B22, an online pressure gauge 6, an online liquid level gauge 18, a gas distributor 24, an explosion-proof searchlight 16, etc.
[0033] The stirrer 28 installed on the synthesis kettle of the device has two layers of stirring blades, one layer on the upper and lower parts, each with three stirring blades. The angle between the stirring blades and the plane is 30 - 50º, the material mixing is more uniform, the dissolution efficiency of flake soda is higher, and the problem of pipeline blockage is reduced.
[0034] The methyl chloride gas distributor 24 of the device is in a ring tube shape, made of stainless steel pipe. A number of air inlet holes 241 are arranged on the ring tube for the escape of methyl chloride gas. The aperture is 1 - 2 mm, the gas distribution is more uniform, and the reaction is more complete.
[0035] Pneumatic cut-off valves 21 are installed on both the feed and discharge pipelines of the synthesis kettle of the device and are connected to a remote control system. It can be operated manually on-site and remotely controlled. The degree of automation is high, reducing human participation, and it is safe and reliable. The function of the pneumatic cut-off valve 21 is to remotely control the feeding and discharging of the device. In case of an emergency, it can remotely respond and cut off the reaction. At the same time, it is also a safety guarantee with dual control.
[0036] The servo variable-frequency motor of the device is provided with an adjustment switch and is connected to a remote control system. The motor speed can be adjusted manually and remotely. A wire protection net is additionally installed outside the servo variable-frequency motor to respond and handle emergencies promptly, which is safe and reliable.
[0037] An online thermometer 8 and an online pressure gauge 6 are installed on the device, and an online liquid level gauge 18 is installed at the kettle side to detect the reaction situation in the kettle. The analyzed data is transmitted to the remote control system, and remote monitoring, analysis, and adjustment can be carried out, reducing the participation of on-site personnel.
[0038] The inside of the synthesis kettle of the device adopts heating coils 27 and is heated by saturated steam. The heating efficiency is higher and more stable. The online thermometer 8 is used for detection, and the temperature control is more accurate, reducing the occurrence of side reactions and ensuring high product quality.
[0039] The above is only the preferred embodiment of the present utility model and is not intended to limit the present utility model. Any modifications, equivalent replacements, improvements, etc. made within the spirit and principle of the present utility model shall be included within the protection scope of the present utility model.
Claims
1. A synthesis reactor for producing diethylene glycol dimethyl ether, comprising a reactor body and a reactor cover, characterized in that: The upper end of the kettle cover is provided with a nitrogen pipeline, a flake caustic soda feed pipeline, a monoether feed pipeline, a safety pressure relief pipeline, a tail gas exhaust pipeline, a stirring motor, an online thermometer, an online pressure gauge, an explosion-proof searchlight, a sight glass and an observation port; one side of the kettle body is provided with an online liquid level gauge; the kettle body is provided with a cooling water interlayer; the outer side of the cooling water interlayer is provided with an insulation layer; the outer side of the insulation layer is provided with an aluminum alloy layer; an agitator is provided in the kettle body; a heating coil is provided around the outer side of the agitator; a gas distributor is provided in the kettle body below the agitator; a discharge pipeline and a chloroform inlet pipeline connected to the gas distributor are provided at the lower end of the kettle body; an online flowmeter A and an online flowmeter B are respectively installed on the monoether feed pipeline and the discharge pipeline; the detection data of the online thermometer, the online pressure gauge, the online liquid level gauge, the online flowmeter A and the online flowmeter B are transmitted to the remote control system.
2. The synthesis reactor for producing diethylene glycol dimethyl ether according to claim 1, characterized in that: The stirring blades of the stirrer are divided into two layers, one layer at the top and one layer at the bottom, each layer has three stirring blades, and the angle between the stirring blades and the plane is 30-50 degrees.
3. The synthesis reactor for producing diethylene glycol dimethyl ether according to claim 1, characterized in that: The gas distributor is in the shape of an annular tube, and a plurality of gas outlet holes are arranged on the annular tube, and the diameter of the gas outlet holes is 1 to 2 mm.
4. The synthesis reactor for producing diethylene glycol dimethyl ether according to claim 1, characterized in that: The upper end of the heating coil extends outward from the kettle body and is connected to the steam inlet, the lower end of the heating coil extends upward from the kettle cover and is connected to the steam outlet, and a steam water outlet is provided at the bottom of the heating coil.
5. The synthesis reactor for producing diethylene glycol dimethyl ether according to claim 4, characterized in that: The nitrogen pipeline, the flake caustic soda feed pipeline, the monoether feed pipeline, the safety pressure relief pipeline, the tail gas discharge pipeline at a position close to the kettle cover, the chloromethane intake pipeline, the discharge pipeline at a position close to the kettle body, the steam inlet, the steam outlet, and the steam water outlet are all provided with control valves.
6. The synthesis reactor for producing diethylene glycol dimethyl ether according to claim 5, characterized in that: The control valves on the caustic soda flake feed pipeline, the monoether feed pipeline, the tail gas discharge pipeline, the methyl chloride intake pipeline, and the discharge pipeline are connected to a pneumatic shut-off valve, and the pneumatic shut-off valve is connected to a remote control system.
7. The synthesis reactor for producing diethylene glycol dimethyl ether according to claim 1, characterized in that: The stirring motor is a servo variable frequency motor, the servo variable frequency motor is provided with an adjustment switch and is connected to a remote control system, and a wire protection net is additionally installed outside the servo variable frequency motor.
8. The synthesis reactor for producing diethylene glycol dimethyl ether according to claim 1, characterized in that: The explosion-proof searchlight is installed above the opposite side of the observation port, and the sight glass is located below the explosion-proof searchlight.
9. The synthesis reactor for producing diethylene glycol dimethyl ether according to claim 1, characterized in that: A bursting disc and a safety valve are installed on the safety pressure relief pipeline.