CN102817112B - Preparation method of activated carbon fibers - Google Patents
Preparation method of activated carbon fibers Download PDFInfo
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Abstract
The invention provides a preparation method of activated carbon fibers. The preparation method comprises the following steps: a) carbonizing polyimide fibers under the atmosphere of nitrogen to obtain carbonized fibers; and b) activating the carbonized fibers in water vapor to obtain the activated carbon fibers. The activated carbon fibers prepared by the preparation method have the characteristic of good tensile strength and tearing strength.
Description
Technical field
The present invention relates to material with carbon element preparation field, be specifically related to a kind of preparation method of fibre active carbon.
Background technology
Fibre active carbon is a kind of emerging, efficient sorbing material, and because it has, specific area is large, micropore is flourishing, adsorption/desorption speed is regenerated soon and easily, and therefore, people can reuse for a long time; In addition, it also has the adaptable advantage of consumption less and to equipment in good filling, winding performance, use.In addition, because abundant organo-functional group is contained on its surface of fibre active carbon, so it also has good redox characteristic, the organic matter in gas phase and liquid phase and inorganic impurity are all had to good suction-operated; Add, described fibre active carbon possesses stronger acid and alkali-resistance, corrosion-resistant, high-low temperature resistant and has good electric conductivity, it can be applied in such as in environmental protection, chemical industry, electric power, the electronics energy, hydrometallurgy, medical treatment and bioengineering etc. field, especially in the application of the aspects such as air cleaning, purification of water quality, sewage disposal, organic solvent recovery, fibre active carbon more becomes indispensable material.
Although the fibre active carbon providing in prior art can meet the requirement of applying in above-mentioned field, but protection and the field such as shield facility in such as military protection suit, protecting tent, nuclear industry, stretch-proof and the lear energy of the fibre active carbon need using are stronger, so the fibre active carbon that existing viscose, polyacrylonitrile fibre, furfural fiber, pitch fibers etc. are prepared all can not meet the needs of above-mentioned application.So all beginning one's study, those skilled in the art there is the composite of high tensile and anti tear, all there are the patent of this respect in Germany and Japan, its method is bonded at existing commercial fibre active carbon on the material that other intensity is high by inorganic glue lattice point formula, improves the bulk strength of material to meet above-mentioned needs.
Although the method for prior art has improved stretch-proof and the lear energy of product, composite has reduced the surface area of fibre active carbon because of adhesion process, thereby has reduced its absorption property and gas permeability, causes barrier propterty to be under some influence; Although composite has increased material monolithic intensity on the other hand, local strength does not still improve.As can be seen here, develop a kind of have compared with the tencel active carbon of high tensile, tearing toughness to meet the needs of the field such as military project, space flight, nuclear industry and radiation protection application, just become current fibre active carbon field problem demanding prompt solution.
Summary of the invention
The technical problem to be solved in the present invention is to provide a kind of stretch-proof that has, the preparation method of the fibre active carbon that tearing toughness is good.
In order to solve above technical problem, the invention provides a kind of preparation method of fibre active carbon, comprising:
A) by polyimide fiber carbonization under the atmosphere of nitrogen, obtain carbon fibre;
B) described carbon fibre is activated in water vapour, obtain fibre active carbon.
Preferably, step a) is specially:
A11) polyimide fiber is heated in nitrogen atmosphere to 300 ~ 350 ℃ of insulation 1h, is then heated to 400 ~ 450 ℃ of insulation 1h;
A12) by step a11) heating after polyimide fiber continue to be heated to 550 ~ 1000 ℃ of carbonization 1 ~ 5h, obtain carbon fibre.
Preferably, step a) is specially:
A21) polyimide fiber speed intensification with 2 ℃ per minute in nitrogen atmosphere is warming up to 500 ℃ from room temperature;
A22) by step a21) heating after polyimide fiber continue to be heated to 550 ~ 1000 ℃, carbonization 1 ~ 5h, obtains carbon fibre.
Preferably, described polyimide fiber is: polyimides cloth or polyimides felt.
Preferably, between step a), also comprise described polyimide fiber is processed through chemical activation.
Preferably, described chemical activation is specially
Polyimide fiber is flooded after 10 ~ 60min in phosphoric acid or phosphate solution, take out, drain standby carbonization and steam activation and use.
Preferably, described phosphate is, ammonium phosphate, diammonium hydrogen phosphate and ammonium dihydrogen phosphate (ADP) one or both.
Preferably, the concentration of described phosphoric acid or aqueous phosphatic is 0.5wt% ~ 10wt%.
Preferably, step b) is specially:
B11) carbon fibre step a) being obtained heats in water vapour, carries out activation processing;
The temperature of described activation processing is 600 ~ 800 ℃.
The invention provides a kind of preparation method of fibre active carbon, use polyimide fiber first carries out carbonization and then activates, and obtains fibre active carbon.It is tight that polyimides has intermolecular combination, the feature that mechanical strength is high, mechanical property is good.As raw material, be spun into fiber, then pass through carbonization, activating process, prepare and there is the very tencel active carbon of high-tensile strength.
The specific embodiment
In order further to understand the present invention, below in conjunction with embodiment, the preferred embodiments of the invention are described, but should be appreciated that these are described is the restriction for further illustrating the features and advantages of the present invention rather than patent of the present invention being required.
The present invention uses polyimides as raw material, and the raw materials such as polyimide fiber silk, polyimides cloth or polyimides felt, polyimide film, polyimides paper are obtained to fibre active carbon after carbonization, activation processing.
According to the present invention, polyimides is a kind of polymer that contains imide group repetitive, because it has the molecular structure of homogeneous, and most polyimides all contains aromatic rings, reaches more than 400 ℃ so high temperature resistant, long-term serviceability temperature scope-200～300 ℃, without sharp melting point, high insulating property, 103 hertz of lower dielectric constants are 4.0, dielectric loss only 0.004～0.007, belongs to F to H class F insulating material F.
According to the present invention, the polyimides that the present invention selects is preparation by the following method preferably:
The polyamic acid solution of take carries out the preparation of polyimide fiber as raw material by spin processes, polyamic acid can be dissolved in aprotic solvent, thereby in the design of polyimide fiber chemical constitution, there is unlimited possibility, obtain the polyimide fiber that chemical constitution is suitable.
The present invention mixes dianhydride and diamines in organic solvent, obtains polyamic acid solution after polymerization reaction take place, specifically comprises:.
In the present invention, described dianhydride includes but not limited to equal benzene dianhydride (PMDA), biphenyl dianhydride (BPDA), benzophenone dianhydride (BTDA), diphenyl ether dianhydride (ODPA), diphenyl sulfide dianhydride (TDPA), diphenyl sulfone dianhydride (SDPA), triphen two ether dianhydrides (HQDPA), Bisphenol A Type Diether Dianhydride (BPADA), Bisphenol F type two ether dianhydrides (BPFDA), '-biphenyl diphenol two ether dianhydrides etc., can be wherein one or more; When being wherein multiple, the present invention is not particularly limited the mol ratio of this multiple dianhydride, and those skilled in the art can select according to the performance of target fibers, determine.Described dianhydride is preferably one or more in PMDA, BPDA, TDPA and ODPA.
In the present invention, described diamines includes but not limited to p-phenylenediamine (PPD) (PPD), m-phenylene diamine (MPD) (MPD), diphenylmethane diamine (MDA), diphenyl ether diamines (ODA), triphen two ether diamines (HQDPA), 4,4 '-bis-(4-amino-benzene oxygen) biphenyl (BAPB), 2, two [4-(4-amino-benzene oxygen) phenyl] propane (BAPP) of 2-, 5 (6)-amino-2-(4 '-aminophenyl) benzimidazole (PABZ), 5-amino-2-(4-aminophenyl) benzoxazole (PABO), 2,5-bis-(4-aminophenyl) pyrimidines (PRM) etc. can be wherein one or more; When being wherein multiple, the present invention is not particularly limited the mol ratio of this multiple diamines, and those skilled in the art can select according to the performance of target fibers, determine.Described diamines is preferably one or more in ODA, MDA, PPD and PABZ.
The present invention carries out polymerization to described dianhydride and diamines with equimolar ratio.Be preferably 1:0.95 ~ 1.05, more preferably 1:1.
In the present invention, described aprotic solvent includes but not limited to dimethyl formamide (DMF), dimethylacetylamide (DMAc), dimethyl sulfoxide (DMSO) (DMSO), 1-METHYLPYRROLIDONE (NMP) etc.
Polyimide fiber prepared by said method is raw material, and its raw-material form is preferably cloth, felt, film, paper or silk.Described polyimides, under the protection of nitrogen, is carried out to carbonization treatment, in high temperature furnace, complete.The temperature of carbonization is preferably 550 ℃ ~ 1000 ℃.
First kind of way:
A11) polyimide fiber is heated in nitrogen atmosphere to 300 ~ 350 ℃ of insulation 1h, is then heated to 400 ~ 450 ℃ of insulation 1h;
A12) by step a11) heating after polyimide fiber continue to be heated to 550 ~ 1000 ℃ of carbonization 1 ~ 5h, obtain carbon fibre.
The second way is:
A21) polyimide fiber speed intensification with 2 ℃ per minute in nitrogen atmosphere is warming up to 500 ℃ from room temperature;
A22) by step a21) heating after polyimide fiber continue to be heated to 550 ~ 1000 ℃, carbonization 1 ~ 5h, obtains carbon fibre.
The carbon fibre obtaining after carbonization need to pass through activation processing, and activation is one polyimide fiber is oxidized to pore-creating process.According to the present invention, what activation adopted is physically activated or chemical activation and the physically activated technique combining, described physically activated preferred water steam is activator, the activator that chemical activation is used is preferably phosphoric acid or phosphate, one or both in phosphate preferably phosphoric acid ammonium, diammonium hydrogen phosphate and ammonium dihydrogen phosphate (ADP).Described phosphoric acid or phosphate are the aqueous solution, and concentration is 0.5wt% ~ 10wt%.According to the present invention, if select chemical activation, the step such as described in that, chemical activation step of polyimide fiber should will first carry out polyimide fiber again carbonization before carburising step after chemical activation, physically activated.
According to the present invention, described polyimide fiber is physically activated in steam, carry out as follows: carbon fibre b11) step a) being obtained heats in water vapour, carry out activation processing; The temperature of described activation processing is 600 ~ 800 ℃.
Chemical activation carries out as follows: polyimide fiber (cloth or felt) is flooded to 10～60min in phosphoric acid or aqueous phosphatic, and taking-up drains, and then by step a) carbonization and step b), in steam, activates.The concentration of described phosphoric acid or aqueous phosphatic is preferably 0.5wt%～10wt%, and more preferably 1wt% ~ 8wt%, most preferably is 4wt% ~ 6wt%.。
The fibre active carbon specific area that the present invention prepares is 900m
2/ g～2200m
2/ g, product yield is 6wt%～38wt%.Fibre active carbon cloth intensity is 1.0MPa～6.1MPa; The intensity of fibre active carbon felt is 0.20MPa～0.60MPa.The intensity of active carbon and specific area have the relation of direct correspondence.When therefore intensity is compared, the intensity level that can only get identical specific area compares.Polyimide fiber active carbon cloth prepared by the present invention and the intensity of felt are the more than 8 times of domestic several major vendor like product intensity.
The ASAP2420 type specific-surface area detection instrument that specific area Shi Yong of the present invention U.S. Merck & Co., Inc produces is measured, and intensity is that the WSM-100N type universal testing machine of producing with Changchun intelligence instrument Co., Ltd is measured.
Feature of the present invention is that preparation technology is simple, with short production cycle, condition and range is wide, be easy to industrialization, product strength is high, can extend the service life of fibre active carbon, has played again the effect in expanded application field.
Embodiment 1
Get 29.36g polyimides cloth, pack the stainless steel reaction pipe of internal diameter 68mm into, at 99.999%N
2protection under, room temperature is raised to 200 ℃ of half an hour; 200 ℃ to 300 ℃ one hour, constant temperature one hour; 300 ℃ to 400 ℃ one hour, constant temperature one hour; 400 ℃ to 600 ℃ one hour, constant temperature one hour; Stop logical N
2, then in pipe, add water, (adding water speed is 10.15 mls/g of sample * hour), activates 10 hours, while being cooled to 300 ℃, stops adding water, and logical N
2be down to room temperature.Finally record the yield 21.9% of product, specific area is 900m
2/ g, slight 2.43MPa stretches.
Embodiment 2
Get the polyimides felt of 11.7g, at 300ml, soak one hour in 0.5% ammonium phosphate solution, taking-up drains, and is then packed into the stainless steel reaction pipe of 68mm, at 99.999%N
2under protection, from room temperature, be raised to 250 ℃ of half an hour, constant temperature one hour; 250 ℃ to 300 ℃ half an hour, constant temperature one hour; From 300 ℃ to 700 ℃, heat up per half an hour 100 ℃, and respectively 400 ℃, 500 ℃, 700 each constant temperature one hour, drop to room temperature after completing carbonization.Activation is at N
2under atmosphere, be raised to 250 ℃ half an hour, constant temperature half an hour, be then raised to 650 ℃ half an hour, stop N
2add water, 650 ℃ of activation 6 hours, adding water speed was 4.69 mls/g of sample * hour, and when temperature drops to 300 ℃, logical N cuts off the water
2, and be down to room temperature.The product yield finally recording is 31.6%, specific area 1080m
2/ g, TENSILE STRENGTH 0.51MPa.
Embodiment 3
Get the polyimides cloth of 34.84g, packed into internal diameter and be in the stainless steel reaction pipe of 39mm and lead at N
2protection be raised to 200 ℃ lower half an hour, then with one hour, be raised to 300 ℃ and 400 ℃ respectively, and constant temperature one hour, 400 ℃ be raised to 700 ℃ two hours, constant temperature one hour, completes carbonization.Activation is to activate four hours at the temperature of 675 ℃, and adding water speed is 397ml/h.The yield of the product finally recording is 10.4%, and specific area is 1357m
2/ g, TENSILE STRENGTH 1.11MPa.
Embodiment 4
Get the polyimides felt of 68.05g, pack in internal diameter 68mm stainless steel reaction pipe, at N
2under the protection of gas, be raised to 250 ℃ half an hour, within one hour, be raised to 350 ℃, constant temperature one hour, is raised to 1000 ℃ for two hours, and constant temperature 4 hours completes carbonization experiment.In activation test, at N
2under the atmosphere of gas, be raised to 300 ℃ from room temperature half an hour, and constant temperature half an hour, and then 300 ℃ are raised to 700 ℃ of half an hour, and constant temperature three hours, and logical steam activation, is warmed up to 600 ℃ and adds water, and adding water speed is 349ml/h, is cooled to 300 ℃ and cuts off the water, and changes logical N
2be down to room temperature.The product yield 26.5% finally recording, specific area 1307m
2/ g, TENSILE STRENGTH 0.43MPa.
Embodiment 5
Get the polyimides cloth of 35.08g, packing internal diameter into is in the stainless steel reaction pipe of 39mm, and carbonization operates as example 3, cools to 500 ℃ after carbonization, is then raised to 700 ℃ from 500 ℃ half an hour, while being warming up to 600 ℃, stops N
2change water, adding water speed is 298ml/h.700 ℃ of constant temperature activate four hours.The product yield 10.3% finally recording, specific area 1529m
2/ g, TENSILE STRENGTH 0.95MPa.
Embodiment 6
Get the polyimides felt of 35.91g, in 1%(weight ratio) to soak one hour in ammonium phosphate solution, taking-up drains, carbonization, the logical embodiment 5 of activation act, adding water speed is 284ml/h.Finally record product yield 12.7%, specific area 1504m
2/ g, TENSILE STRENGTH 0.42MPa.
Embodiment 7
Get the polyimides felt of 19.27g, packing internal diameter into is in 39mm stainless steel reaction pipe, at N
2under the protection of gas, be raised to 250 ℃ from room temperature half an hour, 250 ℃ to 350 ℃ one hour, constant temperature one hour; 350 ℃ be raised to 600 ℃ one hour, 600 ℃ to 850 ℃ half an hour, constant temperature five hours, completes carbonization experiment, is cooled to room temperature.Activation is at N
2protection under, be raised to 300 ℃ from room temperature half an hour, constant temperature half an hour; 300 ℃ are raised to 700 ℃ of half an hour, in the time of 600 ℃, stop N
2and start to add water, and adding water speed is 259ml/h, 700 ℃ activate four hours, are cooled to 300 ℃ and cut off the water, logical N
2, be then down to room temperature.The product yield 6.1% finally recording, specific area 2186m
2/ g, TENSILE STRENGTH 0.31MPa.
Embodiment 8
Get 46.58g polyimides cloth, packing internal diameter into is in 39mm stainless steel reaction pipe, at N
2protect and be raised to 200 ℃ lower half an hour, then with one hour, be raised to 300 ℃ and 400 ℃ respectively, and 300 ℃ and 400 ℃ of each constant temperature one hour, 400 ℃ be raised to 550 ℃ two hours, constant temperature one hour, completes carbonization.Activation is that adding water speed was 355ml/h 650 ℃ of activation 4 hours.The product yield 14.3% finally recording, specific area 1415m
2/ g, TENSILE STRENGTH 4.23MPa.
Embodiment 9
Get 36.28g polyimides cloth, pack in internal diameter 39mm reaction tube, at N
2under the protection of gas, be raised to 200 ℃ half an hour, then with one hour, be raised to 300 ℃, 400 ℃ and 550 ℃ respectively, and within one hour, complete carbonization at 300 ℃, 400 ℃ and 550 ℃ of each constant temperature.After carbonization, be raised to 650 ℃ half an hour, and at 650 ℃, pass into steam and (stop logical N
2) 4 hours, adding water speed is 352ml/h.Product yield is 23.6%, specific area 1136m
2/ g, TENSILE STRENGTH is 4.74MPa.We compare the viscose glue base fibre active carbon cloth of this result and domestic two main manufacturer production, and the specific area mean value of these two products is 1106m
2/ g, average strength is 0.43MPa.The polyimide fiber active carbon cloth intensity that we prepare is 11 times of the said goods.The intensity and the specific area that should be noted that fibre active carbon have certain corresponding relation, only have the directly contrast of the approaching sample of specific area.
Embodiment 10
Get 23.08g polyimides felt, packing internal diameter into is in 39mm reaction tube, at N
2under the protection of gas, be raised to 250 ℃ half an hour, within one hour, be raised to 350 ℃, constant temperature, after one hour, is raised to 700 ℃ for one hour, and then constant temperature completes carbonization for three hours.Activation experiment is at N
2under the protection of gas, be raised to 300 ℃ half an hour, and constant temperature half an hour, then with half an hour, be raised to 700 ℃ from 300 ℃, while being warmed up to 600 ℃, add water, adding water speed is 251ml/h.700 ℃ of steam activations cool to 300 ℃ naturally after three hours, stop adding water, and logical N2 gas is down to room temperature.Product yield 17.4%, specific area 1248m
2/ g, the slight 0.40MPa that stretches, this intensity is viscose glue base fibre active carbon felt (the specific area 1209m of domestic certain manufacturer production
2/ g) 7.8 of intensity 0.051MPa times.
Above the preparation method of a kind of fibre active carbon provided by the invention is described in detail; having applied specific case herein sets forth principle of the present invention and embodiment; the explanation of above embodiment is just for helping to understand method of the present invention and core concept thereof; should be understood that; for those skilled in the art; under the premise without departing from the principles of the invention; can also carry out some improvement and modification to the present invention, these improvement and modification also fall in the protection domain of the claims in the present invention.
Claims (7)
1. a preparation method for fibre active carbon, is characterized in that comprising:
A) by polyimide fiber carbonization under the atmosphere of nitrogen, obtain carbon fibre;
B) described carbon fibre is activated in water vapour, obtain fibre active carbon; Described step a) is specially:
A11) polyimide fiber is heated in nitrogen atmosphere to 300～350 ℃ of insulation 1h, is then heated to 400～450 ℃ of insulation 1h;
A12) by step a11) heating after polyimide fiber continue to be heated to 550～1000 ℃ of carbonization 1～5h, obtain carbon fibre.
2. preparation method according to claim 1, is characterized in that, described polyimide fiber is: polyimides cloth or polyimides felt.
3. preparation method according to claim 1, is characterized in that, step a)-also comprise before described polyimide fiber processed through chemical activation.
4. preparation method according to claim 3, is characterized in that, described chemical activation is specially
Polyimide fiber is flooded after 10～60min in phosphoric acid or phosphate solution, take out, drain standby carbonization and steam activation and use.
5. preparation method according to claim 4, is characterized in that, described phosphate is, ammonium phosphate, diammonium hydrogen phosphate and ammonium dihydrogen phosphate (ADP) one or both.
6. preparation method according to claim 4, is characterized in that, the concentration of described phosphoric acid or aqueous phosphatic is 0.5wt%～10wt%.
7. preparation method according to claim 1, is characterized in that, step b) be specially:
B11) carbon fibre step a) being obtained heats in water vapour, carries out activation processing; The temperature of described activation processing is 600～800 ℃.
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| CN103320904B (en) * | 2013-06-20 | 2015-03-18 | 中国科学院理化技术研究所 | Water vapor activation preparation method and device of micro-porous active carbon fibers |
| CN103408112B (en) * | 2013-08-01 | 2015-06-03 | 昆明理工大学 | Electrochemical oxidation device |
| CN107892745B (en) * | 2017-10-31 | 2020-12-01 | 宁波惠璞新材料有限公司 | Thermoplastic polybenzoxazole imide and preparation method thereof |
| CN110144728B (en) * | 2019-06-11 | 2021-08-24 | 江苏先诺新材料科技有限公司 | Polyimide fiber eyelet fabric |
| CN110130093A (en) * | 2019-06-17 | 2019-08-16 | 湖南创景新材料技术有限公司 | A kind of activated carbon fiber cloth and its production method |
| CN114262646B (en) * | 2021-12-28 | 2024-04-16 | 山东中大药业有限公司 | Detergent for removing pesticide residues of traditional Chinese medicine plants and preparation method thereof |
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| CN1036799C (en) * | 1993-05-16 | 1997-12-24 | 中山大学 | Process for preparing active carbon fibre |
| CN1040866C (en) * | 1994-07-03 | 1998-11-25 | 中国科学院长春应用化学研究所 | Preparation method of viscose fiber activated carbon |
| CN101230502B (en) * | 2007-12-13 | 2010-10-27 | 中国人民解放军总后勤部军需装备研究所 | Method for preparing anesthesia activated carbon fiber |
| CN102719935A (en) * | 2012-06-07 | 2012-10-10 | 北京林业大学 | Preparation method of active wood-based carbon fibers |
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| CN1068604A (en) * | 1992-07-17 | 1993-02-03 | 中山大学 | The two steps of inner liner and hermetic type legal system is equipped with the technology of activated carbon fiber |
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Effective date of registration: 20130419 Address after: 130103 Jilin province Changchun Chaoqun Street hi tech Development Zone No. 666B Applicant after: Changchun Hipolyking Co., Ltd. Applicant after: JILIN HIPOLYKING POLYIMIDE MATERIAL CO., LTD. Address before: 130103 Jilin province Changchun Chaoqun Street hi tech Development Zone No. 666B Applicant before: Changchun Hipolyking Co., Ltd. |
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Owner name: LV XIAOYI Free format text: FORMER OWNER: JILIN HIPOLYKING MATERIAL CO., LTD. Effective date: 20140825 |
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Effective date of registration: 20140825 Address after: 130103 Jilin province Changchun Chaoqun Street hi tech Development Zone No. 666B Applicant after: Changchun Hipolyking Co., Ltd. Applicant after: Lv Xiaoyi Address before: 130103 Jilin province Changchun Chaoqun Street hi tech Development Zone No. 666B Applicant before: Changchun Hipolyking Co., Ltd. Applicant before: JILIN HIPOLYKING POLYIMIDE MATERIAL CO., LTD. |
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