Dissolving device for preparing diethylene glycol monoethylene diether

Abstract

The utility model relates to the technical field of preparation of diethylene glycol monoethylene diether, and particularly discloses a dissolving device for preparation of diethylene glycol monoethylene diether, which comprises a tank body, a discharge pipe arranged at the bottom of the tank body and provided with a discharge valve, and a top cover arranged at the top of the tank body, a pressure release valve, a pressure sensor, a dropper, a PH probe and an oxygen concentration analyzer are integrated at the top of the top cover, a liquid outlet of the dropper, the pressure sensor, the PH probe and a detection probe of the oxygen concentration analyzer all extend into the tank body, and a stirring mechanism is combined with a crushing cutter, so that uniform mixing of a high-viscosity material and low-boiling-point vinyl ether is realized, the reaction is accelerated, and the reaction efficiency is improved. Microbubble groups generated by the annular nitrogen distribution pipe are combined to enhance liquid turbulence, improve the reaction conversion rate and reduce by-products, and a pressure release valve, a pressure sensor and oxygen concentration real-time monitoring are combined, so that the oxygen concentration in the tank is kept stable, and the risk of burning explosion is completely eradicated.

Description

Technical Field

[0001] This utility model relates to the field of diethylene glycol monoethylene diether preparation technology, and specifically discloses a dissolution device for preparing diethylene glycol monoethylene diether. Background Technology

[0002] The preparation of diethylene glycol monovinyl diether requires the mixing and dissolution of diethylene glycol, vinyl ether, and catalyst under specific conditions.

[0003] When using traditional dissolving devices, due to the high viscosity of diethylene glycol at room temperature (approximately 30 cP), traditional stirring devices (such as single paddle stirrers) struggle to achieve uniform mixing of high-viscosity materials and low-boiling-point vinyl ethers. This results in insufficient contact of reactants, a low reaction rate, and an increase in byproducts. Vinyl ethers are highly volatile at room temperature (e.g., methyl vinyl ether has a boiling point of only 35°C). Traditional equipment lacks inert gas protection and pressure relief mechanisms, which can easily lead to the formation of flammable vapor-air mixtures, posing a risk of combustion and explosion. Therefore, improvements are needed. Summary of the Invention

[0004] This invention proposes a dissolving device for the preparation of diethylene glycol monoethylene diether. By combining a stirring mechanism with a pulverizing blade, it achieves uniform mixing of high-viscosity materials and low-boiling-point vinyl ethers, accelerating the reaction. In addition, the microbubble clusters generated by the annular nitrogen distribution pipe enhance liquid turbulence, improve the reaction conversion rate, and reduce by-products. Furthermore, the device incorporates a pressure relief valve, a pressure sensor, and real-time oxygen concentration monitoring to maintain a stable oxygen concentration inside the tank and eliminate the risk of combustion and explosion.

[0005] This invention is implemented as follows: a dissolving device for preparing diethylene glycol monoethylene diether includes a tank, a discharge pipe with a discharge valve at the bottom of the tank, and a top cover at the top of the tank. The top cover integrates a pressure relief valve, a pressure sensor, a dropper, a pH probe, and an oxygen concentration analyzer. The outlet of the dropper, the pressure sensor, the pH probe, and the detection probe of the oxygen concentration analyzer all extend into the interior of the tank. A stirring mechanism is provided inside the tank. The stirring mechanism includes a rotating shaft and a first motor. The first motor is fixed to the top of the top cover, and its output end is coaxially and fixedly connected to the rotating shaft. Multiple first crushing blades are fixedly installed on the upper part of the outer circumference of the rotating shaft, multiple symmetrically distributed stirring rods are fixedly installed in the middle, and multiple stirring blades are fixedly installed at the bottom.

[0006] A bracket is fixedly installed at the bottom of the outer circumference of the tank, and an annular nitrogen distribution pipe is fixedly installed at the bottom of the bracket. A nitrogen inlet pipe is connected to the outer wall of the annular nitrogen distribution pipe. An air flow regulating valve is provided on the outer wall of the nitrogen inlet pipe. Nozzles are evenly distributed on the annular nitrogen distribution pipe. A solenoid valve is installed on the outer wall of each nozzle, and the other end extends into the interior of the tank.

[0007] As a preferred embodiment of the dissolving apparatus for preparing diethylene glycol monoethylene diether according to this utility model, the jacket of the tank is provided with two symmetrically distributed heating plates, and the interior of the tank is provided with a temperature sensor.

[0008] In a preferred embodiment of the dissolving apparatus for preparing diethylene glycol monoethylene diether according to this utility model, multiple stirring rods located on the same side are fixedly connected to a scraper, and the scraper is in close contact with the inner wall of the tank.

[0009] As a preferred embodiment of the dissolving apparatus for preparing diethylene glycol monoethylene diether according to this utility model, the top of the top cover is connected to a feeding pipe with a sealing cap and a feed pipe, and the top of the top cover is fixedly connected to a metering pump connected to the feed pipe.

[0010] As a preferred embodiment of the dissolving apparatus for preparing diethylene glycol monoethylene diether according to this utility model, two symmetrical second motors are installed at the bottom of the tank. The output end of the second motor passes through the tank through a mechanical seal and is equipped with a second crushing blade for crushing the particulate matter deposited at the bottom of the tank.

[0011] As a preferred embodiment of the dissolving apparatus for preparing diethylene glycol monoethylene diether of this utility model, the inner wall of the tank and the surface of the stirring mechanism are coated with a polytetrafluoroethylene anti-corrosion coating, a fixing frame is fixedly installed on the outer wall of the tank, and a PLC touch screen all-in-one machine is fixedly installed on the outer wall of the fixing frame.

[0012] The beneficial effects of this utility model are:

[0013] (1) The first motor enables the middle stirring rod and the bottom blade to form a three-stage stirring structure, which realizes the uniform mixing of high viscosity materials and low boiling point vinyl ether. The top crushing blade and the bottom second crushing blade specifically treat the deposited particles and further crush the catalyst particles, realizing the gradient crushing and dispersion of solid materials, shortening the dissolution time, accelerating the reaction, and combining the microbubble group generated by the annular nitrogen distribution pipe to enhance liquid turbulence, improve the reaction conversion rate, and reduce by-products.

[0014] (2) The annular nitrogen distribution pipe evenly introduces nitrogen into the tank through the nozzle to maintain the oxygen concentration, inhibit the oxidative degradation of raw materials (such as vinyl monomers) in the synthesis of diethylene glycol monoethylene diether, improve the purity of the product, and, in combination with the pressure relief valve, pressure sensor, and real-time oxygen concentration monitoring (oxygen concentration analyzer), ensure that the oxygen concentration in the tank is stable at <1%, eliminating the risk of combustion and explosion. Attached Figure Description

[0015] Figure 1 This is a front sectional view of a dissolving apparatus for preparing diethylene glycol monoethylene diether according to the present invention;

[0016] Figure 2This is a top view of the tank body and the annular nitrogen distribution pipe of this utility model;

[0017] Figure 3 This is a structural diagram of the first shredding blade of this utility model;

[0018] Figure 4 This is a structural diagram of the stirring blade of this utility model.

[0019] In the diagram: 1. Tank body; 101. Heating plate; 102. Temperature sensor; 103. Discharge pipe; 2. Top cover; 201. Feeding pipe; 202. Feed inlet pipe; 203. Metering pump; 204. Pressure relief valve; 205. Pressure sensor; 206. Dropper; 207. pH probe; 208. Oxygen concentration analyzer; 3. Rotating shaft; 301. First crushing blade; 302. Stirring rod; 3021. Scraper; 303. First motor; 4. Support; 401. Annular nitrogen distribution pipe; 402. Nozzle; 403. Solenoid valve; 404. Nitrogen inlet pipe; 5. Stirring blade; 6. Second motor; 601. Second crushing blade; 7. Fixing frame. Detailed Implementation

[0020] The present invention will be further described below with reference to the accompanying drawings and specific embodiments to aid in understanding its content. Unless otherwise specified, the methods used in this invention are conventional methods; the raw materials and apparatus used, unless otherwise specified, are conventional commercially available products.

[0021] Please see Figure 1-4 A dissolving device for preparing diethylene glycol monoethylene diether includes a tank 1, a discharge pipe 103 with a discharge valve at the bottom of the tank 1, and a top cover 2 at the top of the tank 1. The top cover 2 integrates a pressure relief valve 204, a pressure sensor 205, a dropper 206, a pH probe 207, and an oxygen concentration analyzer 208. The outlet of the dropper 206 and the detection probes of the pressure sensor 205, pH probe 207, and oxygen concentration analyzer 208 all extend into the interior of the tank 1. A stirring mechanism is provided inside the tank 1. The stirring mechanism includes a rotating shaft 3 and a first motor 303. The first motor 303 is fixed to the top of the top cover 2 and its output end is coaxially and fixedly connected to the rotating shaft 3. Multiple first crushing blades 301 are fixedly installed on the upper part of the outer circumference of the rotating shaft 3, multiple symmetrically distributed stirring rods 302 are fixedly installed in the middle part, and multiple stirring blades 5 are fixedly installed at the bottom.

[0022] A bracket 4 is fixedly installed at the bottom of the outer circumference of the tank 1. An annular nitrogen distribution pipe 401 is fixedly installed at the bottom of the bracket 4. A nitrogen inlet pipe 404 is connected to the outer wall of the annular nitrogen distribution pipe 401. An air flow regulating valve is installed on the outer wall of the nitrogen inlet pipe 404. Spray nozzles 402 are evenly distributed on the annular nitrogen distribution pipe 401. A solenoid valve 403 is installed on the outer wall of the spray nozzle 402 and the other end extends into the interior of the tank 1.

[0023] In this embodiment: solid raw material catalyst can be added into tank 1 through feeding pipe 201 on top cover 2; liquid raw material is injected into tank through feed pipe 202 after the flow rate is precisely controlled by metering pump 203; dropper 206 can realize the drop-by-drop addition of trace amounts of liquid raw material; pressure sensor 205, pH probe 207, and oxygen concentration analyzer 208 collect data on tank pressure, pH, and oxygen concentration in real time.

[0024] The first crushing blade 301 of the stirring mechanism rotates at high speed to initially crush the catalyst, reduce the particle size, and increase the dissolution contact area. The stirring rod 302 drives the solution to flow radially and circumferentially. In conjunction with the scraper 3021 that is attached to the inner wall of the tank, the material adhering to the tank wall is removed to avoid local agglomeration. The stirring blade 5 forms a vortex at the bottom of the tank 1 to accelerate the suspension of the settled material. In conjunction with the second crushing blade 601 driven by the second motor 6 at the bottom, the sedimented particles are crushed in real time to prevent dead corner residue.

[0025] Nitrogen gas is introduced into the tank through the annular nitrogen distribution pipe 401 via the nozzle 402. The nitrogen flow rate is controlled by the solenoid valve 403 and the air flow regulating valve to form an inert gas environment, inhibit the oxidation reaction of the raw materials, and ensure the safety of the dissolution process.

[0026] As a technical optimization of this utility model, two symmetrically distributed heating plates 101 are provided inside the jacket of the tank body 1, and a temperature sensor 102 is provided inside the tank body 1.

[0027] In this embodiment: the symmetrically distributed heating plates 101 generate heat after being powered on, and transfer the heat to the inner wall of the tank 1, so that the reaction system is heated to the set temperature. The temperature sensor 102 monitors the liquid phase temperature in the tank in real time and feeds the data back to the PLC touch screen all-in-one machine, which can adjust the temperature in the tank 1 in real time.

[0028] As a technical optimization of this utility model, multiple stirring rods 302 located on the same side are fixedly connected to a scraper 3021, and the scraper 3021 is in close contact with the inner wall of the tank 1.

[0029] In this embodiment: when the scraper 3021 rotates with the stirring rod 302, its edge is in close contact with the inner wall of the tank 1, scraping off the high-viscosity material (such as diethylene glycol or catalyst slurry) adhering to the wall. After removing the material adhering to the wall, the heat transfer efficiency between the tank wall and the reaction liquid is improved, preventing local overheating or cooling dead zones.

[0030] As a technical optimization of this utility model, the top of the top cover 2 is connected to a feeding pipe 201 with a sealing cover and a feed pipe 202, and the top of the top cover 2 is fixedly connected to a metering pump 203 connected to the feed pipe 202.

[0031] In this embodiment: the block catalyst is added through the sealing cover of the feed pipe 201 to prevent air from entering the tank 1. Liquid raw materials such as diethylene glycol are delivered by the metering pump 203 through the feed pipe 202 at a preset flow rate with an error of ≤±1%. The connection between the sealing cover and the pipe flange is sealed with an O-ring to prevent vinyl ether vapor from escaping.

[0032] As a technical optimization of this utility model, two symmetrical second motors 6 are installed at the bottom of the tank body 1. The output end of the second motor 6 passes through the tank body 1 through a mechanical seal and is equipped with a second crushing blade 601 for crushing the particulate matter deposited at the bottom of the tank body 1.

[0033] In this embodiment: the second motor 6 drives the second crushing blade 601 to rotate at high speed (800-1200rpm), further crushing the incompletely crushed catalyst particles deposited at the bottom of the tank to ≤0.5mm. The crushed particles are then reintroduced into the reaction system by the vortex generated by the stirring blade 5, thus avoiding bottom blockage.

[0034] As a technical optimization of this utility model, the inner wall of the tank 1 and the surface of the stirring mechanism are coated with a polytetrafluoroethylene anti-corrosion coating, and a fixing frame 7 is fixedly installed on the outer wall of the tank 1. A PLC touch screen all-in-one machine is fixedly installed on the outer wall of the fixing frame 7.

[0035] In this embodiment: the polytetrafluoroethylene anti-corrosion coating on the inner wall of the tank 1 and the surface of the stirring mechanism ensures corrosion resistance and extends the equipment life; the integrated PLC touch screen is electrically connected to the heating plate 101, temperature sensor 102, metering pump 203, pressure relief valve 204, pressure sensor 205, pH probe 207, oxygen concentration analyzer 208, first motor 303, second motor 6, air flow regulating valve, and solenoid valve 403. The integrated PLC touch screen integrates all detection signals (temperature, pressure, pH, oxygen concentration, etc.), displays process parameters in real time, and automatically adjusts the stirring speed, heating power, nitrogen flow rate, and feed rate of metering pump 203 according to the preset program to achieve fully automated control of the dissolution process.

[0036] The working principle and usage process of this utility model are as follows: In use, connect the nitrogen inlet pipe 404 to a nitrogen source (nitrogen tank). Add diethylene glycol to tank 1 quantitatively via feed pipe 202 and metering pump 203. Add block catalyst (such as sodium hydroxide) to tank 1 via feed pipe 201. Simultaneously, start the first motor 303, causing the first crushing blade 301 to rotate at high speed (300-500 rpm) with the rotating shaft 3, breaking the block catalyst into small particles. At the same time, the stirring rod 302 pushes the material radially. Incompletely crushed particles deposited at the bottom of the tank are further crushed by the second crushing blade 601 driven by the second motor 6 to prevent agglomeration. Then, start the heating plate 101 in the jacket to raise the temperature, maintaining the reaction temperature of tank 1 at 50-80℃ (feedback from temperature sensor 102 to PLC adjustment). Then, the reaction is carried out through the drip pipe 206... Vinyl ether is added slowly to avoid excessive local concentrations that could lead to evaporation. The pH probe 207 monitors the acidity and alkalinity of the reaction solution in real time. If the activity of the catalyst (such as acidic resin) decreases, an automatic replenishment signal is triggered, opening the air flow regulating valve on the nitrogen inlet pipe 404 to allow nitrogen to enter the annular nitrogen distribution pipe 401. The nitrogen enters the tank 1 through the nozzle 402 in the form of microporous bubbles, replacing the air in the tank until the oxygen concentration is <1% (monitored in real time by the oxygen concentration analyzer 208). The solenoid valve 403 and the air flow regulating valve control the nitrogen flow to form an inert gas environment, inhibiting the oxidation reaction of the raw materials and ensuring the safety of the dissolution process. The stirring blade 5 generates axial flow to promote the mass transfer between the liquid phase materials (diethylene glycol and vinyl ether) and the catalyst particles. The scraper 3021 rotates against the tank wall to remove adhering materials and avoid local overheating or reaction dead zones.

[0037] Pressure sensor 205 monitors the pressure inside the tank in real time. If the pressure exceeds the set threshold, pressure relief valve 204 opens immediately to release excess gas to the waste gas treatment system (not shown in the figure). The pH, temperature and oxygen concentration data are monitored by the PLC touch screen all-in-one machine. After the preset reaction time is reached, heating and stirring are automatically stopped, and the discharge valve of discharge pipe 103 is opened to discharge the product.

[0038] In the description of this utility model, it should be understood that the terms "left", "right", "up", "down", "top", "bottom", "front", "back", "inner", "outer", "back", "middle", etc., indicate the orientation or positional relationship based on the orientation or positional relationship shown in the accompanying drawings. They are only for the convenience of describing this utility model and simplifying the description, and do not indicate or imply that the device or element referred to must have a specific orientation, or be constructed and operated in a specific orientation. Therefore, they should not be construed as limitations on this utility model.

[0039] However, the above description is only a specific embodiment of this utility model and should not be construed as limiting the scope of implementation of this utility model. Therefore, any substitution of equivalent components or equivalent changes and modifications made in accordance with the scope of protection of this utility model should still fall within the scope of the claims of this utility model.

Claims

1. A dissolving device for preparing diethylene glycol monovinyl ether, comprising a tank body (1), a discharge pipe (103) provided with a discharge valve at the bottom of the tank body (1), and a top cover (2) provided at the top of the tank body (1), characterized in that: The top cover (2) integrates a pressure relief valve (204), a pressure sensor (205), a dropper (206), a pH probe (207), and an oxygen concentration analyzer (208). The outlet of the dropper (206) and the detection probes of the pressure sensor (205), pH probe (207), and oxygen concentration analyzer (208) all extend into the interior of the tank (1). The tank (1) is equipped with a stirring mechanism inside; the stirring mechanism includes a rotating shaft (3) and a first motor (303). The first motor (303) is fixed to the top of the top cover (2) and its output end is coaxially fixedly connected to the rotating shaft (3). Multiple first crushing blades (301) are fixedly installed on the upper part of the outer circumference of the rotating shaft (3), multiple symmetrically distributed stirring rods (302) are fixedly installed in the middle part, and multiple stirring blades (5) are fixedly installed at the bottom. A bracket (4) is fixedly installed at the bottom of the outer circumference of the tank (1). An annular nitrogen distribution pipe (401) is fixedly installed at the bottom of the bracket (4). A nitrogen inlet pipe (404) is connected to the outer wall of the annular nitrogen distribution pipe (401). An air flow regulating valve is provided on the outer wall of the nitrogen inlet pipe (404). Nozzles (402) are evenly distributed on the annular nitrogen distribution pipe (401). A solenoid valve (403) is installed on the outer wall of the nozzle (402) and the other end extends into the interior of the tank (1).

2. A dissolving device for preparing diethylene glycol monovinyl ether according to claim 1, characterized in that: The tank (1) has two symmetrically distributed heating plates (101) inside its jacket, and a temperature sensor (102) is installed inside the tank (1).

3. The dissolving apparatus for preparing diethylene glycol monoethylene diether according to claim 1, characterized in that: Multiple stirring rods (302) located on the same side are fixedly connected to a scraper (3021), and the scraper (3021) is in close contact with the inner wall of the tank (1).

4. The dissolving apparatus for preparing diethylene glycol monovinyl ether according to claim 1, characterized by: The top of the top cover (2) is connected to a feeding pipe (201) with a sealing cap and a feed pipe (202), and a metering pump (203) connected to the feed pipe (202) is fixedly connected to the top of the top cover (2).

5. The dissolving apparatus for preparing diethylene glycol monovinyl ether according to claim 1, characterized by: Two symmetrical second motors (6) are installed at the bottom of the tank (1). The output end of the second motor (6) passes through the tank (1) through a mechanical seal and is equipped with a second crushing blade (601) for crushing the particles deposited at the bottom of the tank (1).

6. The dissolving apparatus for preparing diethylene glycol monovinyl ether according to claim 1, characterized by: The inner wall of the tank (1) and the surface of the stirring mechanism are coated with polytetrafluoroethylene anti-corrosion coating. A fixing frame (7) is fixedly installed on the outer wall of the tank (1), and a PLC touch screen all-in-one machine is fixedly installed on the outer wall of the fixing frame (7).

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