CN116005282A - Uniform and continuous micro-nanofiber supercritical spinning method - Google Patents
Uniform and continuous micro-nanofiber supercritical spinning method Download PDFInfo
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- CN116005282A CN116005282A CN202310211687.2A CN202310211687A CN116005282A CN 116005282 A CN116005282 A CN 116005282A CN 202310211687 A CN202310211687 A CN 202310211687A CN 116005282 A CN116005282 A CN 116005282A
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- 239000000835 fiber Substances 0.000 claims abstract description 30
- 229920000642 polymer Polymers 0.000 claims abstract description 23
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- 230000005494 condensation Effects 0.000 claims abstract description 14
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- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 8
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims description 6
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- CYRMSUTZVYGINF-UHFFFAOYSA-N trichlorofluoromethane Chemical compound FC(Cl)(Cl)Cl CYRMSUTZVYGINF-UHFFFAOYSA-N 0.000 description 1
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Classifications
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
- Y02P70/50—Manufacturing or production processes characterised by the final manufactured product
- Y02P70/62—Manufacturing or production processes characterised by the final manufactured product related technologies for production or treatment of textile or flexible materials or products thereof, including footwear
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- Spinning Methods And Devices For Manufacturing Artificial Fibers (AREA)
Abstract
The invention relates to a uniform and continuous micro-nano fiber supercritical spinning method, which comprises the following steps: the first step: introducing high-pressure inert gas into the device, conveying the spinning solution from the high-pressure chamber to the low-pressure chamber, and primarily reducing the pressure of the spinning solution; and a second step of: opening a spinning nozzle, spraying spinning solution from the spinning nozzle, solidifying fiber-forming polymer, and forming fiber plexifilamentary under the restraint of the spinning nozzle; and a third step of: and in the spinning chamber, the solvent which is gasified and diffused is condensed and recovered by utilizing a condensation reflux pipeline, so that the recycling is realized. Compared with the prior art, the uniform and continuous micro-nano fiber supercritical spinning method can continuously produce, improve the production efficiency, and the non-woven fabric prepared by spinning has more excellent barrier puncture resistance, high raw material utilization rate and no pollution to the environment.
Description
Technical Field
The invention relates to the technical field of spinning, in particular to a uniform and continuous micro-nano fiber supercritical spinning method.
Background
The existing mature spinning methods comprise melt spinning, solution spinning, dry spinning and the like, wherein the melt spinning has the advantages of high winding speed, no need of solvent and precipitant, simple operation equipment and short process flow, but the fiber-forming polymer with higher decomposition temperature is limited to use the spinning method; the solution spinning is divided into wet spinning, dry spinning and dry-wet spinning, wherein the high polymer concentrated solution is quantitatively extruded from a spinning hole, the solution is finely solidified into fibers through a coagulating bath or hot air and hot inert gas, the wet spinning is mainly used for spinning viscose fiber, cuprammonium fiber, polyacrylonitrile fiber, polyvinyl formal fiber and the like, the dry spinning is mainly used for spinning acetate fiber, polyurethane fiber, polyvinyl chloride fiber and the like, and also used for spinning polyacrylonitrile fiber, polyvinyl alcohol fiber and the like, the dry-wet spinning combines high-temperature spinning and low-temperature coagulation, the process condition is easy to adjust, and the temperature of a spinneret is not limited by the temperature of the coagulating bath, so the method is particularly suitable for spinning polymer solutions with high molecular weight, high concentration and high viscosity, such as high polymer liquid crystal spinning of aramid fiber and the like. Compared with the existing mature spinning method, the newly developed supercritical spinning method has the advantages of being wider in scope, higher in production efficiency of materials in a supercritical state, and excellent in barrier and puncture preventing performances of the produced fabric.
The preparation of micro-nano fibers based on a supercritical spinning method has the following technical problems: firstly, the pressure in a preposed reaction kettle is too high, so that the subsequent spinning fiber forming effect is affected; secondly, at the spinning position, the pressure is released instantaneously, so that the fiber shape is not well controlled, and proper constraint is needed; and thirdly, during spinning, the solvent volatilizes, so that unnecessary waste and even environmental pollution are caused, and a recovery system needs to be improved. To overcome these problems, researchers have made a great deal of experimental exploration in succession. CN106574401a discloses a method of flash spinning plexifilamentary strands and sheets having a thickness of less than 12m 2 A BET surface area per gram, an extrusion value of at least 0.9mm/g, wherein the fiber strands comprise predominantly fibers formed from polyethylene having a total crystallinity index of less than 55%, and sheets made therefrom; however, the method does not consider the recovery and reuse of the solvent, so that raw materials are wasted, the cost is increased, and even certain pollution is caused to the environment; CN107740198A discloses a spinning device and a spinning method thereof, wherein a spinning solution is sprayed out from a spinneret to form a fiber plexifilamentary, and an air amplifier is used for carrying out secondary drawing to realize uniform fiber opening. However, the method is mainly focused on the position of a spinning nozzle, and the pressure received from the reaction kettle is subjected to pressure reduction regulation, so that the spinning pressure of a subsequent nozzle is reduced.
Therefore, there is a need to develop a uniform and continuous micro-nanofiber spinning method with simple preparation process, high raw material solvent utilization rate, high spinning speed and excellent performance.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide a uniform and continuous micro-nano fiber supercritical spinning method.
The aim of the invention can be achieved by the following technical scheme:
the invention aims to provide a uniform and continuous micro-nanofiber supercritical spinning method, which comprises the following steps of:
the first step: introducing high-pressure inert gas into the micro-nano fiber supercritical spinning device, conveying spinning solution from a high-pressure chamber to a low-pressure chamber, and primarily reducing the pressure of the spinning solution;
and a second step of: opening a spinning nozzle, spraying spinning solution from the spinning nozzle, solidifying fiber-forming polymer, and forming fiber plexifilamentary under the restraint of the spinning nozzle;
and a third step of: and in the spinning chamber, the solvent which is gasified and diffused is condensed and recovered by utilizing a condensation reflux pipeline, so that the recycling is realized.
Further, the micro-nano fiber supercritical spinning device comprises a spinning chamber, a high-pressure chamber and a low-pressure chamber which are arranged in the spinning chamber, a condensation backflow pipeline which is arranged in the spinning chamber, and a spinning plate which is connected with the low-pressure chamber; and the spinning plate is provided with a spinning nozzle.
Further, the high-pressure inert gas in the first step refers to a common inert gas, and can be one of nitrogen, argon, helium and carbon dioxide, and the pressure of the inert gas is controlled to be 8-14MPa.
Further, the spinning solution in the first step refers to a uniform and stable supercritical fluid spinning solution prepared as required, and the fiber-forming polymer is uniformly dispersed in the mixed solvent and shows supercritical fluid properties under the corresponding high-temperature and high-pressure environment.
Further, the high-pressure chamber in the first step refers to a closed space directly connected with the reaction kettle, and the internal pressure of the high-pressure chamber is kept consistent with the pressure of the reaction kettle, and can be controlled within a range of 8-14MPa.
Further, the low pressure chamber in the first step refers to a closed space tightly connected with the high pressure chamber, and has a unique shape and a corresponding space size, and the pressure range can be maintained at 4-6MPa in order to obtain the pressure reducing function and facilitate the flow of the spinning solution.
Further, the step of transferring the spinning solution from the high pressure chamber to the low pressure chamber means that the pressure of the spinning solution can be reduced by 3-4MPa by pushing the supercritical fluid spinning solution under the pushing of the gas pressure.
Further, the spinneret orifice in the second step refers to a spinneret plate with a unique shape design, and small holes with unique shapes are uniformly distributed on the spinneret orifice.
Further, the number of the holes of the spinneret holes is one selected from 1 hole, 2 holes, 3 holes, 4 holes and 5 holes, and the diameter of the spinneret holes is 0.5-1.5 mm.
Further, the spinning solution in the second step is sprayed out from a spinning nozzle to be sprayed out ultrafast.
Further, the spinning solution in the second step is sprayed out from the spinning nozzle due to the release of instantaneous huge pressure, and the spraying speed is maintained to be about 340m/s.
Further, the fiber plexifilamentary in the second step is the unique plexifilamentary phenomenon in the flashing effect, is a collection of a part of fibers, and is beneficial to enhancing the penetration resistance and barrier property of the later flashing fabric.
Further, the spinning chamber in the third step refers to an integrated space with good tightness, comprises a high-pressure chamber, a low-pressure chamber, a spinning device and the like, is favorable for limiting solvent volatilization and improves solvent recovery efficiency.
Further, the condensation, recovery, gasification and diffusion of the solvent in the third step refers to recovery of the mixed solvent sprayed under high pressure, and full separation and recovery of the mixed solvent are realized by utilizing the principle of sudden drop of different cold air temperatures.
The mechanism of the invention is introduced as follows:
spinning with supercritical fluids is a strong innovation in the spinning field, where a large number of state changes and controls are involved, with stringent requirements on the three-phase transition conditions of the fiber-forming polymer. With the increase of temperature and pressure, the physical properties of the fiber-forming polymer change, and under the condition of reaching specific temperature and pressure, the temperature and pressure at the three-phase junction of the fiber-forming polymer can show a gas-liquid undivided state, namely a supercritical state, and the fiber-forming polymer has lower viscosity, higher density, fluidity and better dissolution performance. Based on the excellent physical properties, the fiber-forming polymer and the solvent are transferred smoothly in the high-pressure chamber and the low-pressure chamber, and the uniformity of the mixture is not influenced by flow.
For the fiber-forming polymer selected in the process, such as high-density polyethylene, the unique physical property is subjected to temperature and pressure change, and the state change is remarkable, so that after spinning at a spinning nozzle, the pressure is released instantaneously and is consistent with the atmospheric pressure, the rapid phase separation of the polymer and the solvent can be realized, and a pure solid polymer plexifilamentary is obtained, and the phase change process is shown in figure 1.
In the invention, a new spinning path is developed, a new spinning method is found for other excellent polymers such as high-density polyethylene, the temperature and pressure of the polymers are controlled, the real-time state of the polymers is further controlled by virtue of the excellent solubility of the main solvent and the auxiliary solvent, the polymers are in a supercritical state from solid state to gas-liquid indiscriminate state and then are sprayed out from a tiny spinning nozzle, the polymers are rapidly solidified, and the solvents are rapidly volatilized, so that fiber-forming polymer plexifilaments are obtained, and the effect is shown in figure 2.
Compared with the prior art, the invention has the following beneficial effects:
1) The uniform and continuous micro-nano fiber supercritical spinning method provided by the technical scheme has wide sources of available spinning raw materials in the spinning process, and can finish the spinning process of most compounds.
2) The uniform and continuous micro-nano fiber supercritical spinning method provided by the technical scheme has simple operation process for the spinning solution obtained by preparation, and can meet the large-scale and rapid spinning requirements.
3) The uniform and continuous micro-nano fiber supercritical spinning method provided by the technical scheme has the advantages that the obtained sample is excellent in puncture resistance and barrier property, the solvent is fully recovered in the production process, and the method is nontoxic and harmless to the environment.
Drawings
FIG. 1 is a three-phase diagram of a supercritical fluid dope.
FIG. 2 is an SEM image of the overall fiber morphology of the micro-nanofibers of example 1 of the present invention.
Detailed Description
The invention will now be described in detail with reference to the drawings and specific examples. Features such as a part model, a material name, a connection structure, a control method and the like which are not explicitly described in the technical scheme are all regarded as common technical features disclosed in the prior art.
The invention relates to a uniform and continuous micro-nano fiber supercritical spinning method, which comprises the following steps:
the first step: introducing high-pressure inert gas into the micro-nano fiber supercritical spinning device, conveying the supercritical fluid spinning solution polymer from a high-pressure chamber to a low-pressure chamber, and primarily reducing the pressure of the spinning solution;
and a second step of: continuously introducing inert gas, opening a spinning nozzle, enabling spinning solution to be sprayed out of the spinning nozzle in an ultra-rapid mode, solidifying fiber-forming polymers, and forming fiber plexifilaments under the constraint of the spinning nozzle;
and a third step of: in the spinning room, a plurality of condensing pipes are used for condensing, recovering and gasifying and diffusing solvents, and recycling is realized completely.
Example 1
The embodiment provides a uniform and continuous micro-nano fiber supercritical spinning method, which comprises the following steps:
the first step: continuously blowing high-pressure inert gas nitrogen before a high-pressure chamber, maintaining the outlet pressure of a gas cylinder at about 9MPa, injecting the prepared high-density polyethylene spinning solution into the high-pressure chamber, and utilizing high pressure to push the flow of the supercritical fluid spinning solution to reach the low-pressure chamber; under the action of the main solvent and the auxiliary solvent, the pressure is generally maintained at about 5MPa, and the preliminary phase separation of the high-density polyethylene and the mixed spinning solution is realized in a low-pressure chamber, so that the preparation is made for the subsequent spinning.
And a second step of: the pneumatic valve is controlled to open the spinning nozzle, the high-density polyethylene supercritical fluid spinning solution is rapidly sprayed out of the spinning nozzle, the speed test reaches 340m/s, the spinning solution pressure is balanced with the atmospheric pressure instantaneously, the high-density polyethylene is separated from the solvent, and the high-density polyethylene fiber plexifilamentary is obtained, as shown in figure 2, the fiber which is not opened is sprayed out of the spinning nozzle, and the fiber has good surface morphology, but the fiber which is not opened is a bundle of fibers, and the fiber diameter is thicker and needs further fiber opening treatment.
And a third step of: and (3) opening a condensation reflux device, condensing and refluxing the main solvent R22 and the auxiliary solvent R114 gasified at the spinning nozzle through a condensation pipe, setting different condensation temperatures, and realizing independent and complete recycling of the two solvents.
Example 2
A uniform and continuous micro-nano fiber supercritical spinning method comprises the following specific steps:
the first step: continuously blowing high-pressure inert gas carbon dioxide in front of a high-pressure chamber, maintaining the outlet pressure of a gas cylinder at about 10MPa, injecting the prepared high-density polyethylene and polypropylene mixed spinning solution into the high-pressure chamber, and utilizing high pressure to push the supercritical fluid spinning solution to flow so as to reach the low-pressure chamber; under the action of the main solvent and the auxiliary solvent, the pressure is correspondingly maintained at about 5.5MPa at the moment, and the primary phase separation of the high-density polyethylene and polypropylene mixed solution and the mixed spinning solution is realized in the low-pressure chamber, so that the preparation is made for the subsequent spinning.
And a second step of: and controlling a pneumatic valve, opening a spinning nozzle, rapidly spraying the high-density polyethylene and polypropylene mixed supercritical fluid spinning solution from the spinning nozzle, and performing speed test to reach 300m/s, wherein the spinning solution pressure is balanced with the atmospheric pressure instantly, and the high-density polyethylene and the polypropylene are separated from a solvent and rapidly solidified to obtain the plexifilamentary fiber bundle with the high-density polyethylene and the polypropylene mixed. And a third step of: and (3) opening a condensation reflux device, condensing and refluxing a main solvent methylene dichloride and an auxiliary solvent 1H-2H-perfluoroethane gasified at a spinning nozzle through a condensation pipe, setting different condensation temperatures, and realizing independent and complete recycling of the two solvents.
Example 3
A uniform and continuous micro-nano fiber supercritical spinning method comprises the following specific steps:
the first step: continuously blowing high-pressure inert gas nitrogen before a high-pressure chamber, maintaining the outlet pressure of a gas cylinder at about 8MPa, injecting the prepared polyvinylidene fluoride spinning solution into the high-pressure chamber, and utilizing high pressure to push the flow of the supercritical fluid spinning solution to reach the low-pressure chamber; under the action of the main solvent and the auxiliary solvent, the pressure is generally maintained at about 5MPa at the moment, and the preliminary phase separation of the polyvinylidene fluoride supercritical fluid spinning solution is realized in a low-pressure chamber, so that the preparation is made for the subsequent spinning.
And a second step of: and controlling a pneumatic valve, opening a spinning nozzle, rapidly spraying the polyvinylidene fluoride supercritical fluid spinning solution from the spinning nozzle, and rapidly solidifying the polyvinylidene fluoride supercritical fluid spinning solution to obtain the polyvinylidene fluoride plexifilamentary fiber bundle, wherein the speed test reaches 340m/s, and the supercritical fluid spinning solution is instantaneously balanced with the atmospheric pressure, so that the polyvinylidene fluoride is separated from the solvent.
And a third step of: and (3) opening a condensation reflux device, condensing and refluxing a main solvent trichloro-monofluoromethane gasified at a spinning nozzle and an auxiliary solvent 1H, 2H-perfluorohexane through a condensation pipe, setting different condensation temperatures, and realizing independent and complete recycling of the two solvents.
The previous description of the embodiments is provided to facilitate a person of ordinary skill in the art in order to make and use the present invention. It will be apparent to those skilled in the art that various modifications can be readily made to these embodiments and the generic principles described herein may be applied to other embodiments without the use of the inventive faculty. Therefore, the present invention is not limited to the above-described embodiments, and those skilled in the art, based on the present disclosure, should make improvements and modifications without departing from the scope of the present invention.
Claims (10)
1. The uniform and continuous micro-nanofiber supercritical spinning method is characterized by comprising the following steps of:
the first step: introducing high-pressure inert gas into the micro-nano fiber supercritical spinning device, conveying spinning solution from a high-pressure chamber to a low-pressure chamber, and primarily reducing the pressure of the spinning solution;
and a second step of: opening a spinning nozzle, spraying spinning solution from the spinning nozzle, solidifying fiber-forming polymer, and forming fiber plexifilamentary under the restraint of the spinning nozzle;
and a third step of: and in the spinning chamber, the solvent which is gasified and diffused is condensed and recovered by utilizing a condensation reflux pipeline, so that the recycling is realized.
2. The method according to claim 1, wherein the high-pressure inert gas in the first step is one selected from nitrogen, argon, helium and carbon dioxide;
the pressure range of the high-pressure inert gas is controlled between 8 and 14MPa.
3. The method of claim 1, wherein the high pressure chamber in the first step is controlled to be in the range of 8-14MPa.
4. A uniform and continuous micro-nano fiber supercritical spinning method according to claim 3, wherein the low pressure chamber in the first step is a closed space tightly connected with the high pressure chamber, and the pressure range is maintained between 4MPa and 6MPa.
5. The method according to claim 4, wherein the spinning solution is fed from the high pressure chamber to the low pressure chamber in the first step to reduce the pressure of the spinning solution to 3-4MPa.
6. The method for supercritical spinning uniform and continuous micro-nano fiber according to claim 1, wherein the spinneret in the second step is a spinneret plate, and the spinneret holes are uniformly distributed on the spinneret plate.
7. The method for supercritical spinning uniform and continuous micro-nano fiber according to claim 6, wherein the number of the spinning holes is one selected from 1 hole, 2 holes, 3 holes, 4 holes and 5 holes, and the diameter of the spinning holes is 0.5-1.5 mm.
8. The method according to claim 1, wherein the jet speed of the spinning solution from the spinning nozzle in the second step is maintained at 340m/s.
9. A uniform, continuous, micro-nanofiber supercritical spinning process according to claim 1, wherein said plexifilamentary filaments in the second step are a collection of fibers.
10. The method according to claim 1, wherein the spinning chamber in the third step is an integrated space with good tightness, and comprises a high-pressure chamber, a low-pressure chamber and a spinning device.
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| CN107097492A (en) * | 2017-04-01 | 2017-08-29 | 东华大学 | Ultralight aeroge heat insulating material with Waterproof Breathable function and preparation method thereof |
| CN108360254A (en) * | 2018-04-25 | 2018-08-03 | 宁波大千纺织品有限公司 | A kind of functionality anti-fatigue health-caring knitting fabric and preparation method thereof |
| CN111691060A (en) * | 2020-06-10 | 2020-09-22 | 东华大学 | High polymer fiber based on instantaneous pressure-release spinning method, and preparation method and application thereof |
| CN111705368A (en) * | 2020-06-10 | 2020-09-25 | 东华大学 | Method for preparing polypropylene fiber aggregate based on instantaneous pressure-release spinning method and application |
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