CN102864503B - Electrostatic spinning device for scale production of micro-nano-fiber - Google Patents

Abstract

The invention belongs to the technical field of electrospinning devices, and relates to a large-scale electrospinning device for preparing micro-nano fibers. The liquid supply tank contains an electrospinning precursor solution, and the liquid supply pump communicates with the liquid supply tank pipeline and passes through a conduit. The spinning solution is delivered to the metal chain; a DC motor is installed at the left end of the upper side of the insulating base, and a governor is made at the center of the front side to control the DC motor; the insulating drive pulley is fixed on the shaft of the DC motor to move synchronously, and the passive pulley is fixed on the The insulating rod at the right end of the upper side of the insulating base rotates around the insulating rod, and the metal chain wraps around between the driving pulley and the driven pulley, and the rotation of the DC motor turns into a metal chain drive; The chain is in sliding contact, and the parallel distance between the spinning collector and the insulating base is 10-100cm; the overall structure is simple, the principle is reliable, the operation is convenient, the electrospinning efficiency is high, the spinning quality is good, it can be industrialized, and the production environment is friendly.

Description

A kind of electrospinning device for preparing micro-nano fibers

Technical field:

The invention belongs to the technical field of electrospinning devices, and relates to an electrospinning device with a linear nozzle structure capable of rapidly and large-scale preparation of micro-nano fibers, in particular to an electro-spinning device for preparing micro-nano fibers in a large-scale manner.

Background technique:

Nanofiber materials prepared by electrospinning have the characteristics of large specific surface area and small pore size. Application prospects. However, at present, its production equipment is still dominated by single-needle electrospinning equipment, and its productivity is extremely low (0.1-1 g/hour). It is mainly used for scientific research, and it is difficult to meet the needs of industrialization and industrialization. In recent years, scientists and related professional researchers from all over the world have been tackling this problem. Based on the idea of increasing production by obtaining multiple jets, they have successively proposed electrospinning devices with single needles, multiple needles, and needles. Considering the easy clogging of the needle supply liquid and the structural complexity of the multi-needle arrangement, the nozzleless electrospinning device has received extensive attention. At present, the results of some researchers in the world have initially moved electrospinning from the laboratory to the stage of application. The representative one is the nanometer fiber produced by the Czech Liberec Technical University and ELMARCO. The fiber spinning machine "Nano Spider", the nanofiber mat prepared by it has initially entered the stage of commercial application. This spinning machine eliminates the limitation of the spinneret and improves the production efficiency of electrospinning; Perfect, it has strict requirements on the spinning liquid, and the electric field strength required for electrospinning is very large; it also needs auxiliary systems such as vacuum devices and blowing devices to complete the spinning process; the spinning device structure is relatively complicated, and the spinning The process requirements are high, and the film on the cylinder is easy to become thicker and thicker, and it is not easy to form a Taylor cone. Many universities and scientific research institutes in China are also engaged in large-scale research on electrospinning, such as: mentioned in the Chinese patent "Multi-nozzle electrospinning device for coaxial composite continuous nano/micron fibers" (patent application number 200310109222) The spinning device increases the spinning volume to a certain extent by adding nozzles, but the structure of the equipment is relatively complicated, and the process is not easy to control. Disadvantages such as uniformity; Chinese patent "Composite preparation method and device for ultra-fine polymer fiber high-speed air-blown electrospinning" (patent application number 200710009595) through high-speed airflow to increase the speed of electrospinning, compared with single-needle spinning, the speed can be increased by 10 It has a good application prospect, but this patent is highly dependent on external conditions (high-speed airflow) and has a relatively complex structure.

Invention content:

The purpose of the present invention is to overcome the shortcomings of the prior art, and seek to design and manufacture a kind of electrospinning device that can be used to prepare micro-nano fibers in a large-scale mode. The fine metal chain is used as the spinning nozzle, which is realized by the transmission of the thin metal chain. The coating of the spinning solution on the metal chain and the high voltage will form a one-dimensional spray on the metal chain, and the effect of increasing the spinning output can be achieved by increasing the number of jets.

In order to achieve the above object, the main structure of the present invention includes a liquid supply kettle, an insulating conduit, a liquid supply pump, an insulating drive pulley, a DC motor, an insulating base, a metal chain, a governor, a spinning collector, a metal rod brush, Positive pole of high-voltage power supply, insulated passive pulley, negative pole of high-voltage power supply, high-voltage power supply, micro-nano fiber and insulating rod; the solution of electrospinning precursor is contained in the liquid supply kettle of box structure, and two liquid supply pumps and liquid supply pumps installed symmetrically The kettle pipeline is connected, and the solution is drawn from the liquid supply kettle, and the spinning solution is evenly transported to different positions on the metal chain with a width of 1-4mm through respective insulating conduits with a diameter of 2-4mm; the upper side of the plate-type insulating base A DC motor is installed at the left end, and a governor is formed at the center of the front side of the plate-type insulating base, and the governor is used to control the speed of the DC motor fixed on the insulating base; the length of the insulating base of the plate-type structure × width × The insulated drive pulley with a height of 500×80×5mm and a radius of 10-20mm is fixed on the shaft of the DC motor and moves synchronously. The radius of the insulated passive pulley is 10-20mm, which is fixed and installed on the right side of the insulating substrate. On the insulating rod, the insulating passive pulley automatically rotates around the insulating rod, and the metal chain is wound between the driving pulley and the passive pulley. The distance between the centers of the two pulleys is 400-600mm. The rotation of the DC motor is converted into The transmission of the metal chain; the upper end of the metal rod brush vertically fixed on the right side of the insulating base is in sliding contact with the metal chain, and the lower end of the metal rod brush is firmly fixed on the insulating base, and the positive pole of the high-voltage power supply is connected to the high-voltage power supply. The output positive electrode of the spinning collector is electrically connected to the metal chain to introduce the charge from the high voltage power supply; the spinning collector is electrically connected to the negative electrode of the high voltage power supply, and the geometric dimensions of the spinning collector are 600×100×5mm in length×width×height. The spinning collector and the insulating base are suspended and fixed in parallel, and the parallel distance between the two can be adjusted between 10-100 cm, so as to collect the micro-nano fibers prepared by electrospinning.

The operating environment temperature of the device of the present invention is 20-30 ℃, and the relative humidity of the environment is 30-60%RH; Slowly add absolute ethanol under magnetic stirring, and after magnetic stirring at room temperature, let it stand to obtain the PVP electrospinning precursor solution; then add the prepared PVP/ethanol spinning solution to the liquid supply tank to adjust the spinning collection The height between the pole and the metal chain is 15 cm, turn on the governor switch, the DC motor rotates clockwise, and adjust the speed to 150 rpm, turn on the high-voltage power switch, and adjust its voltage to 15 kV, the high-voltage power generated The charge is transmitted to the metal chain through the metal rod brush, and a high-voltage electric field is generated between the spinning collector; the two liquid supply pumps are respectively turned on, so that the spinning precursor solution in the liquid supply kettle is pumped to the On the metal chain; there is a small gap between the conduit opening and the metal chain. After the spinning solution comes out of the insulating conduit, it will stick to the metal chain due to the transmission of the metal chain. There is a high voltage between the metal chain and the spinning collector. Electrostatic field, the solution adhering to the metal chain produces a Taylor cone and forms a jet, the jet is split, stretched, solidified in the air, and finally deposited on the spinning collector; after spinning, turn off the liquid supply pump Power supply, when the electrospinning of the residual solution on the metal chain is completed and no more jets are produced, turn off the power supply of the high-voltage power supply; finally adjust the governor, turn off the DC motor, and the spinning process is over, and PVP micro-nano fibers are obtained.

Compared with the prior art, the present invention has the advantages of simple structure, relying only on the transmission of metal chains for spinning, and does not require additional atmosphere and auxiliary facilities; It can carry out long-term continuous electrospinning; the third is high spinning rate, using thin metal chains as linear nozzles, and the metal chains are composed of small metal buckles nested with each other. In addition, each raised metal button is equivalent to a spinneret, and the densely arranged spinnerets in the one-dimensional direction greatly increase the spinning rate, and the silk production of a single device can reach about 70 grams per hour. (The spinning material is polyvinylpyrrolidone PVP micro-nano fibers with a molecular weight of 1.3 million); Fourth, the spinning volume is easy to control. The liquid supply pump supplies the solution to the spinning section through the catheter. Under the premise of normal spinning, the spinning volume is completely It is determined by the liquid supply speed. Therefore, by controlling the liquid supply speed, the control of the spinning amount (including the thickness of the fiber film) can be easily realized; the overall structure is simple, the principle is reliable, the operation is convenient, the electrospinning efficiency is high, and the spinning The quality is good, it can be produced industrially, and the production environment is friendly.

Description of drawings:

Fig. 1 is the principle schematic diagram of the main structure of the present invention adopting the linear spinning nozzle type.

Fig. 2 is a schematic diagram of the structure and principle of the present invention to realize the electrospun fiber spinning process.

Fig. 3 is an optical microscope photo of polyvinylpyrrolidone PVP micro-nano fibers prepared in the present invention.

Detailed ways:

Further description will be given below through the embodiments and in conjunction with the accompanying drawings.

Example:

The main structure of this embodiment includes a liquid supply kettle 1, an insulating conduit 2, a liquid supply pump 3, an insulating drive pulley 4, a DC motor 5, an insulating base 6, a metal chain 7, a governor 8, a spinning collector 9, Metal rod brush 10, positive pole of high voltage power supply 11, insulated passive pulley 12, negative pole of high voltage power supply 13, high voltage power supply 14, micro-nano fiber 15 and insulating rod 16; electrospinning precursor is filled in liquid supply kettle 1 of box structure Solution, two symmetrically installed liquid supply pumps 3 are in communication with the liquid supply kettle 1, and the solution is drawn from the liquid supply kettle 1, and are respectively passed through the respective insulated conduits 2 with a diameter of 2-4mm to the metal pipes with a width of 1-4mm. Different positions on the chain 7 evenly convey the spinning solution; a DC motor 5 is installed on the left end of the upper side of the plate-type insulating base 6, and a governor 8 is formed at the center of the front side of the plate-type insulating base 6, and the governor 8 is used for Control the rotational speed of the DC motor 5 fixed on the insulating base 6; the length × width × height of the insulating base 6 of the plate structure is 500 × 80 × 5mm respectively, and the insulating driving pulley 4 with a radius of 10-20mm is fixed on the DC motor 5 and synchronously interlocking, the radius of the insulating passive pulley 12 is 10-20 mm, fixedly installed on the insulating rod 16 upright on the right end of the upper side of the insulating substrate 6, the insulating passive pulley 12 automatically rotates around the insulating rod 16, and the metal chain 7 Surrounded between the driving pulley 4 and the driven pulley 12, the distance between the centers of the two pulleys is 400-600mm, the rotation of the DC motor 5 is converted into the transmission of the metal chain 7 through two insulating pulleys; the vertical type is fixed on the insulating base The upper end of the metal rod brush 10 on the rear side of the right end of the seat 6 is in sliding contact with the metal chain 7, and the lower end of the metal rod brush 10 is firmly fixed on the insulating base 6, and the positive electrode 11 of the high voltage power supply and the output positive electrode of the high voltage power supply 14 are connected to each other. Connected, the charge from the high-voltage power supply is introduced to the metal chain 7; the spinning collector 9 is electrically connected to the negative electrode 13 of the high-voltage power supply, and the geometric dimensions of the spinning collector 9 are 600×100×5 mm in length×width×height. The spinning collector 9 and the insulating base 6 are suspended and fixed in parallel, and the parallel distance between the two can be adjusted between 10-100 cm, so as to collect the micro-nano fibers 15 prepared by electrospinning.

The ambient temperature implemented in this embodiment is 24.5°C, and the relative humidity of the environment is 43%RH; the specific preparation process is:

1) Solution selection: The selected spinning solution is polyvinylpyrrolidone PVP solution with a mass percentage of 13%. First, 13 grams of PVP (molecular weight: 1.3 million) particles are slowly added to 87 grams of absolute ethanol under magnetic stirring. Magnetic stirring for 4 hours, and then standing for 0.5 hours to obtain a uniform and transparent PVP electrospinning precursor solution with a mass percentage of 13%;

2) Operation method: first add the prepared PVP/ethanol spinning solution into the liquid supply kettle 1, adjust the height between the spinning collector 9 and the metal chain 7 to 15 cm, turn on the governor switch 8, and the motor Rotate clockwise, and adjust the rotating speed to 150 revolutions per minute (rpm), turn on the high-voltage power switch 14, and adjust its voltage to 15 kV. At this time, the charge generated by the high-voltage power supply will pass through the metal rod brush 10 to the metal chain 7 , and generate a high-voltage electric field with the spinning collector 9; open two liquid supply pumps 3 respectively, and the spinning precursor solution in the liquid supply kettle 1 will be pumped to the metal chain 7 through the respective conduits 2; insulated conduits There is a very small gap between the mouth and the metal chain 7. After the solution comes out from the insulating conduit 2, due to the transmission of the metal chain 7, the solution will stick to the metal chain 7, and there is a gap between the metal chain 7 and the spinning collector 9. In the high-voltage electrostatic field, the solution adhering to the metal chain 7 will produce a Taylor cone and form a jet, which will be split, stretched, solidified in the air, and finally deposited on the spinning collector 9, as shown in Figure 2; After the spinning is finished, first turn off the liquid supply pump power supply 3, and after about 30 seconds, after the electrospinning of the residual solution on the metal chain 7 is completed, and when there is no longer jet flow, turn off the power supply of the high voltage power supply 14; finally adjust the governor 8. Turn off the DC motor 5, and the spinning process is over; Fig. 3 is an optical microscope photo of the PVP micro-nano fiber prepared in this embodiment, the fiber is in a disordered state, uniform in thickness, and the same as the micro-nano fiber produced by electrospinning with a single needle. There is not much difference in the morphology of the fibers.

Claims (2)

1. An electrospinning device for preparing micro-nano fibers in a large-scale mode is characterized in that it includes a liquid supply kettle, an insulating conduit, a liquid supply pump, an insulating drive pulley, a DC motor, an insulating base, a metal chain, a governor, a spinning Wire collector, metal rod brush, positive pole of high voltage power supply, insulated passive pulley, negative pole of high voltage power supply, high voltage power supply, micro-nano fiber and insulating rod; the electrospinning precursor solution is filled in the box-type liquid supply tank, which is symmetrically installed The two liquid supply pumps are connected with the pipeline of the liquid supply kettle, and the solution is drawn from the liquid supply kettle, and are evenly transported to different positions on the metal chain with a width of 1-4mm through their respective insulated conduits with a diameter of 2-4mm. Silk solution; a DC motor is installed at the left end of the upper side of the plate-type insulating base, and a governor is made at the center of the front side of the plate-type insulating base, and the governor is used to control the speed of the DC motor fixed on the insulating base; the plate-type structure The length × width × height of the insulating base is 500 × 80 × 5mm respectively, and the insulating driving pulley with a radius of 10-20mm is fixed on the shaft of the DC motor and synchronized. The radius of the insulating passive pulley is 10-20mm. Installed on the insulating rod upright on the right side of the upper side of the insulating substrate, the insulating passive pulley automatically rotates around the insulating rod, and the metal chain is wound between the driving pulley and the passive pulley, the distance between the centers of the two pulleys is 400-600mm, DC motor The rotation of the metal rod is converted into the transmission of the metal chain through two insulated pulleys; the upper end of the metal rod brush vertically fixed on the right side of the insulating base is in sliding contact with the metal chain, and the lower end of the metal rod brush is firmly fixed on the insulating base , and the positive pole of the high-voltage power supply is electrically connected to the positive pole of the output of the high-voltage power supply, and the charge from the high-voltage power supply is introduced to the metal chain; the spinning collector is electrically connected to the negative pole of the high-voltage power supply, and the geometric dimensions of the spinning collector are length × width The x height is 600 x 100 x 5mm, and the spinning collector and the insulating base are suspended and fixed in parallel, and the parallel distance between the two can be adjusted between 10-100 cm to collect micro-nano fibers prepared by electrospinning . 2. The electrospinning device for preparing micro-nano fibers according to claim 1, characterized in that the operating environment temperature is 20-30°C, and the relative humidity of the environment is 30-60%RH; the spinning solution selected first is The mass percentage is 13% polyvinylpyrrolidone PVP solution, the PVP particle that molecular weight is 1,300,000 is slowly added in the dehydrated alcohol under magnetic stirring, leaves standstill after magnetic stirring at room temperature and promptly obtains PVP electrospinning precursor solution; Add the prepared PVP/ethanol spinning solution into the liquid supply tank, adjust the height between the spinning collector and the metal chain to be 15 cm, turn on the governor switch, the DC motor rotates clockwise, and adjust the speed to 150 rpm / minute, turn on the high-voltage power switch, adjust its voltage to 15 kV, the charge generated by the high-voltage power supply is transmitted to the metal chain through the metal rod brush, and a high-voltage electric field is generated between the spinning collector; Pump, so that the spinning precursor solution in the liquid supply tank is pumped to the metal chain through the respective insulating conduits; The transmission will stick to the metal chain. There is a high-voltage electrostatic field between the metal chain and the spinning collector. The solution adhered to the metal chain will produce a Taylor cone and form a jet. The jet will be split, stretched, and solidified in the air. , and finally deposited on the spinning collector; after spinning, first turn off the power of the liquid supply pump, and when the residual solution on the metal chain is electrospun and no jets are produced, turn off the power of the high voltage power supply; finally adjust the speed device, the DC motor is turned off, the spinning process ends, and micro-nano fibers are produced.