Automatic dichloromethane water removal device
By employing stratification and condensation technology in an automated dichloromethane dehydration unit, the problem of low separation efficiency between dichloromethane and water has been solved, achieving efficient and low-cost dichloromethane purification.
Patent Information
- Application Number
- CN202423122069.X
- Authority / Receiving Office
- CN · China
- Patent Type
- Utility models(China)
- Current Assignee / Owner
- Filing Date
- 2024-12-17
- Publication Date
- 2025-12-05
- Estimated Expiration
- 2034-12-17
AI Technical Summary
Existing methods for separating dichloromethane and water are inefficient, complex to operate, and difficult to achieve high-purity separation. Traditional methods also suffer from problems such as high equipment costs, susceptibility to contamination, and the need for frequent replacement of adsorbents.
An automated dichloromethane dehydration device is adopted, which achieves effective separation of dichloromethane and water through a stratification, transfer and re-condensation process. The device utilizes a liquid stratification detector and a condenser to achieve effective separation. Combined with a jacket structure and refrigerant, multiple dehydration processes are performed to ensure the separation effect.
It achieves efficient separation of dichloromethane and water, with dichloromethane containing little or no water, thus improving dehydration efficiency and yield, preventing dichloromethane from evaporating and escaping, and reducing operating costs.
Smart Images
Figure CN223628621U_ABST
Abstract
Description
TECHNICAL FIELD
[0001] The utility model relates to dichloromethane water removal device technical field especially automatic dichloromethane water removal device. BACKGROUND
[0002] Most organic solvents have low boiling point, are easy to evaporate, are combustible and toxic, and their vapors emitted into the air can pollute the environment and are flammable and explosive. A large amount of organic solvents such as diethyl ether, acetone and dichloromethane are needed in pharmaceutical industry. The organic solvents contain a lot of impurities, which have a serious impact on the reuse of the solvents. In industrial production, considering economic and social benefits, the solvents must be recycled after use. The purpose of solvent recovery is to remove impurities affecting production, realize the reuse of solvents, reduce costs and protect the environment.
[0003] In chemical production, it is often necessary to effectively separate organic solvents and water. The separation process of dichloromethane, as a commonly used organic solvent, and water is particularly important. The traditional separation method has problems such as low efficiency and complex operation, and it is difficult to achieve high-purity separation.
[0004] There are many methods for removing water from dichloromethane, including membrane filtration, adsorption and fractional distillation. Among them, the membrane filtration method uses a hydrophobic and oleophilic membrane with a pore size of 0.001-20 μm. The separation mechanism is based on the difference in surface tension between dichloromethane and water. The separation of dichloromethane and water is realized. The adsorption method is to add an adsorbent such as calcium chloride or molecular sieve to the water-containing dichloromethane. The adsorbent adsorbs water by physical or chemical adsorption, thereby achieving water removal of dichloromethane. The fractional distillation method uses the difference in boiling point between dichloromethane and water. According to the difference in relative volatility between dichloromethane and water, the separation is carried out. By heating, the mixed solution of dichloromethane and water is boiled. Dichloromethane is first volatilized into a gas, and then a relatively pure dichloromethane is obtained by condensation and collection.
[0005] However, these methods have their own advantages and disadvantages. The membrane filtration method has the advantages of low energy consumption, easy operation and good water removal effect, and does not cause secondary pollution. However, the overall equipment cost of the membrane device is high, and the membrane may be contaminated or damaged, which needs to be replaced or maintained regularly, increasing the operating cost. For dichloromethane solution containing a large amount of solid particles or impurities, the membrane holes may be blocked, affecting the filtration effect. The adsorbent method is simple to operate and requires low equipment, but introduces new impurities (adsorbent) during the dehydration process, which needs to be separated and treated afterwards, causing secondary pollution. The adsorption capacity of the adsorbent is limited, and the adsorbent may need to be replaced or regenerated frequently, increasing the recovery cost. For dichloromethane with high water content, the adsorption effect may not be ideal. The fractional distillation method has a wide range of applications, but has high equipment investment and energy consumption. SUMMARY
[0006] The utility model wants to solve the technical problem of overcoming the deficiency in the prior art, provide a kind of automatic dichloromethane water removal device, through the process of layering, transfer and recondensation, the effective separation of dichloromethane and water is realized.
[0007] The utility model solves the technical problems of the technical scheme that it employs is:
[0008] A kind of automatic dichloromethane water removal device, raw material tank, first reaction kettle, second reaction kettle and finished product tank are sequentially connected by pipeline;Liquid layering detector is equipped at the bottom discharge port of the first reaction kettle, temperature detector for detecting the temperature in the kettle and mass sensor for detecting the liquid quality in the kettle are installed on the second reaction kettle;
[0009] Third pipeline is equipped at the bottom discharge port of the second reaction kettle, first circulation pipeline, circulating pump, second circulation pipeline and condenser are sequentially connected on the third pipeline, third circulation pipeline is connected with the top end circulating feed inlet of the second reaction kettle.
[0010] Further, first feed pipeline is equipped at the raw material tank discharge port, and the first feed pipeline is connected with the top end feed inlet of the first reaction kettle, and feed pump is equipped on the first feed pipeline;First pipeline is equipped at the bottom discharge port of the first reaction kettle, and the first pipeline is connected with second pipeline and waste water pipeline respectively, and the second pipeline is connected with the top end feed inlet of the second reaction kettle, and waste water pipeline is connected with sewage station;Product pipeline and fourth pipeline are further connected on the third pipeline, and the product pipeline is connected with the feed inlet of finished product tank, and the fourth pipeline is connected with the return inlet of raw material tank;Second feed pipeline for the mixed solution of dichloromethane and water is equipped on the raw material tank.
[0011] Further, return pipeline is connected between the second circulation pipeline and the third circulation pipeline, and eighth valve is installed on the return pipeline.
[0012] Further, the shell of the first reaction kettle is jacket structure, and the shell of the second reaction kettle is jacket structure, and the bottom of the first reaction kettle and the second reaction kettle is respectively provided with refrigerant inlet communicated with the jacket structure, and the top of the first reaction kettle and the second reaction kettle is respectively provided with refrigerant outlet communicated with the jacket structure.
[0013] Further, nitrogen inlet pipe and vent pipe are respectively provided on the top of the raw material tank, the first reaction kettle, the second reaction kettle and the finished product tank, and cold trap is provided on the vent pipe.
[0014] Further, fourth valve is provided on the third pipeline, and sixth valve is provided on the first circulation pipeline.
[0015] Further, the condenser is stainless steel spiral plate condenser or glass disc type condenser.
[0016] Further, the first pipeline and the third pipeline are respectively provided with a sight glass for observing the inside of the pipeline.
[0017] Further, the first pipeline is provided with a first valve, the second pipeline is provided with a third valve, the wastewater pipeline is provided with a second valve, the finished product pipeline is provided with a fifth valve, and the fourth pipeline is provided with a seventh valve.
[0018] Further, the wastewater pipeline is provided with a ninth valve, and the ninth valve is arranged close to the sewage station.
[0019] The utility model discloses the beneficial effect is: the utility model discloses simple structure, reasonable in design has the following advantages:
[0020] (1), the mixed solution of dichloromethane and water to be handled is stratified in the first reation kettle, realizes primary water removal, is transferred to the second reation kettle, realizes again water removal through condensation, after two times water removal, the water content in dichloromethane is less or even does not contain water, and the water removal efficiency is high, realizes the effective separation of dichloromethane and water;
[0021] (2), the first reation kettle bottom discharge port is equipped with liquid layered detector, and the layered condition of mixed solution in the first reation kettle is detected in real time, when the layered interface is clear and stable, then subsequent operation is carried out, ensures that the separation effect is more thorough, this can avoid the separation insufficient or low efficiency problem caused by the insufficient or excessive static time;
[0022] (3), the vent pipeline of the first reation kettle, the second reation kettle, raw material tank and finished product tank is all provided with cold trap, and the material liquid can avoid dichloromethane volatilization escape during mutual transfer between the first reation kettle, the second reation kettle, raw material tank and finished product tank, improves the finished product rate. BRIEF DESCRIPTION OF DRAWINGS
[0023] In order to more clearly illustrate the specific embodiment of the utility model or the technical scheme in the prior art, the following will be briefly introduced the drawings needed to be used in the specific embodiment or the prior art description, obviously, the drawings in the following description are some embodiments of the utility model, and for those skilled in the art, other drawings can be obtained according to these drawings without creative labor.
[0024] Figure 1 It is the structural schematic diagram of the utility model.
[0025] In the figure: 1. first reactor, 2. second reactor, 3. raw material tank, 4. finished product tank, 5. sewage station, 6. first feeding pipeline, 7. feeding pump, 8. liquid layering detector, 9. first pipeline, 10. second pipeline, 11. waste water pipeline, 12. finished product pipeline, 13. third pipeline, 14. first circulation pipeline, 15. circulation pump, 16. second circulation pipeline, 17. return material pipeline, 18. condenser, 19. third circulation pipeline, 20. temperature detector, 21. mass sensor, 22. fourth pipeline, 23. second feeding pipeline, 24. eighth valve, 25. nitrogen inlet pipe, 26. vent pipe, 27. first valve, 28. second valve, 29. third valve, 30. ninth valve, 31. fourth valve, 32. fifth valve, 33. sixth valve, 34. seventh valve. DETAILED DESCRIPTION
[0026] It should be noted that the following detailed description is exemplary in nature and is intended to provide further description of the present application. Unless otherwise defined, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this application belongs.
[0027] It is to be understood that the terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of example embodiments in accordance with the present application. As used herein, the singular forms "a", "an" and "the" are intended to include the plural forms as well, unless the context clearly indicates otherwise. It will be further understood that the terms "comprises" and / or "comprising," when used in this specification, specify the presence of stated features, steps, operations, elements, and / or components, but do not preclude the presence or addition of one or more other features, steps, operations, elements, components, and / or groups thereof.
[0028] The technical solutions of the present application will be described clearly and completely below in conjunction with embodiments. Obviously, the described embodiments are only part of the embodiments of the present application, rather than all the embodiments. Based on the embodiments in the present application, all other embodiments obtained by those skilled in the art without creative labor fall within the scope of protection of the present application.
[0029] As Figure 1The automatic dichloromethane water removal device is connected with a raw material tank 3, a first reaction kettle 1, a second reaction kettle 2 and a finished product tank 4 in sequence through pipelines; the first reaction kettle 1 is provided with a liquid layering detector 8 at a bottom discharge port; the second reaction kettle 2 is provided with a temperature detector 20 for detecting the temperature in the kettle and a mass sensor 21 for detecting the mass of liquid in the kettle; the second reaction kettle 2 is provided with a third pipeline 13 at a bottom discharge port; the third pipeline 13 is connected with a first circulation pipeline 14, a circulation pump 15, a second circulation pipeline 16 and a condenser 18 in sequence; the condenser 18 is connected with a third circulation pipeline 19; and the third circulation pipeline 19 is connected with a top circulation inlet of the second reaction kettle 2. The automatic dichloromethane water removal device further comprises a controller for controlling the operation of the device.
[0030] Dichloromethane (CH2Cl2) is an organic solvent that is insoluble in water. When dichloromethane and water are mixed, the two liquids do not form a homogeneous solution due to the difference in polarity between them. Water is a polar molecule because its oxygen atom has a negative charge and its hydrogen atom has a positive charge. Dichloromethane, although also a polar molecule, has a weaker intermolecular force that is not strong enough to form a stable solution with water. When dichloromethane and water are mixed, they will naturally separate into layers due to the difference in density and polarity. Dichloromethane has a higher density than water, so it will form a layer below the water. After the mixed solution of dichloromethane and water to be treated is introduced into the first reaction kettle 1, dichloromethane and water will separate into layers by standing.
[0031] The liquid layering detector 8 uses optical refractive index sensors, conductivity sensors and color sensors to improve the accuracy of the transfer process of the mixed solution.
[0032] The raw material tank 3 is provided with a first feeding pipeline 6 connected with a top feeding inlet of the first reaction kettle 1, and the first feeding pipeline 6 is provided with a feeding pump 7; the first reaction kettle 1 is provided with a first pipeline 9 at a bottom discharge port, and the first pipeline 9 is connected with a second pipeline 10 and a wastewater pipeline 11 respectively, the second pipeline 10 is connected with a top feeding inlet of the second reaction kettle 2, and the wastewater pipeline 11 is connected with a sewage station 5; the third pipeline 13 is further connected with a finished product pipeline 12 and a fourth pipeline 22, the finished product pipeline 12 is connected with a feeding inlet of the finished product tank 4, and the fourth pipeline 22 is connected with a return inlet of the raw material tank 3; the raw material tank 3 is provided with a second feeding pipeline 23 for introducing a mixed solution of dichloromethane and water.
[0033] The second circulation pipeline 16 and the third circulation pipeline 19 are connected with a return pipeline 17, and the return pipeline 17 is provided with an eighth valve 24.
[0034] The shell of the first reactor 1 is a jacket structure, and the shell of the second reactor 2 is also a jacket structure. The bottom of the first reactor 1 and the bottom of the second reactor 2 are respectively provided with a refrigerant inlet communicating with the jacket structure. The top of the first reactor 1 and the top of the second reactor 2 are respectively provided with a refrigerant outlet communicating with the jacket structure.
[0035] The top of the raw material tank 3, the top of the first reactor 1, the top of the second reactor 2 and the top of the finished product tank 4 are respectively provided with a nitrogen inlet pipe 25 and a vent pipe 26. The vent pipe 26 is provided with a cold trap.
[0036] The third pipeline 13 is provided with a fourth valve 31, and the first circulation pipeline 14 is provided with a sixth valve 33.
[0037] The condenser 18 is a stainless steel spiral plate condenser or a glass-lined disc condenser. The heat transfer area is greatly increased compared with the reactor jacket, which can quickly cool the dichloromethane from room temperature to about 2℃.
[0038] The first pipeline 9 and the third pipeline 13 are respectively provided with a sight glass for observing the internal condition of the pipeline.
[0039] The first pipeline 9 is provided with a first valve 27, the second pipeline 10 is provided with a third valve 29, the waste water pipeline 11 is provided with a second valve 28, the finished product pipeline 12 is provided with a fifth valve 32, and the fourth pipeline 22 is provided with a seventh valve 34. The waste water pipeline 11 is also provided with a ninth valve 30, which is arranged close to the sewage station 5.
[0040] The first valve 27 is a pneumatic regulating valve, the second valve 28 is a pneumatic shut-off valve, the third valve 29 is a pneumatic regulating valve, the fourth valve 31 is a pneumatic regulating valve, the fifth valve 32 is a pneumatic shut-off valve, the sixth valve 33 is a pneumatic shut-off valve, the seventh valve 34 is a manual shut-off valve, the eighth valve 24 is a manual shut-off valve, and the ninth valve 30 is a ball valve.
[0041] The controller adjusts the opening degree of the first valve 27, the third valve 29 and the fourth valve 31 in real time according to the monitored parameters, so as to realize accurate control of the transfer flow of dichloromethane and avoid affecting the subsequent process due to excessive or insufficient flow. When the controller detects a strong signal of dichloromethane, the opening degree of the third valve 29 can be appropriately increased to speed up the transfer speed. When the signal is weak or unstable, the opening degree of the third valve 29 is reduced to ensure that the water content of the transferred dichloromethane is always kept at a low level.
[0042] The working process of the automatic dichloromethane water removal device is as follows:
[0043] (1), the mixed solution of dichloromethane and water to be treated is introduced into the raw material tank 3, the feed pump 7 is working, and the mixed solution of dichloromethane and water is introduced into the first reaction kettle 1 through the first feed pipeline 6; after the mixed solution of dichloromethane and water enters the first reaction kettle 1, it is placed for 10-20 minutes, dichloromethane and water are layered to form two obvious liquid layers, and dichloromethane is below water; At this time, the first valve 27 and the third valve 29 are opened, and the nitrogen inlet pipe 25 of the first reaction kettle 1 is introduced into nitrogen, and the vent pipe 26 of the second reaction kettle 2 is working, the dichloromethane at the bottom of the first reaction kettle 1 is introduced into the second reaction kettle 2 in turn through the first pipeline 9 and the second pipeline 10, and the dichloromethane aqueous solution at the bottom of the first reaction kettle 1 is subjected to primary water removal, and the water content is less;
[0044] (2), when the dichloromethane aqueous solution after primary water removal is transferred to the second reaction kettle 2, the liquid layering detector 8 installed at the bottom discharge port of the first reaction kettle 1 always detects the properties of the flowing liquid in the pipeline, when the optical refractive index range, the electric conductivity signal and the color are not in the corresponding range of dichloromethane, the controller automatically closes the third valve 29, opens the second valve 28 and the ninth valve 30, and the water in the upper layer of the first reaction kettle 1 is discharged to the sewage station 5, at this time, the water contains a small amount of dichloromethane, which can be treated into the sewage station 5; At the same time, the first reaction kettle 1 stops introducing nitrogen, and the second reaction kettle 2 stops venting;
[0045] (3), when the dichloromethane aqueous solution in the first reaction kettle 1 is completely transferred to the second reaction kettle 2, the fourth valve 31, the sixth valve 33 and the circulating pump 15 are opened, the dichloromethane aqueous solution is cooled and circulated through the condenser 18, during which the temperature detector 20 monitors the liquid temperature in the second reaction kettle 2 in real time, when the temperature monitoring value is close to 2℃, the controller will automatically close the fourth valve 31, the sixth valve 33 and the circulating pump 15, and the circulation is automatically terminated; The eighth valve 24 is set to be opened 60 seconds after the circulating pump 15 is closed, so that the residual dichloromethane aqueous solution in the condenser 18 is introduced into the second reaction kettle 2 through the return pipeline 17;
[0046] (4), the jacket of the second reaction kettle 2 is connected with refrigerant, under the action of the jacket, the fluid in the kettle is slowly cooled to zero degree below zero, due to the density difference, water is floating on the surface of dichloromethane, the freezing point of dichloromethane is-96.7 ℃, and the freezing point of water is 0 ℃; due to the different freezing temperatures, a layer of ice will be formed on the surface of the liquid in the kettle, when the temperature in the second reaction kettle 2 reaches-5 ℃ and lasts for 30-60 minutes, the fourth valve 31 and the fifth valve 32 are automatically opened, at the same time, the second reaction kettle 2 is connected with nitrogen, and the emptying pipe 26 of the product tank 4 works, so that the lower layer of dichloromethane in the second reaction kettle 2 is transferred to the product tank 4 through the product pipeline 12; the mass sensor 21 arranged on the second reaction kettle 2, when the weight of 3000L dichloromethane in the second reaction kettle 2 is reduced to 50-100L, the controller automatically closes the fifth valve 32, at this time, the dichloromethane in the second reaction kettle 2 does not contain water (or the water content is not more than 0.05%, which meets the use requirement);
[0047] (5), the ice in the second reaction kettle 2 melts at room temperature, at this time, the melted water contains part of dichloromethane, the controller opens the seventh valve 34, and the melted water and dichloromethane are discharged and transferred to the raw material tank 3, a new batch of dichloromethane and water mixed solution is supplemented in the raw material tank 3, and is transported to the first reaction kettle 1 through the feed pump 7, and the above water removal operation is repeated.
[0048] In summary, the utility model has the advantages of simple structure, reasonable design and the following advantages:
[0049] (1), the mixed solution of dichloromethane and water to be treated is statically stratified in the first reaction kettle 1, so that the water is removed initially; the mixed solution is transferred to the second reaction kettle 2, and the water is removed again through condensation, and after two times of water removal, the water content in the dichloromethane is small or even no water, and the water removal efficiency is high;
[0050] (2), the liquid stratification detector 8 is arranged at the bottom discharge port of the first reaction kettle 1, the stratification of the mixed solution in the first reaction kettle 1 is detected in real time, when the stratification interface is clear and stable, the subsequent operation is carried out, so that the separation effect is more thorough, and the problems of insufficient or excessive separation time and low efficiency caused by insufficient or excessive separation time can be avoided;
[0051] (3), the emptying pipelines of the first reaction kettle 1, the second reaction kettle 2, the raw material tank 3 and the product tank 4 are all provided with cold traps, so that the dichloromethane can be prevented from escaping and volatilizing during the mutual transfer of the liquid between the first reaction kettle 1, the second reaction kettle 2, the raw material tank 3 and the product tank 4, and the product yield is improved.
[0052] Finally, it should be noted that: the above embodiments are used to illustrate the technical solutions of the present application, but not limited to them; although the present application has been described in detail with reference to the foregoing embodiments, those skilled in the art should understand that: it can still modify the technical solutions recorded in the foregoing embodiments, or make equivalent replacement to part or all of the technical features; and these modifications or replacements do not make the essence of the corresponding technical solutions deviate from the scope of the technical solutions of the embodiments of the present application.
Claims
1. An automated dichloromethane dewatering device, characterized in that: The raw material tank (3), the first reactor (1), the second reactor (2) and the finished product tank (4) are connected in sequence through pipelines; the first reactor (1) is equipped with a liquid stratification detector (8) at the bottom outlet, and the second reactor (2) is equipped with a temperature detector (20) for detecting the temperature inside the reactor and a mass sensor (21) for detecting the quality of the liquid inside the reactor. The bottom outlet of the second reactor (2) is provided with a third pipeline (13), and the third pipeline (13) is connected in sequence to the first circulation pipeline (14), the circulation pump (15), the second circulation pipeline (16) and the condenser (18). The outlet of the condenser (18) is connected to the third circulation pipeline (19), and the third circulation pipeline (19) is connected to the top circulation inlet of the second reactor (2).
2. The automated dichloromethane dewatering device according to claim 1, characterized in that: The raw material tank (3) is provided with a first feed pipe (6) at the outlet, which is connected to the top feed port of the first reactor (1). A feed pump (7) is provided on the first feed pipe (6). The first reactor (1) is provided with a first pipe (9) at the bottom outlet, which is connected to a second pipe (10) and a wastewater pipe (11). The second pipe (10) is connected to the top feed port of the second reactor (2), and the wastewater pipe (11) is connected to a sewage station (5). The third pipe (13) is also connected to a finished product pipe (12) and a fourth pipe (22). The finished product pipe (12) is connected to the feed port of the finished product tank (4), and the fourth pipe (22) is connected to the return port of the raw material tank (3). The raw material tank (3) is provided with a second feed pipe (23) through which a mixed solution of dichloromethane and water is introduced.
3. The automated dichloromethane dewatering device according to claim 1, characterized in that: A return pipe (17) is connected between the second circulation pipe (16) and the third circulation pipe (19), and an eighth valve (24) is installed on the return pipe (17).
4. The automated dichloromethane dewatering device according to claim 1, characterized in that: The shell of the first reactor (1) is a jacketed structure, the shell of the second reactor (2) is a jacketed structure, the bottom of the first reactor (1) and the second reactor (2) are respectively provided with a coolant inlet that connects to the jacketed structure, and the top of the first reactor (1) and the second reactor (2) are respectively provided with a coolant outlet that connects to the jacketed structure.
5. The automated dichloromethane dewatering device according to claim 1, characterized in that: The top of the raw material tank (3), the first reactor (1), the second reactor (2) and the finished product tank (4) are respectively provided with a nitrogen inlet pipe (25) and a vent pipe (26), and a cold trap is provided on the vent pipe (26).
6. The automated dichloromethane dewatering device according to claim 1, characterized in that: The third pipeline (13) is equipped with a fourth valve (31), and the first circulation pipeline (14) is equipped with a sixth valve (33).
7. The automated dichloromethane dewatering device according to claim 1, characterized in that: The condenser (18) is a stainless steel spiral plate condenser or a glass-lined disc condenser.
8. The automated dichloromethane dewatering device according to claim 2, characterized in that: The first pipeline (9) and the third pipeline (13) are respectively equipped with sight glasses to facilitate observation of the internal conditions of the pipeline.
9. The automated dichloromethane dewatering device according to claim 2, characterized in that: The first pipeline (9) is equipped with a first valve (27), the second pipeline (10) is equipped with a third valve (29), the wastewater pipeline (11) is equipped with a second valve (28), the finished product pipeline (12) is equipped with a fifth valve (32), and the fourth pipeline (22) is equipped with a seventh valve (34).
10. The automated dichloromethane dewatering device according to claim 9, characterized in that: The wastewater pipeline (11) is equipped with a ninth valve (30), which is located near the sewage station (5).