CN115337907B - Composite magnetic charcoal adsorbent and preparation method and application thereof - Google Patents

Composite magnetic charcoal adsorbent and preparation method and application thereof Download PDF

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CN115337907B
CN115337907B CN202211270447.1A CN202211270447A CN115337907B CN 115337907 B CN115337907 B CN 115337907B CN 202211270447 A CN202211270447 A CN 202211270447A CN 115337907 B CN115337907 B CN 115337907B
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furnace dust
drying
sieving
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CN115337907A (en
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王一同
王福平
李俊国
曾亚南
康乐乐
姬睿
王晓嫚
李涛
王亚军
张喜
刘宝
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North China University of Science and Technology
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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
    • B01J20/28002—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
    • 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
    • B01J2220/4825—Polysaccharides or cellulose materials, e.g. starch, chitin, sawdust, wood, straw, cotton
    • 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
    • B01J2220/4875—Sorbents characterised by the starting material used for their preparation the starting material being a waste, residue or of undefined composition
    • B01J2220/4887—Residues, wastes, e.g. garbage, municipal or industrial sludges, compost, animal manure; fly-ashes
    • 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
    • C02F2101/22—Chromium or chromium compounds, e.g. chromates
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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    • C02F2209/06—Controlling or monitoring parameters in water treatment pH

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Abstract

The invention discloses a composite magnetic charcoal adsorbent and a preparation method and application thereof, wherein the preparation method comprises the following steps: grinding and sieving electric furnace dust, and drying at 75-105 ℃ to obtain pretreated electric furnace dust; washing, drying, crushing and screening rice hulls to obtain pretreated rice hulls; (1) adding acid and deionized water into pretreated electric furnace dust, magnetically stirring in an oil bath kettle at 65-95 deg.C for 30-60 min, filtering, and collecting filtrate; (2) adding alkali and pretreated rice hull into the obtained filtrate, stirring, filtering to obtain filter residue, and drying the filter residue in an oven at 85-105 deg.C to constant weight; (3) and (3) sieving the filter residue obtained in the step (2), calcining under inert gas, cooling, washing to be neutral, drying to constant weight, and sieving to obtain the product, wherein the yield is more than 80%, and the removal rate of hexavalent chromium ions can reach more than 75%.

Description

Composite magnetic charcoal adsorbent and preparation method and application thereof
Technical Field
The invention relates to a preparation method of a sewage adsorbent, belongs to the field of solid adsorbents, and particularly relates to a composite magnetic charcoal adsorbent and a preparation method and application thereof.
Background
Water is an important resource required for human and other organisms to live and proliferate. The rapid development of industry, the rapid increase of population, the change of agricultural activities and the like lead to the sharp reduction of available water resources, and seriously threaten the survival and development of human beings. The harm brought by the waste water generated by the industries such as metallurgy, electroplating, printing, battery manufacturing and the like is a huge problem to be faced worldwide, and is paid attention by a plurality of international researchers. Unlike organic pollutants, heavy metals in wastewater cannot be degraded by microorganisms and can therefore accumulate at toxic levels in the soil, water and food chain. The heavy metals mainly comprise gold (Au), silver (Ag), copper (Cu), iron (Fe), mercury (Hg), lead (Pb), cadmium (Cd), chromium (Cr) and the like, and once the heavy metals are accumulated in a human body to a certain degree, the heavy metals can directly influence physiological and biochemical functions of the human body. For example, hg and Pb can affect development of the nervous system and can cause skin damage. Hexavalent chromium ions are classified as one of carcinogenic heavy metals and have the characteristics of high toxicity and difficulty in removal, and the highest acceptable level of the hexavalent chromium ions specified by the World Health Organization (WHO), european Union, united states and China drinking water standards is 50 mug/L, 100 mug/L and 50 mug/L respectively. Therefore, the exploration of a method for effectively and efficiently removing the heavy metals in the sewage is very important.
Chemical precipitation, reverse osmosis, ion exchange and photocatalytic processes are conventional methods for treating heavy metal contaminated water bodies, but all have some drawbacks. If the chemical precipitation method can produce polluted heavy metal toxic sludge and can produce secondary harm to the environment, the reverse osmosis method belongs to one of membrane filtration technologies and has better removal efficiency, but the water treatment amount is smaller and the cost is more expensive. Ion exchange is costly and not conducive to large-scale applications, and the photocatalytic process requires a complex and costly photocatalyst preparation process, limiting its development. The adsorption method is a method for removing heavy metals in aquatic environment, which has low cost, easy application and environmental protection, and has the characteristics of high adsorption performance, mild reaction condition, renewability and the like, so that the method has application potential. Commonly used adsorbents include nanomaterials, activated carbon, graphene adsorbents, and some composites. In recent years, biochar has been favored by researchers in the field of adsorbent preparation, in addition to having characteristics of large specific surface area, abundant pore structures and functional groups, good chemical stability, low preparation cost, and the like. However, the adsorption and carrying of heavy metal ions by the original biochar has some disadvantages, such as low removal efficiency, poor adsorption selectivity, difficulty in secondary recovery and the like, and the adsorption characteristics of the biochar can be improved by a proper modification means.
Disclosure of Invention
In order to solve the problems, the invention uses the biochar and the electric furnace dust as raw materials, and realizes the efficient removal of heavy metals in sewage by preparing the adsorbent with high adsorption property and easy recovery.
All percentages used herein are by weight unless otherwise indicated.
One of the purposes of the invention is to provide a preparation method of a composite magnetic biochar adsorbent, which comprises the following steps:
step I, electric furnace dust pretreatment:
grinding the electric furnace dust by using a ball mill, sieving, and drying at 75-105 ℃ to obtain pretreated electric furnace dust;
step II, rice hull pretreatment:
washing and drying the collected rice hulls, crushing the rice hulls by a crusher, and sieving the crushed rice hulls to obtain pretreated rice hulls;
step III, preparation of the composite magnetic charcoal adsorbent:
(1) adding acid and deionized water into pretreated electric furnace dust, and placing in oil bath pan 65-95% o Magnetically stirring for 30-60 min under C, filtering, and collecting filtrate;
(2) adding alkali and pretreated rice hull into the obtained filtrate, mechanically stirring at room temperature at rotation speed of 800-1000 r/min for more than 8 hr, filtering to obtain filter residue, and placing the filter residue at 85-105 o C, drying in an oven to constant weight;
(3) and (3) sieving the filter residue obtained in the step (2), calcining under inert gas, cooling, washing to be neutral, drying to constant weight, and sieving to obtain the composite magnetic charcoal adsorbent.
Further, the sieving in the step I is specifically to sieve through a 150-200 mesh sieve; and the sieving in the step II and the step III is to pass through a 10-20-mesh sieve.
Further, in the step III, the mass volume ratio of the pretreated electric furnace dust to the deionized water is 1.
Further, in the step III, the mass ratio of the pretreated electric furnace dust to the pretreated rice hulls is 1.
Further, in the step III, the acid includes at least one of hydrochloric acid, sulfuric acid, and nitric acid, and the acid concentration is analytically pure.
Further, in the step III, the volume ratio of the acid to the deionized water is 3.
Further, in the step III, the alkali comprises at least one of KOH, naOH and ammonia water, and the volume ratio of the addition amount of the alkali to the acid is 1-1.5mol/L and is 6.
Further, the inert gas includes nitrogen, argon or helium.
Further, in the step III, the specific parameters of the calcination are as follows: calcining temperature is 500-900 deg.C o C, the heating rate is 5-7 ℃/min, and the calcination time is more than 2 h.
The invention also aims to provide a composite magnetic charcoal adsorbent, which is prepared by the method.
The invention also aims to provide an application of the composite magnetic charcoal adsorbent in treatment of wastewater containing hexavalent chromium ions.
The invention also aims to provide a method for treating the wastewater containing the hexavalent chromium ions, which comprises the following steps:
step i, adjusting the pH value of the hexavalent chromium ion-containing wastewater to 1;
and ii, adding 3.5-4g/L of the composite magnetic charcoal adsorbent into the wastewater, placing the wastewater in an oscillation box, setting the ambient temperature to be room temperature, and setting the adsorption time to be more than 22 h.
Further, the adsorption time is 22-28h.
Further, the initial concentration of the hexavalent chromium ions in the hexavalent chromium ion-containing wastewater is 400-500 mg/L.
Compared with the prior art, the invention has the following advantages:
1. the invention takes electric furnace dust and biochar as raw materials, and the composite magnetic biochar adsorbent is obtained by coprecipitation and high-temperature calcination under the condition of inert gas, and has the magnetic size of 11.35 Am 2 The composite magnetic biochar adsorbent synthesized by the invention can be separated from hexavalent chromium ion solution under the action of an external magnetic field after reaction, and the yield of the adsorbent is over 80 percent.
2. The composite magnetic charcoal adsorbent synthesized by the invention has high adsorption activity, and the removal rate can reach more than 75% when hexavalent chromium ion-containing wastewater is treated through determination.
3. The composite magnetic biochar adsorbent synthesized by the invention has larger specific surface area and abundant pore structures (including micropores and mesopores) so as to provide sufficient adsorption sites for supporting Fe on the surface of the biochar 3 O 4 And Fe not only provides magnetism, but also plays an important role in the process of adsorbing hexavalent chromium ions.
4. The invention realizes the recycling of resources and effectively reduces the environmental pollution by recycling the electric furnace dust and the rice hull solid waste.
Detailed Description
The present invention will be described in further detail with reference to examples.
Examples 1 to 3
A preparation method of a composite magnetic charcoal adsorbent comprises the following steps:
the method comprises the following steps:
step I, electric furnace dust pretreatment:
grinding the electric furnace dust by using a ball mill, sieving the ground electric furnace dust by using a 150-mesh sieve, and drying the electric furnace dust at the temperature of 105 ℃ to obtain pretreated electric furnace dust;
step II, rice hull pretreatment:
washing and drying the collected rice hulls, crushing the rice hulls by a crusher, and sieving the crushed rice hulls by a 20-mesh sieve to obtain pretreated rice hulls;
step III, preparation of the composite magnetic charcoal adsorbent:
(1) 4g of pretreated electric furnace dust is taken, added with analytically pure hydrochloric acid and 40mL of deionized water and put in an oil bath pot for 75 percent o Magnetically stirring for 40 min under C, filtering, and collecting filtrate;
(2) adding 300mL of KOH of 1mol/L and 40g of pretreated rice hulls into the obtained filtrate, mechanically stirring for 8 hours at room temperature under the condition that the rotating speed is 800 r/min, filtering, and placing filter residues obtained by filtering in 105 o C, drying in an oven to constant weight;
(3) filtering the filter residue obtained in the step (2) by a 20-mesh screen, and heating to 600 ℃ at the speed of 5 ℃/min under inert gas o And C, calcining for 2h, cooling, washing to be neutral, drying to constant weight, and sieving with a 200-mesh sieve to obtain the composite magnetic charcoal adsorbent.
The pH of the initial solution containing hexavalent chromium ions is =1, the initial concentration of hexavalent chromium ions is 500 mg/L, the addition amount of the adsorbent is 4g/L, the adsorption time is 1680 min, and the temperature is 25% o And C, performing the test under the condition of C, and simultaneously performing recovery on the adsorbent through an external magnetic field to determine the recovery rate of the adsorbent through 3 times of parallel recovery experiments. The adsorption effect and recovery rate under different conditions of the addition amount of analytically pure hydrochloric acid are shown in table 1.
TABLE 1 parameters and Effect of examples 1-3
Figure 405998DEST_PATH_IMAGE001
Example 4-6 a method of preparing a composite magnetic biochar adsorbent:
the method comprises the following steps:
step I, electric furnace dust pretreatment:
grinding the electric furnace dust by using a ball mill, sieving the ground electric furnace dust by using a 150-mesh sieve, and drying the electric furnace dust at the temperature of 105 ℃ to obtain pretreated electric furnace dust;
step II, rice hull pretreatment:
washing and drying the collected rice hulls, crushing the rice hulls by a crusher, and sieving the crushed rice hulls by a 20-mesh sieve to obtain pretreated rice hulls;
step III, preparation of the composite magnetic charcoal adsorbent:
(1) 4g of the pretreated electric furnace dust is taken, added with 30mL of analytically pure hydrochloric acid and 40mL of deionized water and put in an oil bath pan for 75 g o Magnetically stirring for 40 min under C, filtering, and collecting filtrate;
(2) adding 1mol/L KOH and 40g pretreated rice hull into the obtained filtrate, mechanically stirring for 8h at room temperature under the condition of the rotating speed of 800 r/min, filtering, and placing filter residue obtained by filtering in 105 o C, drying in an oven to constant weight;
(3) filtering the filter residue obtained in the step (2) by a 20-mesh screen, and then filtering the filter residue by 5 times under inert gas o The temperature rises to 600 ℃ at a rate of C/min o And C, calcining for 2h, cooling, washing to neutrality, drying to constant weight, and sieving with a 200-mesh sieve to obtain the composite magnetic charcoal adsorbent.
The pH of the initial solution containing hexavalent chromium ions is =1, the initial concentration of hexavalent chromium ions is 500 mg/L, the addition amount of the adsorbent is 4g/L, the adsorption time is 1680 min, and the temperature is 25% o And C, performing the test under the condition of C, and simultaneously performing recovery on the adsorbent through an external magnetic field to determine the recovery rate of the adsorbent through 3 times of parallel recovery experiments. The adsorption effect and recovery rate at different KOH addition levels are shown in table 2.
TABLE 2 parameters and Effect of examples 4-6
Figure 900564DEST_PATH_IMAGE002
Examples 7 to 10
A preparation method of a composite magnetic charcoal adsorbent comprises the following steps:
the method comprises the following steps:
step I, electric furnace dust pretreatment:
grinding the electric furnace dust by using a ball mill, sieving the ground electric furnace dust by using a 150-mesh sieve, and drying the electric furnace dust at the temperature of 105 ℃ to obtain pretreated electric furnace dust;
step II, rice hull pretreatment:
washing and drying the collected rice hulls, crushing the rice hulls by a crusher, and sieving the crushed rice hulls by a 20-mesh sieve to obtain pretreated rice hulls;
step III, preparation of the composite magnetic charcoal adsorbent:
(1) 4g of the pretreated electric furnace dust is taken, added with 30mL of analytically pure hydrochloric acid and 40mL of deionized water and put in an oil bath pan for 75 g o Magnetically stirring for 40 min under C, filtering, and collecting filtrate;
(2) adding 300mL of KOH of 1mol/L and 40g of pretreated rice hulls into the obtained filtrate, mechanically stirring for 8 hours at room temperature under the condition of the rotating speed of 800 r/min, filtering, and placing filter residues obtained by filtering in 105 o C, drying in an oven to constant weight;
(3) filtering the filter residue obtained in the step (2) by a 20-mesh screen, and then filtering the filter residue by 5 times under inert gas o And (3) heating at the speed of C/min, calcining for 2h, cooling, washing to be neutral, drying to constant weight, and sieving with a 200-mesh sieve to obtain the composite magnetic charcoal adsorbent.
The pH of the initial solution containing hexavalent chromium ions is =1, the initial concentration of hexavalent chromium ions is 500 mg/L, the addition amount of the adsorbent is 4g/L, the adsorption time is 1680 min, and the temperature is 25% o And C, testing under the condition of C, and simultaneously, recovering the adsorbent through an external magnetic field to determine the recovery rate of the adsorbent through 3 times of parallel recovery experiments. The adsorption effect and recovery rate under different calcination temperature conditions are shown in table 3.
TABLE 3 parameters and Effect of examples 7-10
Figure 826319DEST_PATH_IMAGE003
Examples 11 to 15
A preparation method of a composite magnetic charcoal adsorbent comprises the following steps:
the method comprises the following steps:
step I, electric furnace dust pretreatment:
grinding the electric furnace dust by using a ball mill, sieving the ground electric furnace dust by using a 150-mesh sieve, and drying the electric furnace dust at the temperature of 105 ℃ to obtain pretreated electric furnace dust;
step II, rice hull pretreatment:
washing and drying the collected rice hulls, crushing the rice hulls by a crusher, and sieving the crushed rice hulls by a 20-mesh sieve to obtain pretreated rice hulls;
step III, preparation of the composite magnetic charcoal adsorbent:
(1) 4g of the pretreated electric furnace dust is taken, added with 30mL of analytically pure hydrochloric acid and 40mL of deionized water and put in an oil bath pan for 75 g o Magnetically stirring for 40 min under C, filtering, and collecting filtrate;
(2) adding 300mL of KOH of 1mol/L and 40g of pretreated rice hulls into the obtained filtrate, mechanically stirring for 8 hours at room temperature under the condition that the rotating speed is 800 r/min, filtering, and placing filter residues obtained by filtering in 105 o C, drying in an oven to constant weight;
(3) filtering the filter residue obtained in the step (2) by a 20-mesh screen, and then filtering the filter residue by 5 times under inert gas o The temperature rises to 800 ℃ at a rate of C/min o And C, calcining for 2h, cooling, washing to be neutral, drying to constant weight, and sieving with a 200-mesh sieve to obtain the composite magnetic charcoal adsorbent.
A treatment method of hexavalent chromium ion-containing wastewater comprises the following steps:
step i, adjusting the pH value of the hexavalent chromium ion-containing wastewater to 1 by using HCl;
step ii, adding the composite magnetic charcoal adsorbent into 200mL of wastewater, placing the wastewater in an oscillating box, and setting the temperature to be 25 DEG o C. The effects under the conditions of different amounts of the composite magnetic charcoal adsorbent, adsorption time, and initial concentration of hexavalent chromium ions are shown in table 4.
TABLE 4 parameters and effects of examples 11-15
Figure 821957DEST_PATH_IMAGE004
Comparative example 1 a method for preparing a composite magnetic biochar adsorbent:
the method comprises the following steps:
step I, electric furnace dust pretreatment:
grinding the electric furnace dust by using a ball mill, sieving the ground electric furnace dust by using a 150-mesh sieve, and drying the electric furnace dust at the temperature of 105 ℃ to obtain pretreated electric furnace dust;
step II, rice hull pretreatment:
washing and drying the collected rice hulls, crushing the rice hulls by a crusher, and sieving the crushed rice hulls by a 20-mesh sieve to obtain pretreated rice hulls;
step III, preparation of the composite magnetic charcoal adsorbent:
(1) 4g of the pretreated electric furnace dust is taken, added with 20 mL of analytically pure hydrochloric acid and 40mL of deionized water and put in an oil bath pan for 75 g o Magnetically stirring for 40 min under C, filtering, and collecting filtrate;
(2) adding 300mL of KOH of 1mol/L and 40g of pretreated rice hulls into the obtained filtrate, mechanically stirring for 8 hours at room temperature under the condition that the rotating speed is 800 r/min, filtering, and placing filter residues obtained by filtering in 105 o C, drying in an oven to constant weight;
(3) filtering the filter residue obtained in the step (2) by a 20-mesh screen, and heating to 500 ℃ at the speed of 5 ℃/min under inert gas o And C, calcining for 2h, cooling, washing to be neutral, drying to constant weight, and sieving with a 200-mesh sieve to obtain the composite magnetic charcoal adsorbent.
The pH of the initial solution containing hexavalent chromium ions is =1, the initial concentration of hexavalent chromium ions is 500 mg/L, the addition amount of the adsorbent is 4g/L, the adsorption time is 1680 min, and the temperature is 25% o The removal rate of hexavalent chromium ions is 59.19% by testing under the condition C, and meanwhile, the recovery rate of the adsorbent is 51.78% by testing the recovery of the adsorbent through an external magnetic field through 3 parallel recovery experiments.
Comparative example 2
A preparation method of a composite magnetic biochar adsorbent comprises the following steps:
the method comprises the following steps:
step I, electric furnace dust pretreatment:
grinding the electric furnace dust by using a ball mill, sieving the ground electric furnace dust by using a 150-mesh sieve, and drying the electric furnace dust at the temperature of 105 ℃ to obtain pretreated electric furnace dust;
step II, rice hull pretreatment:
washing and drying the collected rice hulls, crushing the rice hulls by a crusher, and sieving the crushed rice hulls by a 20-mesh sieve to obtain pretreated rice hulls;
step III, preparation of the composite magnetic charcoal adsorbent:
(1) 4g of the pretreated electric furnace dust is taken, added with 20 mL of analytically pure hydrochloric acid and 40mL of deionized water and put in an oil bath pan for 75 g o Magnetically stirring for 40 min under C, filtering, and collecting filtrate;
(2) adding 300mL of KOH of 1mol/L and 40g of pretreated rice hulls into the obtained filtrate, mechanically stirring for 8 hours at room temperature under the condition of the rotating speed of 800 r/min, filtering, and placing filter residues obtained by filtering in 105 o C, drying in an oven to constant weight;
(3) filtering the filter residue obtained in the step (2) by a 20-mesh screen, and heating to 600 ℃ at the speed of 5 ℃/min under inert gas o And C, calcining for 2h, cooling, washing to be neutral, drying to constant weight, and sieving with a 200-mesh sieve to obtain the composite magnetic charcoal adsorbent.
The pH of the initial solution containing hexavalent chromium ions is =1, the initial concentration of hexavalent chromium ions is 500 mg/L, the addition amount of the adsorbent is 4g/L, the adsorption time is 1680 min, and the temperature is 25% o The removal rate of hexavalent chromium ions is 69.19% by testing under the condition C, and meanwhile, the recovery rate of the adsorbent is 65.13% by testing through 3 parallel recovery experiments.
Comparative example 3
A preparation method of a composite magnetic charcoal adsorbent comprises the following steps:
the method comprises the following steps:
step I, electric furnace dust pretreatment:
grinding the electric furnace dust by using a ball mill, sieving the ground electric furnace dust by using a 150-mesh sieve, and drying the electric furnace dust at the temperature of 105 ℃ to obtain pretreated electric furnace dust;
step II, rice hull pretreatment:
washing and drying the collected rice hulls, crushing the rice hulls by a crusher, and sieving the crushed rice hulls by a 20-mesh sieve to obtain pretreated rice hulls;
step III, preparation of the composite magnetic charcoal adsorbent:
(1) 4g of the pretreated electric furnace dust is taken, added with 30mL of analytically pure hydrochloric acid and 40mL of deionized water and put in an oil bath pan for 75 g o Magnetically stirring for 40 min under C, filtering, and collecting filtrate;
(2) adding 140mL of KOH of 1mol/L and 40g of pretreated rice hulls into the obtained filtrate, mechanically stirring for 8 hours at room temperature under the condition of the rotating speed of 800 r/min, filtering, and placing filter residues obtained by filtering in 105 o C, drying in an oven to constant weight;
(3) filtering the filter residue obtained in the step (2) by a 20-mesh screen, and then filtering the filter residue by 5 times under inert gas o Heating to 500 deg.C/min o And C, calcining for 2h, cooling, washing to be neutral, drying to constant weight, and sieving with a 200-mesh sieve to obtain the composite magnetic charcoal adsorbent.
The pH of the initial solution containing hexavalent chromium ions is =1, the initial concentration of hexavalent chromium ions is 500 mg/L, the addition amount of the adsorbent is 4g/L, the adsorption time is 1680 min, and the temperature is 25% o The removal rate of hexavalent chromium ions is 49.19% by testing under the condition C, and meanwhile, the recovery rate of the adsorbent is 32.78% by testing the recovery of the adsorbent through an external magnetic field through 3 parallel recovery experiments.
Comparative example 4
A preparation method of a composite magnetic charcoal adsorbent comprises the following steps:
the method comprises the following steps:
step I, electric furnace dust pretreatment:
grinding the electric furnace dust by using a ball mill, sieving the ground electric furnace dust by using a 150-mesh sieve, and drying the electric furnace dust at the temperature of 105 ℃ to obtain pretreated electric furnace dust;
step II, rice hull pretreatment:
washing and drying the collected rice hulls, crushing the rice hulls by a crusher, and sieving the crushed rice hulls by a 20-mesh sieve to obtain pretreated rice hulls;
step III, preparation of the composite magnetic charcoal adsorbent:
(1) 4g of the pretreated electric furnace dust is taken, added with 30mL of analytically pure hydrochloric acid and 40mL of deionized water, and put in an oil bath pan for 75 g o Magnetically stirring for 40 min under C, filtering, and collecting filtrate;
(2) adding 140mL of KOH of 1mol/L and 40g of pretreated rice hulls into the obtained filtrate, mechanically stirring for 8 hours at room temperature under the condition that the rotating speed is 800 r/min, filtering, and placing filter residues obtained by filtering in 105 o C, drying in an oven to constant weight;
(3) filtering the filter residue obtained in the step (2) by a 20-mesh screen, and heating to 600 ℃ at the speed of 5 ℃/min under inert gas o And C, calcining for 2h, cooling, washing to be neutral, drying to constant weight, and sieving with a 200-mesh sieve to obtain the composite magnetic charcoal adsorbent.
The pH of the initial solution containing hexavalent chromium ions is =1, the initial concentration of hexavalent chromium ions is 500 mg/L, the addition amount of the adsorbent is 4g/L, the adsorption time is 1680 min, and the temperature is 25% o The removal rate of hexavalent chromium ions is 71.45% by testing under the condition C, and meanwhile, the recovery rate of the adsorbent is 65.23% by testing the recovery of the adsorbent through an external magnetic field through 3 parallel recovery experiments.
Comparative example 5
A preparation method of a composite magnetic charcoal adsorbent comprises the following steps:
the method comprises the following steps:
step I, electric furnace dust pretreatment:
grinding the electric furnace dust by using a ball mill, sieving the ground electric furnace dust by using a 150-mesh sieve, and drying the electric furnace dust at the temperature of 105 ℃ to obtain pretreated electric furnace dust;
step II, rice hull pretreatment:
washing and drying the collected rice hulls, crushing the rice hulls by a crusher, and sieving the crushed rice hulls by a 20-mesh sieve to obtain pretreated rice hulls;
step III, preparation of the composite magnetic charcoal adsorbent:
(1) taking 4g of pretreated electric furnace dust, adding 30mL of analytically pure hydrochloric acid and 40mL of deionized waterThen, in an oil bath pan 75 o Magnetically stirring for 40 min under C, filtering, and collecting filtrate;
(2) adding 330mL of KOH of 1mol/L and 40g of pretreated rice hulls into the obtained filtrate, mechanically stirring for 8 hours at room temperature under the condition of the rotating speed of 800 r/min, filtering, and placing filter residues obtained by filtering in 105 o C, drying in an oven to constant weight;
(3) filtering the filter residue obtained in the step (2) by a 20-mesh screen, and then heating to 400 ℃ at the speed of 5 ℃ per min under inert gas o And C, calcining for 2h, cooling, washing to be neutral, drying to constant weight, and sieving with a 200-mesh sieve to obtain the composite magnetic charcoal adsorbent.
The pH of the initial solution containing hexavalent chromium ions is =1, the initial concentration of hexavalent chromium ions is 500 mg/L, the addition amount of the adsorbent is 4g/L, the adsorption time is 1680 min, and the temperature is 25% o The removal rate of hexavalent chromium ions is 69.25% by testing under the condition C, and meanwhile, the recovery rate of the adsorbent is 69.12% by testing through 3 parallel recovery experiments.
Comparative example 6
A preparation method of a composite magnetic biochar adsorbent comprises the following steps:
the method comprises the following steps:
step I, electric furnace dust pretreatment:
grinding the electric furnace dust by using a ball mill, sieving the ground electric furnace dust by using a 150-mesh sieve, and drying the electric furnace dust at the temperature of 105 ℃ to obtain pretreated electric furnace dust;
step II, rice hull pretreatment:
washing and drying the collected rice hulls, crushing the rice hulls by a crusher, and sieving the crushed rice hulls by a 20-mesh sieve to obtain pretreated rice hulls;
step III, preparation of the composite magnetic charcoal adsorbent:
(1) 4g of the pretreated electric furnace dust is taken, added with 30mL of analytically pure hydrochloric acid and 40mL of deionized water and put in an oil bath pan for 75 g o Magnetically stirring for 40 min under C, filtering, and collecting filtrate;
(2) to the resulting filtrate was added 360 mL of 1mol/L KOH and 40g of pretreated rice hullsMechanically stirring at room temperature at 800 r/min for 8 hr, filtering, and placing the filter residue at 105 o C, drying in an oven to constant weight;
(3) filtering the filter residue obtained in the step (2) by a 20-mesh screen, and then filtering the filter residue by 5 times under inert gas o The temperature rises to 800 ℃ at a rate of C/min o And C, calcining for 2h, cooling, washing to be neutral, drying to constant weight, and sieving with a 200-mesh sieve to obtain the composite magnetic charcoal adsorbent.
A treatment method of hexavalent chromium ion-containing wastewater comprises the following steps:
step i, adjusting the pH value of the hexavalent chromium ion-containing wastewater to 2 by using HCl;
step ii, adding the composite magnetic charcoal adsorbent into 200mL of wastewater, placing the wastewater in an oscillating box, and setting the temperature to be 25 DEG o And C, the initial concentration of hexavalent chromium ions is 500 mg/L, the addition amount of the adsorbent is 4g/L, the adsorption time is 1680 min, the removal rate of the hexavalent chromium ions is 56.25% through measurement, and meanwhile, the recovery rate of the adsorbent is 91.14% through the measurement of 3 parallel recovery experiments by using the adsorbent to recover through an external magnetic field.
While the preferred embodiments of the present application have been described, additional variations and modifications in those embodiments may occur to those skilled in the art once they learn of the basic inventive concepts. Therefore, it is intended that the appended claims be interpreted as including preferred embodiments and all alterations and modifications as fall within the scope of the application. It will be apparent to those skilled in the art that various changes and modifications may be made in the present application without departing from the spirit and scope of the application. Thus, if such modifications and variations of the present application fall within the scope of the claims of the present application and their equivalents, the present application is intended to include such modifications and variations as well.

Claims (1)

1. A treatment method of hexavalent chromium ion-containing wastewater is characterized by comprising the following steps:
i, adjusting the pH value of the hexavalent chromium ion wastewater to 1;
step ii, adding 4g/L of composite magnetic charcoal adsorbent into the wastewater with the initial concentration of hexavalent chromium ions of 400-500 mg/L, placing the wastewater in an oscillation box, setting the environment temperature to be room temperature and the adsorption time to be 28h,
the composite magnetic charcoal adsorbent is prepared by the following method:
step I, electric furnace dust pretreatment:
grinding the electric furnace dust by using a ball mill, sieving, and drying at 75-105 ℃ to obtain pretreated electric furnace dust;
step II, rice hull pretreatment:
washing and drying the collected rice hulls, crushing the rice hulls by a crusher, and sieving the crushed rice hulls to obtain pretreated rice hulls;
step III, preparation of the composite magnetic charcoal adsorbent:
(1) taking 4g of pretreated electric furnace dust, adding 30mL of analytically pure hydrochloric acid and 40mL of deionized water, magnetically stirring for 30-60 min at 65-95 ℃ in an oil bath kettle, and filtering to obtain filtrate for later use;
(2) adding 300mL of KOH of 1mol/L and 40g of pretreated rice hull into the obtained filtrate, stirring at room temperature, filtering to obtain filter residue, and placing the filter residue obtained by filtering in a range of 85-105 o C, drying in an oven to constant weight;
(3) sieving the filter residue obtained in the step (2), calcining under inert gas, cooling, washing to neutrality, drying to constant weight, and sieving to obtain the composite magnetic charcoal adsorbent;
in the step III, the specific parameters of the calcination are as follows: the calcining temperature is 800-900 ℃, the heating rate is 5 ℃/min, and the calcining time is more than 2 h.
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