Membrane separation device

By designing a membrane separation device including an external operating box and a plate and frame membrane assembly, the existing plate and frame membrane separation device has solved the problems of high sealing complexity, large pressure loss and low loading density, and achieved higher sealing, lower pressure loss and higher density usage efficiency.

CN119869228APending Publication Date: 2025-04-25NINGBO UNIV +1
View PDF 0 Cites 0 Cited by

Patent Information

Application Number
CN202411972697.9
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2024-12-30
Publication Date
2025-04-25

AI Technical Summary

Technical Problem

The existing plate-frame membrane separation devices have high sealing complexity, large pressure loss and low loading density, which limit their application in confined spaces.

Method used

A membrane separation device including an external operating box and a plate-frame membrane assembly is designed. The plate and frame membrane assembly clamps the diaphragm through the front clamping plate, the rear clamping plate and the intermediate clamping plate, and forms a sealed space through the liquid flow channel groove and the cushion assembly to improve sealing and pressure transfer efficiency.

Benefits of technology

The membrane setting density is improved, the sealing structure is simplified, the pressure loss is reduced, and the use is unlimited in spaces with limited sizes and is more efficient.

✦ Generated by Eureka AI based on patent content.

Smart Images

  • Figure CN119869228A_ABST
    Figure CN119869228A_ABST
Patent Text Reader

Abstract

The invention discloses a membrane separation device which comprises an external operation box and a plate frame membrane assembly, the external operation box comprises a box body, an external panel is connected to the box body in a sealed mode, and a raw material liquid inlet pipeline, a raw material liquid outlet pipeline and a vacuumizing pipeline which penetrate through the external panel from outside to inside and are communicated with the interior of the box body are arranged on the external panel. The plate frame membrane assembly is arranged, and when the plate frame membrane assembly is provided with a plurality of membranes, the membrane arrangement density of the whole device is improved, so that the positions of the membranes are close, the use of the device in a space scene with a limited size is not limited and interfered, and the efficiency is higher; a sealed space is formed by the cushion layer assembly, the liquid flow channel groove and the surface of the film layer, so that raw material liquid fully flows on the surface of the film layer, the sealing effect is good, and the sealing structure is simple.
Need to check novelty before this filing date? Find Prior Art

Description

Technical Field

[0001] The invention relates to the technical field of membrane separation, and in particular to a membrane separation device. Background Art

[0002] The pervaporation technology in membrane separation technology has the advantages of strong separation ability, high efficiency, low energy consumption, environmental protection and strong compatibility, and has become a research hotspot in real industrial applications. Specifically, the pervaporation technology uses the vapor pressure difference of the components on both sides of the membrane as the driving force for mass transfer, and realizes the effective separation of the mixture based on the "dissolution-diffusion" or "adsorption-separation" mechanism. In this way, a new method can be provided for the efficient separation of the target product. In the composition of the membrane separation device, the performance of the pervaporation membrane is the key factor determining the separation effect. To achieve better separation effects, structural design improvements of the membrane separation device can be achieved, which can significantly improve the separation performance of the membrane, thereby reducing the cost and energy consumption in the separation process. In addition, the integrated process design of pervaporation technology and various process flows can make the production and separation of the target product coherent, form a flow-type production line, improve production efficiency and reduce costs. The above-mentioned integrated process design also has the advantages of reducing pollution and sustainable production.

[0003] The structure of the membrane separation device is the core component of the entire production line. The pervaporation process involves phase change and vacuum operation, so the membrane assembly needs to have a high degree of sealing. In addition, the structure of the membrane separation device must provide sufficient flow space for the gas on the permeate side to facilitate gas discharge. Gas discharge helps to ensure the vacuum degree on the permeate side, thereby maintaining low resistance and pressure drop on the permeate side, which helps to improve the separation efficiency of the entire system. The membrane separation device needs to be able to withstand a certain pressure and have good tolerance to organic solvents, which is the key to ensuring the stability and service life of the membrane assembly in harsh chemical environments.

[0004] At present, according to the structural form, the membrane separation devices used in the pervaporation process on the market can be mainly divided into plate-and-frame type, tube type and hollow fiber type. Plate-and-frame membrane separation devices are widely used because of their simple manufacturing and assembly, easy maintenance and replacement, and high operating stability.

[0005] The existing plate-and-frame membrane separation device still has some defects in industrial application, including:

[0006] 1. The sealing complexity is high;

[0007] 2. Large pressure loss;

[0008] 3. The packing density of the plate and frame membrane separation device is low, and its use is limited in space scenarios with limited size. Summary of the invention

[0009] The object of the present invention is to provide a membrane separation device to address the above-mentioned problems of high sealing complexity, low packing density of plate-and-frame membrane separation devices, and limited use in space scenarios with limited size.

[0010] In order to achieve its purpose, the present invention adopts the following technical solution:

[0011] A membrane separation device, comprising: an external operation box and a plate-and-frame membrane assembly;

[0012] The external operation box comprises a box body, an external panel is sealedly connected to the box body, and a raw material liquid inlet pipeline, a raw material liquid outlet pipeline and a vacuum pipeline are arranged on the external panel, which penetrate the external panel from the outside to the inside and are connected to the inside of the box body;

[0013] The plate-frame membrane assembly comprises a front clamping plate and a rear clamping plate which are positioned opposite to each other, N intermediate clamping plates are arranged between the front clamping plate and the rear clamping plate, N is an integer greater than or equal to 0, at least one diaphragm is arranged between the front clamping plate and the rear clamping plate, and when the number of the diaphragms is two or more, two adjacent diaphragms are separated by the intermediate clamping plate, and the front clamping plate, the rear clamping plate and the intermediate clamping plate are all provided with liquid flow channel grooves on their surfaces facing the diaphragms;

[0014] A cushion layer assembly is provided on both sides of the diaphragm, a hole for connecting the liquid flow channel groove and the diaphragm is formed in the middle of the cushion layer assembly, one side surface of the cushion layer assembly is connected to the diaphragm, and the other side surface opposite to the surface of the front clamping plate, the rear clamping plate or the middle clamping plate is correspondingly attached, the liquid flow channel groove is located on the inner side of the annular cushion layer assembly, and an independent space is formed between the liquid flow channel groove, the cushion layer assembly and the diaphragm for membrane separation of the raw liquid;

[0015] The cushion layer assembly comprises a template and a sealing gasket which are bonded to each other to form a layered structure, wherein the template is connected to the diaphragm, and the sealing gasket is bonded to the front clamping plate, the rear clamping plate or the middle clamping plate respectively;

[0016] The front clamping plate, the rear clamping plate and the middle clamping plate are connected to each other through an intermediate pipeline, and the intermediate pipeline includes an inlet pipe hole and an outlet pipe hole provided on the front clamping plate, the rear clamping plate and the middle clamping plate, the inlet pipe hole is connected to the raw material liquid inlet pipe line, and the outlet pipe hole is connected to the raw material liquid outlet pipe line;

[0017] The front clamping plate, the rear clamping plate and the middle clamping plate are clamped and connected by a connecting structure to form an independent space seal between the liquid flow channel groove, the cushion layer assembly and the diaphragm.

[0018] In some preferred embodiments, the intermediate pipeline further includes a connecting pipe for connecting the front clamping plate, the rear clamping plate, the middle clamping plate, the mold plate and the sealing gasket, and a sealing ring for sealing the connection between the connecting pipes.

[0019] In some preferred embodiments, the box body and the external panel are detachably connected, and an embedded structure is formed on the connecting surface of the box body and the external panel to enable the box body and the external panel to be embeddedly connected, and a sealing gasket is provided at the embedded structure to achieve vacuum sealing.

[0020] In some preferred embodiments, the membrane sheet includes a membrane layer and a flat support body, the flat support body is in a plate shape, and the membrane layer is synthesized on the surface of the flat support body.

[0021] In some preferred embodiments, the membrane layer is one or more of an inorganic membrane, an organic membrane and a mixed matrix membrane.

[0022] In some preferred embodiments, the membrane layer is a ZIF-8 / PMPS mixed matrix membrane.

[0023] In some preferred embodiments, the material of the flat support includes α-Al2O3.

[0024] In some preferred embodiments, the connection structure is a bolt mechanism.

[0025] In some preferred embodiments, the liquid flow channel is S-shaped.

[0026] In some preferred embodiments, a mold hole is formed on the mold plate, a via hole is formed on the sealing gasket, and the mold hole and the via hole are positioned opposite each other, and the aperture of the via hole is smaller than the aperture of the mold hole, so that the side surface of the sealing gasket is exposed to the mold hole, and the diaphragm is embedded in the mold hole and contacts the surface of the sealing gasket.

[0027] The beneficial effects of the present invention are:

[0028] 1. By setting a plate-frame membrane assembly, and when the plate-frame membrane assembly is provided with multiple membranes, the membrane setting density of the entire device is increased, so that the positions of the membranes are closely spaced, and thus the use in space scenes with limited size is not restricted or interfered, and the efficiency is higher;

[0029] 2. A sealed space is formed by the cushion layer assembly, the liquid flow channel and the membrane surface, so that the raw material liquid can fully flow on the membrane surface, with good sealing effect and simple sealing structure;

[0030] 3. The liquid flow grooves on the front clamping plate, the middle clamping plate and the rear clamping plate are used for the flow of the raw liquid and are subject to air pressure and hydraulic pressure. At the same time, the liquid flow grooves completely cover the diaphragm to increase the force of hydraulic and air pressure in the membrane separation action, greatly reducing the pressure loss. BRIEF DESCRIPTION OF THE DRAWINGS

[0031] Figure 1 It is a schematic diagram of the exploded structure of the external operation box in one embodiment of the present invention.

[0032] Figure 2 It is a schematic structural diagram of a plate-frame membrane assembly with three membranes assembled in a box in one embodiment of the present invention.

[0033] Figure 3 Schematic diagram of the exploded structure of a plate-frame membrane assembly in one embodiment of the present invention.

[0034] Figure 4 Schematic diagram of the structure of a diaphragm in one embodiment of the present invention.

[0035] Figure 5 -a is a schematic diagram of the structure of the front clamping plate in one embodiment of the present invention.

[0036] Figure 5 -b is a schematic diagram of the structure of a sealing gasket in one embodiment of the present invention.

[0037] Figure 5 -c is a schematic diagram of the structure of the pad in one embodiment of the present invention.

[0038] Figure 5 -d is a schematic diagram of the structure of the diaphragm in one embodiment of the present invention.

[0039] Figure 5 -e is a schematic diagram of the structure in which the front clamping plate, the sealing gasket, the backing plate and the diaphragm are assembled into a whole in one embodiment of the present invention.

[0040] In the attached figure:

[0041] External operating box-100;

[0042] Box body-110; external panel-120, raw material liquid inlet pipeline-121, raw material liquid outlet pipeline-122, vacuum pipeline-123;

[0043] Plate and frame membrane assembly-200;

[0044] Front clamping plate 210; rear clamping plate 220; middle clamping plate 230; diaphragm 240, membrane layer 241, flat plate support 242; cushion layer assembly 250, mold plate 251, mold hole 2511, sealing gasket 252, through hole 2521; middle pipeline 260, inlet pipe hole 261, outlet pipe hole 262, connecting pipe 263, sealing ring 264; liquid flow channel groove 200-a. DETAILED DESCRIPTION

[0045] The present invention will be further described below in conjunction with embodiments, but the present invention is not limited thereto.

[0046] The experimental methods in the following examples are conventional methods unless otherwise specified.

[0047] Example 1: Membrane separation device of the present invention

[0048] refer to Figure 1-5 As shown, a membrane separation device includes an external operation box 100 and a plate-frame membrane assembly 200 .

[0049] The external operation box 100 includes a box body 110, and an external panel 120 is sealed and connected to the box body 110. The box body 110 is hollow, and one side is open to accommodate other components. The external panel 120 is used to close the opening of the box body 110 so that the interior of the box body 110 forms a completely sealed space.

[0050] In some preferred embodiments, the box 110 is made of acrylic glass. Acrylic glass is transparent, so that the box 110 can be viewed directly from the outside, and is lighter. The external panel 120 is made of metal material.

[0051] The external panel 120 is provided with a raw material liquid inlet pipeline 121, a raw material liquid outlet pipeline 122 and a vacuum pipeline 123 which penetrate the external panel 120 from the outside to the inside and are connected to the inside of the box. The raw material liquid inlet pipeline 121 is used to inject raw material liquid, such as n-butanol solution, from the outside. After the raw material liquid undergoes osmotic separation treatment in the box 110, it is discharged to the outside through the raw material liquid outlet pipeline 122. The vacuum pipeline 123 is used to perform a vacuum operation on the box 110 to keep it in a vacuum state.

[0052] In some preferred embodiments, the raw material liquid inlet pipeline 121, the raw material liquid outlet pipeline 122 and the vacuum pipeline 123 are all provided with connecting pipes for connecting to external devices.

[0053] In specific implementation, the raw liquid inlet pipeline 121 is connected to a circulation pump for injecting raw liquid. The raw liquid outlet pipeline 122 is connected to a hose for conveying the raw liquid after flowing through the membrane surface to the raw liquid tank. The vacuum pipeline 123 is connected to a device for condensing and collecting permeate and a vacuum pump for vacuuming is connected to the rear end. Under the action of vacuum negative pressure, membrane separation occurs.

[0054] like Figure 2-3 As shown, the plate-frame membrane assembly 200 includes a front clamping plate 210 and a rear clamping plate 220 that are positioned opposite to each other, N intermediate clamping plates 230 are arranged between the front clamping plate 210 and the rear clamping plate 220, N is an integer greater than or equal to 0, at least one diaphragm 240 is arranged between the front clamping plate 210 and the rear clamping plate 220, and when the number of diaphragms 240 is two or more, two adjacent diaphragms 240 are separated by the intermediate clamping plate 230, and liquid flow channel grooves 200-a are arranged on the surfaces of the front clamping plate 210, the rear clamping plate 220 and the intermediate clamping plate 230 facing the diaphragm 240.

[0055] In some embodiments, the plate-frame membrane assembly 200 is provided with a single membrane sheet 240 , and the membrane sheet 240 is directly clamped and fixed by the front clamping plate 210 and the rear clamping plate 220 .

[0056] In some embodiments, Figure 2 As shown, the plate-frame membrane assembly 200 is provided with three diaphragms 240, and two adjacent diaphragms 240 are separated and clamped by an intermediate clamping plate 230, and the two ends of the whole generate pressure toward the middle through the front clamping plate 210 and the rear clamping plate 220, thereby achieving clamping.

[0057] In some embodiments, the plate-frame membrane assembly 200 is provided with four diaphragms 240, and two adjacent diaphragms 240 are separated and clamped by an intermediate clamping plate 230, and the two ends of the whole generate pressure toward the middle through the front clamping plate 210 and the rear clamping plate 220, thereby achieving clamping.

[0058] The pad layer assembly 250 is provided on both sides of the diaphragm 240. A hole for connecting the liquid flow channel 200-a and the diaphragm 240 is formed in the middle of the pad layer assembly 250. The surface of one side of the pad layer assembly 250 is connected to the diaphragm 240, and the surface of the other side opposite to the position corresponds to the surface of the front clamping plate 210 or the rear clamping plate 220 or the middle clamping plate 230. The liquid flow channel 200-a is located inside the annular pad layer assembly 250. An independent space is formed between the liquid flow channel 200-a, the pad layer assembly 250 and the diaphragm 240 for membrane separation of the raw material liquid. The function of the pad layer assembly 250 is to cooperate with each clamping plate and the surface of the diaphragm 240, thereby providing a space for the flow of the raw material liquid, so that the raw material liquid can fully contact with the diaphragm 240, and a good membrane separation process can be achieved. The raw material liquid flows in the liquid flow channel 200-a to achieve full contact with the diaphragm 240. The cushion layer assembly 250 contacts the diaphragm 240 and the surfaces of the front clamping plate 210 , the rear clamping plate 220 and the middle clamping plate 230 , and achieves sealing through externally applied pressure to prevent liquid leakage.

[0059] The cushion layer assembly 250 includes a mold plate 251 and a sealing gasket 252 which are bonded to each other to form a layered structure to further enhance the sealing effect. The mold plate 251 is connected to the diaphragm 240 , and the sealing gasket 252 is bonded to the front clamping plate 210 , the rear clamping plate 220 , or the middle clamping plate 230 .

[0060] In some preferred embodiments, a hole 2511 is formed on the mold plate 251, and a through hole 2521 is formed on the sealing gasket 252, and the hole 2511 and the through hole 2521 are positioned opposite each other, and the aperture of the through hole 2521 is smaller than the aperture of the hole 2511, so that the side surface of the sealing gasket 252 is exposed to the hole 2511, and the diaphragm 240 is embedded in the hole 2511 and contacts the surface of the sealing gasket 252. The mold plate 251 is used to support, limit and fix the diaphragm 240. The sealing gasket 252 supports and seals the diaphragm 240. The diaphragm 240 is arranged by setting the hole 2511 and the through hole 2521, which, on the one hand, ensures that the diaphragm 240 is firmly placed and provides support for the diaphragm 240, and on the other hand, the surface of the diaphragm 240 is exposed to the liquid flow channel 200-a, thereby ensuring that the raw material liquid is in full contact with the surface of the diaphragm 240.

[0061] In some specific embodiments, Figure 5 As shown, Figure 5 The diaphragm 240, the hole 2511 and the through hole 2521 are all square, and the side lengths of the hole 2511 and the diaphragm 240 are 10 cm, and the side length of the through hole 2521 is 9.2 cm. Thus, after the diaphragm 240 is embedded in the hole 2511, the through hole 2521 has a smaller side length, so it contacts the surface of the sealing gasket 252. Figure 5The installation and matching structure of the middle front clamping plate 210, the mold plate 251, the sealing gasket 252 and the diaphragm 240 is schematically shown, and the installation and matching structure of the rear clamping plate 220 and the middle clamping plate 230, the mold plate 251, the sealing gasket 252 and the diaphragm 240 is similar.

[0062] In a specific implementation, the sealing gasket 252 is made of rubber material to facilitate sealing and protect the diaphragm 240; the mold plate 251 is made of metal material to ensure the shape stability of the mold plate 251 and the effect of serving as a supporting component in the overall structure.

[0063] The front clamping plate 210, the rear clamping plate 220 and the middle clamping plate 230 are connected to each liquid flow channel 200-a through the intermediate pipeline 260, and the intermediate pipeline 260 includes an inlet pipe hole 261 and an outlet pipe hole 262 arranged on the front clamping plate 210, the rear clamping plate 220 and the middle clamping plate 230, the inlet pipe hole 261 is connected to the raw material liquid inlet pipe line 121, and the outlet pipe hole 262 is connected to the raw material liquid outlet pipe line 122.

[0064] In a specific implementation, the raw material liquid injected from the outside enters through the raw material liquid inlet pipeline 121, and flows into the liquid flow channel groove 200-a along the intermediate pipeline 260, so as to achieve full contact with the diaphragm 240, and realize membrane separation under the action of hydraulic pressure and gas pressure. The raw material liquid enters the tube hole 261 from the intermediate pipeline 260, and is discharged through the discharge tube hole 262 and the raw material liquid outlet pipeline 122.

[0065] The front clamping plate 210 , the rear clamping plate 220 and the middle clamping plate 230 are clamped together by a connecting structure to form an independent space seal between the liquid channel groove 200 - a , the cushion layer assembly 250 and the diaphragm 240 .

[0066] refer to Figure 2 and 3 As shown, the intermediate pipeline 260 is positioned perpendicularly to the front clamping plate 210 , the rear clamping plate 220 and the intermediate clamping plate 230 as a whole.

[0067] In some preferred embodiments, the connection mechanism is a bolt mechanism, which is used for clamping and has the effects of accurate positioning, anti-buffering and anti-vibration, and compensation for structural thermal deformation.

[0068] In some preferred embodiments, Figure 2 As shown, the intermediate pipeline 260 also includes a connecting pipe 263 for connecting the front clamping plate 210, the rear clamping plate 220, the intermediate clamping plate 230, the mold plate 251 and the sealing gasket 252, and a sealing ring 264 for sealing the connection of the connecting pipe 263. The connecting pipe 263 is used for connection, and at the same time, the sealing ring 264 ensures the sealing effect of the connection to prevent leakage.

[0069] In some preferred embodiments, the liquid flow channel 200-a on the middle clamping plate 230 is in the shape of a hollow hole that penetrates from front to back, so as to reduce the structural weight and improve efficiency while achieving the use effect.

[0070] In some preferred embodiments, Figure 3 As shown, the liquid flow channel 200-a is S-shaped, and the overall structure of the S-shaped liquid flow channel 200-a is compact, close to the form of a full plate surface. The advantage of this structural form is that it provides a sufficiently long channel length for the raw material liquid. When the raw material liquid flows, enough raw material liquid contacts the membrane 240, thereby separating the raw material liquid more efficiently.

[0071] In some preferred embodiments, the box body 110 and the external panel 120 are detachably connected, and an embedded structure is formed on the connection surface of the box body 110 and the external panel 120, so that the box body 110 and the external panel 120 are embedded and connected, and a sealing gasket is provided at the embedded structure to achieve vacuum sealing. In a specific implementation, the embedded structure is a mortise and tenon structure, and a mortise groove is provided on one side of the surface at the connection between the box body 110 and the external panel 120, and a protruding tenon block is provided on the other side. The connection between the box body 110 and the external panel 120 is sealed.

[0072] In some preferred embodiments, the box body 110 and the external panel 120 are detachably connected by a bolt mechanism.

[0073] The connection between the box body 110 and the external panel 120 needs to be accurately positioned to avoid the problem of misalignment. A bolt structure can be used to achieve accurate positioning through bolts and bolt holes to ensure accurate installation of each component.

[0074] To address the problem that external impact and vibration may cause damage to the box body 110 and the external panel 120 after they are connected, a bolt mechanism can be used to add spring washers to the bolts to achieve shock absorption and buffering effects, thereby preventing impact and vibration from affecting the connection structure of each component.

[0075] Regarding the connection between the box body 110 and the external panel 120, in case of large temperature difference, deformation may occur. The bolt connection can make way through threaded fitting to compensate for thermal expansion of the structural connection, thereby continuously ensuring the stability of the connection.

[0076] In some preferred embodiments, Figure 4 As shown, the membrane 240 includes a membrane layer 241 and a flat support body 242 . The flat support body 242 is in a plate shape, and the membrane layer 241 is synthesized on the surface of the flat support body 242 .

[0077] In some preferred embodiments, the membrane layer 241 is one or more of an inorganic membrane, an organic membrane, and a mixed matrix membrane. Any type of membrane layer can be used for membrane separation. When performing membrane separation treatment of a target product (e.g., alcohols), the type of membrane is selected adaptively in consideration of the material properties of the target product.

[0078] In some preferred embodiments, membrane layer 241 is a ZIF-8 / PMPS mixed matrix membrane (which can be used to separate butanol).

[0079] In some preferred embodiments, the material of the flat support 242 includes α-Al2O3. The advantages of α-Al2O3 are its excellent physical and chemical properties such as high temperature resistance, high hardness, wear resistance, chemical stability and electrical insulation. At the same time, the particle size distribution of α-Al2O3 is uniform and the formability is good, which helps to manufacture a support with uniform performance.

[0080] In some preferred embodiments, the connection structure is a bolt mechanism. The front clamping plate 210 and the rear clamping plate 220 are connected and fixed by the bolt structure, which is more convenient to operate.

[0081] Based on the schemes in the above embodiments, a method for membrane separation of n-butanol solution (n-butanol solution as raw material liquid) by the above membrane separation device is also provided, wherein the n-butanol solution is pumped into the above membrane assembly through a circulation system with a circulation pump, and the above membrane assembly is vacuumed by a vacuum pump, and the specific operation includes the following steps:

[0082] S100, starting the circulation pump to stabilize the circulation system, and pumping the n-butanol solution into the membrane separation device, and into the membrane according to the set path;

[0083] S200, starting the vacuum pump to evacuate the box to provide a negative pressure environment for the membrane separation process;

[0084] S300, the n-butanol solution is subjected to membrane separation treatment through a membrane under the action of gas pressure and hydraulic pressure. After the substance passes through the membrane, it is discharged from the membrane separation device through a set discharge path, and is condensed and collected.

[0085] Example 2: Preparation method of ZIF-8 / PMPS mixed matrix membrane

[0086] The preparation method of the ZIF-8 / PMPS mixed matrix membrane sheet of Example 1 is carried out according to the following steps:

[0087] S1. Preparation of Solution A:

[0088] 0.75 g ZIF-8 was added to 14.25 g isooctane (CAS No.: 540-84-1) to prepare a ZIF-8 dispersion. 0.5 g crosslinking agent TEOS (tetraethyl orthosilicate, CAS No.: 562-90-3) and 5.75 g isooctane were added to the ZIF-8 dispersion and mixed by probe ultrasonic in an ice-water bath under the ultrasonic conditions of 60% probe ultrasonic amplitude and 5 min; then magnetic stirring was performed under the conditions of 600 rpm and 1 h to obtain liquid A.

[0089] S2. Preparation of Solution B:

[0090] Take 5 g of organic PMPS (polymethylphenylsiloxane, CAS No.: 9004-73-3) and add it to 20 g of isooctane. Stir magnetically for 1 h at a stirring speed of 600 rpm to mix evenly to obtain liquid B.

[0091] S3. Preparation of casting solution

[0092] Pour liquid A into liquid B, and mix the mixed solution by probe ultrasonic mixing in an ice-water bath. The ultrasonic conditions are: probe ultrasonic amplitude: 60%, ultrasonic time: 5min, and then magnetic stirring. The magnetic stirring conditions are: speed: 600rpm, stirring time: 1h. Then add catalyst DBTDL (dibutyltin dilaurate, CAS No.: 77-58-7) and stir evenly (magnetic stirring conditions are: speed: 400rpm, stirring time: 10s) to form a uniform and stable casting solution. The mass ratio of catalyst / crosslinker / PMPS / ZIF-8 / isooctane in the casting solution is: 1:10:100:15:800.

[0093] S4. Preparation of mixed matrix flat membrane

[0094] Pour the casting liquid into the casting liquid tank, fix the fully cleaned and dried α-Al2O3 flat plate support (thickness 6mm) to the automatic lifting machine through the membrane assembly, and adjust the speed of the support body immersing in the casting liquid (viscosity 40cP~50cP) to 180mm min -1 The residence time is 10s, and then the support is pulled out from the casting liquid at a pulling speed of 60mm min -1 The support with the casting liquid adhered to the surface was placed at room temperature of 25°C to dry for 24 hours, then placed in a forced air drying oven at 100°C for 12 hours, and finally placed in a vacuum drying oven at 100°C for 12 hours to obtain a ZIF-8 / PMPS mixed matrix membrane sheet with stable performance, the membrane sheet comprising a flat support and a membrane layer synthesized on the surface of the flat support, the membrane layer being the ZIF-8 / PMPS mixed matrix membrane.

Claims

1. A membrane separation device, characterized in that: include: An external operating box (100) and a plate-and-frame membrane assembly (200); The external operation box (100) comprises a box body (110), an external panel (120) is sealedly connected to the box body (110), and the external panel (120) is provided with a raw material liquid inlet pipeline (121), a raw material liquid outlet pipeline (122) and a vacuum pipeline (123) which penetrate the external panel (120) from the outside to the inside and are connected to the inside of the box body; The plate-frame membrane assembly (200) comprises a front clamping plate (210) and a rear clamping plate (220) which are positioned opposite to each other, N intermediate clamping plates (230) are arranged between the front clamping plate (210) and the rear clamping plate (220), N is an integer greater than or equal to 0, at least one diaphragm (240) is arranged between the front clamping plate (210) and the rear clamping plate (220), and when the number of the diaphragms (240) is two or more, two adjacent diaphragms (240) are separated by the intermediate clamping plate (230), and liquid flow channel grooves (200-a) are arranged on the surfaces of the front clamping plate (210), the rear clamping plate (220) and the intermediate clamping plate (230) facing the diaphragms (240); A cushion layer assembly (250) is provided on both sides of the diaphragm (240), and a hole for connecting the liquid flow channel (200-a) and the diaphragm (240) is formed in the middle of the cushion layer assembly (250). One side surface of the cushion layer assembly (250) is connected to the diaphragm (240), and the other side surface opposite to the surface of the front clamping plate (210) or the rear clamping plate (220) or the middle clamping plate (230) is correspondingly attached. The liquid flow channel (200-a) is located on the inner side of the annular cushion layer assembly (250), and an independent space is formed between the liquid flow channel (200-a), the cushion layer assembly (250) and the diaphragm (240) for membrane separation of the raw liquid; The cushion layer assembly (250) comprises a mold plate (251) and a sealing gasket (252) which are bonded to each other to form a layered structure, wherein the mold plate (251) is connected to the diaphragm (240), and the sealing gasket (252) is bonded to the front clamping plate (210) or the rear clamping plate (220) or the middle clamping plate (230) respectively; The front clamping plate (210), the rear clamping plate (220) and the middle clamping plate (230) are connected to each of the liquid flow channel grooves (200-a) via an intermediate pipeline (260), and the intermediate pipeline (260) includes an inlet pipe hole (261) and an outlet pipe hole (262) arranged on the front clamping plate (210), the rear clamping plate (220) and the middle clamping plate (230), the inlet pipe hole (261) is connected to the raw material liquid inlet pipe line (121), and the outlet pipe hole (262) is connected to the raw material liquid outlet pipe line (122); The front clamping plate (210), the rear clamping plate (220) and the middle clamping plate (230) are clamped and connected via a connecting structure to seal the independent space formed between the liquid flow channel (200-a), the cushion layer assembly (250) and the diaphragm (240).

2. The membrane separation device according to claim 1, characterized in that: Also includes: The intermediate pipeline (260) also includes a connecting pipe (263) for connecting the front clamping plate (210), the rear clamping plate (220), the intermediate clamping plate (230), the mold plate (251) and the sealing gasket (252), and a sealing ring (264) for sealing the connection between the connecting pipe (263).

3. The membrane separation device according to claim 1, characterized in that: Also includes: The box body (110) and the external panel (120) are detachably connected, and an embedded structure is formed on the connection surface of the box body (110) and the external panel (120) so that the box body (110) and the external panel (120) are embeddedly connected, and a sealing gasket is provided at the embedded structure to achieve vacuum sealing.

4. The membrane separation device according to claim 1, characterized in that: Also includes: The membrane sheet (240) comprises a membrane layer (241) and a flat plate support body (242), the flat plate support body (242) is in a plate shape, and the membrane layer (241) is synthesized on the surface of the flat plate support body (242).

5. The membrane separation device according to claim 4, characterized in that: Also includes: The film layer (241) is one or more of an inorganic film, an organic film and a mixed matrix film.

6. The membrane separation device according to claim 4, characterized in that: Also includes: The membrane layer (241) is a ZIF-8 / PMPS mixed matrix membrane.

7. The membrane separation device according to claim 4, characterized in that: Also includes: The material of the flat plate support (242) includes α-Al2O3.

8. The membrane separation device according to claim 1, characterized in that: Also includes: The connecting structure is a bolt mechanism.

9. The membrane separation device according to claim 1, characterized in that: Also includes: The liquid flow channel (200-a) is S-shaped.

10. The membrane separation device according to claim 1, characterized in that: Also includes: A mold hole (2511) is formed on the mold plate (251), and a through hole (2521) is formed on the sealing gasket (252), and the mold hole (2511) and the through hole (2521) are positioned opposite each other, and the aperture of the through hole (2521) is smaller than the aperture of the mold hole (2511), so that the side surface of the sealing gasket (252) is exposed to the mold hole (2511), and the diaphragm (240) is embedded in the mold hole (2511) and contacts the surface of the sealing gasket (252).