CN102936764A - Preparation method of polyacrylonitrile-based carbon nanofibers - Google Patents
Preparation method of polyacrylonitrile-based carbon nanofibers Download PDFInfo
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- CN102936764A CN102936764A CN2012104912159A CN201210491215A CN102936764A CN 102936764 A CN102936764 A CN 102936764A CN 2012104912159 A CN2012104912159 A CN 2012104912159A CN 201210491215 A CN201210491215 A CN 201210491215A CN 102936764 A CN102936764 A CN 102936764A
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Abstract
The invention relates to a preparation method of carbon nanofibers and particularly relates to a preparation method of polyacrylonitrile-based carbon nanofibers. The preparation method comprises the following steps: dissolving polyacrylonitrile into a solvent to form a spinning solution, supplying the spinning solution to a spinning die head with a series of spinning holes, and extruding from the spinning holes to form fine spinning solution flow; blowing and extruding the fine spinning solution flow by utilizing one high-speed jet air flow at an included angle being 0-30 degrees, thus refining the fine solution flow and promoting the evaporation of the solvent to form polyacrylonitrile nanofibers, wherein the temperature of the high-speed jet air flow is 20-80 DEG C, and the speed of the high-speed jet air flow is higher than the extruding speed of the fine solution flow by 500-3000 times; and arranging the polyacrylonitrile nanofibers in air atmosphere being 160-300 DEG C to conduct pre-oxidization treatment and conduct carbonization treatment in the nitrogen atmosphere being 900-1800 DEG C to obtain the carbon nanofibers. The preparation method has the advantages of high production efficiency, simple process, uniform diameter distribution of fibers and the like, and is suitable for large-scale production.
Description
Technical field
The present invention relates to a kind of preparation method of carbon nano-fiber, particularly a kind of preparation method of polyacrylonitrile base nano carbon fibre.
Background technology
Carbon fiber is the fibrous material that the phosphorus content that is transformed through a series of heat treatment by organic fibrous material is greater than 90%, there is the performance of a series of excellences such as high specific strength, high ratio modulus, high temperature resistant, corrosion-resistant, endurance, radioresistance, conduction, heat transfer, damping, noise reduction and relative density be little, belong to typical high-performance fiber.
Carbon nano-fiber is as a kind of Novel Carbon Nanomaterials, it is the quasi-one-dimensional material between CNT (carbon nano-tube) and common carbon fibers, having the material with carbon element feature, to have again a textile fabric soft, there is excellent Physical and mechanical properties and chemical stability, as large as specific area, mechanical strength and Young's modulus are high, good conductivity, thermal conductivity and excellent heat stability etc.Along with going deep into that people study the carbon nano-fiber excellent properties, its Application Areas is also more and more extensive, can be widely used in the fields such as Aero-Space, efficient adsorption material, reinforcing material, energy environment.
At present, the method for preparing carbon nano-fiber is mainly vapor growth method, as Chinese invention patent CN1292984C, and CN1172846C and CN1061706C etc.The materials such as carbon black easily appear in the method in process of production, need to further purify, and production cost is high, and this method can only obtain length be several microns to nearly hundred micron/nano carbon fibers, be difficult to bring into play the advantage of carbon nano-fiber.In the recent period some research papers and patent have proposed to utilize the method for electrostatic spinning to prepare the method for carbon nano-fiber, to be the presoma that utilizes carbon fiber carry out spinning as the solution of polyacrylonitrile to the method, obtain polyacrylonitrile nanofiber, then carry out pre-oxidation, carbonization treatment, obtain carbon nano-fiber.The method can obtain continuous carbon nano-fiber, and fiber is pure, has certain advantage.But correlative study at present is mainly based on laboratory equipment research, rare large-scale production equipment, spinning efficiency low (spinning speed is generally the 0.5-3mL/h/ spinneret orifice).
Summary of the invention
For the deficiencies in the prior art; the technical problem that quasi-solution of the present invention is determined is; provide a kind of solution jet spinning method of utilizing to prepare polyacrylonitrile nanofiber; make again the method for carbon nano-fiber through pre-oxidation, carbonization treatment; this preparation method has the advantages such as production efficiency is high, technique is simple, distribution of fiber diameters is even, is suitable for large-scale production.
A kind of preparation method of polyacrylonitrile base nano carbon fibre, is characterized in that, comprises the following steps:
(1) preparation of spinning solution: polyacrylonitrile is dissolved in solvent to the spinning solution that the formation mass concentration is the 6-20% homogeneous;
Described polyacrylonitrile is polyacrylonitrile homopolymers or copolymer, and viscosity average molecular weigh is 8-30 ten thousand, and wherein the acrylonitrile segment accounts for more than 85%, and all the other are methyl acrylate, acrylic acid, acrylamide, itaconic acid or Sodium styrene sulfonate;
Described solvent is one or both and the above mixture in DMF, DMA and dimethyl sulfoxide (DMSO);
(2) solution jet spinning method prepares polyacrylonitrile nanofiber: spinning solution is fed to a spray silk die head with the speed of 5-30mL/h/ spinneret orifice, spinning solution is extruded from spinneret orifice and formed the solution thread, utilize at least one high velocity air with the winding-up of the jet angle with spinning solution thread 0-30 degree spinning solution thread simultaneously, the slenderizing of realization to the spinning solution thread, accelerate solvent evaporates in spinning solution, the polyacrylonitrile nanofiber that the formation diameter is 10nm~1 μ m simultaneously;
Described solution jet spinning method is to utilize high velocity air to extrude thread to spinning solution carry out ultra-fine stretching and promote solvent evaporates and obtain the spinning process of ultra-fine even nanofiber, the processing step of this spinning process is " a kind of preparation method of polymeric nano-micro fiber non-woven fabric " who announces in Chinese invention patent ZL201110041792.3, the basic principle of the method is to utilize high velocity air to extrude thread to solution to be jetted, impel the division of solution thread to produce jet, in the volatilization of fluidic operation Solvent, be solidified into fiber:
The temperature of described high velocity jet air-flow is 20-80 ℃, and air velocity higher than spinning solution thread speed 500-3000 doubly.
(3) pre-oxidation treatment: described polyacrylonitrile nanofiber is carried out in air atmosphere to pre-oxidation and obtain the pre-oxidation nanofiber, Pre oxidation is 160~300 ℃, and preoxidation time is 2-3h;
Also comprise simultaneously polyacrylonitrile nanofiber is carried out to stretch processing in described pre-oxidation treatment, draw ratio is 1.3-5 times:
(4) carbonization treatment: described pre-oxidation nanofiber is carried out to carbonization in nitrogen atmosphere and obtain carbon nano-fiber, carburizing temperature is 900-1800 ℃, and carbonization time is 0.5-3h.
The diameter of the polyacrylonitrile base nano carbon fibre made is 10nm-1 μ m.
Nanofiber prepared by the present invention is the polyacrylonitrile nanofiber by the solution jet spinning is made, carry out again pre-oxidation treatment, carbonization treatment and make, vapor growth method, electrostatic spinning process have been replaced, the fibre diameter fine distinction is evenly distributed, and generally at 10nm-1 μ m, representative value is 100nm-500nm, technical process is simple, energy consumption is low, with short production cycle, the productive rate advantages of higher.Prepared carbon nano-fiber have fibre diameter thin, be evenly distributed, crystal habit is good, thermal stability is excellent, can be widely used in the fields such as Aero-Space, efficient adsorption material, reinforcing material, energy environment.
The accompanying drawing explanation
The polyacrylonitrile nanofiber preparation facilities schematic diagram that Fig. 1 is the embodiment of the present invention:
In figure: 1, spinning solution storage tank; 2, spray silk die head; 21, spinneret orifice; 22, spray silk air gap; 3, hothouse; 4, collect lace curtaining; 5, pressure controller; 6, vacuum chamber; 7, air exhauster.
The ESEM picture of the carbon nano-fiber that Fig. 2 is the embodiment of the present invention 1.
The diameter distribution map that Fig. 3 is carbon fiber in Fig. 2.
The specific embodiment
Further illustrate the present invention below in conjunction with embodiment.
The preparation method of a kind of carbon nano-fiber disclosed by the invention (is called for short the preparation method, referring to Fig. 1), its processing step is as follows: polyacrylonitrile is dissolved in solvent and forms spinning solution, again spinning solution is fed to the spray silk die head 2 that contains a series of spinneret orifices through feeding mechanism, spinning solution is extruded from the spinneret orifice 21 of spray silk die head 2, formed the spinning solution thread; Simultaneously at least one high velocity jet air-flow enters a spray silk die head 2, and blows to extruding spinning solution thread via the air gap 12 of spray silk die head 2 with the jet angle of 0-30 degree; The high velocity jet air-flow is realized the slenderizing to described spinning solution thread, accelerates the solvent evaporates in spinning solution simultaneously, forms polyacrylonitrile nanofiber; Polyacrylonitrile nanofiber is placed in to oxidation furnace pre-oxidation treatment under oxygen atmosphere, and Pre oxidation is 160-300 ℃, and preoxidation time is 2-3h; The pre-oxidation nanofiber is carried out in nitrogen atmosphere to carbonization and obtain carbon nano-fiber, carburizing temperature is 900-1800 ℃, and heating rate is 1-15 ℃/min, and the insulation processing time is 0.5-3h.
Polyacrylonitrile of the present invention is polyacrylonitrile homopolymers or copolymer, and molecular weight is 8-30 ten thousand, and wherein the acrylonitrile segment accounts for more than 85%, and all the other are methyl acrylate, acrylic acid, acrylamide, itaconic acid or Sodium styrene sulfonate.
Described solvent is at least one in DMF, DMA or dimethyl sulfoxide (DMSO), and while adopting the multi-solvents co-mixing system, the mixed proportion of various solvents is circumscribed not.
The temperature of described high velocity jet air-flow is 20-80 ℃, and than the high 500-3000 of the extruded velocity of spinning solution thread doubly, the injection angle of high velocity jet air-flow and spinning solution thread is 0-30 to the jet velocity of high velocity jet air-flow
.。
For improving the mechanical property of carbon nano-fiber, further feature of the present invention is, in the pre-oxidation treatment process, polyacrylonitrile nanofiber carried out to stretch processing, draw ratio be 1.3-5 doubly.
The present invention does not address part and is applicable to prior art.
Below provide specific embodiments of the invention, but the claim protection domain of patent application is not subject to the restriction of specific embodiment.
Embodiment 1.
(1) preparation of spinning solution: the polyacrylonitrile of viscosity average molecular weigh 90,000 is dissolved in DMF with the ratio of mass fraction 12%, stir until mix, make spinning solution;
(2) solution jet spinning method prepares polyacrylonitrile nanofiber: spinning solution is fed to a spray silk die head 2 through measuring pump with the speed of 12mL/h/ spinneret orifice, makes spinning solution extrude and form the spinning solution thread from the spinneret orifice 21 of spray silk die head 2; The high velocity jet air-flow that is simultaneously 40 ℃ by two bursts of temperature blows to extruding spinning solution thread via air gap 12 with the jet angle of 30 °, air velocity is controlled 800 times for solution thread extruded velocity, and high velocity air stretching solution thread also promotes solvent evaporates to make it to form polyacrylonitrile nanofiber;
(3) pre-oxidation treatment: prepared polyacrylonitrile nanofiber is placed in to pre-oxidation furnace, processes 2h, obtain pre-oxidized fibers for 190 ℃;
(4) carbonization treatment: pre-oxidized fibers is carried out in nitrogen atmosphere to carbonization and obtain carbon nano-fiber, carburizing temperature is 1000 ℃, and heating rate is 8 ℃/min, and the insulation processing time is 2h, obtains carbon nano-fiber.
As shown in Figure 2, as shown in Figure 3, its diameter distributes mainly at 100-340nm its diameter distribution map the ESEM of the carbon nano-fiber made as seen, and average diameter is 170nm.
(1) preparation of spinning solution: the polyacrylonitrile of viscosity average molecular weigh 120,000 is dissolved in DMA with the ratio of mass fraction 10%, stir until mix, make spinning solution;
(2) solution jet spinning method prepares polyacrylonitrile nanofiber: spinning solution is fed to a spray silk die head 2 through measuring pump with the speed of 22mL/h/ spinneret orifice, makes spinning solution extrude and form the spinning solution thread from the spinneret orifice 21 of spray silk die head 2; The high velocity jet air-flow that is simultaneously 50 ℃ by two bursts of temperature blows to extruding spinning solution thread via air gap 12 with the jet angle of 15 °, air velocity is controlled 1200 times for solution thread extruded velocity, and high velocity air stretching solution thread also promotes solvent evaporates to make it to form polyacrylonitrile nanofiber;
(3) pre-oxidation treatment: prepared polyacrylonitrile nanofiber is placed in to pre-oxidation furnace, processes 3h, obtain pre-oxidized fibers for 200 ℃;
(4) carbonization treatment: pre-oxidized fibers is carried out in nitrogen atmosphere to carbonization and obtain carbon nano-fiber, carburizing temperature is 1100 ℃, and heating rate is 10 ℃/min, and the insulation processing time is 2h, obtains carbon nano-fiber.
(1) preparation of spinning solution: by the polyacrylonitrile of viscosity average molecular weigh 280,000 with the ratio of mass fraction 8% dissolve in DMA/dimethyl sulfoxide (DMSO) (1: 1, v/v) in, stir until mix, make spinning solution;
(2) solution jet spinning method prepares polyacrylonitrile nanofiber: spinning solution is fed to a spray silk die head 2 through measuring pump with the speed of 30mL/h/ spinneret orifice, makes spinning solution extrude and form the spinning solution thread from the spinneret orifice 21 of spray silk die head 2; The high velocity jet air-flow that is simultaneously 50 ℃ by two bursts of temperature blows to extruding spinning solution thread via air gap 12 with the jet angle of 8 °, air velocity is controlled 2200 times for solution thread extruded velocity, and high velocity air stretching solution thread also promotes solvent evaporates to make it to form polyacrylonitrile nanofiber;
(3) pre-oxidation treatment: prepared polyacrylonitrile nanofiber is placed in to pre-oxidation furnace, carries out tension draft, drafting multiple is 2.5 times, processes 3h, obtains pre-oxidized fibers for 220 ℃;
(4) carbonization treatment: pre-oxidized fibers is carried out in nitrogen atmosphere to carbonization and obtain carbon nano-fiber, carburizing temperature is 1800 ℃, and heating rate is 10 ℃/min, and the insulation processing time is 3h, obtains carbon nano-fiber.
Claims (5)
1. the preparation method of a polyacrylonitrile base nano carbon fibre, is characterized in that, comprises the following steps:
(1) preparation of spinning solution: polyacrylonitrile is dissolved in solvent to the spinning solution that the formation mass concentration is the 6-20% homogeneous;
(2) solution jet spinning method prepares polyacrylonitrile nanofiber: spinning solution is fed to a spray silk die head with the speed of 5-30mL/h/ spinneret orifice, spinning solution is extruded from spinneret orifice and formed the solution thread, utilize at least one high velocity air with the winding-up of the jet angle with spinning solution thread 0-30 degree spinning solution thread simultaneously, the slenderizing of realization to the spinning solution thread, accelerate solvent evaporates in spinning solution, the polyacrylonitrile nanofiber that the formation diameter is 10nm~1 μ m simultaneously;
(3) pre-oxidation treatment: described polyacrylonitrile nanofiber is carried out in air atmosphere to pre-oxidation and obtain the pre-oxidation nanofiber, Pre oxidation is 160~300 ℃, and preoxidation time is 2-3h;
(4) carbonization treatment: described pre-oxidation nanofiber is carried out to carbonization in nitrogen atmosphere and obtain carbon nano-fiber, carburizing temperature is 900-1800 ℃, and carbonization time is 0.5-3h.
2. the preparation method of polyacrylonitrile base nano carbon fibre according to claim 1, it is characterized in that, in described step (1), polyacrylonitrile is polyacrylonitrile homopolymers or copolymer, viscosity average molecular weigh is 8-30 ten thousand, wherein the acrylonitrile segment accounts for more than 85%, and all the other are methyl acrylate, acrylic acid, acrylamide, itaconic acid or Sodium styrene sulfonate.
3. the preparation method of polyacrylonitrile base nano carbon fibre according to claim 1, it is characterized in that, solvent in described step (1) is one or both and the above mixture in DMF, DMA and dimethyl sulfoxide (DMSO).
4. the preparation method of polyacrylonitrile base nano carbon fibre according to claim 1, is characterized in that, the temperature of described step (2) high speed jet-stream wind is 20-80 ℃, and air velocity higher than spinning solution thread speed 500-3000 doubly.
5. the preparation method of polyacrylonitrile base nano carbon fibre according to claim 1, is characterized in that, in described pre-oxidation treatment, also comprises simultaneously polyacrylonitrile nanofiber is carried out to stretch processing, and draw ratio is 1.3-5 times.
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