A purification device

Abstract

The utility model relates to a kind of purification device, it is related to purification equipment technical field, including distillation column, the top of the distillation column is provided with condenser pipe, the outer surface of the condenser pipe is provided with heat recovery preheating pipe, the outer surface of the heat recovery preheating pipe is inlaid to the outer surface of the distillation column outside, by the heat conducting medium of ladder type, it can utilize the condensing waste heat of condenser pipe and the heat dissipation of distillation column, raw material is preheated to approach boiling point, substantially reduce the heating load of distillation column, reduce the energy consumption of heating, spiral feed pipe increases the contact area with heat conducting medium, cooperate gradient boiling point heat conducting medium, can be targeted absorption different temperature zone heat, improve energy utilization rate, and by the mechanical self-adapting structure of condenser pipe built-in, according to steam pressure automatic regulation delamination interception and impurity discharge, without manual intervention, improve the batch consistency of purity processing.

Description

Technical Field

[0001] This utility model relates to the field of purification equipment technology, specifically to a purification device. Background Technology

[0002] Dimethylformamide (DMF) is an important organic compound, which is a colorless, transparent or pale yellow liquid with a fishy or slightly peculiar odor. It has good chemical reactivity and can undergo substitution, addition, condensation and other reactions with a variety of compounds. DMF has a wide range of applications in chemical, pharmaceutical, and pesticide fields. As an important intermediate for drug synthesis, the demand for DMF is increasing year by year.

[0003] Impurities are inevitable in industrial-grade or crude DMF. These impurities directly affect its performance, safety, and even the quality of the final product in different fields. In order to make DMF suitable for application scenarios, avoid the harm of impurities, and ensure product quality and safety, DMF needs to be purified to ensure its purity. Only by purifying and removing harmful substances such as moisture, acid / alkaline impurities, and solid particles can DMF meet the performance requirements of specific fields and avoid reaction failures, equipment damage, product scrapping, and even safety risks caused by impurities.

[0004] In existing DMF purification systems, distillation is the main purification method. Since DMF has a boiling point of 153℃, it easily forms azeotropes with impurities. Traditional batch distillation requires heating the entire DMF feedstock to above the boiling point. In order to break the azeotropic system of DMF with impurities such as water and dimethylamine, it is often necessary to introduce an extractant or use negative pressure distillation, which increases the heating / cooling energy consumption. Furthermore, traditional purification relies on manual adjustment of parameters such as heating power and reflux ratio, resulting in low operational precision and easy differences in the purity of different batches of DMF, leading to low batch stability. Utility Model Content

[0005] This utility model addresses the technical problems existing in the prior art by providing a purification device.

[0006] The technical solution of this utility model to solve the above-mentioned technical problems is as follows: A purification apparatus includes a distillation column, a condenser tube at the top of the distillation column, a heat recovery preheating tube on the outer surface of the condenser tube, and the outer side of the outer surface of the heat recovery preheating tube being embedded in the outer surface of the distillation column. The heat recovery preheating tube includes a heat exchange tube embedded in the outer surface of the distillation column, the heat exchange tube being wrapped around the outer surface of the condenser tube, and a spiral feed pipe fixedly connected inside the heat exchange tube. The feed pipe spirally distributes itself on the outer surface of the condenser tube, the outlet of the feed pipe extends into the interior of the distillation column, and the inlet of the feed pipe extends to the outer side of the heat exchange tube. Two partition plates are fixedly connected inside the heat exchange tube, dividing the interior of the heat exchange tube into three chambers. The three chambers of the heat exchange tube are filled with a heat-conducting medium, the boiling point of which increases sequentially from top to bottom.

[0007] The beneficial effects of this utility model are as follows: By using a stepped heat transfer medium, the residual heat from the condenser and the heat dissipation from the distillation column can be utilized to preheat the raw material to near the boiling point, significantly reducing the heating load of the distillation column and reducing heating energy consumption. The spiral feed pipe increases the contact area with the heat transfer medium, and in conjunction with the heat transfer medium with a gradient boiling point, it can selectively absorb heat from different temperature zones, improving energy utilization. Furthermore, through the built-in mechanical adaptive structure of the condenser, it automatically adjusts the layered interception and impurity discharge according to the steam pressure, without the need for manual intervention, thus improving the batch consistency of purity processing.

[0008] Furthermore, the condenser includes a cooling pipe fixedly connected to the top of the distillation column. A spring damper is fixedly connected to the top of the inner part of the cooling pipe, and a steam stratification gate is fixedly connected to the bottom of the spring damper. The steam stratification gate is slidably connected to the inner side of the cooling pipe, and a miscellaneous gas discharge pipe is fixedly connected to the top of the steam stratification gate. The top of the miscellaneous gas discharge pipe extends to the outer side of the top of the cooling pipe. The steam stratification gate can block the steam, causing it to accumulate and stratify. Then, the channel is opened and closed according to the steam pressure to separate the low-boiling-point impurity steam from the DMF steam.

[0009] Furthermore, the steam stratification gate includes a frame base fixedly connected to the bottom end of the spring damper, and an opening and closing spring is fixedly connected to the middle of the bottom end of the frame base. The opening and closing spring adaptively adjusts the position of the moving gate body according to the air pressure.

[0010] Furthermore, two support columns are fixedly connected to the bottom outer side of the frame base, and a movable gate body is slidably connected to the bottom end of the opening and closing spring and is controlled by the movement control channel.

[0011] Furthermore, the bottom of the movable gate is a slope, and a valve column is fixedly connected to the lowest point of the bottom of the movable gate. The bottom ends of the two support columns are fixedly connected to a layered guide plate. Both the upper and lower ends of the layered guide plate are slopes parallel to the bottom of the movable gate. The slope design of the layered guide plate will guide the mixed gas accumulated below to be layered. Due to its lower density, the impurity gas will be in the upper layer, and the DMF gas will be in the lower layer.

[0012] Furthermore, the layered guide plate has a flow guide hole that can enter the valve column through the bottom of the valve column. The top of the layered guide plate is fixedly connected to the bottom of the impurity gas discharge pipe. After the DMF gas below is exposed in the flow guide hole, it enters the cooling pipe to continue to condense. At the same time, the impurity gas discharge pipe is opened to discharge the impurity gas above.

[0013] Furthermore, the miscellaneous gas exhaust pipe includes an exhaust pipe fixedly connected to the top of the layered guide plate. The top of the exhaust pipe extends to the outside of the top of the cooling pipe. A ball valve is rotatably connected inside the exhaust pipe. The ball valve is located between the movable gate and the layered guide plate. The ball valve can control the opening and closing state of the miscellaneous gas exhaust pipe.

[0014] Furthermore, the ball valve extends to the outside of the exhaust pipe on both sides and is fixedly connected with opening and closing gears. The outer side of the opening and closing gears is meshed with a synchronous rack. The top of the synchronous rack is fixedly connected to the bottom of the moving gate body. The synchronous rack will drive the opening and closing gears to rotate as the moving gate body moves synchronously. Attached Figure Description

[0015] Figure 1 This is a structural diagram of the present invention; Figure 2 This is a cross-sectional view of the heat recovery preheating pipe of this utility model; Figure 3 This is a cross-sectional view of the condenser tube of this utility model; Figure 4 This is a cross-sectional view of the steam stratification gate assembly of this utility model; Figure 5 This is an exploded view of the steam stratification gate of this utility model; Figure 6 This is a cross-sectional view of the mixed gas pipe structure of this utility model.

[0016] The attached diagram lists the components represented by each number as follows: 1. Condenser; 11. Spring damper; 12. Miscellaneous gas drain pipe; 121. Exhaust pipe; 122. Ball valve; 123. Opening and closing gear; 124. Synchronizing rack; 13. Steam stratification gate; 131. Frame base; 132. Opening and closing spring; 133. Moving gate body; 134. Support column; 135. Stratification guide plate; 136. Valve column; 137. Flow guide hole; 14. Cooling pipe; 2. Heat recovery preheating pipe; 21. Feed pipe; 22. Heat exchange pipe; 23. Divider plate; 3. Distillation column. Detailed Implementation

[0017] The technical solutions of the embodiments of this application will be clearly and completely described below with reference to the accompanying drawings. Obviously, the described embodiments are only some embodiments of this application, and not all embodiments. Based on the embodiments of this application, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of this application.

[0018] In the description of this application, the terms "first" and "second" are used for descriptive purposes only and should not be construed as indicating or implying relative importance or implicitly specifying the number of indicated technical features. Thus, a feature defined as "first" or "second" may explicitly or implicitly include one or more of the stated features. In the description of this application, "multiple" means two or more, unless otherwise explicitly specified.

[0019] In the description of this application, it should also be noted that, unless otherwise expressly specified and limited, the terms "set up," "install," "connect," and "link" should be interpreted broadly. For example, they can refer to a fixed connection, a detachable connection, or an integral connection; they can refer to a mechanical connection or an electrical connection; they can refer to a direct connection or an indirect connection through an intermediate medium; and they can refer to the internal connection of two components. Those skilled in the art can understand the specific meaning of the above terms in this technology based on the specific circumstances.

[0020] In the description of this application, spatial relation terms such as “below,” “under,” “below,” “below,” “above,” “over,” etc., are used herein to describe the relationship between an element or feature shown in the figures and other elements or features. It should be understood that, in addition to the orientation shown in the figures, spatial relation terms also include different orientations of the device in use and operation. For example, if the device in the figures is flipped, an element or feature described as “below,” “under,” or “below” will be oriented “over” the other element or feature. Therefore, the exemplary terms “below” and “under” can include both upper and lower orientations. Furthermore, the device may also include other orientations (e.g., rotated 90 degrees or other orientations), and the spatial descriptive terms used herein are interpreted accordingly.

[0021] In the description of this application, the term "for example" is used to mean "used as an example, illustration, or description." Any embodiment described as "for example" in this application is not necessarily to be construed as being more preferred or advantageous than other embodiments. The following description is provided to enable any person skilled in the art to implement and use the present invention. Details are set forth in the following description for purposes of explanation. It should be understood that those skilled in the art will recognize that the present invention can be implemented without using these specific details. In other instances, well-known structures and processes will not be described in detail to avoid obscuring the description of the present invention with unnecessary detail. Therefore, the present invention is not intended to be limited to the embodiments shown, but is consistent with the broadest scope of the principles and features disclosed in this application.

[0022] Example 1 Figure 1 This is a structural diagram of a purification apparatus provided for an embodiment of the present utility model. Figure 1 The device includes a distillation column 3, a condenser 1 is provided at the top of the distillation column 3, and a heat recovery preheating pipe 2 is provided on the outer surface of the condenser 1. The outer side of the outer surface of the heat recovery preheating pipe 2 is embedded in the outer side of the outer surface of the distillation column 3.

[0023] With distillation column 3 as the core purification unit, the raw material first enters the heat recovery preheating pipe 2. The condenser pipe 1 is used to process the steam purified by distillation column 3, while the heat recovery preheating pipe 2 can simultaneously contact the heat of condenser pipe 1 and distillation column 3. During operation, distillation column 3 heats and distills the internal material, and the generated DMF vapor rises to the top condenser pipe 1, which condenses the vapor. At the same time, the heat recovery preheating pipe 2 can initially absorb the heat emitted by condenser pipe 1 and distillation column 3, preparing for the subsequent preheating of raw materials.

[0024] Distillation column 3 vaporizes the raw material into steam by heating, which is existing technology and will not be described in detail here.

[0025] Figure 2 This is a cross-sectional view of the heat recovery preheating pipe of this utility model. Figure 2 As shown, the heat recovery preheating pipe 2 includes a heat exchange pipe 22 embedded in the outer surface of the distillation column 3. The heat exchange pipe 22 is wrapped around the outer surface of the condenser pipe 1. A spiral feed pipe 21 is fixedly connected inside the heat exchange pipe 22. The feed pipe 21 is spirally distributed on the outer surface of the condenser pipe 1. The outlet of the feed pipe 21 extends into the interior of the distillation column 3, and the inlet of the feed pipe 21 extends to the outside of the heat exchange pipe 22. Two partition plates 23 are fixedly connected inside the heat exchange pipe 22. The two partition plates 23 divide the interior of the heat exchange pipe 22 into three chambers. The three chambers of the heat exchange pipe 22 are filled with a heat-conducting medium, and the boiling point of the heat-conducting medium increases sequentially from top to bottom.

[0026] The crude DMF raw material enters through the inlet of the feed pipe 21. Since the feed pipe 21 is spirally distributed and wrapped around the outer surface of the condenser 1, it can fully contact the heat transfer medium in the heat exchange tube 22. Furthermore, the heat exchange tube 22 is divided into three chambers by two partition plates 23, and the boiling point of the heat transfer medium in the three chambers increases sequentially from top to bottom. When the condenser 1 releases residual heat and the distillation column 3 releases heat, the heat is transferred to the heat transfer medium in different chambers of the heat exchange tube 22. The heat transfer medium with a boiling point gradient distribution can selectively absorb heat from different temperature zones and transfer the heat to the raw material in the spiral feed pipe 21, thereby achieving gradient preheating of the raw material. The preheated raw material directly enters the interior of the distillation column 3 through the outlet of the feed pipe 21, reducing the subsequent heating load of the distillation column 3.

[0027] Example 2 Based on Embodiment 1, the present invention can be further improved as follows: Figure 3 This is a cross-sectional view of the condenser tube of this utility model. Figure 3 As shown, the condenser 1 includes a cooling pipe 14 fixedly connected to the top of the distillation column 3. A spring damper 11 is fixedly connected to the top of the inner part of the cooling pipe 14. A steam stratification gate 13 is fixedly connected to the bottom of the spring damper 11. The steam stratification gate 13 is slidably connected to the inner side of the cooling pipe 14. A miscellaneous gas discharge pipe 12 is fixedly connected to the top of the steam stratification gate 13. The top of the miscellaneous gas discharge pipe 12 extends to the outer side of the top of the cooling pipe 14.

[0028] The mixed steam generated by heating and distillation in the distillation column 3 rises into the cooling pipe 14 of the condenser 1. The spring damper 11 provides elastic support and buffer adjustment for the steam stratification gate 13 at the bottom, so that the steam stratification gate 13 can be stably slidably connected to the inside of the cooling pipe 14. When the mixed steam flows through the steam stratification gate 13, the steam stratification gate 13 can first block the mixed steam, causing the mixed gas to stratify. When the gas pressure of the mixed gas reaches the threshold of the steam stratification gate 13, the low boiling point impurity steam at the top enters the impurity gas discharge pipe 12 and is finally discharged through the impurity gas discharge pipe 12, while the DMF steam at the bottom continues to condense in the cooling pipe 14 after passing through the steam stratification gate 13.

[0029] Figure 4 This is a cross-sectional view of the steam stratification gate assembly of this utility model. Figure 5 This is an exploded view of the steam stratification gate of this utility model. Figure 4 and Figure 5As shown, the steam stratification gate 13 includes a frame base 131 fixedly connected to the bottom end of the spring damper 11. An opening and closing spring 132 is fixedly connected to the middle of the bottom end of the frame base 131. Two support columns 134 are fixedly connected to the outer side of the bottom end of the frame base 131. A movable gate body 133 is slidably connected to the outer surface of the support column 134 and fixedly connected to the bottom end of the opening and closing spring 132. The bottom end of the movable gate body 133 is an inclined surface. A valve column 136 is fixedly connected to the lowest point of the bottom end of the movable gate body 133. A stratification guide plate 135 is fixedly connected to the bottom end of the two support columns 134. Both the upper and lower ends of the stratification guide plate 135 are inclined surfaces parallel to the bottom end of the movable gate body 133. A guide hole 137 is opened through the stratification guide plate 135 below the valve column 136, allowing the valve column 136 to enter. The top end of the stratification guide plate 135 is fixedly connected to the bottom end of the miscellaneous gas discharge pipe 12.

[0030] After the mixed steam enters the steam stratification gate 13 area, the frame seat 131 serves as the basic support structure. The inclined design of the stratification guide plate 135 guides the mixed gas accumulated below to stratify. Due to its lower density, the impurity gas will be in the upper layer, and the DMF gas will be in the lower layer.

[0031] Two support columns 134 provide a sliding track for the movable gate body 133. When the pressure of the mixed steam reaches the threshold of the deformation of the opening and closing spring 132, the mixed steam pushes the valve column 136, thereby causing the movable gate body 133 to slide up and down along the support columns 134. After the DMF gas is exposed to the guide hole 137, it continues to condense in the cooling pipe 14. At the same time, the impurity gas discharge pipe 12 is opened to discharge impurity gas. The opening and closing spring 132 elastically expands and contracts according to the sliding amplitude of the movable gate body 133, realizing adaptive adjustment of the position of the movable gate body 133 according to the gas pressure. When the pressure of the mixed gas suddenly increases significantly, the opening and closing spring 132 reaches the compression limit and will continue to push the frame seat 131 to cause the entire layered guide plate 135 to urgently discharge the mixed gas and prevent internal failure.

[0032] Figure 6 This is a cross-sectional view of the mixed gas pipe structure of this utility model. (See image below.) Figure 6 As shown, the miscellaneous gas exhaust pipe 12 includes an exhaust pipe 121 fixedly connected to the top of the layered guide plate 135. The top of the exhaust pipe 121 extends to the outer side of the top of the cooling pipe 14. A ball valve 122 is rotatably connected inside the exhaust pipe 121. The ball valve 122 is located between the movable gate body 133 and the layered guide plate 135. Both sides of the ball valve 122 extend to the outer side of the exhaust pipe 121 and are fixedly connected to the opening and closing gear 123. A synchronous rack 124 is meshed on the outer side of the opening and closing gear 123. The top of the synchronous rack 124 is fixedly connected to the bottom of the movable gate body 133.

[0033] When the movable gate body 133 slides along the support column 134, the synchronous rack 124 fixed at its bottom end will move synchronously with the movable gate body 133. The movement of the synchronous rack 124 will drive the opening and closing gear 123 to rotate, which in turn drives the ball valve 122 to rotate in the exhaust pipe 121. The rotation of the ball valve 122 can control the opening and closing degree of the exhaust pipe 121. When it is necessary to discharge impurity steam, the ball valve 122 rotates to the open state, and the impurity steam is discharged along the top outlet of the exhaust pipe 121, realizing the synchronous opening of the exhaust pipe 121 and the guide hole 137.

[0034] Ball valve 122 is existing technology and will not be explained here.

[0035] While embodiments or examples of this disclosure have been described with reference to the accompanying drawings, it should be understood that the above embodiments are merely exemplary embodiments or examples, and the scope of this utility model is not limited by these embodiments or examples, but only by the granted claims and their equivalents. Various elements in the embodiments or examples may be omitted or replaced by their equivalents. Furthermore, the steps may be performed in a different order than that described in this disclosure. Further, various elements in the embodiments or examples may be combined in various ways. Importantly, as the technology evolves, many elements described herein can be replaced by equivalents that appear after this disclosure.

Claims

1. A purification apparatus, characterized in that, include: A distillation column (3) is provided with a condenser (1) at the top of the distillation column (3), and a heat recovery preheating pipe (2) is provided on the outer surface of the condenser (1). The outer side of the outer surface of the heat recovery preheating pipe (2) is embedded in the outer side of the outer surface of the distillation column (3). The heat recovery preheating tube (2) includes a heat exchange tube (22) embedded in the outer surface of the distillation tower (3). The heat exchange tube (22) is wrapped around the outer surface of the condenser tube (1). A spiral feed tube (21) is fixedly connected inside the heat exchange tube (22). The feed tube (21) is spirally distributed on the outer surface of the condenser tube (1). The outlet of the feed tube (21) extends into the interior of the distillation tower (3). The inlet of the feed tube (21) extends into the outside of the heat exchange tube (22). Two partition plates (23) are fixedly connected inside the heat exchange tube (22). The two partition plates (23) divide the interior of the heat exchange tube (22) into three chambers. The three chambers of the heat exchange tube (22) are filled with a heat-conducting medium. The boiling point of the heat-conducting medium increases from top to bottom.

2. The purification apparatus according to claim 1, characterized in that, The condenser (1) includes a cooling pipe (14) fixedly connected to the top of the distillation column (3). A spring damper (11) is fixedly connected to the top of the inner part of the cooling pipe (14). A steam stratification gate (13) is fixedly connected to the bottom of the spring damper (11). The steam stratification gate (13) is slidably connected to the inner side of the cooling pipe (14). A miscellaneous gas discharge pipe (12) is fixedly connected to the top of the steam stratification gate (13). The top of the miscellaneous gas discharge pipe (12) extends to the outer side of the top of the cooling pipe (14).

3. The purification apparatus according to claim 2, characterized in that, The steam stratification gate (13) includes a frame seat (131) fixedly connected to the bottom end of the spring damper (11), and an opening and closing spring (132) is fixedly connected to the middle of the bottom end of the frame seat (131).

4. The purification apparatus according to claim 3, characterized in that, Two support columns (134) are fixedly connected to the bottom outer side of the frame base (131), and a movable gate body (133) that is slidably connected to the bottom of the opening and closing spring (132) is fixedly connected to the bottom of the support column (134).

5. The purification apparatus according to claim 4, characterized in that, The bottom end of the movable gate (133) is an inclined surface. A valve column (136) is fixedly connected to the lowest point of the bottom end of the movable gate (133). The bottom ends of the two support columns (134) are fixedly connected to a layered guide plate (135). The upper and lower ends of the layered guide plate (135) are both inclined surfaces parallel to the bottom end of the movable gate (133).

6. The purification apparatus according to claim 5, characterized in that, The layered guide plate (135) has a flow guide hole (137) that can enter the valve column (136) through the bottom of the valve column (136), and the top of the layered guide plate (135) is fixedly connected to the bottom of the miscellaneous gas pipe (12).

7. The purification apparatus according to claim 5, characterized in that, The miscellaneous gas exhaust pipe (12) includes an exhaust pipe (121) fixedly connected to the top of the layered guide plate (135). The top of the exhaust pipe (121) extends to the outside of the top of the cooling pipe (14). A ball valve (122) is rotatably connected inside the exhaust pipe (121). The ball valve (122) is located between the movable gate body (133) and the layered guide plate (135).

8. The purification apparatus according to claim 7, characterized in that, The ball valve (122) extends to the outside of the exhaust pipe (121) on both sides and is fixedly connected to the opening and closing gear (123). The opening and closing gear (123) is meshed with the outside of the synchronous rack (124), and the top of the synchronous rack (124) is fixedly connected to the bottom of the movable gate body (133).

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