CN117720105A - Modified coconut shell activated carbon and preparation method thereof - Google Patents
Modified coconut shell activated carbon and preparation method thereof Download PDFInfo
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- CN117720105A CN117720105A CN202311741204.6A CN202311741204A CN117720105A CN 117720105 A CN117720105 A CN 117720105A CN 202311741204 A CN202311741204 A CN 202311741204A CN 117720105 A CN117720105 A CN 117720105A
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 208
- 235000013162 Cocos nucifera Nutrition 0.000 title claims abstract description 76
- 244000060011 Cocos nucifera Species 0.000 title claims abstract description 76
- 238000002360 preparation method Methods 0.000 title claims abstract description 22
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 82
- 150000004676 glycans Chemical class 0.000 claims abstract description 59
- 229920001282 polysaccharide Polymers 0.000 claims abstract description 57
- 239000005017 polysaccharide Substances 0.000 claims abstract description 57
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 53
- 240000008042 Zea mays Species 0.000 claims abstract description 46
- 235000007244 Zea mays Nutrition 0.000 claims abstract description 46
- 229940089639 cornsilk Drugs 0.000 claims abstract description 46
- 239000001231 zea mays silk Substances 0.000 claims abstract description 46
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 42
- -1 sulfuric acid modified activated carbon Chemical class 0.000 claims abstract description 25
- 238000001035 drying Methods 0.000 claims abstract description 24
- 238000010438 heat treatment Methods 0.000 claims abstract description 24
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 21
- 239000005539 carbonized material Substances 0.000 claims abstract description 18
- 230000004913 activation Effects 0.000 claims abstract description 14
- 238000003763 carbonization Methods 0.000 claims abstract description 14
- 238000001816 cooling Methods 0.000 claims abstract description 14
- 238000005406 washing Methods 0.000 claims abstract description 14
- 239000012153 distilled water Substances 0.000 claims abstract description 10
- 238000003756 stirring Methods 0.000 claims abstract description 9
- NVVGMIRCFUVBOB-UHFFFAOYSA-N acetic acid;iron Chemical compound [Fe].CC(O)=O NVVGMIRCFUVBOB-UHFFFAOYSA-N 0.000 claims abstract description 7
- 238000010000 carbonizing Methods 0.000 claims abstract description 7
- 238000005520 cutting process Methods 0.000 claims abstract description 7
- 239000000463 material Substances 0.000 claims abstract description 7
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 39
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 28
- 229910052742 iron Inorganic materials 0.000 claims description 20
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 17
- 239000008367 deionised water Substances 0.000 claims description 14
- 229910021641 deionized water Inorganic materials 0.000 claims description 14
- 239000000706 filtrate Substances 0.000 claims description 13
- 238000000034 method Methods 0.000 claims description 10
- 239000007787 solid Substances 0.000 claims description 10
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 9
- 238000000967 suction filtration Methods 0.000 claims description 7
- 235000019441 ethanol Nutrition 0.000 claims description 6
- 238000001914 filtration Methods 0.000 claims description 6
- 230000001376 precipitating effect Effects 0.000 claims description 6
- 238000007789 sealing Methods 0.000 claims description 6
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 claims description 3
- 239000002244 precipitate Substances 0.000 claims description 3
- 230000001105 regulatory effect Effects 0.000 claims description 3
- 239000001509 sodium citrate Substances 0.000 claims description 3
- HRXKRNGNAMMEHJ-UHFFFAOYSA-K trisodium citrate Chemical compound [Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O HRXKRNGNAMMEHJ-UHFFFAOYSA-K 0.000 claims description 3
- 229940038773 trisodium citrate Drugs 0.000 claims description 3
- 238000005303 weighing Methods 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 2
- 238000004321 preservation Methods 0.000 claims description 2
- 239000002441 uremic toxin Substances 0.000 abstract description 13
- 239000003463 adsorbent Substances 0.000 abstract description 4
- DDRJAANPRJIHGJ-UHFFFAOYSA-N creatinine Chemical compound CN1CC(=O)NC1=N DDRJAANPRJIHGJ-UHFFFAOYSA-N 0.000 description 36
- 238000001179 sorption measurement Methods 0.000 description 36
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 21
- 239000004202 carbamide Substances 0.000 description 20
- 229940109239 creatinine Drugs 0.000 description 18
- 230000000052 comparative effect Effects 0.000 description 8
- 239000000203 mixture Substances 0.000 description 6
- 230000004048 modification Effects 0.000 description 6
- 238000012986 modification Methods 0.000 description 6
- 239000000126 substance Substances 0.000 description 6
- 239000011148 porous material Substances 0.000 description 5
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 4
- 230000001276 controlling effect Effects 0.000 description 4
- 230000007935 neutral effect Effects 0.000 description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- CREXVNNSNOKDHW-UHFFFAOYSA-N azaniumylideneazanide Chemical group N[N] CREXVNNSNOKDHW-UHFFFAOYSA-N 0.000 description 3
- 238000004090 dissolution Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 208000001647 Renal Insufficiency Diseases 0.000 description 2
- LEHOTFFKMJEONL-UHFFFAOYSA-N Uric Acid Chemical compound N1C(=O)NC(=O)C2=C1NC(=O)N2 LEHOTFFKMJEONL-UHFFFAOYSA-N 0.000 description 2
- TVWHNULVHGKJHS-UHFFFAOYSA-N Uric acid Natural products N1C(=O)NC(=O)C2NC(=O)NC21 TVWHNULVHGKJHS-UHFFFAOYSA-N 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 230000007423 decrease Effects 0.000 description 2
- 238000000605 extraction Methods 0.000 description 2
- 125000000524 functional group Chemical group 0.000 description 2
- 125000005842 heteroatom Chemical group 0.000 description 2
- 201000006370 kidney failure Diseases 0.000 description 2
- 150000004804 polysaccharides Polymers 0.000 description 2
- 230000000630 rising effect Effects 0.000 description 2
- 231100000331 toxic Toxicity 0.000 description 2
- 230000002588 toxic effect Effects 0.000 description 2
- 229940116269 uric acid Drugs 0.000 description 2
- 239000012190 activator Substances 0.000 description 1
- 230000006907 apoptotic process Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 210000001124 body fluid Anatomy 0.000 description 1
- 239000010839 body fluid Substances 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 238000007385 chemical modification Methods 0.000 description 1
- 230000006378 damage Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
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- 238000009792 diffusion process Methods 0.000 description 1
- 230000004064 dysfunction Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 238000004108 freeze drying Methods 0.000 description 1
- 241000411851 herbal medicine Species 0.000 description 1
- 230000003914 insulin secretion Effects 0.000 description 1
- 210000005027 intestinal barrier Anatomy 0.000 description 1
- 230000007358 intestinal barrier function Effects 0.000 description 1
- MVZXTUSAYBWAAM-UHFFFAOYSA-N iron;sulfuric acid Chemical compound [Fe].OS(O)(=O)=O MVZXTUSAYBWAAM-UHFFFAOYSA-N 0.000 description 1
- 238000001000 micrograph Methods 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 150000004965 peroxy acids Chemical class 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 150000003254 radicals Chemical class 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000010992 reflux Methods 0.000 description 1
- 230000008929 regeneration Effects 0.000 description 1
- 238000011069 regeneration method Methods 0.000 description 1
- 208000024891 symptom Diseases 0.000 description 1
- 239000003053 toxin Substances 0.000 description 1
- 231100000765 toxin Toxicity 0.000 description 1
- 108700012359 toxins Proteins 0.000 description 1
- 229940045136 urea Drugs 0.000 description 1
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- Carbon And Carbon Compounds (AREA)
Abstract
The invention belongs to the field of adsorbent preparation, and particularly discloses modified coconut shell activated carbon and a preparation method thereof, wherein the preparation method comprises the following steps: step (1): drying coconut shells, putting the coconut shells into a carbonization furnace, heating, preserving heat, carbonizing, and cooling to obtain carbonized materials; step (2): crushing the carbonized material, introducing nitrogen, heating, stopping introducing nitrogen, switching to steam for activation, stopping heating, cutting off the steam, introducing nitrogen, cooling to room temperature to obtain an activated material, rinsing and drying to obtain activated coconut shell activated carbon; step (3): crushing activated coconut shell activated carbon, adding the crushed activated carbon into sulfuric acid solution, oscillating at constant temperature, washing with distilled water to neutrality, and drying to constant weight to obtain sulfuric acid modified activated carbon; step (4): adding sulfuric acid modified activated carbon into the corn silk polysaccharide iron-acetic acid solution, stirring in a water bath, and drying to obtain the modified coconut shell activated carbon. The modified coconut shell activated carbon provided by the invention can quickly and efficiently adsorb uremic toxins.
Description
Technical Field
The invention relates to modified coconut shell activated carbon and a preparation method thereof, belonging to the field of preparation of adsorbents.
Background
Uremic toxins are substances which have a significant increase in body fluid concentration and toxic effects in renal failure patients, including uremic toxins including urea, uric acid, creatinine, and the like, which increase in body concentration and can cause uremic symptoms and multiple system dysfunction in renal failure patients.
The activated carbon is used as an adsorbent with excellent adsorption performance, has the characteristics of stable physical and chemical properties, regeneration, environmental protection and the like, is widely applied to various industries, but the traditional activated carbon has certain limitation in adsorption performance, has certain adsorption capacity only for other organic matters such as creatinine, uric acid and the like, and has very weak adsorption effect on urea serving as uremic toxin with the highest content. Urea has been identified as being associated with insulin release, free radical production, apoptosis and intestinal barrier disruption.
Many studies have shown that by surface modifying activated carbon, its adsorption capacity for certain specific substances can be improved, and the adsorption characteristics of activated carbon depend not only on its pore structure but also on its surface chemistry, which determines the chemisorption of activated carbon. The chemical properties mainly determine the types and the number of the chemical functional groups on the surface, the surface heteroatoms and the compounds, and the adsorption of different adsorbents by different surface functional groups, heteroatoms and compounds is obviously different. Therefore, the activated carbon with higher selectivity for uremic toxin adsorption is prepared by chemical modification of the surface structure.
Disclosure of Invention
Aiming at the defects in the prior art, the invention provides modified coconut shell activated carbon and a preparation method thereof. According to the invention, the coconut shell is used for preparing the activated carbon, and then the sulfuric acid is used for modifying the coconut shell activated carbon, so that the total specific surface area of the inside of the activated carbon is increased, a plurality of closed holes in the inside are opened, a plurality of mesopores and micropores are formed, and the adsorption rate of uremic toxins is obviously increased. In addition, the prepared corn silk polysaccharide iron is loaded on the sulfuric acid modified coconut shell activated carbon, so that the adsorption quantity of the activated carbon on uremic toxins is improved.
In order to achieve the above purpose, the technical scheme adopted by the invention is as follows:
the invention provides a preparation method of modified coconut shell activated carbon, which comprises the following steps:
step (1): drying coconut shells, putting the coconut shells into a carbonization furnace, heating, preserving heat, carbonizing, and cooling to obtain carbonized materials;
step (2): crushing the carbonized material, introducing nitrogen, heating, stopping introducing nitrogen, switching to steam for activation, stopping heating, cutting off the steam, introducing nitrogen, cooling to room temperature to obtain an activated material, rinsing and drying to obtain activated coconut shell activated carbon;
step (3): crushing activated coconut shell activated carbon, adding the crushed activated carbon into sulfuric acid solution, oscillating at constant temperature, washing with distilled water to neutrality, and drying to constant weight to obtain sulfuric acid modified activated carbon;
step (4): adding sulfuric acid modified activated carbon into the corn silk polysaccharide iron-acetic acid solution, uniformly stirring in a water bath, and drying to obtain the modified coconut shell activated carbon.
Preferably, in the step (1), the temperature is raised to 650-750 ℃, and the heat preservation carbonization time is 2-3h.
The applicant finds that the carbonization of coconut shells is performed at 650-750 ℃ by controlling the temperature rise, the carbonization effect is good, the carbon content of the carbonized material is high, and the performance of the activated carbon is also improved. However, the carbonization temperature is not too high, the carbonization time is not too long, otherwise, the yield of carbonized materials is reduced.
Preferably, the temperature is raised to 850-950 ℃ in the step (2), and the water vapor activation time is 4-5h.
The applicant finds that the water vapor is used as an activator, so that the surface of the prepared activated carbon is cleaner, the production process is simple, and equipment cannot be corroded. But the water vapor activation speed is higher, the activation duration is strictly controlled, and the reduction of the comprehensive performance of the activated carbon is avoided. In addition, the temperature is raised to 850-950 ℃ to enable the prepared activated carbon to have stronger adsorption capacity, because all decomposable substances in coconut shells can be removed at the temperature, rich pore structures and huge specific surface areas are generated, and the adsorption capacity of the activated carbon is improved.
Preferably, the concentration of the sulfuric acid solution in the step (3) is 1mol/L to 10mol/L.
The applicant finds that after modification by using concentrated sulfuric acid, a large number of rugged lamellar structures are generated on the surface of the coconut shell activated carbon, and the irregularity degree is increased along with the rising of the concentration of the sulfuric acid, because the surface of the activated carbon is eroded by the sulfuric acid to expose a large number of internal structures, the total specific surface area of the activated carbon is greatly increased, and meanwhile, a large number of internal closed holes are opened, so that a plurality of medium-pore micropores are directly exposed, and the adsorption rate is improved.
Preferably, in the step (4), the mass ratio of the corn silk polysaccharide iron to the sulfuric acid modified activated carbon is 1 (30-40).
Further preferably, in the step (4), the mass ratio of the corn silk polysaccharide iron to the sulfuric acid modified activated carbon is 1:35.
The applicant finds that the adsorption efficiency of the prepared modified coconut shell activated carbon on urea can be obviously improved by regulating and controlling the mass ratio of corn silk polysaccharide iron to sulfuric acid modified activated carbon. This is probably because a proper amount of corn silk polysaccharide is loaded on the sulfuric acid modified coconut shell activated carbon, so that the pores in the activated carbon are not blocked on one hand; on the other hand, the amino nitrogen atoms in the iron ions and uremic toxins can form coordination bonds, so that the adsorption capacity of the activated carbon to the toxins is improved.
Preferably, the preparation method of the corn silk polysaccharide iron in the step (4) comprises the following steps:
step S1: weighing stigma Maydis, adding deionized water, performing constant temperature water bath, vacuum filtering, repeating the above steps for 2 times, mixing filtrates, concentrating the filtrate, adding anhydrous ethanol into the concentrated solution, sealing, standing in shade, filtering to obtain solid, washing the solid with anhydrous ethanol, acetone, and diethyl ether, redissolving with distilled water, dialyzing with flowing water, precipitating with ethanol, and separating to obtain powdery stigma Maydis polysaccharide;
step S2: placing corn silk polysaccharide and trisodium citrate in a beaker, adding deionized water, stirring at constant temperature, regulating pH, dropwise adding ferric trichloride solution until solid appears in the solution, stopping dropwise adding, continuing heating and stirring, performing suction filtration, adding equal volume of absolute ethyl alcohol into filtrate, sealing, placing in a dark place, performing suction filtration, washing precipitate with absolute ethyl alcohol and acetone respectively, redissolving, dialyzing with deionized water, precipitating with alcohol, and separating to obtain powdery corn silk polysaccharide iron.
Preferably, in the step S1, the mass ratio of the corn silk to the deionized water is 1 (10-20), and the volume ratio of the concentrated filtrate to the absolute ethyl alcohol is 1 (2-3).
Further preferably, in the step S1, the mass ratio of the corn silk to the deionized water is 1:16, and the volume ratio of the concentrated filtrate to the absolute ethyl alcohol is 1:3.
Applicants found that controlling the mass ratio of corn silk to deionized water to be 1:16 better extracted the polysaccharide in the corn silk. The viscosity of the solution under the condition can promote molecular diffusion and accelerate polysaccharide dissolution, which is favorable for polysaccharide component precipitation and improves polysaccharide yield. However, if the volume of deionized water is too large, the temperature rising speed of the extraction system is relatively slow, which is unfavorable for the dissolution of polysaccharide. In addition, the volume ratio of the concentrated filtrate to the absolute ethyl alcohol is controlled to be 1:3, so that the polysaccharide can be better precipitated, and the polysaccharide yield is improved.
Preferably, the temperature of the water bath in the step S1 is 80-90 ℃, and the water bath duration is 2.5-3.5h.
Further preferably, the temperature of the water bath is 90℃and the duration of the water bath is 3 hours.
The applicant has unexpectedly found that controlling the water bath temperature and duration can increase the yield of corn silk polysaccharide, and as the water bath temperature increases, the yield of polysaccharide increases, but after the reflux temperature exceeds 90 ℃, the yield of polysaccharide decreases. The reason may be that an increase in temperature helps the molecules to diffuse rapidly, accelerating the polysaccharide dissolution. However, the stability of the polysaccharide is deteriorated due to the excessively high temperature, and the degradation and destruction of the internal structure of the polysaccharide are easily caused, resulting in the decrease of the yield of the polysaccharide. Meanwhile, the water bath time is strictly controlled, and when the water bath time is not more than 3 hours, the stability of the polysaccharide structure can be maintained, the polysaccharide is prevented from being denatured in a hot environment, and the extracted polysaccharide can be kept in a higher yield.
Preferably, the pH is adjusted to 8-9 in step S2. In the extraction process of corn silk polysaccharide, the pH of the solution is strictly controlled, the polysaccharide structure is easily damaged in the peracid environment, and the polysaccharide is easily degraded in the overbased environment, so that the quality of the polysaccharide is affected.
The second aspect of the invention provides modified coconut shell activated carbon obtained by the preparation method.
The invention has the beneficial effects that:
(1) According to the invention, the total specific surface area of the coconut shell activated carbon is increased by modifying the coconut shell activated carbon with sulfuric acid, the closed pores in the activated carbon are opened, a plurality of mesopore micropores are directly exposed, the adsorption sites are increased, and the adsorption rate of the activated carbon on uremic toxins is improved.
(2) According to the invention, the polysaccharide is extracted from the corn silk, the corn silk polysaccharide and the iron solution are synthesized into the corn silk polysaccharide iron, and then the corn silk polysaccharide iron is loaded on the sulfuric acid modified coconut shell activated carbon, so that the corn silk polysaccharide iron can form a coordination bond with an amino nitrogen atom in uremic toxins, and the adsorption efficiency of the activated carbon on the uremic toxins is remarkably improved.
(3) The modified coconut shell activated carbon provided by the invention has high binding capacity and quick dynamic characteristics on uremic toxins, does not release toxic byproducts, and can adsorb uremic toxins more quickly and efficiently.
Drawings
FIG. 1 is a scanning electron microscope image of coconut shell activated carbon (200 meshes) prepared by the invention before and after modification;
FIG. 2 is a graph showing the kinetics of adsorbed creatinine after the sulfuric acid modified activated carbon of different mesh numbers is modified by sulfuric acid of different concentrations;
FIG. 3 shows Langmuir isotherms of different mesh sulfuric acid modified activated carbon of the present invention for adsorbing creatinine after modification with sulfuric acid of different concentrations;
FIG. 4 is a graph showing the kinetics of urea adsorption of different mesh sulfuric acid modified activated carbon of the present invention after modification with sulfuric acid of different concentrations;
FIG. 5 shows Langmuir isotherms of different mesh sulfuric acid modified activated carbon of the present invention for adsorption of urea after modification with sulfuric acid of different concentrations;
in FIGS. 2 to 5, the modified activated carbon used was 5 mesh (5-10 mesh: 5 mesh), 50 mesh (50-100 mesh: 50 mesh) and 200 mesh (200-500 mesh: 200 mesh), respectively; in FIGS. 1 to 5, sulfuric acid concentrations of 1mol/L,6mol/L and 10mol/L, respectively, were used.
Detailed Description
The present invention will be described in further detail with reference to the following examples in order to make the objects, technical solutions and advantages of the present invention more apparent. It should be understood that the specific embodiments described herein are for purposes of illustration only and are not intended to limit the scope of the invention.
In order to better illustrate the embodiments of the present invention, the following examples are provided for further illustration.
The 5 mesh, 50 mesh and 200 mesh Activated Carbon (AC) was modified with 1mol/L,6mol/L and 10mol/L sulfuric acid, respectively, and it can be seen from FIG. 1 that the 200 mesh activated carbon modified with sulfuric acid produced a large number of rugged lamellar structures on the surface thereof, and the degree of irregularity increased as the sulfuric acid concentration increased, exposing a large number of internal structures; from the adsorption kinetics of the activated carbon in the attached figures 2 and 3 to creatinine and the results of Langmuir isothermal experimental study, it can be seen that the adsorption capacity of the 6mol/L sulfuric acid modified 200 mesh activated carbon to creatinine is highest; from the adsorption kinetics of the activated carbon to urea and the adsorption kinetics of the Langmuir isothermal experimental study results of the activated carbon shown in the figures 4 and 5, the adsorption capacity of the 200-mesh activated carbon modified by 6mol/L sulfuric acid to urea is highest.
Thus, all examples and comparative examples in the present invention used 6mol/L sulfuric acid to modify 200 mesh activated carbon to prepare modified coconut shell activated carbon.
The preparation steps of the corn silk polysaccharide/corn silk polysaccharide iron used in examples 1-4 were as follows:
step (1): weighing 100g of corn silk, adding 1600mL of deionized water, carrying out suction filtration in a constant-temperature water bath at 90 ℃ for 3 hours, repeating the above operation for 2 times, combining the filtrates, concentrating the filtrate, adding absolute ethyl alcohol which is 3 times the volume of the concentrated solution into the concentrated solution, sealing, standing in a shady place for 48 hours, filtering to obtain a solid, washing the solid with absolute ethyl alcohol, acetone and diethyl ether respectively, redissolving the solid with distilled water, dialyzing with flowing water, precipitating with alcohol, filtering, washing and freeze-drying to obtain brownish red powdery corn silk polysaccharide;
step (2): placing 10g of corn silk polysaccharide and 1.0g of trisodium citrate into a beaker, adding deionized water, stirring at constant temperature of 80 ℃, adjusting pH to 8-9 with sodium hydroxide solution, and dripping 1 mol.L -1 Stopping dripping until solid appears in the ferric trichloride solution, continuing heating and stirring for 1h, performing suction filtration, adding equal volume of absolute ethyl alcohol into the filtrate, sealing, standing in the dark for 24h, performing suction filtration, washing the precipitate with absolute ethyl alcohol and acetone respectively, re-dissolving, dialyzing with deionized water, precipitating with ethanol, and separating to obtain powdery corn silk polysaccharide iron.
The obtained corn silk polysaccharide/corn silk polysaccharide iron is respectively dissolved in 0.5% acetic acid solution to obtain corn silk polysaccharide-sulfuric acid solution/corn silk polysaccharide iron-sulfuric acid solution.
The corn silk is purchased from Shandong colorful herbal medicine industry.
Example 1
The preparation method of the modified coconut shell activated carbon comprises the following steps:
step (1): drying 1kg of coconut shell, putting into a carbonization furnace, heating to 650 ℃, preserving heat and carbonizing for 3 hours, and cooling to obtain carbonized materials;
step (2): crushing the carbonized material, introducing nitrogen for 25min, heating to 850 ℃, stopping introducing nitrogen, switching to steam for activation for 5h, stopping heating, cutting off the steam, introducing nitrogen, cooling to room temperature to obtain an activated material, rinsing and drying to obtain activated coconut shell activated carbon;
step (3): crushing activated coconut shell activated carbon, adding the crushed activated carbon with 200 meshes into a 6mol/L sulfuric acid solution, oscillating for 6 hours at constant temperature, washing with distilled water to be neutral, and drying to constant weight to obtain sulfuric acid modified activated carbon;
step (4): 21g of sulfuric acid modified activated carbon is added into 10mL of 60g/L corn silk polysaccharide iron-acetic acid solution, the mixture is stirred for 2 hours in a water bath at 30 ℃, and the mixture is dried to obtain the modified coconut shell activated carbon.
Example 2
The preparation method of the modified coconut shell activated carbon comprises the following steps:
step (1): drying 1kg of coconut shell, putting into a carbonization furnace, heating to 750 ℃, preserving heat and carbonizing for 2 hours, and cooling to obtain carbonized materials;
step (2): crushing the carbonized material, introducing nitrogen for 30min, heating to 950 ℃, stopping introducing nitrogen, switching to steam for activation for 4h, stopping heating, cutting off the steam, introducing nitrogen, cooling to room temperature to obtain an activated material, rinsing and drying to obtain activated coconut shell activated carbon;
step (3): crushing activated coconut shell activated carbon, adding the crushed activated carbon with 200 meshes into a 6mol/L sulfuric acid solution, oscillating for 6 hours at constant temperature, washing with distilled water to be neutral, and drying to constant weight to obtain sulfuric acid modified activated carbon;
step (4): 24g of sulfuric acid modified activated carbon is added into 10mL of 60g/L corn silk polysaccharide iron-acetic acid solution, the mixture is stirred for 2 hours in a water bath at 30 ℃, and the mixture is dried to obtain the modified coconut shell activated carbon.
Example 3
The preparation method of the modified coconut shell activated carbon comprises the following steps:
step (1): drying 1kg of coconut shell, putting into a carbonization furnace, heating to 700 ℃, preserving heat and carbonizing for 2 hours, and cooling to obtain carbonized materials;
step (2): crushing the carbonized material to 200 meshes, introducing nitrogen for 30min, heating to 900 ℃, stopping introducing nitrogen, switching to steam for activation for 4h, stopping heating, cutting off the steam, introducing nitrogen, cooling to room temperature to obtain an activated material, rinsing and drying to obtain activated coconut shell activated carbon;
step (3): crushing activated coconut shell activated carbon, adding the crushed activated carbon with 200 meshes into a 6mol/L sulfuric acid solution, oscillating for 6 hours at constant temperature, washing with distilled water to be neutral, and drying to constant weight to obtain sulfuric acid modified activated carbon;
step (4): 18g of sulfuric acid modified activated carbon is added into 10mL of 60g/L corn silk polysaccharide iron-acetic acid solution, the mixture is stirred for 2 hours in a water bath at 30 ℃, and the mixture is dried to obtain the modified coconut shell activated carbon.
Example 4
The procedure for the preparation of the modified coconut shell activated carbon in this example was identical to that of example 1, except that the temperature was increased to 900℃in step (1).
Example 5
The preparation process of the modified coconut shell activated carbon in this example was identical to the preparation step in example 1, except that the water vapor activation time period in step (1) was 6 hours.
Comparative example 1
The procedure for the preparation of the modified coconut shell activated carbon in this comparative example was the same as that of example 1, except that 50mL of 60g/L corn silk polysaccharide-acetic acid solution was used instead of 10mL of 60g/L corn silk polysaccharide iron-acetic acid solution in step (4).
Comparative example 2
The preparation method of the sulfuric acid modified activated carbon comprises the following steps:
step (1): drying 1kg of coconut shell, putting into a carbonization furnace, heating to 650 ℃, preserving heat and carbonizing for 3 hours, and cooling to obtain carbonized materials;
step (2): crushing the carbonized material, introducing nitrogen for 25min, heating to 850 ℃, stopping introducing nitrogen, switching to steam for activation for 5h, stopping heating, cutting off the steam, introducing nitrogen, cooling to room temperature to obtain an activated material, rinsing and drying to obtain activated coconut shell activated carbon;
step (3): crushing activated coconut shell activated carbon, adding the crushed activated carbon with 200 meshes into a 6mol/L sulfuric acid solution, oscillating for 6 hours at constant temperature, washing with distilled water to be neutral, and drying to constant weight to obtain the sulfuric acid modified activated carbon.
Adsorption performance test of modified coconut shell activated carbon
Urea adsorption performance determination: 0.1g of modified coconut shell activated carbon is taken to adsorb 20mL of urea solution (the mass concentration of the urea solution is 300 mg/L), and the urea concentration in the solution is measured after 2 hours at 37 ℃.
Creatinine adsorption performance determination: 0.1g of modified coconut shell activated carbon was taken to adsorb 50mL of creatinine solution (the mass concentration of the creatinine solution is 200 mg/L), and the creatinine concentration in the solution was measured after 2 hours at 37 ℃.
The adsorption capacities of the coconut shell activated carbon for urea and creatinine are shown in table 1.
TABLE 1
| Numbering device | Adsorption capacity of urea (mg/g) | Creatinine adsorption capacity (mg/g) |
| Example 1 | 55.2 | 88.1 |
| Example 2 | 54.3 | 87.9 |
| Example 3 | 56.8 | 89.8 |
| Example 4 | 38.1 | 73.4 |
| Example 5 | 35.9 | 70.7 |
| Comparative example 1 | 41.7 | 72.2 |
| Comparative example 2 | 25.5 | 68.6 |
As can be seen from the results in Table 1, in examples 1-3, the modification of the activated carbon with sulfuric acid solution increases the internal voids of the activated carbon, and significantly increases the specific surface area thereof; the sulfuric acid modified activated carbon is loaded with corn silk polysaccharide iron, and both polysaccharide and iron can form coordination bonds with amino nitrogen atoms of urea and creatinine, so that the prepared modified coconut shell activated carbon has higher adsorption capacity on urea and creatinine.
In example 4, the carbonization temperature is higher, the yield of carbonized materials is reduced, and the performance of the obtained carbonized materials is also reduced, so that the adsorption capacity of the prepared modified coconut shell activated carbon on urea and creatinine is relatively reduced.
In example 5, the water vapor activation time is longer, and the water vapor activation speed is higher, so that the comprehensive performance of the activated carbon is reduced, and the adsorption capacity of the prepared modified coconut shell activated carbon on urea and creatinine is relatively reduced.
The corn silk polysaccharide used in comparative example 1 has no iron-complexing effect, so that the adsorption capacity of the prepared modified coconut shell activated carbon on urea and creatinine is relatively reduced.
In comparative example 2, corn silk polysaccharide iron is not loaded, so that the prepared sulfuric acid modified activated carbon has minimum adsorption capacity to urea and creatinine.
The technical features of the above-described embodiments may be arbitrarily combined, and all possible combinations of the technical features in the above-described embodiments are not described for brevity of description, however, as long as there is no contradiction between the combinations of the technical features, they should be considered as the scope of the description.
Claims (10)
1. The preparation method of the modified coconut shell activated carbon is characterized by comprising the following steps of:
step (1): drying coconut shells, putting the coconut shells into a carbonization furnace, heating, preserving heat, carbonizing, and cooling to obtain carbonized materials;
step (2): crushing the carbonized material, introducing nitrogen, heating, stopping introducing nitrogen, switching to steam for activation, stopping heating, cutting off the steam, introducing nitrogen, cooling to room temperature to obtain an activated material, rinsing and drying to obtain activated coconut shell activated carbon;
step (3): crushing activated coconut shell activated carbon, adding the crushed activated carbon into sulfuric acid solution, oscillating at constant temperature, washing with distilled water to neutrality, and drying to constant weight to obtain sulfuric acid modified activated carbon;
step (4): adding sulfuric acid modified activated carbon into the corn silk polysaccharide iron-acetic acid solution, stirring in a water bath, and drying to obtain the modified coconut shell activated carbon.
2. The method for preparing modified coconut shell activated carbon according to claim 1, wherein the temperature is raised to 650-750 ℃ in the step (1), and the heat preservation carbonization time is 2-3h.
3. The method for preparing modified coconut shell activated carbon according to claim 1, wherein in the step (2), the temperature is raised to 850-950 ℃, and the water vapor activation time is 4-5h.
4. The method for producing modified coconut shell activated carbon according to claim 1, wherein the concentration of the sulfuric acid solution in the step (3) is 1mol/L to 10mol/L.
5. The method for preparing modified coconut shell activated carbon according to claim 1, wherein the mass ratio of corn silk polysaccharide iron to sulfuric acid modified activated carbon in the step (4) is 1 (30-40).
6. The method for preparing modified coconut shell activated carbon according to claim 5, wherein the preparation steps of corn silk polysaccharide iron in the step (4) are as follows:
step S1: weighing stigma Maydis, adding deionized water, performing constant temperature water bath, filtering, repeating the above steps for 2 times, mixing filtrates, concentrating the filtrate, adding absolute ethanol into the concentrated solution, sealing, standing in shade, filtering to obtain solid, sequentially washing the solid with absolute ethanol, acetone and diethyl ether, redissolving with distilled water, dialyzing with flowing water, precipitating with ethanol, and separating to obtain powdery stigma Maydis polysaccharide;
step S2: placing corn silk polysaccharide and trisodium citrate in a beaker, adding deionized water, stirring at constant temperature, regulating pH, dropwise adding ferric trichloride solution until solid appears in the solution, stopping dropwise adding, continuing heating and stirring, performing suction filtration, adding equal volume of absolute ethyl alcohol into filtrate, sealing, placing in a dark place, performing suction filtration, washing precipitate with absolute ethyl alcohol and acetone respectively, redissolving, dialyzing with deionized water, precipitating with alcohol, and separating to obtain powdery corn silk polysaccharide iron.
7. The method for preparing modified coconut shell activated carbon according to claim 6, wherein in the step S1, the mass ratio of corn silk to deionized water is 1 (10-20), and the volume ratio of concentrated filtrate to absolute ethyl alcohol is 1 (2-3).
8. The method for preparing modified coconut shell activated carbon according to claim 6, wherein the water bath temperature in the step S1 is 80-90 ℃ and the water bath time is 2.5-3.5h.
9. The method for preparing modified coconut shell activated carbon as recited in claim 6, wherein the pH is adjusted to 8-9 in step S2.
10. A modified coconut activated carbon obtained by the process of any one of claims 1-9.
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