CN105170073A - Preparation method for magnetic ferro-manganese type hydrotalcite roasted material - Google Patents
Preparation method for magnetic ferro-manganese type hydrotalcite roasted material Download PDFInfo
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- CN105170073A CN105170073A CN201510611154.9A CN201510611154A CN105170073A CN 105170073 A CN105170073 A CN 105170073A CN 201510611154 A CN201510611154 A CN 201510611154A CN 105170073 A CN105170073 A CN 105170073A
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- deionized water
- magnetic
- type hydrotalcite
- ferrimanganic
- aeration
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Abstract
The invention belongs to the technical field of water treatment material preparation methods, and particularly relates to a preparation method for a magnetic ferro-manganese type hydrotalcite roasted material. The main technical problems that according to existing ferro-manganese hydrotalcite, after treatment, a water body is difficult to separate and recycle, and the cost is high are solved. When the magnetic ferro-manganese type hydrotalcite roasted material prepared through the method is used for treating arsenic-containing sewage, the maximum adsorption capacity reaches 8.7 mg/g, and excellent adsorption performance is achieved; after adsorption saturation, the magnetic ferro-manganese type hydrotalcite roasted material has high forming strength and therefore can be directly taken out to be replaced or recycled; meanwhile, adsorbent has high magnetism, in this way, even if the magnetic ferro-manganese type hydrotalcite roasted material is crashed in the using process, a magnet can be simply used for water body separation, and the effluent quality is prevented from being affected.
Description
Technical field
The invention belongs to material for water treatment preparation method technical field, be specifically related to a kind of preparation method of magnetic ferrimanganic type hydrotalcite calcining matter.
Background technology
Arsenic is the widely distributed poisonous carcinogen of one of occurring in nature, Long Term Contact and drink the contaminated arsenic water body that exceeds standard human organ can be caused to produce canceration, brings out cutaneum carcinoma, cancer of the stomach etc.China have people up to a million because water in arsenic content overproof life and produce all receive serious impact, last century there occurs the contamination accident of a lot of zonal drinking water arsenic since the eighties, therefore, the arsenic pollution problem solving drinking water is very necessary and urgent.
Current, the processing method that water body arsenic pollutes comprises bioanalysis, ion-exchange, chemical precipitation method and absorption method.Biological restoration is the method relying on microorganism and plant to reduce arsenic content in water body, the method environmental protection non-secondary pollution, but shortcoming to be reparation speed slow and excessive cycle; Ion-exchange is current study hotspot, but the too high the method that makes of the disposal cost that has high input is difficult to effectively be promoted; Chemical precipitation method method is simple and processing speed is fast, but the waste residue of precipitation is difficult to be disposed preferably, easily causes serious secondary pollution; Simple and the sorbing material of absorption method method easily obtains and reclaims, and prospect is more optimistic, but long action time, adsorption capacity difference becomes the bottleneck of its Developing Extension.In a word, the processing method that current water body arsenic pollutes all is subject to the restriction of respective not enough feature, is difficult to obtain large-scale popularization, therefore, researches and develops new arsenic process material and technology and just seems and be necessary very much.
Arsenic mainly exists with the form of arsenate in water body.Hydrotalcite is also called layered bi-metal oxide (LDH), has absorption property extremely efficiently to the anion in water body, and LDH good stability, can reuse through regeneration process, become a focus of research.Publication number is the preparation that application discloses a kind of ferromanganese type hydrotalcite calcining matter of CN103769037A and the application in the absorption of arsenic pollutant effluents thereof, this patent application with manganese salt and molysite for Material synthesis ferrimanganic hydrotalcite, and then carry out roasting, finally for the treatment of containing arsenic sewage.The sewage that the ferrimanganic type hydrotalcite process prepared in this way is polluted by arsenic is difficult to carry out water body separation and recovery after processing is completed, separating treatment is carried out by centrifugal method although also mention in patent, but the corollary equipment that this process need is extra and add a large amount of cost payouts in reality is disposed of sewage in a large number, very difficult acquisition is promoted on a large scale.
Summary of the invention
The object of the invention is to solve existing ferrimanganic hydrotalcite and deposit the high technical problem of water body difficult separation and recycling and cost after treatment, a kind of preparation method of magnetic ferrimanganic type hydrotalcite calcining matter is provided.
For solving the problems of the technologies described above, the technical solution used in the present invention is:
A preparation method for magnetic ferrimanganic type hydrotalcite calcining matter, comprises the following steps:
1) first by deionized water aeration deoxygenation 20 minutes, then by FeCl
36H
2o and FeSO
47H
2o is dissolved in the deionized water after aeration deoxygenation, continues aeration agitation until fully dissolve; Described deionized water, FeCl
36H
2o and FeSO
47H
2the mass ratio of O is 400 ︰ 2 ︰ 1;
2) to step 1) solution in drip sodium hydroxide solution that concentration is 2 ~ 4mol/L until pH value of solution is 10.5 ~ 11.5, continue aeration agitation 5 minutes obtained suspension;
3) obtained suspension is placed in dark place crystallization 36 ~ 48h;
4) remove the supernatant after crystallization, in remaining suspension liquid, add the deionized water with remaining suspension liquid after isopyknic aeration deoxygenation, ultrasonic disperse 30 minutes;
5) by MnCl
24H
2o and FeCl
36H
2make metal salt solution in deionized water after O adds aeration deoxygenation, and in metal salt solution, add the hydrochloric acid that concentration is 0.5mol/L, stir for subsequent use; Described deionized water, MnCl
24H
2o and FeCl
36H
2the mass ratio of O is 13 ︰ 2.0 ~ 2.5 ︰ 1, and described concentration is the consumption of the hydrochloric acid of 0.5mol/L is 0.05% of metal salt solution volume;
6) by NaOH and Na
2cO
3add in the deionized water after aeration deoxygenation, make aqueous slkali for subsequent use; Described deionized water, NaOH and Na
2cO
3mass ratio be 10.5 ~ 11.0 ︰ 1.13 ︰ 1;
7) by step 4) water-bath that is placed in 60 DEG C of obtained suspension heats, under stirring, step 5 is added in suspension) obtained metal salt solution and step 6) obtained aqueous slkali, control pH of suspension in the scope of 10.5 ~ 11.5 by regulating rate of addition; Described metal salt solution is identical with the addition of aqueous slkali, and addition is step 1) in 0.5 times of deionized water addition; At the temperature of 60 DEG C, continue stirring 10 minutes after being added dropwise to complete, then bath temperature is heated to 80 DEG C, continue to stir 48h at the temperature of 80 DEG C;
8) by step 7) obtained reactant liquor carries out repeated centrifugation, washes twice, dry, grinding, obtains magnetic ferrimanganic type hydrotalcite;
9) by obtained magnetic ferrimanganic type hydrotalcite and Al
2o
3evenly obtained slurry is for subsequent use to add deionized water for stirring, described deionized water, magnetic ferrimanganic type hydrotalcite and Al
2o
3mass ratio be 4 ︰ 2 ~ 2.5 ︰ 1;
10) use mould that obtained slurry is made the spheric granules that diameter is 2 ~ 3mm, spheric granules is placed in Muffle furnace, at the temperature lower calcination 4 ~ 5h of 400 ~ 450 DEG C, namely obtains magnetic ferrimanganic type hydrotalcite calcining matter.
The magnetic ferrimanganic type hydrotalcite calcining matter process adopting the present invention to prepare reaches 8.7mg/g containing the maximum adsorption capacity of arsenic sewage, shows excellent absorption property.Do arsenic removal experiment with the former high-arsenic underground water (Co=370ug/L) getting arsenic content standard (10ug/L) 37 times, 40min can make the arsenic content of underground water decline 91.6%, has treatment effeciency fast.React initial pH to have between 2-12 and excellent go arsenic ability, have good treatment effect to general water body.Reach absorption saturated after magnetic ferrimanganic type hydrotalcite calcining matter because its there is higher shaping strength, therefore can directly take out change reclaim.Magnetic ferrimanganic type hydrotalcite calcining matter arsenic removal efficiency after regeneration is good, and Repeatability reaches 72.6%, has higher reusing.This adsorbent has stronger magnetic simultaneously, even if the use procedure of magnetic ferrimanganic type hydrotalcite calcining matter occurs broken, magnet also can be utilized simply to carry out water body separation, avoid effluent quality to be affected.Therefore, compared with background technology, the present invention has that preparation technology is simple, arsenic removal efficiency is high, cost is low, shaping strength is high, it is strong compared with ferromagnetism, repeatability to have, adsorb and saturatedly easily change the advantage reclaiming and can carry out regeneration, environmental protection and non-secondary pollution afterwards.
Detailed description of the invention
Embodiment 1
The preparation method of a kind of magnetic ferrimanganic type hydrotalcite calcining matter in the present embodiment, comprises the following steps:
1) first by deionized water aeration deoxygenation 20 minutes, then by the FeCl of 2.50g
36H
2the FeSO of O and 1.25g
47H
2o is dissolved in the deionized water after the aeration deoxygenation of 500ml, continues aeration agitation until fully dissolve;
2) to step 1) solution in drip sodium hydroxide solution that concentration is 2mol/L until pH is 10.5, continue aeration agitation 5 minutes obtained suspension;
3) obtained suspension is placed in dark place crystallization 36h;
4) remove the supernatant after crystallization, in remaining suspension liquid, add the deionized water with remaining suspension liquid after isopyknic aeration deoxygenation, ultrasonic disperse 30 minutes;
5) by the MnCl of 38.46g
24H
2the FeCl of O and 19.23g
36H
2make metal salt solution in deionized water after O joins the aeration deoxygenation of 250ml, and the concentration adding 0.13ml in metal salt solution is the hydrochloric acid of 0.5mol/L, stirs for subsequent use;
6) by the Na of NaOH and 23.81g of 26.9g
2cO
3join in the deionized water after the aeration deoxygenation of 250ml, make aqueous slkali for subsequent use;
7) by step 4) water-bath that is placed in 60 DEG C of obtained suspension heats, under stirring, step 5 is added in suspension) obtained metal salt solution and step 6) obtained aqueous slkali, control pH of suspension in the scope of 10.5 ~ 11.5 by regulating rate of addition; Metal salt solution is identical with the addition of aqueous slkali, is 250ml; At the temperature of 60 DEG C, continue stirring 10 minutes after being added dropwise to complete, then bath temperature is heated to 80 DEG C, continue to stir 48h at the temperature of 80 DEG C;
8) by step 7) obtained reactant liquor carries out repeated centrifugation, washes twice, dry, grinding, obtains magnetic ferrimanganic type hydrotalcite;
9) by the obtained magnetic ferrimanganic type hydrotalcite of 30g and the Al of 15g
2o
3the deionized water for stirring adding 60ml evenly obtained slurry is for subsequent use;
10) use mould that obtained slurry is made the spheric granules that diameter is 2 ~ 3mm, spheric granules is placed in Muffle furnace, at the temperature lower calcination 4h of 400 DEG C, namely obtains magnetic ferrimanganic type hydrotalcite calcining matter.
Embodiment 2
The preparation method of a kind of magnetic ferrimanganic type hydrotalcite calcining matter in the present embodiment, comprises the following steps:
1) first by deionized water aeration deoxygenation 20 minutes, then by the FeCl of 2.50g
36H
2the FeSO of O and 1.25g
47H
2o is dissolved in the deionized water after the aeration deoxygenation of 500ml, continues aeration agitation until fully dissolve;
2) to step 1) solution in drip sodium hydroxide solution that concentration is 4mol/L until pH value of solution is 11, continue aeration agitation 5 minutes obtained suspension;
3) obtained suspension is placed in dark place crystallization 48h;
4) remove the supernatant after crystallization, in remaining suspension liquid, add the deionized water with remaining suspension liquid after isopyknic aeration deoxygenation, ultrasonic disperse 30 minutes;
5) by the MnCl of 43.77g
24H
2the FeCl of O and 19.23g
36H
2make metal salt solution in deionized water after O adds the aeration deoxygenation of 250ml, and the concentration adding 0.13ml in metal salt solution is the hydrochloric acid of 0.5mol/L, stirs for subsequent use;
6) by the Na of NaOH and 23.26g of 26.18g
2cO
3add in the deionized water after the aeration deoxygenation of 250ml, make aqueous slkali for subsequent use;
7) by step 4) water-bath that is placed in 60 DEG C of obtained suspension heats, under stirring, step 5 is added in suspension) obtained metal salt solution and step 6) obtained aqueous slkali, control pH of suspension in the scope of 10.5 ~ 11.5 by regulating rate of addition; Metal salt solution is identical with the addition of aqueous slkali, is 250ml; At the temperature of 60 DEG C, continue stirring 10 minutes after being added dropwise to complete, then bath temperature is heated to 80 DEG C, continue to stir 48h at the temperature of 80 DEG C;
8) by step 7) obtained reactant liquor carries out repeated centrifugation, washes twice, dry, grinding, obtains magnetic ferrimanganic type hydrotalcite;
9) by the obtained magnetic ferrimanganic type hydrotalcite of 33.75g and the Al of 15g
2o
3the deionized water for stirring adding 60ml evenly obtained slurry is for subsequent use;
10) use mould that obtained slurry is made the spheric granules that diameter is 2 ~ 3mm, spheric granules is placed in Muffle furnace, at the temperature lower calcination 5h of 450 DEG C, namely obtains magnetic ferrimanganic type hydrotalcite calcining matter.
Embodiment 3
The preparation method of a kind of magnetic ferrimanganic type hydrotalcite calcining matter in the present embodiment, comprises the following steps:
1) first by deionized water aeration deoxygenation 20 minutes, then by the FeCl of 2.5g
36H
2the FeSO of O and 1.25g
47H
2o is dissolved in the deionized water after the aeration deoxygenation of 500ml, continues aeration agitation until fully dissolve;
2) to step 1) solution in drip sodium hydroxide solution that concentration is 3mol/L until pH value of solution is 11.5, continue aeration agitation 5 minutes obtained suspension;
3) obtained suspension is placed in dark place crystallization 40h;
4) remove the supernatant after crystallization, in remaining suspension liquid, add the deionized water with remaining suspension liquid after isopyknic aeration deoxygenation, ultrasonic disperse 30 minutes;
5) by the MnCl of 48.08g
24H
2the FeCl of O and 19.23g
36H
2make metal salt solution in deionized water after O joins the aeration deoxygenation of 250ml, and the concentration adding 0.13ml in metal salt solution is the hydrochloric acid of 0.5mol/L, stirs for subsequent use;
6) by the Na of NaOH and 22.72g of 25.68g
2cO
3join in the deionized water after the aeration deoxygenation of 250ml, make aqueous slkali for subsequent use;
7) by step 4) water-bath that is placed in 60 DEG C of obtained suspension heats, under stirring, step 5 is added in suspension) obtained metal salt solution and step 6) obtained aqueous slkali, control pH of suspension in the scope of 10.5 ~ 11.5 by regulating rate of addition; Metal salt solution is identical with the addition of aqueous slkali, is 250ml; At the temperature of 60 DEG C, continue stirring 10 minutes after being added dropwise to complete, then bath temperature is heated to 80 DEG C, continue to stir 48h at the temperature of 80 DEG C;
8) by step 7) obtained reactant liquor carries out repeated centrifugation, washes twice, dry, grinding, obtains magnetic ferrimanganic type hydrotalcite;
9) by the obtained magnetic ferrimanganic type hydrotalcite of 37.5g and the Al of 15g
2o
3the deionized water for stirring adding 60ml evenly obtained slurry is for subsequent use;
10) use mould that obtained slurry is made the spheric granules that diameter is 2 ~ 3mm, spheric granules is placed in Muffle furnace, at the temperature lower calcination 4.5h of 420 DEG C, namely obtains magnetic ferrimanganic type hydrotalcite calcining matter.
Using method of the present invention is: add a certain amount of magnetic ferrimanganic type hydrotalcite calcining matter to containing in As groundwater, and slowly after vibration a period of time, centrifugation, measures the arsenic concentration in solution;
Wherein, the concentration of arsenic adopts By Hydride Generation Atomic Absorption Spectrometry spectrophotometer (HG-AAS).
Fe
3o
4the computing formula of-Mn-FeLDO to the adsorption rate of arsenic from underwater is as follows:
R(％)＝(1-Ct/Co)╳100
Wherein R is adsorption rate, and Co is the initial concentration of arsenic from underwater, and Ct is the residual concentration of reaction t time, and unit is ug/L.
Reclaim after process and reach the saturated magnetic ferrimanganic type hydrotalcite calcining matter of absorption, immersion desorb 2h is carried out by the alkaline NaOH solution that concentration is 0.3mol/L, use deionized water soaking and washing again, under 80 DEG C of conditions after dry 16 hours at 450 DEG C of temperature lower calcination 4h, finally obtain regeneration magnetic ferrimanganic type hydrotalcite calcining matter, with the process of regeneration magnetic ferrimanganic type hydrotalcite calcining matter containing As groundwater.
Claims (1)
1. a preparation method for magnetic ferrimanganic type hydrotalcite calcining matter, is characterized in that: comprise the following steps:
1) first by deionized water aeration deoxygenation 20 minutes, then by FeCl
36H
2o and FeSO
47H
2o is dissolved in the deionized water after aeration deoxygenation, continues aeration agitation until fully dissolve; Described deionized water, FeCl
36H
2o and FeSO
47H
2the mass ratio of O is 400 ︰ 2 ︰ 1;
2) to step 1) solution in drip sodium hydroxide solution that concentration is 2 ~ 4mol/L until pH value of solution is 10.5 ~ 11.5, continue aeration agitation 5 minutes obtained suspension;
3) obtained suspension is placed in dark place crystallization 36 ~ 48h;
4) remove the supernatant after crystallization, in remaining suspension liquid, add the deionized water with remaining suspension liquid after isopyknic aeration deoxygenation, ultrasonic disperse 30 minutes;
5) by MnCl
24H
2o and FeCl
36H
2make metal salt solution in deionized water after O adds aeration deoxygenation, and in metal salt solution, add the hydrochloric acid that concentration is 0.5mol/L, stir for subsequent use; Described deionized water, MnCl
24H
2o and FeCl
36H
2the mass ratio of O is 13 ︰ 2.0 ~ 2.5 ︰ 1, and described concentration is the consumption of the hydrochloric acid of 0.5mol/L is 0.05% of metal salt solution volume;
6) by NaOH and Na
2cO
3add in the deionized water after aeration deoxygenation, make aqueous slkali for subsequent use; Described deionized water, NaOH and Na
2cO
3mass ratio be 10.5 ~ 11.0 ︰ 1.13 ︰ 1;
7) by step 4) water-bath that is placed in 60 DEG C of obtained suspension heats, under stirring, step 5 is added in suspension) obtained metal salt solution and step 6) obtained aqueous slkali, control pH of suspension in the scope of 10.5 ~ 11.5 by regulating rate of addition; Described metal salt solution is identical with the addition of aqueous slkali, and addition is step 1) in 0.5 times of deionized water addition; At the temperature of 60 DEG C, continue stirring 10 minutes after being added dropwise to complete, then bath temperature is heated to 80 DEG C, continue to stir 48h at the temperature of 80 DEG C;
8) by step 7) obtained reactant liquor carries out repeated centrifugation, washes twice, dry, grinding, obtains magnetic ferrimanganic type hydrotalcite;
9) by obtained magnetic ferrimanganic type hydrotalcite and Al
2o
3evenly obtained slurry is for subsequent use to add deionized water for stirring, described deionized water, magnetic ferrimanganic type hydrotalcite and Al
2o
3mass ratio be 4 ︰ 2 ~ 2.5 ︰ 1;
10) use mould that obtained slurry is made the spheric granules that diameter is 2 ~ 3mm, spheric granules is placed in Muffle furnace, at the temperature lower calcination 4 ~ 5h of 400 ~ 450 DEG C, namely obtains magnetic ferrimanganic type hydrotalcite calcining matter.
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|---|---|---|---|
| CN201510611154.9A CN105170073A (en) | 2015-09-23 | 2015-09-23 | Preparation method for magnetic ferro-manganese type hydrotalcite roasted material |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105948085A (en) * | 2016-04-21 | 2016-09-21 | 巢湖学院 | Preparation method of magnetic hydrotalcite |
| CN106669681A (en) * | 2016-12-14 | 2017-05-17 | 华南理工大学 | Ni/Cu/Al/Fe hydrotalcite precursor catalyst with magnetism and preparation method and application thereof |
| CN110252304A (en) * | 2018-03-12 | 2019-09-20 | 中国石油化工股份有限公司 | Fe-series catalyst and its preparation method and application and carbon nanotube and preparation method thereof |
| CN111003776A (en) * | 2019-12-30 | 2020-04-14 | 昆明理工大学 | Method for treating nonferrous smelting arsenic-containing wastewater by using ferromanganese ore |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101422719A (en) * | 2008-11-24 | 2009-05-06 | 哈尔滨工程大学 | Magnetic composite oxides preparation method and use of magnetic composite oxides as anionic pollutant absorbent |
| US20130260990A1 (en) * | 2012-03-28 | 2013-10-03 | Samsung Electronics Co., Ltd. | Adsorbent for carbon dioxide, method of preparing the same, and capture module for carbon dioxide including the same |
| CN103769037A (en) * | 2014-02-27 | 2014-05-07 | 南京农业大学 | Preparation method of roasted ferro-manganese hydrotalcite and application of roasted ferro-manganese hydrotalcite in adsorption of arsenic-polluted wastewater |
-
2015
- 2015-09-23 CN CN201510611154.9A patent/CN105170073A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101422719A (en) * | 2008-11-24 | 2009-05-06 | 哈尔滨工程大学 | Magnetic composite oxides preparation method and use of magnetic composite oxides as anionic pollutant absorbent |
| US20130260990A1 (en) * | 2012-03-28 | 2013-10-03 | Samsung Electronics Co., Ltd. | Adsorbent for carbon dioxide, method of preparing the same, and capture module for carbon dioxide including the same |
| CN103769037A (en) * | 2014-02-27 | 2014-05-07 | 南京农业大学 | Preparation method of roasted ferro-manganese hydrotalcite and application of roasted ferro-manganese hydrotalcite in adsorption of arsenic-polluted wastewater |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105948085A (en) * | 2016-04-21 | 2016-09-21 | 巢湖学院 | Preparation method of magnetic hydrotalcite |
| CN106669681A (en) * | 2016-12-14 | 2017-05-17 | 华南理工大学 | Ni/Cu/Al/Fe hydrotalcite precursor catalyst with magnetism and preparation method and application thereof |
| CN110252304A (en) * | 2018-03-12 | 2019-09-20 | 中国石油化工股份有限公司 | Fe-series catalyst and its preparation method and application and carbon nanotube and preparation method thereof |
| CN110252304B (en) * | 2018-03-12 | 2021-12-17 | 中国石油化工股份有限公司 | Iron-based catalyst, preparation method and application thereof, carbon nano tube and preparation method thereof |
| CN111003776A (en) * | 2019-12-30 | 2020-04-14 | 昆明理工大学 | Method for treating nonferrous smelting arsenic-containing wastewater by using ferromanganese ore |
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