CN101033559A - Gas layer propulsion electrostatic spinning apparatus and industrial application thereof - Google Patents
Gas layer propulsion electrostatic spinning apparatus and industrial application thereof Download PDFInfo
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- CN101033559A CN101033559A CN 200610024393 CN200610024393A CN101033559A CN 101033559 A CN101033559 A CN 101033559A CN 200610024393 CN200610024393 CN 200610024393 CN 200610024393 A CN200610024393 A CN 200610024393A CN 101033559 A CN101033559 A CN 101033559A
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Abstract
This invention relates to a static filature device pushed by a gas layer and its industrial application, in which, the device includes: a gas circulation push device, a gas drying and heating device, a sealed filaturing room, and air inlet at the top of the sealed room, a material room at the upper part of the sealed room, a spinneret at the lower part of the material room, electrode connected on the spinneret, a material receiving device at the lower part of the sealed room, an air outlet at the lower-right part of the room, a cooling device cooling gas flow with solvent and a solvent recovering device, which can make static filature to molding to polymers, increases spinning efficiency greatly by applying multiple sprayers, controls the temperature and humid of the entry flows to alter the temperature and humid of filature raw liquid, and further more, the pushed gas flow can drive the volatiled solvent in the process to flow out to be recovered.
Description
Technical field
The present invention relates to a kind of electrostatic spinning apparatus and commercial Application thereof.
Background technology
Electrostatic spinning is to utilize mechanical force to promote polymer solution to flow out from spinning head, under electrostatic force, thread is stretched, solvent evaporates, and then solidify and make fiberizing.The fiber that makes in this way has the little advantage of diameter, usually between several nanometers to tens micron.
The conventional electrostatic spin processes is at normal temperatures, open type is carried out, the spinning solution temperature is without adjusting, concentration is generally not high, the quantity of solvent that needs is bigger than dry-spinning and wet spinning, and normally 5～10 of fibrous raw material times, in the spinning process, solvent directly evaporate in the environment, causes solvent loss and contaminated environment.It is under (1) room temperature to the specific requirement of spinning solution and solvent, spinning solution can reach certain fine concentration of one-tenth, and viscosity is lower, the part spinning solution is because the characteristic of polymer itself, must under higher concentration, could become fine, at this moment solution viscosity is often higher, is unfavorable for the outflow that thread is uniform and stable.(2) solvent boiling point is suitable, at room temperature is easy to volatilization, owing to do not reclaim, so the price of solvent will suitably require can not harm be arranged to operating personnel than higher to toxicity.These require to have limited greatly the application of electrospinning process, inevitably can cause certain pollution to environment simultaneously.Therefore, change to advance the mode of polymer solution, the regulator solution temperature improves productive rate, and solvent can be reclaimed and reuse, and these all have great importance on economy and ecological view, also be those skilled in the art the problem of ten minutes concern.
Summary of the invention
The technical issues that need to address of the present invention are to disclose a kind of gas layer propulsion electrostatic spinning apparatus and commercial Application thereof, to overcome the above-mentioned defective that prior art exists, satisfy the needs of field of textiles development.
Electrostatic spinning apparatus of the present invention comprises:
The gas circulation propulsion plant;
The gas drying heater that is connected by pipeline with the gas circulation propulsion plant;
The airtight spinning chamber that is connected by pipeline with the gas drying heater, said airtight spinning chamber is an airtight container, comprise supplies room, air inlet, the spinning chamber, spinning head, electrode, material receiver and dc source, said supplies room is arranged on the top of airtight spinning chamber, air inlet is arranged on the supplies room top, and be connected by pipeline with the gas drying heater, said spinning chamber is arranged on the supplies room below, material receiver is arranged on the below in spinning chamber, said spinning head is arranged on the supplies room below, one end is connected with supplies room, the other end is connected with the spinning chamber, said electrode is arranged on the spinning head, and electrode is connected with dc source by lead, and said gas outlet is arranged on airtight spinning chamber bottom;
The cooling device that solvent-laden air-flow is cooled off that is connected by pipeline with the gas outlet of airtight spinning chamber;
The solvent recovery unit that is connected by pipeline with an end of cooling device;
The other end of cooling device is connected with the gas circulation propulsion plant by pipeline.
Device of the present invention can be used for the spinning of polymer, and spinning process comprises the steps:
With the spinning solution of polymer and the solvent composition supplies room of packing into, gas is forced into 0.1～2Mpa through the gas circulation propulsion plant earlier, obtain propulsive force, air-flow velocity is 0.0001～100m/s, pass through the dry heat device again, gas is heated to 0～150 ℃, enter supplies room by air inlet then, the flow velocity of spinning solution with 10～1000m/s flowed out from spinning head, under the effect of electrostatic force, form the solution thread, in the spinning chamber, solvent constantly volatilizees, and final thread moulding is collected on the material receiver.The solvent that volatilizes is discharged from the gas outlet under the drive of air-flow, becomes liquid condition behind apparatus for supercooling once more, can reclaim and utilization once more.Obtain propulsive force through cooled air-flow once more through the gas circulation propulsion plant, use in drying heating back.
Said polymer comprises poly, poly-a kind of in benzamide, poly butyric ester-poly-hydroxyl pentanoate copolymer or the poly-cellulose acetate;
Said solvent is selected from the N that contains additive, dinethylformamide, the N,N-dimethylacetamide that contains additive, chloroform or acetone, and said additive is selected from CaCl
2Or LiCl, its weight concentration in solvent is 0.1～5%.
Spinning voltage is 5～40KV, and in the solvent, the weight concentration of polymer is 0.1～20%.
Effect of the present invention is very significant:
Gas blanket advances the solution in the supplies room to flow out from a plurality of spinning heads, has improved the spinning productive rate greatly, and the air-flow behind the heat drying has improved the temperature of stoste, makes former fluid viscosity descend easier outflow of thread and uniform and stable.
Gas blanket plays the effect of environment control in air chamber, by the temperature to air-flow, the control of humidity can realize the environment control to the electrostatic spinning forming process.
Gas drives the solvent that volatilizees in the spinning process and flows out from the gas outlet, and after cooling, solvent becomes liquid state, recovery that can be easily and effectively.Can dissolve high polymer once more, use in the spinning process afterwards.Reduced harm greatly to environment.
Cooled gas behind heat drying, reuses again, and convenient economical, wastage is little.
Description of drawings
Fig. 1 is that gas-bearing formation of the present invention advances the electrostatic spinning apparatus structural representation.
The specific embodiment
As seen from Figure 1, gas-bearing formation of the present invention advances electrostatic spinning apparatus to comprise:
Gas circulation propulsion plant 1;
The gas drying heater 2 that is connected by pipeline with gas circulation propulsion plant 1;
The airtight spinning chamber 3 that is connected by pipeline with gas drying heater 2, said airtight spinning chamber 3 is an airtight container, comprise supplies room 5, air inlet 4, gas outlet 9, spinning chamber 12, spinning head 6, electrode 7 and material receiver 8, said supplies room 5 is arranged on the top of airtight spinning chamber 3, air inlet 4 is arranged on supplies room 5 tops, and be connected by pipeline with gas drying heater 2, said spinning chamber 12 is arranged on supplies room 5 belows, material receiver 8 is arranged on the below in spinning chamber 12, said spinning head 6 is arranged on supplies room 5 belows, one end is connected with supplies room 5, the other end is connected with spinning chamber 12, spinning head 6 apertures are preferably 1 μ m～2mm, preferred spinning head number is 1～20, said electrode 7 is arranged on the spinning head 6, and said gas outlet 9 is arranged on airtight spinning chamber 3 bottoms, and spinning chamber 12 preferred height L are 0.5～2m;
The dc source 13 that is connected by lead with electrode 7;
The cooling device 10 that solvent-laden air-flow is cooled off that is connected by pipeline with the gas outlet 9 of airtight spinning chamber 3;
The solvent recovery unit 11 that is connected by pipeline with an end of cooling device 10;
The other end of cooling device 10 is connected with gas circulation propulsion plant 1 by pipeline.
Said gas circulation propulsion plant 1 is general air transporting arrangement, and as chemical field gas compressor commonly used etc., its effect is to carry gas, there is no special requirement.
Said spinning head 6 is electrostatic spinning spinning head commonly used, as Electrospinning ofNanofibers:Reinventing the Wheel? Dan Li, Younan Xia, 2004,16, No.14,1151-1170, the technology of Advanced Materials bibliographical information, those skilled in the art can select as required.
Said gas drying heater 2 also is a kind of heat-exchange apparatus of routine, and as tubulation or plate type heat exchanger, those skilled in the art can select as required.
Embodiment 1
Adopt device as shown in Figure 1 to carry out spinning.Wherein:
Said gas circulation propulsion plant 1 is a gas compressor, is spinning head 6 as Electrospinning of Nanofibers:Reinventing the Wheel? Dan Li, Younan Xia, 2004,16, No.14,1151-1170, the technology of Advanced Materials bibliographical information, gas drying heater 2 is tubular heat exchangers.
Spinning condition is: spinneret orifice diameter is 1 μ m; The confined chamber height is 1m; The spinning head number is 10; The flow velocity (single hole) of spinning solution with 2ml/h sprayed from spinning head, and gas flow temperature is 60 ℃; The voltage that applies is 15KV; Gas is air, and pressure is 0.35Mpa; Air-flow velocity is 0.5m/s;
Spinning process is: be poly and the 2wt%CaCl of 15wt% with weight concentration
2N, dinethylformamide solution injecting material chamber, the air-flow of crossing with heat drying promotes, solution is by uniform and stable extruding from each spinning head, the solution that is extruded forms the solution thread under electrostatic force, the solution thread travels forward at a high speed, along with the volatilization of solvent and the drawing-off of electrostatic force, the solution thread finally is solidified into fibre, is collected on the material receiver of confined chamber bottom.The solvent that volatilizes in the process flows out from the gas outlet of confined chamber right lower quadrant with air-flow, becomes liquid after cooling off, and is collected in the solvent recovery unit subsequently.
The spinning result is as follows: average fibre diameter is 150nm, and solvent recovering rate is 80%.
Embodiment 2
Adopt device as shown in Figure 1 to carry out spinning.Wherein: spinning condition is: spinneret orifice diameter is 100 μ m; The confined chamber height is 1m; The spinning head number is 15; The flow velocity of spinning solution with 0.15ml/h sprayed from spinning head, and gas flow temperature is 70 ℃; The voltage that applies is 20KV; Gas is air, and pressure is 0.8Mpa; Air-flow velocity is 1.2m/s; Other are with embodiment 1.
Spinning process is: with weight concentration is the poly of 12wt% and the N of 3wt%LiCl, N-dimethylacetamide solution injecting material chamber, the air-flow of crossing with heat drying promotes, solution is by uniform and stable extruding from each spinning head, the solution that is extruded forms the solution thread under electrostatic force, the solution thread travels forward at a high speed, along with the volatilization of solvent and the drawing-off of electrostatic force, the solution thread finally is solidified into fibre, is collected on the material receiver of confined chamber bottom.The solvent that volatilizes in the process flows out from the gas outlet of confined chamber right lower quadrant with air-flow, becomes liquid after cooling off, and is collected in the solvent recovery unit subsequently.
The spinning result is as follows: average fibre diameter is 100nm, and solvent recovering rate is 87%.
Embodiment 3
Adopt device as shown in Figure 1 to carry out spinning.Wherein: spinning condition is: spinneret orifice diameter is 250 μ m; The confined chamber height is 0.8m; The spinning head number is 10; The flow velocity (single hole) of spinning solution with 0.5ml/h sprayed from spinning head, and pressure is 60 ℃ for the 0.4Mpa gas flow temperature; Air-flow velocity is 0.8m/s; The voltage that applies is 12KV; Other are with embodiment 1.
Spinning process is: be the poly-N to benzamide and 2wt%LiCl of 15wt% with weight concentration, N-dimethylacetamide solution injecting material chamber, the air-flow of crossing with heat drying promotes, solution is by uniform and stable extruding from each spinning head, the solution that is extruded forms the solution thread under electrostatic force, the solution thread travels forward at a high speed, along with the volatilization of solvent and the drawing-off of electrostatic force, the solution thread finally is solidified into fibre, is collected on the material receiver of confined chamber bottom.The solvent that volatilizes in the process flows out from the gas outlet of confined chamber right lower quadrant with air-flow, becomes liquid after cooling off, and is collected in the solvent recovery unit subsequently.
The spinning result is as follows: average fibre diameter is 135nm, and solvent recovering rate is 89%.
Embodiment 4
Adopt device as shown in Figure 1 to carry out spinning.Wherein: spinning condition is: spinneret orifice diameter is 100 μ m; The confined chamber height is 1.5m; The spinning head number is 20; The flow velocity of spinning solution with 0.45ml/h sprayed from spinning head, and pressure is 0.2Mpa, and gas flow temperature is 35 ℃; Air-flow velocity is 0.25m/s; The voltage that applies is 20KV; Other are with embodiment 1.
Spinning process is: be the chloroformic solution injecting material chamber of the poly butyric ester one poly-hydroxyl pentanoate copolymer of 0.7wt% with weight concentration, the air-flow of crossing with heat drying promotes, solution is by uniform and stable extruding from each spinning head, the solution that is extruded forms the solution thread under electrostatic force, the solution thread travels forward at a high speed, along with the volatilization of solvent and the drawing-off of electrostatic force, the solution thread finally is solidified into fibre, is collected on the material receiver of confined chamber bottom.The solvent that volatilizes in the process flows out from the gas outlet of confined chamber right lower quadrant with air-flow, becomes liquid after cooling off, and is collected in the solvent recovery unit subsequently.
The spinning result is as follows: average fibre diameter is 150nm, and solvent recovering rate is 90%.
Embodiment 5
Adopt device as shown in Figure 1 to carry out spinning.Wherein: spinning condition is: spinneret orifice diameter is 100 μ m; The confined chamber height is 1m; The spinning head number is 10; The flow velocity (single hole) of spinning solution with 0.5ml/h sprayed from spinning head, and pressure is 25 ℃ for the 0.5Mpa gas flow temperature; Air-flow velocity is 0.78m/s; The voltage that applies is 13KV; Other are with embodiment 1.
Spinning process is: the acetone soln injecting material chamber that with weight concentration is the poly-cellulose acetate of 10wt%, the air-flow of crossing with heat drying promotes, solution is by uniform and stable extruding from each spinning head, the solution that is extruded forms the solution thread under electrostatic force, the solution thread travels forward at a high speed, along with the volatilization of solvent and the drawing-off of electrostatic force, the solution thread finally is solidified into fibre, is collected on the material receiver of confined chamber bottom.The solvent that volatilizes in the process flows out from the gas outlet of confined chamber right lower quadrant with air-flow, becomes liquid after cooling off, and is collected in the solvent recovery unit subsequently.
The spinning result is as follows: average fibre diameter is 110nm, and solvent recovering rate is 92%.
Claims (9)
1. a gas layer propulsion electrostatic spinning apparatus is characterized in that, comprising:
Gas circulation propulsion plant (1);
The gas drying heater (2) that is connected by pipeline with gas circulation propulsion plant (1);
The airtight spinning chamber (3) that is connected by pipeline with gas drying heater (2), said airtight spinning chamber (3) is an airtight container, comprise supplies room (5), air inlet (4), gas outlet 9, spinning chamber (12), spinning head (6), electrode (7) and material receiver (8), said supplies room (5) is arranged on the top of airtight spinning chamber (3), air inlet (4) is arranged on supplies room (5) top, and be connected by pipeline with gas drying heater (2), said spinning chamber (12) is arranged on supplies room (5) below, material receiver (8) is arranged on the below of spinning chamber (12), said spinning head (6) is arranged on supplies room (5) below, one end is connected with supplies room (5), the other end is connected with spinning chamber (12), said electrode (7) is arranged on the spinning head (6), electrode (7) is connected with dc source (13) by lead, and said gas outlet (9) are arranged on airtight spinning chamber (3) bottom;
The dc source (13) that is connected by lead with electrode (7);
The cooling device (10) that solvent-laden air-flow is cooled off that is connected by pipeline with the gas outlet (9) of airtight spinning chamber (3);
The solvent recovery unit (11) that is connected by pipeline with an end of cooling device (10);
The other end of cooling device (10) is connected with gas circulation propulsion plant (1) by pipeline.
2. gas layer propulsion electrostatic spinning apparatus according to claim 1 is characterized in that, spinning head (6) aperture is 1 μ m～2mm.
3. gas layer propulsion electrostatic spinning apparatus according to claim 1 is characterized in that, the spinning head number is 1～20.
4. according to claim 1,2 or 3 described gas layer propulsion electrostatic spinning apparatus, it is characterized in that the height L of spinning chamber (12) is 0.5～2m.
5. the commercial Application of each described gas layer propulsion electrostatic spinning apparatus of claim 1～4 is characterized in that, is used for the spinning of polymer.
6. application according to claim 5 is characterized in that, comprises the steps:
With the spinning solution of polymer and the solvent composition supplies room of packing into, gas is forced into 0.1～2Mpa through the gas circulation propulsion plant earlier, passes through the dry heat device again, gas is heated to 0～150 ℃, enter supplies room by air inlet then, the flow velocity of spinning solution with 0.005～100000 μ l/h flowed out from spinning head, form the solution thread, in the spinning chamber, solvent evaporates, the thread moulding is collected on the material receiver, in the solvent, the weight concentration of polymer is 0.1～20%.
7. application according to claim 6 is characterized in that, said polymer comprises poly, poly-a kind of in benzamide, poly butyric ester-poly-hydroxyl pentanoate copolymer or the poly-cellulose acetate.
8. application according to claim 7 is characterized in that said solvent is selected from the N that contains additive, dinethylformamide, the N,N-dimethylacetamide that contains additive, chloroform or acetone, and said additive is selected from CaCl
2Or LiCl, its weight concentration in solvent is 0.1～5%.
9. application according to claim 8 is characterized in that, spinning voltage is 5～40KV.
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