Method for preparing silicon-based composite fiber membrane by jet electrospinning

Abstract

The present invention discloses a method for preparing a silicon-based composite fiber membrane by jet electrospinning, belonging to the field of electrospinning. The method comprises: preparing a PAN spinning solution with a mass fraction of 12% to achieve electrospinning conditions, and preparing a SiO2 spinning solution to achieve electrospinning conditions; providing a support frame at each end of a drum receiver, and providing an injector on each support frame; injecting the SiO2 spinning solution as a matrix into one injector, and injecting the PAN spinning solution as a carrier into the other injector; connecting each injector to a high-voltage power supply, and connecting the other end of each high-voltage power supply to the drum receiver, and adjusting the high-voltage power supply to a predetermined voltage; after adjustment, starting the high-voltage power supply to spin to form fibers, rotating the drum receiver to collect the fibers, and interlacing the SiO2 fibers and PAN fibers around the drum receiver to form a fiber membrane. The present invention utilizes electrospinning technology to mix and stack the two fibers, thereby enhancing their mechanical properties.

Description

Technical Field

[0001] The invention relates to the field of electrostatic spinning, and in particular to a method for preparing a silicon-based composite fiber membrane by jet electrospinning. Background Art

[0002] With the rise of new materials, research has begun on electrospun fiber membranes. Fiber membranes prepared by electrospinning have been widely used in industry, medicine, agronomy, and other research fields due to their large specific surface area, high porosity, excellent mechanical properties, and re-cleanability. However, with the advancement of technology, the requirements for the mechanical properties of fiber membranes are also gradually increasing. The mechanical properties of currently used pure SiO2 fiber membranes are gradually insufficient to meet existing requirements. Therefore, how to provide a method for preparing fiber membranes with higher mechanical properties is an urgent problem that those skilled in the art need to solve. Summary of the Invention

[0003] In view of this, the present invention provides a method for preparing a silicon-based composite fiber membrane by jet electrospinning. The present invention utilizes electrospinning technology to mix and stack two fibers together, thereby enhancing the mechanical properties.

[0004] In order to achieve the above object, the present invention adopts the following technical solutions:

[0005] A method for preparing a silicon-based composite fiber membrane by jet electrospinning comprises:

[0006] S10: Prepare spinning solution

[0007] Prepare PAN spinning solution with a mass fraction of 12% to achieve electrospinning conditions, and prepare SiO2 spinning solution to achieve electrospinning conditions;

[0008] S20: Design and debugging of the device

[0009] A support frame is set at both ends of the drum receiver, and an injector is set on each of the two support frames. SiO2 spinning solution is used as a matrix to inject SiO2 spinning solution into one injector, and PAN spinning solution is used as a carrier to inject PAN spinning solution into the other injector.

[0010] S30: Debugging of high voltage power supply

[0011] Connect the two injectors to a high-voltage power supply respectively, and connect the other ends of the two high-voltage power supplies to the roller receiver, and adjust the high-voltage power supplies to the predetermined voltage;

[0012] S40: Spinning to prepare fiber membranes

[0013] After debugging is completed, the high-voltage power supply is started to spin to form SiO2 fibers and PAN fibers, and the roller receiver is rotated to collect the SiO2 fibers and PAN fibers. The SiO2 fibers and PAN fibers are interwoven around the roller receiver to form a fiber membrane.

[0014] Preferably, the volume ratio of the SiO2 spinning solution and the PAN spinning solution is 1:1.

[0015] Preferably, in step S10, the ethyl orthosilicate solution and the anhydrous ethanol solution are measured and mixed in a molar ratio of 1:2 to form a mixed solution A, and then 1% dilute hydrochloric acid and deionized water are measured and mixed in a molar ratio of 0.01:2.5 to form a mixed solution B. The mixed solution B is mixed with the mixed solution A and heated for 40 minutes to prepare a SiO2 spinning solution that meets the electrospinning conditions.

[0016] Preferably, in step S10, polyacrylonitrile powder with an average molecular weight of 150,000 is mixed with 12 wt% of N,N-dimethylamide and stirred for 24 hours until the solution turns light yellow, thereby preparing a PAN spinning solution meeting electrospinning conditions.

[0017] Preferably, in step S20, the position of the injector for injecting SiO2 spinning solution is kept parallel to the upper end of the drum receiver, and the position of the injector for injecting PAN spinning solution is kept parallel to the lower end of the drum receiver.

[0018] Preferably, in step S20, a copper wire for connecting to a high-voltage power supply is provided in the injector.

[0019] Preferably, in step S30, the high voltage power supply connected to the ejector for injecting SiO2 spinning solution is modulated to 20KV, and the high voltage power supply connected to the ejector for injecting PAN spinning solution is modulated to 15KV.

[0020] Preferably, in step S40, the rotation speed of the drum receiver is 120 r / min.

[0021] The beneficial effects of the present invention are:

[0022] The present invention utilizes a high-voltage potential difference to form a Taylor cone for electrospinning. After producing two types of fibers, these fibers are then received by a rotating drum receiver. The two fibers are then mixed and superimposed to form a silicon-based composite fiber membrane, which not only enhances its mechanical properties but also modifies its internal structure. This composite fiber membrane significantly improves its mechanical properties compared to pure SiO2 fiber membranes. As a filtration separation membrane, it exhibits a higher water flux than silica during filtration. Additional aspects and advantages of the present invention will be apparent from the following description. BRIEF DESCRIPTION OF THE DRAWINGS

[0023] In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the following briefly introduces the drawings required for use in the embodiments or the description of the prior art. Obviously, the drawings described below are merely embodiments of the present invention. For ordinary technicians in this field, other drawings can be obtained based on the provided drawings without paying any creative work.

[0024] Figure 1 is a schematic diagram of the electrospinning device of the present invention;

[0025] Figure 2 1 is a highly schematic diagram of the jet spinning needle tube in the electrospinning device of the present invention;

[0026] Figure 3 This is a diagram of the spinning solution and spinning principle of the present invention.

[0027] Among them, in the figure:

[0028] 1. Drum receiver; 2. Support frame; 3. Injector for injecting SiO2 spinning solution; 4. Injector for injecting PAN spinning solution; 5. High-voltage power supply. DETAILED DESCRIPTION

[0029] The following will clearly and completely describe the technical solutions in the embodiments of the present invention in conjunction with the accompanying drawings. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without making creative efforts are within the scope of protection of the present invention.

[0030] See attached Figure 1-3 The present invention discloses a method for preparing a silicon-based composite fiber membrane by jet electrospinning, comprising:

[0031] S10: Prepare spinning solution

[0032] Prepare PAN spinning solution with a mass fraction of 12% to achieve electrospinning conditions, and prepare SiO2 spinning solution to achieve electrospinning conditions;

[0033] S20: Design and debugging of the device

[0034] A support frame 2 is respectively provided at both ends of the drum receiver 1, and an injector is respectively provided on the two support frames 2. The SiO2 spinning solution is used as the matrix and the SiO2 spinning solution is injected into one injector, and the PAN spinning solution is used as the carrier and the PAN spinning solution is injected into the other injector; the injector preferably includes a needle tube and a nozzle, the needle tube capacity is preferably 10 mL, the opening diameter is 2 mm, and the nozzle is placed at the opening position of the needle tube to improve the injection effect.

[0035] S30: Debugging of high voltage power supply 5

[0036] The two ejectors are respectively connected to a high-voltage power supply 5, and the other ends of the two high-voltage power supplies 5 are connected to the roller receiver 1, and the high-voltage power supply 5 is adjusted to a predetermined voltage; the two high-voltage sources provide electric field forces for the organic spinning solution PAN and the inorganic spinning solution SiO2 respectively, and spinning is performed by the electric field force jet.

[0037] S40: Spinning to prepare fiber membranes

[0038] After the debugging is completed, the high-voltage power supply 5 is started to spin to form SiO2 fibers and PAN fibers, and the drum receiver 1 is rotated to collect the SiO2 fibers and PAN fibers. The SiO2 fibers and PAN fibers are interwoven around the drum receiver 1 to form a fiber membrane.

[0039] After cooling, the prepared SiO2 spinning solution is poured into a 10mL syringe and placed on the support frame 2 on one side of the roller receiver 1. The syringe is kept parallel to the upper end of the roller receiver 1 and kept 20cm away from the roller receiver 1. The prepared PAN spinning solution is poured into the syringe and placed on the support frame 2 on the other side of the roller receiver 1. The syringe is kept parallel to the lower end of the roller receiver 1 and kept 15cm away from the roller receiver 1. The high-voltage power supply 5 is connected to the roller receiver 1 and the copper wire in the syringe respectively to form a high-voltage potential difference. The high-voltage power supply 5 connected to the injector 3 injected with SiO2 spinning solution is modulated to 20KV, and the high-voltage power supply 5 connected to the injector 4 injected with PAN spinning solution is modulated to 15KV. The high-voltage potential difference is used to form a Taylor cone for electrospinning to prepare two fibers. The two fibers are received by the rotating roller receiver 1, and the two fibers are mixed and superimposed together to form a silicon-based composite fiber membrane.

[0040] In this embodiment, preferably, the volume ratio of the SiO2 spinning solution and the PAN spinning solution is 1:1.

[0041] In this embodiment, preferably, in step S10, the ethyl orthosilicate solution and the anhydrous ethanol solution are measured and mixed in a molar ratio of 1:2 to form a mixed solution A, and then 1% dilute hydrochloric acid and deionized water are measured and mixed in a molar ratio of 0.01:2.5 to form a mixed solution B. The mixed solution B is mixed with the mixed solution A and heated for 40 minutes to prepare a SiO2 spinning solution that meets the electrospinning conditions.

[0042] In this embodiment, preferably, in step S10, polyacrylonitrile powder with an average molecular weight of 150,000 is mixed with 12 wt% of N,N-dimethylamide and stirred for 24 hours until the solution turns light yellow to prepare a PAN spinning solution meeting electrospinning conditions.

[0043] In this embodiment, preferably, in step S20, the injector 3 for injecting the SiO2 spinning solution is parallel to the upper end of the drum receiver 1, and the injector 4 for injecting the PAN spinning solution is parallel to the lower end of the drum receiver 1. This prevents the drum receiver 1 from receiving the solution in a counterclockwise direction, thereby achieving stacking and preparing the silicon-based composite fiber membrane.

[0044] In this embodiment, preferably, in step S20, a copper wire for connecting to a high-voltage power supply 5 is provided in the injector. The copper wire is inserted into the needle tube, and two high-voltage power supplies 5 are placed next to the two support frames 2, with one end connected to the copper wire in the needle tube and the other end connected to the roller receiver 1, forming a high-voltage electric field.

[0045] In this embodiment, preferably, in step S30, the high voltage power supply 5 connected to the injector 3 for injecting SiO2 spinning solution is modulated to 20KV, and the high voltage power supply 5 connected to the injector 4 for injecting PAN spinning solution is modulated to 15KV.

[0046] In this embodiment, preferably, in step S40, the rotation speed of the drum receiver 1 is 120 r / min.

[0047] The prepared silica-based fiber membranes were characterized and tested using mechanical properties, scanning electron microscopy, and Fourier transform infrared (FTIR) analysis. Comparative mechanical performance experiments revealed that, at the same thickness, the silica-based composite fiber membrane exhibited approximately 10 times the mechanical properties of the pure SiO2 fiber membrane compared to the silica-based composite fiber membrane. The silica fiber membrane was hydrophilic, while the silica-based composite fiber membrane was super-hydrophilic. FTIR analysis revealed the presence of a characteristic absorption peak (C=O) of polyacrylonitrile in the silica-based composite fiber membrane. Scanning electron microscopy revealed no beading in either membrane.

[0048] The above description of the disclosed embodiments is intended to enable one skilled in the art to implement or use the present invention. Various modifications to the embodiments will be readily apparent to one skilled in the art, and the general principles defined herein may be implemented in other embodiments without departing from the spirit or scope of the present invention. Therefore, the present invention is not limited to the embodiments shown herein but is to be construed in the widest manner consistent with the principles and novel features disclosed herein.

Claims

1. A method for preparing a silicon-based composite fiber membrane by jet electrospinning, characterized in that: include: S10: Prepare spinning solution Prepare PAN spinning solution with a mass fraction of 12% to achieve electrospinning conditions, and prepare SiO2 spinning solution to achieve electrospinning conditions; S20: Design and debugging of the device A support frame is set at both ends of the drum receiver, and an injector is set on each of the two support frames. SiO2 spinning solution is used as a matrix to inject SiO2 spinning solution into one injector, and PAN spinning solution is used as a carrier to inject PAN spinning solution into the other injector. S30: Debugging of high voltage power supply Connect the two injectors to a high-voltage power supply respectively, and connect the other ends of the two high-voltage power supplies to the roller receiver, and adjust the high-voltage power supplies to the predetermined voltage; S40: Spinning to prepare fiber membranes After debugging is completed, the high-voltage power supply is started to spin to form SiO2 fibers and PAN fibers, and the roller receiver is rotated to collect the SiO2 fibers and PAN fibers. The SiO2 fibers and PAN fibers are interwoven around the roller receiver to form a fiber membrane; In step S20, the position of the injector for injecting SiO2 spinning solution is kept parallel to the upper end of the drum receiver, and the injector for injecting PAN spinning solution is kept parallel to the lower end of the drum receiver; In step S20, a copper wire for connecting to a high-voltage power supply is provided in the injector.

2. The method for preparing a silicon-based composite fiber membrane by jet electrospinning according to claim 1, characterized in that: The volume ratio of SiO2 spinning solution and PAN spinning solution is 1:

1.

3. The method for preparing a silicon-based composite fiber membrane by jet electrospinning according to claim 1, characterized in that: In step S10, ethyl orthosilicate solution and anhydrous ethanol solution are measured and mixed in a molar ratio of 1:2 to form a mixed solution A, and then 1% dilute hydrochloric acid and deionized water are measured and mixed in a molar ratio of 0.01:2.5 to form a mixed solution B. After mixing the mixed solution B and the mixed solution A, they are heated for 40 minutes to prepare a SiO2 spinning solution that meets the electrospinning conditions.

4. The method for preparing a silicon-based composite fiber membrane by jet electrospinning according to claim 1, characterized in that: In step S10, polyacrylonitrile powder with an average molecular weight of 150,000 is mixed with 12 wt% of N,N-dimethylamide and stirred for 24 hours until the solution turns light yellow, thereby preparing a PAN spinning solution that meets electrospinning conditions.

5. The method for preparing a silicon-based composite fiber membrane by jet electrospinning according to claim 1, characterized in that: In step S30, the high voltage power supply connected to the ejector for injecting SiO2 spinning solution is modulated to 20KV, and the high voltage power supply connected to the ejector for injecting PAN spinning solution is modulated to 15KV.

6. The method for preparing a silicon-based composite fiber membrane by jet electrospinning according to claim 1, characterized in that: In step S40, the rotation speed of the drum receiver is 120 r / min.

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