CN112301440A - Circulating fluid power spinning device and method - Google Patents
Circulating fluid power spinning device and method Download PDFInfo
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- CN112301440A CN112301440A CN202011172822.XA CN202011172822A CN112301440A CN 112301440 A CN112301440 A CN 112301440A CN 202011172822 A CN202011172822 A CN 202011172822A CN 112301440 A CN112301440 A CN 112301440A
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- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
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Abstract
The invention relates to a circulating fluid power spinning device and a method. The circulating fluid power spinning device comprises a spinning stock solution injection mechanism, a solidification mechanism and a fiber collection mechanism, wherein the spinning stock solution injection mechanism is in fluid communication with a first connecting pipe; the coagulation mechanism comprises a coagulation bath barrel and a coagulation bath, a liquid inlet and a liquid outlet are formed in the upper end of the coagulation bath barrel, the first connecting pipe is provided with a spinning solution outlet, and the spinning solution outlet is positioned in the coagulation bath barrel; the coagulating bath tank is provided with a driving assembly, the driving assembly is connected with a second connecting pipe, the second connecting pipe is provided with a coagulating bath outlet, and the coagulating bath outlet is positioned in the coagulating bath barrel; the liquid outlet is used for allowing the coagulated fiber and the coagulating bath to flow out from the coagulating bath barrel. The coagulation bath can circularly flow, and in the preparation process of the hydrogel fiber, the fiber can be drawn by the shearing and stretching force of the flowing coagulation bath, the stretching force and the stretching part are controllable, the fiber is uniform in thickness and controllable in diameter, the production efficiency is high, and the method has an industrial prospect.
Description
Technical Field
The invention relates to the technical field of fiber preparation, in particular to a circulating fluid power spinning device and a circulating fluid power spinning method.
Background
The hydrogel fiber is a novel fiber with swelling property, stimulation response property, slow release property, immobilization property and the like, and has good application prospect in the fields of tissue engineering, biomedicine, textile, high polymer materials and the like. The existing spinning methods of hydrogel fibers include a microfluidic spinning method, an electrostatic spinning method, a wet spinning method and the like.
The microfluidic spinning refers to that fiber forming solution flows along the liquid flowing direction in a microchannel of a microfluidic chip without contacting the inner wall of the microchannel by utilizing the laminar flow characteristic of the fiber forming solution, and then is extruded in the microfluidic chip to be solidified into fibers, wherein the solidification mode comprises photopolymerization, double diffusion and the like. Compared with the traditional spinning process, the micro-fluidic spinning can be finished at normal temperature and normal pressure, has the advantages of controllable fiber shape and size, simple process and the like, and has wide application prospect in the fields of biological materials and the like. The microfluidic spinning device can produce nano-sized hydrogel fibers in which a continuous flow of a pre-gel solution is coated with a second solution and then cross-linked or solidified to produce continuous fibers.
Electrostatic spinning is the best method for preparing nanometer superfine fiber at present, and is to draw solution or melt of high polymer into filaments under the traction of electric field force, so as to obtain the micro-nanometer fiber with better continuity. In the electrostatic spinning process, viscoelastic fluid such as polymer melt or polymer solution is filled in an injector, 10-50 kV high-voltage static electricity is applied between a jetting needle head and a receiving device, a small amount of viscoelastic fluid is stably conveyed to the jetting needle head of the injector at a certain speed by an injection pump, and a high-voltage electrostatic field instantaneously generates potential difference between the needle head and the receiving device; with the increase of voltage, conical liquid drops are firstly formed at the needle head of the injector; when the voltage is increased to a critical value, the electrostatic field force borne by the polymer solution or the melt is enough to overcome the surface tension and viscous resistance of the fluid, and a charged jet flow is ejected from the top end of the Taylor cone to the direction of a cathode; the charged jet flow undergoes an unstable motion and stretching process, is rapidly refined in diameter through solvent volatilization or melt solidification, is solidified into superfine fibers, and is randomly deposited on the surface of a receiving device in a spiral mode. A simple, efficient process is often used to prepare hydrogel fibers.
In wet spinning, a thin stream of stock solution extruded from a spinneret orifice enters a coagulation bath, a solvent in the thin stream of stock solution diffuses into the coagulation bath, a coagulant permeates into the thin stream, and the thin stream of coagulant is precipitated in the coagulation bath to form fibers. The wet-spun polymer must have the appropriate structure and molecular weight. In addition, the method is suitable for producing natural fibers, such as chitosan-sodium alginate fibers, which cannot be prepared by melt spinning or dry spinning, because the method maintains a strong interchain hydroxyl force.
However, the above methods have low efficiency of microfluidic production of fibers and are difficult to mass-produce; electrostatic spinning is harsh on temperature and humidity conditions and is difficult to form single continuous filament type hydrogel fibers; and the drawing process of the wet spinning has higher requirements on the strength of the fiber.
Disclosure of Invention
In order to solve the technical problems, the invention aims to provide a circulating fluid dynamic spinning device and a circulating fluid dynamic spinning method, wherein a coagulation bath is in a circulating flowing state, the concentration is easy to keep stable, in the hydrogel fiber preparation process, the fiber can be drawn by the shearing and drawing force of the flowing coagulation bath, and the drawing force and the drawing part applied to the hydrogel fiber are controllable, so that the prepared hydrogel fiber is uniform in thickness and controllable in diameter, can be continuously produced, and has an industrial prospect.
The first object of the invention is to provide a circulating fluid dynamic spinning device for preparing hydrogel fiber, which comprises a spinning solution injection mechanism, a solidification mechanism and a fiber collection mechanism, wherein the spinning solution injection mechanism is used for containing spinning solution and injecting the spinning solution into the solidification mechanism, the spinning solution is solidified in the solidification mechanism to form solidified fiber, meanwhile, the flow of a solidification bath in the solidification mechanism is used for drafting the as-formed solidified fiber, and the fiber collection mechanism is used for collecting the solidified fiber; wherein:
the spinning dope injection mechanism is in fluid communication with the first connecting pipe;
the coagulation mechanism comprises a coagulation bath barrel and a coagulation bath groove positioned below the coagulation bath barrel, the coagulation bath barrel is arranged along the vertical direction, the upper end of the coagulation bath barrel is provided with a liquid inlet, the lower end of the coagulation bath barrel is provided with a liquid outlet, the lower end of the coagulation bath barrel is conical, a first connecting pipe is provided with a spinning liquid outlet, the spinning liquid outlet is positioned in the coagulation bath barrel, and the first connecting pipe is arranged along the vertical direction; the coagulating bath tank is used for containing coagulating bath, the coagulating bath tank is provided with a driving component, the driving component is connected with one end of a second connecting pipe, the second connecting pipe is provided with a coagulating bath outlet, and the coagulating bath outlet is positioned in the coagulating bath barrel; the liquid outlet is used for allowing the coagulated fiber and the coagulating bath to flow out from the coagulating bath barrel;
the fiber collecting mechanism comprises a filtering component and a fiber collecting component, the filtering component is right opposite to the lower part of the liquid outlet, and the filtering component is used for separating the solidified fibers and the solidified bath.
Further, the spinning solution injection mechanism comprises an injection pump and an injector, the spinning solution is contained in the injector, and the injection pump is used for driving the flow of the spinning solution in the injector; the syringe is in fluid communication with the first connecting tube.
Further, when the spinning dope injection mechanism includes a coaxial needle injection mechanism, a hollow fiber can be prepared.
Furthermore, the first connecting pipe is sleeved in the coagulation bath barrel and can move up and down relative to the coagulation bath barrel; the first connecting pipe is arranged along the vertical direction and is coaxial with the coagulating bath barrel; the second connection pipe is located outside the first connection pipe.
Further, the first connecting pipe is connected with a first height adjusting assembly, and the coagulation bath barrel is connected with a second height adjusting assembly.
Further, the inner diameter of the liquid inlet is larger than that of the liquid outlet. The difference between the inner diameters of the liquid inlet and the liquid outlet and the height of the liquid level of the coagulation bath in the coagulation bath barrel can cause the speed of the liquid in the coagulation bath barrel when the liquid flows through all the positions in the coagulation bath barrel to be different. The fiber is drawn by the coagulating bath fluid during the forming process, so that the shape, thickness and length of the fiber are affected, and the drawing force of the coagulating bath fluid can be controlled by the difference between the inner diameters of the liquid inlet and the liquid outlet and the liquid level of the coagulating bath.
Further, the filter assembly comprises a filter screen, a support assembly supporting the filter screen, and a third height adjustment assembly for adjusting the height of the support assembly.
Further, the fiber collecting assembly comprises a traversing unit and a winding unit, wherein the traversing unit can move left and right, the winding unit is fixedly connected with the traversing unit and can rotate for winding, and solidified fibers are orderly collected on a winding shaft of the winding unit through the combined action of the traversing unit and the winding unit.
Further, the traversing unit comprises a controller, a micro sliding table, a cloth feeding driver, a zero switch and a switching power supply.
Further, the winding unit comprises a speed reduction motor, a long shaft and a direct current power supply, and the reel is arranged on the long shaft. The speed reducing motor is arranged along the vertical direction, the miniature sliding table is connected with the speed reducing motor, the long shaft is arranged along the horizontal direction and connected with the speed reducing motor, and the speed reducing motor drives the long shaft to move around the axis of the speed reducing motor.
The controller in the transverse unit can adjust the micro sliding table to drive the cured fiber to move transversely, the reducing motor on the winding unit drives the long shaft to rotate around the axis of the reducing motor through the direct-current power supply, and the micro sliding table moves left and right and rotates with the long shaft to uniformly wind the fiber on the long shaft. The rotation speed of the long shaft can be controlled by a direct current power supply. The collected hydrogel fiber has certain uniformity, the diameter can be effectively controlled, and the hydrogel fiber can be continuously produced.
The second purpose of the invention is to provide a circulating fluid power spinning method, which is prepared by adopting the circulating fluid power spinning device of the invention and comprises the following steps:
injecting spinning solution into a first connecting pipe through a spinning solution injection mechanism, and injecting the spinning solution into a coagulating bath barrel through a spinning solution outlet;
driving the coagulation bath to flow into the second connecting pipe from the coagulation bath tank by using the driving assembly, and flowing into the coagulation bath barrel through the coagulation bath outlet, wherein the coagulation bath flowing into the coagulation bath barrel flows out of the first connecting pipe and flows out of the liquid outlet at the lower end of the coagulation bath barrel and then flows into the coagulation bath tank again, so that the circulating flow of the coagulation bath in the coagulation bath tank and the coagulation bath barrel is completed;
the spinning solution extruded from the spinning solution outlet is solidified under the action of the coagulating bath in the coagulating bath barrel, is simultaneously drawn and driven by the flowing coagulating bath, flows out from a liquid outlet at the lower end of the coagulating bath barrel and is intercepted in the filtering component under the action of the filtering component, and the fiber collecting component collects the fibers intercepted in the filtering component to finish the spinning process.
Further, the spinning dope comprises a water-soluble alginate solution and the coagulation bath comprises a metal salt solution. Preferably, the water-soluble alginate includes sodium alginate, potassium alginate, and the like. The metal salt comprises calcium chloride (CaCl)2) Barium chloride, and the like. When the spinning solution is injected into the coagulating bath barrel with a certain height at a certain speed, the sodium alginate once contacts with CaCl in the coagulating bath2Calcium ions in the solution undergo ion exchange reaction to form a cross-linked network structure, so that the solid hydrogel is formed. When the sodium alginate jet flow is injected into the calcium chloride solution, the crosslinking gelling reaction and the fluid drafting are almost instantly completed at the same time, so that the calcium alginate hydrogel obtained by crosslinking still keeps a continuous cylinder shape instantly formed by extruding the sodium alginate jet flow, and then forms a fiber shape.
Further, the inner diameter of the liquid inlet is larger than that of the liquid outlet, and the ratio of the two is preferably larger than 10: 1.
Further, the inner diameter of the liquid outlet is larger than the inner diameter of the spinning liquid outlet, and the ratio of the two is preferably larger than 1.5: 1.
Further, the ratio of the distance from the spinning solution outlet to the liquid outlet of the coagulation bath barrel to the height of the liquid level of the coagulation bath in the coagulation bath barrel is less than 1: 3.
In the invention, the key point of spinning the fiber with uniform thickness is to control the stability of the liquid level of the coagulating bath in the coagulating bath. The liquid level of the coagulating bath is influenced by the flow of the liquid inlet and the liquid outlet.
By the scheme, the invention at least has the following advantages:
the circulating fluid power spinning device is small and easy to control, has a simple structure, is easy to adjust spinning parameters, can realize the circulating flow of the coagulating bath in the coagulating bath tank and the coagulating bath barrel, and can realize the drafting of fibers under the dual actions of gravity and the flowing force of the coagulating bath.
The circulating hydrodynamic spinning device is used for circulating hydrodynamic spinning, because the coagulating bath barrel is arranged along the vertical direction, the liquid (including spinning solution and coagulating bath) entering the coagulating bath barrel flows out from the liquid outlet under the action of the gravity of the coagulating bath barrel, and because the coagulating bath circularly flows in the coagulating bath barrel and the coagulating bath barrel, when the spinning solution is injected into a proper position in the coagulating bath barrel, the solution is solidified to form fibers while being contacted with the coagulating bath, and the shearing and drawing force of the flowing coagulating bath is applied to the fibers, thereby being beneficial to quickly forming the fibers with uniform thickness and continuity. In addition, in the spinning process, the liquid flow rate on the axis in the coagulation bath cylinder, which is closer to the liquid outlet, is higher, and the shearing and drawing force is higher; the distribution of the liquid velocity in the coagulation bath barrel and the velocity at the liquid outlet are related to the liquid level height of the spinning solution outlet and the coagulation bath outlet in the coagulation bath barrel and the diameters of the spinning solution outlet and the coagulation bath outlet, so that the shape, thickness and length of the fiber can be changed under the action of various forces, and the controllable spinning of the fiber is realized.
The foregoing description is only an overview of the technical solutions of the present invention, and in order to make the technical solutions of the present invention more clearly understood and to implement them in accordance with the contents of the description, the following description is made with reference to the preferred embodiments of the present invention and the accompanying detailed drawings.
Drawings
FIG. 1 is a schematic view of a portion of the construction of a recirculating fluid dynamic spinning apparatus (only a portion of the fiber collection assembly is shown);
FIG. 2 is a schematic structural view of the fiber collection mechanism (filter assembly not shown);
FIG. 3 is an SEM test of fibers prepared with varying port diameters;
FIG. 4 is a graph showing results of thickness measurements of fibers prepared by varying the diameter of the exit orifice;
FIG. 5 is a photograph of fibers formed at various locations in a coagulation bath barrel;
FIG. 6 is a photograph of products produced under different spinning parameters;
FIG. 7 is a photograph of a fiber prepared with a gauge of 23G for a needle, d2 ═ 5 mm;
FIG. 8 shows the results of fiber thickness measurements obtained with needles of different gauges;
FIG. 9 is an SEM test of fibers from different gauge needles;
FIG. 10 is a surface topography of a fiber prepared with varying exit port diameters;
FIG. 11 is the results of thickness measurements of fibers prepared with varying exit port diameters;
description of reference numerals:
10-a syringe pump; 11-a syringe; 12-a first connection pipe; 13-a first height adjustment assembly; 20-a coagulating bath tank; 21-a drive assembly; 22-a second connecting tube; 23-a second height adjustment assembly; 24-a coagulating bath cylinder; 30-a filter screen; 31-a support assembly; 32-adjusting rod; 33-a reduction motor; 34-long axis; 35-a direct current power supply; 36-a micro slide; 37-a switching power supply; 38-a controller; 39-run in driver; 40-zero switch.
Detailed Description
The following examples are given to further illustrate the embodiments of the present invention. The following examples are intended to illustrate the invention but are not intended to limit the scope of the invention.
Example 1
Referring to the attached drawings, the circulating fluid dynamic spinning device for preparing hydrogel fibers comprises a spinning solution injection mechanism, a solidification mechanism and a fiber collection mechanism. The spinning solution injection mechanism is used for containing spinning solution and injecting the spinning solution into the solidification mechanism, the spinning solution is solidified in the solidification mechanism to form solidified fibers and is subjected to drafting of a flowing solidification bath, and the fiber collection mechanism is used for collecting the solidified fibers.
The spinning solution injection mechanism comprises an injection pump 10 and an injector 11, the injector 11 is filled with the spinning solution, the injection pump 10 is used for driving the flow of the spinning solution in the injector 11 and adjusting the injection speed of the spinning solution, and the injector 11 is in fluid communication with the first connecting pipe 12. The first connection pipe 12 has a spinning liquid outlet. The first connection pipe 12 is disposed in a vertical direction. The first connecting pipe 12 is a hollow iron pipe. A first height adjustment assembly 13 is connected to the first connecting tube 12. The bottom of the hollow iron tube is connected with a luer connector through hot melt adhesive, a needle head is fixed on the luer connector, and the outlet of the needle head is a spinning solution outlet.
The coagulation mechanism includes a coagulation bath barrel 24 and a coagulation bath 20 located below the coagulation bath barrel 24. A section of thick bamboo 24 is bathed in the solidification and sets up along vertical direction, and a section of thick bamboo 24 upper end is bathed in the solidification has the inlet, the lower extreme has the liquid outlet, and the solidification is bathed and is got into from the inlet, and a section of thick bamboo 24 lower extreme is bathed in the solidification is the toper, and conical bottom is equipped with the extension pipe, and the tip of extension pipe is located to the liquid outlet, and the internal diameter of inlet is greater. The difference in the inner diameters of the inlet and outlet ports results in different velocities of the liquid as it flows through. The liquid outlet of the coagulation bath barrel 24 is used for allowing the coagulated fiber and the coagulation bath to flow out of the coagulation bath barrel 24.
The first connecting pipe 12 is sleeved in the coagulating bath barrel 24 and can move up and down relative to the coagulating bath barrel 24; the first connecting pipe 12 is arranged in the vertical direction and is coaxial with the coagulation bath barrel 24. The spinning dope outlet is located in the coagulation bath barrel 24, from which the spinning dope flows into the coagulation bath barrel 24 and is solidified after contacting with the coagulation bath, forming a solidified fiber. Since the first connecting pipe 12 is connected with the first height adjusting block 13, the height of the spinning liquid outlet is correspondingly adjustable. The coagulation bath cylinder 24 is connected with a second height adjusting component 23, and correspondingly, the height of the coagulation bath cylinder 24 relative to the coagulation bath 20 can also be adjusted according to actual requirements. Preferably, the first height adjustment assembly 13 includes an iron stand and a butterfly clamp for clamping the first connection pipe 12. The second height adjusting assembly 23 includes an iron stand and an iron clamp for clamping a coagulation bath barrel 24.
The coagulation bath 20 is rectangular parallelepiped. The coagulating bath tank 20 is used for containing coagulating bath, a driving component 21 is arranged in the coagulating bath tank 20, and the driving component 21 is preferably a water suction pump with the power of 2.5 w. The driving assembly 21 is connected with one end of a second connection pipe 22 through a pumping pipe, the second connection pipe 22 has a coagulation bath outlet, and the coagulation bath outlet is located in a coagulation bath barrel 24. The second connection pipe 22 is located outside the first connection pipe 12. The driving assembly 21 is used for pumping the coagulation bath into the second connecting pipe 22, the coagulation bath flows out from the coagulation bath outlet and enters the coagulation bath barrel 24, and flows downwards under the action of gravity, so that a circulating fluid is formed in the coagulation bath barrel, and due to the difference of the inner diameters of the liquid inlet and the liquid outlet, the coagulation bath has a flow speed difference at two positions, so that a gradient flow speed is formed in the height direction in the coagulation bath barrel 24. The downwardly flowing coagulation bath exits the coagulation bath barrel 24 from the outlet port.
The fiber collecting mechanism comprises a filtering component and a fiber collecting component, the filtering component is right opposite to the lower part of the liquid outlet, and the filtering component is used for separating the solidified fibers and the solidified bath. The filter assembly includes a filter net 30, a support assembly 31 supporting the filter net 30, and a third height adjusting assembly for adjusting the height of the support assembly 31. The filter screen 30 includes a bottom wall and a side wall, and the bottom wall is provided with filter holes. The supporting component 31 is an iron ring, the third height adjusting component comprises an adjusting rod 32 and an adjusting screw, and the adjusting rod 32 is fixedly connected with the supporting component 31.
A filter screen 30 is located between coagulation bath barrel 24 and coagulation bath 20. The solidified fiber flowing out of the liquid outlet and the coagulating bath are separated by the action of the filter screen 30, the solidified fiber is intercepted in the filter screen 30, the coagulating bath falls into the coagulating bath 20 below through the filter screen 30, and the circulating flow of the coagulating bath is completed.
The fiber collecting assembly comprises a traversing unit and a winding unit, the traversing unit and the winding unit, the traversing unit can move left and right, and solidified fibers are wound on the winding unit through the traversing unit. The traverse unit includes a controller 38, a micro slide table 36, a cloth feeding driver 39, a zero point switch 40, and a switching power supply 37.
The controller 38 sends a pulse signal to control the driver, which has four input ports and two output ports. The working state can be manually and automatically operated. The speed of the micro sliding table 36 is adjustable, the diameter of the screw rod is 6mm, the sliding block moves by 2mm when the motor rotates by one circle, and the effective running distance of the sliding block is 200 mm. The output current of the cloth-in driver 39 is adjustable from 0.3A to 2A, the supply voltage is 12 VDC to 36VDC, and functions of offline, enabling, locking and the like are supported to play roles in overvoltage, undervoltage and overcurrent protection. The zero switch 40 is small in size and convenient to install. The switching power supply 37 controls the operation of the entire circuit of the traverse unit.
The winding unit comprises a speed reducing motor 33, a long shaft 34 and a direct current power supply 35, wherein a reel is arranged on the long shaft 34. The major axis 34 has a diameter of 8mm and a length of 10cm, and the rotation speed can reach 250 rpm. The voltage of the speed reducing motor 33 is 24V, and the fiber can be uniformly wound on the long shaft 34 by connecting with the DC power supply 35. The speed reducing motor 33 is arranged along the vertical direction, the micro sliding table 36 is connected with the speed reducing motor 33, the long shaft 34 is arranged along the horizontal direction and connected with the speed reducing motor 33, and the speed reducing motor 33 drives the long shaft 34 to move around the axis of the speed reducing motor 33. The controller 38 in the traverse unit can adjust the micro sliding table 36 to drive the cured fiber to move transversely, the reducing motor 33 on the winding unit drives the long shaft 34 to rotate around the axis of the micro sliding table through the direct current power supply 35, and the fiber can be uniformly wound on the reel on the long shaft 34 due to the left-right movement of the micro sliding table 36 and the self-rotation of the long shaft 34. The rotational speed of the shaft 34 can be controlled by a dc power supply 35. The collected hydrogel fiber has certain uniformity, the diameter can be effectively controlled, and the hydrogel fiber can be continuously produced.
Example 2
A cyclic hydrodynamic spinning process, carried out using the apparatus of example 1, comprising the following steps:
the spinning solution is injected into the first connecting pipe 12 through a spinning solution injection mechanism and is injected into the coagulating bath barrel 24 through a spinning solution outlet; wherein the spinning solution is sodium alginate aqueous solution.
The driving component 21 is used for driving the coagulation bath to flow into the second connecting pipe 22 from the coagulation bath 20 and flow into the coagulation bath barrel 24 through a coagulation bath outlet, the coagulation bath flowing into the coagulation bath barrel 24 flows out of the first connecting pipe 12 and flows out of a liquid outlet at the lower end of the coagulation bath barrel 24 and then flows into the coagulation bath 20 again, and the circulating flow of the coagulation bath in the coagulation bath 20 and the coagulation bath barrel 24 is completed; wherein the coagulating bath is calcium chloride water solution.
The spinning solution flowing out through the spinning solution outlet is solidified under the action of the coagulating bath in the coagulating bath barrel 24, flows out through the liquid outlet at the lower end of the coagulating bath barrel 24 and is intercepted in the filtering component under the action of the filtering component, and the fiber collecting component collects the fibers intercepted in the filtering component, so that the spinning process is completed. Specifically, the fibers trapped in the filtration module are wound onto the long shaft 34 by the traverse unit and through the reduction motor 33, the reduction motor 33 controls its winding speed by the direct current power source 35, and the collection speed of the fibers can be changed by changing the number of voltages.
In the process of forming the fiber, the form, thickness and length of the fiber are affected by the drawing of the coagulation bath fluid due to the difference in flow velocity between the two ports of the coagulation bath tube 24, and the drawing force of the coagulation bath fluid can be controlled by the position of the spinning solution outlet in the coagulation bath tube and the liquid level of the coagulation bath.
Wherein the height of the coagulation bath barrel 24 itself is 28 cm. The height of the coagulation bath (i.e. the distance between the liquid surface and the liquid outlet of the coagulation bath) was 24 cm. The injection speed of the dope was 300ml/h, the diameter of the liquid inlet was designated as d1, the diameter of the liquid outlet was designated as d2, and the distance from the dope outlet to the liquid outlet of the coagulation bath tube 24 (i.e., the height of the dope outlet) was designated as d 3. The specifications of needles connected with the luer connector are respectively 21G, 22G and 23G, wherein the inner diameter of the needle 21G is 0.51mm, and the outer diameter is 0.82 mm; the inner diameter of the 22G needle is 0.41mm, and the outer diameter is 0.73 mm; the 23G needle had an inner diameter of 0.33mm and an outer diameter of 0.63 mm.
The shape and length of the fiber can be changed under the action of gravity. Therefore, the morphology as formed from the fibers at the height of the different spin fluid outlets was tested. The spinning conditions were set as follows:
d 1-55 mm, d 2-3 mm, and d 3-45 mm, 55mm, and 65mm, respectively. The gauge of the luer connected needle was 21 g.
As shown in fig. 3, fig. 3a1-a2 are SEM test images of the surface of the fiber prepared under the condition that d3 is 45 mm; fig. 3b1-b2 are SEM test pictures of the surface of fibers prepared under the condition that d3 is 55 mm; fig. 3c1-c2 are SEM test pictures of the surface of fibers prepared under the condition that d3 is 65 mm. FIG. 4 is a graph showing the results of thickness measurement of fibers obtained under different conditions of d 3. Wherein the abscissa represents d3 and the ordinate represents the fiber thickness. The results show that the shape and thickness of the fibers formed by different heights of the spinning solution outlet are different, the higher the height of the spinning solution outlet is, the larger the shearing force applied to the spinning solution flowing out of the coagulating bath barrel 24 is, the larger the impact force applied to the fibers is, the more obvious the longitudinal stripe structure on the fiber surface is, and the deeper the groove is. The lower the height of the spinning solution outlet, the less the impact force on the fiber and the shallower the longitudinal striations on the fiber surface. It can also be seen from FIG. 4 that the above conditions produce fibers having diameters between 66 and 72 μm. As d3 increases, the diameter of the fiber becomes finer because the fiber is subjected to longer shear drawing at higher positions in coagulation bath barrel 24, and thus the diameter of the fiber can be adjusted by changing the height of the spinning solution outlet.
Fig. 5 is a photograph of fibers formed at different positions of the coagulation bath tube 24 under the condition of d3 being 55mm, and it is apparent that the fibers formed under the same condition have good uniformity in the whole and uniform thickness.
The exit orifice diameters d2 were varied, as was the flow rate of the coagulation bath in the barrel, and therefore the morphology of the fibers formed at the various exit orifice diameters was tested. The spinning conditions were set as follows:
d 1-55 mm, d 2-1 mm, 3mm, 5mm, d 3-55 mm. The specification of the needle head connected with the luer connector is 21G, 22G and 23G respectively.
When the diameter of the spinning solution outlet is large and the diameter of the liquid outlet is small, for example, when d2 is 1mm and the gauge of the needle is 23G, the spinning solution cannot be discharged, and gel-like particles are formed after the spinning solution is discharged through the spinning solution outlet (fig. 6). When d2 is 5mm and the gauge of the needle is 23G, the fibers cannot be continuously produced, as shown in fig. 7, a section of non-continuous irregularly shaped gel is formed instead of continuous hydrogel fibers. When d2 is 1mm and the gauge of the needle is 22G, the fiber can be continuously produced, and uniform and continuous hydrogel fibers can be obtained. Therefore, under a certain liquid level height and a certain spinning solution outlet height, the continuous output of the fibers is related to the diameter of the spinning solution outlet and the diameter of the liquid outlet, and the proper matching of the two is the key point that the fibers can be uniformly and continuously output.
The size of the diameter of the spinning solution outlet also affects the thickness of the produced fiber. The spinning conditions were set as follows:
d 1-55 mm, d 2-3 mm and d 3-55 mm. The specification of the luer-connected needles were 21G, 22G, 23G, respectively, and the thickness of the resulting fibers was as shown in fig. 8, in which the abscissa represents the luer specification and the ordinate represents the fiber thickness. As can be seen from FIG. 8, the smaller the needle diameter, the finer the fiber, the greater the difference in thickness between the fibers spun from the 21G needle and the 22G needle, and the lesser the difference between the fibers spun from the 22G and the 23G needle. The diameters of the needles of the three parts are different, and the shapes of the spun fibers are also different. Fig. 9 is a schematic diagram of fibers spun by needles 21G, 22G and 23G, the needle gauge corresponding to fig. 9a1-a2 is 21G, the needle gauge corresponding to fig. 9b1-b2 is 22G, and the needle gauge corresponding to fig. 9c1-c2 is 23G, and it is seen from the above figure that the fiber surface has a plurality of longitudinally extending stripe structures, the thicker the inner diameter of the needle, the more obvious the stripe structures are, and the macroscopically smooth fiber surface has no groove structure.
The size of the diameter of the liquid outlet determines the flow rate of the coagulation bath in the coagulation bath barrel 24, and the larger the diameter of the liquid outlet, the faster the flow rate of the coagulation bath in the coagulation bath barrel 24, and the larger the diameter and morphology of the fibers. The spinning conditions were set as follows:
d 1-55 mm, d 2-1 mm, 3mm or 5mm, and d 3-55 mm. The luer connected needle had a 23G gauge needle. Fig. 10 is a surface topography plot for fibers prepared under conditions of d 2-1 mm or 5mm, where fig. 10a1-a2 are the results for d 2-5 mm; results for d2 of 10b1-b2 were 1mm, and the results showed that the larger the port diameter, the finer the fibers. The longitudinal striation structure of the surface of the fiber is more obvious as the diameter of the liquid outlet is increased. FIG. 11 is the results of diameter tests of fibers prepared under the above three conditions, wherein the abscissa represents the size of d2 and the ordinate represents the thickness of the fiber, showing that the larger the outlet diameter, the finer the fiber.
When the device and the method are adopted to prepare the hydrogel fiber, the liquid level height of the coagulation bath barrel 24, the diameter of the liquid inlet, the diameter of the liquid outlet and the diameter and the height of the spinning solution outlet can be selected according to the diameter and the length of the hydrogel fiber to be produced. Then selecting the injection pump 10 and adjusting the flow rate and flow velocity of the liquid in the injector 11, adjusting the speeds of the traversing unit and the winding unit according to the parameters to collect the fiber, and after all the spinning parameters are adjusted, starting to spin the hydrogel fiber.
The device of the invention has small volume and easy control, and can eliminate a plurality of complex factors in the forming process of the industrial spinning machine so as to observe and explore various influencing factors in the forming process of the fiber.
The above is only a preferred embodiment of the present invention, and is not intended to limit the present invention, it should be noted that, for those skilled in the art, many modifications and variations can be made without departing from the technical principle of the present invention, and these modifications and variations should also be regarded as the protection scope of the present invention.
Claims (10)
1. A hydrokinetic spinning device, characterized by: the spinning solution collecting device comprises a spinning solution injecting mechanism, a solidifying mechanism and a fiber collecting mechanism, wherein the spinning solution injecting mechanism is used for containing spinning solution and injecting the spinning solution into the solidifying mechanism, the spinning solution is solidified in the solidifying mechanism to form solidified fibers, and the fiber collecting mechanism is used for collecting and drafting the solidified fibers; wherein:
the spinning dope injection mechanism is in fluid communication with the first connecting pipe;
the coagulation mechanism comprises a coagulation bath barrel and a coagulation bath groove positioned below the coagulation bath barrel, the coagulation bath barrel is arranged along the vertical direction, the upper end of the coagulation bath barrel is provided with a liquid inlet, the lower end of the coagulation bath barrel is provided with a liquid outlet, the lower end of the coagulation bath barrel is conical, the first connecting pipe is provided with a spinning solution outlet, the spinning solution outlet is positioned in the coagulation bath barrel, and the first connecting pipe is arranged along the vertical direction; the coagulation bath is used for containing a coagulation bath, a driving assembly is arranged on the coagulation bath and is connected with one end of a second connecting pipe, the second connecting pipe is provided with a coagulation bath outlet, and the coagulation bath outlet is positioned in the coagulation bath barrel; the liquid outlet is used for allowing the solidified fiber and the solidification bath to flow out of the solidification bath barrel;
the fiber collecting mechanism comprises a filtering component and a fiber collecting component, the filtering component is right opposite to the lower part of the liquid outlet, and the filtering component is used for separating the solidified fibers and the solidified bath.
2. The hydrokinetic spinning device of claim 1, wherein: the spinning stock solution injection mechanism comprises an injection pump and an injector, the spinning stock solution is contained in the injector, and the injection pump is used for driving the flow of the spinning stock solution in the injector; the syringe is in fluid communication with the first connecting tube.
3. The hydrokinetic spinning device of claim 1, wherein: the first connecting pipe is sleeved in the coagulation bath barrel and can move up and down relative to the coagulation bath barrel; the first connecting pipe is arranged along the vertical direction and is coaxial with the coagulation bath barrel; the second connection pipe is located outside the first connection pipe.
4. The hydrokinetic spinning device of claim 1, wherein: the first connecting pipe is connected with a first height adjusting assembly, and the coagulating bath barrel is connected with a second height adjusting assembly.
5. The hydrokinetic spinning device of claim 1, wherein: the filter assembly comprises a filter screen, a support assembly for supporting the filter screen and a third height adjusting assembly for adjusting the height of the support assembly.
6. The hydrokinetic spinning device of claim 1, wherein: the fiber collecting assembly comprises a traversing unit and a winding unit, wherein the traversing unit can move left and right, the winding unit is fixedly connected with the traversing unit and can rotate for winding, and the solidified fiber is collected on a reel of the winding unit through the traversing unit.
7. The hydrokinetic spinning device of claim 6, wherein: the traversing unit comprises a controller, a micro sliding table, a cloth feeding driver, a zero switch and a switching power supply.
8. The hydrokinetic spinning device of claim 6, wherein: the winding unit comprises a speed reducing motor, a long shaft and a direct-current power supply, and the reel is arranged on the long shaft.
9. A circulating hydrodynamic spinning method, characterized by being produced with the circulating hydrodynamic spinning device of any one of claims 1 to 8, comprising the steps of:
injecting a spinning solution into a first connecting pipe through a spinning solution injection mechanism, and injecting the spinning solution into the coagulating bath barrel through the spinning solution outlet;
the driving component is used for driving the coagulation bath to flow into the second connecting pipe from the coagulation bath tank and flow into the coagulation bath barrel through the coagulation bath outlet, the coagulation bath flowing into the coagulation bath barrel flows out of the first connecting pipe and flows out of a liquid outlet at the lower end of the coagulation bath barrel and then flows into the coagulation bath tank again, and the circulating flow of the coagulation bath in the coagulation bath tank and the coagulation bath barrel is completed;
the spinning solution flowing out from the spinning solution outlet is solidified under the action of the coagulating bath in the coagulating bath barrel, flows out from a liquid outlet at the lower end of the coagulating bath barrel after being drawn by the flowing of the coagulating bath in the coagulating bath barrel, and is trapped in the filtering component under the action of the filtering component, and the fiber collecting component collects the fibers trapped in the filtering component, so that the spinning process is completed.
10. The cyclic hydrodynamic spinning process of claim 9, wherein: the spinning dope comprises a water-soluble alginate solution, and the coagulation bath comprises a metal salt solution.
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| CN202011172822.XA CN112301440A (en) | 2020-10-28 | 2020-10-28 | Circulating fluid power spinning device and method |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| WO2023112804A1 (en) * | 2021-12-16 | 2023-06-22 | 日東電工株式会社 | Fibrous structure, scaffold material for cultured meat, and method for manufacturing fibrous structure |
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