A membrane separation experimental device

Abstract

The utility model discloses a kind of membrane separation experimental devices, including raw material supply assembly, heating assembly, first separation assembly, second separation assembly, reflux cooling assembly, and vacuum assembly, raw material supply assembly includes raw material tank and extraction piece, raw material tank is connected with extraction piece;Heating assembly is connected with extraction piece, heating assembly is used to heat raw material;First separation assembly is connected with heating assembly, first separation assembly is used to separate mixed solution;Second separation assembly is used to separate mixed solution before the working of first separation assembly, to determine optimal experimental parameter;Reflux cooling assembly is connected with raw material tank and first separation assembly respectively, and reflux cooling assembly is used to cool and reflux to raw material tank after the separation of residual liquid;Vacuum assembly is connected with first separation assembly and second separation assembly respectively.The utility model can realize the continuous penetration evaporation separation of mixed solution.

Description

Technical Field

[0001] This utility model relates to the field of chemical experimental equipment technology, and in particular to a membrane separation experimental device. Background Technology

[0002] Pervaporation is a molecular separation membrane technology that combines membrane permeation and evaporation. It utilizes the different diffusion efficiencies of the components in a mixture within a membrane module to allow components with high affinity to the separation membrane to pass preferentially through the membrane module. It is often used for the separation and purification of mixed systems with similar boiling points that are prone to forming azeotropes, such as the separation of isomers and the separation of organic solvents / water. Pervaporation membrane separation is considered a suitable alternative.

[0003] However, most pervaporation membrane separation devices currently used in laboratories operate intermittently, failing to achieve continuous separation. This results in low efficiency in raw material and energy utilization, and significant energy consumption during the product condensation stage. Furthermore, existing membrane separation experimental devices place the mixture in a raw material bottle and position the pervaporation membrane above it. Separation is achieved by heating the raw material bottle to vaporize the mixture, which then contacts the membrane surface. However, this type of membrane separation experimental device generally allows for the passage of media or fluids at relatively low operating temperatures, making it difficult to meet the practical requirements for separating high-temperature media or fluids under high-temperature conditions. In actual use, if this device is required to separate high-temperature media or fluids, the pervaporation membrane is highly prone to leakage, leading to the failure of the entire separation experiment. Utility Model Content

[0004] This invention aims to solve at least one of the aforementioned technical problems in the prior art. Therefore, the purpose of this invention is to provide a membrane separation experimental device capable of continuous permeation-evaporation separation of a mixed liquid, avoiding the problem of sealing failure or leakage of the first separation component due to high-temperature media or fluids, ensuring the stability and efficiency of the separation process of the first separation component, and reducing energy waste and operational errors caused by unreasonable experimental parameters.

[0005] The membrane separation experimental apparatus according to a first aspect embodiment of the present invention includes: A raw material supply assembly, comprising a raw material tank and an extraction component, wherein the raw material tank is connected to the extraction component; A heating assembly, connected to the extraction component, is used to heat the raw material; A first separation component is connected to the heating component and is used to separate the mixture. A reflux cooling assembly is connected to the raw material tank and the first separation assembly, respectively. The reflux cooling assembly is used to cool the residual liquid after separation and reflux it back to the raw material tank. A second separation component is used to separate the mixture before the first separation component operates, in order to determine optimal experimental parameters; A vacuum assembly, which is connected to both the first separation assembly and the second separation assembly.

[0006] The membrane separation experimental apparatus according to the embodiments of this utility model has at least the following beneficial effects: The mixture in the raw material tank is extracted to the first separation component for separation via the extraction element, enabling continuous pervaporation separation of the mixture. Simultaneously, the first separation component allows for a working temperature of up to 200°C through the medium or fluid, making it suitable for the separation and purification of most azeotropic mixture systems, avoiding sealing failure or leakage of the first separation component due to high-temperature medium or fluid. Furthermore, the second separation component separates the mixture before the first separation component operates, which helps to explore suitable separation conditions for the continuous pervaporation separation of the first separation component, thereby determining the optimal experimental parameters, ensuring the stability and efficiency of the separation process of the first separation component, and reducing energy waste and operational errors caused by unreasonable experimental parameters. In addition, the reflux cooling component is connected to both the raw material tank and the first separation component, cooling the residual liquid after separation and returning it to the raw material tank, which helps to improve the utilization rate of the raw material and achieve continuous pervaporation separation.

[0007] According to some embodiments of the present invention, the membrane separation experimental apparatus further includes a product collection component. The first separation component includes a first housing, which is provided with a first air inlet, a first air outlet, and a second air outlet. The first air inlet and the first air outlet are disposed opposite each other on the lower side of the first housing along a first direction, and the second air outlet is disposed on the upper side of the first housing along a second direction. The first direction and the second direction are perpendicular to each other. The first air inlet is connected to the heating component, the first air outlet is connected to the reflux cooling component, and the second air outlet is connected to the product collection component.

[0008] According to some embodiments of the present invention, the first outer shell includes a first housing, a second housing, and a third housing connected sequentially along the second direction. The first air inlet and the first air outlet are disposed on opposite sides of the first housing. The second housing is provided with a first mounting groove, and a first membrane element is disposed in the first mounting groove. The first membrane element is used to separate the mixture. The second air outlet is disposed on the third housing.

[0009] According to some embodiments of the present invention, the first membrane component includes a first separation membrane, a first gasket, and a first connector. The first separation membrane is in contact with the bottom surface of the first mounting groove. The first gasket is disposed on the top of the first separation membrane. The first connector is disposed on the top of the first gasket. The first connector is connected to the second housing to limit the position of the first separation membrane.

[0010] According to some embodiments of the present invention, the membrane separation experimental device further includes a product collection component. The second separation component includes a raw material bottle, a second outer shell, and a second membrane element. The raw material bottle is disposed at the bottom of the second outer shell, the second outer shell is provided with a second mounting groove, and the second membrane element is disposed in the second mounting groove. The second outer casing is provided with a second air inlet and a third air outlet arranged opposite to each other along a second direction. Both the second air inlet and the third air outlet are connected to the second mounting groove. The second air inlet is connected to the raw material bottle, and the third air outlet is connected to the product collection assembly.

[0011] According to some embodiments of the present invention, the second outer shell includes a fourth shell and a fifth shell, the fourth shell and the fifth shell are covered and disposed together, the second mounting groove and the second air inlet are both disposed in the fourth shell, and the third air outlet is disposed in the fifth shell.

[0012] According to some embodiments of the present invention, the second membrane component includes a second separation membrane, a second gasket, and a second connector. The second separation membrane is in contact with the bottom surface of the second mounting groove. The second gasket is disposed on the top of the second separation membrane. The second connector is disposed on the top of the second gasket. The second connector is connected to the fourth housing to limit the position of the second separation membrane.

[0013] According to some embodiments of the present invention, the heating assembly includes a heating tube and a protective component. The protective component is disposed on the outside of the heating tube and includes a first protective part and a second protective part, wherein the first protective part and the second protective part are detachably connected.

[0014] According to some embodiments of the present invention, the raw material tank includes a tank body and a cover body, the tank body and the cover body are closed together, the tank body is provided with a receiving cavity, the mixed liquid is disposed in the receiving cavity, and the tank body is connected to the heating component; The cover is provided with a feed inlet, a nitrogen inlet, a temperature test piece, and a pressure test piece. The feed inlet and the nitrogen inlet are both connected to the accommodating cavity. The test ends of the temperature test piece and the pressure test piece are both located inside the accommodating cavity.

[0015] According to some embodiments of the present invention, the membrane separation experimental device further includes a control component, which is connected to the raw material tank, the heating component, the first separation component, and the second separation component.

[0016] Additional aspects and advantages of this invention will be set forth in part in the description which follows, and in part will be obvious from the description, or may be learned by practice of the invention. Attached Figure Description

[0017] The present invention will be further described below with reference to the accompanying drawings and embodiments, wherein: Figure 1 This is a schematic diagram of the membrane separation experimental device according to an embodiment of the present invention; Figure 2 for Figure 1 The diagram shows the structure of the raw material tank in the membrane separation experimental apparatus. Figure 3 for Figure 1 A cross-sectional view of the first separation component of the membrane separation experimental apparatus shown. Figure 4 for Figure 1 A split view of the first separation component of the membrane separation experimental apparatus shown. Figure 5 for Figure 4 The diagram shows the structure of the second housing of the first separation component. Figure 6 for Figure 1 A cross-sectional view of the second separation component of the membrane separation experimental apparatus shown. Figure 7 for Figure 1 A split view of the second separation component of the membrane separation experimental apparatus shown; Figure 8 for Figure 7 The diagram shows the structure of the fourth housing of the second separation component; Figure 9 for Figure 1 The diagram shows the structure of the heating component of the membrane separation experimental apparatus.

[0018] Reference numerals: 100, Raw material supply assembly; 110, Raw material tank; 111, Tank body; 1111, Tank rim; 1112, First connecting hole; 1113, Receiving cavity; 112, Cover; 1121, Second connecting hole; 1122, Feed inlet; 1123, Nitrogen inlet; 113, Temperature testing piece; 114, Pressure testing piece; 115, Thermostatic bath; 120, Extraction piece; 200. Heating assembly; 210. Heating element; 220. Protective component; 300, First separation component; 310, First outer shell; 311, First air inlet; 312, First air outlet; 313, Second air outlet; 314, First housing; 3141, First chamber; 315, Second housing; 3151, First mounting groove; 3152, First opening; 3153, First sealing groove; 3154, Second sealing groove; 316, Third housing; 3161, Second chamber; 320, First membrane element; 321, First separation membrane; 322, First gasket; 323, First connector; 330, First sealing ring; 340, Second sealing ring; 350, Pipe insulation heating jacket; 400. Second separation component; 410. Second housing; 411. Fourth housing; 4111. Second mounting groove; 4112. Second air inlet; 4113. Second opening; 4114. Third sealing groove; 4115. Fourth sealing groove; 412. Fifth housing; 4121. Third air outlet; 420. Second membrane element; 421. Second separation membrane; 422. Second gasket; 423. Second connector; 430. Third sealing ring; 440. Fourth sealing ring; 450. Oil bath; 500. Vacuum assembly; 510. Vacuum pump; 520. Buffer tank; 530. Dryer; 600. Reflow cooling assembly; 700. Product collection assembly; 710. Cooling component; 720. Receiving tank; 730. Refrigeration circulation pump; 740. Serpentine cold trap; 750. Liquid nitrogen cup. Detailed Implementation

[0019] The embodiments of this utility model are described in detail below. Examples of these embodiments are shown in the accompanying drawings, wherein the same or similar reference numerals denote the same or similar elements or elements having the same or similar functions throughout. The embodiments described below with reference to the accompanying drawings are exemplary and are only used to explain this utility model, and should not be construed as limiting this utility model.

[0020] In the description of this utility model, it should be understood that the directional descriptions, such as up, down, front, back, left, right, etc., indicate the directional or positional relationship based on the directional 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.

[0021] In the description of this utility model, "several" means one or more, "multiple" means two or more, "greater than," "less than," and "exceeding" are understood to exclude the stated number, while "above," "below," and "within" are understood to include the stated number. The use of "first" and "second" in the description is merely for distinguishing technical features and should not be construed as indicating or implying relative importance, or implicitly indicating the number of indicated technical features, or implicitly indicating the order of the indicated technical features.

[0022] In the description of this utility model, unless otherwise explicitly defined, terms such as "setting," "installation," and "connection" should be interpreted broadly, and those skilled in the art can reasonably determine the specific meaning of the above terms in this utility model in conjunction with the specific content of the technical solution.

[0023] In the description of this utility model, the terms "one embodiment," "some embodiments," "illustrative embodiment," "example," "specific example," or "some examples," etc., refer to specific features, structures, materials, or characteristics described in connection with that embodiment or example, which are included in at least one embodiment or example of this utility model. In this specification, the illustrative expressions of the above terms do not necessarily refer to the same embodiment or example. Furthermore, the specific features, structures, materials, or characteristics described may be combined in any suitable manner in one or more embodiments or examples.

[0024] Reference Figure 1 This utility model provides a membrane separation experimental device, including a raw material supply component 100, a heating component 200, a first separation component 300, a second separation component 400, and a vacuum component 500. The raw material supply component 100 includes a raw material tank 110 and an extraction component 120, with the raw material tank 110 connected to the extraction component 120. The heating component 200 is connected to the extraction component 120 and is used to heat the raw material. The first separation component 300 is connected to the heating component 200 and is used to separate the mixture. The second separation component 400 is used to separate the mixture before the first separation component 300 operates to determine the optimal experimental parameters. The vacuum component 500 is connected to both the first separation component 300 and the second separation component 400.

[0025] The mixture in the raw material tank 110 is extracted by the extraction component 120 and transferred to the first separation component 300 for separation, enabling continuous pervaporation separation of the mixture. Simultaneously, since the mixture enters the first separation component 300 after being heated and vaporized by the heating component 200, the first separation component 300 can operate at a temperature of up to 200°C, making it suitable for the separation and purification of most azeotropic mixtures. This avoids the problem of sealing failure or leakage of the first separation component 300 due to high-temperature media or fluids. Furthermore, the second separation component 400 separates the mixture before the first separation component 300 operates, which helps to explore suitable separation conditions for the continuous pervaporation separation of the first separation component 300, thereby determining the optimal experimental parameters, ensuring the stability and efficiency of the separation process of the first separation component 300, and reducing the risk of energy waste and operational errors caused by unreasonable experimental parameters.

[0026] Reference Figure 1 , Figure 2 In some embodiments, the raw material tank 110 includes a tank body 111 and a cover 112. The tank body 111 and the cover 112 are fitted together. The top of the tank body 111 is provided with a tank rim 1111, and the tank rim 1111 is provided with a plurality of first connecting holes 1112. The cover 112 is provided with a plurality of second connecting holes 1121 corresponding to the first connecting holes 1112. The connector passes through the second connecting holes 1121 and cooperates with the corresponding first connecting holes 1112, so that the cover 112 is evenly stressed and tightly pressed against the top of the tank body 111, preventing the liquid to be separated in the tank body 111 from leaking from the connection between the cover 112 and the tank body 111. At the same time, it can also prevent external air, dust and other impurities from entering the tank and contaminating the raw materials, thus ensuring the purity of the raw materials.

[0027] Reference Figure 1 , Figure 2 In some embodiments, the tank 111 is provided with a receiving cavity 1113, the mixed liquid is disposed in the receiving cavity 1113, and the tank 111 is connected to the heating component 200; the cover 112 is provided with a feed inlet 1122, a nitrogen inlet 1123, a temperature test element 113 and a pressure test element 114, the feed inlet 1122 and the nitrogen inlet 1123 are both connected to the receiving cavity 1113, and the test end of the temperature test element 113 and the test end of the pressure test element 114 are both disposed in the receiving cavity 1113. Specifically, the mixture enters the containment chamber 1113 through the feed inlet 1122, and nitrogen enters the containment chamber 1113 through the nitrogen inlet 1123. Nitrogen serves as the carrier used in the experiment, propelling the gas phase components to the product collection assembly 700. The temperature test piece 113 can be set as a temperature control sensor to monitor the temperature in the middle of the raw material tank 110, and the pressure test piece 114 can be set as a pressure gauge to read the gas pressure in the raw material tank 110 in real time.

[0028] Reference Figure 1 , Figure 2 In some embodiments, the raw material tank 110 is connected to the constant temperature bath 115, which can stabilize the temperature of the mixture and ensure the stability of the properties of the added and returned mixtures. This prevents the difference in the properties of the mixture from affecting the subsequent heating and vaporization efficiency and the separation effect of the first separation component 300, thus avoiding affecting the final experimental results. In addition, the outlet of the raw material tank 110 and the extraction component 120 are equipped with matching flanges, which are connected to the inlet of the extraction component 120 through a stainless steel gas pipe. This prevents the mixture from leaking from the connection point during transportation. At the same time, the stainless steel gas pipe is high temperature resistant and corrosion resistant, which can adapt to the transportation requirements of high temperature mixtures and prevent the gas pipe from deforming or being damaged due to excessive material temperature or chemical properties. This ensures that the transportation process of the mixture from the raw material tank 110 to the extraction component 120 is sealed and smooth. In addition, a level gauge is installed on the side of the raw material tank 110 to monitor the liquid level of the raw material tank 110 in real time, so that the staff can keep track of the remaining raw material. When the liquid level is too low, the mixture can be replenished in time through the feed inlet 1122 to avoid the extraction component 120 from being empty or the separation process being interrupted due to insufficient mixture, thus ensuring the stability of the continuous separation of the device.

[0029] In some embodiments, the extraction component 120 is configured as a circulation pump, which provides stable and controllable power for the delivery of the mixture in the raw material tank 110, ensuring that the mixture is delivered from the raw material tank 110 to the heating component 200 at a uniform and stable flow rate. Of course, in actual design, the structure of the extraction component 120 can be designed according to actual needs.

[0030] Reference Figure 1 , Figure 3 In some embodiments, the membrane separation experimental apparatus further includes a product collection component 700. The first separation component 300 includes a first housing 310, which is provided with a first air inlet 311, a first air outlet 312, and a second air outlet 313. The first air inlet 311 and the first air outlet 312 are disposed opposite each other on the lower side of the first housing 310 along a first direction, and the second air outlet 313 is disposed on the upper side of the first housing 310 along a second direction. The first direction and the second direction are perpendicular to each other. The first air inlet 311 is connected to the heating component 200, and the vaporized steam after being heated by the heating component 200 enters the first separation component 300 for separation, which is beneficial to improving the utilization rate of raw materials and realizing continuous pervaporation separation. The first air outlet 312 is connected to the reflux cooling component 600, which cools the separated residual liquid and returns it to the raw material tank 110. The second air outlet 313 is connected to the product collection component 700, which is used to collect pervaporation products.

[0031] Reference Figure 3It should be noted that the first direction is the X direction, and the second direction is the Z direction.

[0032] Reference Figure 3 , Figure 4 In some embodiments, the first housing 310 includes a first housing 314, a second housing 315, and a third housing 316 connected sequentially along a second direction. A first air inlet 311 and a first air outlet 312 are located on opposite sides of the first housing 314, ensuring that the steam heated by the heating assembly 200 forms a gas channel within the first housing 314. Furthermore, the second housing 315 is provided with a first mounting groove 3151, within which a first membrane element 320 is disposed. The first membrane element 320 is used to separate the mixture. A second air outlet 313 is located on the third housing 316, and the second air outlet 313 guides the pervaporation products separated by the first membrane element 320 to the product collection assembly 700, preventing the pervaporation products from remaining in the first housing 310 and ensuring the purity of the pervaporation products.

[0033] In some embodiments, the first housing 314 is provided with a first thread, and the second housing 315 is provided with a second thread. The first thread mates with the second thread to connect the first housing 314 and the second housing 315. The second housing 315 is provided with a third thread, and the third housing 316 is provided with a fourth thread. The third thread mates with the fourth thread to connect the second housing 315 and the third housing 316. During the assembly or maintenance of the experimental device, disassembly and assembly can be quickly achieved by screwing on the first housing 314, the second housing 315, and the third housing 316. This facilitates the replacement, cleaning, or repair of the first membrane element 320, reducing the operational difficulty and time cost of device maintenance, and solving the problem of difficulty in replacing internal membrane elements in integrated housings. In addition, the threaded engagement can form a tight sealing structure. Even in high-temperature environments, the sealing performance of the threaded connection can prevent high-temperature steam or pervaporation products from leaking from the housing connection gaps, avoiding experimental failure or material waste due to leakage.

[0034] Reference Figure 3 , Figure 4In some embodiments, the first housing 314 is provided with a first chamber 3141, and the third housing 316 is provided with a second chamber 3161. The first chamber 3141, the second chamber 3161, and the first mounting groove 3151 are interconnected. This allows steam heated by the heating assembly 200 to enter the first chamber 3141 of the first housing 314 through the first air inlet 311 and then flow through the connecting path to the first membrane element 320 in the first mounting groove 3151 of the second housing 315. This ensures sufficient contact between the steam and the first membrane element 320, avoiding problems such as steam stagnation and local pressure buildup caused by disconnected or poorly connected chambers. It also ensures that the steam maintains a stable flow rate and distribution during the flow process, improving the utilization rate of the first membrane element 320. Simultaneously, The pervaporation products separated by the first membrane 320 can quickly enter the second chamber 3161 through the connecting path, and then be discharged to the product collection assembly 700 from the second outlet 313 of the third housing 316. Meanwhile, the residual vapor that has not passed through the first membrane 320 can flow from the first chamber 3141 to the reflux cooling assembly 600 through the first outlet 312, avoiding secondary mixing of the pervaporation products and the residual liquid, ensuring product purity, and also allowing the residual liquid to quickly leave the membrane area, reducing the interference of unseparated components in the residual liquid on the separation effect of the first membrane 320, and improving the overall separation efficiency.

[0035] Reference Figure 3 , Figure 4In some embodiments, the first membrane element 320 includes a first separation membrane 321, a first gasket 322, and a first connector 323. The first separation membrane 321 contacts the bottom surface of the first mounting groove 3151. The first gasket 322 is disposed on top of the first separation membrane 321, and the first connector 323 is disposed on top of the first gasket 322. The first connector 323 is connected to the second housing 315 to limit the first separation membrane 321. Specifically, the second housing 315 is provided with a first opening 3152, which communicates with the first housing 314 and the first mounting groove 3151. The first separation membrane 321 covers the first opening 3152, and the permeate side of the first separation membrane 321 faces the second outlet 313 of the third housing 316, so that the high-temperature steam flowing in from the first housing 314 must pass through the first separation membrane 321 to complete the separation, avoiding direct leakage of steam without separation and ensuring the effectiveness of the separation process. Furthermore, the first gasket 322 is positioned between the first separation membrane 321 and the first connector 323, protecting the first separation membrane 321 and preventing mechanical damage caused by direct contact between the first connector 323 and the first separation membrane 321. This protects the structural integrity of the first separation membrane 321 and extends its service life. Additionally, the inner wall of the first mounting groove 3151 of the second housing 315 is provided with a fifth thread, and the first connector 323 is provided with a sixth thread. The fifth and sixth threads engage, allowing the first connector 323 to abut against the first gasket 322, and the first gasket 322 to abut against the first separation membrane 321. This ensures the first separation membrane 321 is laid flat at the first opening 3152, preventing wrinkles and loosening, allowing steam to contact the surface of the first separation membrane 321, and ensuring the stability and consistency of the separation effect. Simultaneously, the detachable threaded connection between the first connector 323 and the second housing 315 facilitates the replacement of different specifications of the first separation membrane 321 according to experimental needs, improving the flexibility and adaptability of the device.

[0036] Reference Figure 1 , Figure 3 In some embodiments, the diameter of the first gasket 322 is smaller than the diameter of the first separation membrane 321, and the first connector 323 is provided with a plurality of first vent holes, so that the pervaporation products separated by the first separation membrane 321 pass through the first vent holes into the third housing 316, and are then discharged to the product collection assembly 700 through the second vent 313, ensuring the discharge of pervaporation products and avoiding poor discharge caused by local accumulation.

[0037] Reference Figure 3 , Figure 5In some embodiments, a first sealing groove 3153 is provided at the bottom of the first mounting groove 3151, and the first sealing groove 3153 is arranged around the first opening 3152. A first sealing ring 330 is provided in the first sealing groove 3153. The first sealing ring 330 can fill the gap between the first separation membrane 321 and the first opening 3152 to prevent steam generated by heating by the heating component 200 from leaking from the gap between the first separation membrane 321 and the first opening 3152. Furthermore, since the first connector 323 flattens and presses the first separation membrane 321 into the first opening 3152 through a threaded connection, the first sealing ring 330 can form an elastic buffer between the first separation membrane 321 and the first opening 3152. This can not only compensate for the slight dimensional deviation between the two, but also deform under the pressure of the first connector 323, resulting in a larger sealing contact area and more reliable sealing. This avoids sealing failure caused by insufficient processing precision of the first separation membrane 321 or the first opening 3152. At the same time, the first sealing ring 330 can also reduce the direct friction between the first separation membrane 321 and the second housing 315. Especially when disassembling and assembling the first separation membrane 321, it can reduce the risk of wear on the edge of the first separation membrane 321 and protect the structural integrity of the separation membrane.

[0038] Reference Figure 3 , Figure 5 In some embodiments, a second sealing groove 3154 is provided on the top of the second housing 315. The second sealing groove 3154 surrounds the first mounting groove 3151. A second sealing ring 340 is provided in the second sealing groove 3154. The second sealing ring 340 can fill the connection gap between the second housing 315 and the third housing 316 to form an annular sealing barrier, preventing steam from leaking from the gap between the second housing 315 and the third housing 316, and preventing damage to the vacuum environment inside the device.

[0039] Reference Figure 1 , Figure 3 In some embodiments, the outer side of the first outer shell 310 is wrapped with a pipe insulation heating jacket 350. The pipe insulation heating jacket 350 is used to insulate the first separation component 300. The pipe insulation heating jacket 350 can keep the temperature inside the first outer shell 310 at the optimal range that meets the separation requirements, ensure the stability of the high-temperature steam temperature, ensure the consistency and reliability of the separation efficiency of the first separation membrane 321, and at the same time reduce the energy loss of the heating component 200 and reduce the overall energy consumption of the experiment.

[0040] In some embodiments, the reflux cooling assembly 600 is configured as a reflux water cooler. The reflux water cooler can quickly cool the residual liquid, which remains at a high temperature after separation, preventing the direct reflux of the high-temperature residual liquid and thus avoiding an overall temperature increase in the mixture within the raw material tank 110. Simultaneously, the reaction liquid after pervaporation separation is returned to the raw material tank 110 via the reflux water cooler, which helps improve the utilization rate of the raw materials and achieves continuous pervaporation separation. Of course, in actual design, the structure of the reflux cooling assembly 600 can be configured according to actual needs.

[0041] Reference Figure 6 , Figure 7 In some embodiments, the second separation component 400 includes a raw material bottle (not shown), a second outer shell 410, and a second membrane element 420. The raw material bottle is disposed at the bottom of the second outer shell 410, and the second outer shell 410 is provided with a second mounting groove 4111. The second membrane element 420 is disposed within the second mounting groove 4111. The second outer shell 410 is provided with a second air inlet 4112 and a third air outlet 4121 disposed opposite to each other along a second direction. Both the second air inlet 4112 and the third air outlet 4121 are connected to the second mounting groove 4111. The second air inlet 4112 is connected to the raw material bottle, and the third air outlet 4121 is connected to the product collection component 700. Specifically, the outlet of the raw material bottle is connected to the second inlet 4112 via a gas pipe. During the experiment, a small amount of the mixture to be separated is placed in the raw material bottle, and the second membrane 420 is installed in the second mounting groove 4111 with the permeate side of the second membrane 420 facing the third outlet 4121. The raw material bottle is heated by an oil bath 450 to vaporize the mixture into steam. The steam enters the second membrane 420 through a conduit for separation, providing reliable parameter references for the subsequent formal experiment of the first separation component 300. In addition, the vacuum component 500 is connected to the third outlet 4121 via a gas pipe. The vacuum component 500 can create a pressure difference on both sides of the second membrane 420, which can accelerate the pervaporation products through the second membrane 420 and move towards the third outlet 4121, facilitating the rapid discharge of the products to the product collection component 700 and improving the efficiency of the preliminary experiment. In addition, during the experiment, the vacuum degree of the vacuum component 500 was adjusted multiple times to obtain the optimal vacuum degree. This optimal vacuum degree was then used as the vacuum degree in the experiment of the first separation component 300. This allowed for the selection of the best vacuum conditions suitable for the mixture to be separated. This reduced problems such as material waste and increased energy consumption caused by unreasonable vacuum parameters when directly conducting experiments with the first separation component 300. It also ensured that the first separation component 300 operated under the optimal vacuum degree, thereby improving the separation efficiency and stability of the mixture.

[0042] Reference Figure 6 , Figure 7In some embodiments, the second housing 410 includes a fourth housing 411 and a fifth housing 412, which are fitted together. The second mounting groove 4111 and the second air inlet 4112 are both disposed in the fourth housing 411, and the third air outlet 4121 is disposed in the fifth housing 412. The third air outlet 4121 discharges the pervaporation products separated by the second membrane 420 to the product collection assembly 700, thereby preventing the pervaporation products from remaining in the second housing 410 and ensuring the purity of the pervaporation products.

[0043] In some embodiments, the fourth housing 411 is provided with a seventh thread, and the fifth housing 412 is provided with an eighth thread. The seventh thread and the eighth thread mate to connect the fourth housing 411 and the fifth housing 412. During the assembly or maintenance of the experimental device, the fourth housing 411 and the fifth housing 412 can be quickly disassembled by screwing them on, facilitating the replacement, cleaning, or repair of the second membrane element 420. This reduces the operational difficulty and time cost of device maintenance and solves the problem of difficulty in replacing internal membrane elements in an integrated housing. In addition, the threaded fit can form a tight sealing structure. Even in high-temperature environments, the sealing performance of the threaded connection can prevent high-temperature steam or pervaporation products from leaking from the housing connection gaps, avoiding experimental failure or material waste due to leakage.

[0044] Reference Figure 6 , Figure 7In some embodiments, the second membrane element 420 includes a second separation membrane 421, a second gasket 422, and a second connector 423. The second separation membrane 421 contacts the bottom surface of the second mounting groove 4111. The second gasket 422 is disposed on top of the second separation membrane 421, and the second connector 423 is disposed on top of the second gasket 422. The second connector 423 is connected to the fourth housing 411 to limit the second separation membrane 421. Specifically, the fourth housing 411 is provided with a second opening 4113, which communicates with the fourth housing 411 and the second mounting groove 4111. The second separation membrane 421 covers the second opening 4113, and the permeate side of the second separation membrane 421 faces the third outlet 4121 of the fifth housing 412. This ensures that high-temperature steam flowing into the fourth housing 411 must pass through the second separation membrane 421 to complete separation, preventing steam from leaking directly without separation and ensuring the effectiveness of the separation process. Furthermore, the second gasket 422 is positioned between the second separation membrane 421 and the second connector 423, protecting the second separation membrane 421 and preventing mechanical damage caused by direct contact between the second connector 423 and the second separation membrane 421. This protects the structural integrity of the second separation membrane 421 and extends its service life. Additionally, the inner wall of the second mounting groove 4111 of the fourth housing 411 is provided with a ninth thread, and the second connector 423 is provided with a tenth thread. The ninth and tenth threads mate, allowing the second connector 423 to abut against the second gasket 422, and the second gasket 422 to abut against the second separation membrane 421. This ensures the second separation membrane 421 is smoothly laid out at the second opening 4113, preventing wrinkles and loosening, allowing steam to contact the surface of the second separation membrane 421, and ensuring the stability and consistency of the separation effect. Simultaneously, the detachable threaded connection between the second connector 423 and the fourth housing 411 facilitates the replacement of different specifications of the second separation membrane 421 according to experimental needs, improving the flexibility and adaptability of the device.

[0045] Reference Figure 1 , Figure 6 In some embodiments, the diameter of the second gasket 422 is smaller than the diameter of the second separation membrane 421, and the second connector 423 is provided with a plurality of second vent holes, so that the pervaporation products separated by the second separation membrane 421 pass through the second vent holes into the fifth housing 412, and are then discharged to the product collection assembly 700 through the third vent 4121, ensuring the discharge of pervaporation products and avoiding poor discharge caused by local accumulation.

[0046] Reference Figure 6 , Figure 8In some embodiments, a third sealing groove 4114 is provided at the bottom of the second mounting groove 4111, and the third sealing groove 4114 is arranged around the second opening 4113. A third sealing ring 430 is provided in the third sealing groove 4114. The third sealing ring 430 can fill the gap between the second separation membrane 421 and the second opening 4113 to prevent steam generated by heating by the oil bath 450 from leaking from the gap between the second separation membrane 421 and the second opening 4113. Furthermore, since the second connector 423 presses the second separation membrane 421 flat against the second opening 4113 via a threaded connection, the third sealing ring 430 can form an elastic buffer between the second separation membrane 421 and the second opening 4113. This not only compensates for minor dimensional deviations between the two, but also deforms under the pressure of the second connector 423, resulting in a larger sealing contact area and more reliable sealing. This avoids sealing failure caused by insufficient machining precision of the second separation membrane 421 or the second opening 4113. At the same time, the third sealing ring 430 can also reduce direct friction between the second separation membrane 421 and the second housing 315. Especially when disassembling and assembling the second separation membrane 421, it can reduce the risk of wear on the edge of the second separation membrane 421 and protect the structural integrity of the separation membrane.

[0047] Reference Figure 6 , Figure 8 In some embodiments, a fourth sealing groove 4115 is provided on the top of the fourth housing 411. The fourth sealing groove 4115 surrounds the second mounting groove 4111. A fourth sealing ring 440 is provided in the fourth sealing groove 4115. The fourth sealing ring 440 can fill the connection gap between the fourth housing 411 and the fifth housing 412 to form an annular sealing barrier, preventing steam from leaking from the gap between the fourth housing 411 and the fifth housing 412, and preventing damage to the vacuum environment inside the device.

[0048] In some embodiments, the raw material bottle is equipped with a first temperature measuring component (not shown in the figure). The first temperature measuring component measures the temperature inside the raw material bottle. By repeatedly adjusting the temperature of the oil bath 450, the optimal heating temperature is obtained. This heating temperature is then used as the heating temperature during the experiment of the first separation component 300. This allows for the selection of the best heating conditions suitable for the mixture to be separated, reducing problems such as raw material waste and increased energy consumption caused by unreasonable heating temperatures when directly conducting experiments with the first separation component 300. This ensures that the first separation component 300 operates at the optimal heating temperature, improving the separation efficiency and stability of the mixture.

[0049] Reference Figure 1 , Figure 9In some embodiments, the heating assembly 200 includes a heating tube 210 and a protective element 220. The protective element 220 is disposed outside the heating tube 210, providing protection for the heating tube 210 and preventing damage from direct contact with external objects during experiments. It also prevents workers from accidentally touching the high-temperature heating tube 210 and causing burns, thus improving operational safety. Furthermore, the protective element 220 includes a first protective part and a second protective part, which are detachably connected. Specifically, the first protective part and the second protective part are connected by a latch (not shown in the figure), facilitating subsequent replacement of the heating tube 210 and simplifying the operation. When the heating tube 210 malfunctions or needs to be replaced with a different specification heating tube according to experimental requirements, it is not necessary to disassemble the entire heating assembly 200. Simply opening the latch allows separation of the first and second protective parts, enabling direct removal or installation of the heating tube 210. This simple and convenient operation reduces maintenance and replacement time costs.

[0050] In some embodiments, the protective component 220 is configured as a mesh metal protective layer that can wrap around the outside of the heating tube 210 to prevent damage to the heating tube 210 caused by collisions or scratches from external objects during the experiment. It also prevents workers from accidentally touching the high-temperature heating tube 210 and getting burned, providing double safety protection for both the heating tube 210 and the operator. At the same time, the protective component 220 is configured with a mesh structure, which has good air permeability and heat dissipation. After the experiment, the residual heat of the heating tube 210 can be quickly diffused to the outside through the mesh, promoting the rapid cooling of the heating component 200, shortening the time for the device to switch from the high-temperature working state to the safe state at room temperature, accelerating the connection efficiency of the experimental process, and improving the overall experimental progress.

[0051] In some embodiments, the heating tube 210 can be configured as a coiled silicon carbide furnace tube. Silicon carbide material has high temperature resistance, thermal stability and high thermal conductivity, which can achieve the 200°C high temperature operating conditions required by the first separation component 300. Long-term use is not prone to damage due to high temperature aging or thermal expansion and contraction, thus extending the service life of the heating tube 210 and reducing the frequency and cost of consumable replacement. The coiled structure design increases the contact area between the heating tube 210 and the mixed liquid, so that the material can fully contact the tube wall when flowing through the heating tube 210, resulting in more uniform heating and avoiding local overheating or insufficient heating. This ensures that the mixed liquid can be heated to the target vaporization temperature, providing a stable steam feedstock for the subsequent separation of the mixed liquid by the first separation component 300, and ensuring the consistency of separation efficiency and product purity.

[0052] In some embodiments, the heating component 200 also includes a temperature control sensor, which can monitor the heating temperature of the heating component 200 in real time, realize the control of the heating process, ensure that the heating temperature is stable within the optimal range required for the experiment, avoid the unstable vaporization efficiency of the mixture or the performance of the separation membrane due to temperature fluctuations, and at the same time facilitate the control component to adjust the heating power in a timely manner according to the sensor feedback, realize intelligent temperature control, and improve heating accuracy and experimental repeatability.

[0053] In some embodiments, the inlet of the heating component 200 is connected to the outlet of the extraction component 120 via a stainless steel gas pipe, which is wrapped with a pipe heating jacket. Stainless steel has excellent high-temperature resistance and structural strength, capable of withstanding the conveying requirements of high-temperature materials and preventing deformation or damage to the stainless steel gas pipe due to high temperatures. The pipe heating jacket surrounding the stainless steel gas pipe keeps the flowing mixture within the pipe warm, preventing temperature drops due to heat loss during the conveying process from the extraction component 120 to the heating component 200. This ensures a stable initial temperature of the mixture entering the heating component 200, reduces the additional energy consumption of the heating component 200, and prevents condensation and blockage of the pipe due to cooling within the stainless steel gas pipe, ensuring smooth transport of the mixture.

[0054] Reference Figure 1 In some embodiments, the product collection component 700 is connected to the first separation component 300 and the second separation component 400, and is used to collect pervaporation products. The product collection component 700 includes a cooling element 710 and a receiving tank 720. The cooling element 710 is connected to the receiving tank 720 via a pipe. The pervaporation products are cooled by the cooling element 710 and flow into the receiving tank 720 for collection. The cooling element 710 can rapidly cool the high-temperature gaseous products into a liquid state, facilitating product storage in the receiving tank 720. Simultaneously, the products generated by the high-temperature separation of the first separation component 300 can enter the cooling element 710 through the second outlet 313, and a small amount of products generated by the second separation component 400 can also enter the cooling element 710 through the third outlet 4121, without the need for additional switching of the collection path. Furthermore, the first separation component 300 and the second separation component 400 share the same cooling element 710, which is beneficial for exploring optimal separation conditions for continuous pervaporation experiments.

[0055] In some embodiments, the cooling element 710 is configured as a reflux water cooler. Of course, in actual design, the structure of the cooling element 710 can be designed according to actual needs. In addition, the stainless steel shell of the reflux water cooler is connected to the side of the reflux water cooler, and the reflux water cooler 730 can continuously provide low-temperature cooling water to the reflux water cooler to ensure that the reflux water cooler always maintains its cooling function.

[0056] Reference Figure 1In some embodiments, the product collection component 700 is connected to the vacuum component 500 via a serpentine cold trap 740. The serpentine cold trap 740 is housed in a liquid nitrogen cup 750, which holds liquid nitrogen. The ultra-low temperature of the liquid nitrogen in the serpentine cold trap 740 causes the vapor to condense into a liquid state before being delivered to the vacuum pump 510, thereby preventing pervaporation products from entering the vacuum component 500 and preventing organic matter or corrosive components in the products from adhering to the internal components of the vacuum component 500. This ensures the normal operation of the vacuum component 500, extends its service life, and reduces equipment maintenance costs. Secondly, the serpentine cold trap 740 increases the contact area and contact time between the vapor and the cold trap wall, allowing the vapor to fully exchange heat with the ultra-low temperature wall as it flows through the cold trap, ensuring thorough condensation and preventing the loss of pervaporation products due to entering the vacuum component 500.

[0057] Reference Figure 1 In some embodiments, the vacuum assembly 500 includes a vacuum pump 510, a buffer tank 520, a pressure gauge, and a dryer 530. The inlet of the buffer tank 520 is connected to the outlet of the serpentine cold trap 740, and the outlet of the buffer tank 520 is connected to the dryer 530. The inlet of the vacuum pump 510 is connected to the dryer 530. Since the vacuum pump 510 may experience instantaneous fluctuations in vacuum level due to changes in the intake air volume during the pumping process, the buffer tank 520 stabilizes the vacuum level fluctuations generated by the vacuum pump 510 during operation. This ensures that the airflow entering from the serpentine cold trap 740 is stabilized in the buffer tank 520 before entering the dryer 530, preventing vacuum level fluctuations from being directly transmitted to the first separation assembly 300 and the second separation assembly 400. This prevents pressure difference fluctuations from affecting the separation and extraction efficiency of pervaporation products, ensuring the consistency of experimental results. In addition, a pressure gauge is installed on the buffer tank 520 to monitor the vacuum level inside the tank in real time, allowing operators to intuitively understand the operating status of the vacuum system. The pressure gauge data also serves as a basis for adjusting the parameters of the vacuum pump 510, ensuring the vacuum level matches experimental requirements. Simultaneously, the bottom of the buffer tank 520 has an adjustable outlet valve, facilitating the drainage of any accumulated condensate without stopping the system. This prevents condensate from entering the dryer 530 or vacuum pump 510, causing blockages and corrosion, ensuring continuous operation of the vacuum system and improving operational convenience. Furthermore, the dryer 530, located between the buffer tank 520 and the vacuum pump 510, adsorbs residual water vapor or trace liquid impurities in the gas flow, preventing these impurities from entering the vacuum pump 510 and avoiding damage due to moisture. This protects the sealing performance and lifespan of the vacuum pump 510, reducing equipment maintenance costs. Finally, the vacuum pump 510 is designed as a single-stage rotary vane vacuum pump. Of course, in actual design, the structure of the vacuum pump 510 can be customized according to specific needs.

[0058] In some embodiments, the membrane separation experimental apparatus further includes a control component connected to the raw material tank 110, the heating component 200, the first separation component 300, and the second separation component 400, respectively. This control component can monitor the vacuum level, temperature, or pressure of each key component of the experimental apparatus in real time, is easy to operate, and ensures the stability of the experimental results. Specifically, the control component includes a vacuum measurement and control system and a temperature measurement and control system. The vacuum measurement and control system is connected to the vacuum component 500 and measures and controls the vacuum level of the vacuum component 500. The temperature measurement and control system is connected to the heating component 200 and the oil bath 450, and can measure and control the heating temperature of the heating component 200 and the oil bath 450.

[0059] It should be noted that the real-time monitoring of the vacuum degree, temperature or pressure of each key component of the experimental device by the control component is existing technology, and this utility model has not made any improvements to this part, so its principle and process will not be described in detail.

[0060] In some embodiments, the membrane separation experimental apparatus further includes an operation panel, which includes a main switch, a temperature controller, a vacuum controller, and a pipeline insulation controller. The operation panel employs a dual control system, with an industrial touchscreen as the host computer and the temperature controller as the slave computer, ensuring that the instrument remains controllable even if some instruments malfunction.

[0061] It should be noted that the operation panel is existing technology, and this utility model has not made any improvements to this part, so its principle and process will not be described in detail.

[0062] In some embodiments, the membrane separation experimental apparatus is mounted on an instrument rack equipped with four swivel casters for easy movement. Furthermore, the wiring for each instrument and apparatus is concealed in a cabinet at the back of the instrument rack using a back panel wiring method, maintaining the tidiness of the experimental apparatus.

[0063] The embodiments of the present invention have been described in detail above with reference to the accompanying drawings. However, the present invention is not limited to the above embodiments. Within the scope of knowledge possessed by those skilled in the art, various changes can be made without departing from the spirit of the present invention. Furthermore, the embodiments of the present invention and the features thereof can be combined with each other unless otherwise specified.

Claims

1. A membrane separation experimental apparatus, characterized in that, include: A raw material supply assembly, comprising a raw material tank and an extraction component, wherein the raw material tank is connected to the extraction component; A heating assembly, connected to the extraction component, is used to heat the raw material; A first separation component is connected to the heating component and is used to separate the mixture. A reflux cooling assembly is connected to the raw material tank and the first separation assembly, respectively. The reflux cooling assembly is used to cool the residual liquid after separation and reflux it back to the raw material tank. A second separation component is used to separate the mixture before the first separation component operates, in order to determine optimal experimental parameters; A vacuum assembly, which is connected to both the first separation assembly and the second separation assembly.

2. The membrane separation experiment apparatus according to claim 1, wherein The membrane separation experimental apparatus further includes a product collection component. The first separation component includes a first housing, which is provided with a first air inlet, a first air outlet, and a second air outlet. The first air inlet and the first air outlet are disposed opposite each other on the lower side of the first housing along a first direction, and the second air outlet is disposed on the upper side of the first housing along a second direction. The first direction and the second direction are perpendicular to each other. The first air inlet is connected to the heating component, the first air outlet is connected to the reflux cooling component, and the second air outlet is connected to the product collection component.

3. The membrane separation experiment apparatus according to claim 2, wherein The first housing includes a first housing, a second housing, and a third housing connected sequentially along the second direction. The first air inlet and the first air outlet are located on opposite sides of the first housing. The second housing is provided with a first mounting groove, and a first membrane element is provided in the first mounting groove. The first membrane element is used to separate the mixture. The second air outlet is located on the third housing.

4. The membrane separation experiment apparatus according to claim 3, wherein The first membrane component includes a first separation membrane, a first gasket, and a first connector. The first separation membrane is in contact with the bottom surface of the first mounting groove. The first gasket is disposed on the top of the first separation membrane. The first connector is disposed on the top of the first gasket. The first connector is connected to the second housing to limit the position of the first separation membrane.

5. The membrane separation experiment apparatus according to claim 1, wherein The membrane separation experimental device further includes a product collection component. The second separation component includes a raw material bottle, a second outer shell, and a second membrane element. The raw material bottle is disposed at the bottom of the second outer shell, the second outer shell is provided with a second mounting groove, and the second membrane element is disposed in the second mounting groove. The second outer casing is provided with a second air inlet and a third air outlet arranged opposite to each other along a second direction. Both the second air inlet and the third air outlet are connected to the second mounting groove. The second air inlet is connected to the raw material bottle, and the third air outlet is connected to the product collection assembly.

6. The membrane separation experiment apparatus according to claim 5, wherein The second outer casing includes a fourth casing and a fifth casing, the fourth casing being fitted over the fifth casing, the second mounting groove and the second air inlet being disposed within the fourth casing, and the third air outlet being disposed within the fifth casing.

7. The membrane separation experiment apparatus according to claim 6, wherein The second membrane element includes a second separation membrane, a second gasket, and a second connector. The second separation membrane is in contact with the bottom surface of the second mounting groove. The second gasket is disposed on the top of the second separation membrane. The second connector is disposed on the top of the second gasket. The second connector is connected to the fourth housing to limit the position of the second separation membrane.

8. The membrane separation experiment apparatus according to claim 1, wherein The heating assembly includes a heating tube and a protective component. The protective component is disposed on the outside of the heating tube and includes a first protective part and a second protective part, which are detachably connected.

9. The membrane separation experiment apparatus according to claim 1, wherein The raw material tank includes a tank body and a cover, the tank body and the cover are closed together, the tank body is provided with a receiving cavity, the mixed liquid is placed in the receiving cavity, and the tank body is connected to the heating component; The cover is provided with a feed inlet, a nitrogen inlet, a temperature test piece, and a pressure test piece. The feed inlet and the nitrogen inlet are both connected to the accommodating cavity. The test ends of the temperature test piece and the pressure test piece are both located inside the accommodating cavity.

10. The membrane separation experimental apparatus according to claim 1, characterized in that, The membrane separation experimental apparatus further includes a control component, which is connected to the raw material tank, the heating component, the first separation component, and the second separation component.

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