CN116553542A - Method for preparing high-performance coconut shell activated carbon through gasification activation and application of high-performance coconut shell activated carbon - Google Patents
Method for preparing high-performance coconut shell activated carbon through gasification activation and application of high-performance coconut shell activated carbon Download PDFInfo
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 108
- 235000013162 Cocos nucifera Nutrition 0.000 title claims abstract description 92
- 244000060011 Cocos nucifera Species 0.000 title claims abstract description 92
- 238000000034 method Methods 0.000 title claims abstract description 44
- 230000004913 activation Effects 0.000 title claims abstract description 36
- 238000002309 gasification Methods 0.000 title claims abstract description 23
- 238000000498 ball milling Methods 0.000 claims abstract description 19
- 230000008569 process Effects 0.000 claims abstract description 16
- 239000007795 chemical reaction product Substances 0.000 claims abstract description 9
- 238000001354 calcination Methods 0.000 claims abstract description 8
- 238000010438 heat treatment Methods 0.000 claims description 19
- 239000002028 Biomass Substances 0.000 claims description 13
- 238000001035 drying Methods 0.000 claims description 10
- 239000002994 raw material Substances 0.000 claims description 8
- 229910052593 corundum Inorganic materials 0.000 claims description 7
- 239000010431 corundum Substances 0.000 claims description 7
- 238000001816 cooling Methods 0.000 claims description 6
- 229910001385 heavy metal Inorganic materials 0.000 claims description 6
- JPVYNHNXODAKFH-UHFFFAOYSA-N Cu2+ Chemical compound [Cu+2] JPVYNHNXODAKFH-UHFFFAOYSA-N 0.000 claims description 4
- 229910001431 copper ion Inorganic materials 0.000 claims description 4
- 150000002500 ions Chemical class 0.000 claims description 4
- -1 polytetrafluoroethylene Polymers 0.000 claims description 4
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 4
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 4
- 238000007873 sieving Methods 0.000 claims description 4
- 230000003213 activating effect Effects 0.000 claims description 3
- 239000000356 contaminant Substances 0.000 claims description 3
- 239000012299 nitrogen atmosphere Substances 0.000 claims description 3
- 238000001179 sorption measurement Methods 0.000 abstract description 14
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 abstract description 10
- 230000000694 effects Effects 0.000 abstract description 9
- 229910052757 nitrogen Inorganic materials 0.000 abstract description 5
- 125000004432 carbon atom Chemical group C* 0.000 abstract description 4
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 abstract description 3
- 230000009286 beneficial effect Effects 0.000 abstract description 3
- 239000013043 chemical agent Substances 0.000 abstract description 3
- 238000005265 energy consumption Methods 0.000 abstract description 3
- 238000005087 graphitization Methods 0.000 abstract description 3
- 238000009776 industrial production Methods 0.000 abstract description 3
- 229910052717 sulfur Inorganic materials 0.000 abstract description 3
- 239000011593 sulfur Substances 0.000 abstract description 3
- 239000013078 crystal Substances 0.000 abstract description 2
- 239000003446 ligand Substances 0.000 abstract description 2
- 239000000203 mixture Substances 0.000 abstract description 2
- 229910052698 phosphorus Inorganic materials 0.000 abstract description 2
- 239000011574 phosphorus Substances 0.000 abstract description 2
- 239000003814 drug Substances 0.000 abstract 1
- IISBACLAFKSPIT-UHFFFAOYSA-N bisphenol A Chemical compound C=1C=C(O)C=CC=1C(C)(C)C1=CC=C(O)C=C1 IISBACLAFKSPIT-UHFFFAOYSA-N 0.000 description 20
- 239000010949 copper Substances 0.000 description 12
- 229910052799 carbon Inorganic materials 0.000 description 7
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 5
- 229910052802 copper Inorganic materials 0.000 description 5
- 238000011065 in-situ storage Methods 0.000 description 5
- 238000004519 manufacturing process Methods 0.000 description 5
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 4
- 239000007789 gas Substances 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- 230000008901 benefit Effects 0.000 description 3
- 229910002091 carbon monoxide Inorganic materials 0.000 description 3
- 239000000446 fuel Substances 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 230000009467 reduction Effects 0.000 description 3
- 238000006722 reduction reaction Methods 0.000 description 3
- 239000002699 waste material Substances 0.000 description 3
- 239000012190 activator Substances 0.000 description 2
- 239000006227 byproduct Substances 0.000 description 2
- 229910002092 carbon dioxide Inorganic materials 0.000 description 2
- 239000001569 carbon dioxide Substances 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 238000002485 combustion reaction Methods 0.000 description 2
- 239000003344 environmental pollutant Substances 0.000 description 2
- 230000036541 health Effects 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 239000002957 persistent organic pollutant Substances 0.000 description 2
- 231100000719 pollutant Toxicity 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 238000000197 pyrolysis Methods 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 238000010792 warming Methods 0.000 description 2
- 239000002918 waste heat Substances 0.000 description 2
- 239000002351 wastewater Substances 0.000 description 2
- 238000003911 water pollution Methods 0.000 description 2
- 241000282412 Homo Species 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical group [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 238000003556 assay Methods 0.000 description 1
- 239000012298 atmosphere Substances 0.000 description 1
- 150000001720 carbohydrates Chemical class 0.000 description 1
- 235000014633 carbohydrates Nutrition 0.000 description 1
- 150000001721 carbon Chemical class 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 229920002678 cellulose Polymers 0.000 description 1
- 239000001913 cellulose Substances 0.000 description 1
- 239000003610 charcoal Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000003245 coal Substances 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000004134 energy conservation Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 230000003203 everyday effect Effects 0.000 description 1
- 125000005842 heteroatom Chemical group 0.000 description 1
- 239000010903 husk Substances 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 229920005610 lignin Polymers 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000010815 organic waste Substances 0.000 description 1
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N phenol group Chemical group C1(=CC=CC=C1)O ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 1
- 230000029553 photosynthesis Effects 0.000 description 1
- 238000010672 photosynthesis Methods 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 238000010248 power generation Methods 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 230000009919 sequestration Effects 0.000 description 1
- 239000012265 solid product Substances 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 241000894007 species Species 0.000 description 1
- 239000011550 stock solution 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
- C01B32/336—Preparation characterised by gaseous activating agents
-
- 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
-
- 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
- B01J20/30—Processes for preparing, regenerating, or reactivating
-
- 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
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Environmental & Geological Engineering (AREA)
- Analytical Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Materials Engineering (AREA)
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Water Supply & Treatment (AREA)
- Carbon And Carbon Compounds (AREA)
Abstract
A method for preparing high-performance coconut shell activated carbon by gasification activation and application thereof relate to a method for preparing high-performance coconut shell activated carbon. The invention aims to solve the problems of high energy consumption, long activation time and high cost of externally added medicaments in the prior art. The method comprises the following steps: 1. crushing coconut shells; 2. ball milling the crushed coconut shells and coconut bran; 3. calcining by sectional temperature control; 4. and (3) introducing hot steam into the reaction product for activation to obtain the high-performance coconut shell activated carbon. The method improves the performance of the activated carbon on two microcosmic levels of atomic composition and atomic configuration, and improves the graphitization degree of carbon atoms on one hand; on the other hand, nitrogen/sulfur/phosphorus hetero atoms are introduced to synchronously influence the spin effect, the charge effect, the ligand effect and the like of carbon atoms in the crystal lattice, so that the adsorption of organic matters is further enhanced. The whole process of the invention does not need to add chemical agents, has simple process flow and is beneficial to industrial production.
Description
Technical Field
The invention relates to a method for preparing high-performance coconut shell activated carbon.
Background
Global warming is an environmental problem that humans are facing in common, and global warming is increasingly exacerbated by the large amount of carbon dioxide emissions. In addition to taking measures to limit industrial carbon emissions, for CO in the atmosphere 2 The same is important for fixing and sealing. Crops play an indispensable role in carbon sequestration, and they fix carbon dioxide in the air into self-organic carbohydrates through photosynthesis. Coconut shells are a common agricultural byproduct, and currently, the annual production of coconut shell waste is up to 300 ten thousand tons worldwide, and the annual production of coconut shell waste in China is about 27 ten thousand tons, namely 740 tons of coconut shells are discarded every day on average. However, in many places, coconut shells are still regarded as garbage, and are usually discarded directly or burned in the open air, which not only limits the recycling of the coconut shells, but also is harmful to human health and aggravates environmental pollution and greenhouse effect.
Coconut shell is used as biomass rich in lignin and cellulose, and under the gasification of biomass, CO and CO can be generated on one hand 2 、H 2 、CH 4 And the like, can be directly used as fuel of an internal combustion engine, and can also be further processed and utilized, such as power generation, hydrogen production, liquid fuel production and the like, so that the consumption of fossil energy is reduced; on the other hand, biomass charcoal, which is a solid byproduct, can be converted into activated charcoal with high added value through further physical activation or chemical activation. Because of the high specific surface area and the porous structural characteristics, the activated carbon has excellent adsorption capacity, and meanwhile, the activated carbon has higher chemical stability, can bear the effects of high temperature and high pressure, and can be used in a larger pH range. At presentActivated carbon has been widely used in the fields of water pollution treatment, catalyst carrier development, and the like.
The existing method for preparing the activated carbon by using the coconut shells mainly comprises physical activation and chemical activation. Traditional physical activation is usually carried out with a single CO 2 The biomass raw material is activated, the process has high required temperature and long reaction time, and waste heat cannot be effectively utilized, so that higher energy consumption is often caused; in addition, the activators used in the existing chemical activation methods can be classified into basic (e.g., KOH, naOH) and acidic (e.g., H) 3 PO 4 ) Activators, which are not only generally costly but also corrosive to the production equipment, require post-treatment of the activated carbon produced and are therefore not suitable for large-scale production.
Disclosure of Invention
The invention aims to solve the problems of high energy consumption, long activation time and high cost of externally added agents in the prior art, and provides a method for preparing high-performance coconut shell activated carbon by gasification activation and application thereof.
The method for preparing the high-performance coconut shell activated carbon by gasification and activation is specifically completed by the following steps:
1. crushing coconut shells serving as raw materials in a crusher, sieving, and drying to obtain crushed coconut shells;
2. placing the crushed coconut shells, coconut brans and corundum balls into a planetary polytetrafluoroethylene ball milling tank, and then placing the ball milling tank into a planetary ball mill for ball milling to obtain mixed biomass;
3. placing the mixed biomass into a tube furnace for sectional temperature control calcination to obtain a reaction product;
4. and (3) introducing hot steam into the reaction product for activation to obtain the high-performance coconut shell activated carbon.
The principle of the invention is as follows:
the invention takes coconut shells as raw materials, adopts coconut bran to carry out doping modification, contains nitrogen, sulfur and phosphorus heteroatoms, and prepares high-performance activated carbon under the combination of gasification and activation, so that the method for comprehensively utilizing the coconut shells is achieved. Benefit (benefit)The method of the invention can prepare high-performance active carbon scientifically, reasonably, efficiently and environmentally-friendly, and obtain CO and CH 4 、H 2 And the like. The combustible gas generated in the biomass gasification process can replace coal as clean energy, and the combustion waste heat can be used for heating; meanwhile, the coconut shell activated carbon has a high specific surface area and a rich pore structure, has a certain graphitization degree, and can effectively adsorb bisphenol A (BPA) and heavy metal copper ions which are emerging pollutants; the invention can effectively realize the resource utilization of waste, energy conservation, emission reduction and water pollution treatment, and meanwhile, no chemical agent is needed to be added in the whole process, the process flow is simple, and the invention is beneficial to industrial production.
Compared with the prior art, the invention has the following beneficial effects:
1. the coconut husk is used as a raw material, the coconut bran is doped and modified, and all the raw materials come from a coconut processing industry chain;
2. the method improves the performance of the activated carbon on two microcosmic levels of atomic composition and atomic configuration, and improves the graphitization degree of carbon atoms on one hand; on the other hand, nitrogen/sulfur/phosphorus hetero atoms are introduced to synchronously influence the spin effect, the charge effect, the ligand effect and the like of carbon atoms in crystal lattices, so that the adsorption of organic matters is further enhanced;
3. the method adopts gasification and activation combination, realizes the gasification and activation combination by sectional temperature control, prepares the activated carbon and simultaneously generates clean combustible gas; the combustible components in the coconut shells are subjected to processes of drying, pyrolysis, oxidation, reduction and the like at high temperature to generate CO and H 2 、CH 4 And clean gas fuel; the solid product biochar generated by gasification is subjected to steam activation to further prepare active carbon; a large amount of heat released in the oxidation stage can be used in the drying, pyrolysis and reduction stages through heat conduction, so that the comprehensive utilization of gas, solid and heat in gasification preparation is realized; meanwhile, no chemical agent is needed to be added in the whole process, the process flow is simple, and the industrial production is facilitated.
Drawings
FIG. 1 is a graph of adsorption kinetics of activated carbon HC prepared in example 1 and H5P1-C prepared in example 2 to BPA;
FIG. 2 shows the process of example 1The prepared activated carbon HC and H5P1-C prepared in example 2 were combined with a metal-to-metal copper (Cu 2+ ) Is a graph of adsorption kinetics;
FIG. 3 shows the results of adsorption measurements of the coconut shell activated carbon HC prepared in example 1, the H5P1-C prepared in example 2, and the H3P3-C prepared in example 3.
Detailed Description
The first embodiment is as follows: the method for preparing the high-performance coconut shell activated carbon by gasification and activation is specifically completed by the following steps:
1. crushing coconut shells serving as raw materials in a crusher, sieving, and drying to obtain crushed coconut shells;
2. placing the crushed coconut shells, coconut brans and corundum balls into a planetary polytetrafluoroethylene ball milling tank, and then placing the ball milling tank into a planetary ball mill for ball milling to obtain mixed biomass;
3. placing the mixed biomass into a tube furnace for sectional temperature control calcination to obtain a reaction product;
4. and (3) introducing hot steam into the reaction product for activation to obtain the high-performance coconut shell activated carbon.
The second embodiment is as follows: the present embodiment differs from the specific embodiment in that: the drying temperature in the first step is 180-200 ℃, and the drying time is 2-3 h. The other steps are the same as in the first embodiment.
And a third specific embodiment: this embodiment differs from the first or second embodiment in that: in the first step, the coconut shells are crushed in a crusher and then are sieved by a sieve with 100-200 meshes. The other steps are the same as those of the first or second embodiment.
The specific embodiment IV is as follows: one difference between this embodiment and the first to third embodiments is that: the mass ratio of the crushed coconut shells to the coconut bran in the second step is (3-6) and (0-3). The other steps are the same as those of the first to third embodiments.
Fifth embodiment: one to four differences between the present embodiment and the specific embodiment are: the mass ratio of the total mass of the crushed coconut shells and the crushed coconut bran to the corundum balls in the second step is 6:100. Other steps are the same as those of the first to fourth embodiments.
Specific embodiment six: the present embodiment differs from the first to fifth embodiments in that: the ball milling speed in the second step is 650 r/min-750/min, and the ball milling time is 1.5 h-2 h. Other steps are the same as those of the first to fifth embodiments.
Seventh embodiment: one difference between the present embodiment and the first to sixth embodiments is that: the specific process of the sectional temperature control calcination in the third step comprises the following steps: under the protection of nitrogen atmosphere, heating to 200-600 ℃ at a heating rate of 5-10 ℃ per minute for 2-3 h, heating to 600-800 ℃ at a heating rate of 5-10 ℃ per minute, heating for 2-3 h, cooling to 650-600 ℃ at a cooling rate of 5-10 ℃ per minute, and preserving heat for 1.5-2 h at 650-600 ℃. Other steps are the same as those of embodiments one to six.
Eighth embodiment: one difference between the present embodiment and the first to seventh embodiments is that: the specific process of hot steam activation in the fourth step comprises the following steps: heating the tube furnace to 800-950 ℃, introducing steam into the tube furnace, and activating reheat steam for 2-3 h to obtain the coconut shell activated carbon. The other steps are the same as those of embodiments one to seven.
Detailed description nine: the embodiment is a high-performance coconut shell activated carbon for adsorbing organic pollutants and heavy metal ions. Other steps are the same as those of embodiments one to eight.
Detailed description ten: the difference between this embodiment and the ninth embodiment is that: the organic pollutant is bisphenol A; the heavy metal ions are copper ions. The other steps are the same as in embodiment nine.
The following examples are used to verify the benefits of the present invention:
example 1: the method for preparing the high-performance coconut shell activated carbon by gasification and activation is completed according to the following steps:
1. crushing coconut shells serving as a raw material in a crusher, sieving the crushed coconut shells by a 200-mesh sieve, and drying the crushed coconut shells at 200 ℃ for 2 hours to obtain crushed coconut shells;
2. placing the crushed coconut shells, coconut brans and corundum balls into a planetary polytetrafluoroethylene ball milling tank, and then placing the ball milling tank into a planetary ball mill for ball milling to obtain mixed biomass;
the mass ratio of the crushed coconut shells to the coconut bran in the second step is 6:0;
the mass ratio of the total mass of the crushed coconut shells and the crushed coconut brans to the corundum balls is 6:100;
the ball milling speed in the second step is 700rpm, and the ball milling time is 2 hours;
3. placing the mixed biomass into a tube furnace for sectional temperature control calcination to obtain a reaction product;
the specific process of the sectional temperature control calcination in the third step comprises the following steps: heating to 600 ℃ at a heating rate of 10 ℃/min under the protection of nitrogen atmosphere for 2 hours, heating to 800 ℃ at a heating rate of 10 ℃/min, heating for 2 hours, cooling to 600 ℃ at a cooling rate of 10 ℃/min, and preserving heat for 2 hours at 600 ℃;
4. and (3) introducing hot steam into the reaction product for activation to obtain the high-performance coconut shell activated carbon.
The specific process of hot steam activation in the fourth step comprises the following steps: and (3) heating the tube furnace to 800 ℃, introducing steam into the tube furnace, and activating reheat steam for 2 hours to obtain the coconut shell activated carbon (HC).
Example 2: the difference between this embodiment and embodiment 1 is that: the mass ratio of the crushed coconut shells to the coconut bran in the second step is 5:1; and step four, obtaining the in-situ nitrogen-doped high-performance coconut shell activated carbon (H5P 1-C). Other steps and parameters were the same as in example 1.
Example 3: the difference between this embodiment and embodiment 1 is that: the mass ratio of the crushed coconut shells to the coconut bran in the second step is 3:3; and step four, obtaining the in-situ nitrogen-doped high-performance coconut shell activated carbon (H3P 3-C). Other steps and parameters were the same as in example 1.
The embodiment of the invention comprises bisphenol A (BPA) and metallic cupric (Cu) 2+ ) Waste water is used as typical organic waste difficult to degradeAnd (3) water. Contains BPA and metallic cupric (Cu) 2+ ) The wastewater has the property of being difficult to biodegrade, not only seriously damages the aquatic ecosystem, but also seriously threatens human health. The examples thus select phenolic species as the target contaminant. Taking the samples as the absorption evaluation of bisphenol A (BPA) and heavy metal copper ions which are emerging pollutants in water treatment, wherein the specific operation method comprises the following steps:
the prepared standard stock solution of BPA with the concentration of 5g/L is diluted to 50mg/L, 100mg/L, 150mg/L, 200mg/L, 250mg/L and 300mg/L by deionized water respectively. The dosage of the active carbon HC and the H5P1-C is 0.5g/L, a 100mL reaction system is prepared, the reaction system is placed on a magnetic stirrer with constant temperature of 25 ℃ and is stirred for 12 hours at a speed of 300rpm, and then sampling is carried out to determine the concentration of BPA.
Metallic bivalent copper (Cu) 2+ ) The concentration gradient of the solution was set to 30mg/L, 50mg/L, 100mg/L, 150mg/L, 200mg/L, 300mg/L, and the rest of the procedure was the same as that of the BPA assay.
The invention prepares the high-performance active carbon (H5P 1-C) by using the heteroatom doping modification and gasification activation combined technology, has the maximum adsorption capacity of 161.29mg/g to BPA and has the maximum adsorption capacity to metal bivalent copper (Cu) 2+ ) The maximum adsorption amount was 6.45mg/g. The method is improved by 62.10 percent and 24.28 percent respectively compared with the prior modification.
FIG. 1 is a graph of adsorption kinetics of activated carbon HC and H5P1-C to BPA;
FIG. 2 shows activated carbon HC and H5P1-C vs. metallic copper (Cu 2+ ) Is a graph of adsorption kinetics;
FIG. 3 shows the results of adsorption measurements of coconut shell activated carbon HC, in situ doped nitrogen activated carbon H5P1-C, and in situ doped nitrogen activated carbon H3P 3-C;
as can be seen from fig. 3: when the coconut shell powder and the coconut bran powder are doped in situ according to the proportion of 5:1, the adsorption saturation capacity is highest, and bisphenol A (BPA) and metallic bivalent copper (Cu) are treated in water 2+ ) The adsorption effect of (2) is best.
Claims (10)
1. A method for preparing high-performance coconut shell activated carbon by gasification and activation is characterized by comprising the following steps:
1. crushing coconut shells serving as raw materials in a crusher, sieving, and drying to obtain crushed coconut shells;
2. placing the crushed coconut shells, coconut brans and corundum balls into a planetary polytetrafluoroethylene ball milling tank, and then placing the ball milling tank into a planetary ball mill for ball milling to obtain mixed biomass;
3. placing the mixed biomass into a tube furnace for sectional temperature control calcination to obtain a reaction product;
4. and (3) introducing hot steam into the reaction product for activation to obtain the high-performance coconut shell activated carbon.
2. The method for preparing high-performance coconut shell activated carbon by gasification and activation according to claim 1, wherein the drying temperature in the step one is 180-200 ℃ and the drying time is 2-3 h.
3. The method for preparing high-performance coconut shell activated carbon by gasification and activation according to claim 1, wherein in the first step, the coconut shell is crushed in a crusher and then passes through a 100-200-mesh sieve.
4. The method for preparing high-performance coconut shell activated carbon by gasification and activation according to claim 1, wherein the mass ratio of the crushed coconut shell to the coconut bran in the second step is (3-6): 0-3.
5. The method for preparing high-performance coconut shell activated carbon by gasification and activation as claimed in claim 1, wherein the mass ratio of the total mass of the crushed coconut shells and coconut bran to the corundum balls in the second step is 6:100.
6. The method for preparing high-performance coconut shell activated carbon by gasification and activation according to claim 1, wherein the ball milling speed in the second step is 650 r/min-750/min, and the ball milling time is 1.5 h-2 h.
7. The method for preparing high-performance coconut shell activated carbon by gasification and activation according to claim 1, which is characterized in that the specific process of the sectional temperature-control calcination in the step three is as follows: under the protection of nitrogen atmosphere, heating to 200-600 ℃ at a heating rate of 5-10 ℃ per minute for 2-3 h, heating to 600-800 ℃ at a heating rate of 5-10 ℃ per minute, heating for 2-3 h, cooling to 650-600 ℃ at a cooling rate of 5-10 ℃ per minute, and preserving heat for 1.5-2 h at 650-600 ℃.
8. The method for preparing high-performance coconut shell activated carbon by gasification and activation according to claim 1, wherein the specific process of hot steam activation in the fourth step is as follows: heating the tube furnace to 800-950 ℃, introducing steam into the tube furnace, and activating reheat steam for 2-3 h to obtain the coconut shell activated carbon.
9. The use of a high performance coconut shell activated carbon as recited in claim 1, wherein the high performance coconut shell activated carbon is used for adsorbing organic contaminants and heavy metal ions.
10. The use of a high performance coconut shell activated carbon as recited in claim 9 wherein said organic contaminant is bisphenol a; the heavy metal ions are copper ions.
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