An extraction apparatus for diethylene glycol dibutyl ether

Abstract

The utility model discloses a kind of extraction equipment for diethylene glycol dibutyl ether, it is related to chemical reaction device technical field, including reaction kettle, condenser, spiral water lift and at least one fraction receiving tank;The reaction kettle is equipped with heating jacket, temperature detection device and stirring device, the upper portion of the reaction kettle is connected with spiral water lift, and lower portion is equipped with discharge valve;The utility model can make the moisture of reaction generation and inherent water in material timely, continuously leave reaction system by integrated water lift, break reaction balance, effectively promote williamson ether synthesis reaction to positive direction, to significantly improve raw material conversion rate;Design for the particularity of diethylene glycol dibutyl ether synthesis process, solve high-boiling, water-containing system separation problem, with short process, high yield, solvent recyclable etc. Characteristic, meet the economic environmental protection requirement of green chemical industry.

Description

Technical Field

[0001] This utility model relates to the field of chemical reaction equipment technology, and in particular to an extraction device for diethylene glycol dibutyl ether. Background Technology

[0002] Diethylene glycol dibutyl ether is a colorless and transparent liquid with a freezing point of -60.2℃, a boiling point of 256℃, a relative density of 0.8853 (20 / 20℃), a refractive index of 1.4235, and a flash point of 47℃. It is miscible with ethers, alcohols, esters, ketones, and halogenated hydrocarbons, slightly soluble in water, and forms an azeotropic mixture with 94.7% water, with an azeotropic point of 99.8℃.

[0003] Due to its high boiling point, high flash point, low specific gravity, low toxicity, and low pollution, and because its molecule contains two ether bonds with oxygen atoms, diethylene glycol dibutyl ether (DEGE) is a safe and environmentally friendly solvent, with performance superior to DEGE monobutyl ether (DIE). DEGE shows excellent application prospects in coatings, inks, fatty acid separation and extraction, fragrances, pharmaceuticals, metal separation (especially gold extraction), chemical coupling, reaction intermediates, brake fluid formulation, aviation gasoline antifreeze, metal cleaning, and mineral flotation.

[0004] In the process of synthesizing diethylene glycol dibutyl ether by the Williamson reaction of diethylene glycol butyl ether and chlorobutane, the reaction is not complete due to the relationship between activity and steric hindrance. The reaction solution contains 20% to 25% unreacted diethylene glycol butyl ether and about 2.5% water, which has a great impact on the distillation product diethylene glycol dibutyl ether.

[0005] Therefore, in response to the above phenomenon, an extraction device for diethylene glycol dibutyl ether is proposed to meet the needs of practical use. Utility Model Content

[0006] This invention provides an extraction device for diethylene glycol dibutyl ether, which can effectively improve the raw material conversion rate and has the advantages of being green, economical, and efficient, resulting in a high-content, high-quality product.

[0007] To achieve the above objectives, this utility model provides an extraction device for diethylene glycol dibutyl ether, comprising a reaction vessel, a condenser, a spiral water lifter, and at least one fraction receiving tank; the reaction vessel is equipped with a heating jacket, a temperature detection device, and a stirring device; the spiral water lifter is connected above the reaction vessel and a discharge valve is provided below it; the condenser is located above the spiral water lifter and is used to condense the steam from the reaction vessel; the upper end of the spiral water lifter is connected to both the condenser and the reaction vessel, and is used to separate and discharge water; the fraction receiving tank is connected to the spiral water lifter and is used to receive the separated liquid.

[0008] Preferably, the reactor is provided with a sight glass and a feeding port at the top.

[0009] Preferably, the lining material of the reactor is glass-lined glass or polytetrafluoroethylene.

[0010] Preferably, the heating jacket contains heat-conducting oil as a heat transfer medium and is covered with insulation material on the outside.

[0011] Preferably, the condenser is a shell-and-tube condenser, and a cooling medium is provided in the cavity between the shell and the internal tubes of the shell-and-tube condenser.

[0012] Preferably, a vacuum tube is connected above the condenser, and a vacuum valve is provided on the vacuum tube.

[0013] Preferably, the stirring device is an anchor-type stirrer, and the surface of the anchor-type stirrer is covered with a protective layer of the same material as the lining of the reactor.

[0014] Preferably, the spiral water pump includes a spiral tube and a small storage tank located below the spiral tube, the small storage tank being equipped with a liquid level detection device.

[0015] Preferably, the connecting pipeline between the spiral water lifter and the reactor is provided with a water lifter insulation layer.

[0016] Preferably, the upper part of the fraction receiving tank is connected to a vacuum tube via a connecting pipe to maintain the system at an isobaric state.

[0017] Compared with related technologies, the extraction device for diethylene glycol dibutyl ether provided by this utility model has the following beneficial effects:

[0018] This invention integrates a water extractor, which enables the water generated in the reaction and the water inherent in the materials to leave the reaction system in a timely and continuous manner, breaking the reaction equilibrium and effectively promoting the Williamson ether synthesis reaction in the positive direction, thereby significantly improving the raw material conversion rate.

[0019] This invention features a staged distillation receiving capability, which can further distill off and separate unreacted raw materials (such as diethylene glycol monobutyl ether) after dehydration, thereby concentrating the reaction solution. This makes the subsequent distillation operation of the target product, diethylene glycol dibutyl ether, more efficient and energy-saving, ultimately yielding a high-purity, high-quality product.

[0020] This invention employs a spiral capillary water extractor with a heat preservation design, combined with a vacuum system and an isobaric connection to the receiving tank, ensuring smooth vapor-liquid flow and a clear interface during distillation and separation. It also achieves automatic reflux of the water-carrying agent and effective water discharge, resulting in continuous and stable operation.

[0021] This invention is designed specifically for the synthesis process of diethylene glycol dibutyl ether, solving the problem of separating high-boiling-point, water-containing systems. It features a short process, high yield, and recyclable solvent, meeting the economic and environmental requirements of green chemistry. Attached Figure Description

[0022] Figure 1 This is a schematic diagram of the overall structure of this utility model.

[0023] Labels in the diagram: 1. Reactor; 2. Heating jacket; 3. Water lifter insulation layer; 4. Cooling medium; 5. Vacuum tube; 6. First receiving tank; 7. Second receiving tank; 8. Third receiving tank; 9. First temperature probe; 10. Second temperature probe; 11. Condenser; 12. Discharge valve; 13. Water lifter valve; 14. First feed valve; 15. Second feed valve; 16. Third feed valve; 17. First discharge valve; 18. Second discharge valve; 19. Third discharge valve; 20. Vacuum valve; 21. Stirring device; 22. Connecting pipe; 23. Spiral water lifter. Detailed Implementation

[0024] The preferred embodiments of the present invention will now be described in detail with reference to the accompanying drawings. These embodiments are implemented based on the technical solution of the present invention, and it should be understood that these embodiments are for illustrative purposes only and not for limiting the scope of the present invention.

[0025] like Figure 1 As shown, the extraction equipment provided by this utility model includes a reaction vessel 1, a condenser 11, a spiral water lifter 23, and multiple fraction receiving tanks (first receiving tank 6, second receiving tank 7, and third receiving tank 8). The reaction vessel 1 is equipped with a heating jacket 2, a temperature detection device, and a stirring device 21. The upper part of the reaction vessel 1 is connected to the spiral water lifter 23, and the lower part of the reaction vessel 1 is equipped with a discharge pipe controlled by a discharge valve 12. The condenser 11 is fixed above the spiral water lifter 23, and the material vapor is cooled in the condenser 11 and then flows back into the spiral water lifter 23. The upper end of the spiral water lifter 23 is connected to the condenser 11, and the spiral water lifter 23 is connected to the reaction vessel 1 through a side pipe. The side pipe connecting to the reaction vessel 1 is equipped with a water lifter insulation layer 3, and the lower end of the spiral water lifter 23 is connected to multiple fraction receiving tanks through a water lifter valve 13. The temperature detection device includes a first temperature probe 9 and a second temperature probe 10; the first temperature probe 9 is inserted into the reactor 1 to monitor the internal temperature of the reactor 1, and the second temperature probe 10 is inserted into the side tube to monitor the temperature in the side tube.

[0026] A sight glass and a feeding port are installed on the top of the reactor 1. Its lining is preferably made of glass-lined glass or polytetrafluoroethylene (PTFE), with stainless steel being a secondary option, to prevent corrosion from the reactants. The heating jacket 2 uses heat transfer oil as the heat transfer medium and is covered with insulation material. The condenser 11 is a shell-and-tube condenser. Cooling medium 4 flows through the cavity between the shell and the internal tubes. Cooling medium 4 enters through the lower port and exits through the upper port to ensure sufficient condensation effect. A vacuum tube 5 is installed at the top of the condenser 11, controlled by a vacuum valve 20. The stirring device 21 is an anchor-type stirrer. The surface of the stirring device 21 is covered with a protective layer of the same material as the lining of the reactor 1. A reducer and motor are connected to the upper end of the stirring device 21 for easy adjustment of the stirring speed.

[0027] In this embodiment, the spiral water extractor 23 is designed as a spiral capillary tube, with the bottom of the spiral capillary tube connected to the side tube via a connecting capillary tube. A small storage tank is designed below the spiral tube to store the separated water, and a level gauge is installed on the small storage tank. During operation, the interface between the water and the water-carrying agent must not be higher than the lower end of the connecting capillary tube to facilitate the return of the water-carrying agent into the reaction vessel 1.

[0028] In this embodiment, three fraction receiving tanks are provided, including a first receiving tank 6, a second receiving tank 7, and a third receiving tank 8. The first receiving tank 6 is equipped with a first inlet valve 14 and a first outlet valve 17 at its upper and lower ends, respectively; the second receiving tank 7 is equipped with a second inlet valve 15 and a second outlet valve 18 at its upper and lower ends, respectively; and the third receiving tank 8 is equipped with a third inlet valve 16 and a third outlet valve 19 at its upper and lower ends, respectively. Furthermore, the upper ends of each fraction receiving tank are connected by a thin stainless steel tube and then connected to a vacuum tube 5 via a connecting pipe 22 to ensure that the entire system is under isobaric conditions.

[0029] The specific operation process is as follows:

[0030] Before adding the reactants to reactor 1, close the discharge valve 12, add the reactants, close the feed port, turn on the stirring device 21, and control the speed at 100 r / min. Start heating in the heating jacket 2 and gradually raise the temperature to the normal reaction temperature of the materials. Stir the reaction for a certain period of time. Turn on the vacuum valve 20 and the vacuum pump to slowly reduce the pressure inside the reactor, so that the distillate is discharged evenly.

[0031] Stage 1: The distillate mainly consists of water-carrying agent and water. After being cooled by the condenser 11, the distillate vapor enters the spiral water lifter 23 and stratifies in the lower small storage tank. When a certain amount of water is stored, the water lifter valve 13 is opened to allow the lower layer of water to enter the first receiving tank 6. It is necessary to ensure that the stratification interface is lower than the upper side pipe opening of the small storage tank to facilitate the water-carrying agent to flow back into the reaction vessel 1 through the side pipe.

[0032] Second stage: When the distillate becomes clear and no longer separates into layers, it enters the second stage of distillation. The distillate in this stage is the pre-reaction fraction. After being cooled by steam, it enters the second receiving tank 7 through the spiral water lifter 23. When the second temperature probe 10 of the water lifter displays the boiling point temperature of the target product at that pressure, the crude target product is received and stored in the third receiving tank 8 for future rectification.

[0033] When the temperature of the second temperature probe 10 of the water pump continues to rise, the temperature of the reactor 1 is cooled down. When the temperature of the reactor 1 drops to the specified temperature, the vacuum pump and vacuum valve 20 are turned off, and the material in the reactor 1 is removed for later use.

[0034] The above embodiments are for illustrative purposes only and are not intended to limit the scope of this utility model. Those skilled in the art should understand that many changes, modifications, and even equivalents can be made to this utility model within the spirit and scope defined by the claims, all of which will fall within the protection scope of this utility model.

Claims

1. An extraction apparatus for diethylene glycol dibutyl ether, characterized in that, The apparatus includes a reaction vessel, a condenser, a spiral water lifter, and at least one fraction receiving tank. The reaction vessel is equipped with a heating jacket, a temperature detection device, and a stirring device. The spiral water lifter is connected to the top of the reaction vessel, and a discharge valve is located at the bottom of the reaction vessel. The condenser is positioned above the spiral water lifter and is used to condense the steam from the reaction vessel. The upper end of the spiral water lifter is connected to both the condenser and the reaction vessel and is used to separate and discharge water. The fraction receiving tank is connected to the spiral water lifter and is used to receive the separated liquid.

2. The extraction apparatus according to claim 1, characterized in that, The reactor is equipped with a sight glass and a feeding port on its upper part.

3. The extraction apparatus according to claim 1, characterized in that, The lining material of the reactor is glass enamel or polytetrafluoroethylene.

4. The extraction apparatus according to claim 1, characterized in that, The heating jacket contains heat-conducting oil as the heat transfer medium and is covered with insulation material on the outside.

5. The extraction apparatus according to claim 1, characterized in that, The condenser is a shell-and-tube condenser, and a cooling medium is provided in the cavity between the shell and the internal tubes of the shell-and-tube condenser.

6. The extraction apparatus according to claim 1 or 5, characterized in that, A vacuum tube is connected above the condenser, and a vacuum valve is installed on the vacuum tube.

7. The extraction apparatus according to claim 1, characterized in that, The stirring device is an anchor-type stirrer, and the surface of the anchor-type stirrer is covered with a protective layer of the same material as the inner lining of the reactor.

8. The extraction apparatus according to claim 1, characterized in that, The spiral water pump includes a spiral tube and a small storage tank located below the spiral tube. The small storage tank is equipped with a liquid level detection device.

9. The extraction apparatus according to claim 1 or 8, characterized in that, The connecting pipe between the spiral water lifter and the reactor is equipped with a water lifter insulation layer.

10. The extraction apparatus according to claim 1, characterized in that, The upper part of the fraction receiving tank is connected to the vacuum tube via a connecting pipe to maintain the system at an isobaric state.

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