CN107021526A - A kind of preparation and application of MnO4 intercalation layered composite metal hydroxides - Google Patents
A kind of preparation and application of MnO4 intercalation layered composite metal hydroxides Download PDFInfo
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- CN107021526A CN107021526A CN201710192214.7A CN201710192214A CN107021526A CN 107021526 A CN107021526 A CN 107021526A CN 201710192214 A CN201710192214 A CN 201710192214A CN 107021526 A CN107021526 A CN 107021526A
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- mno4
- composite metal
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- metal hydroxides
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G49/00—Compounds of iron
- C01G49/009—Compounds containing, besides iron, two or more other elements, with the exception of oxygen or hydrogen
-
- 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
-
- 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
- C02F1/72—Treatment of water, waste water, or sewage by oxidation
- C02F1/725—Treatment of water, waste water, or sewage by oxidation by catalytic oxidation
-
- 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
-
- 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
- C02F2101/30—Organic compounds
Abstract
The present invention relates to the MnO4 intercalation layered composite metal hydroxides preparation method and application for removing water pollutant, the layered composite metal hydroxides will be by that will contain Mg2+、Fe3+Solution mix and react in deionized water with sodium hydroxide and sodium carbonate liquor, aged, separation of solid and liquid, drying and calcining, then structural remodeling intercalation is carried out in permanganate solution, to be target product after obtained drying precipitate, the arsenic that the material can be used in absorption water, the organic pollution in MnO4, and then oxidative degradation water is can release during arsenic-adsorbing.Compared with prior art, the present invention has synthesized the MnO4 intercalation layered composite metal hydroxides of novelty, the material can be while arsenic in adsorbing water, synergistic oxidation organic pollution, realize and arsenic in water and the synchronous of organic pollution are removed, have the advantages that to prepare convenient, utilization ratio height, be not required to additionally add oxidant.
Description
Technical field
The present invention relates to water treatment field, and in particular to a kind of system of MnO4 intercalation layered composite metal hydroxides
It is standby with application.
Background technology
Arsenic is that the arsenic pollution in a kind of element with toxicity and carcinogenicity of generally existing in nature, drinking water source is asked
Topic is the environmental problem by global concern, at present arsenic pollution problem in the world with the presence of the big region of more than ten of country, China
It is also one of arsenic pollution more serious country.Arsenic pollution in China's some areas underground water and river is very serious, at present,
Coagulation, co-precipitation, UF membrane, absorption etc. are included to the minimizing technology of arsenic in water.Absorption method is with its economical and efficient, easy to operate etc.
Advantage is used widely in Hydraulic Projects are drunk.Meanwhile, the earth's surface and groundwater environment of many countries and regions are all received
The pollution of organic pollution materials, concentration range is ngL-1~μ gL-1, and change with geographical position and season, such as
The organic pollution such as medicine and personal care articles, incretion interferent turns into the ring that people generally face in global range in water
Border problem.More seriously, arsenic has been had been detected by many regional rivers and lake as drinking water source of China
And the combined pollution of all kinds of organic pollution formation, during this kind of water pollution control, arsenic, organic pollution will necessarily be related to
Synchronous removal problem.
Layered composite metal hydroxides (LDHs) are to pass through non-co- by positively charged main layer board and interlayer anion
The compound of the interaction assembling of valence link.Its structure is similar to shepardite Mg (OH)2, chemical composition has below formula
[M2+ 1-xM3+ x(OH)2]x+(An-)x/n·mH2O, wherein, M2+And M3+Respectively divalence and Tricationic, X are trivalent metal sun
Ion and the mol ratio of cation total amount, i.e. M3+/(M2++M3+).A is the anion of interlayer, and n is its charge number.Due to LDHs's
Interlayer anion can carry out ion exchange with extraneous anion, therefore in environmental area, available for anionic pollutant in water
Adsorption.How by layered composite metal oxide applications organic pollution it is synchronous with arsenic element combined pollution remove
Processing in, be the problem highly studied.
The content of the invention
Arsenic-adsorbing is had concurrently it is an object of the present invention to overcome the above-mentioned drawbacks of the prior art and provide one kind, is urged
Change the preparation and application of the MnO4 intercalation layered composite metal hydroxides of oxidation organic pollution ability.
The purpose of the present invention can be achieved through the following technical solutions：A kind of MnO4 intercalation layered composite metal hydrogen
Oxide, the formula of the MnO4 intercalation layered composite metal hydroxides is [Mg2+ 1-xFe3+ x(OH)2]x+(MnO4 -)x·
mH2O, wherein x=0.2~0.33.
A kind of preparation method of MnO4 intercalation layered composite metal hydroxides as described above, including following step
Suddenly：
(1) by Mg2+Salt and Fe3+Salt is dissolved in deionized water in proportion, obtains the first solution；By NaOH and Na2CO3Mixing
And be dissolved in deionized water and obtain the second solution；Permanganate is dissolved in deionized water, the 3rd solution is obtained；
(2) the first solution and the second solution are pressed into Mg2+、Fe3+Material amount sum and the second solution in NaOH thing
The ratio between amount of matter is 1：(2~4) are mixed, and stirring obtains separation of solid and liquid after slurries, ageing, and by solid sediment clean to
Neutrality, dries and calcines, obtain calcined product；
(3) calcined product is added into the 3rd solution, separation of solid and liquid is carried out after reaction, obtained solid cleaned and
Dry, produce the MnO4 intercalation layered composite metal hydroxides.
The Mg2+Salt is the nitrate of magnesium, the Fe3+Salt is the nitrate of iron, in first solution, Mg2+Concentration
For 200~800mmolL-1, Mg2+With Fe3+Molar concentration ratio be (2~4)：1.
In second solution, NaOH concentration is 500~2400mmolL-1, Na2CO3Molar concentration rate with NaOH is
0.25:1。
The permanganate is KMnO4, MnO in the 3rd solution4 -Concentration be 20~50mmolL-1。
PH value of solution is kept to be 9~11 in whipping process described in step (2), so that precipitation by metallic ion is complete.
The treatment temperature of step (2) described ageing is 80~90 DEG C, and digestion time is 18~24h, and the calcination time is
400~500 DEG C, control digestion time and temperature are in order that presoma has more preferably layer structure, 400~500 DEG C of calcinings
The laminate of presoma can be kept not collapse and the carbonate of interlayer is fully removed.
Step (3) described drying temperature is -20~-10 DEG C, the safety of drying process is fully ensured that, while also ensure that nothing
Other anion enter interlayer.
A kind of application of MnO4 intercalation layered composite metal hydroxides as described above, the MnO4 intercalation layer
Shape complex metal hydroxide is used for the synergistic oxidation degraded of the Adsorption of arsenic or organic pollution in water.
The organic pollution includes medicine soluble in water and personal care articles, incretion interferent or persistence are organic
Pollutant.
When arsenic and synergistic oxidation degradable organic pollutant that layered composite metal hydroxides are used in Adsorption water
When, described layered composite metal hydroxides are added in the water containing arsenic and organic pollution, make the inorganic dirt in water
Thing absorption is contaminated on layered composite metal hydroxides, because anion is high manganese ion between the material laminate of synthesis, tool
There is preferable ion-exchange capacity, thus the ability of absorption pollutant is stronger, and while the inorganic pollutions such as arsenic-adsorbing,
, can be with the organic pollution in synergistic oxidation water because interlayer displacement effect displaces MnO4.
Compared with prior art, beneficial effects of the present invention are embodied in following several respects：
(1) it is high to the process sensitivity of arsenic element；
(2) combined pollution of arsenic element and the formation of each type organic can be effectively removed, it is applied widely；
(3) MnO4 intercalation layered composite metal hydroxides of the invention are prepared simply, and cost is low.
Embodiment
Embodiments of the invention are elaborated below, the present embodiment is carried out lower premised on technical solution of the present invention
Implement, give detailed embodiment and specific operating process, but protection scope of the present invention is not limited to following implementations
Example.
Embodiment 1
A kind of MnO4 intercalation layered composite metal hydroxides for being used to remove water pollutant, its preparation method bag
Include following steps：
(1) 100ml the first solution is prepared, contains 200mmolL-1Mg2+And 50mmolL-1Fe3+, it is another to prepare
100ml the second solution, contains 500mmolL-1NaOH and 125mmolL-1Na2CO3, separately prepare 20mmolL-1's
Liquor potassic permanganate.
(2) the first good solution of above-mentioned configuration and the second solution are added drop-wise to the burning of the deionized water containing 100ml simultaneously
In cup, it is stirred vigorously during dropwise addition, while controlling the pH value of course of reaction to be maintained at 10, the slurries that reaction is obtained exist
It is aged 24 hours at 80 DEG C, then carries out separation of solid and liquid, obtained solid sediment is cleaned to supernatant with deionized water is in
Neutrality, is then dried at 80 DEG C, and is calcined at 400 DEG C, and obtained calcined product is added in liquor potassic permanganate and carried out
Reaction.
(3) centrifuged after reacting, and use deionized water rinsing sediment, dried at -10 DEG C, produced MnO4 and insert
Layer layered composite metal hydroxides.
The layered composite metal hydroxides prepared are used for the removal of arsenic in water, containing 1.0mgL-1Pentavalent arsenic water
Sample, the concentration of arsenic is less than 0.01mgL after material adsorption treatment-1, less than national drinking water standard limit value.
Embodiment 2
A kind of MnO4 intercalation layered composite metal hydroxides for being used to remove water pollutant, its preparation method bag
Include following steps：
(1) 100ml the first solution is prepared, contains 800mmolL-1Mg2+And 200mmolL-1Fe3+, it is another to prepare
100ml the second solution, contains 2000mmolL-1NaOH and 500mmolL-1Na2CO3, separately prepare 50mmolL-1
Liquor potassic permanganate.
(2) the first good solution of above-mentioned configuration and the second solution are added drop-wise to the burning of the deionized water containing 100ml simultaneously
In cup, it is stirred vigorously during dropwise addition, while controlling the pH value of course of reaction to be maintained at 11, the slurries that reaction is obtained exist
It is aged 18 hours at 90 DEG C, then carries out separation of solid and liquid, obtained solid sediment is cleaned to supernatant with deionized water is in
Neutrality, is then dried at 80 DEG C, and is calcined at 500 DEG C, and obtained calcined product is added in liquor potassic permanganate and carried out
Reaction.
(3) centrifuged after reacting, and use deionized water rinsing sediment, dried at -20 DEG C, produced MnO4 and insert
Layer layered composite metal hydroxides.
The layered composite metal hydroxides prepared are used for the removal of arsenic in water, containing 0.5mgL-1Pentavalent arsenic and
0.5mg·L-1The water sample of trivalent arsenic, the concentration of total arsenic is less than 0.01mgL after material adsorption treatment-1, drunk less than country
Water quality standard limit value.
Embodiment 3
A kind of MnO4 intercalation layered composite metal hydroxides for being used to remove water pollutant, its preparation method bag
Include following steps：
(1) 100ml the first solution is prepared, contains 200mmolL-1Mg2+And 100mmolL-1Fe3+, it is another to prepare
100ml the second solution, contains 600mmolL-1NaOH and 150mmolL-1Na2CO3, separately prepare 30mmolL-1's
Liquor potassic permanganate.
(2) the first good solution of above-mentioned configuration and the second solution are added drop-wise to the burning of the deionized water containing 100ml simultaneously
In cup, it is stirred vigorously during dropwise addition, while controlling the pH value of course of reaction to be maintained at 9, the slurries that reaction is obtained exist
It is aged 24 hours at 90 DEG C, then carries out separation of solid and liquid, obtained solid sediment is cleaned to supernatant with deionized water is in
Neutrality, is then dried at 80 DEG C, and is calcined at 450 DEG C, and obtained calcined product is added in liquor potassic permanganate and carried out
Reaction.
(3) centrifuged after reacting, and use deionized water rinsing sediment, dried at -10 DEG C, produced MnO4 and insert
Layer layered composite metal hydroxides.
The layered composite metal hydroxides prepared are used for the purification of arsenic-containing water, containing 0.8mgL-1Pentavalent arsenic and
0.2mg·L-1The water sample of trivalent arsenic, the concentration of total arsenic is less than 0.01mgL after material adsorption treatment-1, drunk less than country
Water quality standard limit value.
Embodiment 4
A kind of MnO4 intercalation layered composite metal hydroxides for being used to remove water pollutant, its preparation method bag
Include following steps：
(1) 100ml the first solution is prepared, contains 600mmolL-1Mg2+、150mmol·L-1Fe3+, it is another to prepare
100ml the second solution, contains 1500mmolL-1NaOH and 375mmolL-1Na2CO3, separately prepare 40mmolL-1
Liquor potassic permanganate.
(2) the first good solution of above-mentioned configuration and the second solution are added drop-wise to the burning of the deionized water containing 100ml simultaneously
In cup, it is stirred vigorously during dropwise addition, while controlling the pH value of course of reaction to be maintained at 10, the slurries that reaction is obtained exist
It is aged 24 hours at 80 DEG C, then carries out separation of solid and liquid, obtained solid sediment is cleaned to supernatant with deionized water is in
Neutrality, is then dried at 80 DEG C, and is calcined at 450 DEG C, and obtained calcined product is added in liquor potassic permanganate and carried out
Reaction.
(3) centrifuged after reacting, and use deionized water rinsing sediment, dried at -20 DEG C, produced MnO4 and insert
Layer layered composite metal hydroxides.
The layered composite metal hydroxides prepared are used for the purification containing arsenic and organic pollution water, contained
1.0mg·L-1The water sample of pentavalent arsenic and micro quantity organic pollutant, the concentration of total arsenic is less than 0.01mg after material adsorption treatment
L-1, less than national drinking water standard limit value.Simultaneously the MnO4 that can be displaced in arsenic adsorption process of organic pollution from
Sub- oxidative degradation.
Embodiment 5
A kind of MnO4 intercalation layered composite metal hydroxides for being used to remove water pollutant, its preparation method bag
Include following steps：
(1) 100ml the first solution is prepared, contains 800mmolL-1Mg2+、400mmol·L-1Fe3+, it is another to prepare
100ml the second solution, contains 2400mmolL-1NaOH and 600mmolL-1Na2CO3, separately prepare 35mmolL-1
Liquor potassic permanganate.
(2) the first good solution of above-mentioned configuration and the second solution are added drop-wise to the burning of the deionized water containing 100ml simultaneously
In cup, it is stirred vigorously during dropwise addition, while controlling the pH value of course of reaction to be maintained at 9, the slurries that reaction is obtained exist
It is aged 24 hours at 90 DEG C, then carries out separation of solid and liquid, obtained solid sediment is cleaned to supernatant with deionized water is in
Neutrality, is then dried at 80 DEG C, and is calcined at 450 DEG C, and obtained calcined product is added in liquor potassic permanganate and carried out
Reaction.
(3) centrifuged after reacting, and use deionized water rinsing sediment, dried at -10 DEG C, produced MnO4 and insert
Layer layered composite metal hydroxides.
The layered composite metal hydroxides prepared are used for the purification containing arsenic and organic pollution water, containing 1mg
L-1The water sample of pentavalent arsenic, the concentration of total arsenic is less than 0.01mgL after material adsorption treatment-1, less than national drinking water standard limit
Value, while the high manganese ion oxidative degradation that organic pollution can be displaced in arsenic adsorption process.
Embodiment 6
A kind of MnO4 intercalation layered composite metal hydroxides for being used to remove water pollutant, its preparation method bag
Include following steps：
(1) 100ml the first solution is prepared, contains 300mmolL-1Mg2+、75mmol·L-1Fe3+, it is another to prepare
100ml the second solution, contains 750mmolL-1NaOH and 187.5mmolL-1Na2CO3, separately prepare 25mmolL-1
Liquor potassic permanganate.
(2) the first good solution of above-mentioned configuration and the second solution are added drop-wise to the burning of the deionized water containing 100ml simultaneously
In cup, it is stirred vigorously during dropwise addition, while controlling the pH value of course of reaction to be maintained at 10, the slurries that reaction is obtained exist
It is aged 24 hours at 80 DEG C, then carries out separation of solid and liquid, obtained solid sediment is cleaned to supernatant with deionized water is in
Neutrality, is then dried at 80 DEG C, and is calcined at 480 DEG C, and obtained calcined product is added in liquor potassic permanganate and carried out
Reaction.
(3) centrifuged after reacting, and use deionized water rinsing sediment, dried at -15 DEG C, produced MnO4 and insert
Layer layered composite metal hydroxides.
The layered composite metal hydroxides prepared are used for the purification containing arsenic and organic pollution water, contained
0.8mg·L-1Pentavalent arsenic and 0.2mgL-1The water sample of trivalent arsenic and organic pollution, total arsenic is dense after material adsorption treatment
Degree is less than 0.01mgL-1, less than national drinking water standard limit value.Organic pollution can be replaced in arsenic adsorption process simultaneously
The high manganese ion oxidative degradation gone out.
Claims (9)
1. a kind of preparation method of MnO4 intercalation layered composite metal hydroxides, it is characterised in that methods described includes
Following steps：
(1) by Mg2+Salt and Fe3+Salt is dissolved in deionized water in proportion, obtains the first solution；By NaOH and Na2CO3Mix and molten
The second solution is obtained in deionized water；Permanganate is dissolved in deionized water, the 3rd solution is obtained；
(2) the first solution and the second solution are pressed into Mg2+、Fe3+Material amount sum and the second solution in NaOH material
The ratio between amount is 1：(2~4) are mixed, and stirring obtains separation of solid and liquid after slurries, ageing, and solid sediment is cleaned into
Property, dry and calcine, obtain calcined product；
(3) calcined product is added into the 3rd solution, separation of solid and liquid is carried out after reaction, obtained solid is cleaned and done
It is dry, produce the MnO4 intercalation layered composite metal hydroxides.
2. a kind of preparation method of MnO4 intercalation layered composite metal hydroxides according to claim 1, it is special
Levy and be, the Mg2+Salt is the nitrate of magnesium, the Fe3+In the nitrate of salt iron, first solution, Mg2+Concentration be
200~800mmolL-1, Mg2+With Fe3+Molar concentration ratio be (2~4)：1.
3. a kind of preparation method of MnO4 intercalation layered composite metal hydroxides according to claim 1, it is special
Levy and be, in second solution, NaOH concentration is 500~2400mmolL-1, Na2CO3Molar concentration rate with NaOH is
0.25:1。
4. a kind of preparation method of MnO4 intercalation layered composite metal hydroxides according to claim 1, it is special
Levy and be, the permanganate is KMnO4, MnO in the 3rd solution4 -Concentration be 20~50mmolL-1。
5. a kind of preparation method of MnO4 intercalation layered composite metal hydroxides according to claim 1, it is special
Levy and be, keep pH value of solution to be 9~11 in whipping process described in step (2).
6. a kind of preparation method of MnO4 intercalation layered composite metal hydroxides according to claim 1, it is special
Levy and be, the treatment temperature of step (2) described ageing is 80~90 DEG C, and digestion time is 18~24h, and the calcination time is
400~500 DEG C.
7. a kind of preparation method of MnO4 intercalation layered composite metal hydroxides according to claim 1, it is special
Levy and be, step (3) described drying temperature is -20~-10 DEG C.
8. a kind of MnO4 intercalation layered composite metal hydroxide obtained using such as any methods described of claim 1~7
The application of thing, it is characterised in that the MnO4 intercalation layered composite metal hydroxides are used for the absorption of arsenic element in water
Remove or the synergistic oxidation of arsenic element and organic pollution is degraded.
9. a kind of application of MnO4 intercalation layered composite metal hydroxides according to claim 8, its feature exists
In the organic pollution includes medicine soluble in water and personal care articles, incretion interferent or persistency organic contaminant
Thing.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110813257A (en) * | 2018-08-14 | 2020-02-21 | 河南工业大学 | Preparation and use method of magnetic adsorption catalytic material for synchronously removing nitrate and perchlorate in water |
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| CN1321138A (en) * | 1999-07-08 | 2001-11-07 | 水泽化学工业株式会社 | Composite polybasic salt, process for producing same, and use |
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| CN1321138A (en) * | 1999-07-08 | 2001-11-07 | 水泽化学工业株式会社 | Composite polybasic salt, process for producing same, and use |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110813257A (en) * | 2018-08-14 | 2020-02-21 | 河南工业大学 | Preparation and use method of magnetic adsorption catalytic material for synchronously removing nitrate and perchlorate in water |
| CN110813257B (en) * | 2018-08-14 | 2023-01-10 | 河南工业大学 | Preparation and use method of magnetic adsorption catalytic material for synchronously removing nitrate and perchlorate in water |
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