CN108160026A - One kind absorbs the method with restoring Cr (VI) based on iron magnesia-alumina hydrotalcite - Google Patents

One kind absorbs the method with restoring Cr (VI) based on iron magnesia-alumina hydrotalcite Download PDF

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CN108160026A
CN108160026A CN201711380880.XA CN201711380880A CN108160026A CN 108160026 A CN108160026 A CN 108160026A CN 201711380880 A CN201711380880 A CN 201711380880A CN 108160026 A CN108160026 A CN 108160026A
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iron
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张文涛
周东升
严桂林
陈显飞
张佩聪
王益群
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Chengdu Univeristy of Technology
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/06Solid 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
    • B01J20/08Solid 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
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01FCOMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
    • C01F7/00Compounds of aluminium
    • C01F7/78Compounds containing aluminium and two or more other elements, with the exception of oxygen and hydrogen
    • C01F7/782Compounds containing aluminium and two or more other elements, with the exception of oxygen and hydrogen containing carbonate ions, e.g. dawsonite
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01GCOMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G49/00Compounds of iron
    • C01G49/009Compounds containing, besides iron, two or more other elements, with the exception of oxygen or hydrogen
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/28Treatment of water, waste water, or sewage by sorption
    • C02F1/281Treatment of water, waste water, or sewage by sorption using inorganic sorbents
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/70Treatment of water, waste water, or sewage by reduction
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00Crystal-structural characteristics
    • C01P2002/70Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
    • C01P2002/72Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00Crystal-structural characteristics
    • C01P2002/80Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
    • C01P2002/85Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70 by XPS, EDX or EDAX data
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00Nature of the contaminant
    • C02F2101/10Inorganic compounds
    • C02F2101/20Heavy metals or heavy metal compounds
    • C02F2101/22Chromium or chromium compounds, e.g. chromates

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (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)
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  • Solid-Sorbent Or Filter-Aiding Compositions (AREA)

Abstract

The present invention relates to a kind of preparation and application for heavy metal adsorption and the houghite of reduction, specific steps include:a)With formula M g6‑xFexAl2(OH)16CO3·4H2O (x=0.3 ~ 1.2) is target, stoichiometrically weighs each raw material, and deionized water is added in magnesium raw material, iron material, aluminum feedstock and forms solution A, and deionized water is added in alkali metal and carbonated starting material and forms solution B;b)Solution A is added drop-wise in solution B, and the mixing suspension formed is poured into autoclave, 120 ~ 180 DEG C is risen to and is heat-treated.Finally, Mg is formed after filtering, washing and dry6‑xFexAl2(OH)16CO3·4H2O samples;c)Sample is added in potassium bichromate solution, one group of supernatant is taken to do adsorption rate test, while detect the reducing degree of Cr in material (VI) per 2h.Iron magnesia-alumina hydrotalcite prepared by the present invention has heavy metal good adsorption capacity, and pass through Fe2+The recycling of the material is realized to the Reduced separating of heavy metal.This method is easy to operate, and absorbing and reducing is efficient, at low cost, will not cause secondary pollution.

Description

One kind absorbs the method with restoring Cr (VI) based on iron magnesia-alumina hydrotalcite
Technical field
Metal uptake and the preparation and application of the iron magnesia-alumina hydrotalcite of reduction are used for the present invention relates to a kind of, specially Mg6-xFexAl2(OH)16CO3·4H2The preparation method of O belongs to environment functional material and heavy metal processing technology field.
Background technology
Chromate waste water is essentially from industries such as mining, metallurgical, plating, process hides and bichromate productions.It is produced in industrial production If raw chromium slag air storage, drenched and soaked by sleet, contained chromium is dissolved meeting in permeate the ground water or entrance river, lake Serious pollution environment.In heavy metal pollution type, pollution of chromium comes second.The toxicity of chromium is related there are valence state with it, ring Chromium in border mainly exists with two kinds of valence states of Cr (III) and Cr (VI), and Cr (III) exists with cationic form, and Cr (VI) is then Exist with chromate anionic form, wherein Cr (VI) hundreds of times higher than Cr (III) toxicity, and be easily absorbed by the body and in body Interior accumulation causes the diseases such as rhinitis, tuberculosis, diarrhea, bronchitis, dermatitis.
Recognizing environment and the ecological hazard of Cr (VI), domestic and international many scholars are thrown oneself into the environmental improvement of Cr (VI), In acid condition, the oxidisability of Cr (VI) and stability are relatively strong, it is difficult to by oxidative degradation.At present, water body or chromium slag are removed In leachate the method for Cr (VI) mainly have chemical precipitation method, ion-exchange, absorption method, membrane separation process, electrolytic reduction and Chemical reagent reduction method etc., wherein absorption method is most widely used.Compared with other methods, absorption method has removal rate height, behaviour Make the advantages that easy, adsorbent is renewable, be widely used in the processing of chromate waste water.It is main that more absorption adsorbent is studied at present There are natural mineral matter, agriculture and forestry organic waste material, polymer, resin, microbial flocculant and charcoal (carbon) matter adsorbent etc..But it inhales Attached method is only transferred to Cr (VI) in another phase from a phase, not only cannot fundamentally remove Cr (VI), but also in follow-up Cr (VI) secondary pollution is easily generated in processing procedure.Under certain condition, if promoting high toxicity Cr (VI) to non-toxic Cr (III) transformation can effectively avoid secondary pollution of the chromium to environment.However, still seeking a kind of active set Cr (VI) suction at present Materials and methods that are attached and being reduced to Cr (III) one.
Invention content
The present invention for current Cr (VI) sorbing materials there are the defects of, the Mg that a kind of reduced form Fe (II) participates in is provided6- xFexAl2(OH)16CO3·4H2O houghite preparation methods.For the present invention using iron magnalium salt as raw material, prepared by hydrothermal reaction at low temperature.It should Method raw material is cheap, simple for process, and using Fe (II) part substitution Mg (II), is provided for Cr (VI) to the transformation of Cr (III) Reducing environment realizes the environment-protective circulating absorption of Cr (VI), effectively avoids secondary pollution, and the green processing for practical chromate waste water carries For theoretical direction and technical support.
To achieve the above object, the present invention prepares Mg6-xFexAl2(OH)16CO3·4H2O houghites and its absorbing and reducing The step of Cr (VI), includes:
a)It stoichiometrically weighs containing magnesium raw material, iron-bearing material, aluminum-containing raw material and alkali metal hydroxide and carbonated starting material, Deionized water is added in containing magnesium raw material, iron-bearing material, aluminum-containing raw material and forms homogeneous solution A, in alkali metal hydroxide and carbon Deionized water is added in hydrochlorate raw material and forms homogeneous solution B;Wherein, stoichiometric ratio is to adulterate the Mg of Fe (II)6Al2(OH)16CO3·4H2O is target product, general formula Mg6-xFexAl2(OH)16CO3·4H2O, Fe doping x:0.3~1.2;
B) solution A is added drop-wise in solution B under magnetic agitation, and the mixing suspension formed is poured into autoclave, 120 ~ 180 DEG C of heat treatments for carrying out 6 ~ 18h are risen to again after 1h is preheated at 60 ~ 80 DEG C.Finally, after washed, suction filtration and drying Form Mg6-xFexAl2(OH)16CO3·4H2O samples;
C) sample is added in 6 groups of potassium bichromate solutions being configured, after being sufficiently stirred, one of which is taken at interval of 2h Supernatant do adsorption rate test, while detect the reducing degree of Cr in sorbing material (VI).
Wherein, the magnesium raw material that contains is magnesium nitrate or magnesium chloride;The iron-bearing material is ferrous nitrate or frerrous chloride;Institute Aluminum-containing raw material is stated as aluminum nitrate or aluminium chloride;The alkali metal hydroxide is sodium hydroxide or potassium hydroxide;The alkali gold It is sodium carbonate or potassium carbonate to belong to carbonate.
In step a, Fe (II) dopings are limited as 0.3 ~ 1.2, it, can not when content is too small since Fe (II) is reducing agent Effectively reduction Cr (VI) is Cr (III);During too high levels, the layer structure of raw water talcum cannot keep.
In step b, Mg6-xFexAl2(OH)16CO3·4H2The drying process of O carries out in vacuum drying chamber, in order to avoid largely Fe2+It is oxidized to Fe before use3+
Preferably, raw material initial concentration is the mol/L of 0.2 mol/L ~ 0.6 in step a.
Preferably, the speed that solution A is added dropwise in step b is 10 ~ 30 drops/min.
Preferably, preheating temperature is 60 ~ 80 DEG C in step b.
Preferably, hydro-thermal reaction carries out at being 120 ~ 180 DEG C in temperature in step b.
Preferably, all potassium bichromate solution initial concentrations are 80 ~ 100 mg/L in step c.
Beneficial effects of the present invention:
For the present invention using iron magnalium salt as raw material, prepared by hydrothermal reaction at low temperature.This method raw material is cheap, simple for process, and uses Fe (II) part substitution Mg (II), provides reducing environment to the transformation of Cr (III) for Cr (VI), effectively avoids secondary pollution, realizes The environment-protective circulating absorption of Cr (VI), the green processing for practical chromate waste water provide theoretical direction and technical support.
Description of the drawings
Fig. 1 is 1 gained Mg of the embodiment of the present invention5.7Fe0.3Al2(OH)16CO3·4H2The XRD diagram of O, as shown in Figure 1:Implement The XRD results of 1 gained fluorescent material of example to be consistent with the diffraction maximum of standard hydrotalcite-like compound, and unknown explict occurrence Fe (II) or Other impurity peaks.
Fig. 2 is Cr (VI) adsorption rate figure of 1 gained sorbing material of the embodiment of the present invention, as shown in Figure 2:1 gained of embodiment Mg5.7Fe0.3Al2(OH)16CO3·4H2O materials have apparent absorption to Cr (VI), and than the magnalium hydrotalcite of undoped Fe (II) Adsorption effect is good.
Fig. 3 is the Mg after the embodiment of the present invention 1 is adsorbed5.7Fe0.3Al2(OH)16CO3·4H2The XPS figures of the Fe elements of O, by The Fe 2p peaks of Fig. 3 are understood:Into hydrotalcite-like compound Fe (II) it is oxidized after be changed into Fe (III), it is meant that for absorption after Cr (VI) provide reducing environment.
Fig. 4 is the Mg after the embodiment of the present invention 1 is adsorbed5.7Fe0.3Al2(OH)16CO3·4H2The XPS figures of the Cr elements of O, by Fig. 4 is understood:The Cr (VI) on houghite is adsorbed, through Fe2+It is changed into nontoxic Cr (III) after reduction, avoids at the later stage Secondary pollution during reason.
Fig. 5 is 2 gained Mg of the embodiment of the present invention5.4Fe0.6Al2(OH)16CO3·4H2The XRD diagram of O, as shown in Figure 5:Implement The XRD results of 2 gained fluorescent material of example to be consistent with the diffraction maximum of standard hydrotalcite-like compound, and unknown explict occurrence Fe (II) or Other impurity peaks.
Fig. 6 is Cr (VI) adsorption rate figure of 2 gained sorbing material of the embodiment of the present invention, as shown in Figure 6:2 gained of embodiment Mg5.4Fe0.6Al2(OH)16CO3·4H2O materials have apparent absorption to Cr (VI), and than the magnalium hydrotalcite of undoped Fe (II) Adsorption effect is good.
Fig. 7 is 3 gained Mg of the embodiment of the present invention4.8Fe1.2Al2(OH)16CO3·4H2The XRD diagram of O, as shown in Figure 7:Implement The XRD results of 3 gained fluorescent material of example to be consistent with the diffraction maximum of standard hydrotalcite-like compound, and unknown explict occurrence Fe (II) or Other impurity peaks.
Fig. 8 is Cr (VI) adsorption rate figure of 3 gained sorbing material of the embodiment of the present invention, as shown in Figure 8:3 gained of embodiment Mg4.8Fe1.2Al2(OH)16CO3·4H2O materials have apparent absorption to Cr (VI), and than the magnalium hydrotalcite of undoped Fe (II) Adsorption effect is good.
Specific embodiment
The present invention prepares Mg6-xFexAl2(OH)16CO3·4H2O houghites and its step of absorbing and reducing Cr (VI), wrap It includes:
A) it stoichiometrically weighs former containing magnesium raw material, iron-bearing material, aluminum-containing raw material and alkali metal hydroxide and carbonate Material, in containing magnesium raw material, iron-bearing material, aluminum-containing raw material adding in deionized water forms homogeneous solution A, in alkali metal hydroxide and Deionized water is added in carbonated starting material and forms homogeneous solution B;Wherein, stoichiometric ratio is to adulterate the Mg of Fe (II)6Al2 (OH)16CO3·4H2O is target product, general formula Mg6-xFexAl2(OH)16CO3·4H2O, Fe doping x:0.3~1.2;
B) solution A is added drop-wise in solution B under magnetic agitation, and the mixing suspension formed is poured into autoclave, 120 ~ 180 DEG C of heat treatments for carrying out 6 ~ 18h are risen to again after 1h is preheated at 60 ~ 80 DEG C.Finally, after washed, suction filtration and drying Form Mg6-xFexAl2(OH)16CO3·4H2O samples;
C) sample is added in 6 groups of potassium bichromate solutions being configured, after being sufficiently stirred, one of which is taken at interval of 2h Supernatant do adsorption rate test, while detect the reducing degree of Cr in sorbing material (VI).
Wherein, the magnesium raw material that contains is magnesium nitrate or magnesium chloride;The iron-bearing material is ferrous nitrate or frerrous chloride;Institute Aluminum-containing raw material is stated as aluminum nitrate or aluminium chloride;The alkali metal hydroxide is sodium hydroxide or potassium hydroxide;The alkali gold It is sodium carbonate or potassium carbonate to belong to carbonate.
In step a, Fe is limited2+Doping is 0.3 ~ 1.2,, can not be effective when content is too small since Fe (II) is reducing agent It is Cr (III) to restore Cr (VI);During too high levels, the layer structure of raw water talcum cannot keep.
In step b, Mg6-xFexAl2(OH)16CO3·4H2The drying process of O carries out in vacuum drying chamber, in order to avoid largely Fe (II) be oxidized to Fe (III) before use.
Preferably, raw material initial concentration is the mol/L of 0.2 mol/L ~ 0.6 in step a.
Preferably, the speed that solution A is added dropwise in step b is 10 ~ 30 drops/min.
Preferably, preheating temperature is 60 ~ 80 DEG C in step b.
Preferably, hydro-thermal reaction carries out at being 120 ~ 180 DEG C in temperature in step b.
Preferably, all potassium bichromate solution initial concentrations are 80 ~ 100 mg/L in step c.
The specific embodiment of the present invention is further described with reference to embodiment, is not therefore limited the present invention System is among the embodiment described range.
Embodiment 1
Building-up process:
1) by Mg5.7Fe0.3Al2(OH)16CO3·4H2The stoichiometric ratio of O weighs raw material magnesium nitrate(Mg(NO3)2)1.6872g、 Ferrous nitrate(Fe(NO3)2)0.1079g, aluminum nitrate(Al(NO3)3·9H2O)1.5005g, sodium hydroxide(NaOH)1.28g with carbon Sour sodium(Na2CO3)0.212g, in Mg (NO3)2、Fe(NO3)2、Al(NO3)3·9H2Deionized water is added in O and forms homogeneous solution A, in NaOH and Na2CO3Middle addition deionized water forms homogeneous solution B.
2) solution A is added drop-wise in solution B under magnetic agitation, and the mixing suspension formed is poured into reaction under high pressure 120 DEG C of heat treatments for carrying out 15h are risen to again after 1h is preheated in kettle, at 60 DEG C.Finally, it is formed after washed, suction filtration and drying Mg5.7Fe0.3Al2(OH)16CO3·4H2O samples;
3) sample is added in a concentration of 80 mg/L potassium bichromate solutions of 6 groups be configured, after being sufficiently stirred, at interval of 2h takes the supernatant of one of which to do adsorption rate test, while detects the reducing degree of Cr in sorbing material (VI).
Fig. 1 is 1 gained Mg of the embodiment of the present invention5.7Fe0.3Al2(OH)16CO3·4H2The XRD diagram of O, as shown in Figure 1:Implement The XRD results of 1 gained fluorescent material of example to be consistent with the diffraction maximum of standard hydrotalcite-like compound, and unknown explict occurrence Fe (II) or Other impurity peaks.Fig. 2 is Cr (VI) adsorption rate figure of 1 gained sorbing material of the embodiment of the present invention, as shown in Figure 2:1 institute of embodiment Obtain Mg5.7Fe0.3Al2(OH)16CO3·4H2O materials have Cr (VI) apparent absorption, and the hydrotalcite than undoped Fe (II) is inhaled Attached effect is good.Fig. 3 is the Mg after the embodiment of the present invention 1 is adsorbed5.7Fe0.3Al2(OH)16CO3·4H2The XPS figures of the Fe elements of O, by The Fe 2p peaks of Fig. 3 are understood:Into hydrotalcite-like compound Fe (II) it is oxidized after be changed into Fe (III), it is meant that for absorption after Cr (VI) provide reducing environment.Fig. 4 is the Mg after the embodiment of the present invention 1 is adsorbed5.7Fe0.3Al2(OH)16CO3·4H2The Cr of O The XPS figures of element, as shown in Figure 4:The Cr (VI) on houghite is adsorbed, is changed into nontoxic Cr after Fe (II) reduction (III), secondary pollution during post-processing is avoided.
Embodiment 2
Building-up process:
1) by Mg5.4Fe0.6Al2(OH)16CO3·4H2The stoichiometric ratio of O weighs raw material magnesium chloride(MgCl2)1.0283g, chlorine Change ferrous(FeCl2)0.1521g, aluminium chloride(AlCl3)0.5334g, potassium hydroxide(KOH)1.7952g with potassium carbonate(K2CO3) 0.2764g, in MgCl2、FeCl2、AlCl3Middle addition deionized water forms homogeneous solution A, in KOH and K2CO3Middle addition deionization Water forms homogeneous solution B.
2) solution A is added drop-wise in solution B under magnetic agitation, and the mixing suspension formed is poured into reaction under high pressure 180 DEG C of heat treatments for carrying out 18h are risen to again after 1h is preheated in kettle, at 70 DEG C.Finally, it is formed after washed, suction filtration and drying Mg5.4Fe0.6Al2(OH)16CO3·4H2O samples;
3) sample is added in a concentration of 90 mg/L potassium bichromate solutions of 6 groups be configured, after being sufficiently stirred, at interval of 2h takes the supernatant of one of which to do adsorption rate test, while detects the reducing degree of Cr in sorbing material (VI).
Fig. 5 is 2 gained Mg of the embodiment of the present invention5.4Fe0.6Al2(OH)16CO3·4H2The XRD diagram of O, as shown in Figure 5:Implement The XRD results of 2 gained fluorescent material of example to be consistent with the diffraction maximum of standard hydrotalcite-like compound, and unknown explict occurrence Fe (II) or Other impurity peaks.Fig. 6 is Cr (VI) adsorption rate figure of 2 gained sorbing material of the embodiment of the present invention, as shown in Figure 6:2 institute of embodiment Obtain Mg5.4Fe0.6Al2(OH)16CO3·4H2O materials have Cr (VI) apparent absorption, and the hydrotalcite than undoped Fe (II) is inhaled Attached effect is good.
Embodiment 3
Building-up process:
1) by Mg4.8Fe1.2Al2(OH)16CO3·4H2The stoichiometric ratio of O weighs raw material magnesium nitrate(Mg(NO3)2)1.4208g、 Frerrous chloride(FeCl2)0.3042g, aluminum nitrate(Al(NO3)3·9H2O)1.5005g, sodium hydroxide(NaOH)1.28g with carbonic acid Potassium(K2CO3)0.2764g, in Mg (NO3)2、FeCl2、Al(NO3)3·9H2Deionized water is added in O and forms homogeneous solution A, NaOH and K2CO3Middle addition deionized water forms homogeneous solution B.
2) solution A is added drop-wise in solution B under magnetic agitation, and the mixing suspension formed is poured into reaction under high pressure 150 DEG C of heat treatments for carrying out 12h are risen to again after 1h is preheated in kettle, at 80 DEG C.Finally, it is formed after washed, suction filtration and drying Mg4.8Fe1.2Al2(OH)16CO3·4H2O samples;
3) sample is added in a concentration of 100 mg/L potassium bichromate solutions of 6 groups be configured, after being sufficiently stirred, every The supernatant of one of which is taken to do adsorption rate test every 2h, while detect the reducing degree of Cr in sorbing material (VI).
Fig. 7 is 3 gained Mg of the embodiment of the present invention4.8Fe1.2Al2(OH)16CO3·4H2The XRD diagram of O, as shown in Figure 7:Implement The XRD results of 3 gained fluorescent material of example to be consistent with the diffraction maximum of standard hydrotalcite-like compound, and unknown explict occurrence Fe (II) or Other impurity peaks.Fig. 8 is Cr (VI) adsorption rate figure of 3 gained sorbing material of the embodiment of the present invention, as shown in Figure 8:3 institute of embodiment Obtain Mg4.8Fe1.2Al2(OH)16CO3·4H2O materials have Cr (VI) apparent absorption, and the hydrotalcite than undoped Fe (II) is inhaled Attached effect is good.

Claims (10)

1. the present invention prepares Mg using hydro-thermal method6-xFexAl2(OH)16CO3·4H2O sorbing materials, step include:
a)It stoichiometrically weighs containing magnesium raw material, iron-bearing material, aluminum-containing raw material and alkali metal hydroxide and carbonated starting material, Deionized water is added in containing magnesium raw material, iron-bearing material, aluminum-containing raw material and forms homogeneous solution A, in alkali metal hydroxide and carbon Deionized water is added in hydrochlorate raw material and forms homogeneous solution B;Wherein, stoichiometric ratio is with Fe2+The Mg of doping6Al2(OH)16CO3·4H2O is target product, general formula Mg6-xFexAl2(OH)16CO3·4H2O, Fe doping x:0.3~1.2;B) magnetic Solution A is added drop-wise in solution B, and the mixing suspension formed is poured into autoclave under power stirring, 60 ~ 80 DEG C The heat treatment of 120 ~ 180 DEG C of 6 ~ 18h of progress is risen to after lower preheating 1h again;Finally, Mg is formed after washed, suction filtration and drying6- xFexAl2(OH)16CO3·4H2O samples;C) sample is added in 6 groups of potassium bichromate solutions being configured, waits to be sufficiently stirred Afterwards, the supernatant of one of which is taken to do adsorption rate test at interval of 2h, while detects the reducing degree of Cr in sorbing material (VI); Wherein, the magnesium raw material that contains is magnesium nitrate or magnesium chloride;The iron-bearing material is ferrous nitrate or frerrous chloride;It is described former containing aluminium Expect for aluminum nitrate or aluminium chloride;The alkali metal hydroxide is sodium hydroxide or potassium hydroxide;The alkali carbonate For sodium carbonate or potassium carbonate.
2. Mg according to claim 16-xFexAl2(OH)16CO3·4H2The preparation method of O, which is characterized in that in step a Iron-bearing material uses low price Fe2+Salt.
3. Mg according to claim 1 or 26-xFexAl2(OH)16CO3·4H2The preparation method of O, which is characterized in that step Fe in a2+The stoichiometry of doping is 0.3 ~ 1.2.
4. according to claims 1 to 3 any one of them Mg6-xFexAl2(OH)16CO3·4H2The preparation method of O, feature exist In raw material initial concentration is the mol/L of 0.2 mol/L ~ 0.6 in step a.
5. according to Claims 1 to 4 any one of them Mg6-xFexAl2(OH)16CO3·4H2The preparation method of O, feature exist In forming solution using magnetic agitation mode in step a, mixing speed is 400 ~ 1000 rad/min.
6. Mg according to claims 1 to 56-xFexAl2(OH)16CO3·4H2The preparation method of O, which is characterized in that step Solution A is added drop-wise in solution B in b, so that iron magnesium aluminium ion precipitates completely.
7. according to claim 1~6 any one of them Mg6-xFexAl2(OH)16CO3·4H2The preparation method of O, feature exist In the speed that solution A is added dropwise in step b is 10 ~ 30 drops/min.
8. according to claim 1~7 any one of them Mg6-xFexAl2(OH)16CO3·4H2The preparation method of O, feature exist In preheating temperature is 60 ~ 80 DEG C in step b.
9. according to claim 1~8 any one of them Mg6-xFexAl2(OH)16CO3·4H2The preparation method of O, feature exist In hydro-thermal reaction carries out at being 120 ~ 180 DEG C in temperature in step b.
10. according to claim 1~9 any one of them Mg6-xFexAl2(OH)16CO3·4H2The preparation method of O, feature exist In all potassium bichromate solution initial concentrations are 80 ~ 100 mg/L in step c.
CN201711380880.XA 2017-12-20 2017-12-20 One kind absorbs the method with restoring Cr (VI) based on iron magnesia-alumina hydrotalcite Pending CN108160026A (en)

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CN107500367A (en) * 2017-09-13 2017-12-22 太原理工大学 A kind of preparation method of chlorion intercalation NiAl-HTLcs
CN109529758A (en) * 2018-12-13 2019-03-29 东华理工大学 Mg-Fe double-metal hydroxide adsorbent, preparation method and application
CN109852392A (en) * 2018-12-13 2019-06-07 中国科学院南京土壤研究所 A kind of electroplating enterprise moves composition and its application of contaminated soil of site reparation
CN110817970A (en) * 2019-12-11 2020-02-21 宝鸡文理学院 Preparation of M from water supply sludge2+-Al3+-Fe3+Method for preparing hydrotalcite-like material and application thereof
CN113233569A (en) * 2021-04-17 2021-08-10 北京化工大学 Method for quickly removing manganese ions in wastewater and application of manganese-containing product in precious metal recovery
CN114870870A (en) * 2022-04-29 2022-08-09 成都理工大学 Magnetic environment purifying material for co-processing MO and Cr (VI) pollution and preparation method thereof
CN115382500A (en) * 2022-09-21 2022-11-25 北京化工大学 Reductive hydrotalcite and preparation method and application thereof
CN115814775A (en) * 2022-11-23 2023-03-21 成都理工大学 Regeneration method of lithium-aluminum layered double hydroxide adsorbent
CN115845792A (en) * 2022-10-21 2023-03-28 黑龙江省科学院高技术研究院 Preparation method and application of transition metal doped magnesium-aluminum layered double hydroxide material

Cited By (13)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107500367A (en) * 2017-09-13 2017-12-22 太原理工大学 A kind of preparation method of chlorion intercalation NiAl-HTLcs
CN107500367B (en) * 2017-09-13 2019-04-30 太原理工大学 A kind of preparation method of chloride ion intercalation NiAl-HTLcs
CN109529758A (en) * 2018-12-13 2019-03-29 东华理工大学 Mg-Fe double-metal hydroxide adsorbent, preparation method and application
CN109852392A (en) * 2018-12-13 2019-06-07 中国科学院南京土壤研究所 A kind of electroplating enterprise moves composition and its application of contaminated soil of site reparation
CN110817970B (en) * 2019-12-11 2022-03-29 宝鸡文理学院 Preparation of M from water supply sludge2+-Al3+-Fe3+Method for preparing hydrotalcite-like material and application thereof
CN110817970A (en) * 2019-12-11 2020-02-21 宝鸡文理学院 Preparation of M from water supply sludge2+-Al3+-Fe3+Method for preparing hydrotalcite-like material and application thereof
CN113233569A (en) * 2021-04-17 2021-08-10 北京化工大学 Method for quickly removing manganese ions in wastewater and application of manganese-containing product in precious metal recovery
CN114870870A (en) * 2022-04-29 2022-08-09 成都理工大学 Magnetic environment purifying material for co-processing MO and Cr (VI) pollution and preparation method thereof
CN115382500A (en) * 2022-09-21 2022-11-25 北京化工大学 Reductive hydrotalcite and preparation method and application thereof
CN115382500B (en) * 2022-09-21 2024-01-30 北京化工大学 Reductive hydrotalcite and preparation method and application thereof
CN115845792A (en) * 2022-10-21 2023-03-28 黑龙江省科学院高技术研究院 Preparation method and application of transition metal doped magnesium-aluminum layered double hydroxide material
CN115845792B (en) * 2022-10-21 2024-02-23 黑龙江省科学院高技术研究院 Preparation method and application of transition metal doped magnesium-aluminum layered double hydroxide material
CN115814775A (en) * 2022-11-23 2023-03-21 成都理工大学 Regeneration method of lithium-aluminum layered double hydroxide adsorbent

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