CN101748560B - Spinning method of electrostatically spun composite material of multiple nano level holes - Google Patents
Spinning method of electrostatically spun composite material of multiple nano level holes Download PDFInfo
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- CN101748560B CN101748560B CN2009102322969A CN200910232296A CN101748560B CN 101748560 B CN101748560 B CN 101748560B CN 2009102322969 A CN2009102322969 A CN 2009102322969A CN 200910232296 A CN200910232296 A CN 200910232296A CN 101748560 B CN101748560 B CN 101748560B
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Abstract
The present invention relates to a spinning method of a composite material, particularly to a spinning method of an electrostatically spun composite material of multiple nano level holes. The method comprises the following steps: (1) uniform spinning solution is prepared by dissolving a polymer in a solvent; (2) short fibers are orderly paved on an electrostatic spinning receiving plate to form an ordered short fiber layer; (3) spinning solution is added to a syringe of an electrostatic spinning device, the spinning solution is squeezed out under the control of a micro injection pump, and electrostatic spinning is carried out after the syringe spout is connected with a high voltage positive pole and the receiving plate is connected with a negative pole. As the ordered short fiber layer is paved on the electrostatic spinning receiving plate, the composite material of multiple nano level holes can be conveniently and simply spun. The composite material combines the super specific surface area of nano fibers and the unique style and performance of the short fibers. The composite material has boundless application prospects, and is an important discovery in the material field.
Description
Technical field
The present invention relates to a kind of spinning method of composite, especially a kind of spinning method of nanometer porous electrostatically spun composite material.
Background technology
Electrostatic spinning technique (Anton Formhals; 1930US1975504; J Sha Luopuaike 2005, thus CN1849418) be to make the spining technology of polymer fiber by between polymer solution jetting device and dash receiver, applying electric field.It is the important method of making the 1-1000nm superfine fibre that static spins.This method at first with on polymer solution or the molten mass band several thousand to volt static up to ten thousand, polymer is accelerated at charged capillary conical point.When electric field was enough big, polymer can overcome surface tension and form the injection thread.Thread is solvent evaporation, polymer cure in course of injection, finally is attracted on the receiving system, forms the fibrofelt of similar non-weaving cloth shape.
The staple fibre that electrostatic spinning technique and traditional spinning process is required combines, thereby can be basic unit with the electrostatic spinning nano fiber by the spinning of additional fibre layers on dash receiver, staple fibre spins nanometer porous composite for the static that strengthens body, and this composite can be with the superhigh specific surface area characteristics of nanofiber and unique wearability perfect adaptation of staple fibre.In the electrostatic spinning technique spinning process, nanofiber is owing to be subjected to the high pressure effect, be adsorbed on the dash receiver that is connected in electrode one end, thereby can pass the space between staple fibre and stick on the recipient, and staple fibre is coated in the nano fibrous membrane, thereby form the composite that has nanoscale hole, porous along with gathering of nanofiber.
This composite has improved the brute force of original nano fibrous membrane greatly because of comprising staple fibre as strengthening body; The inner space of composite has been expanded in the adding of staple fibre, thereby air content significantly increases the thermal property that has strengthened nano-fiber composite film.
Summary of the invention
The spinning method that the purpose of this invention is to provide a kind of nanometer porous electrostatically spun composite material can prepare and has nanometer porous composite.
According to technical scheme provided by the invention, the spinning method of described nanometer porous electrostatically spun composite material comprises the following steps:
(1), polymer dissolution is made the spinning solution of homogeneous in solvent;
(2), with ordered short fiber be laid in static and spin and form ordered short fiber layer on the dash receiver;
(3), spinning solution is joined in the syringe of electrostatic spinning device, extruded by micro-injection pump control, the syringe spout connects high-voltage positive electrode, and dash receiver connects negative pole, carries out electrostatic spinning.
The thickness of described ordered short fiber layer is 1～10mm, adopts the staple fibre carded sliver or ripe even lay.Described staple fibre is cotton fiber or wool fibre or various staple fibre; The length of described staple fibre is 38～121mm.
Described solvent is a kind of material in water, carrene, dimethyl formamide, dimethylacetylamide, metacresol, sulfuric acid, dimethyl formamide, formic acid, acetate, propionic acid, isopropyl alcohol, acetone and the hexafluoroisopropanol.
Described polymer is a kind of material in polyethylene glycol, polyvinyl alcohol, polyacrylonitrile, PLA, acetate fiber, bamboo fibre, silk fibroin or the polyurethane elastomer.
Electrostatic spinning parameter in the described step (3) is voltage 5～30kV; The speed of micro-injection pump is 0.1～5.0 milliliter/hour; 18～30 ℃ of spinning environment temperatures; The spinning envionmental humidity is 40～70%RH; Distance between dash receiver and the syringe spout is 5.0～30.0 centimetres.
Utilizing the diameter of the electrostatically spun composite material that described spinning method makes is 1～1000nm.
A kind of electrostatic spinning device of electrostatically spun composite material is to comprise propulsion plant, syringe, dash receiver, high-voltage device, the orderly layer of short fiber; Described propulsion plant is arranged on the syringe, and the syringe spout connects high-voltage anode, and dash receiver connects negative pole, the positive orderly layer of short fiber of laying of dash receiver; At the dash receiver upper and lower side transmission device is installed.
The present invention is because at the static orderly layer of short fiber that spun on the dash receiver lay, and can have nanometer porous composite by convenient and simple spinning, this composite combines the individual style and the performance of the superhigh specific surface area and the staple fibre of nanofiber, application prospect is unlimited, will be an important discovery of material circle.
Description of drawings
Fig. 1 is an electrostatic spinning device.
The specific embodiment
The invention will be further described below in conjunction with concrete drawings and Examples.
Use electrostatic spinning device to prepare electrostatically spun composite material among the present invention, electrostatic spinning device comprises propulsion plant 1, syringe 2, syringe needle 3, dash receiver 4, short fiber layer 5, high pressure generator 6 in order.Described propulsion plant 1 is arranged on the syringe 2, and syringe needle 3 connects high-voltage anode, and dash receiver 4 connects negative pole, the dash receiver 4 positive short fiber layers 5 in order of laying.
Embodiment one: the spinning method of nanometer porous electrostatically spun composite material
With acetone: dimethylacetylamide is made into the homogeneous solvent by 2: 1 volume ratio; molecular weight distribution be 30000, acetyl turns to 39.8% cellulose diacetate and is dissolved in the spinning solution that makes homogeneous in this solvent, the cellulose diacetate mass fraction is 11% in the spinning solution.With length is that the diacetate fiber of 121mm is laid in static in an orderly manner and spins the orderly layer of the short fiber that forms 10mm on the dash receiver; Spinning solution is joined in the syringe of electrostatic spinning device, extruded by micro-injection pump control, the syringe spout connects high-voltage anode, and dash receiver connects negative pole, carries out electrostatic spinning.Electrostatic spinning voltage is 20kV, and the speed of micro-injection pump is 0.8 milliliter/hour, 25 ℃ of spinning environment temperatures, and the spinning envionmental humidity is 50%RH, the distance between dash receiver and the syringe spout is 12.0 centimetres; The average diameter of the electrostatically spun composite material that makes is 800nm.
Embodiment two: the spinning method of nanometer porous electrostatically spun composite material
With relative molecular mass is that 75000 polyacrylonitrile is dissolved in the spinning solution that makes homogeneous in the dimethylacetylamide, and the mass fraction of polyacrylonitrile is 10% in the solution; With length is that the cotton fiber of 38mm is laid in static in an orderly manner and spins the orderly layer of the short fiber that forms 5mm on the dash receiver; Spinning solution is joined in the syringe of electrostatic spinning device, extruded by micro-injection pump control, the syringe spout connects high-voltage anode, and dash receiver connects negative pole, carries out electrostatic spinning.Electrostatic spinning voltage is 30kV, and the speed of micro-injection pump is 0.5 milliliter/hour, 28 ℃ of spinning environment temperatures, and the spinning envionmental humidity is 50%RH, the distance between dash receiver and the syringe spout is 11.5 centimetres.
Embodiment three: the spinning method of nanometer porous electrostatically spun composite material
With mean molecule quantity is that 10000 PLA is dissolved in the spinning solution that makes homogeneous in the carrene, and the mass fraction of PLA is 8% in the solution; With length is that the wool fibre of 60mm is laid in static in an orderly manner and spins the orderly layer of the short fiber that forms 5mm on the dash receiver; Spinning solution is joined in the syringe of electrostatic spinning device, extruded by micro-injection pump control, the syringe spout connects high-voltage anode, and dash receiver connects negative pole, carries out electrostatic spinning.Electrostatic spinning voltage is 15kV, and the speed of micro-injection pump is 0.8 milliliter/hour, 25 ℃ of spinning environment temperatures, and the spinning envionmental humidity is 65%RH, the distance between dash receiver and the syringe spout is 20 centimetres; The diameter of the electrostatically spun composite material that makes is 1000nm.
Claims (1)
1. the spinning method of a nanometer porous electrostatically spun composite material is characterized in that: comprise the following steps:
(1), polymer dissolution is made the spinning solution of homogeneous in solvent;
(2), with ordered short fiber be laid in static and spin and form ordered short fiber layer on the dash receiver;
(3), spinning solution is joined in the syringe of electrostatic spinning device, extruded by micro-injection pump control, the syringe spout connects the positive pole of high voltage source, and dash receiver connects the negative pole of high voltage source, carries out electrostatic spinning;
The thickness of described ordered short fiber layer is 1～10mm;
Described staple fibre is cotton fiber or wool fibre or various staple fibre; The length of described staple fibre is 38～121mm;
Described solvent is a kind of material in water, carrene, dimethyl formamide, dimethylacetylamide, metacresol, sulfuric acid, dimethyl formamide, formic acid, acetate, propionic acid, isopropyl alcohol, acetone and the hexafluoroisopropanol;
Described polymer is a kind of material in polyethylene glycol, polyvinyl alcohol, polyacrylonitrile, PLA, cellulose acetate, bamboo cellulose, silk fibroin or the polyurethane elastomer;
Electrostatic spinning parameter in the described step (3) is voltage 5～30kV; The speed of micro-injection pump is 0.1～5.0 milliliter/hour; 18～30 ℃ of spinning environment temperatures; The spinning envionmental humidity is 40～65%RH; Distance between dash receiver and the syringe spout is 5.0～30.0 centimetres.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN2009102322969A CN101748560B (en) | 2009-12-11 | 2009-12-11 | Spinning method of electrostatically spun composite material of multiple nano level holes |
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| CN2009102322969A CN101748560B (en) | 2009-12-11 | 2009-12-11 | Spinning method of electrostatically spun composite material of multiple nano level holes |
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| CN101748560A CN101748560A (en) | 2010-06-23 |
| CN101748560B true CN101748560B (en) | 2011-11-02 |
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Families Citing this family (11)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102268745B (en) * | 2011-06-17 | 2013-02-20 | 北京化工大学常州先进材料研究院 | Method for preparing porous polyacrylonitrile (PAN) nano fibres by electrospinning method |
| CN102920067A (en) * | 2012-06-07 | 2013-02-13 | 江南大学 | Preparation method of nanofiber sandwich type protective facial mask |
| CN102912502B (en) * | 2012-11-01 | 2015-02-11 | 江南大学 | Device and method for spinning nanofiber and filament composite yarns |
| CN103225120B (en) * | 2013-03-05 | 2016-08-31 | 长春理工大学 | A kind of two bursts of parallel nanoribbon bundle of magneto-optic double-function and preparation method thereof |
| CN103225121B (en) * | 2013-03-05 | 2016-08-10 | 长春理工大学 | Magnetic up-conversion luminescence dual-functional coaxial composite nanofiber and preparation method thereof |
| CN103243481B (en) * | 2013-05-20 | 2016-06-08 | 东华大学 | A kind of electrospinning process prepared containing micro-nano ball fiber |
| CN103394334B (en) * | 2013-07-11 | 2015-07-08 | 东华大学 | Preparation method of aminated nanofiber membrane with high specific surface area |
| WO2015046637A1 (en) * | 2013-09-25 | 2015-04-02 | 도레이첨단소재 주식회사 | Polylactic acid blended non-woven fabric having improved flexibility and method for preparing same |
| CN104213331A (en) * | 2014-09-12 | 2014-12-17 | 天津工业大学 | Preparation method of electrostatic spinning polylactic acid nano-pore fiber membrane |
| CN111826728B (en) * | 2020-07-03 | 2022-05-06 | 东华大学 | Self-curling electrostatic spinning micro-nanofiber with wool fibers as receiving substrate |
| CN112030246A (en) * | 2020-09-30 | 2020-12-04 | 松山湖材料实验室 | Electrostatic spinning device and system |
Citations (4)
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| CN101078134A (en) * | 2007-06-27 | 2007-11-28 | 东华大学 | Preparation of natural material/polymer material coaxial electrostatic spinning nano fibre |
| CN100362148C (en) * | 2006-04-21 | 2008-01-16 | 东南大学 | Preparing low density porous tin dioxide nano fiber laser target material by electro-static spinning method |
| CN101560718A (en) * | 2009-05-22 | 2009-10-21 | 东华大学 | Method for preparing functional nano fibrous membrane by multi-component consolute single-step method |
| CN201358360Y (en) * | 2009-02-19 | 2009-12-09 | 浙江大学 | Multi-nozzle spherical surface film-formation electrostatic spinning film-making device of hollow circular-ring pipelines |
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- 2009-12-11 CN CN2009102322969A patent/CN101748560B/en not_active Expired - Fee Related
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100362148C (en) * | 2006-04-21 | 2008-01-16 | 东南大学 | Preparing low density porous tin dioxide nano fiber laser target material by electro-static spinning method |
| CN101078134A (en) * | 2007-06-27 | 2007-11-28 | 东华大学 | Preparation of natural material/polymer material coaxial electrostatic spinning nano fibre |
| CN201358360Y (en) * | 2009-02-19 | 2009-12-09 | 浙江大学 | Multi-nozzle spherical surface film-formation electrostatic spinning film-making device of hollow circular-ring pipelines |
| CN101560718A (en) * | 2009-05-22 | 2009-10-21 | 东华大学 | Method for preparing functional nano fibrous membrane by multi-component consolute single-step method |
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Assignee: Wujiang Hantong Textile Co., Ltd. Assignor: Jiangnan University Contract record no.: 2012320010141 Denomination of invention: Spinning method of electrostatically spun composite material of multiple nano level holes Granted publication date: 20111102 License type: Exclusive License Open date: 20100623 Record date: 20120613 |
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Effective date of registration: 20171127 Address after: Ying Town Industrial Park in Xinxiang County of Henan province Zhao 453000 Patentee after: Henan Hua'ou purification equipment limited company Address before: 214122 Jiangsu Province, Wuxi City Lake Road No. 1800, Jiangnan University Patentee before: Jiangnan University |
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