CN104692378A - Bamboo-based macroporous biological activated carbon and preparation method thereof - Google Patents
Bamboo-based macroporous biological activated carbon and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a bamboo-based macroporous biological activated carbon and a preparation method thereof. The method comprises the following steps: mixing and briquetting bamboo and a bonding agent, charing, introducing an activator for an activation reaction to obtain the bamboo-based macroporous biological activated carbon. In the above method, the activator is selected from at least one of vapor, carbon dioxide, oxygen and air; and the bonding agent is selected from one of coal tar, coal tar pitch, wood tar, phenolic resin, furfural resin and paper pulp waste liquid or the bonding agent is without the bonding agent. The usage amount of the bonding agent accounts for 0-35% of bamboo mass, and can be increased and decreased according to the requirement of the activated carbon products. The usage amount of the activator is 0.1kg-1kg/h, in the charing step, temperature is 450-600 DEG C, and time is 0.5-2.5 hours. The biological activated carbon has beneficial effect of adsorption function and easy regeneration.
Description
Technical field
The present invention relates to a kind of bamboo base macropore biological activated carbon and preparation method thereof.
Background technology
Biological activated carbon (BAC) technology has obtained a wide range of applications and has obtained good result in the advanced water treatment process of China: rely on synergy that is biological and gac to extend the life-span of gac
[1] [2], reducing cost of harnessing the river, providing strong technical support for carrying out GB5749-2006 " drinking water sanitary standard ", thus paved road for the popularization of further treatment technique centered by biological activated carbon.But there is a technical bottleneck in biological activated carbon (BAC): when water temperature is lower than 11 DEG C, its treatment effect just declines [3].China is vast in territory, and the area of water temperature≤11 DEG C is quite large.If this problem does not solve, this technology can be made undoubtedly to be restricted in the popularization of northern China.
The major cause that biological activated carbon (BAC) meets the decline of subzero treatment effect is: the gac that BAC is used at present is all developed based on adsorption function, its pore texture is based on micropore, without macropore (diameter > 0.1 μm), therefore microorganism can only be attached on the outside surface of gac, thus cause extraneous water temperature larger on its impact.In addition, the treatment effect of biological activated carbon not only depends on that the performance (adsorptive capacity) of gac also depends on the amount of the microorganism that gac holds, and particularly uses the later stage (after being generally half a year), when biological action becomes to take as the leading factor, all the more so.Improve biological loading amount and just must improve the surface-area that can hold microorganism, research shows, the outer surface area of gac is extremely limited, and its dimensional unit is cm
2/ cm
3, and the specific surface area that macropore provides can reach m
2/ cm
3degree.Be afraid of the technical bottleneck of low temperature to solve biological activated carbon (BAC) and the more surface for microorganic adhesion is provided, this seminar have developed biological activated carbon (BAC) gac-macropore biological activated carbon, its maximum diameter of hole reaches tens to hundreds of micron, thus to come in and go out gac hole procreation provides " livable " condition for microorganism: reduce outside temperature to the impact of microorganism active, improve the loading amount of microorganism on units activity charcoal, this will be conducive to solving China biological activated carbon technical barrier that reduces of (<11 DEG C) effect at low temperatures.
The relevant research of Japan illustrates: this microorganism entering macropore can the treatment effect of (19.6 DEG C) under (1 DEG C, 3.6 DEG C) have normal temperature at low temperatures, its pilot experiment carries out in Hokkaido (Heilongjiang Province corresponding to China) university of Japan, the 2 years by a definite date time (on November 1,31 days to 1996 October in 1994), result shows: under the condition of water temperature 1 DEG C, adopts PICABIOL gac to make NH
3-N is almost completely oxidized
[4].PICA is a gac manufacturers, and PICABIOL is the registered trademark of its gac used for purifying drinking water.
This bacterium-sized that can enter gac macropore has much, is by the K.GAID of France the earliest
[7]propose, its mean sizes is 1 ~ 2 μm × 0.5 μm.These bacteriums to enter the micropore of gac and mesopore obviously, nor can enter all macropores of gac.The hole that only has those microorganisms to enter (also or surface that can be close) is only effective.Therefore find out this threshold value, and produce the product (biological activated carbon gac) that this active porosity accounts for main composition this technology of biological activated carbon just can be made more perfect.
Reference
[1]Wang，B.Z.Yin，J.et al.，A Preliminary Study on Efficiency and Mechanism ofTHMs Removal in Ozonation and BAC Processes[J].Ozone Science&.Engineering.2010,6（4）：261.
[2] Liu Jianguang, Zhang Chunyang, looks into people's light etc. and the drinking water advanced treatment process activity charcoal cycle of operation inquires into [J]. water supply and drainage, 2011,37(5): 35 ~ 40
[3] Zhou Yunluo, Qi Da, Wang Zhansheng, Yu Qing. ozone one bioactive carbon technique and biological action research [J] thereof. Shanghai water utilities, 2003,19 (4): 5-8.
[4] large bamboo hat with a conical crown and broad brim is former stretches Jie. for the wooden of ozone charcoal process and ature of coal granulated active carbon [J]. and water channel association magazine (day), 1997,66 (12): 20-29.
[5]www.picacarbon.com.Email:contact-Pica@veoliawater.com
[6] yellow development. activated carbon technology basis [M]. Beijing: weapon industry press, 2006.
[7] K.GAID. carries out the mechanism [J] of biopurification on the activated carbon. wate research (method), 1982,16 (1): 7-17.
Summary of the invention
Be afraid of the technical bottleneck of low temperature to solve biological activated carbon (BAC) and provide how applicable microorganism growth to multiply, for the surface of microorganic adhesion, solve China biological activated carbon technical barrier that reduces of (<11 DEG C) effect at low temperatures, the invention provides a kind of bamboo base macropore biological activated carbon and preparation method thereof.
The method preparing bamboo base macropore biological activated carbon provided by the invention, comprises the steps:
Wherein, method one comprises the steps:
By bamboo chip and caking agent mixing briquetting, after charing, pass into activator and carry out priming reaction, obtain described bamboo base macropore biological activated carbon;
Method two comprises the steps:
By bamboo chip briquetting, after charing, pass into activator and carry out priming reaction, obtain described bamboo base macropore biological activated carbon.
In aforesaid method, described activator is all selected from least one in water vapour, carbonic acid gas, oxygen and air;
Described caking agent is selected from least one in coal tar, coal-tar pitch, wood tar oil, resol, furfuryl resin and spent pulping liquor.
In described method one, the consumption of caking agent is the 0-35% of bamboo quality, is specially 25%, 33% or 25-33%, and the consumption of described caking agent is not 0;
In described method one and two, the consumption of activator is 0.1kg/h-1kg/h, is specially 0.4kg/h, 0.6kg/h, 1kg/h, 0.4-0.6kg/h or 0.6-1kg/h.Depending on activated carbon product requirement and increase and decrease.
In described carbonization, temperature is 450-600 DEG C, is specially 500 DEG C, 550 DEG C, 500-550 DEG C; Time is 0.5-2.5 hour, is specially 1.5 hours, 1.8 hours or 1.5-1.8 hour; Carbonization process essence is that the thermopolymerization of open loop material becomes condensed ring and forms the process of hole blank.
In described activation step, temperature is 700-1000 DEG C, is specially 800 DEG C, 850 DEG C, 800-850 DEG C; Time is 1-3.5 hour, is specially 2 hours, 3 hours, 2-3 hour.Reactivation process is then the oxidation capacity relying on gas under high temperature, removes hole middle reaches make pore former process from charcoal.
The bamboo base macropore biological activated carbon prepared according to the method described above, also belongs to protection scope of the present invention.
Wherein, the aperture of described bamboo base macropore biological activated carbon is 0.3nm-400 μm;
Aperture is greater than
the pore volume in the hole ratio that accounts for pore volume porose in described bamboo base macropore biological activated carbon be 30-70%, be specially 61.6%.
The application of bamboo base macropore biological activated carbon in water treatment that the invention described above provides, also belongs to protection scope of the present invention.
Wherein, described water is feedwater.Described water treatment is except the organic pollutant in anhydrating.
The present invention both can provide cylindrical activated carbon, can provide broken charcoal and Powdered Activated Carbon again.
Owing to have employed technical scheme provided by the present invention, described in principle of work of the present invention and working process, make the present invention compared with existing known technology, thus obtain following beneficial effect:
1, because raw materials of the present invention is renewable energy source, thus obtain economize on resources, the beneficial effect of Sustainable development.
2, because the present invention comprises micropore, mesopore and macroporous structure, thus the beneficial effect that microbial metabolites is tightly held by activated carbon again is obtained.
3, because the present invention comprises mesopore and macroporous structure, thus the beneficial effect making gac have more multi-transfer-channel is obtained.
4, because the present invention comprises macroporous structure, thus the beneficial effect of the specific surface area larger compared with gac outside surface is obtained.
5, because the present invention comprises micron order macroporous structure, thus the beneficial effect making microorganism enter gac internal surface and reduction extraneous thermal effect is obtained.
6, due to described in 4,5 of the present invention, thus the beneficial effect of higher biological loading amount is obtained.
7, because the present invention comprises micropore and central hole structure, thus the beneficial effect making biological activated carbon have adsorption function concurrently is obtained.
8, because hole of the present invention is comparatively large, thus the beneficial effect that saturated activity charcoal is easy to regeneration is obtained.
9, due to described in above each bar of the present invention, thus the beneficial effect of " utilizing biological activated carbon pore texture to select biological activated carbon gac " new approaches is obtained.
10, due to described in new approaches of the present invention, thus the beneficial effect providing " biological activated carbon gac " product innovation under these new approaches instruct, make contributions for technical progress of industry is obtained.
12, due to described in above each bar of the present invention, thus the beneficial effect overcoming and solve the many deficiencies, defect and the drawback that exist in existing known technology is obtained.
13, due to described in above each bar of the present invention, thus the water treatment that the gac obtaining application and have " biological activated carbon pore texture " carries out taken into full account microorganism practical factor, " livable " condition be provided for it, reach biological degradation effect thoroughly and the beneficial effect such as the object economized on resources to the greatest extent.
14, because design science of the present invention is reasonable, effect stability reliable, thus cost of manufacture beneficial effect low, easy to utilize is obtained.
Accompanying drawing explanation
Fig. 1 is the electron micrograph (500X) of the macropore in macropore biological activated carbon
Fig. 2 is mesopore, microporosity electron micrograph contrast (1000X) of biological activated carbon gac.
Fig. 3 is the N of gac
2absorption/desorption isotherm.
Fig. 4 is the activated carbon capillary pore size distribution curve that H-K method calculates.
Fig. 5 is the gac mesopore pore volume integral distribution curve that BJH method calculates.
Fig. 6 is the gac mesopore pore size distribution plan that BJH method calculates.
Fig. 7 is the accumulation macro-pore size dis-tribution curve of the gac that mercury penetration method calculates.
Fig. 8 is the gac macropore pore size distribution curve that mercury penetration method calculates.
Embodiment
Below in conjunction with specific embodiment, the present invention is further elaborated, but the present invention is not limited to following examples.Described method is ordinary method if no special instructions.Described starting material all can obtain from open commercial sources if no special instructions.
Embodiment 1,
Briquetting after bamboo chip and caking agent coal tar being mixed with the ratio of mass ratio 8:2, carries out charing after 1.8 hours in 500 DEG C, under the high temperature of 850 DEG C, carries out priming reaction (C+H with 0.8kg water vapour
2o → CO+H
2and C+CO
2→ 2CO) 2.0 hours, obtain bamboo base macropore biological activated carbon provided by the invention.
Institute goes out product and is finished product, can carry out corresponding aftertreatment, as fragmentation, grinding etc. according to customer demand.
After this products production, carry out biological activity absorption and the flushing test of gac pillar, through certification test, obtained the good result of expection.
The sign of the biological large mesoporous activated carbon of embodiment 1 gained bamboo base
Experiment
1.1 raw materials, reagent and instrument
FEI Quanta200 type environmental scanning electron microscope (ESEM), company of FEI Czech; The full-automatic specific surface area of Autosorb-iQ2-MP type and lacunarity analysis instrument, Merck & Co., Inc of the U.S.; The full-automatic mercury injection apparatus of AutoPore IV9500 high-performance, Merck & Co., Inc of the U.S.; Electronic analytical balance, Shanghai.
The sign of 1.2 gacs
Iodine sorption value and the methylene blue adsorption value of gac measure according to GB/T12496.8-1999 and GB/T12496.10-1999; The surface topography of gac is analyzed with environmental scanning electronic microscope (ESEM); The pore texture of gac mesopore, micropore adopts specific surface area and lacunarity analysis instrument to measure; The macropore test of gac adopts mercury penetration method to carry out according to GB-T%2021650.1-2008.
Result and discussion
2.1 Study on adsorption properties
Gac removes the superior adsorbent of organic pollutants, and the absorption property of gac is except outside the Pass having with starting material, technological process, and also huge with it specific surface area, pore volume, hydrophobicity are relevant.The adsorptive power of gac and absorption behavior, characterize usually through its absorption to methylene blue, honey, iodine etc.In water treatment, iodine number (I) and methylene radical blue value (MB) are two important indicators characterizing activated carbon pore structure.Iodine molecule can only enter the true micropore of gac, and in the secondary micropore that methylene blue molecular energy enters gac and mesopore, the adsorptive value of methylenum coeruleum is high, then remove the effective of stink.Methylenum coeruleum adsorptive value >=the 180mg/g of regulation granulated active carbon, iodine number >=950mg/g in CJ/T345-2010 " Drinking Water water purification plant coal mass active carbon ".
The iodine number of embodiment 1 gained bamboo base macropore biological activated carbon is 1074mg/g, and be greater than 950mg/g, methylene radical blue value is 195mg/g, is greater than 180mg/g; Intensity is 95%, reaches more than 90%, and namely the leading indicator of this gac all meets the technical requirement of CJ/T345-2010 " Drinking Water water purification plant coal mass active carbon ".
2.2 electron microscopic observation
The high adsorption capacity of gac, mainly because it contains flourishing pore texture, carries out microcosmic observation by scanning electron microscope (SEM) to gac, not only can see the characteristic of activated carbon surface, clearly can also see pore texture.This experiment adopts FEI Quanta200 type environmental scanning electron microscope (ESEM), under high vacuum pattern (30KV), observes from the angle of microcosmic the pattern of bamboo bits gac and bamboo chip gac and pore structure characteristic.
Specific operation process is as follows: by pretreated activated carbon sample, paste in sample disc with conductive resin, put into spraying plating instrument metal spraying 60S, then sample disc is fixed on after on scanning electron microscope Stage microscope, adjusting focal length, contrast gradient, choose suitable view, observes heterogeneous microstructure, and take pictures under certain magnification, scanning result is as shown in Figure 1 and Figure 2.
As can be seen from electron micrograph Fig. 1 and Fig. 2 of gac, the surface of gac all forms hole not of uniform size, and the structure in hole has round, slit-type and irregular type.This some holes not only plays the effect of transport passage in adsorption process, can also play good capillary condensation effect, considerably increase the adsorptive power of gac
2.3 nitrogen adsorption desorption isotherms are analyzed
Nitrogen adsorption-the desorption isotherm obtained under the liquid nitrogen temperature of 77K is the important means of Study On The Activated Carbon pore texture and charcoal absorption interaction of molecules process.Adsorption isothermal line is the specific descriptions of adsorption phase nanoreactor, and different adsorption isotherm thread shape corresponds to different adsorption mechanism, correctly judges thermoisopleth type, is very important for calculating sorbent material parameter of pore structure.By activated carbon sample at 120 DEG C after normal pressure and vacuum-drying, in the specific surface area and pore distribution instrument (Autosorb-iQ2-MP) of Kang Ta company of the U.S., carry out under 77K sample N2 adsorption desorption test.Within 1985, common thermoisopleth is divided into 6 classes with application federation IUPAC by international pure chemistry.The comparative analysis of adsorption isothermal line and Standerd isotherm by experiment, determines isothermal type, contributes to the understanding to adsorption process essence.The adsorption/desorption isotherms of two kinds of gacs as shown in Figure 3.
Fig. 3 result shows, the thermoisopleth of macropore biological activated carbon belongs to the mating type of I type and II type, adsorptive capacity sharply rises along with the increase of relative pressure at the beginning, adsorption rate is very fast, when relative pressure reaches 0.04, adsorptive capacity tends towards stability gradually, owing to containing a small amount of mesopore and macropore in sample, absorption platform non-horizontal, but have the offset level line of certain slope, and desorption curve does not overlap with adsorption curve, has obvious hysteresis, show in gac, have kapillary coacervation to occur, namely gac has mesopore to exist; When relative pressure is greater than 0.9, the adsorption isothermal line of gac has " de-tail " phenomenon, illustrates in gac to there is macropore.
2.4 specific surface areas and pore distribution test (macropore, in, micropore)
According to peaceful (DUBININ) partitioning of USSR (Union of Soviet Socialist Republics) academy of sciences academician Doby, the Pore classification of gac is as follows: micropore
mesopore
macropore
micropore can be divided into true micropore again
with secondary micropore
the peaceful academician of Doby also points out that the gac of research and production time micropore prosperity is the vital task of gac worker.For understanding specific surface area size and the pore volume distribution situation of two kinds of gacs, this experiment adopts the specific surface area of Kang Ta company of the U.S. and pore distribution instrument (Autosorb-iQ2-MP) and mercury injection apparatus respectively, measures respectively to the mesopore of these two kinds of gacs, micropore and macropore.By the adsorption isothermal line recorded, by BET method calculated specific surface area; Mesopore volume distribution is calculated by BJH method; Micropore size distribution is calculated by HK method; Micropore volume is drawn by t-plot method; Macro-pore size dis-tribution is provided by mercury penetration method.By N under 77K
2the pore structure parameter that adsorption isothermal line and mercury penetration method calculate is shown in Table 2.
The BET specific surface area of table 2, the large mesoporous activated carbon of this embodiment gained bamboo base and pore volume distribution
From the data of table 2, this gac all has flourishing pore texture, and especially macropore and microvoid structure, its total hole volume is: 1.3061ml/g, and the ratio that it is big or middle, the pore volume of micropore accounts for total hole volume is respectively: 61.6%, 6.7%, 31.7%.Its concrete void distribution will describe in detail below.
2.4.1 micropore size distribution
Fig. 4 is according to N
2suction/desorption isotherm, adopts the micropore size distribution curve that H-K method calculates.As seen from the figure, the micropore of this gac is multimodal distribution, and peak pore diameter is respectively 0.55nm, 1.25nm, 1.55nm.
2.4.2 mesopore pore size distribution
See shown in Fig. 5, Fig. 6 with the mesopore pore size distribution curve that BJH method calculates.
As shown in Figure 5, wherein pore distribution curve is unimodal dispersion substantially, and peak pore diameter is 4nm, and wherein pore distribution scope is comparatively wide, all has more distribution at diameter 4 ~ 30nm.From gac mesopore pore volume cumulative distribution table (Fig. 6), to 30nm from diameter 4nm, the pore volume of its mesopore increases sharply, almost constant more than its volume after 30nm.
2.4.3 macropore diameter distribution
The mesopore larger for aperture and macropore cannot be determined by absorption method, adopt mercury penetration method can determine the pore size distribution in this part hole.Adopt the large pore distribution of AutoPore IV9500 high-performance full-automatic mercury injection apparatus (Merck & Co., Inc of the U.S.) gac to test, this instrument can survey the hole of pore diameter range 0.003 to 1000 μm, and it enters mercury or mercury ejection volume accuracy is better than 0.1 μ L.
Testing method is as follows: first, is placed in by sample in vacuum drying oven, dries 1 hour under 150 DEG C of conditions, then before opening oven door, first recharges dry nitrogen, and avoid it again to contact with air; After sample cooling, sample and test.The macropore accumulation pore distribution curve of gac and macropore diameter distribution curve are respectively as shown in Figure 7, Figure 8.
Fig. 8 is the gac macropore pore size distribution curve that mercury penetration method calculates.As shown in Figure 8, the macropore of this gac claims multimodal to distribute, and being wherein less than 7 μm of scopes at diameter has a wider peak distribution, and integrated distribution is between 0.3 μm to 3 μm; Between 7 μm and 80 μm, the hole of gac then presents the distribution of trough shape; In aperture, 80 μm within the scope of 0.1 μm, and this gac presents multimodal distribution at 190 μm, 250 μm, 310 μm places.
Embodiment 2
Briquetting after bamboo chip and caking agent coal tar, coal-tar pitch being mixed with the ratio of mass ratio 7.5:1.5:1, carries out charing after 1.5 hours in 550 DEG C, under the high temperature of 800 DEG C, carries out priming reaction 3.0 hours (C+H with 1.8kg water vapour
2o → CO+H
2and C+CO
2→ 2CO), generate the internal pore structure of the prosperity required by absorption, obtain bamboo base macropore biological activated carbon provided by the invention.
Institute goes out product and is finished product, can carry out corresponding aftertreatment, as fragmentation, grinding etc. according to customer demand.
The iodine number of this embodiment gained bamboo base macropore biological activated carbon is 1104mg/g, and be greater than 950mg/g, methylene radical blue value is 206mg/g, is greater than 180mg/g; Intensity is 92%, reaches more than 90%, and namely the leading indicator of this gac all meets the technical requirement of CJ/T345-2010 " Drinking Water water purification plant coal mass active carbon ".
Embodiment 3
By direct for bamboo chip briquetting, carry out charing after 1.5 hours in 550 DEG C, under the high temperature of 850 DEG C, carry out priming reaction 3.0 hours (C+H with 3kg water vapour
2o → CO+H
2and C+CO
2→ 2CO), generate the internal pore structure of the prosperity required by absorption, obtain bamboo base macropore biological activated carbon provided by the invention.
Institute goes out product and is finished product, can carry out corresponding aftertreatment, as fragmentation, grinding etc. according to customer demand.
The iodine number of this embodiment gained bamboo base macropore biological activated carbon is 1200mg/g, and be greater than 950mg/g, methylene radical blue value is 230mg/g, is greater than 180mg/g; Intensity is 89%.
The above, be only preferred embodiment of the present invention, not does any pro forma restriction to the present invention; The those of ordinary skill of all industry, all can by specification be attached implements the present invention swimmingly; But all those skilled in the art, are not departing within the scope of technical solution of the present invention, when utilizing disclosed above technology contents, and a little change made, modify with differentiation equivalent variations, be Equivalent embodiments of the present invention; Meanwhile, all according to substantial technological of the present invention to the change of any equivalent variations that above embodiment is done, modify and differentiation etc., all still belong in the scope of technical scheme of the present invention.
Claims (8)
1. preparing a method for bamboo base macropore biological activated carbon, is method one or two;
Wherein, method one comprises the steps:
By bamboo chip and caking agent mixing briquetting, after charing, pass into activator and carry out priming reaction, obtain described bamboo base macropore biological activated carbon;
Method two comprises the steps:
By bamboo chip briquetting, after charing, pass into activator and carry out priming reaction, obtain described bamboo base macropore biological activated carbon.
2. method according to claim 1, is characterized in that: described activator is all selected from least one in water vapour, carbonic acid gas, oxygen and air;
Described caking agent is selected from least one in coal tar, coal-tar pitch, wood tar oil, resol, furfuryl resin and spent pulping liquor.
3. method according to claim 1 and 2, is characterized in that: in described method one, and the consumption of caking agent is the 0-35% of bamboo quality, and the consumption of described caking agent is not 0;
In described method one and two, the consumption of activator is 0.1kg-1kg/h.
4., according to the arbitrary described method of claim 1-3, it is characterized in that: in described carbonization, temperature is 450-600 DEG C; Time is 0.5-2.5 hour;
In described activation step, temperature is 700-1000 DEG C; Time is 1-3.5 hour.
5. the bamboo base macropore biological activated carbon for preparing of the arbitrary described method of claim 1-4.
6. gac according to claim 5, is characterized in that: the aperture of described bamboo base macropore biological activated carbon is 0.3 nanometer to 400 micron;
Aperture is greater than
the pore volume in the hole ratio that accounts for pore volume porose in described bamboo base macropore biological activated carbon be 30-70%, be specially 61.6%.
7. the application of bamboo base macropore biological activated carbon in water treatment described in claim 5 or 6.
8. application according to claim 7, is characterized in that: described water is feedwater;
Described water treatment is except the organic pollutant in anhydrating.
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