CN105944655B - A kind of iron aluminium composite material for adsorbing trivalent arsenic and its application - Google Patents

A kind of iron aluminium composite material for adsorbing trivalent arsenic and its application Download PDF

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CN105944655B
CN105944655B CN201610420731.0A CN201610420731A CN105944655B CN 105944655 B CN105944655 B CN 105944655B CN 201610420731 A CN201610420731 A CN 201610420731A CN 105944655 B CN105944655 B CN 105944655B
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iron aluminium
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mixed liquor
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CN105944655A (en
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罗琳
孟成奇
张嘉超
魏建宏
周耀宇
高军
张凤凤
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Hunan Agricultural University
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/0203—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04
    • B01J20/0225—Compounds of Fe, Ru, Os, Co, Rh, Ir, Ni, Pd, Pt
    • B01J20/0229—Compounds of Fe
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/0203—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04
    • B01J20/0248—Compounds of B, Al, Ga, In, Tl
    • 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
    • B01J20/28014—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 form
    • 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
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2220/00—Aspects relating to sorbent materials
    • B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
    • B01J2220/48—Sorbents characterised by the starting material used for their preparation
    • B01J2220/4806—Sorbents characterised by the starting material used for their preparation the starting material being of inorganic character
    • 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
    • C02F2101/103—Arsenic compounds

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Abstract

The present invention relates to a kind of composite material for adsorbing trivalent arsenic, it is prepared by the following method：1) it is 1 by the ratio between ferrous and hydrogen peroxide amount of material into green vitriol solution:0.8~1.2 adds hydrogenperoxide steam generator, and mixed solution is obtained after reaction；2) it is 1 by the ratio between amount of material of iron aluminium into the mixed solution：0.15~1.5 adds the alundum (Al2O3) after calcination, obtains iron aluminium mixed liquor；3) the iron aluminium composite material is obtained after the iron aluminium mixed liquor being carried out constant temperature oscillation, drying, grinding；The pH of the mixed solution or iron aluminium mixed liquor is adjusted to 5.5~6.5 in preparation process.The material prepared relative to bioanalysis, preparation method of the present invention is simple, and operability is stronger, is more conducive to realize industrialized production.

Description

A kind of iron aluminium composite material for adsorbing trivalent arsenic and its application
Technical field
The present invention relates to the adsorbing domain of trivalent arsenic in water, and in particular to a kind of iron aluminium composite material.
Background technology
Arsenic is not only harmful trace element, and each system organ of human body is deposited as first kind carcinogen In different degrees of harm.Compared to pentavalent arsenic, the toxicity bigger of trivalent arsenic, and it is also more difficult in processing.Common water The processing method of middle arsenic generally has the precipitation method, absorption method, oxidizing process, ion-exchange, biochemical process etc..Compared to other methods, Absorption method is widely paid close attention to due to the arsenic-containing waste water that its is simple and practicable, cost is low, the big concentration of suitable treatment water is low. Studying the more arsenic adsorbent material that removes at present mainly has metalliferous mineral, agriculture and industry waste, resinae adsorbent, the absorption of charcoal class Agent, biological adsorption agent and compound adsorbent.From the point of view of adsorption effect biological adsorption agent and metalliferous mineral material especially iron, The metalliferous mineral such as zirconium, manganese material is preferable to trivalent arsenic adsorption effect.
Early period passes through to haydite, the sour screening experiment for changing activated carbon, hydrotalcite, ferroso-ferric oxide, mineral substance synthetic material It was found that its adsorption effect to trivalent arsenic is not ideal.Find that arsenic can be by α-Al by consulting literatures2O3Very strong absorption is (such as Halter and Pfeifer (2001) Primary Study α-Al2O3Suction-operated to pentavalent arsenic).But the country is to aluminium as adsorbent The research for adsorbing trivalent arsenic is relatively fewer.Therefore, absorption of the iron aluminium composite material to trivalent arsenic is studied, to trivalent arsenic in processing water With certain research directive significance.
The content of the invention
The object of the present invention is to provide a kind of iron aluminium composite material for adsorbing trivalent arsenic in water.Iron aluminium of the present invention is answered Condensation material is prepared by the following method：
1) it is 1 by the ratio between ferrous and hydrogen peroxide amount of material into green vitriol solution:0.8~1.2 adds Enter hydrogenperoxide steam generator, mixed solution is obtained after reaction；
2) it is 1 by the ratio between amount of material of iron aluminium into the mixed solution：0.15~1.5 adds three oxidations after calcination Two aluminium, obtain iron aluminium mixed liquor；
3) the iron aluminium composite material is obtained after the iron aluminium mixed liquor being carried out constant temperature oscillation, drying, grinding；
The pH of the mixed solution or iron aluminium mixed liquor is adjusted to 5.5~6.5.
Preferably, the pH of the mixed solution is adjusted to 5.5~6.5.
The method for calcinating of the alundum (Al2O3) is that alundum (Al2O3) is calcined 1~4h at 950~1050 DEG C, crosses 80 ~120 mesh sieves.Alundum (Al2O3) is calcined under these conditions, can be increased the specific surface area of alundum (Al2O3) to greatest extent, be carried Its high absorption property.
In the process for preparation of the green vitriol solution, a certain amount of FeSO is weighed4·7H2O is dissolved in distilled water In after, low-grade fever makes it be dissolved as light green solution.
The mass concentration of the hydrogenperoxide steam generator is 25~35%.
The condition of the vibration for the iron aluminium mixed liquor at 20~30 DEG C, 120~180r/min vibrate 22~26h. Vibrated under these conditions, it can be achieved that coming into full contact with for iron and aluminium, has and utilize the good iron aluminium composite material of forming properties.
Iron aluminium composite material after grinding is crossed to the sieve of 150~200 mesh.Cross 150~200 mesh sieves composite material have compared with Big specific surface area, can both realize the abundant absorption to arsenic, and will not also influence settleability because particle is too small.
Preferably, composite material of the present invention is prepared by the following method：
1) it is 1 by the ratio between ferrous and hydrogen peroxide amount of material into green vitriol solution:1 adds peroxidating Hydrogen solution, obtains mixed solution, the pH of the mixed solution is adjusted to 6 after reaction；
2) it is 1 by the ratio between amount of material of iron aluminium into the mixed solution：0.15~0.25 adds three oxygen after calcination Change two aluminium, obtain iron aluminium mixed liquor；
3) by the iron aluminium mixed liquor at 24~26 DEG C, 140~160r/min vibrates 22~26h, then 102~ Dried at 108 DEG C to constant weight, 180 mesh sieves are crossed after grinding and obtain the iron aluminium composite material；
The method for calcinating of the alundum (Al2O3) is that alundum (Al2O3) is calcined 3~5h at 950~1050 DEG C, crosses 100 ~180 mesh sieves；
The concentration of the hydrogenperoxide steam generator is 25~35%.
Further preferably, composite material of the present invention is prepared by the following method：
1) it is 1 by the ratio between ferrous and hydrogen peroxide amount of material into green vitriol solution:1 adds peroxidating Hydrogen solution, obtains mixed solution, the pH of the mixed solution is adjusted to 6 after reaction；
2) it is 1 by the ratio between amount of material of iron aluminium into the mixed solution：0.2 adds the alundum (Al2O3) after calcination, Obtain iron aluminium mixed liquor；
3) by the iron aluminium mixed liquor at 24~26 DEG C, 140~160r/min vibrates 22~26h, then 102~ Dried at 108 DEG C to constant weight, 180 mesh sieves are crossed after grinding and obtain the iron aluminium composite material；
The method for calcinating of the alundum (Al2O3) is that alundum (Al2O3) is calcined 3~5h at 950~1050 DEG C, crosses 100 ~180 mesh sieves；
The concentration of the hydrogenperoxide steam generator is 25~35%.
The iron aluminium composite material prepared by method of the present invention, carries out X-ray diffraction, according to Prague side to it The interplanar distance d that composite material spectral line is calculated in journey is respectively 0.4641nm, 0.2777nm, 0.2638nm.Control《X-ray Diffraction identifies table》(geology bureau of Liaoning Province, 1977) understand, which shows similar with lepidocrocite (card number 412c) Phase character.Absorption of the lepidocrocite thing to arsenic is mainly shared by the bidentate angle of arsenic oxygen tetrahedron and adjacent iron oxygen octahedra Form what internal layer coordinated and realized.
It is another object of the present invention to protect application of the composite material of the present invention in terms of trivalent arsenic in adsorbing water.
Specifically, application process includes the following steps：At 15~35 DEG C, the composite material is added to pH as 6.5 In the waste water of~8.5 trivalent arsenic, 30~240min is vibrated.
Preferably, application process includes the following steps：At 25 DEG C, by the composite material be added to pH be 7~8 three In the waste water of valency arsenic, 30~240min is vibrated.
Composite material of the present invention, has the advantages that：
1) it is preferable to the adsorption effect of trivalent arsenic.Iron aluminium composite material crystal structure is more perfect, and the addition of aluminium is conducive to The formation of crystallizable mineral, combines even closer between particle.The formation of crystal structure result in the increase of average pore size, compare The reduction of area.The formation of this structure is beneficial to the increase of adsorption effect.
2) preparation method is simple.Relative to bioanalysis prepare material, the material preparation method is simple, operability compared with By force.It is more conducive to realize industrialized production.
Iron aluminium compound arsenic-removing adsorbent provided by the present invention can be used in removing the trivalent arsenic in waste water.By to compound Iron aluminum carries out X-ray diffraction, and the interplanar distance d that composite material spectral line is calculated according to Bragg equation is respectively 0.4641nm、0.2777nm、0.2638nm.Control《X-ray diffraction identifies table》(geology bureau of Liaoning Province, 1977) understands, this is multiple Condensation material shows the similar phase character with lepidocrocite (card number 412c).Absorption of the lepidocrocite thing to arsenic mainly passes through arsenic Share to form what internal layer coordinated and realized in the bidentate angle of oxygen tetrahedron and adjacent iron oxygen octahedra.
Brief description of the drawings
Fig. 1 is the compound arsenic adsorbent electron microscope of iron aluminium prepared by the present invention；
Fig. 2 is the compound arsenic adsorbent pictorial diagram of iron aluminium prepared by the present invention；
Fig. 3 is the compound arsenic adsorbent adsorption dynamics adsorption kinetics figure of iron aluminium prepared by the present invention；
The adsorption isotherm line chart of Fig. 4,5 for the compound arsenic adsorbent of iron aluminium prepared by the present invention to arsenic.
Embodiment
Following embodiments are used to illustrate the present invention, but are not limited to the scope of the present invention.
Embodiment 1
The present embodiment is related to a kind of iron aluminium composite material for adsorbing trivalent arsenic in water, is prepared by the following method：
Alundum (Al2O3) is calcined into 2h at 1000 DEG C, crosses 100 mesh sieves；
Green vitriol is dissolved in water, low-grade fever becomes light green solution；
1) it is 1 by the ratio between ferrous and hydrogen peroxide amount of material into green vitriol solution:1, which adds concentration, is 30% hydrogenperoxide steam generator, is slowly added during addition and constantly vibrates, and mixed solution is obtained after reaction, and will be described mixed The pH for closing solution is adjusted to 6；
2) it is 1 by the ratio between amount of material of iron aluminium into the mixed solution：0.2 adds the alundum (Al2O3) after calcination, Obtain iron aluminium mixed liquor；
3) the iron aluminium mixed liquor is placed in 25 DEG C, vibrates 24h on the constant temperature oscillator of 150r/min, taking-up is placed in 105 Dried in DEG C constant temperature bellows to constant weight, grind and simultaneously cross 180 mesh sieves, obtain the composite material.Its electron microscope such as Fig. 1, pictorial diagram Such as Fig. 2.
Embodiment 2
The present embodiment is related to a kind of iron aluminium composite material for adsorbing trivalent arsenic in water, is prepared by the following method：
Alundum (Al2O3) is calcined into 2h at 1000 DEG C, crosses 100 mesh sieves；
Green vitriol is dissolved in water, low-grade fever becomes light green solution；
1) it is 1 by the ratio between ferrous and hydrogen peroxide amount of material into green vitriol solution:1, which adds concentration, is 30% hydrogenperoxide steam generator, is slowly added during addition and constantly vibrates, and mixed solution is obtained after reaction, and will be described mixed The pH for closing solution is adjusted to 6；
2) it is 1 by the ratio between amount of material of iron aluminium into the mixed solution：0.5 adds the alundum (Al2O3) after calcination, Obtain iron aluminium mixed liquor；
3) the iron aluminium mixed and is placed in 25 DEG C, vibrate 24h on the constant temperature oscillator of 150r/min, taking-up is placed in 105 DEG C Dried in constant temperature bellows to constant weight, grind and cross 180 mesh sieves, obtain the composite material.
Embodiment 3
The present embodiment is related to a kind of iron aluminium composite material for adsorbing trivalent arsenic in water, is prepared by the following method：
Alundum (Al2O3) is calcined into 2h at 1000 DEG C, crosses 100 mesh sieves；
Green vitriol is dissolved in water, low-grade fever becomes light green solution；
1) it is 1 by the ratio between ferrous and hydrogen peroxide amount of material into green vitriol solution:1, which adds concentration, is 30% hydrogenperoxide steam generator, is slowly added during addition and constantly vibrates, and mixed solution is obtained after reaction, and will be described mixed The pH for closing solution is adjusted to 6；
2) it is 1 by the ratio between amount of material of iron aluminium into the mixed solution：0.8 adds the alundum (Al2O3) after calcination, Obtain iron aluminium mixed liquor；
3) the iron aluminium mixed and is placed in 25 DEG C, vibrate 24h on the constant temperature oscillator of 150r/min, taking-up is placed in 105 DEG C Dried in constant temperature bellows to constant weight, grind and cross 180 mesh sieves, obtain the composite material.
Embodiment 4
The present embodiment is related to a kind of iron aluminium composite material for adsorbing trivalent arsenic in water, is prepared by the following method：
Alundum (Al2O3) is calcined into 4h at 950 DEG C, crosses 100 mesh sieves；
Green vitriol is dissolved in water, low-grade fever becomes light green solution；
1) it is 1 by the ratio between ferrous and hydrogen peroxide amount of material into green vitriol solution:1, which adds concentration, is 25% hydrogenperoxide steam generator, is slowly added during addition and constantly vibrates, and mixed solution is obtained after reaction, and will be described mixed The pH for closing solution is adjusted to 6；
2) it is 1 by the ratio between amount of material of iron aluminium into the mixed solution：1 adds the alundum (Al2O3) after calcination, obtains Iron aluminium mixed liquor；
3) the iron aluminium mixed liquor is placed in 25 DEG C, vibrates 24h on the constant temperature oscillator of 150r/min, taking-up is placed in 105 Dried in DEG C constant temperature bellows to constant weight, grind and simultaneously cross 180 mesh sieves, obtain the composite material.
Embodiment 5
The present embodiment is related to a kind of iron aluminium composite material for adsorbing trivalent arsenic in water, is prepared by the following method：
Alundum (Al2O3) is calcined into 2h at 1000 DEG C, crosses 100 mesh sieves；
Green vitriol is dissolved in water, low-grade fever becomes light green solution；
1) it is 1 by the ratio between ferrous and hydrogen peroxide amount of material into green vitriol solution:1, which adds concentration, is 30% hydrogenperoxide steam generator, is slowly added during addition and constantly vibrates, and mixed solution is obtained after reaction, and will be described mixed The pH for closing solution is adjusted to 6；
2) it is 1 by the ratio between amount of material of iron aluminium into the mixed solution：1.5 add the alundum (Al2O3) after calcination, Obtain iron aluminium mixed liquor；
3) the iron aluminium mixed liquor is placed in 25 DEG C, vibrates 24h on the constant temperature oscillator of 150r/min, taking-up is placed in 105 Dried in DEG C constant temperature bellows to constant weight, grind and simultaneously cross 180 mesh sieves, obtain the composite material.
Embodiment 6
The present embodiment is related to a kind of iron aluminium composite material for adsorbing trivalent arsenic in water, is prepared by the following method：
Alundum (Al2O3) is calcined into 2h at 1000 DEG C, crosses 100 mesh sieves；
Green vitriol is dissolved in water, low-grade fever becomes light green solution；
1) it is 1 by the ratio between ferrous and hydrogen peroxide amount of material into green vitriol solution:1, which adds concentration, is 30% hydrogenperoxide steam generator, is slowly added during addition and constantly vibrates, and mixed solution is obtained after reaction；
2) it is 1 by the ratio between amount of material of iron aluminium into the mixed solution：0.2 adds the alundum (Al2O3) after calcination, Iron aluminium mixed liquor is obtained, and the pH of the iron aluminium mixed solution is adjusted to 6；
3) the iron aluminium mixed liquor is placed in 25 DEG C, vibrates 24h on the constant temperature oscillator of 150r/min, taking-up is placed in 105 Dried in DEG C constant temperature bellows to constant weight, grind and simultaneously cross 180 mesh sieves, obtain the composite material.
Embodiment 7
The present embodiment is related to a kind of iron aluminium composite material for adsorbing trivalent arsenic in water, is prepared by the following method：
Alundum (Al2O3) is calcined into 2h at 1000 DEG C, crosses 100 mesh sieves；
Green vitriol is dissolved in water, low-grade fever becomes light green solution；
1) it is 1 by the ratio between ferrous and hydrogen peroxide amount of material into green vitriol solution:1, which adds concentration, is 30% hydrogenperoxide steam generator, is slowly added during addition and constantly vibrates, and mixed solution is obtained after reaction；
2) it is 1 by the ratio between amount of material of iron aluminium into the mixed solution：0.5 adds the alundum (Al2O3) after calcination, Iron aluminium mixed liquor is obtained, and the pH of the iron aluminium mixed solution is adjusted to 6；
3) the iron aluminium mixed liquor is placed in 25 DEG C, vibrates 24h on the constant temperature oscillator of 150r/min, taking-up is placed in 105 Dried in DEG C constant temperature bellows to constant weight, grind and simultaneously cross 180 mesh sieves, obtain the composite material.
Embodiment 8
The present embodiment is related to a kind of iron aluminium composite material for adsorbing trivalent arsenic in water, is prepared by the following method：
Alundum (Al2O3) is calcined into 4h at 950 DEG C, crosses 80 mesh sieves；
Green vitriol is dissolved in water, low-grade fever becomes light green solution；
1) it is 1 by the ratio between ferrous and hydrogen peroxide amount of material into green vitriol solution:0.8 adds concentration For 30% hydrogenperoxide steam generator, it is slowly added during addition and constantly vibrates, mixed solution is obtained after reaction；
2) it is 1 by the ratio between amount of material of iron aluminium into the mixed solution：0.8 adds the alundum (Al2O3) after calcination, Iron aluminium mixed liquor is obtained, and the pH of the iron aluminium mixed solution is adjusted to 5.5；
3) the iron aluminium mixed and is placed in 20 DEG C, vibrate 26h on the constant temperature oscillator of 120r/min, taking-up is placed in 105 DEG C Dried in constant temperature bellows to constant weight, grind and cross 200 mesh sieves, obtain the composite material.
Embodiment 9
The present embodiment is related to a kind of iron aluminium composite material for adsorbing trivalent arsenic in water, is prepared by the following method：
Alundum (Al2O3) is calcined into 1h at 1050 DEG C, crosses 120 mesh sieves；
Green vitriol is dissolved in water, low-grade fever becomes light green solution；
1) it is 1 by the ratio between ferrous and hydrogen peroxide amount of material into green vitriol solution:1.2 add concentration For 25% hydrogenperoxide steam generator, it is slowly added during addition and constantly vibrates, mixed solution is obtained after reaction；
2) it is 1 by the ratio between amount of material of iron aluminium into the mixed solution：1 adds the alundum (Al2O3) after calcination, obtains Iron aluminium mixed liquor, and the pH of the iron aluminium mixed solution is adjusted to 6.5；
3) the iron aluminium mixed and is placed in 30 DEG C, vibrate 22h on the constant temperature oscillator of 180r/min, taking-up is placed in 105 DEG C Dried in constant temperature bellows to constant weight, grind and cross 150 mesh sieves, obtain the composite material.
Embodiment 10
The present embodiment is related to a kind of iron aluminium composite material for adsorbing trivalent arsenic in water, is prepared by the following method：
Alundum (Al2O3) is calcined into 2h at 1000 DEG C, crosses 100 mesh sieves；
Green vitriol is dissolved in water, low-grade fever becomes light green solution；
1) it is 1 by the ratio between ferrous and hydrogen peroxide amount of material into green vitriol solution:1, which adds concentration, is 30% hydrogenperoxide steam generator, is slowly added during addition and constantly vibrates, and mixed solution is obtained after reaction；
2) it is 1 by the ratio between amount of material of iron aluminium into the mixed solution：1.5 add the alundum (Al2O3) after calcination, Iron aluminium mixed liquor is obtained, and the pH of the iron aluminium mixed solution is adjusted to 6；
3) the iron aluminium mixed and is placed in 25 DEG C, vibrate 24h on the constant temperature oscillator of 150r/min, taking-up is placed in 105 DEG C Dried in constant temperature bellows to constant weight, grind and cross 180 mesh sieves, obtain the composite material.
Application examples 1：
Heavy metal adsorption experiment is carried out to the iron aluminium composite material that embodiment 1-10 is supplied, specific method is：
Material 1-10 is added to initial concentration by the iron aluminium composite material that embodiment 1~10 is stated by the solid-to-liquid ratio of 10g/L In the trivalent arsenic solution of 20mg/l, to shake 60min, rotating speed 150r/min, handling result such as table 1 at 25 DEG C.
The treatment effect of iron aluminium composite material prepared by 1 distinct methods of table to trivalent arsenic waste water
Remarks：Trivalent arsenic ion concentration is 20mg/L, volume 50mL, pH=7.0
1 fruit of table shows that embodiment 1-10 is shown has good adsorption effect to trivalent arsenic, wherein 2,4-7,9 effect Fruit is preferable, all more than 80%.Embodiment 3,10 effects are more preferable, and all 88% or so, 1 effect of embodiment is preferably 94.30%.
Application examples 2：Adsorption isotherm experiment
Application examples 2.1：
Weigh 1.319g and analyze pure As2O3In 100mL beakers, adding a certain amount of sodium hydroxide makes its dissolving, spend from Sub- water dilutes and adjusts PH=7, shifts and is settled in 1000mL volumetric flasks, simulates the water containing trivalent arsenic, the trivalent arsenic deposit Liquid concentration is 1000mg/L.
Take iron aluminium composite material in 0.5g case study on implementation 1 in equipped with 40ml difference trivalents arsenic concentration (5,10,20,50, 100th, 150,200,250 and 500mg/l) solution in.The constant temperature oscillation 60min at 15 DEG C respectively, filters and uses atomic fluorescence Remaining As (III) concentration in photometry measure filtrate.
Application examples 2.2
Compared with application examples 2.1, difference lies in the constant temperature oscillation 60min at 25 DEG C for it.Application examples 2.3
Compared with application examples 2.1, difference lies in the constant temperature oscillation 60min at 35 DEG C for it.
The experimental data of application examples 2.1~2.3 is fitted using Freundlich equations and Langmuir equations, is intended Close obtained relevant parameter (being shown in Table 2).Composite material is measured at different temperatures to the isothermal adsorption capacity of trivalent arsenic (see Fig. 4 And Fig. 5).As can be seen from the figure as the increase of solution concentration, adsorbent adsorption capacity are continuously increased, finally tend to balance, Its maximal absorptive capacity Q35℃=28.17mg/l<Q15℃=29.94mg/L<Q25℃=35.34mg/l.The trend shows temperature to multiple The adsorption effect of condensation material has a certain impact, and, at 25 DEG C, adsorption effect is optimal for it.
Table 2Langmuir and Freundlich equation model parameter
Experimental example 3：The adsorption kinetic data
Weigh 1.319g and analyze pure As2O3In 100mL beakers, adding a certain amount of sodium hydroxide makes its dissolving, spend from Sub- water dilutes and adjusts PH=7, shifts and is settled in 1000mL volumetric flasks, simulates the water containing trivalent arsenic, the trivalent arsenic deposit Liquid concentration is 1000mg/L.
Storing solution is diluted to 20mg/l, takes the iron aluminium composite material in 0.5g case study on implementation 1 in equipped with 40ml, 20mg/l Trivalent arsenic solution white plastic bottle in.Constant temperature oscillation 5,30,60,90,120,240,360min at 25 DEG C, filtering are used in combination Remaining As (III) concentration in Atomic fluorophotometry measure filtrate (adsorption dynamics adsorption kinetics relevant parameter is shown in Table 3).
Handling result is shown in Fig. 3, from figure 3, it can be seen that it is very big to the rate of adsorption of arsenic in preceding 30min composite materials, Adsorbance has 0mg/g to increase to 1.67mg/g, belongs to the fast reaction stage.Increase over time, the rate of adsorption gradually slows down And tend to balance, 30min-6h adsorbances increase to 1.75mg/g by 1.67mg/g, belong to the slow reaction stage.Hereafter absorption speed Rate remains unchanged substantially.The absorption of the composite material can be good at being fitted with second-order kinetics model, show early period three Valency arsenic is transferred to solid phase speed from liquid phase, and diffusion velocity of the later stage trivalent arsenic in solid phase is slower, when 4 is small or so Material has basically reached saturation absorption.
3 second-order kinetics fitting parameter of table
Although above the present invention is made to retouch in detail with general explanation, embodiment and experiment State, but on the basis of the present invention, it can be made some modifications or improvements, this is apparent to those skilled in the art 's.Therefore, these modifications or improvements without departing from theon the basis of the spirit of the present invention, belong to claimed Scope.

Claims (10)

1. a kind of iron aluminium composite material for adsorbing trivalent arsenic, it is characterised in that be prepared by the following method：
1) it is 1 by the ratio between ferrous and hydrogen peroxide amount of material into green vitriol solution:0.8~1.2 added Hydrogen peroxide solution, after reaction mixed solution, adjust the pH value of the mixed solution to 5.5~6.5；
2) it is 1 by the ratio between amount of material of iron aluminium into the mixed solution after adjusting pH：0.15~1.5 adds three oxygen after calcination Change two aluminium, obtain iron aluminium mixed liquor；
3) the iron aluminium composite material is obtained after the iron aluminium mixed liquor being carried out constant temperature oscillation, drying, grinding；
Or it is prepared by the following method:
1) it is 1 by the ratio between ferrous and hydrogen peroxide amount of material into green vitriol solution:0.8~1.2 added Hydrogen peroxide solution, obtains mixed solution after reaction；
2) it is 1 by the ratio between amount of material of iron aluminium into the mixed solution：0.15~1.5 adds three oxidations two after calcination Aluminium, obtains iron aluminium mixed liquor, and the pH of the iron aluminium mixed liquor is adjusted to 5.5~6.5；
3) the iron aluminium composite material is obtained after the iron aluminium mixed liquor after adjusting pH being carried out constant temperature oscillation, drying, grinding.
2. composite material according to claim 1, it is characterised in that adjust the pH of the mixed solution to 5.5~ 6.5。
3. composite material according to claim 1 or 2, it is characterised in that the method for calcinating of the alundum (Al2O3) is to incite somebody to action Alundum (Al2O3) calcines 1~4h at 950~1050 DEG C, crosses 80~120 mesh sieves.
4. composite material according to claim 1 or 2, it is characterised in that the mass concentration of the hydrogenperoxide steam generator is 25~35%.
5. composite material according to claim 4, it is characterised in that the condition of the vibration is by the iron aluminium mixed liquor At 20~30 DEG C, 120~180r/min vibrates 22~26h.
6. composite material according to claim 1 or 5, it is characterised in that the iron aluminium composite material after grinding is crossed 150~ The sieve of 200 mesh.
7. composite material according to claim 1, it is characterised in that be prepared by the following method：
1) it is 1 by the ratio between ferrous and hydrogen peroxide amount of material into green vitriol solution:1 addition hydrogen peroxide is molten Liquid, obtains mixed solution, the pH of the mixed solution is adjusted to 6 after reaction；
2) it is 1 by the ratio between amount of material of iron aluminium into the mixed solution：0.15~0.25 adds three oxidations two after calcination Aluminium, obtains iron aluminium mixed liquor；
3) by the iron aluminium mixed liquor at 24~26 DEG C, 140~160r/min vibrates 22~26h, then at 102~108 DEG C Lower drying crosses 180 mesh sieves and obtains the iron aluminium composite material to constant weight after grinding；
The method for calcinating of the alundum (Al2O3) is, alundum (Al2O3) is calcined 3~5h at 950~1050 DEG C, cross 100~ 180 mesh sieves；
The mass concentration of the hydrogenperoxide steam generator is 25~35%.
8. application of any one of claim 1~7 composite material in terms of trivalent arsenic in adsorbing water.
9. application according to claim 8, it is characterised in that include the following steps：, will be described compound at 15~35 DEG C Material is added in the aqueous solution for the trivalent arsenic that pH is 6.5~8.5, vibrates 30~300min.
10. application according to claim 8 or claim 9, it is characterised in that include the following steps：, will be described compound at 25 DEG C Material is added in the waste water for the trivalent arsenic that pH is 7~8, vibrates 30~240min.
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CN104098165A (en) * 2014-07-29 2014-10-15 徐锁龙 Preparation method and preparation equipment for composite polyiron water purifying agent

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CN104098165A (en) * 2014-07-29 2014-10-15 徐锁龙 Preparation method and preparation equipment for composite polyiron water purifying agent

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