CN105271171A - Preparation method of N-doped hierarchical pore carbon material with shrimp shells as carbon sources - Google Patents
Preparation method of N-doped hierarchical pore carbon material with shrimp shells as carbon sources Download PDFInfo
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Abstract
The invention relates to a preparation method of an N-doped hierarchical pore carbon material with shrimp shells as carbon sources and belongs to the technical field of environment function material preparation. The preparation method is characterized in that the non-toxic and cheap shrimp shells serve as the carbon sources, under the protection effect of nitrogen, an N-doped hierarchical pore biomass carbon material is obtained through high-temperature calcination, treatment through diluted hydrochloric acid, repeated washing through a mixed solution of ethyl alcohol and distilled water and drying to constant weight, the N-doped hierarchical pore biomass carbon material is mixed with potassium hydroxide at different ratios, the mixture is calcined under the protective effect of nitrogen, treated through hot distilled water, and treated through diluted hydrochloric acid so that impurities such as potassium carbonate generated in the reaction process can be removed, impurities repeatedly flushed through distilled water, and filtered and dried to constant weight, and the N-doped hierarchical pore carbon material is obtained. The preparation method is successfully applied to removal of sulfamethazine and chloramphenicol in the water environment, and the N-doped hierarchical pore carbon material has excellent regeneration performance.
Description
Technical field
The present invention relates to a kind of preparation method of the multi-stage porous carbon material that adulterates with the shrimp shell N that is carbon source, belong to environment functional material preparation field.
Background technology
Microbiotic occupies the 3rd in mankind's medical usage quantity, accounts for more than 6% of prescription drugs total amount, in the survival dose of animal husbandry and aquaculture, more occupies critical role; Sulfamethazine and paraxin all have antibacterial effect, it is a kind of microbiotic for prevention and therapy bacterial infection disease, therefore disease prevention and the treatment of human and animal is widely used in, but, most microbiotic can not be absorbed by body completely, and have the microbiotic up to more than 85% can enter environment with prototype or metabolite form via patient and poultry beast fecaluria, through different approaches, soil and water is polluted; Microbiotic distributes in the environment, move and stability existence comprises bacterium, hydrobiont, soil organisms and plant generation harm to Environment-Ecosystem, and the health of harm humans; Chinese scholars research has confirmed in soil and water surrounding to there is the residual of paraxin and sulfa antibiotics, therefore, to set up and treatment process that development is effectively economic removes the residual extremely urgent of paraxin in water surrounding and sulfa antibiotics.
Adsorption separating method is the most frequently used method, its adsorptive capacity is large, rate of adsorption is fast, equipment is simple, easy to operate etc., biomass charcoal is the class height aromatize insoluble solid matter produced through pyrolysis charring when anoxic wholly or in part by plant biomass, be mainly high stability carbonaceous organism, there is large quantity micropore gap and high-specific surface area, again after activation of potassium hydroxide, form N doping multi-stage porous carbon material, its specific surface area is large, porosity is flourishing, high adsorption capacity, in recent years, be applied to the removal of pollutent in water surrounding by extensive concern.
The preparation of traditional N doping multi-stage porous carbon material, can prepare as template and there is the comparatively large and more uniform N doped porous carbon material of pore size distribution of high-specific surface area, structurally ordered, pore volume, but the preparation process loaded down with trivial details cycle is long, cost height is difficult to realize industrial application, and N doping carbon material prepared by chemical Vapor deposition process, preparation condition process is harsh, more difficultly realize scale operation, prepared by ammonia process carbon material in the process of N doping multi-stage porous carbon material and employ poisonous ammonia, and need high-temperature operation; The organism remains of employing economy, environmental protection prepare the multi-stage porous carbon material of N doping through calcining and activating, its preparation process is without the need to passing through template synthesis hole, therefore avoid and use the loaded down with trivial details of hard template method, operating process is simple, with low cost, its preparation process does not have the use of objectionable impurities, therefore avoids the use of objectionable impurities, environmental protection.Strong and the complex steps of, chemical corrosion large compared to the preparation process energy consumption of traditional N doping carbon material, present method has green, environmental protection, gentleness, cheapness and advantage efficiently.
Summary of the invention
The object of this invention is to provide a kind of preparation method of the multi-stage porous carbon material that adulterates with the shrimp shell N that is carbon source, the N prepared by the method adulterates, and multi-stage porous carbon material to be mainly used in sulfamethazine in water surrounding and paraxin fast, high efficiency separation.
The present invention relates to a kind of preparation method of the multi-stage porous carbon material that adulterates with the shrimp shell N that is carbon source, belong to environment functional material field.
The present invention with nontoxic, cheap shrimp shell for carbon source; under the provide protection of nitrogen; through high-temperature calcination; use dilute hydrochloric acid process, more repeatedly clean with the mixing solutions of ethanol and distilled water, dry to constant weight; obtain the multi-stage porous biomass charcoal material of N doping; mix in varing proportions with potassium hydroxide again, under the provide protection of nitrogen, 700
oc-850
ocalcine under C condition, then through overheated distilled water process, then through dilute hydrochloric acid process, the impurity such as the salt of wormwood produced in removing reaction process, more repeatedly rinse through distilled water, filtering drying, to constant weight, obtains the multi-stage porous carbon material of N doping.
By modern analysis and test instrumental characterizings such as TEM, SEM, XRD, BET and FT-IR, disclose the physics-chem characteristic of the multi-stage porous carbon material that to adulterate with the shrimp shell N that is carbon source, utilize Staticadsorption experiment research with the shrimp shell N doping multi-stage porous carbon material that is carbon source to the adsorption isothermal line of sulfamethazine in water surrounding and paraxin, kinetics and regenerability.
the technical solution used in the present invention is:
A preparation method for the N being carbon source with shrimp shell doping multi-stage porous carbon material, carries out according to following step:
Shrimp shell is put into porcelain boat, is placed in tube furnace, under the provide protection of nitrogen, with 5
othe heat-up rate of C/min is raised to 400 from room temperature
oc also calcines two hours at such a temperature, after reflection terminates, naturally cools to room temperature; The dilute hydrochloric acid that product adds 2mol/L reacts, and after terminating, carries out repeatedly clear extremely neutral also eccysis decon and the grains of sand, be placed in drying in oven to constant weight with ethanol and distilled water to total overall reaction, obtains N doping multi-stage porous biomass carbon material and is expressed as C-400; Adulterated by the N of preparation biomass charcoal material and potassium hydroxide is that 1:1-1:3 joins respectively in mortar and grinds even with mass ratio, pours in nickel pot, covers and pinch pot cover, put into tube furnace, respectively with 5
oc/min rises to 700 from room temperature
oc-850
oc is also incubated one hour, calcinate is first with the distilled water cleaning of heat, then the dilute hydrochloric acid reaction adding 2mol/L is extremely neutral, more repeatedly cleans with distilled water, dry to constant weight, obtain the N that nitrogen content is different, pore texture the is different doping multi-stage porous carbon material of different batches.
Technological merit of the present invention: with shrimp shell as carbon source, nontoxic, pollution-free, environmental protection, cheapness, renewable; The aftertreatment of calcinate is simple to operation; Nitrogen content difference is obtained by the potassium hydroxide adding different ratios, the N doping multi-stage porous carbon material that porosity distribution is different, by selecting optimum proportioning to the absorption of sulfamethazine in water surrounding and paraxin test, in removal water that can be efficient, quick, a large amount of, sulfamethazine and paraxin is residual.
figure of description
Fig. 1 C-400 (a, b) and the scanning electron microscope (SEM) photograph of N-HPC-850-2 (c, d), as can be known from Fig. 1: the pore size distribution scope of N-HPC-850-2 is larger, wherein micropore, mesoporous and macropore depositing, have larger pore texture, particle diameter is less, and the particle distribution of C-400 is in disorder, there is the irregular pore texture in a few place, surface tissue smoother, agglomeration is serious, and deduction activation of potassium hydroxide thus produces considerable influence to the shape characteristic of carbon material.
The transmission electron microscope picture of Fig. 2 C-400 (a) and NHPC-850-2 (b); Can find out that the surperficial smoother of C-400 does not have obvious pore texture from figure a, can find out that from b the thin carbon surface structure of N-HPC-850-2 has more microvoid structure, after this shows KOH activation, the shape characteristic of carbon material there occurs larger change, porosity showed increased.
The infrared spectrogram of Fig. 3 C-400 and N-HPC-850-2; As can be known from Fig. 3: 3500cm
-1the stretching vibration peak of O-H, 1740-1600cm
-1the stretching vibration peak of C=O, 1260-1050cm
-1be C-O stretching vibration peak, illustrate after activation of potassium hydroxide, a lot of functional group all disappears.
The N of Fig. 4 N-HPC-700-2, N-HPC-850-1 and N-HPC-850-2
2adsorption-desorption figure (a) and graph of pore diameter distribution (b) thereof; As can be seen from figure a, classify according to IUPAC, N-HPC-700-2 and N-HPC-850-1 belongs to I type adsorption/desorption curve, and N-HPC-850-2 belongs to the I adsorption/desorption curve be combined with IV type, shows to there is typical micropore and meso-hole structure in N-HPC-850-2; Can find out that the aperture of N-HPC-850-2 is mainly distributed between 2.0 to 4.0 nanometers from figure b.
Table 1 shows N-HPC-700-2, the concrete distribution situation of N-HPC-850-1 and N-HPC-850-2 pore texture, and total specific surface area of N-HPC-700-2, N-HPC-850-1 and N-HPC-850-2 is respectively 1943m as can be seen from Table 1
2/ g, 2580m
2/ g and 3171m
2/ g; Overall porosity is respectively 1.021cm
3/ g, 1.227cm
3/ g and 1.934cm
3/ g, illustrates that N-HPC-850-2 has hierarchical porous structure and has higher specific surface area and porosity.
Fig. 5 solution ph adsorbs the impact of sulfamethazine and paraxin to N-HPC-850-2.As can be seen from Figure 5: when pH value is 6.0, reach maximum value to sulfamethazine adsorptive capacity, therefore, in planar water, when sulfamethazine, the optimal ph of solution is 6.0; PH value is remarkable on the impact of paraxin adsorptive capacity, and therefore, in planar water, when paraxin, solution is not subject to the impact of pH value.
Fig. 6 N-HPC-850-2 is to the adsorption isothermal line matched curve figure of sulfamethazine (a) with paraxin (b); As can be known from Fig. 4: 25
oc, the N-HPC-850-2 maximum adsorption capacity to sulfamethazine and paraxin is respectively 643.5mgg
-1and 676.1mgg
-1; 35
oc, the N-HPC-850-2 maximum adsorption capacity to sulfamethazine and paraxin is respectively 672.0mgg
-1and 714.8mgg
-1; 45
oc, the N-HPC-850-2 maximum adsorption capacity to sulfamethazine and paraxin is respectively 699.3mgg
-1and 742.4mgg
-1, this illustrates 45
oc demonstrates good adsorption effect, meets Langmuir Isothermal Model well to the adsorption test data of two kinds of materials simultaneously.
Fig. 7 N-HPC-850-2 is to the kinetics matched curve of sulfamethazine; As can be seen from Figure 7: adsorption equilibrium reaches very soon, experimental data is matching pseudo-second order kinetic equation well, in whole time range, N-HPC-850-2 to sulfamethazine adsorptive capacity all very fast reach maximal absorptive capacity, show good absorption property, under identical concentration, temperature is higher, and the time that absorption reaches balance is shorter.And adsorption process meets pseudo-second order kinetic model.
Fig. 8 N-HPC-850-2 is to the kinetics matched curve of paraxin; As can be seen from Figure 8: adsorption equilibrium reaches very soon, experimental data matching pseudo-second order kinetic equation well.In whole time range, N-HPC-850-2 to paraxin adsorptive capacity all very fast reach maximal absorptive capacity, show good absorption property.Under identical concentration, temperature is higher, and the time that absorption reaches balance is shorter.And adsorption process meets pseudo-second order kinetic model.
Embodiment
1, below in conjunction with concrete embodiment, the present invention will be further described:
A certain amount of shrimp shell is put into porcelain boat, is placed in tube furnace, under the provide protection of nitrogen, with 5
othe heat-up rate of C/min is raised to 400 from room temperature
oc also calcines two hours at such a temperature, after reflection terminates, naturally cools to room temperature; The dilute hydrochloric acid that product adds 2mol/L reacts, and after terminating, carries out repeatedly clear extremely neutral also eccysis decon and the grains of sand, be placed in drying in oven to constant weight with ethanol and distilled water to total overall reaction, obtains N doping multi-stage porous biomass carbon material; Adulterated by the N of preparation biomass charcoal material and potassium hydroxide joins respectively in mortar with the mass ratio that 1:0,1:1,1:2,1:3 tetra-kinds is different and grinds even, pours in nickel pot, covers and pinch pot cover, put into tube furnace, respectively with 5
oc/min rises to 700 from room temperature
oc, 800
oc and 850
oc is also incubated one hour, and calcinate is first with the distilled water cleaning of heat, then the dilute hydrochloric acid reaction adding 2mol/L is extremely neutral, repeatedly clean with distilled water again, dry to constant weight, obtain N-HPC-700-0, N-HPC-700-1, N-HPC-700-2, N-HPC-700-3, N-HPC-800-0, N-HPC-800-1, N-HPC-800-2, N-HPC-800-3, N-HPC-850-0, N-HPC-850-1, N-HPC-850-2(850
oc calcines, and adulterate biomass charcoal material of N is 1:2 from the mass ratio of potassium hydroxide) N that nitrogen content is different, pore texture is different of different batches to adulterate multi-stage porous carbon material, and selects optimum proportioning by adsorption experiment.
2, below in conjunction with concrete embodiment, the present invention will be further described:
In the present invention, in specific embodiments, absorption property evaluation is carried out by the following method: utilize Staticadsorption experiment to complete; The sulfamethazine of 10ml different concns and chloromycetin solution are joined respectively in centrifuge tube, respectively to wherein adding 3mgN-HPC-850-2, be placed in water bath with thermostatic control and leave standstill 12h, pH value controls at 3-9, adsorption temp 25-45
oc, investigates solution ph, temperature to the impact of adsorbent tetracycline molecule; After absorption, by collected by centrifugation, obtain clear liquid at the middle and upper levels, the tetracycline molecule concentration uv-vis spectra do not adsorbed records, and according to result calculate loading capacity (
q e, μm ol/g).
Wherein
c 0(μm ol/L) and
c e(μm ol/L) is the concentration of sulfamethazine and paraxin before and after absorption respectively,
wg () is adsorbent amount,
v(mL) be test fluid volume.
Experiment examination example 1: get 3mgN-HPC-850-2 and join in the centrifuge tube of 10ml, then get respectively 10ml starting point concentration be respectively 20,50,80,80,100,120,150,180,200,220, the sulfamethazine solution and 20 of 250mg/L, 50,80,80,100,120,150,180,200,220,250, the chloromycetin solution of 280mg/L joins in centrifuge tube, centrifuge tube is placed in the water-bath of three differing tempss (298K, 308K and 318K) and leaves standstill 12.0h; After absorption, collecting by filtration supernatant liquid, is not measured by the sulfamethazine molecular conecentration ultraviolet-visible pectrophotometer adsorbed, and calculates loading capacity; Fig. 6 (a) and (b) result shows the absorption situation of N-HPC-850-2 to sulfamethazine and paraxin respectively, along with the rising of temperature and concentration, adsorptive capacity increases gradually, finally reaches adsorption equilibrium, proves to there is a large amount of holes and larger specific surface area.
Experiment examination example 2: get sulfamethazine that 10ml starting point concentration is 150mgl/L respectively and chloromycetin solution joins in centrifuge tube, add 3mgN-HPC-850-2 respectively, centrifuge tube is placed on separately respectively in the water-bath of 298K, 308K, 318K and leaves standstill 5,15,30,60,90,120,180 minutes respectively; After having left standstill, collecting by filtration supernatant liquid, is not measured by the sulfamethazine that adsorbs and paraxin molecular conecentration ultraviolet-visible pectrophotometer, and calculates loading capacity according to result; Fig. 7 and Fig. 8 result shows: N-HPC-850-2 has good kinetics of adsorption performance to sulfamethazine and paraxin, substantially reaches adsorption equilibrium in 3.0h.
Table 1
Claims (9)
1. the preparation method of the multi-stage porous carbon material that to adulterate with the shrimp shell N that is carbon source, it is characterized in that: with nontoxic, cheap shrimp shell is carbon source, under the provide protection of nitrogen, through high-temperature calcination, use dilute hydrochloric acid process, repeatedly clean with the mixing solutions of ethanol and distilled water again, dry to constant weight, obtain the multi-stage porous biomass charcoal material of N doping, mix in varing proportions with potassium hydroxide again, calcine under the provide protection of nitrogen, again through overheated distilled water process, again through dilute hydrochloric acid process, the impurity such as the salt of wormwood produced in removing reaction process, repeatedly rinse through distilled water again, filtering drying is to constant weight, obtain the multi-stage porous carbon material of N doping.
2. the preparation method of a kind of multi-stage porous carbon material that adulterates with the shrimp shell N that is carbon source as claimed in claim 1; it is characterized in that described with nontoxic, cheap shrimp shell for carbon source; under the provide protection of nitrogen; through high-temperature calcination; refer to dilute hydrochloric acid process: shrimp shell is put into porcelain boat; be placed in tube furnace, under the provide protection of nitrogen, with 5
othe heat-up rate of C/min is raised to 400 from room temperature
oc also calcines two hours at such a temperature, after reflection terminates, naturally cools to room temperature; Product adds the dilute hydrochloric acid reaction of 2mol/L.
3. the preparation method of a kind of multi-stage porous carbon material that adulterates with the shrimp shell N that is carbon source as claimed in claim 1; it is characterized in that described mixing in varing proportions with potassium hydroxide again; calcine under the provide protection of nitrogen; again through overheated distilled water process; refer to through dilute hydrochloric acid process again: adulterated by the N of preparation biomass charcoal material and potassium hydroxide are that 1:1-1:3 joins respectively in mortar and grinds even with mass ratio, pour in nickel pot, cover and pinch pot cover; put into tube furnace, respectively with 5
oc/min rises to 700 from room temperature
oc-850
oc is also incubated one hour, and calcinate is first with the distilled water cleaning of heat, then the dilute hydrochloric acid reaction adding 2mol/L is extremely neutral.
4. the preparation method of a kind of multi-stage porous carbon material that adulterates with the shrimp shell N that is carbon source as claimed in claim 3, is characterized in that: the adulterate mass ratio of biomass charcoal material and potassium hydroxide of N is 1:2.
5. the preparation method of a kind of multi-stage porous carbon material that adulterates with the shrimp shell N that is carbon source as claimed in claim 3, is characterized in that: rise to 850 from room temperature
oc is also incubated one hour.
6. the N for preparing of preparation method adulterates the purposes of multi-stage porous carbon material to sulfamethazine in water surrounding and paraxin fractionation by adsorption as claimed in claim 1.
7. the N for preparing of preparation method adulterates the purposes of multi-stage porous carbon material to sulfamethazine in water surrounding and paraxin fractionation by adsorption as claimed in claim 6, it is characterized in that: the sulfamethazine of 10ml different concns and chloromycetin solution are joined in centrifuge tube respectively, respectively to wherein adding 3mgN-HPC-850-2, be placed in water bath with thermostatic control and leave standstill 12h, pH value controls at 3-9, adsorption temp 25-45
oc, investigates solution ph, temperature to the impact of adsorbent tetracycline molecule; After absorption, by collected by centrifugation, obtain clear liquid at the middle and upper levels, the tetracycline molecule concentration uv-vis spectra do not adsorbed records, and calculates loading capacity according to result.
8. the N for preparing of preparation method adulterates the purposes of multi-stage porous carbon material to sulfamethazine in water surrounding and paraxin fractionation by adsorption as claimed in claim 6, it is characterized in that: adsorption temp is 45
oc.
9. the N for preparing of preparation method adulterates the purposes of multi-stage porous carbon material to sulfamethazine in water surrounding and paraxin fractionation by adsorption as claimed in claim 6, it is characterized in that: in planar water, when sulfamethazine, the pH value of solution is 6.0.
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