CN103920460A - Method for preparing high-performance biomass activated carbon fibers - Google Patents
Method for preparing high-performance biomass activated carbon fibers Download PDFInfo
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- CN103920460A CN103920460A CN201410143977.9A CN201410143977A CN103920460A CN 103920460 A CN103920460 A CN 103920460A CN 201410143977 A CN201410143977 A CN 201410143977A CN 103920460 A CN103920460 A CN 103920460A
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- nacf
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Abstract
The invention relates to a method for preparing high-performance biomass activated carbon fibers from a loofah sponge. The method comprises the following steps: (1) performing alkali treatment, namely soaking a cylindrical loofah sponge in an aqueous solution of sodium hydroxide for degumming, washing till the loofah sponge is neutral, and drying to obtain the dried loofah sponge subjected to alkali treatment; (2) modifying, namely mixing the dried loofah sponge subjected to alkali treatment with a water-soluble phenolic resin, fully impregnating for 24-48 hours, and drying after impregnation; (3) performing carbon activation, namely pre-oxidizing the modified loofah sponge at a certain temperature for 2 hours, and carbonizing the impregnated loofah sponge with inert protective gas, thereby obtaining biomass activated carbon fibers; and (4) performing after-treatment, namely soaking the biomass activated carbon fibers in dilute acid to remove ash in the product, washing by water till the product is neutral, and drying to obtain the high-performance biomass activated carbon fibers. Compared with a conventional method for preparing biomass activated carbon fibers, the method has the advantages that the preparation process is low in preparation cost, free of pollution and environmentally friendly, and the product is high in compressive strength and can serve as a filter material and an electrode.
Description
Technical field
The present invention relates to a kind of preparation method of active carbon, particularly a kind of agricultural products luffa that utilizes is for raw material, with the water-soluble phenolic resin modified high-performance biomass NACF of preparing.
Background technology
Sponge gourd (Luffa cylindria) has another name called day sieve wadding, day network and becomes melon etc., belongs to annual Curcurbitaceae and climbs up by holding on to vegetation.Sponge gourd divides general sponge gourd (Luffa cylindvica Roem) and has rib sponge gourd (Luffa acutangula Roxb), originate in India, be distributed widely in the torrid zone, subtropical zone and the Temperate Region in China in Asia, sponge gourd is one of vegetables in summer, therefore in China's Jiangsu-zhejiang Shanghai Area and Guangdong, Guangxi plantation is very general.Generally using tender melon as dish use, do the tasty and refreshing deliciousness of soup taste.Luffa (Vegetable Sponge of Luffa) has another name called sponge gourd net, day sieve line, day sieve muscle etc., it is the three-dimensional fiber tube bank that skin thick in the fruit after sponge gourd maturation and multidirectional fibrage form, three major polymers: cellulose, hemicellulose and lignin form, and its content of cellulose is up to more than 60%.At present, the research of luffa mainly concentrates on its medical value and prepares shower used in everyday, bath accessory.< < Compendium of Materia Medica > > records it and can lead to people's train of thought internal organs, and goes wind removing toxic substances, and detumescence is reduced phlegm, and Eradicates pain desinsection is controlled all blood sick.Aspect routine use article, existing multinomial invention, as luffa soap, luffa mattress, Luffa sponge cleaning brush, Loofah insole etc.
As from the foregoing, at present all also more original to the processing of luffa and treatment technology, mostly utilized its natural vascular structure.
The preparation of activated carbon from activated sludge fiber at present is mainly divided into two large classes, physically activated and chemical activation by activation method.
Physically activated most employing CO
2and steam.First biological material is prepared and become carbon base body under inert gas shielding, then at high temperature pass into CO
2or steam (steam need to pass through other inert gas carrier gas), pass through CO
2with steam, the etching action of carbon base body is formed to hole, thereby prepare absorbent charcoal material.Physically activated method can be prepared the active carbon of bigger serface, but physically activated needs reach very high activation temperature, could occur obvious activation effect, and temperature must reach more than 800 ℃, just can make the active carbon of bigger serface.This is very high to its experiment equipment requirement, and energy consumption is large, and because temperature is high, the productive rate of product is very low.
Chemical activation is to adopt chemical activating agent impregnated carbon material, thereby utilizes chemical activating agent at high temperature to react the method that makes active carbon material with material with carbon element.Chemical activation method is generally that carbonisation carries out together with activation process, has just constructed hole in carbonization.The drilling mechanism of chemical activating agent is generally: activator occupies physical space, and at high temperature etching carbon base body, finally gasifies and discharge.The activator that is mainly used as now chemical activation mainly contains: ZnC1
2, KOH, NaOH, H
3pO
4and K
2cO
3.It is lower that chemical activation is compared physically activated temperature conditions requirement, only need to maintain inert atmosphere, generally, below 900 ℃, just can obtain high performance active carbon.And due to the adding of chemical activating agent, the Surface Groups of Active Carbons content of preparation is abundanter, the active carbon of preparing has more functional.But adding of chemical activating agent likely makes activated carbon surface with special groups, likely the processing of some feature pollutants played to inhibitory action, the application of therefore also having limited to NACF.
Summary of the invention
Technical problem to be solved by this invention is that a kind of preparation method of high-performance biomass NACF is provided for the deficiency of above-mentioned prior art existence, the method has that cost is low, absorption property good, the feature of environmental protection, the product preparing, can keep original shape, and have good compression strength.
The present invention is that the technical scheme that the problem of the above-mentioned proposition of solution adopts is:
A high-performance biomass NACF preparation method, it comprises the steps:
1) alkali treatment: cylinder luffa is soaked and come unstuck in sodium hydrate aqueous solution, then clean to neutral, obtain the dried loofah of alkali treatment after oven dry;
2) modification: the dried loofah of alkali treatment is mixed with water soluble phenol resin, fully flood 24-48h, dipping is dried later;
3) carbonization-activation: first by the pre-oxidation 2h at a certain temperature of the luffa after modification, then, under inert protective gas, the luffa after dipping is carried out to carbonization-activation, obtain activated carbon from activated sludge fiber;
4) post processing: activated carbon from activated sludge fiber is soaked to remove the ash content in product with diluted acid, then be washed with water to neutrality, dry and obtain high-performance biomass NACF.
Press such scheme, the preparation technology of described luffa is: the vegetable silk melon and fruit after normal growth maturation is real, through natural air drying or after drying, cut into the long cylinder of 5～10cm, the sponge gourd seed of removing epidermis and hole inside, obtains cylinder luffa;
Press such scheme, the mass fraction of described sodium hydrate aqueous solution is 2%～5%.
Press such scheme, step 2) described in water soluble phenol resin solid content between 35%～37%.
Press such scheme, the temperature 160-200 ℃ of pre-oxidation described in step 3)
Press such scheme, the temperature 600-850 ℃ of charing described in step 3).
Press such scheme, the diluted acid described in step 4) is the conventional aqueous acids such as hydrochloric acid, sulfuric acid, acetic acid, nitric acid, and concentration is 0.5～1.5mol/L.
Press such scheme, step 2), the temperature of drying described in step 3) and step 4) is 100～105 ℃, the time is 10～20h.
For the high-performance biomass NACF that utilizes now living beings to prepare for raw material, the product majority preparing is all Powdered.Activated carbon from activated sludge fiber of the present invention is a kind ofly to take luffa as primary raw material, water soluble phenol resin modification, carry out again a kind of tubular active carbon that charing, activation, post processing form, the product preparing, well kept original form, there is certain compression strength, and in whole production process, do not produce any poisonous and hazardous material.
Principle of the present invention is: phenolic resins with come unstuck after luffa while mixing, a large amount of holes in luffa are filled by phenolic resins, thereby the hole of luffa is reduced, density increases, and also just means that intensity strengthens to a certain extent.Luffa is after water soluble phenol resin modification, rising along with carbonization temperature, together with the soft amorphous carbon that phenolic resins generation glass charcoal generates with luffa at high temperature can be grown in, fade away in interface, bond strength between two kinds of charcoals increases, and activated carbon from activated sludge resistant fiber Compressive Strength is increased; And the mechanical property of glass charcoal is better than amorphous carbon, glass charcoal is more, and compression strength is just higher.
Compared with prior art, the invention has the beneficial effects as follows:
The product sponge gourd ripening fruits of crops of take is prepared activated carbon from activated sludge fiber as raw material, opened up the kind of natural plants NACF raw materials and prepared approach, compare with the approach of preparing of existing activated carbon from activated sludge fiber, preparation technology is simple and clear, consuming time short, power consumption is few, preparation cost is low, and absorption property is good, reclaims and regenerates simple and convenient, there is certain compression strength, can be used as filtrate and electrode and use.
Plantation quantity at China's sponge gourd is huge, therefore utilize luffa to prepare activated carbon from activated sludge fiber for raw material exploitation, compare with technology with existing other raw materials, the feature that possesses cost low (economy), facility and environmental protection (cleaning), means, approach and the novelty for raising China activated carbon from activated sludge fiber, prepared are all significant.
Accompanying drawing explanation
Fig. 1 is process chart of the present invention.
Fig. 2 is the product iodine sorption value thermoisopleth of the embodiment of the present invention 1 preparation.
Fig. 3 is product iodine sorption value thermoisopleth prepared by comparative example.
Fig. 4 is the photo of the product high-performance biomass NACF of the embodiment of the present invention 1 preparation.
Fig. 5 is product photo prepared by comparative example.
The specific embodiment
In order to understand better the present invention, below in conjunction with specific embodiment, further describe content of the present invention, but content of the present invention is not only confined to the following examples.
In following embodiment, adopt the vegetable silk melon and fruit after normal growth maturation real, through natural air drying or after drying, cut into the long cylinder of 5～10cm, remove the sponge gourd seed of epidermis and hole inside, obtain cylinder luffa [the string vascular bundle cylinder (strong but pliable in texture) that inside interweaves and is netted].
Embodiment 1:
A preparation method for high-performance biomass NACF, it comprises the steps:
1) pretreatment: cylinder luffa is soaked in 2% sodium hydrate aqueous solution to 24h(and remove surperficial wax, ash content and other little molecules), then solution is filtered, luffa is cleaned repeatedly to neutrality, finally luffa is put into baking oven and dried 12h at 105 ℃, obtain the dried loofah of cylinder alkali treatment;
2) modification: taking out the dried loofah of above alkali treatment from baking oven, put into beaker, is 35% water soluble phenol resin toward adding solid content in beaker, fully submergence, more than dipping 24h, dipping luffa is later put into baking oven dries 12h at 105 ℃;
3) charcoal activation: the luffa after dipping is put into high temperature resistance furnace the inside, and pre-oxidation 2h at 200 ℃, then puts into high temperature resistance furnace the inside and carry out carbonization-activation, leads to protective gas N in high temperature resistance furnace
2, N
2speed be controlled at 0.6L/min, activation temperature is 850 ℃, obtains activated carbon from activated sludge fiber;
4) post processing: gained activated carbon from activated sludge fiber is soaked to 1h with 1M hydrochloric acid solution, to remove the ash content in product, the deionized water of reusable heat is extremely neutral by product cyclic washing, put into baking oven and dry 12h at 105 ℃, obtain activated carbon from activated sludge fiber (final products, sealing is stored in drier, standby).
In order better to show performance and the effect of this activated carbon from activated sludge fiber, it is carried out to iodine sorption value mensuration and compressive strength determination.
The assay method of iodine sorption value adopts the mensuration > > of GB < < GB/T7702.7-2008 ature of coal granular activated carbon experimental technique iodine sorption value to measure.According to adsorption isotherm, see Fig. 2, the E value while getting residual concentration c=0.02mol/L is iodine sorption value, calculates E=341.084mg/g.Pressure when intensity test adopts universal hydraulic testing machine test sample broken, compression strength P=198Mpa.
Comparative example:
Be with the difference of embodiment 1: (the NH that is 30% by mass concentration
4)
2hPO
4replace the water soluble phenol resin that solid content is 35%.
The assay method of iodine sorption value adopts the mensuration > > of GB < < GB/T7702.7-2008 ature of coal granular activated carbon experimental technique iodine sorption value to measure.According to adsorption isotherm, see Fig. 3, draw E value.E=471mg/g。
Embodiment 1 is compared known with comparative example, from iodine sorption value, both absorption properties are more or less the same, all there is good absorption property, but the product preparing in comparative example is pulverous, the product preparing in embodiment 1 can well maintain original form, also just makes the recovery of product and regenerates simple and convenient, there is certain compression strength, can be used as filtrate and electrode and use.That is to say, the high-performance biomass NACF product that the present invention prepares, owing to can maintaining this raw-material original form of luffa, has had the series of advantages such as compression strength is good, use is reclaimed conveniently, purposes is more extensive.
Embodiment 2:
A preparation method for high-performance biomass NACF, it comprises the steps:
1) pretreatment: cylinder luffa is soaked in 2% sodium hydrate aqueous solution to 24h(and remove surperficial wax, ash content and other little molecules), then solution is filtered, luffa is cleaned repeatedly to neutrality, finally luffa is put into baking oven and dried 12h at 105 ℃, obtain the dried loofah of cylinder alkali treatment;
2) modification: taking out the dried loofah of above alkali treatment from baking oven, put into beaker, is 35% water soluble phenol resin toward adding solid content in beaker, fully submergence, more than dipping 24h, dipping luffa is later put into baking oven dries 12h at 105 ℃;
3) charcoal activation: the luffa after dipping is put into high temperature resistance furnace the inside, and pre-oxidation 2h at 200 ℃, then puts into high temperature resistance furnace the inside and carry out carbonization-activation, leads to protective gas N in high temperature resistance furnace
2, N
2speed be controlled at 0.6L/min, activation temperature is 800 ℃, obtains activated carbon from activated sludge fiber;
4) post processing: gained activated carbon from activated sludge fiber product is soaked to 1h with 1M hydrochloric acid solution, and to remove the ash content in product, the deionized water of reusable heat to neutral, put into product cyclic washing baking oven and dried 12h at 105 ℃, obtains activated carbon from activated sludge fiber.
In order better to show performance and the effect of this activated carbon from activated sludge fiber, it is carried out to iodine sorption value mensuration and compressive strength determination.
The assay method of iodine sorption value adopts the mensuration > > of GB < < GB/T7702.7-2008 ature of coal granular activated carbon experimental technique iodine sorption value to measure.According to adsorption isotherm, the E value while getting residual concentration c=0.02mol/L is iodine sorption value, E=301.23mg/g.Pressure when intensity test adopts universal hydraulic testing machine test sample broken, draws compression strength, P=165Mpa.
Embodiment 3:
A preparation method for high-performance biomass NACF, it comprises the steps:
1) pretreatment: cylinder luffa is soaked in 2% sodium hydrate aqueous solution to 24h(and remove surperficial wax, ash content and other little molecules), then solution is filtered, luffa is cleaned repeatedly to neutrality, finally luffa is put into baking oven and dried 12h at 105 ℃, obtain the dried loofah of cylinder alkali treatment;
2) dipping: taking out the dried loofah of above alkali treatment from baking oven, put into beaker, is 35% water soluble phenol resin toward adding solid content in beaker, fully submergence, more than dipping 24h, dipping luffa is later put into baking oven at 105 ℃ of oven dry 12h;
3) charcoal activation: the luffa after dipping is put into high temperature resistance furnace the inside, and pre-oxidation 2h at 200 ℃, then puts into high temperature resistance furnace the inside and carry out carbonization-activation, leads to protective gas N in high temperature resistance furnace
2, N
2speed be controlled at 0.6L/min, activation temperature is 750 ℃, obtains activated carbon from activated sludge fiber;
4) post processing: gained activated carbon from activated sludge fiber product is soaked to 1h with 1M hydrochloric acid solution, and to remove the ash content in product, the deionized water of reusable heat to neutral, put into product cyclic washing baking oven and dried 12h at 105 ℃, obtains activated carbon from activated sludge fiber.
Embodiment 4:
Basic identical with example 1, difference is that the solid content of water soluble phenol resin is 35%, and the activation temperature of active carbon is 700 ℃.
Embodiment 5:
Basic identical with example 2, difference is that the activation temperature of active carbon is 650 ℃.
Embodiment 6:
Basic identical with example 2, difference is that the activation temperature of active carbon is 600 ℃.
Claims (9)
1. a high-performance biomass NACF preparation method, is characterized in that it comprises the steps:
1) alkali treatment: cylinder luffa is soaked and come unstuck in sodium hydrate aqueous solution, then clean to neutral, obtain the dried loofah of alkali treatment after oven dry;
2) modification: the dried loofah of alkali treatment is mixed with water soluble phenol resin, fully flood 24-48h, dipping is dried later;
3) charcoal activation: first by the luffa after modification at pre-oxidation 2h, then, under inert protective gas, the luffa after dipping is carried out to charing, obtain activated carbon from activated sludge fiber;
4) post processing: activated carbon from activated sludge fiber is soaked to remove the ash content in product with diluted acid, then be washed with water to neutrality, dry and obtain high-performance biomass NACF.
2. a kind of high-performance biomass NACF preparation method according to claim 1, the preparation technology who it is characterized in that described luffa is: the vegetable silk melon and fruit after normal growth maturation is real, through natural air drying or after drying, cut into the long cylinder of 5～10cm, the sponge gourd seed of removing epidermis and hole inside, obtains cylinder luffa.
3. a kind of high-performance biomass NACF preparation method according to claim 1, the mass fraction that it is characterized in that sodium hydrate aqueous solution described in step 1) is 2%～5%.
4. a kind of high-performance biomass NACF preparation method according to claim 1, is characterized in that step 2) described in water soluble phenol resin solid content between 35%～37%.
5. a kind of high-performance biomass NACF preparation method according to claim 1, is characterized in that the temperature 160-200 ℃ of pre-oxidation described in step 3).
6. a kind of high-performance biomass NACF preparation method according to claim 1, is characterized in that the temperature 600-850 ℃ of charing described in step 3).
7. a kind of high-performance biomass NACF preparation method according to claim 1, is characterized in that the diluted acid described in step 4) is a kind of or any several aqueous solution in hydrochloric acid, sulfuric acid, acetic acid, nitric acid.
8. a kind of high-performance biomass NACF preparation method according to claim 1, the concentration that it is characterized in that diluted acid described in step 4) is 0.5～1.5mol/L.
9. a kind of high-performance biomass NACF preparation method according to claim 1, is characterized in that step 2), the temperature of drying described in step 3) and step 4) is 100～105 ℃.
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Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104108713A (en) * | 2014-07-25 | 2014-10-22 | 哈尔滨工业大学深圳研究生院 | Preparation methods and application of porous carbon from towel gourd vegetable sponge and composite material of porous carbon |
| CN104692381A (en) * | 2015-03-04 | 2015-06-10 | 河南工程学院 | Preparation method of superhigh-specific-area activated carbon fibers |
| CN106219541A (en) * | 2016-07-29 | 2016-12-14 | 句容市百诚活性炭有限公司 | A kind of method utilizing dreg to prepare activated carbon |
| CN107128898A (en) * | 2017-06-27 | 2017-09-05 | 上海应用技术大学 | A kind of preparation method of day trailing plants muscle nitrogen-doped carbon nano material |
| CN107151015A (en) * | 2017-06-27 | 2017-09-12 | 上海应用技术大学 | A kind of preparation method of luffa nitrogen-doped carbon nano material |
| CN107180975A (en) * | 2017-06-30 | 2017-09-19 | 武汉理工大学 | A kind of modified biomass NACF cage air cathode and the microbiological fuel cell of assembling |
| CN107471773A (en) * | 2015-09-01 | 2017-12-15 | 蒋春花 | A kind of sandwich sheet and preparation method |
| CN107601673A (en) * | 2017-10-27 | 2018-01-19 | 盛世园林集团股份有限公司 | A kind of microbiological fuel cell for wastewater treatment couples compound flow constructed wetland system |
| CN108579782A (en) * | 2018-03-21 | 2018-09-28 | 武汉理工大学 | A kind of visible light-responded composite material and its preparation and application |
| CN109205620A (en) * | 2018-11-16 | 2019-01-15 | 大连理工大学 | A kind of carbon bionic nano material and preparation method |
| CN111261848A (en) * | 2018-11-30 | 2020-06-09 | 杭州怡莱珂科技有限公司 | Biological microcrystalline graphite-carbon nano-film carbon electrode and preparation method thereof and battery |
| CN114130355A (en) * | 2021-11-18 | 2022-03-04 | 中广核研究院有限公司 | Application of activated carbon fiber in preparation of gas adsorbing material or iodine filtering device, gas adsorbing material and iodine filtering device |
| CN114130355B (en) * | 2021-11-18 | 2024-05-03 | 中广核研究院有限公司 | Use of activated carbon fiber in preparation of gas adsorption material or in manufacturing iodine filtering device, gas adsorption material and iodine filtering device |
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| CN104108713B (en) * | 2014-07-25 | 2016-04-27 | 哈尔滨工业大学深圳研究生院 | A kind ofly come from the porous carbon of Vegetable Sponge of Luffa and the preparation method of matrix material thereof and application |
| CN104108713A (en) * | 2014-07-25 | 2014-10-22 | 哈尔滨工业大学深圳研究生院 | Preparation methods and application of porous carbon from towel gourd vegetable sponge and composite material of porous carbon |
| CN104692381A (en) * | 2015-03-04 | 2015-06-10 | 河南工程学院 | Preparation method of superhigh-specific-area activated carbon fibers |
| CN107471773A (en) * | 2015-09-01 | 2017-12-15 | 蒋春花 | A kind of sandwich sheet and preparation method |
| CN106219541A (en) * | 2016-07-29 | 2016-12-14 | 句容市百诚活性炭有限公司 | A kind of method utilizing dreg to prepare activated carbon |
| CN107128898A (en) * | 2017-06-27 | 2017-09-05 | 上海应用技术大学 | A kind of preparation method of day trailing plants muscle nitrogen-doped carbon nano material |
| CN107151015A (en) * | 2017-06-27 | 2017-09-12 | 上海应用技术大学 | A kind of preparation method of luffa nitrogen-doped carbon nano material |
| CN107180975A (en) * | 2017-06-30 | 2017-09-19 | 武汉理工大学 | A kind of modified biomass NACF cage air cathode and the microbiological fuel cell of assembling |
| CN107601673A (en) * | 2017-10-27 | 2018-01-19 | 盛世园林集团股份有限公司 | A kind of microbiological fuel cell for wastewater treatment couples compound flow constructed wetland system |
| CN108579782A (en) * | 2018-03-21 | 2018-09-28 | 武汉理工大学 | A kind of visible light-responded composite material and its preparation and application |
| CN109205620A (en) * | 2018-11-16 | 2019-01-15 | 大连理工大学 | A kind of carbon bionic nano material and preparation method |
| CN111261848A (en) * | 2018-11-30 | 2020-06-09 | 杭州怡莱珂科技有限公司 | Biological microcrystalline graphite-carbon nano-film carbon electrode and preparation method thereof and battery |
| CN111261848B (en) * | 2018-11-30 | 2021-03-23 | 杭州怡莱珂科技有限公司 | Biological microcrystalline graphite-carbon nano-film carbon electrode and preparation method thereof and battery |
| CN114130355A (en) * | 2021-11-18 | 2022-03-04 | 中广核研究院有限公司 | Application of activated carbon fiber in preparation of gas adsorbing material or iodine filtering device, gas adsorbing material and iodine filtering device |
| CN114130355B (en) * | 2021-11-18 | 2024-05-03 | 中广核研究院有限公司 | Use of activated carbon fiber in preparation of gas adsorption material or in manufacturing iodine filtering device, gas adsorption material and iodine filtering device |
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Application publication date: 20140716 |