CN101049972A - Method for synthesizing composite hydroxide of iron and aluminum, and application - Google Patents
Method for synthesizing composite hydroxide of iron and aluminum, and application Download PDFInfo
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- CN101049972A CN101049972A CN 200710104379 CN200710104379A CN101049972A CN 101049972 A CN101049972 A CN 101049972A CN 200710104379 CN200710104379 CN 200710104379 CN 200710104379 A CN200710104379 A CN 200710104379A CN 101049972 A CN101049972 A CN 101049972A
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Abstract
This invention discloses a method for synthesizing Fe-Al composite hydroxide and its application. The method comprises: utilizing analytical pure FeCl3.6H2O and AlCl3.6H2O as the raw materials, calculating the raw material amounts according to Fe(III)/Al(III) mol ratio of (1-9):(9-1) with a total concentration of Fe(III) and Al(III) as 1 mol/L, preparing Fe(III) and Al(III) mixed solution, precipitating to obtain Fe-Al composite hydroxide, filtering, washing, drying, grinding, sieving to obtain the final product, and performing static adsorption of Fe-Al composite hydroxide to As at 25 plus and minus 1 deg.C. This invention has such advantages as low raw material cost, simple synthesis method, and simple As removal method by adsorption. The residual As concentration is decreased from 2 mg/L to lower than 0.01 mg/L after the Fe-Al composite hydroxide adsorption treatment.
Description
Technical field
The present invention relates to a kind of synthetic method and application thereof that removes arsenic adsorbent material iron aluminum complex hydroxide.
Background technology
Advantages such as the removal method to arsenic in the water mainly contains the precipitator method, coagulating sedimentation method, absorption method, ion exchange method, membrane separation process etc. both at home and abroad, and wherein absorption method is simple to operate owing to having, effect of removing arsenic good, the sorbent material kind is many receive much concern.At present, the more arsenic-removing adsorption agent of application has the ion-exchange-resin process of gac, active iron oxide compound, active aluminium oxide, slag, load and modification etc.But these arsenic-removing adsorption agent loading capacities are low, and adsorptive power is limited, fail to make the arsenic concentration of handling back arsenic-containing water sample to be lower than 0.01mgL
-1, do not reach the water quality standard for drinking water that The World Health Organization (WHO) revised in 1993.The compound material has iron carbonyl solution-montmorillonite Complex, polymerization iron carbonyl-montmorillonite Complex, column type clay ferric oxide mixture.Its main component of the sorbing material that has in these materials is an iron-aluminium oxide, and they also are the essential substance of arsenic-adsorbing, may be to have more impurity in the mineral, and these compound systems fail to make the arsenic concentration of handling back arsenic-containing water sample to be lower than 0.01mgL
-1The iron aluminium hydroxide has the ability of good adsorption zwitterion, is that the development and the application of the sorbent material of main adsorption component obtained concern both domestic and external with iron or aluminum oxide.But do not have up to now, about the report of making arsenic in the sorbent material removal water with the synthetic complex hydroxide of iron aluminium.
Summary of the invention
Purpose of the present invention is exactly low in order to overcome existing arsenic-removing adsorption agent loading capacity, the defective that adsorptive power is limited, under normal temperature condition, adopt the precipitator method, utilize analytical pure iron(ic) chloride, aluminum chloride and sodium hydroxide to prepare the iron aluminum complex hydroxide and make sorbent material and remove arsenic in the water.
The invention provides a class and remove the synthetic method of arsenic adsorbent material iron-aluminum hydroxide complex, and remove the top condition of arsenic in the tap water.Should remove arsenic adsorbent material iron aluminum complex hydroxide can not only make the arsenic concentration of handling back arsenic-containing water sample be lower than 0.01mgL
-1, and loading capacity is big.
Its detailed process of the present invention can be divided into following several stages:
1. with analytical pure FeCl
36H
2O and AlCl
36H
2O is a raw material, is guaranteeing that the iron and aluminum ions total concn is 1molL
-1Condition under, Fe (III): Al (III)=1～9 in molar ratio: 9～1 and institute's obtain solution volumeter calculate required FeCl
36H
2O and AlCl
36H
2O, preparation iron and aluminum ions mixing solutions.
2. adopt the precipitator method to prepare the iron aluminum complex hydroxide.
3. filter, washing, dry, grind, sieve, get product.
4. under (25 ± 1) ℃ condition, carry out the Static Adsorption of iron-aluminum hydroxide complex to arsenic.
Its concrete steps are:
(1) with analytical pure FeCl
36H
2O and AlCl
36H
2O is a raw material, is guaranteeing that the iron and aluminum ions total concn is 1molL
-1Condition under, Fe (III): Al (III)=1～9 in molar ratio: 9～1 calculate required FeCl
36H
2O and AlCl
36H
2O accurately takes by weighing FeCl
36H
2O and AlCl
36H
2O places small beaker, quantitatively to change 500ml volumetric flask and constant volume after the water dissolution over to scale, makes iron aluminium mixing solutions.
(2) above-mentioned mixing solutions is poured in the 2000ml beaker, under induction stirring, used 3molL earlier
-1NaOH solution is regulated between pH value to 3.0～8.0 of each reaction soln, continues stir about after 30 minutes, uses 0.1molL again
-1HNO
3Or 0.1molL
-1NaOH the pH value of solution is transferred to 7.4.Continue to stir 0.5 hour, and removed supernatant liquor after leaving standstill clarification, with the ultrapure water washing precipitate for several times after, on the vacuum filtration machine, filter and washing.Solid matter, grinds and mistake 180 mesh sieves after about 20 hours 105 ℃ of following dryings, and screen underflow matter is sealed in and promptly gets the sorbing material product in the igelite bottle.
(3) iron-aluminum hydroxide complex adopts Static Adsorption to the absorption property of arsenic.Adsorption experiment all carries out under (25 ± 1) ℃.Accurately take by weighing iron-aluminum hydroxide complex sorbent material 0.100g in a series of 100ml vinyon bottles, to regulate the pH value in advance, volume is that As (V) solution that contains of 50ml joins respectively in above-mentioned each sorbent material, build bottle cap and shake up, under room temperature, place 5 angels adsorb fully reach balance (every day with hand moving several times, about 2 minutes at every turn).In adsorption process, for the pH value that makes solution in each vinyon bottle remains in the scope of setting, available 0.1molL
-1HNO
3Solution or 0.1molL
-1NaOH solution be adjusted to designated value, a pH value was regulated in 1 hour in every interval in incipient 6 hours of absorption reaction, it is smaller to react after 6 hours the pH variation.After 5 days absorption reaction, solution is filled in the vinyl plastics test tube with 0.25 μ m filter membrane syringe filter, for the 2ml～3ml filtrate that prevents when beginning filter discard need not, filtrate is with 0.2% HNO
3Solution dilution is used to analyze wherein As (V), the content of Fe (III) and Al (III).Because the adsorptive power of iron aluminum complex hydroxide is by iron and the common decision of aluminium hydroxide.The effect of the different iron aluminum complex hydroxide arsenic-adsorbings of forming obviously is better than ironic hydroxide and aluminium hydroxide.Thereby make the arsenic concentration of handling back arsenic-containing water sample be lower than 0.01mgL
-1
The prices of raw and semifnished materials of the present invention are cheap, and synthetic method is simple, and the processing method of absorption arsenic removal is simple and convenient and easy to study, can make initial arsenic concentration less than 2mgL
-1The arsenic-containing water sample, after the compound hydroxide adsorption treatment of iron aluminium the residue arsenic concentration be lower than 0.01mgL
-1
Embodiment
Embodiment
With analytical pure FeCl
36H
2O and AlCl
36H
2O is a raw material, is guaranteeing that the iron and aluminum ions total concn is 1molL
-1Condition under, Fe (III): Al (III)=8: 2 calculates required FeCl in molar ratio
36H
2O and AlCl
36H
2The amount of O is 113.721g and 25.394g respectively.The FeCl of accurate weighing 111.424g
36H
2The AlCl of O and 24.881g
36H
2O in small beaker, quantitatively to change 500ml volumetric flask and constant volume after the water dissolution over to scale, makes iron aluminium mixing solutions.Above-mentioned mixing solutions is poured in the 2000ml beaker, under induction stirring, used 3molL earlier
-1The pH value to 5.0 of NaOH solution conditioned reaction solution continued stir about after 30 minutes, used 0.1molL again
-1HNO
3Or 0.1molL
-1NaOH the pH value of solution is transferred to 7.4.Continue to stir 0.5 hour, and removed supernatant liquor after leaving standstill clarification, with the ultrapure water washing precipitate for several times after, on the vacuum filtration machine, filter and washing.Solid matter, grinds and mistake 180 mesh sieves after about 20 hours 105 ℃ of following dryings, and screen underflow matter is sealed in and promptly gets the sorbing material product in the igelite bottle.
Iron-aluminum hydroxide complex adopts Static Adsorption to the absorption property of arsenic.Adsorption experiment all carries out under (25 ± 1) ℃.Accurately take by weighing iron-aluminum hydroxide complex sorbent material 0.100g in a 100ml vinyon bottle, will regulate the pH value in advance is 6.0, is 2mgL with As (V) concentration
-1Volume is that the solution of 50ml joins in the above-mentioned sorbent material, builds bottle cap and shakes up, under room temperature, place 5 angels adsorb fully reach balance (every day with hand moving several times, about 2 minutes at every turn).In adsorption process, for the pH value that makes solution in the vinyon bottle remains on 6.0, available 0.1molL
-1HNO
3Solution or 0.1molL
-1NaOH solution regulate, a pH value was regulated in 1 hour in every interval in incipient 6 hours of absorption reaction, it is smaller to react after 6 hours the pH variation.After 5 days absorption reaction, each solution all is filled in the 10ml vinyon test tube (2ml～3ml during beginning discard need not) with 0.25 μ m filter membrane syringe filter, draws 5ml filtrate in the 50ml volumetric flask, the HNO with 0.2%
3The solution constant volume is used to analyze wherein As (V) to scale, the content of Fe (III) and Al (III).Arsenic concentration calculates adsorption rate and the adsorptive capacity of iron-aluminum hydroxide complex to arsenic during by initial arsenic concentration and adsorption equilibrium.Because the adsorptive power of iron aluminum complex hydroxide is by iron and the common decision of aluminium hydroxide.The effect of the different iron aluminum complex hydroxide arsenic-adsorbings of forming obviously is better than ironic hydroxide and aluminium hydroxide.Thereby make the arsenic concentration of handling back arsenic-containing water sample be lower than 0.01mgL
-1
Fe (III), Al (III) use K respectively
2CrO
7With the EDTA titration measuring; The thing of iron-aluminum hydroxide complex then adopts the RIGAKU x-ray powder diffraction instrument to test with structure, diffraction angle scope 2 θ=10～60 °; Specific surface and pore structure analysis adopt U.S. NOVA 1200e specific surface determinator to measure; The pattern of sample and particle diameter adopt scanning electron microscope to observe, and the JSM-5610LV type scanning electron microscope of NEC is adopted in the Electronic Speculum test; The pH value of solution value adopts the PHS-3 type acidometer of Shanghai thunder magnetic instrument plant to measure; The mensuration of the arsenic in the solution adopts U.S. PE-AA700 Atomic Absorption Spectroscopy AAS.
Claims (2)
1. the synthetic method of an iron aluminum complex hydroxide is characterized in that the steps include:
(1) with analytical pure FeCl
36H
2O and AlCl
36H
2O is a raw material, is guaranteeing that the iron and aluminum ions total concn is 1molL
-1Condition under, Fe (III): Al (III)=1～9 in molar ratio: 9～1 calculate required FeCl
36H
2O and AlCl
36H
2O accurately takes by weighing FeCl
36H
2O and AlCl
36H
2O places small beaker, quantitatively to change 500ml volumetric flask and constant volume after the water dissolution over to scale, makes iron aluminium mixing solutions;
(2) above-mentioned mixing solutions is poured in the 2000ml beaker, under induction stirring, used 3molL earlier
-1NaOH solution is regulated the pH value of each reaction soln between the 3.0-8.0, continues stir about after 30 minutes, uses 0.1molL again
-1HNO
3Or 0.1molL
-1NaOH the pH value of solution is transferred to 7.4; Continue to stir 0.5 hour, and removed supernatant liquor after leaving standstill clarification, with the ultrapure water washing precipitate for several times after, on the vacuum filtration machine, filter and washing; Solid matter, grinds and mistake 180 mesh sieves after about 20 hours 105 ℃ of following dryings, and screen underflow matter is sealed in and promptly gets sorbing material product iron aluminum complex hydroxide in the igelite bottle.
2. the application of an iron aluminum complex hydroxide is characterized in that iron aluminum complex hydroxide that the described method of claim 1 makes can make sorbent material and remove arsenic in the water.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200710104379 CN101049972A (en) | 2007-05-10 | 2007-05-10 | Method for synthesizing composite hydroxide of iron and aluminum, and application |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200710104379 CN101049972A (en) | 2007-05-10 | 2007-05-10 | Method for synthesizing composite hydroxide of iron and aluminum, and application |
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|---|---|
| CN101049972A true CN101049972A (en) | 2007-10-10 |
Family
ID=38781610
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|---|---|---|---|
| CN 200710104379 Pending CN101049972A (en) | 2007-05-10 | 2007-05-10 | Method for synthesizing composite hydroxide of iron and aluminum, and application |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101507911B (en) * | 2008-11-11 | 2011-06-29 | 中国科学院生态环境研究中心 | Defluorination absorbing material based on aluminum base composite oxides and its preparation method and use and special device of the preparation method |
| CN104667887A (en) * | 2015-01-28 | 2015-06-03 | 中山大学 | Modified resin for removing arsenic from low-concentration arsenic-containing water and preparation method thereof |
| CN105948324A (en) * | 2016-06-23 | 2016-09-21 | 陈朝民 | Method for removing arsenic in sewage |
| CN106219707A (en) * | 2016-09-19 | 2016-12-14 | 上海城市水资源开发利用国家工程中心有限公司 | The preparation facilities of a kind of energy-efficient control aluminum control algae ferrum aluminum compound coagulant and method |
| CN111282541A (en) * | 2020-02-27 | 2020-06-16 | 清上(苏州)环境科技有限公司 | Arsenic removal composite material and preparation method thereof |
| CN115501852A (en) * | 2022-09-01 | 2022-12-23 | 广州大学 | Preparation method and application of metal-doped alumina hydrate with high adsorption performance |
-
2007
- 2007-05-10 CN CN 200710104379 patent/CN101049972A/en active Pending
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101507911B (en) * | 2008-11-11 | 2011-06-29 | 中国科学院生态环境研究中心 | Defluorination absorbing material based on aluminum base composite oxides and its preparation method and use and special device of the preparation method |
| CN104667887A (en) * | 2015-01-28 | 2015-06-03 | 中山大学 | Modified resin for removing arsenic from low-concentration arsenic-containing water and preparation method thereof |
| CN105948324A (en) * | 2016-06-23 | 2016-09-21 | 陈朝民 | Method for removing arsenic in sewage |
| CN106219707A (en) * | 2016-09-19 | 2016-12-14 | 上海城市水资源开发利用国家工程中心有限公司 | The preparation facilities of a kind of energy-efficient control aluminum control algae ferrum aluminum compound coagulant and method |
| CN106219707B (en) * | 2016-09-19 | 2023-11-14 | 上海城市水资源开发利用国家工程中心有限公司 | Preparation device and method of efficient energy-saving aluminum-control algae-control iron-aluminum composite coagulant |
| CN111282541A (en) * | 2020-02-27 | 2020-06-16 | 清上(苏州)环境科技有限公司 | Arsenic removal composite material and preparation method thereof |
| CN115501852A (en) * | 2022-09-01 | 2022-12-23 | 广州大学 | Preparation method and application of metal-doped alumina hydrate with high adsorption performance |
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