CN105854796B - A kind of preparation method and application of magnetism bimetallic oxide/carbon composite - Google Patents

A kind of preparation method and application of magnetism bimetallic oxide/carbon composite Download PDF

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CN105854796B
CN105854796B CN201610213298.3A CN201610213298A CN105854796B CN 105854796 B CN105854796 B CN 105854796B CN 201610213298 A CN201610213298 A CN 201610213298A CN 105854796 B CN105854796 B CN 105854796B
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carbon composite
water
heavy metal
bimetallic oxide
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CN105854796A (en
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孟嘉
闫良国
于海琴
闫涛
杜斌
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University of Jinan
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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
    • B01J20/06—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04
    • B01J20/08—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04 comprising aluminium oxide or hydroxide; comprising bauxite
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00—Treatment of water, waste water, or sewage
    • C02F1/28—Treatment of water, waste water, or sewage by sorption
    • C02F1/281—Treatment of water, waste water, or sewage by sorption using inorganic sorbents
    • 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
    • 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

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  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
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  • Chemical Kinetics & Catalysis (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Hydrology & Water Resources (AREA)
  • Engineering & Computer Science (AREA)
  • Environmental & Geological Engineering (AREA)
  • Water Supply & Treatment (AREA)
  • Solid-Sorbent Or Filter-Aiding Compositions (AREA)
  • Water Treatment By Sorption (AREA)

Abstract

The present invention relates to the preparations and application of magnetic bimetallic oxide/carbon composite, belong to composite material preparation and water-treatment technology field.The mixed base suspension of the mixing salt solution of magnesium nitrate and aluminum nitrate and sodium hydroxide and sodium carbonate is added dropwise in the beaker of the distilled water containing ferroso-ferric oxide of 60 DEG C of heating by the present invention, control ph 10 or so, continue 6~12 h of stirring, stands 3~6 h, obtain magnetic hydrotalcite suspension；Magnetic hydrotalcite suspension obtained is added in Congo red waste water, vibrates 3 h；Then it dry, pulverize, be placed in high temperature process furnances, heat 2 ~ 4 h at 500 ~ 800 DEG C under nitrogen protection, obtain magnetic bimetallic oxide/carbon composite；It is applied to the removal of lead in water, cadmium, copper ion, works well.Magnetic bimetallic oxide/carbon composite prepared by the present invention, preparation process is simple, and condition is easily-controllable, and adsorption capacity is high, can effectively remove the heavy metal ion in water.

Description

A kind of preparation method and application of magnetism bimetallic oxide/carbon composite
Technical field
The present invention relates to a kind of preparation methods of magnetic bimetallic oxide/carbon composite, and applied to a huge sum of money in water The removal for belonging to ion belongs to composite material preparation and water-treatment technology field.
Background technology
Hydrotalcite is a kind of anionic clay quickly grown in recent years, is a kind of stratiform with two dimension pattern plate structure Compound, typical chemical general formula are：[M1-x 2+Mx 3+(OH)2][An-]x/n·yH2O, wherein M2+And M3+Respectively on laminate Divalent and trivalent metal cation；An-It is interlayer anion；X is M3+With（M2++M3+）Molar ratio, usual range be from 0.17 to 0.33；Y is the number of interlayer hydrone.The structure of hydrotalcite is special, and the anion of interlayer has interchangeability, main layer Cation on plate has Modulatory character, has memory effect, high-temperature roasting product can be changed into hydrotalcite in water, and compare table Area and pore structure is larger makes it have preferable adsorptivity, can be widely used in Industrial Wastewater Treatment.
Hydrotalcite removes the organic dyestuff in water removal as adsorbent, not only of low cost, but also effect is preferable.By magnetic base Matter is assembled with hydrotalcite, the magnetic hydrotalcite of the tool prepared, and has higher adsorption capacity, and can use Magneto separate Technology separates and recovers, and has renewable, environmentally safe.
In recent years, with industrial or agricultural and the fast development of economy, the heavy metal pollution in all kinds of water environments aggravates increasingly, The maximum feature of heavy metal pollution, which is heavy metal, to degrade in the environment, once i.e. water body or soil is contaminated by heavy metals, from The catharsis of body cannot be by abatement of pollution.Heavy metal pollution can generate serious harm to human body and environment, be easy in organism Interior accumulation leads to organism teratogenesis or mutation, or even dead.The present invention utilizes the discarded magnetic neatly after absorption congo red Stone is raw material, by high temperature cabonization, prepares magnetic bimetallic oxide/carbon composite, to water middle and high concentration heavy metal from The adsorption capacity of son is high, can effectively handle the waste water containing heavy metal.
Invention content
Purpose of the present invention is to the discarded magnetic hydrotalcites to adsorb dyestuff as raw material, and one is prepared by the method for high temperature cabonization Magnetic bimetallic oxide/the carbon composite of kind, and as adsorbent, realize the removal of heavy metal ion in water.
Technical solution
A kind of preparation method of magnetism bimetallic oxide/carbon composite, includes the following steps：
（1）1.0 g iron chloride and 3.0 g sodium acetates are dissolved in 20 mL ethylene glycol, 10 mL ethylenediamines are then added, are formed Clear solution is encapsulated in the reaction kettle of polytetrafluoroethylene (PTFE) and heats 8 h at 200 DEG C, is then cooled to room temperature, the black that will be obtained Solid is washed with water for several times, obtains Fe3O4；
（2）By magnesium nitrate and aluminum nitrate distillation water dissolution, NaOH and Na2CO3 With distillation water dissolution, in 60 DEG C of water-baths and Under conditions of being stirred continuously, two parts of solution instillations are filled and are dispersed with Fe3O4Distilled water beaker in, maintenance system pH is 10 6~12 h of stirring is continued in left and right after being added dropwise to complete, stand 3~6 h, be washed with distilled water to neutrality, obtain magnetic magnalium neatly The suspension of stone；
（3）Congo red waste water is added in the suspension of magnetic mg_al hydrotalcite, with magnet after 3 h of stirring and adsorbing Separation 5 minutes, obtains the solid for adsorbing Congo red magnetic mg_al hydrotalcite；
（4）The magnetic mg_al hydrotalcite for adsorbing Congo red dry, pulverize, be placed in high temperature process furnances, in nitrogen protection Be carbonized 2 ~ 4 h at 500 ~ 800 DEG C lower, is ground up, sieved, obtains magnetic bimetallic oxide/carbon composite.
The above method is prepared for magnetic double gold using the magnetic hydrotalcite for adsorbing congo red as raw material by high temperature cabonization Belong to oxide/carbon composite material.During preparing ferroso-ferric oxide, using iron chloride as source of iron, ethylene glycol is solvent and right Ferric ion carries out partial solvent thermal reduction, and sodium acetate is reaction promoter, and ethylenediamine is coating agent and provides four oxygen of synthesis Change three ironing surface amino groups.During preparing magnetic hydrotalcite, magnesium nitrate, aluminum nitrate, sodium hydroxide, sodium carbonate, The usage ratio of ferroso-ferric oxide is：0.05 mol：0.025 mol：0.15 mol：0.05 mol：0.0083 mol, four oxidations Three ironing surface amino make it be easy to be combined with hydrotalcite, and addition does not influence the synthesis of magnetic hydrotalcite, but can cause to produce The difference of object magnetism size.Effective control of pH value is the generation for avoiding hydroxide dephasign.PH value is excessively high to cause Al3+And its The dissolving of his ion, and low pH value can make reaction incomplete.Dynamic and static crystallization after the completion of reaction are to tie in order to obtain The brilliant good hydrotalcite of degree.During high temperature cabonization, nitrogen is protective gas, prevents the entrance of carbon dioxide.High-temperature heating So that the congo red that magnetic hydrotalcite adsorbs fully is carbonized, while destroying the layer structure of hydrotalcite, becomes metal oxide, To obtain magnetic bimetallic oxide/carbon composite.But excessively high temperature makes the memory effect of hydrotalcite disappear, bimetallic Oxide cannot be efficiently translated into hydrotalcite in water, and too low temperature carbonization is incomplete.
Removal by magnetic bimetallic oxide/carbon composite adsorbent of preparation for heavy metal ion in water, step It is rapid as follows：
It takes the heavy metal ion solution of a concentration of 200 ~ 800 mg/L of 20 mL in 50 mL centrifuge tubes, is added 0.05 g's Magnetic bimetallic oxide/carbon composite vibrates 1~5 h, is then centrifuged at room temperature, and supernatant is taken to detect heavy metal Ion concentration, according to the heavy metal ion residual concentration in solution after the initial concentration of heavy metal ion in solution and absorption, meter Calculate the removal rate and adsorbance of heavy metal ion.Heavy metal ion is selected from one of following：Cu2+、Pb2+、Cd2+。
In the method for above-mentioned heavy-metal ion removal, the bimetallic oxide ingredient in composite material has memory effect, It is changed into hydrotalcite in water, to effectively adsorb heavy metal, the carbon component that Congo red carbonization is formed has multiple functions group, Also heavy metal can be effectively adsorbed, this makes the ability of magnetic bimetallic oxide/carbon composite adsorbing heavy metal in water significantly Enhancing is higher than common adsorbent.Meanwhile the magnetism that composite material itself has makes the solid after absorption and liquid add magnetic outside Quick separating is realized under the action of, is easily recycled.
Advantageous effect
（1）The present invention prepares a kind of magnetic bimetallic oxidation to adsorb Congo red discarded magnetic mg_al hydrotalcite as raw material Object/carbon composite is not only recycled discarded hydrotalcite, provides a kind of method of resource of adsorbent, simultaneously A kind of magnetic carbon-containing composite material of tool is obtained；
（2）Magnetic bimetallic oxide/carbon composite prepared by the present invention make full use of hydrotalcite memory effect and Adsorption capacity caused by carbon material surface functional group may be implemented efficiently to go heavy metal ion under smaller dosage It removes, and is easy to realize quick separating under externally-applied magnetic field；
（3）Magnetic bimetallic oxide/carbon composite preparation process of the present invention is simple, easy to spread.
Specific implementation mode
Embodiment 1：The preparation method of magnetic bimetallic oxide/carbon composite
（1）1.0 g iron chloride and 3.0 g sodium acetates are dissolved in 20 mL ethylene glycol, 10 mL ethylenediamines are then added, are formed Clear solution is encapsulated in the reaction kettle of polytetrafluoroethylene (PTFE) and heats 8 h at 200 DEG C, is then cooled to room temperature, the black that will be obtained Solid is washed with water for several times, obtains Fe3O4；
（2）By the distillation water dissolution of 0.05 mol magnesium nitrates and 0.025 mol aluminum nitrates, by 0.15 mol NaOH and 0.05 mol Na2CO3 With distillation water dissolution, in 60 DEG C of water-baths and under conditions of be stirred continuously, two parts of solution is instilled and are filled point Dissipating has 0.0083 mol Fe3O4Distilled water beaker in, maintenance system pH continues stirring 6 10 or so after being added dropwise to complete H stands 3 h, is washed with distilled water to neutrality, obtains the suspension of magnetic mg_al hydrotalcite；
（3）Congo red waste water is added in gained magnetic mg_al hydrotalcite suspension, with magnetic after 3 h of stirring and adsorbing Iron detaches 5 minutes, obtains the solid for adsorbing Congo red magnetic mg_al hydrotalcite；
（4）The magnetic mg_al hydrotalcite for adsorbing Congo red dry, pulverize, be placed in high temperature process furnances, in nitrogen protection Be carbonized 2 h at lower 500 DEG C, is ground up, sieved, and obtains magnetic bimetallic oxide/carbon composite.
Embodiment 2：The preparation method of magnetic bimetallic oxide/carbon composite
（1）1.0 g iron chloride and 3.0 g sodium acetates are dissolved in 20 mL ethylene glycol, 10 mL ethylenediamines are then added and are formed Clear solution is encapsulated in the reaction kettle of polytetrafluoroethylene (PTFE) and heats 8 h at 200 DEG C, is then cooled to room temperature, the black that will be obtained Solid is washed with water for several times, obtains Fe3O4；
（2）By the distillation water dissolution of 0.05 mol magnesium nitrates and 0.025 mol aluminum nitrates, by 0.15 mol NaOH and 0.05 mol Na2CO3 With distillation water dissolution, in 60 DEG C of water-baths and under conditions of be stirred continuously, two parts of solution is instilled and are filled point Dissipating has 0.0083 mol Fe3O4Distilled water beaker in, maintenance system pH continues stirring 12 10 or so after being added dropwise to complete H stands 6 h, is washed with distilled water to neutrality, obtains the suspension of magnetic mg_al hydrotalcite；
（3）Congo red waste water is added in gained magnetic mg_al hydrotalcite suspension, with magnetic after 3 h of stirring and adsorbing Iron detaches 5 minutes, obtains the solid for adsorbing Congo red magnetic mg_al hydrotalcite；
（4）The magnetic mg_al hydrotalcite for adsorbing Congo red dry, pulverize, be placed in high temperature process furnances, in nitrogen protection Be carbonized 3 h at lower 600 DEG C, is ground up, sieved, and obtains magnetic bimetallic oxide/carbon composite.
Embodiment 3：The preparation method of magnetic bimetallic oxide/carbon composite
（1）1.0 g iron chloride and 3.0 g sodium acetates are dissolved in 20 mL ethylene glycol, 10 mL ethylenediamines are then added, are formed Clear solution is encapsulated in the reaction kettle of polytetrafluoroethylene (PTFE) and heats 8 h at 200 DEG C, is then cooled to room temperature, the black that will be obtained Solid is washed with water for several times, obtains Fe3O4；
（2）By the distillation water dissolution of 0.05 mol magnesium nitrates and 0.025 mol aluminum nitrates, by 0.15 mol NaOH and 0.05 mol Na2CO3 With distillation water dissolution, in 60 DEG C of water-baths and under conditions of be stirred continuously, two parts of solution is instilled and are filled point Dissipating has 0.0083 mol Fe3O4Distilled water beaker in, maintenance system pH continues stirring 8 10 or so after being added dropwise to complete H stands 6 h, is washed with distilled water to neutrality, obtains the suspension of magnetic mg_al hydrotalcite；
（3）Congo red waste water is added in gained magnetic mg_al hydrotalcite suspension, with magnetic after 3 h of stirring and adsorbing Iron detaches 5 minutes, obtains adsorbing the outstanding solid of Congo red magnalium hydrotalcite；
（4）The magnetic mg_al hydrotalcite suspension for adsorbing Congo red dry, pulverize, be placed in high temperature process furnances, in nitrogen Be carbonized 4 h at lower 800 DEG C of gas shielded, is ground up, sieved, obtains magnetic bimetallic oxide/carbon composite.
Embodiment 4：Heavy metal ion Cu2+Removal
Take the Cu of a concentration of 200 mg/L of 20 mL2+The magnetic bimetallic of 0.05 g is added in 50 mL centrifuge tubes in solution Oxide/carbon composite material vibrates 5 h at 25 DEG C, is then centrifuged, and supernatant is taken to detect Cu2+Concentration, according in solution Cu2+Initial concentration and absorption after Cu in solution2+Residual concentration, calculate Cu2+Removal rate reach 99.50%.
Embodiment 5：Heavy metal ion Cd2+Removal
Take the Cd of a concentration of 400 mg/L of 20 mL2+The magnetic bimetallic of 0.05 g is added in 50 mL centrifuge tubes in solution Oxide/carbon composite material vibrates 3 h at 25 DEG C, is then centrifuged, and supernatant is taken to detect Cd2+Concentration, according in solution Cd2+Initial concentration and absorption after Cd in solution2+Residual concentration, calculate Cd2+Removal rate reach 99.43%.
Embodiment 6：Heavy metal ion Pb2+Removal
Take the Pb of a concentration of 800 mg/L of 20 mL2+The magnetic bimetallic of 0.05 g is added in 50 mL centrifuge tubes in solution Oxide/carbon composite material vibrates 1 h at 25 DEG C, is then centrifuged, and supernatant is taken to detect Pb2+Concentration, according in solution Pb2+Initial concentration and absorption after Pb in solution2+Residual concentration, calculate Pb2+Removal rate reach 88.73%.

Claims (3)

1. a kind of application as adsorbent of magnetism bimetallic oxide/carbon composite, which is characterized in that
The preparation method of magnetic bimetallic oxide/carbon composite includes the following steps：
（1）1.0g iron chloride and 3.0g sodium acetates are dissolved in 20mL ethylene glycol, 10mL ethylenediamines are then added, is formed transparent molten Liquid is encapsulated in the reaction kettle of polytetrafluoroethylene (PTFE) and heats 8h at 200 DEG C, is then cooled to room temperature, and obtained black solid is used Water washing for several times, obtains Fe3O4；
（2）By magnesium nitrate and aluminum nitrate distillation water dissolution, NaOH and Na2CO3With water dissolution is distilled, in 60 DEG C of water-baths and constantly Under conditions of stirring, two parts of solution instillations are filled and are dispersed with Fe3O4Distilled water beaker in, maintenance system pH 10 or so, Continue 6~12h of stirring after being added dropwise to complete, stand 3~6h, be washed with distilled water to neutrality, obtains the outstanding of magnetic mg_al hydrotalcite Turbid；
（3）Congo red waste water is added in the suspension of magnetic mg_al hydrotalcite, 5 are detached with magnet after stirring and adsorbing 3h Minute, obtain the solid for adsorbing Congo red magnetic mg_al hydrotalcite；
（4）The magnetic mg_al hydrotalcite for adsorbing Congo red dry, pulverize, be placed in high temperature process furnances, under nitrogen protection 500 Be carbonized 2~4h at~800 DEG C, is ground up, sieved, obtains magnetic bimetallic oxide/carbon composite；
The removal as adsorbent for heavy metal ion in water of above-mentioned magnetism bimetallic oxide/carbon composite, step It is as follows：
Take the heavy metal ion solution of a concentration of 200~800mg/L of 20mL in 50mL centrifuge tubes, the magnetism that 0.05g is added is double Metal oxide/carbon composite vibrates 1~5h at 25 DEG C, is then centrifuged, and takes supernatant detection heavy metal ion dense Degree calculates heavy metal according to the heavy metal ion residual concentration in solution after the initial concentration of heavy metal ion in solution and absorption The removal rate of ion.
2. a kind of application as adsorbent of magnetic bimetallic oxide/carbon composite according to claim 1, It is characterized in that, magnesium nitrate, aluminum nitrate, sodium hydroxide, sodium carbonate, the usage ratio of ferroso-ferric oxide is 0.05mol： 0.025mol：0.15mol：0.05mol：0.0083mol.
3. a kind of application as adsorbent of magnetic bimetallic oxide/carbon composite according to claim 1, It is characterized in that, the heavy metal ion is selected from one of following：Cu2+、Pb2+、Cd2+。
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CN107126925B (en) * 2017-06-12 2019-12-20 扬州工业职业技术学院 Magnetic nano material and application thereof in anegliptin drug detection
CN108568289B (en) * 2018-04-23 2020-08-21 沈阳工业大学 Method for preparing carbon-copper coated ferroferric oxide composite magnetic oil removal particles
CN108745284B (en) * 2018-06-05 2020-04-21 太原理工大学 Magnetic magnalium hydrotalcite/nano onion carbon composite material and preparation method and application thereof
CN109513419B (en) * 2018-11-08 2021-09-21 华南理工大学 Magnetic magnesium-manganese layered double-metal oxide composite material and preparation and application thereof
CN109529793B (en) * 2018-11-14 2021-08-31 济南大学 Preparation method and application of magnetic hydrotalcite loaded titanium dioxide composite material
CN110380027B (en) * 2019-06-28 2022-07-15 惠州学院 Preparation method of carbon-containing bimetallic oxide
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