CN106984258A - A kind of preparation and application of hypochlorite intercalation layered composite metal hydroxides - Google Patents
A kind of preparation and application of hypochlorite intercalation layered composite metal hydroxides Download PDFInfo
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Abstract
The present invention relates to a kind of hypochlorite intercalation layered composite metal hydroxides and its preparation and application for being used to remove water pollutant, by the way that Mg will be contained2+、Fe3+、Ce3+Solution mixed in deionized water with sodium hydroxide and sodium carbonate liquor, stirring reaction, intercalation is carried out after ageing, separation of solid and liquid, drying and calcining in hypochlorite solutions, it is hypochlorite intercalation layered composite metal hydroxides after obtained drying precipitate, the material can be used for being used for the Adsorption to arsenic in water, hypochlorite is can release while arsenic-adsorbing, and then aoxidizes the organic pollution in water, kill bacterium.Compared with prior art, the present invention has synthesized the hypochlorite intercalation layered composite metal hydroxides of novelty, the material effectively absorption water in arsenic simultaneously, it can release hypochlorite, realize that the collaboration to organic pollutants, bacterium is removed, have the advantages that utilization ratio is high, be not required to additionally add oxidant, bactericide.
Description
Technical field
The present invention relates to water treatment field, and in particular to a kind of system of hypochlorite 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 hypochlorite intercalation layered composite metal hydroxides of oxidation organic pollution ability and sterilizing ability.
The purpose of the present invention can be achieved through the following technical solutions：A kind of hypochlorite intercalation layered composite metal hydrogen
Oxide, the formula of the hypochlorite intercalation layered composite metal hydroxides is [Mg2+ 0.75Fe3+ 0.25kCe3+ 0.25(1-k)
(OH)2]0.25+(ClO-)0.25·mH2O, wherein k=0.95~1.
A kind of preparation method of hypochlorite intercalation layered composite metal hydroxides as described above, methods described include with
Under several steps：
(1) by Mg2+Salt, Ce3+Salt and Fe3+Salt is dissolved in deionized water in proportion, obtains the first solution；By NaOH and
Na2CO3Mix and be dissolved in deionized water and obtain the second solution；Hypochlorite is dissolved in deionized water, the 3rd solution is obtained；
(2) the first solution and the second solution are pressed into Mg2+、Ce3+、Fe3+Material amount sum and the second solution in NaOH
The ratio between the amount of material be 1：(2~4) are mixed, and stirring obtains separation of solid and liquid after slurries, ageing, and solid sediment is clear
Neutrality is washed till, 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 hypochlorite intercalation layered composite metal hydroxides.
The Mg2+Salt is the nitrate or hydrochloride of magnesium, the Fe3+Salt is the nitrate or hydrochloride of iron, the Ce3+
Salt is Ce (NO3)3·6H2O, in first solution, Mg2+Concentration be 150~900mmolL-1, Mg2+With Fe3+And Ce3+
The ratio of total mol concentration is 3:1, Ce3+Account for Fe3+And Ce3+The 0~5% of total mol concentration.
In second solution, NaOH concentration is 400~4800mmolL-1, Na2CO3Molar concentration rate with NaOH is
0.25:1。
The hypochlorite is ClO in NaClO, the 3rd solution-Concentration be 20~100mmolL-1。
Keep pH value of solution to be 9~11 in whipping process described in step (2), can so make precipitation by metallic ion complete.
The treatment temperature of step (2) described ageing is 60~80 DEG C, and digestion time is 20~36h, 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, prevents that hypochlorite is decomposed in drying process.
A kind of application of hypochlorite intercalation layered composite metal hydroxides as described above, available for arsenic element in water
The synergistic oxidation degraded of Adsorption or arsenic element and organic pollution.
The organic pollution includes medicine soluble in water and personal care articles, incretion interferent or persistence are organic
Pollutant.
When arsenic, antimony and synergistic oxidation the degraded organic contamination that layered composite metal hydroxides are used in Adsorption water
During thing, described layered composite metal hydroxides are added in the water containing arsenic, antimony and organic pollution, make the nothing in water
Organic pollutants are adsorbed on layered composite metal hydroxides, due between the material laminate of synthesis anion be hypochlorite from
Son, with preferable ion-exchange capacity, thus the ability of absorption pollutant is stronger, and in inorganic pollutions such as arsenic-adsorbing, antimony
While thing, because interlayer displacement effect displaces hypochlorite, the organic pollution killed in water can be cooperateed with.
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 to be used to cooperate with the hypochlorite intercalation layered composite metal hydroxides for removing combined pollution in water removal, it is prepared
Method comprises the following steps：
(1) 100ml the first solution is prepared, contains 150mmolL-1Mg2+、50mmol·L-1Fe3+；It is another to prepare
100ml the second solution, contains 400mmolL-1NaOH and 100mmolL-1Na2CO3；It is another to prepare 20mmolL-1's
Liquor natrii hypochloritis.
(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 36 hours at 60 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 60 DEG C, and is calcined at 400 DEG C, and obtained calcined product is added in liquor natrii hypochloritis and carried out
Reaction.
(3) centrifuged after reacting, and use deionized water rinsing sediment, dried at -10 DEG C, produced hypochlorite 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 to be used to cooperate with the hypochlorite intercalation layered composite metal hydroxides for removing combined pollution in water removal, it is prepared
Method comprises the following steps：
(1) 100ml the first solution is prepared, contains 900mmolL-1Mg2+、285mmol·L-1Fe3+With
15mmol·L-1Ce3+, 100ml the second solution is separately prepared, contains 4800mmolL-1NaOH and 1200mmolL-1's
Na2CO3, separately prepare 100mmolL-1Liquor natrii hypochloritis.
(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 70 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 60 DEG C, and is calcined at 500 DEG C, and obtained calcined product is added in liquor natrii hypochloritis and carried out
Reaction.
(3) centrifuged after reacting, and use deionized water rinsing sediment, dried at -20 DEG C, produced hypochlorite and insert
Layer layered composite metal hydroxides.
The removal for the arsenic that the layered composite metal hydroxides prepared are used in water, containing 0.5mgL-1Pentavalent arsenic
And 0.5mgL-1The water sample of trivalent arsenic, the concentration of total arsenic is less than 0.01mgL after material adsorption treatment-1, less than country's drink
Water supply standard limit value.
Embodiment 3
A kind of to be used to cooperate with the hypochlorite intercalation layered composite metal hydroxides for removing combined pollution in water removal, it is prepared
Method comprises the following steps：
(1) 100ml the first solution is prepared, contains 300mmolL-1Mg2+、95mmol·L-1Fe3+And 5mmol
L-1Ce3+, 100ml the second solution is separately prepared, contains 800mmolL-1NaOH and 200mmolL-1Na2CO3, separately
Prepare 100mmolL-1Liquor natrii hypochloritis.
(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 20 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 60 DEG C, and is calcined at 500 DEG C, and obtained calcined product is added in liquor natrii hypochloritis and carried out
Reaction.
(3) centrifuged after reacting, and use deionized water rinsing sediment, the vacuum freeze drying at -10 DEG C is produced secondary
Chlorate anions intercalation layered composite metal hydroxides.
The layered composite metal hydroxides prepared are used for the purification containing arsenic and organic pollution water, contained
0.5mg·L-1The water sample of pentavalent 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, the oxidable organic pollution of hypochlorite discharged.
Embodiment 4
A kind of to be used to cooperate with the hypochlorite intercalation layered composite metal hydroxides for removing combined pollution in water removal, it is prepared
Method comprises the following steps：
(1) 100ml the first solution is prepared, contains 600mmolL-1Mg2+、190mmol·L-1Fe3+With
10mmol·L-1Ce3+, 100ml the second solution is separately prepared, contains 1600mmolL-1NaOH and 400mmolL-1's
Na2CO3, separately prepare 100mmolL-1Liquor natrii hypochloritis.
(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 control the pH value of course of reaction to be maintained at 10.5, the slurries that reaction is obtained
It is aged 36 hours at 70 DEG C, then carries out separation of solid and liquid, obtained solid sediment is cleaned with deionized water to supernatant
In neutrality, then dry, and calcined at 500 DEG C at 60 DEG C, obtained calcined product is added in liquor natrii hypochloritis
Row reaction.
(3) centrifuged after reacting, and use deionized water rinsing sediment, dried at -10 DEG C, produced hypochlorite and insert
Layer layered composite metal hydroxides.
By the layered composite metal hydroxides prepared be used for containing arsenic and micro quantity organic pollutant, bacterium water it is net
Change, containing 1.0mgL-1Pentavalent arsenic, micro quantity organic pollutant and the water sample of bacterium, the concentration of total arsenic is small after material adsorption treatment
In 0.01mgL-1, less than national drinking water standard limit value, the oxidable organic pollutants of hypochlorite discharged, killing
Bacterium.
Embodiment 5
A kind of to be used to cooperate with the hypochlorite intercalation layered composite metal hydroxides for removing combined pollution in water removal, it is prepared
Method comprises the following steps：
(1) 100ml the first solution is prepared, contains 450mmolL-1Mg2+、142.5mmol·L-1Fe3+With
7.5mmol·L-1Ce3+, 100ml the second solution is separately prepared, contains 1200mmolL-1NaOH and 300mmolL-1's
Na2CO3, separately prepare 100mmolL-1Liquor natrii hypochloritis.
(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 control the pH value of course of reaction to be maintained at 9.5, the slurries that reaction is obtained
It is aged 24 hours at 80 DEG C, then carries out separation of solid and liquid, obtained solid sediment is cleaned with deionized water to supernatant
In neutrality, then dry, and calcined at 500 DEG C at 60 DEG C, obtained calcined product is added in liquor natrii hypochloritis
Row reaction.
(3) centrifuged after reacting, and use deionized water rinsing sediment, dried at -10 DEG C, produced hypochlorite and insert
Layer layered composite metal hydroxides.
By the layered composite metal hydroxides prepared be used for containing arsenic and micro quantity organic pollutant, bacterium water it is net
Change, containing 0.5mgL-1Pentavalent arsenic, micro quantity organic pollutant and the water sample of bacterium, the concentration of total arsenic is small after material adsorption treatment
In 0.01mgL-1, less than national drinking water standard limit value, the oxidable organic pollutants of hypochlorite discharged, killing
Bacterium.
Embodiment 6
A kind of to be used to cooperate with the hypochlorite intercalation layered composite metal hydroxides for removing combined pollution in water removal, it is prepared
Method comprises the following steps：
(1) 100ml the first solution is prepared, contains 100mmolL-1Mg2+、285mmol·L-1Fe3+With
15mmol·L-1Ce3+, 100ml the second solution is separately prepared, contains 900mmolL-1NaOH and 900mmolL-1's
Na2CO3, separately prepare 100mmolL-1Liquor natrii hypochloritis.
(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 65 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 60 DEG C, and is calcined at 500 DEG C, and obtained calcined product is added in liquor natrii hypochloritis and carried out
Reaction.
(3) centrifuged after reacting, and use deionized water rinsing sediment, dried at -10 DEG C, produced hypochlorite and insert
Layer layered composite metal hydroxides.
By the layered composite metal hydroxides prepared be used for containing arsenic and micro quantity organic pollutant, bacterium water it is net
Change, containing 0.8mgL-1Pentavalent arsenic, micro quantity organic pollutant and the water sample of bacterium, the concentration of total arsenic is small after material adsorption treatment
In 0.01mgL-1, less than national drinking water standard limit value, the oxidable organic pollutants of hypochlorite discharged, killing
Bacterium.
Claims (9)
1. a kind of preparation method of hypochlorite intercalation layered composite metal hydroxides, it is characterised in that methods described includes
Following steps：
(1) by Mg2+Salt, Ce3+Salt and Fe3+Salt is dissolved in deionized water in proportion, obtains the first solution；By NaOH and Na2CO3It is mixed
Merging, which is dissolved in deionized water, obtains the second solution；Hypochlorite is dissolved in deionized water, the 3rd solution is obtained；
(2) the first solution and the second solution are pressed into Mg2+、Ce3+、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 is cleaned and done
It is dry, produce the hypochlorite intercalation layered composite metal hydroxides.
2. a kind of preparation method of hypochlorite intercalation layered composite metal hydroxides according to claim 1, it is special
Levy and be, the Mg2+Salt is the nitrate or hydrochloride of magnesium, the Fe3+Salt is the nitrate or hydrochloride of iron, the Ce3+
Salt is Ce (NO3)3·6H2In O, first solution, Mg2+Concentration be 150~900mmolL-1, Mg2+With Fe3+And Ce3+
The ratio of total mol concentration is 3:1, Ce3+Account for Fe3+And Ce3+The 0~5% of total mol concentration.
3. a kind of preparation method of hypochlorite intercalation layered composite metal hydroxides according to claim 1, it is special
Levy and be, in second solution, NaOH concentration is 400~4800mmolL-1, Na2CO3Molar concentration rate with NaOH is
0.25:1。
4. a kind of preparation method of hypochlorite intercalation layered composite metal hydroxides according to claim 1, it is special
Levy and be, the hypochlorite is ClO in NaClO, the 3rd solution-Concentration be 20~100mmolL-1。
5. a kind of preparation method of hypochlorite 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 hypochlorite intercalation layered composite metal hydroxides according to claim 1, it is special
Levy and be, the treatment temperature of step (2) described ageing is 60~80 DEG C, and digestion time is 20~36h, and the calcination time is
400~500 DEG C.
7. a kind of preparation method of hypochlorite 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. one kind is using the hypochlorite intercalation layered composite metal hydroxides as obtained by claim 1~7 any methods described
Application, it is characterised in that the hypochlorite intercalation layered composite metal hydroxides are used for the absorption of arsenic element in water and gone
Remove or the synergistic oxidation of arsenic element and organic pollution is degraded.
9. a kind of application of hypochlorite 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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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110078186A (en) * | 2019-05-17 | 2019-08-02 | 上海大学 | A kind of dual-functional nanometer removes the preparation method and application of algae material |
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