CN106179216A - The preparation method of a kind of Magnetic Activated hydro-thermal charcoal and application - Google Patents

The preparation method of a kind of Magnetic Activated hydro-thermal charcoal and application Download PDF

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Publication number
CN106179216A
CN106179216A CN201610606211.9A CN201610606211A CN106179216A CN 106179216 A CN106179216 A CN 106179216A CN 201610606211 A CN201610606211 A CN 201610606211A CN 106179216 A CN106179216 A CN 106179216A
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hydro
charcoal
thermal
thermal charcoal
magnetic activated
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王博
郭仕林
李法云
范志平
杨登越
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Liaoning Shihua University
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Liaoning Shihua University
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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
    • B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/0203—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04
    • B01J20/0225—Compounds of Fe, Ru, Os, Co, Rh, Ir, Ni, Pd, Pt
    • B01J20/0229—Compounds of Fe
    • 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
    • B01J20/0203—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04
    • B01J20/024—Compounds of Zn, Cd, Hg
    • B01J20/0244—Compounds of Zn
    • 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
    • B01J20/28002—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 physical properties
    • B01J20/28009—Magnetic properties
    • 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
    • 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
    • C02F1/288—Treatment of water, waste water, or sewage by sorption using composite sorbents, e.g. coated, impregnated, multi-layered
    • 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
    • B01J2220/00—Aspects relating to sorbent materials
    • B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
    • B01J2220/46—Materials comprising a mixture of inorganic and organic materials
    • 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
    • B01J2220/00—Aspects relating to sorbent materials
    • B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
    • B01J2220/48—Sorbents characterised by the starting material used for their preparation
    • B01J2220/4806—Sorbents characterised by the starting material used for their preparation the starting material being of inorganic character
    • 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
    • B01J2220/00—Aspects relating to sorbent materials
    • B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
    • B01J2220/48—Sorbents characterised by the starting material used for their preparation
    • B01J2220/4812—Sorbents characterised by the starting material used for their preparation the starting material being of organic character
    • B01J2220/4843—Algae, aquatic plants or sea vegetals, e.g. seeweeds, eelgrass
    • 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

Abstract

The present invention relates to preparation method and the application of a kind of Magnetic Activated hydro-thermal charcoal, comprise the steps: that water plant powder and deionized water are carried out hydro-thermal reaction in a kettle. prepares hydro-thermal charcoal；Subsequently by hydro-thermal charcoal, FeCl3、ZnCl2It is dried after being sufficiently mixed with deionized water；Then dried biased sample is put in box atmosphere furnace; it is pyrolyzed in target temperature final temperature under nitrogen protective condition; prepare Magnetic Activated hydro-thermal charcoal; utilize the Magnetic Activated hydro-thermal biological carbon materials prepared by the method can the effectively heavy metal lead in a large amount of water body of Adsorption and copper; in the soil that composite prepared by this method also can add lead to, copper exceeds standard; reduce Lead In Soil, the biological effectiveness of copper, play the purpose of resistance control heavy metal.

Description

The preparation method of a kind of Magnetic Activated hydro-thermal charcoal and application
Technical field
The invention belongs to water-treatment technology field, be specifically related to the preparation method of a kind of Magnetic Activated hydro-thermal charcoal and answer With.
Background technology
Along with developing rapidly of China's economy, increasing to water demand amount, but the pollution problem of simultaneously water resource The most serious.In numerous water pollute, heavy metal pollution account for sizable ratio.And heavy metal pollution is easily at biology Chain is enriched with and expands, and toxicity is relatively big, therefore in water heavy metals exceeding standard and the problem serious harm that causes thereof to giving birth to State environment and the life and health of the mankind.Wherein, China's lead (Pb) pollutes and copper (Cu) pollutes and is particularly acute.In recent years, China Occur in that a lot of lead contamination and copper staining contamination accident successively.As 2009, the blood lead that just exposes more than 2010 exceeds standard thing Part, causes the Fujian Zijin Mining copper-containing acid waste water seepage event etc. of river, spit of fland large area malignant pollution for 2010.
Existing include ion exchange, absorption, coagulation, a large amount for the treatment of technologies of membrane filtration, for remove lead in waste water, Copper.In these methods, absorption be known one more economically with simple processing method.Therefore, low cost, high power capacity are found Heavy metal lead and the demand of adsorbent of copper increase.
Recently, the charcoal made with agricultural wastes (such as plant straw, excrement of animals etc.), owing to its raw material compares Single, it is substantially free of Toxic matter, and improves water body environment aspect as adsorbent and show positive role and receive much concern.Raw Thing charcoal is by plant biomass in the case of anoxia wholly or in part, through the difficulty of the class height aromatization that cracking carbonization produces Fusibleness solids.There is porous and substantial amounts of surface negative charge shows stronger heavy metal adsorption, it is possible to absorption bag Include lead, copper in interior various heavy.Therefore can be using charcoal as the lead in adsorbent polluted water body, copper.
But, charcoal itself prepared by traditional cracking charring has that productivity is relatively low, specific surface area is relatively low and is difficult to The problems such as separation and recovery, cause actual application the most limited.
Summary of the invention
It is contemplated that in place of overcoming the deficiencies in the prior art, and provide one to utilize water plant garbage as former material Material, the method preparing Magnetic Activated hydro-thermal charcoal；Solve in prior art the charcoal productivity of preparation and specific surface area relatively Problem low, that be difficult to separation and recovery.
For solving above-mentioned technical problem, the present invention is achieved in that
Utilize water plant garbage as raw material, the method preparing Magnetic Activated hydro-thermal charcoal, can be real as follows Execute:
Step (1), by water plant natural air drying so that it is inner aqueous rate be less than 10%, then pulverized 100 mesh sieve, it is thus achieved that Water plant powder；
Step (2), weigh step (1) described water plant powder, put in reactor and add deionized water；
Baking oven put into by step (3), step (2) described reactor, temperature programming to target temperature, when keeping final temperature to be pyrolyzed one section Between；After pyrolytic process terminates, take out product and clean with ethanol and deionized water successively, dry at 80 DEG C and both prepared water Hot charcoal；
Step (4), weigh step (3) described hydro-thermal charcoal, grind 100 mesh sieve, it is thus achieved that hydro-thermal charcoal powder；
Step (5), weigh step (4) described hydro-thermal charcoal powder, with FeCl3And ZnCl2Mixing, joins deionized water In, it is thus achieved that biased sample；
Step (6), by step (5) described biased sample, put in gas bath constant temperature oscillator certain with certain rotating speed constant temperature oscillation Time, at a temperature of 80 DEG C, after taking-up, it is dried to obtain hydro-thermal charcoal powder, FeCl3And ZnCl2Be sufficiently mixed thing；
Step (7), weigh step (6) described hydro-thermal charcoal powder, FeCl3And ZnCl2The thing that is sufficiently mixed be placed in box In atmosphere furnace, in stove, it is passed through certain flow rate nitrogen；Temperature programming, to target temperature, keeps the pyrolysis of certain time final temperature；Pyrolysis After process terminates, take out after charcoal naturally cools to room temperature, be cleaned multiple times to neutrality with deionized water；In 80 DEG C of drying, I.e. prepare Magnetic Activated hydro-thermal charcoal.
Further, the one during water plant is phragmites communis, Herba Typhae or hay grass described in described step (1).
Further, in described step (2), the mass volume ratio of water plant powder and deionized water is 1:50；Wherein water The mass unit of raw plant powder is gram, and the unit of deionized water volume is milliliter.
Further, in described step (3), baking oven target temperature is 200 DEG C；At 200 DEG C, final temperature pyrolysis continues 6 h.
Further, hydro-thermal charcoal powder, FeCl in described step (5)3、ZnCl2Mass volume ratio with deionized water Ratio is 4:2:1:20, wherein water plant powder, FeCl3、ZnCl2Mass unit be gram that the unit of deionized water volume is milli Rise.
Further, biased sample 150 r min in gas bath constant temperature oscillator in described step (6)-1Constant temperature oscillation, The concussion time is 24 h.
Further, in described step (7), in box atmosphere furnace, nitrogen flow rate is 400 mL/min；Programmed rate control 4 DEG C/min of system；Target temperature is 500 DEG C；At 500 DEG C, final temperature pyrolysis continues 90 min.
Advantages of the present invention effect is as follows:
The present invention utilizes the water plant garbage being widely present nearby water bodies to prepare charcoal as raw material, the employing of innovation The higher hydro-thermal method of productivity prepares charcoal, and with FeCl3As Magnetic reagent, ZnCl2As activator, use novel synchronization The method of the hot charcoal of activated and magnetic water, prepares the Magnetic Activated water that productivity is high and not only have bigger serface but also can simply reclaim Hot charcoal, the application of extension hydro-thermal charcoal.Magnetic Activated hydro-thermal charcoal can be used to process contaminated by heavy metals water Body or the emergency processing to burst heavy metal pollution accident water body, be a class have that great potential is novel, environmental protection and low cost Adsorbent.The recycling being prepared as abandoned biomass of Magnetic Activated hydro-thermal charcoal provides road, for organic dirt Dye controls to provide the technology of " green ", it is to avoid the environmental problem that abandoned biomass causes, it is achieved " treatment of wastes with processes of wastes against one another, recycling economy " Purpose.
Compared with prior art, the present invention has a characteristic that
(1) the Magnetic Activated hydro-thermal charcoal that the present invention provides, the water plant garbage of utilization is very cheap and easy Obtain raw material.
(2) the Magnetic Activated hydro-thermal charcoal that the present invention provides, uses hydro-thermal method and is prepared, prepared by this kind of method Charcoal higher with charcoal productivity prepared by traditional cracking carbonizatin method.
(3) compared with existing charcoal or class charcoal adsorber technologies, the Magnetic Activated hydro-thermal that the present invention provides is biological Charcoal, owing to activation has bigger specific surface area, the adsorption effect of heavy metal lead, copper etc. is more preferable.
(4) the Magnetic Activated hydro-thermal charcoal that the present invention provides, has stronger magnetic, can lead to after using in water body Cross magnetic force to reclaim.
(5) Magnetic Activated hydro-thermal charcoal prepared by the present invention, has suitable stability, can use pickling etc. after absorption Way desorption and regeneration is reused.
(6) Magnetic Activated hydro-thermal charcoal prepared by the present invention, it is also possible to extra environmental benefit, such as carbon sequestration are provided And soil improvement.
(7) preparation method that the present invention provides is simple, cheap, it is easy to industrialized production.
Accompanying drawing explanation
The invention will be further described with detailed description of the invention below in conjunction with the accompanying drawings.Protection scope of the present invention not only office It is limited to the statement of following content.
Fig. 1 is the process flow diagram of the present invention；
Fig. 2 is the scanning electron microscope (SEM) photograph of Magnetic Activated hydro-thermal phragmites communis charcoal；
Fig. 3 is the 10 g Magnetic Activated hydro-thermal phragmites communis charcoal adsorption effect figure to the waste water that 1 L lead content is 100 mg/L.
Fig. 4 is the 10 g Magnetic Activated hydro-thermal phragmites communis charcoal adsorption effect to the waste water that 1 L copper content is 100 mg/L Figure.
Detailed description of the invention
The constant-temperature table that the present invention uses Ai Ce company limited to produce in an embodiment is stirred, and uses Shanghai travel incognito stove The box atmosphere furnace of MXQ that industry company limited produces carries out high temperature anaerobic cracking, uses north point Rayleigh WFX-310 atomic absorption instrument Measure heavy metal lead and the concentration of copper.
Embodiment Al
(1) by phragmites communis natural air drying so that it is inner aqueous rate is less than 10%, then pulverizes 100 mesh sieve, it is thus achieved that water plant Powder；
(2) weigh step (1) described phragmites communis powder, put in reactor and add a certain amount of deionized water.Phragmites communis powder with The mass volume ratio of deionized water is 1:50；Wherein the mass unit of phragmites communis powder is gram, and the unit of deionized water volume is milli Rise；
(3) baking oven put into by step (2) described reactor, temperature programming to 200 DEG C, keeps final temperature to be pyrolyzed 6 h；Pyrolytic process terminates After, take out product and clean with ethanol and deionized water successively, dry at 80 DEG C and both prepared hydro-thermal phragmites communis charcoal；
(4) weigh step (3) described hydro-thermal phragmites communis charcoal, ground 100 mesh sieve, it is thus achieved that hydro-thermal phragmites communis biology powdered carbon End；
(5) the described a certain amount of hydro-thermal phragmites communis charcoal powder of step (4), FeCl are weighed3、ZnCl2And deionized water is with 4:2: 1:20 mixes, it is thus achieved that biased sample.Wherein hydro-thermal phragmites communis charcoal powder, FeCl3、ZnCl2Mass unit be gram, deionization The unit of water volume is milliliter；
(6) by step (5) described biased sample, put in gas bath constant temperature oscillator with 150 r min-1Constant temperature oscillation 24 h, At a temperature of 80 DEG C, hydro-thermal phragmites communis charcoal powder, FeCl it is dried to obtain after taking-up3And ZnCl2Be sufficiently mixed thing.
(7) step (6) described hydro-thermal phragmites communis charcoal powder, FeCl are weighed3And ZnCl2The thing that is sufficiently mixed be placed in case In formula atmosphere furnace, being passed through 400 mL/min flow velocity nitrogen in stove, programmed rate controls 4 DEG C/min, and target temperature is 500 DEG C, at 500 DEG C, final temperature pyrolysis continues 90 min.After pyrolytic process terminates, take after phragmites communis charcoal naturally cools to room temperature Go out, be cleaned multiple times to neutrality with deionized water；In 80 DEG C of drying, i.e. prepare Magnetic Activated hydro-thermal phragmites communis charcoal.
Embodiment A2
(1) by Herba Typhae natural air drying so that it is inner aqueous rate is less than 10%, then pulverizes 100 mesh sieve, it is thus achieved that water plant Powder；
(2) weigh step (1) described typha powder, put in reactor and add a certain amount of deionized water.Typha powder with The mass volume ratio of deionized water is 1:50；Wherein the mass unit of typha powder is gram, and the unit of deionized water volume is milli Rise；
(3) baking oven put into by step (2) described reactor, temperature programming to 200 DEG C, keeps final temperature to be pyrolyzed 6 h；Pyrolytic process terminates After, take out product and clean with ethanol and deionized water successively, dry at 80 DEG C and both prepared hydro-thermal Herba Typhae charcoal；
(4) weigh step (3) described hydro-thermal Herba Typhae charcoal, ground 100 mesh sieve, it is thus achieved that hydro-thermal Herba Typhae biology powdered carbon End；
(5) the described a certain amount of hydro-thermal Herba Typhae charcoal powder of step (4), FeCl are weighed3、ZnCl2And deionized water is with 4:2: 1:20 mixes, it is thus achieved that biased sample.Wherein hydro-thermal Herba Typhae charcoal powder, FeCl3、ZnCl2Mass unit be gram, deionization The unit of water volume is milliliter；
(6) by step (5) described biased sample, put in gas bath constant temperature oscillator with 150 r min-1Constant temperature oscillation 24 h, At a temperature of 80 DEG C, hydro-thermal Herba Typhae charcoal powder, FeCl it is dried to obtain after taking-up3And ZnCl2Be sufficiently mixed thing.
(7) step (6) described hydro-thermal Herba Typhae charcoal powder, FeCl are weighed3And ZnCl2The thing that is sufficiently mixed be placed in case In formula atmosphere furnace, being passed through 400 mL/min flow velocity nitrogen in stove, programmed rate controls 4 DEG C/min, and target temperature is 500 DEG C, at 500 DEG C, final temperature pyrolysis continues 90 min.After pyrolytic process terminates, take after Herba Typhae charcoal naturally cools to room temperature Go out, be cleaned multiple times to neutrality with deionized water；In 80 DEG C of drying, i.e. prepare Magnetic Activated hydro-thermal Herba Typhae charcoal.
Embodiment A3
(1) by hay grass natural air drying so that it is inner aqueous rate is less than 10%, then pulverizes 100 mesh sieve, it is thus achieved that water plant Powder；
(2) weigh step (1) described hay grass meal end, put in reactor and add a certain amount of deionized water.Hay grass meal end with The mass volume ratio of deionized water is 1:50；Wherein the mass unit at hay grass meal end be gram that the unit of deionized water volume is in the least Rise；
(3) baking oven put into by step (2) described reactor, temperature programming to 200 DEG C, keeps final temperature to be pyrolyzed 6 h；Pyrolytic process terminates After, take out product and clean with ethanol and deionized water successively, dry at 80 DEG C and both prepared hydro-thermal hay grass charcoal；
(4) weigh step (3) described hydro-thermal hay grass charcoal, ground 100 mesh sieve, it is thus achieved that hydro-thermal hay grass biology powdered carbon End；
(5) the described a certain amount of hydro-thermal hay grass charcoal powder of step (4), FeCl are weighed3、ZnCl2And deionized water is with 4:2: 1:20 mixes, it is thus achieved that biased sample.Wherein hydro-thermal hay grass charcoal powder, FeCl3、ZnCl2Mass unit be gram, deionization The unit of water volume is milliliter；
(6) by step (5) described biased sample, put in gas bath constant temperature oscillator with 150 r min-1Constant temperature oscillation 24 h, At a temperature of 80 DEG C, hydro-thermal hay grass charcoal powder, FeCl it is dried to obtain after taking-up3And ZnCl2Be sufficiently mixed thing.
(7) step (6) described hydro-thermal hay grass charcoal powder, FeCl are weighed3And ZnCl2The thing that is sufficiently mixed be placed in case In formula atmosphere furnace, being passed through 400 mL/min flow velocity nitrogen in stove, programmed rate controls 4 DEG C/min, and target temperature is 500 DEG C, at 500 DEG C, final temperature pyrolysis continues 90 min.After pyrolytic process terminates, take after hay grass charcoal naturally cools to room temperature Go out, be cleaned multiple times to neutrality with deionized water；In 80 DEG C of drying, i.e. prepare Magnetic Activated hydro-thermal hay grass charcoal.
See Fig. 1 scanning electron microscope result it can be seen that by the hydro-thermal charcoal smooth surface of activation, there is many holes Cave, and form micropore, cause charcoal specific surface area to expand, be so more beneficial for providing more adsorption potential into modification biological charcoal Point.
See Fig. 2 and understand the hydro-thermal charcoal prepared by synchronous magnetizing activation method, possess good magnetic, can be by magnetic Ferrum reclaims.
Magnetic Activated hydro-thermal charcoal is to the adsorption effect of lead and copper substantially (see Fig. 3,4).By Magnetic Activated for 10 g It is 100 mg L that hydro-thermal phragmites communis charcoal is added to concentration-11 L height lead water body in, at initial 20 min to the absorption of lead Through tending to stable, lead content reduces rapidly in 20 min, and the clearance at the 20th min lead has reached 78.78%, the 320 min, lead clearance reaches the highest, is 85.22%.10 g Magnetic Activated hydro-thermal phragmites communis charcoal is added to concentration is 100 mg·L-11 L high-copper water body in, at initial 40 min, it is stable that the absorption of lead tended to, lead content is fast in 40 min Prompt drop is low, and the clearance at the 40th min lead has reached 82.52%, and at the 320th min, lead clearance reaches the highest, for 87.31%.The higher rate of adsorption has great significance for reality application, and the rate of adsorption comparatively fast may insure that higher going Except efficiency.
Through the adsorption of Magnetic Activated hydro-thermal charcoal, absorption quickly reaches balance, lead and copper by quick adsorption Removing, the Magnetic Activated hydro-thermal charcoal after absorption can be reclaimed by Magnet, then by recycling after acid solution eluting.
The foregoing is only the preferred embodiments of the present invention, be not limited to the present invention, for the skill of this area For art personnel, the present invention can have various modifications and variations.All within the spirit and principles in the present invention, that is made any repaiies Change, equivalent, improvement etc., should be included within the scope of the present invention.

Claims (8)

1. the preparation method of a Magnetic Activated hydro-thermal charcoal, it is characterised in that comprise the steps:
Step (1), by water plant natural air drying so that it is inner aqueous rate be less than 10%, then pulverized 100 mesh sieve, it is thus achieved that Water plant powder；
Step (2), weigh step (1) described water plant powder, put in reactor and add deionized water；
Baking oven put into by step (3), step (2) described reactor, temperature programming to target temperature, when keeping final temperature to be pyrolyzed one section Between；After pyrolytic process terminates, take out product and clean with ethanol and deionized water successively, dry at 80 DEG C and both prepared water Hot charcoal；
Step (4), weigh step (3) described hydro-thermal charcoal, grind 100 mesh sieve, it is thus achieved that hydro-thermal charcoal powder；
Step (5), weigh step (4) described hydro-thermal charcoal powder, with FeCl3And ZnCl2Mixing, joins deionized water In, it is thus achieved that biased sample；
Step (6), by step (5) described biased sample, put in gas bath constant temperature oscillator certain with certain rotating speed constant temperature oscillation Time, at a temperature of 80 DEG C, after taking-up, it is dried to obtain hydro-thermal charcoal powder, FeCl3And ZnCl2Be sufficiently mixed thing；
Step (7), weigh step (6) described hydro-thermal charcoal powder, FeCl3And ZnCl2The thing that is sufficiently mixed be placed in box gas In atmosphere stove, in stove, it is passed through certain flow rate nitrogen；Temperature programming, to target temperature, keeps the pyrolysis of certain time final temperature；It was pyrolyzed After journey terminates, take out after charcoal naturally cools to room temperature, be cleaned multiple times to neutrality with deionized water；In 80 DEG C of drying, i.e. Prepare Magnetic Activated hydro-thermal charcoal.
The preparation method of a kind of Magnetic Activated hydro-thermal charcoal the most according to claim 1, it is characterised in that: described step (1) one during water plant is phragmites communis, Herba Typhae or hay grass in.
The preparation method of a kind of Magnetic Activated hydro-thermal charcoal the most according to claim 1, it is characterised in that: described step (2), in, water plant powder is 1:50 with the mass volume ratio of deionized water；Wherein the mass unit of water plant powder is Gram, the unit of deionized water volume is milliliter.
The preparation method of a kind of Magnetic Activated hydro-thermal charcoal the most according to claim 1, it is characterised in that: described step (3) in, baking oven target temperature is 200 DEG C；At 200 DEG C, final temperature pyrolysis continues 6 h.
The preparation method of a kind of Magnetic Activated hydro-thermal charcoal the most according to claim 1, it is characterised in that: described step (5) hydro-thermal charcoal powder, FeCl in3、ZnCl2With the mass volume ratio of deionized water than for 4:2:1:20, wherein water plant Powder, FeCl3、ZnCl2Mass unit be gram that the unit of deionized water volume is milliliter.
The preparation method of a kind of Magnetic Activated hydro-thermal charcoal the most according to claim 1, it is characterised in that: described step (6) biased sample 150 r min in gas bath constant temperature oscillator-1Constant temperature oscillation, the concussion time is 24 h.
The preparation method of a kind of Magnetic Activated hydro-thermal charcoal the most according to claim 1, it is characterised in that: described step (7) in, in box atmosphere furnace, nitrogen flow rate is 400 mL/min；Programmed rate controls 4 DEG C/min；Target temperature is 500 ℃；At 500 DEG C, final temperature pyrolysis continues 90 min.
The preparation method of a kind of Magnetic Activated hydro-thermal charcoal the most according to claim 1, it is characterised in that prepare magnetic Activate hydro-thermal charcoal heavy metal lead in Adsorption water body or soil and the application of copper.
CN201610606211.9A 2016-07-29 2016-07-29 The preparation method of a kind of Magnetic Activated hydro-thermal charcoal and application Pending CN106179216A (en)

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CN112023878A (en) * 2020-08-04 2020-12-04 安徽农业大学 Preparation method of magnetic porous tea residue biochar for removing tetracycline in water body
CN112169755A (en) * 2020-09-24 2021-01-05 武汉理工大学 Preparation method of hydrothermally synthesized zinc chloride activated magnetic sludge biochar applied to tetracycline removal in water
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CN116969601A (en) * 2023-08-01 2023-10-31 上海师范大学 Method and device for fixing carbon in farmland tail water circulation

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CN109225129A (en) * 2017-07-11 2019-01-18 内蒙古大学 A kind of production method of the preceding modified microballoon functionality straw charcoal of hydro-thermal preparation
CN107876008A (en) * 2017-10-20 2018-04-06 福建省农业科学院农业生态研究所 A kind of fen adsorbent, preparation method and applications
CN107876008B (en) * 2017-10-20 2021-01-26 福建省农业科学院农业生态研究所 Adsorbent for methane tank, preparation method and application thereof
CN108117073A (en) * 2017-12-29 2018-06-05 中南民族大学 A kind of method and application that porous carbon materials are prepared using water hyacinth
CN108816189A (en) * 2018-06-19 2018-11-16 北京师范大学 A kind of preparation of biomass carbon and its absorption to brufen
CN110965075A (en) * 2018-09-29 2020-04-07 中国科学院大连化学物理研究所 Preparation and application of carbon dioxide electrochemical reduction electrode
CN109759011A (en) * 2019-01-23 2019-05-17 南阳师范学院 The preparation method of straw base magnetic bio charcoal
CN110065942A (en) * 2019-04-12 2019-07-30 华南理工大学 A kind of rice base graininess micropore/ultramicropore carbon material and preparation method thereof
CN110065942B (en) * 2019-04-12 2022-08-12 华南理工大学 Rice-based granular microporous/ultramicroporous carbon material and preparation method thereof
CN110075795A (en) * 2019-04-26 2019-08-02 福建工程学院 A kind of preparation method having magnetic tubulose active carbon
CN111298766A (en) * 2019-10-30 2020-06-19 中国科学院广州地球化学研究所 Activated and oxidized biochar and preparation method and application thereof
CN111054308A (en) * 2019-12-11 2020-04-24 佛山科学技术学院 Magnetic biochar and preparation method thereof
CN112023878A (en) * 2020-08-04 2020-12-04 安徽农业大学 Preparation method of magnetic porous tea residue biochar for removing tetracycline in water body
CN112169755A (en) * 2020-09-24 2021-01-05 武汉理工大学 Preparation method of hydrothermally synthesized zinc chloride activated magnetic sludge biochar applied to tetracycline removal in water
CN112387249A (en) * 2020-11-11 2021-02-23 内蒙古科技大学 Porous biochar/zinc ferrite composite material and preparation method and application thereof
CN112844311A (en) * 2020-12-28 2021-05-28 中国环境科学研究院 Iris pseudacorus attapulgite composite powder modified heavy metal adsorbent
CN116969601A (en) * 2023-08-01 2023-10-31 上海师范大学 Method and device for fixing carbon in farmland tail water circulation
CN116969601B (en) * 2023-08-01 2024-03-19 上海师范大学 Method and device for fixing carbon in farmland tail water circulation

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Application publication date: 20161207