CN114250630B - Pyrolytic carbonyl iron coating carbon fiber and preparation method thereof - Google Patents
Pyrolytic carbonyl iron coating carbon fiber and preparation method thereof Download PDFInfo
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- CN114250630B CN114250630B CN202011007526.4A CN202011007526A CN114250630B CN 114250630 B CN114250630 B CN 114250630B CN 202011007526 A CN202011007526 A CN 202011007526A CN 114250630 B CN114250630 B CN 114250630B
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/83—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with metals; with metal-generating compounds, e.g. metal carbonyls; Reduction of metal compounds on textiles
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
- D06M2101/40—Fibres of carbon
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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
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
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Abstract
The invention belongs to the technical field of wave-absorbing material preparation, and discloses a pyrolytic carbonyl iron coated carbon fiber and a preparation method thereof. The magnetic saturation intensity of the coated carbon fiber finished product is more than 15emu/g, the magnetic property is strong, the weight is light, and the coated carbon fiber finished product can be added into foam, honeycomb or wave-absorbing coating to play the roles of absorbing and enhancing.
Description
Technical Field
The invention belongs to the technical field of preparation of wave-absorbing materials, and particularly relates to pyrolytic carbonyl iron-coated carbon fibers and a preparation method thereof.
Background
The absorbing material for radar stealth is widely applied to stealth defense systems of military platforms such as ocean, land and the like, and can effectively reduce the radar reflection area of a target, so that the target is more difficult to find. In order to obtain a microwave absorbing material excellent in performance, combining magnetic loss with a dielectric material is an effective method for improving electromagnetic wave absorption characteristics. The carbon fiber has higher specific strength and specific modulus, and also has excellent performances in conduction, reflection and absorption, electromagnetic shielding and electron antagonism, and is an ideal wave-absorbing material with dual functions of mechanical bearing and reducing radar wave reflection cross section. At present, the wave absorbing performance of the carbonaceous material is improved by surface modification of carbon fibers, carbon nanotubes and graphene, coating of various magnetic particles and the like, and the advantages and disadvantages of respective dielectric loss and magnetic loss can be effectively fused when Fe, co and Ni metal-based magnetic materials are combined with the carbonaceous wave absorbing material, so that the light wave absorbing composite material with wide absorption frequency band is prepared. However, currently, the magnetic coating is generally prepared on the carbon fiber by adopting methods such as electroplating, electroless plating, reduction and the like. Disadvantages of these methods are: 1. oil stains on the surface of the carbon fiber are difficult to clean, so that the particle load is not firm; 2. the electroplating method has high requirements on equipment and has certain pollution to the environment.
Disclosure of Invention
Aiming at the defects and shortcomings of the prior art that the carbon fiber has too high dielectric constant and poor impedance matching property, the invention aims to provide the pyrolytic carbonyl iron coating carbon fiber with good wave absorbing performance in a very wide frequency band range and a preparation method thereof,
the invention discloses a preparation method of pyrolytic carbonyl iron-coated carbon fiber, which comprises the following steps:
dispersing the pretreated carbon fiber in an organic solvent to obtain a carbon fiber-containing solution, then adding carbonyl iron to obtain slurry, carrying out pyrolysis reaction under a protective atmosphere, carrying out solid-liquid separation, washing the obtained solid phase, soaking the solid phase in a coupling agent-containing mixed solution, and drying to obtain the coated carbon fiber.
In the preferred scheme, the carbon fiber is cut into 30-40 cm, then is subjected to heat treatment at 400-600 ℃ for 40-50 min, and is cut into 2-5 mm; and (5) drying to obtain the pretreated carbon fiber.
Further preferably, the drying temperature is 75-85 ℃ and the drying time is 10-12 h.
In the actual operation process, after the carbon fiber is cut into 30-40 cm, knotting the two ends of the carbon fiber, and then placing the knotted fiber into a tube furnace for heat treatment.
Preferably, the organic solvent is xylene.
In a preferred scheme, the mass ratio of the carbon fiber to the dimethylbenzene is 0.5:9-15.
In a preferred scheme, the carbon fibers are dispersed in an organic solvent under stirring, the stirring speed is 800-2000 rpm, and the stirring time is 10-30 min.
The carbon fiber can be fully dispersed in the organic solvent by stirring at high speed, so that the uniformity of the coating is ensured.
In the actual operation process, the high-speed stirring of the dispersing machine is adopted to realize the dispersion of the carbon fiber in the organic solvent.
In a preferred scheme, the mass ratio of the carbon fiber to carbonyl iron is 0.5:1-3. The hydroxyl iron is controlled in the range, so that the whole carbon fiber is uniformly coated with the iron coating, and the hydroxyl can be completely decomposed.
Preferably, the pyrolysis reaction is performed by the following steps: heating to 90-110 ℃ from normal temperature for 40-80 min, heating to 120-140 ℃ for 300-420 min, heating to 150-160 ℃ for 2000-3000 min, preserving heat for 2000-3000 min at 150-160 ℃, and cooling to normal temperature for 60-180 min.
The inventors found that controlling the pyrolysis process within the above-described preferred range allows the carbon fibers to be uniformly coated with the iron coating, while if the process is not followed, such as too high an early temperature and too fast a temperature rise, the hydroxy iron will decompose too fast and the micro-nano will accumulate, resulting in uneven coating.
In a preferred scheme, the pyrolysis reaction is carried out under stirring, wherein the stirring mode is that the stirring is carried out for 1-2 min at a rotating speed of 30-60 r/min, and then the stirring is carried out for 1-5 min at a rotating speed of 20-30 r/min every 1-2 h. In the intermittent stirring mode adopted by the invention, the inventor finds that the final coating can be uniform by adopting the stirring mode, and if continuous stirring or too high stirring speed is adopted, carbon fibers are agglomerated, so that the coating is nonuniform.
In a preferred scheme, the obtained solid phase is washed with absolute ethanol for more than 3 times.
In a preferred scheme, in the mixed solution containing the coupling agent, the coupling agent is KH550, and the mass fraction of the coupling agent is 0.3-0.6 wt%.
In a preferred scheme, the solvent in the mixed solution containing the coupling agent is ethanol water solution, and the mass fraction of ethanol in the ethanol water solution is 90-95 wt%.
Preferably, the soaking is carried out under stirring for 30-60 min
In a preferred scheme, the drying process is that the materials are tedded for 10 to 12 hours at room temperature and then dried for 10 to 20 hours at the temperature of 40 to 60 ℃.
The invention also provides the pyrolytic carbonyl iron-coated carbon fiber prepared by the preparation method.
And the surface of the coated carbon fiber is uniformly coated with the micro-nano iron coating.
Compared with the prior art, the invention has the following advantages and effects compared with the prior art:
(1) The invention adopts a high-temperature pyrolysis reaction method, can use simple equipment to prepare the carbon fiber with the surface coated with the magnetic micro-nano iron coating, can effectively and conveniently control the content of the iron coating on the surface of the carbon fiber through the adjustment of reaction time, and finally can regulate and control the wave absorbing performance of the magnetic modified carbon fiber.
(2) The preparation method of the carbon fiber surface coated magnetic iron coating is simple, enriches the design and preparation science of the wave-absorbing material, and has important guiding significance for the research and development of novel wave-absorbing materials.
(3) According to the invention, the magnetic iron-containing coating is uniformly introduced and coated on the surface of the carbon fiber, and the modified carbon fiber has two electromagnetic wave loss mechanisms of dielectric loss and magnetic loss, so that the modified carbon fiber has good wave absorbing performance in a very wide frequency band range; the invention uses carbon fiber coated with magnetic micro-nano iron coating as absorbent and uses foam as matrix to prepare layered composite material, and uses vector network analyzer to measure wave absorbing property.
Detailed Description
The following description of the embodiments of the present invention will provide a clear and detailed description of the technical solutions of the embodiments of the present invention, where the described embodiments are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
For the sake of clarity, the following is a detailed description by way of examples.
Example 1
S1, cutting carbon fibers into 30cm long, knotting two ends of the carbon fibers, putting the knotted fibers into a tube furnace, firing at 500 ℃ for 40min, cooling and taking out; cutting into chopped carbon fibers;
s2, drying the carbon fiber at 80 ℃ for 10 hours;
s3, sealing the reaction kettle, adding about 2/3 of solvent into the 6 gas washing cylinders, introducing nitrogen, and using soapy water to test whether the reaction kettle cover leaks gas or not, wherein no bubbles exist, and the reaction kettle is qualified in sealing.
S4, adding 500g of carbon fiber and 12kg of solvent xylene into a barrel, and dispersing for 30min at a high speed of 800 rpm by using a dispersing machine.
S5, adding the dispersed xylene fiber soaking solution into a reaction kettle; weighing a certain amount of pentacarbonyl iron, loading into a reaction kettle, and flushing a carbonyl iron container and a funnel with retained xylene; and (3) rapidly sealing the reaction kettle, introducing nitrogen, continuously igniting by a lighter for 30min, and observing whether the flame is extinguished immediately at the air outlet, wherein the flame is extinguished immediately to indicate that the air in the reaction kettle is replaced by the nitrogen.
S6, setting a temperature rise program for the reaction kettle: firstly, the temperature is raised to 100 ℃ from normal temperature for 60min, then raised to 130 ℃ for 360min, then raised to 155 ℃ for 2400min, and then kept at 155 ℃ for 2400min, and then cooled to normal temperature for 60 min. 88 hours altogether
S7, starting stirring at 30r/min for 2min, and then stirring at 20r/min for 1min every 1 h;
s8, setting a parameter of the water chiller at-2 ℃, opening a water outlet valve of the water chiller, and starting the water chiller.
And S9, cooling the reaction kettle to room temperature, closing a nitrogen valve, and closing the water chiller and a water outlet valve of the water chiller. Slowly opening the blanking valve to avoid liquid splashing, releasing dimethylbenzene, taking out above the solid fiber, and filtering by using a 80-mesh screen.
S10, washing the coated fibers with absolute ethyl alcohol for 3 times; the mixture of coupling agent, 95% ethanol and 0.4wt% KH550 was used for the post-treatment, and the mixture was immersed for 30 minutes with stirring and then filtered.
S11, tedding for 10 hours at room temperature, and then placing the obtained product into a baking oven to be dried for 10 hours at a low temperature of 40 ℃ to obtain the carbonyl iron coating carbon fiber magnetic wave-absorbing composite material.
The electromagnetic wave loss of the prepared material is smaller than-8 dB in the frequency range of 4.35-18GHz and smaller than-11 dB in the frequency range of 26.5-40GHz according to the measurement of GJB2038A-2011 'method for testing the reflectivity of radar absorbing material'.
Example 2
S1, cutting carbon fiber into 40cm long, knotting two ends of the carbon fiber, putting the knotted fiber into a tube furnace, firing at 500 ℃ for 40min, cooling and taking out; cutting into chopped carbon fibers;
s2, drying the carbon fiber at 80 ℃ for 12 hours;
s3, sealing the reaction kettle, adding about 2/3 of solvent into the 6 gas washing cylinders, introducing nitrogen, and using soapy water to test whether the reaction kettle cover leaks gas or not, wherein no bubbles exist, and the reaction kettle is qualified in sealing.
S4, adding 500g of carbon fiber and 10kg of solvent xylene into a barrel, and dispersing at a high speed of 1000 revolutions per minute for 20 minutes by using a dispersing machine.
S5, adding the dispersed xylene fiber soaking solution into a reaction kettle; weighing a certain amount of pentacarbonyl iron, loading into a reaction kettle, and flushing a carbonyl iron container and a funnel with retained xylene; and (3) rapidly sealing the reaction kettle, introducing nitrogen, continuously igniting by a lighter for 30min, and observing whether the flame is extinguished immediately at the air outlet, wherein the flame is extinguished immediately to indicate that the air in the reaction kettle is replaced by the nitrogen.
And S6, after the nitrogen replacement is finished, a heating button is turned on to start heating, and after the reaction is started, the reaction is continuous and continuous, and 2 people are required to take turns on duty. The temperature raising program of the reaction kettle is that the temperature is firstly raised to 100 ℃ from normal temperature for 60min, then raised to 130 ℃ for 360min, then raised to 155 ℃ for 2400min, and then kept at 155 ℃ for 2400min, and then cooled to normal temperature for 60 min. 88 hours altogether
S7, starting stirring at 60r/min for 1min, and then stirring at 20r/min for 2min every 2 h;
s8, setting a parameter of the water chiller at-2 ℃, opening a water outlet valve of the water chiller, and starting the water chiller.
And S9, cooling the reaction kettle to room temperature, closing a nitrogen valve, and closing the water chiller and a water outlet valve of the water chiller. Slowly opening the blanking valve to avoid liquid splashing, releasing dimethylbenzene, taking out above the solid fiber, and filtering by using a 80-mesh screen.
S10, washing the coated fibers with absolute ethyl alcohol for 3 times; the mixture of coupling agent was subjected to post-treatment with 95% ethanol and 0.5wt% KH550, and after soaking for 30min with stirring, the mixture was filtered.
S11, tedding for 10 hours at room temperature, and then placing the obtained product into a baking oven to be dried for 10 hours at the low temperature of 50 ℃ to obtain the carbonyl iron coating carbon fiber magnetic wave-absorbing composite material.
The electromagnetic wave loss of the prepared material is smaller than-8 dB in the frequency range of 4.78-12.56GHz and smaller than-10 dB in the frequency range of 26.5-40GHz according to the measurement of GJB2038A-2011 'method for testing the reflectivity of radar absorbing material'.
Comparative example 1
Other conditions were the same as in example 1 except that the stirring was continued at a rotational speed of 30 to 60r/min in the comparative example, and after solid-liquid separation, carbon fibers were found to be agglomerated, and no plating was formed inside after washing and drying, resulting in uneven plating.
Comparative example 2
Other conditions were the same as in example 1, except that the temperature program was set differently, and the temperature program set in comparative example 2 was first heated from room temperature to 100℃over 60min, then to 130℃over 90min, then to 155℃over 1200min, and then to 3600min at 155℃and then cooled to room temperature over 60 min. After solid-liquid separation, 88 hours total, it was found that some carbon fibers had surface and vessel accumulated a lot of iron powder, resulting in uneven plating.
Comparative example 3
Other conditions are the same as those of the embodiment 1, except that the addition amount of carbonyl iron is different, the mass ratio of the carbon fiber to the carbonyl iron in the comparative example is 0.5:4, and after solid-liquid separation, the carbon fiber in the reaction kettle is found to have sporadic sparks, and the carbonyl iron is incompletely decomposed, pollutes the environment, is easy to naturally and is very dangerous.
Finally, it should be noted that the above description is only a preferred embodiment of the present invention, and those skilled in the art can make many similar changes without departing from the principles of the present invention and the scope of the claims, which are all within the scope of the present invention.
Claims (7)
1. A preparation method of pyrolytic carbonyl iron coating carbon fiber is characterized by comprising the following steps: the method comprises the following steps:
dispersing the pretreated carbon fiber in an organic solvent to obtain a carbon fiber-containing solution, then adding carbonyl iron to obtain slurry, carrying out pyrolysis reaction under a protective atmosphere, carrying out solid-liquid separation, washing the obtained solid phase, soaking the solid phase in a coupling agent-containing mixed solution, and drying to obtain the coated carbon fiber;
the mass ratio of the carbon fiber to the carbonyl iron is 0.5:1-3;
the pyrolysis reaction is carried out by the following steps: heating to 90-110 ℃ from normal temperature for 40-80 min, heating to 120-140 ℃ for 300-420 min, heating to 150-160 ℃ for 2000-3000 min, preserving heat for 2000-3000 min at 150-160 ℃, and cooling to normal temperature for 60-180 min;
and (3) carrying out pyrolysis reaction under stirring, wherein the stirring mode is that stirring is carried out for 1-2 min at a rotating speed of 30-60 r/min, and then stirring is carried out for 1-5 min at a rotating speed of 20-30 r/min at intervals of 1-2 h.
2. The method for preparing pyrolytic carbonyl iron coated carbon fiber according to claim 1, wherein the method comprises the following steps: cutting the carbon fiber into 30-40 cm, then performing heat treatment at 400-600 ℃ for 40-50 min, and cutting into 2-5 mm; and (5) drying to obtain the pretreated carbon fiber.
3. The method for preparing pyrolytic carbonyl iron coated carbon fiber according to claim 1, wherein the method comprises the following steps: the organic solvent is dimethylbenzene; the mass ratio of the carbon fiber to the dimethylbenzene is 0.5:9-15.
4. The method for preparing pyrolytic carbonyl iron coated carbon fiber according to claim 1, wherein the method comprises the following steps: the carbon fiber is dispersed in the organic solvent under stirring, the stirring speed is 800-2000 rpm, and the stirring time is 10-30 min.
5. The method for preparing pyrolytic carbonyl iron coated carbon fiber according to claim 1, wherein the method comprises the following steps: in the mixed solution containing the coupling agent, the coupling agent is KH550, and the mass fraction of the coupling agent is 0.3-0.6wt%;
in the mixed solution containing the coupling agent, the solvent is ethanol water solution, and the mass fraction of ethanol in the ethanol water solution is 90-95wt%.
6. The method for preparing pyrolytic carbonyl iron coated carbon fiber according to claim 1, wherein the method comprises the following steps:
the soaking is carried out under stirring, the soaking time is 30-60 min,
the drying process is that the materials are tedded for 10 to 12 hours at room temperature and then dried for 10 to 20 hours at the temperature of 40 to 60 ℃.
7. The pyrolytic carbonyl iron coated carbon fiber prepared by the preparation method according to any one of claims 1 to 6, characterized in that: and the surface of the coated carbon fiber is uniformly coated with the micro-nano iron coating.
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