CN102817112A - Preparation method of activated carbon fibers - Google Patents
Preparation method of activated carbon fibers Download PDFInfo
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- CN102817112A CN102817112A CN2012103347842A CN201210334784A CN102817112A CN 102817112 A CN102817112 A CN 102817112A CN 2012103347842 A CN2012103347842 A CN 2012103347842A CN 201210334784 A CN201210334784 A CN 201210334784A CN 102817112 A CN102817112 A CN 102817112A
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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 the material with carbon element preparation field, be specifically related to a kind of preparation method of fibre active carbon.
Background technology
The fiber-reactive charcoal is a kind of emerging, high-efficiency absorption material, and specific area is big, micropore is flourishing because it has, adsorption/desorption speed is fast and be prone to regeneration, and therefore, people can reuse for a long time; In addition, it also has in good filling, winding performance, the use and to consume less and to the adaptable advantage of equipment.In addition, because abundant organo-functional group is contained on its surface of fiber-reactive charcoal,, organic matter in gas phase and the liquid phase and inorganic impurity all there is the good adsorption effect so it also has good redox characteristic; Add; Said fiber-reactive charcoal possesses stronger acid and alkali-resistance, corrosion-resistant, high-low temperature resistant and has excellent conducting performance; Make it can be applied in such as in environmental protection, chemical industry, electric power, the electronics energy, hydrometallurgy, medical treatment and bioengineering or the like the field; Especially in the application of aspects such as air cleaning, purification of water quality, sewage disposal, organic solvent recovery, the fiber-reactive charcoal more becomes indispensable material.
Though the fiber-reactive charcoal that provides in the prior art can satisfy the requirement of in above-mentioned field, using; But fields such as protection and shield facility in such as military protective clothing, protection tent, nuclear industry; The stretch-proof and the lear energy of the fiber-reactive charcoal that need to use are stronger, so the fiber-reactive charcoal that existing viscose, polyacrylonitrile fibre, furfural fiber, pitch fibers etc. are prepared all can not satisfy the needs of above-mentioned application.So those skilled in the art all begin one's study and have high tensile and stretch the composite with anti tear; Germany and the Japanese patent that this respect is all arranged; Its method is bonded at existing commercial fibre active carbon on the high material of other intensity with inorganic glue lattice point formula, and the bulk strength that improves material is to satisfy above-mentioned needs.
Though the method for prior art has improved the stretch-proof and the lear energy of product, composite has reduced the surface area of fiber-reactive charcoal because of adhesion process, thereby has reduced its absorption property and gas permeability, causes barrier propterty to be under some influence; Though composite has increased material monolithic intensity on the other hand, local strength does not still improve.This shows that developing a kind of tencel active carbon with higher stretch-proof, tearing toughness just becomes present fiber-reactive charcoal field problem demanding prompt solution with the needs that satisfy fields application such as military project, space flight, nuclear industry and radiation protection.
Summary of the invention
The technical problem that the present invention will solve is to provide a kind of stretch-proof that has, the preparation method of 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) with polyimide fiber carbonization under the atmosphere of nitrogen, obtain carbon fibre;
B) with the activation in water vapour of said carbon fibre, obtain the fiber-reactive charcoal.
Preferably, step a) is specially:
A11) polyimide fiber is heated to 300 ~ 350 ℃ of insulation 1h in nitrogen atmosphere, is heated to 400 ~ 450 ℃ of insulation 1h then;
A12) with 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 ℃ of per minutes in nitrogen atmosphere is warming up to 500 ℃ from room temperature;
A22) with step a21) heating after polyimide fiber continue to be heated to 550 ~ 1000 ℃, carbonization 1 ~ 5h obtains carbon fibre.
Preferably, said polyimide fiber is: polyimides cloth or polyimides felt.
Preferably, between step a), also comprise said polyimide fiber through the chemical activation processing.
Preferably, said chemical activation is specially
Polyimide fiber flooded 10 ~ 60min in phosphoric acid or phosphate solution after, take out, drain carbonization fully and steam activation usefulness.
Preferably, said phosphate does, ammonium phosphate, diammonium hydrogen phosphate and ammonium dihydrogen phosphate (ADP) one or both.
Preferably, the concentration of said phosphoric acid or aqueous phosphatic is 0.5wt% ~ 10wt%.
Preferably, step b) is specially:
B11) carbon fibre that step a) is obtained heats in water vapour, carries out activation processing;
The temperature of said activation processing is 600 ~ 800 ℃.
The invention provides a kind of preparation method of fibre active carbon, use polyimide fiber to carry out carbonization earlier and then carry out activation, obtain the fiber-reactive charcoal.It is tight that polyimides has intermolecular combination, the characteristics that mechanical strength is high, mechanical property is good.Be spun into fiber as raw material, pass through carbonization, activating process again, prepare and have 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 just restriction for further specifying feature and advantage of the present invention rather than patent of the present invention being required is described.
The present invention uses polyimides as raw material, with obtaining the fiber-reactive charcoal after the carbonization of raw materials such as polyimide fiber silk, polyimides cloth or polyimides felt, polyimide film, polyimides paper process, the activation processing.
According to the present invention, polyimides is a kind of polymer that contains the imide group repetitive, because it has the molecular structure of homogeneous; And most polyimides all contains aromatic rings, thus high temperature resistant reaching more than 400 ℃, long-term serviceability temperature scope-200～300 ℃; No sharp melting point, high insulating property, 103 hertz of following 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 for use is preferably through following method preparation:
With the polyamic acid solution is raw material carries out polyimide fiber through spin processes preparation; Polyamic acid can be dissolved in the aprotic solvent; Thereby in the design of polyimide fiber chemical constitution, have unlimited possibility, obtain the suitable polyimide fiber of chemical constitution.
The present invention mixes dianhydride and diamines in organic solvent, obtain polyamic acid solution behind the polymerization reaction take place, specifically comprises:.
In the present invention; Said 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 two ether dianhydrides (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 does not have particular restriction to the mol ratio of this multiple dianhydride, and those skilled in the art can select according to the performance of target fibers, confirm.Said dianhydride is preferably one or more among PMDA, BPDA, TDPA and the ODPA.
In the present invention; Said 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 '-two (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-two (4-aminophenyl) pyrimidines (PRM) etc. can be wherein one or more; When being wherein multiple, the present invention does not have particular restriction to the mol ratio of this multiple diamines, and those skilled in the art can select according to the performance of target fibers, confirm.Said diamines is preferably one or more among ODA, MDA, PPD and the PABZ.
The present invention to said dianhydride and diamines with etc. mol ratio carry out polymerization.Be preferably 1:0.95 ~ 1.05, more preferably 1:1.
In the present invention, said aprotic solvent includes but not limited to dimethyl formamide (DMF), dimethylacetylamide (DMAc), dimethyl sulfoxide (DMSO) (DMSO), N-Methyl pyrrolidone (NMP) etc.
With the polyimide fiber of method for preparing is raw material, and its raw-material form is preferably cloth, felt, film, paper or silk.Said polyimides under protection of nitrogen gas, is carried out carbonization treatment, in high temperature furnace, accomplish.The temperature of carbonization is preferably 550 ℃ ~ 1000 ℃.
First kind of mode:
A11) polyimide fiber is heated to 300 ~ 350 ℃ of insulation 1h in nitrogen atmosphere, is heated to 400 ~ 450 ℃ of insulation 1h then;
A12) with 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 ℃ of per minutes in nitrogen atmosphere is warming up to 500 ℃ from room temperature;
A22) with step a21) heating after polyimide fiber continue to be heated to 550 ~ 1000 ℃, carbonization 1 ~ 5h obtains carbon fibre.
The carbon fibre that obtains after the carbonization need pass through activation processing, activation be one with polyimide fiber oxidation pore-creating process.According to the present invention; What activation was adopted is physically activated or chemical activation and physically activated process combined; Said physically activated preferred water steam is an activator; The activator that chemical activation uses is preferably phosphoric acid or phosphate, one or both in phosphate preferably phosphoric acid ammonium, diammonium hydrogen phosphate and the ammonium dihydrogen phosphate (ADP).Said phosphoric acid or phosphate are the aqueous solution, and concentration is 0.5wt% ~ 10wt%.Steps such as according to the present invention, if select chemical activation, the chemical activation step of that said polyimide fiber should be in before the carburising step, promptly wants earlier polyimide fiber to be carried out carbonization again through behind the chemical activation, and is physically activated.
According to the present invention, said polyimide fiber is physically activated in steam, and carry out according to following method: the carbon fibre that b11) step a) is obtained heats in water vapour, carries out activation processing; The temperature of said activation processing is 600 ~ 800 ℃.
Chemical activation then carries out as follows: polyimide fiber (cloth or felt) is flooded 10～60min in phosphoric acid or aqueous phosphatic, taking-up drains, then a) carbonization and step b) activation in steam set by step.The concentration of said phosphoric acid or aqueous phosphatic is preferably 0.5wt%～10wt%, and more preferably 1wt% ~ 8wt% most preferably is 4wt% ~ 6wt%.。
The fiber-reactive charcoal specific area that the present invention prepares is 900m
2/ g～2200m
2/ g, the product yield is 6wt%～38wt%.Fiber-reactive charcoal cloth intensity is 1.0MPa～6.1MPa; The intensity of fiber-reactive charcoal felt is 0.20MPa～0.60MPa.The intensity of active carbon and specific area have direct corresponding relationship.When therefore intensity being compared, the intensity level that can only get identical specific area compares.The polyimide fiber active carbon cloth of the present invention's preparation and the intensity of felt are more than 8 times of domestic several major vendor like product intensity.
Specific area of the present invention is to measure with the ASAP2420 type specific area tester that U.S. Merck & Co., Inc produces, and intensity is to measure with the WSM-100N type universal testing machine that intelligence instrument Co., Ltd in Changchun produces.
Characteristics of the present invention are that preparation technology is simple, with short production cycle, condition and range is wide, be easy to industrialization, product strength is high, can prolong the service life of fiber-reactive charcoal, have played the effect in expanded application field again.
Embodiment 1
Get 29.36g polyimides cloth, the stainless steel reaction pipe of the internal diameter 68mm that packs into is 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, in pipe, add water then, (adding water speed is 10.15 milliliters/gram sample * hour), activation 10 hours when being cooled to 300 ℃, stops to add water, and logical N
2Reduce to room temperature.Record the yield 21.9% of product at last, specific area is 900m
2/ g, slight 2.43MPa stretches.
Embodiment 2
Get the polyimides felt of 11.7g, at 300ml, soaked in 0.5% the ammonium phosphate solution one hour, taking-up drains, then with the stainless steel reaction pipe of its 68mm that packs into, at 99.999%N
2Protection is raised to 250 ℃ of half an hour from room temperature, constant temperature one hour down; 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 accomplishing carbonization.Activation is at N
2Under the atmosphere, be raised to 250 ℃ half an hour, constant temperature half an hour be raised to 650 ℃ then half an hour, stop N
2Add water, 650 ℃ of activation 6 hours, adding water speed was 4.69 milliliters/gram sample * hour, and when temperature dropped to 300 ℃, logical N cut off the water
2, and reduce to room temperature.The product yield that records at last is 31.6%, specific area 1080m
2/ g, TENSILE STRENGTH 0.51MPa.
Embodiment 3
Get the polyimides cloth of 34.84g, with in its internal diameter of packing into stainless steel reaction pipe that is 39mm and lead at N
2Protection be raised to 200 ℃ following half an hour, be raised to 300 ℃ and 400 ℃ with one hour respectively then, and constant temperature one hour, 400 ℃ be raised to 700 ℃ two hours, constant temperature one hour is accomplished carbonization.Activation is activation four hours under 675 ℃ temperature, and adding water speed is 397ml/h.The yield of the product that records at last is 10.4%, and specific area is 1357m
2/ g, TENSILE STRENGTH 1.11MPa.
Embodiment 4
Get the polyimides felt of 68.05g, in the internal diameter 68mm stainless steel reaction pipe of packing into, at N
2Under the protection of gas, be raised to 250 ℃ half an hour, be raised to 350 ℃ in one hour, constant temperature one hour was raised to 1000 ℃ in two hours, and constant temperature 4 hours is accomplished the carbonization experiment.In the 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 300 ℃ are raised to 700 ℃ of half an hour then, and constant temperature three hours, and the activation of water flowing steam 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
2Reduce to room temperature.The product yield 26.5% that records at last, specific area 1307m
2/ g, TENSILE STRENGTH 0.43MPa.
Embodiment 5
Get the polyimides cloth of 35.08g, the internal diameter of packing into is in the stainless steel reaction pipe of 39mm, and carbonization is operated like instance 3, cools to 500 ℃ after the carbonization, is raised to 700 ℃ from 500 ℃ half an hour then, when being warming up to 600 ℃, stops N
2Change water, adding water speed is 298ml/h.700 ℃ of constant temperature activation four hours.The product yield 10.3% that records at last, specific area 1529m
2/ g, TENSILE STRENGTH 0.95MPa.
Embodiment 6
Get the polyimides felt of 35.91g, in 1% (weight ratio) ammonium phosphate solution, soaked one hour, taking-up drains, carbonization, the logical embodiment 5 of activation act, and adding water speed is 284ml/h.Record product yield 12.7% at last, specific area 1504m
2/ g, TENSILE STRENGTH 0.42MPa.
Embodiment 7
Get the polyimides felt of 19.27g, the internal diameter of packing into is in the 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 is accomplished the 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 begin to add water, and adding water speed is 259ml/h, 700 ℃ of activation four hours are cooled to 300 ℃ and cut off the water, logical N
2, reduce to room temperature then.The product yield 6.1% that records at last, specific area 2186m
2/ g, TENSILE STRENGTH 0.31MPa.
Embodiment 8
Get 46.58g polyimides cloth, the internal diameter of packing into is in the 39mm stainless steel reaction pipe, at N
2Protect to be raised to 200 ℃ following half an hour, be raised to 300 ℃ and 400 ℃ with one hour respectively then, and 300 ℃ and 400 ℃ of each constant temperature one hour, 400 ℃ be raised to 550 ℃ two hours, constant temperature one hour is accomplished carbonization.Activation is 650 ℃ of activation 4 hours, and adding water speed is 355ml/h.The product yield 14.3% that records at last, specific area 1415m
2/ g, TENSILE STRENGTH 4.23MPa.
Embodiment 9
Get 36.28g polyimides cloth, in the internal diameter 39mm reaction tube of packing into, at N
2Under the protection of gas, be raised to 200 ℃ half an hour, be raised to 300 ℃, 400 ℃ and 550 ℃ with one hour respectively then, and 300 ℃, 400 ℃ and 550 ℃ of each constant temperature completion in hour carbonization.Be raised to 650 ℃ half an hour after the carbonization, and (stop logical N at 650 ℃ of feeding steam
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 fiber-reactive charcoal cloth of this result and domestic two main manufacturer production, and the specific area mean value of this two tame product is 1106m
2/ g, average strength are 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 the fiber-reactive charcoal have certain corresponding relation, have only the directly contrast of the approaching sample of specific area.
Embodiment 10
Get 23.08g polyimides felt, the internal diameter of packing into is in the 39mm reaction tube, at N
2Under the protection of gas, be raised to 250 ℃ half an hour, be raised to 350 ℃ in one hour, constant temperature was raised to 700 ℃ in one hour after one hour, and constant temperature was accomplished carbonization in three hours then.Activation experiment is at N
2Under the protection of gas, be raised to 300 ℃ half an hour, and constant temperature half an hour, with being raised to 700 ℃ from 300 ℃ half an hour, add water when being warmed up to 600 ℃ then, adding water speed is 251ml/h.700 ℃ of steam activations cool to 300 ℃ naturally after three hours, stop to add water, and logical N2 gas is reduced to room temperature.Product yield 17.4%, specific area 1248m
2/ g, the slight 0.40MPa that stretches, this intensity is viscose glue base fiber-reactive charcoal felt (the specific area 1209m of domestic certain manufacturer production
2/ g) 7.8 times of intensity 0.051MPa.
More than a kind of preparation method of fibre active carbon provided by the invention has been carried out detailed introduction; Having used concrete example among this paper sets forth principle of the present invention and embodiment; The explanation of above embodiment just is used for helping to understand method of the present invention and core concept thereof; Should be pointed out that for those skilled in the art, under the prerequisite that does not break away from the principle 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 claim of the present invention.
Claims (9)
1. preparation method of fibre active carbon is characterized in that comprising:
A) with polyimide fiber carbonization under the atmosphere of nitrogen, obtain carbon fibre;
B) with the activation in water vapour of said carbon fibre, obtain the fiber-reactive charcoal.
2. preparation method according to claim 1 is characterized in that step a) is specially:
A11) polyimide fiber is heated to 300 ~ 350 ℃ of insulation 1h in nitrogen atmosphere, is heated to 400 ~ 450 ℃ of insulation 1h then;
A12) with step a11) heating after polyimide fiber continue to be heated to 550 ~ 1000 ℃ of carbonization 1 ~ 5h, obtain carbon fibre.
3. preparation method according to claim 1 is characterized in that step a) is specially:
A21) polyimide fiber speed intensification with 2 ℃ of per minutes in nitrogen atmosphere is warming up to 500 ℃ from room temperature;
A22) with step a21) heating after polyimide fiber continue to be heated to 550 ~ 1000 ℃, carbonization 1 ~ 5h obtains carbon fibre.
4. according to any described preparation method of claim 1 ~ 3, it is characterized in that said polyimide fiber is: polyimides cloth or polyimides felt.
5. according to any described preparation method of claim 1 ~ 3, it is characterized in that, between step a), also comprise said polyimide fiber is handled through chemical activation.
6. preparation method according to claim 5 is characterized in that said chemical activation is specially
Polyimide fiber flooded 10 ~ 60min in phosphoric acid or phosphate solution after, take out, drain carbonization fully and steam activation usefulness.
7. preparation method according to claim 6 is characterized in that, said phosphate does, ammonium phosphate, diammonium hydrogen phosphate and ammonium dihydrogen phosphate (ADP) one or both.
8. preparation method according to claim 6 is characterized in that, the concentration of said phosphoric acid or aqueous phosphatic is 0.5wt% ~ 10wt%.
9. preparation method according to claim 1 is characterized in that step b) is specially:
B11) carbon fibre that step a) is obtained heats in water vapour, carries out activation processing; The temperature of said activation processing is 600 ~ 800 ℃.
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| CN114262646A (en) * | 2021-12-28 | 2022-04-01 | 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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| 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 |
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| 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 |
| CN114262646A (en) * | 2021-12-28 | 2022-04-01 | 山东中大药业有限公司 | Detergent for removing pesticide residues of traditional Chinese medicine plants and preparation method thereof |
| 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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