CN115536022B - Biomass porous carbon material based on mangosteen shells and preparation method thereof - Google Patents
Biomass porous carbon material based on mangosteen shells and preparation method thereof Download PDFInfo
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- 239000003575 carbonaceous material Substances 0.000 title claims abstract description 71
- 240000006053 Garcinia mangostana Species 0.000 title claims abstract description 48
- 235000017048 Garcinia mangostana Nutrition 0.000 title claims abstract description 48
- 239000002028 Biomass Substances 0.000 title claims abstract description 41
- 238000002360 preparation method Methods 0.000 title abstract description 8
- 238000001035 drying Methods 0.000 claims abstract description 21
- 239000002131 composite material Substances 0.000 claims abstract description 18
- 230000003213 activating effect Effects 0.000 claims abstract description 16
- 239000000843 powder Substances 0.000 claims abstract description 13
- 238000005406 washing Methods 0.000 claims abstract description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 9
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- 239000003795 chemical substances by application Substances 0.000 claims abstract description 7
- 238000000034 method Methods 0.000 claims abstract description 7
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- 238000004140 cleaning Methods 0.000 claims abstract description 4
- 238000005554 pickling Methods 0.000 claims abstract description 3
- 238000001179 sorption measurement Methods 0.000 claims description 40
- JIAARYAFYJHUJI-UHFFFAOYSA-L zinc dichloride Chemical compound [Cl-].[Cl-].[Zn+2] JIAARYAFYJHUJI-UHFFFAOYSA-L 0.000 claims description 16
- 239000012190 activator Substances 0.000 claims description 14
- 230000004913 activation Effects 0.000 claims description 12
- 239000000463 material Substances 0.000 claims description 11
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 10
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 9
- 239000000975 dye Substances 0.000 claims description 9
- AVTYONGGKAJVTE-OLXYHTOASA-L potassium L-tartrate Chemical group [K+].[K+].[O-]C(=O)[C@H](O)[C@@H](O)C([O-])=O AVTYONGGKAJVTE-OLXYHTOASA-L 0.000 claims description 8
- 239000011592 zinc chloride Substances 0.000 claims description 8
- 235000005074 zinc chloride Nutrition 0.000 claims description 8
- 239000001472 potassium tartrate Substances 0.000 claims description 7
- 229940111695 potassium tartrate Drugs 0.000 claims description 7
- 235000011005 potassium tartrates Nutrition 0.000 claims description 7
- 238000010438 heat treatment Methods 0.000 claims description 5
- 229910052757 nitrogen Inorganic materials 0.000 claims description 5
- 239000002253 acid Substances 0.000 claims description 4
- 239000003242 anti bacterial agent Substances 0.000 claims description 3
- 229940088710 antibiotic agent Drugs 0.000 claims description 3
- 229910001385 heavy metal Inorganic materials 0.000 claims description 3
- 239000012535 impurity Substances 0.000 claims description 3
- 239000012855 volatile organic compound Substances 0.000 claims description 3
- 239000012298 atmosphere Substances 0.000 claims description 2
- 239000011261 inert gas Substances 0.000 claims description 2
- 238000003760 magnetic stirring Methods 0.000 claims description 2
- 238000012216 screening Methods 0.000 claims 1
- 239000002994 raw material Substances 0.000 abstract description 5
- 238000010000 carbonizing Methods 0.000 abstract description 4
- 238000007598 dipping method Methods 0.000 abstract description 3
- 239000002243 precursor Substances 0.000 abstract description 3
- IQFVPQOLBLOTPF-HKXUKFGYSA-L congo red Chemical compound [Na+].[Na+].C1=CC=CC2=C(N)C(/N=N/C3=CC=C(C=C3)C3=CC=C(C=C3)/N=N/C3=C(C4=CC=CC=C4C(=C3)S([O-])(=O)=O)N)=CC(S([O-])(=O)=O)=C21 IQFVPQOLBLOTPF-HKXUKFGYSA-L 0.000 description 26
- 239000011257 shell material Substances 0.000 description 17
- 239000011148 porous material Substances 0.000 description 11
- 239000000243 solution Substances 0.000 description 11
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 10
- ZCYVEMRRCGMTRW-UHFFFAOYSA-N 7553-56-2 Chemical compound [I] ZCYVEMRRCGMTRW-UHFFFAOYSA-N 0.000 description 9
- 238000002474 experimental method Methods 0.000 description 9
- 229910052740 iodine Inorganic materials 0.000 description 9
- 239000011630 iodine Substances 0.000 description 9
- 239000012086 standard solution Substances 0.000 description 8
- 229910052799 carbon Inorganic materials 0.000 description 6
- 239000000203 mixture Substances 0.000 description 6
- 238000002835 absorbance Methods 0.000 description 4
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Chemical compound [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 description 4
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- 238000006243 chemical reaction Methods 0.000 description 3
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- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
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- 231100000719 pollutant Toxicity 0.000 description 2
- 229910000027 potassium carbonate Inorganic materials 0.000 description 2
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- 235000013162 Cocos nucifera Nutrition 0.000 description 1
- 244000060011 Cocos nucifera Species 0.000 description 1
- FEWJPZIEWOKRBE-JCYAYHJZSA-L L-tartrate(2-) Chemical compound [O-]C(=O)[C@H](O)[C@@H](O)C([O-])=O FEWJPZIEWOKRBE-JCYAYHJZSA-L 0.000 description 1
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- GAMYVSCDDLXAQW-AOIWZFSPSA-N Thermopsosid Natural products O(C)c1c(O)ccc(C=2Oc3c(c(O)cc(O[C@H]4[C@H](O)[C@@H](O)[C@H](O)[C@H](CO)O4)c3)C(=O)C=2)c1 GAMYVSCDDLXAQW-AOIWZFSPSA-N 0.000 description 1
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 1
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- 239000002156 adsorbate Substances 0.000 description 1
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- 150000004636 anthocyanins Chemical class 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 125000004432 carbon atom Chemical group C* 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 229910002091 carbon monoxide Inorganic materials 0.000 description 1
- 239000007833 carbon precursor Substances 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
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- 235000020188 drinking water Nutrition 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
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- 239000000835 fiber Substances 0.000 description 1
- 229930003944 flavone Natural products 0.000 description 1
- 150000002212 flavone derivatives Chemical class 0.000 description 1
- 235000011949 flavones Nutrition 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 239000005431 greenhouse gas Substances 0.000 description 1
- 239000005556 hormone Substances 0.000 description 1
- 229940088597 hormone Drugs 0.000 description 1
- 239000010842 industrial wastewater Substances 0.000 description 1
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- 239000012452 mother liquor Substances 0.000 description 1
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- 239000003973 paint Substances 0.000 description 1
- 238000007146 photocatalysis Methods 0.000 description 1
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- 239000004033 plastic Substances 0.000 description 1
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- 235000013824 polyphenols Nutrition 0.000 description 1
- 229910052573 porcelain Inorganic materials 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 238000010298 pulverizing process Methods 0.000 description 1
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- 229940095064 tartrate Drugs 0.000 description 1
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- VHBFFQKBGNRLFZ-UHFFFAOYSA-N vitamin p Natural products O1C2=CC=CC=C2C(=O)C=C1C1=CC=CC=C1 VHBFFQKBGNRLFZ-UHFFFAOYSA-N 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/30—Active carbon
- C01B32/312—Preparation
- C01B32/342—Preparation characterised by non-gaseous activating agents
- C01B32/348—Metallic compounds
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/04—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of alkali metals, alkaline earth metals or magnesium
- B01J20/041—Oxides or hydroxides
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/06—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/20—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising free carbon; comprising carbon obtained by carbonising processes
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/30—Active carbon
- C01B32/312—Preparation
- C01B32/318—Preparation characterised by the starting materials
- C01B32/324—Preparation characterised by the starting materials from waste materials, e.g. tyres or spent sulfite pulp liquor
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/281—Treatment of water, waste water, or sewage by sorption using inorganic sorbents
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
- C02F2101/20—Heavy metals or heavy metal compounds
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Analytical Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Environmental & Geological Engineering (AREA)
- Materials Engineering (AREA)
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Water Supply & Treatment (AREA)
- Carbon And Carbon Compounds (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
Abstract
The invention provides a biomass porous carbon material based on mangosteen shells and a preparation method thereof, wherein the method comprises the following steps: (1) Cleaning, drying, crushing and sieving the mangosteen shells to obtain mangosteen shell powder; (2) Mixing the mangosteen shell powder with the composite activating agent, stirring, drying, activating, pickling, washing with water and drying to obtain the biomass porous carbon material based on the mangosteen shell. The porous biomass carbon material based on the mangosteen shells is prepared by taking the mangosteen shells as biomass raw materials, drying, crushing, mixing with a composite activating agent in a solution state, dipping, activating to obtain a precursor, and carbonizing at a high temperature.
Description
Technical Field
The invention belongs to the field of materials, and particularly relates to a biomass porous carbon material based on mangosteen shells and a preparation method thereof.
Background
Since organic dyes are widely used in paints, textiles and plastics, a large amount of waste water containing the dye is generated. The discharge of harmful organic dyes into water can damage the water environment and reduce the quality of drinking water. To alleviate this problem, methods for removing organic dyes from industrial wastewater include photocatalysis, adsorption, membrane filtration, etc., wherein adsorption is a mature and superior technology for its economy, convenience, and cost-effectiveness. Therefore, the preparation of the carbon material with high specific surface area and developed pore structure has important practical significance.
Biomass has the advantages of wide sources, low price, easy availability, zero net carbon dioxide emission and the like, and can be used as a raw material for preparing activated carbon. The porous carbon material mainly originates from agricultural wastes, such as coconut shells, rice hulls, wheat straws, sawdust, nut shells and the like, can be used as precursors of the porous carbon material to prepare the porous carbon material capable of removing dyes and other pollutants in wastewater. The biomass porous carbon is a byproduct of biomass pyrolysis and can be divided into micropores (aperture < 2 nm), mesopores (aperture < 2 nm) and macropores (aperture < 50 nm). Because the porous carbon material has a high specific surface area, more active sites can be provided for adsorbing different types of pollutants. Therefore, the catalyst has remarkable adsorption capacity for environmental pollutants such as dyes, heavy metals, volatile organic compounds and the like. Research and development into the extraction of biochar from biomass has provided a means of sustainable utilization of biomass, as well as environmental protection by reducing carbon footprint, pollution and greenhouse gases.
Mangosteen is a tropical fruit with an edible portion that is milky white and a pericarp that is dark red, accounting for about two-thirds of the total weight of the fruit. The pericarp is rich in anthocyanin and flavone, but most mangosteen shells are directly discarded into the environment by people because the pericarp is not well utilized, so that not only is serious waste of biomass resources caused, but also the environment is polluted. The mangosteen shell contains a large amount of fiber components and polyphenols, is a high-quality carbon precursor for preparing the porous carbon material, and can be obtained by drying, crushing, pyrolyzing and carbonizing the porous carbon material.
Disclosure of Invention
In view of the above, the invention aims to overcome the defects in the prior art, and provides a biomass porous carbon material based on mangosteen shells and a preparation method thereof.
In order to achieve the above purpose, the technical scheme of the invention is realized as follows:
the composite activator comprises potassium tartrate and zinc chloride, wherein the mass ratio of the potassium tartrate to the zinc chloride is 1:1-3:5.
a porous biomass carbon material based on mangosteen shells is prepared by stirring, drying, activating, washing and impurity removing the mangosteen shell powder and the composite activating agent in claim 1 or 2.
Further, the mass ratio of the mangosteen shell powder to the composite activator is 1:1-3; the temperature of the activation step is 400-900 ℃, the time is 1h, and the heating rate is 5-15 ℃/min.
The preparation method of the mangosteen shell-based biomass porous carbon material comprises the following steps:
(1) Cleaning, drying, crushing and sieving the mangosteen shells to obtain mangosteen shell powder;
(2) Mixing the mangosteen shell powder with the composite activating agent, stirring, drying, activating, pickling, washing with water and drying to obtain the biomass porous carbon material based on the mangosteen shell.
Further, the sieve mesh diameter of the sieving step in the step (1) is 80 meshes; the temperature of the drying step in the step (1) is 80 ℃ and the time is 4-6h.
Further, the mass ratio of the mangosteen shell powder to the composite activator in the step (2) is 1:1-3.
Further, the activation step in the step (2) adopts a tube furnace to perform activation treatment in an inert atmosphere; the temperature of the activation step is 400-900 ℃, the time is 1h, and the heating rate is 5-15 ℃/min; the inert gas is nitrogen, and the flow rate of the nitrogen is 20-100mL/min.
Further, the stirring step in the step (2) is magnetic stirring, and the time is 20-24 hours; the temperature of the drying step in the step (2) is 80-110 ℃ and the time is 2-3h; the acid liquor of the acid washing step in the step (2) is hydrochloric acid, and the concentration of the hydrochloric acid is 0.5-2mol/L.
The application of the porous biomass carbon material based on the mangosteen shell in preparing an adsorption material is that the porous biomass carbon material is used for adsorbing dyes, heavy metals, volatile organic compounds or antibiotics; the input amount of the biomass porous carbon material is 2-9mg/mL, and the adsorption time is 1-150 minutes.
The application of the composite activator in preparing the adsorption material.
Compared with the prior art, the invention has the following advantages:
the porous biomass carbon material based on the mangosteen shells is prepared by taking the mangosteen shells as biomass raw materials, drying, crushing, mixing with a composite activating agent in a solution state, dipping, activating to obtain a precursor, and carbonizing at a high temperature.
The porous biomass carbon material based on the mangosteen shell can be used for activating biomass by using an organic activator with mild properties and simultaneously can be used for self-activating so as to provide more carbon sources, and the compound inorganic activator can enable the pore structure of the porous carbon material to be more developed, so that the porous carbon material has rich pore structure and high specific surface area, and a new idea is provided for recycling agricultural wastes.
The porous biomass carbon material based on the mangosteen shell has excellent adsorption performance, can be used as an ideal adsorption material, can remove organic dye, antibiotics, environmental hormone and the like in wastewater, and expands the application field of the mangosteen shell.
The porous biomass carbon material based on the mangosteen shells takes the mangosteen shells as raw materials, and is prepared by carbonizing at normal pressure and high temperature, so that the source of the raw materials is wide, the price is low, the production process is simple and feasible, and the large-scale commercial production is possible.
Drawings
FIG. 1 is an electron microscopic view of a porous carbon material A according to example 1 of the present invention;
FIG. 2 is an electron microscopic view of the porous carbon material E according to example 1 of the present invention;
FIG. 3 is a graph showing N of the porous carbon material A according to example 1 of the present invention 2 Adsorption-desorption isotherm plot;
FIG. 4 is a pore size distribution diagram of a porous carbon material A according to example 1 of the present invention;
FIG. 5 is a graph showing the adsorption capacity and the removal rate of Congo red solutions with different concentrations adsorbed by the porous carbon material A according to the embodiment 2 of the present invention;
FIG. 6 is a graph showing the adsorption capacity and removal rate of Congo red solution by porous carbon material A with different input amounts according to example 3 of the present invention;
FIG. 7 is a graph showing the adsorption capacity and removal rate of Congo red solution by porous carbon material A in different time periods according to example 4 of the present invention;
FIG. 8 is a graph showing the adsorption capacity of porous carbon material A versus Congo red solution at various temperatures as described in example 5 of the present invention.
Detailed Description
Unless defined otherwise, technical terms used in the following examples have the same meaning as commonly understood by one of ordinary skill in the art to which the present invention pertains. The test reagents used in the following examples, unless otherwise specified, are all conventional biochemical reagents; the experimental methods are conventional methods unless otherwise specified.
The present invention will be described in detail with reference to examples.
Example 1 preparation of Biomass porous carbon Material
Removing outer hard peel of mangosteen shell, ultrasonically cleaning, drying, pulverizing to obtain mangosteen shell powder, and sieving with 80 mesh sieve;
mixing mangosteen shell powder with the compound activators in different proportions shown in table 1, adding 15ml of deionized water, stirring on a magnetic stirrer for 20h in a solution state, then placing the mixture into a porcelain boat, and drying in an oven at 80 ℃ for 2h to constant weight;
under the nitrogen atmosphere, placing the mixture into a tube furnace, heating to 700 ℃, controlling the heating rate to 5 ℃/min, activating the mixture for 1h at the nitrogen flow rate of 60mL/min, naturally cooling to room temperature, and taking out the mixture;
washing the activated sample with 1mol/L dilute hydrochloric acid to remove inorganic impurities in the product, and repeatedly washing the acid-washed material with deionized water until the acid-washed material is neutral. And then placing the washed material in an oven at 110 ℃ for drying for 4 hours to constant weight, so as to obtain the biomass porous carbon material of the mangosteen shell.
The test data of the prepared biomass porous carbon material are analyzed, and are specifically shown in table 1.
Table 1 test data for biomass porous carbon materials
As shown in Table 1, the iodine value of the porous carbon materials A-F prepared by the composite activator is larger than that of the porous carbon material E prepared by the single activator at the same activation temperature, probably due to the fact that the inorganic part of potassium tartrate forms potassium carbonate and the organic part (tartrate) introduces a carbon source for preparing the activated carbon, and when a certain temperature is reached, the potassium carbonate is decomposed to generate CO 2 With C, CO 2 Can enter into the inner rapid impact material of the mangosteen shell material, and K ions are inserted into the carbon matrix in the form of steam, so that the original pore structure is changed. As can be clearly seen from fig. 1, the porous carbon material a has a "honeycomb-shaped" pore structure, and micropores penetrate through the whole carbon skeleton, compared with fig. 2, the porous carbon material E has a rich pore structure, but mainly uses mesopores and macropores, which also shows that a proper amount of zinc chloride is compounded to react with carbon atoms generated by decomposition to generate a large amount of gas, so that the activation effect is achieved, more micropore structures are formed, and the pores become smaller and more uniform. Therefore, compared with a single activator, the iodine value of the porous carbon material prepared by the composite activation is higher. Compared with the A, B, C, D, the iodine adsorption values of the materials synthesized by dipping in different composite ratios are different, when the ratio of the potassium tartrate to the zinc chloride is 1.5:1, the iodine adsorption value of the porous carbon material A is highest and is 1068mg/g, the porous carbon material B is next to the porous carbon material B, and the porous carbon material C is lowest, so that it is known that the excessive addition of potassium tartrate and zinc chloride can lead to the reduction of the iodine adsorption value, and the reason is that the excessive addition of potassium tartrate can lead to the reduction of the iodine adsorption value due to insufficient pyrolysis of the carbon material, and the reduction of the pore structure. When zinc chloride is added in excess, micropores may collapse, forming more mesopores or macropores, so that the iodine adsorption value is lowered.In contrast to the porous material F, G, when the amount of mangosteen added is much greater than the composite activator, the iodine value also changes, which may be that the amount of activator added is too low, and insufficient activation results in a decrease in iodine value. As shown in FIG. 3, it can be seen that N of the porous carbon material A 2 The adsorption-desorption isotherm diagram has no obvious hysteresis loop, belongs to the I-type adsorption isotherm, is a typical micropore structure, and can be seen from fig. 4, the pore diameter of the porous carbon material A is gathered in the range of 2-10nm, which also shows that the material after composite activation is mainly micropores and mesopores.
Example 2 experiment of the influence of Congo Red solutions of different initial concentrations on adsorption Properties
Experiment for investigating influence of Congo red solutions with different initial concentrations on adsorption performance:
(1) The influence of Congo red standard solutions with different initial concentrations on the adsorption performance is studied by preparing the Congo red standard solutions:
preparing a standard solution: accurately weighing 1000mg of Congo red standard by an analytical balance, putting into a beaker, adding a certain amount of deionized water for dissolution, then fixing the volume into a volumetric flask in 1000mL to prepare 1g/L Congo red mother liquor, rapidly transferring to a blue cover bottle, wrapping with tinfoil, avoiding light, and storing in a refrigerator at 4 ℃;
the initial concentrations of Congo red solutions were set to seven gradients of 100mg/L, 150mg/L, 200mg/L, 250mg/L, 300mg/L, 350mg/L and 400mg/L, respectively, and the mother solutions were diluted to prepare Congo red standard solutions of different concentrations.
(2) Accurately weighing 5mg of porous carbon material A, adding 5mL of Congo red solution, placing on a shaking table at 25 ℃, adsorbing for 24 hours, filtering with a 5mL syringe and a 0.45m filter membrane, detecting the absorbance value of the adsorbed filtrate with a spectrophotometer, respectively making 3 parallel samples, and finally calculating the average value.
The porous carbon material A is used for adsorbing Congo red dye, and as shown in FIG. 5, after the adsorption in a Congo red standard solution with the concentration of 200mg/L for 24 hours, the adsorption capacity reaches to be 168.96mg/g at the maximum, and the removal rate is 84.49%.
Example 3 experiments on the Effect of different quality carbon materials on Congo Red adsorption Properties
Experiment for examining influence of biomass porous carbon materials with different qualities on Congo red adsorption performance:
the input amount of the porous carbon material A is set to be 3mg, 4mg, 5mg, 6mg, 7mg, 8mg and 9mg, seven gradients are respectively added with 5mL of Congo red standard solution with the concentration of 200mg/L, shaking is carried out for 24 hours at the temperature of 25 ℃, then the mixture is filtered, the absorbance value is detected by a spectrophotometer, 3 groups of parallel experiments are respectively carried out, and the average value is obtained.
The porous carbon material A is used for adsorbing Congo red dye, and as shown in FIG. 6, when the carbon material input amount is 5mg, the adsorption capacity reaches the highest point and is 164.71mg/g. The removal rate was 73.82%.
Example 4 experiment of the influence of different adsorption times on Congo Red adsorption Performance
Experiment for examining influence of different adsorption time on Congo red adsorption performance:
weighing 5mg of porous carbon material A, adding 5mL of Congo red standard solution with the concentration of 200mg/L, placing in a shaking table at 25 ℃, sampling at 5min, 25min, 50min, 100min, 150min, 200min, 250min, 300min, 350min and 400min respectively, filtering with a 5mL syringe and a 0.45 μm filter membrane, measuring the absorbance value of the filtrate with a spectrophotometer, and repeating the calculation of the average value three times.
The porous carbon material A is used for adsorbing Congo red dye, and as shown in FIG. 7, the adsorption capacity reaches the highest point at 50min, 94.95mg/g, and the removal rate is 47.52%.
Example 5 experiment to examine the Effect of different temperatures on Congo Red adsorption Performance
20mg of porous carbon material A and 80ml of Congo red standard solution with the concentration of 200mg/L are weighed, vibration operation is carried out for 1min on a vortex oscillator, and then the mixture is respectively put on water bath magnetic stirrers with different temperatures for reaction, wherein the temperatures are 25 ℃, 35 ℃ and 45 ℃. And then respectively taking a proper amount of solution by using a syringe within the time intervals of 5min, 25min, 50min, 100min, 150min, 200min, 250min, 300min, 350min and 400min, filtering, and measuring the absorbance value until the adsorption reaches an equilibrium state.
At different temperatures, the porous carbon material A is used for adsorbing Congo red dye, as shown in FIG. 8, the adsorption rate is faster in the first 100min of the reaction, the adsorption rate is slower between 100min and 400min, the adsorption equilibrium state is basically reached, the adsorption reaction is facilitated by increasing the temperature, and the contact between the adsorbate and the adsorbent is increased, so that the adsorption capacity is improved.
The foregoing description of the preferred embodiments of the invention is not intended to be limiting, but rather is intended to cover all modifications, equivalents, alternatives, and improvements that fall within the spirit and scope of the invention.
Claims (6)
1. A biomass porous carbon material based on mangosteen shells is characterized in that: the biomass porous carbon material is prepared by stirring, drying, activating, washing and removing impurities from mangosteen shell powder and a composite activating agent;
the composite activator is potassium tartrate and zinc chloride, and the mass ratio of the potassium tartrate to the zinc chloride is 1.5:1, a step of;
the mass ratio of the mangosteen shell powder to the composite activator is 1:1-3; the temperature of the activation step is 400-900 ℃, the time is 1h, and the heating rate is 5-15 ℃/min.
2. The method for preparing the mangosteen shell-based biomass porous carbon material, which is characterized by comprising the following steps of: the method comprises the following steps:
(1) Cleaning, drying, crushing and sieving the mangosteen shells to obtain mangosteen shell powder;
(2) Mixing the mangosteen shell powder with the composite activating agent, stirring, drying, activating, pickling, washing with water and drying to obtain the biomass porous carbon material based on the mangosteen shell.
3. The method for preparing the mangosteen shell-based biomass porous carbon material, according to claim 2, is characterized in that: the mesh diameter of the screening step in the step (1) is 80-100 meshes; the temperature of the drying step in the step (1) is 80-120 ℃ and the time is 4-6h.
4. The method for preparing the mangosteen shell-based biomass porous carbon material, according to claim 2, is characterized in that: the activation step in the step (2) adopts a tube furnace to perform activation treatment in inert atmosphere; the inert gas is nitrogen, and the flow rate of the nitrogen is 20-100mL/min.
5. The method for preparing the mangosteen shell-based biomass porous carbon material, according to claim 2, is characterized in that: the stirring step in the step (2) is magnetic stirring, and the time is 20-24 hours; the temperature of the drying step in the step (2) is 80-110 ℃ and the time is 2-3h; the acid liquor of the acid washing step in the step (2) is hydrochloric acid, and the concentration of the hydrochloric acid is 0.5-2mol/L.
6. The use of the mangosteen-shell-based biomass porous carbon material in preparing an adsorption material, which is characterized in that: the biomass porous carbon material is used for adsorbing dyes, heavy metals, volatile organic compounds or antibiotics; the input amount of the biomass porous carbon material is 2-9mg/mL, and the adsorption time is 1-150 minutes.
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| CN102275917A (en) * | 2011-07-26 | 2011-12-14 | 福建农林大学 | Preparation method of high-specific surface area mangosteen shell active carbon rich in mesopores |
| CN109879281A (en) * | 2019-03-19 | 2019-06-14 | 华中科技大学 | A kind of preparation method and product of biomass-based porous charcoal |
| EP3542896A1 (en) * | 2017-12-01 | 2019-09-25 | Jiangsu Academy of Agricultural Sciences | Malic acid and kmno4-based combined and modified cow dung biogas residue hydrochar preparation method |
| CN114804100A (en) * | 2022-05-13 | 2022-07-29 | 中南大学 | Porous carbon with ultrahigh specific surface area and preparation method thereof |
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| CN102275917A (en) * | 2011-07-26 | 2011-12-14 | 福建农林大学 | Preparation method of high-specific surface area mangosteen shell active carbon rich in mesopores |
| EP3542896A1 (en) * | 2017-12-01 | 2019-09-25 | Jiangsu Academy of Agricultural Sciences | Malic acid and kmno4-based combined and modified cow dung biogas residue hydrochar preparation method |
| CN109879281A (en) * | 2019-03-19 | 2019-06-14 | 华中科技大学 | A kind of preparation method and product of biomass-based porous charcoal |
| CN114804100A (en) * | 2022-05-13 | 2022-07-29 | 中南大学 | Porous carbon with ultrahigh specific surface area and preparation method thereof |
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