CN103641113A - Preparation method of biomass-based formed activated carbon - Google Patents
Preparation method of biomass-based formed activated carbon Download PDFInfo
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Abstract
The invention discloses a preparation method of green and clean biomass-based formed activated carbon, and belongs to the field of material preparation. According to the invention, filamentous fungi are used as biomass-based carbon sources, and fruits are used as biological culture media; fruits are pretreated to obtain culture slurry; then filamentous fungi are added; constant temperature oscillation culture is carried out; the cultured slurry is poured into a forming container for solid-liquid separation so as to obtain a formed biomass matrix; the matrix is dried and carbonized to prepare fiber-state formed activated carbon with different forms and dimensions. The preparation process of the invention is simple and low in cost, adopts bacterial culture without introduction of toxic or harmful reagents, and thus prevents secondary pollution. The obtained activated carbon material has excellent carbon dioxide trapping performance of up to 7.3 mmol.g<-1> (25 DEG C, 1 bar) which is far better than that of various carbon materials reported recently.
Description
Technical field
The preparation method who the present invention relates to the clean biomass-based moulding activated carbon of a kind of green, belongs to biomass-based active carbon material preparation field.
Background technology
Moulding active carbon material has a large amount of pore textures and huge specific surface area, there is high adsorption capacity, mechanical strength is high, physical and chemical stability good, lost efficacy after the features such as regeneration is convenient, and be widely used in the frontier science and technology fields such as ultracapacitor, lithium cell, gas delivery, water body purification.
At present, for the conventional raw material of moulding activated carbon preparation, there are synthetic polymer, plant materials, animal body etc.Adopt synthetic polymer can prepare moulding activated carbon, cost is relatively high, and often needs to introduce caking agent, affects the physicochemical characteristics such as its stability, is unfavorable for scale operation and the application of material.（LOPEZ,M.,et?al.Carbon,1996,34,825.）（Martínez-Escandell,M.,et?al.Carbon,2008,46,384.）（
Kerstin,et?al.Materials?Letters,2007,61,2037.）（Liu,Zhenyu,et?al.Carbon,2004,42,423.）。Employing animal and plant body is raw material, and production process cost is low and clean.But the fine and close internal structure that is limited to natural formation, causes carbonized product ionic molecule conduction efficiency not high, and moulding carbon material overall dimensions are difficult to control.Also having the biomass such as the glucose of employing is raw material, prepares moulding activated carbon film, hydrogel and aerogel (Yu, Shu-Hong, et al.Advanced Materials, 2010,22,4691-4695; Advanced Functional Materials, 2011,21,3851; Angewandte Chemie International Education, 2012,51,5101.Liu Tianxi, et al.RSC Advances, 2013,3,14938.).But this method must be introduced template, has not only increased production cost, and knockout course can damage corpus fibrosum, is also unfavorable for the extensive preparation of moulding activated carbon.Nearly 2 years, Yu etc. further adopted bacteria cellulose assembling and high temperature cabonization to prepare carbon fiber aerogel (Yu, Shu-Hong, et al.NPG Asia Materials, 2012,4,1; Angewandte Chemie International Education, 2013,52,2925; Energy & Environmental Science, 2013, Advance Article; Advanced Materials, 2013,25,4746.).Yet the metabolic cycle of bacterium is longer, fermentation efficiency is on the low side, makes that bacteria cellulose preparation cycle is partially long and productive rate is lower.
Therefore, at present the utmost point need to be developed that a class cost is low, efficiency is high and be suitable for the novel preparation method of the moulding activated carbon that mass-producing implements.
Summary of the invention
The object of the invention is, for existing methodical deficiency, to propose a kind of preparation method of the novel forming activated carbon based on filamentous fungus cultivation-moulding-carbonization.
The preparation method that the present invention proposes, take filamentous fungus as biomass-based carbon source, adds in substratum, constant temperature culture, then pours filtrable container molding into and carries out solid-liquid separation, and the bacterium that obtains shaping assembles matrix, be dried to constant weight, then prepare biomass-based moulding activated carbon through carbonization.
The spore inoculating amount of described filamentous fungus in substratum is 10
6～10
7individual every milliliter.
Described substratum is obtained through boiling through the farm crop of squeezing the juice or be rich in sugar, starch based by the melon and fruit, greengrocery crop that are rich in moisture.
The described melon and fruit that is rich in moisture, greengrocery crop comprise watermelon, sugarcane; The described farm crop of being rich in sugar, starch based comprise muskmelon, beet, potato, taro, Chinese yam, lotus root, Ipomoea batatas, millet, mung bean, rice.
In described substratum, be also mixed with inorganic salt.
After the juice of squeezing out being filtered during preparation substratum, add water constant volume to 1L, the juice mass percent of squeezing out is 10-50%; Boiling object and water, according to mass ratio 1:3～1:10 boiling 30～60 minutes, add water constant volume again to 1L after filtration; In 1L substratum, also comprise SODIUMNITRATE 3g, dipotassium hydrogen phosphate 1g, magnesium sulfate MgSO
47H
2o0.5g, Repone K 0.5g, ferrous sulfate 0.01g.
Described filamentous fungus Wei Ge section belongs to one or more of filamentous fungus, comprises Aspergillus sp.F-1CGMCC No.5858, Penicillium Chrysogenum F1CGMCC No.5599.
The temperature that described filamentous fungus is cultivated is 5～37 ℃.
Described filamentous fungus is cultivated in standing or vibration environment and carries out, and hunting speed is for being no more than 200 rpms.
Described filamentous fungus incubation time is 24～108h.
Described carbonization comprises 400-2000 ℃ of calcining 1-24h, 160～250 ℃ of hydro-thermal 1-24h in inert atmosphere, or 180～250 ℃ of gas heat 1～24h.
Beneficial effect:
The present invention proposes the preparation method of the base molded activated carbon of a kind of novel biomass.At present, for the conventional raw material of moulding activated carbon preparation, there are synthetic polymer, plant materials, animal body etc.But often need in these methods to introduce the auxiliary agents such as caking agent or template, cost is high, be unfavorable for mass-producing application.The bacteria cellulose of employing based on opsonigenous substances prepared the technology that moulding carbon is up-to-date proposition, but its fermentation level is lower, yields poorly, and cost is still higher, and its Cheng Mo and forming technique still need to be broken through, at present generally only for biological medicine material.
Therefore, comprehensive more than, the present invention has following beneficial effect
(1) moulding carbon material preparation method cost proposed by the invention is low, pollution-free, and commercial application prospect is high.The conventional farm crop of main employing are substratum, carry out fungus culture and carbonization.The filamentous fungus proposing is fast culture in enormous quantities; cycle is only about 3 days, and without the introducing of poisonous and harmful reagent, gained filtrate is reusable; avoid secondary pollution and reduced production cost, be conducive to obtain on a large scale the industrialized implementation of moulding activated carbon.
(2) the moulding carbon material that the present invention prepares does not need to add any chemical assistant.By fungi solid-liquid separation after cultivating, can once stablize moulding, then drying carbonization prepares the moulding carbon material of different profiles and size, can adapt to the needs of different occasions, condition.
(3) the present invention can select according to carbonization technique, prepares corresponding mould material, hydrogel and aerogel.
(4) carbon material that prepared by the present invention has excellent collecting carbonic anhydride performance, can reach 7.3mmol g
-1(25 ℃, 1bar), be better than all kinds of moulding carbon materials of current bibliographical information.
Penicillium Chrysogenum F1 preserving number CGMCC No.5599, this bacterial strain has been submitted the biological preservation of patent in China Committee for Culture Collection of Microorganisms's common micro-organisms center (CGMCC) of No. 3 Institute of Microorganism, Academia Sinica of No. 1 institute in North Star West Road, Chaoyang District, city, 15 in December, 2011 BeiJing, China.
Aspergillus (Aspergillus sp.) F-1, preserving number is CGMCC No.5858, and in March, 2012, the preservation for patented procedure has been carried out at China Committee for Culture Collection of Microorganisms's common micro-organisms center (CGMCC) of 7 No. 3 Institute of Microorganism, Academia Sinica of No. 1 institute in North Star West Road, Chaoyang District, city, BeiJing, China.
Accompanying drawing explanation
Fig. 1 is the photo of bacterium aggregate in preparation process of the present invention; As seen from the figure, by pressure filtration molding, can obtain the fungi aggregate of specified shape size;
Fig. 2 is the pyrolysis behavior figure of dry rear bacterium aggregate in preparation process of the present invention; As seen from the figure, mainly there is thermosteresis in bacterium aggregate between 250～450 ℃, and this is mainly that the decomposition of thalline polymer causes;
Fig. 3 is photograph and the scanning electron microscope (SEM) photograph of the biomass-based moulding activated carbon prepared of the present invention; As seen from the figure, the carbon material of preparation has typical fibrous micro-nano structure (or one dimension micro-nano structure) and has very high anisotropy, as moulding activated carbon construction unit, not only can improve its mechanical property, and is conducive to the inner mass transfer of carbon body;
Fig. 4 is biomass-based moulding activated carbon collecting carbonic anhydride performance map prepared by the present invention; As seen from the figure, the carbon material of preparation is under 25 ℃, the condition of 1bar, and collecting carbonic anhydride performance reaches 7.3mmol g
-1.
Embodiment
Below in conjunction with embodiment, the present invention is further described, and can not limit the present invention.The mentioned bacterial strain of following Preparation Example is all preserved in Chinese common micro-organisms culture presevation administrative center.
Embodiment 1
The breeding of strains A spergillus sp.F-1 (CGMCC No.5858).Weigh the potato chopping that 200g cleans up, then add the deionized water of general a liter and boil 30 minutes.Then utilize 8 layers of gauze to filter.Deionized water constant volume is to 1L again, and sterilizing 20 minutes is standby in 115 ℃ of high-pressure sterilizing pots.Collect the fungal spore of dull and stereotyped cultured " Aspergillus sp.F-1 ", by 10
6-10
7the inoculum size of individual every milliliter, is inoculated in the substratum of sterilizing, and the shaking table that is then placed in 175 revs/min 37 ℃ of rotating speeds is cultivated 3 days, obtains desired mycelium.
Embodiment 2
Bacterial strain Penicillium Chrysogenum F1(CGMCC No.5599) breeding.Get sugar cane crushing and filter, obtain 200 milliliters of juice, be mixed to get nutrient solution with following inorganic salt: SODIUMNITRATE 3g, dipotassium hydrogen phosphate 1g, magnesium sulfate MgSO
4.
7h
2o0.5g, Repone K 0.5g, ferrous sulfate 0.01g, distilled water constant volume is to 1L.Heating for dissolving, 121 ℃ of sterilizing 20min after packing.Collect the fungal spore of dull and stereotyped cultured " Penicillium Chrysogenum F1CGMCC No.5599 ", by 10
6-10
7the inoculum size of individual every milliliter, is inoculated in the substratum of sterilizing, and the shaking table that is then placed in 175 revs/min 37 ℃ of rotating speeds is cultivated 3 days, obtains desired mycelium.
Embodiment 3
The preparation of carbon film.Pipette the 6.5mg mL of the 250mL that embodiment 1 prepares
-1aspergillus sp.F-1, adopt the Büchner funnel of diameter 30cm to obtain a filter cake by vacuum filtration mode, in the convection oven of 80 ℃, after dry 12h, take out, obtain fiber state carbon film presoma.This presoma is placed in body of heater to 5 ℃ of min of time variable control
-1after being warming up to 800 ℃, be incubated 1h, obtain fiber state carbon film.
Embodiment 4
The preparation of carbon aerogels.Pipette the 6.5mg mL of the 1000mL that embodiment 1 prepares
-1aspergillus sp.F-1, adopt the sand core funnel of diameter 5cm to obtain a fungi hydrogel by vacuum filtration mode, in-15 ℃, vacuum-drying is 2 days, obtains fiber state carbon aerogels presoma.This presoma is placed in body of heater to 5 ℃ of min of time variable control
-1after being warming up to 800 ℃, be incubated 1h, obtain fiber state carbon aerogels.
Embodiment 5
The preparation of carbon aerogels.Pipette the 6.5mg mL of the 100mL that embodiment 1 prepares
-1aspergillus sp.F-1, use excess ethyl alcohol replacing water, then with excessive ether displacement ethanol, adopt the sponge plastics filter screen of diameter 2cm to obtain a fungi gel by gravity filtration mode, vacuum-drying 1h in 80 ℃, obtains fiber state carbon aerogels presoma.This presoma is placed in body of heater to 5 ℃ of min of time variable control
-1after being warming up to 800 ℃, be incubated 1h, obtain fiber state carbon aerogels.
Embodiment 6
The preparation of carbon hydrogel.Pipette the 6.5mg mL of the 1000mL that embodiment 1 prepares
-1aspergillus sp.F-1, adopt the sand core funnel of diameter 5cm to obtain a fungi hydrogel by vacuum filtration mode.With teflin tape, wrap after fungi hydrogel, will wrap body and be placed in sealing in polytetrafluoroethyltank tank, and fix with stainless steel and iron, then reaction system is placed in 200 ℃ of stoves, after reaction 12h, obtain fiber state carbon hydrogel.
Fiber base carbon aerogels can be used for the efficient adsorption of greenhouse gases carbonic acid gas.Adopt the U.S. ASAP2050 of Merck & Co., Inc gas adsorption determinator detection fibers base carbon aerogels absorption property.First 150 degrees Celsius of vacuum outgass 24 hours before absorption.25 degrees Celsius of absorption and control temperature, absorption-desorption pressure range is 0-1bar.As shown in Figure 4, fiber base carbon aerogels has excellent absorption property to carbonic acid gas.When air pressure rises to 1bar, carbon dioxide adsorption can reach 7.3mmol g-1.In simulated condition, sorbent material is generally no more than 6mmol g-1 to carbon dioxide adsorption preferably.When air pressure is down to 0.004bar, the amount of carbon dioxide in aerogel when boosting quite, show that fiber base carbon aerogels not only has high adsorption capacity, also possessed superior desorption of gases ability.
Claims (10)
1. the preparation method of a biomass-based moulding activated carbon, it is characterized in that, take filamentous fungus as biomass-based carbon source, add in substratum, constant temperature culture, then pours filtrable container molding into and carries out solid-liquid separation, and the bacterium that obtains shaping assembles matrix, be dried to constant weight, then prepare biomass-based moulding activated carbon through carbonization.
2. preparation method according to claim 1, is characterized in that, the spore inoculating amount of described filamentous fungus in substratum is 10
6～10
7individual every milliliter.
3. preparation method according to claim 1, is characterized in that, described substratum is obtained through boiling through the farm crop of squeezing the juice or be rich in sugar, starch based by the melon and fruit, greengrocery crop that are rich in moisture.
4. preparation method according to claim 3, is characterized in that, is also mixed with inorganic salt in substratum.
5. according to the preparation method described in claim 3 or 4, it is characterized in that, after the juice of squeezing out is filtered, add water constant volume to 1L, the juice mass percent of squeezing out is 10-50%; Boiling object and water, according to mass ratio 1:3～1:10 boiling 30～60 minutes, add water constant volume again to 1L after filtration; In 1L substratum, also comprise SODIUMNITRATE 3g, dipotassium hydrogen phosphate 1g, magnesium sulfate MgSO
47H
2o0.5g, Repone K 0.5g, ferrous sulfate 0.01g.
6. preparation method according to claim 1, it is characterized in that, described filamentous fungus Wei Ge section belongs to one or more of filamentous fungus, comprises Aspergillus sp.F-1CGMCC No.5858, Penicillium Chrysogenum F1CGMCC No.5599.
7. preparation method according to claim 1, is characterized in that, the temperature that described filamentous fungus is cultivated is 5～37 ℃.
8. preparation method according to claim 1, is characterized in that, described filamentous fungus is cultivated in standing or vibration environment and carries out, and hunting speed is for being no more than 200 rpms.
9. preparation method according to claim 1, is characterized in that, described filamentous fungus incubation time is 24～108h.
10. preparation method according to claim 1, is characterized in that, described carbonization comprises 400-2000 ℃ of calcining 1-24h, 160～250 ℃ of hydro-thermal 1-24h in inert atmosphere, or 180～250 ℃ of gas heat 1～24h.
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