CN114733481B - Method for preparing composite activated carbon - Google Patents

Method for preparing composite activated carbon Download PDF

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CN114733481B
CN114733481B CN202210399146.2A CN202210399146A CN114733481B CN 114733481 B CN114733481 B CN 114733481B CN 202210399146 A CN202210399146 A CN 202210399146A CN 114733481 B CN114733481 B CN 114733481B
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microalgae
activated carbon
diameter
composite activated
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CN114733481A (en
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李立欣
付然
宋春莲
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Pingluo Derun Activated Carbon Co ltd
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Pingluo Derun Activated Carbon Co ltd
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    • 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
    • B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
    • B01J20/28054—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their surface properties or porosity
    • B01J20/28057—Surface area, e.g. B.E.T specific surface area
    • 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
    • B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
    • B01J20/28054—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their surface properties or porosity
    • B01J20/28078—Pore diameter
    • B01J20/2808—Pore diameter being less than 2 nm, i.e. micropores or nanopores
    • 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
    • B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
    • B01J20/28054—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their surface properties or porosity
    • B01J20/28078—Pore diameter
    • B01J20/28083—Pore diameter being in the range 2-50 nm, i.e. mesopores
    • 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
    • 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
    • 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
    • C01B32/354—After-treatment
    • C01B32/378—Purification
    • 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
    • C02F1/283—Treatment of water, waste water, or sewage by sorption using coal, charred products, or inorganic mixtures containing them
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00—Physical properties of inorganic compounds
    • C01P2006/12—Surface area
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00—Physical properties of inorganic compounds
    • C01P2006/16—Pore diameter
    • 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
    • C02F2101/36—Organic compounds containing halogen
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/13—Energy storage using capacitors

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Abstract

The invention belongs to the technical field of waste recycling, and discloses a method for preparing composite activated carbon, which comprises the following steps: pretreating microalgae; mixing raw materials; activating and carbonizing; and (5) treating a carbonized product. The method has the advantages that the harmful algae such as the water bloom red tide are recycled, the effect of purifying the water quality is achieved, the composite activated carbon prepared by the equipment has an excellent effect of removing polychlorinated biphenyl, and the composite activated carbon has extremely high practical value in the field of soil pollution restoration and has a wide application prospect.

Description

Method for preparing composite activated carbon
Technical Field
The invention belongs to the technical field of waste recycling, and particularly relates to a method for preparing composite activated carbon.
Background
In recent years, with a remarkable increase in the municipal sewage treatment level, the excess sludge yield is increasing. The sludge contains a large amount of organic matters, has relatively high carbon content and has the basic condition for preparing the adsorbent; the sludge generally contains a certain flocculant and stabilizer components, and the flocculant can provide a larger molecular cavity after pyrolysis, so that conditions are created for pore formation.
In some nutrient-rich water bodies, harmful microalgae such as microalgae, red tide microalgae and the like are propagated in a large quantity and grow rapidly, and under the high-temperature condition, harmful algae groups emit intolerable malodor and polluted air when decomposed, and meanwhile, a large amount of oxygen dissolved in water is consumed, so that massive fishes are choked and die. The conventional treatment cost is high, the effect is general, and harmful microalgae are not fully utilized, so that resources are wasted.
Polychlorinated biphenyls (PCBs) are typical environmentally persistent organic pollutants, and leakage from landfills, sludge fertilizers enriched with PCBs, and the use of PCBs in pesticide formulations all contribute to PCBs contamination of the soil environment. PCBs can be absorbed by plants and enter food chains, are enriched in organisms, and have strong carcinogenicity. At present, the most commonly used treatment methods for PCBs are physical, chemical and biological.
The activated carbon has the advantages of strong adsorptivity and catalytic performance, high safety, acid and alkali resistance, heat resistance, water and organic solvent insolubility, easy regeneration and the like, and is an environment-friendly adsorbent. Both excess sludge and microalgae are readily available carbonaceous materials and can therefore be used to prepare activated carbon. However, the conventional chemical method for preparing the activated carbon has the disadvantages of high consumption of the activating agent, low recovery rate, harm to the environment caused by the generated waste water and waste gas, and high equipment requirement and high cost. What is needed is a method and process for preparing activated carbon with low cost and stable effect and high removal rate of polychlorinated biphenyl.
Through the above analysis, the problems and defects existing in the prior art are as follows:
(1) The existing technology for preparing the activated carbon by using the excess sludge and the microalgae has the problems of unstable pore structure, low specific surface area and the like of the prepared activated carbon, and also needs various organic chemical agents, thus easily causing secondary pollution.
(2) In the polychlorinated biphenyl soil pollution restoration method, the problems of low treatment efficiency, high treatment cost, easiness in causing secondary pollution and the like exist.
The problems of the stability and specific surface area of the existing activated carbon holes can be effectively solved, the stability and feasibility of the algae-based carbon are improved, the raw material cost of the activated carbon is reduced, and the adsorption performance on polychlorinated biphenyl is improved, so that the research on the preparation method of the composite activated carbon has important significance.
Disclosure of Invention
Aiming at the problems existing in the prior art, the invention provides a method for preparing composite activated carbon.
The invention is realized by a method for preparing composite active carbon, which is characterized in that the method comprises the following steps: pretreating microalgae; mixing raw materials; activating and carbonizing; treating a carbonized product;
the microalgae pretreatment specifically comprises the following steps: the microalgae pumped and filtered from the lake are treated for three times, firstly solid particles with the particle size of more than 0.140mm are selected out, sieved, the particle microalgae with the particle size of 0.081-0.140mm are filtered, the agglomerate with the particle size of 0.002-0.081mm is vibrated and sieved, and the small particle microalgae with the particle size of less than 0.002mm after sieving are cleaned, dried and crushed, and are collected for standby;
the raw materials are mixed, and specifically comprise: mixing the residual sludge powder, the microalgae powder, the potassium carbonate and the ethylene glycol according to the mass ratio of 2:1-3:2:3-5 with a certain amount of distilled water, soaking and mixing fully, drying the mixture, and crushing the dried mixed raw materials after 12 hours;
the activated carbonization specifically comprises the following steps: the pretreated raw materials are put into a crucible, and N is introduced at a flow rate of 200mL/min 2 Air in the device is completely removed for 30min, and N is 2 Under the protection, after the temperature is increased to 900 ℃ from room temperature at the heating rate of 10 ℃/min, ammonia gas is introduced at the flow rate of 150mL/min to purge the active carbon for 2h, and N is the same as the ammonia gas 2 Naturally cooling to room temperature under the protection;
the carbonization product treatment specifically comprises: and (3) treating the carbonized product, sequentially adding 100ml of 1mol/L hydrochloric acid and 500ml of distilled water for acid water washing, stirring and suction-filtering, repeatedly flushing with distilled water until the washing liquid is neutral, suction-filtering, drying and crushing to obtain the composite activated carbon.
By combining all the technical schemes, the invention has the advantages that:
(1) According to the invention, ethylene glycol is added in the preparation process, is an organic solvent, has the capacity of combining two hydroxyl groups with alkali metal salt to form alkoxide, and can regulate and control the aperture of the activated carbon.
(2) The invention is introduced with N 2 Then, NH is introduced 3 The surface of the activated carbon is subjected to reduction treatment to cause the deletion of acidic oxygen-containing groups on the surface of the activated carbon, so that the content of alkaline groups on the surface of the activated carbon is increased, and nitrogen-containing functional groups are introduced while oxygen-containing functional groups are removed from the surface of the activated carbon, so that the adsorption performance of polychlorinated biphenyl is improved.
(3) The composite activated carbon prepared by the invention not only can further improve the adsorption capacity of the activated carbon, but also can relieve the pollution of harmful microalgae and the disposal of sludge to a certain extent, and simultaneously discharges the lake water after the microalgae are removed into the lake water, thereby achieving the effect of purifying the water quality, having great practical application value and low cost and realizing the full utilization of resources.
(4) The surface of the activated carbon sample has a large number of pore structures, the specific surface area is large, the surface of the activated carbon is provided with functional groups such as hydroxyl, nitro, carbonyl and the like, and has nitrogen functional groups, the contribution rate of micropores and mesopores of the activated carbon sample to pore volume is at a higher level, the contribution rate of the micropore volume of the mesopores is higher, and the effect of adsorbing polychlorinated biphenyl is good.
Drawings
FIG. 1 is a flow chart of a preparation method of composite activated carbon provided by the embodiment of the invention.
Fig. 2 is a device diagram of a preparation method of composite activated carbon provided by an embodiment of the invention.
(a-active carbon preparation device figure: 1-1-feed inlet, 1-2-drying device, 1-3-pulverizer, 1-4-inlet pipe, 1-5-exhaust pipe, 1-6-nitrogen, 1-7-crucible, 1-8-exhaust treatment device, 1-9-pump, 1-10-hydrochloric acid, 1-11-distilled water, 1-12-stirrer, 1-14-suction filtration device, 1-15-ammonia gas, 1-16-switch, 1-17 switch
b-harmful algae treatment device diagram: 2-1-a suction filtration device; 2-2-mesh grid; 2-3-macroporous separator plates; 2-4-scraping plate; 2-5-small pore separator; 2-6-water outlet; 2-7 parts of a discharge hole; 2-8 of a drying and crushing device; 2-9 spray heads; 2-10 vibration spring
FIG. 3 is a photograph of a high temperature charred product provided by an embodiment of the present invention.
FIG. 4 is a graph comparing the present invention with commercially available activated carbon to remove polychlorinated biphenyls.
FIG. 5 is a scanning electron microscope image of the catalyst prepared in example 1.
FIG. 6 is a scanning electron microscope image of the catalyst prepared in example 2.
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 view of the problems of the prior art, the present invention provides a method for preparing composite activated carbon, and the present invention is described in detail below with reference to the accompanying drawings.
S101, carrying out three treatments on microalgae pumped and filtered from a lake, firstly, picking out solid particles with the particle size of more than 0.140mm, sieving, filtering out the particles with the particle size of 0.081-0.140mm, vibrating and sieving the agglomerates with the particle size of 0.002-0.081mm, cleaning, drying and crushing the small particles with the particle size of less than 0.002mm after sieving, and collecting for later use;
s102, soaking and mixing the residual sludge powder, the microalgae powder, the potassium carbonate and the ethylene glycol according to the mass ratio of 2:1-3:2:3-5 and a certain amount of distilled water, drying the mixture for 12 hours, and crushing the dried mixed raw materials;
s103, placing the pretreated raw materials into a crucible, and introducing N at a flow rate of 200mL/min 2 Air in the device is completely removed for 30min, and N is 2 Under the protection, after the temperature is increased to 900 ℃ from room temperature at the heating rate of 10 ℃/min, ammonia gas is introduced at the flow rate of 150mL/min to purge the active carbon for 2h, and N is the same as the ammonia gas 2 Naturally cooling to room temperature under the protection;
s104, treating carbonized products, sequentially adding 100ml of 1mol/L hydrochloric acid and 500ml of distilled water for acid water washing, stirring and suction filtering, repeatedly washing with distilled water until the washing liquid is neutral, suction filtering, drying and crushing to obtain the composite activated carbon.
The technical scheme of the invention is further described below with reference to specific embodiments.
Example 1:
the application also provides a method for preparing the composite activated carbon, which specifically comprises the following steps:
(1) The microalgae pumped and filtered from the lake are treated for three times, firstly solid particles with the particle size of more than 0.140mm are selected out, sieved, the particle microalgae with the particle size of 0.081-0.140mm are filtered, the agglomerate with the particle size of 0.002-0.081mm is vibrated and sieved, and the small particle microalgae with the particle size of less than 0.002mm after sieving are cleaned, dried and crushed, and are collected for standby.
(2) Soaking and mixing the residual sludge powder, the microalgae powder, the potassium carbonate and the ethylene glycol according to the mass ratio of 1:1:2:2 and a certain amount of distilled water, drying at 60 ℃ for 12 hours, and crushing the dried mixed raw materials.
(3) The pretreated raw materials are put into a crucible, and N is introduced at a flow rate of 200mL/min 2 Air in the device is completely removed for 30min, and N is 2 Under the protection, after the temperature is increased to 900 ℃ from room temperature at the heating rate of 10 ℃/min, ammonia gas is introduced at the flow rate of 150mL/min to purge the active carbon for 2h, and N is the same as the ammonia gas 2 Naturally cooling to room temperature under the protection.
(4) And (3) treating the carbonized product, sequentially adding 100ml of 1mol/L hydrochloric acid and 500ml of distilled water for acid water washing, stirring and suction-filtering, repeatedly flushing with distilled water until the washing liquid is neutral, suction-filtering, drying and crushing to obtain the composite activated carbon.
The specific surface area of the composite activated carbon prepared in example 1 is 863.07m 2 The adsorption capacity of methylene blue is 696.6111mg/g, the removal rate of 2-ClBP (2-chlorobiphenyl) in soil by using the composite activated carbon prepared in the example 1 is 72.8%, the surface structure of the catalyst is smoother as shown in a scanning electron microscope chart shown in figure 5, a relatively complete pore structure is formed, and micropores account for about 80% -90%.
Example 2
An apparatus for preparing activated carbon, comprising: the device comprises a microalgae treatment area, a raw material mixing area, an activation carbonization area and a carbonization product treatment area. Each zone has access to the next zone, and the switch is turned on.
(1) Microalgae enter a treatment area through a suction filtration device 2-1, large solid particles (branches, leaves and the like) are intercepted outside by a grid 2-2, a large-pore partition board 2-3 intercepts some large-particle algae, the pore diameter of the large-pore partition board is 0.140mm, vibration springs 2-10 are arranged on two sides of the large-pore partition board 2-3, agglomerated microalgae are vibrated by vibration, the vibration frequency is 125rpm, the small-particle microalgae fall onto a small-pore partition board 2-5, the pore diameter of the small-pore partition board is 0.002mm, a spray header 2-9 is opened for cleaning the microalgae, waste water is discharged from a water outlet 2-6, the microalgae are sent into a drying and crushing device 2-8 by a scraping board 2-4, are sent into the drying and crushing device 2-8 for drying and crushing, and enter the next device through a discharge hole 2-7;
(2) Adding excess sludge powder into a raw material mixing area from a feed inlet 1-1, adding microalgae powder, potassium carbonate, ethylene glycol and a certain amount of distilled water according to a mass ratio of 2:1.5:2:3.5, fully soaking and mixing, drying the mixture by a drying device 1-2 at a set temperature of 60 ℃ for 12 hours, starting a pulverizer 1-3 switch, pulverizing the dried mixed raw materials, and improving an activation effect, wherein uniform mixing is facilitated;
(3) After the switch 1-16 is opened, the pretreated raw material enters into the crucible 1-7 of the activated carbonization zone, and is introduced into N at the flow rate of 200mL/min 2 Air in the device is completely removed for 30min, and N is 2 Under the protection, after the temperature is increased to 900 ℃ from room temperature at the heating rate of 10 ℃/min, ammonia gas is introduced at the flow rate of 150mL/min to purge the active carbon for 2h, and N is the same as the ammonia gas 2 Naturally cooling to room temperature under protection, and treating tail gas by a tail gas treatment device 1-8;
(4) After the switch 1-17 is opened, the activated carbonized product enters a carbonized product treatment area, 100ml of 1mol/L hydrochloric acid 1-10 and 500ml of distilled water 1-11 are sequentially added by a pump 1-9 for acid washing, so that impurities, soluble inorganic salt ash and degradation TDS concentration can be removed; the stirrers 1-12 are started, so that the acid water washing is more complete; then, through a suction filtration device 1-14, suction filtration is carried out, whether the washing liquid is neutral or not can be automatically detected, if not, distilled water 1-11 is needed to be continuously added, and the operation is repeated until the washing liquid is neutral;
(5) The sand core hopper 1-13 turns over by 90 degrees, the product after suction filtration is sent to the bottom of the carbonized product treatment area, the drying device 1-2 is started, the carbonized product is dried according to the set 60 ℃, the pulverizer 1-3 is started after 12 hours, the pulverizer 1-3 is rotated to pulverize, and the composite activated carbon is obtained and is collected into the carbon powder storage box.
The specific surface area of the composite activated carbon prepared in example 2 is 912.58m 2 Per gram, the methylene blue adsorption capacity is 705.5901mg/g, the removal rate of 2-ClBP (2-chlorobiphenyl) in soil by using the composite activated carbon prepared in example 2 is 76.5%, the catalyst scanning electron microscope chart is shown in figure 6, and the sample hasThe porous structure is more abundant, complete and uniform, and the micropores account for about 90%.
The embodiment shows that the composite activated carbon prepared by the invention has better performance, and the full utilization of residual sludge and microalgae resources is realized.
The foregoing is merely illustrative of specific embodiments of the present invention, and the scope of the invention is not limited thereto, but any modifications, equivalents, improvements and alternatives falling within the spirit and principles of the present invention will be apparent to those skilled in the art within the scope of the present invention.

Claims (5)

1. A method of preparing a composite activated carbon, the method comprising: pretreating microalgae; mixing raw materials; activating and carbonizing; treating a carbonized product;
microalgae pretreatment comprising: carrying out three treatments on the particle microalgae pumped and filtered from the lake, firstly filtering the particle microalgae through a screen with the diameter of 0.140mm to obtain particle microalgae with the diameter of less than 0.0140mm, secondly filtering the particle microalgae with the diameter of less than 0.140mm through a screen with the diameter of 0.081mm to obtain particle microalgae with the diameter of less than 0.081mm, finally vibrating the particle microalgae with the diameter of less than 0.081mm through a screen with the diameter of 0.002mm, cleaning, drying and crushing the small particle microalgae with the diameter of less than 0.002mm after sieving to obtain microalgae powder, and collecting for later use;
the raw materials are mixed, and specifically comprise: mixing the residual sludge powder, the microalgae powder, the potassium carbonate and the ethylene glycol according to the mass ratio of 2:1-3:2:3-5 and a certain amount of distilled water, soaking and mixing fully, drying the mixture, and crushing the dried mixed raw materials after 12 hours;
the activation carbonization specifically comprises the following steps: the pretreated raw materials are put into a crucible and introduced with N at a flow rate of 200mL/min 2 30 The air in the device is completely removed in min, N 2 Under the protection, after the temperature is increased to 900 ℃ from room temperature at the heating rate of 10 ℃/min, ammonia gas is introduced at the flow rate of 150mL/min to purge the active carbon 2h, and N is the same as the ammonia gas 2 Naturally cooling to room temperature under the protection;
the carbonization product treatment specifically comprises: and (3) treating the carbonized product, sequentially adding 100ml of 1mol/L hydrochloric acid and 500ml distilled water for acid washing, stirring and suction filtering, repeatedly flushing with distilled water until the washing liquid is neutral, suction filtering, drying and crushing to obtain the composite activated carbon.
2. The method for preparing composite activated carbon according to claim 1, wherein in the microalgae pretreatment, the microalgae are passed through screens with three pore diameters of 0.140mm,0.081mm and 0.002mm respectively.
3. A method of preparing composite activated carbon as claimed in claim 1, characterized in that in the activated carbonization, the nitrogen is replaced by one of argon or helium.
4. The method for preparing composite activated carbon according to claim 1, wherein in the activation carbonization, the carbonization temperature is 600-800 ℃.
5. The method for preparing composite activated carbon according to any one of claims 1 to 4, wherein the microalgae used in the microalgae powder is one of water bloom harmful microalgae or red tide harmful microalgae.
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CN111389366B (en) * 2020-04-20 2022-04-26 南华大学 Modification method of activated carbon, modified activated carbon and application thereof

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