CN106984258B - Preparation and application of hypochlorite intercalation layered composite metal hydroxide - Google Patents

Preparation and application of hypochlorite intercalation layered composite metal hydroxide Download PDF

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CN106984258B
CN106984258B CN201710192205.8A CN201710192205A CN106984258B CN 106984258 B CN106984258 B CN 106984258B CN 201710192205 A CN201710192205 A CN 201710192205A CN 106984258 B CN106984258 B CN 106984258B
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芦洪涛
隋铭皓
朱志良
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Tongji University
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Abstract

The invention relates to hypochlorite intercalation layered composite metal hydroxide for removing pollutants in water, and preparation and application thereof2+、Fe3+、Ce3+The solution is mixed with sodium hydroxide and sodium carbonate solution in deionized water, and then the mixture is stirred for reaction, aged, subjected to solid-liquid separation, dried and calcined, and then subjected to intercalation reaction in hypochlorite solution, and the obtained precipitate is dried to obtain hypochlorite intercalation layered composite metal hydroxide. Compared with the prior art, the novel hypochlorite intercalation layered composite metal hydroxide is synthesized, the material can release hypochlorite while effectively adsorbing arsenic in water, realizes the synergistic removal of organic pollutants and bacteria in water, and has the advantages of high utilization efficiency, no need of adding an oxidant or a bactericide additionally and the like.

Description

Preparation and application of hypochlorite intercalation layered composite metal hydroxide
Technical Field
The invention relates to the field of water treatment, in particular to preparation and application of hypochlorite intercalation layered composite metal hydroxide.
Background
Arsenic is a toxic and carcinogenic element commonly existing in nature, the problem of arsenic pollution in drinking water sources is an environmental problem which is concerned by the world, the problem of arsenic pollution in large areas exists in more than ten countries in the world at present, and China is also one of the countries with serious arsenic pollution. Arsenic pollution in underground water and rivers in partial areas of China is very serious, and currently, methods for removing arsenic in water comprise coagulation, coprecipitation, membrane separation, adsorption and the like. Adsorption process in its economyHigh efficiency, convenient operation and the like, and is widely applied to drinking water engineering. Meanwhile, the surface and underground water environments of many countries and regions are polluted by organic pollutants, and the concentration range is ng.L-1～μg·L-1And varies with geographical location and season, organic pollutants such as aquatic drugs and personal care products, endocrine disruptors, etc. have become environmental problems commonly faced by people worldwide. More seriously, the composite pollution formed by arsenic and various organic pollutants is detected in rivers and lakes as drinking water sources in many areas of China, and the problem of synchronous removal of the arsenic and the organic pollutants is inevitably involved in the treatment process of the water pollution.
Layered Double Hydroxides (LDHs) are compounds assembled from positively charged host sheets and interlayer anions by non-covalent interactions. The structure is similar to brucite Mg (OH)2The chemical composition has the following general formula [ M2+ 1-xM3+ x(OH)2]x+(An-)x/n·mH2O, wherein M2+And M3+Respectively divalent and trivalent cations, X being the molar ratio of the trivalent metal cation to the total amount of cations, i.e. M3+/(M2++M3+). A is the anion between the layers and n is the number of charges. Because interlayer anions of the LDHs can be subjected to ion exchange with external anions, the LDHs can be used for adsorbing and removing anionic pollutants in water in the environmental field. How to apply the layered composite metal oxide to the treatment of synchronously removing the organic pollutants and the arsenic element composite pollutants is a very important topic to be researched.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide the preparation and application of the hypochlorite intercalation layered composite metal hydroxide with arsenic adsorption, organic pollutant catalytic oxidation and sterilization capabilities.
The purpose of the invention can be realized by the following technical scheme: hypochlorite intercalation layered composite metal hydroxide, the hypochloriteThe general formula of the intercalation layered composite metal hydroxide is [ Mg2+ 0.75Fe3+ 0.25kCe3+ 0.25(1-k)(OH)2]0.25+(ClO-)0.25·mH2And O, wherein k is 0.95-1.
A method for preparing hypochlorite intercalated layered composite metal hydroxide as described above, comprising the steps of:
(1) mixing Mg2+Salt, Ce3+Salt and Fe3+Dissolving salt in deionized water according to a certain proportion to obtain a first solution; mixing NaOH and Na2CO3Mixing and dissolving in deionized water to obtain a second solution; dissolving hypochlorite in deionized water to obtain a third solution;
(2) mixing the first solution and the second solution as Mg2+、Ce3+、Fe3+The ratio of the sum of the amounts of substances of (a) to the amount of substance of NaOH in the second solution is 1: (2-4) mixing, stirring to obtain slurry, aging, performing solid-liquid separation, cleaning a solid precipitate to be neutral, drying and calcining to obtain a calcined product;
(3) and adding the calcined product into the third solution, carrying out solid-liquid separation after reaction, and cleaning and drying the obtained solid to obtain the hypochlorite intercalation layered composite metal hydroxide.
The Mg2+The salt is nitrate or hydrochloride of magnesium, and the Fe3+The salt is nitrate or hydrochloride of iron, and the Ce3+ salt is Ce (NO)3)3·6H2O, in the first solution, Mg2+Has a concentration of 150 to 900 mmol.L-1，Mg2+With Fe3+And Ce3+The ratio of the total molar concentration is 3:1, Ce3+Is Fe3+And Ce3+0-5% of the total molar concentration.
In the second solution, the concentration of NaOH is 400-4800 mmol.L-1，Na2CO3The molar concentration ratio to NaOH was 0.25: 1.
The hypochlorite is NaClO, and ClO in the third solution-Has a concentration of 20 to 100 mmol.L-1。
And (3) in the stirring process in the step (2), the pH value of the solution is kept to be 9-11, so that metal ions can be completely precipitated.
And (2) aging at the temperature of 60-80 ℃ for 20-36 h, calcining at the temperature of 400-500 ℃, controlling the aging time and the temperature so as to enable the precursor to have a better layered structure, and calcining at the temperature of 400-500 ℃ to ensure that a laminate of the precursor does not collapse and carbonate radicals between layers can be sufficiently removed.
The drying temperature in the step (3) is-20 to-10 ℃, and hypochlorite decomposition is prevented in the drying process.
The application of the hypochlorite intercalation layered composite metal hydroxide can be used for adsorption removal of arsenic element in water or synergistic oxidation degradation of the arsenic element and organic pollutants.
The organic contaminants include drugs and personal care products, endocrine disruptors, or persistent organic contaminants dissolved in water.
When the layered composite metal hydroxide is used for adsorbing and removing arsenic and antimony in water and synergistically oxidizing and degrading organic pollutants, the layered composite metal hydroxide is added into water containing arsenic, antimony and organic pollutants, so that inorganic pollutants in the water are adsorbed on the layered composite metal hydroxide, and the synthesized interlayer anions of the material layers are hypochlorite ions and have better ion exchange capacity, so that the capacity of adsorbing the pollutants is stronger, and the hypochlorite is replaced by the interlayer replacement effect while the inorganic pollutants such as arsenic and antimony are adsorbed, so that the organic pollutants in the water can be synergistically killed.
Compared with the prior art, the beneficial effects of the invention are embodied in the following aspects:
(1) the treatment sensitivity to arsenic element is high;
(2) can effectively remove the composite pollution formed by arsenic element and various organic matters, and has wide application range;
(3) the permanganate intercalation layered composite metal hydroxide is simple to prepare and low in cost.
Detailed Description
The following examples are given for the detailed implementation and specific operation of the present invention, but the scope of the present invention is not limited to the following examples.
Example 1
A hypochlorite intercalation layered composite metal hydroxide for synergistically removing composite pollution in water is prepared by the following steps:
(1) 100ml of a first solution containing 150 mmol. multidot.L of-1Mg of (2)2+、50mmol·L-1Fe (b) of3+(ii) a 100ml of a second solution containing 400 mmol. L was prepared-1NaOH and 100 mmol. multidot.L-1Na of (2)2CO3(ii) a Separately, 20 mmol. L of a surfactant was prepared-1Sodium hypochlorite solution of (2).
(2) And (2) simultaneously dropwise adding the prepared first solution and second solution into a beaker containing 100ml of deionized water, violently stirring in the dropwise adding process, simultaneously controlling the pH value in the reaction process to be kept at 9, aging the slurry obtained by the reaction at 60 ℃ for 36 hours, then carrying out solid-liquid separation, washing the obtained solid precipitate with deionized water until the supernatant is neutral, then drying at 60 ℃, calcining at 400 ℃, and adding the obtained calcined product into a sodium hypochlorite solution for reaction.
(3) And after the reaction, centrifugally separating, washing the precipitate with deionized water, and drying at the temperature of minus 10 ℃ to obtain the hypochlorite intercalation layered composite metal hydroxide.
The prepared layered composite metal hydroxide is used for removing arsenic in water and contains 1.0 mg.L-1The concentration of arsenic after the material adsorption treatment of a pentavalent arsenic water sample is less than 0.01 mg.L-1And is lower than the national drinking water standard limit.
Example 2
A hypochlorite intercalation layered composite metal hydroxide for synergistically removing composite pollution in water is prepared by the following steps:
(1) 100ml of a first solution containing 900 mmol. multidot.L was prepared-1Mg of (2)2+、285mmol·L-1Fe (b) of3+And 15 mmol. L-1Ce of (1)3+And preparing 100ml of a second solution containing 4800 mmol.L-1NaOH and 1200 mmol. multidot.L-1Na of (2)2CO3Separately preparing 100 mmol.L-1Sodium hypochlorite solution of (2).
(2) And (2) simultaneously dropwise adding the prepared first solution and second solution into a beaker containing 100ml of deionized water, violently stirring in the dropwise adding process, simultaneously controlling the pH value in the reaction process to be kept at 10, aging the slurry obtained by the reaction at 70 ℃ for 24 hours, then carrying out solid-liquid separation, washing the obtained solid precipitate with deionized water until the supernatant is neutral, then drying at 60 ℃, calcining at 500 ℃, and adding the obtained calcined product into a sodium hypochlorite solution for reaction.
(3) And after the reaction, centrifugally separating, washing the precipitate with deionized water, and drying at the temperature of minus 20 ℃ to obtain the hypochlorite intercalation layered composite metal hydroxide.
The prepared layered composite metal hydroxide is used for removing arsenic in water and contains 0.5 mg.L-1Pentavalent arsenic and 0.5 mg.L-1The concentration of total arsenic of a trivalent arsenic water sample after material adsorption treatment is less than 0.01 mg.L-1And is lower than the national drinking water standard limit.
Example 3
A hypochlorite intercalation layered composite metal hydroxide for synergistically removing composite pollution in water is prepared by the following steps:
(1) 100ml of a first solution containing 300 mmol. L of-1Mg of (2)2+、95mmol·L-1Fe (b) of3+And 5 mmol. L-1Ce of (1)3+And preparing 100ml of a second solution containing 800 mmol.L-1NaOH and 200 mmol. multidot.L-1Na of (2)2CO3Separately preparing 100 mmol.L-1Sodium hypochlorite solution of (2).
(2) And (2) simultaneously dropwise adding the prepared first solution and second solution into a beaker containing 100ml of deionized water, violently stirring in the dropwise adding process, simultaneously controlling the pH value in the reaction process to be kept at 11, aging the slurry obtained by the reaction at 80 ℃ for 20 hours, then carrying out solid-liquid separation, washing the obtained solid precipitate with deionized water until the supernatant is neutral, then drying at 60 ℃, calcining at 500 ℃, and adding the obtained calcined product into a sodium hypochlorite solution for reaction.
(3) And after the reaction, centrifugally separating, washing the precipitate with deionized water, and carrying out vacuum freeze drying at the temperature of-10 ℃ to obtain the hypochlorite intercalation layered composite metal hydroxide.
The prepared layered composite metal hydroxide is used for purifying water containing arsenic and organic pollutants, and the content of the layered composite metal hydroxide is 0.5 mg.L-1The concentration of total arsenic of a pentavalent arsenic water sample after material adsorption treatment is less than 0.01 mg.L-1And the released hypochlorite can oxidize organic pollutants when the content of the hypochlorite is lower than the national drinking water standard limit.
Example 4
A hypochlorite intercalation layered composite metal hydroxide for synergistically removing composite pollution in water is prepared by the following steps:
(1) 100ml of a first solution containing 600 mmol. multidot.L of-1Mg of (2)2+、190mmol·L-1Fe (b) of3+And 10 mmol. L-1Ce of (1)3+And preparing 100ml of a second solution containing 1600 mmol.L-1NaOH and 400 mmol. multidot.L-1Na of (2)2CO3Separately preparing 100 mmol.L-1Sodium hypochlorite solution of (2).
(2) And (2) simultaneously dropwise adding the prepared first solution and second solution into a beaker containing 100ml of deionized water, violently stirring in the dropwise adding process, simultaneously controlling the pH value in the reaction process to be kept at 10.5, aging the slurry obtained by the reaction at 70 ℃ for 36 hours, then carrying out solid-liquid separation, washing the obtained solid precipitate with deionized water until the supernatant is neutral, then drying at 60 ℃, calcining at 500 ℃, and adding the obtained calcined product into a sodium hypochlorite solution for reaction.
(3) And after the reaction, centrifugally separating, washing the precipitate with deionized water, and drying at the temperature of minus 10 ℃ to obtain the hypochlorite intercalation layered composite metal hydroxide.
The prepared layered composite metal hydroxide is used for purifying water containing arsenic, trace organic pollutants and bacteria, and contains 1.0 mg.L-1The concentration of total arsenic of water sample of pentavalent arsenic, trace organic pollutant and bacteria after material adsorption treatment is less than 0.01 mg.L-1And when the content of the hypochlorite is lower than the national drinking water standard limit, the released hypochlorite can oxidize organic pollutants in water and kill bacteria.
Example 5
A hypochlorite intercalation layered composite metal hydroxide for synergistically removing composite pollution in water is prepared by the following steps:
(1) 100ml of a first solution containing 450 mmol. multidot.L-1Mg of (2)2+、142.5mmol·L-1Fe (b) of3+And 7.5 mmol. multidot.L-1Ce of (1)3+Separately, 100ml of a second solution containing 1200 mmol. L-1NaOH and 300 mmol. multidot.L-1Na of (2)2CO3Separately preparing 100 mmol.L-1Sodium hypochlorite solution of (2).
(2) And (2) simultaneously dropwise adding the prepared first solution and second solution into a beaker containing 100ml of deionized water, violently stirring in the dropwise adding process, simultaneously controlling the pH value in the reaction process to be kept at 9.5, aging the slurry obtained by the reaction at 80 ℃ for 24 hours, then carrying out solid-liquid separation, washing the obtained solid precipitate with deionized water until the supernatant is neutral, then drying at 60 ℃, calcining at 500 ℃, and adding the obtained calcined product into a sodium hypochlorite solution for reaction.
(3) And after the reaction, centrifugally separating, washing the precipitate with deionized water, and drying at the temperature of minus 10 ℃ to obtain the hypochlorite intercalation layered composite metal hydroxide.
The prepared layered composite metal hydroxide is used for purifying water containing arsenic, trace organic pollutants and bacteria, and contains 0.5 mg.L-1The concentration of total arsenic of water sample of pentavalent arsenic, trace organic pollutant and bacteria after material adsorption treatment is less than 0.01 mg.L-1Is lower than the limit value of the national drinking water standard,the released hypochlorite can oxidize organic pollutants in water and kill bacteria.
Example 6
A hypochlorite intercalation layered composite metal hydroxide for synergistically removing composite pollution in water is prepared by the following steps:
(1) 100ml of a first solution containing 100 mmol. L of-1Mg of (2)2+、285mmol·L-1Fe (b) of3+And 15 mmol. L-1Ce of (1)3+And preparing 100ml of a second solution containing 900 mmol.L-1NaOH and 900 mmol. multidot.L-1Na of (2)2CO3Separately preparing 100 mmol.L-1Sodium hypochlorite solution of (2).
(2) And (2) simultaneously dropwise adding the prepared first solution and second solution into a beaker containing 100ml of deionized water, violently stirring in the dropwise adding process, simultaneously controlling the pH value in the reaction process to be kept at 9, aging the slurry obtained by the reaction at 65 ℃ for 24 hours, then carrying out solid-liquid separation, washing the obtained solid precipitate with deionized water until the supernatant is neutral, then drying at 60 ℃, calcining at 500 ℃, and adding the obtained calcined product into a sodium hypochlorite solution for reaction.
(3) And after the reaction, centrifugally separating, washing the precipitate with deionized water, and drying at the temperature of minus 10 ℃ to obtain the hypochlorite intercalation layered composite metal hydroxide.
The prepared layered composite metal hydroxide is used for purifying water containing arsenic, trace organic pollutants and bacteria, and contains 0.8 mg.L-1The concentration of total arsenic of water sample of pentavalent arsenic, trace organic pollutant and bacteria after material adsorption treatment is less than 0.01 mg.L-1And when the content of the hypochlorite is lower than the national drinking water standard limit, the released hypochlorite can oxidize organic pollutants in water and kill bacteria.

Claims (7)

1. The preparation method of the hypochlorite intercalation layered composite metal hydroxide is characterized by comprising the following steps:
(1) mixing Mg2+Salt, Ce3+Salt andFe3+dissolving salt in deionized water according to a certain proportion to obtain a first solution; mixing NaOH and Na2CO3Mixing and dissolving in deionized water to obtain a second solution; dissolving hypochlorite in deionized water to obtain a third solution;
(2) mixing the first solution and the second solution as Mg2+、Ce3+、Fe3+The ratio of the sum of the amounts of substances of (a) to the amount of substance of NaOH in the second solution is 1: (2-4) mixing, stirring to obtain slurry, aging, performing solid-liquid separation, cleaning a solid precipitate to be neutral, drying, and calcining to obtain a calcined product, wherein the aging treatment temperature is 60-80 ℃, the aging time is 20-36 h, and the calcining temperature is 400-500 ℃;
(3) and adding the calcined product into the third solution, carrying out solid-liquid separation after reaction, and cleaning and drying the obtained solid at the drying temperature of-20 to-10 ℃ to obtain the hypochlorite intercalation layered composite metal hydroxide.
2. The method for preparing hypochlorite intercalation layered composite metal hydroxide according to claim 1, wherein said Mg2+The salt is nitrate or hydrochloride of magnesium, and the Fe3+The salt being a nitrate or hydrochloride salt of iron, said Ce3+The salt being Ce (NO)3)3·6H2O, in the first solution, Mg2+Has a concentration of 150 to 900 mmol.L-1，Mg2+With Fe3+And Ce3+The ratio of the total molar concentration is 3:1, Ce3+Is Fe3+And Ce3+0-5% of the total molar concentration.
3. The method for preparing hypochlorite intercalation layered composite metal hydroxide according to claim 1, wherein the concentration of NaOH in the second solution is 400-4800 mmol-L-1，Na2CO3The molar concentration ratio to NaOH was 0.25: 1.
4. The hypochlorite intercalated layered composite metal of claim 1The preparation method of the hydroxide is characterized in that the hypochlorite is NaClO, and ClO in the third solution-Has a concentration of 20 to 100 mmol.L-1。
5. The method for preparing hypochlorite intercalation layered composite metal hydroxide according to claim 1, wherein the pH of the solution is maintained to be 9-11 during the stirring in the step (2).
6. The use of the hypochlorite intercalation layered composite metal hydroxide obtained by the method according to any one of claims 1 to 5, wherein the hypochlorite intercalation layered composite metal hydroxide is used for adsorption removal of arsenic element in water or synergistic oxidative degradation of arsenic element and organic pollutants.
7. The use of the hypochlorite intercalated layered composite metal hydroxide according to claim 6, wherein the organic contaminants comprise drugs and personal care products, endocrine disruptors or persistent organic contaminants dissolved in water.
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CN1926989A (en) * 2006-09-05 2007-03-14 吉林大学 Hypochlorous acid inorganic laminated bimetal hydroxide intercalation sterilization composite material
CN1962046A (en) * 2006-10-20 2007-05-16 山东大学 A heavy metal ion absorbent and application thereof in removal of heavy metal ion
CN106179174A (en) * 2016-07-07 2016-12-07 同济大学 For layered composite metal hydroxides removing water pollutant and its preparation method and application

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