CN115337907A - Composite magnetic charcoal adsorbent and preparation method and application thereof - Google Patents
Composite magnetic charcoal adsorbent and preparation method and application thereof Download PDFInfo
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- CN115337907A CN115337907A CN202211270447.1A CN202211270447A CN115337907A CN 115337907 A CN115337907 A CN 115337907A CN 202211270447 A CN202211270447 A CN 202211270447A CN 115337907 A CN115337907 A CN 115337907A
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- 239000003463 adsorbent Substances 0.000 title claims abstract description 90
- 239000002131 composite material Substances 0.000 title claims abstract description 59
- 239000003610 charcoal Substances 0.000 title claims abstract description 39
- 238000002360 preparation method Methods 0.000 title claims abstract description 33
- 239000000428 dust Substances 0.000 claims abstract description 78
- 241000209094 Oryza Species 0.000 claims abstract description 77
- 235000007164 Oryza sativa Nutrition 0.000 claims abstract description 77
- 235000009566 rice Nutrition 0.000 claims abstract description 77
- 238000001035 drying Methods 0.000 claims abstract description 52
- 238000001914 filtration Methods 0.000 claims abstract description 52
- JOPOVCBBYLSVDA-UHFFFAOYSA-N chromium(6+) Chemical compound [Cr+6] JOPOVCBBYLSVDA-UHFFFAOYSA-N 0.000 claims abstract description 45
- 229910001430 chromium ion Inorganic materials 0.000 claims abstract description 44
- 238000007873 sieving Methods 0.000 claims abstract description 44
- 239000000706 filtrate Substances 0.000 claims abstract description 26
- 238000003756 stirring Methods 0.000 claims abstract description 26
- 238000005406 washing Methods 0.000 claims abstract description 26
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 22
- 238000001354 calcination Methods 0.000 claims abstract description 20
- 239000008367 deionised water Substances 0.000 claims abstract description 17
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 17
- 239000011261 inert gas Substances 0.000 claims abstract description 14
- 238000001816 cooling Methods 0.000 claims abstract description 13
- 238000000227 grinding Methods 0.000 claims abstract description 13
- 239000002253 acid Substances 0.000 claims abstract description 9
- 230000007935 neutral effect Effects 0.000 claims abstract description 7
- 239000003513 alkali Substances 0.000 claims abstract description 5
- 238000000034 method Methods 0.000 claims description 30
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 28
- 238000001179 sorption measurement Methods 0.000 claims description 24
- 239000002351 wastewater Substances 0.000 claims description 24
- 238000010438 heat treatment Methods 0.000 claims description 7
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 4
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 2
- 229910017604 nitric acid Inorganic materials 0.000 claims description 2
- 239000000047 product Substances 0.000 abstract 1
- 238000011084 recovery Methods 0.000 description 27
- 229910052799 carbon Inorganic materials 0.000 description 12
- 238000012360 testing method Methods 0.000 description 12
- 229910001385 heavy metal Inorganic materials 0.000 description 11
- 230000000694 effects Effects 0.000 description 10
- 238000002474 experimental method Methods 0.000 description 9
- 230000000052 comparative effect Effects 0.000 description 6
- 230000004048 modification Effects 0.000 description 6
- 238000012986 modification Methods 0.000 description 6
- 238000011161 development Methods 0.000 description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 3
- 241000282414 Homo sapiens Species 0.000 description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 239000010865 sewage Substances 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 238000009388 chemical precipitation Methods 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 239000011651 chromium Substances 0.000 description 2
- 239000010949 copper Substances 0.000 description 2
- 230000006378 damage Effects 0.000 description 2
- 239000010931 gold Substances 0.000 description 2
- 238000005342 ion exchange Methods 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 230000005389 magnetism Effects 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 230000001699 photocatalysis Effects 0.000 description 2
- 239000011148 porous material Substances 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 238000004064 recycling Methods 0.000 description 2
- 238000001223 reverse osmosis Methods 0.000 description 2
- 230000004083 survival effect Effects 0.000 description 2
- 231100000331 toxic Toxicity 0.000 description 2
- 230000002588 toxic effect Effects 0.000 description 2
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 1
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 241000282412 Homo Species 0.000 description 1
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 1
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 1
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 235000011114 ammonium hydroxide Nutrition 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 239000012752 auxiliary agent Substances 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 229910052793 cadmium Inorganic materials 0.000 description 1
- BDOSMKKIYDKNTQ-UHFFFAOYSA-N cadmium atom Chemical compound [Cd] BDOSMKKIYDKNTQ-UHFFFAOYSA-N 0.000 description 1
- 230000000711 cancerogenic effect Effects 0.000 description 1
- 231100000315 carcinogenic Toxicity 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 229910052804 chromium Inorganic materials 0.000 description 1
- 238000000975 co-precipitation Methods 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000002384 drinking water standard Substances 0.000 description 1
- 238000009713 electroplating Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 230000006870 function Effects 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 229910021389 graphene Inorganic materials 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 239000001307 helium Substances 0.000 description 1
- 229910052734 helium Inorganic materials 0.000 description 1
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 1
- 238000003837 high-temperature calcination Methods 0.000 description 1
- 229910052745 lead Inorganic materials 0.000 description 1
- 239000000696 magnetic material Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000005374 membrane filtration Methods 0.000 description 1
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 description 1
- 229910052753 mercury Inorganic materials 0.000 description 1
- 238000005272 metallurgy Methods 0.000 description 1
- 244000005700 microbiome Species 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 210000000653 nervous system Anatomy 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 230000008520 organization Effects 0.000 description 1
- 230000010355 oscillation Effects 0.000 description 1
- 239000002957 persistent organic pollutant Substances 0.000 description 1
- 239000011941 photocatalyst Substances 0.000 description 1
- 238000007639 printing Methods 0.000 description 1
- 230000035755 proliferation Effects 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 230000037380 skin damage Effects 0.000 description 1
- 239000010802 sludge Substances 0.000 description 1
- 239000002689 soil Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000002910 solid waste Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
Classifications
-
- 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
- C02F2209/00—Controlling or monitoring parameters in water treatment
- C02F2209/06—Controlling or monitoring parameters in water treatment pH
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Analytical Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Inorganic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Engineering & Computer Science (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Processing Of Solid Wastes (AREA)
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 sieving the 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
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 the survival and proliferation of humans and other organisms. 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, have characteristics of large toxicity and difficulty in removal, and the maximum acceptable levels of hexavalent chromium ions specified by the World Health Organization (WHO), european Union, the United states and Chinese drinking water standards are 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 cause secondary harm to the environment, the reverse osmosis method belongs to one of membrane filtration technologies and has better removal efficiency, but the treatment water 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, etc., 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 an oil bath kettle for 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 includes 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 to 1.5 mol/L.
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 calcining 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.
Furthermore, 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 material synthesized by the inventionThe charcoal adsorbent has large specific surface area and rich pore structure (including micropores and mesopores) so as to provide sufficient adsorption sites, and Fe supported on the surface of the charcoal 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 the pretreated electric furnace dust is taken, added with 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 40 g 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 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, 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 conditions of the addition amount of analytically pure hydrochloric acid are shown in table 1.
TABLE 1 parameters and effects of examples 1-3
Example 4-6 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 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 40 g 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 under different KOH addition amounts are shown in Table 2.
TABLE 2 parameters and Effect of examples 4-6
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 40 g 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 Heating at the speed of C/min, calcining for 2h, cooling, washing to neutrality, drying to constant weight, and sieving with 200 mesh sieve to obtain composite magnetic biocharAnd (4) an auxiliary agent.
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 calcination temperature conditions are shown in table 3.
TABLE 3 parameters and Effect of examples 7-10
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 40 g 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 C, calcining for 2h, cooling, washing to neutrality, and drying to constant temperatureAnd sieving the mixture by a 200-mesh sieve after the weight is increased to obtain the composite magnetic biochar 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 biochar 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
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 40 g 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 performing filtration at the speed of 5 ℃/min under inert gasThe temperature is raised to 500 degree at a speed 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 40 g 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 neutrality, drying to constant weight, and sieving with a 200-mesh sieve to obtain the composite magnetic charcoal adsorbent.
The adsorbent is prepared in the condition that the pH of an initial solution containing hexavalent chromium ions is =1, and the initial hexavalent chromium isChromium ion concentration of 500 mg/L, adsorbent addition of 4g/L, adsorption time of 1680 min, and temperature of 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 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) adding 140mL of KOH of 1mol/L and 40 g 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 500 ℃ 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.
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 percent by testing under the condition C, and meanwhile, the adsorbent passes through external magnetism by 3 times of parallel recovery experiment determinationRecovery on site determined the adsorbent recovery to be 32.78%.
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 40 g 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 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 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 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) adding 330mL of KOH of 1mol/L and 40 g 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 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) adding 360 mL of KOH of 1mol/L and 40 g 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 2 by using HCl;
step ii, adding the composite magnetic biochar 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 measurement of 3 parallel recovery experiments by using an external magnetic field to recover the adsorbent.
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 the preferred embodiment and all changes and modifications that fall within the scope of the present 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 (9)
1. The preparation method of the composite magnetic biochar adsorbent is characterized by comprising 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 testa oryzae into the obtained filtrate, stirring at room temperature, filtering to obtain residue, and placing the residue in a temperature range of 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.
2. The preparation method of the composite magnetic biochar adsorbent according to claim 1, wherein in the step III, the mass volume ratio of the pretreated electric furnace dust to the deionized water is 1-8-1.
3. The method for preparing the composite magnetic biochar adsorbent according to claim 1, wherein in the step III, the mass ratio of the pretreated electric furnace dust to the pretreated rice hulls is 1.
4. The method for preparing the composite magnetic biochar adsorbent according to claim 1, wherein in the step III, the acid comprises at least one of hydrochloric acid, sulfuric acid and nitric acid, the volume ratio of the acid to deionized water is 3-5.
5. The method for preparing the composite magnetic biochar adsorbent according to any one of claims 1 to 4, wherein in the step III, the specific parameters of the calcination are as follows: the calcination temperature is 500-900 ℃, the heating rate is 5-7 ℃/min, and the calcination time is more than 2 h.
6. A composite magnetic charcoal adsorbent, which is prepared by the preparation method of the composite magnetic charcoal adsorbent according to any one of claims 1 to 5.
7. Use of the composite magnetic biochar adsorbent of claim 6 in treatment of wastewater containing hexavalent chromium ions.
8. 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-containing wastewater to 1;
step ii, adding 3.5-4g/L of the composite magnetic biochar adsorbent as claimed in claim 6 into the wastewater, placing the wastewater in a shaking box, setting the ambient temperature to be room temperature, and setting the adsorption time to be more than 22 h.
9. The method of treating waste water containing hexavalent chromium ions according to claim 8, wherein an initial concentration of the hexavalent chromium ions in the waste water containing hexavalent chromium ions is 400 to 500 mg/L.
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CN113926459A (en) * | 2021-12-16 | 2022-01-14 | 华北理工大学 | Magnetic carbon-based catalyst and method for preparing biodiesel by using same |
CN114247426A (en) * | 2021-12-10 | 2022-03-29 | 有研资源环境技术研究院(北京)有限公司 | Biochar-loaded natural iron-containing mineral magnetic adsorbent and preparation method and application thereof |
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JP2010001524A (en) * | 2008-06-19 | 2010-01-07 | Jfe Steel Corp | Method of making zinc content in dust in iron manufacturing low |
CN105879834A (en) * | 2014-10-21 | 2016-08-24 | 王欣 | Preparation method of adsorbent for removing phosphorus and heavy metal anions in water as well as application method |
CN111876607A (en) * | 2020-07-07 | 2020-11-03 | 江苏科技大学 | Leaching, enriching and separating process for iron and chromium elements in electric furnace dust |
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